data_publication_text _publ_contact_author_name 'Allan J. Jacobson' _publ_contact_author_address ;Department of Chemistry University of Houston Houston, TX 77204-5003 ; _publ_contact_author_email ajjcob@uh.edu _publ_contact_author_phone 713-743-2785 _publ_contact_author_fax 713-743-2787 data_1 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C20 H12 N2 Ni O4' _chemical_formula_weight 403.03 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' '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' 'N' 'N' 0.0061 0.0033 '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' _symmetry_cell_setting ? _symmetry_space_group_name_H-M 'P 21/n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 9.5589(6) _cell_length_b 12.6776(8) _cell_length_c 13.5121(9) _cell_angle_alpha 90.00 _cell_angle_beta 95.4370(10) _cell_angle_gamma 90.00 _cell_volume 1630.08(18) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description polyhedra _exptl_crystal_colour green _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.642 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 824 _exptl_absorpt_coefficient_mu 1.221 _exptl_absorpt_correction_type 'multiscan' _exptl_absorpt_correction_T_min 'Tmin/Tmax ratio 0.8698' _exptl_absorpt_correction_T_max 'Tmin/Tmax ratio 0.8698' _exptl_absorpt_process_details 'SADABS' _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 'SIMENS SMART/CCD' _diffrn_measurement_method 'narrow frame' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9748 _diffrn_reflns_av_R_equivalents 0.0278 _diffrn_reflns_av_sigmaI/netI 0.0331 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 6 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.21 _diffrn_reflns_theta_max 28.34 _reflns_number_total 3713 _reflns_number_gt 3065 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _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^ > 2sigma(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^)+(0.0371P)^2^+0.6800P] 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 3713 _refine_ls_number_parameters 292 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0403 _refine_ls_R_factor_gt 0.0289 _refine_ls_wR_factor_ref 0.0744 _refine_ls_wR_factor_gt 0.0700 _refine_ls_goodness_of_fit_ref 1.005 _refine_ls_restrained_S_all 1.005 _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 C1 C 0.1813(2) 0.58872(16) 0.08909(14) 0.0280(4) Uani 1 1 d . . . C2 C 0.2473(2) 0.68305(17) 0.06697(16) 0.0324(4) Uani 1 1 d . . . C3 C 0.3906(2) 0.68723(17) 0.07337(15) 0.0313(4) Uani 1 1 d . . . C4 C 0.4701(2) 0.59695(16) 0.10113(13) 0.0258(4) Uani 1 1 d . . . C5 C 0.39572(18) 0.50539(15) 0.12085(12) 0.0214(4) Uani 1 1 d . . . C6 C 0.47049(19) 0.40990(15) 0.14860(12) 0.0217(4) Uani 1 1 d . . . C7 C 0.4584(2) 0.23393(17) 0.19042(15) 0.0314(4) Uani 1 1 d . . . C8 C 0.6053(2) 0.22759(18) 0.20501(17) 0.0366(5) Uani 1 1 d . . . C9 C 0.6852(2) 0.31438(19) 0.18992(15) 0.0338(5) Uani 1 1 d . . . C10 C 0.61848(19) 0.40988(16) 0.16003(13) 0.0261(4) Uani 1 1 d . . . C11 C 0.6918(2) 0.50494(18) 0.13973(15) 0.0316(5) Uani 1 1 d . . . C12 C 0.6212(2) 0.59407(18) 0.11064(15) 0.0318(5) Uani 1 1 d . . . C13 C 0.08559(18) 0.20096(15) 0.08638(13) 0.0229(4) Uani 1 1 d . . . C14 C 0.03765(18) 0.09798(15) 0.04056(13) 0.0207(4) Uani 1 1 d . . . C15 C 0.02814(19) 0.08356(15) -0.06205(13) 0.0223(4) Uani 1 1 d . . . C16 C -0.00878(18) -0.01411(15) -0.10231(13) 0.0225(4) Uani 1 1 d . . . C17 C 0.14070(19) 0.47950(16) 0.48985(14) 0.0247(4) Uani 1 1 d . . . C18 C 0.04046(18) 0.46703(14) 0.40870(13) 0.0206(4) Uani 1 1 d . . . C19 C -0.10057(19) 0.48709(15) 0.41929(13) 0.0241(4) Uani 1 1 d . . . C20 C 0.08775(18) 0.43099(14) 0.31129(13) 0.0214(4) Uani 1 1 d . . . O1 O 0.10194(14) 0.28121(10) 0.03277(9) 0.0274(3) Uani 1 1 d . . . O2 O 0.11354(15) 0.20637(11) 0.17960(10) 0.0311(3) Uani 1 1 d . . . O3 O 0.00394(13) 0.42988(12) 0.23313(9) 0.0284(3) Uani 1 1 d . . . O4 O 0.21345(13) 0.40145(11) 0.31004(9) 0.0242(3) Uani 1 1 d . . . Ni1 Ni 0.18276(2) 0.359724(19) 0.163942(16) 0.02117(8) Uani 1 1 d . . . N1 N 0.25251(15) 0.50144(12) 0.11567(11) 0.0221(3) Uani 1 1 d . . . N2 N 0.39246(16) 0.32283(13) 0.16312(11) 0.0232(3) Uani 1 1 d . . . H1 H 0.085(2) 0.5837(17) 0.0859(16) 0.029(6) Uiso 1 1 d . . . H2 H 0.193(2) 0.743(2) 0.0509(17) 0.037(6) Uiso 1 1 d . . . H3 H 0.435(2) 0.749(2) 0.0554(17) 0.036(6) Uiso 1 1 d . . . H7 H 0.400(2) 0.1738(19) 0.2017(17) 0.032(6) Uiso 1 1 d . . . H8 H 0.643(3) 0.168(2) 0.2221(18) 0.039(7) Uiso 1 1 d . . . H9 H 0.785(3) 0.309(2) 0.1977(18) 0.042(7) Uiso 1 1 d . . . H11 H 0.791(2) 0.5047(18) 0.1432(16) 0.031(6) Uiso 1 1 d . . . H12 H 0.670(2) 0.6556(17) 0.0955(16) 0.029(6) Uiso 1 1 d . . . H15 H 0.052(2) 0.1430(18) -0.1028(17) 0.033(6) Uiso 1 1 d . . . H16 H -0.016(2) -0.0273(16) -0.1735(15) 0.024(5) Uiso 1 1 d . . . H17 H 0.231(2) 0.4636(16) 0.4809(15) 0.023(5) Uiso 1 1 d . . . H19 H -0.170(2) 0.4761(16) 0.3637(15) 0.022(5) 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 C1 0.0267(10) 0.0291(11) 0.0280(9) -0.0018(8) 0.0025(8) 0.0066(8) C2 0.0399(12) 0.0249(10) 0.0320(10) 0.0010(9) 0.0016(9) 0.0075(9) C3 0.0418(12) 0.0236(10) 0.0284(10) -0.0011(8) 0.0035(8) -0.0031(9) C4 0.0300(10) 0.0277(10) 0.0193(8) -0.0036(7) 0.0005(7) -0.0020(8) C5 0.0233(9) 0.0250(9) 0.0158(8) -0.0038(7) 0.0007(6) 0.0003(7) C6 0.0239(9) 0.0248(9) 0.0163(8) -0.0045(7) 0.0014(7) 0.0006(7) C7 0.0393(11) 0.0238(10) 0.0308(10) -0.0022(8) 0.0008(9) 0.0046(9) C8 0.0399(12) 0.0306(12) 0.0373(12) -0.0021(9) -0.0067(9) 0.0159(10) C9 0.0270(10) 0.0421(13) 0.0309(10) -0.0076(9) -0.0039(8) 0.0104(9) C10 0.0231(9) 0.0338(11) 0.0209(9) -0.0072(8) -0.0008(7) 0.0027(8) C11 0.0215(10) 0.0440(13) 0.0290(10) -0.0070(9) 0.0005(8) -0.0043(9) C12 0.0306(10) 0.0368(12) 0.0281(10) -0.0030(9) 0.0030(8) -0.0116(9) C13 0.0195(8) 0.0244(10) 0.0245(9) -0.0031(7) 0.0008(7) -0.0016(7) C14 0.0165(8) 0.0229(9) 0.0224(8) -0.0022(7) -0.0007(6) -0.0004(7) C15 0.0220(9) 0.0243(10) 0.0201(8) 0.0019(7) -0.0008(7) -0.0012(7) C16 0.0222(9) 0.0264(10) 0.0184(8) -0.0009(7) -0.0010(6) -0.0001(7) C17 0.0175(8) 0.0296(10) 0.0273(9) -0.0026(8) 0.0034(7) -0.0002(8) C18 0.0217(8) 0.0182(9) 0.0222(8) -0.0006(7) 0.0039(7) -0.0012(7) C19 0.0203(8) 0.0292(10) 0.0224(9) -0.0029(8) -0.0002(7) -0.0018(8) C20 0.0211(9) 0.0214(9) 0.0218(8) -0.0020(7) 0.0034(7) -0.0030(7) O1 0.0349(7) 0.0220(7) 0.0247(7) -0.0010(5) -0.0013(5) -0.0042(6) O2 0.0432(8) 0.0294(7) 0.0205(6) -0.0038(6) 0.0012(6) -0.0109(6) O3 0.0221(6) 0.0405(8) 0.0223(6) -0.0051(6) 0.0003(5) -0.0006(6) O4 0.0205(6) 0.0291(7) 0.0229(6) -0.0057(5) 0.0018(5) 0.0012(5) Ni1 0.02126(13) 0.02199(13) 0.02024(12) -0.00344(9) 0.00189(8) -0.00212(10) N1 0.0220(7) 0.0234(8) 0.0212(7) -0.0034(6) 0.0027(6) 0.0012(6) N2 0.0265(8) 0.0223(8) 0.0208(7) -0.0037(6) 0.0019(6) 0.0034(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds 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 C1 N1 1.331(3) . ? C1 C2 1.398(3) . ? C1 H1 0.92(2) . ? C2 C3 1.365(3) . ? C2 H2 0.93(2) . ? C3 C4 1.405(3) . ? C3 H3 0.94(2) . ? C4 C5 1.400(3) . ? C4 C12 1.438(3) . ? C5 N1 1.365(2) . ? C5 C6 1.437(3) . ? C6 N2 1.357(2) . ? C6 C10 1.408(3) . ? C7 N2 1.327(3) . ? C7 C8 1.402(3) . ? C7 H7 0.96(2) . ? C8 C9 1.366(3) . ? C8 H8 0.86(3) . ? C9 C10 1.410(3) . ? C9 H9 0.95(2) . ? C10 C11 1.434(3) . ? C11 C12 1.355(3) . ? C11 H11 0.94(2) . ? C12 H12 0.94(2) . ? C13 O2 1.265(2) . ? C13 O1 1.267(2) . ? C13 C14 1.498(3) . ? C13 Ni1 2.4141(18) . ? C14 C15 1.393(2) . ? C14 C16 1.395(3) 3 ? C15 C16 1.385(3) . ? C15 H15 0.97(2) . ? C16 C14 1.395(3) 3 ? C16 H16 0.97(2) . ? C17 C19 1.387(3) 3_566 ? C17 C18 1.395(3) . ? C17 H17 0.90(2) . ? C18 C19 1.393(3) . ? C18 C20 1.503(2) . ? C19 C17 1.387(3) 3_566 ? C19 H19 0.96(2) . ? C20 O4 1.260(2) . ? C20 O3 1.264(2) . ? C20 Ni1 2.4389(17) . ? O1 Ni1 2.1141(13) . ? O2 Ni1 2.0709(14) . ? O3 Ni1 2.2113(13) . ? O4 Ni1 2.0379(12) . ? Ni1 N1 2.0445(16) . ? Ni1 N2 2.0593(15) . ? 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 N1 C1 C2 122.65(19) . . ? N1 C1 H1 116.0(14) . . ? C2 C1 H1 121.3(14) . . ? C3 C2 C1 119.4(2) . . ? C3 C2 H2 120.9(14) . . ? C1 C2 H2 119.7(14) . . ? C2 C3 C4 119.9(2) . . ? C2 C3 H3 119.8(14) . . ? C4 C3 H3 120.2(14) . . ? C5 C4 C3 117.05(18) . . ? C5 C4 C12 119.06(19) . . ? C3 C4 C12 123.89(19) . . ? N1 C5 C4 123.06(17) . . ? N1 C5 C6 117.00(16) . . ? C4 C5 C6 119.94(16) . . ? N2 C6 C10 122.97(17) . . ? N2 C6 C5 117.15(16) . . ? C10 C6 C5 119.88(17) . . ? N2 C7 C8 122.1(2) . . ? N2 C7 H7 116.8(14) . . ? C8 C7 H7 121.1(14) . . ? C9 C8 C7 120.0(2) . . ? C9 C8 H8 121.3(17) . . ? C7 C8 H8 118.7(17) . . ? C8 C9 C10 119.37(19) . . ? C8 C9 H9 120.0(15) . . ? C10 C9 H9 120.6(16) . . ? C9 C10 C6 117.02(19) . . ? C9 C10 C11 124.10(18) . . ? C6 C10 C11 118.88(18) . . ? C12 C11 C10 121.14(18) . . ? C12 C11 H11 119.2(14) . . ? C10 C11 H11 119.6(14) . . ? C11 C12 C4 121.03(19) . . ? C11 C12 H12 120.7(14) . . ? C4 C12 H12 118.3(14) . . ? O2 C13 O1 120.00(17) . . ? O2 C13 C14 119.11(17) . . ? O1 C13 C14 120.87(16) . . ? O2 C13 Ni1 59.07(10) . . ? O1 C13 Ni1 61.02(9) . . ? C14 C13 Ni1 174.95(13) . . ? C15 C14 C16 119.82(17) . 3 ? C15 C14 C13 120.95(17) . . ? C16 C14 C13 119.15(16) 3 . ? C16 C15 C14 119.91(17) . . ? C16 C15 H15 122.3(13) . . ? C14 C15 H15 117.7(13) . . ? C15 C16 C14 120.26(16) . 3 ? C15 C16 H16 122.4(12) . . ? C14 C16 H16 117.4(12) 3 . ? C19 C17 C18 120.23(17) 3_566 . ? C19 C17 H17 122.2(13) 3_566 . ? C18 C17 H17 117.5(13) . . ? C19 C18 C17 119.87(16) . . ? C19 C18 C20 121.33(16) . . ? C17 C18 C20 118.80(16) . . ? C17 C19 C18 119.90(16) 3_566 . ? C17 C19 H19 120.6(12) 3_566 . ? C18 C19 H19 119.5(12) . . ? O4 C20 O3 121.01(16) . . ? O4 C20 C18 117.94(15) . . ? O3 C20 C18 121.05(15) . . ? O4 C20 Ni1 56.61(8) . . ? O3 C20 Ni1 64.48(9) . . ? C18 C20 Ni1 173.65(13) . . ? C13 O1 Ni1 87.36(10) . . ? C13 O2 Ni1 89.34(11) . . ? C20 O3 Ni1 84.47(10) . . ? C20 O4 Ni1 92.31(10) . . ? O4 Ni1 N1 93.42(6) . . ? O4 Ni1 N2 90.76(5) . . ? N1 Ni1 N2 81.42(6) . . ? O4 Ni1 O2 99.37(5) . . ? N1 Ni1 O2 167.04(6) . . ? N2 Ni1 O2 96.19(6) . . ? O4 Ni1 O1 160.38(5) . . ? N1 Ni1 O1 104.51(5) . . ? N2 Ni1 O1 99.62(6) . . ? O2 Ni1 O1 63.18(5) . . ? O4 Ni1 O3 62.10(5) . . ? N1 Ni1 O3 94.01(6) . . ? N2 Ni1 O3 152.30(5) . . ? O2 Ni1 O3 93.85(6) . . ? O1 Ni1 O3 107.94(5) . . ? O4 Ni1 C13 130.62(6) . . ? N1 Ni1 C13 135.87(6) . . ? N2 Ni1 C13 98.22(6) . . ? O2 Ni1 C13 31.59(6) . . ? O1 Ni1 C13 31.62(6) . . ? O3 Ni1 C13 103.76(6) . . ? O4 Ni1 C20 31.08(5) . . ? N1 Ni1 C20 95.33(6) . . ? N2 Ni1 C20 121.77(6) . . ? O2 Ni1 C20 96.72(6) . . ? O1 Ni1 C20 136.39(6) . . ? O3 Ni1 C20 31.05(5) . . ? C13 Ni1 C20 120.37(6) . . ? C1 N1 C5 117.92(17) . . ? C1 N1 Ni1 130.01(13) . . ? C5 N1 Ni1 111.82(12) . . ? C7 N2 C6 118.56(17) . . ? C7 N2 Ni1 128.96(14) . . ? C6 N2 Ni1 111.39(12) . . ? _diffrn_measured_fraction_theta_max 0.915 _diffrn_reflns_theta_full 28.34 _diffrn_measured_fraction_theta_full 0.915 _refine_diff_density_max 0.371 _refine_diff_density_min -0.315 _refine_diff_density_rms 0.057 #===END data_2 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C48 H30 N4 Ni2 O14' _chemical_formula_weight 1004.18 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' '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' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ? _symmetry_space_group_name_H-M 'P 21/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 20.532(3) _cell_length_b 21.505(3) _cell_length_c 18.872(3) _cell_angle_alpha 90.00 _cell_angle_beta 93.862(3) _cell_angle_gamma 90.00 _cell_volume 8314(2) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'plate' _exptl_crystal_colour 'green' _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.125 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.605 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4112 _exptl_absorpt_coefficient_mu 0.986 _exptl_absorpt_correction_type 'multiscan' _exptl_absorpt_correction_T_min 'Tmin/Tmax ratio 0.7550' _exptl_absorpt_correction_T_max 'Tmin/Tmax ratio 0.7550' _exptl_absorpt_process_details 'SADABS' _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 'SIMENS SMART / CCD' _diffrn_measurement_method 'narrow frame' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 53078 _diffrn_reflns_av_R_equivalents 0.0753 _diffrn_reflns_av_sigmaI/netI 0.1208 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 0.99 _diffrn_reflns_theta_max 28.68 _reflns_number_total 19350 _reflns_number_gt 6398 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _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^ > 2sigma(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^)+(0.0476P)^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 19350 _refine_ls_number_parameters 1225 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.2134 _refine_ls_R_factor_gt 0.0573 _refine_ls_wR_factor_ref 0.1465 _refine_ls_wR_factor_gt 0.1032 _refine_ls_goodness_of_fit_ref 0.948 _refine_ls_restrained_S_all 0.948 _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 C1 C 0.5337(3) 0.3965(3) 0.6318(3) 0.0423(16) Uani 1 1 d . . . H1 H 0.5422 0.3542 0.6364 0.051 Uiso 1 1 calc R . . C1S C 0.0741(3) 0.3740(3) 0.3996(3) 0.0424(15) Uani 1 1 d . . . C2 C 0.5758(3) 0.4379(3) 0.6673(3) 0.0482(16) Uani 1 1 d . . . H2 H 0.6118 0.4239 0.6953 0.058 Uiso 1 1 calc R . . C2S C 0.1254(3) 0.3769(3) 0.3468(3) 0.0361(14) Uani 1 1 d . . . C3 C 0.5632(3) 0.5001(3) 0.6601(3) 0.0534(19) Uani 1 1 d . . . H3 H 0.5910 0.5290 0.6830 0.064 Uiso 1 1 calc R . . C3S C 0.1240(3) 0.3357(2) 0.2911(3) 0.0403(15) Uani 1 1 d . . . H3S H 0.0905 0.3066 0.2854 0.048 Uiso 1 1 calc R . . C4 C 0.5095(3) 0.5201(3) 0.6189(3) 0.0408(16) Uani 1 1 d . . . H4 H 0.5004 0.5623 0.6145 0.049 Uiso 1 1 calc R . . C4S C 0.1724(3) 0.3373(3) 0.2434(3) 0.0432(16) Uani 1 1 d . . . H4S H 0.1713 0.3090 0.2060 0.052 Uiso 1 1 calc R . . C5 C 0.4687(3) 0.4766(3) 0.5839(3) 0.0300(14) Uani 1 1 d . . . C5S C 0.2219(3) 0.3801(3) 0.2507(3) 0.0355(14) Uani 1 1 d . . . C6 C 0.4096(3) 0.4927(3) 0.5385(2) 0.0309(14) Uani 1 1 d . . . C6S C 0.2220(3) 0.4230(3) 0.3058(3) 0.0570(18) Uani 1 1 d . . . H6S H 0.2544 0.4532 0.3104 0.068 Uiso 1 1 calc R . . C7 C 0.3903(3) 0.5541(3) 0.5255(3) 0.0439(16) Uani 1 1 d . . . H7 H 0.4148 0.5872 0.5447 0.053 Uiso 1 1 calc R . . C7S C 0.1741(3) 0.4211(3) 0.3539(3) 0.062(2) Uani 1 1 d . . . H7S H 0.1747 0.4496 0.3910 0.074 Uiso 1 1 calc R . . C8 C 0.3340(3) 0.5642(3) 0.4833(3) 0.0509(18) Uani 1 1 d . . . H8 H 0.3200 0.6046 0.4736 0.061 Uiso 1 1 calc R . . C8S C 0.2745(3) 0.3804(3) 0.1992(3) 0.0347(13) Uani 1 1 d . . . C9 C 0.2992(3) 0.5156(3) 0.4559(3) 0.0440(16) Uani 1 1 d . . . H9 H 0.2608 0.5223 0.4278 0.053 Uiso 1 1 calc R . . C9S C 0.4066(3) 0.3771(3) 0.0671(3) 0.0382(14) Uani 1 1 d . . . C10 C 0.3209(3) 0.4561(3) 0.4700(3) 0.0384(15) Uani 1 1 d . . . H10 H 0.2970 0.4227 0.4507 0.046 Uiso 1 1 calc R . . C10S C 0.4583(3) 0.3756(3) 0.0137(3) 0.0341(14) Uani 1 1 d . . . C11 C 0.2786(3) 0.4106(3) 0.8708(3) 0.0370(15) Uani 1 1 d . . . H11 H 0.2919 0.3694 0.8756 0.044 Uiso 1 1 calc R . . C11S C 0.4534(3) 0.3332(2) -0.0422(3) 0.0421(15) Uani 1 1 d . . . H11S H 0.4185 0.3056 -0.0465 0.050 Uiso 1 1 calc R . . C12 C 0.3151(3) 0.4564(3) 0.9056(3) 0.0473(17) Uani 1 1 d . . . H12 H 0.3533 0.4463 0.9325 0.057 Uiso 1 1 calc R . . C12S C 0.5004(3) 0.3320(2) -0.0913(3) 0.0428(15) Uani 1 1 d . . . H12S H 0.4969 0.3034 -0.1283 0.051 Uiso 1 1 calc R . . C13 C 0.2948(3) 0.5173(3) 0.9001(3) 0.0468(17) Uani 1 1 d . . . H13 H 0.3188 0.5488 0.9233 0.056 Uiso 1 1 calc R . . C13S C 0.5524(3) 0.3726(3) -0.0861(3) 0.0355(15) Uani 1 1 d . . . C14 C 0.2384(3) 0.5307(3) 0.8597(3) 0.0368(15) Uani 1 1 d . . . H14 H 0.2233 0.5714 0.8562 0.044 Uiso 1 1 calc R . . C14S C 0.5575(3) 0.4152(3) -0.0310(3) 0.0447(16) Uani 1 1 d . . . H14S H 0.5925 0.4428 -0.0272 0.054 Uiso 1 1 calc R . . C15 C 0.2043(3) 0.4835(3) 0.8243(2) 0.0294(14) Uani 1 1 d . . . C15S C 0.5105(3) 0.4171(3) 0.0186(3) 0.0406(15) Uani 1 1 d . . . H15S H 0.5139 0.4461 0.0553 0.049 Uiso 1 1 calc R . . C16 C 0.1454(3) 0.4945(3) 0.7763(2) 0.0290(14) Uani 1 1 d . . . C16S C 0.6033(3) 0.3703(3) -0.1403(3) 0.0381(14) Uani 1 1 d . . . C17 C 0.1205(3) 0.5530(2) 0.7613(3) 0.0368(15) Uani 1 1 d . . . H17 H 0.1390 0.5882 0.7832 0.044 Uiso 1 1 calc R . . C17S C 0.7390(3) 0.3619(3) -0.2719(3) 0.0383(14) Uani 1 1 d . . . C18 C 0.0679(3) 0.5577(3) 0.7132(3) 0.0497(17) Uani 1 1 d . . . H18 H 0.0499 0.5965 0.7024 0.060 Uiso 1 1 calc R . . C18S C -0.2104(3) 0.3638(3) 0.6757(3) 0.0338(14) Uani 1 1 d . . . C19 C 0.0416(3) 0.5059(3) 0.6811(3) 0.0478(16) Uani 1 1 d . . . H19 H 0.0066 0.5093 0.6474 0.057 Uiso 1 1 calc R . . C19S C -0.2140(3) 0.3255(2) 0.6160(3) 0.0385(14) Uani 1 1 d . . . H19S H -0.2497 0.2993 0.6080 0.046 Uiso 1 1 calc R . . C20 C 0.0675(3) 0.4484(3) 0.6991(3) 0.0381(15) Uani 1 1 d . . . H20 H 0.0489 0.4129 0.6781 0.046 Uiso 1 1 calc R . . C20S C -0.1660(3) 0.3257(2) 0.5683(3) 0.0384(15) Uani 1 1 d . . . H20S H -0.1690 0.2995 0.5290 0.046 Uiso 1 1 calc R . . C21 C 0.4394(3) 0.5515(3) 0.7862(3) 0.0383(15) Uani 1 1 d . . . H21 H 0.4604 0.5869 0.8045 0.046 Uiso 1 1 calc R . . C21S C -0.1134(3) 0.3652(3) 0.5798(3) 0.0351(14) Uani 1 1 d . . . C22 C 0.4665(3) 0.4941(3) 0.8017(3) 0.0450(16) Uani 1 1 d . . . H22 H 0.5049 0.4905 0.8306 0.054 Uiso 1 1 calc R . . C22S C -0.1092(3) 0.4038(3) 0.6391(3) 0.0503(17) Uani 1 1 d . . . H22S H -0.0736 0.4302 0.6469 0.060 Uiso 1 1 calc R . . C23 C 0.4352(3) 0.4418(3) 0.7732(3) 0.0528(19) Uani 1 1 d . . . H23 H 0.4529 0.4025 0.7822 0.063 Uiso 1 1 calc R . . C23S C -0.1575(3) 0.4033(3) 0.6865(3) 0.0494(17) Uani 1 1 d . . . H23S H -0.1544 0.4295 0.7257 0.059 Uiso 1 1 calc R . . C24 C 0.3778(3) 0.4480(3) 0.7314(3) 0.0432(16) Uani 1 1 d . . . H24 H 0.3558 0.4133 0.7128 0.052 Uiso 1 1 calc R . . C24S C -0.0590(3) 0.3659(3) 0.5306(3) 0.0430(15) Uani 1 1 d . . . C25 C 0.3538(3) 0.5073(3) 0.7177(2) 0.0287(14) Uani 1 1 d . . . C26 C 0.2931(3) 0.5191(3) 0.6718(2) 0.0301(14) Uani 1 1 d . . . C27 C 0.2570(3) 0.4719(3) 0.6372(3) 0.0387(15) Uani 1 1 d . . . H27 H 0.2699 0.4306 0.6421 0.046 Uiso 1 1 calc R . . C28 C 0.2023(3) 0.4875(3) 0.5958(3) 0.0511(18) Uani 1 1 d . . . H28 H 0.1774 0.4568 0.5721 0.061 Uiso 1 1 calc R . . C29 C 0.1844(3) 0.5486(3) 0.5895(3) 0.0476(17) Uani 1 1 d . . . H29 H 0.1471 0.5598 0.5617 0.057 Uiso 1 1 calc R . . C30 C 0.2222(3) 0.5935(3) 0.6249(3) 0.0384(15) Uani 1 1 d . . . H30 H 0.2097 0.6349 0.6201 0.046 Uiso 1 1 calc R . . C31 C 0.1876(3) 0.5545(3) 1.0459(3) 0.0392(15) Uani 1 1 d . . . H31 H 0.2060 0.5907 1.0652 0.047 Uiso 1 1 calc R . . C32 C 0.2167(3) 0.4985(3) 1.0650(3) 0.0553(18) Uani 1 1 d . . . H32 H 0.2533 0.4967 1.0968 0.066 Uiso 1 1 calc R . . C33 C 0.1890(3) 0.4454(3) 1.0347(3) 0.0549(19) Uani 1 1 d . . . H33 H 0.2077 0.4068 1.0449 0.066 Uiso 1 1 calc R . . C34 C 0.1339(3) 0.4496(3) 0.9896(3) 0.0430(16) Uani 1 1 d . . . H34 H 0.1146 0.4139 0.9698 0.052 Uiso 1 1 calc R . . C35 C 0.1075(3) 0.5074(2) 0.9741(3) 0.0286(14) Uani 1 1 d . . . C36 C 0.0486(3) 0.5161(3) 0.9264(2) 0.0244(13) Uani 1 1 d . . . C37 C 0.0156(3) 0.4666(3) 0.8929(3) 0.0372(15) Uani 1 1 d . . . H37 H 0.0302 0.4259 0.8991 0.045 Uiso 1 1 calc R . . C38 C -0.0395(3) 0.4804(3) 0.8503(3) 0.0440(16) Uani 1 1 d . . . H38 H -0.0630 0.4484 0.8273 0.053 Uiso 1 1 calc R . . C39 C -0.0599(3) 0.5402(3) 0.8415(3) 0.0458(17) Uani 1 1 d . . . H39 H -0.0970 0.5494 0.8124 0.055 Uiso 1 1 calc R . . C40 C -0.0250(3) 0.5870(3) 0.8761(3) 0.0380(15) Uani 1 1 d . . . H40 H -0.0389 0.6280 0.8701 0.046 Uiso 1 1 calc R . . C41 C 0.4056(3) 0.3207(2) 0.4136(3) 0.0258(13) Uani 1 1 d . . . C42 C 0.4026(3) 0.2959(2) 0.3395(2) 0.0251(13) Uani 1 1 d . . . C43 C 0.4562(3) 0.3033(2) 0.2980(2) 0.0305(14) Uani 1 1 d . . . H43 H 0.4925 0.3258 0.3155 0.037 Uiso 1 1 calc R . . C44 C 0.4550(3) 0.2769(2) 0.2310(3) 0.0305(14) Uani 1 1 d . . . H44 H 0.4899 0.2825 0.2027 0.037 Uiso 1 1 calc R . . C45 C 0.4007(3) 0.2584(2) 0.7059(2) 0.0266(13) Uani 1 1 d . . . C46 C 0.3481(3) 0.2353(2) 0.2464(3) 0.0306(14) Uani 1 1 d . . . H46 H 0.3119 0.2126 0.2292 0.037 Uiso 1 1 calc R . . C47 C 0.3488(3) 0.2629(2) 0.3129(3) 0.0320(14) Uani 1 1 d . . . H47 H 0.3127 0.2590 0.3398 0.038 Uiso 1 1 calc R . . C48 C 0.4028(3) 0.2923(2) 0.6371(3) 0.0250(13) Uani 1 1 d . . . C49 C 0.1578(3) 0.3136(2) 0.6629(3) 0.0248(13) Uani 1 1 d . . . C50 C 0.1554(3) 0.2858(2) 0.5894(3) 0.0302(14) Uani 1 1 d . . . C51 C 0.2105(3) 0.2902(2) 0.5509(2) 0.0352(15) Uani 1 1 d . . . H51 H 0.2475 0.3108 0.5699 0.042 Uiso 1 1 calc R . . C52 C 0.2100(3) 0.2364(2) 0.9841(3) 0.0358(15) Uani 1 1 d . . . H52 H 0.2465 0.2332 0.9577 0.043 Uiso 1 1 calc R . . C53 C 0.1552(3) 0.2676(2) 0.9566(2) 0.0263(13) Uani 1 1 d . . . C54 C 0.1004(3) 0.2726(2) 0.9963(3) 0.0324(14) Uani 1 1 d . . . H54 H 0.0638 0.2944 0.9783 0.039 Uiso 1 1 calc R . . C55 C 0.1009(3) 0.2550(2) 0.5623(3) 0.0297(14) Uani 1 1 d . . . H55 H 0.0642 0.2527 0.5884 0.036 Uiso 1 1 calc R . . C56 C 0.1561(3) 0.3007(2) 0.8862(2) 0.0258(13) Uani 1 1 d . . . C57 C 0.3470(3) 0.7061(2) 0.6169(2) 0.0261(13) Uani 1 1 d . . . C58 C 0.3481(3) 0.7396(2) 0.5481(2) 0.0260(13) Uani 1 1 d . . . C59 C 0.4013(2) 0.7311(2) 0.5051(2) 0.0251(13) Uani 1 1 d . . . H59 H 0.4368 0.7070 0.5215 0.030 Uiso 1 1 calc R . . C60 C 0.4007(3) 0.7413(2) 0.9383(2) 0.0260(13) Uani 1 1 d . . . H60 H 0.4363 0.7461 0.9107 0.031 Uiso 1 1 calc R . . C61 C 0.3473(3) 0.7065(2) 0.9128(2) 0.0261(13) Uani 1 1 d . . . C62 C 0.2952(3) 0.8031(2) 0.4560(3) 0.0307(14) Uani 1 1 d . . . H62 H 0.2600 0.8276 0.4396 0.037 Uiso 1 1 calc R . . C63 C 0.2958(3) 0.7765(2) 0.5227(2) 0.0280(13) Uani 1 1 d . . . H63 H 0.2610 0.7832 0.5509 0.034 Uiso 1 1 calc R . . C64 C 0.3443(3) 0.6821(2) 0.8386(2) 0.0253(13) Uani 1 1 d . . . C65 C 0.0947(3) 0.7007(2) 0.8619(3) 0.0248(13) Uani 1 1 d . . . C66 C 0.0948(3) 0.7307(2) 0.7906(2) 0.0263(13) Uani 1 1 d . . . C67 C 0.0413(3) 0.7639(2) 0.7643(3) 0.0302(14) Uani 1 1 d . . . H67 H 0.0060 0.7690 0.7921 0.036 Uiso 1 1 calc R . . C68 C 0.0393(3) 0.7104(2) 1.1974(3) 0.0326(14) Uani 1 1 d . . . H68 H 0.0022 0.6895 1.1793 0.039 Uiso 1 1 calc R . . C69 C 0.0934(3) 0.7160(2) 1.1568(2) 0.0240(13) Uani 1 1 d . . . C70 C 0.1486(3) 0.7475(2) 1.1840(3) 0.0311(14) Uani 1 1 d . . . H70 H 0.1851 0.7503 1.1576 0.037 Uiso 1 1 calc R . . C71 C 0.1491(3) 0.7256(2) 0.7498(3) 0.0292(13) Uani 1 1 d . . . H71 H 0.1858 0.7038 0.7676 0.035 Uiso 1 1 calc R . . C72 C 0.0923(3) 0.6879(2) 1.0841(3) 0.0277(14) Uani 1 1 d . . . N1 N 0.4812(2) 0.4149(2) 0.5908(2) 0.0319(12) Uani 1 1 d . . . N2 N 0.3761(2) 0.44490(19) 0.5113(2) 0.0286(11) Uani 1 1 d . . . N3 N 0.2246(2) 0.4239(2) 0.8305(2) 0.0279(11) Uani 1 1 d . . . N4 N 0.1188(2) 0.44289(19) 0.7462(2) 0.0254(10) Uani 1 1 d . . . N5 N 0.3842(2) 0.55815(19) 0.7458(2) 0.0285(11) Uani 1 1 d . . . N6 N 0.2760(2) 0.5797(2) 0.6659(2) 0.0291(11) Uani 1 1 d . . . N7 N 0.1348(2) 0.5595(2) 1.0017(2) 0.0298(11) Uani 1 1 d . . . N8 N 0.0286(2) 0.5752(2) 0.9183(2) 0.0292(11) Uani 1 1 d . . . O1 O 0.45762(17) 0.34809(15) 0.43910(15) 0.0285(9) Uani 1 1 d . . . O1S O 0.0815(2) 0.4091(2) 0.4538(2) 0.0644(14) Uani 1 1 d . . . O2 O 0.35850(18) 0.31357(16) 0.45212(16) 0.0333(9) Uani 1 1 d . . . O2S O 0.0270(2) 0.33857(19) 0.3871(2) 0.0503(12) Uani 1 1 d . . . O3 O 0.44597(18) 0.27918(15) 0.59390(16) 0.0311(9) Uani 1 1 d . . . O3S O 0.2693(2) 0.34545(18) 0.14684(19) 0.0484(11) Uani 1 1 d . . . O4 O 0.36338(18) 0.33625(15) 0.62250(16) 0.0296(9) Uani 1 1 d . . . O4S O 0.3235(2) 0.41716(19) 0.2124(2) 0.0591(13) Uani 1 1 d . . . O5 O 0.20735(17) 0.34462(15) 0.68547(16) 0.0294(9) Uani 1 1 d . . . O5S O 0.4148(2) 0.4123(2) 0.1198(2) 0.0645(14) Uani 1 1 d . . . O6 O 0.11085(17) 0.30655(15) 0.70124(16) 0.0289(9) Uani 1 1 d . . . O6S O 0.3556(2) 0.34436(19) 0.05304(19) 0.0514(11) Uani 1 1 d . . . O7 O 0.20014(18) 0.28839(15) 0.84459(16) 0.0319(9) Uani 1 1 d . . . O7S O 0.5972(2) 0.33201(19) -0.18912(19) 0.0520(12) Uani 1 1 d . . . O8 O 0.11348(17) 0.34121(15) 0.86919(16) 0.0290(9) Uani 1 1 d . . . O8S O 0.6515(2) 0.4081(2) -0.1313(2) 0.0635(14) Uani 1 1 d . . . O9 O 0.38856(17) 0.66386(15) 0.63143(16) 0.0289(9) Uani 1 1 d . . . O9S O 0.6939(2) 0.3212(2) -0.2808(2) 0.0637(14) Uani 1 1 d . . . O10 O 0.30331(17) 0.71784(15) 0.65801(16) 0.0331(10) Uani 1 1 d . . . O10S O 0.7417(2) 0.3986(2) -0.2214(2) 0.0714(15) Uani 1 1 d . . . O11 O 0.39204(17) 0.69057(15) 0.80010(16) 0.0324(9) Uani 1 1 d . . . O11S O -0.0669(2) 0.33416(19) 0.4741(2) 0.0534(12) Uani 1 1 d . . . O12 O 0.29470(17) 0.65321(15) 0.81399(16) 0.0309(9) Uani 1 1 d . . . O12S O -0.0101(2) 0.3986(2) 0.5457(2) 0.0719(15) Uani 1 1 d . . . O13 O 0.05079(18) 0.71240(15) 0.90291(16) 0.0310(9) Uani 1 1 d . . . O14 O 0.13886(17) 0.66020(15) 0.87940(15) 0.0282(9) Uani 1 1 d . . . O15 O 0.04376(18) 0.65657(15) 1.06079(16) 0.0307(9) Uani 1 1 d . . . O16 O 0.14016(18) 0.69534(15) 1.04626(16) 0.0316(9) Uani 1 1 d . . . Ni1 Ni 0.41418(3) 0.35894(3) 0.53503(3) 0.02535(18) Uani 1 1 d . . . Ni2 Ni 0.16292(3) 0.36107(3) 0.77915(3) 0.02464(18) Uani 1 1 d . . . Ni3 Ni 0.33941(3) 0.64075(3) 0.71945(3) 0.02459(18) Uani 1 1 d . . . Ni4 Ni 0.08910(3) 0.63975(3) 0.96893(3) 0.02470(18) Uani 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 C1 0.042(4) 0.049(4) 0.036(3) -0.004(3) 0.002(3) 0.002(3) C1S 0.033(4) 0.051(4) 0.043(4) 0.006(3) 0.005(3) 0.005(3) C2 0.033(4) 0.065(5) 0.045(4) -0.002(3) -0.004(3) -0.002(3) C2S 0.033(4) 0.041(4) 0.035(3) 0.003(3) 0.006(3) 0.001(3) C3 0.054(5) 0.067(5) 0.039(4) -0.003(3) 0.004(3) -0.024(4) C3S 0.037(4) 0.034(3) 0.052(4) 0.001(3) 0.018(3) -0.009(3) C4 0.056(5) 0.035(4) 0.031(3) -0.002(3) 0.005(3) -0.015(3) C4S 0.050(4) 0.038(4) 0.043(4) -0.006(3) 0.016(3) 0.005(3) C5 0.036(4) 0.035(4) 0.020(3) -0.004(2) 0.007(2) -0.006(3) C5S 0.030(3) 0.050(4) 0.027(3) 0.000(3) 0.007(3) 0.005(3) C6 0.043(4) 0.032(3) 0.019(3) 0.001(2) 0.013(3) 0.003(3) C6S 0.045(4) 0.080(5) 0.048(4) -0.013(3) 0.015(3) -0.028(4) C7 0.059(5) 0.035(4) 0.039(4) -0.001(3) 0.007(3) -0.003(3) C7S 0.053(5) 0.088(5) 0.046(4) -0.025(4) 0.018(3) -0.019(4) C8 0.070(5) 0.038(4) 0.045(4) 0.005(3) 0.012(4) 0.013(4) C8S 0.031(3) 0.042(4) 0.032(3) 0.000(3) 0.005(3) 0.011(3) C9 0.051(4) 0.043(4) 0.037(3) 0.003(3) 0.000(3) 0.008(3) C9S 0.037(4) 0.038(4) 0.040(4) 0.006(3) 0.008(3) 0.005(3) C10 0.041(4) 0.034(3) 0.041(3) -0.008(3) 0.002(3) -0.003(3) C10S 0.031(3) 0.044(4) 0.028(3) 0.005(3) 0.004(3) 0.005(3) C11 0.031(4) 0.039(4) 0.040(3) 0.000(3) -0.002(3) 0.000(3) C11S 0.040(4) 0.040(4) 0.047(4) 0.001(3) 0.009(3) 0.000(3) C12 0.033(4) 0.064(5) 0.043(4) 0.006(3) -0.012(3) 0.000(4) C12S 0.051(4) 0.038(3) 0.042(3) -0.004(3) 0.018(3) 0.003(3) C13 0.053(5) 0.045(4) 0.040(4) -0.007(3) -0.012(3) -0.018(3) C13S 0.036(4) 0.038(4) 0.033(3) 0.008(3) 0.005(3) 0.005(3) C14 0.040(4) 0.038(4) 0.031(3) 0.003(3) -0.003(3) -0.006(3) C14S 0.041(4) 0.055(4) 0.039(3) 0.000(3) 0.005(3) -0.005(3) C15 0.039(4) 0.030(4) 0.020(3) 0.003(3) 0.006(3) -0.002(3) C15S 0.046(4) 0.047(4) 0.030(3) -0.009(3) 0.011(3) -0.002(3) C16 0.030(3) 0.039(4) 0.018(3) -0.002(3) 0.007(2) 0.001(3) C16S 0.044(4) 0.041(4) 0.031(3) 0.013(3) 0.013(3) 0.005(3) C17 0.047(4) 0.025(3) 0.039(4) -0.003(3) 0.006(3) 0.003(3) C17S 0.034(3) 0.048(4) 0.033(3) 0.000(3) 0.007(3) 0.004(3) C18 0.049(4) 0.046(4) 0.052(4) 0.011(3) -0.008(3) 0.014(3) C18S 0.033(3) 0.034(3) 0.036(3) -0.004(3) 0.007(3) 0.004(3) C19 0.035(4) 0.055(4) 0.051(4) 0.006(3) -0.011(3) 0.000(3) C19S 0.037(4) 0.040(4) 0.039(3) -0.003(3) 0.010(3) -0.011(3) C20 0.027(4) 0.045(4) 0.042(4) 0.006(3) -0.007(3) -0.003(3) C20S 0.044(4) 0.042(4) 0.031(3) 0.001(3) 0.011(3) -0.002(3) C21 0.039(4) 0.039(4) 0.037(3) 0.000(3) -0.001(3) 0.007(3) C21S 0.029(3) 0.043(4) 0.033(3) 0.001(3) 0.005(3) -0.001(3) C22 0.050(4) 0.054(4) 0.031(3) 0.004(3) 0.002(3) 0.022(4) C22S 0.024(3) 0.066(4) 0.061(4) -0.010(3) 0.008(3) -0.020(3) C23 0.079(5) 0.036(4) 0.044(4) 0.004(3) 0.008(4) 0.029(4) C23S 0.041(4) 0.066(4) 0.043(4) -0.023(3) 0.014(3) -0.008(3) C24 0.069(5) 0.029(4) 0.032(3) -0.001(3) 0.007(3) 0.008(3) C24S 0.031(4) 0.055(4) 0.044(4) 0.006(3) 0.008(3) 0.001(3) C25 0.041(4) 0.028(4) 0.019(3) 0.000(2) 0.015(3) -0.002(3) C26 0.035(4) 0.038(4) 0.019(3) 0.002(3) 0.008(3) -0.006(3) C27 0.050(4) 0.034(4) 0.034(3) -0.005(3) 0.012(3) -0.012(3) C28 0.041(4) 0.064(5) 0.047(4) 0.000(3) -0.004(3) -0.021(4) C29 0.040(4) 0.064(5) 0.038(4) -0.003(3) -0.008(3) -0.008(4) C30 0.032(4) 0.054(4) 0.028(3) 0.007(3) -0.002(3) 0.010(3) C31 0.043(4) 0.044(4) 0.029(3) -0.003(3) -0.004(3) 0.010(3) C32 0.052(5) 0.061(5) 0.050(4) 0.001(4) -0.020(3) 0.016(4) C33 0.073(5) 0.039(4) 0.052(4) 0.006(3) 0.005(4) 0.015(4) C34 0.051(5) 0.045(4) 0.032(3) -0.001(3) -0.005(3) -0.001(4) C35 0.038(4) 0.021(3) 0.027(3) 0.001(3) 0.005(3) 0.000(3) C36 0.028(4) 0.025(4) 0.022(3) -0.001(2) 0.010(3) -0.002(3) C37 0.042(4) 0.029(4) 0.041(4) 0.003(3) 0.002(3) -0.003(3) C38 0.043(4) 0.044(4) 0.044(4) -0.004(3) -0.007(3) -0.019(3) C39 0.036(4) 0.052(4) 0.048(4) 0.003(3) -0.010(3) -0.009(3) C40 0.034(4) 0.039(4) 0.040(4) 0.003(3) 0.001(3) 0.000(3) C41 0.028(4) 0.019(3) 0.030(3) -0.001(2) 0.000(3) -0.003(3) C42 0.030(4) 0.027(3) 0.019(3) -0.002(2) 0.004(3) 0.002(3) C43 0.024(3) 0.039(4) 0.029(3) -0.003(3) 0.006(3) -0.007(3) C44 0.024(3) 0.041(4) 0.027(3) 0.000(3) 0.011(3) -0.007(3) C45 0.023(3) 0.037(4) 0.020(3) 0.002(2) 0.005(2) 0.001(3) C46 0.025(4) 0.040(4) 0.027(3) -0.005(3) 0.006(3) -0.003(3) C47 0.030(4) 0.043(4) 0.024(3) -0.003(3) 0.006(3) 0.001(3) C48 0.023(3) 0.030(3) 0.022(3) -0.003(2) 0.006(3) -0.004(3) C49 0.027(4) 0.021(3) 0.026(3) 0.000(2) 0.001(3) 0.003(3) C50 0.036(4) 0.034(4) 0.022(3) 0.000(2) 0.010(3) -0.001(3) C51 0.038(4) 0.043(4) 0.024(3) -0.008(3) 0.001(3) -0.011(3) C52 0.030(4) 0.048(4) 0.031(3) 0.003(3) 0.012(3) 0.009(3) C53 0.032(4) 0.027(3) 0.020(3) -0.003(2) 0.002(3) -0.003(3) C54 0.027(4) 0.040(4) 0.031(3) 0.008(3) 0.006(3) 0.008(3) C55 0.028(4) 0.030(3) 0.032(3) -0.007(3) 0.012(3) -0.005(3) C56 0.021(3) 0.037(4) 0.019(3) -0.001(2) 0.003(3) 0.000(3) C57 0.033(4) 0.025(3) 0.021(3) 0.000(2) 0.003(3) -0.005(3) C58 0.027(4) 0.028(3) 0.024(3) -0.003(2) 0.007(3) -0.006(3) C59 0.022(3) 0.029(3) 0.024(3) 0.004(2) -0.001(2) 0.006(3) C60 0.023(3) 0.033(3) 0.023(3) 0.002(2) 0.010(3) -0.003(3) C61 0.030(4) 0.022(3) 0.026(3) -0.001(2) 0.001(3) 0.000(3) C62 0.028(4) 0.028(3) 0.038(3) -0.001(3) 0.013(3) 0.001(3) C63 0.029(4) 0.033(3) 0.023(3) 0.005(2) 0.006(3) 0.001(3) C64 0.026(4) 0.028(3) 0.023(3) 0.004(2) 0.010(3) 0.006(3) C65 0.025(4) 0.026(3) 0.023(3) -0.003(2) 0.001(3) -0.004(3) C66 0.029(4) 0.032(3) 0.018(3) 0.002(2) 0.005(3) -0.003(3) C67 0.024(3) 0.041(4) 0.027(3) 0.005(3) 0.011(3) 0.005(3) C68 0.019(3) 0.046(4) 0.033(3) -0.009(3) 0.006(3) -0.008(3) C69 0.024(3) 0.025(3) 0.023(3) -0.002(2) -0.001(2) 0.004(3) C70 0.028(4) 0.045(4) 0.021(3) -0.003(3) 0.008(3) 0.000(3) C71 0.023(3) 0.035(3) 0.031(3) 0.001(3) 0.004(3) 0.005(3) C72 0.034(4) 0.029(3) 0.020(3) 0.004(2) 0.006(3) -0.003(3) N1 0.032(3) 0.038(3) 0.026(2) -0.003(2) 0.003(2) -0.004(2) N2 0.031(3) 0.029(3) 0.026(2) -0.003(2) 0.004(2) -0.004(2) N3 0.025(3) 0.035(3) 0.024(2) 0.000(2) -0.002(2) -0.004(2) N4 0.025(3) 0.029(3) 0.022(2) -0.002(2) 0.004(2) 0.002(2) N5 0.034(3) 0.032(3) 0.020(2) 0.001(2) 0.005(2) 0.004(2) N6 0.033(3) 0.034(3) 0.021(2) -0.001(2) 0.008(2) -0.001(2) N7 0.031(3) 0.034(3) 0.024(2) 0.006(2) -0.001(2) 0.000(2) N8 0.028(3) 0.030(3) 0.029(3) 0.000(2) 0.003(2) 0.002(2) O1 0.029(2) 0.035(2) 0.0223(19) 0.0004(17) 0.0031(17) -0.0034(19) O1S 0.053(3) 0.087(4) 0.056(3) -0.025(3) 0.024(2) -0.021(3) O2 0.034(3) 0.041(2) 0.026(2) -0.0042(17) 0.0102(18) -0.0084(19) O2S 0.037(3) 0.065(3) 0.050(3) 0.003(2) 0.008(2) -0.007(2) O3 0.037(3) 0.034(2) 0.0229(19) 0.0054(17) 0.0045(18) 0.0040(18) O3S 0.044(3) 0.062(3) 0.040(2) -0.005(2) 0.007(2) 0.007(2) O4 0.036(3) 0.031(2) 0.0223(19) 0.0061(16) 0.0083(17) 0.0006(19) O4S 0.046(3) 0.081(3) 0.052(3) -0.018(2) 0.021(2) -0.011(3) O5 0.031(2) 0.036(2) 0.0226(19) -0.0056(16) 0.0102(17) -0.0049(19) O5S 0.061(3) 0.084(4) 0.051(3) -0.021(2) 0.019(2) -0.016(3) O6 0.027(2) 0.037(2) 0.023(2) -0.0046(16) 0.0097(17) -0.0048(18) O6S 0.035(3) 0.061(3) 0.059(3) -0.006(2) 0.014(2) -0.004(2) O7 0.038(3) 0.034(2) 0.0251(19) 0.0018(17) 0.0106(18) 0.0024(18) O7S 0.050(3) 0.067(3) 0.040(2) -0.009(2) 0.013(2) -0.008(2) O8 0.030(2) 0.034(2) 0.0240(19) 0.0042(17) 0.0056(17) 0.0049(19) O8S 0.059(3) 0.070(3) 0.063(3) -0.014(2) 0.019(3) -0.024(3) O9 0.029(2) 0.032(2) 0.027(2) 0.0021(17) 0.0054(17) 0.0071(18) O9S 0.061(3) 0.079(3) 0.054(3) -0.013(2) 0.024(2) -0.027(3) O10 0.032(2) 0.042(2) 0.028(2) 0.0030(17) 0.0155(18) 0.0054(19) O10S 0.060(4) 0.097(4) 0.061(3) -0.032(3) 0.036(3) -0.020(3) O11 0.027(2) 0.044(2) 0.027(2) -0.0043(17) 0.0085(18) -0.0027(19) O11S 0.051(3) 0.070(3) 0.040(2) -0.012(2) 0.010(2) -0.008(2) O12 0.029(2) 0.036(2) 0.029(2) -0.0055(17) 0.0051(17) -0.0070(19) O12S 0.042(3) 0.122(4) 0.053(3) -0.032(3) 0.018(2) -0.029(3) O13 0.036(3) 0.033(2) 0.025(2) 0.0050(17) 0.0128(18) 0.0071(18) O14 0.029(2) 0.032(2) 0.0236(19) 0.0028(16) 0.0044(17) 0.0031(18) O15 0.032(2) 0.040(2) 0.0210(19) -0.0046(17) 0.0053(17) -0.008(2) O16 0.034(3) 0.036(2) 0.025(2) -0.0072(17) 0.0088(18) -0.0064(19) Ni1 0.0274(4) 0.0282(4) 0.0209(4) -0.0008(3) 0.0055(3) -0.0011(4) Ni2 0.0267(4) 0.0274(4) 0.0201(4) -0.0005(3) 0.0037(3) -0.0008(4) Ni3 0.0278(5) 0.0275(4) 0.0191(4) 0.0002(3) 0.0052(3) 0.0001(4) Ni4 0.0279(4) 0.0272(4) 0.0194(4) 0.0000(3) 0.0037(3) -0.0002(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds 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 C1 N1 1.342(6) . ? C1 C2 1.382(7) . ? C1S O2S 1.241(7) . ? C1S O1S 1.272(6) . ? C1S C2S 1.498(7) . ? C2 C3 1.367(7) . ? C2S C3S 1.374(7) . ? C2S C7S 1.380(8) . ? C3 C4 1.375(8) . ? C3S C4S 1.386(7) . ? C4 C5 1.393(7) . ? C4S C5S 1.372(7) . ? C5 N1 1.358(6) . ? C5 C6 1.478(7) . ? C5S C6S 1.391(7) . ? C5S C8S 1.500(7) . ? C6 N2 1.321(6) . ? C6 C7 1.395(7) . ? C6S C7S 1.382(7) . ? C7 C8 1.376(8) . ? C8 C9 1.350(7) . ? C8S O3S 1.240(6) . ? C8S O4S 1.292(6) . ? C9 C10 1.374(7) . ? C9S O5S 1.252(6) . ? C9S O6S 1.274(6) . ? C9S C10S 1.513(7) . ? C10 N2 1.353(6) . ? C10S C15S 1.392(7) . ? C10S C11S 1.393(7) . ? C11 N3 1.332(6) . ? C11 C12 1.378(7) . ? C11S C12S 1.382(7) . ? C12 C13 1.376(7) . ? C12S C13S 1.376(7) . ? C13 C14 1.373(7) . ? C13S C14S 1.386(7) . ? C13S C16S 1.511(7) . ? C14 C15 1.380(7) . ? C14S C15S 1.390(7) . ? C15 N3 1.350(6) . ? C15 C16 1.481(7) . ? C16 N4 1.345(6) . ? C16 C17 1.382(7) . ? C16S O7S 1.237(6) . ? C16S O8S 1.283(6) . ? C17 C18 1.367(7) . ? C17S O10S 1.236(6) . ? C17S O9S 1.276(6) . ? C17S C18S 1.483(7) 1_654 ? C18 C19 1.362(7) . ? C18S C23S 1.385(7) . ? C18S C19S 1.393(6) . ? C18S C17S 1.483(7) 1_456 ? C19 C20 1.379(7) . ? C19S C20S 1.378(7) . ? C20 N4 1.338(6) . ? C20S C21S 1.380(7) . ? C21 N5 1.329(6) . ? C21 C22 1.379(7) . ? C21S C22S 1.392(7) . ? C21S C24S 1.501(7) . ? C22 C23 1.385(8) . ? C22S C23S 1.377(7) . ? C23 C24 1.380(8) . ? C24 C25 1.385(7) . ? C24S O12S 1.242(7) . ? C24S O11S 1.268(6) . ? C25 N5 1.350(6) . ? C25 C26 1.492(7) . ? C26 N6 1.353(6) . ? C26 C27 1.393(7) . ? C27 C28 1.366(8) . ? C28 C29 1.367(7) . ? C29 C30 1.383(7) . ? C30 N6 1.338(6) . ? C31 N7 1.327(6) . ? C31 C32 1.380(7) . ? C32 C33 1.382(7) . ? C33 C34 1.372(8) . ? C34 C35 1.380(7) . ? C35 N7 1.341(6) . ? C35 C36 1.471(7) . ? C36 N8 1.340(6) . ? C36 C37 1.390(7) . ? C37 C38 1.376(7) . ? C38 C39 1.361(7) . ? C39 C40 1.376(7) . ? C40 N8 1.338(6) . ? C41 O2 1.257(6) . ? C41 O1 1.285(6) . ? C41 C42 1.493(6) . ? C41 Ni1 2.430(5) . ? C42 C47 1.380(7) . ? C42 C43 1.403(7) . ? C43 C44 1.386(6) . ? C44 C45 1.404(7) 4_565 ? C45 C46 1.371(6) 4_566 ? C45 C44 1.404(7) 4_566 ? C45 C48 1.493(6) . ? C46 C45 1.371(6) 4_565 ? C46 C47 1.387(6) . ? C48 O4 1.262(6) . ? C48 O3 1.275(5) . ? C48 Ni1 2.424(5) . ? C49 O6 1.254(6) . ? C49 O5 1.266(6) . ? C49 C50 1.507(6) . ? C49 Ni2 2.416(5) . ? C50 C55 1.370(7) . ? C50 C51 1.388(7) . ? C51 C52 1.384(6) 4_565 ? C52 C53 1.382(7) . ? C52 C51 1.384(6) 4_566 ? C53 C54 1.397(7) . ? C53 C56 1.507(6) . ? C54 C55 1.380(6) 4_566 ? C55 C54 1.380(6) 4_565 ? C56 O8 1.261(6) . ? C56 O7 1.266(5) . ? C56 Ni2 2.414(5) . ? C57 O10 1.250(6) . ? C57 O9 1.264(6) . ? C57 C58 1.486(6) . ? C57 Ni3 2.405(5) . ? C58 C63 1.394(7) . ? C58 C59 1.416(6) . ? C59 C60 1.393(6) 4_575 ? C60 C61 1.387(7) . ? C60 C59 1.393(6) 4_576 ? C61 C62 1.402(7) 4_576 ? C61 C64 1.494(6) . ? C62 C63 1.383(6) . ? C62 C61 1.402(7) 4_575 ? C64 O12 1.255(6) . ? C64 O11 1.271(5) . ? C64 Ni3 2.413(5) . ? C65 O13 1.253(5) . ? C65 O14 1.285(6) . ? C65 C66 1.492(6) . ? C65 Ni4 2.417(5) . ? C66 C67 1.374(7) . ? C66 C71 1.400(7) . ? C67 C68 1.377(6) 4_575 ? C68 C67 1.377(6) 4_576 ? C68 C69 1.395(7) . ? C69 C70 1.388(7) . ? C69 C72 1.499(6) . ? C70 C71 1.370(6) 4_576 ? C71 C70 1.370(6) 4_575 ? C72 O15 1.259(6) . ? C72 O16 1.262(6) . ? C72 Ni4 2.404(5) . ? N1 Ni1 2.063(4) . ? N2 Ni1 2.045(4) . ? N3 Ni2 2.050(4) . ? N4 Ni2 2.056(4) . ? N5 Ni3 2.046(4) . ? N6 Ni3 2.065(4) . ? N7 Ni4 2.041(4) . ? N8 Ni4 2.055(4) . ? O1 Ni1 2.084(3) . ? O2 Ni1 2.113(3) . ? O3 Ni1 2.122(3) . ? O4 Ni1 2.070(3) . ? O5 Ni2 2.074(3) . ? O6 Ni2 2.114(3) . ? O7 Ni2 2.103(3) . ? O8 Ni2 2.081(3) . ? O9 Ni3 2.062(3) . ? O10 Ni3 2.128(3) . ? O11 Ni3 2.100(3) . ? O12 Ni3 2.078(3) . ? O13 Ni4 2.117(3) . ? O14 Ni4 2.080(3) . ? O15 Ni4 2.054(3) . ? O16 Ni4 2.110(3) . ? 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 N1 C1 C2 122.8(6) . . ? O2S C1S O1S 124.5(6) . . ? O2S C1S C2S 118.2(6) . . ? O1S C1S C2S 117.3(5) . . ? C3 C2 C1 118.3(6) . . ? C3S C2S C7S 119.7(6) . . ? C3S C2S C1S 120.2(5) . . ? C7S C2S C1S 120.2(5) . . ? C2 C3 C4 120.0(6) . . ? C2S C3S C4S 120.2(5) . . ? C3 C4 C5 119.6(6) . . ? C5S C4S C3S 120.7(5) . . ? N1 C5 C4 120.4(5) . . ? N1 C5 C6 115.4(5) . . ? C4 C5 C6 124.2(5) . . ? C4S C5S C6S 118.9(5) . . ? C4S C5S C8S 119.8(5) . . ? C6S C5S C8S 121.2(5) . . ? N2 C6 C7 122.3(6) . . ? N2 C6 C5 115.4(5) . . ? C7 C6 C5 122.4(5) . . ? C7S C6S C5S 120.4(6) . . ? C8 C7 C6 117.9(6) . . ? C2S C7S C6S 120.0(6) . . ? C9 C8 C7 120.1(6) . . ? O3S C8S O4S 123.3(5) . . ? O3S C8S C5S 119.2(5) . . ? O4S C8S C5S 117.5(5) . . ? C8 C9 C10 119.3(6) . . ? O5S C9S O6S 124.4(5) . . ? O5S C9S C10S 118.6(5) . . ? O6S C9S C10S 116.9(5) . . ? N2 C10 C9 121.7(5) . . ? C15S C10S C11S 119.1(5) . . ? C15S C10S C9S 120.9(5) . . ? C11S C10S C9S 120.0(5) . . ? N3 C11 C12 121.6(5) . . ? C12S C11S C10S 120.0(5) . . ? C13 C12 C11 119.4(6) . . ? C13S C12S C11S 121.0(5) . . ? C14 C13 C12 118.8(5) . . ? C12S C13S C14S 119.4(5) . . ? C12S C13S C16S 120.0(5) . . ? C14S C13S C16S 120.6(5) . . ? C13 C14 C15 119.7(5) . . ? C13S C14S C15S 120.3(6) . . ? N3 C15 C14 120.9(5) . . ? N3 C15 C16 116.0(5) . . ? C14 C15 C16 123.1(5) . . ? C14S C15S C10S 120.2(5) . . ? N4 C16 C17 122.0(5) . . ? N4 C16 C15 114.8(5) . . ? C17 C16 C15 123.2(5) . . ? O7S C16S O8S 124.1(5) . . ? O7S C16S C13S 119.0(5) . . ? O8S C16S C13S 116.9(5) . . ? C18 C17 C16 117.9(6) . . ? O10S C17S O9S 122.3(5) . . ? O10S C17S C18S 120.0(5) . 1_654 ? O9S C17S C18S 117.7(5) . 1_654 ? C19 C18 C17 120.5(6) . . ? C23S C18S C19S 118.6(5) . . ? C23S C18S C17S 119.8(5) . 1_456 ? C19S C18S C17S 121.5(5) . 1_456 ? C18 C19 C20 119.3(6) . . ? C20S C19S C18S 121.7(5) . . ? N4 C20 C19 121.1(5) . . ? C19S C20S C21S 119.0(5) . . ? N5 C21 C22 122.3(6) . . ? C20S C21S C22S 119.9(5) . . ? C20S C21S C24S 121.1(5) . . ? C22S C21S C24S 119.0(5) . . ? C21 C22 C23 118.3(6) . . ? C23S C22S C21S 120.6(5) . . ? C24 C23 C22 120.0(6) . . ? C22S C23S C18S 120.1(5) . . ? C23 C24 C25 118.4(6) . . ? O12S C24S O11S 123.7(6) . . ? O12S C24S C21S 119.1(6) . . ? O11S C24S C21S 117.2(5) . . ? N5 C25 C24 121.5(6) . . ? N5 C25 C26 116.0(5) . . ? C24 C25 C26 122.5(5) . . ? N6 C26 C27 122.5(5) . . ? N6 C26 C25 114.4(5) . . ? C27 C26 C25 123.1(6) . . ? C28 C27 C26 118.7(6) . . ? C27 C28 C29 119.5(6) . . ? C28 C29 C30 119.3(6) . . ? N6 C30 C29 122.7(6) . . ? N7 C31 C32 123.7(6) . . ? C31 C32 C33 117.0(6) . . ? C34 C33 C32 120.2(6) . . ? C33 C34 C35 119.0(6) . . ? N7 C35 C34 121.5(5) . . ? N7 C35 C36 115.8(5) . . ? C34 C35 C36 122.6(5) . . ? N8 C36 C37 122.5(5) . . ? N8 C36 C35 115.1(5) . . ? C37 C36 C35 122.4(5) . . ? C38 C37 C36 117.2(5) . . ? C39 C38 C37 120.6(6) . . ? C38 C39 C40 119.2(6) . . ? N8 C40 C39 121.6(6) . . ? O2 C41 O1 119.5(5) . . ? O2 C41 C42 120.9(5) . . ? O1 C41 C42 119.6(5) . . ? O2 C41 Ni1 60.4(3) . . ? O1 C41 Ni1 59.1(2) . . ? C42 C41 Ni1 177.9(4) . . ? C47 C42 C43 119.6(5) . . ? C47 C42 C41 120.4(5) . . ? C43 C42 C41 119.9(5) . . ? C44 C43 C42 119.8(5) . . ? C43 C44 C45 119.7(5) . 4_565 ? C46 C45 C44 120.2(5) 4_566 4_566 ? C46 C45 C48 120.4(5) 4_566 . ? C44 C45 C48 119.3(5) 4_566 . ? C45 C46 C47 120.2(5) 4_565 . ? C42 C47 C46 120.6(5) . . ? O4 C48 O3 119.3(5) . . ? O4 C48 C45 120.0(5) . . ? O3 C48 C45 120.6(5) . . ? O4 C48 Ni1 58.6(3) . . ? O3 C48 Ni1 61.0(2) . . ? C45 C48 Ni1 172.0(4) . . ? O6 C49 O5 120.0(5) . . ? O6 C49 C50 120.3(5) . . ? O5 C49 C50 119.6(5) . . ? O6 C49 Ni2 60.9(3) . . ? O5 C49 Ni2 59.1(2) . . ? C50 C49 Ni2 178.2(4) . . ? C55 C50 C51 120.7(5) . . ? C55 C50 C49 120.7(5) . . ? C51 C50 C49 118.5(5) . . ? C52 C51 C50 119.6(5) 4_565 . ? C53 C52 C51 119.9(5) . 4_566 ? C52 C53 C54 120.1(5) . . ? C52 C53 C56 120.2(5) . . ? C54 C53 C56 119.6(5) . . ? C55 C54 C53 119.6(5) 4_566 . ? C50 C55 C54 120.1(5) . 4_565 ? O8 C56 O7 119.9(4) . . ? O8 C56 C53 120.1(5) . . ? O7 C56 C53 120.0(5) . . ? O8 C56 Ni2 59.5(2) . . ? O7 C56 Ni2 60.5(2) . . ? C53 C56 Ni2 174.8(4) . . ? O10 C57 O9 120.8(5) . . ? O10 C57 C58 119.9(5) . . ? O9 C57 C58 119.2(5) . . ? O10 C57 Ni3 62.0(3) . . ? O9 C57 Ni3 59.0(2) . . ? C58 C57 Ni3 172.6(4) . . ? C63 C58 C59 118.8(5) . . ? C63 C58 C57 121.3(5) . . ? C59 C58 C57 119.8(5) . . ? C60 C59 C58 120.2(5) 4_575 . ? C61 C60 C59 120.1(5) . 4_576 ? C60 C61 C62 119.7(5) . 4_576 ? C60 C61 C64 119.7(5) . . ? C62 C61 C64 120.6(5) 4_576 . ? C63 C62 C61 120.5(5) . 4_575 ? C62 C63 C58 120.6(5) . . ? O12 C64 O11 119.8(5) . . ? O12 C64 C61 120.1(5) . . ? O11 C64 C61 120.1(5) . . ? O12 C64 Ni3 59.4(3) . . ? O11 C64 Ni3 60.4(2) . . ? C61 C64 Ni3 178.9(4) . . ? O13 C65 O14 120.1(5) . . ? O13 C65 C66 121.0(5) . . ? O14 C65 C66 118.7(5) . . ? O13 C65 Ni4 61.0(3) . . ? O14 C65 Ni4 59.3(2) . . ? C66 C65 Ni4 172.3(4) . . ? C67 C66 C71 119.3(5) . . ? C67 C66 C65 120.0(5) . . ? C71 C66 C65 120.8(5) . . ? C66 C67 C68 120.9(5) . 4_575 ? C67 C68 C69 119.5(5) 4_576 . ? C70 C69 C68 119.9(5) . . ? C70 C69 C72 119.7(5) . . ? C68 C69 C72 120.3(5) . . ? C71 C70 C69 119.8(5) 4_576 . ? C70 C71 C66 120.5(5) 4_575 . ? O15 C72 O16 119.9(5) . . ? O15 C72 C69 119.9(5) . . ? O16 C72 C69 120.2(5) . . ? O15 C72 Ni4 58.7(3) . . ? O16 C72 Ni4 61.2(3) . . ? C69 C72 Ni4 178.1(4) . . ? C1 N1 C5 118.9(5) . . ? C1 N1 Ni1 127.2(4) . . ? C5 N1 Ni1 113.9(4) . . ? C6 N2 C10 118.6(5) . . ? C6 N2 Ni1 115.9(4) . . ? C10 N2 Ni1 125.5(4) . . ? C11 N3 C15 119.5(5) . . ? C11 N3 Ni2 126.3(4) . . ? C15 N3 Ni2 114.1(4) . . ? C20 N4 C16 119.2(5) . . ? C20 N4 Ni2 126.0(4) . . ? C16 N4 Ni2 114.8(4) . . ? C21 N5 C25 119.5(5) . . ? C21 N5 Ni3 125.8(4) . . ? C25 N5 Ni3 114.7(4) . . ? C30 N6 C26 117.4(5) . . ? C30 N6 Ni3 127.7(4) . . ? C26 N6 Ni3 114.9(4) . . ? C31 N7 C35 118.6(5) . . ? C31 N7 Ni4 126.8(4) . . ? C35 N7 Ni4 114.7(4) . . ? C40 N8 C36 118.8(5) . . ? C40 N8 Ni4 126.5(4) . . ? C36 N8 Ni4 114.6(4) . . ? C41 O1 Ni1 89.0(3) . . ? C41 O2 Ni1 88.5(3) . . ? C48 O3 Ni1 87.3(3) . . ? C48 O4 Ni1 90.0(3) . . ? C49 O5 Ni2 89.3(3) . . ? C49 O6 Ni2 87.8(3) . . ? C56 O7 Ni2 87.9(3) . . ? C56 O8 Ni2 89.0(3) . . ? C57 O9 Ni3 89.3(3) . . ? C57 O10 Ni3 86.7(3) . . ? C64 O11 Ni3 87.8(3) . . ? C64 O12 Ni3 89.2(3) . . ? C65 O13 Ni4 87.8(3) . . ? C65 O14 Ni4 88.6(3) . . ? C72 O15 Ni4 89.7(3) . . ? C72 O16 Ni4 87.1(3) . . ? N2 Ni1 N1 79.46(18) . . ? N2 Ni1 O4 100.49(15) . . ? N1 Ni1 O4 94.88(15) . . ? N2 Ni1 O1 95.21(14) . . ? N1 Ni1 O1 101.47(15) . . ? O4 Ni1 O1 159.14(13) . . ? N2 Ni1 O2 94.33(15) . . ? N1 Ni1 O2 163.00(15) . . ? O4 Ni1 O2 101.84(13) . . ? O1 Ni1 O2 63.06(13) . . ? N2 Ni1 O3 160.86(14) . . ? N1 Ni1 O3 91.87(16) . . ? O4 Ni1 O3 62.97(13) . . ? O1 Ni1 O3 103.28(13) . . ? O2 Ni1 O3 98.41(13) . . ? N2 Ni1 C48 130.71(17) . . ? N1 Ni1 C48 92.02(17) . . ? O4 Ni1 C48 31.37(14) . . ? O1 Ni1 C48 133.92(15) . . ? O2 Ni1 C48 103.84(15) . . ? O3 Ni1 C48 31.71(14) . . ? N2 Ni1 C41 95.56(16) . . ? N1 Ni1 C41 133.05(17) . . ? O4 Ni1 C41 131.59(16) . . ? O1 Ni1 C41 31.93(14) . . ? O2 Ni1 C41 31.14(14) . . ? O3 Ni1 C41 102.73(15) . . ? C48 Ni1 C41 123.00(17) . . ? N3 Ni2 N4 79.89(17) . . ? N3 Ni2 O5 102.83(15) . . ? N4 Ni2 O5 95.63(14) . . ? N3 Ni2 O8 93.97(14) . . ? N4 Ni2 O8 101.16(14) . . ? O5 Ni2 O8 158.09(13) . . ? N3 Ni2 O7 91.37(15) . . ? N4 Ni2 O7 161.57(14) . . ? O5 Ni2 O7 102.15(13) . . ? O8 Ni2 O7 63.01(13) . . ? N3 Ni2 O6 164.09(14) . . ? N4 Ni2 O6 94.15(15) . . ? O5 Ni2 O6 62.82(13) . . ? O8 Ni2 O6 101.68(13) . . ? O7 Ni2 O6 98.22(13) . . ? N3 Ni2 C56 91.62(16) . . ? N4 Ni2 C56 131.64(17) . . ? O5 Ni2 C56 132.50(16) . . ? O8 Ni2 C56 31.49(14) . . ? O7 Ni2 C56 31.59(14) . . ? O6 Ni2 C56 103.20(15) . . ? N3 Ni2 C49 134.05(17) . . ? N4 Ni2 C49 95.49(16) . . ? O5 Ni2 C49 31.59(14) . . ? O8 Ni2 C49 131.38(16) . . ? O7 Ni2 C49 102.17(15) . . ? O6 Ni2 C49 31.23(14) . . ? C56 Ni2 C49 122.09(17) . . ? N5 Ni3 O9 99.72(15) . . ? N5 Ni3 N6 79.97(18) . . ? O9 Ni3 N6 94.89(14) . . ? N5 Ni3 O12 96.92(14) . . ? O9 Ni3 O12 158.30(13) . . ? N6 Ni3 O12 101.66(15) . . ? N5 Ni3 O11 93.76(16) . . ? O9 Ni3 O11 101.83(13) . . ? N6 Ni3 O11 162.93(14) . . ? O12 Ni3 O11 63.09(13) . . ? N5 Ni3 O10 160.63(14) . . ? O9 Ni3 O10 62.90(12) . . ? N6 Ni3 O10 92.49(16) . . ? O12 Ni3 O10 102.09(13) . . ? O11 Ni3 O10 98.09(13) . . ? N5 Ni3 C57 130.60(17) . . ? O9 Ni3 C57 31.71(14) . . ? N6 Ni3 C57 92.89(17) . . ? O12 Ni3 C57 132.18(16) . . ? O11 Ni3 C57 103.11(15) . . ? O10 Ni3 C57 31.25(14) . . ? N5 Ni3 C64 95.92(16) . . ? O9 Ni3 C64 132.04(16) . . ? N6 Ni3 C64 132.53(17) . . ? O12 Ni3 C64 31.34(14) . . ? O11 Ni3 C64 31.75(15) . . ? O10 Ni3 C64 102.22(15) . . ? C57 Ni3 C64 122.21(17) . . ? N7 Ni4 O15 96.84(15) . . ? N7 Ni4 N8 79.65(18) . . ? O15 Ni4 N8 102.55(15) . . ? N7 Ni4 O14 100.57(15) . . ? O15 Ni4 O14 157.48(13) . . ? N8 Ni4 O14 94.58(14) . . ? N7 Ni4 O16 94.18(16) . . ? O15 Ni4 O16 63.19(13) . . ? N8 Ni4 O16 163.93(15) . . ? O14 Ni4 O16 101.17(13) . . ? N7 Ni4 O13 161.38(14) . . ? O15 Ni4 O13 101.26(13) . . ? N8 Ni4 O13 92.07(15) . . ? O14 Ni4 O13 63.20(12) . . ? O16 Ni4 O13 97.85(13) . . ? N7 Ni4 C72 96.14(17) . . ? O15 Ni4 C72 31.57(15) . . ? N8 Ni4 C72 133.67(18) . . ? O14 Ni4 C72 131.14(16) . . ? O16 Ni4 C72 31.62(15) . . ? O13 Ni4 C72 101.56(15) . . ? N7 Ni4 C65 131.66(17) . . ? O15 Ni4 C65 131.27(16) . . ? N8 Ni4 C65 92.22(17) . . ? O14 Ni4 C65 32.09(14) . . ? O16 Ni4 C65 102.82(15) . . ? O13 Ni4 C65 31.19(14) . . ? C72 Ni4 C65 121.46(17) . . ? _diffrn_measured_fraction_theta_max 0.902 _diffrn_reflns_theta_full 28.68 _diffrn_measured_fraction_theta_full 0.902 _refine_diff_density_max 0.311 _refine_diff_density_min -0.449 _refine_diff_density_rms 0.065 #===END data_3 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C20 H14 N2 Ni O5' _chemical_formula_weight 421.04 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' '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' 'N' 'N' 0.0061 0.0033 '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' _symmetry_cell_setting ? _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.618(3) _cell_length_b 10.058(4) _cell_length_c 11.353(4) _cell_angle_alpha 115.312(6) _cell_angle_beta 92.331(7) _cell_angle_gamma 94.025(7) _cell_volume 884.7(6) _cell_formula_units_Z 2 _cell_measurement_temperature 526(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'plate' _exptl_crystal_colour 'green' _exptl_crystal_size_max 0.225 _exptl_crystal_size_mid 0.175 _exptl_crystal_size_min 0.030 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.581 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 432 _exptl_absorpt_coefficient_mu 1.133 _exptl_absorpt_correction_type 'multiscan' _exptl_absorpt_correction_T_min 'Tmin/Tmax ratio 0.5999' _exptl_absorpt_correction_T_max 'Tmin/Tmax ratio 0.5999' _exptl_absorpt_process_details 'SADABS' _exptl_special_details ; ? ; _diffrn_ambient_temperature 526(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 'SIEMENS SMART/CCD' _diffrn_measurement_method 'narrow frame' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5520 _diffrn_reflns_av_R_equivalents 0.0304 _diffrn_reflns_av_sigmaI/netI 0.0667 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 7 _diffrn_reflns_theta_min 2.25 _diffrn_reflns_theta_max 28.28 _reflns_number_total 3899 _reflns_number_gt 2953 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _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^ > 2sigma(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^)+(0.0520P)^2^+0.0188P] 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 3899 _refine_ls_number_parameters 261 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0699 _refine_ls_R_factor_gt 0.0454 _refine_ls_wR_factor_ref 0.1072 _refine_ls_wR_factor_gt 0.0984 _refine_ls_goodness_of_fit_ref 1.026 _refine_ls_restrained_S_all 1.026 _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 Ni1 Ni 0.22169(4) 0.77503(4) 0.99952(3) 0.02339(13) Uani 1 1 d . . . N1 N 0.2747(3) 0.5906(2) 1.0240(2) 0.0245(5) Uani 1 1 d . . . N2 N 0.4172(3) 0.8647(3) 1.1314(2) 0.0281(5) Uani 1 1 d . . . O1 O 0.2772(2) 0.6916(2) 0.79484(18) 0.0285(5) Uani 1 1 d . . . O2 O 0.0441(2) 0.6636(2) 0.85792(18) 0.0321(5) Uani 1 1 d . . . O3 O 0.0978(2) 0.8285(2) 1.16093(18) 0.0292(5) Uani 1 1 d . . . O4 O 0.0413(3) 1.0576(2) 1.2047(2) 0.0437(6) Uani 1 1 d . . . O5W O 0.1973(3) 0.9756(3) 0.9912(2) 0.0345(5) Uani 1 1 d . . . C1 C 0.2102(3) 0.4510(3) 0.9637(3) 0.0316(7) Uani 1 1 d . . . H1 H 0.1372 0.4254 0.8931 0.038 Uiso 1 1 calc R . . C2 C 0.2479(4) 0.3428(3) 1.0022(3) 0.0372(8) Uani 1 1 d . . . H2 H 0.2043 0.2458 0.9551 0.045 Uiso 1 1 calc R . . C3 C 0.3489(4) 0.3792(3) 1.1092(3) 0.0366(8) Uani 1 1 d . . . H3 H 0.3732 0.3078 1.1367 0.044 Uiso 1 1 calc R . . C4 C 0.4162(3) 0.5264(3) 1.1780(3) 0.0313(7) Uani 1 1 d . . . C5 C 0.3774(3) 0.6267(3) 1.1289(3) 0.0229(6) Uani 1 1 d . . . C6 C 0.4504(3) 0.7762(3) 1.1892(3) 0.0247(6) Uani 1 1 d . . . C7 C 0.5521(3) 0.8219(3) 1.3025(3) 0.0333(7) Uani 1 1 d . . . C8 C 0.5827(4) 0.7192(4) 1.3541(3) 0.0406(8) Uani 1 1 d . . . H8 H 0.6474 0.7503 1.4304 0.049 Uiso 1 1 calc R . . C9 C 0.5195(4) 0.5774(4) 1.2945(3) 0.0412(8) Uani 1 1 d . . . H9 H 0.5431 0.5120 1.3292 0.049 Uiso 1 1 calc R . . C10 C 0.6229(4) 0.9690(4) 1.3548(3) 0.0435(8) Uani 1 1 d . . . H10 H 0.6901 1.0057 1.4302 0.052 Uiso 1 1 calc R . . C11 C 0.5924(4) 1.0556(4) 1.2946(4) 0.0490(9) Uani 1 1 d . . . H11 H 0.6404 1.1516 1.3279 0.059 Uiso 1 1 calc R . . C12 C 0.4894(4) 1.0022(3) 1.1829(3) 0.0373(8) Uani 1 1 d . . . H12 H 0.4702 1.0637 1.1429 0.045 Uiso 1 1 calc R . . C13 C 0.1341(3) 0.6450(3) 0.7677(3) 0.0247(6) Uani 1 1 d . . . C14 C 0.0662(3) 0.5684(3) 0.6286(3) 0.0243(6) Uani 1 1 d . . . C15 C -0.0932(3) 0.5271(3) 0.6031(3) 0.0287(6) Uani 1 1 d . . . H15 H -0.1561 0.5450 0.6719 0.034 Uiso 1 1 calc R . . C16 C 0.1590(3) 0.5410(3) 0.5248(3) 0.0281(6) Uani 1 1 d . . . H16 H 0.2658 0.5684 0.5412 0.034 Uiso 1 1 calc R . . C17 C 0.0087(3) 1.1184(3) 1.4678(3) 0.0269(6) Uani 1 1 d . . . H17 H 0.0149 1.1981 1.4465 0.032 Uiso 1 1 calc R . . C18 C 0.0204(3) 0.8592(3) 1.4062(3) 0.0253(6) Uani 1 1 d . . . H18 H 0.0345 0.7649 1.3438 0.030 Uiso 1 1 calc R . . C19 C 0.0288(3) 0.9774(3) 1.3727(3) 0.0223(6) Uani 1 1 d . . . C20 C 0.0578(3) 0.9536(3) 1.2356(3) 0.0258(6) Uani 1 1 d . . . H1W H 0.144(5) 1.021(4) 1.066(4) 0.069(13) Uiso 1 1 d . . . H2W H 0.137(4) 0.962(4) 0.935(4) 0.045(12) 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 Ni1 0.0282(2) 0.0271(2) 0.01425(18) 0.00886(15) -0.00080(13) 0.00036(14) N1 0.0247(12) 0.0268(12) 0.0202(12) 0.0091(10) 0.0015(10) -0.0012(9) N2 0.0325(14) 0.0278(13) 0.0230(12) 0.0108(11) 0.0008(10) -0.0015(10) O1 0.0286(11) 0.0359(11) 0.0182(10) 0.0097(9) -0.0017(8) 0.0007(9) O2 0.0314(11) 0.0462(13) 0.0155(10) 0.0112(10) -0.0016(9) -0.0003(9) O3 0.0396(12) 0.0293(11) 0.0172(10) 0.0083(9) 0.0057(9) 0.0027(9) O4 0.0791(18) 0.0396(13) 0.0214(11) 0.0183(10) 0.0107(11) 0.0237(12) O5W 0.0447(15) 0.0380(13) 0.0260(12) 0.0184(11) 0.0038(12) 0.0069(11) C1 0.0292(16) 0.0319(16) 0.0275(16) 0.0080(14) 0.0015(13) -0.0039(12) C2 0.0383(18) 0.0253(16) 0.045(2) 0.0119(15) 0.0106(15) -0.0021(13) C3 0.0427(19) 0.0318(17) 0.0442(19) 0.0232(16) 0.0135(16) 0.0090(14) C4 0.0298(16) 0.0382(18) 0.0306(16) 0.0182(15) 0.0072(13) 0.0086(13) C5 0.0219(14) 0.0273(14) 0.0200(13) 0.0106(12) 0.0039(11) 0.0025(11) C6 0.0231(14) 0.0298(15) 0.0199(14) 0.0101(12) 0.0007(11) 0.0001(11) C7 0.0275(16) 0.0403(18) 0.0273(16) 0.0114(15) -0.0036(13) -0.0019(13) C8 0.0363(18) 0.056(2) 0.0294(17) 0.0185(17) -0.0050(14) 0.0071(15) C9 0.046(2) 0.051(2) 0.0360(19) 0.0270(17) -0.0012(16) 0.0130(16) C10 0.0377(19) 0.049(2) 0.0337(18) 0.0119(17) -0.0104(15) -0.0092(15) C11 0.050(2) 0.0363(19) 0.047(2) 0.0095(17) -0.0091(17) -0.0200(16) C12 0.0439(19) 0.0308(17) 0.0376(18) 0.0171(15) -0.0013(15) -0.0077(14) C13 0.0317(16) 0.0283(15) 0.0162(13) 0.0117(12) -0.0015(12) 0.0041(12) C14 0.0326(16) 0.0261(14) 0.0142(13) 0.0091(12) -0.0013(11) 0.0020(11) C15 0.0302(16) 0.0375(17) 0.0174(14) 0.0109(13) 0.0042(12) 0.0017(12) C16 0.0273(15) 0.0324(16) 0.0214(14) 0.0093(13) -0.0020(12) -0.0008(12) C17 0.0352(16) 0.0261(15) 0.0218(14) 0.0125(12) 0.0024(12) 0.0034(12) C18 0.0355(16) 0.0218(14) 0.0162(13) 0.0056(11) 0.0025(12) 0.0053(11) C19 0.0226(14) 0.0290(15) 0.0147(12) 0.0088(12) -0.0003(11) 0.0041(11) C20 0.0276(15) 0.0324(16) 0.0172(13) 0.0107(13) -0.0013(11) 0.0023(12) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds 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 O3 2.046(2) . ? Ni1 O2 2.050(2) . ? Ni1 N1 2.068(2) . ? Ni1 N2 2.079(2) . ? Ni1 O5W 2.084(2) . ? Ni1 O1 2.194(2) . ? Ni1 C13 2.442(3) . ? N1 C1 1.336(4) . ? N1 C5 1.354(3) . ? N2 C12 1.341(4) . ? N2 C6 1.352(4) . ? O1 C13 1.265(3) . ? O2 C13 1.268(3) . ? O3 C20 1.262(3) . ? O4 C20 1.253(3) . ? O5W H1W 0.93(4) . ? O5W H2W 0.76(4) . ? C1 C2 1.388(4) . ? C1 H1 0.9300 . ? C2 C3 1.363(4) . ? C2 H2 0.9300 . ? C3 C4 1.412(4) . ? C3 H3 0.9300 . ? C4 C5 1.398(4) . ? C4 C9 1.437(4) . ? C5 C6 1.441(4) . ? C6 C7 1.406(4) . ? C7 C10 1.416(4) . ? C7 C8 1.422(4) . ? C8 C9 1.350(5) . ? C8 H8 0.9300 . ? C9 H9 0.9300 . ? C10 C11 1.350(5) . ? C10 H10 0.9300 . ? C11 C12 1.395(5) . ? C11 H11 0.9300 . ? C12 H12 0.9300 . ? C13 C14 1.500(4) . ? C14 C15 1.388(4) . ? C14 C16 1.390(4) . ? C15 C16 1.389(4) 2_566 ? C15 H15 0.9300 . ? C16 C15 1.389(4) 2_566 ? C16 H16 0.9300 . ? C17 C18 1.387(4) 2_578 ? C17 C19 1.395(4) . ? C17 H17 0.9300 . ? C18 C17 1.387(4) 2_578 ? C18 C19 1.393(4) . ? C18 H18 0.9300 . ? C19 C20 1.504(4) . ? 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 O3 Ni1 O2 98.90(9) . . ? O3 Ni1 N1 86.83(9) . . ? O2 Ni1 N1 94.40(9) . . ? O3 Ni1 N2 85.66(9) . . ? O2 Ni1 N2 172.74(9) . . ? N1 Ni1 N2 80.15(9) . . ? O3 Ni1 O5W 93.38(9) . . ? O2 Ni1 O5W 93.54(10) . . ? N1 Ni1 O5W 171.94(9) . . ? N2 Ni1 O5W 91.82(10) . . ? O3 Ni1 O1 161.12(8) . . ? O2 Ni1 O1 62.33(8) . . ? N1 Ni1 O1 96.16(8) . . ? N2 Ni1 O1 113.22(9) . . ? O5W Ni1 O1 86.24(9) . . ? O3 Ni1 C13 130.10(9) . . ? O2 Ni1 C13 31.25(9) . . ? N1 Ni1 C13 96.60(9) . . ? N2 Ni1 C13 144.09(10) . . ? O5W Ni1 C13 89.44(10) . . ? O1 Ni1 C13 31.08(8) . . ? C1 N1 C5 117.8(3) . . ? C1 N1 Ni1 130.0(2) . . ? C5 N1 Ni1 111.67(18) . . ? C12 N2 C6 117.9(3) . . ? C12 N2 Ni1 129.7(2) . . ? C6 N2 Ni1 110.94(18) . . ? C13 O1 Ni1 85.38(16) . . ? C13 O2 Ni1 91.73(17) . . ? C20 O3 Ni1 127.97(18) . . ? Ni1 O5W H1W 99(2) . . ? Ni1 O5W H2W 109(3) . . ? H1W O5W H2W 104(4) . . ? N1 C1 C2 122.7(3) . . ? N1 C1 H1 118.7 . . ? C2 C1 H1 118.7 . . ? C3 C2 C1 119.7(3) . . ? C3 C2 H2 120.1 . . ? C1 C2 H2 120.1 . . ? C2 C3 C4 119.3(3) . . ? C2 C3 H3 120.3 . . ? C4 C3 H3 120.3 . . ? C5 C4 C3 117.1(3) . . ? C5 C4 C9 119.1(3) . . ? C3 C4 C9 123.8(3) . . ? N1 C5 C4 123.3(3) . . ? N1 C5 C6 116.9(3) . . ? C4 C5 C6 119.8(3) . . ? N2 C6 C7 123.7(3) . . ? N2 C6 C5 117.0(2) . . ? C7 C6 C5 119.3(3) . . ? C6 C7 C10 116.3(3) . . ? C6 C7 C8 119.4(3) . . ? C10 C7 C8 124.2(3) . . ? C9 C8 C7 121.3(3) . . ? C9 C8 H8 119.3 . . ? C7 C8 H8 119.3 . . ? C8 C9 C4 120.8(3) . . ? C8 C9 H9 119.6 . . ? C4 C9 H9 119.6 . . ? C11 C10 C7 119.7(3) . . ? C11 C10 H10 120.1 . . ? C7 C10 H10 120.1 . . ? C10 C11 C12 120.4(3) . . ? C10 C11 H11 119.8 . . ? C12 C11 H11 119.8 . . ? N2 C12 C11 122.0(3) . . ? N2 C12 H12 119.0 . . ? C11 C12 H12 119.0 . . ? O1 C13 O2 120.5(2) . . ? O1 C13 C14 121.1(3) . . ? O2 C13 C14 118.4(3) . . ? O1 C13 Ni1 63.54(14) . . ? O2 C13 Ni1 57.01(14) . . ? C14 C13 Ni1 175.0(2) . . ? C15 C14 C16 119.3(3) . . ? C15 C14 C13 119.3(3) . . ? C16 C14 C13 121.4(3) . . ? C14 C15 C16 120.2(3) . 2_566 ? C14 C15 H15 119.9 . . ? C16 C15 H15 119.9 2_566 . ? C15 C16 C14 120.5(3) 2_566 . ? C15 C16 H16 119.8 2_566 . ? C14 C16 H16 119.8 . . ? C18 C17 C19 120.6(3) 2_578 . ? C18 C17 H17 119.7 2_578 . ? C19 C17 H17 119.7 . . ? C17 C18 C19 120.3(3) 2_578 . ? C17 C18 H18 119.9 2_578 . ? C19 C18 H18 119.9 . . ? C18 C19 C17 119.1(2) . . ? C18 C19 C20 120.6(2) . . ? C17 C19 C20 120.3(3) . . ? O4 C20 O3 125.3(3) . . ? O4 C20 C19 118.3(3) . . ? O3 C20 C19 116.4(2) . . ? _diffrn_measured_fraction_theta_max 0.887 _diffrn_reflns_theta_full 28.28 _diffrn_measured_fraction_theta_full 0.887 _refine_diff_density_max 0.535 _refine_diff_density_min -0.500 _refine_diff_density_rms 0.080 #===END data_4 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H17 N2 Ni O7' _chemical_formula_weight 504.11 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' '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' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ? _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.7682(12) _cell_length_b 10.6490(13) _cell_length_c 11.2468(14) _cell_angle_alpha 76.685(2) _cell_angle_beta 65.309(2) _cell_angle_gamma 85.612(2) _cell_volume 1034.1(2) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'polyhedra' _exptl_crystal_colour 'green' _exptl_crystal_size_max 0.275 _exptl_crystal_size_mid 0.225 _exptl_crystal_size_min 0.200 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.619 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 518 _exptl_absorpt_coefficient_mu 0.991 _exptl_absorpt_correction_type 'multiscan' _exptl_absorpt_correction_T_min 'Tmin/Tmax ratio 0.7552' _exptl_absorpt_correction_T_max 'Tmin/Tmax ratio 0.7552' _exptl_absorpt_process_details 'SADABS' _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 'SIEMENS SMART/CCD' _diffrn_measurement_method 'narrow frame' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6443 _diffrn_reflns_av_R_equivalents 0.0407 _diffrn_reflns_av_sigmaI/netI 0.0312 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.97 _diffrn_reflns_theta_max 28.31 _reflns_number_total 4497 _reflns_number_gt 4109 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _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^ > 2sigma(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^)+(0.0364P)^2^+0.6176P] 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 SHELXL _refine_ls_extinction_coef 0.0011(8) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 4497 _refine_ls_number_parameters 320 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0349 _refine_ls_R_factor_gt 0.0306 _refine_ls_wR_factor_ref 0.0817 _refine_ls_wR_factor_gt 0.0790 _refine_ls_goodness_of_fit_ref 1.039 _refine_ls_restrained_S_all 1.039 _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 C1 C 0.3495(2) 0.89395(18) 0.28477(18) 0.0269(4) Uani 1 1 d . . . C2 C 0.42522(19) 0.94953(18) 0.13696(17) 0.0262(3) Uani 1 1 d . . . C3 C 0.4969(2) 0.86771(18) 0.04946(18) 0.0305(4) Uani 1 1 d . . . H3 H 0.4946 0.7791 0.0827 0.037 Uiso 1 1 calc R . . C4 C 0.4283(2) 1.08171(18) 0.08750(18) 0.0303(4) Uani 1 1 d . . . H4 H 0.3804 1.1364 0.1457 0.036 Uiso 1 1 calc R . . C5 C 0.1541(2) 1.0025(2) 0.96361(19) 0.0318(4) Uani 1 1 d . . . H5 H 0.2575 1.0042 0.9394 0.038 Uiso 1 1 calc R . . C6 C 0.0991(2) 0.97322(17) 0.87704(17) 0.0259(3) Uani 1 1 d . . . C7 C -0.0558(2) 0.9709(2) 0.91397(19) 0.0309(4) Uani 1 1 d . . . H7 H -0.0935 0.9514 0.8567 0.037 Uiso 1 1 calc R . . C8 C 0.2072(2) 0.94189(18) 0.74530(17) 0.0284(4) Uani 1 1 d . . . C9 C -0.0655(2) 0.8111(2) 0.5355(3) 0.0442(5) Uani 1 1 d . . . H9 H -0.0480 0.8984 0.4953 0.053 Uiso 1 1 calc R . . C10 C -0.2057(3) 0.7558(3) 0.5686(3) 0.0600(8) Uani 1 1 d . . . H10 H -0.2805 0.8064 0.5522 0.072 Uiso 1 1 calc R . . C11 C -0.2319(3) 0.6274(3) 0.6249(3) 0.0605(8) Uani 1 1 d . . . H11 H -0.3245 0.5900 0.6460 0.073 Uiso 1 1 calc R . . C12 C -0.1194(3) 0.5512(3) 0.6512(2) 0.0450(5) Uani 1 1 d . . . C13 C 0.0163(2) 0.61545(19) 0.61788(18) 0.0300(4) Uani 1 1 d . . . C14 C -0.1339(3) 0.4149(3) 0.7083(3) 0.0600(8) Uani 1 1 d . . . H14 H -0.2228 0.3714 0.7291 0.072 Uiso 1 1 calc R . . C15 C -0.0221(4) 0.3489(3) 0.7321(2) 0.0588(7) Uani 1 1 d . . . H15 H -0.0354 0.2608 0.7694 0.071 Uiso 1 1 calc R . . C16 C 0.1170(3) 0.4112(2) 0.7015(2) 0.0434(5) Uani 1 1 d . . . C17 C 0.1339(2) 0.54466(18) 0.64597(17) 0.0297(4) Uani 1 1 d . . . C18 C 0.2393(4) 0.3484(2) 0.7223(2) 0.0560(7) Uani 1 1 d . . . H18 H 0.2336 0.2600 0.7578 0.067 Uiso 1 1 calc R . . C19 C 0.3667(3) 0.4175(3) 0.6904(2) 0.0522(6) Uani 1 1 d . . . H19 H 0.4484 0.3765 0.7034 0.063 Uiso 1 1 calc R . . C20 C 0.3729(2) 0.5497(2) 0.6382(2) 0.0398(5) Uani 1 1 d . . . H20 H 0.4598 0.5960 0.6179 0.048 Uiso 1 1 calc R . . C21 C 0.2987(3) 0.5012(2) 0.9935(2) 0.0433(5) Uani 1 1 d . . . C22 C 0.1446(2) 0.5025(2) 0.99554(19) 0.0366(4) Uani 1 1 d . . . C23 C 0.0854(3) 0.6136(2) 0.9436(2) 0.0410(5) Uani 1 1 d . . . H23 H 0.1425 0.6899 0.9059 0.049 Uiso 1 1 calc R . . C24 C 0.0578(3) 0.3887(2) 1.0523(2) 0.0403(5) Uani 1 1 d . . . H24 H 0.0964 0.3141 1.0875 0.048 Uiso 1 1 calc R . . N1 N 0.04319(17) 0.74315(16) 0.55950(16) 0.0295(3) Uani 1 1 d . . . N2 N 0.26026(17) 0.61286(15) 0.61611(14) 0.0276(3) Uani 1 1 d . . . O1 O 0.28029(16) 0.96593(13) 0.36557(13) 0.0355(3) Uani 1 1 d . . . O2 O 0.35982(15) 0.77444(12) 0.32824(12) 0.0300(3) Uani 1 1 d . . . O1W O 0.46816(17) 0.83881(16) 0.51452(17) 0.0364(3) Uani 1 1 d . . . O3 O 0.15316(14) 0.88348(14) 0.68948(13) 0.0330(3) Uani 1 1 d . . . O4 O 0.34308(17) 0.9747(2) 0.70262(16) 0.0541(5) Uani 1 1 d . . . O5 O 0.3767(2) 0.6106(2) 0.9353(2) 0.0679(5) Uani 1 1 d . . . O6 O 0.3494(2) 0.4045(2) 1.0421(2) 0.0598(5) Uani 1 1 d . . . Ni1 Ni 0.25541(2) 0.80385(2) 0.52529(2) 0.02342(8) Uani 1 1 d . . . H1W H 0.449(3) 0.878(3) 0.571(3) 0.049(8) Uiso 1 1 d . . . H2W H 0.527(3) 0.885(3) 0.447(3) 0.059(9) Uiso 1 1 d . . . H5S H 0.479(5) 0.615(5) 0.937(4) 0.139(18) 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 C1 0.0251(8) 0.0282(9) 0.0262(8) -0.0077(7) -0.0091(7) 0.0030(7) C2 0.0243(8) 0.0287(9) 0.0244(8) -0.0064(7) -0.0088(7) 0.0016(7) C3 0.0347(10) 0.0250(9) 0.0285(9) -0.0067(7) -0.0099(8) 0.0030(7) C4 0.0357(10) 0.0268(9) 0.0271(9) -0.0100(7) -0.0106(8) 0.0067(7) C5 0.0231(8) 0.0416(11) 0.0314(9) -0.0154(8) -0.0080(7) -0.0003(7) C6 0.0265(8) 0.0255(8) 0.0237(8) -0.0082(7) -0.0067(7) -0.0007(7) C7 0.0283(9) 0.0404(10) 0.0278(9) -0.0156(8) -0.0109(7) -0.0002(8) C8 0.0277(9) 0.0306(9) 0.0235(8) -0.0079(7) -0.0060(7) -0.0020(7) C9 0.0401(11) 0.0507(13) 0.0570(13) -0.0292(11) -0.0286(11) 0.0181(10) C10 0.0359(12) 0.091(2) 0.0767(18) -0.0480(17) -0.0338(13) 0.0219(13) C11 0.0299(11) 0.100(2) 0.0633(16) -0.0426(17) -0.0163(11) -0.0076(13) C12 0.0371(11) 0.0632(15) 0.0372(11) -0.0248(11) -0.0080(9) -0.0142(10) C13 0.0284(9) 0.0369(10) 0.0259(8) -0.0155(8) -0.0071(7) -0.0029(7) C14 0.0645(17) 0.0663(17) 0.0440(13) -0.0180(12) -0.0076(12) -0.0386(14) C15 0.087(2) 0.0391(13) 0.0411(12) -0.0088(10) -0.0135(13) -0.0261(13) C16 0.0655(15) 0.0300(10) 0.0268(9) -0.0085(8) -0.0094(10) -0.0044(10) C17 0.0366(10) 0.0282(9) 0.0214(8) -0.0091(7) -0.0072(7) 0.0000(7) C18 0.092(2) 0.0303(11) 0.0367(12) -0.0075(9) -0.0206(13) 0.0172(12) C19 0.0620(15) 0.0486(14) 0.0388(12) -0.0087(10) -0.0190(11) 0.0292(12) C20 0.0333(10) 0.0484(12) 0.0316(10) -0.0073(9) -0.0103(8) 0.0134(9) C21 0.0416(12) 0.0509(13) 0.0379(11) -0.0221(10) -0.0111(9) 0.0043(10) C22 0.0395(11) 0.0390(11) 0.0292(9) -0.0136(8) -0.0093(8) 0.0029(9) C23 0.0476(12) 0.0335(10) 0.0371(11) -0.0063(9) -0.0126(9) -0.0043(9) C24 0.0490(12) 0.0336(10) 0.0375(11) -0.0094(9) -0.0169(9) 0.0056(9) N1 0.0261(7) 0.0351(8) 0.0322(8) -0.0168(7) -0.0131(6) 0.0065(6) N2 0.0263(7) 0.0306(8) 0.0218(7) -0.0064(6) -0.0063(6) 0.0052(6) O1 0.0420(8) 0.0303(7) 0.0255(6) -0.0086(5) -0.0054(6) 0.0084(6) O2 0.0339(7) 0.0270(7) 0.0247(6) -0.0054(5) -0.0085(5) 0.0041(5) O1W 0.0269(7) 0.0439(8) 0.0368(8) -0.0158(7) -0.0074(6) -0.0018(6) O3 0.0267(6) 0.0433(8) 0.0296(7) -0.0190(6) -0.0064(5) -0.0002(6) O4 0.0294(8) 0.0911(14) 0.0377(8) -0.0329(9) 0.0035(6) -0.0210(8) O5 0.0543(11) 0.0695(14) 0.0832(15) -0.0115(11) -0.0328(11) -0.0072(10) O6 0.0520(10) 0.0601(12) 0.0734(12) -0.0218(10) -0.0303(10) 0.0155(9) Ni1 0.02230(13) 0.02463(13) 0.02172(12) -0.00730(8) -0.00658(9) 0.00169(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds 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 C1 O1 1.264(2) . ? C1 O2 1.266(2) . ? C1 C2 1.499(2) . ? C1 Ni1 2.4383(18) . ? C2 C4 1.387(3) . ? C2 C3 1.394(3) . ? C3 C4 1.391(3) 2_675 ? C3 H3 0.9300 . ? C4 C3 1.391(3) 2_675 ? C4 H4 0.9300 . ? C5 C7 1.390(3) 2_577 ? C5 C6 1.392(3) . ? C5 H5 0.9300 . ? C6 C7 1.392(3) . ? C6 C8 1.513(2) . ? C7 C5 1.390(3) 2_577 ? C7 H7 0.9300 . ? C8 O3 1.252(2) . ? C8 O4 1.255(2) . ? C9 N1 1.324(3) . ? C9 C10 1.399(4) . ? C9 H9 0.9300 . ? C10 C11 1.362(5) . ? C10 H10 0.9300 . ? C11 C12 1.406(4) . ? C11 H11 0.9300 . ? C12 C13 1.404(3) . ? C12 C14 1.437(4) . ? C13 N1 1.360(3) . ? C13 C17 1.432(3) . ? C14 C15 1.341(4) . ? C14 H14 0.9300 . ? C15 C16 1.431(4) . ? C15 H15 0.9300 . ? C16 C18 1.402(4) . ? C16 C17 1.407(3) . ? C17 N2 1.357(3) . ? C18 C19 1.365(4) . ? C18 H18 0.9300 . ? C19 C20 1.391(3) . ? C19 H19 0.9300 . ? C20 N2 1.328(2) . ? C20 H20 0.9300 . ? C21 O6 1.222(3) . ? C21 O5 1.317(3) . ? C21 C22 1.495(3) . ? C22 C23 1.391(3) . ? C22 C24 1.394(3) . ? C23 C24 1.382(3) 2_567 ? C23 H23 0.9300 . ? C24 C23 1.382(3) 2_567 ? C24 H24 0.9300 . ? N1 Ni1 2.0707(16) . ? N2 Ni1 2.0618(16) . ? O1 Ni1 2.1299(14) . ? O2 Ni1 2.1053(13) . ? O1W Ni1 2.0879(15) . ? O1W H1W 0.79(3) . ? O1W H2W 0.81(3) . ? O3 Ni1 2.0439(13) . ? O5 H5S 1.01(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 C1 O2 120.28(17) . . ? O1 C1 C2 120.55(16) . . ? O2 C1 C2 119.12(15) . . ? O1 C1 Ni1 60.81(10) . . ? O2 C1 Ni1 59.69(9) . . ? C2 C1 Ni1 173.31(13) . . ? C4 C2 C3 120.01(17) . . ? C4 C2 C1 120.45(16) . . ? C3 C2 C1 119.51(17) . . ? C4 C3 C2 120.16(18) 2_675 . ? C4 C3 H3 119.9 2_675 . ? C2 C3 H3 119.9 . . ? C2 C4 C3 119.83(17) . 2_675 ? C2 C4 H4 120.1 . . ? C3 C4 H4 120.1 2_675 . ? C7 C5 C6 120.54(17) 2_577 . ? C7 C5 H5 119.7 2_577 . ? C6 C5 H5 119.7 . . ? C5 C6 C7 119.41(16) . . ? C5 C6 C8 119.98(16) . . ? C7 C6 C8 120.60(16) . . ? C5 C7 C6 120.05(17) 2_577 . ? C5 C7 H7 120.0 2_577 . ? C6 C7 H7 120.0 . . ? O3 C8 O4 125.73(17) . . ? O3 C8 C6 116.80(16) . . ? O4 C8 C6 117.46(16) . . ? N1 C9 C10 122.2(2) . . ? N1 C9 H9 118.9 . . ? C10 C9 H9 118.9 . . ? C11 C10 C9 119.6(2) . . ? C11 C10 H10 120.2 . . ? C9 C10 H10 120.2 . . ? C10 C11 C12 120.2(2) . . ? C10 C11 H11 119.9 . . ? C12 C11 H11 119.9 . . ? C13 C12 C11 116.3(2) . . ? C13 C12 C14 118.8(2) . . ? C11 C12 C14 125.0(2) . . ? N1 C13 C12 123.4(2) . . ? N1 C13 C17 117.34(17) . . ? C12 C13 C17 119.3(2) . . ? C15 C14 C12 121.5(2) . . ? C15 C14 H14 119.2 . . ? C12 C14 H14 119.2 . . ? C14 C15 C16 121.4(2) . . ? C14 C15 H15 119.3 . . ? C16 C15 H15 119.3 . . ? C18 C16 C17 117.1(2) . . ? C18 C16 C15 124.6(2) . . ? C17 C16 C15 118.2(2) . . ? N2 C17 C16 122.65(19) . . ? N2 C17 C13 116.60(17) . . ? C16 C17 C13 120.75(19) . . ? C19 C18 C16 119.8(2) . . ? C19 C18 H18 120.1 . . ? C16 C18 H18 120.1 . . ? C18 C19 C20 119.3(2) . . ? C18 C19 H19 120.3 . . ? C20 C19 H19 120.3 . . ? N2 C20 C19 122.9(2) . . ? N2 C20 H20 118.6 . . ? C19 C20 H20 118.6 . . ? O6 C21 O5 122.1(2) . . ? O6 C21 C22 122.1(2) . . ? O5 C21 C22 115.8(2) . . ? C23 C22 C24 119.3(2) . . ? C23 C22 C21 122.0(2) . . ? C24 C22 C21 118.7(2) . . ? C24 C23 C22 120.4(2) 2_567 . ? C24 C23 H23 119.8 2_567 . ? C22 C23 H23 119.8 . . ? C23 C24 C22 120.3(2) 2_567 . ? C23 C24 H24 119.9 2_567 . ? C22 C24 H24 119.9 . . ? C9 N1 C13 118.30(19) . . ? C9 N1 Ni1 129.22(16) . . ? C13 N1 Ni1 112.46(12) . . ? C20 N2 C17 118.18(18) . . ? C20 N2 Ni1 128.38(15) . . ? C17 N2 Ni1 113.22(12) . . ? C1 O1 Ni1 87.98(11) . . ? C1 O2 Ni1 89.02(10) . . ? Ni1 O1W H1W 102(2) . . ? Ni1 O1W H2W 118(2) . . ? H1W O1W H2W 105(3) . . ? C8 O3 Ni1 131.01(12) . . ? C21 O5 H5S 118(3) . . ? O3 Ni1 N2 100.70(6) . . ? O3 Ni1 N1 87.45(6) . . ? N2 Ni1 N1 80.28(6) . . ? O3 Ni1 O1W 91.19(6) . . ? N2 Ni1 O1W 91.01(6) . . ? N1 Ni1 O1W 170.76(7) . . ? O3 Ni1 O2 164.25(6) . . ? N2 Ni1 O2 95.05(5) . . ? N1 Ni1 O2 95.00(6) . . ? O1W Ni1 O2 88.78(6) . . ? O3 Ni1 O1 101.83(6) . . ? N2 Ni1 O1 157.25(6) . . ? N1 Ni1 O1 97.58(6) . . ? O1W Ni1 O1 91.64(6) . . ? O2 Ni1 O1 62.43(5) . . ? O3 Ni1 C1 132.96(6) . . ? N2 Ni1 C1 126.34(6) . . ? N1 Ni1 C1 98.96(6) . . ? O1W Ni1 C1 88.65(6) . . ? O2 Ni1 C1 31.29(6) . . ? O1 Ni1 C1 31.21(5) . . ? _diffrn_measured_fraction_theta_max 0.877 _diffrn_reflns_theta_full 28.31 _diffrn_measured_fraction_theta_full 0.877 _refine_diff_density_max 0.392 _refine_diff_density_min -0.466 _refine_diff_density_rms 0.053 #===END data_5 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H14 N2 Ni O5' _chemical_formula_weight 397.02 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' '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' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ? _symmetry_space_group_name_H-M 'P 21/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 13.9683(9) _cell_length_b 17.4489(11) _cell_length_c 13.7737(9) _cell_angle_alpha 90.00 _cell_angle_beta 99.1240(10) _cell_angle_gamma 90.00 _cell_volume 3314.6(4) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'hexagonal' _exptl_crystal_colour 'blue green' _exptl_crystal_size_max 0.550 _exptl_crystal_size_mid 0.375 _exptl_crystal_size_min 0.150 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.591 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1632 _exptl_absorpt_coefficient_mu 1.204 _exptl_absorpt_correction_type 'multiscan' _exptl_absorpt_correction_T_min 'Tmin/Tmax ratio 0.8576' _exptl_absorpt_correction_T_max 'Tmin/Tmax ratio 0.8576' _exptl_absorpt_process_details 'SADABS' _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 'SIEMENS SMART/CCD' _diffrn_measurement_method 'narrow frame' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 20075 _diffrn_reflns_av_R_equivalents 0.0264 _diffrn_reflns_av_sigmaI/netI 0.0303 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.48 _diffrn_reflns_theta_max 28.37 _reflns_number_total 7562 _reflns_number_gt 6149 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _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^ > 2sigma(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^)+(0.0358P)^2^+1.0169P] 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 SHELXL _refine_ls_extinction_coef 0.00050(14) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 7562 _refine_ls_number_parameters 486 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0404 _refine_ls_R_factor_gt 0.0291 _refine_ls_wR_factor_ref 0.0798 _refine_ls_wR_factor_gt 0.0747 _refine_ls_goodness_of_fit_ref 1.044 _refine_ls_restrained_S_all 1.044 _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 Ni1 Ni 0.922303(14) 0.191714(11) 0.914939(16) 0.02591(7) Uani 1 1 d . . . Ni2 Ni 1.564823(14) 0.186111(12) 0.588486(16) 0.02740(7) Uani 1 1 d . . . C1 C 1.07089(12) 0.20877(10) 0.84453(13) 0.0304(4) Uani 1 1 d . . . C2 C 1.16170(12) 0.21210(10) 0.79844(13) 0.0311(4) Uani 1 1 d . . . C3 C 1.25209(13) 0.20529(12) 0.85709(14) 0.0387(4) Uani 1 1 d . . . H3 H 1.2566 0.2020 0.9251 0.046 Uiso 1 1 calc R . . C4 C 1.33568(13) 0.20334(12) 0.81415(14) 0.0381(4) Uani 1 1 d . . . H4 H 1.3962 0.2011 0.8535 0.046 Uiso 1 1 calc R . . C5 C 1.15506(13) 0.21813(11) 0.69694(14) 0.0360(4) Uani 1 1 d . . . H5 H 1.0951 0.2256 0.6579 0.043 Uiso 1 1 calc R . . C6 C 1.23873(13) 0.21286(11) 0.65402(14) 0.0370(4) Uani 1 1 d . . . H6 H 1.2342 0.2147 0.5860 0.044 Uiso 1 1 calc R . . C7 C 1.32885(12) 0.20478(10) 0.71253(13) 0.0313(4) Uani 1 1 d . . . C8 C 1.41893(12) 0.19591(9) 0.66568(13) 0.0300(4) Uani 1 1 d . . . C9 C 0.89923(12) 0.35451(10) 0.96341(13) 0.0297(4) Uani 1 1 d . . . C10 C 0.95143(12) 0.43003(9) 0.98405(12) 0.0281(3) Uani 1 1 d . . . C11 C 1.04956(13) 0.43197(10) 1.02355(13) 0.0333(4) Uani 1 1 d . . . H11 H 1.0831 0.3864 1.0393 0.040 Uiso 1 1 calc R . . C12 C 1.09747(12) 0.50147(10) 1.03943(14) 0.0340(4) Uani 1 1 d . . . H12 H 1.1630 0.5023 1.0661 0.041 Uiso 1 1 calc R . . C13 C 1.40157(12) 0.50933(10) 0.49719(14) 0.0347(4) Uani 1 1 d . . . H13 H 1.3351 0.5152 0.4952 0.042 Uiso 1 1 calc R . . C14 C 1.44157(12) 0.43622(10) 0.50410(14) 0.0340(4) Uani 1 1 d . . . H14 H 1.4019 0.3938 0.5069 0.041 Uiso 1 1 calc R . . C15 C 1.54069(12) 0.42632(9) 0.50682(12) 0.0274(3) Uani 1 1 d . . . C16 C 1.58555(12) 0.34724(10) 0.51690(13) 0.0304(4) Uani 1 1 d . . . C17 C 1.57860(12) 0.16911(10) 0.37161(13) 0.0337(4) Uani 1 1 d . . . H17 H 1.5631 0.2209 0.3668 0.040 Uiso 1 1 calc R . . C18 C 1.59030(14) 0.12985(11) 0.28741(14) 0.0416(4) Uani 1 1 d . . . H18 H 1.5827 0.1548 0.2270 0.050 Uiso 1 1 calc R . . C19 C 1.61344(14) 0.05319(12) 0.29422(14) 0.0420(4) Uani 1 1 d . . . H19 H 1.6221 0.0257 0.2384 0.050 Uiso 1 1 calc R . . C20 C 1.62368(13) 0.01752(10) 0.38476(13) 0.0348(4) Uani 1 1 d . . . H20 H 1.6386 -0.0344 0.3907 0.042 Uiso 1 1 calc R . . C21 C 1.61137(11) 0.06033(9) 0.46682(12) 0.0270(3) Uani 1 1 d . . . C22 C 1.62041(11) 0.02744(9) 0.56720(13) 0.0285(3) Uani 1 1 d . . . C23 C 1.64539(14) -0.04836(10) 0.58872(14) 0.0389(4) Uani 1 1 d . . . H23 H 1.6570 -0.0818 0.5393 0.047 Uiso 1 1 calc R . . C24 C 1.65277(16) -0.07337(12) 0.68483(16) 0.0480(5) Uani 1 1 d . . . H24 H 1.6686 -0.1241 0.7008 0.058 Uiso 1 1 calc R . . C25 C 1.63653(16) -0.02248(13) 0.75652(16) 0.0495(5) Uani 1 1 d . . . H25 H 1.6430 -0.0378 0.8219 0.059 Uiso 1 1 calc R . . C26 C 1.61054(15) 0.05166(12) 0.73000(14) 0.0420(4) Uani 1 1 d . . . H26 H 1.5986 0.0857 0.7786 0.050 Uiso 1 1 calc R . . C27 C 0.89117(13) 0.15864(11) 1.12255(14) 0.0379(4) Uani 1 1 d . . . H27 H 0.9030 0.2106 1.1336 0.045 Uiso 1 1 calc R . . C28 C 0.90497(15) 0.06531(12) 0.75937(14) 0.0426(4) Uani 1 1 d . . . H28 H 0.9124 0.1043 0.7151 0.051 Uiso 1 1 calc R . . C29 C 0.89932(16) -0.00939(13) 0.72619(16) 0.0509(5) Uani 1 1 d . . . H29 H 0.9027 -0.0206 0.6608 0.061 Uiso 1 1 calc R . . C30 C 0.88851(15) -0.06719(12) 0.79208(16) 0.0491(5) Uani 1 1 d . . . H30 H 0.8858 -0.1181 0.7718 0.059 Uiso 1 1 calc R . . C31 C 0.88182(13) -0.04890(10) 0.88809(15) 0.0394(4) Uani 1 1 d . . . H31 H 0.8736 -0.0871 0.9331 0.047 Uiso 1 1 calc R . . C32 C 0.88756(11) 0.02753(9) 0.91651(13) 0.0292(3) Uani 1 1 d . . . C33 C 0.88133(11) 0.05401(10) 1.01785(13) 0.0287(3) Uani 1 1 d . . . C34 C 0.86107(13) 0.00540(11) 1.09177(15) 0.0406(4) Uani 1 1 d . . . H34 H 0.8523 -0.0469 1.0804 0.049 Uiso 1 1 calc R . . C35 C 0.85422(16) 0.03657(14) 1.18293(16) 0.0512(5) Uani 1 1 d . . . H35 H 0.8395 0.0054 1.2333 0.061 Uiso 1 1 calc R . . C36 C 0.86923(16) 0.11356(14) 1.19864(15) 0.0507(5) Uani 1 1 d . . . H36 H 0.8647 0.1351 1.2595 0.061 Uiso 1 1 calc R . . N1 N 1.58871(9) 0.13558(8) 0.46001(10) 0.0276(3) Uani 1 1 d . . . N2 N 1.60179(10) 0.07664(8) 0.63723(11) 0.0316(3) Uani 1 1 d . . . N3 N 0.90019(10) 0.08388(8) 0.85284(11) 0.0312(3) Uani 1 1 d . . . N4 N 0.89587(9) 0.12975(8) 1.03344(10) 0.0278(3) Uani 1 1 d . . . O1 O 1.41088(8) 0.17322(7) 0.57785(9) 0.0346(3) Uani 1 1 d . . . O2 O 1.50069(8) 0.21026(7) 0.71518(9) 0.0368(3) Uani 1 1 d . . . O3 O 0.99132(8) 0.23161(7) 0.79720(9) 0.0358(3) Uani 1 1 d . . . O4 O 1.07553(9) 0.18016(7) 0.92952(9) 0.0345(3) Uani 1 1 d . . . O5 O 0.94743(9) 0.29429(7) 0.98541(10) 0.0365(3) Uani 1 1 d . . . O6 O 0.81281(9) 0.35726(7) 0.92159(11) 0.0463(4) Uani 1 1 d . . . O7 O 1.53107(9) 0.29376(7) 0.53662(10) 0.0379(3) Uani 1 1 d . . . O8 O 1.67256(9) 0.34016(8) 0.50748(12) 0.0478(4) Uani 1 1 d . . . O9W O 0.77655(9) 0.21956(8) 0.86272(10) 0.0343(3) Uani 1 1 d . . . O10W O 1.70814(10) 0.21743(9) 0.64064(14) 0.0439(3) Uani 1 1 d . . . H1 H 0.7451(18) 0.1987(14) 0.8955(19) 0.059(8) Uiso 1 1 d . . . H2 H 0.7780(17) 0.2674(16) 0.8816(18) 0.063(8) Uiso 1 1 d . . . H3 H 1.7169(18) 0.2535(16) 0.6087(19) 0.063(8) Uiso 1 1 d . . . H4 H 1.730(2) 0.224(2) 0.708(3) 0.136(14) 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 Ni1 0.02493(11) 0.02259(12) 0.03158(13) 0.00134(8) 0.00876(8) -0.00025(8) Ni2 0.02615(11) 0.02319(12) 0.03459(13) -0.00332(8) 0.01012(9) -0.00060(8) C1 0.0298(8) 0.0265(8) 0.0370(10) 0.0025(7) 0.0121(7) 0.0007(7) C2 0.0285(8) 0.0279(9) 0.0390(10) 0.0022(7) 0.0118(7) -0.0001(7) C3 0.0338(9) 0.0524(12) 0.0315(10) 0.0046(8) 0.0098(7) 0.0005(8) C4 0.0273(8) 0.0514(11) 0.0361(10) 0.0028(8) 0.0066(7) 0.0001(8) C5 0.0292(9) 0.0455(11) 0.0339(10) -0.0017(8) 0.0066(7) 0.0010(8) C6 0.0341(9) 0.0469(11) 0.0312(10) -0.0049(8) 0.0093(7) -0.0026(8) C7 0.0302(8) 0.0290(9) 0.0367(10) -0.0052(7) 0.0121(7) -0.0033(7) C8 0.0307(8) 0.0247(8) 0.0374(10) -0.0056(7) 0.0135(7) -0.0033(6) C9 0.0320(8) 0.0264(8) 0.0322(9) -0.0010(7) 0.0098(7) -0.0031(7) C10 0.0327(8) 0.0239(8) 0.0281(9) 0.0012(6) 0.0064(7) -0.0018(6) C11 0.0352(9) 0.0229(8) 0.0405(10) 0.0038(7) 0.0020(7) 0.0033(7) C12 0.0294(8) 0.0300(9) 0.0408(10) 0.0015(7) 0.0005(7) -0.0001(7) C13 0.0251(8) 0.0291(9) 0.0513(11) -0.0008(8) 0.0105(7) 0.0005(7) C14 0.0283(8) 0.0259(9) 0.0492(11) -0.0012(8) 0.0103(7) -0.0035(7) C15 0.0303(8) 0.0254(8) 0.0278(9) -0.0021(6) 0.0087(7) 0.0025(6) C16 0.0321(8) 0.0256(9) 0.0347(9) -0.0031(7) 0.0086(7) 0.0028(7) C17 0.0342(9) 0.0302(9) 0.0370(10) 0.0052(7) 0.0064(7) 0.0017(7) C18 0.0502(11) 0.0441(11) 0.0312(10) 0.0065(8) 0.0089(8) 0.0012(9) C19 0.0511(11) 0.0437(11) 0.0325(10) -0.0088(8) 0.0110(8) -0.0001(9) C20 0.0379(9) 0.0294(9) 0.0379(10) -0.0041(7) 0.0083(8) 0.0010(7) C21 0.0234(7) 0.0237(8) 0.0342(9) 0.0001(7) 0.0057(6) -0.0005(6) C22 0.0260(8) 0.0254(8) 0.0337(9) -0.0001(7) 0.0029(7) -0.0026(6) C23 0.0462(10) 0.0286(9) 0.0400(11) -0.0010(8) 0.0012(8) 0.0021(8) C24 0.0592(13) 0.0316(10) 0.0500(13) 0.0127(9) -0.0009(10) 0.0022(9) C25 0.0594(13) 0.0511(13) 0.0376(11) 0.0135(9) 0.0063(9) 0.0011(10) C26 0.0502(11) 0.0436(11) 0.0334(10) 0.0011(8) 0.0102(8) 0.0000(9) C27 0.0371(9) 0.0423(11) 0.0350(10) -0.0051(8) 0.0083(8) 0.0045(8) C28 0.0545(12) 0.0401(11) 0.0353(10) -0.0021(8) 0.0139(9) -0.0007(9) C29 0.0623(13) 0.0503(13) 0.0403(12) -0.0161(10) 0.0088(10) -0.0004(10) C30 0.0543(12) 0.0352(11) 0.0557(14) -0.0162(9) 0.0020(10) -0.0006(9) C31 0.0386(10) 0.0277(9) 0.0496(12) -0.0002(8) 0.0000(8) -0.0017(7) C32 0.0240(8) 0.0264(8) 0.0364(9) 0.0010(7) 0.0027(7) -0.0001(6) C33 0.0229(7) 0.0286(9) 0.0344(9) 0.0031(7) 0.0043(6) 0.0003(6) C34 0.0397(10) 0.0376(10) 0.0448(11) 0.0114(8) 0.0077(8) -0.0018(8) C35 0.0535(12) 0.0637(15) 0.0386(12) 0.0186(10) 0.0147(9) 0.0018(10) C36 0.0581(13) 0.0648(15) 0.0310(11) 0.0004(10) 0.0128(9) 0.0076(11) N1 0.0260(7) 0.0254(7) 0.0324(8) 0.0009(6) 0.0075(6) 0.0004(5) N2 0.0331(7) 0.0304(8) 0.0323(8) -0.0002(6) 0.0082(6) -0.0020(6) N3 0.0339(7) 0.0281(7) 0.0330(8) -0.0010(6) 0.0091(6) 0.0007(6) N4 0.0245(6) 0.0293(7) 0.0303(7) -0.0007(6) 0.0062(5) 0.0007(5) O1 0.0327(6) 0.0350(7) 0.0385(7) -0.0110(5) 0.0131(5) -0.0054(5) O2 0.0287(6) 0.0421(7) 0.0413(7) -0.0121(6) 0.0112(5) -0.0055(5) O3 0.0282(6) 0.0401(7) 0.0408(7) 0.0111(6) 0.0106(5) 0.0033(5) O4 0.0314(6) 0.0356(7) 0.0390(7) 0.0104(5) 0.0135(5) 0.0035(5) O5 0.0370(7) 0.0228(6) 0.0474(8) -0.0005(5) 0.0002(6) 0.0000(5) O6 0.0335(7) 0.0296(7) 0.0734(10) -0.0028(6) 0.0006(6) -0.0015(5) O7 0.0328(6) 0.0234(6) 0.0589(9) 0.0005(6) 0.0116(6) 0.0012(5) O8 0.0347(7) 0.0346(7) 0.0788(11) 0.0044(7) 0.0239(7) 0.0059(6) O9W 0.0287(6) 0.0319(7) 0.0428(8) -0.0021(6) 0.0078(5) -0.0020(5) O10W 0.0329(7) 0.0403(8) 0.0579(10) 0.0022(7) 0.0051(7) -0.0057(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds 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 N4 2.0398(14) . ? Ni1 O5 2.0398(12) . ? Ni1 N3 2.0697(15) . ? Ni1 O9W 2.1058(13) . ? Ni1 O4 2.1274(12) . ? Ni1 O3 2.1306(12) . ? Ni1 C1 2.4444(16) . ? Ni2 O7 2.0382(12) . ? Ni2 N1 2.0512(14) . ? Ni2 N2 2.0631(15) . ? Ni2 O10W 2.0895(14) . ? Ni2 O2 2.1263(12) . ? Ni2 O1 2.1438(12) . ? Ni2 C8 2.4495(16) . ? C1 O3 1.261(2) . ? C1 O4 1.265(2) . ? C1 C2 1.507(2) . ? C2 C5 1.390(3) . ? C2 C3 1.392(3) . ? C3 C4 1.390(2) . ? C3 H3 0.9300 . ? C4 C7 1.388(3) . ? C4 H4 0.9300 . ? C5 C6 1.394(2) . ? C5 H5 0.9300 . ? C6 C7 1.390(3) . ? C6 H6 0.9300 . ? C7 C8 1.510(2) . ? C8 O2 1.259(2) . ? C8 O1 1.261(2) . ? C9 O6 1.253(2) . ? C9 O5 1.259(2) . ? C9 C10 1.511(2) . ? C10 C12 1.389(2) 3_767 ? C10 C11 1.393(2) . ? C11 C12 1.386(2) . ? C11 H11 0.9300 . ? C12 C10 1.389(2) 3_767 ? C12 H12 0.9300 . ? C13 C15 1.389(2) 3_866 ? C13 C14 1.390(2) . ? C13 H13 0.9300 . ? C14 C15 1.390(2) . ? C14 H14 0.9300 . ? C15 C13 1.389(2) 3_866 ? C15 C16 1.513(2) . ? C16 O8 1.249(2) . ? C16 O7 1.261(2) . ? C17 N1 1.338(2) . ? C17 C18 1.379(3) . ? C17 H17 0.9300 . ? C18 C19 1.376(3) . ? C18 H18 0.9300 . ? C19 C20 1.381(3) . ? C19 H19 0.9300 . ? C20 C21 1.388(2) . ? C20 H20 0.9300 . ? C21 N1 1.350(2) . ? C21 C22 1.484(2) . ? C22 N2 1.347(2) . ? C22 C23 1.388(2) . ? C23 C24 1.382(3) . ? C23 H23 0.9300 . ? C24 C25 1.373(3) . ? C24 H24 0.9300 . ? C25 C26 1.377(3) . ? C25 H25 0.9300 . ? C26 N2 1.337(2) . ? C26 H26 0.9300 . ? C27 N4 1.338(2) . ? C27 C36 1.383(3) . ? C27 H27 0.9300 . ? C28 N3 1.339(2) . ? C28 C29 1.379(3) . ? C28 H28 0.9300 . ? C29 C30 1.381(3) . ? C29 H29 0.9300 . ? C30 C31 1.378(3) . ? C30 H30 0.9300 . ? C31 C32 1.389(2) . ? C31 H31 0.9300 . ? C32 N3 1.348(2) . ? C32 C33 1.486(2) . ? C33 N4 1.349(2) . ? C33 C34 1.388(2) . ? C34 C35 1.386(3) . ? C34 H34 0.9300 . ? C35 C36 1.372(3) . ? C35 H35 0.9300 . ? C36 H36 0.9300 . ? O9W H1 0.77(3) . ? O9W H2 0.87(3) . ? O10W H3 0.79(3) . ? O10W H4 0.94(4) . ? 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 N4 Ni1 O5 97.10(5) . . ? N4 Ni1 N3 79.32(6) . . ? O5 Ni1 N3 175.95(5) . . ? N4 Ni1 O9W 96.19(5) . . ? O5 Ni1 O9W 92.53(5) . . ? N3 Ni1 O9W 89.76(6) . . ? N4 Ni1 O4 100.45(5) . . ? O5 Ni1 O4 86.77(5) . . ? N3 Ni1 O4 92.00(5) . . ? O9W Ni1 O4 163.32(5) . . ? N4 Ni1 O3 160.63(5) . . ? O5 Ni1 O3 90.63(5) . . ? N3 Ni1 O3 92.20(5) . . ? O9W Ni1 O3 101.20(5) . . ? O4 Ni1 O3 62.15(5) . . ? N4 Ni1 C1 130.91(6) . . ? O5 Ni1 C1 89.38(6) . . ? N3 Ni1 C1 91.56(6) . . ? O9W Ni1 C1 132.23(6) . . ? O4 Ni1 C1 31.15(5) . . ? O3 Ni1 C1 31.03(5) . . ? O7 Ni2 N1 98.86(5) . . ? O7 Ni2 N2 178.05(5) . . ? N1 Ni2 N2 79.41(6) . . ? O7 Ni2 O10W 92.02(6) . . ? N1 Ni2 O10W 97.53(6) . . ? N2 Ni2 O10W 87.34(6) . . ? O7 Ni2 O2 90.05(5) . . ? N1 Ni2 O2 160.14(5) . . ? N2 Ni2 O2 91.87(5) . . ? O10W Ni2 O2 99.87(6) . . ? O7 Ni2 O1 84.20(5) . . ? N1 Ni2 O1 101.22(5) . . ? N2 Ni2 O1 96.99(5) . . ? O10W Ni2 O1 161.23(6) . . ? O2 Ni2 O1 61.86(5) . . ? O7 Ni2 C8 85.74(5) . . ? N1 Ni2 C8 131.67(6) . . ? N2 Ni2 C8 96.08(6) . . ? O10W Ni2 C8 130.56(6) . . ? O2 Ni2 C8 30.92(5) . . ? O1 Ni2 C8 30.96(5) . . ? O3 C1 O4 121.00(15) . . ? O3 C1 C2 120.13(15) . . ? O4 C1 C2 118.82(15) . . ? O3 C1 Ni1 60.61(8) . . ? O4 C1 Ni1 60.46(8) . . ? C2 C1 Ni1 175.03(13) . . ? C5 C2 C3 119.99(16) . . ? C5 C2 C1 120.01(16) . . ? C3 C2 C1 119.92(16) . . ? C4 C3 C2 120.05(17) . . ? C4 C3 H3 120.0 . . ? C2 C3 H3 120.0 . . ? C7 C4 C3 120.03(17) . . ? C7 C4 H4 120.0 . . ? C3 C4 H4 120.0 . . ? C2 C5 C6 119.65(17) . . ? C2 C5 H5 120.2 . . ? C6 C5 H5 120.2 . . ? C7 C6 C5 120.27(17) . . ? C7 C6 H6 119.9 . . ? C5 C6 H6 119.9 . . ? C4 C7 C6 119.83(16) . . ? C4 C7 C8 120.02(16) . . ? C6 C7 C8 120.13(16) . . ? O2 C8 O1 121.15(15) . . ? O2 C8 C7 119.59(16) . . ? O1 C8 C7 119.25(15) . . ? O2 C8 Ni2 60.22(8) . . ? O1 C8 Ni2 61.01(8) . . ? C7 C8 Ni2 178.09(12) . . ? O6 C9 O5 125.59(16) . . ? O6 C9 C10 117.00(15) . . ? O5 C9 C10 117.32(15) . . ? C12 C10 C11 119.15(15) 3_767 . ? C12 C10 C9 120.12(15) 3_767 . ? C11 C10 C9 120.70(15) . . ? C12 C11 C10 120.26(16) . . ? C12 C11 H11 119.9 . . ? C10 C11 H11 119.9 . . ? C11 C12 C10 120.59(16) . 3_767 ? C11 C12 H12 119.7 . . ? C10 C12 H12 119.7 3_767 . ? C15 C13 C14 121.01(15) 3_866 . ? C15 C13 H13 119.5 3_866 . ? C14 C13 H13 119.5 . . ? C13 C14 C15 120.26(16) . . ? C13 C14 H14 119.9 . . ? C15 C14 H14 119.9 . . ? C13 C15 C14 118.74(15) 3_866 . ? C13 C15 C16 120.43(14) 3_866 . ? C14 C15 C16 120.81(15) . . ? O8 C16 O7 125.44(16) . . ? O8 C16 C15 118.46(15) . . ? O7 C16 C15 116.08(14) . . ? N1 C17 C18 122.59(17) . . ? N1 C17 H17 118.7 . . ? C18 C17 H17 118.7 . . ? C19 C18 C17 118.93(18) . . ? C19 C18 H18 120.5 . . ? C17 C18 H18 120.5 . . ? C18 C19 C20 119.30(17) . . ? C18 C19 H19 120.4 . . ? C20 C19 H19 120.4 . . ? C19 C20 C21 118.97(17) . . ? C19 C20 H20 120.5 . . ? C21 C20 H20 120.5 . . ? N1 C21 C20 121.65(16) . . ? N1 C21 C22 115.16(14) . . ? C20 C21 C22 123.19(15) . . ? N2 C22 C23 121.66(16) . . ? N2 C22 C21 115.04(14) . . ? C23 C22 C21 123.30(16) . . ? C24 C23 C22 118.92(18) . . ? C24 C23 H23 120.5 . . ? C22 C23 H23 120.5 . . ? C25 C24 C23 119.25(18) . . ? C25 C24 H24 120.4 . . ? C23 C24 H24 120.4 . . ? C24 C25 C26 118.91(19) . . ? C24 C25 H25 120.5 . . ? C26 C25 H25 120.5 . . ? N2 C26 C25 122.67(19) . . ? N2 C26 H26 118.7 . . ? C25 C26 H26 118.7 . . ? N4 C27 C36 121.99(19) . . ? N4 C27 H27 119.0 . . ? C36 C27 H27 119.0 . . ? N3 C28 C29 122.55(19) . . ? N3 C28 H28 118.7 . . ? C29 C28 H28 118.7 . . ? C28 C29 C30 118.62(19) . . ? C28 C29 H29 120.7 . . ? C30 C29 H29 120.7 . . ? C31 C30 C29 119.52(19) . . ? C31 C30 H30 120.2 . . ? C29 C30 H30 120.2 . . ? C30 C31 C32 118.89(18) . . ? C30 C31 H31 120.6 . . ? C32 C31 H31 120.6 . . ? N3 C32 C31 121.66(17) . . ? N3 C32 C33 114.69(14) . . ? C31 C32 C33 123.64(16) . . ? N4 C33 C34 121.65(17) . . ? N4 C33 C32 115.11(14) . . ? C34 C33 C32 123.23(16) . . ? C35 C34 C33 118.43(19) . . ? C35 C34 H34 120.8 . . ? C33 C34 H34 120.8 . . ? C36 C35 C34 119.78(18) . . ? C36 C35 H35 120.1 . . ? C34 C35 H35 120.1 . . ? C35 C36 C27 118.96(19) . . ? C35 C36 H36 120.5 . . ? C27 C36 H36 120.5 . . ? C17 N1 C21 118.56(15) . . ? C17 N1 Ni2 126.08(12) . . ? C21 N1 Ni2 115.24(11) . . ? C26 N2 C22 118.54(16) . . ? C26 N2 Ni2 126.37(13) . . ? C22 N2 Ni2 115.08(11) . . ? C28 N3 C32 118.73(16) . . ? C28 N3 Ni1 126.18(13) . . ? C32 N3 Ni1 114.88(11) . . ? C27 N4 C33 119.15(15) . . ? C27 N4 Ni1 125.15(12) . . ? C33 N4 Ni1 115.70(11) . . ? C8 O1 Ni2 88.03(10) . . ? C8 O2 Ni2 88.86(10) . . ? C1 O3 Ni1 88.36(10) . . ? C1 O4 Ni1 88.40(10) . . ? C9 O5 Ni1 124.95(11) . . ? C16 O7 Ni2 130.07(11) . . ? Ni1 O9W H1 107.5(18) . . ? Ni1 O9W H2 98.2(16) . . ? H1 O9W H2 105(2) . . ? Ni2 O10W H3 104.0(19) . . ? Ni2 O10W H4 121(2) . . ? H3 O10W H4 113(3) . . ? _diffrn_measured_fraction_theta_max 0.910 _diffrn_reflns_theta_full 28.37 _diffrn_measured_fraction_theta_full 0.910 _refine_diff_density_max 0.454 _refine_diff_density_min -0.300 _refine_diff_density_rms 0.050