Supplementary Material (ESI) for Chemical Communications This journal is (c) The Royal Society of Chemistry 2003 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 loop_ _publ_author_name 'Maria Vicente' 'Frank R. Fronczek' 'Owendi Ongayi' _publ_contact_author_name 'Dr Maria Vicente' _publ_contact_author_address ; Department of Chemistry Louisiana State University 433 Choppin Hall Baton Rouge Louisiana 70803 UNITED STATES OF AMERICA ; _publ_contact_author_email VICENTE@LSU.EDU _publ_section_title ; Benzoylbiliverdins from chemical oxidation of dodeca-substituted porphyrins ; data_Compound4 _database_code_CSD 211039 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_compound_source 'local laboratory' _chemical_formula_moiety 'C60 H52 N4 Ni O2, C H2 Cl2, C H4 O, 0.5 (H2 O)' _chemical_formula_sum 'C62 H59 Cl2 N4 Ni O3.50' _chemical_formula_weight 1045.74 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' Ni Ni 0.3393 1.1124 '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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_space_group_name_H-M 'P 21/c ' _symmetry_cell_setting Monoclinic 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 18.426(13) _cell_length_b 13.713(13) _cell_length_c 23.955(19) _cell_angle_alpha 90 _cell_angle_beta 101.90(4) _cell_angle_gamma 90 _cell_volume 5923(8) _cell_formula_units_Z 4 _cell_measurement_temperature 100 _cell_measurement_reflns_used 8252 _cell_measurement_theta_min 2.5 _cell_measurement_theta_max 23.3 _exptl_crystal_description plate _exptl_crystal_colour 'dark red' _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.173 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2196 _exptl_absorpt_coefficient_mu 0.464 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.801 _exptl_absorpt_correction_T_max 0.991 _exptl_absorpt_process_details 'HKL Scalepack (Otwinowski & Minor 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'KappaCCD (with Oxford Cryostream)' _diffrn_measurement_method ' \w scans with \k offsets' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% <2 _diffrn_reflns_number 28976 _diffrn_reflns_av_R_equivalents 0.106 _diffrn_reflns_av_sigmaI/netI 0.113 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 2.5 _diffrn_reflns_theta_max 23.3 _reflns_number_total 7610 _reflns_number_gt 4441 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'COLLECT (Nonius, 2000)' _computing_data_reduction 'Denzo and Scalepack (Otwinowski & Minor, 1997)' _computing_cell_refinement 'Denzo and Scalepack (Otwinowski & Minor, 1997)' _computing_structure_solution 'SIR97 (Altomare, et al., 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-3 (Farrugia, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7610 _refine_ls_number_parameters 684 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.192 _refine_ls_R_factor_gt 0.130 _refine_ls_wR_factor_ref 0.370 _refine_ls_wR_factor_gt 0.331 _refine_ls_goodness_of_fit_ref 1.250 _refine_ls_restrained_S_all 1.250 _refine_ls_shift/su_max 0.005 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni1 Ni 0.67543(7) 0.52286(8) 0.16293(5) 0.0567(5) Uani 1 1 d . . . O1 O 0.7076(6) 0.2967(5) 0.1709(3) 0.089(2) Uani 1 1 d . . . O2 O 0.5799(4) 0.5390(4) 0.2438(3) 0.0682(19) Uani 1 1 d . . . N21 N 0.6165(5) 0.4143(5) 0.1477(3) 0.060(2) Uani 1 1 d . . . N22 N 0.6094(5) 0.5965(5) 0.1084(3) 0.0502(19) Uani 1 1 d . . . N23 N 0.7578(5) 0.6011(5) 0.1637(3) 0.063(2) Uani 1 1 d . . . N24 N 0.7196(5) 0.4730(5) 0.2337(3) 0.058(2) Uani 1 1 d . . . C1 C 0.6404(8) 0.3189(8) 0.1563(4) 0.069(3) Uani 1 1 d . . . C2 C 0.5754(7) 0.2544(7) 0.1429(4) 0.066(3) Uani 1 1 d . . . C3 C 0.5152(7) 0.3072(7) 0.1245(3) 0.062(3) Uani 1 1 d . . . C4 C 0.5413(6) 0.4101(6) 0.1245(3) 0.052(3) Uani 1 1 d . . . C5 C 0.5004(7) 0.4932(6) 0.1022(4) 0.058(3) Uani 1 1 d . . . C6 C 0.5358(6) 0.5832(6) 0.0953(3) 0.050(2) Uani 1 1 d . . . C7 C 0.5006(6) 0.6726(6) 0.0691(3) 0.048(2) Uani 1 1 d . . . C8 C 0.5544(6) 0.7388(6) 0.0686(3) 0.052(2) Uani 1 1 d . . . C9 C 0.6258(6) 0.6911(6) 0.0928(3) 0.051(2) Uani 1 1 d . . . C10 C 0.6972(6) 0.7274(6) 0.0988(4) 0.057(3) Uani 1 1 d . . . C11 C 0.7621(6) 0.6738(7) 0.1258(4) 0.059(3) Uani 1 1 d . . . C12 C 0.8372(6) 0.6880(7) 0.1202(4) 0.062(3) Uani 1 1 d . . . C13 C 0.8787(6) 0.6176(8) 0.1550(4) 0.067(3) Uani 1 1 d . . . C14 C 0.8296(6) 0.5649(7) 0.1839(4) 0.061(3) Uani 1 1 d . . . C15 C 0.8465(6) 0.4966(7) 0.2270(4) 0.065(3) Uani 1 1 d . . . C16 C 0.7940(7) 0.4549(7) 0.2539(4) 0.064(3) Uani 1 1 d . . . C17 C 0.8027(7) 0.4010(7) 0.3076(4) 0.069(3) Uani 1 1 d . . . C18 C 0.7315(7) 0.3903(7) 0.3173(4) 0.064(3) Uani 1 1 d . . . C19 C 0.6819(6) 0.4352(7) 0.2705(4) 0.060(3) Uani 1 1 d . . . C20 C 0.6026(6) 0.4579(6) 0.2621(4) 0.053(2) Uani 1 1 d . . . C21 C 0.5794(9) 0.1442(7) 0.1476(4) 0.095(5) Uani 1 1 d . . . H21A H 0.6229 0.1206 0.1332 0.114 Uiso 1 1 calc R . . H21B H 0.5862 0.1251 0.1882 0.114 Uiso 1 1 calc R . . C22 C 0.5132(10) 0.0990(8) 0.1156(5) 0.106(5) Uani 1 1 d . . . H22A H 0.5110 0.0300 0.1273 0.127 Uiso 1 1 calc R . . H22B H 0.5137 0.1007 0.0743 0.127 Uiso 1 1 calc R . . C23 C 0.4451(9) 0.1544(8) 0.1268(5) 0.098(5) Uani 1 1 d . . . H23A H 0.4456 0.1520 0.1682 0.117 Uiso 1 1 calc R . . H23B H 0.3998 0.1203 0.1069 0.117 Uiso 1 1 calc R . . C24 C 0.4404(8) 0.2645(7) 0.1072(4) 0.087(4) Uani 1 1 d . . . H24A H 0.4232 0.2688 0.0653 0.105 Uiso 1 1 calc R . . H24B H 0.4048 0.3004 0.1255 0.105 Uiso 1 1 calc R . . C25 C 0.4197(6) 0.6940(6) 0.0474(4) 0.056(3) Uani 1 1 d . . . H25A H 0.3973 0.6415 0.0211 0.068 Uiso 1 1 calc R . . H25B H 0.3941 0.6951 0.0799 0.068 Uiso 1 1 calc R . . C26 C 0.4089(7) 0.7898(6) 0.0171(4) 0.076(3) Uani 1 1 d . . . H26A H 0.4191 0.7822 -0.0217 0.091 Uiso 1 1 calc R . . H26B H 0.3567 0.8107 0.0130 0.091 Uiso 1 1 calc R . . C27 C 0.4585(7) 0.8661(7) 0.0483(5) 0.078(3) Uani 1 1 d . . . H27A H 0.4491 0.8726 0.0873 0.094 Uiso 1 1 calc R . . H27B H 0.4470 0.9295 0.0287 0.094 Uiso 1 1 calc R . . C28 C 0.5407(6) 0.8421(6) 0.0520(4) 0.056(3) Uani 1 1 d . . . H28A H 0.5540 0.8539 0.0146 0.067 Uiso 1 1 calc R . . H28B H 0.5719 0.8848 0.0806 0.067 Uiso 1 1 calc R . . C29 C 0.8683(7) 0.7537(8) 0.0783(5) 0.076(3) Uani 1 1 d . . . H29A H 0.8461 0.7349 0.0386 0.091 Uiso 1 1 calc R . . H29B H 0.8553 0.8226 0.0838 0.091 Uiso 1 1 calc R . . C30 C 0.9504(7) 0.7432(9) 0.0884(5) 0.087(4) Uani 1 1 d . . . H30A H 0.9731 0.7848 0.1212 0.105 Uiso 1 1 calc R . . H30B H 0.9677 0.7675 0.0545 0.105 Uiso 1 1 calc R . . C31 C 0.9770(7) 0.6406(10) 0.1002(5) 0.097(4) Uani 1 1 d . . . H31A H 1.0314 0.6382 0.1032 0.116 Uiso 1 1 calc R . . H31B H 0.9535 0.5982 0.0681 0.116 Uiso 1 1 calc R . . C32 C 0.9582(7) 0.6028(9) 0.1554(5) 0.083(3) Uani 1 1 d . . . H32A H 0.9702 0.5324 0.1596 0.100 Uiso 1 1 calc R . . H32B H 0.9885 0.6376 0.1883 0.100 Uiso 1 1 calc R . . C33 C 0.8704(7) 0.3732(9) 0.3499(4) 0.084(4) Uani 1 1 d . . . H33A H 0.8972 0.4328 0.3658 0.101 Uiso 1 1 calc R . . H33B H 0.9037 0.3349 0.3307 0.101 Uiso 1 1 calc R . . C34 C 0.8506(8) 0.3128(12) 0.3982(5) 0.116(5) Uani 1 1 d . . . H34A H 0.8431 0.2442 0.3854 0.140 Uiso 1 1 calc R . . H34B H 0.8930 0.3142 0.4312 0.140 Uiso 1 1 calc R . . C35 C 0.7843(7) 0.3458(10) 0.4172(5) 0.095(4) Uani 1 1 d . . . H35A H 0.7940 0.4118 0.4339 0.114 Uiso 1 1 calc R . . H35B H 0.7756 0.3018 0.4480 0.114 Uiso 1 1 calc R . . C36 C 0.7153(6) 0.3495(7) 0.3721(4) 0.071(3) Uani 1 1 d . . . H36A H 0.6781 0.3910 0.3851 0.085 Uiso 1 1 calc R . . H36B H 0.6944 0.2831 0.3651 0.085 Uiso 1 1 calc R . . C37 C 0.4183(6) 0.4832(6) 0.0861(4) 0.058(3) Uani 1 1 d . . . C38 C 0.3767(8) 0.4970(9) 0.1269(4) 0.087(4) Uani 1 1 d . . . H38 H 0.3997 0.5154 0.1647 0.105 Uiso 1 1 calc R . . C39 C 0.2998(9) 0.4835(14) 0.1118(6) 0.139(7) Uani 1 1 d . . . H39 H 0.2708 0.4917 0.1401 0.166 Uiso 1 1 calc R . . C40 C 0.2649(9) 0.4587(11) 0.0568(7) 0.119(5) Uani 1 1 d . . . H40 H 0.2128 0.4481 0.0473 0.143 Uiso 1 1 calc R . . C41 C 0.3084(9) 0.4497(8) 0.0156(5) 0.091(4) Uani 1 1 d . . . H41 H 0.2856 0.4362 -0.0230 0.109 Uiso 1 1 calc R . . C42 C 0.3839(7) 0.4602(6) 0.0307(4) 0.065(3) Uani 1 1 d . . . H42 H 0.4131 0.4516 0.0027 0.078 Uiso 1 1 calc R . . C43 C 0.7094(6) 0.8246(7) 0.0765(4) 0.063(3) Uani 1 1 d . . . C44 C 0.7029(6) 0.8422(7) 0.0190(4) 0.070(3) Uani 1 1 d . . . H44 H 0.6871 0.7921 -0.0081 0.084 Uiso 1 1 calc R . . C45 C 0.7202(7) 0.9372(8) 0.0009(5) 0.086(4) Uani 1 1 d . . . H45 H 0.7157 0.9504 -0.0386 0.103 Uiso 1 1 calc R . . C46 C 0.7435(7) 1.0102(7) 0.0406(5) 0.075(3) Uani 1 1 d . . . H46 H 0.7569 1.0724 0.0285 0.090 Uiso 1 1 calc R . . C47 C 0.7469(7) 0.9924(7) 0.0962(5) 0.072(3) Uani 1 1 d . . . H47 H 0.7604 1.0436 0.1230 0.086 Uiso 1 1 calc R . . C48 C 0.7312(6) 0.9013(7) 0.1149(4) 0.066(3) Uani 1 1 d . . . H48 H 0.7354 0.8903 0.1546 0.079 Uiso 1 1 calc R . . C49 C 0.9254(7) 0.4715(9) 0.2503(5) 0.076(3) Uani 1 1 d . . . C50 C 0.9723(8) 0.5334(11) 0.2900(5) 0.099(4) Uani 1 1 d . . . H50 H 0.9550 0.5937 0.3018 0.119 Uiso 1 1 calc R . . C51 C 1.0491(9) 0.4998(12) 0.3121(6) 0.107(4) Uani 1 1 d . . . H51 H 1.0825 0.5374 0.3392 0.129 Uiso 1 1 calc R . . C52 C 1.0713(8) 0.4123(13) 0.2923(6) 0.103(4) Uani 1 1 d . . . H52 H 1.1214 0.3922 0.3049 0.124 Uiso 1 1 calc R . . C53 C 1.0241(9) 0.3531(11) 0.2551(7) 0.100(4) Uani 1 1 d . . . H53 H 1.0414 0.2924 0.2439 0.120 Uiso 1 1 calc R . . C54 C 0.9530(7) 0.3808(9) 0.2343(5) 0.085(3) Uani 1 1 d . . . H54 H 0.9210 0.3391 0.2086 0.102 Uiso 1 1 calc R . . C55 C 0.5481(6) 0.3868(6) 0.2757(3) 0.057(3) Uani 1 1 d . . . C56 C 0.5651(7) 0.2867(6) 0.2813(4) 0.066(3) Uani 1 1 d . . . H56 H 0.6133 0.2636 0.2798 0.079 Uiso 1 1 calc R . . C57 C 0.5099(8) 0.2227(8) 0.2889(4) 0.073(3) Uani 1 1 d . . . H57 H 0.5207 0.1551 0.2940 0.088 Uiso 1 1 calc R . . C58 C 0.4390(7) 0.2562(8) 0.2892(4) 0.065(3) Uani 1 1 d . . . H58 H 0.4011 0.2113 0.2933 0.079 Uiso 1 1 calc R . . C59 C 0.4233(7) 0.3533(8) 0.2838(4) 0.072(3) Uani 1 1 d . . . H59 H 0.3748 0.3756 0.2849 0.086 Uiso 1 1 calc R . . C60 C 0.4763(7) 0.4185(7) 0.2767(4) 0.066(3) Uani 1 1 d . . . H60 H 0.4644 0.4859 0.2724 0.080 Uiso 1 1 calc R . . Cl1 Cl 0.7856(3) 0.7865(4) 0.2758(2) 0.1569(18) Uani 1 1 d . . . Cl2 Cl 0.7758(5) 0.6612(6) 0.3704(3) 0.252(4) Uani 1 1 d . . . C1S C 0.7536(13) 0.6958(12) 0.3089(7) 0.163(8) Uani 1 1 d . . . H1S1 H 0.6996 0.7080 0.3031 0.195 Uiso 1 1 calc R . . H1S2 H 0.7589 0.6374 0.2858 0.195 Uiso 1 1 calc R . . O2S O 0.1833(9) 0.6719(10) 0.3099(6) 0.061(4) Uani 0.42 1 d P . . C2S C 0.1638(13) 0.6478(14) 0.2481(9) 0.098(7) Uani 0.63 1 d P . . O3S O 0.242(4) 0.611(3) 0.2323(12) 0.28(4) Uani 0.37 1 d P . . C3S C 0.285(2) 0.552(3) 0.2529(13) 0.085(9) Uani 0.37 1 d P . . O4S O 0.170(4) 0.588(3) 0.207(2) 0.13(2) Uani 0.21 1 d P . . O5S O 0.188(2) 0.854(2) 0.4271(15) 0.112(11) Uiso 0.25 1 d P . . O6S O 0.1775(17) 0.7386(19) 0.3701(12) 0.078(8) Uiso 0.25 1 d P . . 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 0.0595(11) 0.0607(8) 0.0504(8) 0.0063(5) 0.0127(6) 0.0023(6) O1 0.088(7) 0.086(5) 0.091(5) 0.009(4) 0.019(5) 0.031(5) O2 0.071(6) 0.060(4) 0.077(4) 0.005(3) 0.023(4) 0.000(3) N21 0.072(7) 0.048(5) 0.060(5) 0.005(3) 0.016(5) 0.015(4) N22 0.061(7) 0.047(4) 0.041(4) 0.003(3) 0.006(4) 0.002(4) N23 0.076(8) 0.065(5) 0.048(4) 0.006(4) 0.014(4) -0.010(4) N24 0.056(7) 0.068(5) 0.051(5) 0.012(4) 0.009(4) 0.006(4) C1 0.098(11) 0.074(7) 0.043(6) 0.012(5) 0.031(6) 0.011(7) C2 0.098(11) 0.054(6) 0.048(6) -0.001(4) 0.024(6) -0.005(6) C3 0.097(10) 0.054(6) 0.034(5) -0.003(4) 0.013(5) -0.001(6) C4 0.076(9) 0.046(5) 0.037(5) -0.005(4) 0.016(5) -0.002(5) C5 0.082(9) 0.056(6) 0.039(5) 0.004(4) 0.020(5) -0.002(5) C6 0.058(8) 0.057(6) 0.035(5) -0.002(4) 0.009(5) 0.007(5) C7 0.051(7) 0.056(5) 0.041(5) -0.006(4) 0.015(4) 0.000(5) C8 0.067(8) 0.051(5) 0.040(5) -0.003(4) 0.011(5) 0.000(5) C9 0.062(8) 0.047(5) 0.043(5) 0.001(4) 0.006(5) -0.001(5) C10 0.072(9) 0.052(5) 0.046(5) -0.002(4) 0.013(5) -0.003(5) C11 0.060(8) 0.076(6) 0.044(5) -0.001(5) 0.016(5) -0.007(5) C12 0.068(9) 0.071(6) 0.049(5) -0.002(5) 0.016(5) -0.012(5) C13 0.055(9) 0.090(7) 0.053(6) 0.001(5) 0.005(5) -0.005(6) C14 0.036(7) 0.084(6) 0.065(6) 0.013(5) 0.012(5) -0.001(5) C15 0.046(8) 0.089(7) 0.061(6) 0.010(5) 0.009(5) 0.007(5) C16 0.073(10) 0.077(6) 0.044(5) 0.004(5) 0.018(6) 0.000(6) C17 0.074(9) 0.089(7) 0.043(6) 0.009(5) 0.009(5) 0.017(6) C18 0.077(9) 0.065(6) 0.053(6) 0.005(4) 0.022(6) 0.012(5) C19 0.067(9) 0.068(6) 0.047(5) 0.007(5) 0.013(5) 0.006(5) C20 0.068(8) 0.047(5) 0.048(5) 0.006(4) 0.018(5) 0.008(5) C21 0.188(16) 0.053(6) 0.044(6) -0.004(5) 0.024(7) -0.004(7) C22 0.192(17) 0.050(6) 0.062(7) -0.002(5) -0.007(8) -0.016(8) C23 0.146(14) 0.074(8) 0.059(7) 0.004(6) -0.012(7) -0.047(8) C24 0.135(13) 0.074(7) 0.045(6) 0.005(5) 0.001(6) -0.043(7) C25 0.071(9) 0.044(5) 0.056(5) 0.001(4) 0.016(5) -0.002(5) C26 0.084(9) 0.064(6) 0.074(7) -0.016(5) 0.000(6) 0.004(6) C27 0.096(11) 0.054(6) 0.078(7) 0.004(5) 0.000(6) 0.007(6) C28 0.065(8) 0.051(5) 0.049(5) 0.005(4) 0.007(5) 0.013(5) C29 0.066(10) 0.081(7) 0.082(7) 0.002(6) 0.019(6) -0.012(6) C30 0.071(11) 0.118(10) 0.077(7) 0.013(7) 0.026(6) -0.011(7) C31 0.072(10) 0.124(10) 0.102(9) 0.028(7) 0.035(7) -0.010(8) C32 0.057(10) 0.105(8) 0.087(8) 0.003(6) 0.014(6) 0.009(6) C33 0.077(10) 0.125(9) 0.056(6) 0.029(6) 0.023(6) 0.026(7) C34 0.074(11) 0.193(14) 0.078(8) 0.046(8) 0.007(7) 0.036(10) C35 0.072(10) 0.150(11) 0.062(7) 0.023(7) 0.009(6) 0.043(8) C36 0.071(9) 0.082(7) 0.063(6) 0.013(5) 0.024(6) 0.018(6) C37 0.065(9) 0.061(5) 0.042(6) -0.005(4) 0.000(5) -0.018(5) C38 0.084(11) 0.138(10) 0.049(6) -0.024(6) 0.034(6) -0.018(7) C39 0.078(14) 0.27(2) 0.074(9) -0.028(10) 0.032(8) -0.046(12) C40 0.083(12) 0.164(13) 0.113(12) -0.036(10) 0.028(10) -0.025(9) C41 0.077(11) 0.102(8) 0.086(8) -0.026(6) 0.001(7) -0.006(7) C42 0.068(9) 0.065(6) 0.063(6) -0.012(5) 0.017(6) -0.010(5) C43 0.066(8) 0.068(6) 0.057(6) 0.009(5) 0.019(5) -0.003(5) C44 0.069(9) 0.079(7) 0.058(6) 0.005(5) 0.003(5) -0.016(5) C45 0.101(11) 0.087(8) 0.066(7) 0.034(6) 0.012(6) -0.018(7) C46 0.087(10) 0.059(6) 0.072(8) 0.009(5) -0.001(6) -0.014(5) C47 0.078(9) 0.059(6) 0.075(8) -0.002(5) 0.011(6) 0.001(5) C48 0.069(8) 0.071(7) 0.055(6) 0.001(5) 0.007(5) -0.011(5) C49 0.063(9) 0.107(9) 0.062(7) 0.020(6) 0.022(6) 0.011(7) C50 0.064(11) 0.148(12) 0.081(8) 0.021(8) 0.002(7) -0.005(9) C51 0.094(14) 0.151(12) 0.072(8) 0.011(8) 0.006(8) -0.012(10) C52 0.058(11) 0.158(14) 0.093(10) 0.013(9) 0.014(8) 0.020(10) C53 0.074(12) 0.119(10) 0.113(11) 0.030(9) 0.035(9) 0.020(9) C54 0.056(10) 0.108(9) 0.092(8) 0.022(7) 0.017(7) 0.002(7) C55 0.078(9) 0.051(6) 0.043(5) 0.003(4) 0.016(5) 0.008(5) C56 0.083(9) 0.057(6) 0.057(6) 0.002(4) 0.012(5) -0.004(6) C57 0.095(11) 0.071(7) 0.050(6) 0.004(5) 0.008(6) 0.000(7) C58 0.079(10) 0.079(8) 0.044(6) -0.007(5) 0.024(5) -0.026(6) C59 0.090(10) 0.068(7) 0.058(6) 0.000(5) 0.015(6) 0.005(6) C60 0.088(10) 0.061(6) 0.051(6) 0.005(4) 0.016(5) 0.005(6) Cl1 0.155(5) 0.178(4) 0.138(3) 0.020(3) 0.031(3) -0.021(3) Cl2 0.306(11) 0.270(8) 0.167(5) 0.058(5) 0.020(6) -0.090(7) C1S 0.24(2) 0.130(12) 0.120(13) 0.048(10) 0.034(13) -0.015(13) O2S 0.062(12) 0.061(8) 0.060(10) 0.026(7) 0.012(8) -0.010(7) C2S 0.104(19) 0.076(12) 0.101(16) 0.032(11) -0.011(12) -0.042(12) O3S 0.50(9) 0.24(4) 0.073(18) -0.06(2) -0.03(3) 0.27(6) C3S 0.08(3) 0.11(2) 0.08(2) -0.014(17) 0.022(17) 0.031(19) O4S 0.22(6) 0.05(2) 0.17(5) 0.05(3) 0.17(5) 0.03(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 Ni1 N21 1.835(8) . ? Ni1 N24 1.853(8) . ? Ni1 N23 1.856(8) . ? Ni1 N22 1.884(7) . ? O1 C1 1.253(14) . ? O2 C20 1.235(10) . ? N21 C1 1.382(12) . ? N21 C4 1.383(12) . ? N22 C6 1.341(12) . ? N22 C9 1.400(11) . ? N23 C11 1.361(11) . ? N23 C14 1.403(12) . ? N24 C19 1.334(11) . ? N24 C16 1.379(13) . ? C1 C2 1.470(16) . ? C2 C3 1.322(14) . ? C2 C21 1.515(14) . ? C3 C24 1.477(16) . ? C3 C4 1.492(12) . ? C4 C5 1.409(13) . ? C5 C6 1.421(13) . ? C5 C37 1.488(15) . ? C6 C7 1.467(12) . ? C7 C8 1.346(12) . ? C7 C25 1.502(13) . ? C8 C9 1.476(13) . ? C8 C28 1.479(12) . ? C9 C10 1.386(13) . ? C10 C11 1.439(14) . ? C10 C43 1.471(12) . ? C11 C12 1.431(14) . ? C12 C13 1.395(14) . ? C12 C29 1.545(13) . ? C13 C14 1.441(13) . ? C13 C32 1.478(15) . ? C14 C15 1.381(13) . ? C15 C16 1.391(14) . ? C15 C49 1.487(15) . ? C16 C17 1.462(13) . ? C17 C18 1.387(14) . ? C17 C33 1.486(15) . ? C18 C19 1.432(14) . ? C18 C36 1.510(13) . ? C19 C20 1.466(14) . ? C20 C55 1.485(13) . ? C21 C22 1.440(18) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 C23 1.54(2) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 C24 1.578(15) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 C26 1.495(12) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 C27 1.486(14) . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C27 C28 1.533(15) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C29 C30 1.488(16) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C30 C31 1.498(16) . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? C31 C32 1.525(15) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C33 C34 1.528(16) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C34 C35 1.460(16) . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? C35 C36 1.490(16) . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? C36 H36A 0.9900 . ? C36 H36B 0.9900 . ? C37 C38 1.373(14) . ? C37 C42 1.385(13) . ? C38 C39 1.402(18) . ? C38 H38 0.9500 . ? C39 C40 1.384(19) . ? C39 H39 0.9500 . ? C40 C41 1.402(18) . ? C40 H40 0.9500 . ? C41 C42 1.370(16) . ? C41 H41 0.9500 . ? C42 H42 0.9500 . ? C43 C44 1.378(13) . ? C43 C48 1.400(13) . ? C44 C45 1.430(13) . ? C44 H44 0.9500 . ? C45 C46 1.385(15) . ? C45 H45 0.9500 . ? C46 C47 1.342(14) . ? C46 H46 0.9500 . ? C47 C48 1.379(13) . ? C47 H47 0.9500 . ? C48 H48 0.9500 . ? C49 C50 1.426(17) . ? C49 C54 1.425(16) . ? C50 C51 1.478(19) . ? C50 H50 0.9500 . ? C51 C52 1.382(19) . ? C51 H51 0.9500 . ? C52 C53 1.374(19) . ? C52 H52 0.9500 . ? C53 C54 1.358(17) . ? C53 H53 0.9500 . ? C54 H54 0.9500 . ? C55 C60 1.398(14) . ? C55 C56 1.409(12) . ? C56 C57 1.384(15) . ? C56 H56 0.9500 . ? C57 C58 1.386(15) . ? C57 H57 0.9500 . ? C58 C59 1.363(14) . ? C58 H58 0.9500 . ? C59 C60 1.360(14) . ? C59 H59 0.9500 . ? C60 H60 0.9500 . ? Cl1 C1S 1.650(15) . ? Cl2 C1S 1.520(16) . ? C1S H1S1 0.9900 . ? C1S H1S2 0.9900 . ? O2S C2S 1.49(3) . ? O2S O6S 1.73(3) . ? C2S O4S 1.31(5) . ? C2S O3S 1.64(6) . ? O3S C3S 1.17(4) . ? O3S O4S 1.37(8) . ? 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 N21 Ni1 N24 90.7(3) . . ? N21 Ni1 N23 157.0(3) . . ? N24 Ni1 N23 90.0(4) . . ? N21 Ni1 N22 91.5(4) . . ? N24 Ni1 N22 158.6(3) . . ? N23 Ni1 N22 96.1(4) . . ? C1 N21 C4 106.5(9) . . ? C1 N21 Ni1 125.5(9) . . ? C4 N21 Ni1 128.0(6) . . ? C6 N22 C9 109.1(7) . . ? C6 N22 Ni1 124.6(6) . . ? C9 N22 Ni1 122.5(7) . . ? C11 N23 C14 108.0(8) . . ? C11 N23 Ni1 125.2(7) . . ? C14 N23 Ni1 120.7(6) . . ? C19 N24 C16 108.2(8) . . ? C19 N24 Ni1 123.9(8) . . ? C16 N24 Ni1 127.3(6) . . ? O1 C1 N21 122.6(11) . . ? O1 C1 C2 128.9(10) . . ? N21 C1 C2 108.5(11) . . ? C3 C2 C1 109.4(10) . . ? C3 C2 C21 126.5(11) . . ? C1 C2 C21 124.0(12) . . ? C2 C3 C24 123.2(10) . . ? C2 C3 C4 105.7(10) . . ? C24 C3 C4 131.1(10) . . ? N21 C4 C5 122.2(8) . . ? N21 C4 C3 109.6(8) . . ? C5 C4 C3 128.2(11) . . ? C4 C5 C6 121.6(10) . . ? C4 C5 C37 117.4(8) . . ? C6 C5 C37 121.1(8) . . ? N22 C6 C5 123.9(8) . . ? N22 C6 C7 108.9(8) . . ? C5 C6 C7 127.1(10) . . ? C8 C7 C6 107.8(9) . . ? C8 C7 C25 123.1(8) . . ? C6 C7 C25 129.1(8) . . ? C7 C8 C9 107.3(8) . . ? C7 C8 C28 124.2(9) . . ? C9 C8 C28 128.3(9) . . ? C10 C9 N22 123.9(9) . . ? C10 C9 C8 129.1(8) . . ? N22 C9 C8 107.0(8) . . ? C9 C10 C11 123.1(8) . . ? C9 C10 C43 120.0(9) . . ? C11 C10 C43 116.9(9) . . ? N23 C11 C12 110.6(9) . . ? N23 C11 C10 121.1(9) . . ? C12 C11 C10 128.2(9) . . ? C13 C12 C11 105.8(8) . . ? C13 C12 C29 124.1(10) . . ? C11 C12 C29 129.5(10) . . ? C12 C13 C14 108.3(10) . . ? C12 C13 C32 121.3(9) . . ? C14 C13 C32 130.3(10) . . ? C15 C14 N23 123.2(9) . . ? C15 C14 C13 129.3(10) . . ? N23 C14 C13 107.3(8) . . ? C14 C15 C16 123.7(10) . . ? C14 C15 C49 119.2(9) . . ? C16 C15 C49 116.8(9) . . ? N24 C16 C15 119.9(9) . . ? N24 C16 C17 108.7(9) . . ? C15 C16 C17 130.9(11) . . ? C18 C17 C16 105.4(9) . . ? C18 C17 C33 123.2(9) . . ? C16 C17 C33 130.8(11) . . ? C17 C18 C19 107.1(8) . . ? C17 C18 C36 123.2(9) . . ? C19 C18 C36 129.2(10) . . ? N24 C19 C18 110.5(10) . . ? N24 C19 C20 117.8(8) . . ? C18 C19 C20 130.9(9) . . ? O2 C20 C19 119.7(8) . . ? O2 C20 C55 118.3(9) . . ? C19 C20 C55 122.1(8) . . ? C22 C21 C2 111.6(11) . . ? C22 C21 H21A 109.3 . . ? C2 C21 H21A 109.3 . . ? C22 C21 H21B 109.3 . . ? C2 C21 H21B 109.3 . . ? H21A C21 H21B 108.0 . . ? C21 C22 C23 109.0(10) . . ? C21 C22 H22A 109.9 . . ? C23 C22 H22A 109.9 . . ? C21 C22 H22B 109.9 . . ? C23 C22 H22B 109.9 . . ? H22A C22 H22B 108.3 . . ? C22 C23 C24 114.7(11) . . ? C22 C23 H23A 108.6 . . ? C24 C23 H23A 108.6 . . ? C22 C23 H23B 108.6 . . ? C24 C23 H23B 108.6 . . ? H23A C23 H23B 107.6 . . ? C3 C24 C23 107.7(10) . . ? C3 C24 H24A 110.2 . . ? C23 C24 H24A 110.2 . . ? C3 C24 H24B 110.2 . . ? C23 C24 H24B 110.2 . . ? H24A C24 H24B 108.5 . . ? C26 C25 C7 111.2(8) . . ? C26 C25 H25A 109.4 . . ? C7 C25 H25A 109.4 . . ? C26 C25 H25B 109.4 . . ? C7 C25 H25B 109.4 . . ? H25A C25 H25B 108.0 . . ? C27 C26 C25 111.6(9) . . ? C27 C26 H26A 109.3 . . ? C25 C26 H26A 109.3 . . ? C27 C26 H26B 109.3 . . ? C25 C26 H26B 109.3 . . ? H26A C26 H26B 108.0 . . ? C26 C27 C28 112.1(9) . . ? C26 C27 H27A 109.2 . . ? C28 C27 H27A 109.2 . . ? C26 C27 H27B 109.2 . . ? C28 C27 H27B 109.2 . . ? H27A C27 H27B 107.9 . . ? C8 C28 C27 109.5(8) . . ? C8 C28 H28A 109.8 . . ? C27 C28 H28A 109.8 . . ? C8 C28 H28B 109.8 . . ? C27 C28 H28B 109.8 . . ? H28A C28 H28B 108.2 . . ? C30 C29 C12 109.8(9) . . ? C30 C29 H29A 109.7 . . ? C12 C29 H29A 109.7 . . ? C30 C29 H29B 109.7 . . ? C12 C29 H29B 109.7 . . ? H29A C29 H29B 108.2 . . ? C29 C30 C31 113.8(10) . . ? C29 C30 H30A 108.8 . . ? C31 C30 H30A 108.8 . . ? C29 C30 H30B 108.8 . . ? C31 C30 H30B 108.8 . . ? H30A C30 H30B 107.7 . . ? C30 C31 C32 111.1(10) . . ? C30 C31 H31A 109.4 . . ? C32 C31 H31A 109.4 . . ? C30 C31 H31B 109.4 . . ? C32 C31 H31B 109.4 . . ? H31A C31 H31B 108.0 . . ? C13 C32 C31 110.4(10) . . ? C13 C32 H32A 109.6 . . ? C31 C32 H32A 109.6 . . ? C13 C32 H32B 109.6 . . ? C31 C32 H32B 109.6 . . ? H32A C32 H32B 108.1 . . ? C17 C33 C34 111.0(11) . . ? C17 C33 H33A 109.4 . . ? C34 C33 H33A 109.4 . . ? C17 C33 H33B 109.5 . . ? C34 C33 H33B 109.4 . . ? H33A C33 H33B 108.0 . . ? C35 C34 C33 114.4(11) . . ? C35 C34 H34A 108.7 . . ? C33 C34 H34A 108.6 . . ? C35 C34 H34B 108.6 . . ? C33 C34 H34B 108.7 . . ? H34A C34 H34B 107.6 . . ? C34 C35 C36 115.3(10) . . ? C34 C35 H35A 108.5 . . ? C36 C35 H35A 108.5 . . ? C34 C35 H35B 108.4 . . ? C36 C35 H35B 108.4 . . ? H35A C35 H35B 107.5 . . ? C35 C36 C18 110.6(10) . . ? C35 C36 H36A 109.5 . . ? C18 C36 H36A 109.5 . . ? C35 C36 H36B 109.5 . . ? C18 C36 H36B 109.5 . . ? H36A C36 H36B 108.1 . . ? C38 C37 C42 120.1(11) . . ? C38 C37 C5 119.4(9) . . ? C42 C37 C5 120.6(9) . . ? C37 C38 C39 118.8(11) . . ? C37 C38 H38 120.6 . . ? C39 C38 H38 120.6 . . ? C40 C39 C38 121.6(12) . . ? C40 C39 H39 119.2 . . ? C38 C39 H39 119.2 . . ? C39 C40 C41 118.2(14) . . ? C39 C40 H40 120.9 . . ? C41 C40 H40 120.9 . . ? C42 C41 C40 120.1(12) . . ? C42 C41 H41 119.9 . . ? C40 C41 H41 120.0 . . ? C41 C42 C37 121.1(10) . . ? C41 C42 H42 119.4 . . ? C37 C42 H42 119.4 . . ? C44 C43 C48 118.6(8) . . ? C44 C43 C10 122.2(9) . . ? C48 C43 C10 119.2(8) . . ? C43 C44 C45 119.0(9) . . ? C43 C44 H44 120.5 . . ? C45 C44 H44 120.5 . . ? C46 C45 C44 120.4(9) . . ? C46 C45 H45 119.8 . . ? C44 C45 H45 119.8 . . ? C47 C46 C45 119.6(9) . . ? C47 C46 H46 120.2 . . ? C45 C46 H46 120.2 . . ? C46 C47 C48 121.2(9) . . ? C46 C47 H47 119.4 . . ? C48 C47 H47 119.4 . . ? C47 C48 C43 121.2(9) . . ? C47 C48 H48 119.4 . . ? C43 C48 H48 119.4 . . ? C50 C49 C54 119.9(12) . . ? C50 C49 C15 121.6(11) . . ? C54 C49 C15 118.4(11) . . ? C49 C50 C51 117.2(13) . . ? C49 C50 H50 121.4 . . ? C51 C50 H50 121.4 . . ? C52 C51 C50 118.5(14) . . ? C52 C51 H51 120.8 . . ? C50 C51 H51 120.7 . . ? C53 C52 C51 122.8(14) . . ? C53 C52 H52 118.6 . . ? C51 C52 H52 118.6 . . ? C54 C53 C52 120.5(14) . . ? C54 C53 H53 119.8 . . ? C52 C53 H53 119.8 . . ? C53 C54 C49 121.0(13) . . ? C53 C54 H54 119.5 . . ? C49 C54 H54 119.5 . . ? C60 C55 C56 119.7(10) . . ? C60 C55 C20 119.0(8) . . ? C56 C55 C20 120.9(10) . . ? C57 C56 C55 118.4(11) . . ? C57 C56 H56 120.8 . . ? C55 C56 H56 120.8 . . ? C56 C57 C58 120.6(10) . . ? C56 C57 H57 119.7 . . ? C58 C57 H57 119.7 . . ? C59 C58 C57 120.3(10) . . ? C59 C58 H58 119.9 . . ? C57 C58 H58 119.9 . . ? C60 C59 C58 120.8(12) . . ? C60 C59 H59 119.6 . . ? C58 C59 H59 119.6 . . ? C59 C60 C55 120.2(10) . . ? C59 C60 H60 119.9 . . ? C55 C60 H60 119.9 . . ? Cl2 C1S Cl1 130.5(14) . . ? Cl2 C1S H1S1 104.6 . . ? Cl1 C1S H1S1 104.6 . . ? Cl2 C1S H1S2 104.6 . . ? Cl1 C1S H1S2 104.6 . . ? H1S1 C1S H1S2 105.7 . . ? C2S O2S O6S 154.7(17) . . ? O4S C2S O2S 148(3) . . ? O4S C2S O3S 54(3) . . ? O2S C2S O3S 104.7(19) . . ? C3S O3S O4S 122(6) . . ? C3S O3S C2S 132(5) . . ? O4S O3S C2S 50(3) . . ? C2S O4S O3S 76(4) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N24 Ni1 N21 C1 -46.6(7) . . . . ? N23 Ni1 N21 C1 45.2(12) . . . . ? N22 Ni1 N21 C1 154.7(7) . . . . ? N24 Ni1 N21 C4 135.1(7) . . . . ? N23 Ni1 N21 C4 -133.1(9) . . . . ? N22 Ni1 N21 C4 -23.5(7) . . . . ? N21 Ni1 N22 C6 31.6(7) . . . . ? N24 Ni1 N22 C6 -64.2(12) . . . . ? N23 Ni1 N22 C6 -170.1(6) . . . . ? N21 Ni1 N22 C9 -172.8(7) . . . . ? N24 Ni1 N22 C9 91.4(12) . . . . ? N23 Ni1 N22 C9 -14.6(7) . . . . ? N21 Ni1 N23 C11 97.9(11) . . . . ? N24 Ni1 N23 C11 -170.2(8) . . . . ? N22 Ni1 N23 C11 -10.8(8) . . . . ? N21 Ni1 N23 C14 -51.2(12) . . . . ? N24 Ni1 N23 C14 40.7(7) . . . . ? N22 Ni1 N23 C14 -159.9(7) . . . . ? N21 Ni1 N24 C19 -47.7(7) . . . . ? N23 Ni1 N24 C19 155.2(7) . . . . ? N22 Ni1 N24 C19 48.2(13) . . . . ? N21 Ni1 N24 C16 121.9(8) . . . . ? N23 Ni1 N24 C16 -35.1(8) . . . . ? N22 Ni1 N24 C16 -142.1(9) . . . . ? C4 N21 C1 O1 171.8(8) . . . . ? Ni1 N21 C1 O1 -6.7(12) . . . . ? C4 N21 C1 C2 -5.7(9) . . . . ? Ni1 N21 C1 C2 175.8(6) . . . . ? O1 C1 C2 C3 -174.5(9) . . . . ? N21 C1 C2 C3 2.8(10) . . . . ? O1 C1 C2 C21 3.1(15) . . . . ? N21 C1 C2 C21 -179.6(8) . . . . ? C1 C2 C3 C24 179.8(8) . . . . ? C21 C2 C3 C24 2.4(14) . . . . ? C1 C2 C3 C4 1.1(9) . . . . ? C21 C2 C3 C4 -176.4(8) . . . . ? C1 N21 C4 C5 -170.1(7) . . . . ? Ni1 N21 C4 C5 8.4(11) . . . . ? C1 N21 C4 C3 6.4(9) . . . . ? Ni1 N21 C4 C3 -175.1(5) . . . . ? C2 C3 C4 N21 -4.7(9) . . . . ? C24 C3 C4 N21 176.7(9) . . . . ? C2 C3 C4 C5 171.5(8) . . . . ? C24 C3 C4 C5 -7.1(14) . . . . ? N21 C4 C5 C6 8.4(12) . . . . ? C3 C4 C5 C6 -167.4(8) . . . . ? N21 C4 C5 C37 -171.4(7) . . . . ? C3 C4 C5 C37 12.8(12) . . . . ? C9 N22 C6 C5 176.0(7) . . . . ? Ni1 N22 C6 C5 -25.7(10) . . . . ? C9 N22 C6 C7 0.5(8) . . . . ? Ni1 N22 C6 C7 158.9(5) . . . . ? C4 C5 C6 N22 0.8(12) . . . . ? C37 C5 C6 N22 -179.4(7) . . . . ? C4 C5 C6 C7 175.5(8) . . . . ? C37 C5 C6 C7 -4.8(12) . . . . ? N22 C6 C7 C8 -1.6(9) . . . . ? C5 C6 C7 C8 -176.9(7) . . . . ? N22 C6 C7 C25 -179.6(7) . . . . ? C5 C6 C7 C25 5.1(13) . . . . ? C6 C7 C8 C9 2.0(9) . . . . ? C25 C7 C8 C9 -179.9(7) . . . . ? C6 C7 C8 C28 -172.3(7) . . . . ? C25 C7 C8 C28 5.9(12) . . . . ? C6 N22 C9 C10 -177.6(7) . . . . ? Ni1 N22 C9 C10 23.5(11) . . . . ? C6 N22 C9 C8 0.7(8) . . . . ? Ni1 N22 C9 C8 -158.2(5) . . . . ? C7 C8 C9 C10 176.4(8) . . . . ? C28 C8 C9 C10 -9.6(14) . . . . ? C7 C8 C9 N22 -1.7(9) . . . . ? C28 C8 C9 N22 172.2(7) . . . . ? N22 C9 C10 C11 -5.0(13) . . . . ? C8 C9 C10 C11 177.1(8) . . . . ? N22 C9 C10 C43 174.5(7) . . . . ? C8 C9 C10 C43 -3.4(13) . . . . ? C14 N23 C11 C12 -0.4(10) . . . . ? Ni1 N23 C11 C12 -152.7(6) . . . . ? C14 N23 C11 C10 -178.2(8) . . . . ? Ni1 N23 C11 C10 29.4(11) . . . . ? C9 C10 C11 N23 -22.8(13) . . . . ? C43 C10 C11 N23 157.6(8) . . . . ? C9 C10 C11 C12 159.8(9) . . . . ? C43 C10 C11 C12 -19.8(13) . . . . ? N23 C11 C12 C13 2.4(10) . . . . ? C10 C11 C12 C13 180.0(9) . . . . ? N23 C11 C12 C29 172.9(9) . . . . ? C10 C11 C12 C29 -9.4(15) . . . . ? C11 C12 C13 C14 -3.3(10) . . . . ? C29 C12 C13 C14 -174.6(9) . . . . ? C11 C12 C13 C32 173.3(9) . . . . ? C29 C12 C13 C32 2.1(15) . . . . ? C11 N23 C14 C15 173.8(9) . . . . ? Ni1 N23 C14 C15 -32.3(12) . . . . ? C11 N23 C14 C13 -1.7(10) . . . . ? Ni1 N23 C14 C13 152.1(6) . . . . ? C12 C13 C14 C15 -172.0(10) . . . . ? C32 C13 C14 C15 11.8(18) . . . . ? C12 C13 C14 N23 3.2(11) . . . . ? C32 C13 C14 N23 -173.0(10) . . . . ? N23 C14 C15 C16 1.6(16) . . . . ? C13 C14 C15 C16 176.0(10) . . . . ? N23 C14 C15 C49 -172.7(9) . . . . ? C13 C14 C15 C49 1.8(17) . . . . ? C19 N24 C16 C15 -172.4(9) . . . . ? Ni1 N24 C16 C15 16.6(13) . . . . ? C19 N24 C16 C17 0.3(10) . . . . ? Ni1 N24 C16 C17 -170.7(6) . . . . ? C14 C15 C16 N24 7.3(15) . . . . ? C49 C15 C16 N24 -178.3(9) . . . . ? C14 C15 C16 C17 -163.6(10) . . . . ? C49 C15 C16 C17 10.8(16) . . . . ? N24 C16 C17 C18 -0.7(11) . . . . ? C15 C16 C17 C18 171.0(10) . . . . ? N24 C16 C17 C33 -172.3(10) . . . . ? C15 C16 C17 C33 -0.7(18) . . . . ? C16 C17 C18 C19 0.8(11) . . . . ? C33 C17 C18 C19 173.2(9) . . . . ? C16 C17 C18 C36 -172.2(9) . . . . ? C33 C17 C18 C36 0.3(16) . . . . ? C16 N24 C19 C18 0.2(10) . . . . ? Ni1 N24 C19 C18 171.6(6) . . . . ? C16 N24 C19 C20 171.2(8) . . . . ? Ni1 N24 C19 C20 -17.4(11) . . . . ? C17 C18 C19 N24 -0.7(11) . . . . ? C36 C18 C19 N24 171.8(9) . . . . ? C17 C18 C19 C20 -170.1(9) . . . . ? C36 C18 C19 C20 2.3(17) . . . . ? N24 C19 C20 O2 -34.9(12) . . . . ? C18 C19 C20 O2 133.9(10) . . . . ? N24 C19 C20 C55 145.9(8) . . . . ? C18 C19 C20 C55 -45.3(14) . . . . ? C3 C2 C21 C22 15.4(15) . . . . ? C1 C2 C21 C22 -161.7(10) . . . . ? C2 C21 C22 C23 -44.4(13) . . . . ? C21 C22 C23 C24 62.2(12) . . . . ? C2 C3 C24 C23 11.4(13) . . . . ? C4 C3 C24 C23 -170.1(9) . . . . ? C22 C23 C24 C3 -43.2(12) . . . . ? C8 C7 C25 C26 9.7(11) . . . . ? C6 C7 C25 C26 -172.6(8) . . . . ? C7 C25 C26 C27 -43.1(12) . . . . ? C25 C26 C27 C28 63.4(12) . . . . ? C7 C8 C28 C27 12.0(11) . . . . ? C9 C8 C28 C27 -161.0(8) . . . . ? C26 C27 C28 C8 -45.6(11) . . . . ? C13 C12 C29 C30 -10.3(14) . . . . ? C11 C12 C29 C30 -179.3(9) . . . . ? C12 C29 C30 C31 40.3(12) . . . . ? C29 C30 C31 C32 -63.9(14) . . . . ? C12 C13 C32 C31 -22.4(14) . . . . ? C14 C13 C32 C31 153.4(11) . . . . ? C30 C31 C32 C13 51.7(14) . . . . ? C18 C17 C33 C34 12.1(16) . . . . ? C16 C17 C33 C34 -177.5(11) . . . . ? C17 C33 C34 C35 -39.7(17) . . . . ? C33 C34 C35 C36 57.3(18) . . . . ? C34 C35 C36 C18 -41.6(15) . . . . ? C17 C18 C36 C35 13.5(14) . . . . ? C19 C18 C36 C35 -157.9(10) . . . . ? C4 C5 C37 C38 86.2(11) . . . . ? C6 C5 C37 C38 -93.5(11) . . . . ? C4 C5 C37 C42 -93.8(10) . . . . ? C6 C5 C37 C42 86.4(11) . . . . ? C42 C37 C38 C39 2.6(18) . . . . ? C5 C37 C38 C39 -177.5(12) . . . . ? C37 C38 C39 C40 -1(2) . . . . ? C38 C39 C40 C41 -2(3) . . . . ? C39 C40 C41 C42 3(2) . . . . ? C40 C41 C42 C37 -2.3(17) . . . . ? C38 C37 C42 C41 -0.8(15) . . . . ? C5 C37 C42 C41 179.2(9) . . . . ? C9 C10 C43 C44 -74.9(13) . . . . ? C11 C10 C43 C44 104.7(12) . . . . ? C9 C10 C43 C48 107.8(11) . . . . ? C11 C10 C43 C48 -72.7(12) . . . . ? C48 C43 C44 C45 1.4(16) . . . . ? C10 C43 C44 C45 -176.0(10) . . . . ? C43 C44 C45 C46 0.3(18) . . . . ? C44 C45 C46 C47 -2.7(19) . . . . ? C45 C46 C47 C48 3.3(18) . . . . ? C46 C47 C48 C43 -1.6(17) . . . . ? C44 C43 C48 C47 -0.8(16) . . . . ? C10 C43 C48 C47 176.7(10) . . . . ? C14 C15 C49 C50 78.4(13) . . . . ? C16 C15 C49 C50 -96.3(13) . . . . ? C14 C15 C49 C54 -104.8(12) . . . . ? C16 C15 C49 C54 80.6(12) . . . . ? C54 C49 C50 C51 1.0(16) . . . . ? C15 C49 C50 C51 177.8(9) . . . . ? C49 C50 C51 C52 1.4(17) . . . . ? C50 C51 C52 C53 -3(2) . . . . ? C51 C52 C53 C54 3(2) . . . . ? C52 C53 C54 C49 0.0(17) . . . . ? C50 C49 C54 C53 -1.7(16) . . . . ? C15 C49 C54 C53 -178.6(10) . . . . ? O2 C20 C55 C60 -10.6(12) . . . . ? C19 C20 C55 C60 168.5(8) . . . . ? O2 C20 C55 C56 162.2(8) . . . . ? C19 C20 C55 C56 -18.6(12) . . . . ? C60 C55 C56 C57 -1.5(13) . . . . ? C20 C55 C56 C57 -174.3(8) . . . . ? C55 C56 C57 C58 2.1(13) . . . . ? C56 C57 C58 C59 -2.1(14) . . . . ? C57 C58 C59 C60 1.4(14) . . . . ? C58 C59 C60 C55 -0.9(14) . . . . ? C56 C55 C60 C59 0.9(13) . . . . ? C20 C55 C60 C59 173.8(8) . . . . ? O6S O2S C2S O4S -173(5) . . . . ? O6S O2S C2S O3S 144(4) . . . . ? O4S C2S O3S C3S -101(8) . . . . ? O2S C2S O3S C3S 52(7) . . . . ? O2S C2S O3S O4S 153(3) . . . . ? O2S C2S O4S O3S -55(5) . . . . ? C3S O3S O4S C2S 120(4) . . . . ? _diffrn_measured_fraction_theta_max 0.89 _diffrn_reflns_theta_full 23.3 _diffrn_measured_fraction_theta_full 0.89 _refine_diff_density_max 1.10 _refine_diff_density_min -0.58 _refine_diff_density_rms 0.131 # END OF CIF for Compound4 data_Compound7 _database_code_CSD 211040 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_compound_source 'local laboratory' _chemical_formula_moiety 'C60 H49 N5 Ni O2, 0.5(H2 O)' _chemical_formula_sum 'C60 H50 N5 Ni O2.50' _chemical_formula_weight 939.76 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' Ni Ni 0.3393 1.1124 '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_space_group_name_H-M 'P 21/c ' _symmetry_cell_setting Monoclinic 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 16.369(7) _cell_length_b 23.960(9) _cell_length_c 13.461(5) _cell_angle_alpha 90 _cell_angle_beta 101.39(2) _cell_angle_gamma 90 _cell_volume 5176(4) _cell_formula_units_Z 4 _cell_measurement_temperature 100 _cell_measurement_reflns_used 6203 _cell_measurement_theta_min 2.5 _cell_measurement_theta_max 22.7 _exptl_crystal_description lath _exptl_crystal_colour green _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.206 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1972 _exptl_absorpt_coefficient_mu 0.423 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.454 _exptl_absorpt_correction_T_max 0.987 _exptl_absorpt_process_details 'HKL Scalepack (Otwinowski & Minor 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'KappaCCD (with Oxford Cryostream)' _diffrn_measurement_method ' \w scans with \k offsets' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% <2 _diffrn_reflns_number 25395 _diffrn_reflns_av_R_equivalents 0.055 _diffrn_reflns_av_sigmaI/netI 0.089 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.6 _diffrn_reflns_theta_max 22.7 _reflns_number_total 6891 _reflns_number_gt 4106 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'COLLECT (Nonius 1999)' _computing_data_reduction 'Denzo and Scalepak (Otwinowski & Minor, 1997)' _computing_cell_refinement 'Denzo and Scalepak (Otwinowski & Minor, 1997)' _computing_structure_solution 'Direct_methods (SIR, Altomare, et al., 1994)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-3 for Windows (Farrugia, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.1855P)^2^+14.0865P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6891 _refine_ls_number_parameters 594 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.172 _refine_ls_R_factor_gt 0.112 _refine_ls_wR_factor_ref 0.341 _refine_ls_wR_factor_gt 0.297 _refine_ls_goodness_of_fit_ref 1.033 _refine_ls_restrained_S_all 1.170 _refine_ls_shift/su_max 0.066 _refine_ls_shift/su_mean 0.005 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 0.20403(9) 0.17740(6) 0.30382(10) 0.0597(6) Uani 1 1 d . . . N21 N 0.2405(6) 0.1020(4) 0.2934(7) 0.066(2) Uani 1 1 d . . . N22 N 0.1084(5) 0.1506(4) 0.3520(6) 0.056(2) Uani 1 1 d . . . N23 N 0.1800(5) 0.2524(4) 0.3353(7) 0.061(2) Uani 1 1 d . . . N24 N 0.2877(6) 0.2030(4) 0.2335(7) 0.067(3) Uani 1 1 d . . . C1 C 0.3220(8) 0.0874(5) 0.2894(9) 0.070(3) Uani 1 1 d . . . C2 C 0.3330(8) 0.0294(6) 0.3196(10) 0.081(4) Uani 1 1 d . . . C3 C 0.2580(9) 0.0086(5) 0.3262(9) 0.076(4) Uani 1 1 d . . . C4 C 0.1968(8) 0.0541(5) 0.3087(8) 0.064(3) Uani 1 1 d . . . C5 C 0.1126(8) 0.0534(5) 0.3099(9) 0.067(3) Uani 1 1 d . . . C6 C 0.0701(7) 0.1008(5) 0.3268(8) 0.061(3) Uani 1 1 d . . . C7 C -0.0153(7) 0.1030(5) 0.3419(9) 0.067(3) Uani 1 1 d . . . C8 C -0.0227(7) 0.1521(5) 0.3882(8) 0.063(3) Uani 1 1 d . . . C9 C 0.0536(7) 0.1818(5) 0.3952(8) 0.058(3) Uani 1 1 d . . . C10 C 0.0734(7) 0.2349(5) 0.4362(8) 0.066(3) Uani 1 1 d . . . C11 C 0.1380(7) 0.2679(5) 0.4116(8) 0.064(3) Uani 1 1 d . . . C12 C 0.1564(8) 0.3254(5) 0.4412(9) 0.069(3) Uani 1 1 d . . . C13 C 0.2000(7) 0.3471(5) 0.3736(9) 0.070(3) Uani 1 1 d . . . C14 C 0.2138(7) 0.3013(5) 0.3076(9) 0.065(3) Uani 1 1 d . . . C15 C 0.2544(7) 0.3043(5) 0.2284(9) 0.071(3) Uani 1 1 d . . . C16 C 0.2875(7) 0.2566(6) 0.1893(8) 0.072(4) Uani 1 1 d . . . C17 C 0.3415(8) 0.2535(6) 0.1143(9) 0.073(3) Uani 1 1 d . . . C18 C 0.3800(8) 0.2024(6) 0.1234(9) 0.078(4) Uani 1 1 d . . . C19 C 0.3461(8) 0.1720(6) 0.2018(9) 0.071(3) Uani 1 1 d . . . C20 C 0.3713(7) 0.1201(6) 0.2394(10) 0.075(3) Uani 1 1 d . . . C21 C 0.4132(9) -0.0049(7) 0.3476(13) 0.107(5) Uani 1 1 d . . . H21A H 0.4320 -0.0158 0.2847 0.129 Uiso 1 1 calc R . . H21B H 0.4573 0.0186 0.3881 0.129 Uiso 1 1 calc R . . C22 C 0.4025(12) -0.0551(7) 0.4051(14) 0.113(5) Uani 1 1 d . . . H22A H 0.4043 -0.0446 0.4766 0.135 Uiso 1 1 calc R . . H22B H 0.4499 -0.0806 0.4037 0.135 Uiso 1 1 calc R . . C23 C 0.3243(13) -0.0854(8) 0.3671(15) 0.133(6) Uani 1 1 d . . . H23A H 0.3207 -0.1171 0.4132 0.160 Uiso 1 1 calc R . . H23B H 0.3269 -0.1012 0.2998 0.160 Uiso 1 1 calc R . . C24 C 0.2452(9) -0.0510(5) 0.3571(11) 0.089(4) Uani 1 1 d . . . H24A H 0.2008 -0.0684 0.3059 0.106 Uiso 1 1 calc R . . H24B H 0.2265 -0.0510 0.4227 0.106 Uiso 1 1 calc R . . C25 C -0.0858(8) 0.0622(5) 0.3089(10) 0.080(4) Uani 1 1 d . . . H25A H -0.0839 0.0483 0.2401 0.096 Uiso 1 1 calc R . . H25B H -0.0784 0.0299 0.3555 0.096 Uiso 1 1 calc R . . C26 C -0.1685(9) 0.0885(6) 0.3081(12) 0.093(4) Uani 1 1 d . . . H26A H -0.2115 0.0590 0.3037 0.112 Uiso 1 1 calc R . . H26B H -0.1837 0.1128 0.2478 0.112 Uiso 1 1 calc R . . C27 C -0.1666(8) 0.1227(6) 0.4031(11) 0.088(4) Uani 1 1 d . . . H27A H -0.2229 0.1382 0.4013 0.105 Uiso 1 1 calc R . . H27B H -0.1533 0.0976 0.4626 0.105 Uiso 1 1 calc R . . C28 C -0.1054(8) 0.1696(5) 0.4173(10) 0.078(4) Uani 1 1 d . . . H28A H -0.0947 0.1817 0.4890 0.093 Uiso 1 1 calc R . . H28B H -0.1293 0.2016 0.3749 0.093 Uiso 1 1 calc R . . C29 C 0.1399(8) 0.3570(5) 0.5291(9) 0.075(3) Uiso 1 1 d . . . C30A C 0.1648(16) 0.4089(11) 0.540(2) 0.092(3) Uiso 0.603(11) 1 d P . . C30B C 0.205(2) 0.4117(17) 0.540(3) 0.092(3) Uiso 0.397(11) 1 d P . . C31A C 0.2035(16) 0.4295(6) 0.470(2) 0.092(3) Uiso 0.603(11) 1 d PD . . C31B C 0.193(3) 0.4446(16) 0.436(3) 0.092(3) Uiso 0.397(11) 1 d P . . C32 C 0.2303(9) 0.4048(5) 0.3768(11) 0.091(4) Uani 1 1 d . . . C33 C 0.3525(9) 0.2972(6) 0.0369(10) 0.091(4) Uani 1 1 d . . . C34A C 0.404(3) 0.2622(18) -0.042(3) 0.092(3) Uiso 0.397(11) 1 d P . . C34B C 0.4170(17) 0.2841(11) -0.017(2) 0.092(3) Uiso 0.603(11) 1 d P . . C35A C 0.4130(15) 0.2237(14) -0.050(2) 0.092(3) Uiso 0.397(11) 1 d PD . . C35B C 0.4498(16) 0.2252(11) -0.0145(19) 0.092(3) Uiso 0.603(11) 1 d P . . C36 C 0.4366(9) 0.1832(7) 0.0585(11) 0.100(5) Uani 1 1 d . . . C37 C 0.0704(7) -0.0026(5) 0.2969(9) 0.070(3) Uani 1 1 d . . . C38 C 0.0538(8) -0.0269(6) 0.2013(10) 0.083(4) Uani 1 1 d . . . H38 H 0.0691 -0.0082 0.1455 0.099 Uiso 1 1 calc R . . C39 C 0.0144(9) -0.0792(5) 0.1873(11) 0.089(4) Uani 1 1 d . . . H39 H 0.0022 -0.0959 0.1220 0.107 Uiso 1 1 calc R . . C40 C -0.0061(9) -0.1056(5) 0.2685(12) 0.094(4) Uani 1 1 d . . . H40 H -0.0322 -0.1411 0.2592 0.112 Uiso 1 1 calc R . . C41 C 0.0098(8) -0.0824(5) 0.3633(11) 0.085(4) Uani 1 1 d . . . H41 H -0.0050 -0.1018 0.4187 0.102 Uiso 1 1 calc R . . C42 C 0.0473(8) -0.0311(5) 0.3778(9) 0.077(3) Uani 1 1 d . . . H42 H 0.0577 -0.0147 0.4433 0.092 Uiso 1 1 calc R . . C43 C 0.0191(8) 0.2606(5) 0.5013(9) 0.069(3) Uani 1 1 d . . . C44 C 0.0285(8) 0.2472(5) 0.6020(9) 0.070(3) Uani 1 1 d . . . H44 H 0.0719 0.2225 0.6319 0.084 Uiso 1 1 calc R . . C45 C -0.0238(9) 0.2687(6) 0.6600(10) 0.085(4) Uani 1 1 d . . . H45 H -0.0169 0.2586 0.7294 0.101 Uiso 1 1 calc R . . C46 C -0.0865(9) 0.3050(6) 0.6180(12) 0.091(4) Uani 1 1 d . . . H46 H -0.1228 0.3197 0.6585 0.110 Uiso 1 1 calc R . . C47 C -0.0967(9) 0.3202(6) 0.5156(12) 0.094(4) Uani 1 1 d . . . H47 H -0.1398 0.3453 0.4864 0.113 Uiso 1 1 calc R . . C48 C -0.0439(8) 0.2984(5) 0.4583(10) 0.077(3) Uani 1 1 d . . . H48 H -0.0498 0.3089 0.3891 0.093 Uiso 1 1 calc R . . C49 C 0.2733(8) 0.3587(5) 0.1851(10) 0.073(3) Uani 1 1 d . . . C50 C 0.3506(9) 0.3832(6) 0.2172(13) 0.102(5) Uani 1 1 d . . . H50 H 0.3921 0.3649 0.2655 0.122 Uiso 1 1 calc R . . C51 C 0.3671(11) 0.4351(7) 0.1781(16) 0.124(6) Uani 1 1 d . . . H51 H 0.4206 0.4515 0.1986 0.149 Uiso 1 1 calc R . . C52 C 0.3064(12) 0.4626(7) 0.1099(15) 0.114(5) Uani 1 1 d . . . H52 H 0.3178 0.4980 0.0838 0.137 Uiso 1 1 calc R . . C53 C 0.2294(11) 0.4385(6) 0.0800(11) 0.099(5) Uani 1 1 d . . . H53 H 0.1870 0.4577 0.0344 0.119 Uiso 1 1 calc R . . C54 C 0.2129(9) 0.3860(5) 0.1162(10) 0.078(4) Uani 1 1 d . . . H54 H 0.1601 0.3691 0.0934 0.093 Uiso 1 1 calc R . . C55 C 0.4521(9) 0.0972(7) 0.2218(11) 0.089(4) Uani 1 1 d . . . C56 C 0.5278(10) 0.1194(7) 0.2735(13) 0.112(5) Uani 1 1 d . . . H56 H 0.5275 0.1458 0.3260 0.134 Uiso 1 1 calc R . . C57 C 0.6023(11) 0.1038(11) 0.2499(18) 0.162(9) Uani 1 1 d . . . H57 H 0.6526 0.1221 0.2797 0.194 Uiso 1 1 calc R . . C58 C 0.6024(14) 0.0602(11) 0.1810(17) 0.156(9) Uani 1 1 d . . . H58 H 0.6543 0.0473 0.1681 0.187 Uiso 1 1 calc R . . C59 C 0.5317(13) 0.0357(10) 0.1321(15) 0.141(7) Uani 1 1 d . . . H59 H 0.5327 0.0065 0.0846 0.169 Uiso 1 1 calc R . . C60 C 0.4558(9) 0.0556(7) 0.1544(12) 0.104(5) Uani 1 1 d . . . H60 H 0.4052 0.0390 0.1207 0.125 Uiso 1 1 calc R . . N1 N 0.2309(16) 0.4874(7) 0.4868(19) 0.206(6) Uiso 0.603(11) 1 d PD . . O1 O 0.1976(16) 0.5158(8) 0.5442(19) 0.206(6) Uiso 0.603(11) 1 d PD . . O2 O 0.2695(17) 0.5083(9) 0.426(2) 0.206(6) Uiso 0.603(11) 1 d PD . . N2 N 0.4859(13) 0.2100(10) -0.0932(19) 0.206(6) Uiso 0.397(11) 1 d PD . . O3 O 0.502(2) 0.2419(12) -0.159(3) 0.206(6) Uiso 0.397(11) 1 d PD . . O4 O 0.509(2) 0.1603(11) -0.089(3) 0.206(6) Uiso 0.397(11) 1 d PD . . O1W O 0.565(2) 0.1083(13) -0.118(2) 0.175(11) Uiso 0.50 1 d P . . 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 0.0573(10) 0.0636(10) 0.0577(9) 0.0032(7) 0.0103(7) -0.0048(7) N21 0.065(6) 0.074(7) 0.059(6) 0.001(5) 0.011(5) -0.001(5) N22 0.059(6) 0.052(5) 0.056(5) 0.004(4) 0.013(5) 0.001(5) N23 0.053(6) 0.067(6) 0.061(6) 0.008(5) 0.006(5) 0.005(5) N24 0.058(6) 0.084(7) 0.059(6) 0.004(5) 0.013(5) -0.010(5) C1 0.069(9) 0.074(9) 0.068(8) 0.000(7) 0.017(7) 0.009(7) C2 0.073(9) 0.096(10) 0.074(8) -0.014(8) 0.018(7) 0.005(8) C3 0.102(11) 0.055(8) 0.074(8) -0.001(6) 0.027(7) 0.013(7) C4 0.089(9) 0.053(7) 0.050(6) -0.001(5) 0.015(6) -0.001(7) C5 0.070(8) 0.070(8) 0.063(7) 0.001(6) 0.015(6) -0.012(7) C6 0.066(8) 0.053(7) 0.063(7) 0.000(6) 0.011(6) 0.001(6) C7 0.065(8) 0.074(8) 0.061(7) 0.019(6) 0.009(6) 0.003(6) C8 0.062(8) 0.065(7) 0.061(7) 0.004(6) 0.012(6) 0.005(6) C9 0.057(7) 0.062(7) 0.055(6) 0.003(6) 0.010(6) -0.003(6) C10 0.068(8) 0.074(8) 0.053(7) 0.014(6) 0.003(6) 0.008(7) C11 0.069(8) 0.062(8) 0.057(7) 0.000(6) 0.000(6) 0.002(6) C12 0.070(8) 0.074(8) 0.059(7) 0.005(6) -0.002(6) 0.012(6) C13 0.064(8) 0.080(8) 0.063(7) -0.005(7) 0.004(6) -0.003(6) C14 0.059(7) 0.074(8) 0.062(7) 0.009(7) 0.012(6) -0.004(6) C15 0.061(8) 0.077(9) 0.070(8) -0.001(7) 0.003(7) 0.002(6) C16 0.062(8) 0.105(11) 0.048(7) 0.018(7) 0.007(6) -0.033(7) C17 0.065(8) 0.092(10) 0.058(7) 0.004(7) 0.001(6) -0.011(7) C18 0.065(8) 0.107(11) 0.066(8) 0.004(8) 0.020(7) -0.012(8) C19 0.060(8) 0.082(9) 0.071(8) -0.007(7) 0.011(6) -0.002(7) C20 0.057(8) 0.093(10) 0.076(8) -0.013(8) 0.014(7) 0.001(7) C21 0.093(11) 0.112(12) 0.118(12) 0.022(10) 0.021(9) 0.032(9) C22 0.125(15) 0.097(12) 0.123(13) 0.002(11) 0.042(12) 0.025(11) C23 0.150(18) 0.122(15) 0.129(15) 0.026(12) 0.030(14) 0.041(14) C24 0.104(11) 0.075(9) 0.091(9) -0.006(7) 0.031(8) 0.012(8) C25 0.071(9) 0.083(9) 0.087(9) 0.017(7) 0.017(7) -0.013(7) C26 0.080(10) 0.093(10) 0.106(11) 0.006(9) 0.020(8) -0.015(8) C27 0.063(8) 0.109(11) 0.091(10) 0.014(9) 0.017(7) -0.017(8) C28 0.073(9) 0.087(9) 0.075(8) 0.018(7) 0.020(7) 0.009(7) C32 0.098(10) 0.069(9) 0.096(10) -0.021(8) -0.008(8) -0.011(7) C33 0.086(9) 0.124(12) 0.069(8) 0.014(8) 0.031(7) -0.014(8) C36 0.091(11) 0.124(12) 0.092(10) 0.000(9) 0.036(9) -0.001(9) C37 0.076(8) 0.065(8) 0.069(8) 0.001(7) 0.017(7) -0.002(6) C38 0.097(10) 0.080(9) 0.075(9) 0.000(7) 0.025(8) -0.007(8) C39 0.116(12) 0.065(9) 0.083(10) -0.010(8) 0.013(9) -0.018(8) C40 0.115(12) 0.059(8) 0.095(11) -0.001(8) -0.009(9) -0.030(8) C41 0.089(10) 0.074(9) 0.090(10) 0.018(8) 0.014(8) -0.024(7) C42 0.086(9) 0.080(9) 0.065(8) 0.003(7) 0.016(7) -0.009(7) C43 0.076(8) 0.073(8) 0.059(7) -0.002(6) 0.017(6) 0.001(7) C44 0.066(8) 0.074(8) 0.064(8) -0.007(6) 0.000(6) 0.008(6) C45 0.091(10) 0.092(10) 0.073(8) -0.016(8) 0.019(8) 0.005(8) C46 0.087(10) 0.099(10) 0.090(11) -0.035(9) 0.022(8) 0.013(8) C47 0.091(10) 0.091(10) 0.099(11) -0.002(9) 0.017(9) 0.017(8) C48 0.076(9) 0.077(8) 0.081(8) 0.007(7) 0.020(7) 0.022(7) C49 0.071(9) 0.064(8) 0.082(9) 0.013(7) 0.011(7) -0.015(7) C50 0.082(10) 0.083(10) 0.139(13) 0.019(9) 0.017(9) -0.018(8) C51 0.091(12) 0.100(13) 0.180(18) 0.024(12) 0.024(12) -0.029(10) C52 0.103(13) 0.097(12) 0.154(16) 0.022(11) 0.054(12) -0.007(11) C53 0.117(14) 0.089(11) 0.095(10) 0.025(9) 0.033(10) 0.013(10) C54 0.080(9) 0.080(9) 0.075(8) 0.007(7) 0.020(7) -0.015(7) C55 0.082(11) 0.109(11) 0.079(9) 0.001(9) 0.018(8) 0.011(8) C56 0.067(11) 0.146(15) 0.121(13) -0.018(11) 0.018(10) 0.008(10) C57 0.061(12) 0.25(3) 0.17(2) -0.05(2) 0.007(12) 0.003(13) C58 0.094(15) 0.24(3) 0.131(16) -0.052(17) 0.015(13) 0.050(16) C59 0.108(15) 0.20(2) 0.114(14) -0.022(14) 0.016(12) 0.042(15) C60 0.079(10) 0.128(13) 0.109(12) -0.008(10) 0.026(9) 0.029(9) _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 N23 1.905(9) . ? Ni1 N24 1.913(9) . ? Ni1 N21 1.916(10) . ? Ni1 N22 1.920(8) . ? N21 C4 1.389(14) . ? N21 C1 1.390(14) . ? N22 C6 1.359(13) . ? N22 C9 1.381(13) . ? N23 C14 1.378(14) . ? N23 C11 1.394(14) . ? N24 C19 1.346(15) . ? N24 C16 1.415(15) . ? C1 C20 1.391(17) . ? C1 C2 1.449(18) . ? C2 C3 1.343(17) . ? C2 C21 1.532(18) . ? C3 C4 1.468(16) . ? C3 C24 1.513(17) . ? C4 C5 1.381(16) . ? C5 C6 1.375(15) . ? C5 C37 1.503(16) . ? C6 C7 1.453(16) . ? C7 C8 1.348(16) . ? C7 C25 1.509(16) . ? C8 C9 1.423(15) . ? C8 C28 1.540(16) . ? C9 C10 1.399(16) . ? C10 C11 1.411(16) . ? C10 C43 1.498(16) . ? C11 C12 1.449(16) . ? C12 C13 1.366(16) . ? C12 C29 1.475(17) . ? C13 C14 1.457(17) . ? C13 C32 1.468(17) . ? C14 C15 1.365(16) . ? C15 C16 1.410(17) . ? C15 C49 1.484(17) . ? C16 C17 1.470(16) . ? C17 C18 1.370(17) . ? C17 C33 1.513(18) . ? C18 C36 1.468(18) . ? C18 C19 1.477(17) . ? C19 C20 1.374(17) . ? C20 C55 1.494(18) . ? C21 C22 1.46(2) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 C23 1.47(2) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 C24 1.52(2) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 C26 1.492(18) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 C27 1.514(19) . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C27 C28 1.492(17) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C29 C30A 1.31(3) . ? C29 C30B 1.68(4) . ? C30A C30B 0.67(4) . ? C30A C31A 1.33(3) . ? C30A C31B 1.78(5) . ? C30B C31A 1.03(4) . ? C30B C31B 1.58(6) . ? C31A C31B 0.58(4) . ? C31A N1 1.461(3) . ? C31A C32 1.53(3) . ? C31B N1 1.31(4) . ? C31B C32 1.45(4) . ? C33 C34B 1.43(3) . ? C33 C34A 1.70(4) . ? C34A C34B 0.64(4) . ? C34A C35A 0.95(4) . ? C34A C35B 1.18(5) . ? C34B C35A 1.51(4) . ? C34B C35B 1.51(4) . ? C35A C35B 0.69(4) . ? C35A N2 1.462(2) . ? C35A C36 1.73(4) . ? C35B C36 1.45(3) . ? C35B N2 1.36(3) . ? C37 C38 1.389(17) . ? C37 C42 1.399(16) . ? C38 C39 1.404(17) . ? C38 H38 0.9500 . ? C39 C40 1.361(19) . ? C39 H39 0.9500 . ? C40 C41 1.368(18) . ? C40 H40 0.9500 . ? C41 C42 1.371(17) . ? C41 H41 0.9500 . ? C42 H42 0.9500 . ? C43 C44 1.371(16) . ? C43 C48 1.409(16) . ? C44 C45 1.368(16) . ? C44 H44 0.9500 . ? C45 C46 1.377(19) . ? C45 H45 0.9500 . ? C46 C47 1.40(2) . ? C46 H46 0.9500 . ? C47 C48 1.371(18) . ? C47 H47 0.9500 . ? C48 H48 0.9500 . ? C49 C54 1.380(17) . ? C49 C50 1.385(18) . ? C50 C51 1.40(2) . ? C50 H50 0.9500 . ? C51 C52 1.38(2) . ? C51 H51 0.9500 . ? C52 C53 1.37(2) . ? C52 H52 0.9500 . ? C53 C54 1.393(18) . ? C53 H53 0.9500 . ? C54 H54 0.9500 . ? C55 C60 1.36(2) . ? C55 C56 1.40(2) . ? C56 C57 1.37(2) . ? C56 H56 0.9500 . ? C57 C58 1.40(3) . ? C57 H57 0.9500 . ? C58 C59 1.35(3) . ? C58 H58 0.9500 . ? C59 C60 1.42(2) . ? C59 H59 0.9500 . ? C60 H60 0.9500 . ? N1 O2 1.235(5) . ? N1 O1 1.236(5) . ? N2 O4 1.246(3) . ? N2 O3 1.243(3) . ? O4 O1W 1.65(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 N23 Ni1 N24 90.4(4) . . ? N23 Ni1 N21 170.6(4) . . ? N24 Ni1 N21 90.1(4) . . ? N23 Ni1 N22 91.3(4) . . ? N24 Ni1 N22 170.3(4) . . ? N21 Ni1 N22 89.7(4) . . ? C4 N21 C1 108.9(10) . . ? C4 N21 Ni1 126.2(8) . . ? C1 N21 Ni1 123.7(8) . . ? C6 N22 C9 105.9(9) . . ? C6 N22 Ni1 125.2(7) . . ? C9 N22 Ni1 127.0(7) . . ? C14 N23 C11 104.8(9) . . ? C14 N23 Ni1 129.0(8) . . ? C11 N23 Ni1 124.7(8) . . ? C19 N24 C16 108.1(10) . . ? C19 N24 Ni1 127.1(9) . . ? C16 N24 Ni1 123.8(8) . . ? N21 C1 C20 122.0(11) . . ? N21 C1 C2 107.4(11) . . ? C20 C1 C2 128.6(12) . . ? C3 C2 C1 108.0(11) . . ? C3 C2 C21 122.4(14) . . ? C1 C2 C21 129.5(13) . . ? C2 C3 C4 108.6(11) . . ? C2 C3 C24 123.1(13) . . ? C4 C3 C24 128.1(12) . . ? C5 C4 N21 123.8(10) . . ? C5 C4 C3 129.8(11) . . ? N21 C4 C3 106.4(11) . . ? C6 C5 C4 122.0(11) . . ? C6 C5 C37 121.4(10) . . ? C4 C5 C37 116.6(11) . . ? N22 C6 C5 122.9(10) . . ? N22 C6 C7 110.0(10) . . ? C5 C6 C7 125.9(11) . . ? C8 C7 C6 105.8(10) . . ? C8 C7 C25 124.6(11) . . ? C6 C7 C25 129.4(11) . . ? C7 C8 C9 108.0(10) . . ? C7 C8 C28 121.2(11) . . ? C9 C8 C28 130.7(11) . . ? N22 C9 C10 122.6(10) . . ? N22 C9 C8 109.6(10) . . ? C10 C9 C8 127.7(11) . . ? C9 C10 C11 122.9(11) . . ? C9 C10 C43 119.1(11) . . ? C11 C10 C43 117.7(11) . . ? N23 C11 C10 121.6(10) . . ? N23 C11 C12 110.5(10) . . ? C10 C11 C12 126.4(11) . . ? C13 C12 C11 106.6(11) . . ? C13 C12 C29 122.8(12) . . ? C11 C12 C29 130.4(12) . . ? C12 C13 C14 106.5(11) . . ? C12 C13 C32 123.9(12) . . ? C14 C13 C32 129.5(12) . . ? C15 C14 N23 122.7(11) . . ? C15 C14 C13 126.4(11) . . ? N23 C14 C13 110.9(10) . . ? C14 C15 C16 122.0(11) . . ? C14 C15 C49 121.6(12) . . ? C16 C15 C49 116.1(11) . . ? C15 C16 N24 123.2(10) . . ? C15 C16 C17 128.7(11) . . ? N24 C16 C17 106.9(12) . . ? C18 C17 C16 108.2(11) . . ? C18 C17 C33 124.4(12) . . ? C16 C17 C33 127.3(13) . . ? C17 C18 C36 124.0(12) . . ? C17 C18 C19 105.9(11) . . ? C36 C18 C19 129.8(14) . . ? N24 C19 C20 124.3(11) . . ? N24 C19 C18 110.1(12) . . ? C20 C19 C18 125.6(12) . . ? C19 C20 C1 121.8(11) . . ? C19 C20 C55 119.0(12) . . ? C1 C20 C55 119.1(13) . . ? C22 C21 C2 112.6(14) . . ? C22 C21 H21A 109.1 . . ? C2 C21 H21A 109.1 . . ? C22 C21 H21B 109.1 . . ? C2 C21 H21B 109.1 . . ? H21A C21 H21B 107.8 . . ? C21 C22 C23 114.1(16) . . ? C21 C22 H22A 108.7 . . ? C23 C22 H22A 108.8 . . ? C21 C22 H22B 108.7 . . ? C23 C22 H22B 108.7 . . ? H22A C22 H22B 107.6 . . ? C22 C23 C24 115.5(16) . . ? C22 C23 H23A 108.4 . . ? C24 C23 H23A 108.4 . . ? C22 C23 H23B 108.5 . . ? C24 C23 H23B 108.4 . . ? H23A C23 H23B 107.5 . . ? C3 C24 C23 112.0(13) . . ? C3 C24 H24A 109.3 . . ? C23 C24 H24A 109.2 . . ? C3 C24 H24B 109.2 . . ? C23 C24 H24B 109.2 . . ? H24A C24 H24B 107.9 . . ? C26 C25 C7 111.7(11) . . ? C26 C25 H25A 109.2 . . ? C7 C25 H25A 109.3 . . ? C26 C25 H25B 109.3 . . ? C7 C25 H25B 109.3 . . ? H25A C25 H25B 107.9 . . ? C25 C26 C27 110.8(12) . . ? C25 C26 H26A 109.4 . . ? C27 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? C27 C26 H26B 109.5 . . ? H26A C26 H26B 108.1 . . ? C28 C27 C26 114.7(11) . . ? C28 C27 H27A 108.6 . . ? C26 C27 H27A 108.5 . . ? C28 C27 H27B 108.6 . . ? C26 C27 H27B 108.7 . . ? H27A C27 H27B 107.6 . . ? C27 C28 C8 111.4(11) . . ? C27 C28 H28A 109.4 . . ? C8 C28 H28A 109.4 . . ? C27 C28 H28B 109.3 . . ? C8 C28 H28B 109.3 . . ? H28A C28 H28B 108.0 . . ? C30A C29 C12 118.5(15) . . ? C30A C29 C30B 21.5(18) . . ? C12 C29 C30B 104.7(17) . . ? C30B C30A C29 112(6) . . ? C30B C30A C31A 49(5) . . ? C29 C30A C31A 117(2) . . ? C30B C30A C31B 62(5) . . ? C29 C30A C31B 120(2) . . ? C31A C30A C31B 14(2) . . ? C30A C30B C31A 102(6) . . ? C30A C30B C31B 96(6) . . ? C31A C30B C31B 8(3) . . ? C30A C30B C29 46(4) . . ? C31A C30B C29 110(3) . . ? C31B C30B C29 110(3) . . ? C31B C31A C30B 158(7) . . ? C31B C31A C30A 133(7) . . ? C30B C31A C30A 29(3) . . ? C31B C31A N1 64(4) . . ? C30B C31A N1 107(3) . . ? C30A C31A N1 114.5(18) . . ? C31B C31A C32 71(5) . . ? C30B C31A C32 129(3) . . ? C30A C31A C32 133.9(17) . . ? N1 C31A C32 111.5(13) . . ? C31A C31B N1 93(5) . . ? C31A C31B C32 86(6) . . ? N1 C31B C32 127(3) . . ? C31A C31B C30B 14(5) . . ? N1 C31B C30B 88(3) . . ? C32 C31B C30B 100(3) . . ? C31A C31B C30A 33(5) . . ? N1 C31B C30A 98(3) . . ? C32 C31B C30A 109(3) . . ? C30B C31B C30A 21.9(15) . . ? C31B C32 C13 117.4(19) . . ? C31B C32 C31A 22.2(17) . . ? C13 C32 C31A 103.8(12) . . ? C34B C33 C17 113.3(16) . . ? C34B C33 C34A 21.5(16) . . ? C17 C33 C34A 103.2(18) . . ? C34B C34A C35A 144(8) . . ? C34B C34A C35B 108(7) . . ? C35A C34A C35B 36(3) . . ? C34B C34A C33 55(5) . . ? C35A C34A C33 132(4) . . ? C35B C34A C33 123(3) . . ? C34A C34B C33 104(6) . . ? C34A C34B C35A 21(5) . . ? C33 C34B C35A 112(2) . . ? C34A C34B C35B 48(5) . . ? C33 C34B C35B 120(2) . . ? C35A C34B C35B 26.6(14) . . ? C35B C35A C34A 91(5) . . ? C35B C35A N2 68(3) . . ? C34A C35A N2 116(3) . . ? C35B C35A C34B 76(4) . . ? C34A C35A C34B 14(3) . . ? N2 C35A C34B 110.0(19) . . ? C35B C35A C36 55(4) . . ? C34A C35A C36 117(4) . . ? N2 C35A C36 98.4(15) . . ? C34B C35A C36 107(2) . . ? C35A C35B C34A 53(4) . . ? C35A C35B C36 102(4) . . ? C34A C35B C36 124(3) . . ? C35A C35B N2 84(3) . . ? C34A C35B N2 108(3) . . ? C36 C35B N2 119(2) . . ? C35A C35B C34B 77(4) . . ? C34A C35B C34B 24(2) . . ? C36 C35B C34B 124(2) . . ? N2 C35B C34B 116(2) . . ? C35B C36 C18 112.4(16) . . ? C35B C36 C35A 23.0(14) . . ? C18 C36 C35A 105.4(13) . . ? C38 C37 C42 118.9(12) . . ? C38 C37 C5 118.9(11) . . ? C42 C37 C5 122.2(11) . . ? C37 C38 C39 120.0(12) . . ? C37 C38 H38 120.0 . . ? C39 C38 H38 120.0 . . ? C40 C39 C38 119.0(13) . . ? C40 C39 H39 120.5 . . ? C38 C39 H39 120.5 . . ? C39 C40 C41 121.9(12) . . ? C39 C40 H40 119.1 . . ? C41 C40 H40 119.0 . . ? C40 C41 C42 119.6(13) . . ? C40 C41 H41 120.2 . . ? C42 C41 H41 120.2 . . ? C41 C42 C37 120.6(12) . . ? C41 C42 H42 119.7 . . ? C37 C42 H42 119.7 . . ? C44 C43 C48 119.2(11) . . ? C44 C43 C10 121.2(11) . . ? C48 C43 C10 119.6(10) . . ? C45 C44 C43 121.0(12) . . ? C45 C44 H44 119.5 . . ? C43 C44 H44 119.5 . . ? C44 C45 C46 120.2(13) . . ? C44 C45 H45 119.9 . . ? C46 C45 H45 119.9 . . ? C45 C46 C47 120.1(13) . . ? C45 C46 H46 120.0 . . ? C47 C46 H46 119.9 . . ? C48 C47 C46 119.2(14) . . ? C48 C47 H47 120.4 . . ? C46 C47 H47 120.4 . . ? C47 C48 C43 120.3(13) . . ? C47 C48 H48 119.8 . . ? C43 C48 H48 119.8 . . ? C54 C49 C50 119.8(12) . . ? C54 C49 C15 120.3(11) . . ? C50 C49 C15 119.9(12) . . ? C49 C50 C51 119.6(15) . . ? C49 C50 H50 120.2 . . ? C51 C50 H50 120.2 . . ? C52 C51 C50 120.5(16) . . ? C52 C51 H51 119.7 . . ? C50 C51 H51 119.8 . . ? C53 C52 C51 119.5(15) . . ? C53 C52 H52 120.3 . . ? C51 C52 H52 120.3 . . ? C52 C53 C54 120.5(15) . . ? C52 C53 H53 119.8 . . ? C54 C53 H53 119.7 . . ? C49 C54 C53 120.1(13) . . ? C49 C54 H54 120.0 . . ? C53 C54 H54 120.0 . . ? C60 C55 C56 117.3(14) . . ? C60 C55 C20 122.3(14) . . ? C56 C55 C20 120.3(14) . . ? C57 C56 C55 121.4(17) . . ? C57 C56 H56 119.3 . . ? C55 C56 H56 119.3 . . ? C56 C57 C58 118.4(19) . . ? C56 C57 H57 120.8 . . ? C58 C57 H57 120.8 . . ? C59 C58 C57 122.3(18) . . ? C59 C58 H58 118.9 . . ? C57 C58 H58 118.8 . . ? C58 C59 C60 117.1(19) . . ? C58 C59 H59 121.4 . . ? C60 C59 H59 121.5 . . ? C55 C60 C59 123.0(17) . . ? C55 C60 H60 118.5 . . ? C59 C60 H60 118.5 . . ? O2 N1 O1 122.6(6) . . ? O2 N1 C31B 103(3) . . ? O1 N1 C31B 122(3) . . ? O2 N1 C31A 117.5(4) . . ? O1 N1 C31A 117.5(4) . . ? C31B N1 C31A 23.3(19) . . ? O4 N2 O3 121.3(2) . . ? O4 N2 C35B 113(2) . . ? O3 N2 C35B 126(2) . . ? O4 N2 C35A 116.9(2) . . ? O3 N2 C35A 117.1(2) . . ? C35B N2 C35A 28.1(15) . . ? N2 O4 O1W 152(2) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N23 Ni1 N21 C4 102(2) . . . . ? N24 Ni1 N21 C4 -164.5(9) . . . . ? N22 Ni1 N21 C4 5.8(9) . . . . ? N23 Ni1 N21 C1 -64(3) . . . . ? N24 Ni1 N21 C1 29.3(9) . . . . ? N22 Ni1 N21 C1 -160.4(9) . . . . ? N23 Ni1 N22 C6 159.5(9) . . . . ? N24 Ni1 N22 C6 59(3) . . . . ? N21 Ni1 N22 C6 -29.9(9) . . . . ? N23 Ni1 N22 C9 -2.6(9) . . . . ? N24 Ni1 N22 C9 -103(2) . . . . ? N21 Ni1 N22 C9 168.0(9) . . . . ? N24 Ni1 N23 C14 2.4(10) . . . . ? N21 Ni1 N23 C14 96(2) . . . . ? N22 Ni1 N23 C14 -168.1(9) . . . . ? N24 Ni1 N23 C11 -161.5(9) . . . . ? N21 Ni1 N23 C11 -68(3) . . . . ? N22 Ni1 N23 C11 28.0(9) . . . . ? N23 Ni1 N24 C19 167.3(10) . . . . ? N21 Ni1 N24 C19 -3.3(10) . . . . ? N22 Ni1 N24 C19 -93(3) . . . . ? N23 Ni1 N24 C16 -25.5(9) . . . . ? N21 Ni1 N24 C16 163.9(9) . . . . ? N22 Ni1 N24 C16 75(3) . . . . ? C4 N21 C1 C20 155.8(11) . . . . ? Ni1 N21 C1 C20 -35.9(15) . . . . ? C4 N21 C1 C2 -9.3(13) . . . . ? Ni1 N21 C1 C2 159.0(8) . . . . ? N21 C1 C2 C3 8.8(14) . . . . ? C20 C1 C2 C3 -155.0(13) . . . . ? N21 C1 C2 C21 -167.5(13) . . . . ? C20 C1 C2 C21 29(2) . . . . ? C1 C2 C3 C4 -4.8(14) . . . . ? C21 C2 C3 C4 171.8(12) . . . . ? C1 C2 C3 C24 -179.3(11) . . . . ? C21 C2 C3 C24 -3(2) . . . . ? C1 N21 C4 C5 -175.7(10) . . . . ? Ni1 N21 C4 C5 16.4(15) . . . . ? C1 N21 C4 C3 6.4(12) . . . . ? Ni1 N21 C4 C3 -161.6(8) . . . . ? C2 C3 C4 C5 -178.6(12) . . . . ? C24 C3 C4 C5 -4(2) . . . . ? C2 C3 C4 N21 -0.8(13) . . . . ? C24 C3 C4 N21 173.3(12) . . . . ? N21 C4 C5 C6 -20.4(18) . . . . ? C3 C4 C5 C6 157.0(12) . . . . ? N21 C4 C5 C37 162.7(10) . . . . ? C3 C4 C5 C37 -19.9(18) . . . . ? C9 N22 C6 C5 -160.4(10) . . . . ? Ni1 N22 C6 C5 34.4(15) . . . . ? C9 N22 C6 C7 7.8(12) . . . . ? Ni1 N22 C6 C7 -157.4(7) . . . . ? C4 C5 C6 N22 -5.6(18) . . . . ? C37 C5 C6 N22 171.1(10) . . . . ? C4 C5 C6 C7 -171.9(11) . . . . ? C37 C5 C6 C7 4.9(18) . . . . ? N22 C6 C7 C8 -7.7(13) . . . . ? C5 C6 C7 C8 160.1(11) . . . . ? N22 C6 C7 C25 168.8(11) . . . . ? C5 C6 C7 C25 -23.4(19) . . . . ? C6 C7 C8 C9 4.2(12) . . . . ? C25 C7 C8 C9 -172.5(11) . . . . ? C6 C7 C8 C28 -179.8(10) . . . . ? C25 C7 C8 C28 3.5(17) . . . . ? C6 N22 C9 C10 176.3(10) . . . . ? Ni1 N22 C9 C10 -18.8(14) . . . . ? C6 N22 C9 C8 -5.1(12) . . . . ? Ni1 N22 C9 C8 159.7(7) . . . . ? C7 C8 C9 N22 0.4(13) . . . . ? C28 C8 C9 N22 -175.1(11) . . . . ? C7 C8 C9 C10 178.9(11) . . . . ? C28 C8 C9 C10 3(2) . . . . ? N22 C9 C10 C11 19.3(17) . . . . ? C8 C9 C10 C11 -158.9(11) . . . . ? N22 C9 C10 C43 -166.7(10) . . . . ? C8 C9 C10 C43 15.1(17) . . . . ? C14 N23 C11 C10 158.5(10) . . . . ? Ni1 N23 C11 C10 -34.4(14) . . . . ? C14 N23 C11 C12 -8.5(12) . . . . ? Ni1 N23 C11 C12 158.7(7) . . . . ? C9 C10 C11 N23 7.8(17) . . . . ? C43 C10 C11 N23 -166.3(10) . . . . ? C9 C10 C11 C12 172.5(11) . . . . ? C43 C10 C11 C12 -1.6(17) . . . . ? N23 C11 C12 C13 8.3(13) . . . . ? C10 C11 C12 C13 -157.9(11) . . . . ? N23 C11 C12 C29 -167.5(11) . . . . ? C10 C11 C12 C29 26.3(19) . . . . ? C11 C12 C13 C14 -4.4(13) . . . . ? C29 C12 C13 C14 171.8(11) . . . . ? C11 C12 C13 C32 179.7(11) . . . . ? C29 C12 C13 C32 -4.1(19) . . . . ? C11 N23 C14 C15 -174.5(11) . . . . ? Ni1 N23 C14 C15 19.1(16) . . . . ? C11 N23 C14 C13 5.6(12) . . . . ? Ni1 N23 C14 C13 -160.7(8) . . . . ? C12 C13 C14 C15 179.5(12) . . . . ? C32 C13 C14 C15 -5(2) . . . . ? C12 C13 C14 N23 -0.7(13) . . . . ? C32 C13 C14 N23 174.9(12) . . . . ? N23 C14 C15 C16 -20.1(18) . . . . ? C13 C14 C15 C16 159.7(12) . . . . ? N23 C14 C15 C49 165.8(11) . . . . ? C13 C14 C15 C49 -14.4(19) . . . . ? C14 C15 C16 N24 -5.5(18) . . . . ? C49 C15 C16 N24 168.9(10) . . . . ? C14 C15 C16 C17 -171.4(11) . . . . ? C49 C15 C16 C17 3.0(18) . . . . ? C19 N24 C16 C15 -159.6(11) . . . . ? Ni1 N24 C16 C15 31.2(15) . . . . ? C19 N24 C16 C17 8.9(12) . . . . ? Ni1 N24 C16 C17 -160.3(7) . . . . ? C15 C16 C17 C18 160.4(12) . . . . ? N24 C16 C17 C18 -7.3(13) . . . . ? C15 C16 C17 C33 -21(2) . . . . ? N24 C16 C17 C33 170.9(12) . . . . ? C16 C17 C18 C36 177.7(12) . . . . ? C33 C17 C18 C36 0(2) . . . . ? C16 C17 C18 C19 2.9(13) . . . . ? C33 C17 C18 C19 -175.3(11) . . . . ? C16 N24 C19 C20 171.2(11) . . . . ? Ni1 N24 C19 C20 -20.0(17) . . . . ? C16 N24 C19 C18 -7.4(13) . . . . ? Ni1 N24 C19 C18 161.4(8) . . . . ? C17 C18 C19 N24 2.7(14) . . . . ? C36 C18 C19 N24 -171.7(13) . . . . ? C17 C18 C19 C20 -175.8(12) . . . . ? C36 C18 C19 C20 10(2) . . . . ? N24 C19 C20 C1 21.0(19) . . . . ? C18 C19 C20 C1 -160.7(12) . . . . ? N24 C19 C20 C55 -162.1(12) . . . . ? C18 C19 C20 C55 16.2(19) . . . . ? N21 C1 C20 C19 8.0(19) . . . . ? C2 C1 C20 C19 169.7(13) . . . . ? N21 C1 C20 C55 -168.9(11) . . . . ? C2 C1 C20 C55 -7(2) . . . . ? C3 C2 C21 C22 -15(2) . . . . ? C1 C2 C21 C22 160.9(14) . . . . ? C2 C21 C22 C23 42(2) . . . . ? C21 C22 C23 C24 -54(2) . . . . ? C2 C3 C24 C23 -7(2) . . . . ? C4 C3 C24 C23 179.8(13) . . . . ? C22 C23 C24 C3 35(2) . . . . ? C8 C7 C25 C26 15.1(17) . . . . ? C6 C7 C25 C26 -160.8(12) . . . . ? C7 C25 C26 C27 -44.7(15) . . . . ? C25 C26 C27 C28 60.5(16) . . . . ? C26 C27 C28 C8 -40.7(16) . . . . ? C7 C8 C28 C27 9.2(16) . . . . ? C9 C8 C28 C27 -175.8(12) . . . . ? C13 C12 C29 C30A 3(2) . . . . ? C11 C12 C29 C30A 178.4(17) . . . . ? C13 C12 C29 C30B -15(2) . . . . ? C11 C12 C29 C30B 160.6(19) . . . . ? C12 C29 C30A C30B -54(7) . . . . ? C12 C29 C30A C31A 0(3) . . . . ? C30B C29 C30A C31A 54(5) . . . . ? C12 C29 C30A C31B 15(3) . . . . ? C30B C29 C30A C31B 69(6) . . . . ? C29 C30A C30B C31A 107(4) . . . . ? C31B C30A C30B C31A -6(2) . . . . ? C29 C30A C30B C31B 113(4) . . . . ? C31A C30A C30B C31B 6(2) . . . . ? C31A C30A C30B C29 -107(4) . . . . ? C31B C30A C30B C29 -113(4) . . . . ? C12 C29 C30B C30A 133(6) . . . . ? C30A C29 C30B C31A -87(7) . . . . ? C12 C29 C30B C31A 46(4) . . . . ? C30A C29 C30B C31B -79(6) . . . . ? C12 C29 C30B C31B 54(3) . . . . ? C30A C30B C31A C31B 46(19) . . . . ? C29 C30B C31A C31B 94(17) . . . . ? C31B C30B C31A C30A -46(19) . . . . ? C29 C30B C31A C30A 47(5) . . . . ? C30A C30B C31A N1 109(6) . . . . ? C31B C30B C31A N1 63(16) . . . . ? C29 C30B C31A N1 156(2) . . . . ? C30A C30B C31A C32 -112(6) . . . . ? C31B C30B C31A C32 -159(19) . . . . ? C29 C30B C31A C32 -65(5) . . . . ? C30B C30A C31A C31B -158(9) . . . . ? C29 C30A C31A C31B 104(7) . . . . ? C29 C30A C31A C30B -97(7) . . . . ? C31B C30A C31A C30B 158(9) . . . . ? C30B C30A C31A N1 -82(6) . . . . ? C29 C30A C31A N1 -179(2) . . . . ? C31B C30A C31A N1 76(7) . . . . ? C30B C30A C31A C32 94(7) . . . . ? C29 C30A C31A C32 -3(5) . . . . ? C31B C30A C31A C32 -107(8) . . . . ? C30B C31A C31B N1 71(17) . . . . ? C30A C31A C31B N1 100(5) . . . . ? C32 C31A C31B N1 -127(3) . . . . ? C30B C31A C31B C32 -163(16) . . . . ? C30A C31A C31B C32 -134(5) . . . . ? N1 C31A C31B C32 127(3) . . . . ? C30A C31A C31B C30B 29(13) . . . . ? N1 C31A C31B C30B -71(17) . . . . ? C32 C31A C31B C30B 163(16) . . . . ? C30B C31A C31B C30A -29(13) . . . . ? N1 C31A C31B C30A -100(5) . . . . ? C32 C31A C31B C30A 134(5) . . . . ? C30A C30B C31B C31A -134(19) . . . . ? C29 C30B C31B C31A -89(17) . . . . ? C30A C30B C31B N1 116(6) . . . . ? C31A C30B C31B N1 -109(18) . . . . ? C29 C30B C31B N1 161(3) . . . . ? C30A C30B C31B C32 -117(5) . . . . ? C31A C30B C31B C32 17(16) . . . . ? C29 C30B C31B C32 -72(3) . . . . ? C31A C30B C31B C30A 134(19) . . . . ? C29 C30B C31B C30A 45(4) . . . . ? C30B C30A C31B C31A 18(8) . . . . ? C29 C30A C31B C31A -83(7) . . . . ? C30B C30A C31B N1 -65(6) . . . . ? C29 C30A C31B N1 -166(3) . . . . ? C31A C30A C31B N1 -83(7) . . . . ? C30B C30A C31B C32 68(6) . . . . ? C29 C30A C31B C32 -33(4) . . . . ? C31A C30A C31B C32 50(6) . . . . ? C29 C30A C31B C30B -101(6) . . . . ? C31A C30A C31B C30B -18(8) . . . . ? C31A C31B C32 C13 56(6) . . . . ? N1 C31B C32 C13 147(3) . . . . ? C30B C31B C32 C13 52(3) . . . . ? C30A C31B C32 C13 31(3) . . . . ? N1 C31B C32 C31A 91(6) . . . . ? C30B C31B C32 C31A -4(4) . . . . ? C30A C31B C32 C31A -25(4) . . . . ? C12 C13 C32 C31B -17(3) . . . . ? C14 C13 C32 C31B 168(2) . . . . ? C12 C13 C32 C31A 1.5(19) . . . . ? C14 C13 C32 C31A -173.4(15) . . . . ? C30B C31A C32 C31B 172(8) . . . . ? C30A C31A C32 C31B 133(7) . . . . ? N1 C31A C32 C31B -51(5) . . . . ? C31B C31A C32 C13 -131(5) . . . . ? C30B C31A C32 C13 41(4) . . . . ? C30A C31A C32 C13 2(4) . . . . ? N1 C31A C32 C13 178.4(19) . . . . ? C18 C17 C33 C34B -9(2) . . . . ? C16 C17 C33 C34B 173.0(16) . . . . ? C18 C17 C33 C34A 11(2) . . . . ? C16 C17 C33 C34A -167.0(18) . . . . ? C17 C33 C34A C34B -121(6) . . . . ? C34B C33 C34A C35A 135(10) . . . . ? C17 C33 C34A C35A 14(6) . . . . ? C34B C33 C34A C35B 90(7) . . . . ? C17 C33 C34A C35B -31(4) . . . . ? C35A C34A C34B C33 -115(12) . . . . ? C35B C34A C34B C33 -118(4) . . . . ? C35B C34A C34B C35A -3(9) . . . . ? C33 C34A C34B C35A 115(12) . . . . ? C35A C34A C34B C35B 3(9) . . . . ? C33 C34A C34B C35B 118(4) . . . . ? C17 C33 C34B C34A 65(6) . . . . ? C17 C33 C34B C35A 45(3) . . . . ? C34A C33 C34B C35A -21(5) . . . . ? C17 C33 C34B C35B 16(3) . . . . ? C34A C33 C34B C35B -49(5) . . . . ? C34B C34A C35A C35B -4(14) . . . . ? C33 C34A C35A C35B -90(5) . . . . ? C34B C34A C35A N2 -70(14) . . . . ? C35B C34A C35A N2 -66(3) . . . . ? C33 C34A C35A N2 -156(3) . . . . ? C35B C34A C35A C34B 4(14) . . . . ? C33 C34A C35A C34B -86(14) . . . . ? C34B C34A C35A C36 46(14) . . . . ? C35B C34A C35A C36 50(4) . . . . ? C33 C34A C35A C36 -40(6) . . . . ? C34A C34B C35A C35B 176(15) . . . . ? C33 C34B C35A C35B -113(4) . . . . ? C33 C34B C35A C34A 72(13) . . . . ? C35B C34B C35A C34A -176(15) . . . . ? C34A C34B C35A N2 116(14) . . . . ? C33 C34B C35A N2 -172.8(19) . . . . ? C35B C34B C35A N2 -60(3) . . . . ? C34A C34B C35A C36 -138(13) . . . . ? C33 C34B C35A C36 -67(2) . . . . ? C35B C34B C35A C36 46(3) . . . . ? N2 C35A C35B C34A 118(3) . . . . ? C34B C35A C35B C34A -1(4) . . . . ? C36 C35A C35B C34A -124(4) . . . . ? C34A C35A C35B C36 124(4) . . . . ? N2 C35A C35B C36 -119(3) . . . . ? C34B C35A C35B C36 123(2) . . . . ? C34A C35A C35B N2 -118(3) . . . . ? C34B C35A C35B N2 -118.7(19) . . . . ? C36 C35A C35B N2 119(3) . . . . ? C34A C35A C35B C34B 1(4) . . . . ? N2 C35A C35B C34B 118.7(19) . . . . ? C36 C35A C35B C34B -123(2) . . . . ? C34B C34A C35B C35A 177(9) . . . . ? C33 C34A C35B C35A 118(5) . . . . ? C34B C34A C35B C36 98(7) . . . . ? C35A C34A C35B C36 -79(5) . . . . ? C33 C34A C35B C36 39(5) . . . . ? C34B C34A C35B N2 -115(6) . . . . ? C35A C34A C35B N2 68(4) . . . . ? C33 C34A C35B N2 -174(3) . . . . ? C35A C34A C35B C34B -177(9) . . . . ? C33 C34A C35B C34B -59(6) . . . . ? C34A C34B C35B C35A -2(7) . . . . ? C33 C34B C35B C35A 79(4) . . . . ? C33 C34B C35B C34A 82(7) . . . . ? C35A C34B C35B C34A 2(7) . . . . ? C34A C34B C35B C36 -98(7) . . . . ? C33 C34B C35B C36 -16(4) . . . . ? C35A C34B C35B C36 -96(4) . . . . ? C34A C34B C35B N2 74(7) . . . . ? C33 C34B C35B N2 156(2) . . . . ? C35A C34B C35B N2 77(3) . . . . ? C35A C35B C36 C18 -76(4) . . . . ? C34A C35B C36 C18 -23(4) . . . . ? N2 C35B C36 C18 -166.2(19) . . . . ? C34B C35B C36 C18 6(3) . . . . ? C34A C35B C36 C35A 54(4) . . . . ? N2 C35B C36 C35A -90(4) . . . . ? C34B C35B C36 C35A 82(4) . . . . ? C17 C18 C36 C35B 2(2) . . . . ? C19 C18 C36 C35B 175.6(16) . . . . ? C17 C18 C36 C35A -21(2) . . . . ? C19 C18 C36 C35A 152.4(16) . . . . ? C34A C35A C36 C35B -69(5) . . . . ? N2 C35A C36 C35B 55(3) . . . . ? C34B C35A C36 C35B -59(4) . . . . ? C35B C35A C36 C18 111(4) . . . . ? C34A C35A C36 C18 42(4) . . . . ? N2 C35A C36 C18 166.6(15) . . . . ? C34B C35A C36 C18 52.5(19) . . . . ? C6 C5 C37 C38 108.4(14) . . . . ? C4 C5 C37 C38 -74.6(15) . . . . ? C6 C5 C37 C42 -71.6(16) . . . . ? C4 C5 C37 C42 105.3(14) . . . . ? C42 C37 C38 C39 0.1(19) . . . . ? C5 C37 C38 C39 -180.0(12) . . . . ? C37 C38 C39 C40 -1(2) . . . . ? C38 C39 C40 C41 1(2) . . . . ? C39 C40 C41 C42 0(2) . . . . ? C40 C41 C42 C37 -1(2) . . . . ? C38 C37 C42 C41 0.8(19) . . . . ? C5 C37 C42 C41 -179.2(12) . . . . ? C9 C10 C43 C44 81.9(15) . . . . ? C11 C10 C43 C44 -103.7(13) . . . . ? C9 C10 C43 C48 -96.7(14) . . . . ? C11 C10 C43 C48 77.6(15) . . . . ? C48 C43 C44 C45 1.8(19) . . . . ? C10 C43 C44 C45 -176.8(12) . . . . ? C43 C44 C45 C46 -1(2) . . . . ? C44 C45 C46 C47 0(2) . . . . ? C45 C46 C47 C48 0(2) . . . . ? C46 C47 C48 C43 1(2) . . . . ? C44 C43 C48 C47 -2(2) . . . . ? C10 C43 C48 C47 176.7(12) . . . . ? C14 C15 C49 C54 -81.5(16) . . . . ? C16 C15 C49 C54 104.1(14) . . . . ? C14 C15 C49 C50 95.8(16) . . . . ? C16 C15 C49 C50 -78.7(16) . . . . ? C54 C49 C50 C51 -1(2) . . . . ? C15 C49 C50 C51 -178.3(14) . . . . ? C49 C50 C51 C52 2(3) . . . . ? C50 C51 C52 C53 0(3) . . . . ? C51 C52 C53 C54 -2(2) . . . . ? C50 C49 C54 C53 -1(2) . . . . ? C15 C49 C54 C53 176.4(12) . . . . ? C52 C53 C54 C49 2(2) . . . . ? C19 C20 C55 C60 -106.4(17) . . . . ? C1 C20 C55 C60 70.7(18) . . . . ? C19 C20 C55 C56 72.0(18) . . . . ? C1 C20 C55 C56 -110.9(16) . . . . ? C60 C55 C56 C57 6(3) . . . . ? C20 C55 C56 C57 -172.1(18) . . . . ? C55 C56 C57 C58 -7(3) . . . . ? C56 C57 C58 C59 5(4) . . . . ? C57 C58 C59 C60 -1(4) . . . . ? C56 C55 C60 C59 -3(2) . . . . ? C20 C55 C60 C59 175.9(16) . . . . ? C58 C59 C60 C55 0(3) . . . . ? C31A C31B N1 O2 133(6) . . . . ? C32 C31B N1 O2 45(4) . . . . ? C30B C31B N1 O2 146(3) . . . . ? C30A C31B N1 O2 165(2) . . . . ? C31A C31B N1 O1 -85(6) . . . . ? C32 C31B N1 O1 -172(3) . . . . ? C30B C31B N1 O1 -72(4) . . . . ? C30A C31B N1 O1 -52(4) . . . . ? C32 C31B N1 C31A -88(7) . . . . ? C30B C31B N1 C31A 13(5) . . . . ? C30A C31B N1 C31A 33(5) . . . . ? C31B C31A N1 O2 -54(7) . . . . ? C30B C31A N1 O2 147(4) . . . . ? C30A C31A N1 O2 178(3) . . . . ? C32 C31A N1 O2 1(4) . . . . ? C31B C31A N1 O1 109(7) . . . . ? C30B C31A N1 O1 -50(4) . . . . ? C30A C31A N1 O1 -19(4) . . . . ? C32 C31A N1 O1 164(3) . . . . ? C30B C31A N1 C31B -159(8) . . . . ? C30A C31A N1 C31B -128(7) . . . . ? C32 C31A N1 C31B 55(6) . . . . ? C35A C35B N2 O4 -105(4) . . . . ? C34A C35B N2 O4 -153(3) . . . . ? C36 C35B N2 O4 -4(3) . . . . ? C34B C35B N2 O4 -177(2) . . . . ? C35A C35B N2 O3 81(5) . . . . ? C34A C35B N2 O3 33(4) . . . . ? C36 C35B N2 O3 -178(2) . . . . ? C34B C35B N2 O3 9(3) . . . . ? C34A C35B N2 C35A -48(4) . . . . ? C36 C35B N2 C35A 100(5) . . . . ? C34B C35B N2 C35A -72(4) . . . . ? C35B C35A N2 O4 88(5) . . . . ? C34A C35A N2 O4 168(5) . . . . ? C34B C35A N2 O4 153(3) . . . . ? C36 C35A N2 O4 42(2) . . . . ? C35B C35A N2 O3 -116(5) . . . . ? C34A C35A N2 O3 -36(5) . . . . ? C34B C35A N2 O3 -50(3) . . . . ? C36 C35A N2 O3 -162(2) . . . . ? C34A C35A N2 C35B 79(5) . . . . ? C34B C35A N2 C35B 65(4) . . . . ? C36 C35A N2 C35B -47(4) . . . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 22.7 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 0.93 _refine_diff_density_min -0.46 _refine_diff_density_rms 0.096 # END OF CIF for Compound7 # END OF FILE