data_xark _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C17 H30 B2 Ca N6 O2' _chemical_formula_weight 412.17 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'B' 'B' 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ca' 'Ca' 0.2262 0.3064 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P21/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 9.4290(4) _cell_length_b 14.4707(6) _cell_length_c 16.7495(7) _cell_angle_alpha 90.00 _cell_angle_beta 104.5230(10) _cell_angle_gamma 90.00 _cell_volume 2212.35(16) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 8083 _cell_measurement_theta_min 2.5 _cell_measurement_theta_max 30.1 _exptl_crystal_description 'irregular' _exptl_crystal_colour 'colorless' _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.237 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 880 _exptl_absorpt_coefficient_mu 0.307 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.9189 _exptl_absorpt_correction_T_max 0.9411 _exptl_absorpt_process_details 'SADABS, Sheldrick, 1997' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 ? _diffrn_measurement_method 'Bruker APEX2' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 42299 _diffrn_reflns_av_R_equivalents 0.0561 _diffrn_reflns_av_sigmaI/netI 0.0374 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.89 _diffrn_reflns_theta_max 30.15 _reflns_number_total 6531 _reflns_number_gt 5191 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker APEX2' _computing_data_reduction 'Bruker APEX2' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL-Plus _computing_publication_material SHELXL-97 _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^)+(0.0407P)^2^+0.7042P] 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 6531 _refine_ls_number_parameters 273 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0528 _refine_ls_R_factor_gt 0.0367 _refine_ls_wR_factor_ref 0.0952 _refine_ls_wR_factor_gt 0.0882 _refine_ls_goodness_of_fit_ref 1.031 _refine_ls_restrained_S_all 1.031 _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 Ca1 Ca 0.53066(3) 0.815121(16) 0.198949(14) 0.01640(7) Uani 1 1 d . . . N1 N 0.46312(12) 0.97798(7) 0.16680(6) 0.0216(2) Uani 1 1 d . . . N2 N 0.47898(11) 1.04108(7) 0.22885(6) 0.0177(2) Uani 1 1 d . . . C1 C 0.42787(15) 1.02661(10) 0.09676(8) 0.0258(3) Uani 1 1 d . . . H1 H 0.4094 1.0002 0.0432 0.031 Uiso 1 1 calc R . . C2 C 0.42174(16) 1.12083(10) 0.11234(9) 0.0276(3) Uani 1 1 d . . . H2 H 0.3994 1.1697 0.0734 0.033 Uiso 1 1 calc R . . C3 C 0.45545(14) 1.12703(9) 0.19702(8) 0.0223(3) Uani 1 1 d . . . H3 H 0.4612 1.1826 0.2279 0.027 Uiso 1 1 calc R . . N3 N 0.71151(11) 0.89309(7) 0.31057(6) 0.0180(2) Uani 1 1 d . . . N4 N 0.67524(11) 0.97251(7) 0.34474(6) 0.01570(19) Uani 1 1 d . . . C4 C 0.85347(13) 0.87873(9) 0.34594(8) 0.0198(2) Uani 1 1 d . . . H4 H 0.9086 0.8280 0.3338 0.024 Uiso 1 1 calc R . . C5 C 0.90996(14) 0.94802(9) 0.40296(8) 0.0210(2) Uani 1 1 d . . . H5 H 1.0072 0.9538 0.4363 0.025 Uiso 1 1 calc R . . C6 C 0.79313(13) 1.00614(9) 0.40019(7) 0.0188(2) Uani 1 1 d . . . H6 H 0.7953 1.0607 0.4320 0.023 Uiso 1 1 calc R . . N5 N 0.38949(11) 0.85870(7) 0.29989(6) 0.0174(2) Uani 1 1 d . . . N6 N 0.41055(11) 0.94234(7) 0.33858(6) 0.01606(19) Uani 1 1 d . . . C7 C 0.30441(13) 0.81060(9) 0.33745(8) 0.0202(2) Uani 1 1 d . . . H7 H 0.2718 0.7493 0.3230 0.024 Uiso 1 1 calc R . . C8 C 0.26930(14) 0.86130(9) 0.40031(8) 0.0217(3) Uani 1 1 d . . . H8 H 0.2103 0.8428 0.4359 0.026 Uiso 1 1 calc R . . C9 C 0.33971(13) 0.94467(9) 0.39917(8) 0.0194(2) Uani 1 1 d . . . H9 H 0.3385 0.9953 0.4351 0.023 Uiso 1 1 calc R . . B1 B 0.51946(15) 1.01399(9) 0.32061(8) 0.0165(2) Uani 1 1 d . . . H1B1 H 0.5140(16) 1.0781(10) 0.3565(9) 0.019(4) Uiso 1 1 d . . . O1 O 0.52475(10) 0.66616(6) 0.26035(6) 0.0244(2) Uani 1 1 d . . . C10 C 0.65367(17) 0.61577(11) 0.30234(9) 0.0327(3) Uani 1 1 d . . . H10A H 0.7095 0.6510 0.3507 0.039 Uiso 1 1 calc R . . H10B H 0.7180 0.6045 0.2648 0.039 Uiso 1 1 calc R . . C11 C 0.5999(2) 0.52448(11) 0.32958(10) 0.0408(4) Uani 1 1 d . . . H11A H 0.6445 0.4715 0.3075 0.049 Uiso 1 1 calc R . . H11B H 0.6246 0.5200 0.3905 0.049 Uiso 1 1 calc R . . C12 C 0.4355(2) 0.52574(11) 0.29452(11) 0.0421(4) Uani 1 1 d . . . H12A H 0.3995 0.4648 0.2712 0.050 Uiso 1 1 calc R . . H12B H 0.3844 0.5427 0.3373 0.050 Uiso 1 1 calc R . . C13 C 0.41313(16) 0.59818(9) 0.22823(9) 0.0267(3) Uani 1 1 d . . . H13A H 0.4257 0.5716 0.1760 0.032 Uiso 1 1 calc R . . H13B H 0.3141 0.6257 0.2183 0.032 Uiso 1 1 calc R . . O2 O 0.30655(10) 0.77658(7) 0.10376(6) 0.0261(2) Uani 1 1 d . . . C14 C 0.29197(16) 0.72262(11) 0.02881(9) 0.0310(3) Uani 1 1 d . . . H14A H 0.3345 0.6602 0.0419 0.037 Uiso 1 1 calc R . . H14B H 0.3422 0.7536 -0.0091 0.037 Uiso 1 1 calc R . . C15 C 0.12953(17) 0.71668(12) -0.00928(9) 0.0360(4) Uani 1 1 d . . . H15A H 0.0853 0.6638 0.0133 0.043 Uiso 1 1 calc R . . H15B H 0.1082 0.7108 -0.0700 0.043 Uiso 1 1 calc R . . C16 C 0.07464(16) 0.80809(11) 0.01570(9) 0.0322(3) Uani 1 1 d . . . H16A H 0.0924 0.8593 -0.0198 0.039 Uiso 1 1 calc R . . H16B H -0.0311 0.8053 0.0137 0.039 Uiso 1 1 calc R . . C17 C 0.16664(16) 0.81837(12) 0.10302(10) 0.0338(3) Uani 1 1 d . . . H17A H 0.1792 0.8844 0.1186 0.041 Uiso 1 1 calc R . . H17B H 0.1201 0.7863 0.1421 0.041 Uiso 1 1 calc R . . B2 B 0.70873(19) 0.76733(11) 0.10976(10) 0.0255(3) Uani 1 1 d . . . H1B2 H 0.763(2) 0.7658(13) 0.1772(12) 0.047(5) Uiso 1 1 d . . . H2B2 H 0.660(2) 0.8393(13) 0.0937(11) 0.045(5) Uiso 1 1 d . . . H3B2 H 0.612(2) 0.7186(13) 0.1014(12) 0.045(5) Uiso 1 1 d . . . H4B2 H 0.786(2) 0.7457(13) 0.0712(11) 0.045(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 Ca1 0.01677(12) 0.01672(11) 0.01572(11) -0.00269(9) 0.00408(8) -0.00099(9) N1 0.0256(6) 0.0221(5) 0.0176(5) 0.0004(4) 0.0062(4) 0.0026(4) N2 0.0173(5) 0.0165(5) 0.0197(5) 0.0014(4) 0.0053(4) 0.0018(4) C1 0.0263(7) 0.0319(7) 0.0198(6) 0.0049(5) 0.0068(5) 0.0055(5) C2 0.0278(7) 0.0271(7) 0.0287(7) 0.0112(6) 0.0084(5) 0.0067(5) C3 0.0203(6) 0.0180(6) 0.0297(7) 0.0058(5) 0.0083(5) 0.0039(5) N3 0.0169(5) 0.0172(5) 0.0202(5) -0.0033(4) 0.0052(4) 0.0009(4) N4 0.0159(5) 0.0149(4) 0.0162(4) -0.0010(4) 0.0038(4) -0.0006(4) C4 0.0175(6) 0.0218(6) 0.0203(6) -0.0008(5) 0.0051(5) 0.0019(4) C5 0.0168(6) 0.0258(6) 0.0187(6) -0.0009(5) 0.0013(4) -0.0017(5) C6 0.0185(6) 0.0201(6) 0.0166(5) -0.0021(4) 0.0024(4) -0.0030(4) N5 0.0168(5) 0.0177(5) 0.0176(5) -0.0025(4) 0.0043(4) -0.0026(4) N6 0.0157(5) 0.0167(5) 0.0160(4) -0.0014(4) 0.0043(4) 0.0009(4) C7 0.0172(6) 0.0217(6) 0.0220(6) 0.0001(5) 0.0054(5) -0.0023(4) C8 0.0190(6) 0.0256(6) 0.0225(6) 0.0029(5) 0.0088(5) 0.0012(5) C9 0.0192(6) 0.0213(6) 0.0190(5) 0.0004(5) 0.0070(5) 0.0038(5) B1 0.0164(6) 0.0161(6) 0.0174(6) -0.0003(5) 0.0049(5) -0.0001(5) O1 0.0212(5) 0.0196(4) 0.0333(5) 0.0015(4) 0.0084(4) -0.0007(3) C10 0.0287(7) 0.0404(8) 0.0282(7) 0.0043(6) 0.0058(6) 0.0095(6) C11 0.0659(12) 0.0246(7) 0.0289(7) -0.0005(6) 0.0067(8) 0.0134(7) C12 0.0610(11) 0.0277(8) 0.0417(9) 0.0051(7) 0.0206(8) -0.0084(7) C13 0.0277(7) 0.0210(6) 0.0331(7) -0.0025(5) 0.0108(6) -0.0052(5) O2 0.0209(5) 0.0320(5) 0.0224(5) -0.0124(4) -0.0001(4) 0.0033(4) C14 0.0296(7) 0.0375(8) 0.0232(6) -0.0143(6) 0.0016(6) 0.0004(6) C15 0.0294(8) 0.0495(9) 0.0263(7) -0.0130(7) 0.0017(6) -0.0097(7) C16 0.0223(7) 0.0432(9) 0.0289(7) 0.0077(6) 0.0025(6) 0.0008(6) C17 0.0204(7) 0.0443(9) 0.0352(8) -0.0150(7) 0.0041(6) 0.0038(6) B2 0.0325(8) 0.0240(7) 0.0235(7) -0.0038(6) 0.0137(6) 0.0008(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 Ca1 O2 2.3725(9) . ? Ca1 O1 2.3950(9) . ? Ca1 N3 2.4652(10) . ? Ca1 N1 2.4653(11) . ? Ca1 N5 2.4813(10) . ? Ca1 B2 2.6052(16) . ? Ca1 H1B2 2.420(19) . ? Ca1 H2B2 2.409(18) . ? Ca1 H3B2 2.417(19) . ? N1 C1 1.3365(16) . ? N1 N2 1.3633(14) . ? N2 C3 1.3495(16) . ? N2 B1 1.5385(17) . ? C1 C2 1.392(2) . ? C1 H1 0.9500 . ? C2 C3 1.377(2) . ? C2 H2 0.9500 . ? C3 H3 0.9500 . ? N3 C4 1.3373(16) . ? N3 N4 1.3651(14) . ? N4 C6 1.3481(15) . ? N4 B1 1.5438(17) . ? C4 C5 1.3951(17) . ? C4 H4 0.9500 . ? C5 C6 1.3775(18) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? N5 C7 1.3330(16) . ? N5 N6 1.3637(14) . ? N6 C9 1.3480(15) . ? N6 B1 1.5412(17) . ? C7 C8 1.3898(18) . ? C7 H7 0.9500 . ? C8 C9 1.3795(18) . ? C8 H8 0.9500 . ? C9 H9 0.9500 . ? B1 H1B1 1.113(14) . ? O1 C10 1.4406(17) . ? O1 C13 1.4425(16) . ? C10 C11 1.525(2) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 C12 1.514(3) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 C13 1.503(2) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? O2 C17 1.4484(17) . ? O2 C14 1.4553(16) . ? C14 C15 1.507(2) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 C16 1.517(2) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 C17 1.509(2) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? B2 H1B2 1.118(19) . ? B2 H2B2 1.142(19) . ? B2 H3B2 1.133(19) . ? B2 H4B2 1.130(18) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Ca1 O1 87.95(4) . . ? O2 Ca1 N3 161.33(3) . . ? O1 Ca1 N3 99.93(3) . . ? O2 Ca1 N1 86.57(4) . . ? O1 Ca1 N1 157.16(4) . . ? N3 Ca1 N1 79.62(4) . . ? O2 Ca1 N5 88.74(3) . . ? O1 Ca1 N5 82.06(3) . . ? N3 Ca1 N5 75.77(3) . . ? N1 Ca1 N5 75.67(3) . . ? O2 Ca1 B2 98.38(4) . . ? O1 Ca1 B2 95.46(4) . . ? N3 Ca1 B2 97.68(4) . . ? N1 Ca1 B2 107.27(4) . . ? N5 Ca1 B2 172.39(5) . . ? O2 Ca1 H1B2 121.2(5) . . ? O1 Ca1 H1B2 85.3(4) . . ? N3 Ca1 H1B2 76.6(5) . . ? N1 Ca1 H1B2 116.3(4) . . ? N5 Ca1 H1B2 147.0(5) . . ? B2 Ca1 H1B2 25.4(4) . . ? O2 Ca1 H2B2 94.2(4) . . ? O1 Ca1 H2B2 121.0(5) . . ? N3 Ca1 H2B2 96.1(4) . . ? N1 Ca1 H2B2 81.5(5) . . ? N5 Ca1 H2B2 156.8(5) . . ? B2 Ca1 H2B2 25.9(5) . . ? H1B2 Ca1 H2B2 44.5(6) . . ? O2 Ca1 H3B2 77.9(5) . . ? O1 Ca1 H3B2 79.4(5) . . ? N3 Ca1 H3B2 120.0(5) . . ? N1 Ca1 H3B2 120.9(5) . . ? N5 Ca1 H3B2 157.4(5) . . ? B2 Ca1 H3B2 25.7(5) . . ? H1B2 Ca1 H3B2 43.4(6) . . ? H2B2 Ca1 H3B2 44.2(6) . . ? C1 N1 N2 105.79(10) . . ? C1 N1 Ca1 133.54(9) . . ? N2 N1 Ca1 120.05(7) . . ? C3 N2 N1 109.90(10) . . ? C3 N2 B1 127.19(11) . . ? N1 N2 B1 122.91(10) . . ? N1 C1 C2 111.35(12) . . ? N1 C1 H1 124.3 . . ? C2 C1 H1 124.3 . . ? C3 C2 C1 104.31(12) . . ? C3 C2 H2 127.8 . . ? C1 C2 H2 127.8 . . ? N2 C3 C2 108.64(12) . . ? N2 C3 H3 125.7 . . ? C2 C3 H3 125.7 . . ? C4 N3 N4 105.86(10) . . ? C4 N3 Ca1 133.63(8) . . ? N4 N3 Ca1 120.33(7) . . ? C6 N4 N3 110.05(10) . . ? C6 N4 B1 127.30(10) . . ? N3 N4 B1 122.65(9) . . ? N3 C4 C5 111.07(11) . . ? N3 C4 H4 124.5 . . ? C5 C4 H4 124.5 . . ? C6 C5 C4 104.54(11) . . ? C6 C5 H5 127.7 . . ? C4 C5 H5 127.7 . . ? N4 C6 C5 108.48(11) . . ? N4 C6 H6 125.8 . . ? C5 C6 H6 125.8 . . ? C7 N5 N6 105.81(10) . . ? C7 N5 Ca1 132.69(8) . . ? N6 N5 Ca1 120.68(7) . . ? C9 N6 N5 109.83(10) . . ? C9 N6 B1 127.62(10) . . ? N5 N6 B1 121.94(9) . . ? N5 C7 C8 111.58(11) . . ? N5 C7 H7 124.2 . . ? C8 C7 H7 124.2 . . ? C9 C8 C7 104.14(11) . . ? C9 C8 H8 127.9 . . ? C7 C8 H8 127.9 . . ? N6 C9 C8 108.64(11) . . ? N6 C9 H9 125.7 . . ? C8 C9 H9 125.7 . . ? N2 B1 N6 110.85(10) . . ? N2 B1 N4 110.00(10) . . ? N6 B1 N4 108.90(10) . . ? N2 B1 H1B1 107.1(7) . . ? N6 B1 H1B1 109.3(8) . . ? N4 B1 H1B1 110.6(8) . . ? C10 O1 C13 106.52(10) . . ? C10 O1 Ca1 123.88(8) . . ? C13 O1 Ca1 123.16(8) . . ? O1 C10 C11 106.33(13) . . ? O1 C10 H10A 110.5 . . ? C11 C10 H10A 110.5 . . ? O1 C10 H10B 110.5 . . ? C11 C10 H10B 110.5 . . ? H10A C10 H10B 108.7 . . ? C12 C11 C10 104.98(12) . . ? C12 C11 H11A 110.8 . . ? C10 C11 H11A 110.8 . . ? C12 C11 H11B 110.8 . . ? C10 C11 H11B 110.8 . . ? H11A C11 H11B 108.8 . . ? C13 C12 C11 103.62(13) . . ? C13 C12 H12A 111.0 . . ? C11 C12 H12A 111.0 . . ? C13 C12 H12B 111.0 . . ? C11 C12 H12B 111.0 . . ? H12A C12 H12B 109.0 . . ? O1 C13 C12 104.24(12) . . ? O1 C13 H13A 110.9 . . ? C12 C13 H13A 110.9 . . ? O1 C13 H13B 110.9 . . ? C12 C13 H13B 110.9 . . ? H13A C13 H13B 108.9 . . ? C17 O2 C14 109.14(10) . . ? C17 O2 Ca1 124.29(8) . . ? C14 O2 Ca1 125.54(8) . . ? O2 C14 C15 105.18(12) . . ? O2 C14 H14A 110.7 . . ? C15 C14 H14A 110.7 . . ? O2 C14 H14B 110.7 . . ? C15 C14 H14B 110.7 . . ? H14A C14 H14B 108.8 . . ? C14 C15 C16 102.38(12) . . ? C14 C15 H15A 111.3 . . ? C16 C15 H15A 111.3 . . ? C14 C15 H15B 111.3 . . ? C16 C15 H15B 111.3 . . ? H15A C15 H15B 109.2 . . ? C17 C16 C15 101.56(12) . . ? C17 C16 H16A 111.5 . . ? C15 C16 H16A 111.5 . . ? C17 C16 H16B 111.5 . . ? C15 C16 H16B 111.5 . . ? H16A C16 H16B 109.3 . . ? O2 C17 C16 105.55(12) . . ? O2 C17 H17A 110.6 . . ? C16 C17 H17A 110.6 . . ? O2 C17 H17B 110.6 . . ? C16 C17 H17B 110.6 . . ? H17A C17 H17B 108.8 . . ? Ca1 B2 H1B2 68.0(10) . . ? Ca1 B2 H2B2 67.4(9) . . ? H1B2 B2 H2B2 108.2(13) . . ? Ca1 B2 H3B2 67.8(10) . . ? H1B2 B2 H3B2 105.4(14) . . ? H2B2 B2 H3B2 106.1(13) . . ? Ca1 B2 H4B2 179.3(9) . . ? H1B2 B2 H4B2 111.9(14) . . ? H2B2 B2 H4B2 113.2(13) . . ? H3B2 B2 H4B2 111.6(13) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O2 Ca1 N1 C1 -55.64(13) . . . . ? O1 Ca1 N1 C1 -132.07(12) . . . . ? N3 Ca1 N1 C1 136.97(13) . . . . ? N5 Ca1 N1 C1 -145.22(13) . . . . ? B2 Ca1 N1 C1 42.07(13) . . . . ? O2 Ca1 N1 N2 134.79(9) . . . . ? O1 Ca1 N1 N2 58.36(14) . . . . ? N3 Ca1 N1 N2 -32.60(9) . . . . ? N5 Ca1 N1 N2 45.21(8) . . . . ? B2 Ca1 N1 N2 -127.50(9) . . . . ? C1 N1 N2 C3 -0.74(14) . . . . ? Ca1 N1 N2 C3 171.42(8) . . . . ? C1 N1 N2 B1 179.84(11) . . . . ? Ca1 N1 N2 B1 -8.00(14) . . . . ? N2 N1 C1 C2 0.52(15) . . . . ? Ca1 N1 C1 C2 -170.11(10) . . . . ? N1 C1 C2 C3 -0.11(16) . . . . ? N1 N2 C3 C2 0.69(15) . . . . ? B1 N2 C3 C2 -179.91(12) . . . . ? C1 C2 C3 N2 -0.35(15) . . . . ? O2 Ca1 N3 C4 177.15(11) . . . . ? O1 Ca1 N3 C4 63.27(12) . . . . ? N1 Ca1 N3 C4 -139.93(12) . . . . ? N5 Ca1 N3 C4 142.38(12) . . . . ? B2 Ca1 N3 C4 -33.68(12) . . . . ? O2 Ca1 N3 N4 -8.50(17) . . . . ? O1 Ca1 N3 N4 -122.38(8) . . . . ? N1 Ca1 N3 N4 34.43(8) . . . . ? N5 Ca1 N3 N4 -43.27(8) . . . . ? B2 Ca1 N3 N4 140.67(9) . . . . ? C4 N3 N4 C6 -0.05(13) . . . . ? Ca1 N3 N4 C6 -175.80(8) . . . . ? C4 N3 N4 B1 180.00(10) . . . . ? Ca1 N3 N4 B1 4.25(14) . . . . ? N4 N3 C4 C5 0.09(14) . . . . ? Ca1 N3 C4 C5 175.03(9) . . . . ? N3 C4 C5 C6 -0.11(14) . . . . ? N3 N4 C6 C5 -0.02(14) . . . . ? B1 N4 C6 C5 179.93(11) . . . . ? C4 C5 C6 N4 0.07(14) . . . . ? O2 Ca1 N5 C7 63.25(11) . . . . ? O1 Ca1 N5 C7 -24.86(11) . . . . ? N3 Ca1 N5 C7 -127.27(11) . . . . ? N1 Ca1 N5 C7 150.03(12) . . . . ? B2 Ca1 N5 C7 -96.3(3) . . . . ? O2 Ca1 N5 N6 -128.75(8) . . . . ? O1 Ca1 N5 N6 143.14(9) . . . . ? N3 Ca1 N5 N6 40.72(8) . . . . ? N1 Ca1 N5 N6 -41.98(8) . . . . ? B2 Ca1 N5 N6 71.7(4) . . . . ? C7 N5 N6 C9 0.33(13) . . . . ? Ca1 N5 N6 C9 -170.52(8) . . . . ? C7 N5 N6 B1 172.08(10) . . . . ? Ca1 N5 N6 B1 1.22(14) . . . . ? N6 N5 C7 C8 -0.06(14) . . . . ? Ca1 N5 C7 C8 169.23(8) . . . . ? N5 C7 C8 C9 -0.22(15) . . . . ? N5 N6 C9 C8 -0.49(14) . . . . ? B1 N6 C9 C8 -171.63(11) . . . . ? C7 C8 C9 N6 0.42(14) . . . . ? C3 N2 B1 N6 125.33(12) . . . . ? N1 N2 B1 N6 -55.35(14) . . . . ? C3 N2 B1 N4 -114.16(13) . . . . ? N1 N2 B1 N4 65.16(14) . . . . ? C9 N6 B1 N2 -130.70(12) . . . . ? N5 N6 B1 N2 59.12(14) . . . . ? C9 N6 B1 N4 108.14(13) . . . . ? N5 N6 B1 N4 -62.04(14) . . . . ? C6 N4 B1 N2 117.40(12) . . . . ? N3 N4 B1 N2 -62.65(14) . . . . ? C6 N4 B1 N6 -120.92(12) . . . . ? N3 N4 B1 N6 59.02(14) . . . . ? O2 Ca1 O1 C10 151.54(10) . . . . ? N3 Ca1 O1 C10 -45.49(10) . . . . ? N1 Ca1 O1 C10 -132.30(11) . . . . ? N5 Ca1 O1 C10 -119.45(10) . . . . ? B2 Ca1 O1 C10 53.31(11) . . . . ? O2 Ca1 O1 C13 3.56(9) . . . . ? N3 Ca1 O1 C13 166.52(9) . . . . ? N1 Ca1 O1 C13 79.72(13) . . . . ? N5 Ca1 O1 C13 92.57(9) . . . . ? B2 Ca1 O1 C13 -94.67(10) . . . . ? C13 O1 C10 C11 -26.24(14) . . . . ? Ca1 O1 C10 C11 -178.67(9) . . . . ? O1 C10 C11 C12 3.95(16) . . . . ? C10 C11 C12 C13 18.50(16) . . . . ? C10 O1 C13 C12 38.37(14) . . . . ? Ca1 O1 C13 C12 -168.96(9) . . . . ? C11 C12 C13 O1 -34.67(15) . . . . ? O1 Ca1 O2 C17 109.85(11) . . . . ? N3 Ca1 O2 C17 -5.82(19) . . . . ? N1 Ca1 O2 C17 -47.97(11) . . . . ? N5 Ca1 O2 C17 27.75(11) . . . . ? B2 Ca1 O2 C17 -154.93(11) . . . . ? O1 Ca1 O2 C14 -83.01(11) . . . . ? N3 Ca1 O2 C14 161.32(12) . . . . ? N1 Ca1 O2 C14 119.17(11) . . . . ? N5 Ca1 O2 C14 -165.11(11) . . . . ? B2 Ca1 O2 C14 12.21(12) . . . . ? C17 O2 C14 C15 -11.76(17) . . . . ? Ca1 O2 C14 C15 179.46(10) . . . . ? O2 C14 C15 C16 32.28(16) . . . . ? C14 C15 C16 C17 -39.81(15) . . . . ? C14 O2 C17 C16 -13.83(17) . . . . ? Ca1 O2 C17 C16 155.12(9) . . . . ? C15 C16 C17 O2 33.35(16) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 28.30 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.367 _refine_diff_density_min -0.300 _refine_diff_density_rms 0.051 #=== data_xkar _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C26 H44 B4 Ca2 N12 O2' _chemical_formula_weight 680.13 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'B' 'B' 0.0013 0.0007 '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' 'Ca' 'Ca' 0.2262 0.3064 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P-1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.1854(6) _cell_length_b 12.8190(6) _cell_length_c 13.8733(7) _cell_angle_alpha 92.260(2) _cell_angle_beta 102.222(2) _cell_angle_gamma 105.636(2) _cell_volume 1862.33(16) _cell_formula_units_Z 2 _cell_measurement_temperature 250(2) _cell_measurement_reflns_used 4096 _cell_measurement_theta_min 2.5 _cell_measurement_theta_max 21.5 _exptl_crystal_description 'flat rhomboid' _exptl_crystal_colour 'colorless' _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.213 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 720 _exptl_absorpt_coefficient_mu 0.347 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.9182 _exptl_absorpt_correction_T_max 0.9465 _exptl_absorpt_process_details 'SADABS, Sheldrick, 1997' _exptl_special_details ; ? ; _diffrn_ambient_temperature 250(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 ? _diffrn_measurement_method 'Bruker APEX2' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 21912 _diffrn_reflns_av_R_equivalents 0.0517 _diffrn_reflns_av_sigmaI/netI 0.0814 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.13 _diffrn_reflns_theta_max 28.32 _reflns_number_total 8988 _reflns_number_gt 4890 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker APEX2' _computing_data_reduction 'Bruker APEX2' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL-Plus _computing_publication_material SHELXL-97 _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^)+(0.0965P)^2^+0.3175P] 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 8988 _refine_ls_number_parameters 452 _refine_ls_number_restraints 11 _refine_ls_R_factor_all 0.1384 _refine_ls_R_factor_gt 0.0694 _refine_ls_wR_factor_ref 0.2048 _refine_ls_wR_factor_gt 0.1745 _refine_ls_goodness_of_fit_ref 1.043 _refine_ls_restrained_S_all 1.043 _refine_ls_shift/su_max 0.031 _refine_ls_shift/su_mean 0.002 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 Ca1 Ca 0.59677(6) 0.24068(5) 0.10818(5) 0.0425(2) Uani 1 1 d . . . N1 N 0.7725(3) 0.2012(3) 0.0510(2) 0.0572(8) Uani 1 1 d . . . N2 N 0.8936(3) 0.2672(3) 0.0836(2) 0.0550(8) Uani 1 1 d . . . C1 C 0.7803(4) 0.1207(4) -0.0075(3) 0.0682(11) Uani 1 1 d . . . H1 H 0.7104 0.0626 -0.0406 0.082 Uiso 1 1 calc R . . C2 C 0.9049(5) 0.1332(4) -0.0134(4) 0.0807(13) Uani 1 1 d . . . H2 H 0.9358 0.0871 -0.0497 0.097 Uiso 1 1 calc R . . C3 C 0.9725(4) 0.2261(4) 0.0443(3) 0.0708(12) Uani 1 1 d . . . H3 H 1.0612 0.2572 0.0551 0.085 Uiso 1 1 calc R . . N3 N 0.7244(3) 0.4224(3) 0.0827(2) 0.0615(9) Uani 1 1 d . . . N4 N 0.8543(3) 0.4503(3) 0.1073(2) 0.0553(8) Uani 1 1 d . . . C4 C 0.6960(4) 0.5136(4) 0.0585(3) 0.0710(12) Uani 1 1 d . . . H4 H 0.6122 0.5186 0.0382 0.085 Uiso 1 1 calc R . . C5 C 0.8027(4) 0.5992(4) 0.0668(3) 0.0705(12) Uani 1 1 d . . . H5 H 0.8070 0.6714 0.0541 0.085 Uiso 1 1 calc R . . C6 C 0.9001(4) 0.5564(3) 0.0972(3) 0.0637(11) Uani 1 1 d . . . H6 H 0.9871 0.5949 0.1095 0.076 Uiso 1 1 calc R . . N5 N 0.7706(3) 0.2988(2) 0.2586(2) 0.0513(7) Uani 1 1 d . . . N6 N 0.8917(3) 0.3454(2) 0.2526(2) 0.0493(7) Uani 1 1 d . . . C7 C 0.7734(4) 0.2914(3) 0.3541(3) 0.0580(10) Uani 1 1 d . . . H7 H 0.7017 0.2614 0.3798 0.070 Uiso 1 1 calc R . . C8 C 0.8965(4) 0.3339(4) 0.4105(3) 0.0713(12) Uani 1 1 d . . . H8 H 0.9243 0.3391 0.4798 0.086 Uiso 1 1 calc R . . C9 C 0.9681(4) 0.3662(3) 0.3440(3) 0.0636(11) Uani 1 1 d . . . H9 H 1.0569 0.3980 0.3593 0.076 Uiso 1 1 calc R . . B1 B 0.9259(4) 0.3716(4) 0.1530(3) 0.0543(11) Uani 1 1 d . . . O1 O 0.4794(2) 0.3255(2) 0.19301(19) 0.0596(7) Uani 1 1 d . B . C10 C 0.3453(4) 0.2867(4) 0.1860(3) 0.0757(12) Uani 1 1 d D . . H10A H 0.3239 0.2150 0.2107 0.091 Uiso 1 1 calc R A 1 H10B H 0.2982 0.2802 0.1168 0.091 Uiso 1 1 calc R A 1 C11 C 0.3106(9) 0.3702(6) 0.2495(12) 0.106(4) Uiso 0.65(3) 1 d PD B 1 H11A H 0.2993 0.3440 0.3133 0.127 Uiso 0.65(3) 1 calc PR B 1 H11B H 0.2321 0.3855 0.2150 0.127 Uiso 0.65(3) 1 calc PR B 1 C11' C 0.3040(8) 0.3903(7) 0.2014(14) 0.070(6) Uiso 0.35(3) 1 d PD B 2 H11C H 0.2753 0.4169 0.1379 0.084 Uiso 0.35(3) 1 calc PR B 2 H11D H 0.2352 0.3766 0.2369 0.084 Uiso 0.35(3) 1 calc PR B 2 C12 C 0.4261(5) 0.4719(4) 0.2639(6) 0.142(3) Uani 1 1 d D . . H12A H 0.4117 0.5212 0.2133 0.170 Uiso 1 1 calc R B 1 H12B H 0.4438 0.5113 0.3297 0.170 Uiso 1 1 calc R B 1 C13 C 0.5359(4) 0.4250(4) 0.2529(5) 0.1047(19) Uani 1 1 d D B . H13A H 0.5957 0.4750 0.2216 0.126 Uiso 1 1 calc R . . H13B H 0.5824 0.4134 0.3179 0.126 Uiso 1 1 calc R . . B2 B 0.4203(5) 0.2251(5) -0.0685(3) 0.0603(12) Uani 1 1 d . . . B3 B 0.5260(5) 0.0452(4) 0.1885(4) 0.0557(11) Uani 1 1 d . . . Ca2 Ca 0.38299(7) 0.12911(6) -0.25962(5) 0.0458(2) Uani 1 1 d . . . N7 N 0.5785(3) 0.2458(2) -0.2969(2) 0.0489(7) Uani 1 1 d . . . N8 N 0.5743(3) 0.2812(2) -0.3887(2) 0.0478(7) Uani 1 1 d . . . C14 C 0.6995(4) 0.2825(3) -0.2480(3) 0.0586(10) Uani 1 1 d . . . H14 H 0.7300 0.2701 -0.1822 0.070 Uiso 1 1 calc R . . C15 C 0.7753(4) 0.3413(3) -0.3053(3) 0.0667(11) Uani 1 1 d . . . H15 H 0.8636 0.3754 -0.2877 0.080 Uiso 1 1 calc R . . C16 C 0.6920(4) 0.3384(3) -0.3937(3) 0.0613(10) Uani 1 1 d . . . H16 H 0.7138 0.3714 -0.4494 0.074 Uiso 1 1 calc R . . N9 N 0.3553(3) 0.0643(2) -0.4332(2) 0.0528(7) Uani 1 1 d . . . N10 N 0.3971(3) 0.1342(2) -0.49813(19) 0.0481(7) Uani 1 1 d . . . C17 C 0.3174(4) -0.0340(3) -0.4832(3) 0.0622(10) Uani 1 1 d . . . H17 H 0.2835 -0.0989 -0.4567 0.075 Uiso 1 1 calc R . . C18 C 0.3338(4) -0.0289(4) -0.5782(3) 0.0700(12) Uani 1 1 d . . . H18 H 0.3143 -0.0871 -0.6276 0.084 Uiso 1 1 calc R . . C19 C 0.3841(4) 0.0778(4) -0.5851(3) 0.0600(10) Uani 1 1 d . . . H19 H 0.4064 0.1079 -0.6418 0.072 Uiso 1 1 calc R . . N11 N 0.3100(3) 0.2700(2) -0.3508(2) 0.0541(8) Uani 1 1 d . . . N12 N 0.3525(3) 0.3025(2) -0.4326(2) 0.0514(7) Uani 1 1 d . . . C20 C 0.2297(4) 0.3265(3) -0.3408(3) 0.0628(10) Uani 1 1 d . . . H20 H 0.1861 0.3210 -0.2894 0.075 Uiso 1 1 calc R . . C21 C 0.2173(4) 0.3943(4) -0.4145(3) 0.0717(12) Uani 1 1 d . . . H21 H 0.1657 0.4417 -0.4237 0.086 Uiso 1 1 calc R . . C22 C 0.2976(4) 0.3765(3) -0.4709(3) 0.0648(11) Uani 1 1 d . . . H22 H 0.3118 0.4110 -0.5277 0.078 Uiso 1 1 calc R . . B4 B 0.4508(4) 0.2566(3) -0.4686(3) 0.0507(10) Uani 1 1 d . . . O2 O 0.1616(3) 0.0424(3) -0.2799(2) 0.0777(9) Uani 1 1 d . . . C23 C 0.1094(7) -0.0234(7) -0.2130(6) 0.106(3) Uiso 0.703(7) 1 d PD C 1 H23A H 0.1161 0.0208 -0.1518 0.127 Uiso 0.703(7) 1 calc PR C 1 H23B H 0.1556 -0.0778 -0.1964 0.127 Uiso 0.703(7) 1 calc PR C 1 C24 C -0.0316(7) -0.0803(9) -0.2621(6) 0.120(3) Uiso 0.703(7) 1 d PD C 1 H24A H -0.0880 -0.0447 -0.2371 0.144 Uiso 0.703(7) 1 calc PR C 1 H24B H -0.0549 -0.1573 -0.2504 0.144 Uiso 0.703(7) 1 calc PR C 1 C25 C -0.0387(7) -0.0674(6) -0.3728(5) 0.100(3) Uiso 0.703(7) 1 d PD C 1 H25A H -0.0222 -0.1293 -0.4060 0.120 Uiso 0.703(7) 1 calc PR C 1 H25B H -0.1224 -0.0610 -0.4064 0.120 Uiso 0.703(7) 1 calc PR C 1 C26 C 0.0672(6) 0.0385(5) -0.3713(5) 0.084(2) Uiso 0.703(7) 1 d PD C 1 H26A H 0.1042 0.0366 -0.4292 0.100 Uiso 0.703(7) 1 calc PR C 1 H26B H 0.0340 0.1019 -0.3708 0.100 Uiso 0.703(7) 1 calc PR C 1 C23' C 0.0894(15) 0.0666(17) -0.2081(16) 0.112(7) Uiso 0.297(7) 1 d PD C 2 H23C H 0.0898 0.1432 -0.2060 0.134 Uiso 0.297(7) 1 calc PR C 2 H23D H 0.1270 0.0517 -0.1415 0.134 Uiso 0.297(7) 1 calc PR C 2 C24' C -0.0475(14) -0.0086(13) -0.2454(13) 0.101(6) Uiso 0.297(7) 1 d PD C 2 H24C H -0.1030 0.0311 -0.2821 0.121 Uiso 0.297(7) 1 calc PR C 2 H24D H -0.0826 -0.0372 -0.1897 0.121 Uiso 0.297(7) 1 calc PR C 2 C25' C -0.0370(14) -0.1017(11) -0.3138(15) 0.074(5) Uiso 0.297(7) 1 d PD C 2 H25C H -0.0471 -0.1698 -0.2826 0.089 Uiso 0.297(7) 1 calc PR C 2 H25D H -0.0989 -0.1138 -0.3777 0.089 Uiso 0.297(7) 1 calc PR C 2 C26' C 0.1007(16) -0.053(2) -0.324(2) 0.142(10) Uiso 0.297(7) 1 d PD C 2 H26C H 0.1499 -0.1030 -0.3001 0.170 Uiso 0.297(7) 1 calc PR C 2 H26D H 0.0987 -0.0501 -0.3952 0.170 Uiso 0.297(7) 1 calc PR C 2 H1B1 H 1.026(4) 0.411(3) 0.166(3) 0.057(10) Uiso 1 1 d . . . H1B2 H 0.324(5) 0.215(4) -0.124(4) 0.117(17) Uiso 1 1 d . . . H2B2 H 0.441(5) 0.303(4) -0.019(4) 0.119(17) Uiso 1 1 d . . . H3B2 H 0.492(5) 0.199(4) -0.079(3) 0.094(16) Uiso 1 1 d . . . H4B2 H 0.392(6) 0.164(5) -0.019(4) 0.13(2) Uiso 1 1 d . . . H1B3 H 0.611(5) 0.052(4) 0.235(4) 0.094(15) Uiso 1 1 d . . . H2B3 H 0.496(4) 0.108(4) 0.209(3) 0.079(13) Uiso 1 1 d . . . H3B3 H 0.464(4) -0.022(3) 0.202(3) 0.063(11) Uiso 1 1 d . . . H4B3 H 0.515(5) 0.038(4) 0.103(4) 0.122(18) Uiso 1 1 d . . . H1B4 H 0.475(3) 0.298(3) -0.531(3) 0.055(10) 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 Ca1 0.0334(4) 0.0510(4) 0.0421(4) 0.0041(3) 0.0083(3) 0.0109(3) N1 0.0385(17) 0.065(2) 0.066(2) -0.0018(17) 0.0121(15) 0.0129(15) N2 0.0361(16) 0.073(2) 0.0607(19) 0.0156(16) 0.0167(14) 0.0179(15) C1 0.063(3) 0.079(3) 0.063(3) -0.004(2) 0.015(2) 0.022(2) C2 0.074(3) 0.105(4) 0.079(3) 0.002(3) 0.036(3) 0.040(3) C3 0.048(2) 0.099(3) 0.078(3) 0.017(3) 0.029(2) 0.031(2) N3 0.0400(18) 0.069(2) 0.076(2) 0.0285(17) 0.0109(15) 0.0156(15) N4 0.0381(17) 0.0617(19) 0.064(2) 0.0180(15) 0.0118(14) 0.0091(14) C4 0.058(3) 0.075(3) 0.087(3) 0.038(2) 0.017(2) 0.026(2) C5 0.076(3) 0.065(3) 0.083(3) 0.033(2) 0.031(2) 0.027(2) C6 0.054(2) 0.060(2) 0.073(3) 0.021(2) 0.016(2) 0.0052(19) N5 0.0451(17) 0.0554(18) 0.0488(18) 0.0089(14) 0.0063(14) 0.0098(14) N6 0.0361(16) 0.0533(17) 0.0525(18) 0.0100(14) 0.0009(13) 0.0096(13) C7 0.059(2) 0.062(2) 0.047(2) 0.0092(18) 0.0049(18) 0.0125(19) C8 0.071(3) 0.084(3) 0.053(2) 0.004(2) -0.007(2) 0.027(2) C9 0.048(2) 0.067(3) 0.063(3) 0.004(2) -0.008(2) 0.0120(19) B1 0.029(2) 0.062(3) 0.067(3) 0.014(2) 0.0051(19) 0.0096(19) O1 0.0440(15) 0.0612(16) 0.0677(17) -0.0189(13) 0.0101(12) 0.0109(12) C10 0.053(3) 0.097(3) 0.085(3) 0.001(3) 0.022(2) 0.031(2) C12 0.171(7) 0.117(5) 0.163(6) -0.017(5) 0.024(5) 0.100(5) C13 0.104(4) 0.077(3) 0.122(5) -0.041(3) 0.046(4) -0.001(3) B2 0.065(3) 0.080(3) 0.037(2) -0.005(2) -0.003(2) 0.036(3) B3 0.058(3) 0.050(3) 0.059(3) 0.016(2) 0.009(2) 0.018(2) Ca2 0.0484(4) 0.0519(4) 0.0366(4) 0.0078(3) 0.0079(3) 0.0148(3) N7 0.0510(18) 0.0512(17) 0.0434(16) 0.0051(13) 0.0081(14) 0.0148(14) N8 0.0540(18) 0.0454(16) 0.0465(17) 0.0063(13) 0.0161(14) 0.0145(14) C14 0.059(2) 0.058(2) 0.051(2) -0.0037(18) 0.0017(19) 0.0131(19) C15 0.056(3) 0.062(2) 0.074(3) 0.002(2) 0.014(2) 0.0044(19) C16 0.065(3) 0.052(2) 0.069(3) 0.0058(19) 0.027(2) 0.0103(19) N9 0.063(2) 0.0538(18) 0.0419(16) 0.0069(14) 0.0094(14) 0.0193(15) N10 0.0532(18) 0.0598(18) 0.0331(15) 0.0036(13) 0.0064(13) 0.0221(14) C17 0.068(3) 0.046(2) 0.066(3) -0.0046(19) 0.001(2) 0.0171(19) C18 0.077(3) 0.077(3) 0.055(3) -0.016(2) -0.002(2) 0.037(3) C19 0.066(3) 0.083(3) 0.036(2) -0.0023(19) 0.0060(17) 0.035(2) N11 0.061(2) 0.0568(18) 0.0527(18) 0.0072(15) 0.0166(15) 0.0270(16) N12 0.0588(19) 0.0542(17) 0.0445(16) 0.0095(14) 0.0087(14) 0.0233(15) C20 0.058(2) 0.072(3) 0.064(3) 0.000(2) 0.011(2) 0.029(2) C21 0.067(3) 0.071(3) 0.077(3) 0.001(2) -0.005(2) 0.038(2) C22 0.077(3) 0.059(2) 0.061(2) 0.014(2) 0.001(2) 0.034(2) B4 0.060(3) 0.055(2) 0.041(2) 0.0136(19) 0.0136(19) 0.021(2) O2 0.0519(17) 0.102(2) 0.0708(19) 0.0231(17) 0.0111(15) 0.0086(16) _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 Ca1 O1 2.369(2) . ? Ca1 N1 2.432(3) . ? Ca1 N5 2.464(3) . ? Ca1 N3 2.465(3) . ? Ca1 B2 2.765(5) . ? Ca1 B3 2.770(5) . ? N1 C1 1.320(5) . ? N1 N2 1.360(4) . ? N2 C3 1.336(5) . ? N2 B1 1.529(6) . ? C1 C2 1.380(6) . ? C2 C3 1.346(6) . ? N3 C4 1.328(5) . ? N3 N4 1.362(4) . ? N4 C6 1.341(5) . ? N4 B1 1.527(5) . ? C4 C5 1.367(6) . ? C5 C6 1.347(6) . ? N5 C7 1.326(4) . ? N5 N6 1.347(4) . ? N6 C9 1.342(4) . ? N6 B1 1.537(5) . ? C7 C8 1.383(5) . ? C8 C9 1.352(6) . ? O1 C13 1.406(5) . ? O1 C10 1.427(5) . ? C10 C11 1.5389(10) . ? C10 C11' 1.5401(10) . ? C11 C12 1.5399(10) . ? C11' C12 1.5384(10) . ? C12 C13 1.5373(10) . ? B2 Ca2 2.778(5) . ? B3 Ca2 2.825(5) 2_655 ? Ca2 O2 2.376(3) . ? Ca2 N9 2.444(3) . ? Ca2 N7 2.462(3) . ? Ca2 N11 2.464(3) . ? Ca2 B3 2.825(5) 2_655 ? N7 C14 1.325(5) . ? N7 N8 1.366(4) . ? N8 C16 1.341(5) . ? N8 B4 1.525(5) . ? C14 C15 1.382(5) . ? C15 C16 1.366(6) . ? N9 C17 1.329(5) . ? N9 N10 1.359(4) . ? N10 C19 1.342(4) . ? N10 B4 1.526(5) . ? C17 C18 1.370(6) . ? C18 C19 1.347(6) . ? N11 C20 1.321(5) . ? N11 N12 1.358(4) . ? N12 C22 1.333(4) . ? N12 B4 1.538(5) . ? C20 C21 1.376(6) . ? C21 C22 1.365(6) . ? O2 C26' 1.28(3) . ? O2 C23 1.393(9) . ? O2 C26 1.458(7) . ? O2 C23' 1.48(2) . ? C23 C24 1.5392(10) . ? C24 C25 1.5396(10) . ? C25 C26 1.5390(10) . ? C23' C24' 1.5397(10) . ? C24' C25' 1.5400(10) . ? C25' C26' 1.5397(10) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Ca1 N1 161.79(10) . . ? O1 Ca1 N5 86.27(10) . . ? N1 Ca1 N5 78.64(10) . . ? O1 Ca1 N3 89.01(10) . . ? N1 Ca1 N3 77.27(11) . . ? N5 Ca1 N3 74.72(10) . . ? O1 Ca1 B2 90.68(13) . . ? N1 Ca1 B2 101.69(14) . . ? N5 Ca1 B2 166.81(14) . . ? N3 Ca1 B2 92.41(14) . . ? O1 Ca1 B3 93.94(13) . . ? N1 Ca1 B3 95.16(14) . . ? N5 Ca1 B3 86.17(13) . . ? N3 Ca1 B3 160.44(13) . . ? B2 Ca1 B3 106.87(16) . . ? C1 N1 N2 106.0(3) . . ? C1 N1 Ca1 133.3(3) . . ? N2 N1 Ca1 120.6(2) . . ? C3 N2 N1 109.1(3) . . ? C3 N2 B1 128.3(3) . . ? N1 N2 B1 122.6(3) . . ? N1 C1 C2 110.9(4) . . ? C3 C2 C1 104.8(4) . . ? N2 C3 C2 109.2(4) . . ? C4 N3 N4 105.1(3) . . ? C4 N3 Ca1 133.7(3) . . ? N4 N3 Ca1 120.7(2) . . ? C6 N4 N3 108.9(3) . . ? C6 N4 B1 129.0(3) . . ? N3 N4 B1 121.5(3) . . ? N3 C4 C5 112.1(4) . . ? C6 C5 C4 104.2(4) . . ? N4 C6 C5 109.7(4) . . ? C7 N5 N6 106.5(3) . . ? C7 N5 Ca1 132.5(3) . . ? N6 N5 Ca1 121.0(2) . . ? C9 N6 N5 109.3(3) . . ? C9 N6 B1 128.9(3) . . ? N5 N6 B1 121.7(3) . . ? N5 C7 C8 110.5(4) . . ? C9 C8 C7 104.8(4) . . ? N6 C9 C8 108.9(4) . . ? N4 B1 N2 111.3(3) . . ? N4 B1 N6 108.8(3) . . ? N2 B1 N6 110.5(3) . . ? C13 O1 C10 112.4(3) . . ? C13 O1 Ca1 122.3(2) . . ? C10 O1 Ca1 125.2(2) . . ? O1 C10 C11 106.9(4) . . ? O1 C10 C11' 104.6(5) . . ? C11 C10 C11' 27.1(6) . . ? C10 C11 C12 103.5(4) . . ? C12 C11' C10 103.6(4) . . ? C13 C12 C11' 105.6(5) . . ? C13 C12 C11 103.5(5) . . ? C11' C12 C11 27.1(6) . . ? O1 C13 C12 106.3(4) . . ? Ca1 B2 Ca2 135.0(2) . . ? Ca1 B3 Ca2 142.7(2) . 2_655 ? O2 Ca2 N9 86.81(11) . . ? O2 Ca2 N7 158.06(10) . . ? N9 Ca2 N7 79.03(10) . . ? O2 Ca2 N11 84.27(11) . . ? N9 Ca2 N11 76.57(10) . . ? N7 Ca2 N11 76.23(10) . . ? O2 Ca2 B2 95.69(15) . . ? N9 Ca2 B2 173.89(14) . . ? N7 Ca2 B2 96.91(15) . . ? N11 Ca2 B2 98.10(13) . . ? O2 Ca2 B3 97.77(13) . 2_655 ? N9 Ca2 B3 93.23(13) . 2_655 ? N7 Ca2 B3 99.67(13) . 2_655 ? N11 Ca2 B3 169.50(13) . 2_655 ? B2 Ca2 B3 91.96(15) . 2_655 ? C14 N7 N8 105.8(3) . . ? C14 N7 Ca2 134.7(3) . . ? N8 N7 Ca2 119.5(2) . . ? C16 N8 N7 109.1(3) . . ? C16 N8 B4 128.3(3) . . ? N7 N8 B4 122.5(3) . . ? N7 C14 C15 111.8(4) . . ? C16 C15 C14 103.9(4) . . ? N8 C16 C15 109.4(4) . . ? C17 N9 N10 105.2(3) . . ? C17 N9 Ca2 133.7(3) . . ? N10 N9 Ca2 120.7(2) . . ? C19 N10 N9 109.4(3) . . ? C19 N10 B4 128.8(3) . . ? N9 N10 B4 121.7(3) . . ? N9 C17 C18 111.5(4) . . ? C19 C18 C17 104.9(4) . . ? N10 C19 C18 109.0(4) . . ? C20 N11 N12 105.3(3) . . ? C20 N11 Ca2 134.3(3) . . ? N12 N11 Ca2 120.4(2) . . ? C22 N12 N11 109.7(3) . . ? C22 N12 B4 128.7(3) . . ? N11 N12 B4 121.5(3) . . ? N11 C20 C21 112.1(4) . . ? C22 C21 C20 103.8(4) . . ? N12 C22 C21 109.1(4) . . ? N8 B4 N10 110.4(3) . . ? N8 B4 N12 110.6(3) . . ? N10 B4 N12 110.7(3) . . ? C26' O2 C23 70.8(11) . . ? C26' O2 C26 63.9(12) . . ? C23 O2 C26 111.9(4) . . ? C26' O2 C23' 107.1(11) . . ? C23 O2 C23' 50.8(8) . . ? C26 O2 C23' 98.7(8) . . ? C26' O2 Ca2 126.0(8) . . ? C23 O2 Ca2 124.3(3) . . ? C26 O2 Ca2 123.1(3) . . ? C23' O2 Ca2 122.0(6) . . ? O2 C23 C24 107.9(6) . . ? C23 C24 C25 103.2(6) . . ? C26 C25 C24 103.2(6) . . ? O2 C26 C25 104.2(5) . . ? O2 C23' C24' 105.8(14) . . ? C23' C24' C25' 105.7(14) . . ? C26' C25' C24' 99.2(14) . . ? O2 C26' C25' 117.5(18) . . ? _diffrn_measured_fraction_theta_max 0.969 _diffrn_reflns_theta_full 28.30 _diffrn_measured_fraction_theta_full 0.971 _refine_diff_density_max 0.872 _refine_diff_density_min -0.495 _refine_diff_density_rms 0.062 #=== data_xaly _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H56 B4 Ca2 N12 O12' _chemical_formula_weight 900.27 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'B' 'B' 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ca' 'Ca' 0.2262 0.3064 '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' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P-1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 14.7469(6) _cell_length_b 16.0986(6) _cell_length_c 21.3320(8) _cell_angle_alpha 73.8910(10) _cell_angle_beta 80.4230(10) _cell_angle_gamma 85.9690(10) _cell_volume 4796.1(3) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 8153 _cell_measurement_theta_min 2.3 _cell_measurement_theta_max 22.9 _exptl_crystal_description 'fragment' _exptl_crystal_colour 'colorless' _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.247 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1904 _exptl_absorpt_coefficient_mu 0.301 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.9151 _exptl_absorpt_correction_T_max 0.9534 _exptl_absorpt_process_details 'SADABS, Sheldrick, 1997' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 ? _diffrn_measurement_method 'Bruker APEX2' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 75459 _diffrn_reflns_av_R_equivalents 0.0741 _diffrn_reflns_av_sigmaI/netI 0.1222 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 1.85 _diffrn_reflns_theta_max 28.21 _reflns_number_total 22400 _reflns_number_gt 11555 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker APEX2' _computing_data_reduction 'Bruker APEX2' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL-Plus _computing_publication_material SHELXL-97 _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^)+(0.1182P)^2^+2.5798P] 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 22400 _refine_ls_number_parameters 1121 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1688 _refine_ls_R_factor_gt 0.0812 _refine_ls_wR_factor_ref 0.2547 _refine_ls_wR_factor_gt 0.2200 _refine_ls_goodness_of_fit_ref 1.085 _refine_ls_restrained_S_all 1.085 _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 Ca1 Ca 0.26658(6) 0.91211(5) 0.18099(4) 0.0237(2) Uani 1 1 d . . . B1 B 0.4027(4) 0.7784(3) 0.2967(3) 0.0285(12) Uani 1 1 d . . . N1 N 0.2842(2) 0.9024(2) 0.29577(18) 0.0277(8) Uani 1 1 d . . . N2 N 0.3437(2) 0.8434(2) 0.32827(18) 0.0285(8) Uani 1 1 d . . . C1 C 0.2485(3) 0.9481(3) 0.3372(2) 0.0292(10) Uani 1 1 d . . . H1 H 0.2050 0.9945 0.3276 0.035 Uiso 1 1 calc R . . C2 C 0.2831(3) 0.9191(3) 0.3966(2) 0.0347(11) Uani 1 1 d . . . H2 H 0.2680 0.9407 0.4343 0.042 Uiso 1 1 calc R . . C3 C 0.3429(3) 0.8536(3) 0.3891(2) 0.0341(11) Uani 1 1 d . . . H3 H 0.3784 0.8204 0.4211 0.041 Uiso 1 1 calc R . . N3 N 0.4356(2) 0.8834(2) 0.18128(18) 0.0294(9) Uani 1 1 d . . . N4 N 0.4672(2) 0.8260(2) 0.23356(18) 0.0271(8) Uani 1 1 d . . . C4 C 0.5094(3) 0.9062(3) 0.1356(2) 0.0310(11) Uani 1 1 d . . . H4 H 0.5080 0.9466 0.0938 0.037 Uiso 1 1 calc R . . C5 C 0.5882(3) 0.8636(3) 0.1566(3) 0.0339(11) Uani 1 1 d . . . H5 H 0.6492 0.8682 0.1332 0.041 Uiso 1 1 calc R . . C6 C 0.5583(3) 0.8136(3) 0.2189(2) 0.0317(11) Uani 1 1 d . . . H6 H 0.5960 0.7760 0.2473 0.038 Uiso 1 1 calc R . . N5 N 0.2833(2) 0.7508(2) 0.23248(18) 0.0298(9) Uani 1 1 d . . . N6 N 0.3419(2) 0.7187(2) 0.27751(18) 0.0286(9) Uani 1 1 d . . . C7 C 0.2468(3) 0.6824(3) 0.2245(2) 0.0307(10) Uani 1 1 d . . . H7 H 0.2029 0.6856 0.1960 0.037 Uiso 1 1 calc R . . C8 C 0.2799(3) 0.6061(3) 0.2625(2) 0.0357(11) Uani 1 1 d . . . H8 H 0.2645 0.5489 0.2649 0.043 Uiso 1 1 calc R . . C9 C 0.3400(3) 0.6313(3) 0.2958(2) 0.0343(11) Uani 1 1 d . . . H9 H 0.3746 0.5938 0.3266 0.041 Uiso 1 1 calc R . . O1 O 0.1089(2) 0.8795(2) 0.20645(16) 0.0337(8) Uani 1 1 d . . . C10 C 0.0368(3) 0.9097(3) 0.2475(3) 0.0436(13) Uani 1 1 d . . . H10A H 0.0625 0.9330 0.2785 0.052 Uiso 1 1 calc R . . H10B H -0.0036 0.8619 0.2723 0.052 Uiso 1 1 calc R . . H10C H 0.0012 0.9554 0.2204 0.052 Uiso 1 1 calc R . . O2 O 0.2644(2) 0.8555(2) 0.08944(15) 0.0351(8) Uani 1 1 d . . . C11 C 0.3342(4) 0.8045(4) 0.0621(3) 0.0529(15) Uani 1 1 d . . . H11A H 0.3596 0.8369 0.0172 0.064 Uiso 1 1 calc R . . H11B H 0.3080 0.7509 0.0607 0.064 Uiso 1 1 calc R . . H11C H 0.3833 0.7905 0.0894 0.064 Uiso 1 1 calc R . . B2 B 0.2568(4) 1.1053(3) 0.1134(3) 0.0284(12) Uani 1 1 d . . . O3 O 0.3018(2) 1.05954(19) 0.16987(15) 0.0306(7) Uani 1 1 d . . . C12 C 0.3544(4) 1.1075(4) 0.1974(3) 0.0530(15) Uani 1 1 d . . . H12A H 0.4013 1.1395 0.1627 0.064 Uiso 1 1 calc R . . H12B H 0.3842 1.0677 0.2322 0.064 Uiso 1 1 calc R . . H12C H 0.3137 1.1482 0.2161 0.064 Uiso 1 1 calc R . . O4 O 0.2142(3) 1.0328(2) 0.10359(19) 0.0517(11) Uani 1 1 d . . . C13 C 0.1663(5) 1.0495(4) 0.0484(4) 0.089(3) Uani 1 1 d . . . H13A H 0.1177 1.0934 0.0519 0.107 Uiso 1 1 calc R . . H13B H 0.1390 0.9961 0.0477 0.107 Uiso 1 1 calc R . . H13C H 0.2095 1.0706 0.0075 0.107 Uiso 1 1 calc R . . O5 O 0.3185(2) 1.1530(2) 0.05573(15) 0.0328(8) Uani 1 1 d . . . C14 C 0.3982(5) 1.1079(4) 0.0347(3) 0.071(2) Uani 1 1 d . . . H14A H 0.4336 1.0862 0.0712 0.085 Uiso 1 1 calc R . . H14B H 0.4360 1.1470 -0.0025 0.085 Uiso 1 1 calc R . . H14C H 0.3803 1.0591 0.0207 0.085 Uiso 1 1 calc R . . O6 O 0.1938(2) 1.1751(2) 0.12367(17) 0.0437(9) Uani 1 1 d . . . C15 C 0.1164(4) 1.1513(4) 0.1746(4) 0.089(3) Uani 1 1 d . . . H15A H 0.0806 1.1087 0.1648 0.107 Uiso 1 1 calc R . . H15B H 0.0776 1.2027 0.1768 0.107 Uiso 1 1 calc R . . H15C H 0.1380 1.1262 0.2171 0.107 Uiso 1 1 calc R . . Ca2 Ca 0.23122(6) 1.28167(5) 0.01841(4) 0.0247(2) Uani 1 1 d . . . B3 B 0.3260(4) 1.4893(4) -0.0127(3) 0.0393(14) Uani 1 1 d . . . N7 N 0.2637(3) 1.3704(3) 0.0880(2) 0.0365(10) Uani 1 1 d . . . N8 N 0.2931(3) 1.4520(3) 0.0614(2) 0.0374(10) Uani 1 1 d . . . C16 C 0.2351(4) 1.3626(4) 0.1520(3) 0.0446(13) Uani 1 1 d . . . H16 H 0.2119 1.3111 0.1830 0.054 Uiso 1 1 calc R . . C17 C 0.2438(4) 1.4395(4) 0.1675(3) 0.0541(16) Uani 1 1 d . . . H17 H 0.2273 1.4518 0.2091 0.065 Uiso 1 1 calc R . . C18 C 0.2819(3) 1.4938(4) 0.1085(3) 0.0483(15) Uani 1 1 d . . . H18 H 0.2978 1.5520 0.1020 0.058 Uiso 1 1 calc R . . N9 N 0.3790(2) 1.3487(2) -0.04229(19) 0.0311(9) Uani 1 1 d . . . N10 N 0.3992(3) 1.4295(2) -0.0402(2) 0.0321(9) Uani 1 1 d . . . C19 C 0.4510(3) 1.3231(3) -0.0805(2) 0.0337(11) Uani 1 1 d . . . H19 H 0.4560 1.2690 -0.0908 0.040 Uiso 1 1 calc R . . C20 C 0.5178(3) 1.3867(3) -0.1032(2) 0.0352(11) Uani 1 1 d . . . H20 H 0.5750 1.3847 -0.1310 0.042 Uiso 1 1 calc R . . C21 C 0.4821(3) 1.4524(3) -0.0765(3) 0.0379(12) Uani 1 1 d . . . H21 H 0.5111 1.5055 -0.0826 0.045 Uiso 1 1 calc R . . N11 N 0.1899(3) 1.4334(2) -0.0436(2) 0.0345(9) Uani 1 1 d . . . N12 N 0.2452(3) 1.5009(2) -0.0518(2) 0.0378(10) Uani 1 1 d . . . C22 C 0.1318(3) 1.4608(3) -0.0874(2) 0.0363(12) Uani 1 1 d . . . H22 H 0.0847 1.4271 -0.0927 0.044 Uiso 1 1 calc R . . C23 C 0.1500(4) 1.5460(3) -0.1244(2) 0.0438(14) Uani 1 1 d . . . H23 H 0.1192 1.5804 -0.1588 0.053 Uiso 1 1 calc R . . C24 C 0.2217(4) 1.5687(3) -0.1000(3) 0.0467(14) Uani 1 1 d . . . H24 H 0.2501 1.6233 -0.1146 0.056 Uiso 1 1 calc R . . O7 O 0.2121(2) 1.24438(19) -0.07977(14) 0.0280(7) Uani 1 1 d . . . C25 C 0.2401(3) 1.2965(3) -0.1457(2) 0.0364(12) Uani 1 1 d . . . H25A H 0.1934 1.3421 -0.1577 0.044 Uiso 1 1 calc R . . H25B H 0.2471 1.2603 -0.1764 0.044 Uiso 1 1 calc R . . H25C H 0.2989 1.3230 -0.1482 0.044 Uiso 1 1 calc R . . O8 O 0.0674(2) 1.2821(2) 0.03053(15) 0.0317(7) Uani 1 1 d . . . C26 C 0.0165(3) 1.3382(3) 0.0654(3) 0.0391(12) Uani 1 1 d . . . H26A H 0.0455 1.3382 0.1036 0.047 Uiso 1 1 calc R . . H26B H -0.0466 1.3181 0.0807 0.047 Uiso 1 1 calc R . . H26C H 0.0154 1.3971 0.0361 0.047 Uiso 1 1 calc R . . H1B1 H 0.440(3) 0.738(2) 0.3358(19) 0.016(10) Uiso 1 1 d . . . H1B3 H 0.356(4) 1.554(4) -0.022(3) 0.066(18) Uiso 1 1 d . . . Ca3 Ca 0.57425(6) 0.25783(6) 0.32382(4) 0.0266(2) Uani 1 1 d . . . B4 B 0.6735(4) 0.1521(4) 0.2010(3) 0.0323(12) Uani 1 1 d . . . N13 N 0.5857(3) 0.1047(2) 0.31772(19) 0.0321(9) Uani 1 1 d . . . N14 N 0.6259(3) 0.0844(2) 0.26155(19) 0.0306(9) Uani 1 1 d . . . C27 C 0.5428(3) 0.0335(3) 0.3549(3) 0.0370(12) Uani 1 1 d . . . H27 H 0.5076 0.0291 0.3972 0.044 Uiso 1 1 calc R . . C28 C 0.5556(3) -0.0330(3) 0.3250(3) 0.0439(13) Uani 1 1 d . . . H28 H 0.5329 -0.0900 0.3418 0.053 Uiso 1 1 calc R . . C29 C 0.6080(3) 0.0017(3) 0.2659(3) 0.0406(12) Uani 1 1 d . . . H29 H 0.6288 -0.0276 0.2329 0.049 Uiso 1 1 calc R . . N15 N 0.7318(3) 0.2450(3) 0.26349(18) 0.0325(9) Uani 1 1 d . . . N16 N 0.7506(3) 0.1949(2) 0.22020(18) 0.0315(9) Uani 1 1 d . . . C30 C 0.8123(3) 0.2730(3) 0.2680(2) 0.0351(11) Uani 1 1 d . . . H30 H 0.8201 0.3099 0.2944 0.042 Uiso 1 1 calc R . . C31 C 0.8838(3) 0.2413(3) 0.2288(2) 0.0380(12) Uani 1 1 d . . . H31 H 0.9477 0.2513 0.2237 0.046 Uiso 1 1 calc R . . C32 C 0.8417(3) 0.1930(3) 0.1997(2) 0.0368(12) Uani 1 1 d . . . H32 H 0.8720 0.1625 0.1696 0.044 Uiso 1 1 calc R . . N17 N 0.5469(3) 0.2659(2) 0.20833(18) 0.0317(9) Uani 1 1 d . . . N18 N 0.6021(3) 0.2195(3) 0.17185(18) 0.0317(9) Uani 1 1 d . . . C33 C 0.4888(3) 0.3111(3) 0.1687(3) 0.0369(12) Uani 1 1 d . . . H33 H 0.4415 0.3492 0.1814 0.044 Uiso 1 1 calc R . . C34 C 0.5058(4) 0.2957(3) 0.1068(3) 0.0448(13) Uani 1 1 d . . . H34 H 0.4750 0.3201 0.0700 0.054 Uiso 1 1 calc R . . C35 C 0.5780(4) 0.2367(3) 0.1118(2) 0.0417(13) Uani 1 1 d . . . H35 H 0.6065 0.2119 0.0777 0.050 Uiso 1 1 calc R . . O9 O 0.6650(2) 0.26689(19) 0.40485(15) 0.0309(7) Uani 1 1 d . . . C36 C 0.7297(4) 0.2037(4) 0.4314(3) 0.0448(13) Uani 1 1 d . . . H36A H 0.7121 0.1467 0.4299 0.054 Uiso 1 1 calc R . . H36B H 0.7311 0.2031 0.4773 0.054 Uiso 1 1 calc R . . H36C H 0.7908 0.2173 0.4054 0.054 Uiso 1 1 calc R . . O10 O 0.6090(2) 0.40744(19) 0.29390(15) 0.0351(8) Uani 1 1 d . . . C37 C 0.5963(4) 0.4711(3) 0.2350(3) 0.0532(15) Uani 1 1 d . . . H37A H 0.6563 0.4873 0.2081 0.064 Uiso 1 1 calc R . . H37B H 0.5650 0.5222 0.2458 0.064 Uiso 1 1 calc R . . H37C H 0.5588 0.4479 0.2102 0.064 Uiso 1 1 calc R . . B5 B 0.3892(4) 0.2536(3) 0.4129(3) 0.0306(12) Uani 1 1 d . . . O11 O 0.4706(2) 0.1958(2) 0.42290(15) 0.0347(8) Uani 1 1 d . . . C38 C 0.4711(4) 0.1404(4) 0.4872(3) 0.0556(17) Uani 1 1 d . . . H38A H 0.4634 0.1750 0.5191 0.067 Uiso 1 1 calc R . . H38B H 0.5297 0.1079 0.4891 0.067 Uiso 1 1 calc R . . H38C H 0.4205 0.1001 0.4981 0.067 Uiso 1 1 calc R . . O12 O 0.4196(2) 0.3044(2) 0.34543(18) 0.0483(10) Uani 1 1 d . . . C39 C 0.3579(5) 0.3696(5) 0.3176(4) 0.100(3) Uani 1 1 d . . . H39A H 0.3102 0.3437 0.3027 0.120 Uiso 1 1 calc R . . H39B H 0.3913 0.4117 0.2800 0.120 Uiso 1 1 calc R . . H39C H 0.3292 0.3988 0.3509 0.120 Uiso 1 1 calc R . . O13 O 0.3037(2) 0.2093(2) 0.42344(16) 0.0349(8) Uani 1 1 d . . . C40 C 0.2991(4) 0.1458(4) 0.3898(4) 0.0653(19) Uani 1 1 d . . . H40A H 0.3085 0.1729 0.3421 0.078 Uiso 1 1 calc R . . H40B H 0.2385 0.1195 0.4032 0.078 Uiso 1 1 calc R . . H40C H 0.3470 0.1012 0.4007 0.078 Uiso 1 1 calc R . . O14 O 0.3662(2) 0.3037(2) 0.46025(19) 0.0505(10) Uani 1 1 d . . . C41 C 0.4339(5) 0.3616(6) 0.4622(5) 0.105(3) Uani 1 1 d . . . H41A H 0.4891 0.3286 0.4756 0.126 Uiso 1 1 calc R . . H41B H 0.4095 0.3944 0.4940 0.126 Uiso 1 1 calc R . . H41C H 0.4496 0.4017 0.4183 0.126 Uiso 1 1 calc R . . Ca4 Ca 0.21072(6) 0.26711(6) 0.50575(4) 0.0272(2) Uani 1 1 d . . . B6 B 0.0076(5) 0.1426(5) 0.5527(4) 0.0505(17) Uani 1 1 d . . . N19 N 0.0929(3) 0.2373(3) 0.4425(2) 0.0503(12) Uani 1 1 d . . . N20 N 0.0273(3) 0.1754(3) 0.4777(3) 0.0541(13) Uani 1 1 d . . . C42 C 0.0885(4) 0.2506(5) 0.3805(3) 0.0628(18) Uani 1 1 d . . . H42 H 0.1274 0.2880 0.3456 0.075 Uiso 1 1 calc R . . C43 C 0.0186(4) 0.2025(5) 0.3719(3) 0.0651(19) Uani 1 1 d . . . H43 H -0.0007 0.2034 0.3313 0.078 Uiso 1 1 calc R . . C44 C -0.0167(5) 0.1536(5) 0.4339(4) 0.0687(19) Uani 1 1 d . . . H44 H -0.0634 0.1121 0.4441 0.082 Uiso 1 1 calc R . . N21 N 0.1754(3) 0.1147(3) 0.5657(2) 0.0411(11) Uani 1 1 d . . . N22 N 0.0874(3) 0.0862(3) 0.5796(3) 0.0490(12) Uani 1 1 d . . . C45 C 0.2236(4) 0.0510(3) 0.6017(3) 0.0460(14) Uani 1 1 d . . . H45 H 0.2878 0.0527 0.6018 0.055 Uiso 1 1 calc R . . C46 C 0.1694(5) -0.0178(4) 0.6389(3) 0.0607(18) Uani 1 1 d . . . H46 H 0.1876 -0.0702 0.6680 0.073 Uiso 1 1 calc R . . C47 C 0.0855(5) 0.0072(4) 0.6240(3) 0.0565(16) Uani 1 1 d . . . H47 H 0.0318 -0.0258 0.6420 0.068 Uiso 1 1 calc R . . N23 N 0.0550(3) 0.2771(3) 0.5735(2) 0.0353(9) Uani 1 1 d . . . N24 N -0.0121(3) 0.2207(3) 0.5795(2) 0.0437(11) Uani 1 1 d . . . C48 C 0.0157(3) 0.3343(3) 0.6052(2) 0.0369(12) Uani 1 1 d . . . H48 H 0.0461 0.3820 0.6095 0.044 Uiso 1 1 calc R . . C49 C -0.0758(3) 0.3149(3) 0.6312(2) 0.0429(14) Uani 1 1 d . . . H49 H -0.1184 0.3449 0.6562 0.051 Uiso 1 1 calc R . . C50 C -0.0906(3) 0.2433(3) 0.6127(3) 0.0456(14) Uani 1 1 d . . . H50 H -0.1471 0.2142 0.6218 0.055 Uiso 1 1 calc R . . O15 O 0.1932(2) 0.4194(2) 0.48167(17) 0.0409(9) Uani 1 1 d . . . C51 C 0.1422(5) 0.4697(4) 0.4359(3) 0.0687(19) Uani 1 1 d . . . H51A H 0.1087 0.4324 0.4189 0.082 Uiso 1 1 calc R . . H51B H 0.1833 0.5064 0.3994 0.082 Uiso 1 1 calc R . . H51C H 0.0983 0.5062 0.4569 0.082 Uiso 1 1 calc R . . O16 O 0.2600(2) 0.2854(2) 0.60170(15) 0.0333(8) Uani 1 1 d . . . C52 C 0.2324(4) 0.2378(3) 0.6681(2) 0.0449(13) Uani 1 1 d . . . H52A H 0.1744 0.2094 0.6717 0.054 Uiso 1 1 calc R . . H52B H 0.2239 0.2771 0.6965 0.054 Uiso 1 1 calc R . . H52C H 0.2799 0.1939 0.6820 0.054 Uiso 1 1 calc R . . H1B4 H 0.702(3) 0.121(3) 0.168(2) 0.026(12) Uiso 1 1 d . . . H1B6 H -0.052(5) 0.100(4) 0.562(3) 0.09(2) Uiso 1 1 d . . . B7 B -0.0340(4) 1.2210(3) -0.0890(3) 0.0301(12) Uani 1 1 d . . . O17 O 0.0556(2) 1.1775(2) -0.07983(16) 0.0327(7) Uani 1 1 d . . . C53 C 0.0708(4) 1.0985(4) -0.0967(3) 0.0515(15) Uani 1 1 d . . . H53A H 0.0298 1.0550 -0.0660 0.062 Uiso 1 1 calc R . . H53B H 0.1349 1.0790 -0.0943 0.062 Uiso 1 1 calc R . . H53C H 0.0583 1.1065 -0.1418 0.062 Uiso 1 1 calc R . . O18 O -0.0269(2) 1.29953(19) -0.06866(16) 0.0320(7) Uani 1 1 d . . . C54 C -0.1053(3) 1.3564(3) -0.0718(3) 0.0434(13) Uani 1 1 d . . . H54A H -0.1207 1.3723 -0.1166 0.052 Uiso 1 1 calc R . . H54B H -0.0918 1.4086 -0.0603 0.052 Uiso 1 1 calc R . . H54C H -0.1575 1.3274 -0.0406 0.052 Uiso 1 1 calc R . . O19 O -0.1103(2) 1.1671(2) -0.05069(15) 0.0328(8) Uani 1 1 d . . . C55 C -0.1143(4) 1.1443(4) 0.0191(2) 0.0456(14) Uani 1 1 d . . . H55A H -0.0559 1.1162 0.0308 0.055 Uiso 1 1 calc R . . H55B H -0.1646 1.1044 0.0400 0.055 Uiso 1 1 calc R . . H55C H -0.1250 1.1965 0.0347 0.055 Uiso 1 1 calc R . . O20 O -0.0526(2) 1.2388(2) -0.15690(15) 0.0321(7) Uani 1 1 d . . . C56 C 0.0090(4) 1.2950(4) -0.2060(3) 0.0479(14) Uani 1 1 d . . . H56A H 0.0119 1.3493 -0.1942 0.057 Uiso 1 1 calc R . . H56B H -0.0127 1.3070 -0.2487 0.057 Uiso 1 1 calc R . . H56C H 0.0704 1.2674 -0.2090 0.057 Uiso 1 1 calc R . . B8 B 0.2686(4) 0.5200(3) 0.5953(3) 0.0291(12) Uani 1 1 d . . . O21 O 0.1833(3) 0.5113(3) 0.5708(2) 0.0536(10) Uani 1 1 d . . . C57 C 0.1236(4) 0.5875(5) 0.5648(3) 0.073(2) Uani 1 1 d . . . H57A H 0.0989 0.5938 0.6089 0.087 Uiso 1 1 calc R . . H57B H 0.0728 0.5817 0.5421 0.087 Uiso 1 1 calc R . . H57C H 0.1588 0.6387 0.5394 0.087 Uiso 1 1 calc R . . O22 O 0.3164(3) 0.4365(2) 0.5963(2) 0.0536(10) Uani 1 1 d . . . C58 C 0.4055(4) 0.4293(4) 0.6197(3) 0.0634(18) Uani 1 1 d . . . H58A H 0.4453 0.4754 0.5909 0.076 Uiso 1 1 calc R . . H58B H 0.4347 0.3729 0.6188 0.076 Uiso 1 1 calc R . . H58C H 0.3961 0.4347 0.6650 0.076 Uiso 1 1 calc R . . O23 O 0.3222(3) 0.5942(2) 0.55549(19) 0.0531(10) Uani 1 1 d . . . C59 C 0.3449(4) 0.5988(4) 0.4860(3) 0.0552(16) Uani 1 1 d . . . H59A H 0.3751 0.5444 0.4808 0.066 Uiso 1 1 calc R . . H59B H 0.3866 0.6467 0.4642 0.066 Uiso 1 1 calc R . . H59C H 0.2886 0.6085 0.4660 0.066 Uiso 1 1 calc R . . O24 O 0.2510(3) 0.5373(3) 0.66109(19) 0.0556(10) Uani 1 1 d . . . C60 C 0.1930(5) 0.4711(5) 0.7096(3) 0.079(2) Uani 1 1 d . . . H60A H 0.1336 0.4709 0.6948 0.095 Uiso 1 1 calc R . . H60B H 0.1831 0.4842 0.7525 0.095 Uiso 1 1 calc R . . H60C H 0.2236 0.4142 0.7138 0.095 Uiso 1 1 calc R . . 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 Ca1 0.0212(5) 0.0252(5) 0.0243(5) -0.0033(4) -0.0091(4) 0.0015(3) B1 0.027(3) 0.029(3) 0.028(3) -0.001(2) -0.012(2) 0.004(2) N1 0.026(2) 0.027(2) 0.028(2) -0.0020(16) -0.0104(16) 0.0052(15) N2 0.027(2) 0.032(2) 0.027(2) -0.0038(16) -0.0122(16) 0.0026(16) C1 0.032(3) 0.025(2) 0.029(2) -0.0025(19) -0.009(2) 0.0015(19) C2 0.042(3) 0.038(3) 0.026(3) -0.011(2) -0.007(2) -0.003(2) C3 0.032(3) 0.045(3) 0.027(3) -0.008(2) -0.013(2) -0.001(2) N3 0.027(2) 0.029(2) 0.031(2) -0.0040(17) -0.0080(17) 0.0022(16) N4 0.021(2) 0.030(2) 0.032(2) -0.0087(17) -0.0122(16) 0.0057(15) C4 0.026(2) 0.033(3) 0.034(3) -0.011(2) -0.001(2) 0.0009(19) C5 0.020(2) 0.038(3) 0.047(3) -0.017(2) -0.006(2) 0.0020(19) C6 0.023(2) 0.039(3) 0.037(3) -0.013(2) -0.011(2) 0.003(2) N5 0.028(2) 0.032(2) 0.030(2) -0.0034(17) -0.0128(17) 0.0003(16) N6 0.028(2) 0.0242(19) 0.032(2) -0.0007(16) -0.0118(17) 0.0035(15) C7 0.025(2) 0.036(3) 0.034(3) -0.011(2) -0.010(2) 0.0025(19) C8 0.039(3) 0.026(2) 0.041(3) -0.008(2) -0.004(2) -0.003(2) C9 0.034(3) 0.030(3) 0.037(3) -0.004(2) -0.013(2) 0.006(2) O1 0.0217(17) 0.0433(19) 0.0363(19) -0.0119(15) -0.0028(14) -0.0006(14) C10 0.031(3) 0.047(3) 0.052(3) -0.012(3) -0.009(2) 0.006(2) O2 0.0288(18) 0.050(2) 0.0304(18) -0.0162(15) -0.0087(14) 0.0065(15) C11 0.030(3) 0.083(4) 0.062(4) -0.046(3) -0.006(3) 0.000(3) B2 0.028(3) 0.028(3) 0.027(3) 0.000(2) -0.012(2) 0.005(2) O3 0.0341(18) 0.0278(17) 0.0306(17) -0.0035(14) -0.0144(14) -0.0010(13) C12 0.077(4) 0.036(3) 0.051(3) -0.003(3) -0.037(3) -0.010(3) O4 0.070(3) 0.0297(19) 0.060(2) 0.0069(17) -0.053(2) -0.0066(17) C13 0.126(6) 0.039(3) 0.114(6) 0.019(4) -0.107(5) -0.023(4) O5 0.0346(18) 0.0310(17) 0.0260(17) -0.0017(14) 0.0000(14) 0.0078(14) C14 0.072(4) 0.048(4) 0.061(4) 0.011(3) 0.021(3) 0.035(3) O6 0.0309(19) 0.0352(19) 0.049(2) 0.0055(16) 0.0055(16) 0.0133(15) C15 0.051(4) 0.069(4) 0.092(5) 0.031(4) 0.041(4) 0.028(3) Ca2 0.0229(5) 0.0239(4) 0.0269(5) -0.0038(4) -0.0093(4) 0.0019(3) B3 0.031(3) 0.030(3) 0.059(4) -0.014(3) -0.006(3) -0.004(2) N7 0.037(2) 0.036(2) 0.040(2) -0.0126(19) -0.0121(19) -0.0001(18) N8 0.031(2) 0.033(2) 0.056(3) -0.023(2) -0.013(2) 0.0041(17) C16 0.048(3) 0.053(3) 0.037(3) -0.019(3) -0.014(3) 0.013(3) C17 0.050(4) 0.070(4) 0.056(4) -0.036(3) -0.022(3) 0.020(3) C18 0.029(3) 0.049(3) 0.080(4) -0.035(3) -0.022(3) 0.009(2) N9 0.025(2) 0.029(2) 0.040(2) -0.0061(18) -0.0120(18) 0.0018(16) N10 0.027(2) 0.0216(19) 0.046(2) -0.0049(17) -0.0089(18) 0.0015(16) C19 0.026(3) 0.035(3) 0.043(3) -0.013(2) -0.009(2) 0.004(2) C20 0.026(3) 0.042(3) 0.039(3) -0.012(2) -0.004(2) -0.004(2) C21 0.024(3) 0.033(3) 0.051(3) -0.001(2) -0.004(2) -0.006(2) N11 0.028(2) 0.031(2) 0.041(2) -0.0024(18) -0.0110(18) 0.0014(17) N12 0.035(2) 0.022(2) 0.051(3) -0.0033(19) -0.006(2) 0.0043(17) C22 0.031(3) 0.042(3) 0.031(3) -0.006(2) -0.008(2) 0.013(2) C23 0.057(4) 0.035(3) 0.033(3) -0.002(2) -0.010(3) 0.023(2) C24 0.051(3) 0.028(3) 0.048(3) 0.003(2) 0.005(3) 0.008(2) O7 0.0282(17) 0.0326(17) 0.0233(16) -0.0054(13) -0.0096(13) 0.0035(13) C25 0.027(3) 0.046(3) 0.031(3) -0.002(2) -0.007(2) 0.005(2) O8 0.0226(16) 0.0358(18) 0.0399(19) -0.0138(15) -0.0097(14) 0.0046(13) C26 0.035(3) 0.044(3) 0.039(3) -0.016(2) -0.005(2) 0.009(2) Ca3 0.0279(5) 0.0271(5) 0.0249(5) -0.0077(4) -0.0037(4) 0.0006(4) B4 0.037(3) 0.036(3) 0.026(3) -0.015(2) -0.004(2) 0.004(2) N13 0.031(2) 0.028(2) 0.037(2) -0.0098(18) -0.0031(18) 0.0028(16) N14 0.033(2) 0.026(2) 0.036(2) -0.0134(17) -0.0069(18) 0.0021(16) C27 0.028(3) 0.035(3) 0.043(3) -0.004(2) -0.002(2) 0.000(2) C28 0.036(3) 0.030(3) 0.064(4) -0.008(3) -0.011(3) -0.006(2) C29 0.036(3) 0.036(3) 0.059(4) -0.022(3) -0.016(3) 0.000(2) N15 0.035(2) 0.037(2) 0.028(2) -0.0114(18) -0.0028(18) -0.0014(17) N16 0.032(2) 0.033(2) 0.027(2) -0.0078(17) -0.0026(17) 0.0023(17) C30 0.034(3) 0.039(3) 0.030(3) -0.002(2) -0.007(2) -0.009(2) C31 0.024(3) 0.052(3) 0.031(3) -0.001(2) -0.003(2) 0.000(2) C32 0.032(3) 0.041(3) 0.033(3) -0.007(2) 0.002(2) 0.009(2) N17 0.035(2) 0.032(2) 0.028(2) -0.0055(17) -0.0102(18) 0.0066(17) N18 0.034(2) 0.038(2) 0.023(2) -0.0072(17) -0.0038(17) -0.0030(17) C33 0.035(3) 0.029(3) 0.046(3) -0.005(2) -0.016(2) 0.000(2) C34 0.052(3) 0.043(3) 0.040(3) -0.003(2) -0.023(3) -0.009(3) C35 0.050(3) 0.048(3) 0.031(3) -0.012(2) -0.009(2) -0.014(3) O9 0.0327(18) 0.0304(17) 0.0300(17) -0.0079(14) -0.0078(14) 0.0022(13) C36 0.052(3) 0.048(3) 0.032(3) -0.005(2) -0.012(2) 0.014(3) O10 0.046(2) 0.0257(17) 0.0308(18) -0.0030(14) -0.0073(15) 0.0001(14) C37 0.084(4) 0.035(3) 0.041(3) 0.000(2) -0.025(3) -0.005(3) B5 0.029(3) 0.033(3) 0.030(3) -0.012(2) 0.001(2) 0.001(2) O11 0.0311(18) 0.0412(19) 0.0295(18) -0.0048(15) -0.0053(14) -0.0020(14) C38 0.035(3) 0.082(4) 0.036(3) 0.004(3) -0.005(2) 0.009(3) O12 0.039(2) 0.043(2) 0.045(2) 0.0037(17) 0.0061(17) 0.0207(16) C39 0.088(5) 0.092(6) 0.068(5) 0.031(4) 0.020(4) 0.058(5) O13 0.0313(18) 0.0373(18) 0.045(2) -0.0239(16) -0.0093(15) 0.0022(14) C40 0.037(3) 0.087(5) 0.099(5) -0.069(4) -0.013(3) 0.003(3) O14 0.034(2) 0.061(2) 0.068(3) -0.042(2) 0.0103(18) -0.0162(17) C41 0.051(4) 0.144(7) 0.156(8) -0.127(7) 0.053(5) -0.054(5) Ca4 0.0233(5) 0.0301(5) 0.0304(5) -0.0107(4) -0.0065(4) 0.0005(4) B6 0.041(4) 0.054(4) 0.062(5) -0.025(4) -0.004(3) -0.006(3) N19 0.045(3) 0.067(3) 0.049(3) -0.032(3) -0.015(2) 0.013(2) N20 0.028(2) 0.065(3) 0.083(4) -0.034(3) -0.024(2) 0.001(2) C42 0.055(4) 0.085(5) 0.054(4) -0.025(3) -0.023(3) 0.022(3) C43 0.051(4) 0.090(5) 0.063(4) -0.017(4) -0.039(3) -0.008(3) C44 0.054(4) 0.093(5) 0.073(5) -0.037(4) -0.026(4) 0.002(4) N21 0.025(2) 0.034(2) 0.062(3) -0.013(2) -0.001(2) -0.0009(17) N22 0.035(3) 0.032(2) 0.076(3) -0.014(2) 0.001(2) -0.0035(19) C45 0.046(3) 0.034(3) 0.051(3) -0.005(3) -0.002(3) 0.008(2) C46 0.061(4) 0.037(3) 0.071(4) -0.010(3) 0.014(3) 0.003(3) C47 0.066(4) 0.035(3) 0.065(4) -0.014(3) 0.008(3) -0.017(3) N23 0.028(2) 0.035(2) 0.045(2) -0.0148(19) -0.0033(19) -0.0027(17) N24 0.024(2) 0.043(3) 0.067(3) -0.022(2) -0.002(2) -0.0031(18) C48 0.040(3) 0.035(3) 0.033(3) -0.006(2) -0.004(2) 0.004(2) C49 0.036(3) 0.043(3) 0.035(3) 0.002(2) 0.004(2) 0.021(2) C50 0.025(3) 0.037(3) 0.064(4) -0.005(3) 0.007(3) 0.007(2) O15 0.051(2) 0.0313(18) 0.042(2) -0.0055(15) -0.0213(17) 0.0048(15) C51 0.092(5) 0.055(4) 0.061(4) -0.010(3) -0.038(4) 0.027(4) O16 0.0332(18) 0.0384(19) 0.0288(18) -0.0072(15) -0.0086(14) -0.0035(14) C52 0.060(4) 0.040(3) 0.036(3) -0.007(2) -0.018(3) 0.000(3) B7 0.028(3) 0.033(3) 0.030(3) -0.006(2) -0.012(2) -0.003(2) O17 0.0282(17) 0.0312(17) 0.0434(19) -0.0120(15) -0.0184(15) 0.0053(13) C53 0.045(3) 0.048(3) 0.075(4) -0.029(3) -0.031(3) 0.013(3) O18 0.0289(17) 0.0287(17) 0.0432(19) -0.0108(14) -0.0203(15) 0.0067(13) C54 0.037(3) 0.040(3) 0.056(3) -0.014(3) -0.019(3) 0.012(2) O19 0.0295(18) 0.0411(19) 0.0280(18) -0.0039(14) -0.0122(14) -0.0053(14) C55 0.046(3) 0.057(3) 0.035(3) -0.006(3) -0.019(2) -0.008(3) O20 0.0253(17) 0.0390(19) 0.0316(18) -0.0040(14) -0.0125(14) -0.0005(14) C56 0.036(3) 0.062(4) 0.040(3) -0.003(3) -0.009(2) -0.006(3) B8 0.035(3) 0.027(3) 0.028(3) -0.010(2) -0.004(2) -0.006(2) O21 0.045(2) 0.056(2) 0.059(3) -0.015(2) -0.0083(19) 0.0040(19) C57 0.045(4) 0.092(5) 0.072(5) -0.013(4) -0.012(3) 0.037(4) O22 0.050(2) 0.049(2) 0.063(3) -0.015(2) -0.018(2) 0.0062(18) C58 0.046(4) 0.068(4) 0.091(5) -0.035(4) -0.039(3) 0.024(3) O23 0.059(3) 0.052(2) 0.048(2) -0.0147(19) -0.0062(19) -0.0007(19) C59 0.068(4) 0.062(4) 0.030(3) -0.007(3) 0.007(3) -0.019(3) O24 0.064(3) 0.053(2) 0.047(2) -0.0095(19) -0.005(2) -0.006(2) C60 0.079(5) 0.094(6) 0.040(4) 0.009(4) 0.016(3) -0.014(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 Ca1 O4 2.352(3) . ? Ca1 O1 2.361(3) . ? Ca1 O2 2.379(3) . ? Ca1 O3 2.404(3) . ? Ca1 N1 2.466(4) . ? Ca1 N3 2.504(4) . ? Ca1 N5 2.535(4) . ? Ca1 B2 3.048(5) . ? B1 N6 1.534(6) . ? B1 N2 1.542(7) . ? B1 N4 1.553(6) . ? N1 C1 1.323(6) . ? N1 N2 1.368(5) . ? N2 C3 1.350(6) . ? C1 C2 1.393(6) . ? C2 C3 1.355(7) . ? N3 C4 1.331(6) . ? N3 N4 1.361(5) . ? N4 C6 1.342(6) . ? C4 C5 1.383(6) . ? C5 C6 1.368(7) . ? N5 C7 1.322(6) . ? N5 N6 1.369(5) . ? N6 C9 1.353(6) . ? C7 C8 1.377(6) . ? C8 C9 1.370(7) . ? O1 C10 1.411(6) . ? O2 C11 1.423(6) . ? B2 O4 1.444(6) . ? B2 O6 1.447(6) . ? B2 O5 1.461(6) . ? B2 O3 1.463(6) . ? B2 Ca2 3.037(5) . ? O3 C12 1.424(6) . ? O4 C13 1.425(6) . ? O5 C14 1.414(6) . ? O5 Ca2 2.372(3) . ? O6 C15 1.431(6) . ? O6 Ca2 2.423(3) . ? Ca2 O8 2.386(3) . ? Ca2 O7 2.397(3) . ? Ca2 N7 2.445(4) . ? Ca2 N9 2.491(4) . ? Ca2 N11 2.521(4) . ? B3 N8 1.535(8) . ? B3 N12 1.536(7) . ? B3 N10 1.546(7) . ? N7 C16 1.334(6) . ? N7 N8 1.350(6) . ? N8 C18 1.337(7) . ? C16 C17 1.386(8) . ? C17 C18 1.374(8) . ? N9 C19 1.341(6) . ? N9 N10 1.370(5) . ? N10 C21 1.349(6) . ? C19 C20 1.400(7) . ? C20 C21 1.370(7) . ? N11 C22 1.336(6) . ? N11 N12 1.359(5) . ? N12 C24 1.347(6) . ? C22 C23 1.398(7) . ? C23 C24 1.365(8) . ? O7 C25 1.434(5) . ? O8 C26 1.423(5) . ? Ca3 O12 2.362(3) . ? Ca3 O10 2.384(3) . ? Ca3 O9 2.395(3) . ? Ca3 O11 2.402(3) . ? Ca3 N15 2.486(4) . ? Ca3 N13 2.497(4) . ? Ca3 N17 2.529(4) . ? Ca3 B5 3.048(5) . ? B4 N16 1.535(7) . ? B4 N18 1.535(7) . ? B4 N14 1.540(7) . ? N13 C27 1.331(6) . ? N13 N14 1.359(5) . ? N14 C29 1.351(6) . ? C27 C28 1.380(7) . ? C28 C29 1.357(7) . ? N15 C30 1.325(6) . ? N15 N16 1.370(5) . ? N16 C32 1.344(6) . ? C30 C31 1.392(7) . ? C31 C32 1.357(7) . ? N17 C33 1.338(6) . ? N17 N18 1.362(5) . ? N18 C35 1.336(6) . ? C33 C34 1.390(7) . ? C34 C35 1.374(8) . ? O9 C36 1.410(6) . ? O10 C37 1.415(6) . ? B5 O14 1.444(6) . ? B5 O13 1.447(6) . ? B5 O12 1.458(6) . ? B5 O11 1.474(6) . ? B5 Ca4 3.053(5) . ? O11 C38 1.415(6) . ? O12 C39 1.408(7) . ? O13 C40 1.413(6) . ? O13 Ca4 2.399(3) . ? O14 C41 1.426(7) . ? O14 Ca4 2.383(3) . ? Ca4 O15 2.366(3) . ? Ca4 O16 2.380(3) . ? Ca4 N21 2.478(4) . ? Ca4 N19 2.515(5) . ? Ca4 N23 2.521(4) . ? B6 N24 1.512(8) . ? B6 N20 1.523(9) . ? B6 N22 1.525(8) . ? N19 C42 1.292(7) . ? N19 N20 1.404(7) . ? N20 C44 1.354(8) . ? C42 C43 1.397(9) . ? C43 C44 1.375(9) . ? N21 C45 1.339(6) . ? N21 N22 1.364(6) . ? N22 C47 1.358(7) . ? C45 C46 1.386(8) . ? C46 C47 1.335(9) . ? N23 C48 1.334(6) . ? N23 N24 1.357(5) . ? N24 C50 1.336(6) . ? C48 C49 1.392(7) . ? C49 C50 1.360(8) . ? O15 C51 1.377(6) . ? O16 C52 1.418(6) . ? B7 O19 1.457(6) . ? B7 O18 1.462(6) . ? B7 O20 1.464(6) . ? B7 O17 1.468(6) . ? O17 C53 1.410(6) . ? O18 C54 1.422(5) . ? O19 C55 1.424(6) . ? O20 C56 1.420(6) . ? B8 O23 1.456(6) . ? B8 O21 1.469(7) . ? B8 O22 1.470(6) . ? B8 O24 1.483(7) . ? O21 C57 1.447(7) . ? O22 C58 1.468(6) . ? O23 C59 1.446(6) . ? O24 C60 1.469(7) . ? 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 O4 Ca1 O1 82.81(12) . . ? O4 Ca1 O2 78.14(13) . . ? O1 Ca1 O2 84.44(11) . . ? O4 Ca1 O3 55.35(11) . . ? O1 Ca1 O3 115.68(11) . . ? O2 Ca1 O3 123.42(11) . . ? O4 Ca1 N1 127.12(13) . . ? O1 Ca1 N1 94.73(12) . . ? O2 Ca1 N1 154.53(12) . . ? O3 Ca1 N1 79.85(11) . . ? O4 Ca1 N3 119.97(13) . . ? O1 Ca1 N3 156.37(12) . . ? O2 Ca1 N3 93.77(12) . . ? O3 Ca1 N3 84.93(11) . . ? N1 Ca1 N3 76.89(12) . . ? O4 Ca1 N5 152.76(12) . . ? O1 Ca1 N5 81.86(12) . . ? O2 Ca1 N5 78.07(12) . . ? O3 Ca1 N5 151.76(11) . . ? N1 Ca1 N5 76.61(12) . . ? N3 Ca1 N5 74.74(12) . . ? O4 Ca1 B2 27.33(13) . . ? O1 Ca1 B2 100.88(13) . . ? O2 Ca1 B2 100.16(13) . . ? O3 Ca1 B2 28.09(12) . . ? N1 Ca1 B2 104.98(14) . . ? N3 Ca1 B2 102.62(13) . . ? N5 Ca1 B2 176.63(14) . . ? N6 B1 N2 111.0(4) . . ? N6 B1 N4 108.2(4) . . ? N2 B1 N4 110.9(4) . . ? C1 N1 N2 105.7(3) . . ? C1 N1 Ca1 132.7(3) . . ? N2 N1 Ca1 121.4(3) . . ? C3 N2 N1 109.7(4) . . ? C3 N2 B1 127.3(4) . . ? N1 N2 B1 122.9(4) . . ? N1 C1 C2 111.0(4) . . ? C3 C2 C1 105.2(4) . . ? N2 C3 C2 108.3(4) . . ? C4 N3 N4 105.6(3) . . ? C4 N3 Ca1 133.3(3) . . ? N4 N3 Ca1 120.6(3) . . ? C6 N4 N3 109.6(4) . . ? C6 N4 B1 127.3(4) . . ? N3 N4 B1 123.0(3) . . ? N3 C4 C5 111.6(4) . . ? C6 C5 C4 104.1(4) . . ? N4 C6 C5 109.1(4) . . ? C7 N5 N6 105.6(4) . . ? C7 N5 Ca1 133.3(3) . . ? N6 N5 Ca1 121.1(3) . . ? C9 N6 N5 109.4(4) . . ? C9 N6 B1 129.0(4) . . ? N5 N6 B1 121.5(3) . . ? N5 C7 C8 112.1(4) . . ? C9 C8 C7 104.5(4) . . ? N6 C9 C8 108.4(4) . . ? C10 O1 Ca1 130.5(3) . . ? C11 O2 Ca1 127.3(3) . . ? O4 B2 O6 114.8(4) . . ? O4 B2 O5 114.3(4) . . ? O6 B2 O5 99.3(3) . . ? O4 B2 O3 98.9(3) . . ? O6 B2 O3 115.5(4) . . ? O5 B2 O3 114.9(4) . . ? O4 B2 Ca2 117.6(3) . . ? O6 B2 Ca2 51.7(2) . . ? O5 B2 Ca2 49.80(19) . . ? O3 B2 Ca2 143.4(3) . . ? O4 B2 Ca1 48.39(19) . . ? O6 B2 Ca1 133.9(3) . . ? O5 B2 Ca1 126.8(3) . . ? O3 B2 Ca1 50.7(2) . . ? Ca2 B2 Ca1 165.2(2) . . ? C12 O3 B2 118.9(4) . . ? C12 O3 Ca1 139.7(3) . . ? B2 O3 Ca1 101.2(3) . . ? C13 O4 B2 117.0(4) . . ? C13 O4 Ca1 138.0(3) . . ? B2 O4 Ca1 104.3(2) . . ? C14 O5 B2 116.6(4) . . ? C14 O5 Ca2 140.3(3) . . ? B2 O5 Ca2 102.1(2) . . ? C15 O6 B2 116.0(4) . . ? C15 O6 Ca2 138.5(3) . . ? B2 O6 Ca2 100.3(3) . . ? O5 Ca2 O8 121.73(11) . . ? O5 Ca2 O7 92.18(11) . . ? O8 Ca2 O7 79.73(11) . . ? O5 Ca2 O6 55.05(10) . . ? O8 Ca2 O6 78.56(11) . . ? O7 Ca2 O6 118.26(12) . . ? O5 Ca2 N7 102.51(13) . . ? O8 Ca2 N7 104.64(12) . . ? O7 Ca2 N7 158.75(12) . . ? O6 Ca2 N7 82.92(14) . . ? O5 Ca2 N9 86.96(12) . . ? O8 Ca2 N9 148.80(12) . . ? O7 Ca2 N9 87.83(12) . . ? O6 Ca2 N9 132.05(12) . . ? N7 Ca2 N9 77.83(14) . . ? O5 Ca2 N11 160.88(12) . . ? O8 Ca2 N11 76.42(12) . . ? O7 Ca2 N11 84.98(12) . . ? O6 Ca2 N11 141.79(13) . . ? N7 Ca2 N11 76.09(14) . . ? N9 Ca2 N11 74.06(12) . . ? O5 Ca2 B2 28.05(12) . . ? O8 Ca2 B2 97.32(13) . . ? O7 Ca2 B2 102.05(13) . . ? O6 Ca2 B2 27.97(13) . . ? N7 Ca2 B2 98.03(14) . . ? N9 Ca2 B2 113.30(13) . . ? N11 Ca2 B2 169.75(14) . . ? N8 B3 N12 110.7(4) . . ? N8 B3 N10 111.7(4) . . ? N12 B3 N10 107.8(5) . . ? C16 N7 N8 106.3(4) . . ? C16 N7 Ca2 130.0(4) . . ? N8 N7 Ca2 121.3(3) . . ? C18 N8 N7 109.3(5) . . ? C18 N8 B3 127.6(5) . . ? N7 N8 B3 122.9(4) . . ? N7 C16 C17 111.2(5) . . ? C18 C17 C16 103.5(5) . . ? N8 C18 C17 109.6(5) . . ? C19 N9 N10 105.8(4) . . ? C19 N9 Ca2 134.0(3) . . ? N10 N9 Ca2 120.2(3) . . ? C21 N10 N9 109.7(4) . . ? C21 N10 B3 126.9(4) . . ? N9 N10 B3 122.0(4) . . ? N9 C19 C20 111.0(4) . . ? C21 C20 C19 104.4(4) . . ? N10 C21 C20 109.1(4) . . ? C22 N11 N12 106.0(4) . . ? C22 N11 Ca2 129.9(3) . . ? N12 N11 Ca2 121.7(3) . . ? C24 N12 N11 110.0(4) . . ? C24 N12 B3 129.8(5) . . ? N11 N12 B3 120.0(4) . . ? N11 C22 C23 110.6(5) . . ? C24 C23 C22 104.8(4) . . ? N12 C24 C23 108.6(5) . . ? C25 O7 Ca2 124.8(3) . . ? C26 O8 Ca2 118.0(3) . . ? O12 Ca3 O10 85.50(12) . . ? O12 Ca3 O9 113.70(13) . . ? O10 Ca3 O9 76.83(11) . . ? O12 Ca3 O11 55.85(11) . . ? O10 Ca3 O11 120.44(12) . . ? O9 Ca3 O11 80.10(11) . . ? O12 Ca3 N15 160.02(13) . . ? O10 Ca3 N15 83.00(12) . . ? O9 Ca3 N15 79.45(12) . . ? O11 Ca3 N15 143.93(12) . . ? O12 Ca3 N13 111.59(13) . . ? O10 Ca3 N13 157.71(12) . . ? O9 Ca3 N13 107.08(12) . . ? O11 Ca3 N13 81.71(12) . . ? N15 Ca3 N13 76.36(13) . . ? O12 Ca3 N17 87.63(13) . . ? O10 Ca3 N17 92.09(12) . . ? O9 Ca3 N17 154.62(12) . . ? O11 Ca3 N17 124.76(12) . . ? N15 Ca3 N17 76.55(13) . . ? N13 Ca3 N17 75.11(13) . . ? O12 Ca3 B5 27.72(13) . . ? O10 Ca3 B5 101.96(13) . . ? O9 Ca3 B5 95.74(13) . . ? O11 Ca3 B5 28.33(13) . . ? N15 Ca3 B5 172.23(14) . . ? N13 Ca3 B5 99.48(14) . . ? N17 Ca3 B5 108.97(14) . . ? N16 B4 N18 111.2(4) . . ? N16 B4 N14 110.3(4) . . ? N18 B4 N14 109.7(4) . . ? C27 N13 N14 105.1(4) . . ? C27 N13 Ca3 132.5(3) . . ? N14 N13 Ca3 120.8(3) . . ? C29 N14 N13 109.5(4) . . ? C29 N14 B4 127.6(4) . . ? N13 N14 B4 122.5(4) . . ? N13 C27 C28 112.2(5) . . ? C29 C28 C27 104.1(4) . . ? N14 C29 C28 109.1(5) . . ? C30 N15 N16 105.9(4) . . ? C30 N15 Ca3 132.2(3) . . ? N16 N15 Ca3 121.6(3) . . ? C32 N16 N15 109.1(4) . . ? C32 N16 B4 129.5(4) . . ? N15 N16 B4 121.4(4) . . ? N15 C30 C31 111.2(5) . . ? C32 C31 C30 104.5(4) . . ? N16 C32 C31 109.3(4) . . ? C33 N17 N18 105.4(4) . . ? C33 N17 Ca3 134.6(3) . . ? N18 N17 Ca3 120.0(3) . . ? C35 N18 N17 109.7(4) . . ? C35 N18 B4 127.7(4) . . ? N17 N18 B4 122.4(4) . . ? N17 C33 C34 111.9(5) . . ? C35 C34 C33 103.3(5) . . ? N18 C35 C34 109.8(5) . . ? C36 O9 Ca3 125.4(3) . . ? C37 O10 Ca3 127.9(3) . . ? O14 B5 O13 99.7(4) . . ? O14 B5 O12 114.6(4) . . ? O13 B5 O12 115.7(4) . . ? O14 B5 O11 114.3(4) . . ? O13 B5 O11 114.3(4) . . ? O12 B5 O11 99.2(4) . . ? O14 B5 Ca3 124.2(3) . . ? O13 B5 Ca3 136.1(3) . . ? O12 B5 Ca3 48.9(2) . . ? O11 B5 Ca3 50.7(2) . . ? O14 B5 Ca4 49.5(2) . . ? O13 B5 Ca4 50.2(2) . . ? O12 B5 Ca4 130.0(3) . . ? O11 B5 Ca4 130.9(3) . . ? Ca3 B5 Ca4 173.6(2) . . ? C38 O11 B5 116.3(4) . . ? C38 O11 Ca3 140.6(3) . . ? B5 O11 Ca3 101.0(3) . . ? C39 O12 B5 116.1(4) . . ? C39 O12 Ca3 139.8(4) . . ? B5 O12 Ca3 103.4(3) . . ? C40 O13 B5 118.5(4) . . ? C40 O13 Ca4 139.1(3) . . ? B5 O13 Ca4 102.2(3) . . ? C41 O14 B5 116.7(4) . . ? C41 O14 Ca4 139.9(3) . . ? B5 O14 Ca4 103.1(3) . . ? O15 Ca4 O16 81.80(11) . . ? O15 Ca4 O14 81.45(13) . . ? O16 Ca4 O14 81.39(12) . . ? O15 Ca4 O13 117.09(12) . . ? O16 Ca4 O13 125.42(11) . . ? O14 Ca4 O13 55.02(12) . . ? O15 Ca4 N21 156.40(14) . . ? O16 Ca4 N21 89.34(14) . . ? O14 Ca4 N21 118.94(14) . . ? O13 Ca4 N21 85.84(13) . . ? O15 Ca4 N19 99.37(14) . . ? O16 Ca4 N19 153.64(14) . . ? O14 Ca4 N19 124.93(15) . . ? O13 Ca4 N19 77.71(13) . . ? N21 Ca4 N19 79.17(16) . . ? O15 Ca4 N23 80.92(13) . . ? O16 Ca4 N23 81.38(12) . . ? O14 Ca4 N23 156.87(13) . . ? O13 Ca4 N23 147.82(12) . . ? N21 Ca4 N23 76.13(13) . . ? N19 Ca4 N23 72.90(14) . . ? O15 Ca4 B5 99.50(14) . . ? O16 Ca4 B5 104.28(13) . . ? O14 Ca4 B5 27.44(13) . . ? O13 Ca4 B5 27.59(13) . . ? N21 Ca4 B5 103.88(14) . . ? N19 Ca4 B5 101.50(15) . . ? N23 Ca4 B5 174.34(15) . . ? N24 B6 N20 107.4(5) . . ? N24 B6 N22 112.7(5) . . ? N20 B6 N22 110.9(5) . . ? C42 N19 N20 107.3(5) . . ? C42 N19 Ca4 134.2(5) . . ? N20 N19 Ca4 116.5(3) . . ? C44 N20 N19 108.4(5) . . ? C44 N20 B6 126.8(6) . . ? N19 N20 B6 124.8(5) . . ? N19 C42 C43 110.6(6) . . ? C44 C43 C42 106.1(6) . . ? N20 C44 C43 107.5(6) . . ? C45 N21 N22 104.8(4) . . ? C45 N21 Ca4 132.5(3) . . ? N22 N21 Ca4 121.3(3) . . ? C47 N22 N21 108.5(5) . . ? C47 N22 B6 129.0(5) . . ? N21 N22 B6 122.2(4) . . ? N21 C45 C46 112.5(5) . . ? C47 C46 C45 103.4(5) . . ? C46 C47 N22 110.8(5) . . ? C48 N23 N24 104.8(4) . . ? C48 N23 Ca4 133.2(3) . . ? N24 N23 Ca4 121.8(3) . . ? C50 N24 N23 111.0(4) . . ? C50 N24 B6 128.2(5) . . ? N23 N24 B6 120.8(4) . . ? N23 C48 C49 111.3(5) . . ? C50 C49 C48 104.5(4) . . ? N24 C50 C49 108.4(5) . . ? C51 O15 Ca4 124.9(3) . . ? C52 O16 Ca4 127.3(3) . . ? O19 B7 O18 113.5(4) . . ? O19 B7 O20 103.1(4) . . ? O18 B7 O20 113.0(4) . . ? O19 B7 O17 112.2(4) . . ? O18 B7 O17 102.5(3) . . ? O20 B7 O17 112.9(4) . . ? C53 O17 B7 116.2(4) . . ? C54 O18 B7 116.0(4) . . ? C55 O19 B7 115.9(4) . . ? C56 O20 B7 116.0(4) . . ? O23 B8 O21 113.8(4) . . ? O23 B8 O22 113.6(4) . . ? O21 B8 O22 102.6(4) . . ? O23 B8 O24 102.0(4) . . ? O21 B8 O24 112.5(4) . . ? O22 B8 O24 112.9(4) . . ? C57 O21 B8 113.1(5) . . ? C58 O22 B8 112.9(4) . . ? C59 O23 B8 115.2(4) . . ? C60 O24 B8 111.5(5) . . ? _diffrn_measured_fraction_theta_max 0.947 _diffrn_reflns_theta_full 28.21 _diffrn_measured_fraction_theta_full 0.947 _refine_diff_density_max 1.826 _refine_diff_density_min -0.533 _refine_diff_density_rms 0.091 #=== data_bcat _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C47 H81 B7 Ca3 N18 O13' _chemical_formula_weight 1302.21 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'B' 'B' 0.0013 0.0007 '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' 'Ca' 'Ca' 0.2262 0.3064 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting hexagonal _symmetry_space_group_name_H-M 'P63/m' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' '-x, -y, z+1/2' 'y, -x+y, z+1/2' 'x-y, x, z+1/2' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' 'x, y, -z-1/2' '-y, x-y, -z-1/2' '-x+y, -x, -z-1/2' _cell_length_a 16.9880(4) _cell_length_b 16.9880(4) _cell_length_c 13.5711(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 3391.80(15) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 5312 _cell_measurement_theta_min 2.4 _cell_measurement_theta_max 24.8 _exptl_crystal_description 'rods' _exptl_crystal_colour 'colorless' _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.275 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1376 _exptl_absorpt_coefficient_mu 0.311 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.9318 _exptl_absorpt_correction_T_max 0.9695 _exptl_absorpt_process_details 'SADABS, Sheldrick, 1997' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 ? _diffrn_measurement_method 'Bruker APEX2' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 40352 _diffrn_reflns_av_R_equivalents 0.0904 _diffrn_reflns_av_sigmaI/netI 0.0463 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 0 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.04 _diffrn_reflns_theta_max 28.27 _reflns_number_total 2920 _reflns_number_gt 2074 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker APEX2' _computing_data_reduction 'Bruker APEX2' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL-Plus _computing_publication_material SHELXL-97 _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^)+(0.0506P)^2^+0.7758P] 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 2920 _refine_ls_number_parameters 162 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0686 _refine_ls_R_factor_gt 0.0405 _refine_ls_wR_factor_ref 0.1035 _refine_ls_wR_factor_gt 0.0954 _refine_ls_goodness_of_fit_ref 1.007 _refine_ls_restrained_S_all 1.007 _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 Ca1 Ca 0.43542(3) 0.23197(3) 0.7500 0.01880(13) Uani 1 2 d S . . N1 N 0.32110(9) 0.13079(10) 0.62915(11) 0.0234(3) Uani 1 1 d . . . N2 N 0.23163(9) 0.08704(9) 0.65621(11) 0.0231(3) Uani 1 1 d . . . C1 C 0.32372(13) 0.09271(12) 0.54437(14) 0.0282(4) Uani 1 1 d . . . H1 H 0.3777 0.1102 0.5079 0.034 Uiso 1 1 calc R . . C2 C 0.23819(13) 0.02454(12) 0.51580(14) 0.0314(4) Uani 1 1 d . . . H2 H 0.2224 -0.0128 0.4588 0.038 Uiso 1 1 calc R . . C3 C 0.18181(12) 0.02334(12) 0.58821(14) 0.0287(4) Uani 1 1 d . . . H3 H 0.1178 -0.0160 0.5904 0.034 Uiso 1 1 calc R . . N3 N 0.31872(13) 0.27718(13) 0.7500 0.0277(5) Uani 1 2 d S . . N4 N 0.22844(13) 0.21332(13) 0.7500 0.0228(4) Uani 1 2 d S . . C4 C 0.32196(18) 0.35639(18) 0.7500 0.0402(8) Uani 1 2 d S . . H4 H 0.3766 0.4135 0.7500 0.048 Uiso 1 2 calc SR . . C5 C 0.2359(2) 0.3461(2) 0.7500 0.0466(9) Uani 1 2 d S . . H5 H 0.2204 0.3926 0.7500 0.056 Uiso 1 2 calc SR . . C6 C 0.17837(18) 0.2546(2) 0.7500 0.0346(6) Uani 1 2 d S . . H6 H 0.1139 0.2249 0.7500 0.041 Uiso 1 2 calc SR . . B1 B 0.19673(19) 0.11123(19) 0.7500 0.0254(6) Uani 1 2 d S . . H1B1 H 0.1230(16) 0.0750(15) 0.7500 0.015(6) Uiso 1 2 d S . . B2 B 0.57586(18) 0.16375(18) 0.7500 0.0221(6) Uani 1 2 d S . . O1 O 0.47757(11) 0.10827(11) 0.7500 0.0259(4) Uani 1 2 d S . . C7 C 0.44202(17) 0.01221(16) 0.7500 0.0321(6) Uani 1 2 d S . . H7A H 0.4644 -0.0049 0.8090 0.039 Uiso 0.50 1 calc PR . . H7B H 0.4644 -0.0049 0.6910 0.039 Uiso 0.50 1 calc PR . . C8 C 0.34099(17) -0.03885(16) 0.7500 0.0299(6) Uani 1 2 d S . . H8A H 0.3187 -0.0337 0.6851 0.036 Uiso 0.50 1 calc PR . . H8B H 0.3185 -0.0135 0.8002 0.036 Uiso 0.50 1 calc PR . . H8C H 0.3192 -0.1030 0.7647 0.036 Uiso 0.50 1 calc PR . . O2 O 0.58531(10) 0.25552(10) 0.7500 0.0211(4) Uani 1 2 d S . . B3 B 0.6667 0.3333 0.7500 0.0211(9) Uani 1 6 d S . . O3 O 0.52700(8) 0.37674(8) 0.66701(10) 0.0252(3) Uani 1 1 d . . . C9 C 0.56137(14) 0.40390(14) 0.57074(16) 0.0380(5) Uani 1 1 d . . . H9A H 0.5978 0.3758 0.5506 0.046 Uiso 1 1 calc R A 1 H9B H 0.6001 0.4708 0.5668 0.046 Uiso 1 1 calc R A 1 C10 C 0.4790(7) 0.3713(7) 0.5064(9) 0.059(3) Uani 0.50 1 d P B 1 H10A H 0.4382 0.3061 0.5170 0.071 Uiso 0.50 1 calc PR B 1 H10B H 0.4978 0.3822 0.4371 0.071 Uiso 0.50 1 calc PR B 1 H10C H 0.4472 0.4044 0.5230 0.071 Uiso 0.50 1 calc PR B 1 C10' C 0.4965(8) 0.3479(8) 0.4926(9) 0.054(2) Uani 0.50 1 d P B 2 H10D H 0.4787 0.2839 0.5023 0.065 Uiso 0.50 1 calc PR B 2 H10E H 0.5254 0.3682 0.4279 0.065 Uiso 0.50 1 calc PR B 2 H10F H 0.4424 0.3544 0.4958 0.065 Uiso 0.50 1 calc PR B 2 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 Ca1 0.0136(2) 0.0155(2) 0.0270(3) 0.000 0.000 0.00703(18) N1 0.0206(7) 0.0254(7) 0.0236(8) -0.0005(6) -0.0008(6) 0.0109(6) N2 0.0201(7) 0.0208(7) 0.0239(8) 0.0007(6) -0.0024(6) 0.0068(6) C1 0.0325(10) 0.0324(9) 0.0234(10) -0.0011(8) -0.0002(8) 0.0190(8) C2 0.0429(11) 0.0283(9) 0.0246(10) -0.0058(8) -0.0084(9) 0.0189(8) C3 0.0273(9) 0.0216(8) 0.0303(10) -0.0030(8) -0.0095(8) 0.0072(7) N3 0.0143(9) 0.0212(10) 0.0476(15) 0.000 0.000 0.0087(8) N4 0.0142(9) 0.0270(11) 0.0270(11) 0.000 0.000 0.0102(8) C4 0.0243(13) 0.0222(13) 0.075(2) 0.000 0.000 0.0124(11) C5 0.0326(15) 0.0369(16) 0.082(3) 0.000 0.000 0.0257(14) C6 0.0236(13) 0.0447(16) 0.0434(18) 0.000 0.000 0.0231(12) B1 0.0192(13) 0.0237(14) 0.0278(16) 0.000 0.000 0.0067(11) B2 0.0195(12) 0.0179(12) 0.0298(15) 0.000 0.000 0.0101(11) O1 0.0167(8) 0.0186(8) 0.0420(11) 0.000 0.000 0.0084(7) C7 0.0266(13) 0.0171(12) 0.0514(18) 0.000 0.000 0.0100(10) C8 0.0253(13) 0.0190(12) 0.0423(17) 0.000 0.000 0.0088(10) O2 0.0162(8) 0.0170(8) 0.0301(10) 0.000 0.000 0.0082(7) B3 0.0205(13) 0.0205(13) 0.022(2) 0.000 0.000 0.0103(7) O3 0.0205(6) 0.0207(6) 0.0310(7) 0.0038(5) -0.0013(5) 0.0076(5) C9 0.0379(11) 0.0344(10) 0.0319(11) 0.0037(9) -0.0026(9) 0.0106(9) C10 0.053(5) 0.054(5) 0.049(6) 0.015(4) -0.020(4) 0.011(3) C10' 0.048(4) 0.065(6) 0.033(3) 0.004(4) -0.009(3) 0.016(3) _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 Ca1 O2 2.3719(16) . ? Ca1 O3 2.4313(12) 10_557 ? Ca1 O3 2.4313(12) . ? Ca1 N3 2.4580(19) . ? Ca1 N1 2.4653(15) . ? Ca1 N1 2.4653(15) 10_557 ? Ca1 O1 2.5365(16) . ? Ca1 B2 2.985(3) 3_665 ? Ca1 B2 3.131(3) . ? N1 C1 1.332(2) . ? N1 N2 1.3667(19) . ? N2 C3 1.350(2) . ? N2 B1 1.544(2) . ? C1 C2 1.386(3) . ? C2 C3 1.365(3) . ? N3 C4 1.319(3) . ? N3 N4 1.366(3) . ? N4 C6 1.346(3) . ? N4 B1 1.537(3) . ? C4 C5 1.383(4) . ? C5 C6 1.361(4) . ? B1 N2 1.544(2) 10_557 ? B2 O1 1.450(3) . ? B2 O3 1.468(2) 11_657 ? B2 O3 1.468(2) 2_655 ? B2 O2 1.485(3) . ? B2 Ca1 2.985(3) 2_655 ? O1 C7 1.429(3) . ? C7 C8 1.486(4) . ? O2 B3 1.3530(15) . ? B3 O2 1.3530(15) 2_655 ? B3 O2 1.3530(15) 3_665 ? O3 C9 1.411(2) . ? O3 B2 1.468(2) 3_665 ? C9 C10' 1.483(12) . ? C9 C10 1.501(12) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Ca1 O3 74.89(4) . 10_557 ? O2 Ca1 O3 74.89(4) . . ? O3 Ca1 O3 55.19(6) 10_557 . ? O2 Ca1 N3 155.90(6) . . ? O3 Ca1 N3 83.80(5) 10_557 . ? O3 Ca1 N3 83.80(5) . . ? O2 Ca1 N1 121.51(4) . . ? O3 Ca1 N1 153.64(5) 10_557 . ? O3 Ca1 N1 106.24(5) . . ? N3 Ca1 N1 74.97(5) . . ? O2 Ca1 N1 121.51(4) . 10_557 ? O3 Ca1 N1 106.24(5) 10_557 10_557 ? O3 Ca1 N1 153.64(5) . 10_557 ? N3 Ca1 N1 74.97(5) . 10_557 ? N1 Ca1 N1 83.41(7) . 10_557 ? O2 Ca1 O1 54.24(5) . . ? O3 Ca1 O1 122.35(4) 10_557 . ? O3 Ca1 O1 122.35(4) . . ? N3 Ca1 O1 149.85(6) . . ? N1 Ca1 O1 82.68(4) . . ? N1 Ca1 O1 82.68(4) 10_557 . ? O2 Ca1 B2 62.88(6) . 3_665 ? O3 Ca1 B2 29.22(3) 10_557 3_665 ? O3 Ca1 B2 29.22(3) . 3_665 ? N3 Ca1 B2 93.02(7) . 3_665 ? N1 Ca1 B2 135.46(4) . 3_665 ? N1 Ca1 B2 135.46(4) 10_557 3_665 ? O1 Ca1 B2 117.13(6) . 3_665 ? O2 Ca1 B2 27.10(6) . . ? O3 Ca1 B2 98.85(5) 10_557 . ? O3 Ca1 B2 98.85(5) . . ? N3 Ca1 B2 177.00(7) . . ? N1 Ca1 B2 102.85(5) . . ? N1 Ca1 B2 102.85(5) 10_557 . ? O1 Ca1 B2 27.15(6) . . ? B2 Ca1 B2 89.98(10) 3_665 . ? C1 N1 N2 105.44(14) . . ? C1 N1 Ca1 135.04(12) . . ? N2 N1 Ca1 118.33(10) . . ? C3 N2 N1 109.46(15) . . ? C3 N2 B1 127.34(16) . . ? N1 N2 B1 123.19(15) . . ? N1 C1 C2 111.84(17) . . ? C3 C2 C1 104.22(16) . . ? N2 C3 C2 109.04(16) . . ? C4 N3 N4 105.52(19) . . ? C4 N3 Ca1 133.63(17) . . ? N4 N3 Ca1 120.84(14) . . ? C6 N4 N3 109.7(2) . . ? C6 N4 B1 129.2(2) . . ? N3 N4 B1 121.12(19) . . ? N3 C4 C5 111.6(2) . . ? C6 C5 C4 104.8(2) . . ? N4 C6 C5 108.4(2) . . ? N4 B1 N2 109.61(13) . 10_557 ? N4 B1 N2 109.61(13) . . ? N2 B1 N2 111.0(2) 10_557 . ? O1 B2 O3 116.22(13) . 11_657 ? O1 B2 O3 116.22(13) . 2_655 ? O3 B2 O3 100.24(18) 11_657 2_655 ? O1 B2 O2 99.63(18) . . ? O3 B2 O2 112.59(14) 11_657 . ? O3 B2 O2 112.59(14) 2_655 . ? O1 B2 Ca1 157.03(16) . 2_655 ? O3 B2 Ca1 53.97(9) 11_657 2_655 ? O3 B2 Ca1 53.97(9) 2_655 2_655 ? O2 B2 Ca1 103.34(14) . 2_655 ? O1 B2 Ca1 52.96(11) . . ? O3 B2 Ca1 129.57(9) 11_657 . ? O3 B2 Ca1 129.57(9) 2_655 . ? O2 B2 Ca1 46.67(10) . . ? Ca1 B2 Ca1 150.02(9) 2_655 . ? C7 O1 B2 115.73(18) . . ? C7 O1 Ca1 144.38(14) . . ? B2 O1 Ca1 99.90(13) . . ? O1 C7 C8 111.8(2) . . ? B3 O2 B2 123.17(15) . . ? B3 O2 Ca1 130.60(9) . . ? B2 O2 Ca1 106.23(13) . . ? O2 B3 O2 120.0 2_655 . ? O2 B3 O2 120.0 2_655 3_665 ? O2 B3 O2 120.0 . 3_665 ? C9 O3 B2 117.92(14) . 3_665 ? C9 O3 Ca1 135.27(11) . . ? B2 O3 Ca1 96.81(10) 3_665 . ? O3 C9 C10' 113.5(5) . . ? O3 C9 C10 105.1(5) . . ? C10' C9 C10 24.5(4) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 28.27 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.323 _refine_diff_density_min -0.306 _refine_diff_density_rms 0.055 # SQUEEZE RESULTS (APPEND TO CIF) loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 0.000 0.000 0.000 6.8 0.4 2 0.667 0.333 0.250 163.4 30.9 3 0.000 0.000 0.500 6.8 0.4 4 0.333 0.667 0.750 163.5 31.0 _platon_squeeze_details ; ; #===end