#============================================================================= # 1. SUBMISSION DETAILS _publ_contact_author_name 'Jian-Fang Ma' _publ_contact_author_address ; Department of Chemistry Northeast Normal University Changchun 130024 P.R.China ; _publ_contact_author_email majf247@yahoo.com _publ_contact_author_fax +86-431-85098620 _publ_contact_author_phone +86-431-85098620 _publ_requested_journal 'Crystal Growth & Design' #============================================================================= data_Compound-1 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C46 H56 Cd3 N4 O23, 6H2O' _chemical_formula_sum 'C46 H68 Cd3 N4 O29' _chemical_formula_weight 1478.24 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cd' 'Cd' -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' _symmetry_space_group_name_hall '-C 2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 24.6030(14) _cell_length_b 13.1890(5) _cell_length_c 20.2220(13) _cell_angle_alpha 90.00 _cell_angle_beta 124.366(9) _cell_angle_gamma 90.00 _cell_volume 5416.4(5) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 4822 _cell_measurement_theta_min 2.9577 _cell_measurement_theta_max 29.2198 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.813 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2992 _exptl_absorpt_coefficient_mu 1.265 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7511 _exptl_absorpt_correction_T_max 0.8232 _exptl_absorpt_process_details ; CrysAlis (Oxford Diffraction, 2006) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Diffraction Gemini R Ultra' _diffrn_measurement_method '\w scan' _diffrn_detector_area_resol_mean 10.0 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19771 _diffrn_reflns_av_R_equivalents 0.0494 _diffrn_reflns_av_sigmaI/netI 0.0653 _diffrn_reflns_limit_h_min -32 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 2.96 _diffrn_reflns_theta_max 29.28 _reflns_number_total 6447 _reflns_number_gt 4414 _reflns_threshold_expression >2\s(I) _computing_data_collection 'CrysAlisPro(1.171.35.21) (Agilent Tech., 2012)' _computing_cell_refinement 'CrysAlisPro(1.171.35.21) (Agilent Tech., 2012)' _computing_data_reduction 'CrysAlisPro(1.171.35.21) (Agilent Tech., 2012)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0583P)^2^+8.8797P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6447 _refine_ls_number_parameters 402 _refine_ls_number_restraints 24 _refine_ls_R_factor_all 0.0850 _refine_ls_R_factor_gt 0.0495 _refine_ls_wR_factor_ref 0.1319 _refine_ls_wR_factor_gt 0.1142 _refine_ls_goodness_of_fit_ref 1.054 _refine_ls_restrained_S_all 1.053 _refine_ls_shift/su_max 0.015 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cd1 Cd 1.0000 0.12192(4) 0.7500 0.03522(15) Uani 1 2 d S . . Cd2 Cd 0.688526(17) 0.65262(3) 0.43197(2) 0.03461(13) Uani 1 1 d . . . C1 C 0.8105(2) 0.2475(3) 0.6334(3) 0.0268(10) Uani 1 1 d . . . C2 C 0.7944(2) 0.3354(3) 0.5898(3) 0.0271(10) Uani 1 1 d . . . H2 H 0.8265 0.3699 0.5879 0.033 Uiso 1 1 calc R . . C3 C 0.7308(2) 0.3732(3) 0.5484(3) 0.0245(9) Uani 1 1 d . . . C4 C 0.6846(2) 0.3236(3) 0.5539(3) 0.0247(9) Uani 1 1 d . . . H4 H 0.6421 0.3494 0.5268 0.030 Uiso 1 1 calc R . . C5 C 0.6998(2) 0.2359(3) 0.5988(3) 0.0250(9) Uani 1 1 d . . . C6 C 0.7626(2) 0.1978(4) 0.6375(3) 0.0281(10) Uani 1 1 d . . . H6 H 0.7732 0.1380 0.6667 0.034 Uiso 1 1 calc R . . C7 C 0.8793(2) 0.2090(4) 0.6782(3) 0.0315(11) Uani 1 1 d . . . C8 C 0.7146(2) 0.4705(3) 0.5045(3) 0.0261(9) Uani 1 1 d . . . C9 C 0.6511(2) 0.1891(4) 0.6119(3) 0.0290(10) Uani 1 1 d . . . H9A H 0.6311 0.2430 0.6239 0.035 Uiso 1 1 calc R . . H9B H 0.6751 0.1461 0.6590 0.035 Uiso 1 1 calc R . . C10 C 0.6217(2) 0.0405(4) 0.5215(3) 0.0343(11) Uani 1 1 d . . . H10A H 0.6529 0.0656 0.5104 0.041 Uiso 1 1 calc R . . H10B H 0.5852 0.0098 0.4728 0.041 Uiso 1 1 calc R . . C11 C 0.6546(2) -0.0388(4) 0.5857(3) 0.0314(10) Uani 1 1 d . . . H11A H 0.6600 -0.1002 0.5635 0.038 Uiso 1 1 calc R . . H11B H 0.6981 -0.0152 0.6281 0.038 Uiso 1 1 calc R . . C12 C 0.5604(2) -0.1260(4) 0.5647(3) 0.0362(12) Uani 1 1 d . . . H12A H 0.5763 -0.1914 0.5606 0.043 Uiso 1 1 calc R . . H12B H 0.5364 -0.0952 0.5119 0.043 Uiso 1 1 calc R . . C13 C 0.5139(2) -0.1423(5) 0.5894(3) 0.0423(13) Uani 1 1 d . . . H13A H 0.5041 -0.0771 0.6027 0.051 Uiso 1 1 calc R . . H13B H 0.5357 -0.1835 0.6375 0.051 Uiso 1 1 calc R . . C14 C 0.4499(2) -0.1928(4) 0.5267(3) 0.0420(13) Uani 1 1 d . . . H14A H 0.4598 -0.2527 0.5075 0.050 Uiso 1 1 calc R . . H14B H 0.4280 -0.2151 0.5517 0.050 Uiso 1 1 calc R . . C15 C 0.6588(2) -0.1092(4) 0.6983(3) 0.0346(11) Uani 1 1 d . . . H15A H 0.6788 -0.1697 0.6936 0.042 Uiso 1 1 calc R . . H15B H 0.6320 -0.1296 0.7173 0.042 Uiso 1 1 calc R . . C16 C 0.7117(2) -0.0392(4) 0.7580(3) 0.0293(10) Uani 1 1 d . . . C17 C 0.6966(2) 0.0421(4) 0.7887(3) 0.0304(10) Uani 1 1 d . . . H17 H 0.6533 0.0526 0.7722 0.036 Uiso 1 1 calc R . . C18 C 0.7454(2) 0.1074(4) 0.8435(3) 0.0315(10) Uani 1 1 d . . . C19 C 0.8098(2) 0.0921(4) 0.8672(3) 0.0314(10) Uani 1 1 d . . . H19 H 0.8427 0.1361 0.9038 0.038 Uiso 1 1 calc R . . C20 C 0.8252(2) 0.0132(4) 0.8372(3) 0.0290(10) Uani 1 1 d . . . C21 C 0.7768(2) -0.0529(4) 0.7840(3) 0.0294(10) Uani 1 1 d . . . H21 H 0.7879 -0.1078 0.7650 0.035 Uiso 1 1 calc R . . C22 C 0.7287(3) 0.1926(4) 0.8777(4) 0.0443(13) Uani 1 1 d . . . C23 C 0.8946(2) -0.0039(4) 0.8622(3) 0.0377(12) Uani 1 1 d . . . N1 N 0.59674(17) 0.1269(3) 0.5439(2) 0.0286(8) Uani 1 1 d . . . N2 N 0.61674(17) -0.0621(3) 0.6196(2) 0.0278(8) Uani 1 1 d . . . O1 O 0.92326(16) 0.2634(3) 0.6851(3) 0.0569(11) Uani 1 1 d . . . O2 O 0.89190(16) 0.1220(3) 0.7077(2) 0.0418(9) Uani 1 1 d . . . O1W O 0.96809(16) 0.0911(3) 0.6208(2) 0.0470(9) Uani 1 1 d . . . O3 O 0.65650(14) 0.5010(3) 0.46495(19) 0.0326(7) Uani 1 1 d . . . O2W O 1.014(3) -0.068(4) 0.743(4) 0.133(19) Uani 0.25 1 d PU . . O2W' O 0.9858(9) -0.0620(15) 0.7587(13) 0.024(4) Uani 0.25 1 d PU . . O4 O 0.76011(15) 0.5207(3) 0.5091(2) 0.0360(8) Uani 1 1 d . . . O3W O 0.6677(2) 0.5579(3) 0.3267(3) 0.0646(12) Uani 1 1 d . . . O5 O 0.7710(2) 0.2321(3) 0.9424(2) 0.0457(9) Uani 1 1 d . . . O4W O 0.58371(19) 0.6996(4) 0.3835(3) 0.0619(11) Uani 1 1 d . . . O6 O 0.6701(2) 0.2207(4) 0.8380(3) 0.0804(15) Uani 1 1 d . . . O5W O 1.02475(19) -0.1515(3) 0.9546(2) 0.0541(10) Uani 1 1 d . . . O7 O 0.93707(17) 0.0605(4) 0.9069(2) 0.0558(11) Uani 1 1 d . . . H7 H 0.9729 0.0434 0.9165 0.084 Uiso 1 1 calc R . . O6W O 0.5401(3) 0.1508(6) 0.6391(5) 0.128(3) Uani 1 1 d . . . O8 O 0.90659(17) -0.0797(3) 0.8361(2) 0.0539(11) Uani 1 1 d . . . O7W O 0.5980(4) 0.0810(7) 0.8757(5) 0.061(2) Uani 0.50 1 d P . . O8W O 0.9861(19) 0.4599(16) 0.7321(15) 0.112(10) Uani 0.35 1 d PU . . O8W' O 0.9696(16) 0.467(2) 0.749(2) 0.042(7) Uani 0.15 1 d PU . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cd1 0.0218(2) 0.0356(3) 0.0402(3) 0.000 0.0127(2) 0.000 Cd2 0.0390(2) 0.0254(2) 0.0380(2) 0.00301(16) 0.02091(18) -0.00519(14) C1 0.027(2) 0.019(2) 0.028(2) -0.0019(19) 0.012(2) -0.0004(17) C2 0.025(2) 0.028(3) 0.030(2) -0.006(2) 0.016(2) -0.0049(18) C3 0.024(2) 0.026(2) 0.025(2) -0.0025(18) 0.0151(19) -0.0001(17) C4 0.021(2) 0.025(2) 0.026(2) -0.0008(18) 0.0112(19) -0.0017(17) C5 0.023(2) 0.024(2) 0.023(2) 0.0003(18) 0.0098(19) -0.0045(17) C6 0.027(2) 0.021(2) 0.024(2) 0.0017(19) 0.008(2) -0.0012(18) C7 0.025(2) 0.031(3) 0.035(3) -0.004(2) 0.014(2) 0.0020(19) C8 0.035(2) 0.019(2) 0.027(2) -0.0021(18) 0.020(2) -0.0014(18) C9 0.028(2) 0.026(3) 0.028(2) -0.001(2) 0.013(2) -0.0072(19) C10 0.033(2) 0.038(3) 0.031(3) -0.006(2) 0.018(2) -0.011(2) C11 0.027(2) 0.030(3) 0.039(3) -0.004(2) 0.020(2) -0.0022(19) C12 0.028(2) 0.035(3) 0.039(3) -0.003(2) 0.015(2) -0.007(2) C13 0.028(2) 0.053(4) 0.029(3) 0.010(2) 0.006(2) -0.008(2) C14 0.025(2) 0.044(3) 0.042(3) 0.017(3) 0.010(2) -0.005(2) C15 0.031(2) 0.025(3) 0.038(3) 0.004(2) 0.014(2) -0.0004(19) C16 0.032(2) 0.026(3) 0.030(2) 0.003(2) 0.017(2) -0.0018(19) C17 0.030(2) 0.033(3) 0.032(3) 0.005(2) 0.019(2) 0.0056(19) C18 0.041(3) 0.023(3) 0.035(3) -0.001(2) 0.024(2) 0.003(2) C19 0.034(2) 0.026(3) 0.027(2) -0.003(2) 0.013(2) -0.0042(19) C20 0.028(2) 0.031(3) 0.026(2) 0.000(2) 0.014(2) -0.0007(19) C21 0.032(2) 0.027(3) 0.029(2) 0.000(2) 0.017(2) 0.0061(19) C22 0.059(3) 0.029(3) 0.058(4) 0.003(3) 0.041(3) 0.008(3) C23 0.028(2) 0.053(4) 0.026(3) 0.002(2) 0.012(2) 0.003(2) N1 0.0229(18) 0.030(2) 0.028(2) 0.0035(17) 0.0117(17) -0.0043(15) N2 0.0252(18) 0.023(2) 0.031(2) 0.0015(17) 0.0127(17) -0.0043(15) O1 0.0281(18) 0.040(2) 0.092(3) 0.010(2) 0.027(2) 0.0012(16) O2 0.0270(16) 0.039(2) 0.050(2) 0.0100(18) 0.0161(17) 0.0069(15) O1W 0.0339(18) 0.058(3) 0.043(2) -0.0054(19) 0.0186(18) -0.0038(17) O3 0.0262(16) 0.0300(19) 0.0370(19) 0.0072(15) 0.0151(15) 0.0026(13) O2W 0.14(2) 0.12(2) 0.13(2) -0.003(10) 0.070(12) 0.000(9) O2W' 0.017(7) 0.013(6) 0.022(7) 0.001(5) 0.000(5) 0.004(4) O4 0.0369(18) 0.027(2) 0.049(2) 0.0066(16) 0.0267(17) -0.0022(14) O3W 0.104(3) 0.046(3) 0.060(3) -0.010(2) 0.057(3) -0.019(2) O5 0.075(3) 0.026(2) 0.045(2) -0.0071(17) 0.039(2) -0.0021(18) O4W 0.054(2) 0.060(3) 0.069(3) 0.017(2) 0.033(2) 0.013(2) O6 0.064(3) 0.061(3) 0.104(4) -0.026(3) 0.041(3) 0.017(2) O5W 0.047(2) 0.058(3) 0.053(2) 0.003(2) 0.026(2) 0.0114(18) O7 0.0293(18) 0.082(3) 0.052(2) -0.021(2) 0.0202(19) -0.0115(19) O6W 0.115(5) 0.145(7) 0.180(7) 0.055(5) 0.117(5) 0.052(4) O8 0.0335(19) 0.060(3) 0.060(3) -0.012(2) 0.0212(19) 0.0123(18) O7W 0.070(5) 0.060(6) 0.066(5) 0.027(5) 0.046(5) -0.003(4) O8W 0.117(14) 0.101(11) 0.107(14) -0.001(8) 0.057(10) -0.008(9) O8W' 0.043(11) 0.040(11) 0.058(11) 0.004(8) 0.038(9) -0.004(8) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cd1 O2 2.289(3) . ? Cd1 O2 2.289(3) 2_756 ? Cd1 O1W 2.300(4) 2_756 ? Cd1 O1W 2.300(4) . ? Cd1 O1 2.444(4) 2_756 ? Cd1 O1 2.444(4) . ? Cd1 O2W' 2.47(2) 2_756 ? Cd1 O2W' 2.47(2) . ? Cd1 O2W 2.55(5) 2_756 ? Cd1 O2W 2.55(5) . ? Cd1 C7 2.715(4) 2_756 ? Cd1 C7 2.715(4) . ? Cd2 O3W 2.263(4) . ? Cd2 O4W 2.268(4) . ? Cd2 O4 2.337(3) . ? Cd2 O6 2.373(5) 6_565 ? Cd2 O3 2.378(3) . ? Cd2 O5 2.385(4) 4_656 ? Cd2 O5 2.448(4) 6_565 ? Cd2 C8 2.696(4) . ? Cd2 C22 2.752(5) 6_565 ? C1 C2 1.373(6) . ? C1 C6 1.392(6) . ? C1 C7 1.488(6) . ? C2 C3 1.385(6) . ? C2 H2 0.9300 . ? C3 C4 1.369(6) . ? C3 C8 1.482(6) . ? C4 C5 1.385(6) . ? C4 H4 0.9300 . ? C5 C6 1.375(6) . ? C5 C9 1.497(6) . ? C6 H6 0.9300 . ? C7 O1 1.238(6) . ? C7 O2 1.248(6) . ? C8 O3 1.247(5) . ? C8 O4 1.258(5) . ? C9 N1 1.509(6) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 N1 1.482(6) . ? C10 C11 1.500(7) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 N2 1.467(5) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 N2 1.458(6) . ? C12 C13 1.501(7) . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C13 C14 1.509(7) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 N1 1.505(6) 5_656 ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 N2 1.460(6) . ? C15 C16 1.494(7) . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 C21 1.386(6) . ? C16 C17 1.391(7) . ? C17 C18 1.381(7) . ? C17 H17 0.9300 . ? C18 C19 1.386(6) . ? C18 C22 1.494(7) . ? C19 C20 1.361(7) . ? C19 H19 0.9300 . ? C20 C21 1.375(6) . ? C20 C23 1.500(6) . ? C21 H21 0.9300 . ? C22 O5 1.236(7) . ? C22 O6 1.247(7) . ? C22 Cd2 2.752(5) 6_566 ? C23 O8 1.241(6) . ? C23 O7 1.250(6) . ? N1 C14 1.505(6) 5_656 ? O2W O2W' 0.09(7) 2_756 ? O2W O2W 0.88(12) 2_756 ? O2W O2W' 0.91(4) . ? O2W' O2W 0.09(7) 2_756 ? O2W' O2W' 0.94(5) 2_756 ? O5 Cd2 2.385(4) 4_646 ? O5 Cd2 2.448(4) 6_566 ? O6 Cd2 2.373(5) 6_566 ? O7 H7 0.8200 . ? O8W O8W 0.66(6) 2_756 ? O8W O8W' 0.67(5) . ? O8W O8W' 0.93(4) 2_756 ? O8W' O8W 0.93(4) 2_756 ? O8W' O8W' 1.48(6) 2_756 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Cd1 O2 179.92(19) . 2_756 ? O2 Cd1 O1W 90.22(12) . 2_756 ? O2 Cd1 O1W 89.79(13) 2_756 2_756 ? O2 Cd1 O1W 89.79(13) . . ? O2 Cd1 O1W 90.22(12) 2_756 . ? O1W Cd1 O1W 159.6(2) 2_756 . ? O2 Cd1 O1 125.64(13) . 2_756 ? O2 Cd1 O1 54.29(12) 2_756 2_756 ? O1W Cd1 O1 81.97(15) 2_756 2_756 ? O1W Cd1 O1 114.20(15) . 2_756 ? O2 Cd1 O1 54.29(12) . . ? O2 Cd1 O1 125.64(13) 2_756 . ? O1W Cd1 O1 114.20(14) 2_756 . ? O1W Cd1 O1 81.97(15) . . ? O1 Cd1 O1 80.42(18) 2_756 . ? O2 Cd1 O2W' 98.9(4) . 2_756 ? O2 Cd1 O2W' 81.2(4) 2_756 2_756 ? O1W Cd1 O2W' 86.3(5) 2_756 2_756 ? O1W Cd1 O2W' 73.5(5) . 2_756 ? O1 Cd1 O2W' 133.7(4) 2_756 2_756 ? O1 Cd1 O2W' 144.0(4) . 2_756 ? O2 Cd1 O2W' 81.2(4) . . ? O2 Cd1 O2W' 98.9(4) 2_756 . ? O1W Cd1 O2W' 73.5(5) 2_756 . ? O1W Cd1 O2W' 86.3(5) . . ? O1 Cd1 O2W' 144.0(4) 2_756 . ? O1 Cd1 O2W' 133.7(4) . . ? O2W' Cd1 O2W' 22.0(10) 2_756 . ? O2 Cd1 O2W 81.7(13) . 2_756 ? O2 Cd1 O2W 98.4(13) 2_756 2_756 ? O1W Cd1 O2W 74.6(15) 2_756 2_756 ? O1W Cd1 O2W 85.2(15) . 2_756 ? O1 Cd1 O2W 144.2(14) 2_756 2_756 ? O1 Cd1 O2W 133.9(14) . 2_756 ? O2W' Cd1 O2W 20.9(9) 2_756 2_756 ? O2W' Cd1 O2W 1.2(19) . 2_756 ? O2 Cd1 O2W 98.4(13) . . ? O2 Cd1 O2W 81.7(13) 2_756 . ? O1W Cd1 O2W 85.2(15) 2_756 . ? O1W Cd1 O2W 74.6(15) . . ? O1 Cd1 O2W 133.9(14) 2_756 . ? O1 Cd1 O2W 144.2(15) . . ? O2W' Cd1 O2W 1.2(19) 2_756 . ? O2W' Cd1 O2W 20.9(9) . . ? O2W Cd1 O2W 20(3) 2_756 . ? O2 Cd1 C7 152.71(15) . 2_756 ? O2 Cd1 C7 27.22(13) 2_756 2_756 ? O1W Cd1 C7 84.18(13) 2_756 2_756 ? O1W Cd1 C7 104.54(13) . 2_756 ? O1 Cd1 C7 27.12(13) 2_756 2_756 ? O1 Cd1 C7 104.13(14) . 2_756 ? O2W' Cd1 C7 107.3(4) 2_756 2_756 ? O2W' Cd1 C7 122.2(4) . 2_756 ? O2W Cd1 C7 122.0(13) 2_756 2_756 ? O2W Cd1 C7 107.7(13) . 2_756 ? O2 Cd1 C7 27.22(13) . . ? O2 Cd1 C7 152.71(15) 2_756 . ? O1W Cd1 C7 104.54(13) 2_756 . ? O1W Cd1 C7 84.18(13) . . ? O1 Cd1 C7 104.13(14) 2_756 . ? O1 Cd1 C7 27.12(13) . . ? O2W' Cd1 C7 122.2(4) 2_756 . ? O2W' Cd1 C7 107.3(4) . . ? O2W Cd1 C7 107.7(13) 2_756 . ? O2W Cd1 C7 122.0(13) . . ? C7 Cd1 C7 130.0(2) 2_756 . ? O3W Cd2 O4W 98.39(17) . . ? O3W Cd2 O4 84.40(15) . . ? O4W Cd2 O4 137.46(13) . . ? O3W Cd2 O6 78.25(19) . 6_565 ? O4W Cd2 O6 78.74(16) . 6_565 ? O4 Cd2 O6 142.18(14) . 6_565 ? O3W Cd2 O3 82.21(13) . . ? O4W Cd2 O3 82.83(14) . . ? O4 Cd2 O3 55.32(10) . . ? O6 Cd2 O3 150.73(14) 6_565 . ? O3W Cd2 O5 168.84(16) . 4_656 ? O4W Cd2 O5 91.68(15) . 4_656 ? O4 Cd2 O5 84.93(13) . 4_656 ? O6 Cd2 O5 108.64(16) 6_565 4_656 ? O3 Cd2 O5 94.36(12) . 4_656 ? O3W Cd2 O5 99.25(14) . 6_565 ? O4W Cd2 O5 123.55(15) . 6_565 ? O4 Cd2 O5 97.42(12) . 6_565 ? O6 Cd2 O5 53.58(14) 6_565 6_565 ? O3 Cd2 O5 152.60(12) . 6_565 ? O5 Cd2 O5 78.92(12) 4_656 6_565 ? O3W Cd2 C8 82.96(14) . . ? O4W Cd2 C8 110.01(15) . . ? O4 Cd2 C8 27.78(12) . . ? O6 Cd2 C8 160.33(17) 6_565 . ? O3 Cd2 C8 27.55(11) . . ? O5 Cd2 C8 89.10(13) 4_656 . ? O5 Cd2 C8 125.12(13) 6_565 . ? O3W Cd2 C22 88.65(16) . 6_565 ? O4W Cd2 C22 101.64(17) . 6_565 ? O4 Cd2 C22 120.89(14) . 6_565 ? O6 Cd2 C22 26.89(16) 6_565 6_565 ? O3 Cd2 C22 170.35(14) . 6_565 ? O5 Cd2 C22 94.05(15) 4_656 6_565 ? O5 Cd2 C22 26.69(14) 6_565 6_565 ? C8 Cd2 C22 148.08(15) . 6_565 ? C2 C1 C6 119.3(4) . . ? C2 C1 C7 119.7(4) . . ? C6 C1 C7 120.9(4) . . ? C1 C2 C3 120.6(4) . . ? C1 C2 H2 119.7 . . ? C3 C2 H2 119.7 . . ? C4 C3 C2 119.1(4) . . ? C4 C3 C8 120.5(4) . . ? C2 C3 C8 120.2(4) . . ? C3 C4 C5 121.6(4) . . ? C3 C4 H4 119.2 . . ? C5 C4 H4 119.2 . . ? C6 C5 C4 118.5(4) . . ? C6 C5 C9 120.2(4) . . ? C4 C5 C9 121.0(4) . . ? C5 C6 C1 120.8(4) . . ? C5 C6 H6 119.6 . . ? C1 C6 H6 119.6 . . ? O1 C7 O2 120.9(4) . . ? O1 C7 C1 119.4(5) . . ? O2 C7 C1 119.6(4) . . ? O1 C7 Cd1 64.1(2) . . ? O2 C7 Cd1 57.0(2) . . ? C1 C7 Cd1 174.2(3) . . ? O3 C8 O4 121.9(4) . . ? O3 C8 C3 119.2(4) . . ? O4 C8 C3 119.0(4) . . ? O3 C8 Cd2 61.9(2) . . ? O4 C8 Cd2 60.0(2) . . ? C3 C8 Cd2 177.0(3) . . ? C5 C9 N1 116.7(4) . . ? C5 C9 H9A 108.1 . . ? N1 C9 H9A 108.1 . . ? C5 C9 H9B 108.1 . . ? N1 C9 H9B 108.1 . . ? H9A C9 H9B 107.3 . . ? N1 C10 C11 112.7(4) . . ? N1 C10 H10A 109.1 . . ? C11 C10 H10A 109.1 . . ? N1 C10 H10B 109.1 . . ? C11 C10 H10B 109.1 . . ? H10A C10 H10B 107.8 . . ? N2 C11 C10 112.0(4) . . ? N2 C11 H11A 109.2 . . ? C10 C11 H11A 109.2 . . ? N2 C11 H11B 109.2 . . ? C10 C11 H11B 109.2 . . ? H11A C11 H11B 107.9 . . ? N2 C12 C13 113.9(4) . . ? N2 C12 H12A 108.8 . . ? C13 C12 H12A 108.8 . . ? N2 C12 H12B 108.8 . . ? C13 C12 H12B 108.8 . . ? H12A C12 H12B 107.7 . . ? C12 C13 C14 114.4(5) . . ? C12 C13 H13A 108.7 . . ? C14 C13 H13A 108.7 . . ? C12 C13 H13B 108.7 . . ? C14 C13 H13B 108.7 . . ? H13A C13 H13B 107.6 . . ? N1 C14 C13 114.7(4) 5_656 . ? N1 C14 H14A 108.6 5_656 . ? C13 C14 H14A 108.6 . . ? N1 C14 H14B 108.6 5_656 . ? C13 C14 H14B 108.6 . . ? H14A C14 H14B 107.6 . . ? N2 C15 C16 112.1(4) . . ? N2 C15 H15A 109.2 . . ? C16 C15 H15A 109.2 . . ? N2 C15 H15B 109.2 . . ? C16 C15 H15B 109.2 . . ? H15A C15 H15B 107.9 . . ? C21 C16 C17 118.3(4) . . ? C21 C16 C15 121.3(4) . . ? C17 C16 C15 120.4(4) . . ? C18 C17 C16 120.5(4) . . ? C18 C17 H17 119.7 . . ? C16 C17 H17 119.7 . . ? C17 C18 C19 119.5(4) . . ? C17 C18 C22 119.9(4) . . ? C19 C18 C22 120.5(5) . . ? C20 C19 C18 120.6(4) . . ? C20 C19 H19 119.7 . . ? C18 C19 H19 119.7 . . ? C19 C20 C21 119.8(4) . . ? C19 C20 C23 121.1(4) . . ? C21 C20 C23 119.1(4) . . ? C20 C21 C16 121.2(4) . . ? C20 C21 H21 119.4 . . ? C16 C21 H21 119.4 . . ? O5 C22 O6 122.2(5) . . ? O5 C22 C18 121.3(5) . . ? O6 C22 C18 116.5(5) . . ? O5 C22 Cd2 62.8(3) . 6_566 ? O6 C22 Cd2 59.4(3) . 6_566 ? C18 C22 Cd2 175.8(4) . 6_566 ? O8 C23 O7 123.5(5) . . ? O8 C23 C20 118.5(5) . . ? O7 C23 C20 118.0(5) . . ? C10 N1 C14 112.3(4) . 5_656 ? C10 N1 C9 112.9(3) . . ? C14 N1 C9 111.1(4) 5_656 . ? C12 N2 C15 111.6(4) . . ? C12 N2 C11 110.3(4) . . ? C15 N2 C11 110.6(3) . . ? C7 O1 Cd1 88.7(3) . . ? C7 O2 Cd1 95.8(3) . . ? C8 O3 Cd2 90.5(3) . . ? O2W' O2W O2W 109(10) 2_756 2_756 ? O2W' O2W O2W' 105(10) 2_756 . ? O2W O2W O2W' 6(4) 2_756 . ? O2W' O2W Cd1 35(10) 2_756 . ? O2W O2W Cd1 80.1(13) 2_756 . ? O2W' O2W Cd1 75(4) . . ? O2W O2W' O2W 65(10) 2_756 . ? O2W O2W' O2W' 70(10) 2_756 2_756 ? O2W O2W' O2W' 5(4) . 2_756 ? O2W O2W' Cd1 144(10) 2_756 . ? O2W O2W' Cd1 84(4) . . ? O2W' O2W' Cd1 79.0(5) 2_756 . ? C8 O4 Cd2 92.2(3) . . ? C22 O5 Cd2 122.5(4) . 4_646 ? C22 O5 Cd2 90.5(3) . 6_566 ? Cd2 O5 Cd2 101.08(12) 4_646 6_566 ? C22 O6 Cd2 93.7(4) . 6_566 ? C23 O7 H7 109.5 . . ? O8W O8W O8W' 89(7) 2_756 . ? O8W O8W O8W' 46(6) 2_756 2_756 ? O8W' O8W O8W' 133(4) . 2_756 ? O8W O8W' O8W 45(4) . 2_756 ? O8W O8W' O8W' 27(3) . 2_756 ? O8W O8W' O8W' 19(2) 2_756 2_756 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C6 C1 C2 C3 -1.5(7) . . . . ? C7 C1 C2 C3 -179.2(4) . . . . ? C1 C2 C3 C4 2.2(7) . . . . ? C1 C2 C3 C8 177.2(4) . . . . ? C2 C3 C4 C5 -0.9(7) . . . . ? C8 C3 C4 C5 -175.9(4) . . . . ? C3 C4 C5 C6 -1.0(7) . . . . ? C3 C4 C5 C9 172.9(4) . . . . ? C4 C5 C6 C1 1.7(7) . . . . ? C9 C5 C6 C1 -172.3(4) . . . . ? C2 C1 C6 C5 -0.5(7) . . . . ? C7 C1 C6 C5 177.2(4) . . . . ? C2 C1 C7 O1 10.2(7) . . . . ? C6 C1 C7 O1 -167.4(5) . . . . ? C2 C1 C7 O2 -169.1(4) . . . . ? C6 C1 C7 O2 13.2(7) . . . . ? C2 C1 C7 Cd1 -116(3) . . . . ? C6 C1 C7 Cd1 66(4) . . . . ? O2 Cd1 C7 O1 175.3(5) . . . . ? O2 Cd1 C7 O1 -4.6(5) 2_756 . . . ? O1W Cd1 C7 O1 115.0(3) 2_756 . . . ? O1W Cd1 C7 O1 -83.7(3) . . . . ? O1 Cd1 C7 O1 29.8(4) 2_756 . . . ? O2W' Cd1 C7 O1 -150.1(7) 2_756 . . . ? O2W' Cd1 C7 O1 -168.0(6) . . . . ? O2W Cd1 C7 O1 -166.8(16) 2_756 . . . ? O2W Cd1 C7 O1 -151.6(18) . . . . ? C7 Cd1 C7 O1 20.4(3) 2_756 . . . ? O2 Cd1 C7 O2 -179.93(16) 2_756 . . . ? O1W Cd1 C7 O2 -60.3(3) 2_756 . . . ? O1W Cd1 C7 O2 101.0(3) . . . . ? O1 Cd1 C7 O2 -145.5(3) 2_756 . . . ? O1 Cd1 C7 O2 -175.3(5) . . . . ? O2W' Cd1 C7 O2 34.6(7) 2_756 . . . ? O2W' Cd1 C7 O2 16.7(6) . . . . ? O2W Cd1 C7 O2 17.9(16) 2_756 . . . ? O2W Cd1 C7 O2 33.1(18) . . . . ? C7 Cd1 C7 O2 -154.9(3) 2_756 . . . ? O2 Cd1 C7 C1 -56(3) . . . . ? O2 Cd1 C7 C1 124(3) 2_756 . . . ? O1W Cd1 C7 C1 -116(3) 2_756 . . . ? O1W Cd1 C7 C1 45(3) . . . . ? O1 Cd1 C7 C1 158(3) 2_756 . . . ? O1 Cd1 C7 C1 129(4) . . . . ? O2W' Cd1 C7 C1 -22(4) 2_756 . . . ? O2W' Cd1 C7 C1 -39(4) . . . . ? O2W Cd1 C7 C1 -38(4) 2_756 . . . ? O2W Cd1 C7 C1 -23(4) . . . . ? C7 Cd1 C7 C1 149(3) 2_756 . . . ? C4 C3 C8 O3 -8.0(6) . . . . ? C2 C3 C8 O3 177.1(4) . . . . ? C4 C3 C8 O4 170.9(4) . . . . ? C2 C3 C8 O4 -4.1(6) . . . . ? C4 C3 C8 Cd2 102(6) . . . . ? C2 C3 C8 Cd2 -73(6) . . . . ? O3W Cd2 C8 O3 -86.6(3) . . . . ? O4W Cd2 C8 O3 9.8(3) . . . . ? O4 Cd2 C8 O3 -178.0(4) . . . . ? O6 Cd2 C8 O3 -103.9(5) 6_565 . . . ? O5 Cd2 C8 O3 101.2(3) 4_656 . . . ? O5 Cd2 C8 O3 177.0(2) 6_565 . . . ? C22 Cd2 C8 O3 -162.6(3) 6_565 . . . ? O3W Cd2 C8 O4 91.3(3) . . . . ? O4W Cd2 C8 O4 -172.3(3) . . . . ? O6 Cd2 C8 O4 74.1(5) 6_565 . . . ? O3 Cd2 C8 O4 178.0(4) . . . . ? O5 Cd2 C8 O4 -80.8(3) 4_656 . . . ? O5 Cd2 C8 O4 -5.1(3) 6_565 . . . ? C22 Cd2 C8 O4 15.4(4) 6_565 . . . ? O3W Cd2 C8 C3 162(6) . . . . ? O4W Cd2 C8 C3 -102(6) . . . . ? O4 Cd2 C8 C3 71(6) . . . . ? O6 Cd2 C8 C3 145(5) 6_565 . . . ? O3 Cd2 C8 C3 -111(6) . . . . ? O5 Cd2 C8 C3 -10(6) 4_656 . . . ? O5 Cd2 C8 C3 66(6) 6_565 . . . ? C22 Cd2 C8 C3 86(6) 6_565 . . . ? C6 C5 C9 N1 -107.2(5) . . . . ? C4 C5 C9 N1 79.0(6) . . . . ? N1 C10 C11 N2 44.6(5) . . . . ? N2 C12 C13 C14 170.1(4) . . . . ? C12 C13 C14 N1 -72.0(6) . . . 5_656 ? N2 C15 C16 C21 -106.8(5) . . . . ? N2 C15 C16 C17 72.9(6) . . . . ? C21 C16 C17 C18 0.1(7) . . . . ? C15 C16 C17 C18 -179.5(4) . . . . ? C16 C17 C18 C19 0.8(7) . . . . ? C16 C17 C18 C22 -178.2(5) . . . . ? C17 C18 C19 C20 -0.3(7) . . . . ? C22 C18 C19 C20 178.7(5) . . . . ? C18 C19 C20 C21 -1.0(7) . . . . ? C18 C19 C20 C23 179.8(4) . . . . ? C19 C20 C21 C16 2.0(7) . . . . ? C23 C20 C21 C16 -178.9(4) . . . . ? C17 C16 C21 C20 -1.5(7) . . . . ? C15 C16 C21 C20 178.1(4) . . . . ? C17 C18 C22 O5 157.3(5) . . . . ? C19 C18 C22 O5 -21.7(8) . . . . ? C17 C18 C22 O6 -22.0(8) . . . . ? C19 C18 C22 O6 159.0(5) . . . . ? C17 C18 C22 Cd2 -15(6) . . . 6_566 ? C19 C18 C22 Cd2 166(5) . . . 6_566 ? C19 C20 C23 O8 176.5(5) . . . . ? C21 C20 C23 O8 -2.6(7) . . . . ? C19 C20 C23 O7 -5.0(7) . . . . ? C21 C20 C23 O7 175.8(5) . . . . ? C11 C10 N1 C14 -166.1(4) . . . 5_656 ? C11 C10 N1 C9 67.3(5) . . . . ? C5 C9 N1 C10 59.1(5) . . . . ? C5 C9 N1 C14 -68.1(5) . . . 5_656 ? C13 C12 N2 C15 64.2(5) . . . . ? C13 C12 N2 C11 -172.3(4) . . . . ? C16 C15 N2 C12 -172.6(4) . . . . ? C16 C15 N2 C11 64.1(5) . . . . ? C10 C11 N2 C12 76.5(5) . . . . ? C10 C11 N2 C15 -159.5(4) . . . . ? O2 C7 O1 Cd1 4.6(5) . . . . ? C1 C7 O1 Cd1 -174.8(4) . . . . ? O2 Cd1 O1 C7 -2.6(3) . . . . ? O2 Cd1 O1 C7 177.4(3) 2_756 . . . ? O1W Cd1 O1 C7 -74.1(3) 2_756 . . . ? O1W Cd1 O1 C7 92.9(3) . . . . ? O1 Cd1 O1 C7 -150.7(4) 2_756 . . . ? O2W' Cd1 O1 C7 45.8(10) 2_756 . . . ? O2W' Cd1 O1 C7 15.9(8) . . . . ? O2W Cd1 O1 C7 18(2) 2_756 . . . ? O2W Cd1 O1 C7 44(2) . . . . ? C7 Cd1 O1 C7 -164.0(2) 2_756 . . . ? O1 C7 O2 Cd1 -4.9(5) . . . . ? C1 C7 O2 Cd1 174.4(4) . . . . ? O2 Cd1 O2 C7 23(100) 2_756 . . . ? O1W Cd1 O2 C7 122.8(3) 2_756 . . . ? O1W Cd1 O2 C7 -77.6(3) . . . . ? O1 Cd1 O2 C7 42.5(4) 2_756 . . . ? O1 Cd1 O2 C7 2.6(3) . . . . ? O2W' Cd1 O2 C7 -150.9(6) 2_756 . . . ? O2W' Cd1 O2 C7 -163.9(6) . . . . ? O2W Cd1 O2 C7 -162.8(16) 2_756 . . . ? O2W Cd1 O2 C7 -152.1(16) . . . . ? C7 Cd1 O2 C7 45.1(6) 2_756 . . . ? O4 C8 O3 Cd2 -2.1(4) . . . . ? C3 C8 O3 Cd2 176.8(4) . . . . ? O3W Cd2 O3 C8 89.7(3) . . . . ? O4W Cd2 O3 C8 -170.8(3) . . . . ? O4 Cd2 O3 C8 1.2(2) . . . . ? O6 Cd2 O3 C8 138.1(4) 6_565 . . . ? O5 Cd2 O3 C8 -79.6(3) 4_656 . . . ? O5 Cd2 O3 C8 -5.4(4) 6_565 . . . ? C22 Cd2 O3 C8 71.0(9) 6_565 . . . ? O2 Cd1 O2W O2W' 114(85) . . . 2_756 ? O2 Cd1 O2W O2W' -66(85) 2_756 . . 2_756 ? O1W Cd1 O2W O2W' -157(85) 2_756 . . 2_756 ? O1W Cd1 O2W O2W' 26(84) . . . 2_756 ? O1 Cd1 O2W O2W' -83(85) 2_756 . . 2_756 ? O1 Cd1 O2W O2W' 77(85) . . . 2_756 ? O2W' Cd1 O2W O2W' 149(87) . . . 2_756 ? O2W Cd1 O2W O2W' 147(92) 2_756 . . 2_756 ? C7 Cd1 O2W O2W' -74(85) 2_756 . . 2_756 ? C7 Cd1 O2W O2W' 99(84) . . . 2_756 ? O2 Cd1 O2W O2W -33(9) . . . 2_756 ? O2 Cd1 O2W O2W 147(9) 2_756 . . 2_756 ? O1W Cd1 O2W O2W 57(9) 2_756 . . 2_756 ? O1W Cd1 O2W O2W -120(9) . . . 2_756 ? O1 Cd1 O2W O2W 131(8) 2_756 . . 2_756 ? O1 Cd1 O2W O2W -69(10) . . . 2_756 ? O2W' Cd1 O2W O2W -147(92) 2_756 . . 2_756 ? O2W' Cd1 O2W O2W 2(6) . . . 2_756 ? C7 Cd1 O2W O2W 139(8) 2_756 . . 2_756 ? C7 Cd1 O2W O2W -47(9) . . . 2_756 ? O2 Cd1 O2W O2W' -35(3) . . . . ? O2 Cd1 O2W O2W' 145(3) 2_756 . . . ? O1W Cd1 O2W O2W' 55(3) 2_756 . . . ? O1W Cd1 O2W O2W' -122(3) . . . . ? O1 Cd1 O2W O2W' 129(2) 2_756 . . . ? O1 Cd1 O2W O2W' -71(4) . . . . ? O2W' Cd1 O2W O2W' -149(87) 2_756 . . . ? O2W Cd1 O2W O2W' -2(6) 2_756 . . . ? C7 Cd1 O2W O2W' 137(3) 2_756 . . . ? C7 Cd1 O2W O2W' -49(4) . . . . ? O2W' O2W O2W' O2W 142(100) 2_756 . . 2_756 ? Cd1 O2W O2W' O2W 160(57) . . . 2_756 ? O2W O2W O2W' O2W' -142(100) 2_756 . . 2_756 ? Cd1 O2W O2W' O2W' 18(52) . . . 2_756 ? O2W' O2W O2W' Cd1 -18(52) 2_756 . . . ? O2W O2W O2W' Cd1 -160(57) 2_756 . . . ? O2 Cd1 O2W' O2W 114(85) . . . 2_756 ? O2 Cd1 O2W' O2W -66(85) 2_756 . . 2_756 ? O1W Cd1 O2W' O2W -153(85) 2_756 . . 2_756 ? O1W Cd1 O2W' O2W 23(85) . . . 2_756 ? O1 Cd1 O2W' O2W -104(85) 2_756 . . 2_756 ? O1 Cd1 O2W' O2W 99(85) . . . 2_756 ? O2W' Cd1 O2W' O2W -30(83) 2_756 . . 2_756 ? O2W Cd1 O2W' O2W -32(88) . . . 2_756 ? C7 Cd1 O2W' O2W -82(85) 2_756 . . 2_756 ? C7 Cd1 O2W' O2W 106(85) . . . 2_756 ? O2 Cd1 O2W' O2W 145(3) . . . . ? O2 Cd1 O2W' O2W -35(3) 2_756 . . . ? O1W Cd1 O2W' O2W -122(3) 2_756 . . . ? O1W Cd1 O2W' O2W 55(3) . . . . ? O1 Cd1 O2W' O2W -73(3) 2_756 . . . ? O1 Cd1 O2W' O2W 130(4) . . . . ? O2W' Cd1 O2W' O2W 2(5) 2_756 . . . ? O2W Cd1 O2W' O2W 32(88) 2_756 . . . ? C7 Cd1 O2W' O2W -50(3) 2_756 . . . ? C7 Cd1 O2W' O2W 138(3) . . . . ? O2 Cd1 O2W' O2W' 144(2) . . . 2_756 ? O2 Cd1 O2W' O2W' -36(2) 2_756 . . 2_756 ? O1W Cd1 O2W' O2W' -124(2) 2_756 . . 2_756 ? O1W Cd1 O2W' O2W' 53(2) . . . 2_756 ? O1 Cd1 O2W' O2W' -74(3) 2_756 . . 2_756 ? O1 Cd1 O2W' O2W' 128.4(19) . . . 2_756 ? O2W Cd1 O2W' O2W' 30(83) 2_756 . . 2_756 ? O2W Cd1 O2W' O2W' -2(5) . . . 2_756 ? C7 Cd1 O2W' O2W' -52(3) 2_756 . . 2_756 ? C7 Cd1 O2W' O2W' 136(2) . . . 2_756 ? O3 C8 O4 Cd2 2.1(5) . . . . ? C3 C8 O4 Cd2 -176.7(3) . . . . ? O3W Cd2 O4 C8 -85.5(3) . . . . ? O4W Cd2 O4 C8 10.8(4) . . . . ? O6 Cd2 O4 C8 -148.1(3) 6_565 . . . ? O3 Cd2 O4 C8 -1.1(2) . . . . ? O5 Cd2 O4 C8 97.7(3) 4_656 . . . ? O5 Cd2 O4 C8 175.8(3) 6_565 . . . ? C22 Cd2 O4 C8 -170.6(3) 6_565 . . . ? O6 C22 O5 Cd2 103.4(6) . . . 4_646 ? C18 C22 O5 Cd2 -75.9(6) . . . 4_646 ? Cd2 C22 O5 Cd2 103.5(3) 6_566 . . 4_646 ? O6 C22 O5 Cd2 -0.1(6) . . . 6_566 ? C18 C22 O5 Cd2 -179.4(5) . . . 6_566 ? O5 C22 O6 Cd2 0.1(6) . . . 6_566 ? C18 C22 O6 Cd2 179.4(4) . . . 6_566 ? O8W' O8W O8W' O8W -15(7) 2_756 . . 2_756 ? O8W O8W O8W' O8W' 15(7) 2_756 . . 2_756 ? _diffrn_measured_fraction_theta_max 0.872 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.889 _refine_diff_density_min -0.745 _refine_diff_density_rms 0.124 #=========================END data_Compound-2 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C46 H56 Mn3 N4 O23, 7H2O' _chemical_formula_sum 'C46 H70 Mn3 N4 O30' _chemical_formula_weight 1323.88 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Mn' 'Mn' 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' _symmetry_space_group_name_hall '-C 2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 24.492(4) _cell_length_b 13.0355(14) _cell_length_c 20.310(3) _cell_angle_alpha 90.00 _cell_angle_beta 124.676(4) _cell_angle_gamma 90.00 _cell_volume 5332.5(12) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 2075 _cell_measurement_theta_min 2.9813 _cell_measurement_theta_max 29.4031 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.649 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2756 _exptl_absorpt_coefficient_mu 0.802 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.88616 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ; CrysAlis (Oxford Diffraction, 2006) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Diffraction Gemini R Ultra' _diffrn_measurement_method '\w scan' _diffrn_detector_area_resol_mean 10.0 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 18770 _diffrn_reflns_av_R_equivalents 0.0895 _diffrn_reflns_av_sigmaI/netI 0.1390 _diffrn_reflns_limit_h_min -32 _diffrn_reflns_limit_h_max 32 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.99 _diffrn_reflns_theta_max 29.47 _reflns_number_total 6513 _reflns_number_gt 2974 _reflns_threshold_expression >2\s(I) _computing_data_collection 'CrysAlisPro(1.171.35.21) (Agilent Tech., 2012)' _computing_cell_refinement 'CrysAlisPro(1.171.35.21) (Agilent Tech., 2012)' _computing_data_reduction 'CrysAlisPro(1.171.35.21) (Agilent Tech., 2012)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0400P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6513 _refine_ls_number_parameters 412 _refine_ls_number_restraints 28 _refine_ls_R_factor_all 0.1858 _refine_ls_R_factor_gt 0.0788 _refine_ls_wR_factor_ref 0.1702 _refine_ls_wR_factor_gt 0.1409 _refine_ls_goodness_of_fit_ref 1.182 _refine_ls_restrained_S_all 1.187 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mn1 Mn 0.5000 0.62623(9) 0.2500 0.0438(3) Uani 1 2 d SD . . Mn2 Mn 0.31445(4) 0.65107(6) 0.56878(5) 0.0427(3) Uani 1 1 d D . . C1 C 0.3122(2) 0.7498(3) 0.1344(3) 0.0280(11) Uani 1 1 d . . . C2 C 0.2951(2) 0.8383(3) 0.0893(3) 0.0296(11) Uani 1 1 d . . . H2 H 0.3271 0.8728 0.0868 0.036 Uiso 1 1 calc R . . C3 C 0.2316(2) 0.8763(3) 0.0482(3) 0.0264(11) Uani 1 1 d . . . C4 C 0.1846(2) 0.8265(3) 0.0543(3) 0.0288(11) Uani 1 1 d . . . H4 H 0.1419 0.8531 0.0279 0.035 Uiso 1 1 calc R . . C5 C 0.2004(2) 0.7377(3) 0.0991(3) 0.0286(11) Uani 1 1 d . . . C6 C 0.2636(2) 0.7004(3) 0.1379(3) 0.0315(12) Uani 1 1 d . . . H6 H 0.2744 0.6402 0.1675 0.038 Uiso 1 1 calc R . . C7 C 0.3813(3) 0.7113(4) 0.1801(3) 0.0368(12) Uani 1 1 d . . . C8 C 0.2142(3) 0.9735(3) 0.0025(3) 0.0305(12) Uani 1 1 d . . . C9 C 0.1505(2) 0.6913(4) 0.1112(3) 0.0335(12) Uani 1 1 d . . . H9A H 0.1296 0.7464 0.1216 0.040 Uiso 1 1 calc R . . H9B H 0.1740 0.6486 0.1587 0.040 Uiso 1 1 calc R . . C10 C -0.0609(3) 0.6267(4) -0.0664(4) 0.0478(15) Uani 1 1 d . . . H10A H -0.0364 0.5972 -0.0131 0.057 Uiso 1 1 calc R . . H10B H -0.0779 0.6927 -0.0639 0.057 Uiso 1 1 calc R . . C11 C -0.0137(3) 0.6434(4) -0.0909(4) 0.0546(16) Uani 1 1 d . . . H11A H -0.0040 0.5777 -0.1045 0.066 Uiso 1 1 calc R . . H11B H -0.0356 0.6856 -0.1388 0.066 Uiso 1 1 calc R . . C12 C 0.0504(3) 0.6935(4) -0.0281(3) 0.0472(14) Uani 1 1 d . . . H12A H 0.0404 0.7549 -0.0098 0.057 Uiso 1 1 calc R . . H12B H 0.0730 0.7149 -0.0524 0.057 Uiso 1 1 calc R . . C13 C 0.1227(3) 0.5411(4) 0.0215(3) 0.0413(13) Uani 1 1 d . . . H13A H 0.1543 0.5665 0.0111 0.050 Uiso 1 1 calc R . . H13B H 0.0863 0.5093 -0.0271 0.050 Uiso 1 1 calc R . . C14 C 0.1558(3) 0.4625(4) 0.0871(3) 0.0394(13) Uani 1 1 d . . . H14A H 0.1619 0.3997 0.0664 0.047 Uiso 1 1 calc R . . H14B H 0.1994 0.4874 0.1298 0.047 Uiso 1 1 calc R . . C15 C 0.1586(3) 0.3938(4) 0.2009(3) 0.0426(13) Uani 1 1 d . . . H15A H 0.1784 0.3312 0.1977 0.051 Uiso 1 1 calc R . . H15B H 0.1311 0.3757 0.2195 0.051 Uiso 1 1 calc R . . C16 C 0.2130(3) 0.4655(4) 0.2607(3) 0.0336(12) Uani 1 1 d . . . C17 C 0.1984(3) 0.5461(4) 0.2919(3) 0.0359(13) Uani 1 1 d . . . H17 H 0.1549 0.5567 0.2761 0.043 Uiso 1 1 calc R . . C18 C 0.2483(3) 0.6114(3) 0.3469(3) 0.0378(13) Uani 1 1 d . . . C19 C 0.3126(3) 0.5964(4) 0.3689(3) 0.0378(13) Uani 1 1 d . . . H19 H 0.3461 0.6405 0.4056 0.045 Uiso 1 1 calc R . . C20 C 0.3270(3) 0.5175(4) 0.3372(3) 0.0343(12) Uani 1 1 d . . . C21 C 0.2772(3) 0.4519(4) 0.2839(3) 0.0342(12) Uani 1 1 d . . . H21 H 0.2872 0.3971 0.2632 0.041 Uiso 1 1 calc R . . C22 C 0.2337(4) 0.6947(4) 0.3870(4) 0.0533(17) Uani 1 1 d . . . C23 C 0.3970(3) 0.5007(5) 0.3614(4) 0.0469(15) Uani 1 1 d . . . N1 N 0.0970(2) 0.6282(3) 0.0434(3) 0.0363(10) Uani 1 1 d . . . N2 N 0.1164(2) 0.4398(3) 0.1203(3) 0.0374(10) Uani 1 1 d . . . O1 O 0.39453(17) 0.6223(3) 0.2088(2) 0.0471(10) Uani 1 1 d . . . O2 O 0.42609(19) 0.7668(3) 0.1889(3) 0.0623(12) Uani 1 1 d . . . O3 O 0.15493(18) 1.0030(2) -0.0384(2) 0.0370(8) Uani 1 1 d . . . O4 O 0.25914(17) 1.0265(2) 0.0071(2) 0.0413(9) Uani 1 1 d . . . O5 O 0.2804(2) 0.7291(3) 0.4541(3) 0.0631(13) Uani 1 1 d . . . O6 O 0.1769(3) 0.7259(3) 0.3518(3) 0.0834(16) Uani 1 1 d . . . O6W O 0.0362(3) 0.6438(5) 0.1349(5) 0.150(3) Uani 1 1 d . . . O7 O 0.4065(2) 0.4237(3) 0.3332(2) 0.0628(12) Uani 1 1 d . . . H7 H 0.4457 0.4212 0.3493 0.094 Uiso 1 1 calc R . . O8 O 0.4394(2) 0.5649(3) 0.4049(3) 0.0657(12) Uani 1 1 d . . . O1W O 0.53051(19) 0.5938(3) 0.3710(2) 0.0551(10) Uani 1 1 d D . . H1A H 0.5693(11) 0.565(3) 0.409(2) 0.083 Uiso 1 1 d D . . H1B H 0.5012(18) 0.544(2) 0.3452(7) 0.083 Uiso 1 1 d D . . O2W O 0.5000 0.4424(6) 0.2500 0.158(4) Uani 1 2 d SD . . H2A H 0.522(5) 0.383(4) 0.262(11) 0.237 Uiso 1 1 d D . . O3W O 0.4161(2) 0.6942(3) 0.6179(3) 0.0689(13) Uani 1 1 d D . . H3A H 0.3951(7) 0.724(3) 0.5688(11) 0.103 Uiso 1 1 d D . . H3B H 0.424(3) 0.746(3) 0.651(2) 0.103 Uiso 1 1 d D . . O4W O 0.3330(2) 0.5608(3) 0.6691(3) 0.0655(13) Uani 1 1 d D . . H4A H 0.3726(11) 0.593(3) 0.6920(11) 0.098 Uiso 1 1 d D . . H4B H 0.343(2) 0.4932(10) 0.676(4) 0.098 Uiso 1 1 d D . . O5W O 0.4762(2) 0.6532(3) 0.5458(3) 0.0678(12) Uani 1 1 d D . . H5A H 0.475(2) 0.652(3) 0.5891(17) 0.102 Uiso 1 1 d D . . H5B H 0.4805(17) 0.5884(15) 0.5347(8) 0.102 Uiso 1 1 d D . . O8W O 0.0000 0.4640(10) 0.2500 0.183(4) Uani 1 2 d SDU . . H8A H -0.041(3) 0.451(11) 0.238(9) 0.275 Uiso 1 1 d D . . O7W O 0.0979(4) 0.5818(6) 0.3740(5) 0.159(3) Uani 1 1 d D . . H7A H 0.102(5) 0.617(8) 0.338(6) 0.238 Uiso 1 1 d D . . H7B H 0.058(3) 0.603(9) 0.363(7) 0.238 Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mn1 0.0251(7) 0.0538(8) 0.0432(8) 0.000 0.0139(7) 0.000 Mn2 0.0456(6) 0.0335(5) 0.0481(6) -0.0040(4) 0.0261(5) 0.0023(4) C1 0.022(3) 0.028(3) 0.023(3) -0.003(2) 0.006(3) 0.000(2) C2 0.028(3) 0.026(3) 0.038(3) -0.008(2) 0.020(3) -0.007(2) C3 0.027(3) 0.025(2) 0.025(3) -0.006(2) 0.013(3) -0.003(2) C4 0.022(3) 0.034(3) 0.032(3) -0.002(2) 0.016(3) 0.001(2) C5 0.023(3) 0.030(3) 0.027(3) -0.001(2) 0.010(3) -0.003(2) C6 0.028(3) 0.027(3) 0.029(3) 0.000(2) 0.010(3) 0.000(2) C7 0.029(3) 0.038(3) 0.033(3) -0.008(3) 0.012(3) 0.000(3) C8 0.032(3) 0.029(3) 0.031(3) -0.005(2) 0.019(3) -0.004(2) C9 0.029(3) 0.036(3) 0.031(3) 0.000(2) 0.015(3) -0.004(2) C10 0.039(4) 0.042(3) 0.053(4) 0.000(3) 0.020(3) -0.002(3) C11 0.030(3) 0.067(4) 0.045(4) 0.012(3) 0.008(3) -0.014(3) C12 0.029(3) 0.050(3) 0.052(4) 0.013(3) 0.017(3) -0.006(3) C13 0.043(4) 0.042(3) 0.035(3) 0.000(3) 0.020(3) -0.009(3) C14 0.030(3) 0.047(3) 0.040(3) -0.002(3) 0.019(3) -0.003(3) C15 0.045(4) 0.040(3) 0.030(3) 0.007(3) 0.013(3) -0.003(3) C16 0.034(3) 0.034(3) 0.028(3) 0.006(2) 0.015(3) -0.001(2) C17 0.031(3) 0.034(3) 0.042(3) 0.005(3) 0.021(3) 0.007(2) C18 0.049(4) 0.028(3) 0.046(4) 0.002(2) 0.033(3) 0.002(3) C19 0.039(4) 0.040(3) 0.030(3) -0.001(2) 0.017(3) -0.005(3) C20 0.036(3) 0.036(3) 0.029(3) 0.002(2) 0.018(3) -0.002(2) C21 0.038(4) 0.033(3) 0.030(3) 0.006(2) 0.019(3) 0.009(2) C22 0.071(5) 0.042(3) 0.060(5) -0.002(3) 0.045(5) 0.007(4) C23 0.046(4) 0.060(4) 0.044(4) 0.000(3) 0.031(4) 0.004(3) N1 0.027(3) 0.038(2) 0.037(3) 0.006(2) 0.015(2) -0.002(2) N2 0.031(3) 0.038(2) 0.032(3) 0.000(2) 0.012(2) -0.006(2) O1 0.031(2) 0.048(2) 0.053(3) 0.010(2) 0.018(2) 0.0081(18) O2 0.025(2) 0.052(2) 0.092(4) 0.008(2) 0.022(3) 0.0008(19) O3 0.032(2) 0.0347(19) 0.040(2) 0.0067(16) 0.017(2) 0.0010(17) O4 0.040(2) 0.0304(19) 0.058(3) 0.0033(17) 0.031(2) -0.0047(17) O5 0.099(4) 0.040(2) 0.063(3) -0.012(2) 0.054(3) -0.015(2) O6 0.086(4) 0.054(3) 0.110(4) -0.008(3) 0.055(4) 0.030(3) O6W 0.114(6) 0.207(7) 0.176(7) 0.050(6) 0.111(6) 0.054(5) O7 0.040(3) 0.074(3) 0.063(3) -0.005(2) 0.023(3) 0.019(2) O8 0.041(3) 0.095(3) 0.059(3) -0.026(3) 0.027(3) -0.019(3) O1W 0.028(2) 0.071(3) 0.050(3) 0.008(2) 0.013(2) -0.001(2) O2W 0.164(10) 0.062(5) 0.093(7) 0.000 -0.019(7) 0.000 O3W 0.071(3) 0.071(3) 0.067(3) -0.025(2) 0.041(3) -0.019(3) O4W 0.097(4) 0.047(2) 0.066(3) 0.001(2) 0.054(3) 0.006(2) O5W 0.067(3) 0.072(3) 0.066(3) 0.001(2) 0.039(3) 0.012(2) O8W 0.215(9) 0.109(6) 0.162(8) 0.000 0.070(7) 0.000 O7W 0.179(8) 0.133(6) 0.185(8) 0.029(5) 0.116(8) -0.015(5) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mn1 O1W 2.165(4) 2_655 ? Mn1 O1W 2.165(4) . ? Mn1 O1 2.217(3) 2_655 ? Mn1 O1 2.217(3) . ? Mn1 O2 2.370(4) 2_655 ? Mn1 O2 2.370(4) . ? Mn1 O2W 2.396(8) . ? Mn2 O3W 2.165(4) . ? Mn2 O4W 2.166(4) . ? Mn2 O6 2.197(4) 7_566 ? Mn2 O5 2.224(4) . ? Mn2 O4 2.258(3) 4_545 ? Mn2 O3 2.279(3) 4_545 ? Mn2 C8 2.606(5) 4_545 ? C1 C2 1.382(6) . ? C1 C6 1.391(6) . ? C1 C7 1.481(7) . ? C2 C3 1.372(6) . ? C2 H2 0.9300 . ? C3 C4 1.387(6) . ? C3 C8 1.483(6) . ? C4 C5 1.384(6) . ? C4 H4 0.9300 . ? C5 C6 1.365(6) . ? C5 C9 1.505(6) . ? C6 H6 0.9300 . ? C7 O2 1.238(6) . ? C7 O1 1.256(6) . ? C8 O3 1.254(5) . ? C8 O4 1.258(5) . ? C8 Mn2 2.606(5) 4 ? C9 N1 1.496(6) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 N2 1.451(6) 5_565 ? C10 C11 1.512(7) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 C12 1.497(7) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 N1 1.500(7) . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C13 N1 1.484(6) . ? C13 C14 1.501(7) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 N2 1.487(5) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 N2 1.478(6) . ? C15 C16 1.510(7) . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 C21 1.372(6) . ? C16 C17 1.376(6) . ? C17 C18 1.384(7) . ? C17 H17 0.9300 . ? C18 C19 1.383(7) . ? C18 C22 1.517(7) . ? C19 C20 1.362(6) . ? C19 H19 0.9300 . ? C20 C21 1.375(7) . ? C20 C23 1.507(7) . ? C21 H21 0.9300 . ? C22 O6 1.216(7) . ? C22 O5 1.262(7) . ? C23 O8 1.230(6) . ? C23 O7 1.242(6) . ? N2 C10 1.451(6) 5_565 ? O3 Mn2 2.279(3) 4 ? O4 Mn2 2.258(3) 4 ? O6 Mn2 2.197(4) 7_566 ? O7 H7 0.8200 . ? O1W H1A 0.895(10) . ? O1W H1B 0.889(10) . ? O2W H2A 0.900(10) . ? O3W H3A 0.910(10) . ? O3W H3B 0.901(10) . ? O4W H4A 0.903(10) . ? O4W H4B 0.904(10) . ? O5W H5A 0.890(10) . ? O5W H5B 0.896(10) . ? O8W H8A 0.900(10) . ? O7W H7A 0.912(10) . ? O7W H7B 0.911(10) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1W Mn1 O1W 157.5(2) 2_655 . ? O1W Mn1 O1 89.96(14) 2_655 2_655 ? O1W Mn1 O1 89.52(14) . 2_655 ? O1W Mn1 O1 89.52(14) 2_655 . ? O1W Mn1 O1 89.96(14) . . ? O1 Mn1 O1 177.37(19) 2_655 . ? O1W Mn1 O2 114.37(14) 2_655 2_655 ? O1W Mn1 O2 83.65(15) . 2_655 ? O1 Mn1 O2 56.05(12) 2_655 2_655 ? O1 Mn1 O2 126.45(14) . 2_655 ? O1W Mn1 O2 83.65(15) 2_655 . ? O1W Mn1 O2 114.37(14) . . ? O1 Mn1 O2 126.45(14) 2_655 . ? O1 Mn1 O2 56.05(12) . . ? O2 Mn1 O2 78.73(19) 2_655 . ? O1W Mn1 O2W 78.74(10) 2_655 . ? O1W Mn1 O2W 78.74(10) . . ? O1 Mn1 O2W 88.68(10) 2_655 . ? O1 Mn1 O2W 88.68(10) . . ? O2 Mn1 O2W 140.63(10) 2_655 . ? O2 Mn1 O2W 140.63(10) . . ? O3W Mn2 O4W 97.88(17) . . ? O3W Mn2 O6 82.35(17) . 7_566 ? O4W Mn2 O6 79.91(16) . 7_566 ? O3W Mn2 O5 90.65(17) . . ? O4W Mn2 O5 170.75(18) . . ? O6 Mn2 O5 104.88(17) 7_566 . ? O3W Mn2 O4 139.80(13) . 4_545 ? O4W Mn2 O4 84.83(15) . 4_545 ? O6 Mn2 O4 137.02(15) 7_566 4_545 ? O5 Mn2 O4 86.36(14) . 4_545 ? O3W Mn2 O3 82.85(14) . 4_545 ? O4W Mn2 O3 82.49(13) . 4_545 ? O6 Mn2 O3 155.15(17) 7_566 4_545 ? O5 Mn2 O3 95.13(13) . 4_545 ? O4 Mn2 O3 57.61(12) 4_545 4_545 ? O3W Mn2 C8 111.25(15) . 4_545 ? O4W Mn2 C8 83.46(15) . 4_545 ? O6 Mn2 C8 159.88(16) 7_566 4_545 ? O5 Mn2 C8 90.16(14) . 4_545 ? O4 Mn2 C8 28.85(12) 4_545 4_545 ? O3 Mn2 C8 28.77(12) 4_545 4_545 ? C2 C1 C6 118.3(4) . . ? C2 C1 C7 120.4(4) . . ? C6 C1 C7 121.3(4) . . ? C3 C2 C1 121.1(4) . . ? C3 C2 H2 119.5 . . ? C1 C2 H2 119.5 . . ? C2 C3 C4 119.2(4) . . ? C2 C3 C8 120.8(4) . . ? C4 C3 C8 119.9(4) . . ? C3 C4 C5 121.0(4) . . ? C3 C4 H4 119.5 . . ? C5 C4 H4 119.5 . . ? C6 C5 C4 118.5(4) . . ? C6 C5 C9 121.5(4) . . ? C4 C5 C9 119.7(4) . . ? C5 C6 C1 121.9(4) . . ? C5 C6 H6 119.1 . . ? C1 C6 H6 119.1 . . ? O2 C7 O1 120.0(5) . . ? O2 C7 C1 119.7(5) . . ? O1 C7 C1 120.3(4) . . ? O3 C8 O4 121.0(4) . . ? O3 C8 C3 119.3(4) . . ? O4 C8 C3 119.7(5) . . ? O3 C8 Mn2 61.0(2) . 4 ? O4 C8 Mn2 60.0(2) . 4 ? C3 C8 Mn2 175.9(3) . 4 ? C5 C9 N1 115.9(4) . . ? C5 C9 H9A 108.3 . . ? N1 C9 H9A 108.3 . . ? C5 C9 H9B 108.3 . . ? N1 C9 H9B 108.3 . . ? H9A C9 H9B 107.4 . . ? N2 C10 C11 113.7(4) 5_565 . ? N2 C10 H10A 108.8 5_565 . ? C11 C10 H10A 108.8 . . ? N2 C10 H10B 108.8 5_565 . ? C11 C10 H10B 108.8 . . ? H10A C10 H10B 107.7 . . ? C12 C11 C10 114.1(5) . . ? C12 C11 H11A 108.7 . . ? C10 C11 H11A 108.7 . . ? C12 C11 H11B 108.7 . . ? C10 C11 H11B 108.7 . . ? H11A C11 H11B 107.6 . . ? C11 C12 N1 115.4(4) . . ? C11 C12 H12A 108.4 . . ? N1 C12 H12A 108.4 . . ? C11 C12 H12B 108.4 . . ? N1 C12 H12B 108.4 . . ? H12A C12 H12B 107.5 . . ? N1 C13 C14 111.3(4) . . ? N1 C13 H13A 109.4 . . ? C14 C13 H13A 109.4 . . ? N1 C13 H13B 109.4 . . ? C14 C13 H13B 109.4 . . ? H13A C13 H13B 108.0 . . ? N2 C14 C13 112.0(4) . . ? N2 C14 H14A 109.2 . . ? C13 C14 H14A 109.2 . . ? N2 C14 H14B 109.2 . . ? C13 C14 H14B 109.2 . . ? H14A C14 H14B 107.9 . . ? N2 C15 C16 112.4(4) . . ? N2 C15 H15A 109.1 . . ? C16 C15 H15A 109.1 . . ? N2 C15 H15B 109.1 . . ? C16 C15 H15B 109.1 . . ? H15A C15 H15B 107.9 . . ? C21 C16 C17 119.2(5) . . ? C21 C16 C15 120.7(4) . . ? C17 C16 C15 120.1(5) . . ? C16 C17 C18 120.0(5) . . ? C16 C17 H17 120.0 . . ? C18 C17 H17 120.0 . . ? C17 C18 C19 119.6(4) . . ? C17 C18 C22 120.2(5) . . ? C19 C18 C22 120.1(5) . . ? C20 C19 C18 120.5(5) . . ? C20 C19 H19 119.7 . . ? C18 C19 H19 119.7 . . ? C19 C20 C21 119.3(5) . . ? C19 C20 C23 120.6(5) . . ? C21 C20 C23 120.1(4) . . ? C16 C21 C20 121.4(4) . . ? C16 C21 H21 119.3 . . ? C20 C21 H21 119.3 . . ? O6 C22 O5 123.1(6) . . ? O6 C22 C18 117.7(6) . . ? O5 C22 C18 119.2(6) . . ? O8 C23 O7 125.2(5) . . ? O8 C23 C20 118.3(5) . . ? O7 C23 C20 116.4(5) . . ? C13 N1 C12 111.3(4) . . ? C13 N1 C9 113.5(4) . . ? C12 N1 C9 111.4(4) . . ? C10 N2 C15 110.9(4) 5_565 . ? C10 N2 C14 110.5(4) 5_565 . ? C15 N2 C14 111.0(4) . . ? C7 O1 Mn1 95.2(3) . . ? C7 O2 Mn1 88.5(3) . . ? C8 O3 Mn2 90.2(3) . 4 ? C8 O4 Mn2 91.1(3) . 4 ? C22 O5 Mn2 122.5(4) . . ? C22 O6 Mn2 102.3(5) . 7_566 ? C23 O7 H7 109.5 . . ? Mn1 O1W H1A 124(4) . . ? Mn1 O1W H1B 80.4(7) . . ? H1A O1W H1B 107.6(16) . . ? Mn1 O2W H2A 150(7) . . ? Mn2 O3W H3A 79.7(7) . . ? Mn2 O3W H3B 103(4) . . ? H3A O3W H3B 104.7(15) . . ? Mn2 O4W H4A 79.8(7) . . ? Mn2 O4W H4B 125(4) . . ? H4A O4W H4B 104.9(15) . . ? H5A O5W H5B 107.8(16) . . ? H7A O7W H7B 104.1(16) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C6 C1 C2 C3 -0.7(7) . . . . ? C7 C1 C2 C3 -178.5(4) . . . . ? C1 C2 C3 C4 2.1(7) . . . . ? C1 C2 C3 C8 177.6(4) . . . . ? C2 C3 C4 C5 -2.0(7) . . . . ? C8 C3 C4 C5 -177.6(4) . . . . ? C3 C4 C5 C6 0.5(7) . . . . ? C3 C4 C5 C9 174.0(4) . . . . ? C4 C5 C6 C1 1.0(7) . . . . ? C9 C5 C6 C1 -172.4(4) . . . . ? C2 C1 C6 C5 -0.9(7) . . . . ? C7 C1 C6 C5 176.9(4) . . . . ? C2 C1 C7 O2 12.2(7) . . . . ? C6 C1 C7 O2 -165.6(5) . . . . ? C2 C1 C7 O1 -166.9(4) . . . . ? C6 C1 C7 O1 15.3(7) . . . . ? C2 C3 C8 O3 175.7(4) . . . . ? C4 C3 C8 O3 -8.8(6) . . . . ? C2 C3 C8 O4 -6.3(6) . . . . ? C4 C3 C8 O4 169.1(4) . . . . ? C2 C3 C8 Mn2 -92(5) . . . 4 ? C4 C3 C8 Mn2 84(5) . . . 4 ? C6 C5 C9 N1 -106.5(5) . . . . ? C4 C5 C9 N1 80.2(5) . . . . ? N2 C10 C11 C12 -168.1(5) 5_565 . . . ? C10 C11 C12 N1 70.7(6) . . . . ? N1 C13 C14 N2 44.6(6) . . . . ? N2 C15 C16 C21 -103.2(5) . . . . ? N2 C15 C16 C17 76.2(5) . . . . ? C21 C16 C17 C18 -0.9(7) . . . . ? C15 C16 C17 C18 179.7(4) . . . . ? C16 C17 C18 C19 1.3(7) . . . . ? C16 C17 C18 C22 -174.6(5) . . . . ? C17 C18 C19 C20 -0.4(7) . . . . ? C22 C18 C19 C20 175.6(5) . . . . ? C18 C19 C20 C21 -1.0(7) . . . . ? C18 C19 C20 C23 -179.7(4) . . . . ? C17 C16 C21 C20 -0.5(7) . . . . ? C15 C16 C21 C20 178.9(4) . . . . ? C19 C20 C21 C16 1.5(7) . . . . ? C23 C20 C21 C16 -179.8(4) . . . . ? C17 C18 C22 O6 -25.2(8) . . . . ? C19 C18 C22 O6 158.8(5) . . . . ? C17 C18 C22 O5 155.6(5) . . . . ? C19 C18 C22 O5 -20.4(7) . . . . ? C19 C20 C23 O8 -6.2(8) . . . . ? C21 C20 C23 O8 175.1(5) . . . . ? C19 C20 C23 O7 176.1(5) . . . . ? C21 C20 C23 O7 -2.7(7) . . . . ? C14 C13 N1 C12 -166.5(4) . . . . ? C14 C13 N1 C9 66.9(5) . . . . ? C11 C12 N1 C13 67.1(5) . . . . ? C11 C12 N1 C9 -165.2(4) . . . . ? C5 C9 N1 C13 57.9(5) . . . . ? C5 C9 N1 C12 -68.7(5) . . . . ? C16 C15 N2 C10 -174.3(4) . . . 5_565 ? C16 C15 N2 C14 62.5(5) . . . . ? C13 C14 N2 C10 77.1(5) . . . 5_565 ? C13 C14 N2 C15 -159.4(4) . . . . ? O2 C7 O1 Mn1 -5.5(5) . . . . ? C1 C7 O1 Mn1 173.6(4) . . . . ? O1W Mn1 O1 C7 -79.7(3) 2_655 . . . ? O1W Mn1 O1 C7 122.8(3) . . . . ? O1 Mn1 O1 C7 -158.4(3) 2_655 . . . ? O2 Mn1 O1 C7 40.8(3) 2_655 . . . ? O2 Mn1 O1 C7 3.0(3) . . . . ? O2W Mn1 O1 C7 -158.4(3) . . . . ? O1 C7 O2 Mn1 5.1(5) . . . . ? C1 C7 O2 Mn1 -174.0(4) . . . . ? O1W Mn1 O2 C7 90.7(3) 2_655 . . . ? O1W Mn1 O2 C7 -75.2(3) . . . . ? O1 Mn1 O2 C7 176.0(3) 2_655 . . . ? O1 Mn1 O2 C7 -3.0(3) . . . . ? O2 Mn1 O2 C7 -152.8(4) 2_655 . . . ? O2W Mn1 O2 C7 27.2(4) . . . . ? O4 C8 O3 Mn2 -2.6(4) . . . 4 ? C3 C8 O3 Mn2 175.4(4) . . . 4 ? O3 C8 O4 Mn2 2.6(4) . . . 4 ? C3 C8 O4 Mn2 -175.3(3) . . . 4 ? O6 C22 O5 Mn2 97.9(7) . . . . ? C18 C22 O5 Mn2 -83.0(5) . . . . ? O3W Mn2 O5 C22 144.0(5) . . . . ? O4W Mn2 O5 C22 -13.5(12) . . . . ? O6 Mn2 O5 C22 -133.7(4) 7_566 . . . ? O4 Mn2 O5 C22 4.2(5) 4_545 . . . ? O3 Mn2 O5 C22 61.2(5) 4_545 . . . ? C8 Mn2 O5 C22 32.8(5) 4_545 . . . ? O5 C22 O6 Mn2 2.6(7) . . . 7_566 ? C18 C22 O6 Mn2 -176.5(4) . . . 7_566 ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O7 H7 O5W 0.82 2.12 2.696(6) 126.9 5_666 O2W H2A O3W 0.900(10) 2.25(15) 2.884(7) 127(14) 5_666 O4W H4A O2W 0.903(10) 2.67(3) 3.433(4) 142(4) 5_666 O5W H5B O8 0.896(10) 2.570(14) 3.316(6) 141.3(14) 5_666 O1W H1B O2W 0.889(10) 2.33(3) 2.899(6) 122(3) . O3W H3A O5 0.910(10) 2.424(13) 3.121(7) 133.5(9) . O5W H5A O3W 0.890(10) 1.93(3) 2.654(5) 137(3) . O1W H1A O3 0.895(10) 1.94(2) 2.808(5) 162(5) 8_566 O3W H3B O7W 0.901(10) 2.30(4) 2.955(9) 130(4) 7_566 O4W H4B O1 0.904(10) 1.83(2) 2.691(5) 158(4) 6_566 _diffrn_measured_fraction_theta_max 0.879 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.723 _refine_diff_density_min -0.491 _refine_diff_density_rms 0.092 #=========================END data_Compound-3 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C46 H54 N4 O22 Zn3, 6H2O' _chemical_formula_sum 'C46 H66 N4 O28 Zn3' _chemical_formula_weight 1319.14 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Zn' 'Zn' 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' _symmetry_space_group_name_hall ' -C 2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 24.011(2) _cell_length_b 13.1094(8) _cell_length_c 20.548(2) _cell_angle_alpha 90.00 _cell_angle_beta 124.399(15) _cell_angle_gamma 90.00 _cell_volume 5336.6(8) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 2180 _cell_measurement_theta_min 3.1016 _cell_measurement_theta_max 29.1133 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.642 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2736 _exptl_absorpt_coefficient_mu 1.435 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7246 _exptl_absorpt_correction_T_max 0.8030 _exptl_absorpt_process_details ; CrysAlis (Oxford Diffraction, 2006) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Diffraction Gemini R Ultra' _diffrn_measurement_method '\w scan' _diffrn_detector_area_resol_mean 10.0 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16647 _diffrn_reflns_av_R_equivalents 0.0886 _diffrn_reflns_av_sigmaI/netI 0.1083 _diffrn_reflns_limit_h_min -28 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 3.11 _diffrn_reflns_theta_max 25.35 _reflns_number_total 4830 _reflns_number_gt 2710 _reflns_threshold_expression >2\s(I) _computing_data_collection 'CrysAlisPro(1.171.35.21) (Agilent Tech., 2012)' _computing_cell_refinement 'CrysAlisPro(1.171.35.21) (Agilent Tech., 2012)' _computing_data_reduction 'CrysAlisPro(1.171.35.21) (Agilent Tech., 2012)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0500P)^2^+42.2490P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4830 _refine_ls_number_parameters 423 _refine_ls_number_restraints 58 _refine_ls_R_factor_all 0.1501 _refine_ls_R_factor_gt 0.0805 _refine_ls_wR_factor_ref 0.1898 _refine_ls_wR_factor_gt 0.1578 _refine_ls_goodness_of_fit_ref 1.049 _refine_ls_restrained_S_all 1.044 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zn1 Zn 0.0000 0.34597(10) 0.2500 0.0483(4) Uani 1 2 d SD . . Zn2 Zn 0.68117(5) 0.86733(7) 0.90358(6) 0.0568(3) Uani 1 1 d D . . C1 C 0.6913(3) 0.5489(5) 0.7796(4) 0.0375(17) Uani 1 1 d . . . H1 H 0.6459 0.5547 0.7606 0.045 Uiso 1 1 calc R . . C2 C 0.7362(3) 0.6216(5) 0.8304(4) 0.0374(17) Uani 1 1 d . . . C3 C 0.8039(3) 0.6129(5) 0.8608(4) 0.0371(16) Uani 1 1 d . . . H3 H 0.8343 0.6619 0.8955 0.045 Uiso 1 1 calc R . . C4 C 0.8264(3) 0.5303(5) 0.8393(4) 0.0339(16) Uani 1 1 d . . . C5 C 0.7806(3) 0.4593(5) 0.7879(4) 0.0343(16) Uani 1 1 d . . . H5 H 0.7956 0.4037 0.7737 0.041 Uiso 1 1 calc R . . C6 C 0.7123(3) 0.4684(5) 0.7566(4) 0.0330(16) Uani 1 1 d . . . C7 C 0.6624(3) 0.3930(5) 0.6973(4) 0.0433(18) Uani 1 1 d . . . H7A H 0.6861 0.3363 0.6931 0.052 Uiso 1 1 calc R . . H7B H 0.6348 0.3666 0.7143 0.052 Uiso 1 1 calc R . . C8 C 0.6236(3) 0.5514(5) 0.5251(4) 0.0355(16) Uani 1 1 d . . . H8A H 0.6553 0.5778 0.5142 0.043 Uiso 1 1 calc R . . H8B H 0.5869 0.5190 0.4774 0.043 Uiso 1 1 calc R . . C9 C 0.6585(3) 0.4732(5) 0.5894(4) 0.0368(17) Uani 1 1 d . . . H9A H 0.6677 0.4132 0.5693 0.044 Uiso 1 1 calc R . . H9B H 0.7013 0.5005 0.6324 0.044 Uiso 1 1 calc R . . C10 C 0.5631(3) 0.3766(5) 0.5639(4) 0.0365(16) Uani 1 1 d . . . H10A H 0.5815 0.3135 0.5590 0.044 Uiso 1 1 calc R . . H10B H 0.5375 0.4090 0.5124 0.044 Uiso 1 1 calc R . . C11 C 0.5160(3) 0.3520(6) 0.5881(4) 0.0449(19) Uani 1 1 d . . . H11A H 0.5041 0.4149 0.6022 0.054 Uiso 1 1 calc R . . H11B H 0.5397 0.3093 0.6348 0.054 Uiso 1 1 calc R . . C12 C 0.4521(3) 0.2984(6) 0.5255(4) 0.0421(18) Uani 1 1 d . . . H12A H 0.4641 0.2387 0.5082 0.051 Uiso 1 1 calc R . . H12B H 0.4289 0.2750 0.5490 0.051 Uiso 1 1 calc R . . C13 C 0.3502(3) 0.2964(5) 0.3884(4) 0.0329(16) Uani 1 1 d . . . H13A H 0.3251 0.3375 0.3409 0.040 Uiso 1 1 calc R . . H13B H 0.3723 0.2425 0.3786 0.040 Uiso 1 1 calc R . . C14 C 0.3013(3) 0.2485(5) 0.4022(4) 0.0286(15) Uani 1 1 d . . . C15 C 0.3186(3) 0.1633(5) 0.4492(3) 0.0273(14) Uani 1 1 d . . . H15 H 0.3627 0.1392 0.4764 0.033 Uiso 1 1 calc R . . C16 C 0.2724(3) 0.1129(5) 0.4572(3) 0.0287(15) Uani 1 1 d . . . C17 C 0.2061(3) 0.1477(5) 0.4154(4) 0.0312(15) Uani 1 1 d . . . H17 H 0.1742 0.1132 0.4193 0.037 Uiso 1 1 calc R . . C18 C 0.1876(3) 0.2324(5) 0.3688(4) 0.0316(15) Uani 1 1 d . . . C19 C 0.2357(3) 0.2829(5) 0.3631(4) 0.0341(16) Uani 1 1 d . . . H19 H 0.2233 0.3413 0.3321 0.041 Uiso 1 1 calc R . . C20 C 0.1164(4) 0.2685(7) 0.3241(4) 0.0462(19) Uani 1 1 d . . . C21 C 0.2942(3) 0.0227(5) 0.5098(4) 0.0322(15) Uani 1 1 d . . . C22 C 0.7070(4) 0.7128(7) 0.8461(5) 0.056(2) Uani 1 1 d . . . C23 C 0.9001(4) 0.5219(7) 0.8683(5) 0.050(2) Uani 1 1 d . . . N1 N 0.6186(2) 0.4435(4) 0.6192(3) 0.0342(13) Uani 1 1 d . . . N2 N 0.4038(2) 0.3623(4) 0.4543(3) 0.0292(12) Uani 1 1 d . . . O1 O 0.7451(3) 0.7647(4) 0.9049(4) 0.0620(16) Uani 1 1 d . . . O2' O 0.6444(8) 0.7187(12) 0.8145(10) 0.060(4) Uani 0.40 1 d PU . . O2 O 0.6493(6) 0.7437(9) 0.7901(7) 0.066(3) Uani 0.60 1 d PU . . O3 O 0.9395(3) 0.5885(5) 0.9110(4) 0.0729(18) Uani 1 1 d . . . O4 O 0.9149(2) 0.4473(6) 0.8441(3) 0.078(2) Uani 1 1 d . . . H4 H 0.9552 0.4491 0.8618 0.117 Uiso 1 1 calc RD . . O5 O 0.1019(2) 0.3500(5) 0.2859(3) 0.0579(15) Uani 1 1 d . . . O6 O 0.0732(3) 0.2208(5) 0.3252(4) 0.0703(18) Uani 1 1 d . . . O7 O 0.3554(2) 0.0037(4) 0.5544(3) 0.0485(13) Uani 1 1 d . . . O8 O 0.2512(2) -0.0328(4) 0.5086(3) 0.0439(12) Uani 1 1 d . . . O6W' O 0.6148(7) 0.5872(10) 0.8932(8) 0.076(4) Uani 0.50 1 d PU . . O6W O 0.5673(12) 0.5758(18) 0.8582(14) 0.060(6) Uani 0.25 1 d PU . . O7W O 0.5211(11) 0.4807(18) 0.7509(16) 0.077(7) Uani 0.25 1 d PU . . O1W O 0.0215(3) 0.4237(7) 0.3456(5) 0.120(3) Uani 1 1 d D . . H1A H 0.061(2) 0.436(11) 0.392(3) 0.180 Uiso 1 1 d D . . H1B H -0.009(4) 0.413(8) 0.358(5) 0.180 Uiso 1 1 d D . . O2W O 0.6497(4) 0.9579(5) 0.8119(3) 0.082(2) Uani 1 1 d D . . H2A H 0.643(5) 1.0259(12) 0.807(3) 0.123 Uiso 1 1 d D . . H2B H 0.622(4) 0.928(2) 0.7644(5) 0.123 Uiso 1 1 d D . . O3W O 0.6363(5) 0.7850(5) 0.9408(7) 0.150(4) Uani 1 1 d D . . H3A H 0.594(3) 0.803(6) 0.925(6) 0.225 Uiso 1 1 d D . . H3B H 0.636(6) 0.7172(10) 0.935(7) 0.225 Uiso 1 1 d D . . O4W O 0.4654(3) 0.3400(6) 0.3675(4) 0.087(2) Uani 1 1 d D . . H4A H 0.466(3) 0.407(2) 0.359(5) 0.130 Uiso 1 1 d D . . H4B H 0.505(2) 0.326(4) 0.412(4) 0.130 Uiso 1 1 d D . . O5W O 1.0329(3) 0.3505(5) 0.9463(4) 0.0680(16) Uani 1 1 d D . . H5A H 0.9923(7) 0.322(2) 0.926(3) 0.102 Uiso 1 1 d D . . H5B H 1.046(4) 0.375(7) 0.994(3) 0.102 Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.0204(6) 0.0543(9) 0.0568(8) 0.000 0.0136(6) 0.000 Zn2 0.0739(7) 0.0433(6) 0.0616(7) -0.0116(5) 0.0433(6) -0.0026(5) C1 0.035(4) 0.040(4) 0.044(4) 0.009(4) 0.026(3) 0.001(3) C2 0.048(4) 0.027(4) 0.047(4) 0.007(3) 0.033(4) 0.011(3) C3 0.039(4) 0.031(4) 0.041(4) -0.005(3) 0.022(3) -0.007(3) C4 0.031(3) 0.038(4) 0.034(4) 0.000(3) 0.020(3) 0.000(3) C5 0.040(4) 0.027(4) 0.035(4) 0.000(3) 0.021(3) 0.005(3) C6 0.035(4) 0.035(4) 0.029(4) 0.009(3) 0.018(3) 0.001(3) C7 0.042(4) 0.035(4) 0.036(4) 0.008(3) 0.011(3) -0.008(3) C8 0.041(4) 0.033(4) 0.035(4) -0.001(3) 0.024(3) -0.001(3) C9 0.028(3) 0.037(4) 0.042(4) 0.001(3) 0.018(3) -0.002(3) C10 0.030(3) 0.034(4) 0.039(4) 0.000(3) 0.015(3) -0.003(3) C11 0.032(4) 0.057(5) 0.034(4) 0.008(4) 0.012(3) -0.003(4) C12 0.030(4) 0.046(5) 0.042(4) 0.009(3) 0.016(3) -0.006(3) C13 0.031(3) 0.038(4) 0.027(4) -0.002(3) 0.015(3) -0.006(3) C14 0.029(3) 0.027(4) 0.026(4) 0.004(3) 0.013(3) 0.000(3) C15 0.020(3) 0.031(4) 0.028(3) -0.003(3) 0.012(3) -0.002(3) C16 0.028(3) 0.034(4) 0.024(3) -0.003(3) 0.014(3) -0.004(3) C17 0.021(3) 0.041(4) 0.035(4) -0.012(3) 0.018(3) -0.009(3) C18 0.025(3) 0.033(4) 0.032(4) -0.004(3) 0.014(3) 0.003(3) C19 0.037(4) 0.030(4) 0.031(4) 0.002(3) 0.016(3) 0.002(3) C20 0.031(4) 0.054(5) 0.041(5) -0.012(4) 0.013(4) 0.006(4) C21 0.031(4) 0.036(4) 0.029(4) -0.004(3) 0.017(3) -0.010(3) C22 0.055(5) 0.056(6) 0.053(6) 0.004(5) 0.028(5) -0.002(4) C23 0.035(4) 0.070(6) 0.044(5) 0.004(4) 0.022(4) 0.013(4) N1 0.028(3) 0.034(3) 0.038(3) 0.005(3) 0.017(3) -0.007(2) N2 0.024(3) 0.032(3) 0.027(3) 0.003(2) 0.012(2) -0.004(2) O1 0.073(4) 0.058(4) 0.069(4) -0.019(3) 0.049(4) -0.002(3) O2' 0.060(5) 0.060(5) 0.060(5) 0.0000(10) 0.034(3) 0.0006(10) O2 0.066(3) 0.066(3) 0.067(3) -0.0005(10) 0.037(2) 0.0014(10) O3 0.041(3) 0.086(5) 0.083(5) -0.010(4) 0.030(3) -0.013(3) O4 0.034(3) 0.131(6) 0.047(3) -0.021(4) 0.009(3) 0.032(3) O5 0.037(3) 0.065(4) 0.060(4) 0.009(3) 0.020(3) 0.019(3) O6 0.027(3) 0.073(4) 0.094(5) -0.004(3) 0.023(3) -0.002(3) O7 0.033(3) 0.052(3) 0.046(3) 0.015(2) 0.013(2) -0.002(2) O8 0.042(3) 0.043(3) 0.045(3) 0.011(2) 0.024(2) -0.004(2) O6W' 0.076(4) 0.076(4) 0.076(4) 0.0009(10) 0.043(2) 0.0000(10) O6W 0.060(6) 0.060(6) 0.060(6) 0.0001(10) 0.034(3) -0.0003(10) O7W 0.077(7) 0.076(7) 0.077(7) 0.0000(7) 0.043(4) -0.0001(7) O1W 0.035(3) 0.187(8) 0.132(6) -0.106(6) 0.043(4) -0.030(4) O2W 0.117(5) 0.075(5) 0.047(4) 0.009(3) 0.042(4) 0.039(4) O3W 0.218(10) 0.052(5) 0.318(14) -0.039(7) 0.234(11) -0.030(6) O4W 0.073(4) 0.125(6) 0.078(5) 0.024(4) 0.053(4) 0.026(4) O5W 0.059(3) 0.072(4) 0.072(4) 0.003(3) 0.036(3) 0.007(3) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 O1W 2.006(6) . ? Zn1 O1W 2.006(6) 2 ? Zn1 O5 2.120(5) . ? Zn1 O5 2.120(5) 2 ? Zn1 O6 2.259(6) 2 ? Zn1 O6 2.259(6) . ? Zn1 C20 2.521(7) 2 ? Zn1 C20 2.521(7) . ? Zn2 O3W 1.960(8) . ? Zn2 O2W 1.980(6) . ? Zn2 O1 2.031(5) . ? Zn2 O8 2.073(5) 2_666 ? Zn2 O7 2.359(5) 2_666 ? Zn2 O2' 2.469(16) . ? Zn2 C21 2.545(7) 2_666 ? Zn2 C22 2.591(9) . ? C1 C6 1.364(9) . ? C1 C2 1.375(10) . ? C1 H1 0.9300 . ? C2 C3 1.377(9) . ? C2 C22 1.509(11) . ? C3 C4 1.389(9) . ? C3 H3 0.9300 . ? C4 C5 1.371(9) . ? C4 C23 1.520(9) . ? C5 C6 1.387(9) . ? C5 H5 0.9300 . ? C6 C7 1.500(9) . ? C7 N1 1.486(8) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 N2 1.486(8) 5_666 ? C8 C9 1.499(9) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 N1 1.452(8) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 N1 1.458(8) . ? C10 C11 1.505(10) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 C12 1.508(9) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 N2 1.507(8) . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C13 C14 1.494(9) . ? C13 N2 1.506(8) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 C19 1.378(8) . ? C14 C15 1.378(9) . ? C15 C16 1.377(8) . ? C15 H15 0.9300 . ? C16 C17 1.393(8) . ? C16 C21 1.484(9) . ? C17 C18 1.367(9) . ? C17 H17 0.9300 . ? C18 C19 1.393(9) . ? C18 C20 1.488(9) . ? C19 H19 0.9300 . ? C20 O6 1.224(9) . ? C20 O5 1.252(9) . ? C21 O7 1.240(7) . ? C21 O8 1.252(7) . ? C21 Zn2 2.545(7) 2_646 ? C22 O1 1.229(9) . ? C22 O2' 1.260(17) . ? C22 O2 1.267(13) . ? C23 O3 1.222(10) . ? C23 O4 1.236(9) . ? N2 C8 1.486(8) 5_666 ? O2' O2 0.665(17) . ? O4 H4 0.8200 . ? O7 Zn2 2.359(5) 2_646 ? O8 Zn2 2.073(5) 2_646 ? O6W' O6W 0.95(2) . ? O7W O7W 0.99(4) 2_656 ? O1W H1A 0.902(10) . ? O1W H1B 0.900(10) . ? O2W H2A 0.902(11) . ? O2W H2B 0.901(10) . ? O3W H3A 0.897(10) . ? O3W H3B 0.896(10) . ? O4W H4A 0.898(10) . ? O4W H4B 0.898(10) . ? O5W H5A 0.897(10) . ? O5W H5B 0.900(10) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1W Zn1 O1W 118.9(6) . 2 ? O1W Zn1 O5 92.2(2) . . ? O1W Zn1 O5 86.3(2) 2 . ? O1W Zn1 O5 86.3(2) . 2 ? O1W Zn1 O5 92.2(2) 2 2 ? O5 Zn1 O5 177.1(3) . 2 ? O1W Zn1 O6 135.2(3) . 2 ? O1W Zn1 O6 91.6(3) 2 2 ? O5 Zn1 O6 123.7(2) . 2 ? O5 Zn1 O6 58.8(2) 2 2 ? O1W Zn1 O6 91.6(3) . . ? O1W Zn1 O6 135.2(3) 2 . ? O5 Zn1 O6 58.8(2) . . ? O5 Zn1 O6 123.7(2) 2 . ? O6 Zn1 O6 86.8(3) 2 . ? O1W Zn1 C20 112.3(3) . 2 ? O1W Zn1 C20 91.7(3) 2 2 ? O5 Zn1 C20 152.7(3) . 2 ? O5 Zn1 C20 29.7(2) 2 2 ? O6 Zn1 C20 29.0(2) 2 2 ? O6 Zn1 C20 106.8(3) . 2 ? O1W Zn1 C20 91.7(3) . . ? O1W Zn1 C20 112.3(3) 2 . ? O5 Zn1 C20 29.7(2) . . ? O5 Zn1 C20 152.7(3) 2 . ? O6 Zn1 C20 106.8(3) 2 . ? O6 Zn1 C20 29.0(2) . . ? C20 Zn1 C20 132.5(4) 2 . ? O3W Zn2 O2W 134.6(4) . . ? O3W Zn2 O1 102.0(3) . . ? O2W Zn2 O1 106.8(3) . . ? O3W Zn2 O8 109.9(3) . 2_666 ? O2W Zn2 O8 98.1(3) . 2_666 ? O1 Zn2 O8 101.1(2) . 2_666 ? O3W Zn2 O7 82.8(2) . 2_666 ? O2W Zn2 O7 82.7(2) . 2_666 ? O1 Zn2 O7 158.8(2) . 2_666 ? O8 Zn2 O7 58.22(17) 2_666 2_666 ? O3W Zn2 O2' 79.0(5) . . ? O2W Zn2 O2' 89.0(4) . . ? O1 Zn2 O2' 55.8(4) . . ? O8 Zn2 O2' 156.9(4) 2_666 . ? O7 Zn2 O2' 144.8(4) 2_666 . ? O3W Zn2 C21 97.4(3) . 2_666 ? O2W Zn2 C21 89.9(2) . 2_666 ? O1 Zn2 C21 130.2(2) . 2_666 ? O8 Zn2 C21 29.25(18) 2_666 2_666 ? O7 Zn2 C21 28.97(17) 2_666 2_666 ? O2' Zn2 C21 173.8(4) . 2_666 ? O3W Zn2 C22 94.2(3) . . ? O2W Zn2 C22 95.5(3) . . ? O1 Zn2 C22 27.6(2) . . ? O8 Zn2 C22 128.2(2) 2_666 . ? O7 Zn2 C22 173.5(2) 2_666 . ? O2' Zn2 C22 28.7(4) . . ? C21 Zn2 C22 157.5(2) 2_666 . ? C6 C1 C2 120.9(6) . . ? C6 C1 H1 119.5 . . ? C2 C1 H1 119.5 . . ? C3 C2 C1 120.4(6) . . ? C3 C2 C22 122.7(7) . . ? C1 C2 C22 116.8(6) . . ? C2 C3 C4 119.4(6) . . ? C2 C3 H3 120.3 . . ? C4 C3 H3 120.3 . . ? C5 C4 C3 119.2(6) . . ? C5 C4 C23 120.1(6) . . ? C3 C4 C23 120.5(6) . . ? C4 C5 C6 121.4(6) . . ? C4 C5 H5 119.3 . . ? C6 C5 H5 119.3 . . ? C1 C6 C5 118.6(6) . . ? C1 C6 C7 120.6(6) . . ? C5 C6 C7 120.8(6) . . ? N1 C7 C6 109.7(5) . . ? N1 C7 H7A 109.7 . . ? C6 C7 H7A 109.7 . . ? N1 C7 H7B 109.7 . . ? C6 C7 H7B 109.7 . . ? H7A C7 H7B 108.2 . . ? N2 C8 C9 112.7(5) 5_666 . ? N2 C8 H8A 109.1 5_666 . ? C9 C8 H8A 109.1 . . ? N2 C8 H8B 109.1 5_666 . ? C9 C8 H8B 109.1 . . ? H8A C8 H8B 107.8 . . ? N1 C9 C8 112.5(5) . . ? N1 C9 H9A 109.1 . . ? C8 C9 H9A 109.1 . . ? N1 C9 H9B 109.1 . . ? C8 C9 H9B 109.1 . . ? H9A C9 H9B 107.8 . . ? N1 C10 C11 113.4(6) . . ? N1 C10 H10A 108.9 . . ? C11 C10 H10A 108.9 . . ? N1 C10 H10B 108.9 . . ? C11 C10 H10B 108.9 . . ? H10A C10 H10B 107.7 . . ? C10 C11 C12 114.3(6) . . ? C10 C11 H11A 108.7 . . ? C12 C11 H11A 108.7 . . ? C10 C11 H11B 108.7 . . ? C12 C11 H11B 108.7 . . ? H11A C11 H11B 107.6 . . ? N2 C12 C11 115.0(6) . . ? N2 C12 H12A 108.5 . . ? C11 C12 H12A 108.5 . . ? N2 C12 H12B 108.5 . . ? C11 C12 H12B 108.5 . . ? H12A C12 H12B 107.5 . . ? C14 C13 N2 115.7(5) . . ? C14 C13 H13A 108.4 . . ? N2 C13 H13A 108.4 . . ? C14 C13 H13B 108.4 . . ? N2 C13 H13B 108.4 . . ? H13A C13 H13B 107.4 . . ? C19 C14 C15 117.8(6) . . ? C19 C14 C13 120.9(6) . . ? C15 C14 C13 121.1(6) . . ? C16 C15 C14 121.9(6) . . ? C16 C15 H15 119.1 . . ? C14 C15 H15 119.1 . . ? C15 C16 C17 119.1(6) . . ? C15 C16 C21 119.5(6) . . ? C17 C16 C21 121.3(6) . . ? C18 C17 C16 120.2(6) . . ? C18 C17 H17 119.9 . . ? C16 C17 H17 119.9 . . ? C17 C18 C19 119.3(6) . . ? C17 C18 C20 119.7(6) . . ? C19 C18 C20 121.0(7) . . ? C14 C19 C18 121.6(6) . . ? C14 C19 H19 119.2 . . ? C18 C19 H19 119.2 . . ? O6 C20 O5 120.6(7) . . ? O6 C20 C18 121.1(8) . . ? O5 C20 C18 118.3(7) . . ? O6 C20 Zn1 63.5(4) . . ? O5 C20 Zn1 57.1(4) . . ? C18 C20 Zn1 174.8(6) . . ? O7 C21 O8 121.1(6) . . ? O7 C21 C16 118.8(6) . . ? O8 C21 C16 120.1(6) . . ? O7 C21 Zn2 67.2(4) . 2_646 ? O8 C21 Zn2 54.0(3) . 2_646 ? C16 C21 Zn2 173.9(5) . 2_646 ? O1 C22 O2' 118.8(11) . . ? O1 C22 O2 122.7(9) . . ? O2' C22 O2 30.5(8) . . ? O1 C22 C2 118.0(7) . . ? O2' C22 C2 120.2(10) . . ? O2 C22 C2 117.4(9) . . ? O1 C22 Zn2 49.9(4) . . ? O2' C22 Zn2 70.3(8) . . ? O2 C22 Zn2 75.1(6) . . ? C2 C22 Zn2 167.4(6) . . ? O3 C23 O4 125.0(7) . . ? O3 C23 C4 119.2(7) . . ? O4 C23 C4 115.8(8) . . ? C9 N1 C10 111.2(5) . . ? C9 N1 C7 110.0(5) . . ? C10 N1 C7 110.6(5) . . ? C8 N2 C13 113.8(5) 5_666 . ? C8 N2 C12 111.5(5) 5_666 . ? C13 N2 C12 110.6(5) . . ? C22 O1 Zn2 102.5(5) . . ? O2 O2' C22 75(2) . . ? O2 O2' Zn2 92(2) . . ? C22 O2' Zn2 81.0(9) . . ? O2' O2 C22 74(2) . . ? C23 O4 H4 109.5 . . ? C20 O5 Zn1 93.1(5) . . ? C20 O6 Zn1 87.5(5) . . ? C21 O7 Zn2 83.9(4) . 2_646 ? C21 O8 Zn2 96.8(4) . 2_646 ? Zn1 O1W H1A 131(7) . . ? Zn1 O1W H1B 113.3(12) . . ? H1A O1W H1B 105.9(16) . . ? Zn2 O2W H2A 130(5) . . ? Zn2 O2W H2B 115.1(12) . . ? H2A O2W H2B 109.2(15) . . ? Zn2 O3W H3A 117.3(14) . . ? Zn2 O3W H3B 117.4(14) . . ? H3A O3W H3B 107.1(17) . . ? H4A O4W H4B 106.6(17) . . ? H5A O5W H5B 106.5(17) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C6 C1 C2 C3 -1.7(10) . . . . ? C6 C1 C2 C22 174.3(6) . . . . ? C1 C2 C3 C4 0.4(10) . . . . ? C22 C2 C3 C4 -175.4(7) . . . . ? C2 C3 C4 C5 0.3(10) . . . . ? C2 C3 C4 C23 176.5(6) . . . . ? C3 C4 C5 C6 0.3(10) . . . . ? C23 C4 C5 C6 -175.9(6) . . . . ? C2 C1 C6 C5 2.3(10) . . . . ? C2 C1 C6 C7 -176.2(6) . . . . ? C4 C5 C6 C1 -1.6(10) . . . . ? C4 C5 C6 C7 176.9(6) . . . . ? C1 C6 C7 N1 67.0(8) . . . . ? C5 C6 C7 N1 -111.5(7) . . . . ? N2 C8 C9 N1 48.2(7) 5_666 . . . ? N1 C10 C11 C12 170.0(6) . . . . ? C10 C11 C12 N2 -68.3(8) . . . . ? N2 C13 C14 C19 107.1(7) . . . . ? N2 C13 C14 C15 -78.4(8) . . . . ? C19 C14 C15 C16 0.4(9) . . . . ? C13 C14 C15 C16 -174.2(6) . . . . ? C14 C15 C16 C17 1.2(9) . . . . ? C14 C15 C16 C21 -178.9(6) . . . . ? C15 C16 C17 C18 -1.6(9) . . . . ? C21 C16 C17 C18 178.5(6) . . . . ? C16 C17 C18 C19 0.4(9) . . . . ? C16 C17 C18 C20 179.6(6) . . . . ? C15 C14 C19 C18 -1.7(10) . . . . ? C13 C14 C19 C18 173.0(6) . . . . ? C17 C18 C19 C14 1.2(10) . . . . ? C20 C18 C19 C14 -177.9(6) . . . . ? C17 C18 C20 O6 -3.6(10) . . . . ? C19 C18 C20 O6 175.6(7) . . . . ? C17 C18 C20 O5 175.4(6) . . . . ? C19 C18 C20 O5 -5.4(10) . . . . ? C17 C18 C20 Zn1 147(6) . . . . ? C19 C18 C20 Zn1 -34(6) . . . . ? O1W Zn1 C20 O6 90.3(5) . . . . ? O1W Zn1 C20 O6 -147.4(5) 2 . . . ? O5 Zn1 C20 O6 -178.2(8) . . . . ? O5 Zn1 C20 O6 5.1(8) 2 . . . ? O6 Zn1 C20 O6 -48.4(6) 2 . . . ? C20 Zn1 C20 O6 -32.5(4) 2 . . . ? O1W Zn1 C20 O5 -91.5(5) . . . . ? O1W Zn1 C20 O5 30.8(6) 2 . . . ? O5 Zn1 C20 O5 -176.8(4) 2 . . . ? O6 Zn1 C20 O5 129.8(4) 2 . . . ? O6 Zn1 C20 O5 178.2(8) . . . . ? C20 Zn1 C20 O5 145.6(5) 2 . . . ? O1W Zn1 C20 C18 -62(6) . . . . ? O1W Zn1 C20 C18 60(6) 2 . . . ? O5 Zn1 C20 C18 30(6) . . . . ? O5 Zn1 C20 C18 -147(6) 2 . . . ? O6 Zn1 C20 C18 159(6) 2 . . . ? O6 Zn1 C20 C18 -152(6) . . . . ? C20 Zn1 C20 C18 175(6) 2 . . . ? C15 C16 C21 O7 10.7(9) . . . . ? C17 C16 C21 O7 -169.4(6) . . . . ? C15 C16 C21 O8 -169.3(6) . . . . ? C17 C16 C21 O8 10.7(9) . . . . ? C15 C16 C21 Zn2 177(4) . . . 2_646 ? C17 C16 C21 Zn2 -3(5) . . . 2_646 ? C3 C2 C22 O1 -22.5(11) . . . . ? C1 C2 C22 O1 161.6(7) . . . . ? C3 C2 C22 O2' 177.4(12) . . . . ? C1 C2 C22 O2' 1.5(14) . . . . ? C3 C2 C22 O2 142.6(10) . . . . ? C1 C2 C22 O2 -33.3(12) . . . . ? C3 C2 C22 Zn2 -38(3) . . . . ? C1 C2 C22 Zn2 146(2) . . . . ? O3W Zn2 C22 O1 -108.0(6) . . . . ? O2W Zn2 C22 O1 116.3(6) . . . . ? O8 Zn2 C22 O1 11.5(7) 2_666 . . . ? O7 Zn2 C22 O1 -170.3(18) 2_666 . . . ? O2' Zn2 C22 O1 -165.9(12) . . . . ? C21 Zn2 C22 O1 13.0(10) 2_666 . . . ? O3W Zn2 C22 O2' 57.8(10) . . . . ? O2W Zn2 C22 O2' -77.8(10) . . . . ? O1 Zn2 C22 O2' 165.9(12) . . . . ? O8 Zn2 C22 O2' 177.4(9) 2_666 . . . ? O7 Zn2 C22 O2' -4(3) 2_666 . . . ? C21 Zn2 C22 O2' 178.9(9) 2_666 . . . ? O3W Zn2 C22 O2 89.4(8) . . . . ? O2W Zn2 C22 O2 -46.2(7) . . . . ? O1 Zn2 C22 O2 -162.5(10) . . . . ? O8 Zn2 C22 O2 -151.0(7) 2_666 . . . ? O7 Zn2 C22 O2 27(2) 2_666 . . . ? O2' Zn2 C22 O2 31.6(9) . . . . ? C21 Zn2 C22 O2 -149.5(8) 2_666 . . . ? O3W Zn2 C22 C2 -90(3) . . . . ? O2W Zn2 C22 C2 135(3) . . . . ? O1 Zn2 C22 C2 18(2) . . . . ? O8 Zn2 C22 C2 30(3) 2_666 . . . ? O7 Zn2 C22 C2 -152(2) 2_666 . . . ? O2' Zn2 C22 C2 -148(3) . . . . ? C21 Zn2 C22 C2 31(3) 2_666 . . . ? C5 C4 C23 O3 176.5(7) . . . . ? C3 C4 C23 O3 0.3(11) . . . . ? C5 C4 C23 O4 -1.7(10) . . . . ? C3 C4 C23 O4 -177.9(7) . . . . ? C8 C9 N1 C10 74.9(7) . . . . ? C8 C9 N1 C7 -162.2(6) . . . . ? C11 C10 N1 C9 -174.2(6) . . . . ? C11 C10 N1 C7 63.2(7) . . . . ? C6 C7 N1 C9 65.7(7) . . . . ? C6 C7 N1 C10 -171.0(6) . . . . ? C14 C13 N2 C8 -58.4(7) . . . 5_666 ? C14 C13 N2 C12 68.0(7) . . . . ? C11 C12 N2 C8 -65.3(7) . . . 5_666 ? C11 C12 N2 C13 167.0(6) . . . . ? O2' C22 O1 Zn2 -15.2(13) . . . . ? O2 C22 O1 Zn2 20.2(12) . . . . ? C2 C22 O1 Zn2 -175.6(6) . . . . ? O3W Zn2 O1 C22 75.8(6) . . . . ? O2W Zn2 O1 C22 -68.8(6) . . . . ? O8 Zn2 O1 C22 -170.8(5) 2_666 . . . ? O7 Zn2 O1 C22 177.0(6) 2_666 . . . ? O2' Zn2 O1 C22 8.1(7) . . . . ? C21 Zn2 O1 C22 -173.5(5) 2_666 . . . ? O1 C22 O2' O2 106(2) . . . . ? C2 C22 O2' O2 -94(2) . . . . ? Zn2 C22 O2' O2 94.1(19) . . . . ? O1 C22 O2' Zn2 12.3(10) . . . . ? O2 C22 O2' Zn2 -94.1(19) . . . . ? C2 C22 O2' Zn2 172.3(8) . . . . ? O3W Zn2 O2' O2 164(2) . . . . ? O2W Zn2 O2' O2 28(2) . . . . ? O1 Zn2 O2' O2 -83(2) . . . . ? O8 Zn2 O2' O2 -80(2) 2_666 . . . ? O7 Zn2 O2' O2 104(2) 2_666 . . . ? C21 Zn2 O2' O2 109(4) 2_666 . . . ? C22 Zn2 O2' O2 -75(2) . . . . ? O3W Zn2 O2' C22 -120.7(10) . . . . ? O2W Zn2 O2' C22 103.3(9) . . . . ? O1 Zn2 O2' C22 -7.9(7) . . . . ? O8 Zn2 O2' C22 -5.2(18) 2_666 . . . ? O7 Zn2 O2' C22 179.1(5) 2_666 . . . ? C21 Zn2 O2' C22 -176(3) 2_666 . . . ? Zn2 O2' O2 C22 80.3(7) . . . . ? O1 C22 O2 O2' -92(2) . . . . ? C2 C22 O2 O2' 104(2) . . . . ? Zn2 C22 O2 O2' -76.2(19) . . . . ? O6 C20 O5 Zn1 1.9(8) . . . . ? C18 C20 O5 Zn1 -177.1(5) . . . . ? O1W Zn1 O5 C20 89.5(5) . . . . ? O1W Zn1 O5 C20 -151.7(5) 2 . . . ? O5 Zn1 O5 C20 148.9(4) 2 . . . ? O6 Zn1 O5 C20 -62.2(5) 2 . . . ? O6 Zn1 O5 C20 -1.0(4) . . . . ? C20 Zn1 O5 C20 -65.1(9) 2 . . . ? O5 C20 O6 Zn1 -1.8(7) . . . . ? C18 C20 O6 Zn1 177.2(6) . . . . ? O1W Zn1 O6 C20 -90.5(5) . . . . ? O1W Zn1 O6 C20 45.1(7) 2 . . . ? O5 Zn1 O6 C20 1.1(4) . . . . ? O5 Zn1 O6 C20 -177.2(4) 2 . . . ? O6 Zn1 O6 C20 134.2(6) 2 . . . ? C20 Zn1 O6 C20 155.5(4) 2 . . . ? O8 C21 O7 Zn2 -1.6(6) . . . 2_646 ? C16 C21 O7 Zn2 178.5(6) . . . 2_646 ? O7 C21 O8 Zn2 1.8(7) . . . 2_646 ? C16 C21 O8 Zn2 -178.2(5) . . . 2_646 ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 1.470 _refine_diff_density_min -1.267 _refine_diff_density_rms 0.099 #=========================END data_Compound-4 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C46 H54 Co3 N4 O22, 5.75H2O' _chemical_formula_sum 'C46 H65.50 Co3 N4 O27.75' _chemical_formula_weight 1295.31 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Co' 'Co' 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' _symmetry_space_group_name_hall '-C 2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 23.792(2) _cell_length_b 13.0153(5) _cell_length_c 20.729(2) _cell_angle_alpha 90.00 _cell_angle_beta 123.785(13) _cell_angle_gamma 90.00 _cell_volume 5334.9(7) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 3123 _cell_measurement_theta_min 3.0491 _cell_measurement_theta_max 29.1566 _exptl_crystal_description block _exptl_crystal_colour purple _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.613 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2690 _exptl_absorpt_coefficient_mu 1.018 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7922 _exptl_absorpt_correction_T_max 0.8540 _exptl_absorpt_process_details ; CrysAlis (Oxford Diffraction, 2006) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Diffraction Gemini R Ultra' _diffrn_measurement_method '\w scan' _diffrn_detector_area_resol_mean 10.0 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15495 _diffrn_reflns_av_R_equivalents 0.0650 _diffrn_reflns_av_sigmaI/netI 0.0850 _diffrn_reflns_limit_h_min -28 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 3.44 _diffrn_reflns_theta_max 25.35 _reflns_number_total 4762 _reflns_number_gt 2937 _reflns_threshold_expression >2\s(I) _computing_data_collection 'CrysAlisPro(1.171.35.21) (Agilent Tech., 2012)' _computing_cell_refinement 'CrysAlisPro(1.171.35.21) (Agilent Tech., 2012)' _computing_data_reduction 'CrysAlisPro(1.171.35.21) (Agilent Tech., 2012)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0100P)^2^+90.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4762 _refine_ls_number_parameters 422 _refine_ls_number_restraints 51 _refine_ls_R_factor_all 0.1380 _refine_ls_R_factor_gt 0.0892 _refine_ls_wR_factor_ref 0.1843 _refine_ls_wR_factor_gt 0.1607 _refine_ls_goodness_of_fit_ref 0.974 _refine_ls_restrained_S_all 0.971 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 1.0000 0.15562(11) 0.2500 0.0451(4) Uani 1 2 d S . . Co2 Co 0.68434(7) 0.62934(8) -0.09543(7) 0.0603(4) Uani 1 1 d D . . C1 C 0.8121(3) 0.2681(5) 0.1317(4) 0.0307(14) Uani 1 1 d . . . C2 C 0.7635(3) 0.2191(5) 0.1374(4) 0.0317(14) Uani 1 1 d . . . H2 H 0.7754 0.1614 0.1689 0.038 Uiso 1 1 calc R . . C3 C 0.6987(3) 0.2538(5) 0.0979(3) 0.0285(14) Uani 1 1 d . . . C4 C 0.6819(3) 0.3387(5) 0.0500(4) 0.0322(14) Uani 1 1 d . . . H4 H 0.6378 0.3634 0.0224 0.039 Uiso 1 1 calc R . . C5 C 0.7296(3) 0.3870(5) 0.0427(4) 0.0285(14) Uani 1 1 d . . . C6 C 0.7952(3) 0.3519(5) 0.0853(4) 0.0341(15) Uani 1 1 d . . . H6 H 0.8281 0.3857 0.0823 0.041 Uiso 1 1 calc R . . C7 C 0.6472(3) 0.2067(5) 0.1097(4) 0.0324(15) Uani 1 1 d . . . H7A H 0.6242 0.2617 0.1178 0.039 Uiso 1 1 calc R . . H7B H 0.6710 0.1659 0.1568 0.039 Uiso 1 1 calc R . . C8 C 0.8839(3) 0.2301(6) 0.1779(4) 0.0396(17) Uani 1 1 d . . . C9 C 0.7098(3) 0.4775(5) -0.0101(4) 0.0325(15) Uani 1 1 d . . . C10 C 0.4370(3) 0.1236(5) -0.0672(4) 0.0370(16) Uani 1 1 d . . . H10A H 0.4616 0.0921 -0.0162 0.044 Uiso 1 1 calc R . . H10B H 0.4176 0.1873 -0.0639 0.044 Uiso 1 1 calc R . . C11 C 0.4851(3) 0.1471(6) -0.0899(4) 0.0426(17) Uani 1 1 d . . . H11A H 0.4622 0.1889 -0.1365 0.051 Uiso 1 1 calc R . . H11B H 0.4983 0.0833 -0.1022 0.051 Uiso 1 1 calc R . . C12 C 0.5486(3) 0.2030(5) -0.0272(4) 0.0387(16) Uani 1 1 d . . . H12A H 0.5738 0.2248 -0.0488 0.046 Uiso 1 1 calc R . . H12B H 0.5352 0.2643 -0.0123 0.046 Uiso 1 1 calc R . . C13 C 0.6232(4) 0.0518(5) 0.0271(4) 0.0375(16) Uani 1 1 d . . . H13A H 0.6547 0.0775 0.0152 0.045 Uiso 1 1 calc R . . H13B H 0.5870 0.0167 -0.0186 0.045 Uiso 1 1 calc R . . C14 C 0.6588(3) -0.0233(5) 0.0920(4) 0.0393(16) Uani 1 1 d . . . H14A H 0.6701 -0.0838 0.0741 0.047 Uiso 1 1 calc R . . H14B H 0.7008 0.0070 0.1338 0.047 Uiso 1 1 calc R . . C15 C 0.6603(4) -0.1044(5) 0.1982(4) 0.0438(18) Uani 1 1 d . . . H15A H 0.6832 -0.1629 0.1938 0.053 Uiso 1 1 calc R . . H15B H 0.6320 -0.1293 0.2149 0.053 Uiso 1 1 calc R . . C16 C 0.7117(3) -0.0305(5) 0.2575(4) 0.0353(15) Uani 1 1 d . . . C17 C 0.6919(3) 0.0527(5) 0.2800(4) 0.0394(16) Uani 1 1 d . . . H17 H 0.6462 0.0614 0.2596 0.047 Uiso 1 1 calc R . . C18 C 0.7373(3) 0.1246(5) 0.3322(4) 0.0371(16) Uani 1 1 d . . . C19 C 0.8045(3) 0.1109(5) 0.3611(4) 0.0394(16) Uani 1 1 d . . . H19 H 0.8356 0.1586 0.3964 0.047 Uiso 1 1 calc R . . C20 C 0.8279(3) 0.0283(5) 0.3395(4) 0.0355(15) Uani 1 1 d . . . C21 C 0.7805(3) -0.0415(5) 0.2883(4) 0.0361(15) Uani 1 1 d . . . H21 H 0.7948 -0.0980 0.2737 0.043 Uiso 1 1 calc R . . C22 C 0.8996(4) 0.0155(7) 0.3673(5) 0.0507(19) Uani 1 1 d . . . C23 C 0.7124(4) 0.2152(6) 0.3514(5) 0.053(2) Uani 1 1 d . . . N1 N 0.5944(2) 0.1397(4) 0.0445(3) 0.0308(12) Uani 1 1 d . . . N2 N 0.6179(3) -0.0545(4) 0.1222(3) 0.0348(13) Uani 1 1 d . . . O1 O 0.8983(2) 0.1506(4) 0.2170(3) 0.0475(12) Uani 1 1 d . . . O2 O 0.9286(3) 0.2776(4) 0.1765(3) 0.0614(15) Uani 1 1 d . . . O3 O 0.7539(2) 0.5319(4) -0.0068(3) 0.0444(12) Uani 1 1 d . . . O4 O 0.6486(2) 0.4967(4) -0.0570(3) 0.0451(12) Uani 1 1 d . . . O5 O 0.9156(3) -0.0581(5) 0.3429(3) 0.0746(19) Uani 1 1 d . . . O6 O 0.9405(3) 0.0815(5) 0.4117(4) 0.0773(19) Uani 1 1 d . . . H6A H 0.9752 0.0774 0.4123 0.116 Uiso 1 1 calc R . . O7W O 0.5000 0.730(2) -0.2500 0.161(12) Uani 0.50 2 d SP . . O7 O 0.6526(4) 0.2380(5) 0.3126(5) 0.091(2) Uani 1 1 d . . . O8 O 0.7516(3) 0.2691(4) 0.4074(3) 0.0629(15) Uani 1 1 d . . . O6W O 0.4059(9) 0.9262(14) -0.3767(11) 0.040(4) Uani 0.25 1 d PU . . O8W O 0.4971(13) 0.816(2) -0.3038(16) 0.014(6) Uani 0.13 1 d PU . . O9W O 0.5138(19) 1.020(2) -0.259(2) 0.118(11) Uani 0.25 1 d PU . . O1W O 1.0265(5) 0.0949(9) 0.3589(6) 0.045(3) Uani 0.50 1 d PU . . O1W' O 1.0210(6) 0.0557(10) 0.3339(8) 0.064(3) Uani 0.50 1 d PU . . O2W O 0.6543(3) 0.5417(5) -0.1871(3) 0.0667(16) Uani 1 1 d D . . H2A H 0.645(5) 0.476(2) -0.184(3) 0.100 Uiso 1 1 d D . . H2B H 0.640(5) 0.552(2) -0.2369(16) 0.100 Uiso 1 1 d D . . O3W O 0.6437(3) 0.7156(5) -0.0503(4) 0.0726(17) Uani 1 1 d D . . H3B H 0.6654(10) 0.748(7) -0.003(3) 0.109 Uiso 1 1 d D . . H3A H 0.5990(8) 0.721(6) -0.067(3) 0.109 Uiso 1 1 d D . . O4W O 1.0352(3) -0.1480(6) 0.4493(4) 0.0786(19) Uani 1 1 d D . . H4A H 1.040(5) -0.126(8) 0.493(3) 0.118 Uiso 1 1 d D . . H4B H 1.003(4) -0.108(7) 0.411(3) 0.118 Uiso 1 1 d D . . O5W O 0.5259(5) 0.1437(7) 0.1233(5) 0.107(2) Uani 1 1 d DU . . H5A H 0.529(7) 0.081(3) 0.143(6) 0.161 Uiso 1 1 d D . . H5B H 0.534(7) 0.189(6) 0.160(5) 0.161 Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0236(7) 0.0477(9) 0.0527(9) 0.000 0.0143(7) 0.000 Co2 0.0819(9) 0.0457(6) 0.0621(8) 0.0074(5) 0.0454(7) 0.0004(6) C1 0.022(3) 0.032(3) 0.033(4) -0.007(3) 0.012(3) -0.005(3) C2 0.031(4) 0.031(3) 0.030(4) -0.002(3) 0.015(3) -0.001(3) C3 0.028(3) 0.035(4) 0.023(3) -0.004(3) 0.014(3) -0.003(3) C4 0.027(3) 0.034(4) 0.034(4) -0.004(3) 0.016(3) 0.000(3) C5 0.024(3) 0.034(3) 0.029(3) -0.005(3) 0.016(3) -0.006(3) C6 0.027(3) 0.045(4) 0.034(4) -0.003(3) 0.019(3) -0.006(3) C7 0.026(3) 0.042(4) 0.031(4) -0.002(3) 0.016(3) -0.007(3) C8 0.025(4) 0.051(4) 0.040(4) -0.006(4) 0.016(3) 0.002(3) C9 0.027(4) 0.039(4) 0.030(4) 0.002(3) 0.015(3) -0.001(3) C10 0.027(4) 0.039(4) 0.037(4) 0.001(3) 0.012(3) -0.004(3) C11 0.030(4) 0.051(4) 0.039(4) 0.007(3) 0.014(3) -0.007(3) C12 0.024(3) 0.044(4) 0.036(4) 0.011(3) 0.009(3) -0.003(3) C13 0.043(4) 0.039(4) 0.037(4) -0.004(3) 0.027(4) -0.005(3) C14 0.035(4) 0.036(4) 0.048(4) 0.004(3) 0.023(4) -0.002(3) C15 0.043(4) 0.037(4) 0.034(4) 0.004(3) 0.011(4) -0.010(3) C16 0.035(4) 0.039(4) 0.026(4) 0.007(3) 0.014(3) 0.000(3) C17 0.028(4) 0.049(4) 0.039(4) 0.008(3) 0.018(3) 0.000(3) C18 0.034(4) 0.040(4) 0.042(4) 0.002(3) 0.024(4) 0.002(3) C19 0.038(4) 0.036(4) 0.036(4) -0.006(3) 0.015(3) -0.011(3) C20 0.033(4) 0.038(4) 0.037(4) 0.003(3) 0.020(3) -0.001(3) C21 0.043(4) 0.031(3) 0.034(4) 0.004(3) 0.021(3) 0.006(3) C22 0.042(5) 0.063(5) 0.044(5) -0.003(4) 0.022(4) -0.001(4) C23 0.055(5) 0.052(5) 0.064(6) 0.004(4) 0.040(5) 0.005(4) N1 0.024(3) 0.034(3) 0.029(3) -0.003(2) 0.012(2) -0.004(2) N2 0.032(3) 0.037(3) 0.029(3) 0.006(2) 0.013(3) -0.004(2) O1 0.024(2) 0.054(3) 0.051(3) 0.012(3) 0.012(2) 0.010(2) O2 0.030(3) 0.070(4) 0.078(4) 0.009(3) 0.026(3) 0.000(3) O3 0.038(3) 0.043(3) 0.054(3) 0.009(2) 0.027(3) -0.005(2) O4 0.035(3) 0.050(3) 0.041(3) 0.010(2) 0.015(3) -0.002(2) O5 0.043(3) 0.114(5) 0.047(3) -0.017(3) 0.013(3) 0.030(3) O6 0.040(3) 0.086(5) 0.102(5) -0.014(4) 0.036(4) -0.008(3) O7W 0.17(3) 0.12(2) 0.20(3) 0.000 0.11(3) 0.000 O7 0.075(5) 0.077(5) 0.127(6) -0.010(4) 0.060(5) 0.022(4) O8 0.078(4) 0.047(3) 0.061(4) -0.007(3) 0.038(4) 0.007(3) O6W 0.041(4) 0.040(4) 0.040(4) 0.0002(10) 0.023(3) 0.0002(10) O8W 0.014(6) 0.014(6) 0.014(6) 0.0001(10) 0.008(3) -0.0001(10) O9W 0.118(11) 0.118(11) 0.118(11) 0.0000(10) 0.066(6) 0.0000(10) O1W 0.045(3) 0.045(3) 0.045(3) -0.0004(10) 0.0252(17) 0.0003(10) O1W' 0.064(4) 0.064(4) 0.064(4) 0.0004(10) 0.036(2) -0.0002(10) O2W 0.084(4) 0.067(4) 0.051(4) -0.002(3) 0.039(4) -0.020(3) O3W 0.078(4) 0.064(4) 0.088(5) 0.004(3) 0.055(4) 0.001(3) O4W 0.062(4) 0.099(5) 0.068(4) 0.017(4) 0.032(4) 0.027(4) O5W 0.107(3) 0.110(3) 0.107(3) 0.0012(10) 0.0609(16) -0.0001(10) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 O1W' 1.999(12) 2_755 ? Co1 O1W' 1.999(12) . ? Co1 O1 2.117(4) . ? Co1 O1 2.117(4) 2_755 ? Co1 O1W 2.130(10) 2_755 ? Co1 O1W 2.130(10) . ? Co1 O2 2.202(6) 2_755 ? Co1 O2 2.202(6) . ? Co1 C8 2.492(7) 2_755 ? Co1 C8 2.492(7) . ? Co2 O2W 1.977(6) . ? Co2 O3W 2.020(6) . ? Co2 O8 2.051(6) 6_565 ? Co2 O3 2.083(5) . ? Co2 O4 2.256(5) . ? Co2 O7 2.364(7) 6_565 ? Co2 C9 2.492(6) . ? C1 C6 1.359(9) . ? C1 C2 1.381(8) . ? C1 C8 1.503(9) . ? C2 C3 1.361(9) . ? C2 H2 0.9300 . ? C3 C4 1.387(9) . ? C3 C7 1.507(8) . ? C4 C5 1.377(8) . ? C4 H4 0.9300 . ? C5 C6 1.376(9) . ? C5 C9 1.495(9) . ? C6 H6 0.9300 . ? C7 N1 1.508(8) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 O1 1.239(8) . ? C8 O2 1.243(8) . ? C9 O4 1.247(7) . ? C9 O3 1.235(7) . ? C10 N2 1.469(8) 5_655 ? C10 C11 1.492(9) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 C12 1.522(9) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 N1 1.508(8) . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C13 N1 1.476(8) . ? C13 C14 1.489(9) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 N2 1.476(8) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 N2 1.467(8) . ? C15 C16 1.503(9) . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 C17 1.363(9) . ? C16 C21 1.393(9) . ? C17 C18 1.383(9) . ? C17 H17 0.9300 . ? C18 C19 1.371(9) . ? C18 C23 1.471(10) . ? C19 C20 1.395(9) . ? C19 H19 0.9300 . ? C20 C21 1.375(9) . ? C20 C22 1.476(10) . ? C21 H21 0.9300 . ? C22 O6 1.239(9) . ? C22 O5 1.238(9) . ? C23 O7 1.220(10) . ? C23 O8 1.227(10) . ? N2 C10 1.469(8) 5_655 ? O6 H6A 0.8200 . ? O7W O8W 1.56(3) . ? O7W O8W 1.56(3) 2_654 ? O7 Co2 2.364(7) 6_566 ? O8 Co2 2.051(6) 6_566 ? O9W O9W 0.91(6) 2_654 ? O1W O1W' 0.687(14) . ? O2W H2A 0.899(10) . ? O2W H2B 0.901(10) . ? O3W H3B 0.918(9) . ? O3W H3A 0.919(9) . ? O4W H4A 0.899(10) . ? O4W H4B 0.899(10) . ? O5W H5A 0.895(10) . ? O5W H5B 0.896(10) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1W' Co1 O1W' 98.9(8) 2_755 . ? O1W' Co1 O1 90.6(4) 2_755 . ? O1W' Co1 O1 87.1(4) . . ? O1W' Co1 O1 87.1(4) 2_755 2_755 ? O1W' Co1 O1 90.6(4) . 2_755 ? O1 Co1 O1 176.5(3) . 2_755 ? O1W' Co1 O1W 18.8(4) 2_755 2_755 ? O1W' Co1 O1W 117.7(6) . 2_755 ? O1 Co1 O1W 92.0(3) . 2_755 ? O1 Co1 O1W 86.7(3) 2_755 2_755 ? O1W' Co1 O1W 117.7(6) 2_755 . ? O1W' Co1 O1W 18.8(4) . . ? O1 Co1 O1W 86.7(3) . . ? O1 Co1 O1W 92.0(3) 2_755 . ? O1W Co1 O1W 136.5(6) 2_755 . ? O1W' Co1 O2 142.6(4) 2_755 2_755 ? O1W' Co1 O2 98.3(4) . 2_755 ? O1 Co1 O2 123.3(2) . 2_755 ? O1 Co1 O2 59.68(19) 2_755 2_755 ? O1W Co1 O2 131.3(3) 2_755 2_755 ? O1W Co1 O2 82.8(3) . 2_755 ? O1W' Co1 O2 98.3(4) 2_755 . ? O1W' Co1 O2 142.6(4) . . ? O1 Co1 O2 59.68(19) . . ? O1 Co1 O2 123.3(2) 2_755 . ? O1W Co1 O2 82.8(3) 2_755 . ? O1W Co1 O2 131.3(3) . . ? O2 Co1 O2 87.8(3) 2_755 . ? O1W' Co1 C8 115.6(4) 2_755 2_755 ? O1W' Co1 C8 94.2(4) . 2_755 ? O1 Co1 C8 153.1(2) . 2_755 ? O1 Co1 C8 29.8(2) 2_755 2_755 ? O1W Co1 C8 110.9(3) 2_755 2_755 ? O1W Co1 C8 86.1(3) . 2_755 ? O2 Co1 C8 29.9(2) 2_755 2_755 ? O2 Co1 C8 107.8(2) . 2_755 ? O1W' Co1 C8 94.2(4) 2_755 . ? O1W' Co1 C8 115.6(4) . . ? O1 Co1 C8 29.8(2) . . ? O1 Co1 C8 153.1(2) 2_755 . ? O1W Co1 C8 86.1(3) 2_755 . ? O1W Co1 C8 110.9(3) . . ? O2 Co1 C8 107.8(2) 2_755 . ? O2 Co1 C8 29.9(2) . . ? C8 Co1 C8 134.2(3) 2_755 . ? O2W Co2 O3W 139.1(3) . . ? O2W Co2 O8 105.0(2) . 6_565 ? O3W Co2 O8 101.3(2) . 6_565 ? O2W Co2 O3 100.5(2) . . ? O3W Co2 O3 106.2(2) . . ? O8 Co2 O3 98.2(2) 6_565 . ? O2W Co2 O4 83.8(2) . . ? O3W Co2 O4 83.7(2) . . ? O8 Co2 O4 157.5(2) 6_565 . ? O3 Co2 O4 59.57(17) . . ? O2W Co2 O7 82.2(3) . 6_565 ? O3W Co2 O7 87.0(3) . 6_565 ? O8 Co2 O7 56.4(2) 6_565 6_565 ? O3 Co2 O7 153.7(2) . 6_565 ? O4 Co2 O7 146.1(2) . 6_565 ? O2W Co2 C9 92.3(2) . . ? O3W Co2 C9 95.8(2) . . ? O8 Co2 C9 127.8(2) 6_565 . ? O3 Co2 C9 29.64(18) . . ? O4 Co2 C9 29.93(18) . . ? O7 Co2 C9 174.0(2) 6_565 . ? C6 C1 C2 119.9(6) . . ? C6 C1 C8 120.0(6) . . ? C2 C1 C8 120.1(6) . . ? C3 C2 C1 121.2(6) . . ? C3 C2 H2 119.4 . . ? C1 C2 H2 119.4 . . ? C2 C3 C4 118.3(6) . . ? C2 C3 C7 121.3(6) . . ? C4 C3 C7 120.3(6) . . ? C3 C4 C5 121.1(6) . . ? C3 C4 H4 119.5 . . ? C5 C4 H4 119.5 . . ? C6 C5 C4 119.2(6) . . ? C6 C5 C9 120.9(5) . . ? C4 C5 C9 119.9(6) . . ? C5 C6 C1 120.3(6) . . ? C5 C6 H6 119.9 . . ? C1 C6 H6 119.9 . . ? C3 C7 N1 115.9(5) . . ? C3 C7 H7A 108.3 . . ? N1 C7 H7A 108.3 . . ? C3 C7 H7B 108.3 . . ? N1 C7 H7B 108.3 . . ? H7A C7 H7B 107.4 . . ? O1 C8 O2 120.0(6) . . ? O1 C8 C1 119.7(6) . . ? O2 C8 C1 120.3(7) . . ? O1 C8 Co1 58.1(3) . . ? O2 C8 Co1 62.0(4) . . ? C1 C8 Co1 176.1(5) . . ? O4 C9 O3 121.0(6) . . ? O4 C9 C5 119.0(5) . . ? O3 C9 C5 120.0(6) . . ? O4 C9 Co2 64.5(3) . . ? O3 C9 Co2 56.5(3) . . ? C5 C9 Co2 176.5(4) . . ? N2 C10 C11 112.9(6) 5_655 . ? N2 C10 H10A 109.0 5_655 . ? C11 C10 H10A 109.0 . . ? N2 C10 H10B 109.0 5_655 . ? C11 C10 H10B 109.0 . . ? H10A C10 H10B 107.8 . . ? C10 C11 C12 113.6(6) . . ? C10 C11 H11A 108.8 . . ? C12 C11 H11A 108.8 . . ? C10 C11 H11B 108.8 . . ? C12 C11 H11B 108.8 . . ? H11A C11 H11B 107.7 . . ? N1 C12 C11 114.2(5) . . ? N1 C12 H12A 108.7 . . ? C11 C12 H12A 108.7 . . ? N1 C12 H12B 108.7 . . ? C11 C12 H12B 108.7 . . ? H12A C12 H12B 107.6 . . ? N1 C13 C14 113.4(5) . . ? N1 C13 H13A 108.9 . . ? C14 C13 H13A 108.9 . . ? N1 C13 H13B 108.9 . . ? C14 C13 H13B 108.9 . . ? H13A C13 H13B 107.7 . . ? N2 C14 C13 112.6(5) . . ? N2 C14 H14A 109.1 . . ? C13 C14 H14A 109.1 . . ? N2 C14 H14B 109.1 . . ? C13 C14 H14B 109.1 . . ? H14A C14 H14B 107.8 . . ? N2 C15 C16 110.8(5) . . ? N2 C15 H15A 109.5 . . ? C16 C15 H15A 109.5 . . ? N2 C15 H15B 109.5 . . ? C16 C15 H15B 109.5 . . ? H15A C15 H15B 108.1 . . ? C17 C16 C21 117.7(6) . . ? C17 C16 C15 120.6(6) . . ? C21 C16 C15 121.6(6) . . ? C16 C17 C18 122.5(6) . . ? C16 C17 H17 118.8 . . ? C18 C17 H17 118.8 . . ? C19 C18 C17 117.9(6) . . ? C19 C18 C23 122.2(7) . . ? C17 C18 C23 119.8(6) . . ? C18 C19 C20 122.4(6) . . ? C18 C19 H19 118.8 . . ? C20 C19 H19 118.8 . . ? C19 C20 C21 117.0(6) . . ? C19 C20 C22 122.8(7) . . ? C21 C20 C22 120.1(6) . . ? C16 C21 C20 122.5(6) . . ? C16 C21 H21 118.8 . . ? C20 C21 H21 118.8 . . ? O6 C22 O5 123.3(7) . . ? O6 C22 C20 118.2(7) . . ? O5 C22 C20 118.5(7) . . ? O7 C23 O8 118.6(8) . . ? O7 C23 C18 120.9(8) . . ? O8 C23 C18 120.4(8) . . ? C13 N1 C12 111.2(5) . . ? C13 N1 C7 113.5(5) . . ? C12 N1 C7 110.6(5) . . ? C10 N2 C15 110.2(5) 5_655 . ? C10 N2 C14 110.6(5) 5_655 . ? C15 N2 C14 110.8(5) . . ? C8 O1 Co1 92.1(4) . . ? C8 O2 Co1 88.1(4) . . ? C9 O3 Co2 93.8(4) . . ? C9 O4 Co2 85.6(4) . . ? C22 O6 H6A 109.5 . . ? O8W O7W O8W 88(2) . 2_654 ? C23 O7 Co2 85.0(6) . 6_566 ? C23 O8 Co2 99.8(5) . 6_566 ? O1W' O1W Co1 69.8(15) . . ? O1W O1W' Co1 91.4(16) . . ? Co2 O2W H2A 117(3) . . ? Co2 O2W H2B 135.8(17) . . ? H2A O2W H2B 106.2(16) . . ? Co2 O3W H3B 128.3(13) . . ? Co2 O3W H3A 128.2(12) . . ? H3B O3W H3A 102.5(12) . . ? H4A O4W H4B 106.7(17) . . ? H5A O5W H5B 107.7(17) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C6 C1 C2 C3 -0.6(9) . . . . ? C8 C1 C2 C3 178.1(6) . . . . ? C1 C2 C3 C4 1.4(9) . . . . ? C1 C2 C3 C7 -174.3(6) . . . . ? C2 C3 C4 C5 -0.2(9) . . . . ? C7 C3 C4 C5 175.5(6) . . . . ? C3 C4 C5 C6 -1.7(9) . . . . ? C3 C4 C5 C9 179.2(6) . . . . ? C4 C5 C6 C1 2.5(9) . . . . ? C9 C5 C6 C1 -178.4(6) . . . . ? C2 C1 C6 C5 -1.4(9) . . . . ? C8 C1 C6 C5 179.9(6) . . . . ? C2 C3 C7 N1 -106.7(7) . . . . ? C4 C3 C7 N1 77.7(7) . . . . ? C6 C1 C8 O1 -176.3(6) . . . . ? C2 C1 C8 O1 4.9(10) . . . . ? C6 C1 C8 O2 3.0(10) . . . . ? C2 C1 C8 O2 -175.7(6) . . . . ? C6 C1 C8 Co1 -122(7) . . . . ? C2 C1 C8 Co1 59(8) . . . . ? O1W' Co1 C8 O1 83.9(6) 2_755 . . . ? O1W' Co1 C8 O1 -18.1(6) . . . . ? O1 Co1 C8 O1 175.7(4) 2_755 . . . ? O1W Co1 C8 O1 100.8(5) 2_755 . . . ? O1W Co1 C8 O1 -37.9(5) . . . . ? O2 Co1 C8 O1 -126.8(4) 2_755 . . . ? O2 Co1 C8 O1 -176.9(7) . . . . ? C8 Co1 C8 O1 -143.6(4) 2_755 . . . ? O1W' Co1 C8 O2 -99.2(6) 2_755 . . . ? O1W' Co1 C8 O2 158.9(6) . . . . ? O1 Co1 C8 O2 176.9(7) . . . . ? O1 Co1 C8 O2 -7.3(7) 2_755 . . . ? O1W Co1 C8 O2 -82.2(5) 2_755 . . . ? O1W Co1 C8 O2 139.0(5) . . . . ? O2 Co1 C8 O2 50.1(6) 2_755 . . . ? C8 Co1 C8 O2 33.4(4) 2_755 . . . ? O1W' Co1 C8 C1 28(8) 2_755 . . . ? O1W' Co1 C8 C1 -74(8) . . . . ? O1 Co1 C8 C1 -56(7) . . . . ? O1 Co1 C8 C1 120(8) 2_755 . . . ? O1W Co1 C8 C1 45(8) 2_755 . . . ? O1W Co1 C8 C1 -94(8) . . . . ? O2 Co1 C8 C1 177(100) 2_755 . . . ? O2 Co1 C8 C1 127(8) . . . . ? C8 Co1 C8 C1 160(8) 2_755 . . . ? C6 C5 C9 O4 168.2(6) . . . . ? C4 C5 C9 O4 -12.8(9) . . . . ? C6 C5 C9 O3 -11.7(9) . . . . ? C4 C5 C9 O3 167.3(6) . . . . ? C6 C5 C9 Co2 -2(8) . . . . ? C4 C5 C9 Co2 177(100) . . . . ? O2W Co2 C9 O4 -73.4(4) . . . . ? O3W Co2 C9 O4 66.5(4) . . . . ? O8 Co2 C9 O4 175.7(4) 6_565 . . . ? O3 Co2 C9 O4 179.4(6) . . . . ? O7 Co2 C9 O4 -52(2) 6_565 . . . ? O2W Co2 C9 O3 107.3(4) . . . . ? O3W Co2 C9 O3 -112.9(4) . . . . ? O8 Co2 C9 O3 -3.7(5) 6_565 . . . ? O4 Co2 C9 O3 -179.4(6) . . . . ? O7 Co2 C9 O3 129(2) 6_565 . . . ? O2W Co2 C9 C5 97(7) . . . . ? O3W Co2 C9 C5 -123(7) . . . . ? O8 Co2 C9 C5 -14(8) 6_565 . . . ? O3 Co2 C9 C5 -10(7) . . . . ? O4 Co2 C9 C5 170(8) . . . . ? O7 Co2 C9 C5 119(7) 6_565 . . . ? N2 C10 C11 C12 -170.1(6) 5_655 . . . ? C10 C11 C12 N1 67.1(8) . . . . ? N1 C13 C14 N2 49.8(8) . . . . ? N2 C15 C16 C17 66.1(8) . . . . ? N2 C15 C16 C21 -110.7(7) . . . . ? C21 C16 C17 C18 -0.6(10) . . . . ? C15 C16 C17 C18 -177.5(6) . . . . ? C16 C17 C18 C19 0.6(10) . . . . ? C16 C17 C18 C23 177.2(6) . . . . ? C17 C18 C19 C20 0.3(10) . . . . ? C23 C18 C19 C20 -176.2(7) . . . . ? C18 C19 C20 C21 -1.2(10) . . . . ? C18 C19 C20 C22 177.0(7) . . . . ? C17 C16 C21 C20 -0.4(10) . . . . ? C15 C16 C21 C20 176.5(6) . . . . ? C19 C20 C21 C16 1.3(10) . . . . ? C22 C20 C21 C16 -177.0(6) . . . . ? C19 C20 C22 O6 -0.2(11) . . . . ? C21 C20 C22 O6 178.0(7) . . . . ? C19 C20 C22 O5 -177.3(7) . . . . ? C21 C20 C22 O5 0.9(11) . . . . ? C19 C18 C23 O7 163.2(8) . . . . ? C17 C18 C23 O7 -13.2(11) . . . . ? C19 C18 C23 O8 -17.2(11) . . . . ? C17 C18 C23 O8 166.4(7) . . . . ? C14 C13 N1 C12 -169.8(5) . . . . ? C14 C13 N1 C7 64.7(7) . . . . ? C11 C12 N1 C13 65.4(7) . . . . ? C11 C12 N1 C7 -167.5(5) . . . . ? C3 C7 N1 C13 58.8(7) . . . . ? C3 C7 N1 C12 -67.0(7) . . . . ? C16 C15 N2 C10 -173.4(6) . . . 5_655 ? C16 C15 N2 C14 63.9(7) . . . . ? C13 C14 N2 C10 73.3(7) . . . 5_655 ? C13 C14 N2 C15 -164.2(6) . . . . ? O2 C8 O1 Co1 -3.1(7) . . . . ? C1 C8 O1 Co1 176.3(5) . . . . ? O1W' Co1 O1 C8 -97.4(6) 2_755 . . . ? O1W' Co1 O1 C8 163.7(6) . . . . ? O1 Co1 O1 C8 -146.8(4) 2_755 . . . ? O1W Co1 O1 C8 -78.7(5) 2_755 . . . ? O1W Co1 O1 C8 144.9(5) . . . . ? O2 Co1 O1 C8 65.8(5) 2_755 . . . ? O2 Co1 O1 C8 1.8(4) . . . . ? C8 Co1 O1 C8 70.1(8) 2_755 . . . ? O1 C8 O2 Co1 3.0(7) . . . . ? C1 C8 O2 Co1 -176.4(6) . . . . ? O1W' Co1 O2 C8 84.1(6) 2_755 . . . ? O1W' Co1 O2 C8 -32.3(9) . . . . ? O1 Co1 O2 C8 -1.8(4) . . . . ? O1 Co1 O2 C8 176.0(4) 2_755 . . . ? O1W Co1 O2 C8 94.8(5) 2_755 . . . ? O1W Co1 O2 C8 -54.7(6) . . . . ? O2 Co1 O2 C8 -133.0(5) 2_755 . . . ? C8 Co1 O2 C8 -155.5(3) 2_755 . . . ? O4 C9 O3 Co2 -0.7(7) . . . . ? C5 C9 O3 Co2 179.3(5) . . . . ? O2W Co2 O3 C9 -76.0(4) . . . . ? O3W Co2 O3 C9 72.7(4) . . . . ? O8 Co2 O3 C9 177.1(4) 6_565 . . . ? O4 Co2 O3 C9 0.4(4) . . . . ? O7 Co2 O3 C9 -169.4(5) 6_565 . . . ? O3 C9 O4 Co2 0.6(6) . . . . ? C5 C9 O4 Co2 -179.3(5) . . . . ? O2W Co2 O4 C9 105.6(4) . . . . ? O3W Co2 O4 C9 -113.4(4) . . . . ? O8 Co2 O4 C9 -9.0(8) 6_565 . . . ? O3 Co2 O4 C9 -0.4(4) . . . . ? O7 Co2 O4 C9 171.6(5) 6_565 . . . ? O8 C23 O7 Co2 -3.0(8) . . . 6_566 ? C18 C23 O7 Co2 176.7(7) . . . 6_566 ? O7 C23 O8 Co2 3.5(9) . . . 6_566 ? C18 C23 O8 Co2 -176.2(6) . . . 6_566 ? O1W' Co1 O1W O1W' 2(2) 2_755 . . . ? O1 Co1 O1W O1W' 90.6(16) . . . . ? O1 Co1 O1W O1W' -86.2(16) 2_755 . . . ? O1W Co1 O1W O1W' 1.2(15) 2_755 . . . ? O2 Co1 O1W O1W' -145.2(16) 2_755 . . . ? O2 Co1 O1W O1W' 134.2(15) . . . . ? C8 Co1 O1W O1W' -115.4(16) 2_755 . . . ? C8 Co1 O1W O1W' 108.4(16) . . . . ? O1W' Co1 O1W' O1W -178.6(19) 2_755 . . . ? O1 Co1 O1W' O1W -88.4(16) . . . . ? O1 Co1 O1W' O1W 94.3(16) 2_755 . . . ? O1W Co1 O1W' O1W -179.1(12) 2_755 . . . ? O2 Co1 O1W' O1W 34.8(16) 2_755 . . . ? O2 Co1 O1W' O1W -62.3(19) . . . . ? C8 Co1 O1W' O1W 64.7(16) 2_755 . . . ? C8 Co1 O1W' O1W -79.5(16) . . . . ? _diffrn_measured_fraction_theta_max 0.972 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.971 _refine_diff_density_max 1.878 _refine_diff_density_min -1.219 _refine_diff_density_rms 0.100 #=========================END data_Compound-5 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C46 H58 Fe3 N4 O24, 6.5H2O' _chemical_formula_sum 'C46 H71 Fe3 N4 O30.50' _chemical_formula_weight 1335.62 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Fe' 'Fe' 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' _symmetry_space_group_name_hall '-C 2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 24.104(2) _cell_length_b 13.0540(9) _cell_length_c 21.0090(16) _cell_angle_alpha 90.00 _cell_angle_beta 124.662(10) _cell_angle_gamma 90.00 _cell_volume 5437.3(7) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 3440 _cell_measurement_theta_min 2.8868 _cell_measurement_theta_max 29.0001 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.632 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2788 _exptl_absorpt_coefficient_mu 0.891 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8146 _exptl_absorpt_correction_T_max 0.8706 _exptl_absorpt_process_details ; CrysAlis (Oxford Diffraction, 2006) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Diffraction Gemini R Ultra' _diffrn_measurement_method '\w scan' _diffrn_detector_area_resol_mean 10.0 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15570 _diffrn_reflns_av_R_equivalents 0.0586 _diffrn_reflns_av_sigmaI/netI 0.0740 _diffrn_reflns_limit_h_min -28 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 3.12 _diffrn_reflns_theta_max 25.35 _reflns_number_total 4978 _reflns_number_gt 3095 _reflns_threshold_expression >2\s(I) _computing_data_collection 'CrysAlisPro(1.171.35.21) (Agilent Tech., 2012)' _computing_cell_refinement 'CrysAlisPro(1.171.35.21) (Agilent Tech., 2012)' _computing_data_reduction 'CrysAlisPro(1.171.35.21) (Agilent Tech., 2012)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0200P)^2^+50.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4978 _refine_ls_number_parameters 393 _refine_ls_number_restraints 18 _refine_ls_R_factor_all 0.1181 _refine_ls_R_factor_gt 0.0707 _refine_ls_wR_factor_ref 0.1555 _refine_ls_wR_factor_gt 0.1339 _refine_ls_goodness_of_fit_ref 0.960 _refine_ls_restrained_S_all 0.963 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.5000 0.16795(9) -0.2500 0.0508(3) Uani 1 2 d S . . Fe2 Fe 0.15794(5) 0.63717(7) -0.61158(6) 0.0613(3) Uani 1 1 d . . . C1 C 0.1254(3) 0.0543(4) -0.4737(3) 0.0429(13) Uani 1 1 d . . . H1A H 0.1575 0.0823 -0.4830 0.051 Uiso 1 1 calc R . . H1B H 0.0899 0.0207 -0.5209 0.051 Uiso 1 1 calc R . . C2 C 0.1604(3) -0.0236(4) -0.4105(3) 0.0427(13) Uani 1 1 d . . . H2A H 0.1705 -0.0833 -0.4297 0.051 Uiso 1 1 calc R . . H2B H 0.2028 0.0047 -0.3680 0.051 Uiso 1 1 calc R . . C3 C 0.0644(2) -0.1226(4) -0.4365(3) 0.0449(14) Uani 1 1 d . . . H3A H 0.0826 -0.1866 -0.4406 0.054 Uiso 1 1 calc R . . H3B H 0.0393 -0.0903 -0.4870 0.054 Uiso 1 1 calc R . . C4 C 0.0168(3) -0.1452(5) -0.4130(3) 0.0500(15) Uani 1 1 d . . . H4A H 0.0044 -0.0809 -0.4011 0.060 Uiso 1 1 calc R . . H4B H 0.0407 -0.1857 -0.3659 0.060 Uiso 1 1 calc R . . C5 C -0.0468(2) -0.2013(4) -0.4728(3) 0.0483(15) Uani 1 1 d . . . H5A H -0.0344 -0.2625 -0.4882 0.058 Uiso 1 1 calc R . . H5B H -0.0696 -0.2230 -0.4491 0.058 Uiso 1 1 calc R . . C6 C 0.1643(3) -0.1067(4) -0.3056(3) 0.0517(16) Uani 1 1 d . . . H6A H 0.1894 -0.1610 -0.3099 0.062 Uiso 1 1 calc R . . H6B H 0.1370 -0.1371 -0.2901 0.062 Uiso 1 1 calc R . . C7 C 0.2123(3) -0.0312(4) -0.2455(3) 0.0406(13) Uani 1 1 d . . . C8 C 0.2798(3) -0.0344(4) -0.2129(3) 0.0429(13) Uani 1 1 d . . . H8 H 0.2973 -0.0878 -0.2258 0.051 Uiso 1 1 calc R . . C9 C 0.3237(3) 0.0404(4) -0.1606(3) 0.0477(14) Uani 1 1 d . . . C10 C 0.2967(3) 0.1192(4) -0.1427(3) 0.0533(16) Uani 1 1 d . . . H10 H 0.3249 0.1696 -0.1079 0.064 Uiso 1 1 calc R . . C11 C 0.2278(3) 0.1239(4) -0.1763(3) 0.0497(15) Uani 1 1 d . . . C12 C 0.1871(3) 0.0479(4) -0.2264(3) 0.0460(14) Uani 1 1 d . . . H12 H 0.1411 0.0501 -0.2480 0.055 Uiso 1 1 calc R . . C13 C 0.3968(3) 0.0373(7) -0.1282(4) 0.071(2) Uani 1 1 d . . . C14 C 0.1983(4) 0.2127(6) -0.1610(5) 0.071(2) Uani 1 1 d . . . C15 C 0.1480(2) 0.2088(4) -0.3923(3) 0.0352(12) Uani 1 1 d . . . H15A H 0.1250 0.2620 -0.3835 0.042 Uiso 1 1 calc R . . H15B H 0.1740 0.1688 -0.3452 0.042 Uiso 1 1 calc R . . C16 C 0.1963(2) 0.2593(4) -0.4060(3) 0.0319(11) Uani 1 1 d . . . C17 C 0.2628(2) 0.2270(4) -0.3659(3) 0.0355(12) Uani 1 1 d . . . H17 H 0.2758 0.1692 -0.3346 0.043 Uiso 1 1 calc R . . C18 C 0.3101(2) 0.2781(4) -0.3711(3) 0.0358(12) Uani 1 1 d . . . C19 C 0.2906(2) 0.3637(4) -0.4180(3) 0.0387(13) Uani 1 1 d . . . H19 H 0.3224 0.3994 -0.4211 0.046 Uiso 1 1 calc R . . C20 C 0.2244(2) 0.3965(4) -0.4603(3) 0.0320(11) Uani 1 1 d . . . C21 C 0.1783(2) 0.3455(4) -0.4526(3) 0.0331(12) Uani 1 1 d . . . H21 H 0.1342 0.3695 -0.4792 0.040 Uiso 1 1 calc R . . C22 C 0.3817(3) 0.2428(5) -0.3253(3) 0.0446(14) Uani 1 1 d . . . C23 C 0.2036(3) 0.4877(4) -0.5118(3) 0.0399(13) Uani 1 1 d . . . N1 N 0.09542(19) 0.1399(3) -0.4558(2) 0.0356(10) Uani 1 1 d . . . N2 N 0.1200(2) -0.0558(3) -0.3814(2) 0.0384(10) Uani 1 1 d . . . O1 O 0.39686(18) 0.1620(3) -0.2869(2) 0.0593(11) Uani 1 1 d . . . O2 O 0.42580(18) 0.2918(3) -0.3261(3) 0.0715(14) Uani 1 1 d . . . O1W O 0.47910(19) 0.0863(4) -0.3458(3) 0.0755(14) Uani 1 1 d . . . O3 O 0.14086(18) 0.5063(3) -0.5579(2) 0.0523(10) Uani 1 1 d . . . O2W O 0.1502(2) 0.5323(4) -0.6919(2) 0.0718(13) Uani 1 1 d . . . O4 O 0.24550(19) 0.5425(3) -0.5114(2) 0.0530(10) Uani 1 1 d . . . O3W O 0.0510(3) 0.6578(6) -0.6739(4) 0.129(3) Uani 1 1 d . . . O5 O 0.4348(3) 0.1020(5) -0.0810(4) 0.122(2) Uani 1 1 d . . . O4W O 0.1572(3) 0.7429(4) -0.5340(3) 0.112(2) Uani 1 1 d . . . O6 O 0.4160(2) -0.0303(5) -0.1538(3) 0.105(2) Uani 1 1 d . . . H6 H 0.4568 -0.0256 -0.1324 0.157 Uiso 1 1 calc R . . O5W O 0.0333(2) 0.1560(5) -0.3702(3) 0.0952(17) Uani 1 1 d . . . O7 O 0.1355(3) 0.2242(5) -0.2027(4) 0.114(2) Uani 1 1 d . . . O6W O 0.5189(3) -0.1506(4) -0.0644(4) 0.1065(19) Uani 1 1 d . . . O8 O 0.2337(3) 0.2722(4) -0.1075(3) 0.0858(16) Uani 1 1 d . . . O7W O 0.0648(8) 0.9101(16) -0.6436(11) 0.059(5) Uani 0.25 1 d PU . . O8W O 0.0202(9) 1.0172(12) -0.7537(14) 0.172(7) Uani 0.50 1 d PU . . O9W O 0.1038(7) 0.9179(11) -0.6144(8) 0.110(4) Uani 0.50 1 d PU . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.0279(6) 0.0551(7) 0.0599(8) 0.000 0.0194(5) 0.000 Fe2 0.0655(6) 0.0638(6) 0.0601(6) 0.0156(5) 0.0390(5) 0.0071(5) C1 0.044(3) 0.045(3) 0.046(3) -0.008(3) 0.029(3) -0.013(3) C2 0.036(3) 0.045(3) 0.051(3) -0.002(3) 0.027(3) -0.002(2) C3 0.032(3) 0.047(3) 0.046(3) -0.005(3) 0.016(3) -0.008(2) C4 0.034(3) 0.061(4) 0.040(3) 0.005(3) 0.012(3) -0.007(3) C5 0.031(3) 0.051(3) 0.047(3) 0.009(3) 0.012(3) -0.010(3) C6 0.041(3) 0.042(3) 0.047(4) 0.005(3) 0.011(3) -0.004(3) C7 0.039(3) 0.037(3) 0.033(3) 0.007(2) 0.013(2) 0.000(2) C8 0.043(3) 0.045(3) 0.036(3) 0.004(3) 0.020(3) 0.003(3) C9 0.045(3) 0.054(4) 0.038(3) 0.000(3) 0.020(3) -0.013(3) C10 0.068(4) 0.041(3) 0.049(4) -0.009(3) 0.032(3) -0.019(3) C11 0.069(4) 0.042(3) 0.049(4) 0.002(3) 0.040(3) -0.001(3) C12 0.043(3) 0.052(4) 0.043(3) 0.009(3) 0.025(3) -0.003(3) C13 0.044(4) 0.110(6) 0.048(4) 0.008(4) 0.019(3) -0.006(4) C14 0.098(6) 0.060(5) 0.071(5) 0.001(4) 0.057(5) 0.006(4) C15 0.032(3) 0.042(3) 0.034(3) -0.002(2) 0.020(2) -0.005(2) C16 0.026(2) 0.037(3) 0.030(3) -0.003(2) 0.014(2) -0.002(2) C17 0.036(3) 0.033(3) 0.035(3) 0.001(2) 0.019(2) 0.000(2) C18 0.026(3) 0.042(3) 0.037(3) -0.006(2) 0.017(2) -0.001(2) C19 0.032(3) 0.047(3) 0.044(3) -0.007(3) 0.025(2) -0.009(2) C20 0.027(2) 0.038(3) 0.030(3) -0.004(2) 0.016(2) -0.004(2) C21 0.023(2) 0.041(3) 0.032(3) -0.007(2) 0.014(2) -0.002(2) C22 0.028(3) 0.056(4) 0.047(3) -0.008(3) 0.019(3) -0.001(3) C23 0.035(3) 0.045(3) 0.041(3) -0.004(3) 0.022(3) -0.008(3) N1 0.028(2) 0.041(2) 0.038(2) 0.001(2) 0.0186(19) -0.0033(19) N2 0.033(2) 0.038(2) 0.036(2) 0.003(2) 0.0138(19) -0.0048(19) O1 0.035(2) 0.066(3) 0.069(3) 0.017(2) 0.024(2) 0.013(2) O2 0.027(2) 0.076(3) 0.102(4) 0.012(3) 0.030(2) 0.001(2) O1W 0.039(2) 0.094(3) 0.084(3) -0.036(3) 0.030(2) -0.013(2) O3 0.041(2) 0.059(2) 0.046(2) 0.0152(19) 0.0185(19) -0.0008(19) O2W 0.086(3) 0.079(3) 0.054(3) -0.005(2) 0.042(3) -0.023(3) O4 0.046(2) 0.059(2) 0.056(3) 0.013(2) 0.030(2) -0.007(2) O3W 0.072(4) 0.196(7) 0.126(5) 0.072(5) 0.060(4) 0.046(4) O5 0.054(3) 0.119(5) 0.129(5) -0.016(4) 0.014(3) -0.039(3) O4W 0.174(6) 0.108(4) 0.093(4) 0.029(3) 0.098(4) 0.061(4) O6 0.040(3) 0.198(7) 0.060(3) -0.016(4) 0.019(2) 0.010(3) O5W 0.073(3) 0.140(5) 0.091(4) 0.019(4) 0.058(3) 0.022(3) O7 0.105(5) 0.106(5) 0.140(6) -0.033(4) 0.074(4) 0.016(4) O6W 0.109(4) 0.092(4) 0.152(6) 0.009(4) 0.094(4) 0.013(3) O8 0.144(5) 0.055(3) 0.081(4) -0.014(3) 0.078(4) -0.001(3) O7W 0.025(7) 0.071(9) 0.064(9) -0.019(7) 0.015(6) -0.010(7) O8W 0.173(11) 0.156(9) 0.203(10) -0.006(8) 0.116(8) 0.017(7) O9W 0.134(9) 0.099(7) 0.111(8) -0.006(6) 0.079(7) 0.006(7) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 O1W 2.070(4) . ? Fe1 O1W 2.070(4) 2_654 ? Fe1 O1 2.144(4) . ? Fe1 O1 2.144(4) 2_654 ? Fe1 O2 2.261(4) 2_654 ? Fe1 O2 2.261(4) . ? Fe2 O2W 2.097(5) . ? Fe2 O8 2.137(5) 6_565 ? Fe2 O3W 2.143(5) . ? Fe2 O4W 2.143(5) . ? Fe2 O3 2.210(4) . ? Fe2 O4 2.315(4) . ? C1 N1 1.491(6) . ? C1 C2 1.495(7) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 N2 1.475(6) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 N2 1.461(6) . ? C3 C4 1.513(7) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 C5 1.508(7) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 N1 1.505(6) 5_554 ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 N2 1.477(6) . ? C6 C7 1.498(7) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 C8 1.360(7) . ? C7 C12 1.369(8) . ? C8 C9 1.399(7) . ? C8 H8 0.9300 . ? C9 C10 1.379(8) . ? C9 C13 1.484(8) . ? C10 C11 1.388(8) . ? C10 H10 0.9300 . ? C11 C12 1.371(8) . ? C11 C14 1.487(9) . ? C12 H12 0.9300 . ? C13 O5 1.225(9) . ? C13 O6 1.252(9) . ? C14 O7 1.255(9) . ? C14 O8 1.228(8) . ? C15 C16 1.501(6) . ? C15 N1 1.507(6) . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 C21 1.389(7) . ? C16 C17 1.385(6) . ? C17 C18 1.377(7) . ? C17 H17 0.9300 . ? C18 C19 1.384(7) . ? C18 C22 1.493(7) . ? C19 C20 1.381(7) . ? C19 H19 0.9300 . ? C20 C21 1.382(7) . ? C20 C23 1.490(7) . ? C21 H21 0.9300 . ? C22 O1 1.249(7) . ? C22 O2 1.250(6) . ? C23 O4 1.234(6) . ? C23 O3 1.271(6) . ? N1 C5 1.505(6) 5_554 ? O6 H6 0.8200 . ? O8 Fe2 2.137(5) 6_566 ? O7W O9W 0.784(17) . ? O8W O8W 1.07(3) 2_553 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1W Fe1 O1W 118.0(3) . 2_654 ? O1W Fe1 O1 92.24(16) . . ? O1W Fe1 O1 85.62(16) 2_654 . ? O1W Fe1 O1 85.62(16) . 2_654 ? O1W Fe1 O1 92.24(16) 2_654 2_654 ? O1 Fe1 O1 175.9(2) . 2_654 ? O1W Fe1 O2 135.44(17) . 2_654 ? O1W Fe1 O2 91.34(19) 2_654 2_654 ? O1 Fe1 O2 124.72(16) . 2_654 ? O1 Fe1 O2 58.81(15) 2_654 2_654 ? O1W Fe1 O2 91.34(19) . . ? O1W Fe1 O2 135.44(17) 2_654 . ? O1 Fe1 O2 58.81(15) . . ? O1 Fe1 O2 124.72(16) 2_654 . ? O2 Fe1 O2 88.8(2) 2_654 . ? O2W Fe2 O8 94.38(18) . 6_565 ? O2W Fe2 O3W 93.7(2) . . ? O8 Fe2 O3W 131.2(2) 6_565 . ? O2W Fe2 O4W 175.4(2) . . ? O8 Fe2 O4W 89.4(2) 6_565 . ? O3W Fe2 O4W 81.8(3) . . ? O2W Fe2 O3 87.08(16) . . ? O8 Fe2 O3 144.12(18) 6_565 . ? O3W Fe2 O3 84.3(2) . . ? O4W Fe2 O3 91.48(19) . . ? O2W Fe2 O4 90.08(17) . . ? O8 Fe2 O4 86.70(18) 6_565 . ? O3W Fe2 O4 141.28(19) . . ? O4W Fe2 O4 92.85(18) . . ? O3 Fe2 O4 57.43(13) . . ? N1 C1 C2 113.3(4) . . ? N1 C1 H1A 108.9 . . ? C2 C1 H1A 108.9 . . ? N1 C1 H1B 108.9 . . ? C2 C1 H1B 108.9 . . ? H1A C1 H1B 107.7 . . ? N2 C2 C1 113.0(4) . . ? N2 C2 H2A 109.0 . . ? C1 C2 H2A 109.0 . . ? N2 C2 H2B 109.0 . . ? C1 C2 H2B 109.0 . . ? H2A C2 H2B 107.8 . . ? N2 C3 C4 112.5(5) . . ? N2 C3 H3A 109.1 . . ? C4 C3 H3A 109.1 . . ? N2 C3 H3B 109.1 . . ? C4 C3 H3B 109.1 . . ? H3A C3 H3B 107.8 . . ? C3 C4 C5 115.0(5) . . ? C3 C4 H4A 108.5 . . ? C5 C4 H4A 108.5 . . ? C3 C4 H4B 108.5 . . ? C5 C4 H4B 108.5 . . ? H4A C4 H4B 107.5 . . ? N1 C5 C4 114.7(4) 5_554 . ? N1 C5 H5A 108.6 5_554 . ? C4 C5 H5A 108.6 . . ? N1 C5 H5B 108.6 5_554 . ? C4 C5 H5B 108.6 . . ? H5A C5 H5B 107.6 . . ? N2 C6 C7 110.5(4) . . ? N2 C6 H6A 109.5 . . ? C7 C6 H6A 109.5 . . ? N2 C6 H6B 109.5 . . ? C7 C6 H6B 109.5 . . ? H6A C6 H6B 108.1 . . ? C8 C7 C12 118.7(5) . . ? C8 C7 C6 122.3(5) . . ? C12 C7 C6 118.9(5) . . ? C7 C8 C9 121.8(5) . . ? C7 C8 H8 119.1 . . ? C9 C8 H8 119.1 . . ? C10 C9 C8 118.1(5) . . ? C10 C9 C13 121.1(6) . . ? C8 C9 C13 120.8(6) . . ? C9 C10 C11 120.5(5) . . ? C9 C10 H10 119.7 . . ? C11 C10 H10 119.7 . . ? C12 C11 C10 119.0(5) . . ? C12 C11 C14 120.5(6) . . ? C10 C11 C14 120.4(6) . . ? C11 C12 C7 121.8(5) . . ? C11 C12 H12 119.1 . . ? C7 C12 H12 119.1 . . ? O5 C13 O6 123.0(7) . . ? O5 C13 C9 119.9(8) . . ? O6 C13 C9 117.0(7) . . ? O7 C14 O8 119.8(7) . . ? O7 C14 C11 118.6(7) . . ? O8 C14 C11 121.5(7) . . ? C16 C15 N1 116.5(4) . . ? C16 C15 H15A 108.2 . . ? N1 C15 H15A 108.2 . . ? C16 C15 H15B 108.2 . . ? N1 C15 H15B 108.2 . . ? H15A C15 H15B 107.3 . . ? C21 C16 C17 117.7(4) . . ? C21 C16 C15 121.7(4) . . ? C17 C16 C15 120.3(5) . . ? C18 C17 C16 121.8(5) . . ? C18 C17 H17 119.1 . . ? C16 C17 H17 119.1 . . ? C19 C18 C17 119.1(4) . . ? C19 C18 C22 120.5(5) . . ? C17 C18 C22 120.4(5) . . ? C18 C19 C20 120.6(5) . . ? C18 C19 H19 119.7 . . ? C20 C19 H19 119.7 . . ? C19 C20 C21 119.1(5) . . ? C19 C20 C23 120.3(5) . . ? C21 C20 C23 120.5(4) . . ? C16 C21 C20 121.6(4) . . ? C16 C21 H21 119.2 . . ? C20 C21 H21 119.2 . . ? O1 C22 O2 120.1(5) . . ? O1 C22 C18 118.9(5) . . ? O2 C22 C18 121.0(5) . . ? O4 C23 O3 120.6(5) . . ? O4 C23 C20 121.4(5) . . ? O3 C23 C20 118.0(5) . . ? C1 N1 C5 111.3(4) . 5_554 ? C1 N1 C15 112.7(4) . . ? C5 N1 C15 110.5(4) 5_554 . ? C3 N2 C6 111.1(4) . . ? C3 N2 C2 111.5(4) . . ? C6 N2 C2 109.4(4) . . ? C22 O1 Fe1 93.2(3) . . ? C22 O2 Fe1 87.8(4) . . ? C23 O3 Fe2 92.9(3) . . ? C23 O4 Fe2 89.0(3) . . ? C13 O6 H6 109.5 . . ? C14 O8 Fe2 100.4(5) . 6_566 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 C1 C2 N2 47.2(6) . . . . ? N2 C3 C4 C5 171.8(4) . . . . ? C3 C4 C5 N1 -68.6(7) . . . 5_554 ? N2 C6 C7 C8 -111.7(6) . . . . ? N2 C6 C7 C12 63.9(7) . . . . ? C12 C7 C8 C9 0.2(8) . . . . ? C6 C7 C8 C9 175.8(5) . . . . ? C7 C8 C9 C10 -0.4(8) . . . . ? C7 C8 C9 C13 -177.6(5) . . . . ? C8 C9 C10 C11 -0.3(9) . . . . ? C13 C9 C10 C11 176.9(6) . . . . ? C9 C10 C11 C12 1.3(9) . . . . ? C9 C10 C11 C14 -175.8(6) . . . . ? C10 C11 C12 C7 -1.5(8) . . . . ? C14 C11 C12 C7 175.5(5) . . . . ? C8 C7 C12 C11 0.8(8) . . . . ? C6 C7 C12 C11 -175.0(5) . . . . ? C10 C9 C13 O5 4.6(10) . . . . ? C8 C9 C13 O5 -178.2(7) . . . . ? C10 C9 C13 O6 -172.4(6) . . . . ? C8 C9 C13 O6 4.8(10) . . . . ? C12 C11 C14 O7 -9.9(10) . . . . ? C10 C11 C14 O7 167.1(7) . . . . ? C12 C11 C14 O8 167.7(6) . . . . ? C10 C11 C14 O8 -15.3(10) . . . . ? N1 C15 C16 C21 79.2(6) . . . . ? N1 C15 C16 C17 -107.4(5) . . . . ? C21 C16 C17 C18 0.3(7) . . . . ? C15 C16 C17 C18 -173.3(5) . . . . ? C16 C17 C18 C19 -0.4(8) . . . . ? C16 C17 C18 C22 178.3(5) . . . . ? C17 C18 C19 C20 -1.2(8) . . . . ? C22 C18 C19 C20 -179.9(5) . . . . ? C18 C19 C20 C21 2.9(7) . . . . ? C18 C19 C20 C23 -179.0(5) . . . . ? C17 C16 C21 C20 1.4(7) . . . . ? C15 C16 C21 C20 174.9(4) . . . . ? C19 C20 C21 C16 -3.0(7) . . . . ? C23 C20 C21 C16 178.9(4) . . . . ? C19 C18 C22 O1 -176.0(5) . . . . ? C17 C18 C22 O1 5.3(8) . . . . ? C19 C18 C22 O2 2.7(8) . . . . ? C17 C18 C22 O2 -176.0(5) . . . . ? C19 C20 C23 O4 -8.2(8) . . . . ? C21 C20 C23 O4 169.9(5) . . . . ? C19 C20 C23 O3 170.0(5) . . . . ? C21 C20 C23 O3 -12.0(7) . . . . ? C2 C1 N1 C5 -165.8(4) . . . 5_554 ? C2 C1 N1 C15 69.4(5) . . . . ? C16 C15 N1 C1 58.5(6) . . . . ? C16 C15 N1 C5 -66.7(5) . . . 5_554 ? C4 C3 N2 C6 65.3(6) . . . . ? C4 C3 N2 C2 -172.3(4) . . . . ? C7 C6 N2 C3 -168.5(5) . . . . ? C7 C6 N2 C2 68.0(6) . . . . ? C1 C2 N2 C3 73.7(5) . . . . ? C1 C2 N2 C6 -163.0(4) . . . . ? O2 C22 O1 Fe1 -2.0(6) . . . . ? C18 C22 O1 Fe1 176.8(4) . . . . ? O1W Fe1 O1 C22 -89.1(4) . . . . ? O1W Fe1 O1 C22 152.9(4) 2_654 . . . ? O1 Fe1 O1 C22 -148.0(3) 2_654 . . . ? O2 Fe1 O1 C22 64.4(4) 2_654 . . . ? O2 Fe1 O1 C22 1.1(3) . . . . ? O1 C22 O2 Fe1 1.9(6) . . . . ? C18 C22 O2 Fe1 -176.9(5) . . . . ? O1W Fe1 O2 C22 90.7(4) . . . . ? O1W Fe1 O2 C22 -43.2(5) 2_654 . . . ? O1 Fe1 O2 C22 -1.1(3) . . . . ? O1 Fe1 O2 C22 176.3(3) 2_654 . . . ? O2 Fe1 O2 C22 -133.9(4) 2_654 . . . ? O4 C23 O3 Fe2 2.1(6) . . . . ? C20 C23 O3 Fe2 -176.1(4) . . . . ? O2W Fe2 O3 C23 90.8(3) . . . . ? O8 Fe2 O3 C23 -2.6(5) 6_565 . . . ? O3W Fe2 O3 C23 -175.1(4) . . . . ? O4W Fe2 O3 C23 -93.6(4) . . . . ? O4 Fe2 O3 C23 -1.1(3) . . . . ? O3 C23 O4 Fe2 -2.0(5) . . . . ? C20 C23 O4 Fe2 176.2(4) . . . . ? O2W Fe2 O4 C23 -85.3(3) . . . . ? O8 Fe2 O4 C23 -179.7(4) 6_565 . . . ? O3W Fe2 O4 C23 10.7(5) . . . . ? O4W Fe2 O4 C23 91.1(4) . . . . ? O3 Fe2 O4 C23 1.2(3) . . . . ? O7 C14 O8 Fe2 5.2(9) . . . 6_566 ? C11 C14 O8 Fe2 -172.4(5) . . . 6_566 ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.592 _refine_diff_density_min -0.621 _refine_diff_density_rms 0.080 #=========================END data_Compound-6 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C94 H150 Co3 N16 O16, 5H2O' _chemical_formula_sum 'C94 H160 Co3 N16 O21' _chemical_formula_weight 2027.17 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Co' 'Co' 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.9750(6) _cell_length_b 14.5480(7) _cell_length_c 16.0630(9) _cell_angle_alpha 81.074(5) _cell_angle_beta 86.503(5) _cell_angle_gamma 86.458(4) _cell_volume 2525.3(2) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 3539 _cell_measurement_theta_min 2.8329 _cell_measurement_theta_max 29.1431 _exptl_crystal_description block _exptl_crystal_colour pink _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.333 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1085 _exptl_absorpt_coefficient_mu 0.563 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8768 _exptl_absorpt_correction_T_max 0.9154 _exptl_absorpt_process_details ; CrysAlis (Oxford Diffraction, 2006) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Diffraction Gemini R Ultra' _diffrn_measurement_method '\w scan' _diffrn_detector_area_resol_mean 10.0 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15716 _diffrn_reflns_av_R_equivalents 0.0417 _diffrn_reflns_av_sigmaI/netI 0.0882 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.84 _diffrn_reflns_theta_max 25.35 _reflns_number_total 9210 _reflns_number_gt 5952 _reflns_threshold_expression >2\s(I) _computing_data_collection 'CrysAlisPro(1.171.35.21) (Agilent Tech., 2012)' _computing_cell_refinement 'CrysAlisPro(1.171.35.21) (Agilent Tech., 2012)' _computing_data_reduction 'CrysAlisPro(1.171.35.21) (Agilent Tech., 2012)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0754P)^2^+2.0232P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9210 _refine_ls_number_parameters 640 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1113 _refine_ls_R_factor_gt 0.0644 _refine_ls_wR_factor_ref 0.1745 _refine_ls_wR_factor_gt 0.1482 _refine_ls_goodness_of_fit_ref 1.019 _refine_ls_restrained_S_all 1.019 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.5000 0.5000 0.5000 0.0270(2) Uani 1 2 d S . . Co2 Co 0.5000 0.0000 1.0000 0.0362(2) Uani 1 2 d S . . Co3 Co 1.0000 0.5000 1.0000 0.0365(2) Uani 1 2 d S . . C1 C 0.5562(4) 0.1862(3) 0.5517(3) 0.0286(9) Uani 1 1 d . . . C2 C 0.4424(4) 0.1723(3) 0.5927(3) 0.0301(10) Uani 1 1 d . . . H2 H 0.3886 0.2233 0.5977 0.036 Uiso 1 1 calc R . . C3 C 0.4076(4) 0.0837(3) 0.6264(3) 0.0291(9) Uani 1 1 d . . . C4 C 0.4910(4) 0.0086(3) 0.6231(3) 0.0293(10) Uani 1 1 d . . . H4 H 0.4689 -0.0506 0.6474 0.035 Uiso 1 1 calc R . . C5 C 0.6070(4) 0.0199(3) 0.5842(3) 0.0271(9) Uani 1 1 d . . . C6 C 0.6367(4) 0.1091(3) 0.5462(2) 0.0281(9) Uani 1 1 d . . . H6 H 0.7118 0.1173 0.5166 0.034 Uiso 1 1 calc R . . C7 C 0.5915(4) 0.2836(3) 0.5146(3) 0.0348(10) Uani 1 1 d . . . C8 C 0.2785(4) 0.0678(3) 0.6628(3) 0.0372(11) Uani 1 1 d . . . C9 C 0.6938(4) -0.0640(3) 0.5822(3) 0.0301(10) Uani 1 1 d . . . H9A H 0.6644 -0.1144 0.6239 0.036 Uiso 1 1 calc R . . H9B H 0.6922 -0.0836 0.5273 0.036 Uiso 1 1 calc R . . C10 C 0.8302(4) -0.0166(3) 0.6791(2) 0.0263(9) Uani 1 1 d . . . H10A H 0.8147 -0.0680 0.7239 0.032 Uiso 1 1 calc R . . H10B H 0.7656 0.0311 0.6839 0.032 Uiso 1 1 calc R . . C11 C 0.9514(4) 0.0233(3) 0.6942(2) 0.0283(9) Uani 1 1 d . . . H11A H 0.9476 0.0361 0.7518 0.034 Uiso 1 1 calc R . . H11B H 1.0157 -0.0248 0.6898 0.034 Uiso 1 1 calc R . . C12 C 1.0186(4) 0.0911(3) 0.5489(2) 0.0298(10) Uani 1 1 d . . . H12A H 0.9431 0.0800 0.5245 0.036 Uiso 1 1 calc R . . H12B H 1.0701 0.0342 0.5516 0.036 Uiso 1 1 calc R . . C13 C 1.0823(4) 0.1674(3) 0.4900(3) 0.0312(10) Uani 1 1 d . . . H13A H 1.1593 0.1785 0.5124 0.037 Uiso 1 1 calc R . . H13B H 1.0316 0.2248 0.4854 0.037 Uiso 1 1 calc R . . C14 C 1.1053(4) 0.1370(3) 0.4030(2) 0.0281(9) Uani 1 1 d . . . H14A H 1.0269 0.1306 0.3802 0.034 Uiso 1 1 calc R . . H14B H 1.1460 0.1861 0.3658 0.034 Uiso 1 1 calc R . . C15 C 0.8976(4) 0.1918(3) 0.6386(2) 0.0294(9) Uani 1 1 d . . . H15A H 0.9294 0.2454 0.6020 0.035 Uiso 1 1 calc R . . H15B H 0.8224 0.1773 0.6159 0.035 Uiso 1 1 calc R . . C16 C 0.8694(4) 0.2168(3) 0.7253(2) 0.0275(9) Uani 1 1 d . . . C17 C 0.7614(4) 0.1921(3) 0.7706(3) 0.0330(10) Uani 1 1 d . . . H17 H 0.7065 0.1581 0.7477 0.040 Uiso 1 1 calc R . . C18 C 0.7345(4) 0.2177(3) 0.8497(3) 0.0333(10) Uani 1 1 d . . . C19 C 0.8175(4) 0.2688(3) 0.8826(3) 0.0332(10) Uani 1 1 d . . . H19 H 0.8000 0.2866 0.9354 0.040 Uiso 1 1 calc R . . C20 C 0.9247(4) 0.2937(3) 0.8389(3) 0.0309(10) Uani 1 1 d . . . C21 C 0.9508(4) 0.2671(3) 0.7604(3) 0.0307(10) Uani 1 1 d . . . H21 H 1.0238 0.2831 0.7309 0.037 Uiso 1 1 calc R . . C22 C 0.6217(4) 0.1867(3) 0.9035(3) 0.0434(12) Uani 1 1 d . . . C23 C 1.0096(4) 0.3547(3) 0.8739(3) 0.0378(11) Uani 1 1 d . . . C24 C 0.6536(5) 0.5336(4) 0.3491(3) 0.0503(13) Uani 1 1 d . . . H24A H 0.7266 0.5184 0.3158 0.060 Uiso 1 1 calc R . . H24B H 0.6378 0.6006 0.3392 0.060 Uiso 1 1 calc R . . C25 C 0.5467(5) 0.4861(4) 0.3235(3) 0.0521(13) Uani 1 1 d . . . H25A H 0.5313 0.5084 0.2647 0.063 Uiso 1 1 calc R . . H25B H 0.5645 0.4194 0.3299 0.063 Uiso 1 1 calc R . . C26 C 0.3200(5) 0.4678(3) 0.3619(3) 0.0481(13) Uani 1 1 d . . . C27 C 0.2741(6) 0.5148(4) 0.2775(4) 0.0720(18) Uani 1 1 d . . . H27A H 0.2613 0.5806 0.2781 0.108 Uiso 1 1 calc R . . H27B H 0.1984 0.4894 0.2678 0.108 Uiso 1 1 calc R . . H27C H 0.3336 0.5041 0.2332 0.108 Uiso 1 1 calc R . . C28 C 0.3395(6) 0.3623(4) 0.3618(4) 0.0673(17) Uani 1 1 d . . . H28A H 0.4000 0.3508 0.3184 0.101 Uiso 1 1 calc R . . H28B H 0.2639 0.3373 0.3514 0.101 Uiso 1 1 calc R . . H28C H 0.3669 0.3328 0.4157 0.101 Uiso 1 1 calc R . . C29 C 0.2249(4) 0.4885(4) 0.4308(3) 0.0494(13) Uani 1 1 d . . . H29A H 0.1469 0.4706 0.4150 0.059 Uiso 1 1 calc R . . H29B H 0.2185 0.5556 0.4291 0.059 Uiso 1 1 calc R . . C30 C 0.2404(4) 0.4447(3) 0.5233(3) 0.0459(13) Uani 1 1 d . . . H30 H 0.2760 0.3811 0.5236 0.055 Uiso 1 1 calc R . . C31 C 0.1174(5) 0.4384(5) 0.5734(4) 0.082(2) Uani 1 1 d . . . H31A H 0.1299 0.4099 0.6304 0.124 Uiso 1 1 calc R . . H31B H 0.0649 0.4015 0.5479 0.124 Uiso 1 1 calc R . . H31C H 0.0800 0.4998 0.5732 0.124 Uiso 1 1 calc R . . C32 C 0.5867(5) 0.0529(4) 1.1463(3) 0.0524(14) Uani 1 1 d . . . H32A H 0.5534 0.0023 1.1859 0.063 Uiso 1 1 calc R . . H32B H 0.6066 0.1015 1.1775 0.063 Uiso 1 1 calc R . . C33 C 0.7008(5) 0.0181(4) 1.0997(3) 0.0551(14) Uani 1 1 d . . . H33A H 0.7393 0.0699 1.0647 0.066 Uiso 1 1 calc R . . H33B H 0.7589 -0.0122 1.1397 0.066 Uiso 1 1 calc R . . C34 C 0.7662(4) -0.0875(3) 0.9941(3) 0.0436(12) Uani 1 1 d . . . C35 C 0.8284(5) -0.0107(4) 0.9346(3) 0.0583(15) Uani 1 1 d . . . H35A H 0.8610 0.0316 0.9668 0.087 Uiso 1 1 calc R . . H35B H 0.7700 0.0225 0.8973 0.087 Uiso 1 1 calc R . . H35C H 0.8936 -0.0376 0.9021 0.087 Uiso 1 1 calc R . . C36 C 0.8618(5) -0.1414(4) 1.0518(4) 0.0716(17) Uani 1 1 d . . . H36A H 0.8235 -0.1902 1.0896 0.107 Uiso 1 1 calc R . . H36B H 0.8960 -0.0997 1.0837 0.107 Uiso 1 1 calc R . . H36C H 0.9255 -0.1681 1.0179 0.107 Uiso 1 1 calc R . . C37 C 0.7122(5) -0.1542(4) 0.9447(3) 0.0533(14) Uani 1 1 d . . . H37A H 0.6720 -0.2007 0.9852 0.064 Uiso 1 1 calc R . . H37B H 0.7799 -0.1863 0.9175 0.064 Uiso 1 1 calc R . . C38 C 0.6213(5) -0.1180(3) 0.8770(3) 0.0434(12) Uani 1 1 d . . . H38 H 0.6542 -0.0634 0.8413 0.052 Uiso 1 1 calc R . . C39 C 0.6088(6) -0.1932(4) 0.8224(4) 0.0647(16) Uani 1 1 d . . . H39A H 0.5528 -0.1708 0.7792 0.097 Uiso 1 1 calc R . . H39B H 0.5786 -0.2478 0.8568 0.097 Uiso 1 1 calc R . . H39C H 0.6873 -0.2084 0.7967 0.097 Uiso 1 1 calc R . . C40 C 1.1644(5) 0.3904(4) 1.1102(3) 0.0537(14) Uani 1 1 d . . . H40A H 1.1678 0.3365 1.0812 0.064 Uiso 1 1 calc R . . H40B H 1.1978 0.3713 1.1651 0.064 Uiso 1 1 calc R . . C41 C 1.2401(5) 0.4661(4) 1.0595(3) 0.0529(13) Uani 1 1 d . . . H41A H 1.2383 0.5196 1.0889 0.063 Uiso 1 1 calc R . . H41B H 1.3244 0.4429 1.0531 0.063 Uiso 1 1 calc R . . C42 C 1.2366(4) 0.5807(4) 0.9260(3) 0.0462(12) Uani 1 1 d . . . H42 H 1.2062 0.6329 0.9548 0.055 Uiso 1 1 calc R . . C43 C 1.3755(5) 0.5817(5) 0.9180(4) 0.0734(18) Uani 1 1 d . . . H43A H 1.4072 0.5730 0.9732 0.110 Uiso 1 1 calc R . . H43B H 1.3991 0.6405 0.8873 0.110 Uiso 1 1 calc R . . H43C H 1.4076 0.5324 0.8884 0.110 Uiso 1 1 calc R . . C44 C 1.1819(5) 0.5954(4) 0.8385(3) 0.0499(13) Uani 1 1 d . . . H44A H 1.2358 0.6343 0.8001 0.060 Uiso 1 1 calc R . . H44B H 1.1845 0.5352 0.8194 0.060 Uiso 1 1 calc R . . C45 C 1.0522(5) 0.6384(3) 0.8287(3) 0.0489(13) Uani 1 1 d . . . C46 C 1.0400(6) 0.7351(4) 0.8566(4) 0.0681(17) Uani 1 1 d . . . H46A H 1.0564 0.7292 0.9153 0.102 Uiso 1 1 calc R . . H46B H 0.9585 0.7614 0.8482 0.102 Uiso 1 1 calc R . . H46C H 1.0975 0.7749 0.8238 0.102 Uiso 1 1 calc R . . C47 C 1.0269(6) 0.6464(4) 0.7347(3) 0.0693(17) Uani 1 1 d . . . H47A H 0.9457 0.6731 0.7255 0.104 Uiso 1 1 calc R . . H47B H 1.0341 0.5855 0.7181 0.104 Uiso 1 1 calc R . . H47C H 1.0850 0.6854 0.7016 0.104 Uiso 1 1 calc R . . N1 N 0.8214(3) -0.0498(2) 0.59837(19) 0.0228(7) Uani 1 1 d . . . N2 N 0.9888(3) 0.1101(2) 0.63725(19) 0.0244(7) Uani 1 1 d . . . O1 O 0.5164(3) 0.3487(2) 0.5284(2) 0.0388(7) Uani 1 1 d . . . O2 O 0.6918(3) 0.2928(2) 0.4746(3) 0.0611(11) Uani 1 1 d . . . O1W O 0.2999(6) 0.2602(4) 0.7770(3) 0.127(2) Uani 1 1 d . . . O3 O 0.2120(3) 0.1386(2) 0.6771(2) 0.0454(8) Uani 1 1 d . . . H3 H 0.2508 0.1856 0.6638 0.068 Uiso 1 1 calc R . . O2W O 0.3933(8) 0.3595(5) 0.8947(5) 0.071(2) Uani 0.50 1 d P . . O4 O 0.2428(3) -0.0116(2) 0.6735(3) 0.0598(11) Uani 1 1 d . . . O3W O 0.3101(11) 0.7934(6) 0.6828(6) 0.089(3) Uani 0.50 1 d P . . O5 O 0.5771(3) 0.1125(3) 0.8911(2) 0.0585(10) Uani 1 1 d . . . O4W O 0.2012(11) 0.8146(7) 0.6432(8) 0.113(4) Uani 0.50 1 d P . . O6 O 0.5858(3) 0.2337(2) 0.9594(2) 0.0605(11) Uani 1 1 d . . . O7 O 0.9795(3) 0.3766(2) 0.94527(19) 0.0431(8) Uani 1 1 d . . . O8 O 1.1009(4) 0.3814(3) 0.8291(3) 0.0726(13) Uani 1 1 d . . . N3 N 0.6719(4) 0.5020(3) 0.4393(2) 0.0356(9) Uani 1 1 d . . . H48 H 0.695(5) 0.446(4) 0.445(3) 0.053 Uiso 1 1 d . . . N4 N 0.4378(4) 0.5072(3) 0.3778(2) 0.0361(9) Uani 1 1 d . . . H49 H 0.432(5) 0.559(4) 0.367(3) 0.054 Uiso 1 1 d . . . N5 N 0.4968(4) 0.0897(3) 1.0838(3) 0.0415(10) Uani 1 1 d . . . H50 H 0.522(5) 0.134(4) 1.056(4) 0.062 Uiso 1 1 d . . . N6 N 0.6637(3) -0.0482(3) 1.0472(2) 0.0403(10) Uani 1 1 d . . . H51 H 0.636(5) -0.096(4) 1.086(3) 0.060 Uiso 1 1 d . . . N7 N 1.0357(4) 0.4257(3) 1.1209(2) 0.0426(10) Uani 1 1 d . . . H52 H 1.043(5) 0.483(4) 1.144(3) 0.064 Uiso 1 1 d . . . N8 N 1.1899(4) 0.4938(3) 0.9760(3) 0.0422(10) Uani 1 1 d . . . H53 H 1.204(5) 0.450(4) 0.946(3) 0.063 Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0243(4) 0.0295(4) 0.0270(4) -0.0050(3) 0.0000(3) -0.0010(4) Co2 0.0281(5) 0.0483(5) 0.0336(5) -0.0136(4) 0.0057(4) -0.0016(4) Co3 0.0375(5) 0.0405(5) 0.0345(5) -0.0138(4) -0.0073(4) -0.0001(4) C1 0.025(2) 0.030(2) 0.032(2) -0.0098(18) -0.0050(18) 0.0009(19) C2 0.025(2) 0.031(2) 0.035(2) -0.0072(18) -0.0044(18) 0.0050(19) C3 0.021(2) 0.037(2) 0.030(2) -0.0095(18) -0.0018(17) -0.002(2) C4 0.027(2) 0.030(2) 0.031(2) -0.0048(17) -0.0040(18) -0.004(2) C5 0.023(2) 0.028(2) 0.032(2) -0.0068(17) -0.0059(18) -0.0018(18) C6 0.022(2) 0.034(2) 0.030(2) -0.0099(18) -0.0006(17) -0.0036(19) C7 0.033(3) 0.031(2) 0.040(3) -0.0063(19) -0.002(2) -0.001(2) C8 0.024(2) 0.046(3) 0.042(3) -0.008(2) 0.000(2) 0.000(2) C9 0.027(2) 0.029(2) 0.035(2) -0.0084(18) 0.0000(19) -0.0053(19) C10 0.023(2) 0.033(2) 0.023(2) -0.0068(17) 0.0044(17) -0.0030(18) C11 0.027(2) 0.035(2) 0.024(2) -0.0082(17) 0.0021(17) -0.0025(19) C12 0.028(2) 0.033(2) 0.031(2) -0.0161(18) 0.0102(18) -0.0040(19) C13 0.034(2) 0.027(2) 0.033(2) -0.0110(18) 0.0113(19) -0.0006(19) C14 0.027(2) 0.026(2) 0.029(2) -0.0023(17) 0.0047(18) 0.0054(18) C15 0.027(2) 0.036(2) 0.027(2) -0.0114(18) 0.0020(18) 0.0006(19) C16 0.027(2) 0.028(2) 0.029(2) -0.0104(17) 0.0012(18) 0.0034(18) C17 0.029(2) 0.035(2) 0.038(3) -0.0181(19) 0.0033(19) -0.004(2) C18 0.029(2) 0.037(2) 0.034(2) -0.0108(19) 0.0076(19) -0.002(2) C19 0.037(3) 0.036(2) 0.028(2) -0.0144(18) 0.0047(19) 0.001(2) C20 0.031(2) 0.033(2) 0.031(2) -0.0135(18) -0.0012(19) 0.001(2) C21 0.025(2) 0.036(2) 0.032(2) -0.0111(18) 0.0056(18) -0.0010(19) C22 0.040(3) 0.046(3) 0.045(3) -0.015(2) 0.014(2) -0.006(2) C23 0.033(3) 0.041(3) 0.044(3) -0.020(2) 0.000(2) 0.000(2) C24 0.038(3) 0.064(3) 0.045(3) -0.003(2) 0.011(2) 0.003(3) C25 0.054(3) 0.071(4) 0.032(3) -0.019(2) 0.001(2) 0.005(3) C26 0.048(3) 0.050(3) 0.051(3) -0.013(2) -0.021(3) -0.003(3) C27 0.072(4) 0.088(4) 0.060(4) -0.014(3) -0.036(3) 0.003(4) C28 0.066(4) 0.058(4) 0.086(4) -0.031(3) -0.021(3) -0.007(3) C29 0.032(3) 0.056(3) 0.062(3) -0.011(3) -0.014(2) -0.001(2) C30 0.032(3) 0.039(3) 0.066(3) -0.002(2) -0.003(2) -0.008(2) C31 0.041(4) 0.108(5) 0.092(5) 0.007(4) -0.001(3) -0.022(4) C32 0.044(3) 0.078(4) 0.038(3) -0.022(3) -0.003(2) 0.002(3) C33 0.037(3) 0.081(4) 0.050(3) -0.021(3) -0.004(2) 0.002(3) C34 0.032(3) 0.050(3) 0.046(3) -0.004(2) 0.013(2) 0.001(2) C35 0.045(3) 0.068(4) 0.060(4) -0.009(3) 0.019(3) -0.010(3) C36 0.052(4) 0.078(4) 0.077(4) 0.003(3) -0.006(3) 0.018(3) C37 0.047(3) 0.047(3) 0.062(4) -0.006(3) 0.019(3) -0.001(3) C38 0.046(3) 0.044(3) 0.039(3) -0.010(2) 0.015(2) -0.001(2) C39 0.072(4) 0.066(4) 0.059(4) -0.026(3) 0.013(3) 0.004(3) C40 0.058(4) 0.058(3) 0.046(3) -0.011(2) -0.013(3) 0.011(3) C41 0.044(3) 0.066(3) 0.051(3) -0.015(3) -0.012(3) 0.007(3) C42 0.039(3) 0.054(3) 0.049(3) -0.020(2) 0.010(2) -0.007(3) C43 0.057(4) 0.086(4) 0.078(4) -0.014(3) 0.008(3) -0.013(3) C44 0.062(4) 0.049(3) 0.042(3) -0.018(2) 0.004(3) -0.003(3) C45 0.060(4) 0.044(3) 0.042(3) -0.005(2) 0.002(2) -0.002(3) C46 0.079(4) 0.047(3) 0.078(4) -0.015(3) 0.008(3) -0.005(3) C47 0.084(5) 0.076(4) 0.045(3) -0.001(3) -0.005(3) 0.001(4) N1 0.0205(17) 0.0231(17) 0.0249(18) -0.0053(13) 0.0019(14) -0.0004(14) N2 0.0252(18) 0.0262(17) 0.0228(17) -0.0096(13) 0.0061(14) -0.0006(15) O1 0.0349(18) 0.0285(16) 0.052(2) -0.0071(14) 0.0023(15) 0.0037(15) O2 0.046(2) 0.0338(19) 0.097(3) -0.0041(18) 0.028(2) -0.0038(17) O1W 0.136(5) 0.157(5) 0.104(4) -0.065(4) 0.031(4) -0.069(4) O3 0.0242(17) 0.048(2) 0.067(2) -0.0220(17) 0.0061(16) -0.0023(16) O2W 0.095(6) 0.039(4) 0.085(6) -0.034(4) -0.038(5) 0.029(4) O4 0.0282(19) 0.038(2) 0.110(3) -0.0095(19) 0.0147(19) -0.0027(16) O3W 0.119(9) 0.056(5) 0.085(7) -0.001(4) 0.017(6) -0.001(6) O5 0.051(2) 0.065(2) 0.065(2) -0.0299(19) 0.0236(18) -0.027(2) O4W 0.100(8) 0.085(7) 0.159(11) -0.049(7) 0.080(8) -0.039(7) O6 0.066(3) 0.056(2) 0.062(2) -0.0282(18) 0.038(2) -0.016(2) O7 0.049(2) 0.0465(19) 0.0393(19) -0.0249(15) -0.0013(15) -0.0051(16) O8 0.059(3) 0.092(3) 0.081(3) -0.056(2) 0.030(2) -0.040(2) N3 0.032(2) 0.031(2) 0.043(2) -0.0050(18) 0.0035(17) 0.0017(18) N4 0.039(2) 0.036(2) 0.034(2) -0.0099(18) -0.0024(17) 0.003(2) N5 0.034(2) 0.051(3) 0.039(2) -0.0095(18) 0.0134(18) -0.006(2) N6 0.031(2) 0.048(2) 0.040(2) -0.0044(18) 0.0036(18) 0.0006(19) N7 0.050(3) 0.040(2) 0.040(2) -0.0101(18) -0.0067(19) 0.002(2) N8 0.040(2) 0.049(2) 0.041(2) -0.0186(19) -0.0032(19) 0.003(2) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 N3 2.070(4) . ? Co1 N3 2.070(4) 2_666 ? Co1 N4 2.103(4) . ? Co1 N4 2.103(4) 2_666 ? Co1 O1 2.176(3) 2_666 ? Co1 O1 2.176(3) . ? Co2 N5 2.013(4) 2_657 ? Co2 N5 2.013(4) . ? Co2 N6 2.035(4) . ? Co2 N6 2.035(4) 2_657 ? Co2 O5 2.357(3) . ? Co2 O5 2.357(3) 2_657 ? Co3 N8 2.095(4) . ? Co3 N8 2.095(4) 2_767 ? Co3 N7 2.117(4) 2_767 ? Co3 N7 2.117(4) . ? Co3 O7 2.147(3) 2_767 ? Co3 O7 2.147(3) . ? C1 C2 1.388(6) . ? C1 C6 1.395(6) . ? C1 C7 1.513(6) . ? C2 C3 1.385(6) . ? C2 H2 0.9300 . ? C3 C4 1.386(6) . ? C3 C8 1.517(6) . ? C4 C5 1.390(6) . ? C4 H4 0.9300 . ? C5 C6 1.395(6) . ? C5 C9 1.505(6) . ? C6 H6 0.9300 . ? C7 O2 1.244(5) . ? C7 O1 1.253(5) . ? C8 O4 1.227(5) . ? C8 O3 1.268(5) . ? C9 N1 1.472(5) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 N1 1.463(5) . ? C10 C11 1.530(5) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 N2 1.503(5) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 N2 1.500(5) . ? C12 C13 1.518(5) . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C13 C14 1.533(5) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 N1 1.461(5) 2_756 ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 C16 1.504(5) . ? C15 N2 1.508(5) . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 C21 1.386(5) . ? C16 C17 1.389(6) . ? C17 C18 1.388(6) . ? C17 H17 0.9300 . ? C18 C19 1.388(6) . ? C18 C22 1.516(6) . ? C19 C20 1.372(6) . ? C19 H19 0.9300 . ? C20 C21 1.383(6) . ? C20 C23 1.513(6) . ? C21 H21 0.9300 . ? C22 O6 1.242(5) . ? C22 O5 1.260(5) . ? C23 O8 1.243(5) . ? C23 O7 1.257(5) . ? C24 N3 1.471(6) . ? C24 C25 1.506(7) . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C25 N4 1.481(6) . ? C25 H25A 0.9700 . ? C25 H25B 0.9700 . ? C26 N4 1.497(6) . ? C26 C27 1.522(7) . ? C26 C29 1.525(7) . ? C26 C28 1.538(7) . ? C27 H27A 0.9600 . ? C27 H27B 0.9600 . ? C27 H27C 0.9600 . ? C28 H28A 0.9600 . ? C28 H28B 0.9600 . ? C28 H28C 0.9600 . ? C29 C30 1.538(7) . ? C29 H29A 0.9700 . ? C29 H29B 0.9700 . ? C30 N3 1.483(6) 2_666 ? C30 C31 1.530(7) . ? C30 H30 0.9800 . ? C31 H31A 0.9600 . ? C31 H31B 0.9600 . ? C31 H31C 0.9600 . ? C32 N5 1.468(6) . ? C32 C33 1.520(7) . ? C32 H32A 0.9700 . ? C32 H32B 0.9700 . ? C33 N6 1.467(6) . ? C33 H33A 0.9700 . ? C33 H33B 0.9700 . ? C34 N6 1.508(6) . ? C34 C37 1.514(7) . ? C34 C35 1.522(6) . ? C34 C36 1.537(7) . ? C35 H35A 0.9600 . ? C35 H35B 0.9600 . ? C35 H35C 0.9600 . ? C36 H36A 0.9600 . ? C36 H36B 0.9600 . ? C36 H36C 0.9600 . ? C37 C38 1.530(7) . ? C37 H37A 0.9700 . ? C37 H37B 0.9700 . ? C38 N5 1.471(6) 2_657 ? C38 C39 1.521(7) . ? C38 H38 0.9800 . ? C39 H39A 0.9600 . ? C39 H39B 0.9600 . ? C39 H39C 0.9600 . ? C40 N7 1.481(7) . ? C40 C41 1.523(7) . ? C40 H40A 0.9700 . ? C40 H40B 0.9700 . ? C41 N8 1.470(6) . ? C41 H41A 0.9700 . ? C41 H41B 0.9700 . ? C42 N8 1.489(6) . ? C42 C43 1.523(7) . ? C42 C44 1.541(7) . ? C42 H42 0.9800 . ? C43 H43A 0.9600 . ? C43 H43B 0.9600 . ? C43 H43C 0.9600 . ? C44 C45 1.525(8) . ? C44 H44A 0.9700 . ? C44 H44B 0.9700 . ? C45 N7 1.496(6) 2_767 ? C45 C46 1.537(7) . ? C45 C47 1.538(7) . ? C46 H46A 0.9600 . ? C46 H46B 0.9600 . ? C46 H46C 0.9600 . ? C47 H47A 0.9600 . ? C47 H47B 0.9600 . ? C47 H47C 0.9600 . ? N1 C14 1.461(5) 2_756 ? O3 H3 0.8200 . ? O3W O4W 1.384(15) . ? N3 C30 1.483(6) 2_666 ? N3 H48 0.82(5) . ? N4 H49 0.75(5) . ? N5 C38 1.471(6) 2_657 ? N5 H50 0.78(5) . ? N6 H51 0.91(5) . ? N7 C45 1.496(6) 2_767 ? N7 H52 0.96(5) . ? N8 H53 0.86(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N3 Co1 N3 180.0 . 2_666 ? N3 Co1 N4 84.32(15) . . ? N3 Co1 N4 95.68(15) 2_666 . ? N3 Co1 N4 95.68(15) . 2_666 ? N3 Co1 N4 84.32(15) 2_666 2_666 ? N4 Co1 N4 180.000(1) . 2_666 ? N3 Co1 O1 89.39(13) . 2_666 ? N3 Co1 O1 90.61(13) 2_666 2_666 ? N4 Co1 O1 83.51(13) . 2_666 ? N4 Co1 O1 96.49(13) 2_666 2_666 ? N3 Co1 O1 90.61(13) . . ? N3 Co1 O1 89.39(13) 2_666 . ? N4 Co1 O1 96.49(13) . . ? N4 Co1 O1 83.51(13) 2_666 . ? O1 Co1 O1 180.00(16) 2_666 . ? N5 Co2 N5 180.000(1) 2_657 . ? N5 Co2 N6 94.79(17) 2_657 . ? N5 Co2 N6 85.21(17) . . ? N5 Co2 N6 85.21(17) 2_657 2_657 ? N5 Co2 N6 94.79(17) . 2_657 ? N6 Co2 N6 180.000(1) . 2_657 ? N5 Co2 O5 88.54(14) 2_657 . ? N5 Co2 O5 91.46(14) . . ? N6 Co2 O5 96.92(15) . . ? N6 Co2 O5 83.08(15) 2_657 . ? N5 Co2 O5 91.46(14) 2_657 2_657 ? N5 Co2 O5 88.54(14) . 2_657 ? N6 Co2 O5 83.08(15) . 2_657 ? N6 Co2 O5 96.92(15) 2_657 2_657 ? O5 Co2 O5 180.0 . 2_657 ? N8 Co3 N8 180.000(1) . 2_767 ? N8 Co3 N7 93.86(16) . 2_767 ? N8 Co3 N7 86.14(16) 2_767 2_767 ? N8 Co3 N7 86.14(16) . . ? N8 Co3 N7 93.86(16) 2_767 . ? N7 Co3 N7 180.000(1) 2_767 . ? N8 Co3 O7 87.65(14) . 2_767 ? N8 Co3 O7 92.35(14) 2_767 2_767 ? N7 Co3 O7 94.09(14) 2_767 2_767 ? N7 Co3 O7 85.91(14) . 2_767 ? N8 Co3 O7 92.35(14) . . ? N8 Co3 O7 87.65(14) 2_767 . ? N7 Co3 O7 85.91(14) 2_767 . ? N7 Co3 O7 94.09(14) . . ? O7 Co3 O7 180.00(7) 2_767 . ? C2 C1 C6 118.7(4) . . ? C2 C1 C7 120.1(4) . . ? C6 C1 C7 121.2(4) . . ? C3 C2 C1 121.1(4) . . ? C3 C2 H2 119.4 . . ? C1 C2 H2 119.4 . . ? C2 C3 C4 119.1(4) . . ? C2 C3 C8 120.8(4) . . ? C4 C3 C8 120.1(4) . . ? C3 C4 C5 121.5(4) . . ? C3 C4 H4 119.2 . . ? C5 C4 H4 119.2 . . ? C4 C5 C6 118.1(4) . . ? C4 C5 C9 119.3(3) . . ? C6 C5 C9 122.5(4) . . ? C5 C6 C1 121.3(4) . . ? C5 C6 H6 119.3 . . ? C1 C6 H6 119.3 . . ? O2 C7 O1 125.6(4) . . ? O2 C7 C1 118.2(4) . . ? O1 C7 C1 116.2(4) . . ? O4 C8 O3 123.8(4) . . ? O4 C8 C3 118.6(4) . . ? O3 C8 C3 117.6(4) . . ? N1 C9 C5 115.2(3) . . ? N1 C9 H9A 108.5 . . ? C5 C9 H9A 108.5 . . ? N1 C9 H9B 108.5 . . ? C5 C9 H9B 108.5 . . ? H9A C9 H9B 107.5 . . ? N1 C10 C11 116.8(3) . . ? N1 C10 H10A 108.1 . . ? C11 C10 H10A 108.1 . . ? N1 C10 H10B 108.1 . . ? C11 C10 H10B 108.1 . . ? H10A C10 H10B 107.3 . . ? N2 C11 C10 117.8(3) . . ? N2 C11 H11A 107.9 . . ? C10 C11 H11A 107.9 . . ? N2 C11 H11B 107.9 . . ? C10 C11 H11B 107.9 . . ? H11A C11 H11B 107.2 . . ? N2 C12 C13 115.8(3) . . ? N2 C12 H12A 108.3 . . ? C13 C12 H12A 108.3 . . ? N2 C12 H12B 108.3 . . ? C13 C12 H12B 108.3 . . ? H12A C12 H12B 107.4 . . ? C12 C13 C14 109.0(3) . . ? C12 C13 H13A 109.9 . . ? C14 C13 H13A 109.9 . . ? C12 C13 H13B 109.9 . . ? C14 C13 H13B 109.9 . . ? H13A C13 H13B 108.3 . . ? N1 C14 C13 115.4(3) 2_756 . ? N1 C14 H14A 108.4 2_756 . ? C13 C14 H14A 108.4 . . ? N1 C14 H14B 108.4 2_756 . ? C13 C14 H14B 108.4 . . ? H14A C14 H14B 107.5 . . ? C16 C15 N2 113.4(3) . . ? C16 C15 H15A 108.9 . . ? N2 C15 H15A 108.9 . . ? C16 C15 H15B 108.9 . . ? N2 C15 H15B 108.9 . . ? H15A C15 H15B 107.7 . . ? C21 C16 C17 119.0(4) . . ? C21 C16 C15 119.8(4) . . ? C17 C16 C15 121.1(3) . . ? C18 C17 C16 120.8(4) . . ? C18 C17 H17 119.6 . . ? C16 C17 H17 119.6 . . ? C19 C18 C17 118.7(4) . . ? C19 C18 C22 118.9(4) . . ? C17 C18 C22 122.3(4) . . ? C20 C19 C18 121.4(4) . . ? C20 C19 H19 119.3 . . ? C18 C19 H19 119.3 . . ? C19 C20 C21 119.3(4) . . ? C19 C20 C23 120.2(4) . . ? C21 C20 C23 120.4(4) . . ? C20 C21 C16 120.8(4) . . ? C20 C21 H21 119.6 . . ? C16 C21 H21 119.6 . . ? O6 C22 O5 125.6(4) . . ? O6 C22 C18 117.0(4) . . ? O5 C22 C18 117.3(4) . . ? O8 C23 O7 125.2(4) . . ? O8 C23 C20 117.9(4) . . ? O7 C23 C20 116.9(4) . . ? N3 C24 C25 109.1(4) . . ? N3 C24 H24A 109.9 . . ? C25 C24 H24A 109.9 . . ? N3 C24 H24B 109.9 . . ? C25 C24 H24B 109.9 . . ? H24A C24 H24B 108.3 . . ? N4 C25 C24 108.6(4) . . ? N4 C25 H25A 110.0 . . ? C24 C25 H25A 110.0 . . ? N4 C25 H25B 110.0 . . ? C24 C25 H25B 110.0 . . ? H25A C25 H25B 108.3 . . ? N4 C26 C27 109.9(4) . . ? N4 C26 C29 108.5(4) . . ? C27 C26 C29 108.0(5) . . ? N4 C26 C28 109.7(4) . . ? C27 C26 C28 109.8(4) . . ? C29 C26 C28 110.8(4) . . ? C26 C27 H27A 109.5 . . ? C26 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C26 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C26 C28 H28A 109.5 . . ? C26 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C26 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C26 C29 C30 120.6(4) . . ? C26 C29 H29A 107.2 . . ? C30 C29 H29A 107.2 . . ? C26 C29 H29B 107.2 . . ? C30 C29 H29B 107.2 . . ? H29A C29 H29B 106.8 . . ? N3 C30 C31 112.6(5) 2_666 . ? N3 C30 C29 109.1(4) 2_666 . ? C31 C30 C29 111.5(4) . . ? N3 C30 H30 107.9 2_666 . ? C31 C30 H30 107.9 . . ? C29 C30 H30 107.9 . . ? C30 C31 H31A 109.5 . . ? C30 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C30 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? N5 C32 C33 108.2(4) . . ? N5 C32 H32A 110.0 . . ? C33 C32 H32A 110.0 . . ? N5 C32 H32B 110.0 . . ? C33 C32 H32B 110.0 . . ? H32A C32 H32B 108.4 . . ? N6 C33 C32 107.8(4) . . ? N6 C33 H33A 110.2 . . ? C32 C33 H33A 110.2 . . ? N6 C33 H33B 110.2 . . ? C32 C33 H33B 110.2 . . ? H33A C33 H33B 108.5 . . ? N6 C34 C37 107.7(4) . . ? N6 C34 C35 111.3(4) . . ? C37 C34 C35 110.4(4) . . ? N6 C34 C36 109.6(4) . . ? C37 C34 C36 109.0(4) . . ? C35 C34 C36 108.7(4) . . ? C34 C35 H35A 109.5 . . ? C34 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C34 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C34 C36 H36A 109.5 . . ? C34 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C34 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C34 C37 C38 120.4(4) . . ? C34 C37 H37A 107.2 . . ? C38 C37 H37A 107.2 . . ? C34 C37 H37B 107.2 . . ? C38 C37 H37B 107.2 . . ? H37A C37 H37B 106.9 . . ? N5 C38 C39 112.0(4) 2_657 . ? N5 C38 C37 110.5(4) 2_657 . ? C39 C38 C37 108.9(4) . . ? N5 C38 H38 108.5 2_657 . ? C39 C38 H38 108.5 . . ? C37 C38 H38 108.5 . . ? C38 C39 H39A 109.5 . . ? C38 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C38 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? N7 C40 C41 110.1(4) . . ? N7 C40 H40A 109.6 . . ? C41 C40 H40A 109.6 . . ? N7 C40 H40B 109.6 . . ? C41 C40 H40B 109.6 . . ? H40A C40 H40B 108.2 . . ? N8 C41 C40 109.3(4) . . ? N8 C41 H41A 109.8 . . ? C40 C41 H41A 109.8 . . ? N8 C41 H41B 109.8 . . ? C40 C41 H41B 109.8 . . ? H41A C41 H41B 108.3 . . ? N8 C42 C43 113.9(5) . . ? N8 C42 C44 108.6(4) . . ? C43 C42 C44 111.1(4) . . ? N8 C42 H42 107.7 . . ? C43 C42 H42 107.7 . . ? C44 C42 H42 107.7 . . ? C42 C43 H43A 109.5 . . ? C42 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C42 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C45 C44 C42 119.4(4) . . ? C45 C44 H44A 107.5 . . ? C42 C44 H44A 107.5 . . ? C45 C44 H44B 107.5 . . ? C42 C44 H44B 107.5 . . ? H44A C44 H44B 107.0 . . ? N7 C45 C44 109.1(4) 2_767 . ? N7 C45 C46 110.8(4) 2_767 . ? C44 C45 C46 111.1(4) . . ? N7 C45 C47 108.9(4) 2_767 . ? C44 C45 C47 106.6(5) . . ? C46 C45 C47 110.3(5) . . ? C45 C46 H46A 109.5 . . ? C45 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? C45 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? C45 C47 H47A 109.5 . . ? C45 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? C45 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? C14 N1 C10 110.3(3) 2_756 . ? C14 N1 C9 109.5(3) 2_756 . ? C10 N1 C9 111.5(3) . . ? C12 N2 C11 111.0(3) . . ? C12 N2 C15 111.2(3) . . ? C11 N2 C15 113.8(3) . . ? C7 O1 Co1 138.3(3) . . ? C8 O3 H3 109.5 . . ? C22 O5 Co2 123.9(3) . . ? C23 O7 Co3 132.9(3) . . ? C24 N3 C30 114.8(4) . 2_666 ? C24 N3 Co1 106.6(3) . . ? C30 N3 Co1 113.8(3) 2_666 . ? C24 N3 H48 108(4) . . ? C30 N3 H48 110(4) 2_666 . ? Co1 N3 H48 103(4) . . ? C25 N4 C26 117.5(4) . . ? C25 N4 Co1 106.0(3) . . ? C26 N4 Co1 122.1(3) . . ? C25 N4 H49 100(5) . . ? C26 N4 H49 109(4) . . ? Co1 N4 H49 98(4) . . ? C32 N5 C38 112.6(4) . 2_657 ? C32 N5 Co2 107.1(3) . . ? C38 N5 Co2 118.9(3) 2_657 . ? C32 N5 H50 109(4) . . ? C38 N5 H50 107(4) 2_657 . ? Co2 N5 H50 102(4) . . ? C33 N6 C34 114.8(4) . . ? C33 N6 Co2 107.9(3) . . ? C34 N6 Co2 122.5(3) . . ? C33 N6 H51 103(3) . . ? C34 N6 H51 108(3) . . ? Co2 N6 H51 97(3) . . ? C40 N7 C45 117.8(4) . 2_767 ? C40 N7 Co3 103.0(3) . . ? C45 N7 Co3 123.2(3) 2_767 . ? C40 N7 H52 103(3) . . ? C45 N7 H52 114(3) 2_767 . ? Co3 N7 H52 92(3) . . ? C41 N8 C42 115.6(4) . . ? C41 N8 Co3 104.6(3) . . ? C42 N8 Co3 113.5(3) . . ? C41 N8 H53 111(4) . . ? C42 N8 H53 107(4) . . ? Co3 N8 H53 105(4) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C6 C1 C2 C3 -1.3(6) . . . . ? C7 C1 C2 C3 179.4(4) . . . . ? C1 C2 C3 C4 3.8(6) . . . . ? C1 C2 C3 C8 -173.3(4) . . . . ? C2 C3 C4 C5 -2.2(6) . . . . ? C8 C3 C4 C5 174.9(4) . . . . ? C3 C4 C5 C6 -1.7(6) . . . . ? C3 C4 C5 C9 -179.8(4) . . . . ? C4 C5 C6 C1 4.3(6) . . . . ? C9 C5 C6 C1 -177.6(4) . . . . ? C2 C1 C6 C5 -2.9(6) . . . . ? C7 C1 C6 C5 176.5(4) . . . . ? C2 C1 C7 O2 -176.4(4) . . . . ? C6 C1 C7 O2 4.2(6) . . . . ? C2 C1 C7 O1 4.5(6) . . . . ? C6 C1 C7 O1 -174.8(4) . . . . ? C2 C3 C8 O4 163.1(4) . . . . ? C4 C3 C8 O4 -14.0(6) . . . . ? C2 C3 C8 O3 -14.1(6) . . . . ? C4 C3 C8 O3 168.8(4) . . . . ? C4 C5 C9 N1 -138.6(4) . . . . ? C6 C5 C9 N1 43.4(5) . . . . ? N1 C10 C11 N2 63.9(5) . . . . ? N2 C12 C13 C14 -179.8(3) . . . . ? C12 C13 C14 N1 -58.2(5) . . . 2_756 ? N2 C15 C16 C21 78.5(5) . . . . ? N2 C15 C16 C17 -102.9(4) . . . . ? C21 C16 C17 C18 0.4(6) . . . . ? C15 C16 C17 C18 -178.3(4) . . . . ? C16 C17 C18 C19 0.3(7) . . . . ? C16 C17 C18 C22 -175.9(4) . . . . ? C17 C18 C19 C20 -0.4(7) . . . . ? C22 C18 C19 C20 175.9(4) . . . . ? C18 C19 C20 C21 -0.1(7) . . . . ? C18 C19 C20 C23 176.1(4) . . . . ? C19 C20 C21 C16 0.8(7) . . . . ? C23 C20 C21 C16 -175.4(4) . . . . ? C17 C16 C21 C20 -0.9(6) . . . . ? C15 C16 C21 C20 177.7(4) . . . . ? C19 C18 C22 O6 24.9(7) . . . . ? C17 C18 C22 O6 -158.9(5) . . . . ? C19 C18 C22 O5 -150.8(5) . . . . ? C17 C18 C22 O5 25.4(7) . . . . ? C19 C20 C23 O8 -174.6(5) . . . . ? C21 C20 C23 O8 1.6(7) . . . . ? C19 C20 C23 O7 3.3(7) . . . . ? C21 C20 C23 O7 179.5(4) . . . . ? N3 C24 C25 N4 57.1(6) . . . . ? N4 C26 C29 C30 -65.2(6) . . . . ? C27 C26 C29 C30 175.6(4) . . . . ? C28 C26 C29 C30 55.3(6) . . . . ? C26 C29 C30 N3 79.8(5) . . . 2_666 ? C26 C29 C30 C31 -155.3(5) . . . . ? N5 C32 C33 N6 -54.2(6) . . . . ? N6 C34 C37 C38 65.9(5) . . . . ? C35 C34 C37 C38 -55.8(6) . . . . ? C36 C34 C37 C38 -175.2(4) . . . . ? C34 C37 C38 N5 -71.6(5) . . . 2_657 ? C34 C37 C38 C39 165.0(4) . . . . ? N7 C40 C41 N8 -60.0(5) . . . . ? N8 C42 C44 C45 80.7(5) . . . . ? C43 C42 C44 C45 -153.3(5) . . . . ? C42 C44 C45 N7 -64.3(5) . . . 2_767 ? C42 C44 C45 C46 58.2(6) . . . . ? C42 C44 C45 C47 178.3(4) . . . . ? C11 C10 N1 C14 72.5(4) . . . 2_756 ? C11 C10 N1 C9 -165.6(3) . . . . ? C5 C9 N1 C14 178.4(3) . . . 2_756 ? C5 C9 N1 C10 56.1(4) . . . . ? C13 C12 N2 C11 -167.8(4) . . . . ? C13 C12 N2 C15 64.4(4) . . . . ? C10 C11 N2 C12 -67.9(5) . . . . ? C10 C11 N2 C15 58.6(4) . . . . ? C16 C15 N2 C12 -177.1(3) . . . . ? C16 C15 N2 C11 56.6(4) . . . . ? O2 C7 O1 Co1 0.3(8) . . . . ? C1 C7 O1 Co1 179.2(3) . . . . ? N3 Co1 O1 C7 -2.1(4) . . . . ? N3 Co1 O1 C7 177.9(4) 2_666 . . . ? N4 Co1 O1 C7 82.3(5) . . . . ? N4 Co1 O1 C7 -97.7(5) 2_666 . . . ? O1 Co1 O1 C7 114(100) 2_666 . . . ? O6 C22 O5 Co2 -35.6(8) . . . . ? C18 C22 O5 Co2 139.7(3) . . . . ? N5 Co2 O5 C22 -165.5(4) 2_657 . . . ? N5 Co2 O5 C22 14.5(4) . . . . ? N6 Co2 O5 C22 -70.8(4) . . . . ? N6 Co2 O5 C22 109.2(4) 2_657 . . . ? O5 Co2 O5 C22 -35(100) 2_657 . . . ? O8 C23 O7 Co3 32.4(8) . . . . ? C20 C23 O7 Co3 -145.3(3) . . . . ? N8 Co3 O7 C23 -56.3(4) . . . . ? N8 Co3 O7 C23 123.7(4) 2_767 . . . ? N7 Co3 O7 C23 37.4(4) 2_767 . . . ? N7 Co3 O7 C23 -142.6(4) . . . . ? O7 Co3 O7 C23 -177(100) 2_767 . . . ? C25 C24 N3 C30 -169.6(4) . . . 2_666 ? C25 C24 N3 Co1 -42.6(5) . . . . ? N3 Co1 N3 C24 88(100) 2_666 . . . ? N4 Co1 N3 C24 15.8(3) . . . . ? N4 Co1 N3 C24 -164.2(3) 2_666 . . . ? O1 Co1 N3 C24 -67.8(3) 2_666 . . . ? O1 Co1 N3 C24 112.2(3) . . . . ? N3 Co1 N3 C30 -145(100) 2_666 . . 2_666 ? N4 Co1 N3 C30 143.3(3) . . . 2_666 ? N4 Co1 N3 C30 -36.7(3) 2_666 . . 2_666 ? O1 Co1 N3 C30 59.7(3) 2_666 . . 2_666 ? O1 Co1 N3 C30 -120.3(3) . . . 2_666 ? C24 C25 N4 C26 179.0(4) . . . . ? C24 C25 N4 Co1 -40.3(5) . . . . ? C27 C26 N4 C25 -68.5(6) . . . . ? C29 C26 N4 C25 173.6(4) . . . . ? C28 C26 N4 C25 52.3(6) . . . . ? C27 C26 N4 Co1 157.5(4) . . . . ? C29 C26 N4 Co1 39.6(5) . . . . ? C28 C26 N4 Co1 -81.6(5) . . . . ? N3 Co1 N4 C25 13.6(3) . . . . ? N3 Co1 N4 C25 -166.4(3) 2_666 . . . ? N4 Co1 N4 C25 -125(100) 2_666 . . . ? O1 Co1 N4 C25 103.6(3) 2_666 . . . ? O1 Co1 N4 C25 -76.4(3) . . . . ? N3 Co1 N4 C26 152.0(4) . . . . ? N3 Co1 N4 C26 -28.0(4) 2_666 . . . ? N4 Co1 N4 C26 14(100) 2_666 . . . ? O1 Co1 N4 C26 -118.0(4) 2_666 . . . ? O1 Co1 N4 C26 62.0(4) . . . . ? C33 C32 N5 C38 175.1(4) . . . 2_657 ? C33 C32 N5 Co2 42.6(5) . . . . ? N5 Co2 N5 C32 -101(100) 2_657 . . . ? N6 Co2 N5 C32 -17.3(3) . . . . ? N6 Co2 N5 C32 162.7(3) 2_657 . . . ? O5 Co2 N5 C32 -114.1(3) . . . . ? O5 Co2 N5 C32 65.9(3) 2_657 . . . ? N5 Co2 N5 C38 130(100) 2_657 . . 2_657 ? N6 Co2 N5 C38 -146.3(4) . . . 2_657 ? N6 Co2 N5 C38 33.7(4) 2_657 . . 2_657 ? O5 Co2 N5 C38 116.9(4) . . . 2_657 ? O5 Co2 N5 C38 -63.1(4) 2_657 . . 2_657 ? C32 C33 N6 C34 178.2(4) . . . . ? C32 C33 N6 Co2 37.7(5) . . . . ? C37 C34 N6 C33 179.8(4) . . . . ? C35 C34 N6 C33 -59.0(6) . . . . ? C36 C34 N6 C33 61.3(5) . . . . ? C37 C34 N6 Co2 -46.1(5) . . . . ? C35 C34 N6 Co2 75.0(5) . . . . ? C36 C34 N6 Co2 -164.6(3) . . . . ? N5 Co2 N6 C33 168.2(3) 2_657 . . . ? N5 Co2 N6 C33 -11.8(3) . . . . ? N6 Co2 N6 C33 -140(100) 2_657 . . . ? O5 Co2 N6 C33 79.1(3) . . . . ? O5 Co2 N6 C33 -100.9(3) 2_657 . . . ? N5 Co2 N6 C34 31.5(3) 2_657 . . . ? N5 Co2 N6 C34 -148.5(3) . . . . ? N6 Co2 N6 C34 83(100) 2_657 . . . ? O5 Co2 N6 C34 -57.6(3) . . . . ? O5 Co2 N6 C34 122.4(3) 2_657 . . . ? C41 C40 N7 C45 -178.4(4) . . . 2_767 ? C41 C40 N7 Co3 42.5(4) . . . . ? N8 Co3 N7 C40 -15.2(3) . . . . ? N8 Co3 N7 C40 164.8(3) 2_767 . . . ? N7 Co3 N7 C40 91(100) 2_767 . . . ? O7 Co3 N7 C40 -103.1(3) 2_767 . . . ? O7 Co3 N7 C40 76.9(3) . . . . ? N8 Co3 N7 C45 -151.5(4) . . . 2_767 ? N8 Co3 N7 C45 28.5(4) 2_767 . . 2_767 ? N7 Co3 N7 C45 -46(100) 2_767 . . 2_767 ? O7 Co3 N7 C45 120.6(4) 2_767 . . 2_767 ? O7 Co3 N7 C45 -59.4(4) . . . 2_767 ? C40 C41 N8 C42 167.3(4) . . . . ? C40 C41 N8 Co3 41.8(5) . . . . ? C43 C42 N8 C41 51.6(6) . . . . ? C44 C42 N8 C41 176.0(4) . . . . ? C43 C42 N8 Co3 172.5(4) . . . . ? C44 C42 N8 Co3 -63.2(4) . . . . ? N8 Co3 N8 C41 -88(100) 2_767 . . . ? N7 Co3 N8 C41 165.4(3) 2_767 . . . ? N7 Co3 N8 C41 -14.6(3) . . . . ? O7 Co3 N8 C41 71.5(3) 2_767 . . . ? O7 Co3 N8 C41 -108.5(3) . . . . ? N8 Co3 N8 C42 145(100) 2_767 . . . ? N7 Co3 N8 C42 38.6(3) 2_767 . . . ? N7 Co3 N8 C42 -141.4(3) . . . . ? O7 Co3 N8 C42 -55.3(3) 2_767 . . . ? O7 Co3 N8 C42 124.7(3) . . . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.898 _refine_diff_density_min -0.566 _refine_diff_density_rms 0.074 #=========================END data_Compound-7 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C110 H184 N20 Ni4 O16, 2.5H2O' _chemical_formula_sum 'C110 H189 N20 Ni4 O18.50' _chemical_formula_weight 2322.65 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ni' 'Ni' 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.6170(6) _cell_length_b 14.3185(5) _cell_length_c 18.6289(7) _cell_angle_alpha 88.841(3) _cell_angle_beta 69.413(4) _cell_angle_gamma 79.690(3) _cell_volume 3341.7(2) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 3491 _cell_measurement_theta_min 3.1198 _cell_measurement_theta_max 29.1173 _exptl_crystal_description block _exptl_crystal_colour pink _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.154 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1249 _exptl_absorpt_coefficient_mu 0.618 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8658 _exptl_absorpt_correction_T_max 0.9076 _exptl_absorpt_process_details ; CrysAlis (Oxford Diffraction, 2006) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Diffraction Gemini R Ultra' _diffrn_measurement_method '\w scan' _diffrn_detector_area_resol_mean 10.0 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 20444 _diffrn_reflns_av_R_equivalents 0.0665 _diffrn_reflns_av_sigmaI/netI 0.1472 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 3.13 _diffrn_reflns_theta_max 25.35 _reflns_number_total 12011 _reflns_number_gt 4963 _reflns_threshold_expression >2\s(I) _computing_data_collection 'CrysAlisPro(1.171.35.21) (Agilent Tech., 2012)' _computing_cell_refinement 'CrysAlisPro(1.171.35.21) (Agilent Tech., 2012)' _computing_data_reduction 'CrysAlisPro(1.171.35.21) (Agilent Tech., 2012)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0100P)^2^+8.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 12011 _refine_ls_number_parameters 821 _refine_ls_number_restraints 125 _refine_ls_R_factor_all 0.2197 _refine_ls_R_factor_gt 0.1071 _refine_ls_wR_factor_ref 0.2268 _refine_ls_wR_factor_gt 0.1925 _refine_ls_goodness_of_fit_ref 1.202 _refine_ls_restrained_S_all 1.198 _refine_ls_shift/su_max 0.092 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni1 Ni -1.0000 1.0000 2.0000 0.0669(5) Uani 1 2 d SD . . Ni2 Ni -0.5000 0.5000 2.0000 0.0647(5) Uani 1 2 d S . . Ni3 Ni 0.20117(8) 0.19360(8) 1.47930(6) 0.0633(4) Uani 1 1 d D . . C1 C -0.6974(6) 0.9015(6) 1.8008(4) 0.061(2) Uani 1 1 d . . . C2 C -0.5956(6) 0.9183(5) 1.7628(4) 0.057(2) Uani 1 1 d . . . H2 H -0.5744 0.9697 1.7792 0.069 Uiso 1 1 calc R . . C3 C -0.5242(6) 0.8610(6) 1.7010(4) 0.056(2) Uani 1 1 d . . . C4 C -0.5602(7) 0.7891(6) 1.6745(5) 0.081(3) Uani 1 1 d . . . H4 H -0.5132 0.7514 1.6320 0.097 Uiso 1 1 calc R . . C5 C -0.6642(7) 0.7699(7) 1.7087(5) 0.095(4) Uani 1 1 d . . . C6 C -0.7305(7) 0.8284(6) 1.7724(5) 0.078(3) Uani 1 1 d . . . H6 H -0.7998 0.8182 1.7970 0.094 Uiso 1 1 calc R . . C7 C -0.7728(7) 0.9657(6) 1.8674(5) 0.072(3) Uani 1 1 d . . . C8 C -0.4142(7) 0.8761(7) 1.6610(5) 0.080(3) Uani 1 1 d . . . C9 C -0.7126(7) 0.7071(7) 1.6699(6) 0.090(3) Uani 1 1 d . . . H9A H -0.7732 0.6866 1.7082 0.108 Uiso 1 1 calc R . . H9B H -0.7379 0.7435 1.6333 0.108 Uiso 1 1 calc R . . C10 C -0.6272(9) 0.5575(8) 1.6865(7) 0.107(4) Uani 1 1 d . . . H10A H -0.6983 0.5446 1.7133 0.129 Uiso 1 1 calc R . . H10B H -0.6055 0.5872 1.7234 0.129 Uiso 1 1 calc R . . C11 C -0.5527(8) 0.4656(7) 1.6569(5) 0.092(3) Uani 1 1 d . . . H11A H -0.5828 0.4321 1.6274 0.110 Uiso 1 1 calc R . . H11B H -0.5528 0.4282 1.7009 0.110 Uiso 1 1 calc R . . C12 C -0.4366(7) 0.4656(6) 1.6076(5) 0.069(2) Uani 1 1 d . . . H12A H -0.4347 0.5134 1.5697 0.083 Uiso 1 1 calc R . . H12B H -0.4003 0.4840 1.6400 0.083 Uiso 1 1 calc R . . C13 C -0.297(2) 0.3570(18) 1.5020(15) 0.057(7) Uani 0.30 1 d PU . . C13' C -0.3960(10) 0.3563(9) 1.5015(7) 0.071(4) Uani 0.70 1 d P . . C14 C -0.3332(9) 0.4121(7) 1.4317(5) 0.093(3) Uani 1 1 d . . . C15 C -0.3719(8) 0.3011(6) 1.6221(5) 0.080(3) Uani 1 1 d . . . H15A H -0.3488 0.2404 1.5935 0.095 Uiso 1 1 calc R . . H15B H -0.4426 0.3015 1.6595 0.095 Uiso 1 1 calc R . . C16 C -0.0001(7) 0.2574(8) 1.6255(5) 0.086(3) Uani 1 1 d . . . C17 C -0.3078(7) 0.4063(7) 1.8543(5) 0.077(3) Uani 1 1 d . . . C18 C -0.2663(6) 0.3593(6) 1.7767(4) 0.059(2) Uani 1 1 d . . . C19 C -0.3362(6) 0.3490(6) 1.7374(5) 0.063(2) Uani 1 1 d . . . H19 H -0.4092 0.3699 1.7615 0.076 Uiso 1 1 calc R . . C20 C -0.2976(6) 0.3086(6) 1.6642(5) 0.057(2) Uani 1 1 d . . . C21 C -0.1895(7) 0.2771(5) 1.6284(5) 0.061(2) Uani 1 1 d . . . H21 H -0.1631 0.2485 1.5793 0.073 Uiso 1 1 calc R . . C22 C -0.1187(7) 0.2885(6) 1.6665(4) 0.062(2) Uani 1 1 d . . . C23 C -0.1589(6) 0.3296(6) 1.7379(4) 0.067(2) Uani 1 1 d . . . H23 H -0.1117 0.3382 1.7620 0.080 Uiso 1 1 calc R . . C25 C -1.2104(12) 1.1219(12) 1.8690(10) 0.196(8) Uani 1 1 d . . . H25A H -1.1888 1.1807 1.8503 0.294 Uiso 1 1 calc R . . H25B H -1.2684 1.1339 1.9174 0.294 Uiso 1 1 calc RD . . H25C H -1.2331 1.0934 1.8328 0.294 Uiso 1 1 calc R . . C26 C -1.0226(12) 1.0317(9) 1.8059(7) 0.158(6) Uani 1 1 d . . . H26A H -0.9969 1.0893 1.7880 0.238 Uiso 1 1 calc R . . H26B H -1.0457 1.0061 1.7686 0.238 Uiso 1 1 calc R . . H26C H -0.9662 0.9864 1.8133 0.238 Uiso 1 1 calc R . . C27 C -1.1136(11) 1.0526(10) 1.8799(7) 0.120(5) Uani 1 1 d . . . C28 C -1.1548(10) 0.9588(11) 1.9070(6) 0.126(5) Uani 1 1 d . . . H28A H -1.2146 0.9749 1.9548 0.151 Uiso 1 1 calc R . . H28B H -1.1838 0.9406 1.8698 0.151 Uiso 1 1 calc R . . C29 C -1.0863(10) 0.8717(9) 1.9199(7) 0.105(4) Uani 1 1 d D . . C30 C -1.120(4) 0.771(3) 1.924(2) 0.081(13) Uani 0.35 1 d PU . . C30A C -1.079(18) 0.765(6) 1.892(13) 0.31(3) Uani 0.15 1 d PDU . . C30B C -1.161(2) 0.8019(17) 1.9202(17) 0.093(9) Uani 0.50 1 d P . . C31 C -0.9945(11) 0.8017(8) 2.0072(8) 0.130(5) Uani 1 1 d D . . H31A H -1.0303 0.7475 2.0162 0.156 Uiso 1 1 calc R . . H31B H -0.9292 0.7855 1.9630 0.156 Uiso 1 1 calc R . . C32 C -0.9681(10) 0.8217(8) 2.0750(7) 0.110(4) Uani 1 1 d . . . H32A H -0.9179 0.7688 2.0826 0.132 Uiso 1 1 calc RD . . H32B H -1.0319 0.8320 2.1206 0.132 Uiso 1 1 calc R . . C33 C -0.5080(12) 0.7993(9) 1.9248(9) 0.163(6) Uani 1 1 d . . . H33A H -0.4383 0.8100 1.9197 0.245 Uiso 1 1 calc R . . H33B H -0.5576 0.8216 1.9749 0.245 Uiso 1 1 calc R . . H33C H -0.5305 0.8329 1.8865 0.245 Uiso 1 1 calc R . . C34 C -0.4261(9) 0.6496(10) 1.8341(6) 0.139(5) Uani 1 1 d . . . H34A H -0.3558 0.6587 1.8290 0.208 Uiso 1 1 calc R . . H34B H -0.4477 0.6836 1.7956 0.208 Uiso 1 1 calc R . . H34C H -0.4256 0.5831 1.8278 0.208 Uiso 1 1 calc R . . C35 C -0.5040(11) 0.6867(9) 1.9133(7) 0.112(4) Uani 1 1 d . . . C36 C -0.6176(9) 0.6761(8) 1.9226(6) 0.099(3) Uani 1 1 d . . . H36A H -0.6630 0.6963 1.9750 0.118 Uiso 1 1 calc R . . H36B H -0.6412 0.7205 1.8894 0.118 Uiso 1 1 calc R . . C37 C -0.6371(7) 0.5837(8) 1.9070(5) 0.087(3) Uani 1 1 d . . . H37 H -0.5825 0.5574 1.8582 0.104 Uiso 1 1 calc R . . C38 C -0.7497(8) 0.5948(8) 1.8984(6) 0.115(4) Uani 1 1 d . . . H38A H -0.7621 0.5335 1.8879 0.172 Uiso 1 1 calc R . . H38B H -0.7513 0.6352 1.8570 0.172 Uiso 1 1 calc R . . H38C H -0.8041 0.6225 1.9452 0.172 Uiso 1 1 calc R . . C39 C -0.6465(8) 0.4183(7) 1.9554(6) 0.088(3) Uani 1 1 d D . . H39A H -0.5940 0.3906 1.9070 0.105 Uiso 1 1 calc R . . H39B H -0.7171 0.4205 1.9534 0.105 Uiso 1 1 calc R . . C40 C -0.6337(8) 0.3584(8) 2.0221(6) 0.098(3) Uani 1 1 d D . . H40A H -0.6893 0.3835 2.0700 0.117 Uiso 1 1 calc R . . H40B H -0.6390 0.2931 2.0136 0.117 Uiso 1 1 calc R . . C41 C 0.153(2) 0.4902(19) 1.3886(16) 0.118(8) Uani 0.50 1 d PU . . C41' C 0.191(2) 0.4523(18) 1.3475(15) 0.114(8) Uani 0.50 1 d PU . . C42 C 0.1403(10) 0.3727(9) 1.4028(8) 0.112(4) Uani 1 1 d D A . C43 C 0.1365(10) 0.3065(11) 1.3419(6) 0.125(5) Uani 1 1 d . . . H43A H 0.1030 0.3451 1.3104 0.150 Uiso 1 1 calc R . . H43B H 0.2097 0.2827 1.3093 0.150 Uiso 1 1 calc R . . C44 C 0.0857(10) 0.2276(9) 1.3615(7) 0.097(3) Uani 1 1 d U A . C45 C -0.0229(13) 0.2576(11) 1.4074(9) 0.182(6) Uani 1 1 d U . . H45A H -0.0567 0.2032 1.4211 0.273 Uiso 1 1 calc R . . H45B H -0.0580 0.2991 1.3791 0.273 Uiso 1 1 calc R . . H45C H -0.0279 0.2909 1.4531 0.273 Uiso 1 1 calc R . . C46 C 0.083(2) 0.1867(16) 1.2880(10) 0.300(14) Uani 1 1 d . . . H46A H 0.0444 0.1350 1.2996 0.450 Uiso 1 1 calc R . . H46B H 0.1545 0.1639 1.2537 0.450 Uiso 1 1 calc R . . H46C H 0.0481 0.2351 1.2641 0.450 Uiso 1 1 calc R . . C47 C 0.1045(10) 0.0638(10) 1.4242(7) 0.118(4) Uani 1 1 d D A . H47A H 0.0333 0.0799 1.4624 0.141 Uiso 1 1 calc R . . H47B H 0.1004 0.0283 1.3819 0.141 Uiso 1 1 calc R . . C48 C 0.1732(9) 0.0072(8) 1.4570(7) 0.103(4) Uani 1 1 d D . . H48A H 0.1424 -0.0475 1.4789 0.123 Uiso 1 1 calc R . . H48B H 0.2412 -0.0159 1.4168 0.123 Uiso 1 1 calc R . . C49 C 0.2337(17) -0.0802(12) 1.5938(14) 0.167(11) Uani 0.71(2) 1 d P A 1 C49' C 0.379(2) -0.0391(19) 1.4993(16) 0.064(11) Uani 0.29(2) 1 d PU A 2 C50 C 0.2694(11) 0.0098(7) 1.5524(8) 0.112(4) Uani 1 1 d . . . C51 C 0.2739(10) 0.0738(10) 1.6126(9) 0.112(4) Uani 1 1 d . A . C52 C 0.3285(8) 0.1601(9) 1.5880(7) 0.105(4) Uani 1 1 d DU . . C53 C 0.334(3) 0.197(4) 1.6778(13) 0.076(16) Uani 0.25 1 d PDU A . C53A C 0.319(3) 0.219(4) 1.667(2) 0.099(7) Uani 0.25 1 d PDU A . C53' C 0.317(5) 0.042(5) 1.625(4) 0.36(3) Uani 0.50 1 d PDU A . C54 C 0.4394(14) 0.1384(14) 1.5480(11) 0.125(7) Uani 0.60 1 d PD A . C54' C 0.374(3) 0.199(3) 1.637(3) 0.16(2) Uani 0.40 1 d P A . C55 C 0.2939(7) 0.3186(7) 1.5379(6) 0.081(3) Uani 1 1 d D . . H55A H 0.3640 0.3058 1.4981 0.097 Uiso 1 1 calc R A . H55B H 0.2996 0.3507 1.5813 0.097 Uiso 1 1 calc R . . C56 C 0.2174(10) 0.3817(8) 1.5083(7) 0.111(4) Uani 1 1 d . A . H56A H 0.2430 0.4403 1.4912 0.133 Uiso 1 1 calc R . . H56B H 0.1478 0.3974 1.5484 0.133 Uiso 1 1 calc R . . N1 N -0.6314(7) 0.6217(5) 1.6293(5) 0.090(3) Uani 1 1 d . . . N2 N -0.3791(6) 0.3766(5) 1.5686(4) 0.075(2) Uani 1 1 d . . . O1 O -0.8633(5) 0.9416(4) 1.9015(3) 0.083(2) Uani 1 1 d . . . O2 O -0.7437(5) 1.0330(5) 1.8860(4) 0.133(3) Uani 1 1 d . . . O3 O -0.3752(6) 0.9307(7) 1.6935(5) 0.151(4) Uani 1 1 d . . . O4 O -0.3610(4) 0.8346(4) 1.5993(3) 0.0818(19) Uani 1 1 d . . . O5 O -0.4043(4) 0.4347(4) 1.8877(3) 0.0785(18) Uani 1 1 d . . . O4W O -0.427(2) 1.1080(17) 1.7577(14) 0.088(7) Uani 0.25 1 d PU . . O6 O -0.2395(7) 0.4112(5) 1.8855(5) 0.118(2) Uani 1 1 d U . . O5W O 0.202(2) 0.3580(16) 1.8452(14) 0.090(8) Uani 0.25 1 d P . . O7 O 0.0372(4) 0.2299(4) 1.5585(3) 0.0710(16) Uani 1 1 d . . . O8 O 0.0533(7) 0.2632(6) 1.6674(5) 0.131(3) Uani 1 1 d U . . O1W O -0.6563(16) 1.1980(14) 1.8566(11) 0.062(6) Uani 0.25 1 d PU . . O2W O 0.1056(19) 0.4135(16) 1.7348(13) 0.082(7) Uani 0.25 1 d PU . . O3W O -0.069(2) 0.5053(17) 1.8683(14) 0.092(8) Uani 0.25 1 d PU . . N3 N -1.0642(7) 0.8844(6) 1.9902(5) 0.091(3) Uani 1 1 d . . . H3D H -1.105(6) 0.900(5) 2.025(7) 0.136 Uiso 1 1 d D . . N4 N -0.9196(7) 0.9094(7) 2.0595(5) 0.107(3) Uani 1 1 d D . . H4D H -0.8494(10) 0.8794(12) 2.0423(15) 0.160 Uiso 1 1 d D . . N5 N -0.6312(5) 0.5139(6) 1.9689(4) 0.077(2) Uani 1 1 d D . . H5D H -0.694(4) 0.532(3) 2.007(4) 0.116 Uiso 1 1 d D . . N6 N -0.5244(6) 0.3628(6) 2.0253(5) 0.084(2) Uani 1 1 d D . . H6D H -0.4907(13) 0.326(6) 1.982(3) 0.126 Uiso 1 1 d D . . N7 N 0.2102(7) 0.3282(6) 1.4422(5) 0.094(3) Uani 1 1 d D . . H7D H 0.2719(13) 0.324(7) 1.402(2) 0.141 Uiso 1 1 d D . . N8 N 0.1452(6) 0.1523(7) 1.3961(5) 0.099(3) Uani 1 1 d D . . H8D H 0.2142(11) 0.124(2) 1.378(6) 0.149 Uiso 1 1 d D . . N9 N 0.1915(6) 0.0581(6) 1.5161(5) 0.089(3) Uani 1 1 d D A . H9D H 0.1246(15) 0.0667(10) 1.5504(9) 0.133 Uiso 1 1 d D . . N10 N 0.2591(5) 0.2325(5) 1.5607(4) 0.073(2) Uani 1 1 d D A . H10D H 0.191(2) 0.2550(15) 1.590(4) 0.109 Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.0514(10) 0.0624(10) 0.0595(10) -0.0247(7) 0.0154(8) -0.0109(7) Ni2 0.0432(9) 0.0913(12) 0.0467(9) -0.0129(8) -0.0036(7) -0.0030(8) Ni3 0.0415(6) 0.0750(8) 0.0557(7) -0.0127(5) 0.0049(5) -0.0097(5) C1 0.044(5) 0.070(6) 0.046(5) -0.013(4) 0.016(4) -0.013(4) C2 0.059(6) 0.057(5) 0.046(5) -0.009(4) -0.004(4) -0.014(4) C3 0.033(4) 0.068(5) 0.049(5) -0.013(4) 0.007(4) -0.006(4) C4 0.066(6) 0.070(6) 0.064(6) -0.030(5) 0.030(5) -0.010(5) C5 0.070(7) 0.090(7) 0.085(7) -0.048(5) 0.030(5) -0.028(5) C6 0.053(6) 0.084(6) 0.068(6) -0.037(5) 0.023(4) -0.027(5) C7 0.062(6) 0.066(6) 0.060(6) -0.025(4) 0.014(5) -0.010(5) C8 0.048(6) 0.086(7) 0.074(7) -0.022(5) 0.017(5) -0.004(5) C9 0.063(6) 0.091(7) 0.097(7) -0.039(6) 0.000(5) -0.017(5) C10 0.101(9) 0.116(9) 0.094(9) -0.033(7) -0.038(7) 0.020(7) C11 0.085(8) 0.118(9) 0.067(7) -0.012(6) -0.023(6) -0.010(6) C12 0.060(6) 0.070(6) 0.079(6) -0.001(5) -0.028(5) -0.009(5) C13 0.057(7) 0.057(7) 0.057(7) 0.0026(11) -0.020(3) -0.0106(16) C13' 0.066(9) 0.097(10) 0.053(8) -0.008(7) -0.021(7) -0.021(7) C14 0.130(9) 0.104(8) 0.041(5) -0.015(5) -0.024(6) -0.023(7) C15 0.091(8) 0.065(6) 0.075(7) -0.011(5) -0.025(6) -0.001(5) C16 0.045(6) 0.154(10) 0.045(6) -0.010(6) -0.008(5) 0.001(6) C17 0.044(6) 0.135(8) 0.047(5) -0.021(5) -0.014(5) -0.004(5) C18 0.040(5) 0.083(6) 0.045(5) -0.010(4) -0.009(4) 0.001(4) C19 0.041(5) 0.075(6) 0.055(5) -0.003(4) 0.001(4) 0.003(4) C20 0.047(5) 0.070(5) 0.054(5) 0.000(4) -0.021(4) -0.003(4) C21 0.057(6) 0.056(5) 0.047(5) 0.001(4) -0.002(4) 0.009(4) C22 0.046(5) 0.079(6) 0.039(5) 0.003(4) 0.002(4) 0.011(4) C23 0.041(5) 0.105(7) 0.043(5) -0.001(4) -0.009(4) 0.005(5) C25 0.142(15) 0.216(18) 0.23(2) 0.004(14) -0.097(14) 0.021(13) C26 0.209(16) 0.141(12) 0.090(10) -0.016(8) -0.004(10) -0.041(11) C27 0.123(11) 0.145(12) 0.069(8) -0.028(7) 0.007(7) -0.048(9) C28 0.110(11) 0.174(14) 0.079(8) -0.045(9) -0.001(7) -0.046(11) C29 0.095(9) 0.097(9) 0.099(9) -0.048(7) 0.007(7) -0.037(7) C30 0.081(13) 0.081(13) 0.081(13) 0.0037(12) -0.029(5) -0.015(3) C30A 0.31(3) 0.31(3) 0.31(3) 0.0143(18) -0.109(11) -0.056(6) C30B 0.11(2) 0.065(16) 0.13(2) -0.005(14) -0.069(19) -0.025(15) C31 0.121(11) 0.079(9) 0.138(12) -0.029(8) 0.029(9) -0.036(8) C32 0.115(10) 0.077(8) 0.128(11) -0.001(7) -0.024(8) -0.030(7) C33 0.220(17) 0.099(10) 0.208(16) 0.038(10) -0.103(14) -0.071(10) C34 0.095(9) 0.234(15) 0.065(8) 0.034(8) -0.005(7) -0.024(9) C35 0.110(11) 0.128(11) 0.094(9) 0.021(7) -0.032(8) -0.028(8) C36 0.110(10) 0.092(8) 0.096(8) 0.000(6) -0.043(7) -0.010(7) C37 0.058(7) 0.130(9) 0.057(6) -0.010(6) -0.014(5) 0.008(6) C38 0.058(7) 0.166(11) 0.106(9) -0.021(7) -0.026(6) 0.015(7) C39 0.081(8) 0.096(8) 0.090(8) -0.009(6) -0.026(6) -0.034(6) C40 0.077(8) 0.121(9) 0.094(8) -0.011(7) -0.021(6) -0.035(6) C41 0.118(8) 0.117(8) 0.118(8) 0.0058(11) -0.042(3) -0.0215(18) C41' 0.114(8) 0.114(8) 0.114(8) 0.0054(11) -0.040(3) -0.0209(18) C42 0.100(10) 0.106(9) 0.119(11) 0.037(8) -0.024(8) -0.027(7) C43 0.105(10) 0.186(14) 0.067(8) 0.012(8) -0.019(7) -0.005(9) C44 0.097(3) 0.098(3) 0.097(3) 0.0040(10) -0.0347(15) -0.0175(12) C45 0.182(6) 0.182(6) 0.182(6) 0.0086(11) -0.064(2) -0.0336(15) C46 0.44(4) 0.33(3) 0.181(19) -0.078(18) -0.22(2) 0.01(2) C47 0.079(9) 0.154(12) 0.122(10) -0.041(9) -0.023(8) -0.045(9) C48 0.074(8) 0.098(9) 0.118(10) -0.041(7) 0.001(7) -0.036(7) C49 0.17(2) 0.074(12) 0.31(3) 0.075(14) -0.15(2) -0.042(12) C49' 0.064(11) 0.064(11) 0.064(11) 0.0029(11) -0.023(4) -0.012(2) C50 0.111(10) 0.057(7) 0.147(11) -0.002(7) -0.025(9) -0.008(6) C51 0.098(9) 0.103(10) 0.145(12) 0.018(8) -0.057(9) -0.016(8) C52 0.046(6) 0.113(9) 0.154(11) -0.023(8) -0.045(7) 0.013(6) C53 0.076(16) 0.076(16) 0.076(16) 0.0036(13) -0.027(6) -0.014(3) C53A 0.039(11) 0.118(14) 0.149(15) -0.023(12) -0.059(11) 0.015(11) C53' 0.36(3) 0.36(3) 0.36(3) 0.0165(16) -0.126(9) -0.065(5) C54 0.063(13) 0.127(16) 0.17(2) -0.014(14) -0.034(13) -0.001(11) C54' 0.07(2) 0.18(3) 0.25(5) -0.13(4) -0.11(3) 0.05(2) C55 0.052(6) 0.077(7) 0.107(8) -0.010(6) -0.016(6) -0.018(5) C56 0.100(9) 0.080(8) 0.134(11) -0.018(7) -0.011(8) -0.029(7) N1 0.105(7) 0.062(5) 0.080(6) -0.025(4) -0.006(5) -0.010(4) N2 0.080(6) 0.066(5) 0.060(5) -0.007(4) -0.012(4) 0.007(4) O1 0.059(4) 0.077(4) 0.074(4) -0.031(3) 0.031(3) -0.021(3) O2 0.089(5) 0.118(6) 0.134(6) -0.085(5) 0.055(4) -0.057(4) O3 0.069(5) 0.212(9) 0.134(7) -0.103(6) 0.035(4) -0.060(5) O4 0.043(3) 0.106(5) 0.068(4) -0.029(3) 0.019(3) -0.018(3) O5 0.041(4) 0.114(5) 0.056(4) -0.020(3) 0.003(3) 0.007(3) O4W 0.088(7) 0.088(7) 0.088(7) 0.0038(11) -0.031(3) -0.0165(17) O6 0.117(3) 0.120(3) 0.117(3) 0.0039(10) -0.0417(13) -0.0212(11) O5W 0.12(2) 0.075(16) 0.11(2) -0.029(14) -0.085(18) -0.009(14) O7 0.045(3) 0.109(5) 0.040(3) -0.005(3) 0.000(3) 0.003(3) O8 0.130(3) 0.133(3) 0.130(3) 0.0047(10) -0.0465(14) -0.0230(11) O1W 0.063(6) 0.062(6) 0.063(6) 0.0027(11) -0.022(2) -0.0120(14) O2W 0.082(7) 0.082(7) 0.082(7) 0.0033(11) -0.029(3) -0.0152(16) O3W 0.092(8) 0.093(8) 0.093(8) 0.0037(11) -0.033(3) -0.0173(17) N3 0.070(6) 0.071(6) 0.093(7) -0.035(5) 0.026(5) -0.025(5) N4 0.074(6) 0.125(8) 0.103(7) -0.006(6) -0.009(5) -0.017(5) N5 0.049(5) 0.115(7) 0.056(5) -0.016(4) -0.009(4) 0.000(4) N6 0.066(6) 0.108(7) 0.066(6) -0.001(5) -0.013(4) -0.009(5) N7 0.079(6) 0.085(6) 0.092(7) 0.010(5) 0.002(5) -0.017(5) N8 0.061(6) 0.135(8) 0.078(6) -0.036(5) 0.015(5) -0.035(6) N9 0.052(5) 0.075(5) 0.119(7) -0.015(5) -0.002(5) -0.016(4) N10 0.043(5) 0.079(5) 0.086(6) -0.005(4) -0.003(4) -0.024(4) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 N3 2.044(8) 2_379 ? Ni1 N3 2.044(8) . ? Ni1 N4 2.096(10) . ? Ni1 N4 2.096(10) 2_379 ? Ni1 O1 2.152(5) . ? Ni1 O1 2.152(5) 2_379 ? Ni2 N5 2.040(8) 2_469 ? Ni2 N5 2.040(8) . ? Ni2 N6 2.068(9) 2_469 ? Ni2 N6 2.068(9) . ? Ni2 O5 2.162(5) . ? Ni2 O5 2.162(5) 2_469 ? Ni3 N10 2.066(8) . ? Ni3 N7 2.044(8) . ? Ni3 N9 2.056(8) . ? Ni3 N8 2.089(9) . ? Ni3 O4 2.124(5) 2_568 ? Ni3 O7 2.175(5) . ? C1 C2 1.380(10) . ? C1 C6 1.391(10) . ? C1 C7 1.500(10) . ? C2 C3 1.381(9) . ? C2 H2 0.9300 . ? C3 C4 1.384(11) . ? C3 C8 1.474(11) . ? C4 C5 1.408(11) . ? C4 H4 0.9300 . ? C5 C6 1.393(10) . ? C5 C9 1.529(12) . ? C6 H6 0.9300 . ? C7 O1 1.278(9) . ? C7 O2 1.206(9) . ? C8 O4 1.219(9) . ? C8 O3 1.286(11) . ? C9 N1 1.503(11) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 N1 1.403(12) . ? C10 C11 1.491(13) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 C12 1.524(12) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 N2 1.430(10) . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C13 N2 1.34(3) . ? C13 C13' 1.36(3) . ? C13 C14 1.69(3) . ? C13' N2 1.394(13) . ? C13' C14 1.575(15) . ? C14 N1 1.498(12) 2_468 ? C15 N2 1.469(10) . ? C15 C20 1.499(11) . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 O7 1.213(9) . ? C16 O8 1.252(11) . ? C16 C22 1.511(11) . ? C17 O5 1.234(9) . ? C17 O6 1.269(10) . ? C17 C18 1.481(10) . ? C18 C23 1.373(10) . ? C18 C19 1.417(11) . ? C19 C20 1.376(10) . ? C19 H19 0.9300 . ? C20 C21 1.378(10) . ? C21 C22 1.415(11) . ? C21 H21 0.9300 . ? C22 C23 1.348(10) . ? C23 H23 0.9300 . ? C25 C27 1.573(17) . ? C25 H25A 0.9600 . ? C25 H25B 0.9600 . ? C25 H25C 0.9600 . ? C26 C27 1.486(15) . ? C26 H26A 0.9600 . ? C26 H26B 0.9600 . ? C26 H26C 0.9600 . ? C27 N4 1.500(14) 2_379 ? C27 C28 1.553(16) . ? C28 C29 1.488(16) . ? C28 H28A 0.9700 . ? C28 H28B 0.9700 . ? C29 N3 1.465(15) . ? C29 C30B 1.55(3) . ? C29 C30A 1.602(10) . ? C29 C30 1.58(4) . ? C30 C30B 0.68(4) . ? C30 C30A 0.7(2) . ? C30A C30B 1.1(2) . ? C31 C32 1.476(15) . ? C31 N3 1.481(15) . ? C31 H31A 0.9700 . ? C31 H31B 0.9700 . ? C32 N4 1.498(12) . ? C32 H32A 0.9700 . ? C32 H32B 0.9700 . ? C33 C35 1.619(16) . ? C33 H33A 0.9600 . ? C33 H33B 0.9600 . ? C33 H33C 0.9600 . ? C34 C35 1.520(15) . ? C34 H34A 0.9600 . ? C34 H34B 0.9600 . ? C34 H34C 0.9600 . ? C35 N6 1.463(13) 2_469 ? C35 C36 1.529(15) . ? C36 C37 1.450(13) . ? C36 H36A 0.9700 . ? C36 H36B 0.9700 . ? C37 N5 1.524(12) . ? C37 C38 1.576(12) . ? C37 H37 0.9800 . ? C38 H38A 0.9600 . ? C38 H38B 0.9600 . ? C38 H38C 0.9600 . ? C39 N5 1.461(11) . ? C39 C40 1.537(13) . ? C39 H39A 0.9700 . ? C39 H39B 0.9700 . ? C40 N6 1.523(12) . ? C40 H40A 0.9700 . ? C40 H40B 0.9700 . ? C41 C41' 0.89(3) . ? C41 C42 1.73(3) . ? C41' C42 1.60(3) . ? C42 N7 1.452(14) . ? C42 C43 1.513(16) . ? C43 C44 1.404(14) . ? C43 H43A 0.9700 . ? C43 H43B 0.9700 . ? C44 C45 1.415(17) . ? C44 C46 1.516(16) . ? C44 N8 1.504(14) . ? C45 H45A 0.9600 . ? C45 H45B 0.9600 . ? C45 H45C 0.9600 . ? C46 H46A 0.9600 . ? C46 H46B 0.9600 . ? C46 H46C 0.9600 . ? C47 C48 1.420(14) . ? C47 N8 1.485(14) . ? C47 H47A 0.9700 . ? C47 H47B 0.9700 . ? C48 N9 1.446(13) . ? C48 H48A 0.9700 . ? C48 H48B 0.9700 . ? C49 C50 1.553(19) . ? C49' C50 1.52(3) . ? C50 N9 1.511(14) . ? C50 C51 1.487(19) . ? C50 C53' 1.79(8) . ? C51 C53' 0.77(8) . ? C51 C52 1.534(16) . ? C52 C54' 1.44(3) . ? C52 C54 1.408(18) . ? C52 N10 1.480(13) . ? C52 C53A 1.67(4) . ? C52 C53 1.794(10) . ? C52 C53' 1.82(5) . ? C53 C54' 0.77(6) . ? C53A C54' 0.77(4) . ? C54 C54' 1.74(4) . ? C55 N10 1.403(10) . ? C55 C56 1.501(13) . ? C55 H55A 0.9700 . ? C55 H55B 0.9700 . ? C56 N7 1.503(13) . ? C56 H56A 0.9700 . ? C56 H56B 0.9700 . ? N1 C14 1.498(12) 2_468 ? O4 Ni3 2.124(5) 2_568 ? N3 H3D 0.70(9) . ? N4 C27 1.500(14) 2_379 ? N4 H4D 0.919(10) . ? N5 H5D 0.898(10) . ? N6 C35 1.463(13) 2_469 ? N6 H6D 0.902(10) . ? N7 H7D 0.900(10) . ? N8 H8D 0.901(10) . ? N9 H9D 0.899(10) . ? N10 H10D 0.903(10) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N3 Ni1 N3 180.0(5) 2_379 . ? N3 Ni1 N4 95.7(4) 2_379 . ? N3 Ni1 N4 84.3(4) . . ? N3 Ni1 N4 84.3(4) 2_379 2_379 ? N3 Ni1 N4 95.7(4) . 2_379 ? N4 Ni1 N4 180.0(4) . 2_379 ? N3 Ni1 O1 92.3(2) 2_379 . ? N3 Ni1 O1 87.7(2) . . ? N4 Ni1 O1 83.1(3) . . ? N4 Ni1 O1 96.9(3) 2_379 . ? N3 Ni1 O1 87.7(2) 2_379 2_379 ? N3 Ni1 O1 92.3(2) . 2_379 ? N4 Ni1 O1 96.9(3) . 2_379 ? N4 Ni1 O1 83.1(3) 2_379 2_379 ? O1 Ni1 O1 180.000(2) . 2_379 ? N5 Ni2 N5 180.000(2) 2_469 . ? N5 Ni2 N6 85.3(3) 2_469 2_469 ? N5 Ni2 N6 94.7(3) . 2_469 ? N5 Ni2 N6 94.7(3) 2_469 . ? N5 Ni2 N6 85.3(3) . . ? N6 Ni2 N6 180.000(2) 2_469 . ? N5 Ni2 O5 91.2(2) 2_469 . ? N5 Ni2 O5 88.8(2) . . ? N6 Ni2 O5 97.1(3) 2_469 . ? N6 Ni2 O5 82.9(3) . . ? N5 Ni2 O5 88.8(2) 2_469 2_469 ? N5 Ni2 O5 91.2(2) . 2_469 ? N6 Ni2 O5 82.9(3) 2_469 2_469 ? N6 Ni2 O5 97.1(3) . 2_469 ? O5 Ni2 O5 180.000(2) . 2_469 ? N10 Ni3 N7 85.5(4) . . ? N10 Ni3 N9 94.9(4) . . ? N7 Ni3 N9 179.6(4) . . ? N10 Ni3 N8 178.9(3) . . ? N7 Ni3 N8 95.0(4) . . ? N9 Ni3 N8 84.6(4) . . ? N10 Ni3 O4 88.0(2) . 2_568 ? N7 Ni3 O4 82.1(3) . 2_568 ? N9 Ni3 O4 98.0(3) . 2_568 ? N8 Ni3 O4 91.1(3) . 2_568 ? N10 Ni3 O7 91.7(2) . . ? N7 Ni3 O7 95.1(3) . . ? N9 Ni3 O7 84.8(3) . . ? N8 Ni3 O7 89.3(3) . . ? O4 Ni3 O7 177.1(2) 2_568 . ? C2 C1 C6 118.4(7) . . ? C2 C1 C7 120.3(7) . . ? C6 C1 C7 121.1(7) . . ? C3 C2 C1 121.9(7) . . ? C3 C2 H2 119.1 . . ? C1 C2 H2 119.1 . . ? C2 C3 C4 117.8(7) . . ? C2 C3 C8 122.7(8) . . ? C4 C3 C8 119.4(7) . . ? C3 C4 C5 123.4(7) . . ? C3 C4 H4 118.3 . . ? C5 C4 H4 118.3 . . ? C6 C5 C4 115.6(8) . . ? C6 C5 C9 119.4(8) . . ? C4 C5 C9 123.4(7) . . ? C5 C6 C1 122.8(8) . . ? C5 C6 H6 118.6 . . ? C1 C6 H6 118.6 . . ? O1 C7 O2 125.2(7) . . ? O1 C7 C1 115.8(8) . . ? O2 C7 C1 118.9(8) . . ? O4 C8 O3 121.3(8) . . ? O4 C8 C3 119.7(9) . . ? O3 C8 C3 118.9(8) . . ? N1 C9 C5 110.6(8) . . ? N1 C9 H9A 109.5 . . ? C5 C9 H9A 109.5 . . ? N1 C9 H9B 109.5 . . ? C5 C9 H9B 109.5 . . ? H9A C9 H9B 108.1 . . ? N1 C10 C11 114.0(9) . . ? N1 C10 H10A 108.8 . . ? C11 C10 H10A 108.8 . . ? N1 C10 H10B 108.8 . . ? C11 C10 H10B 108.8 . . ? H10A C10 H10B 107.6 . . ? C10 C11 C12 119.8(9) . . ? C10 C11 H11A 107.4 . . ? C12 C11 H11A 107.4 . . ? C10 C11 H11B 107.4 . . ? C12 C11 H11B 107.4 . . ? H11A C11 H11B 106.9 . . ? N2 C12 C11 114.7(7) . . ? N2 C12 H12A 108.6 . . ? C11 C12 H12A 108.6 . . ? N2 C12 H12B 108.6 . . ? C11 C12 H12B 108.6 . . ? H12A C12 H12B 107.6 . . ? N2 C13 C13' 62.2(14) . . ? N2 C13 C14 108.4(18) . . ? C13' C13 C14 61.1(13) . . ? C13 C13' N2 58.4(12) . . ? C13 C13' C14 70.0(13) . . ? N2 C13' C14 112.4(9) . . ? N1 C14 C13' 100.0(8) 2_468 . ? N1 C14 C13 133.2(12) 2_468 . ? C13' C14 C13 48.9(10) . . ? N2 C15 C20 115.2(8) . . ? N2 C15 H15A 108.5 . . ? C20 C15 H15A 108.5 . . ? N2 C15 H15B 108.5 . . ? C20 C15 H15B 108.5 . . ? H15A C15 H15B 107.5 . . ? O7 C16 O8 124.9(9) . . ? O7 C16 C22 121.9(9) . . ? O8 C16 C22 113.3(9) . . ? O5 C17 O6 122.4(8) . . ? O5 C17 C18 121.2(8) . . ? O6 C17 C18 116.3(8) . . ? C23 C18 C19 117.3(7) . . ? C23 C18 C17 121.9(8) . . ? C19 C18 C17 120.7(7) . . ? C20 C19 C18 120.9(7) . . ? C20 C19 H19 119.5 . . ? C18 C19 H19 119.5 . . ? C21 C20 C19 119.7(8) . . ? C21 C20 C15 119.7(8) . . ? C19 C20 C15 120.5(8) . . ? C20 C21 C22 119.9(7) . . ? C20 C21 H21 120.1 . . ? C22 C21 H21 120.1 . . ? C23 C22 C21 119.0(8) . . ? C23 C22 C16 121.6(9) . . ? C21 C22 C16 119.3(7) . . ? C22 C23 C18 123.1(8) . . ? C22 C23 H23 118.4 . . ? C18 C23 H23 118.4 . . ? C27 C25 H25A 109.5 . . ? C27 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C27 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C27 C26 H26A 109.5 . . ? C27 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C27 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? N4 C27 C26 111.3(11) 2_379 . ? N4 C27 C28 108.6(10) 2_379 . ? C26 C27 C28 108.5(10) . . ? N4 C27 C25 111.6(11) 2_379 . ? C26 C27 C25 111.0(13) . . ? C28 C27 C25 105.6(12) . . ? C29 C28 C27 123.4(12) . . ? C29 C28 H28A 106.5 . . ? C27 C28 H28A 106.5 . . ? C29 C28 H28B 106.5 . . ? C27 C28 H28B 106.5 . . ? H28A C28 H28B 106.5 . . ? C28 C29 N3 110.3(9) . . ? C28 C29 C30B 96.6(15) . . ? N3 C29 C30B 118.0(14) . . ? C28 C29 C30A 127(9) . . ? N3 C29 C30A 117(9) . . ? C30B C29 C30A 41(8) . . ? C28 C29 C30 121(2) . . ? N3 C29 C30 106.0(18) . . ? C30B C29 C30 24.9(17) . . ? C30A C29 C30 24(8) . . ? C30B C30 C30A 111(10) . . ? C30B C30 C29 75(5) . . ? C30A C30 C29 80(6) . . ? C30 C30A C30B 35(10) . . ? C30 C30A C29 76(5) . . ? C30B C30A C29 67(4) . . ? C30 C30B C30A 34(10) . . ? C30 C30B C29 80(5) . . ? C30A C30B C29 72(5) . . ? C32 C31 N3 111.6(10) . . ? C32 C31 H31A 109.3 . . ? N3 C31 H31A 109.3 . . ? C32 C31 H31B 109.3 . . ? N3 C31 H31B 109.3 . . ? H31A C31 H31B 108.0 . . ? C31 C32 N4 106.7(10) . . ? C31 C32 H32A 110.4 . . ? N4 C32 H32A 110.4 . . ? C31 C32 H32B 110.4 . . ? N4 C32 H32B 110.4 . . ? H32A C32 H32B 108.6 . . ? C35 C33 H33A 109.5 . . ? C35 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C35 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C35 C34 H34A 109.5 . . ? C35 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C35 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? N6 C35 C36 108.5(9) 2_469 . ? N6 C35 C34 112.1(10) 2_469 . ? C36 C35 C34 110.9(10) . . ? N6 C35 C33 108.7(10) 2_469 . ? C36 C35 C33 105.9(11) . . ? C34 C35 C33 110.5(10) . . ? C37 C36 C35 118.9(10) . . ? C37 C36 H36A 107.6 . . ? C35 C36 H36A 107.6 . . ? C37 C36 H36B 107.6 . . ? C35 C36 H36B 107.6 . . ? H36A C36 H36B 107.0 . . ? C36 C37 N5 112.7(8) . . ? C36 C37 C38 109.8(9) . . ? N5 C37 C38 109.7(8) . . ? C36 C37 H37 108.2 . . ? N5 C37 H37 108.2 . . ? C38 C37 H37 108.2 . . ? C37 C38 H38A 109.5 . . ? C37 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C37 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? N5 C39 C40 107.6(8) . . ? N5 C39 H39A 110.2 . . ? C40 C39 H39A 110.2 . . ? N5 C39 H39B 110.2 . . ? C40 C39 H39B 110.2 . . ? H39A C39 H39B 108.5 . . ? N6 C40 C39 107.5(8) . . ? N6 C40 H40A 110.2 . . ? C39 C40 H40A 110.2 . . ? N6 C40 H40B 110.2 . . ? C39 C40 H40B 110.2 . . ? H40A C40 H40B 108.5 . . ? C41' C41 C42 67(3) . . ? C41 C41' C42 82(3) . . ? N7 C42 C43 112.1(11) . . ? N7 C42 C41' 111.3(13) . . ? C43 C42 C41' 98.0(14) . . ? N7 C42 C41 109.8(13) . . ? C43 C42 C41 123.6(14) . . ? C41' C42 C41 30.6(11) . . ? C44 C43 C42 121.4(10) . . ? C44 C43 H43A 107.0 . . ? C42 C43 H43A 107.0 . . ? C44 C43 H43B 107.0 . . ? C42 C43 H43B 107.0 . . ? H43A C43 H43B 106.7 . . ? C43 C44 C45 110.1(12) . . ? C43 C44 C46 107.0(14) . . ? C45 C44 C46 104.5(14) . . ? C43 C44 N8 111.9(11) . . ? C45 C44 N8 114.1(11) . . ? C46 C44 N8 108.8(12) . . ? C44 C45 H45A 109.5 . . ? C44 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? C44 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? C44 C46 H46A 109.5 . . ? C44 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? C44 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? C48 C47 N8 110.1(10) . . ? C48 C47 H47A 109.6 . . ? N8 C47 H47A 109.6 . . ? C48 C47 H47B 109.6 . . ? N8 C47 H47B 109.6 . . ? H47A C47 H47B 108.1 . . ? N9 C48 C47 113.1(10) . . ? N9 C48 H48A 109.0 . . ? C47 C48 H48A 109.0 . . ? N9 C48 H48B 109.0 . . ? C47 C48 H48B 109.0 . . ? H48A C48 H48B 107.8 . . ? N9 C50 C51 110.5(9) . . ? N9 C50 C49 111.4(12) . . ? C51 C50 C49 105.9(13) . . ? N9 C50 C49' 117.8(15) . . ? C51 C50 C49' 113.1(15) . . ? C49 C50 C49' 96.8(14) . . ? N9 C50 C53' 135(3) . . ? C51 C50 C53' 25(3) . . ? C49 C50 C53' 93.1(16) . . ? C49' C50 C53' 94(3) . . ? C53' C51 C50 100(7) . . ? C53' C51 C52 99(3) . . ? C50 C51 C52 118.9(11) . . ? C54' C52 C54 75.3(17) . . ? C54' C52 N10 113.6(18) . . ? C54 C52 N10 120.9(13) . . ? C54' C52 C51 120(3) . . ? C54 C52 C51 115.2(12) . . ? N10 C52 C51 109.0(9) . . ? C54' C52 C53A 27.5(19) . . ? C54 C52 C53A 102.8(18) . . ? N10 C52 C53A 98(2) . . ? C51 C52 C53A 108(2) . . ? C54' C52 C53 25(2) . . ? C54 C52 C53 96.9(9) . . ? N10 C52 C53 112.0(18) . . ? C51 C52 C53 100(2) . . ? C53A C52 C53 14(3) . . ? C54' C52 C53' 102(3) . . ? C54 C52 C53' 96(2) . . ? N10 C52 C53' 134(2) . . ? C51 C52 C53' 25(2) . . ? C53A C52 C53' 100(4) . . ? C53 C52 C53' 88(3) . . ? C54' C53 C52 51(3) . . ? C54' C53A C52 60(4) . . ? C51 C53' C50 55(6) . . ? C51 C53' C52 56(3) . . ? C50 C53' C52 92(3) . . ? C52 C54 C54' 53.3(11) . . ? C53A C54' C53 33(7) . . ? C53A C54' C52 93(5) . . ? C53 C54' C52 104(4) . . ? C53A C54' C54 144(5) . . ? C53 C54' C54 145(6) . . ? C52 C54' C54 51.4(14) . . ? N10 C55 C56 110.7(8) . . ? N10 C55 H55A 109.5 . . ? C56 C55 H55A 109.5 . . ? N10 C55 H55B 109.5 . . ? C56 C55 H55B 109.5 . . ? H55A C55 H55B 108.1 . . ? C55 C56 N7 107.3(9) . . ? C55 C56 H56A 110.3 . . ? N7 C56 H56A 110.3 . . ? C55 C56 H56B 110.3 . . ? N7 C56 H56B 110.3 . . ? H56A C56 H56B 108.5 . . ? C10 N1 C9 105.8(8) . . ? C10 N1 C14 115.7(8) . 2_468 ? C9 N1 C14 106.8(8) . 2_468 ? C13 N2 C13' 59.5(12) . . ? C13 N2 C12 130.7(13) . . ? C13' N2 C12 115.6(8) . . ? C13 N2 C15 109.9(13) . . ? C13' N2 C15 119.8(8) . . ? C12 N2 C15 112.3(7) . . ? C7 O1 Ni1 133.4(5) . . ? C8 O4 Ni3 140.3(6) . 2_568 ? C17 O5 Ni2 134.1(6) . . ? C16 O7 Ni3 131.7(6) . . ? C29 N3 C31 114.2(9) . . ? C29 N3 Ni1 117.6(7) . . ? C31 N3 Ni1 105.6(8) . . ? C29 N3 H3D 122(9) . . ? C31 N3 H3D 106(6) . . ? Ni1 N3 H3D 88(10) . . ? C32 N4 C27 118.2(10) . 2_379 ? C32 N4 Ni1 107.7(7) . . ? C27 N4 Ni1 121.4(8) 2_379 . ? C32 N4 H4D 97.0(12) . . ? C27 N4 H4D 81(2) 2_379 . ? Ni1 N4 H4D 128.3(14) . . ? C39 N5 C37 115.6(8) . . ? C39 N5 Ni2 107.4(6) . . ? C37 N5 Ni2 117.0(6) . . ? C39 N5 H5D 96.8(12) . . ? C37 N5 H5D 104(6) . . ? Ni2 N5 H5D 115(6) . . ? C35 N6 C40 117.3(9) 2_469 . ? C35 N6 Ni2 121.6(7) 2_469 . ? C40 N6 Ni2 106.3(6) . . ? C35 N6 H6D 107(6) 2_469 . ? C40 N6 H6D 92.1(12) . . ? Ni2 N6 H6D 108(7) . . ? C42 N7 C56 119.1(10) . . ? C42 N7 Ni3 119.6(7) . . ? C56 N7 Ni3 104.3(7) . . ? C42 N7 H7D 96.9(14) . . ? C56 N7 H7D 109(6) . . ? Ni3 N7 H7D 107(6) . . ? C47 N8 C44 121.7(10) . . ? C47 N8 Ni3 104.6(7) . . ? C44 N8 Ni3 118.6(7) . . ? C47 N8 H8D 94.6(13) . . ? C44 N8 H8D 129(5) . . ? Ni3 N8 H8D 78(8) . . ? C48 N9 C50 119.5(9) . . ? C48 N9 Ni3 106.0(8) . . ? C50 N9 Ni3 118.9(6) . . ? C48 N9 H9D 97.5(13) . . ? C50 N9 H9D 110.2(19) . . ? Ni3 N9 H9D 101.2(11) . . ? C55 N10 C52 117.6(8) . . ? C55 N10 Ni3 106.1(6) . . ? C52 N10 Ni3 119.4(6) . . ? C55 N10 H10D 99.8(12) . . ? C52 N10 H10D 121(5) . . ? Ni3 N10 H10D 87(6) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C6 C1 C2 C3 -4.4(13) . . . . ? C7 C1 C2 C3 -179.6(8) . . . . ? C1 C2 C3 C4 4.4(13) . . . . ? C1 C2 C3 C8 -178.2(9) . . . . ? C2 C3 C4 C5 -1.9(15) . . . . ? C8 C3 C4 C5 -179.5(10) . . . . ? C3 C4 C5 C6 -0.3(16) . . . . ? C3 C4 C5 C9 165.4(10) . . . . ? C4 C5 C6 C1 0.3(16) . . . . ? C9 C5 C6 C1 -166.0(10) . . . . ? C2 C1 C6 C5 2.0(15) . . . . ? C7 C1 C6 C5 177.1(10) . . . . ? C2 C1 C7 O1 -176.4(8) . . . . ? C6 C1 C7 O1 8.5(14) . . . . ? C2 C1 C7 O2 1.3(15) . . . . ? C6 C1 C7 O2 -173.7(10) . . . . ? C2 C3 C8 O4 -167.2(9) . . . . ? C4 C3 C8 O4 10.2(14) . . . . ? C2 C3 C8 O3 15.1(15) . . . . ? C4 C3 C8 O3 -167.5(10) . . . . ? C6 C5 C9 N1 -154.2(10) . . . . ? C4 C5 C9 N1 40.6(15) . . . . ? N1 C10 C11 C12 54.2(14) . . . . ? C10 C11 C12 N2 -166.7(9) . . . . ? C14 C13 C13' N2 -134.5(12) . . . . ? N2 C13 C13' C14 134.5(12) . . . . ? C13 C13' C14 N1 140.2(14) . . . 2_468 ? N2 C13' C14 N1 -178.7(9) . . . 2_468 ? N2 C13' C14 C13 41.1(13) . . . . ? N2 C13 C14 N1 -101.5(18) . . . 2_468 ? C13' C13 C14 N1 -59.8(18) . . . 2_468 ? N2 C13 C14 C13' -41.7(13) . . . . ? O5 C17 C18 C23 178.2(9) . . . . ? O6 C17 C18 C23 -5.1(14) . . . . ? O5 C17 C18 C19 2.4(14) . . . . ? O6 C17 C18 C19 179.1(9) . . . . ? C23 C18 C19 C20 1.6(12) . . . . ? C17 C18 C19 C20 177.6(8) . . . . ? C18 C19 C20 C21 0.4(12) . . . . ? C18 C19 C20 C15 -177.8(8) . . . . ? N2 C15 C20 C21 -80.8(9) . . . . ? N2 C15 C20 C19 97.4(10) . . . . ? C19 C20 C21 C22 -1.4(12) . . . . ? C15 C20 C21 C22 176.8(8) . . . . ? C20 C21 C22 C23 0.5(12) . . . . ? C20 C21 C22 C16 -177.5(8) . . . . ? O7 C16 C22 C23 -171.9(9) . . . . ? O8 C16 C22 C23 8.1(14) . . . . ? O7 C16 C22 C21 6.0(14) . . . . ? O8 C16 C22 C21 -174.0(9) . . . . ? C21 C22 C23 C18 1.6(13) . . . . ? C16 C22 C23 C18 179.5(8) . . . . ? C19 C18 C23 C22 -2.6(13) . . . . ? C17 C18 C23 C22 -178.5(8) . . . . ? N4 C27 C28 C29 -63.7(14) 2_379 . . . ? C26 C27 C28 C29 57.5(16) . . . . ? C25 C27 C28 C29 176.5(11) . . . . ? C27 C28 C29 N3 73.1(13) . . . . ? C27 C28 C29 C30B -163.7(14) . . . . ? C27 C28 C29 C30A -134(10) . . . . ? C27 C28 C29 C30 -162(2) . . . . ? C28 C29 C30 C30B -4(6) . . . . ? N3 C29 C30 C30B 123(5) . . . . ? C30A C29 C30 C30B -116(24) . . . . ? C28 C29 C30 C30A 112(24) . . . . ? N3 C29 C30 C30A -121(24) . . . . ? C30B C29 C30 C30A 116(25) . . . . ? C29 C30 C30A C30B -70(10) . . . . ? C30B C30 C30A C29 70(10) . . . . ? C28 C29 C30A C30 -84(25) . . . . ? N3 C29 C30A C30 67(24) . . . . ? C30B C29 C30A C30 -36(15) . . . . ? C28 C29 C30A C30B -49(15) . . . . ? N3 C29 C30A C30B 102(11) . . . . ? C30 C29 C30A C30B 36(15) . . . . ? C29 C30 C30B C30A 73(12) . . . . ? C30A C30 C30B C29 -73(12) . . . . ? C29 C30A C30B C30 -99(14) . . . . ? C30 C30A C30B C29 99(14) . . . . ? C28 C29 C30B C30 177(5) . . . . ? N3 C29 C30B C30 -66(6) . . . . ? C30A C29 C30B C30 34(14) . . . . ? C28 C29 C30B C30A 143(14) . . . . ? N3 C29 C30B C30A -100(14) . . . . ? C30 C29 C30B C30A -34(14) . . . . ? N3 C31 C32 N4 -55.4(12) . . . . ? N6 C35 C36 C37 -70.2(13) 2_469 . . . ? C34 C35 C36 C37 53.4(14) . . . . ? C33 C35 C36 C37 173.2(10) . . . . ? C35 C36 C37 N5 72.6(12) . . . . ? C35 C36 C37 C38 -164.8(9) . . . . ? N5 C39 C40 N6 -56.3(10) . . . . ? C41 C41' C42 N7 -93(3) . . . . ? C41 C41' C42 C43 149(3) . . . . ? C41' C41 C42 N7 99(3) . . . . ? C41' C41 C42 C43 -37(3) . . . . ? N7 C42 C43 C44 70.5(15) . . . . ? C41' C42 C43 C44 -172.5(14) . . . . ? C41 C42 C43 C44 -154.4(15) . . . . ? C42 C43 C44 C45 58.9(17) . . . . ? C42 C43 C44 C46 171.8(14) . . . . ? C42 C43 C44 N8 -69.1(15) . . . . ? N8 C47 C48 N9 54.0(12) . . . . ? N9 C50 C51 C53' -178(3) . . . . ? C49 C50 C51 C53' 61(3) . . . . ? C49' C50 C51 C53' -43(3) . . . . ? N9 C50 C51 C52 -71.7(13) . . . . ? C49 C50 C51 C52 167.5(12) . . . . ? C49' C50 C51 C52 62.7(18) . . . . ? C53' C50 C51 C52 106(3) . . . . ? C53' C51 C52 C54' -47(7) . . . . ? C50 C51 C52 C54' -153.7(18) . . . . ? C53' C51 C52 C54 40(7) . . . . ? C50 C51 C52 C54 -66.7(17) . . . . ? C53' C51 C52 N10 180(7) . . . . ? C50 C51 C52 N10 73.0(13) . . . . ? C53' C51 C52 C53A -74(7) . . . . ? C50 C51 C52 C53A 178.9(19) . . . . ? C53' C51 C52 C53 -63(7) . . . . ? C50 C51 C52 C53 -169.4(16) . . . . ? C50 C51 C52 C53' -107(7) . . . . ? C54 C52 C53 C54' 28(7) . . . . ? N10 C52 C53 C54' -99(6) . . . . ? C51 C52 C53 C54' 146(6) . . . . ? C53A C52 C53 C54' -87(13) . . . . ? C53' C52 C53 C54' 124(7) . . . . ? C54 C52 C53A C54' -2(7) . . . . ? N10 C52 C53A C54' -127(7) . . . . ? C51 C52 C53A C54' 120(7) . . . . ? C53 C52 C53A C54' 64(9) . . . . ? C53' C52 C53A C54' 96(7) . . . . ? C52 C51 C53' C50 -122(2) . . . . ? C50 C51 C53' C52 122(2) . . . . ? N9 C50 C53' C51 3(4) . . . . ? C49 C50 C53' C51 -122(3) . . . . ? C49' C50 C53' C51 141(3) . . . . ? N9 C50 C53' C52 -42(3) . . . . ? C51 C50 C53' C52 -45(2) . . . . ? C49 C50 C53' C52 -168(2) . . . . ? C49' C50 C53' C52 95(3) . . . . ? C54' C52 C53' C51 140(6) . . . . ? C54 C52 C53' C51 -144(6) . . . . ? N10 C52 C53' C51 -1(9) . . . . ? C53A C52 C53' C51 112(7) . . . . ? C53 C52 C53' C51 119(7) . . . . ? C54' C52 C53' C50 -176(2) . . . . ? C54 C52 C53' C50 -100(2) . . . . ? N10 C52 C53' C50 44(5) . . . . ? C51 C52 C53' C50 44(5) . . . . ? C53A C52 C53' C50 156(2) . . . . ? C53 C52 C53' C50 163(3) . . . . ? N10 C52 C54 C54' 109(2) . . . . ? C51 C52 C54 C54' -116(3) . . . . ? C53A C52 C54 C54' 1(4) . . . . ? C53 C52 C54 C54' -12(3) . . . . ? C53' C52 C54 C54' -101(4) . . . . ? C52 C53A C54' C53 -112(10) . . . . ? C52 C53A C54' C54 3(10) . . . . ? C52 C53 C54' C53A 73(11) . . . . ? C52 C53 C54' C54 -41(5) . . . . ? C54 C52 C54' C53A 178(8) . . . . ? N10 C52 C54' C53A 60(8) . . . . ? C51 C52 C54' C53A -71(7) . . . . ? C53 C52 C54' C53A -31(8) . . . . ? C53' C52 C54' C53A -89(7) . . . . ? C54 C52 C54' C53 -151(7) . . . . ? N10 C52 C54' C53 91(7) . . . . ? C51 C52 C54' C53 -40(7) . . . . ? C53A C52 C54' C53 31(8) . . . . ? C53' C52 C54' C53 -58(7) . . . . ? N10 C52 C54' C54 -117.7(15) . . . . ? C51 C52 C54' C54 110.9(16) . . . . ? C53A C52 C54' C54 -178(8) . . . . ? C53 C52 C54' C54 151(7) . . . . ? C53' C52 C54' C54 93(2) . . . . ? C52 C54 C54' C53A -4(13) . . . . ? C52 C54 C54' C53 55(8) . . . . ? N10 C55 C56 N7 -58.3(11) . . . . ? C11 C10 N1 C9 178.1(9) . . . . ? C11 C10 N1 C14 60.1(13) . . . 2_468 ? C5 C9 N1 C10 79.4(11) . . . . ? C5 C9 N1 C14 -156.8(8) . . . 2_468 ? C14 C13 N2 C13' 41.2(12) . . . . ? C13' C13 N2 C12 -98.9(16) . . . . ? C14 C13 N2 C12 -58(2) . . . . ? C13' C13 N2 C15 113.5(11) . . . . ? C14 C13 N2 C15 154.7(11) . . . . ? C14 C13' N2 C13 -46.5(14) . . . . ? C13 C13' N2 C12 123.8(15) . . . . ? C14 C13' N2 C12 77.3(11) . . . . ? C13 C13' N2 C15 -96.8(15) . . . . ? C14 C13' N2 C15 -143.3(9) . . . . ? C11 C12 N2 C13 150.9(18) . . . . ? C11 C12 N2 C13' 80.3(11) . . . . ? C11 C12 N2 C15 -62.1(10) . . . . ? C20 C15 N2 C13 81.4(15) . . . . ? C20 C15 N2 C13' 146.9(9) . . . . ? C20 C15 N2 C12 -72.5(10) . . . . ? O2 C7 O1 Ni1 0.2(17) . . . . ? C1 C7 O1 Ni1 177.8(6) . . . . ? N3 Ni1 O1 C7 5.9(10) 2_379 . . . ? N3 Ni1 O1 C7 -174.1(10) . . . . ? N4 Ni1 O1 C7 -89.5(9) . . . . ? N4 Ni1 O1 C7 90.5(9) 2_379 . . . ? O1 Ni1 O1 C7 174(100) 2_379 . . . ? O3 C8 O4 Ni3 8.8(18) . . . 2_568 ? C3 C8 O4 Ni3 -168.8(6) . . . 2_568 ? O6 C17 O5 Ni2 0.5(16) . . . . ? C18 C17 O5 Ni2 176.9(6) . . . . ? N5 Ni2 O5 C17 -4.2(9) 2_469 . . . ? N5 Ni2 O5 C17 175.8(9) . . . . ? N6 Ni2 O5 C17 81.3(9) 2_469 . . . ? N6 Ni2 O5 C17 -98.7(9) . . . . ? O5 Ni2 O5 C17 -140(100) 2_469 . . . ? O8 C16 O7 Ni3 -6.8(17) . . . . ? C22 C16 O7 Ni3 173.2(6) . . . . ? N10 Ni3 O7 C16 -3.3(9) . . . . ? N7 Ni3 O7 C16 -88.9(9) . . . . ? N9 Ni3 O7 C16 91.5(9) . . . . ? N8 Ni3 O7 C16 176.1(9) . . . . ? O4 Ni3 O7 C16 -86(5) 2_568 . . . ? C28 C29 N3 C31 -178.9(9) . . . . ? C30B C29 N3 C31 71.6(16) . . . . ? C30A C29 N3 C31 25(9) . . . . ? C30 C29 N3 C31 48.0(19) . . . . ? C28 C29 N3 Ni1 -54.3(11) . . . . ? C30B C29 N3 Ni1 -163.9(13) . . . . ? C30A C29 N3 Ni1 150(9) . . . . ? C30 C29 N3 Ni1 172.6(17) . . . . ? C32 C31 N3 C29 175.3(9) . . . . ? C32 C31 N3 Ni1 44.6(10) . . . . ? N3 Ni1 N3 C29 -124(100) 2_379 . . . ? N4 Ni1 N3 C29 -145.9(8) . . . . ? N4 Ni1 N3 C29 34.1(8) 2_379 . . . ? O1 Ni1 N3 C29 -62.6(8) . . . . ? O1 Ni1 N3 C29 117.4(8) 2_379 . . . ? N3 Ni1 N3 C31 5(94) 2_379 . . . ? N4 Ni1 N3 C31 -17.1(6) . . . . ? N4 Ni1 N3 C31 162.9(6) 2_379 . . . ? O1 Ni1 N3 C31 66.2(6) . . . . ? O1 Ni1 N3 C31 -113.8(6) 2_379 . . . ? C31 C32 N4 C27 179.0(10) . . . 2_379 ? C31 C32 N4 Ni1 36.7(11) . . . . ? N3 Ni1 N4 C32 169.1(7) 2_379 . . . ? N3 Ni1 N4 C32 -10.9(7) . . . . ? N4 Ni1 N4 C32 -17(100) 2_379 . . . ? O1 Ni1 N4 C32 -99.2(7) . . . . ? O1 Ni1 N4 C32 80.8(7) 2_379 . . . ? N3 Ni1 N4 C27 28.2(8) 2_379 . . 2_379 ? N3 Ni1 N4 C27 -151.8(8) . . . 2_379 ? N4 Ni1 N4 C27 -158(100) 2_379 . . 2_379 ? O1 Ni1 N4 C27 119.9(8) . . . 2_379 ? O1 Ni1 N4 C27 -60.1(8) 2_379 . . 2_379 ? C40 C39 N5 C37 178.0(7) . . . . ? C40 C39 N5 Ni2 45.4(8) . . . . ? C36 C37 N5 C39 -178.0(8) . . . . ? C38 C37 N5 C39 59.4(10) . . . . ? C36 C37 N5 Ni2 -50.0(9) . . . . ? C38 C37 N5 Ni2 -172.6(6) . . . . ? N5 Ni2 N5 C39 -72(100) 2_469 . . . ? N6 Ni2 N5 C39 160.8(6) 2_469 . . . ? N6 Ni2 N5 C39 -19.2(6) . . . . ? O5 Ni2 N5 C39 63.8(6) . . . . ? O5 Ni2 N5 C39 -116.2(6) 2_469 . . . ? N5 Ni2 N5 C37 156(100) 2_469 . . . ? N6 Ni2 N5 C37 29.0(6) 2_469 . . . ? N6 Ni2 N5 C37 -151.0(6) . . . . ? O5 Ni2 N5 C37 -68.0(6) . . . . ? O5 Ni2 N5 C37 112.0(6) 2_469 . . . ? C39 C40 N6 C35 177.8(9) . . . 2_469 ? C39 C40 N6 Ni2 37.9(8) . . . . ? N5 Ni2 N6 C35 31.3(8) 2_469 . . 2_469 ? N5 Ni2 N6 C35 -148.7(8) . . . 2_469 ? N6 Ni2 N6 C35 -141(85) 2_469 . . 2_469 ? O5 Ni2 N6 C35 121.9(8) . . . 2_469 ? O5 Ni2 N6 C35 -58.1(8) 2_469 . . 2_469 ? N5 Ni2 N6 C40 169.0(6) 2_469 . . . ? N5 Ni2 N6 C40 -11.0(6) . . . . ? N6 Ni2 N6 C40 -3(82) 2_469 . . . ? O5 Ni2 N6 C40 -100.3(6) . . . . ? O5 Ni2 N6 C40 79.7(6) 2_469 . . . ? C43 C42 N7 C56 -175.8(9) . . . . ? C41' C42 N7 C56 75.6(15) . . . . ? C41 C42 N7 C56 42.9(15) . . . . ? C43 C42 N7 Ni3 -46.0(12) . . . . ? C41' C42 N7 Ni3 -154.6(12) . . . . ? C41 C42 N7 Ni3 172.7(11) . . . . ? C55 C56 N7 C42 179.4(8) . . . . ? C55 C56 N7 Ni3 43.0(9) . . . . ? N10 Ni3 N7 C42 -153.8(8) . . . . ? N9 Ni3 N7 C42 17(59) . . . . ? N8 Ni3 N7 C42 27.2(8) . . . . ? O4 Ni3 N7 C42 117.6(8) 2_568 . . . ? O7 Ni3 N7 C42 -62.5(8) . . . . ? N10 Ni3 N7 C56 -17.7(6) . . . . ? N9 Ni3 N7 C56 154(58) . . . . ? N8 Ni3 N7 C56 163.3(6) . . . . ? O4 Ni3 N7 C56 -106.3(7) 2_568 . . . ? O7 Ni3 N7 C56 73.6(7) . . . . ? C48 C47 N8 C44 -177.4(9) . . . . ? C48 C47 N8 Ni3 -39.4(10) . . . . ? C43 C44 N8 C47 177.5(9) . . . . ? C45 C44 N8 C47 51.7(15) . . . . ? C46 C44 N8 C47 -64.5(16) . . . . ? C43 C44 N8 Ni3 45.0(12) . . . . ? C45 C44 N8 Ni3 -80.8(12) . . . . ? C46 C44 N8 Ni3 163.0(12) . . . . ? N10 Ni3 N8 C47 79(18) . . . . ? N7 Ni3 N8 C47 -165.1(7) . . . . ? N9 Ni3 N8 C47 14.8(7) . . . . ? O4 Ni3 N8 C47 112.8(7) 2_568 . . . ? O7 Ni3 N8 C47 -70.1(7) . . . . ? N10 Ni3 N8 C44 -142(18) . . . . ? N7 Ni3 N8 C44 -25.5(8) . . . . ? N9 Ni3 N8 C44 154.4(8) . . . . ? O4 Ni3 N8 C44 -107.7(7) 2_568 . . . ? O7 Ni3 N8 C44 69.5(7) . . . . ? C47 C48 N9 C50 -175.5(10) . . . . ? C47 C48 N9 Ni3 -37.7(10) . . . . ? C51 C50 N9 C48 -178.7(9) . . . . ? C49 C50 N9 C48 -61.3(15) . . . . ? C49' C50 N9 C48 49.3(17) . . . . ? C53' C50 N9 C48 180.0(17) . . . . ? C51 C50 N9 Ni3 48.9(12) . . . . ? C49 C50 N9 Ni3 166.3(11) . . . . ? C49' C50 N9 Ni3 -83.1(15) . . . . ? C53' C50 N9 Ni3 48(2) . . . . ? N10 Ni3 N9 C48 -168.1(6) . . . . ? N7 Ni3 N9 C48 21(59) . . . . ? N8 Ni3 N9 C48 10.9(6) . . . . ? O4 Ni3 N9 C48 -79.5(6) 2_568 . . . ? O7 Ni3 N9 C48 100.6(6) . . . . ? N10 Ni3 N9 C50 -30.1(8) . . . . ? N7 Ni3 N9 C50 159(98) . . . . ? N8 Ni3 N9 C50 148.9(8) . . . . ? O4 Ni3 N9 C50 58.6(8) 2_568 . . . ? O7 Ni3 N9 C50 -121.3(8) . . . . ? C56 C55 N10 C52 177.1(9) . . . . ? C56 C55 N10 Ni3 40.4(9) . . . . ? C54' C52 N10 C55 41(3) . . . . ? C54 C52 N10 C55 -45.0(15) . . . . ? C51 C52 N10 C55 178.0(9) . . . . ? C53A C52 N10 C55 65(2) . . . . ? C53 C52 N10 C55 68.1(19) . . . . ? C53' C52 N10 C55 178(4) . . . . ? C54' C52 N10 Ni3 172(2) . . . . ? C54 C52 N10 Ni3 85.8(13) . . . . ? C51 C52 N10 Ni3 -51.2(11) . . . . ? C53A C52 N10 Ni3 -163.8(19) . . . . ? C53 C52 N10 Ni3 -161.0(16) . . . . ? C53' C52 N10 Ni3 -51(4) . . . . ? N7 Ni3 N10 C55 -12.0(6) . . . . ? N9 Ni3 N10 C55 168.1(6) . . . . ? N8 Ni3 N10 C55 104(18) . . . . ? O4 Ni3 N10 C55 70.2(5) 2_568 . . . ? O7 Ni3 N10 C55 -107.0(5) . . . . ? N7 Ni3 N10 C52 -147.7(7) . . . . ? N9 Ni3 N10 C52 32.3(7) . . . . ? N8 Ni3 N10 C52 -31(18) . . . . ? O4 Ni3 N10 C52 -65.5(7) 2_568 . . . ? O7 Ni3 N10 C52 117.3(7) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N3 H3D O2 0.70(9) 2.21(7) 2.885(9) 164(10) 2_379 N5 H5D O6 0.898(10) 2.00(5) 2.773(10) 144(7) 2_469 N8 H8D O3 0.901(10) 2.13(3) 3.012(10) 165(9) 2_568 N9 H9D O7 0.899(10) 2.407(18) 2.856(10) 111.1(11) . N10 H10D O8 0.903(10) 1.900(19) 2.769(11) 161(4) . _diffrn_measured_fraction_theta_max 0.981 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.981 _refine_diff_density_max 0.893 _refine_diff_density_min -0.576 _refine_diff_density_rms 0.084 #=========================END data_Compound-8 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C62 H90 N8 Ni3 O22, 6H2O' _chemical_formula_sum 'C62 H102 N8 Ni3 O28' _chemical_formula_weight 1583.65 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ni' 'Ni' 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.1977(7) _cell_length_b 11.2936(7) _cell_length_c 14.7885(9) _cell_angle_alpha 70.036(6) _cell_angle_beta 88.302(5) _cell_angle_gamma 79.258(5) _cell_volume 1725.83(18) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 4215 _cell_measurement_theta_min 2.9094 _cell_measurement_theta_max 29.2176 _exptl_crystal_description strip _exptl_crystal_colour yellow _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.524 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 838 _exptl_absorpt_coefficient_mu 0.901 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8128 _exptl_absorpt_correction_T_max 0.8692 _exptl_absorpt_process_details ; CrysAlis (Oxford Diffraction, 2006) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Diffraction Gemini R Ultra' _diffrn_measurement_method '\w scan' _diffrn_detector_area_resol_mean 10.0 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10658 _diffrn_reflns_av_R_equivalents 0.0274 _diffrn_reflns_av_sigmaI/netI 0.0512 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.92 _diffrn_reflns_theta_max 25.35 _reflns_number_total 6279 _reflns_number_gt 4968 _reflns_threshold_expression >2\s(I) _computing_data_collection 'CrysAlisPro(1.171.35.21) (Agilent Tech., 2012)' _computing_cell_refinement 'CrysAlisPro(1.171.35.21) (Agilent Tech., 2012)' _computing_data_reduction 'CrysAlisPro(1.171.35.21) (Agilent Tech., 2012)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0757P)^2^+2.5348P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6279 _refine_ls_number_parameters 509 _refine_ls_number_restraints 26 _refine_ls_R_factor_all 0.0697 _refine_ls_R_factor_gt 0.0524 _refine_ls_wR_factor_ref 0.1530 _refine_ls_wR_factor_gt 0.1398 _refine_ls_goodness_of_fit_ref 1.032 _refine_ls_restrained_S_all 1.035 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni1 Ni 1.5000 1.0000 0.5000 0.02177(18) Uani 1 2 d S . . Ni2 Ni 0.5000 0.5000 1.0000 0.02631(19) Uani 1 2 d S . . Ni3 Ni 1.0000 1.0000 1.0000 0.0340(2) Uani 1 2 d S . . C1 C 1.1555(4) 0.9087(4) 0.5872(3) 0.0281(8) Uani 1 1 d . . . C2 C 1.1476(4) 0.9609(4) 0.6599(3) 0.0309(9) Uani 1 1 d . . . H2 H 1.2051 1.0084 0.6649 0.037 Uiso 1 1 calc R . . C3 C 1.0568(4) 0.9438(4) 0.7248(3) 0.0300(9) Uani 1 1 d . . . C4 C 0.9704(4) 0.8740(4) 0.7164(3) 0.0316(9) Uani 1 1 d . . . H4 H 0.9091 0.8611 0.7605 0.038 Uiso 1 1 calc R . . C5 C 0.9749(3) 0.8239(4) 0.6434(3) 0.0279(8) Uani 1 1 d . . . C6 C 1.0674(4) 0.8412(4) 0.5790(3) 0.0285(9) Uani 1 1 d . . . H6 H 1.0706 0.8072 0.5297 0.034 Uiso 1 1 calc R . . C7 C 1.2565(4) 0.9324(4) 0.5180(3) 0.0292(9) Uani 1 1 d . . . C8 C 1.0519(5) 1.0005(5) 0.8031(3) 0.0448(12) Uani 1 1 d . . . C9 C 0.8753(3) 0.7554(4) 0.6309(3) 0.0330(9) Uani 1 1 d . . . H9A H 0.8299 0.7334 0.6893 0.040 Uiso 1 1 calc R . . H9B H 0.8195 0.8128 0.5788 0.040 Uiso 1 1 calc R . . C10 C 0.8314(4) 0.6001(4) 0.5645(3) 0.0310(9) Uani 1 1 d . . . H10A H 0.7583 0.5998 0.6014 0.037 Uiso 1 1 calc R . . H10B H 0.8601 0.5139 0.5639 0.037 Uiso 1 1 calc R . . C11 C 0.8021(4) 0.6915(4) 0.4624(3) 0.0310(9) Uani 1 1 d . . . H11A H 0.7457 0.7671 0.4640 0.037 Uiso 1 1 calc R . . H11B H 0.8762 0.7186 0.4344 0.037 Uiso 1 1 calc R . . C12 C 0.8342(3) 0.5275(4) 0.3795(3) 0.0283(8) Uani 1 1 d . . . H12A H 0.8654 0.4627 0.4403 0.034 Uiso 1 1 calc R . . H12B H 0.7904 0.4878 0.3456 0.034 Uiso 1 1 calc R . . C13 C 0.9390(4) 0.5727(4) 0.3208(3) 0.0358(10) Uani 1 1 d . . . H13A H 0.9837 0.6115 0.3547 0.043 Uiso 1 1 calc R . . H13B H 0.9083 0.6375 0.2599 0.043 Uiso 1 1 calc R . . C14 C 1.0244(4) 0.4626(4) 0.3020(3) 0.0336(9) Uani 1 1 d . . . H14A H 0.9802 0.4268 0.2655 0.040 Uiso 1 1 calc R . . H14B H 1.0901 0.4956 0.2633 0.040 Uiso 1 1 calc R . . C15 C 0.6321(3) 0.5922(4) 0.4409(3) 0.0280(8) Uani 1 1 d . . . H15A H 0.5831 0.6608 0.4585 0.034 Uiso 1 1 calc R . . H15B H 0.6525 0.5184 0.4992 0.034 Uiso 1 1 calc R . . C16 C 0.5573(3) 0.5577(4) 0.3733(3) 0.0244(8) Uani 1 1 d . . . C17 C 0.4802(3) 0.6515(3) 0.3030(3) 0.0270(8) Uani 1 1 d . . . H17 H 0.4781 0.7375 0.2943 0.032 Uiso 1 1 calc R . . C18 C 0.4059(3) 0.6193(4) 0.2451(3) 0.0282(9) Uani 1 1 d . . . C19 C 0.4097(3) 0.4914(4) 0.2583(3) 0.0262(8) Uani 1 1 d . . . H19 H 0.3618 0.4691 0.2186 0.031 Uiso 1 1 calc R . . C20 C 0.4838(3) 0.3966(3) 0.3299(3) 0.0239(8) Uani 1 1 d . . . C21 C 0.5574(3) 0.4303(3) 0.3871(3) 0.0244(8) Uani 1 1 d . . . H21 H 0.6074 0.3665 0.4353 0.029 Uiso 1 1 calc R . . C22 C 0.3164(4) 0.7179(4) 0.1717(3) 0.0353(10) Uani 1 1 d . . . C23 C 0.4731(3) 0.2592(3) 0.3503(3) 0.0260(8) Uani 1 1 d . . . C24 C 0.7264(5) 0.4974(6) 1.1494(3) 0.0548(14) Uani 1 1 d . . . H24A H 0.7255 0.4170 1.1998 0.082 Uiso 1 1 calc R . . H24B H 0.6470 0.5505 1.1410 0.082 Uiso 1 1 calc R . . H24C H 0.7845 0.5397 1.1662 0.082 Uiso 1 1 calc R . . C25 C 0.7613(4) 0.4737(4) 1.0562(3) 0.0363(10) Uani 1 1 d . . . C26 C 0.8868(4) 0.3894(5) 1.0686(4) 0.0556(14) Uani 1 1 d . . . H26A H 0.8871 0.3105 1.1209 0.083 Uiso 1 1 calc R . . H26B H 0.9459 0.4332 1.0823 0.083 Uiso 1 1 calc R . . H26C H 0.9066 0.3715 1.0105 0.083 Uiso 1 1 calc R . . C27 C 0.7640(4) 0.5975(4) 0.9738(3) 0.0391(10) Uani 1 1 d . . . H27A H 0.8356 0.6291 0.9835 0.047 Uiso 1 1 calc R . . H27B H 0.7742 0.5774 0.9150 0.047 Uiso 1 1 calc R . . C28 C 0.6569(4) 0.7043(4) 0.9581(3) 0.0373(10) Uani 1 1 d . . . H28 H 0.6427 0.7209 1.0188 0.045 Uiso 1 1 calc R . . C29 C 0.6844(5) 0.8252(5) 0.8827(4) 0.0555(14) Uani 1 1 d . . . H29A H 0.6155 0.8936 0.8734 0.083 Uiso 1 1 calc R . . H29B H 0.7010 0.8102 0.8231 0.083 Uiso 1 1 calc R . . H29C H 0.7540 0.8484 0.9039 0.083 Uiso 1 1 calc R . . C30 C 0.4375(4) 0.7650(4) 0.9281(4) 0.0434(11) Uani 1 1 d . . . H30A H 0.4465 0.8463 0.8801 0.052 Uiso 1 1 calc R . . H30B H 0.4284 0.7763 0.9902 0.052 Uiso 1 1 calc R . . C31 C 0.3294(4) 0.7225(4) 0.9033(3) 0.0441(11) Uani 1 1 d . . . H31A H 0.3324 0.7234 0.8374 0.053 Uiso 1 1 calc R . . H31B H 0.2555 0.7790 0.9097 0.053 Uiso 1 1 calc R . . N1 N 0.9245(3) 0.6387(3) 0.6098(2) 0.0261(7) Uani 1 1 d . . . N2 N 0.7476(3) 0.6340(3) 0.3988(2) 0.0261(7) Uani 1 1 d . . . O1 O 1.3234(2) 1.0037(3) 0.5302(2) 0.0324(6) Uani 1 1 d . . . O2 O 1.2691(3) 0.8815(3) 0.4552(2) 0.0426(8) Uani 1 1 d . . . O3 O 0.9998(3) 0.9518(3) 0.8776(2) 0.0416(8) Uani 1 1 d . . . O4 O 1.1388(12) 1.0597(14) 0.8073(9) 0.063(4) Uani 0.40 1 d PU . . O4' O 1.0828(9) 1.1096(7) 0.7809(6) 0.060(2) Uani 0.60 1 d PU . . O5 O 0.3166(4) 0.8335(3) 0.1571(3) 0.0648(11) Uani 1 1 d . . . O6 O 0.2469(3) 0.6776(3) 0.1288(2) 0.0440(8) Uani 1 1 d . . . H6A H 0.2018 0.7387 0.0905 0.066 Uiso 1 1 calc R . . O7 O 0.4614(3) 0.2241(3) 0.2804(2) 0.0453(8) Uani 1 1 d . . . O8 O 0.4737(3) 0.1939(2) 0.43674(18) 0.0297(6) Uani 1 1 d . . . O4W O 1.3397(5) 1.1322(5) 0.7364(4) 0.051(2) Uani 0.722(13) 1 d P A 1 O4W' O 1.2823(12) 1.1915(15) 0.7863(11) 0.063(7) Uani 0.278(13) 1 d P A 2 O6W O 0.5348(5) 0.9072(5) 0.0890(3) 0.0977(16) Uani 1 1 d . . . O1W O 1.5288(3) 1.0318(3) 0.63002(19) 0.0324(6) Uani 1 1 d D . . H1A H 1.598(2) 1.061(3) 0.615(3) 0.049 Uiso 1 1 d D . . H1B H 1.548(3) 0.9495(16) 0.667(3) 0.049 Uiso 1 1 d D . . O2W O 1.0147(3) 0.8074(3) 1.0817(2) 0.0432(8) Uani 1 1 d D . . H2A H 0.981(5) 0.763(5) 1.062(3) 0.065 Uiso 1 1 d D . . H2B H 1.003(5) 0.820(5) 1.132(2) 0.065 Uiso 1 1 d D . . O3W O 0.8139(3) 1.0148(4) 0.9992(3) 0.0532(9) Uani 1 1 d D . . H3A H 0.782(4) 0.943(3) 1.026(4) 0.080 Uiso 1 1 d D . . H3B H 0.760(4) 1.069(4) 0.953(3) 0.080 Uiso 1 1 d D . . N3 N 0.5443(3) 0.6667(3) 0.9310(2) 0.0304(7) Uani 1 1 d D . . H32 H 0.550(4) 0.669(5) 0.8708(13) 0.046 Uiso 1 1 d D . . N4 N 0.3315(3) 0.5898(3) 0.9712(2) 0.0315(8) Uani 1 1 d D . . H33 H 0.304(4) 0.596(5) 1.0266(19) 0.047 Uiso 1 1 d D . . O5W O 1.1643(6) 0.7251(5) 0.3845(4) 0.0956(16) Uani 1 1 d D . . H5A H 1.159(9) 0.781(6) 0.3234(19) 0.143 Uiso 1 1 d D . . H5B H 1.192(8) 0.765(6) 0.421(4) 0.143 Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.0275(4) 0.0166(3) 0.0228(3) -0.0071(3) 0.0062(3) -0.0082(3) Ni2 0.0235(4) 0.0314(4) 0.0263(4) -0.0110(3) 0.0010(3) -0.0083(3) Ni3 0.0392(5) 0.0324(4) 0.0311(4) -0.0127(3) -0.0028(3) -0.0046(3) C1 0.029(2) 0.026(2) 0.031(2) -0.0118(17) 0.0031(17) -0.0078(17) C2 0.037(2) 0.031(2) 0.032(2) -0.0133(18) 0.0009(18) -0.0179(18) C3 0.041(2) 0.027(2) 0.028(2) -0.0134(17) 0.0041(17) -0.0133(18) C4 0.030(2) 0.036(2) 0.034(2) -0.0170(18) 0.0065(17) -0.0106(18) C5 0.027(2) 0.030(2) 0.032(2) -0.0164(17) -0.0002(16) -0.0074(17) C6 0.031(2) 0.031(2) 0.030(2) -0.0177(17) -0.0019(17) -0.0069(17) C7 0.029(2) 0.025(2) 0.033(2) -0.0101(17) 0.0025(17) -0.0042(17) C8 0.063(3) 0.048(3) 0.039(3) -0.026(2) 0.014(2) -0.029(2) C9 0.020(2) 0.042(2) 0.049(3) -0.030(2) 0.0044(18) -0.0074(17) C10 0.028(2) 0.035(2) 0.037(2) -0.0171(19) -0.0010(17) -0.0136(18) C11 0.031(2) 0.033(2) 0.040(2) -0.0231(19) -0.0009(18) -0.0108(17) C12 0.024(2) 0.031(2) 0.035(2) -0.0190(18) 0.0004(16) -0.0034(16) C13 0.033(2) 0.033(2) 0.040(2) -0.0090(19) -0.0021(19) -0.0081(18) C14 0.027(2) 0.045(3) 0.033(2) -0.018(2) 0.0001(17) -0.0072(18) C15 0.024(2) 0.031(2) 0.033(2) -0.0146(17) 0.0017(16) -0.0088(17) C16 0.0205(18) 0.027(2) 0.0279(19) -0.0111(16) 0.0042(15) -0.0063(15) C17 0.030(2) 0.0185(18) 0.034(2) -0.0099(16) 0.0008(17) -0.0056(16) C18 0.026(2) 0.024(2) 0.033(2) -0.0079(17) -0.0021(17) -0.0030(16) C19 0.025(2) 0.029(2) 0.0265(19) -0.0104(17) 0.0001(16) -0.0076(16) C20 0.0254(19) 0.0208(18) 0.0252(19) -0.0067(15) 0.0036(15) -0.0062(15) C21 0.0237(19) 0.0222(18) 0.0254(19) -0.0052(15) -0.0033(15) -0.0045(15) C22 0.037(2) 0.027(2) 0.039(2) -0.0103(19) -0.0098(19) 0.0002(18) C23 0.027(2) 0.0201(19) 0.030(2) -0.0050(17) -0.0001(16) -0.0080(16) C24 0.055(3) 0.078(4) 0.040(3) -0.026(3) -0.001(2) -0.024(3) C25 0.026(2) 0.051(3) 0.035(2) -0.017(2) -0.0007(18) -0.0115(19) C26 0.031(3) 0.061(3) 0.071(4) -0.018(3) -0.009(2) -0.007(2) C27 0.030(2) 0.054(3) 0.044(3) -0.023(2) 0.0096(19) -0.021(2) C28 0.036(2) 0.042(2) 0.042(2) -0.020(2) 0.0039(19) -0.018(2) C29 0.050(3) 0.049(3) 0.072(4) -0.018(3) 0.006(3) -0.025(2) C30 0.042(3) 0.033(2) 0.053(3) -0.011(2) 0.003(2) -0.010(2) C31 0.035(2) 0.041(3) 0.048(3) -0.006(2) -0.004(2) -0.006(2) N1 0.0206(16) 0.0321(18) 0.0339(17) -0.0198(15) 0.0000(13) -0.0089(13) N2 0.0232(16) 0.0264(17) 0.0336(17) -0.0146(14) -0.0009(13) -0.0082(13) O1 0.0290(15) 0.0298(15) 0.0471(17) -0.0204(13) 0.0121(13) -0.0149(12) O2 0.0431(18) 0.056(2) 0.0456(18) -0.0335(16) 0.0149(14) -0.0229(15) O3 0.059(2) 0.0456(18) 0.0307(16) -0.0209(14) 0.0068(15) -0.0212(16) O4 0.071(7) 0.089(8) 0.063(7) -0.055(6) 0.023(5) -0.046(6) O4' 0.102(6) 0.044(4) 0.052(4) -0.028(3) 0.025(4) -0.041(4) O5 0.082(3) 0.0252(17) 0.077(3) -0.0083(17) -0.045(2) 0.0025(17) O6 0.0418(18) 0.0382(17) 0.0472(18) -0.0144(15) -0.0206(15) 0.0072(14) O7 0.083(2) 0.0277(16) 0.0295(15) -0.0088(13) -0.0028(16) -0.0211(16) O8 0.0427(17) 0.0186(13) 0.0269(14) -0.0058(12) 0.0060(12) -0.0080(12) O4W 0.059(4) 0.042(3) 0.053(3) -0.011(2) -0.008(3) -0.018(3) O4W' 0.046(8) 0.058(10) 0.053(10) 0.025(8) -0.007(7) -0.018(7) O6W 0.139(5) 0.082(3) 0.065(3) -0.013(2) -0.020(3) -0.022(3) O1W 0.0428(17) 0.0295(15) 0.0280(15) -0.0114(12) 0.0057(13) -0.0126(13) O2W 0.059(2) 0.0337(17) 0.0383(18) -0.0155(15) -0.0010(16) -0.0059(15) O3W 0.0421(19) 0.063(2) 0.045(2) -0.0049(17) -0.0095(15) -0.0105(17) N3 0.0316(18) 0.0339(18) 0.0295(17) -0.0137(15) 0.0023(15) -0.0103(15) N4 0.0254(18) 0.0367(19) 0.0332(18) -0.0126(16) -0.0002(15) -0.0064(15) O5W 0.137(5) 0.090(4) 0.095(3) -0.059(3) 0.030(3) -0.060(3) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 O1 2.010(3) 2_876 ? Ni1 O1 2.010(3) . ? Ni1 O8 2.033(2) 1_665 ? Ni1 O8 2.033(2) 2_766 ? Ni1 O1W 2.117(3) 2_876 ? Ni1 O1W 2.117(3) . ? Ni2 N4 1.952(3) . ? Ni2 N4 1.952(3) 2_667 ? Ni2 N3 1.959(3) . ? Ni2 N3 1.959(3) 2_667 ? Ni3 O3W 2.060(3) 2_777 ? Ni3 O3W 2.060(3) . ? Ni3 O3 2.061(3) . ? Ni3 O3 2.061(3) 2_777 ? Ni3 O2W 2.074(3) 2_777 ? Ni3 O2W 2.074(3) . ? C1 C2 1.385(5) . ? C1 C6 1.386(5) . ? C1 C7 1.502(6) . ? C2 C3 1.371(6) . ? C2 H2 0.9300 . ? C3 C4 1.390(5) . ? C3 C8 1.498(5) . ? C4 C5 1.375(5) . ? C4 H4 0.9300 . ? C5 C6 1.381(6) . ? C5 C9 1.519(5) . ? C6 H6 0.9300 . ? C7 O2 1.241(5) . ? C7 O1 1.255(4) . ? C8 O3 1.234(5) . ? C8 O4' 1.274(8) . ? C8 O4 1.293(12) . ? C9 N1 1.462(5) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 N1 1.462(4) . ? C10 C11 1.513(6) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 N2 1.509(4) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 C13 1.500(6) . ? C12 N2 1.502(5) . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C13 C14 1.521(6) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 N1 1.455(5) 2_766 ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 N2 1.504(5) . ? C15 C16 1.513(5) . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 C17 1.382(5) . ? C16 C21 1.382(5) . ? C17 C18 1.387(5) . ? C17 H17 0.9300 . ? C18 C19 1.383(5) . ? C18 C22 1.499(5) . ? C19 C20 1.379(5) . ? C19 H19 0.9300 . ? C20 C21 1.385(5) . ? C20 C23 1.503(5) . ? C21 H21 0.9300 . ? C22 O5 1.249(5) . ? C22 O6 1.254(5) . ? C23 O8 1.238(4) . ? C23 O7 1.244(5) . ? C24 C25 1.517(6) . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? C25 N4 1.504(5) 2_667 ? C25 C27 1.514(6) . ? C25 C26 1.520(7) . ? C26 H26A 0.9600 . ? C26 H26B 0.9600 . ? C26 H26C 0.9600 . ? C27 C28 1.494(6) . ? C27 H27A 0.9700 . ? C27 H27B 0.9700 . ? C28 N3 1.509(5) . ? C28 C29 1.517(6) . ? C28 H28 0.9800 . ? C29 H29A 0.9600 . ? C29 H29B 0.9600 . ? C29 H29C 0.9600 . ? C30 N3 1.463(6) . ? C30 C31 1.481(6) . ? C30 H30A 0.9700 . ? C30 H30B 0.9700 . ? C31 N4 1.488(6) . ? C31 H31A 0.9700 . ? C31 H31B 0.9700 . ? N1 C14 1.455(5) 2_766 ? O4 O4' 0.773(13) . ? O6 H6A 0.8200 . ? O8 Ni1 2.033(2) 1_445 ? O1W H1A 0.895(10) . ? O1W H1B 0.892(10) . ? O2W H2A 0.808(18) . ? O2W H2B 0.804(18) . ? O3W H3A 0.904(10) . ? O3W H3B 0.901(10) . ? N3 H32 0.881(10) . ? N4 C25 1.504(5) 2_667 ? N4 H33 0.887(10) . ? O5W H5A 0.904(10) . ? O5W H5B 0.900(10) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Ni1 O1 180.000(1) 2_876 . ? O1 Ni1 O8 87.46(11) 2_876 1_665 ? O1 Ni1 O8 92.54(11) . 1_665 ? O1 Ni1 O8 92.54(11) 2_876 2_766 ? O1 Ni1 O8 87.46(11) . 2_766 ? O8 Ni1 O8 180.000(1) 1_665 2_766 ? O1 Ni1 O1W 88.90(11) 2_876 2_876 ? O1 Ni1 O1W 91.10(11) . 2_876 ? O8 Ni1 O1W 94.02(10) 1_665 2_876 ? O8 Ni1 O1W 85.98(10) 2_766 2_876 ? O1 Ni1 O1W 91.10(11) 2_876 . ? O1 Ni1 O1W 88.90(11) . . ? O8 Ni1 O1W 85.98(10) 1_665 . ? O8 Ni1 O1W 94.02(10) 2_766 . ? O1W Ni1 O1W 180.000(1) 2_876 . ? N4 Ni2 N4 180.000(1) . 2_667 ? N4 Ni2 N3 86.04(14) . . ? N4 Ni2 N3 93.96(14) 2_667 . ? N4 Ni2 N3 93.96(14) . 2_667 ? N4 Ni2 N3 86.04(14) 2_667 2_667 ? N3 Ni2 N3 180.000(1) . 2_667 ? O3W Ni3 O3W 180.000(1) 2_777 . ? O3W Ni3 O3 92.11(14) 2_777 . ? O3W Ni3 O3 87.89(14) . . ? O3W Ni3 O3 87.89(14) 2_777 2_777 ? O3W Ni3 O3 92.11(14) . 2_777 ? O3 Ni3 O3 180.000(1) . 2_777 ? O3W Ni3 O2W 88.23(14) 2_777 2_777 ? O3W Ni3 O2W 91.77(14) . 2_777 ? O3 Ni3 O2W 91.24(12) . 2_777 ? O3 Ni3 O2W 88.76(12) 2_777 2_777 ? O3W Ni3 O2W 91.77(14) 2_777 . ? O3W Ni3 O2W 88.23(14) . . ? O3 Ni3 O2W 88.76(12) . . ? O3 Ni3 O2W 91.24(12) 2_777 . ? O2W Ni3 O2W 180.000(1) 2_777 . ? C2 C1 C6 118.8(4) . . ? C2 C1 C7 118.5(3) . . ? C6 C1 C7 122.7(3) . . ? C3 C2 C1 121.3(3) . . ? C3 C2 H2 119.3 . . ? C1 C2 H2 119.3 . . ? C2 C3 C4 119.0(3) . . ? C2 C3 C8 119.9(3) . . ? C4 C3 C8 121.1(4) . . ? C5 C4 C3 120.6(4) . . ? C5 C4 H4 119.7 . . ? C3 C4 H4 119.7 . . ? C4 C5 C6 119.7(3) . . ? C4 C5 C9 120.1(4) . . ? C6 C5 C9 120.2(3) . . ? C5 C6 C1 120.6(3) . . ? C5 C6 H6 119.7 . . ? C1 C6 H6 119.7 . . ? O2 C7 O1 125.1(4) . . ? O2 C7 C1 119.6(3) . . ? O1 C7 C1 115.2(3) . . ? O3 C8 O4' 123.6(5) . . ? O3 C8 O4 118.8(7) . . ? O4' C8 O4 35.0(6) . . ? O3 C8 C3 118.9(4) . . ? O4' C8 C3 116.3(5) . . ? O4 C8 C3 116.5(7) . . ? N1 C9 C5 112.0(3) . . ? N1 C9 H9A 109.2 . . ? C5 C9 H9A 109.2 . . ? N1 C9 H9B 109.2 . . ? C5 C9 H9B 109.2 . . ? H9A C9 H9B 107.9 . . ? N1 C10 C11 110.4(3) . . ? N1 C10 H10A 109.6 . . ? C11 C10 H10A 109.6 . . ? N1 C10 H10B 109.6 . . ? C11 C10 H10B 109.6 . . ? H10A C10 H10B 108.1 . . ? N2 C11 C10 113.5(3) . . ? N2 C11 H11A 108.9 . . ? C10 C11 H11A 108.9 . . ? N2 C11 H11B 108.9 . . ? C10 C11 H11B 108.9 . . ? H11A C11 H11B 107.7 . . ? C13 C12 N2 112.8(3) . . ? C13 C12 H12A 109.0 . . ? N2 C12 H12A 109.0 . . ? C13 C12 H12B 109.0 . . ? N2 C12 H12B 109.0 . . ? H12A C12 H12B 107.8 . . ? C12 C13 C14 111.4(3) . . ? C12 C13 H13A 109.3 . . ? C14 C13 H13A 109.3 . . ? C12 C13 H13B 109.3 . . ? C14 C13 H13B 109.3 . . ? H13A C13 H13B 108.0 . . ? N1 C14 C13 112.8(3) 2_766 . ? N1 C14 H14A 109.0 2_766 . ? C13 C14 H14A 109.0 . . ? N1 C14 H14B 109.0 2_766 . ? C13 C14 H14B 109.0 . . ? H14A C14 H14B 107.8 . . ? N2 C15 C16 113.7(3) . . ? N2 C15 H15A 108.8 . . ? C16 C15 H15A 108.8 . . ? N2 C15 H15B 108.8 . . ? C16 C15 H15B 108.8 . . ? H15A C15 H15B 107.7 . . ? C17 C16 C21 119.0(3) . . ? C17 C16 C15 121.0(3) . . ? C21 C16 C15 119.8(3) . . ? C16 C17 C18 120.9(3) . . ? C16 C17 H17 119.6 . . ? C18 C17 H17 119.6 . . ? C19 C18 C17 119.2(3) . . ? C19 C18 C22 118.3(3) . . ? C17 C18 C22 122.4(3) . . ? C20 C19 C18 120.6(3) . . ? C20 C19 H19 119.7 . . ? C18 C19 H19 119.7 . . ? C19 C20 C21 119.5(3) . . ? C19 C20 C23 118.8(3) . . ? C21 C20 C23 121.4(3) . . ? C16 C21 C20 120.8(3) . . ? C16 C21 H21 119.6 . . ? C20 C21 H21 119.6 . . ? O5 C22 O6 124.7(4) . . ? O5 C22 C18 118.1(4) . . ? O6 C22 C18 117.1(3) . . ? O8 C23 O7 127.1(3) . . ? O8 C23 C20 115.0(3) . . ? O7 C23 C20 117.8(3) . . ? C25 C24 H24A 109.5 . . ? C25 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C25 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? N4 C25 C27 107.1(3) 2_667 . ? N4 C25 C24 109.4(4) 2_667 . ? C27 C25 C24 111.9(4) . . ? N4 C25 C26 110.3(4) 2_667 . ? C27 C25 C26 108.2(4) . . ? C24 C25 C26 110.0(4) . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C28 C27 C25 117.9(4) . . ? C28 C27 H27A 107.8 . . ? C25 C27 H27A 107.8 . . ? C28 C27 H27B 107.8 . . ? C25 C27 H27B 107.8 . . ? H27A C27 H27B 107.2 . . ? C27 C28 N3 110.7(3) . . ? C27 C28 C29 109.9(4) . . ? N3 C28 C29 111.9(4) . . ? C27 C28 H28 108.1 . . ? N3 C28 H28 108.1 . . ? C29 C28 H28 108.1 . . ? C28 C29 H29A 109.5 . . ? C28 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C28 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? N3 C30 C31 108.0(4) . . ? N3 C30 H30A 110.1 . . ? C31 C30 H30A 110.1 . . ? N3 C30 H30B 110.1 . . ? C31 C30 H30B 110.1 . . ? H30A C30 H30B 108.4 . . ? C30 C31 N4 107.0(3) . . ? C30 C31 H31A 110.3 . . ? N4 C31 H31A 110.3 . . ? C30 C31 H31B 110.3 . . ? N4 C31 H31B 110.3 . . ? H31A C31 H31B 108.6 . . ? C14 N1 C10 111.5(3) 2_766 . ? C14 N1 C9 109.5(3) 2_766 . ? C10 N1 C9 111.0(3) . . ? C12 N2 C15 111.8(3) . . ? C12 N2 C11 113.6(3) . . ? C15 N2 C11 109.6(3) . . ? C7 O1 Ni1 127.4(3) . . ? C8 O3 Ni3 125.2(3) . . ? O4' O4 C8 71.1(12) . . ? O4 O4' C8 73.8(13) . . ? C22 O6 H6A 109.5 . . ? C23 O8 Ni1 129.2(2) . 1_445 ? Ni1 O1W H1A 98(3) . . ? Ni1 O1W H1B 97(3) . . ? H1A O1W H1B 107.2(16) . . ? Ni3 O2W H2A 119(4) . . ? Ni3 O2W H2B 94(4) . . ? H2A O2W H2B 126(3) . . ? Ni3 O3W H3A 119(3) . . ? Ni3 O3W H3B 127(3) . . ? H3A O3W H3B 105.8(16) . . ? C30 N3 C28 110.1(3) . . ? C30 N3 Ni2 107.2(3) . . ? C28 N3 Ni2 122.2(3) . . ? C30 N3 H32 104(3) . . ? C28 N3 H32 108(3) . . ? Ni2 N3 H32 104(3) . . ? C31 N4 C25 112.6(3) . 2_667 ? C31 N4 Ni2 109.1(3) . . ? C25 N4 Ni2 119.9(3) 2_667 . ? C31 N4 H33 107(3) . . ? C25 N4 H33 101(3) 2_667 . ? Ni2 N4 H33 105(3) . . ? H5A O5W H5B 105.4(16) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C6 C1 C2 C3 1.8(6) . . . . ? C7 C1 C2 C3 179.4(4) . . . . ? C1 C2 C3 C4 -0.8(6) . . . . ? C1 C2 C3 C8 179.4(4) . . . . ? C2 C3 C4 C5 -0.7(6) . . . . ? C8 C3 C4 C5 179.1(4) . . . . ? C3 C4 C5 C6 1.2(6) . . . . ? C3 C4 C5 C9 -175.9(4) . . . . ? C4 C5 C6 C1 -0.1(6) . . . . ? C9 C5 C6 C1 177.0(4) . . . . ? C2 C1 C6 C5 -1.3(6) . . . . ? C7 C1 C6 C5 -178.8(4) . . . . ? C2 C1 C7 O2 176.5(4) . . . . ? C6 C1 C7 O2 -6.0(6) . . . . ? C2 C1 C7 O1 -3.0(5) . . . . ? C6 C1 C7 O1 174.5(4) . . . . ? C2 C3 C8 O3 -155.7(5) . . . . ? C4 C3 C8 O3 24.5(7) . . . . ? C2 C3 C8 O4' 36.6(8) . . . . ? C4 C3 C8 O4' -143.3(6) . . . . ? C2 C3 C8 O4 -2.7(10) . . . . ? C4 C3 C8 O4 177.5(8) . . . . ? C4 C5 C9 N1 -137.6(4) . . . . ? C6 C5 C9 N1 45.4(5) . . . . ? N1 C10 C11 N2 157.3(3) . . . . ? N2 C12 C13 C14 -179.6(3) . . . . ? C12 C13 C14 N1 -59.5(4) . . . 2_766 ? N2 C15 C16 C17 -82.2(5) . . . . ? N2 C15 C16 C21 103.6(4) . . . . ? C21 C16 C17 C18 -1.6(6) . . . . ? C15 C16 C17 C18 -175.8(4) . . . . ? C16 C17 C18 C19 -0.1(6) . . . . ? C16 C17 C18 C22 176.6(4) . . . . ? C17 C18 C19 C20 1.8(6) . . . . ? C22 C18 C19 C20 -175.1(4) . . . . ? C18 C19 C20 C21 -1.8(6) . . . . ? C18 C19 C20 C23 172.1(4) . . . . ? C17 C16 C21 C20 1.6(6) . . . . ? C15 C16 C21 C20 175.9(4) . . . . ? C19 C20 C21 C16 0.1(6) . . . . ? C23 C20 C21 C16 -173.6(3) . . . . ? C19 C18 C22 O5 -177.1(4) . . . . ? C17 C18 C22 O5 6.1(7) . . . . ? C19 C18 C22 O6 2.4(6) . . . . ? C17 C18 C22 O6 -174.3(4) . . . . ? C19 C20 C23 O8 -136.4(4) . . . . ? C21 C20 C23 O8 37.3(5) . . . . ? C19 C20 C23 O7 41.6(5) . . . . ? C21 C20 C23 O7 -144.7(4) . . . . ? N4 C25 C27 C28 70.8(5) 2_667 . . . ? C24 C25 C27 C28 -49.0(5) . . . . ? C26 C25 C27 C28 -170.3(4) . . . . ? C25 C27 C28 N3 -64.3(5) . . . . ? C25 C27 C28 C29 171.6(4) . . . . ? N3 C30 C31 N4 51.8(5) . . . . ? C11 C10 N1 C14 -166.0(3) . . . 2_766 ? C11 C10 N1 C9 71.6(4) . . . . ? C5 C9 N1 C14 77.0(4) . . . 2_766 ? C5 C9 N1 C10 -159.4(3) . . . . ? C13 C12 N2 C15 169.2(3) . . . . ? C13 C12 N2 C11 -66.2(4) . . . . ? C16 C15 N2 C12 -64.6(4) . . . . ? C16 C15 N2 C11 168.5(3) . . . . ? C10 C11 N2 C12 -66.9(4) . . . . ? C10 C11 N2 C15 59.0(4) . . . . ? O2 C7 O1 Ni1 -28.8(6) . . . . ? C1 C7 O1 Ni1 150.6(3) . . . . ? O1 Ni1 O1 C7 -147(100) 2_876 . . . ? O8 Ni1 O1 C7 134.7(3) 1_665 . . . ? O8 Ni1 O1 C7 -45.3(3) 2_766 . . . ? O1W Ni1 O1 C7 40.6(3) 2_876 . . . ? O1W Ni1 O1 C7 -139.4(3) . . . . ? O4' C8 O3 Ni3 -21.0(9) . . . . ? O4 C8 O3 Ni3 19.9(10) . . . . ? C3 C8 O3 Ni3 172.2(3) . . . . ? O3W Ni3 O3 C8 -49.2(4) 2_777 . . . ? O3W Ni3 O3 C8 130.8(4) . . . . ? O3 Ni3 O3 C8 176(100) 2_777 . . . ? O2W Ni3 O3 C8 39.1(4) 2_777 . . . ? O2W Ni3 O3 C8 -140.9(4) . . . . ? O3 C8 O4 O4' -108.4(14) . . . . ? C3 C8 O4 O4' 98.6(14) . . . . ? O3 C8 O4' O4 93.5(15) . . . . ? C3 C8 O4' O4 -99.4(14) . . . . ? O7 C23 O8 Ni1 17.6(6) . . . 1_445 ? C20 C23 O8 Ni1 -164.6(2) . . . 1_445 ? C31 C30 N3 C28 -178.8(4) . . . . ? C31 C30 N3 Ni2 -43.9(4) . . . . ? C27 C28 N3 C30 172.7(4) . . . . ? C29 C28 N3 C30 -64.4(5) . . . . ? C27 C28 N3 Ni2 45.8(5) . . . . ? C29 C28 N3 Ni2 168.7(3) . . . . ? N4 Ni2 N3 C30 19.4(3) . . . . ? N4 Ni2 N3 C30 -160.6(3) 2_667 . . . ? N3 Ni2 N3 C30 100(100) 2_667 . . . ? N4 Ni2 N3 C28 147.6(3) . . . . ? N4 Ni2 N3 C28 -32.4(3) 2_667 . . . ? N3 Ni2 N3 C28 -132(100) 2_667 . . . ? C30 C31 N4 C25 -170.3(4) . . . 2_667 ? C30 C31 N4 Ni2 -34.7(4) . . . . ? N4 Ni2 N4 C31 -101(100) 2_667 . . . ? N3 Ni2 N4 C31 8.7(3) . . . . ? N3 Ni2 N4 C31 -171.3(3) 2_667 . . . ? N4 Ni2 N4 C25 31(100) 2_667 . . 2_667 ? N3 Ni2 N4 C25 140.6(3) . . . 2_667 ? N3 Ni2 N4 C25 -39.4(3) 2_667 . . 2_667 ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O6 H6A O3W 0.82 2.62 3.289(5) 140.2 2_676 O1W H1A O2 0.895(10) 1.875(19) 2.736(4) 161(4) 2_876 O1W H1B O7 0.892(10) 1.869(16) 2.720(4) 159(4) 2_766 _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.614 _refine_diff_density_min -1.286 _refine_diff_density_rms 0.089 #=========================END data_Compound-9 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C110 H188 Cd4 N20 O18, H2O' _chemical_formula_sum 'C110 H190 Cd4 N20 O19' _chemical_formula_weight 2546.42 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cd' 'Cd' -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P b c a' _symmetry_space_group_name_hall '-P 2ac 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' '-x-1/2, y-1/2, z' 'x, -y-1/2, z-1/2' _cell_length_a 18.1000(5) _cell_length_b 23.3079(7) _cell_length_c 29.0723(11) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 12264.8(7) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 11361 _cell_measurement_theta_min 2.7860 _cell_measurement_theta_max 29.2058 _exptl_crystal_description strip _exptl_crystal_colour colorless _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.379 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5336 _exptl_absorpt_coefficient_mu 0.754 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8398 _exptl_absorpt_correction_T_max 0.8889 _exptl_absorpt_process_details ; CrysAlis (Oxford Diffraction, 2006) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Diffraction Gemini R Ultra' _diffrn_measurement_method '\w scan' _diffrn_detector_area_resol_mean 10.0 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 46239 _diffrn_reflns_av_R_equivalents 0.0599 _diffrn_reflns_av_sigmaI/netI 0.0592 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -35 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_theta_min 2.79 _diffrn_reflns_theta_max 25.35 _reflns_number_total 11201 _reflns_number_gt 7046 _reflns_threshold_expression >2\s(I) _computing_data_collection 'CrysAlisPro(1.171.35.21) (Agilent Tech., 2012)' _computing_cell_refinement 'CrysAlisPro(1.171.35.21) (Agilent Tech., 2012)' _computing_data_reduction 'CrysAlisPro(1.171.35.21) (Agilent Tech., 2012)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0395P)^2^+6.8722P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11201 _refine_ls_number_parameters 724 _refine_ls_number_restraints 9 _refine_ls_R_factor_all 0.0871 _refine_ls_R_factor_gt 0.0426 _refine_ls_wR_factor_ref 0.1029 _refine_ls_wR_factor_gt 0.0869 _refine_ls_goodness_of_fit_ref 1.008 _refine_ls_restrained_S_all 1.009 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cd1 Cd 0.515129(16) 0.329884(12) 0.001242(12) 0.04221(10) Uani 1 1 d . . . Cd2 Cd 0.573272(15) 0.201195(13) 0.219141(11) 0.04438(10) Uani 1 1 d . . . C1 C 0.6857(2) 0.33655(19) 0.00224(17) 0.0544(12) Uani 1 1 d . . . H1A H 0.7309 0.3417 -0.0153 0.065 Uiso 1 1 calc R . . H1B H 0.6978 0.3148 0.0297 0.065 Uiso 1 1 calc R . . C2 C 0.6561(2) 0.39437(18) 0.01601(17) 0.0543(12) Uani 1 1 d . . . H2A H 0.6940 0.4156 0.0324 0.065 Uiso 1 1 calc R . . H2B H 0.6430 0.4160 -0.0113 0.065 Uiso 1 1 calc R . . C3 C 0.5564(2) 0.44192(17) 0.06124(18) 0.0545(12) Uani 1 1 d . . . H3 H 0.5378 0.4627 0.0343 0.065 Uiso 1 1 calc R . . C4 C 0.4912(2) 0.4286(2) 0.09322(18) 0.0608(13) Uani 1 1 d . . . H4A H 0.5078 0.3993 0.1145 0.073 Uiso 1 1 calc R . . H4B H 0.4822 0.4629 0.1113 0.073 Uiso 1 1 calc R . . C5 C 0.4166(2) 0.40906(19) 0.07439(17) 0.0557(12) Uani 1 1 d . . . C6 C 0.4252(2) 0.30212(18) 0.08976(17) 0.0572(12) Uani 1 1 d . . . H6A H 0.3775 0.2980 0.1046 0.069 Uiso 1 1 calc R . . H6B H 0.4613 0.3117 0.1132 0.069 Uiso 1 1 calc R . . C7 C 0.4464(2) 0.24622(19) 0.06729(18) 0.0581(13) Uani 1 1 d . . . H7A H 0.4429 0.2152 0.0894 0.070 Uiso 1 1 calc R . . H7B H 0.4130 0.2380 0.0420 0.070 Uiso 1 1 calc R . . C8 C 0.5526(2) 0.19820(17) 0.02943(15) 0.0484(11) Uani 1 1 d . . . H8 H 0.5224 0.1885 0.0026 0.058 Uiso 1 1 calc R . . C9 C 0.6317(2) 0.20758(19) 0.01318(16) 0.0538(12) Uani 1 1 d . . . H9A H 0.6539 0.1700 0.0096 0.065 Uiso 1 1 calc R . . H9B H 0.6579 0.2265 0.0380 0.065 Uiso 1 1 calc R . . C10 C 0.6481(2) 0.2413(2) -0.03082(16) 0.0546(12) Uani 1 1 d . . . C11 C 0.6112(3) 0.4805(2) 0.0867(2) 0.0881(19) Uani 1 1 d . . . H11A H 0.6516 0.4897 0.0667 0.132 Uiso 1 1 calc R . . H11B H 0.6294 0.4608 0.1134 0.132 Uiso 1 1 calc R . . H11C H 0.5867 0.5152 0.0960 0.132 Uiso 1 1 calc R . . C12 C 0.3613(3) 0.4119(2) 0.1139(2) 0.0785(17) Uani 1 1 d . . . H12A H 0.3777 0.3875 0.1385 0.118 Uiso 1 1 calc R . . H12B H 0.3138 0.3991 0.1033 0.118 Uiso 1 1 calc R . . H12C H 0.3576 0.4507 0.1247 0.118 Uiso 1 1 calc R . . C13 C 0.3914(3) 0.4472(2) 0.03554(19) 0.0715(15) Uani 1 1 d . . . H13A H 0.4267 0.4456 0.0109 0.107 Uiso 1 1 calc R . . H13B H 0.3873 0.4860 0.0464 0.107 Uiso 1 1 calc R . . H13C H 0.3442 0.4344 0.0246 0.107 Uiso 1 1 calc R . . C14 C 0.5506(3) 0.1479(2) 0.06228(19) 0.0761(15) Uani 1 1 d U . . H14A H 0.5006 0.1413 0.0720 0.114 Uiso 1 1 calc R . . H14B H 0.5808 0.1561 0.0886 0.114 Uiso 1 1 calc R . . H14C H 0.5690 0.1142 0.0471 0.114 Uiso 1 1 calc R . . C15 C 0.6017(3) 0.2212(2) -0.07061(17) 0.0731(15) Uani 1 1 d . . . H15A H 0.6132 0.2437 -0.0974 0.110 Uiso 1 1 calc R . . H15B H 0.5504 0.2257 -0.0631 0.110 Uiso 1 1 calc R . . H15C H 0.6119 0.1815 -0.0767 0.110 Uiso 1 1 calc R . . C16 C 0.7306(3) 0.2316(2) -0.0426(2) 0.0828(17) Uani 1 1 d . . . H16A H 0.7607 0.2444 -0.0174 0.124 Uiso 1 1 calc R . . H16B H 0.7430 0.2529 -0.0698 0.124 Uiso 1 1 calc R . . H16C H 0.7391 0.1915 -0.0479 0.124 Uiso 1 1 calc R . . C17 C 0.7293(3) 0.1518(2) 0.2440(2) 0.0742(16) Uani 1 1 d . . . H17A H 0.7760 0.1361 0.2336 0.089 Uiso 1 1 calc R . . H17B H 0.7201 0.1373 0.2748 0.089 Uiso 1 1 calc R . . C18 C 0.7350(2) 0.2158(3) 0.24577(19) 0.0723(16) Uani 1 1 d . . . H18A H 0.7772 0.2268 0.2644 0.087 Uiso 1 1 calc R . . H18B H 0.7424 0.2308 0.2150 0.087 Uiso 1 1 calc R . . C19 C 0.6654(3) 0.3032(2) 0.2691(2) 0.0775(16) Uani 1 1 d . . . H19 H 0.6640 0.3188 0.2378 0.093 Uiso 1 1 calc R . . C20 C 0.5952(3) 0.3225(2) 0.2942(2) 0.0823(17) Uani 1 1 d . . . H20A H 0.5919 0.2999 0.3221 0.099 Uiso 1 1 calc R . . H20B H 0.6031 0.3619 0.3036 0.099 Uiso 1 1 calc R . . C21 C 0.5194(3) 0.3202(2) 0.27124(19) 0.0720(15) Uani 1 1 d . . . C22 C 0.4722(3) 0.2280(3) 0.30390(19) 0.0770(16) Uani 1 1 d . . . H22A H 0.4262 0.2437 0.3154 0.092 Uiso 1 1 calc R . . H22B H 0.5092 0.2323 0.3278 0.092 Uiso 1 1 calc R . . C23 C 0.4620(3) 0.1658(3) 0.2937(2) 0.0782(17) Uani 1 1 d . . . H23A H 0.4433 0.1464 0.3208 0.094 Uiso 1 1 calc R . . H23B H 0.4260 0.1613 0.2693 0.094 Uiso 1 1 calc R . . C24 C 0.5288(3) 0.0789(2) 0.2674(2) 0.0832(18) Uani 1 1 d . . . H24 H 0.5016 0.0754 0.2384 0.100 Uiso 1 1 calc R . . C25 C 0.6071(4) 0.0563(2) 0.2598(2) 0.092(2) Uani 1 1 d . . . H25A H 0.6364 0.0692 0.2857 0.110 Uiso 1 1 calc R . . H25B H 0.6044 0.0148 0.2619 0.110 Uiso 1 1 calc R . . C26 C 0.6508(3) 0.0699(2) 0.2169(2) 0.0790(17) Uani 1 1 d . . . C27 C 0.7316(4) 0.3286(3) 0.2934(3) 0.150(4) Uani 1 1 d . . . H27A H 0.7759 0.3177 0.2775 0.225 Uiso 1 1 calc R . . H27B H 0.7334 0.3145 0.3244 0.225 Uiso 1 1 calc R . . H27C H 0.7274 0.3697 0.2938 0.225 Uiso 1 1 calc R . . C28 C 0.4639(4) 0.3518(3) 0.3025(2) 0.114(2) Uani 1 1 d . . . H28A H 0.4159 0.3511 0.2885 0.171 Uiso 1 1 calc R . . H28B H 0.4795 0.3909 0.3064 0.171 Uiso 1 1 calc R . . H28C H 0.4619 0.3332 0.3319 0.171 Uiso 1 1 calc R . . C29 C 0.5179(4) 0.3493(3) 0.2238(2) 0.096(2) Uani 1 1 d . . . H29A H 0.4692 0.3463 0.2109 0.144 Uiso 1 1 calc R . . H29B H 0.5526 0.3306 0.2037 0.144 Uiso 1 1 calc R . . H29C H 0.5310 0.3890 0.2270 0.144 Uiso 1 1 calc R . . C30 C 0.4916(5) 0.0421(3) 0.3024(3) 0.147(3) Uani 1 1 d . . . H30A H 0.4421 0.0555 0.3072 0.220 Uiso 1 1 calc R . . H30B H 0.5185 0.0439 0.3308 0.220 Uiso 1 1 calc R . . H30C H 0.4903 0.0031 0.2916 0.220 Uiso 1 1 calc R . . C31 C 0.6061(3) 0.0563(3) 0.1735(2) 0.097(2) Uani 1 1 d . . . H31A H 0.6348 0.0656 0.1468 0.146 Uiso 1 1 calc R . . H31B H 0.5614 0.0785 0.1735 0.146 Uiso 1 1 calc R . . H31C H 0.5940 0.0161 0.1731 0.146 Uiso 1 1 calc R . . C32 C 0.7217(4) 0.0325(3) 0.2151(3) 0.134(3) Uani 1 1 d . . . H32A H 0.7488 0.0412 0.1876 0.202 Uiso 1 1 calc R . . H32B H 0.7082 -0.0073 0.2151 0.202 Uiso 1 1 calc R . . H32C H 0.7519 0.0406 0.2415 0.202 Uiso 1 1 calc R . . C33 C 0.3422(2) 0.24385(17) -0.08773(14) 0.0399(10) Uani 1 1 d . . . C34 C 0.2740(2) 0.25414(17) -0.10771(14) 0.0408(10) Uani 1 1 d . . . H34 H 0.2577 0.2916 -0.1117 0.049 Uiso 1 1 calc R . . C35 C 0.2303(2) 0.20899(17) -0.12164(14) 0.0381(10) Uani 1 1 d . . . C36 C 0.2563(2) 0.15343(18) -0.11741(15) 0.0440(11) Uani 1 1 d . . . H36 H 0.2266 0.1230 -0.1267 0.053 Uiso 1 1 calc R . . C37 C 0.3257(2) 0.14244(18) -0.09966(15) 0.0463(11) Uani 1 1 d . . . C38 C 0.3667(2) 0.18823(18) -0.08375(16) 0.0479(11) Uani 1 1 d . . . H38 H 0.4121 0.1813 -0.0699 0.058 Uiso 1 1 calc R . . C39 C 0.3880(2) 0.29121(19) -0.06885(17) 0.0489(11) Uani 1 1 d . . . C40 C 0.1516(2) 0.2197(2) -0.13818(15) 0.0430(10) Uani 1 1 d . . . C41 C 0.3569(3) 0.08275(19) -0.10007(19) 0.0657(15) Uani 1 1 d . . . H41A H 0.3173 0.0557 -0.0940 0.079 Uiso 1 1 calc R . . H41B H 0.3762 0.0746 -0.1305 0.079 Uiso 1 1 calc R . . C42 C 0.3870(3) 0.0609(2) -0.0216(2) 0.0750(16) Uani 1 1 d . . . H42A H 0.3491 0.0887 -0.0139 0.090 Uiso 1 1 calc R . . H42B H 0.4266 0.0652 0.0007 0.090 Uiso 1 1 calc R . . C43 C 0.3552(3) 0.0020(2) -0.0169(2) 0.0833(17) Uani 1 1 d . . . H43A H 0.3907 -0.0258 -0.0283 0.100 Uiso 1 1 calc R . . H43B H 0.3112 -0.0008 -0.0359 0.100 Uiso 1 1 calc R . . C44 C 0.3354(3) -0.0129(2) 0.0318(2) 0.0830(18) Uani 1 1 d . . . H44A H 0.2969 0.0130 0.0421 0.100 Uiso 1 1 calc R . . H44B H 0.3153 -0.0515 0.0324 0.100 Uiso 1 1 calc R . . C45 C 0.3669(3) -0.0120(2) 0.1109(2) 0.0676(15) Uani 1 1 d . . . H45A H 0.4054 -0.0240 0.1320 0.081 Uiso 1 1 calc R . . H45B H 0.3271 -0.0398 0.1125 0.081 Uiso 1 1 calc R . . C46 C 0.3386(2) 0.0458(2) 0.12477(18) 0.0607(13) Uani 1 1 d . . . C47 C 0.2649(2) 0.0603(2) 0.12063(17) 0.0581(13) Uani 1 1 d . . . H47 H 0.2313 0.0329 0.1105 0.070 Uiso 1 1 calc R . . C48 C 0.2401(2) 0.1149(2) 0.13127(15) 0.0470(11) Uani 1 1 d . . . C49 C 0.2902(2) 0.15470(19) 0.14681(15) 0.0473(11) Uani 1 1 d . . . H49 H 0.2743 0.1917 0.1536 0.057 Uiso 1 1 calc R . . C50 C 0.3644(2) 0.14067(19) 0.15257(16) 0.0477(11) Uani 1 1 d . . . C51 C 0.3873(2) 0.0866(2) 0.14093(17) 0.0556(13) Uani 1 1 d . . . H51 H 0.4370 0.0772 0.1440 0.067 Uiso 1 1 calc R . . C52 C 0.1591(2) 0.1286(2) 0.12651(17) 0.0538(12) Uani 1 1 d . . . C53 C 0.4174(2) 0.1834(2) 0.17363(16) 0.0511(12) Uani 1 1 d . . . C54 C 0.4771(3) 0.0392(2) -0.0816(2) 0.0772(16) Uani 1 1 d . . . H54A H 0.4841 0.0448 -0.1144 0.093 Uiso 1 1 calc R . . H54B H 0.4654 -0.0009 -0.0766 0.093 Uiso 1 1 calc R . . C55 C 0.5488(3) 0.0536(2) -0.0566(2) 0.0816(17) Uani 1 1 d . . . H55A H 0.5674 0.0902 -0.0676 0.098 Uiso 1 1 calc R . . H55B H 0.5392 0.0571 -0.0239 0.098 Uiso 1 1 calc R . . N9 N 0.4155(2) 0.07401(16) -0.06634(17) 0.0671(12) Uani 1 1 d . . . N10 N 0.3963(2) -0.00999(16) 0.06408(17) 0.0631(11) Uani 1 1 d . . . O1 O 0.43631(18) 0.27743(13) -0.04076(13) 0.0742(11) Uani 1 1 d . . . O2 O 0.37669(18) 0.34071(14) -0.08229(15) 0.0813(12) Uani 1 1 d . . . O3 O 0.13961(15) 0.26638(13) -0.15671(12) 0.0600(9) Uani 1 1 d . . . O4 O 0.10619(16) 0.18215(14) -0.13031(12) 0.0657(10) Uani 1 1 d . . . O5 O 0.48355(15) 0.16626(14) 0.17555(11) 0.0580(8) Uani 1 1 d . . . O6 O 0.39327(17) 0.22952(15) 0.18730(12) 0.0657(9) Uani 1 1 d . . . O7 O 0.13679(16) 0.17342(16) 0.14405(13) 0.0723(10) Uani 1 1 d . . . O8 O 0.12074(17) 0.09354(17) 0.10504(13) 0.0810(12) Uani 1 1 d . . . O2W O 0.7595(5) 0.0948(3) 0.1046(6) 0.208(8) Uani 0.50 1 d P . . O1W O 0.50049(15) 0.39898(13) -0.05580(11) 0.0504(8) Uani 1 1 d D . . H1D H 0.5375(15) 0.400(2) -0.0750(11) 0.076 Uiso 1 1 d D . . H1C H 0.4627(14) 0.3841(18) -0.0695(13) 0.076 Uiso 1 1 d D . . N1 N 0.63251(19) 0.30381(16) -0.02550(13) 0.0470(10) Uani 1 1 d . . . H1E H 0.632(3) 0.318(2) -0.0510(18) 0.071 Uiso 1 1 d . . . N2 N 0.59092(19) 0.38797(14) 0.04547(14) 0.0452(9) Uani 1 1 d . . . H2E H 0.602(3) 0.368(2) 0.0691(17) 0.068 Uiso 1 1 d . . . N3 N 0.42156(19) 0.34919(16) 0.05538(15) 0.0522(10) Uani 1 1 d . . . H3E H 0.387(3) 0.345(2) 0.0412(19) 0.078 Uiso 1 1 d . . . N4 N 0.52250(19) 0.25054(15) 0.05006(14) 0.0446(9) Uani 1 1 d . . . H4E H 0.546(3) 0.260(2) 0.0708(17) 0.067 Uiso 1 1 d . . . N5 N 0.6695(2) 0.1318(2) 0.21291(15) 0.0623(12) Uani 1 1 d . . . H5E H 0.691(3) 0.144(3) 0.192(2) 0.093 Uiso 1 1 d . . . N6 N 0.6666(2) 0.24060(18) 0.26571(14) 0.0572(11) Uani 1 1 d . . . H6E H 0.657(3) 0.222(2) 0.2903(19) 0.086 Uiso 1 1 d . . . N7 N 0.4952(2) 0.2601(2) 0.26313(15) 0.0616(12) Uani 1 1 d . . . H7E H 0.463(3) 0.260(3) 0.246(2) 0.092 Uiso 1 1 d . . . N8 N 0.5323(2) 0.13945(19) 0.27964(15) 0.0615(11) Uani 1 1 d . . . H8E H 0.563(3) 0.148(2) 0.299(2) 0.092 Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cd1 0.03396(16) 0.04374(17) 0.0489(2) 0.00482(16) -0.00573(14) -0.00212(13) Cd2 0.03183(16) 0.0595(2) 0.0419(2) 0.00119(16) 0.00320(14) -0.00389(14) C1 0.034(2) 0.067(3) 0.062(3) 0.004(3) 0.000(2) -0.003(2) C2 0.046(3) 0.052(3) 0.065(4) 0.002(2) -0.005(2) -0.012(2) C3 0.055(3) 0.037(2) 0.071(4) -0.002(2) -0.011(3) 0.003(2) C4 0.063(3) 0.054(3) 0.065(4) -0.007(3) -0.002(3) 0.013(2) C5 0.051(3) 0.054(3) 0.062(3) 0.001(2) 0.005(2) 0.016(2) C6 0.046(3) 0.059(3) 0.067(3) 0.013(3) 0.012(2) 0.007(2) C7 0.047(3) 0.056(3) 0.072(4) 0.018(3) 0.005(2) -0.005(2) C8 0.067(3) 0.037(2) 0.040(3) 0.002(2) 0.002(2) 0.002(2) C9 0.061(3) 0.050(3) 0.051(3) 0.000(2) -0.003(2) 0.014(2) C10 0.057(3) 0.063(3) 0.043(3) -0.005(2) 0.002(2) 0.011(2) C11 0.081(4) 0.056(3) 0.128(6) -0.031(3) -0.010(4) -0.001(3) C12 0.063(3) 0.088(4) 0.085(5) -0.004(3) 0.021(3) 0.023(3) C13 0.058(3) 0.067(3) 0.090(4) 0.009(3) -0.003(3) 0.021(3) C14 0.0788(17) 0.0735(17) 0.0760(18) 0.0002(10) 0.0023(10) 0.0016(10) C15 0.109(4) 0.072(3) 0.039(3) -0.006(3) 0.001(3) -0.004(3) C16 0.073(4) 0.088(4) 0.088(5) -0.001(3) 0.027(3) 0.023(3) C17 0.047(3) 0.100(4) 0.076(4) -0.011(3) -0.013(3) 0.011(3) C18 0.039(3) 0.117(5) 0.061(4) -0.005(3) -0.009(2) -0.010(3) C19 0.079(4) 0.068(3) 0.086(5) -0.004(3) -0.005(3) -0.016(3) C20 0.103(5) 0.081(4) 0.063(4) -0.013(3) -0.012(3) 0.005(3) C21 0.087(4) 0.074(4) 0.056(4) -0.005(3) 0.014(3) 0.017(3) C22 0.064(4) 0.108(5) 0.059(4) 0.005(3) 0.021(3) 0.004(3) C23 0.053(3) 0.117(5) 0.065(4) 0.032(4) 0.014(3) -0.013(3) C24 0.086(4) 0.077(4) 0.087(5) 0.018(3) -0.012(3) -0.017(3) C25 0.128(6) 0.064(4) 0.084(5) 0.003(3) -0.031(4) 0.005(4) C26 0.076(4) 0.067(4) 0.094(5) -0.014(3) -0.022(4) 0.019(3) C27 0.111(6) 0.116(6) 0.223(11) -0.047(6) -0.040(6) -0.034(5) C28 0.142(6) 0.114(5) 0.086(5) -0.035(4) 0.026(4) 0.046(5) C29 0.132(6) 0.082(4) 0.073(5) -0.001(4) 0.008(4) 0.020(4) C30 0.195(9) 0.091(5) 0.154(8) 0.036(5) 0.028(7) -0.046(5) C31 0.105(5) 0.093(4) 0.094(5) -0.028(4) -0.026(4) 0.018(4) C32 0.127(6) 0.112(5) 0.164(8) -0.033(5) -0.049(5) 0.069(5) C33 0.033(2) 0.049(2) 0.037(3) -0.001(2) -0.0027(18) 0.0017(19) C34 0.032(2) 0.049(2) 0.041(3) 0.004(2) -0.0004(19) 0.0030(19) C35 0.027(2) 0.054(3) 0.034(2) 0.002(2) -0.0003(17) 0.0023(19) C36 0.034(2) 0.052(3) 0.046(3) -0.006(2) -0.0065(19) -0.0003(19) C37 0.038(2) 0.051(3) 0.050(3) -0.010(2) -0.005(2) 0.008(2) C38 0.033(2) 0.056(3) 0.054(3) -0.005(2) -0.008(2) 0.007(2) C39 0.034(2) 0.053(3) 0.060(3) -0.002(2) -0.003(2) -0.002(2) C40 0.032(2) 0.063(3) 0.034(3) -0.003(2) -0.0019(18) 0.002(2) C41 0.061(3) 0.056(3) 0.081(4) -0.012(3) -0.026(3) 0.013(2) C42 0.069(4) 0.063(3) 0.094(5) -0.006(3) -0.005(3) 0.016(3) C43 0.084(4) 0.075(4) 0.091(5) -0.007(3) -0.004(4) 0.013(3) C44 0.064(4) 0.090(4) 0.094(5) -0.016(4) -0.004(3) 0.003(3) C45 0.045(3) 0.065(3) 0.093(5) 0.005(3) 0.000(3) 0.001(2) C46 0.035(3) 0.071(3) 0.077(4) -0.001(3) 0.003(2) 0.004(2) C47 0.036(3) 0.073(3) 0.065(4) -0.002(3) 0.001(2) -0.008(2) C48 0.034(2) 0.068(3) 0.040(3) 0.003(2) 0.0047(19) 0.001(2) C49 0.042(3) 0.059(3) 0.041(3) 0.005(2) 0.004(2) 0.005(2) C50 0.035(2) 0.062(3) 0.047(3) 0.007(2) 0.002(2) -0.001(2) C51 0.027(2) 0.073(3) 0.067(4) 0.004(3) 0.000(2) -0.001(2) C52 0.033(3) 0.088(4) 0.040(3) 0.015(3) 0.000(2) 0.010(3) C53 0.036(3) 0.074(3) 0.043(3) 0.006(2) 0.001(2) -0.007(2) C54 0.052(3) 0.084(4) 0.095(5) -0.016(3) 0.002(3) 0.014(3) C55 0.059(3) 0.071(3) 0.114(5) -0.012(3) 0.002(3) 0.012(3) N9 0.059(3) 0.063(3) 0.079(4) -0.007(2) -0.015(2) 0.025(2) N10 0.042(2) 0.064(3) 0.084(4) -0.008(2) -0.009(2) 0.0095(18) O1 0.074(2) 0.064(2) 0.084(3) 0.0097(19) -0.048(2) -0.0175(17) O2 0.058(2) 0.058(2) 0.128(4) 0.007(2) -0.040(2) -0.0063(17) O3 0.0481(19) 0.065(2) 0.067(2) 0.0107(19) -0.0221(16) 0.0068(15) O4 0.0317(16) 0.089(2) 0.076(3) 0.0239(19) -0.0114(16) -0.0127(17) O5 0.0292(16) 0.086(2) 0.059(2) -0.0048(18) -0.0010(14) -0.0080(15) O6 0.0463(19) 0.073(2) 0.078(3) -0.008(2) -0.0008(17) -0.0025(17) O7 0.0418(19) 0.086(2) 0.089(3) -0.007(2) -0.0015(18) 0.0184(17) O8 0.0365(19) 0.124(3) 0.083(3) -0.023(2) -0.0220(18) 0.0075(19) O2W 0.096(7) 0.059(5) 0.47(2) 0.019(8) 0.145(10) -0.004(5) O1W 0.0342(16) 0.0591(19) 0.058(2) 0.0112(16) -0.0026(14) -0.0002(14) N1 0.038(2) 0.054(2) 0.049(3) 0.003(2) -0.0044(18) 0.0014(17) N2 0.040(2) 0.042(2) 0.053(3) 0.0027(18) -0.0021(18) -0.0010(16) N3 0.036(2) 0.057(2) 0.063(3) 0.007(2) -0.0021(19) 0.0034(18) N4 0.044(2) 0.040(2) 0.050(3) 0.0015(18) -0.0031(17) 0.0009(16) N5 0.047(3) 0.084(3) 0.056(3) -0.004(2) -0.007(2) 0.007(2) N6 0.055(2) 0.072(3) 0.045(3) 0.002(2) -0.002(2) -0.009(2) N7 0.056(3) 0.085(3) 0.043(3) 0.001(2) 0.0108(19) 0.010(2) N8 0.063(3) 0.070(3) 0.052(3) 0.009(2) -0.001(2) -0.012(2) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cd1 O1 2.241(3) . ? Cd1 N2 2.317(4) . ? Cd1 O1W 2.327(3) . ? Cd1 N4 2.335(4) . ? Cd1 N1 2.343(4) . ? Cd1 N3 2.355(4) . ? Cd2 O5 2.215(3) . ? Cd2 O3 2.304(3) 3 ? Cd2 N7 2.348(4) . ? Cd2 N6 2.352(4) . ? Cd2 N5 2.385(4) . ? Cd2 N8 2.390(4) . ? C1 N1 1.470(5) . ? C1 C2 1.505(6) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 N2 1.466(5) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 N2 1.477(5) . ? C3 C11 1.529(6) . ? C3 C4 1.534(6) . ? C3 H3 0.9800 . ? C4 C5 1.527(6) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 N3 1.504(6) . ? C5 C13 1.508(6) . ? C5 C12 1.524(6) . ? C6 N3 1.486(6) . ? C6 C7 1.507(6) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 N4 1.469(5) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 N4 1.465(5) . ? C8 C14 1.513(6) . ? C8 C9 1.523(6) . ? C8 H8 0.9800 . ? C9 C10 1.530(6) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 N1 1.493(5) . ? C10 C15 1.504(6) . ? C10 C16 1.547(6) . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? C15 H15C 0.9600 . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C17 N5 1.485(6) . ? C17 C18 1.497(7) . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C18 N6 1.483(6) . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C19 N6 1.462(6) . ? C19 C27 1.512(8) . ? C19 C20 1.533(8) . ? C19 H19 0.9800 . ? C20 C21 1.526(8) . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C21 N7 1.486(7) . ? C21 C29 1.538(7) . ? C21 C28 1.542(7) . ? C22 N7 1.462(7) . ? C22 C23 1.490(7) . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C23 N8 1.470(7) . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C24 N8 1.457(7) . ? C24 C30 1.491(8) . ? C24 C25 1.528(8) . ? C24 H24 0.9800 . ? C25 C26 1.510(8) . ? C25 H25A 0.9700 . ? C25 H25B 0.9700 . ? C26 N5 1.485(7) . ? C26 C31 1.533(8) . ? C26 C32 1.552(7) . ? C27 H27A 0.9600 . ? C27 H27B 0.9600 . ? C27 H27C 0.9600 . ? C28 H28A 0.9600 . ? C28 H28B 0.9600 . ? C28 H28C 0.9600 . ? C29 H29A 0.9600 . ? C29 H29B 0.9600 . ? C29 H29C 0.9600 . ? C30 H30A 0.9600 . ? C30 H30B 0.9600 . ? C30 H30C 0.9600 . ? C31 H31A 0.9600 . ? C31 H31B 0.9600 . ? C31 H31C 0.9600 . ? C32 H32A 0.9600 . ? C32 H32B 0.9600 . ? C32 H32C 0.9600 . ? C33 C38 1.375(5) . ? C33 C34 1.385(5) . ? C33 C39 1.486(6) . ? C34 C35 1.377(5) . ? C34 H34 0.9300 . ? C35 C36 1.383(5) . ? C35 C40 1.525(5) . ? C36 C37 1.382(5) . ? C36 H36 0.9300 . ? C37 C38 1.380(6) . ? C37 C41 1.501(6) . ? C38 H38 0.9300 . ? C39 O2 1.235(5) . ? C39 O1 1.239(5) . ? C40 O4 1.222(5) . ? C40 O3 1.233(5) . ? C41 N9 1.459(6) . ? C41 H41A 0.9700 . ? C41 H41B 0.9700 . ? C42 N9 1.433(7) . ? C42 C43 1.496(7) . ? C42 H42A 0.9700 . ? C42 H42B 0.9700 . ? C43 C44 1.501(8) . ? C43 H43A 0.9700 . ? C43 H43B 0.9700 . ? C44 N10 1.448(6) . ? C44 H44A 0.9700 . ? C44 H44B 0.9700 . ? C45 N10 1.462(6) . ? C45 C46 1.496(6) . ? C45 H45A 0.9700 . ? C45 H45B 0.9700 . ? C46 C51 1.380(6) . ? C46 C47 1.382(6) . ? C47 C48 1.383(6) . ? C47 H47 0.9300 . ? C48 C49 1.375(6) . ? C48 C52 1.506(6) . ? C49 C50 1.391(5) . ? C49 H49 0.9300 . ? C50 C51 1.368(6) . ? C50 C53 1.512(6) . ? C51 H51 0.9300 . ? C52 O7 1.230(6) . ? C52 O8 1.241(6) . ? C53 O6 1.227(5) . ? C53 O5 1.264(5) . ? C54 N9 1.449(6) . ? C54 C55 1.524(7) . ? C54 H54A 0.9700 . ? C54 H54B 0.9700 . ? C55 N10 1.438(6) 5_655 ? C55 H55A 0.9700 . ? C55 H55B 0.9700 . ? N10 C55 1.438(6) 5_655 ? O3 Cd2 2.304(3) 3_455 ? O1W H1D 0.874(10) . ? O1W H1C 0.865(10) . ? N1 H1E 0.81(5) . ? N2 H2E 0.85(5) . ? N3 H3E 0.75(5) . ? N4 H4E 0.77(5) . ? N5 H5E 0.77(5) . ? N6 H6E 0.85(5) . ? N7 H7E 0.76(5) . ? N8 H8E 0.82(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Cd1 N2 176.57(13) . . ? O1 Cd1 O1W 85.23(11) . . ? N2 Cd1 O1W 93.35(12) . . ? O1 Cd1 N4 86.30(12) . . ? N2 Cd1 N4 95.26(13) . . ? O1W Cd1 N4 171.08(12) . . ? O1 Cd1 N1 104.78(14) . . ? N2 Cd1 N1 78.39(13) . . ? O1W Cd1 N1 92.65(11) . . ? N4 Cd1 N1 86.81(13) . . ? O1 Cd1 N3 90.60(14) . . ? N2 Cd1 N3 86.75(13) . . ? O1W Cd1 N3 105.20(12) . . ? N4 Cd1 N3 77.66(13) . . ? N1 Cd1 N3 157.43(13) . . ? O5 Cd2 O3 92.98(11) . 3 ? O5 Cd2 N7 94.91(13) . . ? O3 Cd2 N7 123.42(14) 3 . ? O5 Cd2 N6 178.42(13) . . ? O3 Cd2 N6 87.19(13) 3 . ? N7 Cd2 N6 83.70(15) . . ? O5 Cd2 N5 104.05(13) . . ? O3 Cd2 N5 77.41(13) 3 . ? N7 Cd2 N5 151.34(15) . . ? N6 Cd2 N5 77.52(15) . . ? O5 Cd2 N8 88.41(13) . . ? O3 Cd2 N8 159.86(14) 3 . ? N7 Cd2 N8 76.39(16) . . ? N6 Cd2 N8 91.97(14) . . ? N5 Cd2 N8 82.76(15) . . ? N1 C1 C2 112.2(3) . . ? N1 C1 H1A 109.2 . . ? C2 C1 H1A 109.2 . . ? N1 C1 H1B 109.2 . . ? C2 C1 H1B 109.2 . . ? H1A C1 H1B 107.9 . . ? N2 C2 C1 110.6(3) . . ? N2 C2 H2A 109.5 . . ? C1 C2 H2A 109.5 . . ? N2 C2 H2B 109.5 . . ? C1 C2 H2B 109.5 . . ? H2A C2 H2B 108.1 . . ? N2 C3 C11 112.1(4) . . ? N2 C3 C4 110.0(3) . . ? C11 C3 C4 108.9(4) . . ? N2 C3 H3 108.6 . . ? C11 C3 H3 108.6 . . ? C4 C3 H3 108.6 . . ? C5 C4 C3 121.6(4) . . ? C5 C4 H4A 106.9 . . ? C3 C4 H4A 106.9 . . ? C5 C4 H4B 106.9 . . ? C3 C4 H4B 106.9 . . ? H4A C4 H4B 106.7 . . ? N3 C5 C13 106.9(4) . . ? N3 C5 C12 110.8(4) . . ? C13 C5 C12 109.9(4) . . ? N3 C5 C4 110.9(3) . . ? C13 C5 C4 111.1(4) . . ? C12 C5 C4 107.3(4) . . ? N3 C6 C7 111.0(4) . . ? N3 C6 H6A 109.4 . . ? C7 C6 H6A 109.4 . . ? N3 C6 H6B 109.4 . . ? C7 C6 H6B 109.4 . . ? H6A C6 H6B 108.0 . . ? N4 C7 C6 109.1(3) . . ? N4 C7 H7A 109.9 . . ? C6 C7 H7A 109.9 . . ? N4 C7 H7B 109.9 . . ? C6 C7 H7B 109.9 . . ? H7A C7 H7B 108.3 . . ? N4 C8 C14 112.2(4) . . ? N4 C8 C9 110.9(3) . . ? C14 C8 C9 109.3(4) . . ? N4 C8 H8 108.1 . . ? C14 C8 H8 108.1 . . ? C9 C8 H8 108.1 . . ? C8 C9 C10 121.0(4) . . ? C8 C9 H9A 107.1 . . ? C10 C9 H9A 107.1 . . ? C8 C9 H9B 107.1 . . ? C10 C9 H9B 107.1 . . ? H9A C9 H9B 106.8 . . ? N1 C10 C15 106.1(4) . . ? N1 C10 C9 112.2(4) . . ? C15 C10 C9 112.0(4) . . ? N1 C10 C16 110.4(4) . . ? C15 C10 C16 108.9(4) . . ? C9 C10 C16 107.3(4) . . ? C3 C11 H11A 109.5 . . ? C3 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C3 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C5 C12 H12A 109.5 . . ? C5 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C5 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C5 C13 H13A 109.5 . . ? C5 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C5 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C8 C14 H14A 109.5 . . ? C8 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C8 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C10 C15 H15A 109.5 . . ? C10 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C10 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C10 C16 H16A 109.5 . . ? C10 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C10 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? N5 C17 C18 112.6(4) . . ? N5 C17 H17A 109.1 . . ? C18 C17 H17A 109.1 . . ? N5 C17 H17B 109.1 . . ? C18 C17 H17B 109.1 . . ? H17A C17 H17B 107.8 . . ? N6 C18 C17 110.1(4) . . ? N6 C18 H18A 109.6 . . ? C17 C18 H18A 109.6 . . ? N6 C18 H18B 109.6 . . ? C17 C18 H18B 109.6 . . ? H18A C18 H18B 108.1 . . ? N6 C19 C27 114.3(5) . . ? N6 C19 C20 109.7(4) . . ? C27 C19 C20 108.6(5) . . ? N6 C19 H19 108.0 . . ? C27 C19 H19 108.0 . . ? C20 C19 H19 108.0 . . ? C21 C20 C19 121.8(5) . . ? C21 C20 H20A 106.9 . . ? C19 C20 H20A 106.9 . . ? C21 C20 H20B 106.9 . . ? C19 C20 H20B 106.9 . . ? H20A C20 H20B 106.7 . . ? N7 C21 C20 111.6(4) . . ? N7 C21 C29 105.5(5) . . ? C20 C21 C29 113.1(5) . . ? N7 C21 C28 110.6(5) . . ? C20 C21 C28 108.1(5) . . ? C29 C21 C28 107.8(5) . . ? N7 C22 C23 111.8(5) . . ? N7 C22 H22A 109.3 . . ? C23 C22 H22A 109.3 . . ? N7 C22 H22B 109.3 . . ? C23 C22 H22B 109.3 . . ? H22A C22 H22B 107.9 . . ? N8 C23 C22 110.8(4) . . ? N8 C23 H23A 109.5 . . ? C22 C23 H23A 109.5 . . ? N8 C23 H23B 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 108.1 . . ? N8 C24 C30 114.2(6) . . ? N8 C24 C25 109.2(4) . . ? C30 C24 C25 108.6(6) . . ? N8 C24 H24 108.2 . . ? C30 C24 H24 108.2 . . ? C25 C24 H24 108.2 . . ? C26 C25 C24 122.1(5) . . ? C26 C25 H25A 106.8 . . ? C24 C25 H25A 106.8 . . ? C26 C25 H25B 106.8 . . ? C24 C25 H25B 106.8 . . ? H25A C25 H25B 106.6 . . ? N5 C26 C25 112.9(5) . . ? N5 C26 C31 104.9(5) . . ? C25 C26 C31 111.0(5) . . ? N5 C26 C32 110.7(5) . . ? C25 C26 C32 110.0(6) . . ? C31 C26 C32 106.9(5) . . ? C19 C27 H27A 109.5 . . ? C19 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C19 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C21 C28 H28A 109.5 . . ? C21 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C21 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C21 C29 H29A 109.5 . . ? C21 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C21 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C24 C30 H30A 109.5 . . ? C24 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C24 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C26 C31 H31A 109.5 . . ? C26 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C26 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C26 C32 H32A 109.5 . . ? C26 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C26 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C38 C33 C34 119.1(4) . . ? C38 C33 C39 119.3(4) . . ? C34 C33 C39 121.6(4) . . ? C35 C34 C33 120.2(4) . . ? C35 C34 H34 119.9 . . ? C33 C34 H34 119.9 . . ? C34 C35 C36 119.6(4) . . ? C34 C35 C40 120.3(4) . . ? C36 C35 C40 120.0(4) . . ? C37 C36 C35 121.1(4) . . ? C37 C36 H36 119.5 . . ? C35 C36 H36 119.5 . . ? C38 C37 C36 118.1(4) . . ? C38 C37 C41 121.1(4) . . ? C36 C37 C41 120.7(4) . . ? C33 C38 C37 121.9(4) . . ? C33 C38 H38 119.1 . . ? C37 C38 H38 119.1 . . ? O2 C39 O1 124.6(4) . . ? O2 C39 C33 119.0(4) . . ? O1 C39 C33 116.4(4) . . ? O4 C40 O3 126.6(4) . . ? O4 C40 C35 116.8(4) . . ? O3 C40 C35 116.5(4) . . ? N9 C41 C37 113.4(4) . . ? N9 C41 H41A 108.9 . . ? C37 C41 H41A 108.9 . . ? N9 C41 H41B 108.9 . . ? C37 C41 H41B 108.9 . . ? H41A C41 H41B 107.7 . . ? N9 C42 C43 114.6(5) . . ? N9 C42 H42A 108.6 . . ? C43 C42 H42A 108.6 . . ? N9 C42 H42B 108.6 . . ? C43 C42 H42B 108.6 . . ? H42A C42 H42B 107.6 . . ? C42 C43 C44 112.9(5) . . ? C42 C43 H43A 109.0 . . ? C44 C43 H43A 109.0 . . ? C42 C43 H43B 109.0 . . ? C44 C43 H43B 109.0 . . ? H43A C43 H43B 107.8 . . ? N10 C44 C43 114.8(5) . . ? N10 C44 H44A 108.6 . . ? C43 C44 H44A 108.6 . . ? N10 C44 H44B 108.6 . . ? C43 C44 H44B 108.6 . . ? H44A C44 H44B 107.5 . . ? N10 C45 C46 110.3(4) . . ? N10 C45 H45A 109.6 . . ? C46 C45 H45A 109.6 . . ? N10 C45 H45B 109.6 . . ? C46 C45 H45B 109.6 . . ? H45A C45 H45B 108.1 . . ? C51 C46 C47 118.5(4) . . ? C51 C46 C45 119.6(4) . . ? C47 C46 C45 121.9(4) . . ? C46 C47 C48 121.3(4) . . ? C46 C47 H47 119.4 . . ? C48 C47 H47 119.4 . . ? C49 C48 C47 118.7(4) . . ? C49 C48 C52 121.9(4) . . ? C47 C48 C52 119.4(4) . . ? C48 C49 C50 121.2(4) . . ? C48 C49 H49 119.4 . . ? C50 C49 H49 119.4 . . ? C51 C50 C49 118.6(4) . . ? C51 C50 C53 120.9(4) . . ? C49 C50 C53 120.4(4) . . ? C50 C51 C46 121.7(4) . . ? C50 C51 H51 119.2 . . ? C46 C51 H51 119.2 . . ? O7 C52 O8 125.7(4) . . ? O7 C52 C48 117.5(5) . . ? O8 C52 C48 116.8(5) . . ? O6 C53 O5 126.8(4) . . ? O6 C53 C50 118.9(4) . . ? O5 C53 C50 114.3(4) . . ? N9 C54 C55 112.8(4) . . ? N9 C54 H54A 109.0 . . ? C55 C54 H54A 109.0 . . ? N9 C54 H54B 109.0 . . ? C55 C54 H54B 109.0 . . ? H54A C54 H54B 107.8 . . ? N10 C55 C54 111.2(4) 5_655 . ? N10 C55 H55A 109.4 5_655 . ? C54 C55 H55A 109.4 . . ? N10 C55 H55B 109.4 5_655 . ? C54 C55 H55B 109.4 . . ? H55A C55 H55B 108.0 . . ? C42 N9 C54 115.8(4) . . ? C42 N9 C41 112.3(4) . . ? C54 N9 C41 115.6(4) . . ? C55 N10 C44 113.3(4) 5_655 . ? C55 N10 C45 111.7(4) 5_655 . ? C44 N10 C45 109.0(4) . . ? C39 O1 Cd1 131.8(3) . . ? C40 O3 Cd2 136.5(3) . 3_455 ? C53 O5 Cd2 127.2(3) . . ? Cd1 O1W H1D 113(3) . . ? Cd1 O1W H1C 98(3) . . ? H1D O1W H1C 109(2) . . ? C1 N1 C10 116.1(3) . . ? C1 N1 Cd1 106.1(3) . . ? C10 N1 Cd1 117.4(3) . . ? C1 N1 H1E 107(4) . . ? C10 N1 H1E 108(4) . . ? Cd1 N1 H1E 101(4) . . ? C2 N2 C3 115.8(3) . . ? C2 N2 Cd1 102.2(3) . . ? C3 N2 Cd1 114.8(3) . . ? C2 N2 H2E 110(3) . . ? C3 N2 H2E 108(3) . . ? Cd1 N2 H2E 106(3) . . ? C6 N3 C5 116.1(4) . . ? C6 N3 Cd1 106.0(3) . . ? C5 N3 Cd1 117.8(3) . . ? C6 N3 H3E 108(4) . . ? C5 N3 H3E 105(4) . . ? Cd1 N3 H3E 102(4) . . ? C8 N4 C7 115.6(3) . . ? C8 N4 Cd1 115.6(3) . . ? C7 N4 Cd1 102.0(2) . . ? C8 N4 H4E 111(4) . . ? C7 N4 H4E 106(4) . . ? Cd1 N4 H4E 106(4) . . ? C26 N5 C17 115.1(4) . . ? C26 N5 Cd2 119.0(3) . . ? C17 N5 Cd2 105.8(3) . . ? C26 N5 H5E 122(5) . . ? C17 N5 H5E 90(5) . . ? Cd2 N5 H5E 100(5) . . ? C19 N6 C18 115.3(4) . . ? C19 N6 Cd2 114.7(3) . . ? C18 N6 Cd2 102.8(3) . . ? C19 N6 H6E 116(4) . . ? C18 N6 H6E 107(4) . . ? Cd2 N6 H6E 98(4) . . ? C22 N7 C21 116.0(4) . . ? C22 N7 Cd2 108.3(3) . . ? C21 N7 Cd2 117.4(3) . . ? C22 N7 H7E 108(5) . . ? C21 N7 H7E 109(5) . . ? Cd2 N7 H7E 96(5) . . ? C24 N8 C23 115.8(4) . . ? C24 N8 Cd2 114.6(3) . . ? C23 N8 Cd2 102.8(3) . . ? C24 N8 H8E 116(4) . . ? C23 N8 H8E 106(4) . . ? Cd2 N8 H8E 99(4) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 C1 C2 N2 63.1(5) . . . . ? N2 C3 C4 C5 -77.7(5) . . . . ? C11 C3 C4 C5 159.0(4) . . . . ? C3 C4 C5 N3 70.3(5) . . . . ? C3 C4 C5 C13 -48.3(6) . . . . ? C3 C4 C5 C12 -168.5(4) . . . . ? N3 C6 C7 N4 66.3(5) . . . . ? N4 C8 C9 C10 -75.7(5) . . . . ? C14 C8 C9 C10 160.0(4) . . . . ? C8 C9 C10 N1 70.5(5) . . . . ? C8 C9 C10 C15 -48.7(6) . . . . ? C8 C9 C10 C16 -168.1(4) . . . . ? N5 C17 C18 N6 64.0(6) . . . . ? N6 C19 C20 C21 -73.4(7) . . . . ? C27 C19 C20 C21 161.1(6) . . . . ? C19 C20 C21 N7 67.6(7) . . . . ? C19 C20 C21 C29 -51.2(7) . . . . ? C19 C20 C21 C28 -170.6(5) . . . . ? N7 C22 C23 N8 63.4(6) . . . . ? N8 C24 C25 C26 -75.5(7) . . . . ? C30 C24 C25 C26 159.4(6) . . . . ? C24 C25 C26 N5 65.9(7) . . . . ? C24 C25 C26 C31 -51.7(7) . . . . ? C24 C25 C26 C32 -169.9(5) . . . . ? C38 C33 C34 C35 2.6(6) . . . . ? C39 C33 C34 C35 -174.9(4) . . . . ? C33 C34 C35 C36 -2.8(6) . . . . ? C33 C34 C35 C40 172.5(4) . . . . ? C34 C35 C36 C37 -0.4(6) . . . . ? C40 C35 C36 C37 -175.7(4) . . . . ? C35 C36 C37 C38 3.7(7) . . . . ? C35 C36 C37 C41 -173.1(4) . . . . ? C34 C33 C38 C37 0.9(7) . . . . ? C39 C33 C38 C37 178.4(4) . . . . ? C36 C37 C38 C33 -4.0(7) . . . . ? C41 C37 C38 C33 172.8(4) . . . . ? C38 C33 C39 O2 161.5(4) . . . . ? C34 C33 C39 O2 -21.0(7) . . . . ? C38 C33 C39 O1 -17.4(6) . . . . ? C34 C33 C39 O1 160.1(4) . . . . ? C34 C35 C40 O4 -147.6(4) . . . . ? C36 C35 C40 O4 27.7(6) . . . . ? C34 C35 C40 O3 29.9(6) . . . . ? C36 C35 C40 O3 -154.8(4) . . . . ? C38 C37 C41 N9 24.6(7) . . . . ? C36 C37 C41 N9 -158.7(5) . . . . ? N9 C42 C43 C44 172.3(4) . . . . ? C42 C43 C44 N10 -58.2(6) . . . . ? N10 C45 C46 C51 -82.3(6) . . . . ? N10 C45 C46 C47 95.7(6) . . . . ? C51 C46 C47 C48 1.5(8) . . . . ? C45 C46 C47 C48 -176.5(5) . . . . ? C46 C47 C48 C49 -0.9(7) . . . . ? C46 C47 C48 C52 -179.6(4) . . . . ? C47 C48 C49 C50 -1.0(7) . . . . ? C52 C48 C49 C50 177.7(4) . . . . ? C48 C49 C50 C51 2.2(7) . . . . ? C48 C49 C50 C53 -174.6(4) . . . . ? C49 C50 C51 C46 -1.5(7) . . . . ? C53 C50 C51 C46 175.3(4) . . . . ? C47 C46 C51 C50 -0.3(8) . . . . ? C45 C46 C51 C50 177.8(5) . . . . ? C49 C48 C52 O7 -11.8(7) . . . . ? C47 C48 C52 O7 166.9(5) . . . . ? C49 C48 C52 O8 168.1(4) . . . . ? C47 C48 C52 O8 -13.2(6) . . . . ? C51 C50 C53 O6 -173.7(4) . . . . ? C49 C50 C53 O6 3.1(7) . . . . ? C51 C50 C53 O5 5.6(6) . . . . ? C49 C50 C53 O5 -177.7(4) . . . . ? N9 C54 C55 N10 166.0(5) . . . 5_655 ? C43 C42 N9 C54 -63.1(6) . . . . ? C43 C42 N9 C41 72.8(5) . . . . ? C55 C54 N9 C42 -72.6(6) . . . . ? C55 C54 N9 C41 153.1(5) . . . . ? C37 C41 N9 C42 83.5(5) . . . . ? C37 C41 N9 C54 -140.5(5) . . . . ? C43 C44 N10 C55 -68.2(6) . . . 5_655 ? C43 C44 N10 C45 166.8(4) . . . . ? C46 C45 N10 C55 154.3(4) . . . 5_655 ? C46 C45 N10 C44 -79.8(5) . . . . ? O2 C39 O1 Cd1 5.5(8) . . . . ? C33 C39 O1 Cd1 -175.7(3) . . . . ? N2 Cd1 O1 C39 41(2) . . . . ? O1W Cd1 O1 C39 -24.8(5) . . . . ? N4 Cd1 O1 C39 158.0(5) . . . . ? N1 Cd1 O1 C39 -116.3(5) . . . . ? N3 Cd1 O1 C39 80.4(5) . . . . ? O4 C40 O3 Cd2 -43.7(7) . . . 3_455 ? C35 C40 O3 Cd2 139.1(3) . . . 3_455 ? O6 C53 O5 Cd2 17.3(7) . . . . ? C50 C53 O5 Cd2 -161.9(3) . . . . ? O3 Cd2 O5 C53 -114.1(4) 3 . . . ? N7 Cd2 O5 C53 9.9(4) . . . . ? N6 Cd2 O5 C53 -18(5) . . . . ? N5 Cd2 O5 C53 168.2(4) . . . . ? N8 Cd2 O5 C53 86.1(4) . . . . ? C2 C1 N1 C10 -165.1(4) . . . . ? C2 C1 N1 Cd1 -32.7(4) . . . . ? C15 C10 N1 C1 -163.5(4) . . . . ? C9 C10 N1 C1 73.9(5) . . . . ? C16 C10 N1 C1 -45.7(5) . . . . ? C15 C10 N1 Cd1 69.5(4) . . . . ? C9 C10 N1 Cd1 -53.1(4) . . . . ? C16 C10 N1 Cd1 -172.7(3) . . . . ? O1 Cd1 N1 C1 -178.6(3) . . . . ? N2 Cd1 N1 C1 2.7(3) . . . . ? O1W Cd1 N1 C1 95.6(3) . . . . ? N4 Cd1 N1 C1 -93.3(3) . . . . ? N3 Cd1 N1 C1 -47.1(5) . . . . ? O1 Cd1 N1 C10 -47.0(3) . . . . ? N2 Cd1 N1 C10 134.4(3) . . . . ? O1W Cd1 N1 C10 -132.8(3) . . . . ? N4 Cd1 N1 C10 38.3(3) . . . . ? N3 Cd1 N1 C10 84.6(5) . . . . ? C1 C2 N2 C3 -179.8(4) . . . . ? C1 C2 N2 Cd1 -54.3(4) . . . . ? C11 C3 N2 C2 -56.3(6) . . . . ? C4 C3 N2 C2 -177.6(4) . . . . ? C11 C3 N2 Cd1 -175.2(4) . . . . ? C4 C3 N2 Cd1 63.5(4) . . . . ? O1 Cd1 N2 C2 -131(2) . . . . ? O1W Cd1 N2 C2 -65.3(3) . . . . ? N4 Cd1 N2 C2 112.4(3) . . . . ? N1 Cd1 N2 C2 26.7(2) . . . . ? N3 Cd1 N2 C2 -170.4(3) . . . . ? O1 Cd1 N2 C3 -5(2) . . . . ? O1W Cd1 N2 C3 60.9(3) . . . . ? N4 Cd1 N2 C3 -121.4(3) . . . . ? N1 Cd1 N2 C3 152.9(3) . . . . ? N3 Cd1 N2 C3 -44.1(3) . . . . ? C7 C6 N3 C5 -167.8(3) . . . . ? C7 C6 N3 Cd1 -34.8(4) . . . . ? C13 C5 N3 C6 -163.8(4) . . . . ? C12 C5 N3 C6 -44.1(5) . . . . ? C4 C5 N3 C6 75.0(5) . . . . ? C13 C5 N3 Cd1 68.9(4) . . . . ? C12 C5 N3 Cd1 -171.4(3) . . . . ? C4 C5 N3 Cd1 -52.3(5) . . . . ? O1 Cd1 N3 C6 89.4(3) . . . . ? N2 Cd1 N3 C6 -92.8(3) . . . . ? O1W Cd1 N3 C6 174.6(3) . . . . ? N4 Cd1 N3 C6 3.3(3) . . . . ? N1 Cd1 N3 C6 -44.3(5) . . . . ? O1 Cd1 N3 C5 -138.6(3) . . . . ? N2 Cd1 N3 C5 39.2(3) . . . . ? O1W Cd1 N3 C5 -53.4(3) . . . . ? N4 Cd1 N3 C5 135.3(3) . . . . ? N1 Cd1 N3 C5 87.8(4) . . . . ? C14 C8 N4 C7 -57.0(5) . . . . ? C9 C8 N4 C7 -179.6(4) . . . . ? C14 C8 N4 Cd1 -176.0(3) . . . . ? C9 C8 N4 Cd1 61.4(4) . . . . ? C6 C7 N4 C8 176.8(4) . . . . ? C6 C7 N4 Cd1 -57.0(4) . . . . ? O1 Cd1 N4 C8 62.7(3) . . . . ? N2 Cd1 N4 C8 -120.4(3) . . . . ? O1W Cd1 N4 C8 44.5(9) . . . . ? N1 Cd1 N4 C8 -42.3(3) . . . . ? N3 Cd1 N4 C8 154.1(3) . . . . ? O1 Cd1 N4 C7 -63.5(3) . . . . ? N2 Cd1 N4 C7 113.4(3) . . . . ? O1W Cd1 N4 C7 -81.8(8) . . . . ? N1 Cd1 N4 C7 -168.6(3) . . . . ? N3 Cd1 N4 C7 27.9(3) . . . . ? C25 C26 N5 C17 74.7(6) . . . . ? C31 C26 N5 C17 -164.2(4) . . . . ? C32 C26 N5 C17 -49.1(7) . . . . ? C25 C26 N5 Cd2 -52.4(6) . . . . ? C31 C26 N5 Cd2 68.7(5) . . . . ? C32 C26 N5 Cd2 -176.3(4) . . . . ? C18 C17 N5 C26 -167.9(5) . . . . ? C18 C17 N5 Cd2 -34.3(5) . . . . ? O5 Cd2 N5 C26 -45.2(4) . . . . ? O3 Cd2 N5 C26 -135.2(4) 3 . . . ? N7 Cd2 N5 C26 84.7(5) . . . . ? N6 Cd2 N5 C26 134.9(4) . . . . ? N8 Cd2 N5 C26 41.3(4) . . . . ? O5 Cd2 N5 C17 -176.6(3) . . . . ? O3 Cd2 N5 C17 93.5(3) 3 . . . ? N7 Cd2 N5 C17 -46.7(5) . . . . ? N6 Cd2 N5 C17 3.6(3) . . . . ? N8 Cd2 N5 C17 -90.1(3) . . . . ? C27 C19 N6 C18 -52.6(7) . . . . ? C20 C19 N6 C18 -174.8(4) . . . . ? C27 C19 N6 Cd2 -171.8(5) . . . . ? C20 C19 N6 Cd2 66.0(5) . . . . ? C17 C18 N6 C19 -179.8(4) . . . . ? C17 C18 N6 Cd2 -54.2(4) . . . . ? O5 Cd2 N6 C19 -22(5) . . . . ? O3 Cd2 N6 C19 74.2(3) 3 . . . ? N7 Cd2 N6 C19 -49.8(4) . . . . ? N5 Cd2 N6 C19 152.0(4) . . . . ? N8 Cd2 N6 C19 -125.9(4) . . . . ? O5 Cd2 N6 C18 -148(5) . . . . ? O3 Cd2 N6 C18 -51.7(3) 3 . . . ? N7 Cd2 N6 C18 -175.7(3) . . . . ? N5 Cd2 N6 C18 26.1(3) . . . . ? N8 Cd2 N6 C18 108.2(3) . . . . ? C23 C22 N7 C21 -169.8(4) . . . . ? C23 C22 N7 Cd2 -35.4(5) . . . . ? C20 C21 N7 C22 73.2(6) . . . . ? C29 C21 N7 C22 -163.5(4) . . . . ? C28 C21 N7 C22 -47.2(6) . . . . ? C20 C21 N7 Cd2 -56.9(5) . . . . ? C29 C21 N7 Cd2 66.3(5) . . . . ? C28 C21 N7 Cd2 -177.3(4) . . . . ? O5 Cd2 N7 C22 92.4(3) . . . . ? O3 Cd2 N7 C22 -170.8(3) 3 . . . ? N6 Cd2 N7 C22 -88.3(3) . . . . ? N5 Cd2 N7 C22 -39.3(5) . . . . ? N8 Cd2 N7 C22 5.2(3) . . . . ? O5 Cd2 N7 C21 -133.9(4) . . . . ? O3 Cd2 N7 C21 -37.1(4) 3 . . . ? N6 Cd2 N7 C21 45.3(4) . . . . ? N5 Cd2 N7 C21 94.4(5) . . . . ? N8 Cd2 N7 C21 138.9(4) . . . . ? C30 C24 N8 C23 -50.9(7) . . . . ? C25 C24 N8 C23 -172.7(5) . . . . ? C30 C24 N8 Cd2 -170.4(5) . . . . ? C25 C24 N8 Cd2 67.9(5) . . . . ? C22 C23 N8 C24 -178.2(5) . . . . ? C22 C23 N8 Cd2 -52.5(5) . . . . ? O5 Cd2 N8 C24 55.3(4) . . . . ? O3 Cd2 N8 C24 -39.0(6) 3 . . . ? N7 Cd2 N8 C24 150.8(4) . . . . ? N6 Cd2 N8 C24 -126.2(4) . . . . ? N5 Cd2 N8 C24 -49.0(4) . . . . ? O5 Cd2 N8 C23 -71.1(3) . . . . ? O3 Cd2 N8 C23 -165.4(4) 3 . . . ? N7 Cd2 N8 C23 24.3(3) . . . . ? N6 Cd2 N8 C23 107.4(3) . . . . ? N5 Cd2 N8 C23 -175.5(3) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1W H1D O8 0.874(10) 1.746(12) 2.611(4) 170(4) 3 O1W H1C O2 0.865(10) 1.893(15) 2.731(4) 163(4) . N1 H1E O8 0.81(5) 2.60(5) 3.334(5) 151(5) 3 N2 H2E O4 0.85(5) 2.14(5) 2.972(5) 169(4) 3 N4 H4E O4 0.77(5) 2.45(5) 3.194(5) 163(5) 3 N5 H5E O3 0.77(5) 2.51(6) 2.932(6) 116(5) 3 N6 H6E O7 0.85(5) 2.25(5) 3.103(6) 178(5) 6_656 N7 H7E O6 0.76(5) 2.24(6) 2.962(5) 157(6) . N8 H8E O7 0.82(5) 2.20(5) 3.021(5) 175(6) 6_656 _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.636 _refine_diff_density_min -0.443 _refine_diff_density_rms 0.067 #=========================END data_Compound-10 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C78 H118 Cu2 N12 O17, H2O' _chemical_formula_sum 'C78 H120 Cu2 N12 O18' _chemical_formula_weight 1640.94 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cu' 'Cu' 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.1765(3) _cell_length_b 13.6017(5) _cell_length_c 17.2551(7) _cell_angle_alpha 77.337(3) _cell_angle_beta 86.838(3) _cell_angle_gamma 81.439(3) _cell_volume 2077.35(13) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 3621 _cell_measurement_theta_min 2.8963 _cell_measurement_theta_max 29.0769 _exptl_crystal_description block _exptl_crystal_colour violet _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.312 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 874 _exptl_absorpt_coefficient_mu 0.585 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8724 _exptl_absorpt_correction_T_max 0.9122 _exptl_absorpt_process_details ; CrysAlis (Oxford Diffraction, 2006) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Diffraction Gemini R Ultra' _diffrn_measurement_method '\w scan' _diffrn_detector_area_resol_mean 10.0 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14880 _diffrn_reflns_av_R_equivalents 0.0389 _diffrn_reflns_av_sigmaI/netI 0.0789 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.90 _diffrn_reflns_theta_max 29.14 _reflns_number_total 9185 _reflns_number_gt 5544 _reflns_threshold_expression >2\s(I) _computing_data_collection 'CrysAlisPro(1.171.35.21) (Agilent Tech., 2012)' _computing_cell_refinement 'CrysAlisPro(1.171.35.21) (Agilent Tech., 2012)' _computing_data_reduction 'CrysAlisPro(1.171.35.21) (Agilent Tech., 2012)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0250P)^2^+10.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9185 _refine_ls_number_parameters 527 _refine_ls_number_restraints 51 _refine_ls_R_factor_all 0.1408 _refine_ls_R_factor_gt 0.0895 _refine_ls_wR_factor_ref 0.2053 _refine_ls_wR_factor_gt 0.1777 _refine_ls_goodness_of_fit_ref 0.975 _refine_ls_restrained_S_all 0.975 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.80809(7) 0.84901(5) 0.33372(5) 0.0479(2) Uani 1 1 d D . . C1 C 0.6557(9) 1.0661(5) 0.3383(5) 0.080(3) Uani 1 1 d . . . C2 C 0.5617(8) 1.0501(6) 0.2729(5) 0.079(2) Uani 1 1 d . . . H2A H 0.4783 1.1039 0.2656 0.095 Uiso 1 1 calc R . . H2B H 0.6199 1.0590 0.2239 0.095 Uiso 1 1 calc R . . C3 C 0.5043(7) 0.9529(6) 0.2838(4) 0.069(2) Uani 1 1 d . . . H3 H 0.4641 0.9341 0.3379 0.082 Uiso 1 1 calc R . . C4 C 0.5814(7) 0.7717(6) 0.2748(4) 0.0667(19) Uani 1 1 d . . . H4A H 0.5168 0.7736 0.2317 0.080 Uiso 1 1 calc R . . H4B H 0.5283 0.7518 0.3246 0.080 Uiso 1 1 calc R . . C5 C 0.7135(8) 0.6972(6) 0.2707(4) 0.0680(18) Uani 1 1 d . . . H5A H 0.6862 0.6297 0.2764 0.082 Uiso 1 1 calc R . . H5B H 0.7644 0.7147 0.2198 0.082 Uiso 1 1 calc R . . C6 C 0.9483(9) 0.6285(5) 0.3403(5) 0.073(2) Uani 1 1 d . . . C7 C 1.0340(9) 0.6386(6) 0.4111(6) 0.094(3) Uani 1 1 d . . . H7A H 0.9678 0.6327 0.4571 0.113 Uiso 1 1 calc R . . H7B H 1.1120 0.5812 0.4217 0.113 Uiso 1 1 calc R . . C8 C 1.1014(8) 0.7326(7) 0.4041(6) 0.094(3) Uani 1 1 d . . . C9 C 1.0342(8) 0.9211(6) 0.3987(4) 0.074(2) Uani 1 1 d . . . H9A H 1.0881 0.9400 0.3490 0.089 Uiso 1 1 calc R . . H9B H 1.0992 0.9174 0.4420 0.089 Uiso 1 1 calc R . . C10 C 0.9036(9) 0.9981(6) 0.4029(4) 0.076(2) Uani 1 1 d . . . H10A H 0.8551 0.9828 0.4546 0.091 Uiso 1 1 calc R . . H10B H 0.9337 1.0650 0.3954 0.091 Uiso 1 1 calc R . . C11 C 0.5618(17) 1.0466(9) 0.4144(7) 0.156(5) Uani 1 1 d . . . H11A H 0.6156 1.0552 0.4581 0.233 Uiso 1 1 calc R . . H11B H 0.5383 0.9785 0.4246 0.233 Uiso 1 1 calc R . . H11C H 0.4724 1.0940 0.4084 0.233 Uiso 1 1 calc R . . C12 C 0.6818(11) 1.1771(7) 0.3194(6) 0.112(3) Uani 1 1 d U . . H12A H 0.7385 1.1906 0.2707 0.168 Uiso 1 1 calc R . . H12B H 0.7346 1.1901 0.3617 0.168 Uiso 1 1 calc R . . H12C H 0.5888 1.2205 0.3137 0.168 Uiso 1 1 calc R . . C13 C 0.3816(10) 0.9670(8) 0.2235(6) 0.105(3) Uani 1 1 d U . . H13A H 0.3416 0.9044 0.2292 0.157 Uiso 1 1 calc R . . H13B H 0.4215 0.9859 0.1706 0.157 Uiso 1 1 calc R . . H13C H 0.3050 1.0196 0.2331 0.157 Uiso 1 1 calc R . . C14 C 1.062(2) 0.6548(16) 0.2736(13) 0.135(6) Uani 0.65 1 d PU . . C14' C 1.015(4) 0.633(3) 0.237(2) 0.134(12) Uiso 0.35 1 d P . . C15 C 0.9189(11) 0.5170(7) 0.3548(6) 0.108(3) Uani 1 1 d U . . H15A H 0.8657 0.5080 0.3110 0.162 Uiso 1 1 calc R . . H15B H 0.8616 0.5013 0.4030 0.162 Uiso 1 1 calc R . . H15C H 1.0110 0.4725 0.3593 0.162 Uiso 1 1 calc R . . C16 C 1.216(2) 0.7025(16) 0.4631(13) 0.099(6) Uani 0.50 1 d PU . . C16' C 1.185(2) 0.7331(16) 0.4971(14) 0.103(6) Uani 0.50 1 d PU . . O5 O 0.7183(5) 0.8034(3) 0.4876(2) 0.0671(12) Uani 1 1 d . . . C17 C 0.8849(5) 0.1111(3) 0.9347(3) 0.0317(10) Uani 1 1 d . . . H17 H 0.9360 0.1659 0.9152 0.038 Uiso 1 1 calc R . . C18 C 0.9080(5) 0.0273(3) 0.8992(3) 0.0299(9) Uani 1 1 d . . . C19 C 0.8298(5) -0.0538(3) 0.9284(3) 0.0319(10) Uani 1 1 d . . . H19 H 0.8441 -0.1101 0.9050 0.038 Uiso 1 1 calc R . . C20 C 0.7303(5) -0.0517(3) 0.9920(3) 0.0317(10) Uani 1 1 d . . . C21 C 0.7123(5) 0.0322(3) 1.0272(3) 0.0333(10) Uani 1 1 d . . . H21 H 0.6487 0.0331 1.0710 0.040 Uiso 1 1 calc R . . C22 C 0.7872(5) 0.1141(3) 0.9984(3) 0.0318(10) Uani 1 1 d . . . C23 C 1.0140(5) 0.0258(4) 0.8296(3) 0.0352(10) Uani 1 1 d . . . C24 C 0.6392(6) -0.1355(4) 1.0221(3) 0.0393(11) Uani 1 1 d . . . C25 C 0.7673(5) 0.2026(4) 1.0398(3) 0.0369(11) Uani 1 1 d . . . H25A H 0.7679 0.1766 1.0968 0.044 Uiso 1 1 calc R . . H25B H 0.8497 0.2407 1.0256 0.044 Uiso 1 1 calc R . . C26 C 0.6402(5) 0.3389(4) 0.9372(3) 0.0390(11) Uani 1 1 d . . . H26A H 0.6877 0.2973 0.9015 0.047 Uiso 1 1 calc R . . H26B H 0.7030 0.3894 0.9400 0.047 Uiso 1 1 calc R . . C27 C 0.4918(6) 0.3933(3) 0.9033(3) 0.0379(11) Uani 1 1 d . . . H27A H 0.4497 0.3501 0.8752 0.045 Uiso 1 1 calc R . . H27B H 0.4242 0.4063 0.9463 0.045 Uiso 1 1 calc RD . . C28 C 0.5881(6) 0.4714(4) 0.7756(3) 0.0439(12) Uani 1 1 d . . . H28A H 0.5197 0.4533 0.7419 0.053 Uiso 1 1 calc R . . H28B H 0.6669 0.4148 0.7883 0.053 Uiso 1 1 calc R . . O1 O 1.0624(5) 0.1063(3) 0.7978(2) 0.0545(10) Uani 1 1 d . . . O2 O 1.0496(4) -0.0581(3) 0.8078(2) 0.0426(8) Uani 1 1 d . . . O3 O 0.6139(4) -0.1880(3) 0.9723(2) 0.0490(9) Uani 1 1 d . . . H3A H 0.6531 -0.1665 0.9293 0.074 Uiso 1 1 calc R . . O4 O 0.5890(5) -0.1481(3) 1.0905(2) 0.0626(12) Uani 1 1 d . . . O6 O 0.6266(6) 0.6641(4) 0.4837(4) 0.0920(16) Uani 1 1 d U . . C29 C 0.6759(7) 0.7213(5) 0.5194(4) 0.0603(17) Uani 1 1 d . . . C30 C 0.8890(6) 0.7472(4) 0.7749(4) 0.0502(14) Uani 1 1 d . . . C31 C 0.6518(6) 0.5647(4) 0.7312(3) 0.0414(12) Uani 1 1 d . . . C32 C 0.6342(6) 0.6001(4) 0.6499(3) 0.0441(12) Uani 1 1 d . . . H32A H 0.5799 0.5665 0.6227 0.053 Uiso 1 1 calc R . . C33 C 0.6952(6) 0.6841(4) 0.6083(3) 0.0422(12) Uani 1 1 d . . . C34 C 0.7739(6) 0.7341(4) 0.6490(3) 0.0440(12) Uani 1 1 d . . . H34A H 0.8111 0.7925 0.6220 0.053 Uiso 1 1 calc R . . C35 C 0.7993(6) 0.6987(4) 0.7302(3) 0.0424(12) Uani 1 1 d . . . C36 C 0.7364(6) 0.6132(4) 0.7710(3) 0.0443(12) Uani 1 1 d . . . H36A H 0.7517 0.5890 0.8251 0.053 Uiso 1 1 calc R . . C37 C 0.5786(6) 0.3313(4) 1.0826(3) 0.0363(11) Uani 1 1 d . . . H37A H 0.4878 0.3761 1.0670 0.044 Uiso 1 1 calc R . . H37B H 0.5573 0.2832 1.1309 0.044 Uiso 1 1 calc R . . C38 C 0.6890(6) 0.3938(4) 1.1008(3) 0.0430(12) Uani 1 1 d . . . H38A H 0.7078 0.4446 1.0538 0.052 Uiso 1 1 calc R . . H38B H 0.7811 0.3502 1.1158 0.052 Uiso 1 1 calc R . . C39 C 0.6319(6) 0.4457(4) 1.1678(3) 0.0420(12) Uani 1 1 d . . . H39A H 0.6215 0.3943 1.2158 0.050 Uiso 1 1 calc R . . H39B H 0.7036 0.4870 1.1776 0.050 Uiso 1 1 calc R . . N5 N 0.5112(5) 0.4891(3) 0.8491(2) 0.0354(9) Uani 1 1 d . . . N6 N 0.6261(4) 0.2728(3) 1.0182(2) 0.0320(8) Uani 1 1 d . . . O7 O 0.9421(6) 0.7062(4) 0.8380(3) 0.0782(15) Uani 1 1 d . . . O8 O 0.9081(5) 0.8401(3) 0.7382(3) 0.0634(12) Uani 1 1 d . . . H8A H 0.9582 0.8639 0.7655 0.095 Uiso 1 1 calc R . . N1 N 0.8007(6) 0.9971(4) 0.3401(3) 0.0557(13) Uani 1 1 d D . . H1D H 0.842(7) 1.019(5) 0.296(2) 0.084 Uiso 1 1 d D . . N2 N 0.6243(5) 0.8723(4) 0.2689(3) 0.0552(13) Uani 1 1 d D . . H2D H 0.662(7) 0.886(5) 0.2225(18) 0.083 Uiso 1 1 d D . . N3 N 0.8084(5) 0.6992(3) 0.3349(3) 0.0475(11) Uani 1 1 d D . . H3D H 0.751(6) 0.6908(15) 0.375(2) 0.071 Uiso 1 1 d D . . N4 N 0.9853(5) 0.8216(4) 0.4042(3) 0.0591(14) Uani 1 1 d D . . H4D H 0.917(6) 0.807(6) 0.438(3) 0.089 Uiso 1 1 d D . . O1W O 0.1754(11) 0.3669(6) 1.0129(6) 0.160(3) Uani 1 1 d D . . H1A H 0.111(13) 0.351(11) 0.986(10) 0.240 Uiso 1 1 d D . . H1B H 0.254(3) 0.324(4) 1.021(6) 0.240 Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0418(4) 0.0383(4) 0.0614(5) -0.0086(3) -0.0061(3) 0.0003(3) C1 0.107(6) 0.037(3) 0.084(6) -0.010(3) 0.056(5) 0.005(3) C2 0.079(5) 0.071(5) 0.062(5) 0.009(4) 0.014(4) 0.031(4) C3 0.043(3) 0.103(6) 0.041(3) 0.007(3) 0.004(3) 0.015(3) C4 0.063(4) 0.098(5) 0.043(4) -0.005(3) -0.008(3) -0.035(4) C5 0.085(5) 0.074(5) 0.053(4) -0.021(3) 0.001(3) -0.026(4) C6 0.088(5) 0.038(3) 0.079(5) 0.000(3) 0.016(4) 0.012(3) C7 0.072(5) 0.072(5) 0.107(7) 0.028(5) -0.006(5) 0.020(4) C8 0.052(4) 0.096(6) 0.120(7) 0.004(5) -0.033(4) 0.004(4) C9 0.075(5) 0.097(6) 0.058(4) -0.010(4) -0.004(4) -0.046(4) C10 0.111(6) 0.078(5) 0.054(4) -0.033(4) 0.028(4) -0.046(5) C11 0.243(15) 0.108(9) 0.112(9) -0.025(7) 0.053(10) -0.031(9) C12 0.113(3) 0.111(3) 0.112(3) -0.0237(12) -0.0009(10) -0.0153(11) C13 0.104(3) 0.106(3) 0.104(3) -0.0218(12) -0.0027(10) -0.0131(11) C14 0.135(7) 0.135(7) 0.135(7) -0.0288(17) -0.0029(10) -0.0189(14) C15 0.109(3) 0.107(3) 0.108(3) -0.0228(12) -0.0018(10) -0.0143(11) C16 0.099(6) 0.100(6) 0.099(6) -0.0213(16) -0.0028(10) -0.0137(13) C16' 0.102(6) 0.103(6) 0.103(6) -0.0220(16) -0.0029(10) -0.0140(13) O5 0.084(3) 0.064(3) 0.043(2) 0.014(2) 0.014(2) -0.018(2) C17 0.036(2) 0.028(2) 0.029(2) -0.0007(19) -0.0024(19) -0.0055(19) C18 0.031(2) 0.031(2) 0.027(2) -0.0023(18) -0.0016(18) -0.0037(18) C19 0.034(2) 0.028(2) 0.032(3) -0.0038(19) -0.0021(19) -0.0008(18) C20 0.031(2) 0.029(2) 0.031(2) -0.0008(19) 0.0001(18) -0.0032(18) C21 0.037(2) 0.032(2) 0.027(2) -0.0034(19) 0.0023(19) -0.0001(19) C22 0.034(2) 0.027(2) 0.031(3) -0.0010(19) -0.0030(19) -0.0027(18) C23 0.038(3) 0.036(3) 0.030(3) -0.005(2) 0.000(2) -0.006(2) C24 0.044(3) 0.032(3) 0.039(3) 0.000(2) 0.005(2) -0.008(2) C25 0.044(3) 0.033(2) 0.034(3) -0.009(2) -0.003(2) -0.003(2) C26 0.045(3) 0.036(3) 0.032(3) -0.001(2) 0.009(2) -0.008(2) C27 0.048(3) 0.026(2) 0.036(3) 0.001(2) 0.000(2) -0.007(2) C28 0.066(3) 0.033(3) 0.033(3) -0.008(2) 0.012(2) -0.014(2) O1 0.073(3) 0.038(2) 0.052(2) -0.0072(18) 0.029(2) -0.0186(19) O2 0.051(2) 0.040(2) 0.039(2) -0.0137(16) 0.0105(16) -0.0130(16) O3 0.057(2) 0.045(2) 0.052(2) -0.0181(18) 0.0157(18) -0.0235(18) O4 0.086(3) 0.058(3) 0.046(2) -0.007(2) 0.021(2) -0.032(2) O6 0.0936(18) 0.0935(18) 0.0899(18) -0.0180(10) -0.0026(10) -0.0182(10) C29 0.067(4) 0.075(4) 0.038(3) 0.000(3) 0.010(3) -0.030(3) C30 0.055(3) 0.042(3) 0.053(4) -0.008(3) 0.003(3) -0.009(3) C31 0.059(3) 0.030(2) 0.035(3) -0.004(2) 0.004(2) -0.009(2) C32 0.056(3) 0.046(3) 0.032(3) -0.009(2) 0.007(2) -0.014(2) C33 0.049(3) 0.042(3) 0.031(3) -0.001(2) 0.006(2) -0.007(2) C34 0.047(3) 0.037(3) 0.044(3) -0.001(2) 0.013(2) -0.009(2) C35 0.048(3) 0.035(3) 0.043(3) -0.007(2) 0.003(2) -0.008(2) C36 0.059(3) 0.036(3) 0.037(3) -0.002(2) -0.002(2) -0.009(2) C37 0.048(3) 0.030(2) 0.032(3) -0.008(2) 0.003(2) -0.005(2) C38 0.045(3) 0.033(3) 0.052(3) -0.012(2) -0.004(2) -0.003(2) C39 0.057(3) 0.033(3) 0.037(3) -0.009(2) -0.010(2) -0.005(2) N5 0.051(2) 0.0248(19) 0.028(2) -0.0022(16) 0.0023(18) -0.0053(17) N6 0.047(2) 0.0240(19) 0.024(2) -0.0039(15) 0.0012(16) -0.0044(16) O7 0.106(4) 0.069(3) 0.062(3) 0.003(2) -0.031(3) -0.033(3) O8 0.085(3) 0.048(2) 0.062(3) -0.007(2) -0.009(2) -0.027(2) N1 0.079(4) 0.042(3) 0.044(3) -0.010(2) 0.023(3) -0.010(2) N2 0.046(3) 0.070(3) 0.038(3) 0.007(2) 0.000(2) 0.002(2) N3 0.062(3) 0.039(2) 0.039(3) -0.003(2) 0.005(2) -0.010(2) N4 0.045(3) 0.073(4) 0.056(3) 0.002(3) -0.004(2) -0.021(3) O1W 0.159(8) 0.123(6) 0.161(9) 0.013(5) 0.026(6) 0.017(6) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 N3 2.033(4) . ? Cu1 N2 2.023(5) . ? Cu1 N4 2.025(5) . ? Cu1 N1 2.033(5) . ? C1 N1 1.507(9) . ? C1 C11 1.525(12) . ? C1 C12 1.525(11) . ? C1 C2 1.529(12) . ? C2 C3 1.465(11) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 N2 1.487(8) . ? C3 C13 1.537(11) . ? C3 H3 0.9800 . ? C4 N2 1.461(9) . ? C4 C5 1.468(10) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 N3 1.455(8) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 N3 1.479(8) . ? C6 C7 1.530(12) . ? C6 C15 1.544(11) . ? C6 C14 1.53(2) . ? C6 C14' 1.85(4) . ? C7 C8 1.480(12) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 C16 1.46(2) . ? C8 N4 1.489(10) . ? C8 C16' 1.81(2) . ? C9 N4 1.470(9) . ? C9 C10 1.479(10) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 N1 1.479(9) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? C14 C14' 0.91(4) . ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? C15 H15C 0.9600 . ? C16 C16' 0.81(3) . ? O5 C29 1.239(7) . ? C17 C22 1.384(6) . ? C17 C18 1.392(6) . ? C17 H17 0.9300 . ? C18 C19 1.393(6) . ? C18 C23 1.505(7) . ? C19 C20 1.391(6) . ? C19 H19 0.9300 . ? C20 C21 1.391(6) . ? C20 C24 1.498(6) . ? C21 C22 1.381(6) . ? C21 H21 0.9300 . ? C22 C25 1.514(6) . ? C23 O1 1.246(6) . ? C23 O2 1.270(6) . ? C24 O4 1.228(6) . ? C24 O3 1.281(6) . ? C25 N6 1.503(6) . ? C25 H25A 0.9700 . ? C25 H25B 0.9700 . ? C26 N6 1.496(6) . ? C26 C27 1.531(7) . ? C26 H26A 0.9700 . ? C26 H26B 0.9700 . ? C27 N5 1.457(6) . ? C27 H27A 0.9700 . ? C27 H27B 0.9700 . ? C28 N5 1.465(6) . ? C28 C31 1.511(7) . ? C28 H28A 0.9700 . ? C28 H28B 0.9700 . ? O3 H3A 0.8200 . ? O6 C29 1.239(8) . ? C29 C33 1.519(8) . ? C30 O7 1.202(7) . ? C30 O8 1.316(7) . ? C30 C35 1.471(8) . ? C31 C32 1.389(7) . ? C31 C36 1.386(7) . ? C32 C33 1.386(7) . ? C32 H32A 0.9300 . ? C33 C34 1.373(8) . ? C34 C35 1.399(8) . ? C34 H34A 0.9300 . ? C35 C36 1.407(7) . ? C36 H36A 0.9300 . ? C37 C38 1.501(7) . ? C37 N6 1.513(6) . ? C37 H37A 0.9700 . ? C37 H37B 0.9700 . ? C38 C39 1.513(7) . ? C38 H38A 0.9700 . ? C38 H38B 0.9700 . ? C39 N5 1.476(6) 2_667 ? C39 H39A 0.9700 . ? C39 H39B 0.9700 . ? N5 C39 1.476(6) 2_667 ? O8 H8A 0.8200 . ? N1 H1D 0.850(10) . ? N2 H2D 0.849(10) . ? N3 H3D 0.847(10) . ? N4 H4D 0.846(10) . ? O1W H1A 0.854(10) . ? O1W H1B 0.853(10) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N3 Cu1 N2 85.3(2) . . ? N3 Cu1 N4 93.4(2) . . ? N2 Cu1 N4 176.6(2) . . ? N3 Cu1 N1 175.98(19) . . ? N2 Cu1 N1 95.2(2) . . ? N4 Cu1 N1 85.8(2) . . ? N1 C1 C11 114.9(8) . . ? N1 C1 C12 110.1(7) . . ? C11 C1 C12 108.9(7) . . ? N1 C1 C2 109.1(5) . . ? C11 C1 C2 105.5(8) . . ? C12 C1 C2 108.1(7) . . ? C3 C2 C1 118.2(6) . . ? C3 C2 H2A 107.8 . . ? C1 C2 H2A 107.8 . . ? C3 C2 H2B 107.8 . . ? C1 C2 H2B 107.8 . . ? H2A C2 H2B 107.1 . . ? C2 C3 N2 109.8(5) . . ? C2 C3 C13 107.5(6) . . ? N2 C3 C13 109.9(6) . . ? C2 C3 H3 109.9 . . ? N2 C3 H3 109.9 . . ? C13 C3 H3 109.9 . . ? N2 C4 C5 109.7(5) . . ? N2 C4 H4A 109.7 . . ? C5 C4 H4A 109.7 . . ? N2 C4 H4B 109.7 . . ? C5 C4 H4B 109.7 . . ? H4A C4 H4B 108.2 . . ? N3 C5 C4 107.6(5) . . ? N3 C5 H5A 110.2 . . ? C4 C5 H5A 110.2 . . ? N3 C5 H5B 110.2 . . ? C4 C5 H5B 110.2 . . ? H5A C5 H5B 108.5 . . ? N3 C6 C7 109.1(6) . . ? N3 C6 C15 110.9(7) . . ? C7 C6 C15 107.4(6) . . ? N3 C6 C14 115.8(9) . . ? C7 C6 C14 99.6(10) . . ? C15 C6 C14 113.1(10) . . ? N3 C6 C14' 105.7(13) . . ? C7 C6 C14' 128.1(14) . . ? C15 C6 C14' 94.4(13) . . ? C14 C6 C14' 29.4(12) . . ? C8 C7 C6 117.7(7) . . ? C8 C7 H7A 107.9 . . ? C6 C7 H7A 107.9 . . ? C8 C7 H7B 107.9 . . ? C6 C7 H7B 107.9 . . ? H7A C7 H7B 107.2 . . ? C16 C8 C7 103.3(10) . . ? C16 C8 N4 122.1(12) . . ? C7 C8 N4 110.5(6) . . ? C16 C8 C16' 25.7(10) . . ? C7 C8 C16' 110.3(9) . . ? N4 C8 C16' 97.2(9) . . ? N4 C9 C10 109.0(5) . . ? N4 C9 H9A 109.9 . . ? C10 C9 H9A 109.9 . . ? N4 C9 H9B 109.9 . . ? C10 C9 H9B 109.9 . . ? H9A C9 H9B 108.3 . . ? N1 C10 C9 109.0(5) . . ? N1 C10 H10A 109.9 . . ? C9 C10 H10A 109.9 . . ? N1 C10 H10B 109.9 . . ? C9 C10 H10B 109.9 . . ? H10A C10 H10B 108.3 . . ? C1 C11 H11A 109.5 . . ? C1 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C1 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C1 C12 H12A 109.5 . . ? C1 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C1 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C3 C13 H13A 109.5 . . ? C3 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C3 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C14' C14 C6 95(3) . . ? C14 C14' C6 56(3) . . ? C6 C15 H15A 109.5 . . ? C6 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C6 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C16' C16 C8 103(3) . . ? C16 C16' C8 52(2) . . ? C22 C17 C18 121.0(4) . . ? C22 C17 H17 119.5 . . ? C18 C17 H17 119.5 . . ? C17 C18 C19 118.9(4) . . ? C17 C18 C23 120.2(4) . . ? C19 C18 C23 120.9(4) . . ? C20 C19 C18 120.8(4) . . ? C20 C19 H19 119.6 . . ? C18 C19 H19 119.6 . . ? C21 C20 C19 118.9(4) . . ? C21 C20 C24 119.1(4) . . ? C19 C20 C24 122.0(4) . . ? C22 C21 C20 121.2(4) . . ? C22 C21 H21 119.4 . . ? C20 C21 H21 119.4 . . ? C21 C22 C17 119.1(4) . . ? C21 C22 C25 119.5(4) . . ? C17 C22 C25 121.2(4) . . ? O1 C23 O2 124.3(5) . . ? O1 C23 C18 118.0(4) . . ? O2 C23 C18 117.6(4) . . ? O4 C24 O3 123.8(5) . . ? O4 C24 C20 119.7(5) . . ? O3 C24 C20 116.5(4) . . ? N6 C25 C22 112.4(4) . . ? N6 C25 H25A 109.1 . . ? C22 C25 H25A 109.1 . . ? N6 C25 H25B 109.1 . . ? C22 C25 H25B 109.1 . . ? H25A C25 H25B 107.9 . . ? N6 C26 C27 113.1(4) . . ? N6 C26 H26A 109.0 . . ? C27 C26 H26A 109.0 . . ? N6 C26 H26B 109.0 . . ? C27 C26 H26B 109.0 . . ? H26A C26 H26B 107.8 . . ? N5 C27 C26 110.2(4) . . ? N5 C27 H27A 109.6 . . ? C26 C27 H27A 109.6 . . ? N5 C27 H27B 109.6 . . ? C26 C27 H27B 109.6 . . ? H27A C27 H27B 108.1 . . ? N5 C28 C31 111.4(4) . . ? N5 C28 H28A 109.4 . . ? C31 C28 H28A 109.4 . . ? N5 C28 H28B 109.4 . . ? C31 C28 H28B 109.4 . . ? H28A C28 H28B 108.0 . . ? C24 O3 H3A 109.5 . . ? O6 C29 O5 125.2(6) . . ? O6 C29 C33 117.0(6) . . ? O5 C29 C33 117.7(6) . . ? O7 C30 O8 122.9(6) . . ? O7 C30 C35 123.9(5) . . ? O8 C30 C35 113.2(5) . . ? C32 C31 C36 118.8(5) . . ? C32 C31 C28 121.4(5) . . ? C36 C31 C28 119.7(5) . . ? C31 C32 C33 121.8(5) . . ? C31 C32 H32A 119.1 . . ? C33 C32 H32A 119.1 . . ? C34 C33 C32 118.9(5) . . ? C34 C33 C29 120.0(5) . . ? C32 C33 C29 121.1(5) . . ? C33 C34 C35 121.2(5) . . ? C33 C34 H34A 119.4 . . ? C35 C34 H34A 119.4 . . ? C36 C35 C34 118.7(5) . . ? C36 C35 C30 118.4(5) . . ? C34 C35 C30 122.8(5) . . ? C31 C36 C35 120.4(5) . . ? C31 C36 H36A 119.8 . . ? C35 C36 H36A 119.8 . . ? C38 C37 N6 115.1(4) . . ? C38 C37 H37A 108.5 . . ? N6 C37 H37A 108.5 . . ? C38 C37 H37B 108.5 . . ? N6 C37 H37B 108.5 . . ? H37A C37 H37B 107.5 . . ? C37 C38 C39 110.4(4) . . ? C37 C38 H38A 109.6 . . ? C39 C38 H38A 109.6 . . ? C37 C38 H38B 109.6 . . ? C39 C38 H38B 109.6 . . ? H38A C38 H38B 108.1 . . ? N5 C39 C38 113.0(4) 2_667 . ? N5 C39 H39A 109.0 2_667 . ? C38 C39 H39A 109.0 . . ? N5 C39 H39B 109.0 2_667 . ? C38 C39 H39B 109.0 . . ? H39A C39 H39B 107.8 . . ? C27 N5 C28 111.0(4) . . ? C27 N5 C39 110.8(4) . 2_667 ? C28 N5 C39 111.2(4) . 2_667 ? C26 N6 C25 110.5(4) . . ? C26 N6 C37 114.0(4) . . ? C25 N6 C37 110.3(4) . . ? C30 O8 H8A 109.5 . . ? C10 N1 C1 116.8(6) . . ? C10 N1 Cu1 106.3(4) . . ? C1 N1 Cu1 120.8(4) . . ? C10 N1 H1D 107(5) . . ? C1 N1 H1D 104(5) . . ? Cu1 N1 H1D 99(5) . . ? C4 N2 C3 115.8(5) . . ? C4 N2 Cu1 105.7(4) . . ? C3 N2 Cu1 117.4(4) . . ? C4 N2 H2D 104(5) . . ? C3 N2 H2D 113(5) . . ? Cu1 N2 H2D 100(5) . . ? C5 N3 C6 115.5(5) . . ? C5 N3 Cu1 105.4(4) . . ? C6 N3 Cu1 120.6(4) . . ? C5 N3 H3D 103(5) . . ? C6 N3 H3D 116(4) . . ? Cu1 N3 H3D 93.0(9) . . ? C9 N4 C8 117.4(6) . . ? C9 N4 Cu1 105.7(4) . . ? C8 N4 Cu1 121.6(5) . . ? C9 N4 H4D 117(6) . . ? C8 N4 H4D 112(5) . . ? Cu1 N4 H4D 78(5) . . ? H1A O1W H1B 115(2) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 C1 C2 C3 68.8(7) . . . . ? C11 C1 C2 C3 -55.2(8) . . . . ? C12 C1 C2 C3 -171.5(6) . . . . ? C1 C2 C3 N2 -76.1(7) . . . . ? C1 C2 C3 C13 164.4(6) . . . . ? N2 C4 C5 N3 57.9(7) . . . . ? N3 C6 C7 C8 -71.6(9) . . . . ? C15 C6 C7 C8 168.1(8) . . . . ? C14 C6 C7 C8 50.1(11) . . . . ? C14' C6 C7 C8 57.8(18) . . . . ? C6 C7 C8 C16 -158.6(11) . . . . ? C6 C7 C8 N4 69.2(10) . . . . ? C6 C7 C8 C16' 175.5(9) . . . . ? N4 C9 C10 N1 -55.4(7) . . . . ? N3 C6 C14 C14' -76(3) . . . . ? C7 C6 C14 C14' 168(3) . . . . ? C15 C6 C14 C14' 54(3) . . . . ? N3 C6 C14' C14 115(3) . . . . ? C7 C6 C14' C14 -16(4) . . . . ? C15 C6 C14' C14 -132(3) . . . . ? C7 C8 C16 C16' -109(3) . . . . ? N4 C8 C16 C16' 16(3) . . . . ? C7 C8 C16' C16 78(3) . . . . ? N4 C8 C16' C16 -167(3) . . . . ? C22 C17 C18 C19 0.7(7) . . . . ? C22 C17 C18 C23 179.6(4) . . . . ? C17 C18 C19 C20 -0.2(7) . . . . ? C23 C18 C19 C20 -179.1(4) . . . . ? C18 C19 C20 C21 -1.3(7) . . . . ? C18 C19 C20 C24 177.0(4) . . . . ? C19 C20 C21 C22 2.3(7) . . . . ? C24 C20 C21 C22 -176.1(4) . . . . ? C20 C21 C22 C17 -1.8(7) . . . . ? C20 C21 C22 C25 -178.5(4) . . . . ? C18 C17 C22 C21 0.3(7) . . . . ? C18 C17 C22 C25 176.9(4) . . . . ? C17 C18 C23 O1 -10.5(7) . . . . ? C19 C18 C23 O1 168.4(5) . . . . ? C17 C18 C23 O2 168.6(4) . . . . ? C19 C18 C23 O2 -12.5(7) . . . . ? C21 C20 C24 O4 -24.2(7) . . . . ? C19 C20 C24 O4 157.5(5) . . . . ? C21 C20 C24 O3 153.1(5) . . . . ? C19 C20 C24 O3 -25.2(7) . . . . ? C21 C22 C25 N6 -78.9(5) . . . . ? C17 C22 C25 N6 104.5(5) . . . . ? N6 C26 C27 N5 151.3(4) . . . . ? N5 C28 C31 C32 -133.5(5) . . . . ? N5 C28 C31 C36 50.0(7) . . . . ? C36 C31 C32 C33 -1.9(8) . . . . ? C28 C31 C32 C33 -178.4(5) . . . . ? C31 C32 C33 C34 -0.7(8) . . . . ? C31 C32 C33 C29 179.5(5) . . . . ? O6 C29 C33 C34 167.9(6) . . . . ? O5 C29 C33 C34 -8.0(9) . . . . ? O6 C29 C33 C32 -12.3(9) . . . . ? O5 C29 C33 C32 171.7(6) . . . . ? C32 C33 C34 C35 3.2(8) . . . . ? C29 C33 C34 C35 -177.0(5) . . . . ? C33 C34 C35 C36 -3.1(8) . . . . ? C33 C34 C35 C30 177.0(5) . . . . ? O7 C30 C35 C36 18.8(9) . . . . ? O8 C30 C35 C36 -162.3(5) . . . . ? O7 C30 C35 C34 -161.2(6) . . . . ? O8 C30 C35 C34 17.7(8) . . . . ? C32 C31 C36 C35 2.0(8) . . . . ? C28 C31 C36 C35 178.6(5) . . . . ? C34 C35 C36 C31 0.4(8) . . . . ? C30 C35 C36 C31 -179.6(5) . . . . ? N6 C37 C38 C39 -178.1(4) . . . . ? C37 C38 C39 N5 -57.2(6) . . . 2_667 ? C26 C27 N5 C28 70.7(5) . . . . ? C26 C27 N5 C39 -165.3(4) . . . 2_667 ? C31 C28 N5 C27 -161.8(4) . . . . ? C31 C28 N5 C39 74.5(5) . . . 2_667 ? C27 C26 N6 C25 166.1(4) . . . . ? C27 C26 N6 C37 -69.0(5) . . . . ? C22 C25 N6 C26 -76.7(5) . . . . ? C22 C25 N6 C37 156.3(4) . . . . ? C38 C37 N6 C26 -67.1(5) . . . . ? C38 C37 N6 C25 57.9(5) . . . . ? C9 C10 N1 C1 176.1(5) . . . . ? C9 C10 N1 Cu1 37.8(6) . . . . ? C11 C1 N1 C10 -58.6(9) . . . . ? C12 C1 N1 C10 64.7(8) . . . . ? C2 C1 N1 C10 -176.8(5) . . . . ? C11 C1 N1 Cu1 73.4(9) . . . . ? C12 C1 N1 Cu1 -163.3(6) . . . . ? C2 C1 N1 Cu1 -44.8(7) . . . . ? N3 Cu1 N1 C10 69(3) . . . . ? N2 Cu1 N1 C10 165.7(4) . . . . ? N4 Cu1 N1 C10 -11.1(4) . . . . ? N3 Cu1 N1 C1 -68(3) . . . . ? N2 Cu1 N1 C1 29.4(5) . . . . ? N4 Cu1 N1 C1 -147.4(5) . . . . ? C5 C4 N2 C3 -171.5(5) . . . . ? C5 C4 N2 Cu1 -39.8(6) . . . . ? C2 C3 N2 C4 -177.9(5) . . . . ? C13 C3 N2 C4 -59.8(7) . . . . ? C2 C3 N2 Cu1 56.1(6) . . . . ? C13 C3 N2 Cu1 174.2(5) . . . . ? N3 Cu1 N2 C4 11.6(4) . . . . ? N4 Cu1 N2 C4 -57(4) . . . . ? N1 Cu1 N2 C4 -164.4(4) . . . . ? N3 Cu1 N2 C3 142.4(4) . . . . ? N4 Cu1 N2 C3 74(4) . . . . ? N1 Cu1 N2 C3 -33.6(5) . . . . ? C4 C5 N3 C6 -179.9(5) . . . . ? C4 C5 N3 Cu1 -44.2(6) . . . . ? C7 C6 N3 C5 -179.2(6) . . . . ? C15 C6 N3 C5 -61.2(8) . . . . ? C14 C6 N3 C5 69.5(12) . . . . ? C14' C6 N3 C5 39.9(15) . . . . ? C7 C6 N3 Cu1 52.2(7) . . . . ? C15 C6 N3 Cu1 170.2(5) . . . . ? C14 C6 N3 Cu1 -59.1(12) . . . . ? C14' C6 N3 Cu1 -88.7(14) . . . . ? N2 Cu1 N3 C5 17.9(4) . . . . ? N4 Cu1 N3 C5 -165.2(4) . . . . ? N1 Cu1 N3 C5 115(3) . . . . ? N2 Cu1 N3 C6 150.9(5) . . . . ? N4 Cu1 N3 C6 -32.3(5) . . . . ? N1 Cu1 N3 C6 -112(3) . . . . ? C10 C9 N4 C8 -177.7(6) . . . . ? C10 C9 N4 Cu1 43.0(6) . . . . ? C16 C8 N4 C9 57.6(14) . . . . ? C7 C8 N4 C9 179.2(7) . . . . ? C16' C8 N4 C9 64.3(9) . . . . ? C16 C8 N4 Cu1 -169.9(11) . . . . ? C7 C8 N4 Cu1 -48.3(9) . . . . ? C16' C8 N4 Cu1 -163.2(7) . . . . ? N3 Cu1 N4 C9 166.8(4) . . . . ? N2 Cu1 N4 C9 -125(4) . . . . ? N1 Cu1 N4 C9 -17.2(4) . . . . ? N3 Cu1 N4 C8 29.6(6) . . . . ? N2 Cu1 N4 C8 98(4) . . . . ? N1 Cu1 N4 C8 -154.4(6) . . . . ? _diffrn_measured_fraction_theta_max 0.820 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.971 _refine_diff_density_max 1.369 _refine_diff_density_min -0.673 _refine_diff_density_rms 0.093 #=========================END