# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_L1Zn2 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common '[LZn2(OAc)](CHCl3)2(MeOH)1.5(H2O)0.5' _chemical_melting_point >573 _chemical_formula_moiety C46.50H41Cl6N4O7Zn2 _chemical_formula_sum 'C46.50 H41 Cl6 N4 O7 Zn2' _chemical_formula_weight 1111.27 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 '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 12.2064(6) _cell_length_b 15.2488(7) _cell_length_c 15.5982(7) _cell_angle_alpha 116.2286(12) _cell_angle_beta 105.4117(15) _cell_angle_gamma 98.7661(15) _cell_volume 2385.38(19) _cell_formula_units_Z 2 _cell_measurement_temperature 120 _cell_measurement_reflns_used 18886 _cell_measurement_theta_min 3.04 _cell_measurement_theta_max 25.00 _exptl_crystal_description prismatic _exptl_crystal_colour yellow _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.547 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1132 _exptl_absorpt_coefficient_mu 1.396 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6051 _exptl_absorpt_correction_T_max 0.9335 _exptl_absorpt_process_details 'Rapid AUTO (Rigaku Corp.)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120 _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku R-AXIS Rapid' _diffrn_measurement_method IP _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 18886 _diffrn_reflns_av_R_equivalents 0.0381 _diffrn_reflns_av_sigmaI/netI 0.0506 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.04 _diffrn_reflns_theta_max 25.00 _reflns_number_total 8394 _reflns_number_gt 6742 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Rapid AUTO (Rigaku Corp.)' _computing_cell_refinement 'Rapid AUTO (Rigaku Corp.)' _computing_data_reduction 'Rapid AUTO (Rigaku Corp.)' _computing_structure_solution 'DIRDIF99 (Beurskens et al., 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ORTEP-3 _computing_publication_material ORTEP-3 _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^)+(0.1177P)^2^+5.3412P] 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 8394 _refine_ls_number_parameters 612 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.0775 _refine_ls_R_factor_gt 0.0638 _refine_ls_wR_factor_ref 0.1950 _refine_ls_wR_factor_gt 0.1776 _refine_ls_goodness_of_fit_ref 1.053 _refine_ls_restrained_S_all 1.053 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zn1 Zn 0.33679(5) 0.37369(4) 0.03573(4) 0.02152(18) Uani 1 1 d . . . Zn2 Zn 0.12582(5) 0.24540(4) 0.04636(4) 0.02153(18) Uani 1 1 d . . . C1 C 0.4915(4) 0.2568(4) 0.0395(4) 0.0241(10) Uani 1 1 d . . . C2 C 0.5809(4) 0.3398(3) 0.1299(4) 0.0234(10) Uani 1 1 d . . . C3 C 0.6549(5) 0.3212(4) 0.2017(4) 0.0286(11) Uani 1 1 d . . . H1 H 0.7129 0.3782 0.2641 0.034 Uiso 1 1 calc R . . C4 C 0.6468(5) 0.2234(4) 0.1853(4) 0.0330(12) Uani 1 1 d . . . C5 C 0.5654(5) 0.1418(4) 0.0930(4) 0.0360(12) Uani 1 1 d . . . H2 H 0.5614 0.0737 0.0783 0.043 Uiso 1 1 calc R . . C6 C 0.4886(5) 0.1567(4) 0.0204(4) 0.0298(11) Uani 1 1 d . . . H3 H 0.4335 0.0987 -0.0428 0.036 Uiso 1 1 calc R . . O1 O 0.4100(3) 0.2669(2) -0.0297(3) 0.0262(7) Uani 1 1 d . . . C7 C 0.7250(6) 0.2067(5) 0.2671(5) 0.0476(15) Uani 1 1 d . . . H4 H 0.6750 0.1598 0.2789 0.071 Uiso 1 1 calc R . . H5 H 0.7663 0.2728 0.3316 0.071 Uiso 1 1 calc R . . H6 H 0.7843 0.1766 0.2436 0.071 Uiso 1 1 calc R . . N1 N 0.5053(4) 0.4757(3) 0.1212(3) 0.0226(8) Uani 1 1 d . . . C8 C 0.6000(4) 0.4480(3) 0.1544(3) 0.0235(10) Uani 1 1 d . . . C9 C 0.7135(4) 0.5211(4) 0.2098(4) 0.0260(10) Uani 1 1 d . . . H7 H 0.7812 0.5026 0.2338 0.031 Uiso 1 1 calc R . . C10 C 0.7265(5) 0.6208(4) 0.2296(4) 0.0277(10) Uani 1 1 d . . . H8 H 0.8032 0.6713 0.2681 0.033 Uiso 1 1 calc R . . C11 C 0.6272(4) 0.6468(3) 0.1929(4) 0.0251(10) Uani 1 1 d . . . H9 H 0.6351 0.7147 0.2051 0.030 Uiso 1 1 calc R . . C12 C 0.5174(4) 0.5723(3) 0.1386(3) 0.0228(10) Uani 1 1 d . . . N2 N 0.3052(3) 0.5059(3) 0.0322(3) 0.0203(8) Uani 1 1 d . . . C13 C 0.4038(4) 0.5897(4) 0.0938(4) 0.0238(10) Uani 1 1 d . . . C14 C 0.4015(5) 0.6880(4) 0.1156(4) 0.0274(10) Uani 1 1 d . . . H10 H 0.4718 0.7456 0.1588 0.033 Uiso 1 1 calc R . . C15 C 0.2941(5) 0.6996(4) 0.0727(4) 0.0303(11) Uani 1 1 d . . . H11 H 0.2896 0.7659 0.0869 0.036 Uiso 1 1 calc R . . C16 C 0.1941(5) 0.6152(4) 0.0097(4) 0.0281(10) Uani 1 1 d . . . H12 H 0.1203 0.6235 -0.0195 0.034 Uiso 1 1 calc R . . C17 C 0.1996(4) 0.5162(3) -0.0123(4) 0.0223(9) Uani 1 1 d . . . C18 C 0.0763(4) 0.3261(3) -0.0934(3) 0.0222(9) Uani 1 1 d . . . C19 C 0.0895(4) 0.4248(4) -0.0841(4) 0.0242(10) Uani 1 1 d . . . C20 C -0.0085(5) 0.4389(4) -0.1424(4) 0.0283(11) Uani 1 1 d . . . H13 H -0.0001 0.5048 -0.1358 0.034 Uiso 1 1 calc R . . C21 C -0.1153(5) 0.3627(4) -0.2082(4) 0.0306(11) Uani 1 1 d . . . C22 C -0.1272(5) 0.2662(4) -0.2169(4) 0.0280(10) Uani 1 1 d . . . H14 H -0.2003 0.2122 -0.2626 0.034 Uiso 1 1 calc R . . C23 C -0.0345(4) 0.2474(4) -0.1606(4) 0.0249(10) Uani 1 1 d . . . O2 O 0.1640(3) 0.3058(2) -0.0427(3) 0.0250(7) Uani 1 1 d . . . C24 C -0.2195(5) 0.3831(5) -0.2679(5) 0.0417(14) Uani 1 1 d . . . H15 H -0.2018 0.4574 -0.2408 0.063 Uiso 1 1 calc R . . H16 H -0.2925 0.3569 -0.2602 0.063 Uiso 1 1 calc R . . H17 H -0.2310 0.3483 -0.3411 0.063 Uiso 1 1 calc R . . N3 N 0.0131(4) 0.1274(3) -0.1021(3) 0.0237(8) Uani 1 1 d . . . C25 C -0.0531(4) 0.1403(4) -0.1776(4) 0.0250(10) Uani 1 1 d . . . C26 C -0.1310(5) 0.0545(4) -0.2704(4) 0.0327(11) Uani 1 1 d . . . H18 H -0.1764 0.0630 -0.3243 0.039 Uiso 1 1 calc R . . C27 C -0.1429(5) -0.0425(4) -0.2848(4) 0.0357(12) Uani 1 1 d . . . H19 H -0.2001 -0.1007 -0.3466 0.043 Uiso 1 1 calc R . . C28 C -0.0703(5) -0.0549(4) -0.2078(4) 0.0320(11) Uani 1 1 d . . . H20 H -0.0756 -0.1215 -0.2168 0.038 Uiso 1 1 calc R . . C29 C 0.0086(4) 0.0315(3) -0.1191(4) 0.0241(10) Uani 1 1 d . . . N4 N 0.1722(4) 0.1208(3) 0.0469(3) 0.0226(8) Uani 1 1 d . . . C30 C 0.1043(4) 0.0292(4) -0.0372(4) 0.0243(10) Uani 1 1 d . . . C31 C 0.1279(5) -0.0610(4) -0.0526(4) 0.0283(11) Uani 1 1 d . . . H21 H 0.0774 -0.1250 -0.1118 0.034 Uiso 1 1 calc R . . C32 C 0.2270(5) -0.0566(4) 0.0200(4) 0.0320(12) Uani 1 1 d . . . H22 H 0.2455 -0.1176 0.0112 0.038 Uiso 1 1 calc R . . C33 C 0.2982(5) 0.0377(4) 0.1051(4) 0.0310(11) Uani 1 1 d . . . H23 H 0.3673 0.0419 0.1544 0.037 Uiso 1 1 calc R . . C34 C 0.2690(4) 0.1279(4) 0.1196(4) 0.0254(10) Uani 1 1 d . . . C35 C 0.3577(4) 0.3241(4) 0.2131(4) 0.0237(10) Uani 1 1 d . . . C36 C 0.3442(4) 0.2286(4) 0.2106(4) 0.0252(10) Uani 1 1 d . . . C37 C 0.4133(5) 0.2303(4) 0.3006(4) 0.0322(11) Uani 1 1 d . . . H24 H 0.4033 0.1674 0.3008 0.039 Uiso 1 1 calc R . . C38 C 0.4938(5) 0.3184(4) 0.3873(4) 0.0358(12) Uani 1 1 d . . . C39 C 0.5072(5) 0.4107(4) 0.3866(4) 0.0318(11) Uani 1 1 d . . . H25 H 0.5631 0.4727 0.4452 0.038 Uiso 1 1 calc R . . C40 C 0.4398(5) 0.4125(4) 0.3014(4) 0.0300(11) Uani 1 1 d . . . H26 H 0.4499 0.4763 0.3030 0.036 Uiso 1 1 calc R . . O3 O 0.2943(3) 0.3321(2) 0.1335(2) 0.0252(7) Uani 1 1 d . . . C41 C 0.5663(6) 0.3158(5) 0.4810(5) 0.0470(15) Uani 1 1 d . . . H27 H 0.5455 0.2450 0.4674 0.071 Uiso 1 1 calc R . . H28 H 0.5484 0.3598 0.5405 0.071 Uiso 1 1 calc R . . H29 H 0.6517 0.3409 0.4957 0.071 Uiso 1 1 calc R . . O4 O 0.0227(3) 0.3183(3) 0.1073(3) 0.0304(8) Uani 1 1 d . . . O5 O 0.0918(3) 0.2839(3) 0.2311(3) 0.0352(8) Uani 1 1 d . . . C42 C 0.0330(5) 0.3271(4) 0.1943(4) 0.0280(11) Uani 1 1 d . . . C43 C -0.0327(6) 0.3919(5) 0.2508(5) 0.0485(16) Uani 1 1 d . . . H30 H -0.0515 0.3691 0.2964 0.073 Uiso 1 1 calc R . . H31 H -0.1070 0.3850 0.2010 0.073 Uiso 1 1 calc R . . H32 H 0.0175 0.4641 0.2920 0.073 Uiso 1 1 calc R . . Cl1 Cl 0.1533(4) 0.4721(3) 0.5188(2) 0.169(2) Uani 1 1 d . . . Cl2 Cl 0.2788(2) 0.32747(16) 0.51703(16) 0.0738(6) Uani 1 1 d . . . Cl3 Cl 0.0263(3) 0.2637(5) 0.4547(4) 0.212(3) Uani 1 1 d . . . C44 C 0.1475(9) 0.3401(9) 0.4540(7) 0.097(3) Uani 1 1 d . . . H33 H 0.1388 0.3176 0.3812 0.117 Uiso 1 1 calc R . . Cl4 Cl 0.4439(2) -0.02918(19) 0.32061(19) 0.0862(7) Uani 1 1 d . . . Cl5 Cl 0.6777(3) 0.0859(2) 0.4852(2) 0.1066(9) Uani 1 1 d . . . Cl6 Cl 0.5734(4) -0.1279(2) 0.4187(2) 0.1328(14) Uani 1 1 d . . . C45 C 0.5851(9) -0.0358(7) 0.3816(7) 0.079(2) Uani 1 1 d . . . H34 H 0.6239 -0.0569 0.3298 0.095 Uiso 1 1 calc R . . O6 O 0.3163(4) 0.1107(3) -0.2180(3) 0.0461(10) Uani 1 1 d . . . H35 H 0.3405 0.1628 -0.1589 0.069 Uiso 1 1 calc R . . C46 C 0.2065(8) 0.0520(7) -0.2398(7) 0.091(3) Uani 1 1 d . . . H36 H 0.2062 0.0452 -0.1803 0.136 Uiso 1 1 calc R . . H37 H 0.1871 -0.0163 -0.2997 0.136 Uiso 1 1 calc R . . H38 H 0.1469 0.0848 -0.2552 0.136 Uiso 1 1 calc R . . O7 O 0.1710(17) 0.1053(11) -0.4549(11) 0.105(5) Uani 0.50 1 d PU A -1 H39 H 0.2129 0.0658 -0.4594 0.158 Uiso 0.50 1 calc PR A -1 O8 O 0.019(2) -0.1598(17) -0.5988(19) 0.175(9) Uani 0.50 1 d P B -1 C47 C 0.049(3) 0.050(2) -0.4788(16) 0.123(9) Uani 0.50 1 d PU A -1 H40 H 0.0374 0.0645 -0.4147 0.185 Uiso 0.50 1 calc PR A -1 H41 H 0.0335 -0.0236 -0.5220 0.185 Uiso 0.50 1 calc PR A -1 H42 H -0.0067 0.0735 -0.5159 0.185 Uiso 0.50 1 calc PR A -1 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.0218(3) 0.0165(3) 0.0275(3) 0.0118(2) 0.0096(2) 0.0064(2) Zn2 0.0220(3) 0.0181(3) 0.0267(3) 0.0125(2) 0.0097(2) 0.0073(2) C1 0.026(3) 0.021(2) 0.030(2) 0.014(2) 0.014(2) 0.010(2) C2 0.023(2) 0.020(2) 0.032(2) 0.013(2) 0.016(2) 0.010(2) C3 0.030(3) 0.028(3) 0.031(3) 0.015(2) 0.013(2) 0.013(2) C4 0.039(3) 0.032(3) 0.040(3) 0.022(3) 0.019(3) 0.020(2) C5 0.041(3) 0.024(3) 0.051(3) 0.022(3) 0.020(3) 0.017(2) C6 0.036(3) 0.020(2) 0.033(3) 0.012(2) 0.014(2) 0.014(2) O1 0.0301(19) 0.0205(16) 0.0304(17) 0.0127(15) 0.0136(15) 0.0104(14) C7 0.058(4) 0.038(3) 0.054(4) 0.030(3) 0.014(3) 0.024(3) N1 0.027(2) 0.0180(18) 0.026(2) 0.0102(17) 0.0136(17) 0.0101(17) C8 0.028(3) 0.021(2) 0.024(2) 0.010(2) 0.014(2) 0.013(2) C9 0.023(3) 0.025(2) 0.028(2) 0.013(2) 0.007(2) 0.007(2) C10 0.026(3) 0.023(2) 0.028(2) 0.009(2) 0.009(2) 0.005(2) C11 0.030(3) 0.015(2) 0.026(2) 0.007(2) 0.011(2) 0.007(2) C12 0.028(3) 0.021(2) 0.024(2) 0.012(2) 0.014(2) 0.010(2) N2 0.022(2) 0.0153(18) 0.0245(19) 0.0093(16) 0.0109(16) 0.0069(16) C13 0.028(3) 0.022(2) 0.026(2) 0.013(2) 0.013(2) 0.009(2) C14 0.032(3) 0.017(2) 0.034(3) 0.012(2) 0.017(2) 0.008(2) C15 0.037(3) 0.020(2) 0.039(3) 0.017(2) 0.016(2) 0.013(2) C16 0.028(3) 0.026(2) 0.034(3) 0.017(2) 0.013(2) 0.010(2) C17 0.025(3) 0.023(2) 0.026(2) 0.017(2) 0.012(2) 0.009(2) C18 0.025(3) 0.023(2) 0.024(2) 0.015(2) 0.011(2) 0.010(2) C19 0.025(3) 0.024(2) 0.026(2) 0.013(2) 0.011(2) 0.010(2) C20 0.029(3) 0.026(2) 0.036(3) 0.021(2) 0.010(2) 0.010(2) C21 0.031(3) 0.033(3) 0.032(3) 0.020(2) 0.009(2) 0.013(2) C22 0.029(3) 0.027(2) 0.028(2) 0.014(2) 0.009(2) 0.007(2) C23 0.026(3) 0.023(2) 0.027(2) 0.013(2) 0.011(2) 0.008(2) O2 0.0223(17) 0.0230(16) 0.0326(18) 0.0193(15) 0.0062(14) 0.0055(14) C24 0.034(3) 0.041(3) 0.047(3) 0.028(3) 0.001(3) 0.011(3) N3 0.027(2) 0.0198(19) 0.027(2) 0.0120(17) 0.0137(17) 0.0098(17) C25 0.024(3) 0.023(2) 0.025(2) 0.011(2) 0.008(2) 0.005(2) C26 0.037(3) 0.028(3) 0.030(3) 0.014(2) 0.009(2) 0.007(2) C27 0.036(3) 0.025(3) 0.031(3) 0.010(2) 0.003(2) 0.000(2) C28 0.034(3) 0.024(2) 0.041(3) 0.017(2) 0.016(2) 0.009(2) C29 0.024(3) 0.020(2) 0.030(2) 0.013(2) 0.013(2) 0.006(2) N4 0.023(2) 0.0181(19) 0.029(2) 0.0127(17) 0.0120(17) 0.0062(16) C30 0.024(3) 0.023(2) 0.034(3) 0.018(2) 0.016(2) 0.009(2) C31 0.031(3) 0.019(2) 0.036(3) 0.013(2) 0.015(2) 0.007(2) C32 0.038(3) 0.022(2) 0.048(3) 0.022(2) 0.023(3) 0.015(2) C33 0.032(3) 0.031(3) 0.041(3) 0.025(2) 0.015(2) 0.015(2) C34 0.030(3) 0.026(2) 0.030(2) 0.018(2) 0.019(2) 0.012(2) C35 0.022(2) 0.026(2) 0.030(2) 0.016(2) 0.014(2) 0.011(2) C36 0.023(3) 0.030(3) 0.027(2) 0.016(2) 0.010(2) 0.013(2) C37 0.036(3) 0.032(3) 0.035(3) 0.019(2) 0.016(2) 0.018(2) C38 0.042(3) 0.039(3) 0.031(3) 0.018(3) 0.016(2) 0.022(3) C39 0.030(3) 0.034(3) 0.026(2) 0.012(2) 0.006(2) 0.012(2) C40 0.030(3) 0.027(3) 0.033(3) 0.015(2) 0.013(2) 0.009(2) O3 0.0273(18) 0.0229(16) 0.0257(17) 0.0149(15) 0.0070(14) 0.0059(14) C41 0.052(4) 0.046(3) 0.039(3) 0.021(3) 0.008(3) 0.021(3) O4 0.0287(19) 0.0290(18) 0.040(2) 0.0185(17) 0.0169(16) 0.0159(16) O5 0.041(2) 0.0263(18) 0.040(2) 0.0166(17) 0.0146(17) 0.0155(17) C42 0.028(3) 0.018(2) 0.042(3) 0.018(2) 0.015(2) 0.007(2) C43 0.058(4) 0.059(4) 0.062(4) 0.043(4) 0.038(3) 0.036(3) Cl1 0.162(3) 0.160(3) 0.0691(16) -0.0197(18) -0.0187(18) 0.113(3) Cl2 0.0689(13) 0.0689(12) 0.0681(12) 0.0233(10) 0.0277(10) 0.0145(10) Cl3 0.0553(19) 0.348(8) 0.176(4) 0.125(5) 0.014(2) -0.003(3) C44 0.086(7) 0.126(9) 0.055(5) 0.032(6) 0.016(5) 0.032(7) Cl4 0.0810(16) 0.0790(14) 0.0878(15) 0.0331(13) 0.0291(12) 0.0314(12) Cl5 0.131(2) 0.0796(16) 0.0739(15) 0.0251(13) 0.0131(15) 0.0321(16) Cl6 0.250(5) 0.0884(18) 0.100(2) 0.0599(17) 0.091(3) 0.071(2) C45 0.096(7) 0.080(6) 0.068(5) 0.038(5) 0.034(5) 0.038(5) O6 0.061(3) 0.028(2) 0.036(2) 0.0071(18) 0.021(2) 0.005(2) C46 0.071(6) 0.078(6) 0.070(5) 0.003(5) 0.031(5) -0.014(5) O7 0.171(15) 0.097(9) 0.067(7) 0.050(7) 0.046(9) 0.063(10) O8 0.139(17) 0.149(17) 0.19(2) 0.059(16) 0.084(16) -0.018(14) C47 0.15(2) 0.144(19) 0.069(12) 0.073(14) 0.011(12) 0.018(15) _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 Zn1 O2 1.965(3) . ? Zn1 O1 1.987(3) . ? Zn1 N1 2.040(4) . ? Zn1 O3 2.042(3) . ? Zn1 N2 2.131(4) . ? Zn1 Zn2 3.0763(7) . ? Zn2 O4 1.962(3) . ? Zn2 O3 1.980(3) . ? Zn2 N4 2.066(4) . ? Zn2 O2 2.083(3) . ? Zn2 N3 2.089(4) . ? C1 O1 1.342(6) . ? C1 C2 1.402(7) . ? C1 C6 1.413(6) . ? C2 C3 1.404(7) . ? C2 C8 1.483(6) . ? C3 C4 1.380(7) . ? C3 H1 0.9500 . ? C4 C5 1.374(8) . ? C4 C7 1.523(7) . ? C5 C6 1.392(7) . ? C5 H2 0.9500 . ? C6 H3 0.9500 . ? C7 H4 0.9800 . ? C7 H5 0.9800 . ? C7 H6 0.9800 . ? N1 C8 1.345(6) . ? N1 C12 1.350(6) . ? C8 C9 1.397(7) . ? C9 C10 1.384(7) . ? C9 H7 0.9500 . ? C10 C11 1.391(7) . ? C10 H8 0.9500 . ? C11 C12 1.373(7) . ? C11 H9 0.9500 . ? C12 C13 1.498(7) . ? N2 C13 1.355(6) . ? N2 C17 1.360(6) . ? C13 C14 1.390(6) . ? C14 C15 1.380(7) . ? C14 H10 0.9500 . ? C15 C16 1.370(7) . ? C15 H11 0.9500 . ? C16 C17 1.410(6) . ? C16 H12 0.9500 . ? C17 C19 1.501(7) . ? C18 O2 1.318(5) . ? C18 C23 1.417(7) . ? C18 C19 1.424(6) . ? C19 C20 1.406(7) . ? C20 C21 1.371(7) . ? C20 H13 0.9500 . ? C21 C22 1.396(7) . ? C21 C24 1.527(7) . ? C22 C23 1.388(7) . ? C22 H14 0.9500 . ? C23 C25 1.503(6) . ? C24 H15 0.9800 . ? C24 H16 0.9800 . ? C24 H17 0.9800 . ? N3 C25 1.351(6) . ? N3 C29 1.355(6) . ? C25 C26 1.387(7) . ? C26 C27 1.372(7) . ? C26 H18 0.9500 . ? C27 C28 1.395(7) . ? C27 H19 0.9500 . ? C28 C29 1.369(7) . ? C28 H20 0.9500 . ? C29 C30 1.503(7) . ? N4 C30 1.345(6) . ? N4 C34 1.354(6) . ? C30 C31 1.378(7) . ? C31 C32 1.389(7) . ? C31 H21 0.9500 . ? C32 C33 1.380(8) . ? C32 H22 0.9500 . ? C33 C34 1.409(7) . ? C33 H23 0.9500 . ? C34 C36 1.472(7) . ? C35 O3 1.345(6) . ? C35 C40 1.389(7) . ? C35 C36 1.421(6) . ? C36 C37 1.419(7) . ? C37 C38 1.373(8) . ? C37 H24 0.9500 . ? C38 C39 1.397(7) . ? C38 C41 1.515(7) . ? C39 C40 1.379(7) . ? C39 H25 0.9500 . ? C40 H26 0.9500 . ? C41 H27 0.9800 . ? C41 H28 0.9800 . ? C41 H29 0.9800 . ? O4 C42 1.272(6) . ? O5 C42 1.241(6) . ? C42 C43 1.498(8) . ? C43 H30 0.9800 . ? C43 H31 0.9800 . ? C43 H32 0.9800 . ? Cl1 C44 1.788(12) . ? Cl2 C44 1.731(10) . ? Cl3 C44 1.743(12) . ? C44 H33 1.0000 . ? Cl4 C45 1.775(10) . ? Cl5 C45 1.753(10) . ? Cl6 C45 1.740(9) . ? C45 H34 1.0000 . ? O6 C46 1.354(9) . ? O6 H35 0.8400 . ? C46 H36 0.9800 . ? C46 H37 0.9800 . ? C46 H38 0.9800 . ? O7 C47 1.45(3) . ? O7 H39 0.8400 . ? C47 H40 0.9800 . ? C47 H41 0.9800 . ? C47 H42 0.9800 . ? 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 Zn1 O1 104.24(14) . . ? O2 Zn1 N1 165.93(14) . . ? O1 Zn1 N1 87.95(14) . . ? O2 Zn1 O3 80.80(13) . . ? O1 Zn1 O3 100.25(13) . . ? N1 Zn1 O3 104.23(14) . . ? O2 Zn1 N2 86.05(14) . . ? O1 Zn1 N2 138.31(13) . . ? N1 Zn1 N2 80.12(15) . . ? O3 Zn1 N2 121.37(14) . . ? O2 Zn1 Zn2 41.98(9) . . ? O1 Zn1 Zn2 100.91(9) . . ? N1 Zn1 Zn2 143.35(11) . . ? O3 Zn1 Zn2 39.37(9) . . ? N2 Zn1 Zn2 112.43(10) . . ? O4 Zn2 O3 108.13(14) . . ? O4 Zn2 N4 130.28(14) . . ? O3 Zn2 N4 89.01(14) . . ? O4 Zn2 O2 105.22(13) . . ? O3 Zn2 O2 79.45(13) . . ? N4 Zn2 O2 123.96(14) . . ? O4 Zn2 N3 105.76(15) . . ? O3 Zn2 N3 143.37(14) . . ? N4 Zn2 N3 79.46(15) . . ? O2 Zn2 N3 78.65(13) . . ? O4 Zn2 Zn1 116.91(10) . . ? O3 Zn2 Zn1 40.87(9) . . ? N4 Zn2 Zn1 106.56(11) . . ? O2 Zn2 Zn1 39.12(9) . . ? N3 Zn2 Zn1 109.72(11) . . ? O1 C1 C2 124.0(4) . . ? O1 C1 C6 118.6(4) . . ? C2 C1 C6 117.4(4) . . ? C1 C2 C3 119.4(4) . . ? C1 C2 C8 122.6(4) . . ? C3 C2 C8 118.0(4) . . ? C4 C3 C2 122.6(5) . . ? C4 C3 H1 118.7 . . ? C2 C3 H1 118.7 . . ? C5 C4 C3 117.7(5) . . ? C5 C4 C7 121.3(5) . . ? C3 C4 C7 121.0(5) . . ? C4 C5 C6 121.5(5) . . ? C4 C5 H2 119.2 . . ? C6 C5 H2 119.2 . . ? C5 C6 C1 121.0(5) . . ? C5 C6 H3 119.5 . . ? C1 C6 H3 119.5 . . ? C1 O1 Zn1 112.7(3) . . ? C4 C7 H4 109.5 . . ? C4 C7 H5 109.5 . . ? H4 C7 H5 109.5 . . ? C4 C7 H6 109.5 . . ? H4 C7 H6 109.5 . . ? H5 C7 H6 109.5 . . ? C8 N1 C12 121.6(4) . . ? C8 N1 Zn1 122.4(3) . . ? C12 N1 Zn1 116.0(3) . . ? N1 C8 C9 119.4(4) . . ? N1 C8 C2 118.8(4) . . ? C9 C8 C2 121.8(4) . . ? C10 C9 C8 119.5(4) . . ? C10 C9 H7 120.3 . . ? C8 C9 H7 120.3 . . ? C9 C10 C11 119.9(5) . . ? C9 C10 H8 120.1 . . ? C11 C10 H8 120.1 . . ? C12 C11 C10 118.6(4) . . ? C12 C11 H9 120.7 . . ? C10 C11 H9 120.7 . . ? N1 C12 C11 121.1(4) . . ? N1 C12 C13 114.9(4) . . ? C11 C12 C13 124.0(4) . . ? C13 N2 C17 120.0(4) . . ? C13 N2 Zn1 111.4(3) . . ? C17 N2 Zn1 128.1(3) . . ? N2 C13 C14 122.3(4) . . ? N2 C13 C12 117.0(4) . . ? C14 C13 C12 120.7(4) . . ? C15 C14 C13 118.2(5) . . ? C15 C14 H10 120.9 . . ? C13 C14 H10 120.9 . . ? C16 C15 C14 119.9(4) . . ? C16 C15 H11 120.0 . . ? C14 C15 H11 120.0 . . ? C15 C16 C17 120.7(5) . . ? C15 C16 H12 119.7 . . ? C17 C16 H12 119.7 . . ? N2 C17 C16 118.9(4) . . ? N2 C17 C19 121.5(4) . . ? C16 C17 C19 119.5(4) . . ? O2 C18 C23 119.3(4) . . ? O2 C18 C19 122.1(4) . . ? C23 C18 C19 118.6(4) . . ? C20 C19 C18 118.1(4) . . ? C20 C19 C17 117.7(4) . . ? C18 C19 C17 124.2(4) . . ? C21 C20 C19 123.4(4) . . ? C21 C20 H13 118.3 . . ? C19 C20 H13 118.3 . . ? C20 C21 C22 118.0(4) . . ? C20 C21 C24 121.1(4) . . ? C22 C21 C24 120.9(5) . . ? C23 C22 C21 121.6(5) . . ? C23 C22 H14 119.2 . . ? C21 C22 H14 119.2 . . ? C22 C23 C18 120.3(4) . . ? C22 C23 C25 118.1(4) . . ? C18 C23 C25 121.5(4) . . ? C18 O2 Zn1 135.6(3) . . ? C18 O2 Zn2 116.6(3) . . ? Zn1 O2 Zn2 98.90(13) . . ? C21 C24 H15 109.5 . . ? C21 C24 H16 109.5 . . ? H15 C24 H16 109.5 . . ? C21 C24 H17 109.5 . . ? H15 C24 H17 109.5 . . ? H16 C24 H17 109.5 . . ? C25 N3 C29 120.2(4) . . ? C25 N3 Zn2 125.6(3) . . ? C29 N3 Zn2 114.2(3) . . ? N3 C25 C26 119.3(4) . . ? N3 C25 C23 118.7(4) . . ? C26 C25 C23 121.9(4) . . ? C27 C26 C25 120.5(5) . . ? C27 C26 H18 119.7 . . ? C25 C26 H18 119.7 . . ? C26 C27 C28 119.5(5) . . ? C26 C27 H19 120.3 . . ? C28 C27 H19 120.3 . . ? C29 C28 C27 118.0(5) . . ? C29 C28 H20 121.0 . . ? C27 C28 H20 121.0 . . ? N3 C29 C28 122.0(4) . . ? N3 C29 C30 114.1(4) . . ? C28 C29 C30 123.6(4) . . ? C30 N4 C34 120.6(4) . . ? C30 N4 Zn2 114.6(3) . . ? C34 N4 Zn2 124.5(3) . . ? N4 C30 C31 122.2(4) . . ? N4 C30 C29 116.2(4) . . ? C31 C30 C29 121.3(4) . . ? C30 C31 C32 118.7(5) . . ? C30 C31 H21 120.6 . . ? C32 C31 H21 120.6 . . ? C33 C32 C31 119.0(4) . . ? C33 C32 H22 120.5 . . ? C31 C32 H22 120.5 . . ? C32 C33 C34 120.5(5) . . ? C32 C33 H23 119.7 . . ? C34 C33 H23 119.7 . . ? N4 C34 C33 118.9(5) . . ? N4 C34 C36 120.4(4) . . ? C33 C34 C36 120.7(4) . . ? O3 C35 C40 118.8(4) . . ? O3 C35 C36 122.6(4) . . ? C40 C35 C36 118.6(4) . . ? C37 C36 C35 117.4(5) . . ? C37 C36 C34 117.8(4) . . ? C35 C36 C34 124.6(4) . . ? C38 C37 C36 123.2(5) . . ? C38 C37 H24 118.4 . . ? C36 C37 H24 118.4 . . ? C37 C38 C39 118.1(5) . . ? C37 C38 C41 121.1(5) . . ? C39 C38 C41 120.9(5) . . ? C40 C39 C38 120.4(5) . . ? C40 C39 H25 119.8 . . ? C38 C39 H25 119.8 . . ? C39 C40 C35 122.3(5) . . ? C39 C40 H26 118.9 . . ? C35 C40 H26 118.9 . . ? C35 O3 Zn2 121.5(3) . . ? C35 O3 Zn1 134.4(3) . . ? Zn2 O3 Zn1 99.76(14) . . ? C38 C41 H27 109.5 . . ? C38 C41 H28 109.5 . . ? H27 C41 H28 109.5 . . ? C38 C41 H29 109.5 . . ? H27 C41 H29 109.5 . . ? H28 C41 H29 109.5 . . ? C42 O4 Zn2 113.2(3) . . ? O5 C42 O4 123.1(5) . . ? O5 C42 C43 120.7(5) . . ? O4 C42 C43 116.2(4) . . ? C42 C43 H30 109.5 . . ? C42 C43 H31 109.5 . . ? H30 C43 H31 109.5 . . ? C42 C43 H32 109.5 . . ? H30 C43 H32 109.5 . . ? H31 C43 H32 109.5 . . ? Cl2 C44 Cl3 109.4(6) . . ? Cl2 C44 Cl1 109.0(5) . . ? Cl3 C44 Cl1 110.0(7) . . ? Cl2 C44 H33 109.5 . . ? Cl3 C44 H33 109.5 . . ? Cl1 C44 H33 109.5 . . ? Cl6 C45 Cl5 111.8(5) . . ? Cl6 C45 Cl4 112.8(6) . . ? Cl5 C45 Cl4 110.6(5) . . ? Cl6 C45 H34 107.1 . . ? Cl5 C45 H34 107.1 . . ? Cl4 C45 H34 107.1 . . ? C46 O6 H35 109.5 . . ? O6 C46 H36 109.5 . . ? O6 C46 H37 109.5 . . ? H36 C46 H37 109.5 . . ? O6 C46 H38 109.5 . . ? H36 C46 H38 109.5 . . ? H37 C46 H38 109.5 . . ? 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 Zn1 Zn2 O4 -80.93(18) . . . . ? O1 Zn1 Zn2 O4 179.84(15) . . . . ? N1 Zn1 Zn2 O4 78.4(2) . . . . ? O3 Zn1 Zn2 O4 86.94(19) . . . . ? N2 Zn1 Zn2 O4 -25.69(16) . . . . ? O2 Zn1 Zn2 O3 -167.9(2) . . . . ? O1 Zn1 Zn2 O3 92.90(17) . . . . ? N1 Zn1 Zn2 O3 -8.5(2) . . . . ? N2 Zn1 Zn2 O3 -112.63(18) . . . . ? O2 Zn1 Zn2 N4 123.92(18) . . . . ? O1 Zn1 Zn2 N4 24.69(15) . . . . ? N1 Zn1 Zn2 N4 -76.7(2) . . . . ? O3 Zn1 Zn2 N4 -68.21(18) . . . . ? N2 Zn1 Zn2 N4 179.16(15) . . . . ? O1 Zn1 Zn2 O2 -99.23(17) . . . . ? N1 Zn1 Zn2 O2 159.3(2) . . . . ? O3 Zn1 Zn2 O2 167.9(2) . . . . ? N2 Zn1 Zn2 O2 55.24(18) . . . . ? O2 Zn1 Zn2 N3 39.44(18) . . . . ? O1 Zn1 Zn2 N3 -59.79(15) . . . . ? N1 Zn1 Zn2 N3 -161.2(2) . . . . ? O3 Zn1 Zn2 N3 -152.69(18) . . . . ? N2 Zn1 Zn2 N3 94.68(16) . . . . ? O1 C1 C2 C3 174.2(4) . . . . ? C6 C1 C2 C3 -6.3(7) . . . . ? O1 C1 C2 C8 -4.8(7) . . . . ? C6 C1 C2 C8 174.7(4) . . . . ? C1 C2 C3 C4 2.7(7) . . . . ? C8 C2 C3 C4 -178.2(5) . . . . ? C2 C3 C4 C5 2.4(8) . . . . ? C2 C3 C4 C7 -177.3(5) . . . . ? C3 C4 C5 C6 -3.6(8) . . . . ? C7 C4 C5 C6 176.1(5) . . . . ? C4 C5 C6 C1 -0.2(8) . . . . ? O1 C1 C6 C5 -175.3(5) . . . . ? C2 C1 C6 C5 5.2(7) . . . . ? C2 C1 O1 Zn1 -45.9(5) . . . . ? C6 C1 O1 Zn1 134.6(4) . . . . ? O2 Zn1 O1 C1 -131.5(3) . . . . ? N1 Zn1 O1 C1 55.6(3) . . . . ? O3 Zn1 O1 C1 -48.5(3) . . . . ? N2 Zn1 O1 C1 128.3(3) . . . . ? Zn2 Zn1 O1 C1 -88.5(3) . . . . ? O2 Zn1 N1 C8 175.0(5) . . . . ? O1 Zn1 N1 C8 -34.5(3) . . . . ? O3 Zn1 N1 C8 65.6(4) . . . . ? N2 Zn1 N1 C8 -174.4(4) . . . . ? Zn2 Zn1 N1 C8 71.1(4) . . . . ? O2 Zn1 N1 C12 -8.0(8) . . . . ? O1 Zn1 N1 C12 142.5(3) . . . . ? O3 Zn1 N1 C12 -117.4(3) . . . . ? N2 Zn1 N1 C12 2.6(3) . . . . ? Zn2 Zn1 N1 C12 -111.8(3) . . . . ? C12 N1 C8 C9 1.1(6) . . . . ? Zn1 N1 C8 C9 178.0(3) . . . . ? C12 N1 C8 C2 -178.2(4) . . . . ? Zn1 N1 C8 C2 -1.4(6) . . . . ? C1 C2 C8 N1 31.6(6) . . . . ? C3 C2 C8 N1 -147.5(4) . . . . ? C1 C2 C8 C9 -147.7(5) . . . . ? C3 C2 C8 C9 33.2(6) . . . . ? N1 C8 C9 C10 0.0(7) . . . . ? C2 C8 C9 C10 179.3(4) . . . . ? C8 C9 C10 C11 -0.9(7) . . . . ? C9 C10 C11 C12 0.8(7) . . . . ? C8 N1 C12 C11 -1.2(7) . . . . ? Zn1 N1 C12 C11 -178.3(3) . . . . ? C8 N1 C12 C13 178.2(4) . . . . ? Zn1 N1 C12 C13 1.1(5) . . . . ? C10 C11 C12 N1 0.3(7) . . . . ? C10 C11 C12 C13 -179.1(4) . . . . ? O2 Zn1 N2 C13 171.2(3) . . . . ? O1 Zn1 N2 C13 -81.7(4) . . . . ? N1 Zn1 N2 C13 -6.2(3) . . . . ? O3 Zn1 N2 C13 94.5(3) . . . . ? Zn2 Zn1 N2 C13 137.8(3) . . . . ? O2 Zn1 N2 C17 -0.3(4) . . . . ? O1 Zn1 N2 C17 106.7(4) . . . . ? N1 Zn1 N2 C17 -177.8(4) . . . . ? O3 Zn1 N2 C17 -77.1(4) . . . . ? Zn2 Zn1 N2 C17 -33.8(4) . . . . ? C17 N2 C13 C14 1.3(7) . . . . ? Zn1 N2 C13 C14 -171.1(4) . . . . ? C17 N2 C13 C12 -178.9(4) . . . . ? Zn1 N2 C13 C12 8.7(5) . . . . ? N1 C12 C13 N2 -6.9(6) . . . . ? C11 C12 C13 N2 172.5(4) . . . . ? N1 C12 C13 C14 172.9(4) . . . . ? C11 C12 C13 C14 -7.7(7) . . . . ? N2 C13 C14 C15 0.2(7) . . . . ? C12 C13 C14 C15 -179.6(4) . . . . ? C13 C14 C15 C16 -0.7(7) . . . . ? C14 C15 C16 C17 -0.2(7) . . . . ? C13 N2 C17 C16 -2.2(6) . . . . ? Zn1 N2 C17 C16 168.7(3) . . . . ? C13 N2 C17 C19 177.8(4) . . . . ? Zn1 N2 C17 C19 -11.3(6) . . . . ? C15 C16 C17 N2 1.7(7) . . . . ? C15 C16 C17 C19 -178.3(4) . . . . ? O2 C18 C19 C20 179.1(4) . . . . ? C23 C18 C19 C20 -0.1(7) . . . . ? O2 C18 C19 C17 -3.7(7) . . . . ? C23 C18 C19 C17 177.1(4) . . . . ? N2 C17 C19 C20 -167.6(4) . . . . ? C16 C17 C19 C20 12.4(6) . . . . ? N2 C17 C19 C18 15.2(7) . . . . ? C16 C17 C19 C18 -164.8(4) . . . . ? C18 C19 C20 C21 -0.5(7) . . . . ? C17 C19 C20 C21 -177.9(5) . . . . ? C19 C20 C21 C22 0.4(8) . . . . ? C19 C20 C21 C24 178.8(5) . . . . ? C20 C21 C22 C23 0.5(7) . . . . ? C24 C21 C22 C23 -177.9(5) . . . . ? C21 C22 C23 C18 -1.1(7) . . . . ? C21 C22 C23 C25 -177.8(4) . . . . ? O2 C18 C23 C22 -178.3(4) . . . . ? C19 C18 C23 C22 0.9(7) . . . . ? O2 C18 C23 C25 -1.8(7) . . . . ? C19 C18 C23 C25 177.4(4) . . . . ? C23 C18 O2 Zn1 166.0(3) . . . . ? C19 C18 O2 Zn1 -13.1(7) . . . . ? C23 C18 O2 Zn2 -54.6(5) . . . . ? C19 C18 O2 Zn2 126.2(4) . . . . ? O1 Zn1 O2 C18 -125.6(4) . . . . ? N1 Zn1 O2 C18 23.9(8) . . . . ? O3 Zn1 O2 C18 136.1(4) . . . . ? N2 Zn1 O2 C18 13.4(4) . . . . ? Zn2 Zn1 O2 C18 143.9(5) . . . . ? O1 Zn1 O2 Zn2 90.56(15) . . . . ? N1 Zn1 O2 Zn2 -119.9(5) . . . . ? O3 Zn1 O2 Zn2 -7.76(13) . . . . ? N2 Zn1 O2 Zn2 -130.43(15) . . . . ? O4 Zn2 O2 C18 -38.4(3) . . . . ? O3 Zn2 O2 C18 -144.5(3) . . . . ? N4 Zn2 O2 C18 134.0(3) . . . . ? N3 Zn2 O2 C18 65.1(3) . . . . ? Zn1 Zn2 O2 C18 -152.5(4) . . . . ? O4 Zn2 O2 Zn1 114.14(15) . . . . ? O3 Zn2 O2 Zn1 8.04(13) . . . . ? N4 Zn2 O2 Zn1 -73.53(19) . . . . ? N3 Zn2 O2 Zn1 -142.41(16) . . . . ? O4 Zn2 N3 C25 60.7(4) . . . . ? O3 Zn2 N3 C25 -96.5(4) . . . . ? N4 Zn2 N3 C25 -170.2(4) . . . . ? O2 Zn2 N3 C25 -42.1(4) . . . . ? Zn1 Zn2 N3 C25 -66.2(4) . . . . ? O4 Zn2 N3 C29 -118.5(3) . . . . ? O3 Zn2 N3 C29 84.4(4) . . . . ? N4 Zn2 N3 C29 10.6(3) . . . . ? O2 Zn2 N3 C29 138.7(3) . . . . ? Zn1 Zn2 N3 C29 114.6(3) . . . . ? C29 N3 C25 C26 3.8(7) . . . . ? Zn2 N3 C25 C26 -175.3(4) . . . . ? C29 N3 C25 C23 -172.5(4) . . . . ? Zn2 N3 C25 C23 8.4(6) . . . . ? C22 C23 C25 N3 -156.7(4) . . . . ? C18 C23 C25 N3 26.7(7) . . . . ? C22 C23 C25 C26 27.0(7) . . . . ? C18 C23 C25 C26 -149.6(5) . . . . ? N3 C25 C26 C27 1.5(8) . . . . ? C23 C25 C26 C27 177.7(5) . . . . ? C25 C26 C27 C28 -4.2(8) . . . . ? C26 C27 C28 C29 1.6(8) . . . . ? C25 N3 C29 C28 -6.6(7) . . . . ? Zn2 N3 C29 C28 172.6(4) . . . . ? C25 N3 C29 C30 168.1(4) . . . . ? Zn2 N3 C29 C30 -12.7(5) . . . . ? C27 C28 C29 N3 3.8(7) . . . . ? C27 C28 C29 C30 -170.4(5) . . . . ? O4 Zn2 N4 C30 95.4(3) . . . . ? O3 Zn2 N4 C30 -151.5(3) . . . . ? O2 Zn2 N4 C30 -74.9(3) . . . . ? N3 Zn2 N4 C30 -6.4(3) . . . . ? Zn1 Zn2 N4 C30 -114.1(3) . . . . ? O4 Zn2 N4 C34 -90.7(4) . . . . ? O3 Zn2 N4 C34 22.5(4) . . . . ? O2 Zn2 N4 C34 99.0(4) . . . . ? N3 Zn2 N4 C34 167.5(4) . . . . ? Zn1 Zn2 N4 C34 59.9(4) . . . . ? C34 N4 C30 C31 1.3(7) . . . . ? Zn2 N4 C30 C31 175.5(4) . . . . ? C34 N4 C30 C29 -172.5(4) . . . . ? Zn2 N4 C30 C29 1.7(5) . . . . ? N3 C29 C30 N4 7.4(6) . . . . ? C28 C29 C30 N4 -178.0(4) . . . . ? N3 C29 C30 C31 -166.5(4) . . . . ? C28 C29 C30 C31 8.2(7) . . . . ? N4 C30 C31 C32 -1.7(7) . . . . ? C29 C30 C31 C32 171.8(4) . . . . ? C30 C31 C32 C33 0.2(7) . . . . ? C31 C32 C33 C34 1.6(7) . . . . ? C30 N4 C34 C33 0.6(6) . . . . ? Zn2 N4 C34 C33 -173.1(3) . . . . ? C30 N4 C34 C36 178.9(4) . . . . ? Zn2 N4 C34 C36 5.3(6) . . . . ? C32 C33 C34 N4 -2.0(7) . . . . ? C32 C33 C34 C36 179.6(4) . . . . ? O3 C35 C36 C37 -178.0(4) . . . . ? C40 C35 C36 C37 2.0(7) . . . . ? O3 C35 C36 C34 5.7(7) . . . . ? C40 C35 C36 C34 -174.3(4) . . . . ? N4 C34 C36 C37 156.3(4) . . . . ? C33 C34 C36 C37 -25.3(7) . . . . ? N4 C34 C36 C35 -27.3(7) . . . . ? C33 C34 C36 C35 151.0(5) . . . . ? C35 C36 C37 C38 -1.9(8) . . . . ? C34 C36 C37 C38 174.7(5) . . . . ? C36 C37 C38 C39 0.5(8) . . . . ? C36 C37 C38 C41 -179.4(5) . . . . ? C37 C38 C39 C40 0.9(8) . . . . ? C41 C38 C39 C40 -179.2(5) . . . . ? C38 C39 C40 C35 -0.7(8) . . . . ? O3 C35 C40 C39 179.2(5) . . . . ? C36 C35 C40 C39 -0.8(7) . . . . ? C40 C35 O3 Zn2 -144.3(4) . . . . ? C36 C35 O3 Zn2 35.7(6) . . . . ? C40 C35 O3 Zn1 64.4(6) . . . . ? C36 C35 O3 Zn1 -115.6(5) . . . . ? O4 Zn2 O3 C35 89.9(3) . . . . ? N4 Zn2 O3 C35 -42.5(3) . . . . ? O2 Zn2 O3 C35 -167.4(4) . . . . ? N3 Zn2 O3 C35 -113.3(4) . . . . ? Zn1 Zn2 O3 C35 -159.6(4) . . . . ? O4 Zn2 O3 Zn1 -110.46(15) . . . . ? N4 Zn2 O3 Zn1 117.11(15) . . . . ? O2 Zn2 O3 Zn1 -7.75(13) . . . . ? N3 Zn2 O3 Zn1 46.4(3) . . . . ? O2 Zn1 O3 C35 163.6(4) . . . . ? O1 Zn1 O3 C35 60.7(4) . . . . ? N1 Zn1 O3 C35 -29.8(4) . . . . ? N2 Zn1 O3 C35 -116.8(4) . . . . ? Zn2 Zn1 O3 C35 155.5(5) . . . . ? O2 Zn1 O3 Zn2 8.19(13) . . . . ? O1 Zn1 O3 Zn2 -94.76(15) . . . . ? N1 Zn1 O3 Zn2 174.76(13) . . . . ? N2 Zn1 O3 Zn2 87.79(18) . . . . ? O3 Zn2 O4 C42 -66.9(3) . . . . ? N4 Zn2 O4 C42 37.8(4) . . . . ? O2 Zn2 O4 C42 -150.6(3) . . . . ? N3 Zn2 O4 C42 127.2(3) . . . . ? Zn1 Zn2 O4 C42 -110.4(3) . . . . ? Zn2 O4 C42 O5 -7.8(6) . . . . ? Zn2 O4 C42 C43 173.5(4) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 2.020 _refine_diff_density_min -1.340 _refine_diff_density_rms 0.131 _database_code_depnum_ccdc_archive 'CCDC 938299' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_(L1)2Ni4 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common '[L2Ni4](OAc)2(MeOH)6.5(H2O)4' _chemical_melting_point ? _chemical_formula_moiety C92.50H98N8Ni4O20.50 _chemical_formula_sum 'C92.50 H98 N8 Ni4 O20.50' _chemical_formula_weight 1884.63 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 14.7737(15) _cell_length_b 30.598(3) _cell_length_c 21.7741(19) _cell_angle_alpha 90.00 _cell_angle_beta 107.842(3) _cell_angle_gamma 90.00 _cell_volume 9369.6(15) _cell_formula_units_Z 4 _cell_measurement_temperature 120 _cell_measurement_reflns_used 72452 _cell_measurement_theta_min 3.03 _cell_measurement_theta_max 25.00 _exptl_crystal_description prismatic _exptl_crystal_colour red _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.336 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3940 _exptl_absorpt_coefficient_mu 0.864 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6253 _exptl_absorpt_correction_T_max 0.9186 _exptl_absorpt_process_details 'Rapid AUTO (Rigaku Corp.)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120 _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku R-AXIS Rapid' _diffrn_measurement_method IP _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 72452 _diffrn_reflns_av_R_equivalents 0.2035 _diffrn_reflns_av_sigmaI/netI 0.1840 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -36 _diffrn_reflns_limit_k_max 36 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 3.03 _diffrn_reflns_theta_max 25.00 _reflns_number_total 16465 _reflns_number_gt 5473 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Rapid AUTO (Rigaku Corp.)' _computing_cell_refinement 'Rapid AUTO (Rigaku Corp.)' _computing_data_reduction 'Rapid AUTO (Rigaku Corp.)' _computing_structure_solution 'DIRDIF99 (Beurskens et al., 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ORTEP-3 _computing_publication_material ORTEP-3 _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^)+(0.0563P)^2^+6.1294P] 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 16465 _refine_ls_number_parameters 1474 _refine_ls_number_restraints 509 _refine_ls_R_factor_all 0.2413 _refine_ls_R_factor_gt 0.0897 _refine_ls_wR_factor_ref 0.2334 _refine_ls_wR_factor_gt 0.1797 _refine_ls_goodness_of_fit_ref 1.072 _refine_ls_restrained_S_all 1.081 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni1 Ni -0.06744(10) 0.31433(4) 0.60551(5) 0.0786(4) Uani 1 1 d . . . Ni2 Ni -0.07737(11) 0.24226(3) 0.51370(5) 0.0819(5) Uani 1 1 d . . . Ni3 Ni 0.05249(10) 0.26963(3) 0.43389(5) 0.0801(4) Uani 1 1 d . . . Ni4 Ni 0.04219(10) 0.19684(3) 0.34253(5) 0.0750(4) Uani 1 1 d . . . C1 C -0.2536(9) 0.3058(4) 0.5264(4) 0.083(3) Uani 1 1 d . . . C2 C -0.2750(9) 0.3506(4) 0.5281(4) 0.091(3) Uani 1 1 d . . . C3 C -0.3691(12) 0.3644(4) 0.4976(7) 0.140(5) Uani 1 1 d . . . H1 H -0.3824 0.3946 0.5000 0.168 Uiso 1 1 calc R . . C4 C -0.4427(12) 0.3382(7) 0.4650(8) 0.165(7) Uani 1 1 d . . . C5 C -0.4224(12) 0.2944(6) 0.4649(6) 0.131(5) Uani 1 1 d . . . H2 H -0.4723 0.2748 0.4442 0.157 Uiso 1 1 calc R . . C6 C -0.3322(12) 0.2775(4) 0.4937(5) 0.107(4) Uani 1 1 d . . . H3 H -0.3218 0.2470 0.4920 0.128 Uiso 1 1 calc R . . O1 O -0.1693(6) 0.2874(2) 0.5508(3) 0.079(2) Uani 1 1 d . . . C7 C -0.5438(11) 0.3549(5) 0.4369(9) 0.252(11) Uani 1 1 d . . . H4 H -0.5512 0.3821 0.4585 0.378 Uiso 1 1 calc R . . H5 H -0.5884 0.3329 0.4433 0.378 Uiso 1 1 calc R . . H6 H -0.5569 0.3603 0.3906 0.378 Uiso 1 1 calc R . . N1 N -0.1158(7) 0.3699(2) 0.5967(3) 0.073(2) Uani 1 1 d . . . C8 C -0.2037(9) 0.3835(4) 0.5590(4) 0.085(3) Uani 1 1 d . . . C9 C -0.2204(8) 0.4286(4) 0.5533(5) 0.100(3) Uani 1 1 d . . . H7 H -0.2794 0.4390 0.5255 0.120 Uiso 1 1 calc R . . C10 C -0.1553(10) 0.4575(3) 0.5860(5) 0.103(4) Uani 1 1 d . . . H8 H -0.1704 0.4878 0.5828 0.124 Uiso 1 1 calc R . . C11 C -0.0662(9) 0.4441(3) 0.6246(5) 0.091(3) Uani 1 1 d . . . H9 H -0.0199 0.4646 0.6475 0.109 Uiso 1 1 calc R . . C12 C -0.0473(8) 0.3999(3) 0.6286(4) 0.077(3) Uani 1 1 d . . . N2 N 0.0390(6) 0.3366(3) 0.6658(3) 0.070(2) Uani 1 1 d . . . C13 C 0.0415(8) 0.3804(3) 0.6681(4) 0.074(3) Uani 1 1 d . . . C14 C 0.1183(9) 0.4038(3) 0.7043(5) 0.085(3) Uani 1 1 d . . . H10 H 0.1170 0.4348 0.7053 0.102 Uiso 1 1 calc R . . C15 C 0.1971(8) 0.3810(4) 0.7393(5) 0.086(3) Uani 1 1 d . . . H11 H 0.2526 0.3962 0.7635 0.103 Uiso 1 1 calc R . . C16 C 0.1952(8) 0.3359(4) 0.7390(4) 0.089(3) Uani 1 1 d . . . H12 H 0.2493 0.3199 0.7638 0.106 Uiso 1 1 calc R . . C17 C 0.1123(8) 0.3133(3) 0.7017(4) 0.074(3) Uani 1 1 d . . . C18 C 0.0448(8) 0.2417(3) 0.6544(5) 0.085(3) Uani 1 1 d . . . C19 C 0.1088(8) 0.2659(3) 0.7037(4) 0.084(3) Uani 1 1 d . . . C20 C 0.1707(8) 0.2421(4) 0.7554(4) 0.087(3) Uani 1 1 d . . . H13 H 0.2130 0.2576 0.7903 0.105 Uiso 1 1 calc R . . C21 C 0.1713(9) 0.1972(4) 0.7565(5) 0.094(3) Uani 1 1 d . . . C22 C 0.1040(9) 0.1750(3) 0.7073(5) 0.099(4) Uani 1 1 d . . . H14 H 0.1029 0.1440 0.7090 0.119 Uiso 1 1 calc R . . C23 C 0.0384(8) 0.1958(3) 0.6559(4) 0.091(3) Uani 1 1 d . . . O2 O -0.0085(5) 0.26247(16) 0.6022(3) 0.086(2) Uani 1 1 d . . . C24 C 0.2428(9) 0.1726(3) 0.8116(4) 0.125(4) Uani 1 1 d . . . H15 H 0.2619 0.1911 0.8501 0.188 Uiso 1 1 calc R . . H16 H 0.2990 0.1651 0.7988 0.188 Uiso 1 1 calc R . . H17 H 0.2134 0.1458 0.8211 0.188 Uiso 1 1 calc R . . N3 N -0.0874(6) 0.1840(2) 0.5519(3) 0.083(2) Uani 1 1 d . . . C25 C -0.0337(8) 0.1669(3) 0.6090(4) 0.090(3) Uani 1 1 d . . . C26 C -0.0420(10) 0.1232(3) 0.6237(5) 0.126(5) Uani 1 1 d . . . H18 H -0.0052 0.1115 0.6640 0.151 Uiso 1 1 calc R . . C27 C -0.1054(10) 0.0967(3) 0.5782(6) 0.139(5) Uani 1 1 d . . . H19 H -0.1142 0.0671 0.5883 0.167 Uiso 1 1 calc R . . C28 C -0.1553(10) 0.1135(3) 0.5185(5) 0.130(5) Uani 1 1 d . . . H20 H -0.1961 0.0955 0.4862 0.156 Uiso 1 1 calc R . . C29 C -0.1443(9) 0.1566(3) 0.5075(4) 0.106(4) Uani 1 1 d . . . N4 N -0.1791(6) 0.2197(2) 0.4390(3) 0.084(3) Uani 1 1 d . . . C30 C -0.1991(8) 0.1768(3) 0.4432(4) 0.085(3) Uani 1 1 d . . . C31 C -0.2599(8) 0.1548(3) 0.3936(5) 0.093(3) Uani 1 1 d . . . H21 H -0.2730 0.1248 0.3977 0.111 Uiso 1 1 calc R . . C32 C -0.3023(7) 0.1768(4) 0.3369(4) 0.086(3) Uani 1 1 d . . . H22 H -0.3437 0.1617 0.3012 0.103 Uiso 1 1 calc R . . C33 C -0.2851(7) 0.2208(3) 0.3317(4) 0.085(3) Uani 1 1 d . . . H23 H -0.3143 0.2359 0.2925 0.101 Uiso 1 1 calc R . . C34 C -0.2245(8) 0.2426(3) 0.3842(4) 0.083(3) Uani 1 1 d . . . C35 C -0.1347(8) 0.3135(3) 0.4229(4) 0.081(3) Uani 1 1 d . . . C36 C -0.2154(9) 0.2910(3) 0.3827(5) 0.090(3) Uani 1 1 d . . . C37 C -0.2896(8) 0.3157(4) 0.3427(5) 0.096(3) Uani 1 1 d . . . H24 H -0.3437 0.3006 0.3160 0.115 Uiso 1 1 calc R . . C38 C -0.2891(10) 0.3602(4) 0.3395(5) 0.104(4) Uani 1 1 d . . . C39 C -0.2099(11) 0.3822(3) 0.3779(5) 0.106(4) Uani 1 1 d . . . H25 H -0.2069 0.4131 0.3757 0.127 Uiso 1 1 calc R . . C40 C -0.1357(9) 0.3595(3) 0.4190(4) 0.094(3) Uani 1 1 d . . . H26 H -0.0831 0.3754 0.4458 0.112 Uiso 1 1 calc R . . O3 O -0.0573(5) 0.29378(16) 0.4644(2) 0.079(2) Uani 1 1 d . . . C41 C -0.3714(9) 0.3853(3) 0.2958(5) 0.141(5) Uani 1 1 d . . . H27 H -0.3837 0.3752 0.2512 0.211 Uiso 1 1 calc R . . H28 H -0.3561 0.4165 0.2983 0.211 Uiso 1 1 calc R . . H29 H -0.4282 0.3805 0.3092 0.211 Uiso 1 1 calc R . . C42 C 0.1092(10) 0.1998(3) 0.5245(5) 0.093(4) Uani 1 1 d . . . C43 C 0.1884(8) 0.2234(3) 0.5649(4) 0.083(3) Uani 1 1 d . . . C44 C 0.2641(9) 0.1984(4) 0.6054(4) 0.099(4) Uani 1 1 d . . . H30 H 0.3178 0.2137 0.6319 0.118 Uiso 1 1 calc R . . C45 C 0.2652(12) 0.1549(5) 0.6090(6) 0.128(5) Uani 1 1 d . . . C46 C 0.1895(12) 0.1315(4) 0.5699(6) 0.119(5) Uani 1 1 d . . . H31 H 0.1898 0.1005 0.5716 0.143 Uiso 1 1 calc R . . C47 C 0.1114(9) 0.1540(4) 0.5274(4) 0.103(4) Uani 1 1 d . . . H32 H 0.0597 0.1377 0.5004 0.123 Uiso 1 1 calc R . . O4 O 0.0337(5) 0.21846(17) 0.4832(2) 0.0756(19) Uani 1 1 d . . . C48 C 0.3517(10) 0.1288(4) 0.6526(6) 0.164(6) Uani 1 1 d . . . H33 H 0.3780 0.1103 0.6255 0.247 Uiso 1 1 calc R . . H34 H 0.3308 0.1105 0.6826 0.247 Uiso 1 1 calc R . . H35 H 0.4006 0.1492 0.6770 0.247 Uiso 1 1 calc R . . N5 N 0.1562(6) 0.2934(2) 0.5078(3) 0.075(2) Uani 1 1 d . . . C49 C 0.1983(8) 0.2712(3) 0.5624(4) 0.084(3) Uani 1 1 d . . . C50 C 0.2605(7) 0.2946(4) 0.6158(4) 0.087(3) Uani 1 1 d . . . H36 H 0.2910 0.2797 0.6550 0.105 Uiso 1 1 calc R . . C51 C 0.2756(8) 0.3373(3) 0.6105(4) 0.100(4) Uani 1 1 d . . . H37 H 0.3160 0.3532 0.6459 0.120 Uiso 1 1 calc R . . C52 C 0.2302(8) 0.3585(3) 0.5512(5) 0.094(3) Uani 1 1 d . . . H38 H 0.2400 0.3888 0.5464 0.113 Uiso 1 1 calc R . . C53 C 0.1724(7) 0.3352(3) 0.5011(4) 0.078(3) Uani 1 1 d . . . N6 N 0.0629(6) 0.3279(2) 0.3955(3) 0.079(2) Uani 1 1 d . . . C54 C 0.1220(8) 0.3548(3) 0.4378(4) 0.096(4) Uani 1 1 d . . . C55 C 0.1394(9) 0.3969(3) 0.4236(4) 0.120(5) Uani 1 1 d . . . H39 H 0.1835 0.4147 0.4543 0.144 Uiso 1 1 calc R . . C56 C 0.0903(11) 0.4128(3) 0.3627(5) 0.143(6) Uani 1 1 d . . . H40 H 0.1021 0.4416 0.3507 0.171 Uiso 1 1 calc R . . C57 C 0.0230(9) 0.3861(3) 0.3188(4) 0.109(4) Uani 1 1 d . . . H41 H -0.0130 0.3973 0.2778 0.130 Uiso 1 1 calc R . . C58 C 0.0099(8) 0.3434(3) 0.3359(4) 0.082(3) Uani 1 1 d . . . C59 C -0.0707(8) 0.2703(3) 0.2930(4) 0.086(3) Uani 1 1 d . . . C60 C -0.0631(8) 0.3159(3) 0.2907(4) 0.080(3) Uani 1 1 d . . . C61 C -0.1310(9) 0.3366(3) 0.2403(5) 0.102(4) Uani 1 1 d . . . H42 H -0.1326 0.3677 0.2389 0.122 Uiso 1 1 calc R . . C62 C -0.1974(8) 0.3128(5) 0.1913(4) 0.103(4) Uani 1 1 d . . . C63 C -0.1973(8) 0.2681(4) 0.1928(5) 0.101(4) Uani 1 1 d . . . H43 H -0.2401 0.2520 0.1588 0.122 Uiso 1 1 calc R . . C64 C -0.1353(8) 0.2469(3) 0.2431(4) 0.082(3) Uani 1 1 d . . . O5 O -0.0151(5) 0.24928(16) 0.3452(2) 0.081(2) Uani 1 1 d . . . C65 C -0.2721(9) 0.3396(4) 0.1377(5) 0.145(5) Uani 1 1 d . . . H44 H -0.2453 0.3469 0.1030 0.218 Uiso 1 1 calc R . . H45 H -0.2879 0.3666 0.1564 0.218 Uiso 1 1 calc R . . H46 H -0.3298 0.3221 0.1202 0.218 Uiso 1 1 calc R . . N7 N -0.0663(6) 0.1754(3) 0.2819(3) 0.071(2) Uani 1 1 d . . . C66 C -0.1400(8) 0.1993(4) 0.2449(4) 0.076(3) Uani 1 1 d . . . C67 C -0.2212(8) 0.1769(4) 0.2064(4) 0.090(3) Uani 1 1 d . . . H47 H -0.2735 0.1929 0.1795 0.108 Uiso 1 1 calc R . . C68 C -0.2252(9) 0.1314(4) 0.2076(5) 0.097(3) Uani 1 1 d . . . H48 H -0.2815 0.1168 0.1831 0.116 Uiso 1 1 calc R . . C69 C -0.1480(10) 0.1069(4) 0.2442(5) 0.099(4) Uani 1 1 d . . . H49 H -0.1489 0.0759 0.2440 0.119 Uiso 1 1 calc R . . C70 C -0.0687(9) 0.1307(3) 0.2814(5) 0.078(3) Uani 1 1 d . . . N8 N 0.0877(7) 0.1409(2) 0.3510(4) 0.078(2) Uani 1 1 d . . . C71 C 0.0184(9) 0.1111(3) 0.3214(5) 0.084(3) Uani 1 1 d . . . C72 C 0.0366(10) 0.0670(3) 0.3294(5) 0.105(4) Uani 1 1 d . . . H50 H -0.0100 0.0459 0.3086 0.125 Uiso 1 1 calc R . . C73 C 0.1260(12) 0.0543(4) 0.3694(6) 0.111(4) Uani 1 1 d . . . H51 H 0.1395 0.0240 0.3759 0.134 Uiso 1 1 calc R . . C74 C 0.1944(9) 0.0834(4) 0.3992(5) 0.095(3) Uani 1 1 d . . . H52 H 0.2542 0.0736 0.4266 0.114 Uiso 1 1 calc R . . C75 C 0.1755(9) 0.1280(4) 0.3891(5) 0.079(3) Uani 1 1 d . . . C76 C 0.2300(10) 0.2045(4) 0.4211(4) 0.082(3) Uani 1 1 d . . . C77 C 0.2482(10) 0.1605(4) 0.4169(5) 0.085(3) Uani 1 1 d . . . C78 C 0.3394(13) 0.1470(5) 0.4406(6) 0.127(4) Uani 1 1 d . . . H53 H 0.3531 0.1171 0.4360 0.153 Uiso 1 1 calc R . . C79 C 0.4126(12) 0.1740(8) 0.4709(8) 0.155(7) Uani 1 1 d . . . C80 C 0.3957(14) 0.2179(6) 0.4776(6) 0.136(6) Uani 1 1 d . . . H54 H 0.4454 0.2373 0.4994 0.163 Uiso 1 1 calc R . . C81 C 0.3061(12) 0.2321(4) 0.4519(5) 0.105(4) Uani 1 1 d . . . H55 H 0.2936 0.2624 0.4547 0.127 Uiso 1 1 calc R . . O6 O 0.1455(5) 0.22315(19) 0.3982(2) 0.0748(19) Uani 1 1 d . . . C82 C 0.5195(12) 0.1567(6) 0.4973(8) 0.231(8) Uani 1 1 d . . . H56 H 0.5221 0.1312 0.5250 0.346 Uiso 1 1 calc R . . H57 H 0.5604 0.1798 0.5223 0.346 Uiso 1 1 calc R . . H58 H 0.5417 0.1485 0.4609 0.346 Uiso 1 1 calc R . . O7 O -0.0273(8) -0.0376(3) 0.2927(4) 0.120(3) Uani 0.75 1 d PDU A 1 O8 O -0.1375(9) -0.0007(3) 0.2301(4) 0.123(4) Uani 0.75 1 d PDU A 1 C83 C -0.1132(9) -0.0301(3) 0.2725(4) 0.122(6) Uani 0.75 1 d PDU A 1 C84 C -0.1826(10) -0.0538(5) 0.2960(8) 0.176(7) Uani 0.75 1 d PDU A 1 H59 H -0.2467 -0.0430 0.2736 0.264 Uiso 0.75 1 calc PR A 1 H60 H -0.1682 -0.0490 0.3425 0.264 Uiso 0.75 1 calc PR A 1 H61 H -0.1791 -0.0851 0.2875 0.264 Uiso 0.75 1 calc PR A 1 O9 O -0.3208(17) 0.0168(7) 0.1637(10) 0.103(8) Uani 0.25 1 d PDU B 2 O10 O -0.351(2) -0.0296(10) 0.0900(13) 0.155(11) Uani 0.25 1 d PDU B 2 C85 C -0.3457(14) -0.0205(8) 0.1478(12) 0.134(14) Uani 0.25 1 d PDU B 2 C86 C -0.367(3) -0.0513(10) 0.1932(17) 0.110(13) Uani 0.25 1 d PDU B 2 H62 H -0.3847 -0.0797 0.1720 0.165 Uiso 0.25 1 calc PR B 2 H63 H -0.4204 -0.0400 0.2066 0.165 Uiso 0.25 1 calc PR B 2 H64 H -0.3112 -0.0547 0.2311 0.165 Uiso 0.25 1 calc PR B 2 O11 O 0.0742(19) 0.4565(7) 0.5272(12) 0.116(9) Uani 0.35 1 d PDU C 1 O12 O 0.0553(19) 0.5223(6) 0.5501(12) 0.152(8) Uani 0.35 1 d PDU C 1 C87 C 0.1106(17) 0.4894(8) 0.5562(14) 0.136(10) Uani 0.35 1 d PDU C 1 C88 C 0.2046(19) 0.4860(10) 0.6040(17) 0.181(13) Uani 0.35 1 d PDU C 1 H65 H 0.2242 0.5148 0.6233 0.271 Uiso 0.35 1 calc PR C 1 H66 H 0.2506 0.4757 0.5830 0.271 Uiso 0.35 1 calc PR C 1 H67 H 0.2021 0.4653 0.6378 0.271 Uiso 0.35 1 calc PR C 1 O13 O -0.3230(18) 0.0473(10) 0.3934(11) 0.223(9) Uani 0.40 1 d PDU D 2 O14 O -0.3295(17) 0.0512(8) 0.2974(10) 0.187(8) Uani 0.40 1 d PDU D 2 C89 C -0.2790(17) 0.0423(10) 0.3545(11) 0.158(9) Uani 0.40 1 d PDU D 2 C90 C -0.1754(16) 0.0405(11) 0.3782(14) 0.178(10) Uani 0.40 1 d PDU D 2 H68 H -0.1503 0.0374 0.3416 0.266 Uiso 0.40 1 calc PR D 2 H69 H -0.1554 0.0154 0.4072 0.266 Uiso 0.40 1 calc PR D 2 H70 H -0.1508 0.0675 0.4017 0.266 Uiso 0.40 1 calc PR D 2 O15 O 0.069(2) -0.0373(9) 0.2874(13) 0.121(8) Uani 0.25 1 d PDU E 3 O16 O 0.105(3) -0.0147(19) 0.2068(17) 0.135(17) Uani 0.25 1 d PDU E 3 C91 C 0.133(2) -0.0295(12) 0.2639(14) 0.076(9) Uani 0.25 1 d PDU E 3 C92 C 0.225(2) -0.0506(15) 0.293(2) 0.157(16) Uani 0.25 1 d PDU E 3 H71 H 0.2696 -0.0414 0.2696 0.236 Uiso 0.25 1 calc PR E 3 H72 H 0.2176 -0.0824 0.2898 0.236 Uiso 0.25 1 calc PR E 3 H73 H 0.2509 -0.0420 0.3381 0.236 Uiso 0.25 1 calc PR E 3 O17 O 0.0858(11) -0.0099(6) 0.2294(6) 0.117(4) Uani 0.75 1 d PDU F 1 C93 C 0.1816(14) -0.0277(7) 0.2545(11) 0.162(8) Uani 0.75 1 d PDU F 1 O18 O 0.078(2) 0.0260(8) 0.5060(10) 0.116(7) Uani 0.40 1 d PDU G 1 C94 C 0.163(3) 0.0042(10) 0.5387(17) 0.157(12) Uani 0.40 1 d PDU G 1 O19 O 0.001(2) 0.0401(6) 0.4808(11) 0.114(7) Uani 0.40 1 d PDU H -2 C95 C 0.051(3) 0.0005(11) 0.500(2) 0.154(14) Uani 0.40 1 d PDU H -2 O20 O 0.4122(19) 0.2107(8) 0.2593(9) 0.151(8) Uani 0.50 1 d PDU I 1 C96 C 0.430(3) 0.2558(10) 0.283(2) 0.206(14) Uani 0.50 1 d PDU I 1 O21 O 0.4492(13) 0.2222(6) 0.3204(7) 0.143(6) Uani 0.50 1 d PDU J 2 C97 C 0.430(3) 0.1872(10) 0.2726(16) 0.154(14) Uani 0.50 1 d PDU J 2 O22 O 0.260(3) 0.4712(8) 0.5407(13) 0.156(9) Uani 0.35 1 d PDU K 3 C98 C 0.345(3) 0.4742(18) 0.595(2) 0.201(19) Uani 0.35 1 d PDU K 3 O23 O 0.307(3) 0.4613(12) 0.6595(17) 0.193(13) Uani 0.30 1 d PDU L 2 C99 C 0.297(6) 0.4924(19) 0.610(3) 0.22(2) Uani 0.30 1 d PDU L 2 O24 O 0.451(3) 0.1129(11) 0.2677(17) 0.309(15) Uani 0.50 1 d PDU M 1 C100 C 0.533(3) 0.0905(14) 0.309(2) 0.288(19) Uani 0.50 1 d PDU M 1 O25 O 0.4082(18) 0.0537(9) 0.3400(13) 0.248(11) Uani 0.50 1 d PDU N 2 C101 C 0.448(3) 0.0956(12) 0.328(2) 0.228(15) Uani 0.50 1 d PDU N 2 O26 O 0.524(2) 0.0989(13) 0.1374(19) 0.121(12) Uani 0.20 1 d PDU O 1 C102 C 0.512(4) 0.1389(14) 0.103(2) 0.105(15) Uani 0.20 1 d PDU O 1 O27 O 0.483(2) 0.1060(8) 0.1791(13) 0.145(9) Uani 0.30 1 d PDU P 2 C103 C 0.512(2) 0.1499(11) 0.1912(17) 0.115(11) Uani 0.30 1 d PDU P 2 O28 O 0.5671(15) 0.2288(7) 0.1885(8) 0.114(6) Uani 0.40 1 d PDU Q 1 C104 C 0.541(3) 0.2496(13) 0.1304(14) 0.136(12) Uani 0.40 1 d PDU Q 1 O29 O 0.527(3) 0.2224(11) 0.1283(14) 0.161(13) Uani 0.30 1 d PDU R 3 C105 C 0.534(3) 0.1959(11) 0.1850(12) 0.083(9) Uani 0.30 1 d PDU R 3 O30 O 0.556(2) 0.2719(10) 0.1732(14) 0.141(10) Uani 0.30 1 d PDU S 2 C106 C 0.489(3) 0.2717(17) 0.207(2) 0.182(18) Uani 0.30 1 d PDU S 2 O31 O 0.276(3) -0.0015(13) 0.520(2) 0.222(14) Uani 0.30 1 d PDU T 2 C107 C 0.356(4) -0.0154(18) 0.501(3) 0.183(19) Uani 0.30 1 d PDU T 2 O32 O -0.336(3) -0.0327(9) -0.0257(18) 0.151(11) Uani 0.30 1 d PDU U 1 C108 C -0.342(5) -0.0377(19) 0.039(2) 0.20(2) Uani 0.30 1 d PDU U 1 O33 O -0.081(4) 0.0469(13) 0.428(2) 0.136(13) Uani 0.20 1 d PDU V 3 C109 C -0.042(5) 0.0048(16) 0.449(3) 0.121(17) Uani 0.20 1 d PDU V 3 O34 O -0.468(3) -0.0222(11) 0.2847(18) 0.375(19) Uani 0.50 1 d PU W 1 O35 O -0.592(3) -0.0348(12) 0.1031(18) 0.215(15) Uani 0.30 1 d PU . 1 O36 O 0.464(3) -0.0587(11) 0.3857(18) 0.301(16) Uani 0.40 1 d PU X 1 O37 O 0.3254(9) -0.0315(4) 0.4509(7) 0.162(5) Uani 0.70 1 d PU Y 1 O38 O 0.3942(10) 0.0402(4) 0.5418(6) 0.167(5) Uani 0.70 1 d PU Z 1 O39 O -0.437(2) -0.0452(10) 0.1919(17) 0.307(16) Uani 0.50 1 d PU A 1 O40 O 0.039(2) 0.4670(7) 0.5009(12) 0.111(8) Uani 0.35 1 d PU B 2 O41 O -0.094(2) -0.0209(9) 0.2615(14) 0.068(8) Uani 0.25 1 d PU C 2 O42 O 0.421(3) 0.5146(13) 0.545(2) 0.236(17) Uani 0.30 1 d PU . 1 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 0.1170(12) 0.0722(8) 0.0461(6) -0.0107(6) 0.0241(7) -0.0169(7) Ni2 0.1402(13) 0.0644(7) 0.0418(6) -0.0068(5) 0.0291(7) -0.0167(7) Ni3 0.1364(13) 0.0628(7) 0.0405(6) -0.0025(5) 0.0262(7) -0.0109(7) Ni4 0.1083(11) 0.0671(8) 0.0503(6) -0.0081(5) 0.0255(7) -0.0124(7) C1 0.094(10) 0.103(9) 0.059(6) -0.030(6) 0.035(7) -0.048(8) C2 0.103(11) 0.097(9) 0.059(6) -0.007(6) 0.007(6) -0.029(8) C3 0.108(13) 0.119(11) 0.157(12) 0.016(9) -0.010(10) -0.006(10) C4 0.106(15) 0.165(15) 0.172(14) 0.026(12) -0.034(11) -0.045(13) C5 0.130(16) 0.170(15) 0.079(8) 0.006(9) 0.011(9) -0.043(12) C6 0.158(14) 0.116(9) 0.057(6) -0.010(7) 0.048(8) -0.054(10) O1 0.100(6) 0.086(5) 0.052(4) -0.020(3) 0.024(4) -0.037(4) C7 0.103(14) 0.227(18) 0.31(2) 0.030(15) -0.103(15) -0.017(12) N1 0.108(8) 0.053(5) 0.061(5) -0.009(4) 0.030(5) -0.008(5) C8 0.097(10) 0.092(8) 0.063(6) -0.001(6) 0.021(6) -0.011(7) C9 0.100(10) 0.098(9) 0.089(8) 0.001(7) 0.011(7) 0.002(8) C10 0.119(12) 0.072(7) 0.112(9) -0.021(7) 0.025(8) -0.002(8) C11 0.099(10) 0.089(8) 0.084(7) -0.021(6) 0.028(7) -0.015(7) C12 0.106(10) 0.059(6) 0.069(6) -0.014(5) 0.033(6) -0.021(6) N2 0.077(7) 0.070(5) 0.064(5) -0.028(4) 0.021(4) -0.020(5) C13 0.093(9) 0.078(7) 0.049(5) -0.017(5) 0.019(6) 0.001(7) C14 0.093(10) 0.083(7) 0.083(7) -0.028(6) 0.032(7) -0.022(7) C15 0.081(10) 0.102(9) 0.080(7) -0.033(6) 0.033(7) -0.004(7) C16 0.091(10) 0.112(9) 0.059(6) -0.016(6) 0.018(6) 0.009(7) C17 0.087(9) 0.088(8) 0.053(6) -0.018(6) 0.030(6) -0.004(7) C18 0.138(11) 0.059(6) 0.073(7) 0.000(6) 0.054(7) 0.001(6) C19 0.136(10) 0.082(7) 0.038(5) -0.016(5) 0.034(6) -0.007(7) C20 0.115(10) 0.107(8) 0.044(5) -0.006(6) 0.031(6) 0.017(7) C21 0.139(11) 0.092(8) 0.060(6) 0.002(6) 0.045(7) 0.017(8) C22 0.154(12) 0.085(7) 0.063(6) -0.004(6) 0.042(7) 0.001(7) C23 0.144(11) 0.096(8) 0.035(5) 0.005(5) 0.032(6) 0.001(7) O2 0.159(7) 0.053(4) 0.047(3) -0.002(3) 0.032(4) 0.006(4) C24 0.170(13) 0.126(9) 0.077(7) 0.026(7) 0.035(8) 0.046(8) N3 0.135(8) 0.065(5) 0.048(4) -0.009(4) 0.027(5) -0.025(5) C25 0.154(11) 0.064(6) 0.049(6) -0.005(5) 0.029(6) -0.012(6) C26 0.246(16) 0.065(7) 0.063(6) 0.001(6) 0.041(8) -0.019(8) C27 0.265(18) 0.062(7) 0.087(8) 0.001(7) 0.047(9) -0.034(8) C28 0.246(16) 0.079(8) 0.060(7) -0.011(6) 0.040(8) -0.046(8) C29 0.206(13) 0.063(6) 0.056(6) -0.011(5) 0.049(7) -0.029(7) N4 0.144(8) 0.069(5) 0.039(4) -0.011(4) 0.029(4) -0.015(5) C30 0.141(10) 0.065(6) 0.053(6) -0.011(5) 0.034(6) -0.029(6) C31 0.135(11) 0.073(7) 0.073(7) -0.012(6) 0.037(7) -0.024(7) C32 0.085(8) 0.111(8) 0.061(6) -0.021(6) 0.020(6) -0.014(7) C33 0.099(9) 0.101(8) 0.049(5) -0.016(5) 0.016(5) -0.023(7) C34 0.111(9) 0.085(7) 0.060(6) -0.013(6) 0.034(6) -0.016(6) C35 0.139(11) 0.060(6) 0.044(5) 0.008(5) 0.030(6) 0.008(7) C36 0.144(12) 0.079(7) 0.060(6) -0.027(6) 0.049(7) -0.043(8) C37 0.125(11) 0.085(8) 0.069(7) 0.018(6) 0.018(6) 0.018(7) C38 0.137(13) 0.096(9) 0.074(7) 0.009(7) 0.025(7) 0.009(9) C39 0.175(14) 0.070(7) 0.078(7) 0.018(6) 0.049(8) 0.017(8) C40 0.163(12) 0.061(7) 0.068(6) -0.005(5) 0.051(7) 0.002(7) O3 0.151(7) 0.051(3) 0.045(3) -0.005(3) 0.043(4) -0.005(4) C41 0.160(14) 0.111(9) 0.138(10) 0.036(8) 0.024(9) 0.033(9) C42 0.189(14) 0.042(6) 0.053(6) 0.003(5) 0.045(7) 0.001(7) C43 0.126(10) 0.083(7) 0.044(5) 0.000(5) 0.034(6) -0.006(7) C44 0.141(12) 0.089(8) 0.062(6) 0.021(6) 0.025(7) 0.007(7) C45 0.194(17) 0.094(10) 0.093(9) 0.019(8) 0.040(10) 0.005(10) C46 0.209(17) 0.072(8) 0.094(9) 0.026(7) 0.073(10) 0.027(9) C47 0.173(13) 0.089(8) 0.060(6) -0.002(6) 0.056(7) 0.005(8) O4 0.133(6) 0.053(4) 0.049(3) 0.001(3) 0.039(4) 0.001(4) C48 0.185(16) 0.133(11) 0.170(12) 0.058(10) 0.046(11) 0.065(10) N5 0.122(7) 0.065(5) 0.032(4) -0.002(3) 0.016(4) -0.011(4) C49 0.125(10) 0.068(6) 0.066(6) 0.003(5) 0.039(6) -0.001(6) C50 0.097(9) 0.111(8) 0.054(6) -0.014(6) 0.022(6) -0.018(7) C51 0.152(11) 0.090(8) 0.061(6) -0.018(6) 0.037(7) -0.033(7) C52 0.149(11) 0.074(6) 0.070(6) -0.016(6) 0.050(7) -0.022(7) C53 0.133(10) 0.053(6) 0.046(5) -0.009(5) 0.025(5) -0.023(6) N6 0.126(7) 0.057(4) 0.058(5) 0.000(4) 0.033(5) -0.013(5) C54 0.186(12) 0.043(5) 0.050(6) -0.011(5) 0.022(6) -0.023(6) C55 0.227(15) 0.065(7) 0.057(6) -0.011(5) 0.027(7) -0.040(7) C56 0.290(18) 0.061(7) 0.072(7) 0.009(6) 0.050(9) -0.037(9) C57 0.194(13) 0.061(6) 0.056(6) 0.013(5) 0.017(7) -0.002(7) C58 0.146(10) 0.052(6) 0.048(5) 0.007(5) 0.028(6) 0.004(6) C59 0.142(11) 0.069(7) 0.050(6) 0.002(5) 0.032(6) 0.002(6) C60 0.120(10) 0.080(7) 0.043(5) -0.002(5) 0.027(6) 0.000(6) C61 0.166(12) 0.084(7) 0.057(6) 0.012(6) 0.037(7) 0.007(7) C62 0.107(10) 0.148(11) 0.050(6) 0.007(7) 0.019(6) 0.027(9) C63 0.130(11) 0.094(8) 0.070(7) -0.002(6) 0.015(7) 0.017(8) C64 0.109(10) 0.082(7) 0.052(6) -0.014(6) 0.021(6) -0.001(7) O5 0.149(7) 0.048(3) 0.045(3) -0.008(3) 0.029(4) 0.005(4) C65 0.192(15) 0.142(10) 0.076(7) 0.015(7) 0.003(8) 0.036(10) N7 0.091(7) 0.067(5) 0.058(5) -0.027(4) 0.028(5) -0.022(5) C66 0.068(8) 0.115(9) 0.044(5) -0.021(6) 0.016(5) 0.002(7) C67 0.094(10) 0.112(9) 0.062(6) -0.038(6) 0.020(6) 0.002(7) C68 0.078(10) 0.112(10) 0.105(8) -0.056(7) 0.033(7) -0.021(7) C69 0.114(12) 0.103(9) 0.089(8) -0.041(7) 0.043(8) -0.023(9) C70 0.099(10) 0.076(8) 0.067(6) -0.017(6) 0.037(6) 0.000(7) N8 0.126(9) 0.061(5) 0.058(5) 0.002(4) 0.045(5) 0.006(6) C71 0.120(11) 0.059(7) 0.086(7) -0.022(6) 0.051(7) -0.016(7) C72 0.155(14) 0.063(8) 0.105(9) -0.018(6) 0.054(9) -0.011(7) C73 0.155(15) 0.094(9) 0.093(9) 0.005(7) 0.050(9) 0.042(10) C74 0.096(10) 0.099(9) 0.085(7) -0.013(7) 0.017(7) 0.010(8) C75 0.095(10) 0.075(8) 0.068(6) 0.009(6) 0.025(6) 0.003(7) C76 0.114(12) 0.083(8) 0.048(6) 0.010(6) 0.023(6) -0.007(8) C77 0.081(10) 0.109(10) 0.066(6) 0.023(6) 0.022(6) 0.001(8) C78 0.104(14) 0.147(12) 0.112(10) 0.028(9) 0.003(9) -0.003(11) C79 0.080(14) 0.22(2) 0.126(12) 0.074(13) -0.020(9) -0.002(14) C80 0.130(17) 0.193(17) 0.074(8) 0.018(10) 0.014(9) -0.045(14) C81 0.125(12) 0.129(10) 0.061(7) 0.007(7) 0.026(7) -0.062(11) O6 0.102(6) 0.067(4) 0.050(3) -0.008(3) 0.014(4) -0.025(4) C82 0.142(18) 0.29(2) 0.215(17) 0.056(15) -0.018(14) -0.004(15) O7 0.180(9) 0.090(7) 0.086(7) 0.004(5) 0.037(7) -0.002(7) O8 0.180(11) 0.081(7) 0.104(8) 0.003(5) 0.037(7) -0.001(6) C83 0.180(9) 0.088(13) 0.104(13) 0.008(8) 0.051(11) 0.000(10) C84 0.220(13) 0.129(13) 0.224(16) 0.054(11) 0.137(14) 0.039(12) O9 0.064(17) 0.146(15) 0.104(14) 0.047(12) 0.034(13) -0.018(15) O10 0.12(2) 0.20(2) 0.175(17) -0.014(15) 0.085(19) -0.062(19) C85 0.12(3) 0.140(18) 0.151(19) 0.023(12) 0.05(2) 0.00(2) C86 0.11(3) 0.082(18) 0.14(2) -0.020(17) 0.05(2) -0.02(2) O11 0.119(10) 0.123(9) 0.116(10) 0.000(5) 0.048(5) 0.009(5) O12 0.217(19) 0.099(11) 0.157(18) 0.000(13) 0.081(16) -0.035(13) C87 0.139(18) 0.124(15) 0.17(2) 0.018(15) 0.073(12) -0.048(10) C88 0.18(2) 0.14(2) 0.20(3) 0.054(18) 0.023(16) -0.095(15) O13 0.233(15) 0.24(2) 0.229(14) -0.102(18) 0.119(16) -0.087(18) O14 0.187(15) 0.167(18) 0.219(14) -0.002(17) 0.079(12) 0.023(16) C89 0.207(12) 0.101(19) 0.183(15) -0.040(19) 0.084(10) -0.05(2) C90 0.213(12) 0.164(15) 0.162(14) -0.033(11) 0.066(10) 0.014(12) O15 0.161(16) 0.105(17) 0.108(17) -0.023(14) 0.057(15) -0.048(18) O16 0.16(3) 0.12(3) 0.11(2) 0.05(2) 0.026(16) -0.03(2) C91 0.121(17) 0.029(17) 0.072(14) -0.027(14) 0.020(14) -0.029(16) C92 0.136(18) 0.14(3) 0.16(3) -0.01(2) -0.015(19) 0.00(2) O17 0.151(10) 0.081(8) 0.113(9) 0.008(7) 0.030(8) 0.011(7) C93 0.164(13) 0.125(14) 0.161(15) -0.020(11) -0.003(12) 0.033(12) O18 0.136(15) 0.141(15) 0.075(11) -0.031(11) 0.038(11) -0.054(11) C94 0.189(19) 0.099(16) 0.17(2) -0.023(14) 0.039(15) -0.018(14) O19 0.141(16) 0.117(12) 0.110(13) -0.005(10) 0.077(13) -0.012(11) C95 0.160(17) 0.141(14) 0.162(17) 0.002(10) 0.050(10) 0.010(10) O20 0.178(17) 0.183(13) 0.076(10) 0.003(11) 0.016(10) -0.032(14) C96 0.19(2) 0.198(16) 0.23(2) -0.055(16) 0.064(17) -0.010(17) O21 0.144(13) 0.198(13) 0.072(9) -0.026(9) 0.009(9) 0.006(11) C97 0.13(2) 0.156(19) 0.146(19) -0.039(14) -0.003(15) -0.019(17) O22 0.205(18) 0.100(14) 0.154(16) -0.007(12) 0.043(13) -0.023(15) C98 0.19(2) 0.20(3) 0.20(2) -0.009(19) 0.030(14) 0.006(19) O23 0.18(2) 0.21(2) 0.187(19) -0.027(15) 0.064(16) -0.041(17) C99 0.22(3) 0.21(3) 0.23(3) 0.006(18) 0.06(2) 0.01(2) O24 0.26(2) 0.33(2) 0.33(2) 0.016(17) 0.068(16) 0.012(17) C100 0.28(2) 0.24(2) 0.31(3) 0.022(18) 0.052(17) -0.022(18) O25 0.185(17) 0.264(17) 0.303(19) -0.010(15) 0.084(15) 0.011(14) C101 0.20(2) 0.27(2) 0.25(2) 0.009(17) 0.128(18) 0.037(16) O26 0.075(19) 0.153(18) 0.15(2) 0.003(15) 0.056(16) -0.039(15) C102 0.08(2) 0.126(19) 0.11(2) -0.026(15) 0.027(17) 0.005(18) O27 0.155(18) 0.120(12) 0.138(16) -0.035(13) 0.011(14) 0.065(13) C103 0.036(17) 0.160(15) 0.130(19) 0.030(16) -0.005(14) -0.016(15) O28 0.123(15) 0.148(14) 0.055(9) -0.016(9) 0.004(9) -0.011(12) C104 0.16(2) 0.118(19) 0.114(15) 0.032(14) 0.019(15) -0.010(17) O29 0.14(2) 0.18(2) 0.142(18) 0.078(15) 0.017(15) -0.022(17) C105 0.083(19) 0.113(18) 0.044(12) -0.004(11) 0.007(13) 0.047(15) O30 0.158(17) 0.152(17) 0.098(15) 0.006(14) 0.018(13) -0.060(15) C106 0.16(2) 0.19(3) 0.19(2) 0.013(18) 0.063(18) -0.003(19) O31 0.209(19) 0.20(2) 0.26(2) 0.028(17) 0.081(17) -0.005(17) C107 0.21(2) 0.15(3) 0.18(3) -0.002(18) 0.051(19) -0.019(18) O32 0.167(19) 0.098(15) 0.179(17) -0.009(14) 0.039(16) -0.003(15) C108 0.21(3) 0.21(3) 0.19(2) -0.005(19) 0.06(2) -0.008(19) O33 0.14(2) 0.127(18) 0.15(2) -0.005(16) 0.073(17) 0.004(16) C109 0.14(3) 0.12(2) 0.10(2) 0.009(18) 0.044(18) -0.022(17) O34 0.36(3) 0.34(2) 0.39(2) -0.022(18) 0.065(18) -0.017(18) O35 0.24(2) 0.23(2) 0.19(2) 0.022(17) 0.076(17) -0.031(17) O36 0.30(2) 0.26(2) 0.34(2) -0.057(17) 0.089(18) 0.013(17) O37 0.114(10) 0.172(11) 0.174(10) -0.005(9) 0.005(8) -0.005(8) O38 0.188(12) 0.146(9) 0.147(9) 0.043(8) 0.023(8) 0.070(9) O39 0.30(2) 0.30(2) 0.35(2) 0.041(16) 0.148(18) -0.086(17) O40 0.133(17) 0.106(14) 0.142(16) 0.006(12) 0.112(13) 0.019(13) O41 0.085(16) 0.043(14) 0.073(16) -0.031(12) 0.022(13) 0.006(12) O42 0.22(2) 0.22(2) 0.25(2) 0.031(18) 0.037(18) 0.039(18) _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 O1 1.807(7) . ? Ni1 O2 1.822(6) . ? Ni1 N1 1.832(7) . ? Ni1 N2 1.843(7) . ? Ni1 Ni2 2.9498(14) . ? Ni2 N4 1.971(7) . ? Ni2 O3 1.980(5) . ? Ni2 O2 1.983(5) . ? Ni2 N3 1.993(7) . ? Ni2 O4 2.082(6) . ? Ni2 O1 2.252(7) . ? Ni3 O4 1.965(5) . ? Ni3 O5 1.984(5) . ? Ni3 N5 1.989(7) . ? Ni3 N6 1.995(6) . ? Ni3 O3 2.069(6) . ? Ni3 O6 2.273(7) . ? Ni3 Ni4 2.9591(14) . ? Ni4 O6 1.820(6) . ? Ni4 O5 1.823(5) . ? Ni4 N8 1.828(7) . ? Ni4 N7 1.856(7) . ? C1 O1 1.321(12) . ? C1 C2 1.409(14) . ? C1 C6 1.447(14) . ? C2 C3 1.410(15) . ? C2 C8 1.463(13) . ? C3 C4 1.363(16) . ? C3 H1 0.9500 . ? C4 C5 1.373(17) . ? C4 C7 1.517(19) . ? C5 C6 1.387(16) . ? C5 H2 0.9500 . ? C6 H3 0.9500 . ? C7 H4 0.9800 . ? C7 H5 0.9800 . ? C7 H6 0.9800 . ? N1 C8 1.371(11) . ? N1 C12 1.384(11) . ? C8 C9 1.403(12) . ? C9 C10 1.339(13) . ? C9 H7 0.9500 . ? C10 C11 1.391(13) . ? C10 H8 0.9500 . ? C11 C12 1.377(12) . ? C11 H9 0.9500 . ? C12 C13 1.457(12) . ? N2 C17 1.332(11) . ? N2 C13 1.343(10) . ? C13 C14 1.369(12) . ? C14 C15 1.369(12) . ? C14 H10 0.9500 . ? C15 C16 1.382(12) . ? C15 H11 0.9500 . ? C16 C17 1.425(12) . ? C16 H12 0.9500 . ? C17 C19 1.450(12) . ? C18 O2 1.329(10) . ? C18 C19 1.404(12) . ? C18 C23 1.410(11) . ? C19 C20 1.415(12) . ? C20 C21 1.375(11) . ? C20 H13 0.9500 . ? C21 C22 1.396(13) . ? C21 C24 1.532(12) . ? C22 C23 1.390(12) . ? C22 H14 0.9500 . ? C23 C25 1.514(13) . ? C24 H15 0.9800 . ? C24 H16 0.9800 . ? C24 H17 0.9800 . ? N3 C25 1.358(10) . ? N3 C29 1.358(11) . ? C25 C26 1.389(11) . ? C26 C27 1.393(13) . ? C26 H18 0.9500 . ? C27 C28 1.382(13) . ? C27 H19 0.9500 . ? C28 C29 1.359(11) . ? C28 H20 0.9500 . ? C29 C30 1.517(12) . ? N4 C30 1.357(10) . ? N4 C34 1.369(10) . ? C30 C31 1.352(11) . ? C31 C32 1.377(11) . ? C31 H21 0.9500 . ? C32 C33 1.379(11) . ? C32 H22 0.9500 . ? C33 C34 1.389(11) . ? C33 H23 0.9500 . ? C34 C36 1.486(12) . ? C35 O3 1.362(10) . ? C35 C40 1.411(11) . ? C35 C36 1.422(13) . ? C36 C37 1.396(13) . ? C37 C38 1.364(12) . ? C37 H24 0.9500 . ? C38 C39 1.385(14) . ? C38 C41 1.506(14) . ? C39 C40 1.372(13) . ? C39 H25 0.9500 . ? C40 H26 0.9500 . ? C41 H27 0.9800 . ? C41 H28 0.9800 . ? C41 H29 0.9800 . ? C42 O4 1.328(12) . ? C42 C47 1.403(12) . ? C42 C43 1.428(13) . ? C43 C44 1.419(13) . ? C43 C49 1.470(11) . ? C44 C45 1.332(13) . ? C44 H30 0.9500 . ? C45 C46 1.380(15) . ? C45 C48 1.558(16) . ? C46 C47 1.415(14) . ? C46 H31 0.9500 . ? C47 H32 0.9500 . ? C48 H33 0.9800 . ? C48 H34 0.9800 . ? C48 H35 0.9800 . ? N5 C53 1.319(9) . ? N5 C49 1.344(10) . ? C49 C50 1.434(11) . ? C50 C51 1.338(11) . ? C50 H36 0.9500 . ? C51 C52 1.417(12) . ? C51 H37 0.9500 . ? C52 C53 1.362(11) . ? C52 H38 0.9500 . ? C53 C54 1.478(11) . ? N6 C54 1.341(10) . ? N6 C58 1.378(10) . ? C54 C55 1.367(11) . ? C55 C56 1.390(12) . ? C55 H39 0.9500 . ? C56 C57 1.410(13) . ? C56 H40 0.9500 . ? C57 C58 1.390(10) . ? C57 H41 0.9500 . ? C58 C60 1.479(12) . ? C59 O5 1.343(10) . ? C59 C64 1.402(12) . ? C59 C60 1.405(11) . ? C60 C61 1.391(12) . ? C61 C62 1.411(13) . ? C61 H42 0.9500 . ? C62 C63 1.368(13) . ? C62 C65 1.570(13) . ? C63 C64 1.358(12) . ? C63 H43 0.9500 . ? C64 C66 1.459(12) . ? C65 H44 0.9800 . ? C65 H45 0.9800 . ? C65 H46 0.9800 . ? N7 C66 1.354(10) . ? N7 C70 1.370(10) . ? C66 C67 1.414(12) . ? C67 C68 1.395(12) . ? C67 H47 0.9500 . ? C68 C69 1.392(13) . ? C68 H48 0.9500 . ? C69 C70 1.406(13) . ? C69 H49 0.9500 . ? C70 C71 1.444(13) . ? N8 C75 1.367(11) . ? N8 C71 1.375(11) . ? C71 C72 1.377(12) . ? C72 C73 1.396(14) . ? C72 H50 0.9500 . ? C73 C74 1.353(14) . ? C73 H51 0.9500 . ? C74 C75 1.396(12) . ? C74 H52 0.9500 . ? C75 C77 1.452(13) . ? C76 O6 1.324(12) . ? C76 C77 1.383(13) . ? C76 C81 1.402(14) . ? C77 C78 1.350(15) . ? C78 C79 1.361(18) . ? C78 H53 0.9500 . ? C79 C80 1.382(19) . ? C79 C82 1.60(2) . ? C80 C81 1.342(17) . ? C80 H54 0.9500 . ? C81 H55 0.9500 . ? C82 H56 0.9800 . ? C82 H57 0.9800 . ? C82 H58 0.9800 . ? O7 C83 1.231(8) . ? O8 C83 1.260(8) . ? C83 C84 1.468(8) . ? C84 H59 0.9800 . ? C84 H60 0.9800 . ? C84 H61 0.9800 . ? O9 C85 1.217(12) . ? O10 C85 1.269(12) . ? C85 C86 1.469(12) . ? C86 H62 0.9800 . ? C86 H63 0.9800 . ? C86 H64 0.9800 . ? O11 C87 1.220(12) . ? O12 C87 1.278(12) . ? C87 C88 1.463(12) . ? C88 H65 0.9800 . ? C88 H66 0.9800 . ? C88 H67 0.9800 . ? O13 C89 1.225(12) . ? O14 C89 1.269(12) . ? C89 C90 1.459(12) . ? C90 H68 0.9800 . ? C90 H69 0.9800 . ? C90 H70 0.9800 . ? O15 C91 1.226(12) . ? O16 C91 1.269(12) . ? C91 C92 1.462(13) . ? C92 H71 0.9800 . ? C92 H72 0.9800 . ? C92 H73 0.9800 . ? O17 C93 1.458(16) . ? O18 C94 1.408(19) . ? O19 C95 1.414(19) . ? O20 C96 1.468(18) . ? O21 C97 1.460(18) . ? O22 C98 1.44(2) . ? O23 C99 1.41(2) . ? O24 C100 1.44(2) . ? O25 C101 1.468(19) . ? O26 C102 1.41(2) . ? O27 C103 1.411(19) . ? O28 C104 1.364(18) . ? O29 C105 1.454(19) . ? O30 C106 1.40(2) . ? O31 C107 1.44(2) . ? O32 C108 1.45(2) . ? O33 C109 1.43(2) . ? O35 O42 1.46(4) 4_465 ? O42 O35 1.46(4) 4_666 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Ni1 O2 83.6(3) . . ? O1 Ni1 N1 97.8(4) . . ? O2 Ni1 N1 168.5(3) . . ? O1 Ni1 N2 174.2(4) . . ? O2 Ni1 N2 92.1(3) . . ? N1 Ni1 N2 87.2(4) . . ? O1 Ni1 Ni2 49.7(2) . . ? O2 Ni1 Ni2 41.19(18) . . ? N1 Ni1 Ni2 133.3(2) . . ? N2 Ni1 Ni2 127.8(3) . . ? N4 Ni2 O3 92.0(3) . . ? N4 Ni2 O2 161.1(3) . . ? O3 Ni2 O2 99.3(2) . . ? N4 Ni2 N3 84.0(3) . . ? O3 Ni2 N3 169.0(3) . . ? O2 Ni2 N3 87.4(3) . . ? N4 Ni2 O4 95.2(3) . . ? O3 Ni2 O4 80.9(2) . . ? O2 Ni2 O4 101.5(3) . . ? N3 Ni2 O4 89.2(3) . . ? N4 Ni2 O1 96.9(3) . . ? O3 Ni2 O1 85.0(2) . . ? O2 Ni2 O1 69.3(3) . . ? N3 Ni2 O1 105.6(3) . . ? O4 Ni2 O1 161.7(2) . . ? N4 Ni2 Ni1 133.5(2) . . ? O3 Ni2 Ni1 77.73(13) . . ? O2 Ni2 Ni1 37.24(17) . . ? N3 Ni2 Ni1 112.4(2) . . ? O4 Ni2 Ni1 126.70(17) . . ? O1 Ni2 Ni1 37.73(17) . . ? O4 Ni3 O5 99.7(2) . . ? O4 Ni3 N5 93.0(3) . . ? O5 Ni3 N5 159.4(3) . . ? O4 Ni3 N6 169.3(2) . . ? O5 Ni3 N6 87.3(3) . . ? N5 Ni3 N6 82.7(3) . . ? O4 Ni3 O3 81.6(2) . . ? O5 Ni3 O3 102.4(3) . . ? N5 Ni3 O3 95.4(3) . . ? N6 Ni3 O3 89.1(3) . . ? O4 Ni3 O6 83.6(2) . . ? O5 Ni3 O6 69.3(2) . . ? N5 Ni3 O6 96.3(3) . . ? N6 Ni3 O6 106.5(3) . . ? O3 Ni3 O6 161.6(2) . . ? O4 Ni3 Ni4 77.31(14) . . ? O5 Ni3 Ni4 37.07(16) . . ? N5 Ni3 Ni4 133.4(2) . . ? N6 Ni3 Ni4 112.70(19) . . ? O3 Ni3 Ni4 126.94(17) . . ? O6 Ni3 Ni4 37.92(16) . . ? O6 Ni4 O5 83.8(3) . . ? O6 Ni4 N8 98.0(4) . . ? O5 Ni4 N8 168.8(3) . . ? O6 Ni4 N7 174.3(3) . . ? O5 Ni4 N7 91.4(3) . . ? N8 Ni4 N7 87.2(4) . . ? O6 Ni4 Ni3 50.2(2) . . ? O5 Ni4 Ni3 40.98(17) . . ? N8 Ni4 Ni3 134.1(3) . . ? N7 Ni4 Ni3 126.8(3) . . ? O1 C1 C2 126.5(10) . . ? O1 C1 C6 117.3(12) . . ? C2 C1 C6 116.1(12) . . ? C1 C2 C3 118.5(11) . . ? C1 C2 C8 123.1(11) . . ? C3 C2 C8 118.4(12) . . ? C4 C3 C2 125.6(14) . . ? C4 C3 H1 117.2 . . ? C2 C3 H1 117.2 . . ? C3 C4 C5 115.8(16) . . ? C3 C4 C7 122.8(18) . . ? C5 C4 C7 121.1(16) . . ? C4 C5 C6 122.9(15) . . ? C4 C5 H2 118.6 . . ? C6 C5 H2 118.6 . . ? C5 C6 C1 121.0(13) . . ? C5 C6 H3 119.5 . . ? C1 C6 H3 119.5 . . ? C1 O1 Ni1 124.2(6) . . ? C1 O1 Ni2 135.7(6) . . ? Ni1 O1 Ni2 92.6(3) . . ? C4 C7 H4 109.5 . . ? C4 C7 H5 109.5 . . ? H4 C7 H5 109.5 . . ? C4 C7 H6 109.5 . . ? H4 C7 H6 109.5 . . ? H5 C7 H6 109.5 . . ? C8 N1 C12 120.9(8) . . ? C8 N1 Ni1 127.6(7) . . ? C12 N1 Ni1 111.1(7) . . ? N1 C8 C9 117.4(9) . . ? N1 C8 C2 118.9(10) . . ? C9 C8 C2 123.7(11) . . ? C10 C9 C8 121.6(11) . . ? C10 C9 H7 119.2 . . ? C8 C9 H7 119.2 . . ? C9 C10 C11 121.3(11) . . ? C9 C10 H8 119.3 . . ? C11 C10 H8 119.3 . . ? C12 C11 C10 117.7(10) . . ? C12 C11 H9 121.2 . . ? C10 C11 H9 121.2 . . ? C11 C12 N1 121.0(10) . . ? C11 C12 C13 124.5(10) . . ? N1 C12 C13 114.4(9) . . ? C17 N2 C13 120.4(8) . . ? C17 N2 Ni1 125.7(7) . . ? C13 N2 Ni1 113.8(7) . . ? N2 C13 C14 123.5(10) . . ? N2 C13 C12 112.1(9) . . ? C14 C13 C12 124.4(10) . . ? C13 C14 C15 117.9(10) . . ? C13 C14 H10 121.1 . . ? C15 C14 H10 121.1 . . ? C14 C15 C16 119.6(10) . . ? C14 C15 H11 120.2 . . ? C16 C15 H11 120.2 . . ? C15 C16 C17 120.0(10) . . ? C15 C16 H12 120.0 . . ? C17 C16 H12 120.0 . . ? N2 C17 C16 118.5(9) . . ? N2 C17 C19 121.5(10) . . ? C16 C17 C19 120.0(11) . . ? O2 C18 C19 119.0(8) . . ? O2 C18 C23 118.0(9) . . ? C19 C18 C23 122.9(10) . . ? C18 C19 C20 117.1(9) . . ? C18 C19 C17 121.7(9) . . ? C20 C19 C17 121.2(10) . . ? C21 C20 C19 121.9(10) . . ? C21 C20 H13 119.1 . . ? C19 C20 H13 119.1 . . ? C20 C21 C22 118.3(10) . . ? C20 C21 C24 120.3(10) . . ? C22 C21 C24 121.3(10) . . ? C23 C22 C21 123.5(10) . . ? C23 C22 H14 118.3 . . ? C21 C22 H14 118.3 . . ? C22 C23 C18 116.1(10) . . ? C22 C23 C25 116.6(9) . . ? C18 C23 C25 127.2(9) . . ? C18 O2 Ni1 123.2(5) . . ? C18 O2 Ni2 132.5(5) . . ? Ni1 O2 Ni2 101.6(3) . . ? C21 C24 H15 109.5 . . ? C21 C24 H16 109.5 . . ? H15 C24 H16 109.5 . . ? C21 C24 H17 109.5 . . ? H15 C24 H17 109.5 . . ? H16 C24 H17 109.5 . . ? C25 N3 C29 118.4(8) . . ? C25 N3 Ni2 129.0(6) . . ? C29 N3 Ni2 111.3(6) . . ? N3 C25 C26 120.8(9) . . ? N3 C25 C23 119.1(8) . . ? C26 C25 C23 120.1(9) . . ? C25 C26 C27 118.9(10) . . ? C25 C26 H18 120.5 . . ? C27 C26 H18 120.5 . . ? C28 C27 C26 120.1(9) . . ? C28 C27 H19 120.0 . . ? C26 C27 H19 120.0 . . ? C29 C28 C27 117.9(10) . . ? C29 C28 H20 121.0 . . ? C27 C28 H20 121.0 . . ? N3 C29 C28 123.6(9) . . ? N3 C29 C30 116.4(8) . . ? C28 C29 C30 120.0(10) . . ? C30 N4 C34 119.8(8) . . ? C30 N4 Ni2 114.2(6) . . ? C34 N4 Ni2 125.9(6) . . ? C31 C30 N4 122.1(9) . . ? C31 C30 C29 124.8(9) . . ? N4 C30 C29 113.0(8) . . ? C30 C31 C32 118.8(9) . . ? C30 C31 H21 120.6 . . ? C32 C31 H21 120.6 . . ? C31 C32 C33 120.3(9) . . ? C31 C32 H22 119.8 . . ? C33 C32 H22 119.8 . . ? C32 C33 C34 119.4(9) . . ? C32 C33 H23 120.3 . . ? C34 C33 H23 120.3 . . ? N4 C34 C33 119.4(9) . . ? N4 C34 C36 120.4(9) . . ? C33 C34 C36 120.1(10) . . ? O3 C35 C40 118.2(10) . . ? O3 C35 C36 124.8(9) . . ? C40 C35 C36 117.0(10) . . ? C37 C36 C35 118.2(9) . . ? C37 C36 C34 119.6(10) . . ? C35 C36 C34 122.2(11) . . ? C38 C37 C36 123.8(11) . . ? C38 C37 H24 118.1 . . ? C36 C37 H24 118.1 . . ? C37 C38 C39 118.1(11) . . ? C37 C38 C41 121.7(12) . . ? C39 C38 C41 120.2(12) . . ? C40 C39 C38 120.4(11) . . ? C40 C39 H25 119.8 . . ? C38 C39 H25 119.8 . . ? C39 C40 C35 122.4(11) . . ? C39 C40 H26 118.8 . . ? C35 C40 H26 118.8 . . ? C35 O3 Ni2 118.5(6) . . ? C35 O3 Ni3 121.7(5) . . ? Ni2 O3 Ni3 98.7(3) . . ? C38 C41 H27 109.5 . . ? C38 C41 H28 109.5 . . ? H27 C41 H28 109.5 . . ? C38 C41 H29 109.5 . . ? H27 C41 H29 109.5 . . ? H28 C41 H29 109.5 . . ? O4 C42 C47 117.7(11) . . ? O4 C42 C43 123.9(8) . . ? C47 C42 C43 118.4(11) . . ? C44 C43 C42 116.8(10) . . ? C44 C43 C49 119.4(10) . . ? C42 C43 C49 123.6(10) . . ? C45 C44 C43 124.7(12) . . ? C45 C44 H30 117.7 . . ? C43 C44 H30 117.7 . . ? C44 C45 C46 119.2(13) . . ? C44 C45 C48 122.8(14) . . ? C46 C45 C48 117.9(13) . . ? C45 C46 C47 119.7(12) . . ? C45 C46 H31 120.1 . . ? C47 C46 H31 120.1 . . ? C42 C47 C46 121.2(12) . . ? C42 C47 H32 119.4 . . ? C46 C47 H32 119.4 . . ? C42 O4 Ni3 118.9(6) . . ? C42 O4 Ni2 121.0(5) . . ? Ni3 O4 Ni2 98.8(3) . . ? C45 C48 H33 109.5 . . ? C45 C48 H34 109.5 . . ? H33 C48 H34 109.5 . . ? C45 C48 H35 109.5 . . ? H33 C48 H35 109.5 . . ? H34 C48 H35 109.5 . . ? C53 N5 C49 122.6(8) . . ? C53 N5 Ni3 112.7(6) . . ? C49 N5 Ni3 124.3(6) . . ? N5 C49 C50 118.2(8) . . ? N5 C49 C43 120.7(9) . . ? C50 C49 C43 120.8(9) . . ? C51 C50 C49 120.0(9) . . ? C51 C50 H36 120.0 . . ? C49 C50 H36 120.0 . . ? C50 C51 C52 118.7(9) . . ? C50 C51 H37 120.7 . . ? C52 C51 H37 120.7 . . ? C53 C52 C51 119.9(9) . . ? C53 C52 H38 120.1 . . ? C51 C52 H38 120.1 . . ? N5 C53 C52 120.5(8) . . ? N5 C53 C54 116.2(8) . . ? C52 C53 C54 123.2(8) . . ? C54 N6 C58 119.9(7) . . ? C54 N6 Ni3 112.3(6) . . ? C58 N6 Ni3 127.4(6) . . ? N6 C54 C55 123.5(8) . . ? N6 C54 C53 115.3(7) . . ? C55 C54 C53 121.2(9) . . ? C54 C55 C56 117.8(9) . . ? C54 C55 H39 121.1 . . ? C56 C55 H39 121.1 . . ? C55 C56 C57 119.8(9) . . ? C55 C56 H40 120.1 . . ? C57 C56 H40 120.1 . . ? C58 C57 C56 119.4(9) . . ? C58 C57 H41 120.3 . . ? C56 C57 H41 120.3 . . ? N6 C58 C57 119.4(9) . . ? N6 C58 C60 121.3(8) . . ? C57 C58 C60 119.3(8) . . ? O5 C59 C64 120.5(9) . . ? O5 C59 C60 118.1(9) . . ? C64 C59 C60 121.4(9) . . ? C61 C60 C59 115.8(9) . . ? C61 C60 C58 117.9(9) . . ? C59 C60 C58 126.3(9) . . ? C60 C61 C62 121.8(10) . . ? C60 C61 H42 119.1 . . ? C62 C61 H42 119.1 . . ? C63 C62 C61 120.2(10) . . ? C63 C62 C65 122.3(11) . . ? C61 C62 C65 117.4(11) . . ? C64 C63 C62 119.4(11) . . ? C64 C63 H43 120.3 . . ? C62 C63 H43 120.3 . . ? C63 C64 C59 120.9(10) . . ? C63 C64 C66 118.1(10) . . ? C59 C64 C66 120.9(9) . . ? C59 O5 Ni4 124.3(5) . . ? C59 O5 Ni3 131.9(5) . . ? Ni4 O5 Ni3 102.0(3) . . ? C62 C65 H44 109.5 . . ? C62 C65 H45 109.5 . . ? H44 C65 H45 109.5 . . ? C62 C65 H46 109.5 . . ? H44 C65 H46 109.5 . . ? H45 C65 H46 109.5 . . ? C66 N7 C70 121.4(9) . . ? C66 N7 Ni4 126.5(7) . . ? C70 N7 Ni4 111.9(7) . . ? N7 C66 C67 118.2(10) . . ? N7 C66 C64 121.3(9) . . ? C67 C66 C64 120.5(10) . . ? C68 C67 C66 120.5(10) . . ? C68 C67 H47 119.8 . . ? C66 C67 H47 119.8 . . ? C69 C68 C67 121.0(10) . . ? C69 C68 H48 119.5 . . ? C67 C68 H48 119.5 . . ? C68 C69 C70 116.4(11) . . ? C68 C69 H49 121.8 . . ? C70 C69 H49 121.8 . . ? N7 C70 C69 122.4(10) . . ? N7 C70 C71 113.2(10) . . ? C69 C70 C71 124.3(11) . . ? C75 N8 C71 121.7(9) . . ? C75 N8 Ni4 125.7(8) . . ? C71 N8 Ni4 112.1(8) . . ? N8 C71 C72 120.1(12) . . ? N8 C71 C70 113.9(9) . . ? C72 C71 C70 126.0(12) . . ? C71 C72 C73 117.5(12) . . ? C71 C72 H50 121.2 . . ? C73 C72 H50 121.2 . . ? C74 C73 C72 122.8(11) . . ? C74 C73 H51 118.6 . . ? C72 C73 H51 118.6 . . ? C73 C74 C75 118.9(11) . . ? C73 C74 H52 120.5 . . ? C75 C74 H52 120.5 . . ? N8 C75 C74 119.0(10) . . ? N8 C75 C77 119.9(10) . . ? C74 C75 C77 121.2(12) . . ? O6 C76 C77 125.1(12) . . ? O6 C76 C81 116.5(12) . . ? C77 C76 C81 118.4(13) . . ? C78 C77 C76 117.6(13) . . ? C78 C77 C75 118.3(13) . . ? C76 C77 C75 124.1(12) . . ? C77 C78 C79 123.5(16) . . ? C77 C78 H53 118.3 . . ? C79 C78 H53 118.3 . . ? C78 C79 C80 119.9(16) . . ? C78 C79 C82 122(2) . . ? C80 C79 C82 118(2) . . ? C81 C80 C79 117.3(17) . . ? C81 C80 H54 121.4 . . ? C79 C80 H54 121.4 . . ? C80 C81 C76 123.2(15) . . ? C80 C81 H55 118.4 . . ? C76 C81 H55 118.4 . . ? C76 O6 Ni4 124.2(7) . . ? C76 O6 Ni3 137.7(6) . . ? Ni4 O6 Ni3 91.9(3) . . ? C79 C82 H56 109.5 . . ? C79 C82 H57 109.5 . . ? H56 C82 H57 109.5 . . ? C79 C82 H58 109.5 . . ? H56 C82 H58 109.5 . . ? H57 C82 H58 109.5 . . ? O7 C83 O8 115.2(10) . . ? O7 C83 C84 122.5(9) . . ? O8 C83 C84 122.2(9) . . ? C83 C84 H59 109.5 . . ? C83 C84 H60 109.5 . . ? H59 C84 H60 109.5 . . ? C83 C84 H61 109.5 . . ? H59 C84 H61 109.5 . . ? H60 C84 H61 109.5 . . ? O9 C85 O10 114.3(17) . . ? O9 C85 C86 121.3(16) . . ? O10 C85 C86 124.4(16) . . ? C85 C86 H62 109.5 . . ? C85 C86 H63 109.5 . . ? H62 C86 H63 109.5 . . ? C85 C86 H64 109.5 . . ? H62 C86 H64 109.5 . . ? H63 C86 H64 109.5 . . ? O11 C87 O12 115.4(16) . . ? O11 C87 C88 118.8(16) . . ? O12 C87 C88 124.5(17) . . ? C87 C88 H65 109.5 . . ? C87 C88 H66 109.5 . . ? H65 C88 H66 109.5 . . ? C87 C88 H67 109.5 . . ? H65 C88 H67 109.5 . . ? H66 C88 H67 109.5 . . ? O13 C89 O14 112.0(17) . . ? O13 C89 C90 118.8(16) . . ? O14 C89 C90 126.3(18) . . ? C89 C90 H68 109.5 . . ? C89 C90 H69 109.5 . . ? H68 C90 H69 109.5 . . ? C89 C90 H70 109.5 . . ? H68 C90 H70 109.5 . . ? H69 C90 H70 109.5 . . ? O15 C91 O16 114.1(18) . . ? O15 C91 C92 118.1(17) . . ? O16 C91 C92 124.4(18) . . ? C91 C92 H71 109.5 . . ? C91 C92 H72 109.5 . . ? H71 C92 H72 109.5 . . ? C91 C92 H73 109.5 . . ? H71 C92 H73 109.5 . . ? H72 C92 H73 109.5 . . ? 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 O1 Ni1 Ni2 N4 16.9(4) . . . . ? O2 Ni1 Ni2 N4 155.1(4) . . . . ? N1 Ni1 Ni2 N4 -39.4(5) . . . . ? N2 Ni1 Ni2 N4 -169.8(4) . . . . ? O1 Ni1 Ni2 O3 97.8(3) . . . . ? O2 Ni1 Ni2 O3 -124.0(4) . . . . ? N1 Ni1 Ni2 O3 41.5(4) . . . . ? N2 Ni1 Ni2 O3 -88.9(4) . . . . ? O1 Ni1 Ni2 O2 -138.3(4) . . . . ? N1 Ni1 Ni2 O2 165.5(5) . . . . ? N2 Ni1 Ni2 O2 35.0(4) . . . . ? O1 Ni1 Ni2 N3 -86.8(4) . . . . ? O2 Ni1 Ni2 N3 51.5(4) . . . . ? N1 Ni1 Ni2 N3 -143.0(4) . . . . ? N2 Ni1 Ni2 N3 86.5(4) . . . . ? O1 Ni1 Ni2 O4 166.4(3) . . . . ? O2 Ni1 Ni2 O4 -55.3(4) . . . . ? N1 Ni1 Ni2 O4 110.2(4) . . . . ? N2 Ni1 Ni2 O4 -20.3(4) . . . . ? O2 Ni1 Ni2 O1 138.3(4) . . . . ? N1 Ni1 Ni2 O1 -56.3(4) . . . . ? N2 Ni1 Ni2 O1 173.3(4) . . . . ? O4 Ni3 Ni4 O6 -96.0(3) . . . . ? O5 Ni3 Ni4 O6 138.2(4) . . . . ? N5 Ni3 Ni4 O6 -14.0(4) . . . . ? N6 Ni3 Ni4 O6 87.9(3) . . . . ? O3 Ni3 Ni4 O6 -165.1(3) . . . . ? O4 Ni3 Ni4 O5 125.8(4) . . . . ? N5 Ni3 Ni4 O5 -152.3(4) . . . . ? N6 Ni3 Ni4 O5 -50.3(4) . . . . ? O3 Ni3 Ni4 O5 56.7(3) . . . . ? O6 Ni3 Ni4 O5 -138.2(4) . . . . ? O4 Ni3 Ni4 N8 -39.6(5) . . . . ? O5 Ni3 Ni4 N8 -165.4(5) . . . . ? N5 Ni3 Ni4 N8 42.3(5) . . . . ? N6 Ni3 Ni4 N8 144.3(5) . . . . ? O3 Ni3 Ni4 N8 -108.7(4) . . . . ? O6 Ni3 Ni4 N8 56.3(5) . . . . ? O4 Ni3 Ni4 N7 90.2(4) . . . . ? O5 Ni3 Ni4 N7 -35.6(4) . . . . ? N5 Ni3 Ni4 N7 172.1(4) . . . . ? N6 Ni3 Ni4 N7 -85.9(4) . . . . ? O3 Ni3 Ni4 N7 21.1(3) . . . . ? O6 Ni3 Ni4 N7 -173.8(4) . . . . ? O1 C1 C2 C3 178.1(10) . . . . ? C6 C1 C2 C3 -0.9(14) . . . . ? O1 C1 C2 C8 -0.8(15) . . . . ? C6 C1 C2 C8 -179.8(8) . . . . ? C1 C2 C3 C4 -1(2) . . . . ? C8 C2 C3 C4 177.8(13) . . . . ? C2 C3 C4 C5 3(2) . . . . ? C2 C3 C4 C7 176.1(15) . . . . ? C3 C4 C5 C6 -2(2) . . . . ? C7 C4 C5 C6 -175.8(14) . . . . ? C4 C5 C6 C1 0.5(19) . . . . ? O1 C1 C6 C5 -177.8(10) . . . . ? C2 C1 C6 C5 1.2(14) . . . . ? C2 C1 O1 Ni1 12.9(13) . . . . ? C6 C1 O1 Ni1 -168.2(5) . . . . ? C2 C1 O1 Ni2 -127.8(8) . . . . ? C6 C1 O1 Ni2 51.1(12) . . . . ? O2 Ni1 O1 C1 -179.9(7) . . . . ? N1 Ni1 O1 C1 -11.3(7) . . . . ? N2 Ni1 O1 C1 139(3) . . . . ? Ni2 Ni1 O1 C1 -153.7(8) . . . . ? O2 Ni1 O1 Ni2 -26.2(2) . . . . ? N1 Ni1 O1 Ni2 142.4(3) . . . . ? N2 Ni1 O1 Ni2 -67(3) . . . . ? N4 Ni2 O1 C1 -19.4(9) . . . . ? O3 Ni2 O1 C1 72.0(9) . . . . ? O2 Ni2 O1 C1 173.9(10) . . . . ? N3 Ni2 O1 C1 -105.0(9) . . . . ? O4 Ni2 O1 C1 111.5(11) . . . . ? Ni1 Ni2 O1 C1 148.4(10) . . . . ? N4 Ni2 O1 Ni1 -167.8(3) . . . . ? O3 Ni2 O1 Ni1 -76.4(3) . . . . ? O2 Ni2 O1 Ni1 25.5(2) . . . . ? N3 Ni2 O1 Ni1 106.6(3) . . . . ? O4 Ni2 O1 Ni1 -36.9(9) . . . . ? O1 Ni1 N1 C8 0.4(8) . . . . ? O2 Ni1 N1 C8 96.4(19) . . . . ? N2 Ni1 N1 C8 -176.8(8) . . . . ? Ni2 Ni1 N1 C8 40.2(9) . . . . ? O1 Ni1 N1 C12 -173.1(5) . . . . ? O2 Ni1 N1 C12 -77.1(18) . . . . ? N2 Ni1 N1 C12 9.7(6) . . . . ? Ni2 Ni1 N1 C12 -133.3(5) . . . . ? C12 N1 C8 C9 1.2(13) . . . . ? Ni1 N1 C8 C9 -171.7(6) . . . . ? C12 N1 C8 C2 -177.7(7) . . . . ? Ni1 N1 C8 C2 9.4(12) . . . . ? C1 C2 C8 N1 -10.5(14) . . . . ? C3 C2 C8 N1 170.5(10) . . . . ? C1 C2 C8 C9 170.6(9) . . . . ? C3 C2 C8 C9 -8.3(15) . . . . ? N1 C8 C9 C10 -3.6(15) . . . . ? C2 C8 C9 C10 175.3(10) . . . . ? C8 C9 C10 C11 3.4(17) . . . . ? C9 C10 C11 C12 -0.6(16) . . . . ? C10 C11 C12 N1 -1.7(14) . . . . ? C10 C11 C12 C13 -178.4(9) . . . . ? C8 N1 C12 C11 1.4(12) . . . . ? Ni1 N1 C12 C11 175.4(7) . . . . ? C8 N1 C12 C13 178.4(8) . . . . ? Ni1 N1 C12 C13 -7.6(9) . . . . ? O1 Ni1 N2 C17 24(3) . . . . ? O2 Ni1 N2 C17 -16.8(7) . . . . ? N1 Ni1 N2 C17 174.6(7) . . . . ? Ni2 Ni1 N2 C17 -39.1(8) . . . . ? O1 Ni1 N2 C13 -161(3) . . . . ? O2 Ni1 N2 C13 158.2(6) . . . . ? N1 Ni1 N2 C13 -10.3(6) . . . . ? Ni2 Ni1 N2 C13 136.0(5) . . . . ? C17 N2 C13 C14 2.5(13) . . . . ? Ni1 N2 C13 C14 -172.9(7) . . . . ? C17 N2 C13 C12 -176.5(7) . . . . ? Ni1 N2 C13 C12 8.2(9) . . . . ? C11 C12 C13 N2 176.6(8) . . . . ? N1 C12 C13 N2 -0.3(11) . . . . ? C11 C12 C13 C14 -2.3(14) . . . . ? N1 C12 C13 C14 -179.3(8) . . . . ? N2 C13 C14 C15 1.0(14) . . . . ? C12 C13 C14 C15 179.8(8) . . . . ? C13 C14 C15 C16 -2.7(14) . . . . ? C14 C15 C16 C17 1.1(13) . . . . ? C13 N2 C17 C16 -4.0(12) . . . . ? Ni1 N2 C17 C16 170.8(6) . . . . ? C13 N2 C17 C19 175.5(7) . . . . ? Ni1 N2 C17 C19 -9.7(12) . . . . ? C15 C16 C17 N2 2.3(13) . . . . ? C15 C16 C17 C19 -177.2(8) . . . . ? O2 C18 C19 C20 -174.0(8) . . . . ? C23 C18 C19 C20 2.1(14) . . . . ? O2 C18 C19 C17 5.5(14) . . . . ? C23 C18 C19 C17 -178.5(9) . . . . ? N2 C17 C19 C18 21.2(13) . . . . ? C16 C17 C19 C18 -159.3(9) . . . . ? N2 C17 C19 C20 -159.4(9) . . . . ? C16 C17 C19 C20 20.1(13) . . . . ? C18 C19 C20 C21 2.5(14) . . . . ? C17 C19 C20 C21 -176.9(9) . . . . ? C19 C20 C21 C22 -4.6(14) . . . . ? C19 C20 C21 C24 176.9(9) . . . . ? C20 C21 C22 C23 2.3(15) . . . . ? C24 C21 C22 C23 -179.2(9) . . . . ? C21 C22 C23 C18 2.0(14) . . . . ? C21 C22 C23 C25 -176.2(9) . . . . ? O2 C18 C23 C22 171.9(8) . . . . ? C19 C18 C23 C22 -4.2(14) . . . . ? O2 C18 C23 C25 -10.2(14) . . . . ? C19 C18 C23 C25 173.8(9) . . . . ? C19 C18 O2 Ni1 -42.8(12) . . . . ? C23 C18 O2 Ni1 141.0(7) . . . . ? C19 C18 O2 Ni2 159.6(7) . . . . ? C23 C18 O2 Ni2 -16.6(13) . . . . ? O1 Ni1 O2 C18 -132.6(8) . . . . ? N1 Ni1 O2 C18 129.9(17) . . . . ? N2 Ni1 O2 C18 43.6(8) . . . . ? Ni2 Ni1 O2 C18 -163.4(9) . . . . ? O1 Ni1 O2 Ni2 30.7(3) . . . . ? N1 Ni1 O2 Ni2 -66.7(18) . . . . ? N2 Ni1 O2 Ni2 -153.0(3) . . . . ? N4 Ni2 O2 C18 90.4(12) . . . . ? O3 Ni2 O2 C18 -143.8(8) . . . . ? N3 Ni2 O2 C18 27.4(8) . . . . ? O4 Ni2 O2 C18 -61.2(8) . . . . ? O1 Ni2 O2 C18 135.2(9) . . . . ? Ni1 Ni2 O2 C18 161.0(10) . . . . ? N4 Ni2 O2 Ni1 -70.6(9) . . . . ? O3 Ni2 O2 Ni1 55.2(3) . . . . ? N3 Ni2 O2 Ni1 -133.6(3) . . . . ? O4 Ni2 O2 Ni1 137.7(3) . . . . ? O1 Ni2 O2 Ni1 -25.8(2) . . . . ? N4 Ni2 N3 C25 175.6(8) . . . . ? O3 Ni2 N3 C25 106.7(16) . . . . ? O2 Ni2 N3 C25 -21.2(8) . . . . ? O4 Ni2 N3 C25 80.3(8) . . . . ? O1 Ni2 N3 C25 -88.9(8) . . . . ? Ni1 Ni2 N3 C25 -49.5(8) . . . . ? N4 Ni2 N3 C29 9.1(7) . . . . ? O3 Ni2 N3 C29 -60(2) . . . . ? O2 Ni2 N3 C29 172.2(7) . . . . ? O4 Ni2 N3 C29 -86.2(7) . . . . ? O1 Ni2 N3 C29 104.6(7) . . . . ? Ni1 Ni2 N3 C29 144.0(6) . . . . ? C29 N3 C25 C26 -4.9(15) . . . . ? Ni2 N3 C25 C26 -170.6(8) . . . . ? C29 N3 C25 C23 173.0(9) . . . . ? Ni2 N3 C25 C23 7.3(13) . . . . ? C22 C23 C25 N3 -167.6(9) . . . . ? C18 C23 C25 N3 14.4(15) . . . . ? C22 C23 C25 C26 10.3(14) . . . . ? C18 C23 C25 C26 -167.7(10) . . . . ? N3 C25 C26 C27 1.2(17) . . . . ? C23 C25 C26 C27 -176.7(11) . . . . ? C25 C26 C27 C28 3(2) . . . . ? C26 C27 C28 C29 -3(2) . . . . ? C25 N3 C29 C28 4.5(16) . . . . ? Ni2 N3 C29 C28 172.7(10) . . . . ? C25 N3 C29 C30 -177.0(9) . . . . ? Ni2 N3 C29 C30 -8.9(11) . . . . ? C27 C28 C29 N3 -0.4(19) . . . . ? C27 C28 C29 C30 -178.7(11) . . . . ? O3 Ni2 N4 C30 161.9(6) . . . . ? O2 Ni2 N4 C30 -71.3(12) . . . . ? N3 Ni2 N4 C30 -7.8(7) . . . . ? O4 Ni2 N4 C30 80.9(7) . . . . ? O1 Ni2 N4 C30 -112.9(6) . . . . ? Ni1 Ni2 N4 C30 -123.2(6) . . . . ? O3 Ni2 N4 C34 -14.2(8) . . . . ? O2 Ni2 N4 C34 112.6(10) . . . . ? N3 Ni2 N4 C34 176.1(8) . . . . ? O4 Ni2 N4 C34 -95.2(7) . . . . ? O1 Ni2 N4 C34 71.0(8) . . . . ? Ni1 Ni2 N4 C34 60.7(8) . . . . ? C34 N4 C30 C31 3.3(15) . . . . ? Ni2 N4 C30 C31 -173.1(8) . . . . ? C34 N4 C30 C29 -178.7(8) . . . . ? Ni2 N4 C30 C29 5.0(10) . . . . ? N3 C29 C30 C31 -179.2(10) . . . . ? C28 C29 C30 C31 -0.7(17) . . . . ? N3 C29 C30 N4 2.8(13) . . . . ? C28 C29 C30 N4 -178.7(10) . . . . ? N4 C30 C31 C32 0.3(15) . . . . ? C29 C30 C31 C32 -177.5(9) . . . . ? C30 C31 C32 C33 -1.8(15) . . . . ? C31 C32 C33 C34 -0.1(15) . . . . ? C30 N4 C34 C33 -5.1(14) . . . . ? Ni2 N4 C34 C33 170.7(7) . . . . ? C30 N4 C34 C36 170.1(9) . . . . ? Ni2 N4 C34 C36 -14.1(13) . . . . ? C32 C33 C34 N4 3.6(14) . . . . ? C32 C33 C34 C36 -171.6(9) . . . . ? O3 C35 C36 C37 179.8(8) . . . . ? C40 C35 C36 C37 -0.2(12) . . . . ? O3 C35 C36 C34 2.5(13) . . . . ? C40 C35 C36 C34 -177.5(8) . . . . ? N4 C34 C36 C37 -150.6(9) . . . . ? C33 C34 C36 C37 24.5(13) . . . . ? N4 C34 C36 C35 26.6(13) . . . . ? C33 C34 C36 C35 -158.2(9) . . . . ? C35 C36 C37 C38 0.4(15) . . . . ? C34 C36 C37 C38 177.8(9) . . . . ? C36 C37 C38 C39 0.6(17) . . . . ? C36 C37 C38 C41 -179.6(10) . . . . ? C37 C38 C39 C40 -1.8(16) . . . . ? C41 C38 C39 C40 178.4(9) . . . . ? C38 C39 C40 C35 2.0(15) . . . . ? O3 C35 C40 C39 179.0(8) . . . . ? C36 C35 C40 C39 -1.0(13) . . . . ? C40 C35 O3 Ni2 140.9(6) . . . . ? C36 C35 O3 Ni2 -39.1(10) . . . . ? C40 C35 O3 Ni3 -96.4(8) . . . . ? C36 C35 O3 Ni3 83.6(10) . . . . ? N4 Ni2 O3 C35 39.0(6) . . . . ? O2 Ni2 O3 C35 -125.8(5) . . . . ? N3 Ni2 O3 C35 107.2(17) . . . . ? O4 Ni2 O3 C35 133.9(5) . . . . ? O1 Ni2 O3 C35 -57.7(5) . . . . ? Ni1 Ni2 O3 C35 -95.2(5) . . . . ? N4 Ni2 O3 Ni3 -94.6(3) . . . . ? O2 Ni2 O3 Ni3 100.6(3) . . . . ? N3 Ni2 O3 Ni3 -26.4(18) . . . . ? O4 Ni2 O3 Ni3 0.3(2) . . . . ? O1 Ni2 O3 Ni3 168.7(3) . . . . ? Ni1 Ni2 O3 Ni3 131.2(2) . . . . ? O4 Ni3 O3 C35 -131.9(7) . . . . ? O5 Ni3 O3 C35 -33.7(7) . . . . ? N5 Ni3 O3 C35 135.9(7) . . . . ? N6 Ni3 O3 C35 53.3(7) . . . . ? O6 Ni3 O3 C35 -94.9(9) . . . . ? Ni4 Ni3 O3 C35 -64.8(7) . . . . ? O4 Ni3 O3 Ni2 -0.4(3) . . . . ? O5 Ni3 O3 Ni2 97.8(2) . . . . ? N5 Ni3 O3 Ni2 -92.6(3) . . . . ? N6 Ni3 O3 Ni2 -175.2(3) . . . . ? O6 Ni3 O3 Ni2 36.7(8) . . . . ? Ni4 Ni3 O3 Ni2 66.8(3) . . . . ? O4 C42 C43 C44 -178.8(8) . . . . ? C47 C42 C43 C44 0.0(13) . . . . ? O4 C42 C43 C49 -4.1(14) . . . . ? C47 C42 C43 C49 174.6(8) . . . . ? C42 C43 C44 C45 -1.3(15) . . . . ? C49 C43 C44 C45 -176.2(10) . . . . ? C43 C44 C45 C46 1.7(18) . . . . ? C43 C44 C45 C48 177.9(10) . . . . ? C44 C45 C46 C47 -0.8(18) . . . . ? C48 C45 C46 C47 -177.1(10) . . . . ? O4 C42 C47 C46 179.7(9) . . . . ? C43 C42 C47 C46 0.8(13) . . . . ? C45 C46 C47 C42 -0.4(16) . . . . ? C47 C42 O4 Ni3 -139.7(7) . . . . ? C43 C42 O4 Ni3 39.1(11) . . . . ? C47 C42 O4 Ni2 98.0(8) . . . . ? C43 C42 O4 Ni2 -83.2(10) . . . . ? O5 Ni3 O4 C42 126.2(6) . . . . ? N5 Ni3 O4 C42 -37.4(6) . . . . ? N6 Ni3 O4 C42 -103.3(18) . . . . ? O3 Ni3 O4 C42 -132.5(6) . . . . ? O6 Ni3 O4 C42 58.5(6) . . . . ? Ni4 Ni3 O4 C42 96.5(5) . . . . ? O5 Ni3 O4 Ni2 -100.9(3) . . . . ? N5 Ni3 O4 Ni2 95.4(3) . . . . ? N6 Ni3 O4 Ni2 29.5(18) . . . . ? O3 Ni3 O4 Ni2 0.3(2) . . . . ? O6 Ni3 O4 Ni2 -168.6(3) . . . . ? Ni4 Ni3 O4 Ni2 -130.7(2) . . . . ? N4 Ni2 O4 C42 -137.7(7) . . . . ? O3 Ni2 O4 C42 131.2(7) . . . . ? O2 Ni2 O4 C42 33.5(7) . . . . ? N3 Ni2 O4 C42 -53.7(7) . . . . ? O1 Ni2 O4 C42 91.2(10) . . . . ? Ni1 Ni2 O4 C42 64.0(7) . . . . ? N4 Ni2 O4 Ni3 90.8(3) . . . . ? O3 Ni2 O4 Ni3 -0.4(3) . . . . ? O2 Ni2 O4 Ni3 -98.0(3) . . . . ? N3 Ni2 O4 Ni3 174.7(3) . . . . ? O1 Ni2 O4 Ni3 -40.3(9) . . . . ? Ni1 Ni2 O4 Ni3 -67.5(3) . . . . ? O4 Ni3 N5 C53 -161.8(6) . . . . ? O5 Ni3 N5 C53 70.1(10) . . . . ? N6 Ni3 N5 C53 8.4(6) . . . . ? O3 Ni3 N5 C53 -79.9(6) . . . . ? O6 Ni3 N5 C53 114.3(6) . . . . ? Ni4 Ni3 N5 C53 122.9(6) . . . . ? O4 Ni3 N5 C49 10.9(7) . . . . ? O5 Ni3 N5 C49 -117.2(9) . . . . ? N6 Ni3 N5 C49 -178.9(8) . . . . ? O3 Ni3 N5 C49 92.7(7) . . . . ? O6 Ni3 N5 C49 -73.0(7) . . . . ? Ni4 Ni3 N5 C49 -64.4(8) . . . . ? C53 N5 C49 C50 2.2(14) . . . . ? Ni3 N5 C49 C50 -169.7(7) . . . . ? C53 N5 C49 C43 -171.6(9) . . . . ? Ni3 N5 C49 C43 16.4(12) . . . . ? C44 C43 C49 N5 148.0(9) . . . . ? C42 C43 C49 N5 -26.6(14) . . . . ? C44 C43 C49 C50 -25.8(13) . . . . ? C42 C43 C49 C50 159.7(9) . . . . ? N5 C49 C50 C51 -0.2(14) . . . . ? C43 C49 C50 C51 173.7(9) . . . . ? C49 C50 C51 C52 -0.9(15) . . . . ? C50 C51 C52 C53 0.1(16) . . . . ? C49 N5 C53 C52 -3.1(15) . . . . ? Ni3 N5 C53 C52 169.7(8) . . . . ? C49 N5 C53 C54 179.0(9) . . . . ? Ni3 N5 C53 C54 -8.2(11) . . . . ? C51 C52 C53 N5 1.9(15) . . . . ? C51 C52 C53 C54 179.7(10) . . . . ? O4 Ni3 N6 C54 60(2) . . . . ? O5 Ni3 N6 C54 -169.0(7) . . . . ? N5 Ni3 N6 C54 -7.1(7) . . . . ? O3 Ni3 N6 C54 88.5(7) . . . . ? O6 Ni3 N6 C54 -101.5(7) . . . . ? Ni4 Ni3 N6 C54 -141.3(6) . . . . ? O4 Ni3 N6 C58 -112.6(17) . . . . ? O5 Ni3 N6 C58 18.7(7) . . . . ? N5 Ni3 N6 C58 -179.4(8) . . . . ? O3 Ni3 N6 C58 -83.8(7) . . . . ? O6 Ni3 N6 C58 86.2(8) . . . . ? Ni4 Ni3 N6 C58 46.4(8) . . . . ? C58 N6 C54 C55 -5.5(16) . . . . ? Ni3 N6 C54 C55 -178.4(9) . . . . ? C58 N6 C54 C53 177.7(8) . . . . ? Ni3 N6 C54 C53 4.7(11) . . . . ? N5 C53 C54 N6 2.4(14) . . . . ? C52 C53 C54 N6 -175.5(9) . . . . ? N5 C53 C54 C55 -174.6(10) . . . . ? C52 C53 C54 C55 7.6(16) . . . . ? N6 C54 C55 C56 2.3(18) . . . . ? C53 C54 C55 C56 179.0(11) . . . . ? C54 C55 C56 C57 2.0(19) . . . . ? C55 C56 C57 C58 -3.1(18) . . . . ? C54 N6 C58 C57 4.2(14) . . . . ? Ni3 N6 C58 C57 176.0(7) . . . . ? C54 N6 C58 C60 -173.7(9) . . . . ? Ni3 N6 C58 C60 -2.0(12) . . . . ? C56 C57 C58 N6 0.0(16) . . . . ? C56 C57 C58 C60 177.9(10) . . . . ? O5 C59 C60 C61 -171.4(8) . . . . ? C64 C59 C60 C61 7.6(14) . . . . ? O5 C59 C60 C58 9.1(14) . . . . ? C64 C59 C60 C58 -171.9(9) . . . . ? N6 C58 C60 C61 162.5(8) . . . . ? C57 C58 C60 C61 -15.4(13) . . . . ? N6 C58 C60 C59 -18.0(14) . . . . ? C57 C58 C60 C59 164.1(9) . . . . ? C59 C60 C61 C62 -5.8(14) . . . . ? C58 C60 C61 C62 173.7(9) . . . . ? C60 C61 C62 C63 0.8(16) . . . . ? C60 C61 C62 C65 178.7(9) . . . . ? C61 C62 C63 C64 2.8(16) . . . . ? C65 C62 C63 C64 -175.0(10) . . . . ? C62 C63 C64 C59 -1.0(16) . . . . ? C62 C63 C64 C66 177.1(9) . . . . ? O5 C59 C64 C63 174.6(9) . . . . ? C60 C59 C64 C63 -4.4(15) . . . . ? O5 C59 C64 C66 -3.4(14) . . . . ? C60 C59 C64 C66 177.6(9) . . . . ? C64 C59 O5 Ni4 39.9(12) . . . . ? C60 C59 O5 Ni4 -141.0(7) . . . . ? C64 C59 O5 Ni3 -158.3(7) . . . . ? C60 C59 O5 Ni3 20.8(13) . . . . ? O6 Ni4 O5 C59 135.3(8) . . . . ? N8 Ni4 O5 C59 -124.5(19) . . . . ? N7 Ni4 O5 C59 -41.5(8) . . . . ? Ni3 Ni4 O5 C59 166.2(9) . . . . ? O6 Ni4 O5 Ni3 -31.0(3) . . . . ? N8 Ni4 O5 Ni3 69(2) . . . . ? N7 Ni4 O5 Ni3 152.2(3) . . . . ? O4 Ni3 O5 C59 141.9(8) . . . . ? N5 Ni3 O5 C59 -91.0(11) . . . . ? N6 Ni3 O5 C59 -30.0(8) . . . . ? O3 Ni3 O5 C59 58.5(8) . . . . ? O6 Ni3 O5 C59 -138.7(9) . . . . ? Ni4 Ni3 O5 C59 -164.7(10) . . . . ? O4 Ni3 O5 Ni4 -53.4(3) . . . . ? N5 Ni3 O5 Ni4 73.7(8) . . . . ? N6 Ni3 O5 Ni4 134.7(3) . . . . ? O3 Ni3 O5 Ni4 -136.8(3) . . . . ? O6 Ni3 O5 Ni4 25.9(2) . . . . ? O6 Ni4 N7 C66 -16(3) . . . . ? O5 Ni4 N7 C66 17.2(7) . . . . ? N8 Ni4 N7 C66 -173.9(7) . . . . ? Ni3 Ni4 N7 C66 39.6(8) . . . . ? O6 Ni4 N7 C70 168(3) . . . . ? O5 Ni4 N7 C70 -158.0(6) . . . . ? N8 Ni4 N7 C70 10.9(6) . . . . ? Ni3 Ni4 N7 C70 -135.6(5) . . . . ? C70 N7 C66 C67 1.5(12) . . . . ? Ni4 N7 C66 C67 -173.3(6) . . . . ? C70 N7 C66 C64 -176.9(7) . . . . ? Ni4 N7 C66 C64 8.3(11) . . . . ? C63 C64 C66 N7 161.3(9) . . . . ? C59 C64 C66 N7 -20.6(13) . . . . ? C63 C64 C66 C67 -17.1(13) . . . . ? C59 C64 C66 C67 161.0(9) . . . . ? N7 C66 C67 C68 0.9(13) . . . . ? C64 C66 C67 C68 179.4(8) . . . . ? C66 C67 C68 C69 -3.1(14) . . . . ? C67 C68 C69 C70 2.7(15) . . . . ? C66 N7 C70 C69 -1.9(13) . . . . ? Ni4 N7 C70 C69 173.6(7) . . . . ? C66 N7 C70 C71 176.8(8) . . . . ? Ni4 N7 C70 C71 -7.7(9) . . . . ? C68 C69 C70 N7 -0.2(14) . . . . ? C68 C69 C70 C71 -178.8(9) . . . . ? O6 Ni4 N8 C75 -0.9(7) . . . . ? O5 Ni4 N8 C75 -100(2) . . . . ? N7 Ni4 N8 C75 176.9(7) . . . . ? Ni3 Ni4 N8 C75 -41.1(9) . . . . ? O6 Ni4 N8 C71 170.5(6) . . . . ? O5 Ni4 N8 C71 72(2) . . . . ? N7 Ni4 N8 C71 -11.7(6) . . . . ? Ni3 Ni4 N8 C71 130.3(5) . . . . ? C75 N8 C71 C72 -0.3(13) . . . . ? Ni4 N8 C71 C72 -172.0(7) . . . . ? C75 N8 C71 C70 -178.2(8) . . . . ? Ni4 N8 C71 C70 10.1(9) . . . . ? N7 C70 C71 N8 -1.4(11) . . . . ? C69 C70 C71 N8 177.2(8) . . . . ? N7 C70 C71 C72 -179.2(9) . . . . ? C69 C70 C71 C72 -0.6(15) . . . . ? N8 C71 C72 C73 1.3(14) . . . . ? C70 C71 C72 C73 179.0(10) . . . . ? C71 C72 C73 C74 -0.7(17) . . . . ? C72 C73 C74 C75 -0.9(17) . . . . ? C71 N8 C75 C74 -1.4(13) . . . . ? Ni4 N8 C75 C74 169.2(6) . . . . ? C71 N8 C75 C77 176.9(8) . . . . ? Ni4 N8 C75 C77 -12.5(12) . . . . ? C73 C74 C75 N8 2.0(15) . . . . ? C73 C74 C75 C77 -176.3(9) . . . . ? O6 C76 C77 C78 177.4(9) . . . . ? C81 C76 C77 C78 -2.4(14) . . . . ? O6 C76 C77 C75 -3.2(14) . . . . ? C81 C76 C77 C75 176.9(8) . . . . ? N8 C75 C77 C78 -164.1(10) . . . . ? C74 C75 C77 C78 14.2(14) . . . . ? N8 C75 C77 C76 16.6(13) . . . . ? C74 C75 C77 C76 -165.1(9) . . . . ? C76 C77 C78 C79 3.2(18) . . . . ? C75 C77 C78 C79 -176.2(12) . . . . ? C77 C78 C79 C80 -1(2) . . . . ? C77 C78 C79 C82 -179.1(12) . . . . ? C78 C79 C80 C81 -1(2) . . . . ? C82 C79 C80 C81 176.4(12) . . . . ? C79 C80 C81 C76 2(2) . . . . ? O6 C76 C81 C80 179.9(10) . . . . ? C77 C76 C81 C80 -0.2(15) . . . . ? C77 C76 O6 Ni4 -13.2(12) . . . . ? C81 C76 O6 Ni4 166.6(6) . . . . ? C77 C76 O6 Ni3 130.5(8) . . . . ? C81 C76 O6 Ni3 -49.6(13) . . . . ? O5 Ni4 O6 C76 -177.4(7) . . . . ? N8 Ni4 O6 C76 13.7(7) . . . . ? N7 Ni4 O6 C76 -144(3) . . . . ? Ni3 Ni4 O6 C76 156.5(8) . . . . ? O5 Ni4 O6 Ni3 26.1(2) . . . . ? N8 Ni4 O6 Ni3 -142.9(2) . . . . ? N7 Ni4 O6 Ni3 60(3) . . . . ? O4 Ni3 O6 C76 -73.2(9) . . . . ? O5 Ni3 O6 C76 -176.1(10) . . . . ? N5 Ni3 O6 C76 19.1(10) . . . . ? N6 Ni3 O6 C76 103.3(9) . . . . ? O3 Ni3 O6 C76 -110.0(11) . . . . ? Ni4 Ni3 O6 C76 -150.7(10) . . . . ? O4 Ni3 O6 Ni4 77.5(3) . . . . ? O5 Ni3 O6 Ni4 -25.4(2) . . . . ? N5 Ni3 O6 Ni4 169.8(3) . . . . ? N6 Ni3 O6 Ni4 -106.0(3) . . . . ? O3 Ni3 O6 Ni4 40.7(8) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.457 _refine_diff_density_min -0.765 _refine_diff_density_rms 0.083 _database_code_depnum_ccdc_archive 'CCDC 938300' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_(LH)2Fe2 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common '[(LH)2Fe2Cl2](MeCN)2' _chemical_melting_point ? _chemical_formula_moiety C86H66Cl2Fe2N10O6 _chemical_formula_sum 'C86 H66 Cl2 Fe2 N10 O6' _chemical_formula_weight 1518.09 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 '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 9.8836(7) _cell_length_b 12.5381(7) _cell_length_c 16.4708(9) _cell_angle_alpha 66.5380(17) _cell_angle_beta 70.356(3) _cell_angle_gamma 82.489(2) _cell_volume 1763.36(19) _cell_formula_units_Z 1 _cell_measurement_temperature 120 _cell_measurement_reflns_used 13941 _cell_measurement_theta_min 2.99 _cell_measurement_theta_max 25.00 _exptl_crystal_description prismatic _exptl_crystal_colour brown _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.430 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 786 _exptl_absorpt_coefficient_mu 0.553 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9216 _exptl_absorpt_correction_T_max 0.9467 _exptl_absorpt_process_details 'Rapid AUTO (Rigaku Corp.)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120 _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku R-AXIS Rapid' _diffrn_measurement_method IP _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 13941 _diffrn_reflns_av_R_equivalents 0.0485 _diffrn_reflns_av_sigmaI/netI 0.0703 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.99 _diffrn_reflns_theta_max 25.00 _reflns_number_total 6179 _reflns_number_gt 3888 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Rapid AUTO (Rigaku Corp.)' _computing_cell_refinement 'Rapid AUTO (Rigaku Corp.)' _computing_data_reduction 'Rapid AUTO (Rigaku Corp.)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ORTEP-3 _computing_publication_material ORTEP-3 _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^)+(0.0193P)^2^+5.8927P] 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 6179 _refine_ls_number_parameters 512 _refine_ls_number_restraints 36 _refine_ls_R_factor_all 0.1037 _refine_ls_R_factor_gt 0.0504 _refine_ls_wR_factor_ref 0.1370 _refine_ls_wR_factor_gt 0.0982 _refine_ls_goodness_of_fit_ref 1.035 _refine_ls_restrained_S_all 1.037 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.54813(7) 0.47604(6) 0.09180(4) 0.02762(18) Uani 1 1 d . . . Cl1 Cl 0.60631(12) 0.58052(10) 0.16279(8) 0.0354(3) Uani 1 1 d . . . C1 C 0.5894(5) 0.7033(4) -0.0544(3) 0.0304(11) Uani 1 1 d . . . C2 C 0.7404(5) 0.6954(4) -0.0891(3) 0.0321(11) Uani 1 1 d . . . C3 C 0.8206(6) 0.7993(4) -0.1369(3) 0.0412(12) Uani 1 1 d . . . H1 H 0.9223 0.7949 -0.1601 0.049 Uiso 1 1 calc R . . C4 C 0.7576(6) 0.9076(4) -0.1513(4) 0.0448(13) Uani 1 1 d . . . C5 C 0.6100(6) 0.9127(4) -0.1158(4) 0.0440(13) Uani 1 1 d . . . H2 H 0.5649 0.9864 -0.1244 0.053 Uiso 1 1 calc R . . C6 C 0.5255(6) 0.8122(4) -0.0675(3) 0.0374(12) Uani 1 1 d . . . H3 H 0.4242 0.8180 -0.0435 0.045 Uiso 1 1 calc R . . O1 O 0.5051(3) 0.6073(2) -0.01129(19) 0.0253(7) Uani 1 1 d . . . C7 C 0.8497(7) 1.0169(5) -0.2045(4) 0.0656(18) Uani 1 1 d . . . H4 H 0.7889 1.0845 -0.2236 0.098 Uiso 1 1 calc R . . H5 H 0.9225 1.0100 -0.2598 0.098 Uiso 1 1 calc R . . H6 H 0.8973 1.0265 -0.1643 0.098 Uiso 1 1 calc R . . N1 N 0.7600(4) 0.4876(3) -0.0017(2) 0.0300(9) Uani 1 1 d . . . C8 C 0.8169(5) 0.5840(4) -0.0766(3) 0.0308(11) Uani 1 1 d . . . C9 C 0.9511(5) 0.5772(4) -0.1397(3) 0.0375(12) Uani 1 1 d . . . H7 H 0.9905 0.6439 -0.1937 0.045 Uiso 1 1 calc R . . C10 C 1.0254(5) 0.4756(5) -0.1238(4) 0.0418(12) Uani 1 1 d . . . H8 H 1.1166 0.4714 -0.1666 0.050 Uiso 1 1 calc R . . C11 C 0.9681(5) 0.3784(4) -0.0455(3) 0.0379(12) Uani 1 1 d . . . H9 H 1.0204 0.3077 -0.0327 0.046 Uiso 1 1 calc R . . C12 C 0.8331(5) 0.3862(4) 0.0140(3) 0.0339(11) Uani 1 1 d . . . N2 N 0.6364(4) 0.3120(3) 0.1556(2) 0.0268(8) Uani 1 1 d . . . C13 C 0.7628(5) 0.2869(4) 0.0998(3) 0.0326(11) Uani 1 1 d . . . C14 C 0.8185(5) 0.1767(4) 0.1218(4) 0.0383(12) Uani 1 1 d . . . H10 H 0.9070 0.1609 0.0824 0.046 Uiso 1 1 calc R . . C15 C 0.7436(5) 0.0892(4) 0.2023(4) 0.0410(12) Uani 1 1 d . . . H11 H 0.7795 0.0120 0.2178 0.049 Uiso 1 1 calc R . . C16 C 0.6185(5) 0.1132(4) 0.2594(3) 0.0376(12) Uani 1 1 d . . . H12 H 0.5680 0.0528 0.3152 0.045 Uiso 1 1 calc R . . C17 C 0.5635(5) 0.2269(4) 0.2363(3) 0.0292(10) Uani 1 1 d . . . C18 C 0.3427(5) 0.3506(4) 0.2712(3) 0.0275(10) Uani 1 1 d . . . C19 C 0.4307(5) 0.2538(4) 0.3003(3) 0.0254(10) Uani 1 1 d . . . C20 C 0.3891(5) 0.1783(4) 0.3947(3) 0.0306(10) Uani 1 1 d . . . H13 H 0.4485 0.1136 0.4147 0.037 Uiso 1 1 calc R . . C21 C 0.2652(5) 0.1947(4) 0.4595(3) 0.0305(10) Uani 1 1 d . . . C22 C 0.1824(5) 0.2910(4) 0.4297(3) 0.0289(10) Uani 1 1 d . . . H14 H 0.0971 0.3032 0.4737 0.035 Uiso 1 1 calc R . . C23 C 0.2184(4) 0.3709(4) 0.3380(3) 0.0261(10) Uani 1 1 d . . . O2 O 0.3714(3) 0.4207(2) 0.1821(2) 0.0288(7) Uani 1 1 d . . . C24 C 0.2248(5) 0.1120(4) 0.5604(3) 0.0385(12) Uani 1 1 d . . . H15 H 0.2622 0.0344 0.5642 0.058 Uiso 1 1 calc R . . H16 H 0.1200 0.1082 0.5876 0.058 Uiso 1 1 calc R . . H17 H 0.2661 0.1398 0.5949 0.058 Uiso 1 1 calc R . . N3 N -0.0030(4) 0.4698(3) 0.3797(2) 0.0288(9) Uani 1 1 d . . . C25 C 0.1281(5) 0.4768(4) 0.3160(3) 0.0303(10) Uani 1 1 d . . . C26 C 0.1749(5) 0.5818(4) 0.2399(3) 0.0345(11) Uani 1 1 d . . . H18 H 0.2675 0.5871 0.1956 0.041 Uiso 1 1 calc R . . C27 C 0.0862(5) 0.6763(4) 0.2299(3) 0.0388(12) Uani 1 1 d . . . H19 H 0.1167 0.7473 0.1781 0.047 Uiso 1 1 calc R . . C28 C -0.0478(5) 0.6688(4) 0.2949(3) 0.0352(11) Uani 1 1 d . . . H20 H -0.1110 0.7335 0.2884 0.042 Uiso 1 1 calc R . . C29 C -0.0875(5) 0.5636(4) 0.3702(3) 0.0293(10) Uani 1 1 d . . . N4 N -0.3234(4) 0.6339(3) 0.4348(3) 0.0314(9) Uani 1 1 d . . . C30 C -0.2240(5) 0.5492(4) 0.4483(3) 0.0303(10) Uani 1 1 d . . . C31 C -0.2436(5) 0.4559(4) 0.5328(3) 0.0294(10) Uani 1 1 d . . . H21 H -0.1733 0.3966 0.5410 0.035 Uiso 1 1 calc R . . C32 C -0.3693(5) 0.4517(4) 0.6052(3) 0.0330(11) Uani 1 1 d . . . H22 H -0.3855 0.3890 0.6639 0.040 Uiso 1 1 calc R . . C33 C -0.4700(5) 0.5382(4) 0.5918(3) 0.0315(11) Uani 1 1 d . . . H23 H -0.5559 0.5356 0.6410 0.038 Uiso 1 1 calc R . . C34 C -0.4449(5) 0.6296(4) 0.5054(3) 0.0289(10) Uani 1 1 d . . . C35 C -0.5349(5) 0.8041(4) 0.3921(3) 0.0322(11) Uani 1 1 d . . . C36 C -0.5497(5) 0.7240(4) 0.4840(3) 0.0316(11) Uani 1 1 d . . . C37 C -0.6717(5) 0.7349(4) 0.5544(3) 0.0330(11) Uani 1 1 d . . . H24 H -0.6827 0.6831 0.6168 0.040 Uiso 1 1 calc R . . C38 C -0.7777(5) 0.8181(4) 0.5375(3) 0.0334(11) Uani 1 1 d . . . C39 C -0.7588(5) 0.8927(4) 0.4464(4) 0.0392(12) Uani 1 1 d . . . H25 H -0.8297 0.9500 0.4329 0.047 Uiso 1 1 calc R . . C40 C -0.6408(5) 0.8867(4) 0.3745(3) 0.0387(12) Uani 1 1 d . . . H26 H -0.6315 0.9393 0.3124 0.046 Uiso 1 1 calc R . . O3 O -0.4198(4) 0.8031(3) 0.3182(2) 0.0415(8) Uani 1 1 d . . . H27 H -0.3627 0.7505 0.3369 0.062 Uiso 1 1 calc R . . C41 C -0.9082(5) 0.8222(4) 0.6167(4) 0.0444(13) Uani 1 1 d . . . H28 H -0.9644 0.8918 0.5944 0.067 Uiso 1 1 calc R . . H29 H -0.8778 0.8246 0.6667 0.067 Uiso 1 1 calc R . . H30 H -0.9673 0.7527 0.6404 0.067 Uiso 1 1 calc R . . N5 N 0.8393(16) 1.0602(11) -0.0201(9) 0.098(5) Uani 0.510(9) 1 d PU A 1 C42 C 0.7973(15) 0.9694(11) 0.0294(8) 0.059(4) Uani 0.510(9) 1 d PU A 1 C43 C 0.7469(19) 0.8566(14) 0.0949(10) 0.057(4) Uani 0.510(9) 1 d PU A 1 H31 H 0.6686 0.8632 0.1481 0.085 Uiso 0.510(9) 1 calc PR A 1 H32 H 0.8257 0.8118 0.1164 0.085 Uiso 0.510(9) 1 calc PR A 1 H33 H 0.7119 0.8168 0.0652 0.085 Uiso 0.510(9) 1 calc PR A 1 N6 N 0.9451(15) 0.8848(10) 0.0834(9) 0.082(4) Uani 0.490(9) 1 d PU A 2 C44 C 0.831(2) 0.8852(12) 0.0860(10) 0.061(4) Uani 0.490(9) 1 d PU A 2 C45 C 0.6731(19) 0.8741(17) 0.0944(14) 0.076(6) Uani 0.490(9) 1 d PU A 2 H34 H 0.6646 0.8132 0.0732 0.114 Uiso 0.490(9) 1 calc PR A 2 H35 H 0.6408 0.9483 0.0557 0.114 Uiso 0.490(9) 1 calc PR A 2 H36 H 0.6134 0.8538 0.1595 0.114 Uiso 0.490(9) 1 calc PR A 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 Fe1 0.0224(4) 0.0343(4) 0.0223(4) -0.0095(3) -0.0037(3) 0.0000(3) Cl1 0.0320(7) 0.0451(7) 0.0297(6) -0.0167(5) -0.0067(5) -0.0018(5) C1 0.031(3) 0.033(3) 0.021(2) -0.0059(19) -0.002(2) -0.011(2) C2 0.032(3) 0.040(3) 0.021(2) -0.007(2) -0.007(2) -0.006(2) C3 0.037(3) 0.046(3) 0.036(3) -0.007(2) -0.010(2) -0.015(2) C4 0.052(4) 0.041(3) 0.038(3) -0.007(2) -0.013(3) -0.018(3) C5 0.052(4) 0.035(3) 0.043(3) -0.012(2) -0.016(3) -0.001(2) C6 0.039(3) 0.030(3) 0.038(3) -0.007(2) -0.011(2) -0.002(2) O1 0.0156(15) 0.0325(17) 0.0222(16) -0.0093(13) -0.0002(13) -0.0011(12) C7 0.069(4) 0.049(4) 0.064(4) 0.001(3) -0.021(4) -0.026(3) N1 0.024(2) 0.040(2) 0.023(2) -0.0104(17) -0.0042(17) -0.0035(17) C8 0.023(2) 0.044(3) 0.022(2) -0.009(2) -0.005(2) -0.008(2) C9 0.026(3) 0.057(3) 0.026(3) -0.015(2) -0.002(2) -0.007(2) C10 0.019(3) 0.065(4) 0.040(3) -0.025(3) -0.003(2) 0.004(2) C11 0.021(3) 0.054(3) 0.034(3) -0.021(2) -0.002(2) 0.010(2) C12 0.032(3) 0.040(3) 0.030(3) -0.013(2) -0.010(2) -0.002(2) N2 0.019(2) 0.036(2) 0.025(2) -0.0131(16) -0.0047(16) 0.0002(16) C13 0.027(3) 0.040(3) 0.030(3) -0.014(2) -0.008(2) 0.002(2) C14 0.026(3) 0.042(3) 0.043(3) -0.018(2) -0.008(2) 0.009(2) C15 0.039(3) 0.040(3) 0.046(3) -0.019(2) -0.016(3) 0.011(2) C16 0.035(3) 0.041(3) 0.032(3) -0.012(2) -0.009(2) 0.007(2) C17 0.028(3) 0.031(2) 0.028(3) -0.011(2) -0.010(2) -0.0002(19) C18 0.026(2) 0.033(2) 0.023(2) -0.0087(19) -0.007(2) -0.0055(19) C19 0.025(2) 0.032(2) 0.018(2) -0.0081(18) -0.0060(19) 0.0003(19) C20 0.031(3) 0.034(3) 0.026(3) -0.010(2) -0.010(2) 0.000(2) C21 0.034(3) 0.032(3) 0.025(3) -0.011(2) -0.006(2) -0.007(2) C22 0.022(2) 0.037(3) 0.028(3) -0.014(2) -0.006(2) -0.0031(19) C23 0.019(2) 0.032(2) 0.025(2) -0.0139(19) -0.0003(19) -0.0023(18) O2 0.0246(17) 0.0371(17) 0.0199(16) -0.0083(13) -0.0035(13) -0.0010(13) C24 0.045(3) 0.033(3) 0.030(3) -0.008(2) -0.007(2) -0.001(2) N3 0.023(2) 0.038(2) 0.025(2) -0.0150(17) -0.0013(17) -0.0035(16) C25 0.032(3) 0.035(3) 0.027(3) -0.014(2) -0.008(2) -0.004(2) C26 0.028(3) 0.036(3) 0.029(3) -0.014(2) 0.007(2) -0.001(2) C27 0.035(3) 0.038(3) 0.030(3) -0.012(2) 0.005(2) -0.003(2) C28 0.037(3) 0.033(3) 0.029(3) -0.011(2) -0.004(2) 0.001(2) C29 0.025(3) 0.035(3) 0.028(3) -0.016(2) -0.004(2) 0.001(2) N4 0.033(2) 0.034(2) 0.028(2) -0.0151(17) -0.0055(18) -0.0023(17) C30 0.030(3) 0.032(2) 0.028(3) -0.015(2) -0.003(2) -0.002(2) C31 0.025(2) 0.033(2) 0.027(3) -0.013(2) -0.003(2) 0.0001(19) C32 0.035(3) 0.036(3) 0.026(3) -0.010(2) -0.007(2) -0.004(2) C33 0.025(3) 0.040(3) 0.028(3) -0.014(2) -0.002(2) -0.005(2) C34 0.026(3) 0.036(3) 0.026(2) -0.017(2) -0.002(2) -0.003(2) C35 0.030(3) 0.039(3) 0.023(3) -0.010(2) -0.004(2) -0.001(2) C36 0.025(3) 0.034(3) 0.038(3) -0.019(2) -0.006(2) -0.0006(19) C37 0.033(3) 0.034(3) 0.029(3) -0.012(2) -0.004(2) -0.005(2) C38 0.028(3) 0.032(3) 0.037(3) -0.016(2) -0.003(2) -0.001(2) C39 0.032(3) 0.037(3) 0.046(3) -0.014(2) -0.014(2) 0.007(2) C40 0.038(3) 0.039(3) 0.030(3) -0.008(2) -0.008(2) 0.003(2) O3 0.040(2) 0.045(2) 0.0297(19) -0.0101(15) -0.0052(16) 0.0042(16) C41 0.032(3) 0.049(3) 0.047(3) -0.023(3) 0.000(2) 0.000(2) N5 0.143(10) 0.078(7) 0.071(7) -0.033(6) -0.018(7) -0.024(7) C42 0.090(8) 0.044(6) 0.036(6) -0.013(5) -0.017(6) 0.002(6) C43 0.061(9) 0.062(8) 0.044(7) -0.022(6) -0.006(7) -0.015(7) N6 0.072(8) 0.075(7) 0.089(8) -0.039(6) -0.012(6) 0.013(6) C44 0.082(9) 0.039(7) 0.060(8) -0.026(6) -0.016(7) 0.017(7) C45 0.072(10) 0.085(9) 0.085(10) -0.037(7) -0.041(8) 0.017(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 O2 1.869(3) . ? Fe1 O1 1.962(3) . ? Fe1 N1 2.124(4) . ? Fe1 N2 2.126(4) . ? Fe1 O1 2.200(3) 2_665 ? Fe1 Cl1 2.2983(13) . ? C1 O1 1.353(5) . ? C1 C6 1.393(6) . ? C1 C2 1.414(6) . ? C2 C3 1.407(6) . ? C2 C8 1.471(6) . ? C3 C4 1.382(7) . ? C3 H1 0.9500 . ? C4 C5 1.380(7) . ? C4 C7 1.519(7) . ? C5 C6 1.396(7) . ? C5 H2 0.9500 . ? C6 H3 0.9500 . ? O1 Fe1 2.200(3) 2_665 ? C7 H4 0.9800 . ? C7 H5 0.9800 . ? C7 H6 0.9800 . ? N1 C8 1.351(5) . ? N1 C12 1.352(6) . ? C8 C9 1.399(6) . ? C9 C10 1.361(7) . ? C9 H7 0.9500 . ? C10 C11 1.381(7) . ? C10 H8 0.9500 . ? C11 C12 1.383(6) . ? C11 H9 0.9500 . ? C12 C13 1.482(6) . ? N2 C17 1.362(5) . ? N2 C13 1.363(6) . ? C13 C14 1.371(6) . ? C14 C15 1.379(7) . ? C14 H10 0.9500 . ? C15 C16 1.361(7) . ? C15 H11 0.9500 . ? C16 C17 1.406(6) . ? C16 H12 0.9500 . ? C17 C19 1.477(6) . ? C18 O2 1.328(5) . ? C18 C19 1.415(6) . ? C18 C23 1.421(6) . ? C19 C20 1.409(6) . ? C20 C21 1.382(6) . ? C20 H13 0.9500 . ? C21 C22 1.382(6) . ? C21 C24 1.512(6) . ? C22 C23 1.393(6) . ? C22 H14 0.9500 . ? C23 C25 1.488(6) . ? C24 H15 0.9800 . ? C24 H16 0.9800 . ? C24 H17 0.9800 . ? N3 C29 1.339(6) . ? N3 C25 1.353(6) . ? C25 C26 1.405(6) . ? C26 C27 1.368(6) . ? C26 H18 0.9500 . ? C27 C28 1.381(6) . ? C27 H19 0.9500 . ? C28 C29 1.392(6) . ? C28 H20 0.9500 . ? C29 C30 1.490(6) . ? N4 C30 1.352(6) . ? N4 C34 1.352(6) . ? C30 C31 1.387(6) . ? C31 C32 1.393(6) . ? C31 H21 0.9500 . ? C32 C33 1.375(6) . ? C32 H22 0.9500 . ? C33 C34 1.392(6) . ? C33 H23 0.9500 . ? C34 C36 1.480(6) . ? C35 O3 1.362(5) . ? C35 C40 1.391(6) . ? C35 C36 1.414(6) . ? C36 C37 1.400(6) . ? C37 C38 1.394(6) . ? C37 H24 0.9500 . ? C38 C39 1.379(7) . ? C38 C41 1.507(6) . ? C39 C40 1.373(7) . ? C39 H25 0.9500 . ? C40 H26 0.9500 . ? O3 H27 0.8400 . ? C41 H28 0.9800 . ? C41 H29 0.9800 . ? C41 H30 0.9800 . ? N5 C42 1.135(15) . ? C42 C43 1.42(2) . ? C43 H31 0.9800 . ? C43 H32 0.9800 . ? C43 H33 0.9800 . ? N6 C44 1.11(2) . ? C44 C45 1.54(3) . ? C45 H34 0.9800 . ? C45 H35 0.9800 . ? C45 H36 0.9800 . ? 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 Fe1 O1 106.36(12) . . ? O2 Fe1 N1 163.65(14) . . ? O1 Fe1 N1 85.56(13) . . ? O2 Fe1 N2 87.59(13) . . ? O1 Fe1 N2 155.84(13) . . ? N1 Fe1 N2 77.53(14) . . ? O2 Fe1 O1 86.92(12) . 2_665 ? O1 Fe1 O1 76.21(12) . 2_665 ? N1 Fe1 O1 85.11(12) . 2_665 ? N2 Fe1 O1 85.18(12) . 2_665 ? O2 Fe1 Cl1 96.31(10) . . ? O1 Fe1 Cl1 98.15(9) . . ? N1 Fe1 Cl1 92.92(10) . . ? N2 Fe1 Cl1 99.81(10) . . ? O1 Fe1 Cl1 174.14(8) 2_665 . ? O1 C1 C6 119.3(4) . . ? O1 C1 C2 121.2(4) . . ? C6 C1 C2 119.5(4) . . ? C3 C2 C1 118.1(4) . . ? C3 C2 C8 118.8(4) . . ? C1 C2 C8 123.1(4) . . ? C4 C3 C2 122.7(5) . . ? C4 C3 H1 118.7 . . ? C2 C3 H1 118.7 . . ? C5 C4 C3 118.0(5) . . ? C5 C4 C7 121.7(5) . . ? C3 C4 C7 120.3(5) . . ? C4 C5 C6 121.5(5) . . ? C4 C5 H2 119.2 . . ? C6 C5 H2 119.2 . . ? C1 C6 C5 120.2(5) . . ? C1 C6 H3 119.9 . . ? C5 C6 H3 119.9 . . ? C1 O1 Fe1 119.1(3) . . ? C1 O1 Fe1 121.1(3) . 2_665 ? Fe1 O1 Fe1 103.79(12) . 2_665 ? C4 C7 H4 109.5 . . ? C4 C7 H5 109.5 . . ? H4 C7 H5 109.5 . . ? C4 C7 H6 109.5 . . ? H4 C7 H6 109.5 . . ? H5 C7 H6 109.5 . . ? C8 N1 C12 120.6(4) . . ? C8 N1 Fe1 124.5(3) . . ? C12 N1 Fe1 114.7(3) . . ? N1 C8 C9 119.2(4) . . ? N1 C8 C2 119.9(4) . . ? C9 C8 C2 120.9(4) . . ? C10 C9 C8 120.3(5) . . ? C10 C9 H7 119.9 . . ? C8 C9 H7 119.9 . . ? C9 C10 C11 120.0(5) . . ? C9 C10 H8 120.0 . . ? C11 C10 H8 120.0 . . ? C10 C11 C12 118.6(5) . . ? C10 C11 H9 120.7 . . ? C12 C11 H9 120.7 . . ? N1 C12 C11 121.2(4) . . ? N1 C12 C13 116.1(4) . . ? C11 C12 C13 122.6(4) . . ? C17 N2 C13 119.9(4) . . ? C17 N2 Fe1 124.4(3) . . ? C13 N2 Fe1 114.3(3) . . ? N2 C13 C14 121.7(4) . . ? N2 C13 C12 115.3(4) . . ? C14 C13 C12 123.0(4) . . ? C13 C14 C15 118.8(5) . . ? C13 C14 H10 120.6 . . ? C15 C14 H10 120.6 . . ? C16 C15 C14 120.1(5) . . ? C16 C15 H11 119.9 . . ? C14 C15 H11 119.9 . . ? C15 C16 C17 120.4(5) . . ? C15 C16 H12 119.8 . . ? C17 C16 H12 119.8 . . ? N2 C17 C16 119.0(4) . . ? N2 C17 C19 120.7(4) . . ? C16 C17 C19 120.3(4) . . ? O2 C18 C19 121.3(4) . . ? O2 C18 C23 119.3(4) . . ? C19 C18 C23 119.4(4) . . ? C20 C19 C18 118.5(4) . . ? C20 C19 C17 118.2(4) . . ? C18 C19 C17 123.3(4) . . ? C21 C20 C19 122.5(4) . . ? C21 C20 H13 118.7 . . ? C19 C20 H13 118.7 . . ? C20 C21 C22 117.9(4) . . ? C20 C21 C24 120.9(4) . . ? C22 C21 C24 121.2(4) . . ? C21 C22 C23 122.9(4) . . ? C21 C22 H14 118.6 . . ? C23 C22 H14 118.6 . . ? C22 C23 C18 118.8(4) . . ? C22 C23 C25 118.0(4) . . ? C18 C23 C25 123.2(4) . . ? C18 O2 Fe1 129.7(3) . . ? C21 C24 H15 109.5 . . ? C21 C24 H16 109.5 . . ? H15 C24 H16 109.5 . . ? C21 C24 H17 109.5 . . ? H15 C24 H17 109.5 . . ? H16 C24 H17 109.5 . . ? C29 N3 C25 119.6(4) . . ? N3 C25 C26 120.2(4) . . ? N3 C25 C23 115.1(4) . . ? C26 C25 C23 124.5(4) . . ? C27 C26 C25 119.6(4) . . ? C27 C26 H18 120.2 . . ? C25 C26 H18 120.2 . . ? C26 C27 C28 120.1(4) . . ? C26 C27 H19 120.0 . . ? C28 C27 H19 120.0 . . ? C27 C28 C29 118.1(4) . . ? C27 C28 H20 121.0 . . ? C29 C28 H20 121.0 . . ? N3 C29 C28 122.4(4) . . ? N3 C29 C30 115.2(4) . . ? C28 C29 C30 122.4(4) . . ? C30 N4 C34 119.7(4) . . ? N4 C30 C31 121.9(4) . . ? N4 C30 C29 117.1(4) . . ? C31 C30 C29 120.9(4) . . ? C30 C31 C32 118.1(4) . . ? C30 C31 H21 120.9 . . ? C32 C31 H21 120.9 . . ? C33 C32 C31 120.1(4) . . ? C33 C32 H22 120.0 . . ? C31 C32 H22 120.0 . . ? C32 C33 C34 119.3(4) . . ? C32 C33 H23 120.3 . . ? C34 C33 H23 120.3 . . ? N4 C34 C33 120.8(4) . . ? N4 C34 C36 116.2(4) . . ? C33 C34 C36 122.9(4) . . ? O3 C35 C40 117.6(4) . . ? O3 C35 C36 122.2(4) . . ? C40 C35 C36 120.2(4) . . ? C37 C36 C35 117.0(4) . . ? C37 C36 C34 120.8(4) . . ? C35 C36 C34 122.2(4) . . ? C38 C37 C36 123.3(4) . . ? C38 C37 H24 118.4 . . ? C36 C37 H24 118.4 . . ? C39 C38 C37 117.2(4) . . ? C39 C38 C41 122.6(4) . . ? C37 C38 C41 120.2(4) . . ? C40 C39 C38 122.1(5) . . ? C40 C39 H25 118.9 . . ? C38 C39 H25 118.9 . . ? C39 C40 C35 120.2(5) . . ? C39 C40 H26 119.9 . . ? C35 C40 H26 119.9 . . ? C35 O3 H27 109.5 . . ? C38 C41 H28 109.5 . . ? C38 C41 H29 109.5 . . ? H28 C41 H29 109.5 . . ? C38 C41 H30 109.5 . . ? H28 C41 H30 109.5 . . ? H29 C41 H30 109.5 . . ? N5 C42 C43 177.1(15) . . ? N6 C44 C45 175.0(17) . . ? C44 C45 H34 109.5 . . ? C44 C45 H35 109.5 . . ? H34 C45 H35 109.5 . . ? C44 C45 H36 109.5 . . ? H34 C45 H36 109.5 . . ? H35 C45 H36 109.5 . . ? 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 O1 C1 C2 C3 177.1(4) . . . . ? C6 C1 C2 C3 -0.7(7) . . . . ? O1 C1 C2 C8 -3.5(7) . . . . ? C6 C1 C2 C8 178.7(4) . . . . ? C1 C2 C3 C4 -0.4(7) . . . . ? C8 C2 C3 C4 -179.7(5) . . . . ? C2 C3 C4 C5 1.1(8) . . . . ? C2 C3 C4 C7 -179.2(5) . . . . ? C3 C4 C5 C6 -0.8(8) . . . . ? C7 C4 C5 C6 179.6(5) . . . . ? O1 C1 C6 C5 -176.9(4) . . . . ? C2 C1 C6 C5 1.0(7) . . . . ? C4 C5 C6 C1 -0.2(8) . . . . ? C6 C1 O1 Fe1 -130.3(4) . . . . ? C2 C1 O1 Fe1 51.9(5) . . . . ? C6 C1 O1 Fe1 98.9(4) . . . 2_665 ? C2 C1 O1 Fe1 -78.9(5) . . . 2_665 ? O2 Fe1 O1 C1 139.3(3) . . . . ? N1 Fe1 O1 C1 -52.1(3) . . . . ? N2 Fe1 O1 C1 -97.5(4) . . . . ? O1 Fe1 O1 C1 -138.1(3) 2_665 . . . ? Cl1 Fe1 O1 C1 40.2(3) . . . . ? O2 Fe1 O1 Fe1 -82.55(14) . . . 2_665 ? N1 Fe1 O1 Fe1 86.05(14) . . . 2_665 ? N2 Fe1 O1 Fe1 40.6(3) . . . 2_665 ? O1 Fe1 O1 Fe1 0.0 2_665 . . 2_665 ? Cl1 Fe1 O1 Fe1 178.37(10) . . . 2_665 ? O2 Fe1 N1 C8 160.2(4) . . . . ? O1 Fe1 N1 C8 22.5(3) . . . . ? N2 Fe1 N1 C8 -174.8(4) . . . . ? O1 Fe1 N1 C8 99.0(3) 2_665 . . . ? Cl1 Fe1 N1 C8 -75.4(3) . . . . ? O2 Fe1 N1 C12 -14.2(7) . . . . ? O1 Fe1 N1 C12 -151.8(3) . . . . ? N2 Fe1 N1 C12 10.8(3) . . . . ? O1 Fe1 N1 C12 -75.3(3) 2_665 . . . ? Cl1 Fe1 N1 C12 110.2(3) . . . . ? C12 N1 C8 C9 1.9(6) . . . . ? Fe1 N1 C8 C9 -172.2(3) . . . . ? C12 N1 C8 C2 -175.7(4) . . . . ? Fe1 N1 C8 C2 10.3(6) . . . . ? C3 C2 C8 N1 150.8(4) . . . . ? C1 C2 C8 N1 -28.5(7) . . . . ? C3 C2 C8 C9 -26.7(7) . . . . ? C1 C2 C8 C9 154.0(4) . . . . ? N1 C8 C9 C10 -2.3(7) . . . . ? C2 C8 C9 C10 175.3(4) . . . . ? C8 C9 C10 C11 0.3(7) . . . . ? C9 C10 C11 C12 2.0(7) . . . . ? C8 N1 C12 C11 0.4(7) . . . . ? Fe1 N1 C12 C11 175.0(4) . . . . ? C8 N1 C12 C13 178.1(4) . . . . ? Fe1 N1 C12 C13 -7.3(5) . . . . ? C10 C11 C12 N1 -2.4(7) . . . . ? C10 C11 C12 C13 -179.9(4) . . . . ? O2 Fe1 N2 C17 -6.2(3) . . . . ? O1 Fe1 N2 C17 -132.8(4) . . . . ? N1 Fe1 N2 C17 -179.4(4) . . . . ? O1 Fe1 N2 C17 -93.4(3) 2_665 . . . ? Cl1 Fe1 N2 C17 89.8(3) . . . . ? O2 Fe1 N2 C13 160.2(3) . . . . ? O1 Fe1 N2 C13 33.7(5) . . . . ? N1 Fe1 N2 C13 -12.9(3) . . . . ? O1 Fe1 N2 C13 73.1(3) 2_665 . . . ? Cl1 Fe1 N2 C13 -103.8(3) . . . . ? C17 N2 C13 C14 1.2(7) . . . . ? Fe1 N2 C13 C14 -165.9(4) . . . . ? C17 N2 C13 C12 -179.7(4) . . . . ? Fe1 N2 C13 C12 13.1(5) . . . . ? N1 C12 C13 N2 -3.9(6) . . . . ? C11 C12 C13 N2 173.7(4) . . . . ? N1 C12 C13 C14 175.1(4) . . . . ? C11 C12 C13 C14 -7.3(7) . . . . ? N2 C13 C14 C15 0.4(7) . . . . ? C12 C13 C14 C15 -178.6(5) . . . . ? C13 C14 C15 C16 -1.5(8) . . . . ? C14 C15 C16 C17 0.9(8) . . . . ? C13 N2 C17 C16 -1.8(6) . . . . ? Fe1 N2 C17 C16 164.0(3) . . . . ? C13 N2 C17 C19 176.5(4) . . . . ? Fe1 N2 C17 C19 -17.7(6) . . . . ? C15 C16 C17 N2 0.8(7) . . . . ? C15 C16 C17 C19 -177.5(4) . . . . ? O2 C18 C19 C20 -175.7(4) . . . . ? C23 C18 C19 C20 1.9(6) . . . . ? O2 C18 C19 C17 3.6(7) . . . . ? C23 C18 C19 C17 -178.8(4) . . . . ? N2 C17 C19 C20 -156.9(4) . . . . ? C16 C17 C19 C20 21.4(6) . . . . ? N2 C17 C19 C18 23.9(6) . . . . ? C16 C17 C19 C18 -157.9(4) . . . . ? C18 C19 C20 C21 0.7(7) . . . . ? C17 C19 C20 C21 -178.6(4) . . . . ? C19 C20 C21 C22 -1.8(7) . . . . ? C19 C20 C21 C24 -179.6(4) . . . . ? C20 C21 C22 C23 0.2(7) . . . . ? C24 C21 C22 C23 178.0(4) . . . . ? C21 C22 C23 C18 2.4(7) . . . . ? C21 C22 C23 C25 -174.6(4) . . . . ? O2 C18 C23 C22 174.3(4) . . . . ? C19 C18 C23 C22 -3.4(6) . . . . ? O2 C18 C23 C25 -8.9(6) . . . . ? C19 C18 C23 C25 173.4(4) . . . . ? C19 C18 O2 Fe1 -39.7(6) . . . . ? C23 C18 O2 Fe1 142.6(3) . . . . ? O1 Fe1 O2 C18 -164.3(3) . . . . ? N1 Fe1 O2 C18 60.2(7) . . . . ? N2 Fe1 O2 C18 35.8(4) . . . . ? O1 Fe1 O2 C18 121.1(4) 2_665 . . . ? Cl1 Fe1 O2 C18 -63.8(4) . . . . ? C29 N3 C25 C26 -0.4(6) . . . . ? C29 N3 C25 C23 174.5(4) . . . . ? C22 C23 C25 N3 -18.4(6) . . . . ? C18 C23 C25 N3 164.7(4) . . . . ? C22 C23 C25 C26 156.2(4) . . . . ? C18 C23 C25 C26 -20.7(7) . . . . ? N3 C25 C26 C27 -1.0(7) . . . . ? C23 C25 C26 C27 -175.4(4) . . . . ? C25 C26 C27 C28 0.8(7) . . . . ? C26 C27 C28 C29 0.8(7) . . . . ? C25 N3 C29 C28 2.1(7) . . . . ? C25 N3 C29 C30 -175.1(4) . . . . ? C27 C28 C29 N3 -2.3(7) . . . . ? C27 C28 C29 C30 174.6(4) . . . . ? C34 N4 C30 C31 1.1(7) . . . . ? C34 N4 C30 C29 -175.3(4) . . . . ? N3 C29 C30 N4 -169.0(4) . . . . ? C28 C29 C30 N4 13.9(6) . . . . ? N3 C29 C30 C31 14.6(6) . . . . ? C28 C29 C30 C31 -162.5(4) . . . . ? N4 C30 C31 C32 -0.8(7) . . . . ? C29 C30 C31 C32 175.5(4) . . . . ? C30 C31 C32 C33 0.2(7) . . . . ? C31 C32 C33 C34 0.0(7) . . . . ? C30 N4 C34 C33 -0.8(6) . . . . ? C30 N4 C34 C36 -178.4(4) . . . . ? C32 C33 C34 N4 0.3(7) . . . . ? C32 C33 C34 C36 177.8(4) . . . . ? O3 C35 C36 C37 178.9(4) . . . . ? C40 C35 C36 C37 -1.9(7) . . . . ? O3 C35 C36 C34 -3.3(7) . . . . ? C40 C35 C36 C34 175.9(4) . . . . ? N4 C34 C36 C37 -173.1(4) . . . . ? C33 C34 C36 C37 9.3(7) . . . . ? N4 C34 C36 C35 9.2(6) . . . . ? C33 C34 C36 C35 -168.4(4) . . . . ? C35 C36 C37 C38 1.4(7) . . . . ? C34 C36 C37 C38 -176.4(4) . . . . ? C36 C37 C38 C39 -0.3(7) . . . . ? C36 C37 C38 C41 178.1(4) . . . . ? C37 C38 C39 C40 -0.2(7) . . . . ? C41 C38 C39 C40 -178.6(5) . . . . ? C38 C39 C40 C35 -0.3(8) . . . . ? O3 C35 C40 C39 -179.3(4) . . . . ? C36 C35 C40 C39 1.5(7) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.393 _refine_diff_density_min -0.849 _refine_diff_density_rms 0.111 _database_code_depnum_ccdc_archive 'CCDC 938301' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_L2Zn3 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common '[LZn3(OAc)2](CHCl3)(MeOH)3.5(H2O)' _chemical_melting_point ? _chemical_formula_moiety C78.50H87Cl3N6O12.50Zn3 _chemical_formula_sum 'C78.50 H87 Cl3 N6 O12.50 Zn3' _chemical_formula_weight 1617.00 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 '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 14.6782(11) _cell_length_b 17.4488(14) _cell_length_c 17.5840(11) _cell_angle_alpha 113.1987(19) _cell_angle_beta 109.4448(19) _cell_angle_gamma 98.986(2) _cell_volume 3682.6(5) _cell_formula_units_Z 2 _cell_measurement_temperature 120 _cell_measurement_reflns_used 28905 _cell_measurement_theta_min 3.12 _cell_measurement_theta_max 25.00 _exptl_crystal_description prismatic _exptl_crystal_colour yellow _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.458 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1682 _exptl_absorpt_coefficient_mu 1.146 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6572 _exptl_absorpt_correction_T_max 0.9449 _exptl_absorpt_process_details 'Rapid AUTO (Rigaku Corp.)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120 _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku R-AXIS Rapid' _diffrn_measurement_method IP _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 28905 _diffrn_reflns_av_R_equivalents 0.0695 _diffrn_reflns_av_sigmaI/netI 0.0941 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 3.12 _diffrn_reflns_theta_max 25.00 _reflns_number_total 12931 _reflns_number_gt 8903 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Rapid AUTO (Rigaku Corp.)' _computing_cell_refinement 'Rapid AUTO (Rigaku Corp.)' _computing_data_reduction 'Rapid AUTO (Rigaku Corp.)' _computing_structure_solution 'DIRDIF99 (Beurskens et al., 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ORTEP-3 _computing_publication_material ORTEP-3 _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^)+(0.1094P)^2^+8.9274P] 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 12931 _refine_ls_number_parameters 971 _refine_ls_number_restraints 36 _refine_ls_R_factor_all 0.1122 _refine_ls_R_factor_gt 0.0868 _refine_ls_wR_factor_ref 0.2486 _refine_ls_wR_factor_gt 0.2226 _refine_ls_goodness_of_fit_ref 1.111 _refine_ls_restrained_S_all 1.112 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zn1 Zn 0.56270(6) 0.57681(5) 0.27554(5) 0.0365(2) Uani 1 1 d . . . Zn2 Zn 0.74377(6) 0.62467(5) 0.48611(5) 0.0378(2) Uani 1 1 d . . . Zn3 Zn 0.92646(6) 0.76239(5) 0.50696(5) 0.0386(2) Uani 1 1 d . . . C1 C 0.6167(4) 0.4184(4) 0.2239(4) 0.0360(14) Uani 1 1 d . . . C2 C 0.6074(5) 0.4098(4) 0.1373(4) 0.0373(14) Uani 1 1 d . . . C3 C 0.5895(5) 0.3241(4) 0.0670(4) 0.0429(15) Uani 1 1 d . . . H1 H 0.5787 0.3172 0.0080 0.051 Uiso 1 1 calc R . . C4 C 0.5867(5) 0.2509(4) 0.0795(5) 0.0457(16) Uani 1 1 d . . . C5 C 0.6004(5) 0.2623(5) 0.1656(5) 0.0457(16) Uani 1 1 d . . . H2 H 0.5997 0.2131 0.1765 0.055 Uiso 1 1 calc R . . C6 C 0.6151(5) 0.3426(4) 0.2359(4) 0.0410(15) Uani 1 1 d . . . H3 H 0.6243 0.3472 0.2938 0.049 Uiso 1 1 calc R . . O1 O 0.6277(3) 0.4915(3) 0.2937(3) 0.0376(10) Uani 1 1 d . . . C7 C 0.5644(6) 0.1594(5) -0.0002(5) 0.0548(19) Uani 1 1 d . . . C8 C 0.6248(8) 0.1069(6) 0.0340(6) 0.075(3) Uani 1 1 d . . . H4 H 0.6097 0.0496 -0.0180 0.113 Uiso 1 1 calc R . . H5 H 0.6054 0.0975 0.0787 0.113 Uiso 1 1 calc R . . H6 H 0.6982 0.1398 0.0633 0.113 Uiso 1 1 calc R . . C9 C 0.5903(6) 0.1676(5) -0.0746(5) 0.061(2) Uani 1 1 d . . . H7 H 0.5520 0.2013 -0.0972 0.091 Uiso 1 1 calc R . . H8 H 0.5717 0.1085 -0.1255 0.091 Uiso 1 1 calc R . . H9 H 0.6639 0.1982 -0.0488 0.091 Uiso 1 1 calc R . . C10 C 0.4489(6) 0.1080(5) -0.0463(6) 0.069(2) Uani 1 1 d . . . H10 H 0.4103 0.1420 -0.0682 0.104 Uiso 1 1 calc R . . H11 H 0.4294 0.0986 -0.0017 0.104 Uiso 1 1 calc R . . H12 H 0.4337 0.0507 -0.0984 0.104 Uiso 1 1 calc R . . N1 N 0.6066(4) 0.5599(3) 0.1703(3) 0.0354(12) Uani 1 1 d . . . C11 C 0.6163(5) 0.4839(4) 0.1168(4) 0.0410(15) Uani 1 1 d . . . C12 C 0.6357(6) 0.4784(5) 0.0418(4) 0.0489(18) Uani 1 1 d . . . H13 H 0.6491 0.4280 0.0066 0.059 Uiso 1 1 calc R . . C13 C 0.6353(6) 0.5455(5) 0.0195(5) 0.0527(19) Uani 1 1 d . . . H14 H 0.6412 0.5390 -0.0347 0.063 Uiso 1 1 calc R . . C14 C 0.6261(6) 0.6225(5) 0.0766(5) 0.0501(18) Uani 1 1 d . . . H15 H 0.6276 0.6704 0.0635 0.060 Uiso 1 1 calc R . . C15 C 0.6147(5) 0.6277(4) 0.1529(4) 0.0367(14) Uani 1 1 d . . . N2 N 0.5895(4) 0.7042(4) 0.2881(3) 0.0386(12) Uani 1 1 d . . . C16 C 0.6124(5) 0.7104(5) 0.2224(4) 0.0400(15) Uani 1 1 d . . . C17 C 0.6364(6) 0.7911(5) 0.2218(5) 0.0490(17) Uani 1 1 d . . . H16 H 0.6513 0.7946 0.1745 0.059 Uiso 1 1 calc R . . C18 C 0.6378(6) 0.8651(5) 0.2915(5) 0.0484(17) Uani 1 1 d . . . H17 H 0.6521 0.9203 0.2919 0.058 Uiso 1 1 calc R . . C19 C 0.6186(6) 0.8589(5) 0.3598(5) 0.0474(17) Uani 1 1 d . . . H18 H 0.6218 0.9104 0.4088 0.057 Uiso 1 1 calc R . . C20 C 0.5940(5) 0.7774(4) 0.3586(4) 0.0403(15) Uani 1 1 d . . . C21 C 0.5936(5) 0.7080(4) 0.4611(4) 0.0370(14) Uani 1 1 d . . . C22 C 0.5746(5) 0.7725(4) 0.4346(4) 0.0390(15) Uani 1 1 d . . . C23 C 0.5412(5) 0.8370(5) 0.4841(4) 0.0430(15) Uani 1 1 d . . . H19 H 0.5241 0.8779 0.4634 0.052 Uiso 1 1 calc R . . C24 C 0.5320(5) 0.8440(4) 0.5629(4) 0.0389(14) Uani 1 1 d . . . C25 C 0.5562(5) 0.7830(4) 0.5900(4) 0.0387(14) Uani 1 1 d . . . H20 H 0.5537 0.7881 0.6451 0.046 Uiso 1 1 calc R . . C26 C 0.5842(5) 0.7138(4) 0.5403(4) 0.0358(14) Uani 1 1 d . . . O2 O 0.6213(3) 0.6423(3) 0.4123(3) 0.0364(10) Uani 1 1 d . . . C27 C 0.4968(5) 0.9175(5) 0.6151(4) 0.0435(15) Uani 1 1 d . . . C28 C 0.5631(6) 1.0067(5) 0.6370(5) 0.0540(18) Uani 1 1 d . . . H21 H 0.5405 1.0535 0.6705 0.081 Uiso 1 1 calc R . . H22 H 0.5567 1.0066 0.5797 0.081 Uiso 1 1 calc R . . H23 H 0.6348 1.0174 0.6749 0.081 Uiso 1 1 calc R . . C29 C 0.3843(6) 0.8999(5) 0.5551(5) 0.0566(19) Uani 1 1 d . . . H24 H 0.3612 0.9466 0.5880 0.085 Uiso 1 1 calc R . . H25 H 0.3421 0.8425 0.5415 0.085 Uiso 1 1 calc R . . H26 H 0.3779 0.8992 0.4976 0.085 Uiso 1 1 calc R . . C30 C 0.5040(6) 0.9193(5) 0.7051(5) 0.0546(19) Uani 1 1 d . . . H27 H 0.4813 0.9668 0.7371 0.082 Uiso 1 1 calc R . . H28 H 0.5751 0.9297 0.7443 0.082 Uiso 1 1 calc R . . H29 H 0.4603 0.8625 0.6912 0.082 Uiso 1 1 calc R . . N3 N 0.6635(4) 0.6052(3) 0.5560(3) 0.0351(11) Uani 1 1 d . . . C31 C 0.5967(5) 0.6462(4) 0.5706(4) 0.0356(14) Uani 1 1 d . . . C32 C 0.5376(5) 0.6232(4) 0.6108(4) 0.0422(15) Uani 1 1 d . . . H30 H 0.4909 0.6531 0.6224 0.051 Uiso 1 1 calc R . . C33 C 0.5468(6) 0.5573(5) 0.6338(4) 0.0478(17) Uani 1 1 d . . . H31 H 0.5072 0.5417 0.6619 0.057 Uiso 1 1 calc R . . C34 C 0.6143(5) 0.5135(4) 0.6158(4) 0.0433(16) Uani 1 1 d . . . H32 H 0.6219 0.4677 0.6312 0.052 Uiso 1 1 calc R . . C35 C 0.6703(5) 0.5383(4) 0.5746(4) 0.0391(15) Uani 1 1 d . . . N4 N 0.7743(4) 0.5135(3) 0.4924(3) 0.0368(12) Uani 1 1 d . . . C36 C 0.7393(5) 0.4902(4) 0.5449(4) 0.0393(15) Uani 1 1 d . . . C37 C 0.7615(6) 0.4263(5) 0.5664(5) 0.0471(16) Uani 1 1 d . . . H33 H 0.7327 0.4090 0.6006 0.057 Uiso 1 1 calc R . . C38 C 0.8267(6) 0.3875(5) 0.5371(5) 0.0547(19) Uani 1 1 d . . . H34 H 0.8463 0.3450 0.5539 0.066 Uiso 1 1 calc R . . C39 C 0.8635(5) 0.4100(5) 0.4838(5) 0.0488(17) Uani 1 1 d . . . H35 H 0.9088 0.3833 0.4640 0.059 Uiso 1 1 calc R . . C40 C 0.8343(5) 0.4719(4) 0.4587(4) 0.0385(14) Uani 1 1 d . . . C41 C 0.8714(5) 0.5697(4) 0.3881(4) 0.0414(15) Uani 1 1 d . . . C42 C 0.8670(5) 0.4911(4) 0.3952(4) 0.0394(15) Uani 1 1 d . . . C43 C 0.8944(5) 0.4266(5) 0.3370(5) 0.0455(16) Uani 1 1 d . . . H36 H 0.8895 0.3729 0.3398 0.055 Uiso 1 1 calc R . . C44 C 0.9278(5) 0.4373(5) 0.2764(5) 0.0490(17) Uani 1 1 d . . . C45 C 0.9343(5) 0.5157(5) 0.2724(5) 0.0471(17) Uani 1 1 d . . . H37 H 0.9598 0.5247 0.2324 0.057 Uiso 1 1 calc R . . C46 C 0.9048(5) 0.5822(4) 0.3251(4) 0.0417(15) Uani 1 1 d . . . O3 O 0.8448(3) 0.6327(3) 0.4397(3) 0.0418(10) Uani 1 1 d . . . C47 C 0.9519(6) 0.3630(5) 0.2105(5) 0.057(2) Uani 1 1 d . . . C48 C 0.969(2) 0.2967(12) 0.2406(13) 0.244(14) Uani 1 1 d . . . H38 H 1.0274 0.3254 0.3015 0.366 Uiso 1 1 calc R . . H39 H 0.9842 0.2511 0.1967 0.366 Uiso 1 1 calc R . . H40 H 0.9078 0.2694 0.2436 0.366 Uiso 1 1 calc R . . C49 C 1.0419(9) 0.3973(8) 0.1982(10) 0.137(6) Uani 1 1 d . . . H41 H 1.0330 0.4437 0.1813 0.206 Uiso 1 1 calc R . . H42 H 1.0482 0.3491 0.1495 0.206 Uiso 1 1 calc R . . H43 H 1.1039 0.4217 0.2558 0.206 Uiso 1 1 calc R . . C50 C 0.8642(9) 0.3222(10) 0.1170(9) 0.189(10) Uani 1 1 d . . . H44 H 0.8554 0.3680 0.0989 0.284 Uiso 1 1 calc R . . H45 H 0.8014 0.2955 0.1185 0.284 Uiso 1 1 calc R . . H46 H 0.8785 0.2767 0.0725 0.284 Uiso 1 1 calc R . . N5 N 0.9093(4) 0.7369(4) 0.3747(4) 0.0427(13) Uani 1 1 d . . . C51 C 0.9023(5) 0.6581(5) 0.3085(4) 0.0439(16) Uani 1 1 d . . . C52 C 0.8878(6) 0.6508(5) 0.2218(5) 0.0516(18) Uani 1 1 d . . . H47 H 0.8805 0.5964 0.1737 0.062 Uiso 1 1 calc R . . C53 C 0.8845(6) 0.7210(5) 0.2074(5) 0.0553(19) Uani 1 1 d . . . H48 H 0.8790 0.7167 0.1504 0.066 Uiso 1 1 calc R . . C54 C 0.8889(6) 0.7998(5) 0.2753(5) 0.0513(18) Uani 1 1 d . . . H49 H 0.8853 0.8491 0.2651 0.062 Uiso 1 1 calc R . . C55 C 0.8988(5) 0.8036(4) 0.3578(4) 0.0427(15) Uani 1 1 d . . . N6 N 0.8907(4) 0.8704(4) 0.5023(4) 0.0420(13) Uani 1 1 d . . . C56 C 0.8910(5) 0.8802(4) 0.4305(5) 0.0420(15) Uani 1 1 d . . . C57 C 0.8799(6) 0.9536(5) 0.4228(5) 0.0503(17) Uani 1 1 d . . . H50 H 0.8844 0.9612 0.3734 0.060 Uiso 1 1 calc R . . C58 C 0.8618(6) 1.0164(5) 0.4886(5) 0.0514(18) Uani 1 1 d . . . H51 H 0.8543 1.0681 0.4849 0.062 Uiso 1 1 calc R . . C59 C 0.8547(5) 1.0045(5) 0.5593(5) 0.0471(16) Uani 1 1 d . . . H52 H 0.8383 1.0459 0.6026 0.056 Uiso 1 1 calc R . . C60 C 0.8718(5) 0.9304(4) 0.5668(4) 0.0426(15) Uani 1 1 d . . . C61 C 0.8468(5) 0.8332(4) 0.6409(4) 0.0405(15) Uani 1 1 d . . . C62 C 0.8683(5) 0.9160(4) 0.6437(4) 0.0418(15) Uani 1 1 d . . . C63 C 0.8830(5) 0.9915(5) 0.7248(4) 0.0461(16) Uani 1 1 d . . . H53 H 0.8995 1.0477 0.7276 0.055 Uiso 1 1 calc R . . C64 C 0.8747(5) 0.9876(5) 0.7987(5) 0.0484(17) Uani 1 1 d . A . C65 C 0.8498(6) 0.9058(5) 0.7928(5) 0.0527(18) Uani 1 1 d . . . H54 H 0.8407 0.9005 0.8418 0.063 Uiso 1 1 calc R . . C66 C 0.8376(5) 0.8303(5) 0.7165(4) 0.0480(17) Uani 1 1 d . . . H55 H 0.8226 0.7750 0.7158 0.058 Uiso 1 1 calc R . . O4 O 0.8359(3) 0.7590(3) 0.5703(3) 0.0405(10) Uani 1 1 d . . . C67 C 0.8915(6) 1.0727(5) 0.8851(5) 0.0548(19) Uani 1 1 d . . . C68 C 0.9752(14) 1.0806(12) 0.9688(11) 0.075(7) Uani 0.53(2) 1 d P A 1 H56 H 1.0387 1.0846 0.9614 0.113 Uiso 0.53(2) 1 calc PR A 1 H57 H 0.9552 1.0285 0.9760 0.113 Uiso 0.53(2) 1 calc PR A 1 H58 H 0.9860 1.1339 1.0234 0.113 Uiso 0.53(2) 1 calc PR A 1 C69 C 0.7979(16) 1.0661(16) 0.8960(14) 0.094(9) Uani 0.53(2) 1 d P A 1 H59 H 0.7422 1.0568 0.8400 0.140 Uiso 0.53(2) 1 calc PR A 1 H60 H 0.8069 1.1208 0.9482 0.140 Uiso 0.53(2) 1 calc PR A 1 H61 H 0.7809 1.0162 0.9073 0.140 Uiso 0.53(2) 1 calc PR A 1 C70 C 0.927(3) 1.1546(13) 0.8787(17) 0.135(16) Uani 0.53(2) 1 d P A 1 H62 H 0.8743 1.1532 0.8259 0.202 Uiso 0.53(2) 1 calc PR A 1 H63 H 0.9905 1.1571 0.8709 0.202 Uiso 0.53(2) 1 calc PR A 1 H64 H 0.9400 1.2069 0.9351 0.202 Uiso 0.53(2) 1 calc PR A 1 C71 C 1.0025(13) 1.1268(12) 0.9390(11) 0.057(6) Uani 0.47(2) 1 d P A 2 H65 H 1.0418 1.0912 0.9567 0.086 Uiso 0.47(2) 1 calc PR A 2 H66 H 1.0124 1.1788 0.9943 0.086 Uiso 0.47(2) 1 calc PR A 2 H67 H 1.0262 1.1459 0.9014 0.086 Uiso 0.47(2) 1 calc PR A 2 C72 C 0.854(2) 1.0494(14) 0.9470(16) 0.088(9) Uani 0.47(2) 1 d P A 2 H68 H 0.8929 1.0153 0.9684 0.132 Uiso 0.47(2) 1 calc PR A 2 H69 H 0.7810 1.0140 0.9124 0.132 Uiso 0.47(2) 1 calc PR A 2 H70 H 0.8638 1.1038 1.0000 0.132 Uiso 0.47(2) 1 calc PR A 2 C73 C 0.8254(19) 1.1228(14) 0.8568(12) 0.072(7) Uani 0.47(2) 1 d P A 2 H71 H 0.8444 1.1408 0.8164 0.108 Uiso 0.47(2) 1 calc PR A 2 H72 H 0.8351 1.1754 0.9115 0.108 Uiso 0.47(2) 1 calc PR A 2 H73 H 0.7535 1.0850 0.8240 0.108 Uiso 0.47(2) 1 calc PR A 2 O5 O 0.4113(5) 0.5094(5) 0.2032(4) 0.0693(17) Uani 1 1 d . . . O6 O 0.3639(7) 0.6068(6) 0.2778(6) 0.107(3) Uani 1 1 d . . . C74 C 0.3526(7) 0.5389(7) 0.2117(5) 0.063(2) Uani 1 1 d . . . C75 C 0.2399(9) 0.4919(12) 0.1416(11) 0.148(6) Uani 1 1 d . . . H74 H 0.1990 0.5283 0.1607 0.223 Uiso 1 1 calc R . . H75 H 0.2153 0.4346 0.1382 0.223 Uiso 1 1 calc R . . H76 H 0.2333 0.4828 0.0811 0.223 Uiso 1 1 calc R . . O7 O 1.0604(4) 0.7602(3) 0.5756(4) 0.0618(14) Uani 1 1 d . . . O8 O 1.1178(6) 0.9019(4) 0.6411(5) 0.099(3) Uani 1 1 d . . . C76 C 1.1282(6) 0.8310(5) 0.6302(5) 0.0487(17) Uani 1 1 d . . . C77 C 1.2305(6) 0.8325(6) 0.6925(6) 0.068(2) Uani 1 1 d . . . H77 H 1.2292 0.7718 0.6771 0.102 Uiso 1 1 calc R . . H78 H 1.2425 0.8649 0.7567 0.102 Uiso 1 1 calc R . . H79 H 1.2856 0.8619 0.6835 0.102 Uiso 1 1 calc R . . Cl1 Cl 0.7707(3) 0.7019(3) 0.8302(3) 0.0760(11) Uani 0.75 1 d PU B 1 Cl2 Cl 0.6461(3) 0.8120(3) 0.8507(3) 0.0915(10) Uani 0.75 1 d P B 1 Cl3 Cl 0.7111(3) 0.7464(3) 0.9778(2) 0.0926(11) Uani 0.75 1 d P B 1 C78 C 0.6742(10) 0.7241(9) 0.8652(9) 0.075(3) Uani 0.75 1 d P B 1 H84 H 0.6112 0.6706 0.8253 0.090 Uiso 0.75 1 calc PR B 1 Cl4 Cl 0.8324(9) 0.6707(10) 0.9684(8) 0.108(4) Uani 0.25 1 d PU C 2 Cl5 Cl 0.6368(9) 0.6897(9) 0.8997(8) 0.095(3) Uani 0.25 1 d PU C 2 Cl6 Cl 0.7790(18) 0.7440(14) 0.8375(15) 0.139(6) Uani 0.25 1 d PU C 2 C79 C 0.737(3) 0.660(3) 0.875(3) 0.085(6) Uani 0.25 1 d PU C 2 H85 H 0.7105 0.5980 0.8230 0.102 Uiso 0.25 1 calc PR C 2 C80 C 1.1727(9) 1.0211(10) 0.8537(8) 0.119(5) Uani 1 1 d . . . H80 H 1.0992 0.9883 0.8247 0.179 Uiso 1 1 calc R . . H81 H 1.1913 1.0708 0.9140 0.179 Uiso 1 1 calc R . . H82 H 1.2117 0.9818 0.8612 0.179 Uiso 1 1 calc R . . O9 O 1.1950(6) 1.0528(5) 0.7986(6) 0.116(3) Uani 1 1 d . . . H83 H 1.1739 1.0107 0.7454 0.174 Uiso 1 1 calc R . . C81 C 0.3200(12) 0.7364(11) 0.1849(11) 0.143(5) Uiso 1 1 d . . . H86 H 0.3890 0.7371 0.1907 0.214 Uiso 1 1 calc R . . H87 H 0.3021 0.7801 0.1661 0.214 Uiso 1 1 calc R . . H88 H 0.2707 0.6775 0.1385 0.214 Uiso 1 1 calc R . . O10 O 0.3177(15) 0.7567(13) 0.2672(14) 0.278(9) Uiso 1 1 d . . . H89 H 0.3307 0.7181 0.2822 0.417 Uiso 1 1 calc R . . C82 C 0.1628(12) 0.7392(11) 0.3252(10) 0.136(5) Uiso 1 1 d . . . H90 H 0.2179 0.7344 0.3716 0.205 Uiso 1 1 calc R . . H91 H 0.1389 0.6870 0.2653 0.205 Uiso 1 1 calc R . . H92 H 0.1059 0.7430 0.3423 0.205 Uiso 1 1 calc R . . O11 O 0.1969(13) 0.8092(12) 0.3206(11) 0.237(7) Uiso 1 1 d . . . H93 H 0.2430 0.8044 0.3026 0.355 Uiso 1 1 calc R . . C83 C -0.0004(18) 0.5641(17) 0.0683(16) 0.101(7) Uiso 0.50 1 d P D 1 H95 H -0.0334 0.5554 0.1057 0.151 Uiso 0.50 1 calc PR D 1 H96 H 0.0108 0.5095 0.0341 0.151 Uiso 0.50 1 calc PR D 1 H97 H -0.0444 0.5797 0.0251 0.151 Uiso 0.50 1 calc PR D 1 O12 O 0.0831(16) 0.6246(13) 0.1189(13) 0.130(6) Uiso 0.50 1 d P D 1 H94 H 0.1157 0.6266 0.0881 0.194 Uiso 0.50 1 calc PR D 1 O13 O -0.1339(16) 0.4639(14) 0.0068(14) 0.140(7) Uiso 0.50 1 d P E 2 O14 O 0.0201(13) 0.6134(12) 0.0549(11) 0.103(5) Uiso 0.50 1 d P F 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 Zn1 0.0464(4) 0.0446(5) 0.0311(4) 0.0242(4) 0.0227(3) 0.0167(3) Zn2 0.0457(4) 0.0416(4) 0.0436(5) 0.0286(4) 0.0268(3) 0.0183(3) Zn3 0.0436(4) 0.0337(4) 0.0407(4) 0.0168(4) 0.0227(3) 0.0112(3) C1 0.031(3) 0.043(4) 0.032(3) 0.018(3) 0.012(2) 0.009(3) C2 0.036(3) 0.040(4) 0.025(3) 0.012(3) 0.009(2) 0.006(3) C3 0.045(4) 0.045(4) 0.034(4) 0.015(3) 0.017(3) 0.013(3) C4 0.039(3) 0.037(4) 0.045(4) 0.010(3) 0.013(3) 0.010(3) C5 0.046(4) 0.044(4) 0.046(4) 0.025(3) 0.015(3) 0.013(3) C6 0.040(3) 0.046(4) 0.035(4) 0.021(3) 0.014(3) 0.010(3) O1 0.047(2) 0.041(2) 0.026(2) 0.016(2) 0.0167(19) 0.015(2) C7 0.049(4) 0.045(4) 0.047(4) 0.011(4) 0.011(3) 0.010(3) C8 0.099(7) 0.049(5) 0.066(6) 0.017(4) 0.030(5) 0.035(5) C9 0.070(5) 0.042(4) 0.045(4) 0.002(4) 0.024(4) 0.013(4) C10 0.059(5) 0.043(4) 0.066(5) 0.009(4) 0.011(4) 0.002(4) N1 0.039(3) 0.041(3) 0.026(3) 0.016(2) 0.015(2) 0.011(2) C11 0.042(3) 0.046(4) 0.033(3) 0.018(3) 0.018(3) 0.010(3) C12 0.063(4) 0.047(4) 0.029(3) 0.009(3) 0.027(3) 0.009(3) C13 0.078(5) 0.046(4) 0.034(4) 0.019(3) 0.030(4) 0.008(4) C14 0.062(4) 0.054(4) 0.041(4) 0.029(4) 0.027(3) 0.010(4) C15 0.045(3) 0.040(3) 0.029(3) 0.021(3) 0.015(3) 0.011(3) N2 0.048(3) 0.048(3) 0.031(3) 0.025(3) 0.021(2) 0.019(3) C16 0.043(3) 0.049(4) 0.036(3) 0.028(3) 0.016(3) 0.015(3) C17 0.061(4) 0.062(5) 0.053(4) 0.043(4) 0.035(4) 0.027(4) C18 0.067(4) 0.043(4) 0.055(4) 0.033(4) 0.034(4) 0.025(3) C19 0.066(4) 0.052(4) 0.048(4) 0.031(4) 0.035(4) 0.032(4) C20 0.053(4) 0.045(4) 0.034(3) 0.023(3) 0.023(3) 0.024(3) C21 0.043(3) 0.039(3) 0.033(3) 0.019(3) 0.018(3) 0.018(3) C22 0.046(3) 0.050(4) 0.036(3) 0.027(3) 0.024(3) 0.021(3) C23 0.053(4) 0.046(4) 0.041(4) 0.026(3) 0.024(3) 0.024(3) C24 0.045(3) 0.041(4) 0.036(3) 0.018(3) 0.022(3) 0.018(3) C25 0.043(3) 0.046(4) 0.033(3) 0.021(3) 0.020(3) 0.017(3) C26 0.039(3) 0.041(3) 0.032(3) 0.019(3) 0.018(3) 0.016(3) O2 0.049(2) 0.038(2) 0.032(2) 0.020(2) 0.0234(19) 0.020(2) C27 0.048(4) 0.044(4) 0.035(4) 0.014(3) 0.019(3) 0.017(3) C28 0.055(4) 0.050(4) 0.054(5) 0.021(4) 0.023(4) 0.018(3) C29 0.055(4) 0.059(5) 0.060(5) 0.025(4) 0.029(4) 0.028(4) C30 0.067(5) 0.060(5) 0.042(4) 0.020(4) 0.030(4) 0.030(4) N3 0.043(3) 0.038(3) 0.029(3) 0.019(2) 0.016(2) 0.014(2) C31 0.041(3) 0.036(3) 0.029(3) 0.016(3) 0.017(3) 0.006(3) C32 0.056(4) 0.041(4) 0.035(4) 0.019(3) 0.026(3) 0.014(3) C33 0.060(4) 0.052(4) 0.041(4) 0.029(3) 0.028(3) 0.010(3) C34 0.062(4) 0.041(4) 0.032(3) 0.023(3) 0.022(3) 0.013(3) C35 0.044(3) 0.039(4) 0.030(3) 0.019(3) 0.011(3) 0.008(3) N4 0.045(3) 0.038(3) 0.029(3) 0.017(2) 0.015(2) 0.016(2) C36 0.047(4) 0.037(3) 0.027(3) 0.016(3) 0.010(3) 0.009(3) C37 0.059(4) 0.047(4) 0.044(4) 0.029(3) 0.021(3) 0.021(3) C38 0.059(4) 0.048(4) 0.055(5) 0.032(4) 0.013(4) 0.018(4) C39 0.045(4) 0.040(4) 0.057(4) 0.020(3) 0.019(3) 0.020(3) C40 0.033(3) 0.034(3) 0.035(3) 0.012(3) 0.008(3) 0.006(3) C41 0.042(3) 0.040(4) 0.039(4) 0.014(3) 0.020(3) 0.014(3) C42 0.036(3) 0.037(3) 0.035(3) 0.011(3) 0.012(3) 0.010(3) C43 0.038(3) 0.041(4) 0.049(4) 0.014(3) 0.019(3) 0.011(3) C44 0.042(4) 0.044(4) 0.048(4) 0.010(3) 0.019(3) 0.016(3) C45 0.041(4) 0.053(4) 0.046(4) 0.019(3) 0.025(3) 0.012(3) C46 0.038(3) 0.038(4) 0.040(4) 0.012(3) 0.016(3) 0.010(3) O3 0.045(2) 0.037(2) 0.054(3) 0.022(2) 0.031(2) 0.015(2) C47 0.054(4) 0.051(4) 0.051(5) 0.007(4) 0.028(4) 0.015(4) C48 0.58(4) 0.200(17) 0.239(19) 0.173(16) 0.33(3) 0.31(3) C49 0.105(9) 0.081(8) 0.186(13) -0.004(8) 0.108(10) 0.018(7) C50 0.084(8) 0.168(14) 0.114(11) -0.087(10) 0.000(7) 0.057(9) N5 0.046(3) 0.040(3) 0.049(3) 0.022(3) 0.027(3) 0.011(2) C51 0.041(3) 0.047(4) 0.040(4) 0.016(3) 0.020(3) 0.010(3) C52 0.059(4) 0.048(4) 0.043(4) 0.014(3) 0.028(3) 0.011(3) C53 0.059(4) 0.068(5) 0.045(4) 0.028(4) 0.029(4) 0.018(4) C54 0.060(4) 0.049(4) 0.049(4) 0.024(4) 0.031(4) 0.012(3) C55 0.042(3) 0.041(4) 0.046(4) 0.019(3) 0.025(3) 0.007(3) N6 0.045(3) 0.039(3) 0.046(3) 0.019(3) 0.027(3) 0.008(2) C56 0.042(3) 0.036(3) 0.049(4) 0.022(3) 0.023(3) 0.005(3) C57 0.058(4) 0.051(4) 0.057(4) 0.032(4) 0.035(4) 0.016(3) C58 0.063(4) 0.046(4) 0.064(5) 0.034(4) 0.038(4) 0.022(4) C59 0.056(4) 0.040(4) 0.049(4) 0.021(3) 0.027(3) 0.016(3) C60 0.053(4) 0.032(3) 0.043(4) 0.015(3) 0.025(3) 0.013(3) C61 0.046(4) 0.033(3) 0.038(4) 0.014(3) 0.018(3) 0.008(3) C62 0.044(3) 0.041(4) 0.039(4) 0.017(3) 0.019(3) 0.013(3) C63 0.048(4) 0.040(4) 0.039(4) 0.013(3) 0.016(3) 0.011(3) C64 0.050(4) 0.044(4) 0.037(4) 0.009(3) 0.015(3) 0.015(3) C65 0.063(4) 0.058(5) 0.034(4) 0.015(4) 0.025(3) 0.021(4) C66 0.053(4) 0.047(4) 0.032(4) 0.016(3) 0.012(3) 0.012(3) O4 0.053(3) 0.032(2) 0.042(3) 0.017(2) 0.029(2) 0.013(2) C67 0.065(5) 0.050(4) 0.037(4) 0.009(4) 0.023(3) 0.018(4) C68 0.089(13) 0.059(11) 0.048(10) 0.004(9) 0.025(9) 0.016(9) C69 0.087(14) 0.102(17) 0.046(12) -0.001(12) 0.020(10) 0.039(12) C70 0.27(5) 0.043(11) 0.092(18) 0.010(11) 0.11(3) 0.035(17) C71 0.068(11) 0.043(10) 0.036(9) 0.005(8) 0.018(8) 0.012(8) C72 0.12(2) 0.062(13) 0.057(14) 0.002(11) 0.053(15) 0.009(13) C73 0.098(16) 0.051(12) 0.044(10) 0.008(9) 0.020(10) 0.034(11) O5 0.058(3) 0.106(5) 0.066(4) 0.066(4) 0.026(3) 0.016(3) O6 0.154(7) 0.127(7) 0.110(6) 0.087(6) 0.078(6) 0.091(6) C74 0.069(5) 0.099(7) 0.028(4) 0.037(5) 0.027(4) 0.015(5) C75 0.065(7) 0.235(18) 0.197(15) 0.138(14) 0.063(9) 0.065(9) O7 0.053(3) 0.046(3) 0.072(4) 0.019(3) 0.021(3) 0.020(3) O8 0.114(5) 0.050(4) 0.086(5) 0.040(4) -0.010(4) 0.010(3) C76 0.060(4) 0.055(5) 0.063(5) 0.045(4) 0.038(4) 0.027(4) C77 0.046(4) 0.074(6) 0.065(5) 0.029(5) 0.011(4) 0.011(4) Cl1 0.075(2) 0.101(3) 0.0645(19) 0.044(2) 0.0385(16) 0.031(2) Cl2 0.094(2) 0.109(3) 0.097(2) 0.062(2) 0.052(2) 0.039(2) Cl3 0.117(3) 0.100(3) 0.076(2) 0.048(2) 0.056(2) 0.026(2) C78 0.077(8) 0.087(9) 0.084(8) 0.051(7) 0.051(7) 0.018(7) Cl4 0.090(6) 0.162(11) 0.084(6) 0.067(7) 0.041(5) 0.046(7) Cl5 0.082(5) 0.122(9) 0.072(6) 0.042(6) 0.030(5) 0.029(6) Cl6 0.142(10) 0.153(12) 0.132(9) 0.095(9) 0.059(7) 0.009(9) C79 0.076(12) 0.101(18) 0.085(15) 0.054(13) 0.034(7) 0.020(12) C80 0.071(7) 0.134(12) 0.084(8) -0.002(8) 0.028(6) 0.024(7) O9 0.105(6) 0.076(5) 0.105(6) 0.019(5) 0.014(5) 0.017(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 Zn1 O1 1.960(4) . ? Zn1 O2 1.995(4) . ? Zn1 O5 2.015(6) . ? Zn1 N1 2.086(5) . ? Zn1 N2 2.104(5) . ? Zn2 O3 1.928(4) . ? Zn2 O2 1.986(4) . ? Zn2 N3 2.045(5) . ? Zn2 N4 2.093(5) . ? Zn2 O4 2.111(4) . ? Zn2 Zn3 3.1206(10) . ? Zn3 O7 1.950(5) . ? Zn3 O4 2.006(4) . ? Zn3 O3 2.015(4) . ? Zn3 N6 2.057(6) . ? Zn3 N5 2.104(5) . ? C1 O1 1.316(7) . ? C1 C6 1.417(9) . ? C1 C2 1.427(8) . ? C2 C3 1.427(9) . ? C2 C11 1.472(9) . ? C3 C4 1.376(10) . ? C3 H1 0.9500 . ? C4 C5 1.385(9) . ? C4 C7 1.546(10) . ? C5 C6 1.379(10) . ? C5 H2 0.9500 . ? C6 H3 0.9500 . ? C7 C8 1.523(11) . ? C7 C9 1.529(11) . ? C7 C10 1.539(10) . ? C8 H4 0.9800 . ? C8 H5 0.9800 . ? C8 H6 0.9800 . ? C9 H7 0.9800 . ? C9 H8 0.9800 . ? C9 H9 0.9800 . ? C10 H10 0.9800 . ? C10 H11 0.9800 . ? C10 H12 0.9800 . ? N1 C15 1.332(8) . ? N1 C11 1.352(8) . ? C11 C12 1.409(8) . ? C12 C13 1.373(10) . ? C12 H13 0.9500 . ? C13 C14 1.384(10) . ? C13 H14 0.9500 . ? C14 C15 1.375(8) . ? C14 H15 0.9500 . ? C15 C16 1.494(9) . ? N2 C16 1.344(8) . ? N2 C20 1.358(8) . ? C16 C17 1.401(9) . ? C17 C18 1.378(10) . ? C17 H16 0.9500 . ? C18 C19 1.361(9) . ? C18 H17 0.9500 . ? C19 C20 1.401(10) . ? C19 H18 0.9500 . ? C20 C22 1.486(8) . ? C21 O2 1.347(7) . ? C21 C22 1.409(9) . ? C21 C26 1.411(8) . ? C22 C23 1.397(9) . ? C23 C24 1.398(8) . ? C23 H19 0.9500 . ? C24 C25 1.375(9) . ? C24 C27 1.533(9) . ? C25 C26 1.398(9) . ? C25 H20 0.9500 . ? C26 C31 1.486(9) . ? C27 C28 1.524(10) . ? C27 C29 1.536(10) . ? C27 C30 1.538(9) . ? C28 H21 0.9800 . ? C28 H22 0.9800 . ? C28 H23 0.9800 . ? C29 H24 0.9800 . ? C29 H25 0.9800 . ? C29 H26 0.9800 . ? C30 H27 0.9800 . ? C30 H28 0.9800 . ? C30 H29 0.9800 . ? N3 C31 1.335(8) . ? N3 C35 1.341(8) . ? C31 C32 1.391(8) . ? C32 C33 1.373(9) . ? C32 H30 0.9500 . ? C33 C34 1.385(10) . ? C33 H31 0.9500 . ? C34 C35 1.386(9) . ? C34 H32 0.9500 . ? C35 C36 1.507(10) . ? N4 C36 1.351(8) . ? N4 C40 1.365(8) . ? C36 C37 1.363(9) . ? C37 C38 1.377(11) . ? C37 H33 0.9500 . ? C38 C39 1.373(10) . ? C38 H34 0.9500 . ? C39 C40 1.393(10) . ? C39 H35 0.9500 . ? C40 C42 1.480(9) . ? C41 O3 1.329(8) . ? C41 C42 1.419(9) . ? C41 C46 1.428(9) . ? C42 C43 1.407(9) . ? C43 C44 1.376(10) . ? C43 H36 0.9500 . ? C44 C45 1.386(10) . ? C44 C47 1.543(10) . ? C45 C46 1.403(9) . ? C45 H37 0.9500 . ? C46 C51 1.468(10) . ? C47 C48 1.472(15) . ? C47 C49 1.482(13) . ? C47 C50 1.500(14) . ? C48 H38 0.9800 . ? C48 H39 0.9800 . ? C48 H40 0.9800 . ? C49 H41 0.9800 . ? C49 H42 0.9800 . ? C49 H43 0.9800 . ? C50 H44 0.9800 . ? C50 H45 0.9800 . ? C50 H46 0.9800 . ? N5 C55 1.330(9) . ? N5 C51 1.368(9) . ? C51 C52 1.417(9) . ? C52 C53 1.350(11) . ? C52 H47 0.9500 . ? C53 C54 1.395(10) . ? C53 H48 0.9500 . ? C54 C55 1.383(9) . ? C54 H49 0.9500 . ? C55 C56 1.494(9) . ? N6 C56 1.341(8) . ? N6 C60 1.351(8) . ? C56 C57 1.369(10) . ? C57 C58 1.380(10) . ? C57 H50 0.9500 . ? C58 C59 1.373(9) . ? C58 H51 0.9500 . ? C59 C60 1.403(10) . ? C59 H52 0.9500 . ? C60 C62 1.484(9) . ? C61 O4 1.334(7) . ? C61 C66 1.401(9) . ? C61 C62 1.407(9) . ? C62 C63 1.428(9) . ? C63 C64 1.371(10) . ? C63 H53 0.9500 . ? C64 C65 1.371(11) . ? C64 C67 1.560(9) . ? C65 C66 1.394(10) . ? C65 H54 0.9500 . ? C66 H55 0.9500 . ? C67 C69 1.44(2) . ? C67 C71 1.494(19) . ? C67 C73 1.50(2) . ? C67 C70 1.50(2) . ? C67 C68 1.509(19) . ? C67 C72 1.53(2) . ? C68 H56 0.9800 . ? C68 H57 0.9800 . ? C68 H58 0.9800 . ? C69 H59 0.9800 . ? C69 H60 0.9800 . ? C69 H61 0.9800 . ? C70 H62 0.9800 . ? C70 H63 0.9800 . ? C70 H64 0.9800 . ? C71 H65 0.9800 . ? C71 H66 0.9800 . ? C71 H67 0.9800 . ? C72 H68 0.9800 . ? C72 H69 0.9800 . ? C72 H70 0.9800 . ? C73 H71 0.9800 . ? C73 H72 0.9800 . ? C73 H73 0.9800 . ? O5 C74 1.092(11) . ? O6 C74 1.227(11) . ? C74 C75 1.534(15) . ? C75 H74 0.9800 . ? C75 H75 0.9800 . ? C75 H76 0.9800 . ? O7 C76 1.219(9) . ? O8 C76 1.217(9) . ? C76 C77 1.525(10) . ? C77 H77 0.9800 . ? C77 H78 0.9800 . ? C77 H79 0.9800 . ? Cl1 C78 1.760(13) . ? Cl2 C78 1.739(14) . ? Cl3 C78 1.726(12) . ? C78 H84 1.0000 . ? Cl4 C79 1.69(4) . ? Cl5 C79 1.77(4) . ? Cl6 C79 1.93(4) . ? C79 H85 1.0000 . ? C80 O9 1.389(15) . ? C80 H80 0.9800 . ? C80 H81 0.9800 . ? C80 H82 0.9800 . ? O9 H83 0.8400 . ? C81 O10 1.36(2) . ? C81 H86 0.9800 . ? C81 H87 0.9800 . ? C81 H88 0.9800 . ? O10 H89 0.8400 . ? C82 O11 1.289(19) . ? C82 H90 0.9800 . ? C82 H91 0.9800 . ? C82 H92 0.9800 . ? O11 H93 0.8400 . ? C83 O12 1.24(3) . ? C83 H95 0.9800 . ? C83 H96 0.9800 . ? C83 H97 0.9800 . ? O12 H94 0.8400 . ? 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 Zn1 O2 85.18(17) . . ? O1 Zn1 O5 105.8(2) . . ? O2 Zn1 O5 118.7(2) . . ? O1 Zn1 N1 88.24(19) . . ? O2 Zn1 N1 139.89(18) . . ? O5 Zn1 N1 101.2(2) . . ? O1 Zn1 N2 144.69(19) . . ? O2 Zn1 N2 83.71(18) . . ? O5 Zn1 N2 109.0(2) . . ? N1 Zn1 N2 79.2(2) . . ? O3 Zn2 O2 109.43(18) . . ? O3 Zn2 N3 164.4(2) . . ? O2 Zn2 N3 85.99(18) . . ? O3 Zn2 N4 87.44(19) . . ? O2 Zn2 N4 133.42(19) . . ? N3 Zn2 N4 79.9(2) . . ? O3 Zn2 O4 77.78(17) . . ? O2 Zn2 O4 97.50(18) . . ? N3 Zn2 O4 103.08(18) . . ? N4 Zn2 O4 128.85(19) . . ? O3 Zn2 Zn3 38.65(13) . . ? O2 Zn2 Zn3 103.52(12) . . ? N3 Zn2 Zn3 141.70(14) . . ? N4 Zn2 Zn3 114.92(15) . . ? O4 Zn2 Zn3 39.46(11) . . ? O7 Zn3 O4 111.1(2) . . ? O7 Zn3 O3 100.2(2) . . ? O4 Zn3 O3 78.35(17) . . ? O7 Zn3 N6 127.0(2) . . ? O4 Zn3 N6 87.07(19) . . ? O3 Zn3 N6 132.6(2) . . ? O7 Zn3 N5 109.2(2) . . ? O4 Zn3 N5 137.6(2) . . ? O3 Zn3 N5 82.14(19) . . ? N6 Zn3 N5 79.1(2) . . ? O7 Zn3 Zn2 113.70(17) . . ? O4 Zn3 Zn2 41.99(12) . . ? O3 Zn3 Zn2 36.70(12) . . ? N6 Zn3 Zn2 112.35(15) . . ? N5 Zn3 Zn2 108.25(15) . . ? O1 C1 C6 117.6(5) . . ? O1 C1 C2 125.0(6) . . ? C6 C1 C2 117.4(6) . . ? C3 C2 C1 117.7(6) . . ? C3 C2 C11 118.3(5) . . ? C1 C2 C11 123.9(6) . . ? C4 C3 C2 123.9(6) . . ? C4 C3 H1 118.1 . . ? C2 C3 H1 118.1 . . ? C3 C4 C5 116.9(6) . . ? C3 C4 C7 121.4(6) . . ? C5 C4 C7 121.6(7) . . ? C6 C5 C4 122.3(7) . . ? C6 C5 H2 118.9 . . ? C4 C5 H2 118.9 . . ? C5 C6 C1 121.6(6) . . ? C5 C6 H3 119.2 . . ? C1 C6 H3 119.2 . . ? C1 O1 Zn1 121.7(4) . . ? C8 C7 C9 108.6(7) . . ? C8 C7 C10 109.7(7) . . ? C9 C7 C10 106.6(7) . . ? C8 C7 C4 111.3(6) . . ? C9 C7 C4 111.7(6) . . ? C10 C7 C4 108.9(6) . . ? C7 C8 H4 109.5 . . ? C7 C8 H5 109.5 . . ? H4 C8 H5 109.5 . . ? C7 C8 H6 109.5 . . ? H4 C8 H6 109.5 . . ? H5 C8 H6 109.5 . . ? C7 C9 H7 109.5 . . ? C7 C9 H8 109.5 . . ? H7 C9 H8 109.5 . . ? C7 C9 H9 109.5 . . ? H7 C9 H9 109.5 . . ? H8 C9 H9 109.5 . . ? C7 C10 H10 109.5 . . ? C7 C10 H11 109.5 . . ? H10 C10 H11 109.5 . . ? C7 C10 H12 109.5 . . ? H10 C10 H12 109.5 . . ? H11 C10 H12 109.5 . . ? C15 N1 C11 121.3(5) . . ? C15 N1 Zn1 114.4(4) . . ? C11 N1 Zn1 124.0(4) . . ? N1 C11 C12 118.0(6) . . ? N1 C11 C2 120.5(5) . . ? C12 C11 C2 121.5(6) . . ? C13 C12 C11 120.4(7) . . ? C13 C12 H13 119.8 . . ? C11 C12 H13 119.8 . . ? C12 C13 C14 119.4(6) . . ? C12 C13 H14 120.3 . . ? C14 C13 H14 120.3 . . ? C15 C14 C13 118.2(7) . . ? C15 C14 H15 120.9 . . ? C13 C14 H15 120.9 . . ? N1 C15 C14 122.2(6) . . ? N1 C15 C16 115.7(5) . . ? C14 C15 C16 122.1(6) . . ? C16 N2 C20 120.4(6) . . ? C16 N2 Zn1 113.4(4) . . ? C20 N2 Zn1 125.9(4) . . ? N2 C16 C17 121.4(6) . . ? N2 C16 C15 116.2(6) . . ? C17 C16 C15 122.3(5) . . ? C18 C17 C16 118.5(6) . . ? C18 C17 H16 120.8 . . ? C16 C17 H16 120.8 . . ? C19 C18 C17 119.7(7) . . ? C19 C18 H17 120.1 . . ? C17 C18 H17 120.1 . . ? C18 C19 C20 120.8(7) . . ? C18 C19 H18 119.6 . . ? C20 C19 H18 119.6 . . ? N2 C20 C19 119.1(5) . . ? N2 C20 C22 121.1(6) . . ? C19 C20 C22 119.8(6) . . ? O2 C21 C22 120.7(5) . . ? O2 C21 C26 120.4(6) . . ? C22 C21 C26 118.9(6) . . ? C23 C22 C21 119.2(5) . . ? C23 C22 C20 118.3(6) . . ? C21 C22 C20 122.4(6) . . ? C22 C23 C24 122.6(6) . . ? C22 C23 H19 118.7 . . ? C24 C23 H19 118.7 . . ? C25 C24 C23 116.9(6) . . ? C25 C24 C27 123.1(5) . . ? C23 C24 C27 119.9(6) . . ? C24 C25 C26 123.1(6) . . ? C24 C25 H20 118.5 . . ? C26 C25 H20 118.5 . . ? C25 C26 C21 119.2(6) . . ? C25 C26 C31 117.9(5) . . ? C21 C26 C31 122.8(6) . . ? C21 O2 Zn2 115.0(4) . . ? C21 O2 Zn1 125.2(4) . . ? Zn2 O2 Zn1 119.2(2) . . ? C28 C27 C24 109.8(6) . . ? C28 C27 C29 109.9(6) . . ? C24 C27 C29 108.9(5) . . ? C28 C27 C30 109.2(6) . . ? C24 C27 C30 111.1(6) . . ? C29 C27 C30 108.0(6) . . ? C27 C28 H21 109.5 . . ? C27 C28 H22 109.5 . . ? H21 C28 H22 109.5 . . ? C27 C28 H23 109.5 . . ? H21 C28 H23 109.5 . . ? H22 C28 H23 109.5 . . ? C27 C29 H24 109.5 . . ? C27 C29 H25 109.5 . . ? H24 C29 H25 109.5 . . ? C27 C29 H26 109.5 . . ? H24 C29 H26 109.5 . . ? H25 C29 H26 109.5 . . ? C27 C30 H27 109.5 . . ? C27 C30 H28 109.5 . . ? H27 C30 H28 109.5 . . ? C27 C30 H29 109.5 . . ? H27 C30 H29 109.5 . . ? H28 C30 H29 109.5 . . ? C31 N3 C35 120.7(5) . . ? C31 N3 Zn2 123.3(4) . . ? C35 N3 Zn2 115.2(4) . . ? N3 C31 C32 120.0(6) . . ? N3 C31 C26 118.9(5) . . ? C32 C31 C26 121.1(6) . . ? C33 C32 C31 119.8(7) . . ? C33 C32 H30 120.1 . . ? C31 C32 H30 120.1 . . ? C32 C33 C34 119.6(6) . . ? C32 C33 H31 120.2 . . ? C34 C33 H31 120.2 . . ? C33 C34 C35 118.1(6) . . ? C33 C34 H32 120.9 . . ? C35 C34 H32 120.9 . . ? N3 C35 C34 121.5(6) . . ? N3 C35 C36 115.8(5) . . ? C34 C35 C36 122.6(6) . . ? C36 N4 C40 119.5(6) . . ? C36 N4 Zn2 113.7(4) . . ? C40 N4 Zn2 126.3(4) . . ? N4 C36 C37 122.8(6) . . ? N4 C36 C35 114.5(6) . . ? C37 C36 C35 122.7(6) . . ? C36 C37 C38 118.1(7) . . ? C36 C37 H33 120.9 . . ? C38 C37 H33 120.9 . . ? C39 C38 C37 120.3(7) . . ? C39 C38 H34 119.9 . . ? C37 C38 H34 119.9 . . ? C38 C39 C40 119.9(7) . . ? C38 C39 H35 120.0 . . ? C40 C39 H35 120.0 . . ? N4 C40 C39 119.2(6) . . ? N4 C40 C42 120.6(6) . . ? C39 C40 C42 120.1(6) . . ? O3 C41 C42 121.0(6) . . ? O3 C41 C46 119.0(6) . . ? C42 C41 C46 120.1(6) . . ? C43 C42 C41 117.7(6) . . ? C43 C42 C40 117.9(6) . . ? C41 C42 C40 124.4(6) . . ? C44 C43 C42 123.3(7) . . ? C44 C43 H36 118.3 . . ? C42 C43 H36 118.3 . . ? C43 C44 C45 118.0(6) . . ? C43 C44 C47 121.5(7) . . ? C45 C44 C47 120.4(7) . . ? C44 C45 C46 122.6(6) . . ? C44 C45 H37 118.7 . . ? C46 C45 H37 118.7 . . ? C45 C46 C41 118.2(6) . . ? C45 C46 C51 119.0(6) . . ? C41 C46 C51 122.7(6) . . ? C41 O3 Zn2 130.4(4) . . ? C41 O3 Zn3 124.0(4) . . ? Zn2 O3 Zn3 104.6(2) . . ? C48 C47 C49 108.5(12) . . ? C48 C47 C50 111.7(13) . . ? C49 C47 C50 104.2(11) . . ? C48 C47 C44 112.7(7) . . ? C49 C47 C44 112.4(7) . . ? C50 C47 C44 107.1(7) . . ? C47 C48 H38 109.5 . . ? C47 C48 H39 109.5 . . ? H38 C48 H39 109.5 . . ? C47 C48 H40 109.5 . . ? H38 C48 H40 109.5 . . ? H39 C48 H40 109.5 . . ? C47 C49 H41 109.5 . . ? C47 C49 H42 109.5 . . ? H41 C49 H42 109.5 . . ? C47 C49 H43 109.5 . . ? H41 C49 H43 109.5 . . ? H42 C49 H43 109.5 . . ? C47 C50 H44 109.5 . . ? C47 C50 H45 109.5 . . ? H44 C50 H45 109.5 . . ? C47 C50 H46 109.5 . . ? H44 C50 H46 109.5 . . ? H45 C50 H46 109.5 . . ? C55 N5 C51 121.5(6) . . ? C55 N5 Zn3 113.5(4) . . ? C51 N5 Zn3 124.9(5) . . ? N5 C51 C52 117.9(7) . . ? N5 C51 C46 121.1(6) . . ? C52 C51 C46 120.9(6) . . ? C53 C52 C51 120.1(7) . . ? C53 C52 H47 119.9 . . ? C51 C52 H47 119.9 . . ? C52 C53 C54 120.8(7) . . ? C52 C53 H48 119.6 . . ? C54 C53 H48 119.6 . . ? C55 C54 C53 117.6(7) . . ? C55 C54 H49 121.2 . . ? C53 C54 H49 121.2 . . ? N5 C55 C54 121.9(6) . . ? N5 C55 C56 116.0(6) . . ? C54 C55 C56 122.0(7) . . ? C56 N6 C60 120.6(6) . . ? C56 N6 Zn3 114.8(4) . . ? C60 N6 Zn3 124.5(4) . . ? N6 C56 C57 121.9(6) . . ? N6 C56 C55 115.3(6) . . ? C57 C56 C55 122.7(6) . . ? C56 C57 C58 118.3(6) . . ? C56 C57 H50 120.8 . . ? C58 C57 H50 120.8 . . ? C59 C58 C57 120.3(7) . . ? C59 C58 H51 119.8 . . ? C57 C58 H51 119.8 . . ? C58 C59 C60 119.2(7) . . ? C58 C59 H52 120.4 . . ? C60 C59 H52 120.4 . . ? N6 C60 C59 119.4(6) . . ? N6 C60 C62 119.3(6) . . ? C59 C60 C62 121.3(6) . . ? O4 C61 C66 119.6(6) . . ? O4 C61 C62 122.9(6) . . ? C66 C61 C62 117.5(6) . . ? C61 C62 C63 117.8(6) . . ? C61 C62 C60 124.8(6) . . ? C63 C62 C60 117.3(6) . . ? C64 C63 C62 123.9(7) . . ? C64 C63 H53 118.0 . . ? C62 C63 H53 118.0 . . ? C63 C64 C65 117.1(6) . . ? C63 C64 C67 121.3(7) . . ? C65 C64 C67 121.5(6) . . ? C64 C65 C66 121.3(7) . . ? C64 C65 H54 119.3 . . ? C66 C65 H54 119.3 . . ? C65 C66 C61 122.2(7) . . ? C65 C66 H55 118.9 . . ? C61 C66 H55 118.9 . . ? C61 O4 Zn3 119.4(4) . . ? C61 O4 Zn2 142.0(4) . . ? Zn3 O4 Zn2 98.55(17) . . ? C69 C67 C71 139.2(11) . . ? C69 C67 C73 60.8(14) . . ? C71 C67 C73 113.0(13) . . ? C69 C67 C70 111.3(18) . . ? C71 C67 C70 61.9(16) . . ? C73 C67 C70 54.4(15) . . ? C69 C67 C68 109.2(13) . . ? C71 C67 C68 47.4(10) . . ? C73 C67 C68 140.8(11) . . ? C70 C67 C68 106.5(16) . . ? C69 C67 C72 46.0(13) . . ? C71 C67 C72 108.8(13) . . ? C73 C67 C72 103.7(16) . . ? C70 C67 C72 136.9(12) . . ? C68 C67 C72 65.4(13) . . ? C69 C67 C64 109.2(10) . . ? C71 C67 C64 110.3(8) . . ? C73 C67 C64 109.9(8) . . ? C70 C67 C64 111.4(9) . . ? C68 C67 C64 109.1(9) . . ? C72 C67 C64 111.0(10) . . ? C67 C68 H56 109.5 . . ? C67 C68 H57 109.5 . . ? H56 C68 H57 109.5 . . ? C67 C68 H58 109.5 . . ? H56 C68 H58 109.5 . . ? H57 C68 H58 109.5 . . ? C67 C69 H59 109.5 . . ? C67 C69 H60 109.5 . . ? H59 C69 H60 109.5 . . ? C67 C69 H61 109.5 . . ? H59 C69 H61 109.5 . . ? H60 C69 H61 109.5 . . ? C67 C70 H62 109.5 . . ? C67 C70 H63 109.5 . . ? H62 C70 H63 109.5 . . ? C67 C70 H64 109.5 . . ? H62 C70 H64 109.5 . . ? H63 C70 H64 109.5 . . ? C67 C71 H65 109.5 . . ? C67 C71 H66 109.5 . . ? H65 C71 H66 109.5 . . ? C67 C71 H67 109.5 . . ? H65 C71 H67 109.5 . . ? H66 C71 H67 109.5 . . ? C67 C72 H68 109.5 . . ? C67 C72 H69 109.5 . . ? H68 C72 H69 109.5 . . ? C67 C72 H70 109.5 . . ? H68 C72 H70 109.5 . . ? H69 C72 H70 109.5 . . ? C67 C73 H71 109.5 . . ? C67 C73 H72 109.5 . . ? H71 C73 H72 109.5 . . ? C67 C73 H73 109.5 . . ? H71 C73 H73 109.5 . . ? H72 C73 H73 109.5 . . ? C74 O5 Zn1 123.4(7) . . ? O5 C74 O6 126.9(10) . . ? O5 C74 C75 121.3(11) . . ? O6 C74 C75 111.6(11) . . ? C74 C75 H74 109.5 . . ? C74 C75 H75 109.5 . . ? H74 C75 H75 109.5 . . ? C74 C75 H76 109.5 . . ? H74 C75 H76 109.5 . . ? H75 C75 H76 109.5 . . ? C76 O7 Zn3 117.4(5) . . ? O8 C76 O7 123.7(7) . . ? O8 C76 C77 117.3(8) . . ? O7 C76 C77 118.9(7) . . ? C76 C77 H77 109.5 . . ? C76 C77 H78 109.5 . . ? H77 C77 H78 109.5 . . ? C76 C77 H79 109.5 . . ? H77 C77 H79 109.5 . . ? H78 C77 H79 109.5 . . ? Cl3 C78 Cl2 111.0(8) . . ? Cl3 C78 Cl1 110.9(8) . . ? Cl2 C78 Cl1 109.4(6) . . ? Cl3 C78 H84 108.5 . . ? Cl2 C78 H84 108.5 . . ? Cl1 C78 H84 108.5 . . ? Cl4 C79 Cl5 111(2) . . ? Cl4 C79 Cl6 112(2) . . ? Cl5 C79 Cl6 101(2) . . ? Cl4 C79 H85 110.7 . . ? Cl5 C79 H85 110.7 . . ? Cl6 C79 H85 110.7 . . ? O9 C80 H80 109.5 . . ? O9 C80 H81 109.5 . . ? H80 C80 H81 109.5 . . ? O9 C80 H82 109.5 . . ? H80 C80 H82 109.5 . . ? H81 C80 H82 109.5 . . ? C80 O9 H83 109.5 . . ? O10 C81 H86 109.5 . . ? O10 C81 H87 109.5 . . ? H86 C81 H87 109.5 . . ? O10 C81 H88 109.5 . . ? H86 C81 H88 109.5 . . ? H87 C81 H88 109.5 . . ? C81 O10 H89 109.5 . . ? O11 C82 H90 109.5 . . ? O11 C82 H91 109.5 . . ? H90 C82 H91 109.5 . . ? O11 C82 H92 109.5 . . ? H90 C82 H92 109.5 . . ? H91 C82 H92 109.5 . . ? C82 O11 H93 109.5 . . ? O12 C83 H95 109.5 . . ? O12 C83 H96 109.5 . . ? H95 C83 H96 109.5 . . ? O12 C83 H97 109.5 . . ? H95 C83 H97 109.5 . . ? H96 C83 H97 109.5 . . ? C83 O12 H94 109.5 . . ? 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 O3 Zn2 Zn3 O7 -74.6(3) . . . . ? O2 Zn2 Zn3 O7 -178.9(2) . . . . ? N3 Zn2 Zn3 O7 80.2(3) . . . . ? N4 Zn2 Zn3 O7 -25.9(2) . . . . ? O4 Zn2 Zn3 O7 95.7(3) . . . . ? O3 Zn2 Zn3 O4 -170.3(3) . . . . ? O2 Zn2 Zn3 O4 85.4(2) . . . . ? N3 Zn2 Zn3 O4 -15.5(3) . . . . ? N4 Zn2 Zn3 O4 -121.6(2) . . . . ? O2 Zn2 Zn3 O3 -104.3(3) . . . . ? N3 Zn2 Zn3 O3 154.8(3) . . . . ? N4 Zn2 Zn3 O3 48.7(3) . . . . ? O4 Zn2 Zn3 O3 170.3(3) . . . . ? O3 Zn2 Zn3 N6 132.3(3) . . . . ? O2 Zn2 Zn3 N6 28.0(2) . . . . ? N3 Zn2 Zn3 N6 -72.8(3) . . . . ? N4 Zn2 Zn3 N6 -179.0(2) . . . . ? O4 Zn2 Zn3 N6 -57.4(3) . . . . ? O3 Zn2 Zn3 N5 46.9(3) . . . . ? O2 Zn2 Zn3 N5 -57.4(2) . . . . ? N3 Zn2 Zn3 N5 -158.3(3) . . . . ? N4 Zn2 Zn3 N5 95.6(2) . . . . ? O4 Zn2 Zn3 N5 -142.8(3) . . . . ? O1 C1 C2 C3 -176.1(6) . . . . ? C6 C1 C2 C3 4.6(8) . . . . ? O1 C1 C2 C11 4.6(10) . . . . ? C6 C1 C2 C11 -174.7(6) . . . . ? C1 C2 C3 C4 -4.0(10) . . . . ? C11 C2 C3 C4 175.4(6) . . . . ? C2 C3 C4 C5 1.3(10) . . . . ? C2 C3 C4 C7 178.5(6) . . . . ? C3 C4 C5 C6 0.7(10) . . . . ? C7 C4 C5 C6 -176.5(6) . . . . ? C4 C5 C6 C1 0.2(10) . . . . ? O1 C1 C6 C5 177.7(6) . . . . ? C2 C1 C6 C5 -2.9(9) . . . . ? C6 C1 O1 Zn1 -146.9(4) . . . . ? C2 C1 O1 Zn1 33.7(8) . . . . ? O2 Zn1 O1 C1 176.8(4) . . . . ? O5 Zn1 O1 C1 58.3(5) . . . . ? N1 Zn1 O1 C1 -42.8(4) . . . . ? N2 Zn1 O1 C1 -111.2(5) . . . . ? C3 C4 C7 C8 145.1(7) . . . . ? C5 C4 C7 C8 -37.8(10) . . . . ? C3 C4 C7 C9 23.6(9) . . . . ? C5 C4 C7 C9 -159.3(7) . . . . ? C3 C4 C7 C10 -93.9(8) . . . . ? C5 C4 C7 C10 83.2(8) . . . . ? O1 Zn1 N1 C15 -156.0(4) . . . . ? O2 Zn1 N1 C15 -75.6(5) . . . . ? O5 Zn1 N1 C15 98.3(5) . . . . ? N2 Zn1 N1 C15 -9.2(4) . . . . ? O1 Zn1 N1 C11 30.6(5) . . . . ? O2 Zn1 N1 C11 110.9(5) . . . . ? O5 Zn1 N1 C11 -75.2(5) . . . . ? N2 Zn1 N1 C11 177.4(5) . . . . ? C15 N1 C11 C12 0.2(9) . . . . ? Zn1 N1 C11 C12 173.2(5) . . . . ? C15 N1 C11 C2 179.8(5) . . . . ? Zn1 N1 C11 C2 -7.2(8) . . . . ? C3 C2 C11 N1 162.8(6) . . . . ? C1 C2 C11 N1 -17.9(9) . . . . ? C3 C2 C11 C12 -17.7(9) . . . . ? C1 C2 C11 C12 161.6(6) . . . . ? N1 C11 C12 C13 -5.8(10) . . . . ? C2 C11 C12 C13 174.6(6) . . . . ? C11 C12 C13 C14 6.6(11) . . . . ? C12 C13 C14 C15 -1.8(11) . . . . ? C11 N1 C15 C14 4.6(9) . . . . ? Zn1 N1 C15 C14 -169.0(5) . . . . ? C11 N1 C15 C16 -174.4(6) . . . . ? Zn1 N1 C15 C16 12.0(7) . . . . ? C13 C14 C15 N1 -3.8(10) . . . . ? C13 C14 C15 C16 175.2(6) . . . . ? O1 Zn1 N2 C16 75.7(5) . . . . ? O2 Zn1 N2 C16 148.1(5) . . . . ? O5 Zn1 N2 C16 -93.7(5) . . . . ? N1 Zn1 N2 C16 4.6(4) . . . . ? O1 Zn1 N2 C20 -98.2(6) . . . . ? O2 Zn1 N2 C20 -25.7(5) . . . . ? O5 Zn1 N2 C20 92.5(5) . . . . ? N1 Zn1 N2 C20 -169.3(5) . . . . ? C20 N2 C16 C17 -3.4(9) . . . . ? Zn1 N2 C16 C17 -177.6(5) . . . . ? C20 N2 C16 C15 174.4(6) . . . . ? Zn1 N2 C16 C15 0.2(7) . . . . ? N1 C15 C16 N2 -8.2(8) . . . . ? C14 C15 C16 N2 172.8(6) . . . . ? N1 C15 C16 C17 169.6(6) . . . . ? C14 C15 C16 C17 -9.5(10) . . . . ? N2 C16 C17 C18 1.2(10) . . . . ? C15 C16 C17 C18 -176.5(6) . . . . ? C16 C17 C18 C19 1.6(11) . . . . ? C17 C18 C19 C20 -2.1(11) . . . . ? C16 N2 C20 C19 2.8(9) . . . . ? Zn1 N2 C20 C19 176.3(5) . . . . ? C16 N2 C20 C22 -176.5(6) . . . . ? Zn1 N2 C20 C22 -3.1(9) . . . . ? C18 C19 C20 N2 -0.1(10) . . . . ? C18 C19 C20 C22 179.2(7) . . . . ? O2 C21 C22 C23 176.9(6) . . . . ? C26 C21 C22 C23 -3.8(9) . . . . ? O2 C21 C22 C20 -6.3(10) . . . . ? C26 C21 C22 C20 172.9(6) . . . . ? N2 C20 C22 C23 -155.5(6) . . . . ? C19 C20 C22 C23 25.1(10) . . . . ? N2 C20 C22 C21 27.7(10) . . . . ? C19 C20 C22 C21 -151.6(7) . . . . ? C21 C22 C23 C24 4.2(10) . . . . ? C20 C22 C23 C24 -172.6(6) . . . . ? C22 C23 C24 C25 -0.8(10) . . . . ? C22 C23 C24 C27 178.8(6) . . . . ? C23 C24 C25 C26 -3.1(10) . . . . ? C27 C24 C25 C26 177.3(6) . . . . ? C24 C25 C26 C21 3.4(10) . . . . ? C24 C25 C26 C31 -173.0(6) . . . . ? O2 C21 C26 C25 179.5(6) . . . . ? C22 C21 C26 C25 0.2(9) . . . . ? O2 C21 C26 C31 -4.4(9) . . . . ? C22 C21 C26 C31 176.3(6) . . . . ? C22 C21 O2 Zn2 130.2(5) . . . . ? C26 C21 O2 Zn2 -49.0(7) . . . . ? C22 C21 O2 Zn1 -40.5(8) . . . . ? C26 C21 O2 Zn1 140.3(5) . . . . ? O3 Zn2 O2 C21 -124.2(4) . . . . ? N3 Zn2 O2 C21 58.2(4) . . . . ? N4 Zn2 O2 C21 130.3(4) . . . . ? O4 Zn2 O2 C21 -44.5(4) . . . . ? Zn3 Zn2 O2 C21 -84.2(4) . . . . ? O3 Zn2 O2 Zn1 47.2(3) . . . . ? N3 Zn2 O2 Zn1 -130.5(3) . . . . ? N4 Zn2 O2 Zn1 -58.4(3) . . . . ? O4 Zn2 O2 Zn1 126.8(2) . . . . ? Zn3 Zn2 O2 Zn1 87.1(2) . . . . ? O1 Zn1 O2 C21 -165.4(5) . . . . ? O5 Zn1 O2 C21 -60.0(5) . . . . ? N1 Zn1 O2 C21 113.1(5) . . . . ? N2 Zn1 O2 C21 48.2(5) . . . . ? O1 Zn1 O2 Zn2 24.3(2) . . . . ? O5 Zn1 O2 Zn2 129.6(3) . . . . ? N1 Zn1 O2 Zn2 -57.2(4) . . . . ? N2 Zn1 O2 Zn2 -122.2(3) . . . . ? C25 C24 C27 C28 127.1(7) . . . . ? C23 C24 C27 C28 -52.5(8) . . . . ? C25 C24 C27 C29 -112.6(7) . . . . ? C23 C24 C27 C29 67.8(8) . . . . ? C25 C24 C27 C30 6.2(9) . . . . ? C23 C24 C27 C30 -173.4(6) . . . . ? O3 Zn2 N3 C31 155.5(6) . . . . ? O2 Zn2 N3 C31 -32.7(5) . . . . ? N4 Zn2 N3 C31 -168.1(5) . . . . ? O4 Zn2 N3 C31 64.1(5) . . . . ? Zn3 Zn2 N3 C31 74.2(5) . . . . ? O3 Zn2 N3 C35 -34.2(9) . . . . ? O2 Zn2 N3 C35 137.6(4) . . . . ? N4 Zn2 N3 C35 2.2(4) . . . . ? O4 Zn2 N3 C35 -125.6(4) . . . . ? Zn3 Zn2 N3 C35 -115.6(4) . . . . ? C35 N3 C31 C32 4.0(9) . . . . ? Zn2 N3 C31 C32 173.7(4) . . . . ? C35 N3 C31 C26 -173.9(5) . . . . ? Zn2 N3 C31 C26 -4.1(8) . . . . ? C25 C26 C31 N3 -150.2(6) . . . . ? C21 C26 C31 N3 33.6(9) . . . . ? C25 C26 C31 C32 32.0(9) . . . . ? C21 C26 C31 C32 -144.2(6) . . . . ? N3 C31 C32 C33 -1.2(9) . . . . ? C26 C31 C32 C33 176.6(6) . . . . ? C31 C32 C33 C34 -0.7(10) . . . . ? C32 C33 C34 C35 -0.1(10) . . . . ? C31 N3 C35 C34 -4.8(9) . . . . ? Zn2 N3 C35 C34 -175.4(5) . . . . ? C31 N3 C35 C36 173.0(5) . . . . ? Zn2 N3 C35 C36 2.4(7) . . . . ? C33 C34 C35 N3 2.8(9) . . . . ? C33 C34 C35 C36 -174.8(6) . . . . ? O3 Zn2 N4 C36 163.9(4) . . . . ? O2 Zn2 N4 C36 -81.5(5) . . . . ? N3 Zn2 N4 C36 -6.9(4) . . . . ? O4 Zn2 N4 C36 91.9(4) . . . . ? Zn3 Zn2 N4 C36 135.9(4) . . . . ? O3 Zn2 N4 C40 -7.9(5) . . . . ? O2 Zn2 N4 C40 106.7(5) . . . . ? N3 Zn2 N4 C40 -178.7(5) . . . . ? O4 Zn2 N4 C40 -79.9(5) . . . . ? Zn3 Zn2 N4 C40 -35.9(5) . . . . ? C40 N4 C36 C37 0.1(9) . . . . ? Zn2 N4 C36 C37 -172.3(5) . . . . ? C40 N4 C36 C35 -177.6(5) . . . . ? Zn2 N4 C36 C35 10.0(6) . . . . ? N3 C35 C36 N4 -8.5(8) . . . . ? C34 C35 C36 N4 169.3(6) . . . . ? N3 C35 C36 C37 173.8(6) . . . . ? C34 C35 C36 C37 -8.4(10) . . . . ? N4 C36 C37 C38 3.5(10) . . . . ? C35 C36 C37 C38 -178.9(6) . . . . ? C36 C37 C38 C39 -3.3(11) . . . . ? C37 C38 C39 C40 -0.4(11) . . . . ? C36 N4 C40 C39 -3.9(9) . . . . ? Zn2 N4 C40 C39 167.4(4) . . . . ? C36 N4 C40 C42 175.2(5) . . . . ? Zn2 N4 C40 C42 -13.5(8) . . . . ? C38 C39 C40 N4 4.0(10) . . . . ? C38 C39 C40 C42 -175.0(6) . . . . ? O3 C41 C42 C43 178.7(6) . . . . ? C46 C41 C42 C43 -1.3(9) . . . . ? O3 C41 C42 C40 -0.5(10) . . . . ? C46 C41 C42 C40 179.5(6) . . . . ? N4 C40 C42 C43 -156.8(6) . . . . ? C39 C40 C42 C43 22.2(9) . . . . ? N4 C40 C42 C41 22.4(9) . . . . ? C39 C40 C42 C41 -158.6(6) . . . . ? C41 C42 C43 C44 2.0(10) . . . . ? C40 C42 C43 C44 -178.7(6) . . . . ? C42 C43 C44 C45 -0.3(10) . . . . ? C42 C43 C44 C47 -176.9(6) . . . . ? C43 C44 C45 C46 -2.3(10) . . . . ? C47 C44 C45 C46 174.4(6) . . . . ? C44 C45 C46 C41 3.0(10) . . . . ? C44 C45 C46 C51 -172.6(6) . . . . ? O3 C41 C46 C45 178.9(6) . . . . ? C42 C41 C46 C45 -1.0(9) . . . . ? O3 C41 C46 C51 -5.7(9) . . . . ? C42 C41 C46 C51 174.3(6) . . . . ? C42 C41 O3 Zn2 -32.3(9) . . . . ? C46 C41 O3 Zn2 147.8(5) . . . . ? C42 C41 O3 Zn3 134.7(5) . . . . ? C46 C41 O3 Zn3 -45.2(8) . . . . ? O2 Zn2 O3 C41 -103.7(6) . . . . ? N3 Zn2 O3 C41 67.7(10) . . . . ? N4 Zn2 O3 C41 31.9(6) . . . . ? O4 Zn2 O3 C41 162.6(6) . . . . ? Zn3 Zn2 O3 C41 168.9(7) . . . . ? O2 Zn2 O3 Zn3 87.5(2) . . . . ? N3 Zn2 O3 Zn3 -101.2(7) . . . . ? N4 Zn2 O3 Zn3 -137.0(2) . . . . ? O4 Zn2 O3 Zn3 -6.29(19) . . . . ? O7 Zn3 O3 C41 -53.6(5) . . . . ? O4 Zn3 O3 C41 -163.2(5) . . . . ? N6 Zn3 O3 C41 121.9(5) . . . . ? N5 Zn3 O3 C41 54.6(5) . . . . ? Zn2 Zn3 O3 C41 -169.8(6) . . . . ? O7 Zn3 O3 Zn2 116.2(2) . . . . ? O4 Zn3 O3 Zn2 6.6(2) . . . . ? N6 Zn3 O3 Zn2 -68.3(3) . . . . ? N5 Zn3 O3 Zn2 -135.6(2) . . . . ? C43 C44 C47 C48 -19.5(15) . . . . ? C45 C44 C47 C48 163.9(13) . . . . ? C43 C44 C47 C49 -142.4(10) . . . . ? C45 C44 C47 C49 41.0(12) . . . . ? C43 C44 C47 C50 103.7(11) . . . . ? C45 C44 C47 C50 -72.9(12) . . . . ? O7 Zn3 N5 C55 -117.2(5) . . . . ? O4 Zn3 N5 C55 81.7(5) . . . . ? O3 Zn3 N5 C55 144.7(5) . . . . ? N6 Zn3 N5 C55 8.4(4) . . . . ? Zn2 Zn3 N5 C55 118.5(4) . . . . ? O7 Zn3 N5 C51 67.1(5) . . . . ? O4 Zn3 N5 C51 -94.1(6) . . . . ? O3 Zn3 N5 C51 -31.1(5) . . . . ? N6 Zn3 N5 C51 -167.3(5) . . . . ? Zn2 Zn3 N5 C51 -57.2(5) . . . . ? C55 N5 C51 C52 2.7(9) . . . . ? Zn3 N5 C51 C52 178.1(5) . . . . ? C55 N5 C51 C46 -174.5(6) . . . . ? Zn3 N5 C51 C46 0.9(8) . . . . ? C45 C46 C51 N5 -157.2(6) . . . . ? C41 C46 C51 N5 27.5(9) . . . . ? C45 C46 C51 C52 25.7(9) . . . . ? C41 C46 C51 C52 -149.6(7) . . . . ? N5 C51 C52 C53 2.0(10) . . . . ? C46 C51 C52 C53 179.2(7) . . . . ? C51 C52 C53 C54 -3.9(11) . . . . ? C52 C53 C54 C55 1.2(11) . . . . ? C51 N5 C55 C54 -5.5(10) . . . . ? Zn3 N5 C55 C54 178.6(5) . . . . ? C51 N5 C55 C56 170.3(6) . . . . ? Zn3 N5 C55 C56 -5.6(7) . . . . ? C53 C54 C55 N5 3.5(10) . . . . ? C53 C54 C55 C56 -172.1(6) . . . . ? O7 Zn3 N6 C56 95.8(5) . . . . ? O4 Zn3 N6 C56 -149.9(5) . . . . ? O3 Zn3 N6 C56 -78.6(5) . . . . ? N5 Zn3 N6 C56 -10.1(4) . . . . ? Zn2 Zn3 N6 C56 -115.5(4) . . . . ? O7 Zn3 N6 C60 -81.8(6) . . . . ? O4 Zn3 N6 C60 32.6(5) . . . . ? O3 Zn3 N6 C60 103.8(5) . . . . ? N5 Zn3 N6 C60 172.3(5) . . . . ? Zn2 Zn3 N6 C60 66.9(5) . . . . ? C60 N6 C56 C57 4.9(10) . . . . ? Zn3 N6 C56 C57 -172.7(5) . . . . ? C60 N6 C56 C55 -172.1(6) . . . . ? Zn3 N6 C56 C55 10.3(7) . . . . ? N5 C55 C56 N6 -3.0(8) . . . . ? C54 C55 C56 N6 172.9(6) . . . . ? N5 C55 C56 C57 -180.0(6) . . . . ? C54 C55 C56 C57 -4.1(10) . . . . ? N6 C56 C57 C58 -3.9(11) . . . . ? C55 C56 C57 C58 172.9(6) . . . . ? C56 C57 C58 C59 -0.4(11) . . . . ? C57 C58 C59 C60 3.7(11) . . . . ? C56 N6 C60 C59 -1.5(10) . . . . ? Zn3 N6 C60 C59 175.9(5) . . . . ? C56 N6 C60 C62 177.8(6) . . . . ? Zn3 N6 C60 C62 -4.8(9) . . . . ? C58 C59 C60 N6 -2.8(10) . . . . ? C58 C59 C60 C62 178.0(6) . . . . ? O4 C61 C62 C63 -177.2(6) . . . . ? C66 C61 C62 C63 2.3(9) . . . . ? O4 C61 C62 C60 6.0(11) . . . . ? C66 C61 C62 C60 -174.5(6) . . . . ? N6 C60 C62 C61 -23.8(10) . . . . ? C59 C60 C62 C61 155.4(7) . . . . ? N6 C60 C62 C63 159.3(6) . . . . ? C59 C60 C62 C63 -21.5(10) . . . . ? C61 C62 C63 C64 -1.9(10) . . . . ? C60 C62 C63 C64 175.3(7) . . . . ? C62 C63 C64 C65 -0.6(11) . . . . ? C62 C63 C64 C67 -179.8(7) . . . . ? C63 C64 C65 C66 2.6(11) . . . . ? C67 C64 C65 C66 -178.3(7) . . . . ? C64 C65 C66 C61 -2.0(11) . . . . ? O4 C61 C66 C65 179.0(6) . . . . ? C62 C61 C66 C65 -0.5(10) . . . . ? C66 C61 O4 Zn3 -141.4(5) . . . . ? C62 C61 O4 Zn3 38.1(8) . . . . ? C66 C61 O4 Zn2 43.2(10) . . . . ? C62 C61 O4 Zn2 -137.3(6) . . . . ? O7 Zn3 O4 C61 80.4(5) . . . . ? O3 Zn3 O4 C61 177.0(5) . . . . ? N6 Zn3 O4 C61 -48.4(5) . . . . ? N5 Zn3 O4 C61 -118.7(5) . . . . ? Zn2 Zn3 O4 C61 -177.1(6) . . . . ? O7 Zn3 O4 Zn2 -102.5(2) . . . . ? O3 Zn3 O4 Zn2 -5.90(18) . . . . ? N6 Zn3 O4 Zn2 128.8(2) . . . . ? N5 Zn3 O4 Zn2 58.4(3) . . . . ? O3 Zn2 O4 C61 -177.9(7) . . . . ? O2 Zn2 O4 C61 73.7(7) . . . . ? N3 Zn2 O4 C61 -13.9(7) . . . . ? N4 Zn2 O4 C61 -101.4(7) . . . . ? Zn3 Zn2 O4 C61 175.9(8) . . . . ? O3 Zn2 O4 Zn3 6.18(19) . . . . ? O2 Zn2 O4 Zn3 -102.17(19) . . . . ? N3 Zn2 O4 Zn3 170.22(19) . . . . ? N4 Zn2 O4 Zn3 82.7(3) . . . . ? C63 C64 C67 C69 117.5(14) . . . . ? C65 C64 C67 C69 -61.7(15) . . . . ? C63 C64 C67 C71 -72.7(12) . . . . ? C65 C64 C67 C71 108.1(11) . . . . ? C63 C64 C67 C73 52.5(15) . . . . ? C65 C64 C67 C73 -126.7(14) . . . . ? C63 C64 C67 C70 -6(2) . . . . ? C65 C64 C67 C70 174.9(18) . . . . ? C63 C64 C67 C68 -123.2(11) . . . . ? C65 C64 C67 C68 57.6(13) . . . . ? C63 C64 C67 C72 166.6(15) . . . . ? C65 C64 C67 C72 -12.5(17) . . . . ? O1 Zn1 O5 C74 146.2(6) . . . . ? O2 Zn1 O5 C74 53.0(7) . . . . ? N1 Zn1 O5 C74 -122.5(6) . . . . ? N2 Zn1 O5 C74 -40.2(7) . . . . ? Zn1 O5 C74 O6 -19.5(13) . . . . ? Zn1 O5 C74 C75 166.4(8) . . . . ? O4 Zn3 O7 C76 -93.4(6) . . . . ? O3 Zn3 O7 C76 -174.7(5) . . . . ? N6 Zn3 O7 C76 9.4(7) . . . . ? N5 Zn3 O7 C76 100.1(6) . . . . ? Zn2 Zn3 O7 C76 -138.9(5) . . . . ? Zn3 O7 C76 O8 -3.2(11) . . . . ? Zn3 O7 C76 C77 173.5(5) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 2.543 _refine_diff_density_min -1.309 _refine_diff_density_rms 0.129 _database_code_depnum_ccdc_archive 'CCDC 938302' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_L2Co3 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common '[LCo3(OAc)3(OMe)](MeOH)1.25(Et2O)0.5(H2O)' _chemical_melting_point ? _chemical_formula_moiety C80.25H88Co3N6O13.75 _chemical_formula_sum 'C80.25 H88 Co3 N6 O13.75' _chemical_formula_weight 1533.36 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 15.1439(16) _cell_length_b 15.7323(15) _cell_length_c 17.9697(18) _cell_angle_alpha 76.059(7) _cell_angle_beta 67.877(7) _cell_angle_gamma 66.888(7) _cell_volume 3625.9(6) _cell_formula_units_Z 2 _cell_measurement_temperature 120 _cell_measurement_reflns_used 19937 _cell_measurement_theta_min 1.64 _cell_measurement_theta_max 25.00 _exptl_crystal_description prismatic _exptl_crystal_colour red _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.404 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1605 _exptl_absorpt_coefficient_mu 0.749 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.8960 _exptl_absorpt_correction_T_max 0.9779 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus rotating anode' _diffrn_radiation_monochromator 'multilayer confocal mirror' _diffrn_measurement_device_type 'Bruker APEXII CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 8.333 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 19937 _diffrn_reflns_av_R_equivalents 0.1365 _diffrn_reflns_av_sigmaI/netI 0.3554 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.64 _diffrn_reflns_theta_max 25.00 _reflns_number_total 12623 _reflns_number_gt 4819 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker AXS, 2009)' _computing_cell_refinement 'APEX2 (Bruker AXS, 2009)' _computing_data_reduction 'APEX2 (Bruker AXS, 2009)' _computing_structure_solution 'DIRDIF99 (Beurskens et al., 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ORTEP-3 _computing_publication_material ORTEP-3 _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^)+(0.0694P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 12623 _refine_ls_number_parameters 992 _refine_ls_number_restraints 168 _refine_ls_R_factor_all 0.2532 _refine_ls_R_factor_gt 0.0875 _refine_ls_wR_factor_ref 0.2206 _refine_ls_wR_factor_gt 0.1676 _refine_ls_goodness_of_fit_ref 1.003 _refine_ls_restrained_S_all 1.002 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.80653(10) 0.26240(9) 0.22984(9) 0.0304(4) Uani 1 1 d . . . Co2 Co 0.56985(9) 0.21277(8) 0.32410(8) 0.0266(4) Uani 1 1 d . A . Co3 Co 0.35313(10) 0.31123(8) 0.34584(8) 0.0285(4) Uani 1 1 d . A . C1 C 0.9004(7) 0.1054(7) 0.3198(6) 0.029(3) Uani 1 1 d . . . C2 C 0.9811(7) 0.1363(6) 0.3082(6) 0.028(2) Uani 1 1 d . . . C3 C 1.0661(7) 0.0714(6) 0.3317(6) 0.033(3) Uani 1 1 d . . . H1 H 1.1193 0.0925 0.3259 0.040 Uiso 1 1 calc R . . C4 C 1.0755(8) -0.0191(7) 0.3619(6) 0.041(3) Uani 1 1 d . . . C5 C 0.9932(8) -0.0454(7) 0.3720(6) 0.038(3) Uani 1 1 d . . . H2 H 0.9971 -0.1080 0.3920 0.046 Uiso 1 1 calc R . . C6 C 0.9088(8) 0.0130(7) 0.3552(6) 0.041(3) Uani 1 1 d . . . H3 H 0.8537 -0.0082 0.3672 0.049 Uiso 1 1 calc R . . O1 O 0.8151(5) 0.1591(4) 0.3056(4) 0.0372(18) Uani 1 1 d . . . C7 C 1.1678(8) -0.0885(7) 0.3843(7) 0.041(3) Uani 1 1 d . . . C8 C 1.2417(9) -0.0446(7) 0.3805(8) 0.068(4) Uani 1 1 d . . . H4 H 1.2992 -0.0923 0.3955 0.102 Uiso 1 1 calc R . . H5 H 1.2081 0.0030 0.4180 0.102 Uiso 1 1 calc R . . H6 H 1.2659 -0.0158 0.3254 0.102 Uiso 1 1 calc R . . C9 C 1.2196(9) -0.1666(9) 0.3299(8) 0.077(4) Uani 1 1 d . . . H7 H 1.1706 -0.1950 0.3337 0.115 Uiso 1 1 calc R . . H8 H 1.2757 -0.2138 0.3471 0.115 Uiso 1 1 calc R . . H9 H 1.2457 -0.1413 0.2738 0.115 Uiso 1 1 calc R . . C10 C 1.1352(9) -0.1367(8) 0.4715(8) 0.066(4) Uani 1 1 d . . . H10 H 1.0873 -0.1665 0.4758 0.098 Uiso 1 1 calc R . . H11 H 1.1029 -0.0902 0.5100 0.098 Uiso 1 1 calc R . . H12 H 1.1950 -0.1838 0.4838 0.098 Uiso 1 1 calc R . . N1 N 0.9177(6) 0.2859(5) 0.2357(5) 0.031(2) Uani 1 1 d . . . C11 C 0.9776(8) 0.2309(7) 0.2814(7) 0.038(3) Uani 1 1 d . . . C12 C 1.0405(8) 0.2706(7) 0.2937(6) 0.045(3) Uani 1 1 d . . . H13 H 1.0868 0.2336 0.3224 0.054 Uiso 1 1 calc R . . C13 C 1.0356(8) 0.3615(7) 0.2648(7) 0.045(3) Uani 1 1 d . . . H14 H 1.0732 0.3885 0.2780 0.054 Uiso 1 1 calc R . . C14 C 0.9763(8) 0.4123(7) 0.2170(7) 0.043(3) Uani 1 1 d . . . H15 H 0.9755 0.4734 0.1934 0.052 Uiso 1 1 calc R . . C15 C 0.9178(7) 0.3722(6) 0.2043(6) 0.028(3) Uani 1 1 d . . . N2 N 0.7934(5) 0.3703(5) 0.1545(5) 0.030(2) Uani 1 1 d . . . C16 C 0.8525(7) 0.4184(6) 0.1532(6) 0.034(3) Uani 1 1 d . . . C17 C 0.8501(7) 0.5034(6) 0.1048(6) 0.034(3) Uani 1 1 d . . . H16 H 0.8912 0.5364 0.1041 0.041 Uiso 1 1 calc R . . C18 C 0.7871(8) 0.5369(7) 0.0590(6) 0.042(3) Uani 1 1 d . . . H17 H 0.7831 0.5948 0.0264 0.051 Uiso 1 1 calc R . . C19 C 0.7292(7) 0.4878(6) 0.0596(6) 0.034(3) Uani 1 1 d . . . H18 H 0.6837 0.5133 0.0289 0.041 Uiso 1 1 calc R . . C20 C 0.7360(7) 0.4021(6) 0.1042(6) 0.034(3) Uani 1 1 d U . . C21 C 0.6784(7) 0.2621(6) 0.1532(7) 0.032(3) Uani 1 1 d . . . C22 C 0.6873(7) 0.3405(6) 0.0965(6) 0.030(2) Uani 1 1 d U . . C23 C 0.6590(7) 0.3543(6) 0.0285(6) 0.033(2) Uani 1 1 d U . . H19 H 0.6661 0.4065 -0.0099 0.040 Uiso 1 1 calc R . . C24 C 0.6206(7) 0.2945(7) 0.0140(6) 0.032(3) Uani 1 1 d . . . C25 C 0.6232(7) 0.2124(6) 0.0645(6) 0.033(3) Uani 1 1 d . . . H20 H 0.6060 0.1669 0.0517 0.040 Uiso 1 1 calc R . . C26 C 0.6506(7) 0.1958(6) 0.1336(6) 0.033(3) Uani 1 1 d . . . O2 O 0.6889(4) 0.2514(4) 0.2253(4) 0.0269(16) Uani 1 1 d . . . C27 C 0.5818(8) 0.3165(7) -0.0604(6) 0.038(3) Uani 1 1 d . . . C28 C 0.4866(9) 0.2901(8) -0.0334(7) 0.072(4) Uani 1 1 d . . . H21 H 0.5025 0.2240 -0.0128 0.108 Uiso 1 1 calc R . . H22 H 0.4621 0.3018 -0.0794 0.108 Uiso 1 1 calc R . . H23 H 0.4342 0.3275 0.0094 0.108 Uiso 1 1 calc R . . C29 C 0.5540(9) 0.4166(8) -0.0919(7) 0.065(4) Uani 1 1 d . . . H24 H 0.5006 0.4534 -0.0490 0.098 Uiso 1 1 calc R . . H25 H 0.5294 0.4264 -0.1376 0.098 Uiso 1 1 calc R . . H26 H 0.6135 0.4360 -0.1098 0.098 Uiso 1 1 calc R . . C30 C 0.6637(10) 0.2602(10) -0.1262(8) 0.092(5) Uani 1 1 d . . . H27 H 0.6816 0.1941 -0.1057 0.138 Uiso 1 1 calc R . . H28 H 0.7235 0.2792 -0.1436 0.138 Uiso 1 1 calc R . . H29 H 0.6395 0.2706 -0.1722 0.138 Uiso 1 1 calc R . . N3 N 0.6461(6) 0.0955(5) 0.2611(5) 0.030(2) Uani 1 1 d . . . C31 C 0.6690(7) 0.1023(6) 0.1793(6) 0.028(2) Uani 1 1 d U . . C32 C 0.7117(7) 0.0243(6) 0.1410(6) 0.035(3) Uani 1 1 d . . . H30 H 0.7280 0.0299 0.0840 0.042 Uiso 1 1 calc R . . C33 C 0.7318(8) -0.0626(7) 0.1835(7) 0.047(3) Uani 1 1 d . . . H31 H 0.7591 -0.1170 0.1569 0.057 Uiso 1 1 calc R . . C34 C 0.7111(8) -0.0686(7) 0.2665(7) 0.046(3) Uani 1 1 d . . . H32 H 0.7263 -0.1275 0.2975 0.055 Uiso 1 1 calc R . . C35 C 0.6684(7) 0.0118(6) 0.3032(6) 0.028(2) Uani 1 1 d U . . N4 N 0.5882(5) 0.0970(5) 0.4177(5) 0.028(2) Uani 1 1 d U . . C36 C 0.6442(6) 0.0132(6) 0.3901(6) 0.025(2) Uani 1 1 d U . . C37 C 0.6686(7) -0.0654(6) 0.4445(7) 0.032(3) Uani 1 1 d . . . H33 H 0.7085 -0.1242 0.4249 0.039 Uiso 1 1 calc R . . C38 C 0.6359(7) -0.0586(6) 0.5255(6) 0.034(3) Uani 1 1 d . . . H34 H 0.6551 -0.1113 0.5624 0.041 Uiso 1 1 calc R . . C39 C 0.5752(7) 0.0254(6) 0.5517(6) 0.032(3) Uani 1 1 d . . . H35 H 0.5480 0.0305 0.6081 0.038 Uiso 1 1 calc R . . C40 C 0.5517(7) 0.1047(6) 0.4979(6) 0.028(3) Uani 1 1 d . . . C41 C 0.4182(7) 0.2626(6) 0.4846(6) 0.030(3) Uani 1 1 d . A . C42 C 0.4824(7) 0.1946(6) 0.5281(6) 0.033(3) Uani 1 1 d . . . C43 C 0.4769(7) 0.2113(7) 0.6033(6) 0.036(3) Uani 1 1 d . A . H36 H 0.5195 0.1656 0.6317 0.043 Uiso 1 1 calc R . . C44 C 0.4104(8) 0.2932(7) 0.6376(7) 0.043(3) Uani 1 1 d U . . C45 C 0.3520(8) 0.3557(7) 0.5956(7) 0.042(3) Uani 1 1 d . A . H37 H 0.3061 0.4111 0.6192 0.051 Uiso 1 1 calc R . . C46 C 0.3522(7) 0.3469(6) 0.5185(6) 0.031(3) Uani 1 1 d . . . O3 O 0.4246(4) 0.2423(4) 0.4154(4) 0.0286(17) Uani 1 1 d . . . C47 C 0.3942(15) 0.3023(13) 0.7268(13) 0.049(3) Uani 0.734(15) 1 d PU A 1 C48 C 0.4659(17) 0.2136(13) 0.7669(13) 0.066(5) Uani 0.734(15) 1 d PU A 1 H38 H 0.4462 0.1594 0.7730 0.098 Uiso 0.734(15) 1 calc PR A 1 H39 H 0.4591 0.2259 0.8201 0.098 Uiso 0.734(15) 1 calc PR A 1 H40 H 0.5364 0.2014 0.7322 0.098 Uiso 0.734(15) 1 calc PR A 1 C49 C 0.2877(12) 0.3124(11) 0.7813(10) 0.063(5) Uani 0.734(15) 1 d PU A 1 H41 H 0.2729 0.2564 0.7836 0.094 Uiso 0.734(15) 1 calc PR A 1 H42 H 0.2401 0.3666 0.7600 0.094 Uiso 0.734(15) 1 calc PR A 1 H43 H 0.2809 0.3209 0.8357 0.094 Uiso 0.734(15) 1 calc PR A 1 C50 C 0.4227(17) 0.3849(12) 0.7231(10) 0.063(6) Uani 0.734(15) 1 d PU A 1 H44 H 0.3829 0.4394 0.6955 0.095 Uiso 0.734(15) 1 calc PR A 1 H45 H 0.4949 0.3721 0.6934 0.095 Uiso 0.734(15) 1 calc PR A 1 H46 H 0.4088 0.3970 0.7781 0.095 Uiso 0.734(15) 1 calc PR A 1 C51 C 0.423(3) 0.323(3) 0.710(3) 0.035(5) Uani 0.266(15) 1 d PU A 2 C52 C 0.421(4) 0.243(4) 0.767(4) 0.055(10) Uani 0.266(15) 1 d PU A 2 H47 H 0.3572 0.2318 0.7786 0.082 Uiso 0.266(15) 1 calc PR A 2 H48 H 0.4252 0.2521 0.8176 0.082 Uiso 0.266(15) 1 calc PR A 2 H49 H 0.4779 0.1885 0.7448 0.082 Uiso 0.266(15) 1 calc PR A 2 C53 C 0.517(4) 0.349(3) 0.689(3) 0.054(12) Uani 0.266(15) 1 d PU A 2 H50 H 0.5117 0.4057 0.6502 0.081 Uiso 0.266(15) 1 calc PR A 2 H51 H 0.5769 0.2984 0.6639 0.081 Uiso 0.266(15) 1 calc PR A 2 H52 H 0.5229 0.3607 0.7375 0.081 Uiso 0.266(15) 1 calc PR A 2 C54 C 0.337(4) 0.413(3) 0.735(3) 0.054(11) Uani 0.266(15) 1 d PU A 2 H53 H 0.3479 0.4644 0.6934 0.081 Uiso 0.266(15) 1 calc PR A 2 H54 H 0.3357 0.4264 0.7865 0.081 Uiso 0.266(15) 1 calc PR A 2 H55 H 0.2729 0.4065 0.7422 0.081 Uiso 0.266(15) 1 calc PR A 2 N5 N 0.2916(6) 0.4172(5) 0.4021(5) 0.036(2) Uani 1 1 d . . . C55 C 0.2927(7) 0.4250(6) 0.4749(6) 0.033(3) Uani 1 1 d . A . C56 C 0.2381(8) 0.5106(7) 0.5055(8) 0.054(4) Uani 1 1 d . . . H56 H 0.2359 0.5171 0.5574 0.065 Uiso 1 1 calc R A . C57 C 0.1879(10) 0.5849(8) 0.4629(8) 0.067(4) Uani 1 1 d . A . H57 H 0.1520 0.6424 0.4855 0.080 Uiso 1 1 calc R . . C58 C 0.1877(8) 0.5792(6) 0.3874(7) 0.052(3) Uani 1 1 d . . . H58 H 0.1531 0.6310 0.3570 0.063 Uiso 1 1 calc R A . C59 C 0.2414(8) 0.4931(6) 0.3589(6) 0.037(3) Uani 1 1 d . A . N6 N 0.2892(6) 0.3826(5) 0.2693(5) 0.030(2) Uani 1 1 d . . . C60 C 0.2412(7) 0.4730(7) 0.2826(7) 0.039(3) Uani 1 1 d . A . C61 C 0.1954(7) 0.5387(6) 0.2302(7) 0.037(3) Uani 1 1 d . . . H59 H 0.1610 0.6016 0.2412 0.045 Uiso 1 1 calc R A . C62 C 0.2015(8) 0.5095(7) 0.1604(7) 0.045(3) Uani 1 1 d . A . H60 H 0.1731 0.5534 0.1218 0.054 Uiso 1 1 calc R . . C63 C 0.2485(8) 0.4174(7) 0.1475(7) 0.041(3) Uani 1 1 d . . . H61 H 0.2543 0.3981 0.0991 0.049 Uiso 1 1 calc R A . C64 C 0.2877(7) 0.3522(6) 0.2046(6) 0.032(3) Uani 1 1 d . A . C65 C 0.3944(7) 0.1850(6) 0.2386(6) 0.030(3) Uani 1 1 d . A . C66 C 0.3278(7) 0.2528(6) 0.1976(6) 0.030(3) Uani 1 1 d . . . C67 C 0.2988(7) 0.2205(7) 0.1460(6) 0.036(3) Uani 1 1 d . A . H62 H 0.2530 0.2649 0.1197 0.043 Uiso 1 1 calc R . . C68 C 0.3323(8) 0.1298(7) 0.1317(6) 0.036(3) Uani 1 1 d . . . C69 C 0.4025(8) 0.0662(7) 0.1688(6) 0.039(3) Uani 1 1 d . A . H63 H 0.4303 0.0031 0.1581 0.046 Uiso 1 1 calc R . . C70 C 0.4321(7) 0.0929(6) 0.2201(6) 0.032(3) Uani 1 1 d . . . H64 H 0.4799 0.0475 0.2441 0.039 Uiso 1 1 calc R A . O4 O 0.4213(4) 0.2039(4) 0.2931(4) 0.0292(17) Uani 1 1 d . . . C71 C 0.2964(9) 0.0988(7) 0.0747(7) 0.048(3) Uani 1 1 d U A . C72 C 0.327(2) -0.0082(14) 0.0808(15) 0.071(8) Uani 0.58(2) 1 d PU A 1 H65 H 0.3009 -0.0326 0.1372 0.106 Uiso 0.58(2) 1 calc PR A 1 H66 H 0.4010 -0.0356 0.0618 0.106 Uiso 0.58(2) 1 calc PR A 1 H67 H 0.2986 -0.0239 0.0473 0.106 Uiso 0.58(2) 1 calc PR A 1 C73 C 0.1811(17) 0.134(2) 0.1060(17) 0.092(9) Uani 0.58(2) 1 d PU A 1 H68 H 0.1580 0.1064 0.1618 0.137 Uiso 0.58(2) 1 calc PR A 1 H69 H 0.1549 0.1161 0.0720 0.137 Uiso 0.58(2) 1 calc PR A 1 H70 H 0.1562 0.2018 0.1044 0.137 Uiso 0.58(2) 1 calc PR A 1 C74 C 0.332(2) 0.1385(16) -0.0082(12) 0.060(8) Uani 0.58(2) 1 d PU A 1 H71 H 0.3132 0.2059 -0.0098 0.091 Uiso 0.58(2) 1 calc PR A 1 H72 H 0.3008 0.1257 -0.0413 0.091 Uiso 0.58(2) 1 calc PR A 1 H73 H 0.4057 0.1108 -0.0295 0.091 Uiso 0.58(2) 1 calc PR A 1 C75 C 0.237(3) 0.041(3) 0.120(2) 0.083(10) Uani 0.42(2) 1 d PU A 2 H74 H 0.1778 0.0758 0.1620 0.124 Uiso 0.42(2) 1 calc PR A 2 H75 H 0.2773 -0.0146 0.1460 0.124 Uiso 0.42(2) 1 calc PR A 2 H76 H 0.2134 0.0233 0.0843 0.124 Uiso 0.42(2) 1 calc PR A 2 C76 C 0.234(3) 0.188(2) 0.025(2) 0.076(11) Uani 0.42(2) 1 d PU A 2 H77 H 0.2779 0.2236 -0.0093 0.114 Uiso 0.42(2) 1 calc PR A 2 H78 H 0.1750 0.2271 0.0630 0.114 Uiso 0.42(2) 1 calc PR A 2 H79 H 0.2113 0.1658 -0.0091 0.114 Uiso 0.42(2) 1 calc PR A 2 C77 C 0.390(2) 0.046(2) 0.010(2) 0.074(10) Uani 0.42(2) 1 d PU A 2 H80 H 0.4317 0.0860 -0.0186 0.112 Uiso 0.42(2) 1 calc PR A 2 H81 H 0.3689 0.0303 -0.0284 0.112 Uiso 0.42(2) 1 calc PR A 2 H82 H 0.4294 -0.0105 0.0358 0.112 Uiso 0.42(2) 1 calc PR A 2 O5 O 0.8822(5) 0.1798(4) 0.1500(5) 0.039(2) Uani 1 1 d . . . O6 O 0.9770(6) 0.2594(5) 0.0572(5) 0.068(3) Uani 1 1 d . . . C78 C 0.9451(10) 0.1926(8) 0.0830(10) 0.066(4) Uani 1 1 d . . . C79 C 0.9786(12) 0.1180(10) 0.0261(10) 0.122(7) Uani 1 1 d . . . H83 H 0.9474 0.0703 0.0547 0.182 Uiso 1 1 calc R . . H84 H 1.0524 0.0893 0.0094 0.182 Uiso 1 1 calc R . . H85 H 0.9570 0.1473 -0.0217 0.182 Uiso 1 1 calc R . . O7 O 0.7288(5) 0.3429(4) 0.3146(4) 0.0323(18) Uani 1 1 d . . . O8 O 0.6119(4) 0.2729(4) 0.3878(4) 0.0280(17) Uani 1 1 d . . . C80 C 0.6565(8) 0.3286(7) 0.3768(7) 0.036(3) Uani 1 1 d . A . C81 C 0.6252(8) 0.3852(7) 0.4453(6) 0.047(3) Uani 1 1 d . . . H86 H 0.6653 0.4264 0.4295 0.071 Uiso 1 1 calc R A . H87 H 0.6367 0.3433 0.4934 0.071 Uiso 1 1 calc R . . H88 H 0.5532 0.4225 0.4574 0.071 Uiso 1 1 calc R . . O9 O 0.2463(5) 0.2622(4) 0.4070(4) 0.041(2) Uani 1 1 d . . . O10 O 0.1077(6) 0.3791(5) 0.4146(5) 0.068(2) Uani 1 1 d . . . C82 C 0.1565(10) 0.2943(7) 0.4353(8) 0.051(3) Uani 1 1 d . A . C83 C 0.0947(8) 0.2364(7) 0.4866(7) 0.049(3) Uani 1 1 d . . . H89 H 0.0232 0.2753 0.5029 0.074 Uiso 1 1 calc R A . H90 H 0.1156 0.2077 0.5348 0.074 Uiso 1 1 calc R . . H91 H 0.1042 0.1878 0.4562 0.074 Uiso 1 1 calc R . . O11 O 0.4741(4) 0.3374(4) 0.2843(4) 0.0324(17) Uani 1 1 d . . . C84 C 0.4850(7) 0.4240(6) 0.2810(6) 0.035(3) Uani 1 1 d . A . H92 H 0.5528 0.4230 0.2456 0.052 Uiso 1 1 calc R . . H93 H 0.4755 0.4346 0.3355 0.052 Uiso 1 1 calc R . . H94 H 0.4341 0.4740 0.2597 0.052 Uiso 1 1 calc R . . O12 O 1.0021(14) 0.3741(13) -0.0834(13) 0.105(6) Uiso 0.68(2) 1 d PD B 1 H95 H 0.9893 0.3500 -0.0352 0.157 Uiso 0.68(2) 1 calc PR B 1 C85 C 1.0388(18) 0.3108(15) -0.1305(15) 0.105(6) Uiso 0.68(2) 1 d PD B 1 H96 H 0.9873 0.2837 -0.1229 0.157 Uiso 0.68(2) 1 calc PR B 1 H97 H 1.0975 0.2621 -0.1181 0.157 Uiso 0.68(2) 1 calc PR B 1 H98 H 1.0596 0.3379 -0.1867 0.157 Uiso 0.68(2) 1 calc PR B 1 O13 O 1.099(2) 0.2955(18) -0.0951(19) 0.084(12) Uiso 0.32(2) 1 d PD B 2 H99 H 1.0870 0.2677 -0.0481 0.126 Uiso 0.32(2) 1 calc PR B 2 C86 C 1.009(4) 0.362(4) -0.105(4) 0.084(12) Uiso 0.32(2) 1 d PD B 2 H100 H 0.9775 0.4036 -0.0623 0.126 Uiso 0.32(2) 1 calc PR B 2 H101 H 0.9622 0.3307 -0.1008 0.126 Uiso 0.32(2) 1 calc PR B 2 H102 H 1.0232 0.3981 -0.1578 0.126 Uiso 0.32(2) 1 calc PR B 2 O14 O -0.057(2) 0.981(2) 0.170(2) 0.074(8) Uiso 0.25 1 d PD C 1 H103 H -0.0745 0.9676 0.1358 0.110 Uiso 0.25 1 calc PR C 1 C87 C 0.051(3) 0.944(3) 0.150(3) 0.074(8) Uiso 0.25 1 d PD C 1 H104 H 0.0725 0.9767 0.1761 0.110 Uiso 0.25 1 calc PR C 1 H105 H 0.0815 0.9534 0.0911 0.110 Uiso 0.25 1 calc PR C 1 H106 H 0.0718 0.8776 0.1685 0.110 Uiso 0.25 1 calc PR C 1 C88 C 0.0487(18) 0.8405(16) 0.1938(15) 0.086(3) Uiso 0.50 1 d PD D 2 H107 H 0.0230 0.9016 0.1650 0.129 Uiso 0.50 1 calc PR D 2 H108 H 0.0983 0.7969 0.1546 0.129 Uiso 0.50 1 calc PR D 2 H109 H 0.0810 0.8461 0.2296 0.129 Uiso 0.50 1 calc PR D 2 C89 C -0.0363(17) 0.8058(14) 0.2423(14) 0.086(3) Uiso 0.50 1 d PD D 2 H110 H -0.0890 0.8544 0.2767 0.103 Uiso 0.50 1 calc PR D 2 H111 H -0.0660 0.7986 0.2046 0.103 Uiso 0.50 1 calc PR D 2 O15 O -0.0151(13) 0.7217(10) 0.2924(10) 0.086(3) Uiso 0.50 1 d PD D 2 C90 C -0.0951(16) 0.6861(14) 0.3331(15) 0.086(3) Uiso 0.50 1 d PD D 2 H112 H -0.1314 0.6926 0.2952 0.103 Uiso 0.50 1 calc PR D 2 H113 H -0.1435 0.7237 0.3779 0.103 Uiso 0.50 1 calc PR D 2 C91 C -0.0616(19) 0.5884(13) 0.3658(16) 0.086(3) Uiso 0.50 1 d PD D 2 H114 H -0.1204 0.5678 0.3934 0.129 Uiso 0.50 1 calc PR D 2 H115 H -0.0268 0.5815 0.4043 0.129 Uiso 0.50 1 calc PR D 2 H116 H -0.0150 0.5505 0.3216 0.129 Uiso 0.50 1 calc PR D 2 O16 O -0.0237(18) 0.5534(15) 0.4333(15) 0.124(7) Uiso 0.50 1 d P E 1 O17 O 0.053(2) 0.760(2) 0.268(2) 0.181(11) Uiso 0.50 1 d P F 1 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0332(9) 0.0359(7) 0.0323(10) -0.0014(6) -0.0123(7) -0.0213(6) Co2 0.0342(9) 0.0282(7) 0.0249(10) -0.0044(6) -0.0094(7) -0.0170(6) Co3 0.0332(9) 0.0300(7) 0.0314(10) -0.0035(6) -0.0132(7) -0.0171(6) C1 0.030(7) 0.047(6) 0.017(7) -0.008(5) -0.005(5) -0.021(5) C2 0.037(7) 0.029(5) 0.017(7) 0.007(5) -0.004(5) -0.019(5) C3 0.041(7) 0.034(5) 0.031(8) -0.006(5) -0.010(6) -0.019(5) C4 0.041(7) 0.045(6) 0.046(9) -0.004(6) -0.020(6) -0.019(6) C5 0.035(7) 0.036(5) 0.045(9) 0.001(5) -0.021(6) -0.010(5) C6 0.050(8) 0.042(6) 0.044(9) 0.005(6) -0.020(6) -0.032(6) O1 0.034(5) 0.040(4) 0.048(6) 0.004(4) -0.015(4) -0.027(3) C7 0.038(7) 0.038(6) 0.044(10) 0.000(6) -0.014(6) -0.011(5) C8 0.053(9) 0.062(7) 0.104(12) 0.019(7) -0.053(8) -0.024(7) C9 0.044(9) 0.092(9) 0.076(12) -0.032(9) -0.002(8) -0.007(7) C10 0.046(9) 0.075(8) 0.072(12) -0.005(8) -0.022(8) -0.015(7) N1 0.032(5) 0.041(5) 0.028(6) -0.002(4) -0.006(5) -0.024(4) C11 0.031(7) 0.043(6) 0.039(9) -0.005(5) -0.008(6) -0.014(5) C12 0.047(8) 0.066(7) 0.040(9) -0.003(6) -0.019(6) -0.034(6) C13 0.053(8) 0.044(6) 0.057(9) 0.012(6) -0.028(7) -0.036(6) C14 0.038(7) 0.038(6) 0.065(10) 0.007(6) -0.027(7) -0.021(5) C15 0.034(6) 0.036(5) 0.019(7) -0.002(5) -0.003(5) -0.021(5) N2 0.029(5) 0.034(4) 0.031(6) -0.011(4) -0.004(4) -0.017(4) C16 0.043(7) 0.031(5) 0.034(8) -0.011(5) -0.011(6) -0.015(5) C17 0.051(7) 0.040(6) 0.032(8) 0.006(5) -0.021(6) -0.035(5) C18 0.065(8) 0.057(6) 0.022(8) -0.001(5) -0.014(6) -0.040(6) C19 0.047(7) 0.039(6) 0.024(8) 0.011(5) -0.018(6) -0.024(5) C20 0.044(5) 0.036(4) 0.031(5) -0.011(4) -0.011(4) -0.018(4) C21 0.022(6) 0.039(6) 0.041(8) -0.011(6) -0.005(5) -0.016(5) C22 0.037(5) 0.040(4) 0.025(5) -0.009(4) -0.013(4) -0.019(4) C23 0.033(5) 0.033(4) 0.033(5) 0.001(4) -0.003(4) -0.020(4) C24 0.037(7) 0.050(6) 0.017(7) -0.007(5) -0.007(5) -0.022(5) C25 0.053(7) 0.037(6) 0.026(8) -0.007(5) -0.018(6) -0.025(5) C26 0.026(6) 0.037(6) 0.039(8) -0.018(5) -0.001(5) -0.014(5) O2 0.032(4) 0.042(4) 0.019(5) -0.008(3) -0.009(3) -0.020(3) C27 0.058(8) 0.049(6) 0.015(7) 0.002(5) -0.019(6) -0.022(6) C28 0.090(11) 0.106(10) 0.063(11) 0.019(8) -0.049(9) -0.069(9) C29 0.078(10) 0.086(9) 0.062(11) 0.006(7) -0.049(8) -0.041(8) C30 0.092(12) 0.138(12) 0.042(11) -0.040(9) -0.044(9) 0.004(10) N3 0.037(5) 0.033(4) 0.030(7) -0.003(4) -0.012(4) -0.022(4) C31 0.028(5) 0.034(4) 0.033(5) -0.007(4) -0.014(4) -0.015(3) C32 0.046(7) 0.041(6) 0.027(8) -0.007(5) -0.011(6) -0.020(5) C33 0.057(8) 0.036(6) 0.059(10) -0.025(6) -0.020(7) -0.013(6) C34 0.067(8) 0.037(6) 0.051(10) -0.017(6) -0.024(7) -0.023(6) C35 0.034(5) 0.027(4) 0.034(5) -0.008(4) -0.012(4) -0.018(3) N4 0.031(4) 0.028(3) 0.036(5) -0.008(3) -0.010(3) -0.017(3) C36 0.022(4) 0.027(4) 0.035(5) -0.003(4) -0.008(4) -0.018(3) C37 0.028(6) 0.018(5) 0.061(10) -0.001(5) -0.021(6) -0.013(4) C38 0.054(7) 0.037(6) 0.028(8) 0.001(5) -0.026(6) -0.023(6) C39 0.030(6) 0.038(6) 0.038(8) -0.004(6) -0.009(5) -0.023(5) C40 0.032(6) 0.031(5) 0.031(8) -0.007(5) -0.013(6) -0.016(5) C41 0.031(6) 0.032(5) 0.035(8) -0.001(5) -0.013(6) -0.018(5) C42 0.028(6) 0.041(6) 0.032(8) -0.010(5) 0.007(5) -0.026(5) C43 0.043(7) 0.046(6) 0.027(8) 0.000(5) -0.014(6) -0.022(5) C44 0.039(7) 0.056(6) 0.041(5) -0.022(5) -0.016(5) -0.011(6) C45 0.040(7) 0.038(6) 0.056(9) -0.026(6) -0.017(6) -0.005(5) C46 0.035(7) 0.028(5) 0.042(8) -0.001(5) -0.020(6) -0.016(5) O3 0.033(4) 0.034(3) 0.031(5) -0.008(3) -0.017(3) -0.014(3) C47 0.060(6) 0.060(6) 0.044(5) -0.020(5) -0.025(4) -0.020(4) C48 0.089(11) 0.068(8) 0.053(11) -0.010(7) -0.040(11) -0.021(8) C49 0.074(7) 0.073(10) 0.040(8) -0.019(9) -0.007(6) -0.026(7) C50 0.113(17) 0.074(8) 0.036(12) -0.001(8) -0.040(11) -0.052(12) C51 0.042(8) 0.037(8) 0.029(7) -0.010(5) -0.013(6) -0.012(5) C52 0.04(3) 0.060(16) 0.052(17) 0.017(17) -0.02(2) -0.012(16) C53 0.061(15) 0.08(3) 0.04(3) -0.027(19) -0.008(17) -0.038(17) C54 0.067(17) 0.058(15) 0.02(3) -0.017(14) -0.03(2) 0.014(14) N5 0.037(6) 0.029(4) 0.054(7) -0.005(5) -0.012(5) -0.024(4) C55 0.029(6) 0.028(5) 0.052(9) -0.013(5) -0.012(6) -0.013(5) C56 0.062(9) 0.036(6) 0.083(11) -0.019(7) -0.035(8) -0.017(6) C57 0.091(11) 0.043(7) 0.082(12) -0.031(7) -0.044(9) -0.008(7) C58 0.066(9) 0.025(5) 0.084(11) -0.010(6) -0.042(7) -0.013(6) C59 0.054(8) 0.032(5) 0.042(8) 0.002(5) -0.024(6) -0.026(6) N6 0.032(5) 0.033(4) 0.034(6) -0.007(4) -0.015(4) -0.011(4) C60 0.027(7) 0.037(6) 0.057(9) -0.001(6) -0.018(6) -0.012(5) C61 0.030(7) 0.030(5) 0.047(9) -0.003(5) -0.009(6) -0.008(5) C62 0.048(8) 0.046(6) 0.053(9) 0.011(6) -0.026(7) -0.026(6) C63 0.039(7) 0.048(6) 0.039(9) 0.010(6) -0.014(6) -0.025(6) C64 0.028(6) 0.028(5) 0.041(8) 0.017(5) -0.012(6) -0.020(5) C65 0.036(7) 0.034(5) 0.021(7) 0.000(5) -0.001(5) -0.023(5) C66 0.017(6) 0.038(5) 0.026(8) -0.010(5) 0.006(5) -0.010(5) C67 0.038(7) 0.049(6) 0.030(8) 0.002(5) -0.017(6) -0.022(5) C68 0.044(7) 0.047(6) 0.025(8) -0.001(5) -0.013(6) -0.025(6) C69 0.050(8) 0.040(6) 0.034(8) -0.006(5) -0.010(6) -0.026(6) C70 0.036(7) 0.035(5) 0.032(8) 0.003(5) -0.014(5) -0.020(5) O4 0.032(4) 0.033(3) 0.029(5) -0.011(3) -0.013(3) -0.010(3) C71 0.059(6) 0.058(5) 0.040(7) -0.004(5) -0.022(6) -0.029(5) C72 0.14(2) 0.062(6) 0.053(18) 0.003(9) -0.059(17) -0.056(9) C73 0.059(6) 0.16(2) 0.093(19) -0.058(19) -0.025(11) -0.044(10) C74 0.105(19) 0.082(16) 0.044(9) 0.011(9) -0.046(10) -0.071(16) C75 0.14(3) 0.11(2) 0.06(2) -0.009(14) -0.035(15) -0.10(2) C76 0.12(3) 0.076(15) 0.06(2) -0.015(11) -0.07(2) -0.017(12) C77 0.092(16) 0.08(2) 0.07(2) -0.052(18) -0.024(10) -0.027(11) O5 0.034(5) 0.047(4) 0.040(6) -0.008(4) -0.008(4) -0.020(4) O6 0.079(6) 0.066(5) 0.064(7) -0.016(5) 0.000(5) -0.047(5) C78 0.054(9) 0.060(8) 0.101(15) -0.039(9) -0.023(9) -0.019(7) C79 0.146(16) 0.115(12) 0.098(15) -0.068(11) 0.030(11) -0.070(12) O7 0.038(5) 0.039(4) 0.035(6) -0.001(4) -0.017(4) -0.024(3) O8 0.038(4) 0.041(4) 0.023(5) -0.003(3) -0.014(3) -0.028(3) C80 0.037(7) 0.044(6) 0.034(9) -0.014(6) -0.019(6) -0.010(5) C81 0.070(9) 0.070(7) 0.025(8) -0.008(6) -0.014(6) -0.045(7) O9 0.034(5) 0.035(4) 0.057(6) -0.016(4) -0.002(4) -0.018(4) O10 0.055(6) 0.066(5) 0.081(8) 0.000(5) -0.021(5) -0.023(5) C82 0.049(9) 0.034(6) 0.071(11) -0.012(7) -0.012(8) -0.017(7) C83 0.046(8) 0.046(6) 0.059(10) -0.004(6) -0.014(7) -0.024(6) O11 0.040(4) 0.030(3) 0.034(5) 0.001(3) -0.011(4) -0.023(3) C84 0.029(6) 0.034(5) 0.043(8) 0.008(5) -0.019(6) -0.013(5) _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 Co1 O1 1.848(7) . ? Co1 O5 1.885(7) . ? Co1 O2 1.888(5) . ? Co1 N2 1.892(8) . ? Co1 N1 1.903(6) . ? Co1 O7 1.928(7) . ? Co2 O8 2.037(4) . ? Co2 O11 2.082(6) . ? Co2 N3 2.090(7) . ? Co2 O3 2.142(6) . ? Co2 N4 2.168(8) . ? Co2 O2 2.168(6) . ? Co2 Co3 2.9424(18) . ? Co3 O3 1.831(6) . ? Co3 O4 1.865(5) . ? Co3 N6 1.869(8) . ? Co3 N5 1.885(7) . ? Co3 O11 1.897(6) . ? Co3 O9 1.911(6) . ? C1 O1 1.318(10) . ? C1 C2 1.412(11) . ? C1 C6 1.416(13) . ? C2 C3 1.431(12) . ? C2 C11 1.436(12) . ? C3 C4 1.366(12) . ? C3 H1 0.9500 . ? C4 C5 1.399(12) . ? C4 C7 1.525(13) . ? C5 C6 1.343(12) . ? C5 H2 0.9500 . ? C6 H3 0.9500 . ? C7 C8 1.503(12) . ? C7 C9 1.525(14) . ? C7 C10 1.553(15) . ? C8 H4 0.9800 . ? C8 H5 0.9800 . ? C8 H6 0.9800 . ? C9 H7 0.9800 . ? C9 H8 0.9800 . ? C9 H9 0.9800 . ? C10 H10 0.9800 . ? C10 H11 0.9800 . ? C10 H12 0.9800 . ? N1 C15 1.339(11) . ? N1 C11 1.360(12) . ? C11 C12 1.427(11) . ? C12 C13 1.381(13) . ? C12 H13 0.9500 . ? C13 C14 1.367(13) . ? C13 H14 0.9500 . ? C14 C15 1.378(10) . ? C14 H15 0.9500 . ? C15 C16 1.465(12) . ? N2 C20 1.364(11) . ? N2 C16 1.372(9) . ? C16 C17 1.403(13) . ? C17 C18 1.362(12) . ? C17 H16 0.9500 . ? C18 C19 1.374(10) . ? C18 H17 0.9500 . ? C19 C20 1.379(13) . ? C19 H18 0.9500 . ? C20 C22 1.484(10) . ? C21 O2 1.328(11) . ? C21 C22 1.414(14) . ? C21 C26 1.421(9) . ? C22 C23 1.385(12) . ? C23 C24 1.398(10) . ? C23 H19 0.9500 . ? C24 C25 1.383(13) . ? C24 C27 1.570(12) . ? C25 C26 1.390(13) . ? C25 H20 0.9500 . ? C26 C31 1.478(13) . ? C27 C29 1.485(14) . ? C27 C30 1.503(15) . ? C27 C28 1.527(13) . ? C28 H21 0.9800 . ? C28 H22 0.9800 . ? C28 H23 0.9800 . ? C29 H24 0.9800 . ? C29 H25 0.9800 . ? C29 H26 0.9800 . ? C30 H27 0.9800 . ? C30 H28 0.9800 . ? C30 H29 0.9800 . ? N3 C35 1.335(11) . ? N3 C31 1.365(11) . ? C31 C32 1.358(11) . ? C32 C33 1.374(14) . ? C32 H30 0.9500 . ? C33 C34 1.392(14) . ? C33 H31 0.9500 . ? C34 C35 1.376(11) . ? C34 H32 0.9500 . ? C35 C36 1.466(13) . ? N4 C36 1.351(10) . ? N4 C40 1.353(11) . ? C36 C37 1.396(12) . ? C37 C38 1.367(13) . ? C37 H33 0.9500 . ? C38 C39 1.353(12) . ? C38 H34 0.9500 . ? C39 C40 1.395(13) . ? C39 H35 0.9500 . ? C40 C42 1.474(12) . ? C41 O3 1.318(10) . ? C41 C46 1.420(12) . ? C41 C42 1.433(13) . ? C42 C43 1.404(13) . ? C43 C44 1.396(13) . ? C43 H36 0.9500 . ? C44 C45 1.335(13) . ? C44 C47 1.56(2) . ? C44 C51 1.60(5) . ? C45 C46 1.423(13) . ? C45 H37 0.9500 . ? C46 C55 1.461(13) . ? C47 C50 1.501(19) . ? C47 C49 1.51(2) . ? C47 C48 1.60(3) . ? C48 H38 0.9800 . ? C48 H39 0.9800 . ? C48 H40 0.9800 . ? C49 H41 0.9800 . ? C49 H42 0.9800 . ? C49 H43 0.9800 . ? C50 H44 0.9800 . ? C50 H45 0.9800 . ? C50 H46 0.9800 . ? C51 C52 1.43(7) . ? C51 C53 1.51(5) . ? C51 C54 1.52(6) . ? C52 H47 0.9800 . ? C52 H48 0.9800 . ? C52 H49 0.9800 . ? C53 H50 0.9800 . ? C53 H51 0.9800 . ? C53 H52 0.9800 . ? C54 H53 0.9800 . ? C54 H54 0.9800 . ? C54 H55 0.9800 . ? N5 C55 1.350(12) . ? N5 C59 1.375(12) . ? C55 C56 1.392(12) . ? C56 C57 1.357(15) . ? C56 H56 0.9500 . ? C57 C58 1.382(15) . ? C57 H57 0.9500 . ? C58 C59 1.383(12) . ? C58 H58 0.9500 . ? C59 C60 1.482(14) . ? N6 C60 1.353(11) . ? N6 C64 1.369(11) . ? C60 C61 1.375(13) . ? C61 C62 1.397(13) . ? C61 H59 0.9500 . ? C62 C63 1.375(13) . ? C62 H60 0.9500 . ? C63 C64 1.390(13) . ? C63 H61 0.9500 . ? C64 C66 1.458(12) . ? C65 O4 1.323(9) . ? C65 C70 1.406(11) . ? C65 C66 1.427(13) . ? C66 C67 1.420(11) . ? C67 C68 1.367(12) . ? C67 H62 0.9500 . ? C68 C69 1.397(13) . ? C68 C71 1.565(11) . ? C69 C70 1.368(11) . ? C69 H63 0.9500 . ? C70 H64 0.9500 . ? C71 C75 1.43(3) . ? C71 C74 1.45(2) . ? C71 C73 1.52(2) . ? C71 C77 1.53(3) . ? C71 C72 1.55(2) . ? C71 C76 1.63(3) . ? C72 H65 0.9800 . ? C72 H66 0.9800 . ? C72 H67 0.9800 . ? C73 H68 0.9800 . ? C73 H69 0.9800 . ? C73 H70 0.9800 . ? C74 H71 0.9800 . ? C74 H72 0.9800 . ? C74 H73 0.9800 . ? C75 H74 0.9800 . ? C75 H75 0.9800 . ? C75 H76 0.9800 . ? C76 H77 0.9800 . ? C76 H78 0.9800 . ? C76 H79 0.9800 . ? C77 H80 0.9800 . ? C77 H81 0.9800 . ? C77 H82 0.9800 . ? O5 C78 1.252(15) . ? O6 C78 1.244(13) . ? C78 C79 1.550(15) . ? C79 H83 0.9800 . ? C79 H84 0.9800 . ? C79 H85 0.9800 . ? O7 C80 1.284(11) . ? O8 C80 1.243(9) . ? C80 C81 1.513(12) . ? C81 H86 0.9800 . ? C81 H87 0.9800 . ? C81 H88 0.9800 . ? O9 C82 1.195(12) . ? O10 C82 1.287(13) . ? C82 C83 1.473(14) . ? C83 H89 0.9800 . ? C83 H90 0.9800 . ? C83 H91 0.9800 . ? O11 C84 1.419(8) . ? C84 H92 0.9800 . ? C84 H93 0.9800 . ? C84 H94 0.9800 . ? O12 C85 1.279(16) . ? O12 H95 0.8400 . ? C85 H96 0.9800 . ? C85 H97 0.9800 . ? C85 H98 0.9800 . ? O13 C86 1.40(2) . ? O13 H99 0.8400 . ? C86 H100 0.9800 . ? C86 H101 0.9800 . ? C86 H102 0.9800 . ? O14 C87 1.433(19) . ? O14 H103 0.8400 . ? C87 H104 0.9800 . ? C87 H105 0.9800 . ? C87 H106 0.9800 . ? C88 C89 1.481(17) . ? C88 H107 0.9800 . ? C88 H108 0.9800 . ? C88 H109 0.9800 . ? C89 O15 1.405(16) . ? C89 H110 0.9900 . ? C89 H111 0.9900 . ? O15 C90 1.408(16) . ? C90 C91 1.464(17) . ? C90 H112 0.9900 . ? C90 H113 0.9900 . ? C91 H114 0.9800 . ? C91 H115 0.9800 . ? C91 H116 0.9800 . ? 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 Co1 O5 87.3(3) . . ? O1 Co1 O2 88.0(3) . . ? O5 Co1 O2 87.7(3) . . ? O1 Co1 N2 178.1(3) . . ? O5 Co1 N2 94.3(3) . . ? O2 Co1 N2 91.1(3) . . ? O1 Co1 N1 95.6(3) . . ? O5 Co1 N1 96.7(3) . . ? O2 Co1 N1 174.4(3) . . ? N2 Co1 N1 85.2(3) . . ? O1 Co1 O7 90.5(3) . . ? O5 Co1 O7 177.8(3) . . ? O2 Co1 O7 92.0(2) . . ? N2 Co1 O7 87.9(3) . . ? N1 Co1 O7 83.8(3) . . ? O8 Co2 O11 94.8(2) . . ? O8 Co2 N3 132.5(3) . . ? O11 Co2 N3 124.3(3) . . ? O8 Co2 O3 87.9(2) . . ? O11 Co2 O3 72.2(2) . . ? N3 Co2 O3 126.4(2) . . ? O8 Co2 N4 84.4(2) . . ? O11 Co2 N4 147.6(3) . . ? N3 Co2 N4 75.8(3) . . ? O3 Co2 N4 75.4(3) . . ? O8 Co2 O2 81.8(2) . . ? O11 Co2 O2 84.5(2) . . ? N3 Co2 O2 77.0(2) . . ? O3 Co2 O2 153.7(2) . . ? N4 Co2 O2 127.0(3) . . ? O8 Co2 Co3 107.60(18) . . ? O11 Co2 Co3 39.93(16) . . ? N3 Co2 Co3 119.60(18) . . ? O3 Co2 Co3 38.30(16) . . ? N4 Co2 Co3 109.6(2) . . ? O2 Co2 Co3 123.30(17) . . ? O3 Co3 O4 82.5(2) . . ? O3 Co3 N6 175.7(3) . . ? O4 Co3 N6 96.3(3) . . ? O3 Co3 N5 93.9(3) . . ? O4 Co3 N5 176.0(3) . . ? N6 Co3 N5 87.2(3) . . ? O3 Co3 O11 83.8(3) . . ? O4 Co3 O11 82.4(2) . . ? N6 Co3 O11 92.0(3) . . ? N5 Co3 O11 95.6(3) . . ? O3 Co3 O9 90.3(3) . . ? O4 Co3 O9 88.7(3) . . ? N6 Co3 O9 93.8(3) . . ? N5 Co3 O9 93.1(3) . . ? O11 Co3 O9 169.8(3) . . ? O3 Co3 Co2 46.5(2) . . ? O4 Co3 Co2 59.79(16) . . ? N6 Co3 Co2 129.5(3) . . ? N5 Co3 Co2 116.4(2) . . ? O11 Co3 Co2 44.78(18) . . ? O9 Co3 Co2 125.9(2) . . ? O1 C1 C2 124.2(8) . . ? O1 C1 C6 118.0(7) . . ? C2 C1 C6 117.6(9) . . ? C1 C2 C3 117.6(8) . . ? C1 C2 C11 123.3(9) . . ? C3 C2 C11 118.8(7) . . ? C4 C3 C2 124.2(8) . . ? C4 C3 H1 117.9 . . ? C2 C3 H1 117.9 . . ? C3 C4 C5 115.5(10) . . ? C3 C4 C7 123.8(8) . . ? C5 C4 C7 120.8(9) . . ? C6 C5 C4 123.6(9) . . ? C6 C5 H2 118.2 . . ? C4 C5 H2 118.2 . . ? C5 C6 C1 121.3(8) . . ? C5 C6 H3 119.3 . . ? C1 C6 H3 119.3 . . ? C1 O1 Co1 122.8(5) . . ? C8 C7 C4 113.1(8) . . ? C8 C7 C9 110.6(10) . . ? C4 C7 C9 109.5(8) . . ? C8 C7 C10 107.6(9) . . ? C4 C7 C10 110.5(9) . . ? C9 C7 C10 105.3(9) . . ? C7 C8 H4 109.5 . . ? C7 C8 H5 109.5 . . ? H4 C8 H5 109.5 . . ? C7 C8 H6 109.5 . . ? H4 C8 H6 109.5 . . ? H5 C8 H6 109.5 . . ? C7 C9 H7 109.5 . . ? C7 C9 H8 109.5 . . ? H7 C9 H8 109.5 . . ? C7 C9 H9 109.5 . . ? H7 C9 H9 109.5 . . ? H8 C9 H9 109.5 . . ? C7 C10 H10 109.5 . . ? C7 C10 H11 109.5 . . ? H10 C10 H11 109.5 . . ? C7 C10 H12 109.5 . . ? H10 C10 H12 109.5 . . ? H11 C10 H12 109.5 . . ? C15 N1 C11 121.8(7) . . ? C15 N1 Co1 112.3(6) . . ? C11 N1 Co1 124.4(6) . . ? N1 C11 C12 116.1(9) . . ? N1 C11 C2 119.7(7) . . ? C12 C11 C2 124.0(10) . . ? C13 C12 C11 121.5(10) . . ? C13 C12 H13 119.3 . . ? C11 C12 H13 119.3 . . ? C14 C13 C12 119.6(8) . . ? C14 C13 H14 120.2 . . ? C12 C13 H14 120.2 . . ? C13 C14 C15 117.9(9) . . ? C13 C14 H15 121.0 . . ? C15 C14 H15 121.0 . . ? N1 C15 C14 122.9(9) . . ? N1 C15 C16 113.7(7) . . ? C14 C15 C16 123.4(8) . . ? C20 N2 C16 119.6(8) . . ? C20 N2 Co1 128.5(5) . . ? C16 N2 Co1 111.9(6) . . ? N2 C16 C17 121.3(9) . . ? N2 C16 C15 114.1(8) . . ? C17 C16 C15 124.5(7) . . ? C18 C17 C16 117.9(7) . . ? C18 C17 H16 121.0 . . ? C16 C17 H16 121.0 . . ? C17 C18 C19 120.5(9) . . ? C17 C18 H17 119.7 . . ? C19 C18 H17 119.7 . . ? C18 C19 C20 121.0(9) . . ? C18 C19 H18 119.5 . . ? C20 C19 H18 119.5 . . ? N2 C20 C19 119.2(7) . . ? N2 C20 C22 118.2(8) . . ? C19 C20 C22 122.5(9) . . ? O2 C21 C22 122.4(7) . . ? O2 C21 C26 119.3(8) . . ? C22 C21 C26 118.2(9) . . ? C23 C22 C21 118.8(7) . . ? C23 C22 C20 119.6(9) . . ? C21 C22 C20 121.3(8) . . ? C22 C23 C24 122.7(9) . . ? C22 C23 H19 118.6 . . ? C24 C23 H19 118.6 . . ? C25 C24 C23 118.0(8) . . ? C25 C24 C27 120.8(7) . . ? C23 C24 C27 121.1(8) . . ? C24 C25 C26 120.7(7) . . ? C24 C25 H20 119.6 . . ? C26 C25 H20 119.6 . . ? C25 C26 C21 120.7(9) . . ? C25 C26 C31 119.7(7) . . ? C21 C26 C31 118.7(8) . . ? C21 O2 Co1 118.0(5) . . ? C21 O2 Co2 113.8(5) . . ? Co1 O2 Co2 128.0(3) . . ? C29 C27 C30 109.4(11) . . ? C29 C27 C28 107.3(9) . . ? C30 C27 C28 110.7(9) . . ? C29 C27 C24 113.1(7) . . ? C30 C27 C24 108.3(9) . . ? C28 C27 C24 108.1(8) . . ? C27 C28 H21 109.5 . . ? C27 C28 H22 109.5 . . ? H21 C28 H22 109.5 . . ? C27 C28 H23 109.5 . . ? H21 C28 H23 109.5 . . ? H22 C28 H23 109.5 . . ? C27 C29 H24 109.5 . . ? C27 C29 H25 109.5 . . ? H24 C29 H25 109.5 . . ? C27 C29 H26 109.5 . . ? H24 C29 H26 109.5 . . ? H25 C29 H26 109.5 . . ? C27 C30 H27 109.5 . . ? C27 C30 H28 109.5 . . ? H27 C30 H28 109.5 . . ? C27 C30 H29 109.5 . . ? H27 C30 H29 109.5 . . ? H28 C30 H29 109.5 . . ? C35 N3 C31 119.8(8) . . ? C35 N3 Co2 118.4(7) . . ? C31 N3 Co2 121.7(6) . . ? C32 C31 N3 120.2(9) . . ? C32 C31 C26 121.3(9) . . ? N3 C31 C26 118.5(7) . . ? C31 C32 C33 121.1(10) . . ? C31 C32 H30 119.4 . . ? C33 C32 H30 119.4 . . ? C32 C33 C34 118.1(9) . . ? C32 C33 H31 121.0 . . ? C34 C33 H31 121.0 . . ? C35 C34 C33 119.3(10) . . ? C35 C34 H32 120.4 . . ? C33 C34 H32 120.4 . . ? N3 C35 C34 121.5(9) . . ? N3 C35 C36 115.0(7) . . ? C34 C35 C36 123.5(9) . . ? C36 N4 C40 120.4(8) . . ? C36 N4 Co2 114.7(6) . . ? C40 N4 Co2 124.9(6) . . ? N4 C36 C37 119.8(9) . . ? N4 C36 C35 115.3(8) . . ? C37 C36 C35 124.8(8) . . ? C38 C37 C36 120.7(9) . . ? C38 C37 H33 119.6 . . ? C36 C37 H33 119.6 . . ? C39 C38 C37 118.1(9) . . ? C39 C38 H34 121.0 . . ? C37 C38 H34 121.0 . . ? C38 C39 C40 121.7(9) . . ? C38 C39 H35 119.2 . . ? C40 C39 H35 119.2 . . ? N4 C40 C39 119.2(8) . . ? N4 C40 C42 120.1(9) . . ? C39 C40 C42 120.6(9) . . ? O3 C41 C46 124.4(9) . . ? O3 C41 C42 117.2(8) . . ? C46 C41 C42 118.4(8) . . ? C43 C42 C41 119.8(9) . . ? C43 C42 C40 118.3(10) . . ? C41 C42 C40 121.8(8) . . ? C44 C43 C42 121.9(10) . . ? C44 C43 H36 119.1 . . ? C42 C43 H36 119.1 . . ? C45 C44 C43 117.1(9) . . ? C45 C44 C47 122.1(12) . . ? C43 C44 C47 120.1(12) . . ? C45 C44 C51 119.7(18) . . ? C43 C44 C51 121.2(19) . . ? C47 C44 C51 21.9(16) . . ? C44 C45 C46 125.8(9) . . ? C44 C45 H37 117.1 . . ? C46 C45 H37 117.1 . . ? C41 C46 C45 117.0(9) . . ? C41 C46 C55 122.6(8) . . ? C45 C46 C55 120.2(8) . . ? C41 O3 Co3 128.8(6) . . ? C41 O3 Co2 117.1(5) . . ? Co3 O3 Co2 95.2(3) . . ? C50 C47 C49 111.9(15) . . ? C50 C47 C44 105.9(16) . . ? C49 C47 C44 112.8(12) . . ? C50 C47 C48 107.8(14) . . ? C49 C47 C48 105.7(19) . . ? C44 C47 C48 112.6(14) . . ? C47 C48 H38 109.5 . . ? C47 C48 H39 109.5 . . ? H38 C48 H39 109.5 . . ? C47 C48 H40 109.5 . . ? H38 C48 H40 109.5 . . ? H39 C48 H40 109.5 . . ? C47 C49 H41 109.5 . . ? C47 C49 H42 109.5 . . ? H41 C49 H42 109.5 . . ? C47 C49 H43 109.5 . . ? H41 C49 H43 109.5 . . ? H42 C49 H43 109.5 . . ? C47 C50 H44 109.5 . . ? C47 C50 H45 109.5 . . ? H44 C50 H45 109.5 . . ? C47 C50 H46 109.5 . . ? H44 C50 H46 109.5 . . ? H45 C50 H46 109.5 . . ? C52 C51 C53 115(4) . . ? C52 C51 C54 116(4) . . ? C53 C51 C54 103(4) . . ? C52 C51 C44 100(4) . . ? C53 C51 C44 115(3) . . ? C54 C51 C44 108(3) . . ? C51 C52 H47 109.5 . . ? C51 C52 H48 109.5 . . ? H47 C52 H48 109.5 . . ? C51 C52 H49 109.5 . . ? H47 C52 H49 109.5 . . ? H48 C52 H49 109.5 . . ? C51 C53 H50 109.5 . . ? C51 C53 H51 109.5 . . ? H50 C53 H51 109.5 . . ? C51 C53 H52 109.5 . . ? H50 C53 H52 109.5 . . ? H51 C53 H52 109.5 . . ? C51 C54 H53 109.5 . . ? C51 C54 H54 109.5 . . ? H53 C54 H54 109.5 . . ? C51 C54 H55 109.5 . . ? H53 C54 H55 109.5 . . ? H54 C54 H55 109.5 . . ? C55 N5 C59 120.3(8) . . ? C55 N5 Co3 128.4(7) . . ? C59 N5 Co3 111.3(6) . . ? N5 C55 C56 117.8(10) . . ? N5 C55 C46 120.8(8) . . ? C56 C55 C46 121.4(9) . . ? C57 C56 C55 121.6(10) . . ? C57 C56 H56 119.2 . . ? C55 C56 H56 119.2 . . ? C56 C57 C58 121.7(10) . . ? C56 C57 H57 119.2 . . ? C58 C57 H57 119.2 . . ? C57 C58 C59 115.6(10) . . ? C57 C58 H58 122.2 . . ? C59 C58 H58 122.2 . . ? N5 C59 C58 123.1(9) . . ? N5 C59 C60 114.4(8) . . ? C58 C59 C60 122.3(10) . . ? C60 N6 C64 120.0(8) . . ? C60 N6 Co3 113.2(6) . . ? C64 N6 Co3 126.9(6) . . ? N6 C60 C61 122.5(9) . . ? N6 C60 C59 113.5(9) . . ? C61 C60 C59 124.0(9) . . ? C60 C61 C62 117.6(9) . . ? C60 C61 H59 121.2 . . ? C62 C61 H59 121.2 . . ? C63 C62 C61 120.0(10) . . ? C63 C62 H60 120.0 . . ? C61 C62 H60 120.0 . . ? C62 C63 C64 120.4(9) . . ? C62 C63 H61 119.8 . . ? C64 C63 H61 119.8 . . ? N6 C64 C63 118.9(8) . . ? N6 C64 C66 119.1(9) . . ? C63 C64 C66 122.0(9) . . ? O4 C65 C70 118.8(9) . . ? O4 C65 C66 123.9(8) . . ? C70 C65 C66 117.3(7) . . ? C67 C66 C65 117.3(8) . . ? C67 C66 C64 117.9(9) . . ? C65 C66 C64 124.8(7) . . ? C68 C67 C66 124.6(9) . . ? C68 C67 H62 117.7 . . ? C66 C67 H62 117.7 . . ? C67 C68 C69 116.7(7) . . ? C67 C68 C71 121.9(9) . . ? C69 C68 C71 121.4(8) . . ? C70 C69 C68 121.4(9) . . ? C70 C69 H63 119.3 . . ? C68 C69 H63 119.3 . . ? C69 C70 C65 122.6(9) . . ? C69 C70 H64 118.7 . . ? C65 C70 H64 118.7 . . ? C65 O4 Co3 124.3(6) . . ? C75 C71 C74 139.0(14) . . ? C75 C71 C73 55.8(18) . . ? C74 C71 C73 110.2(17) . . ? C75 C71 C77 111(2) . . ? C74 C71 C77 56.0(15) . . ? C73 C71 C77 145.1(14) . . ? C75 C71 C72 51.6(17) . . ? C74 C71 C72 111.5(14) . . ? C73 C71 C72 105.0(15) . . ? C77 C71 C72 61.4(15) . . ? C75 C71 C68 110.2(14) . . ? C74 C71 C68 110.8(9) . . ? C73 C71 C68 106.5(11) . . ? C77 C71 C68 108.4(12) . . ? C72 C71 C68 112.5(11) . . ? C75 C71 C76 111(2) . . ? C74 C71 C76 51.4(15) . . ? C73 C71 C76 60.7(17) . . ? C77 C71 C76 105(2) . . ? C72 C71 C76 135.8(12) . . ? C68 C71 C76 111.7(11) . . ? C71 C72 H65 109.5 . . ? C71 C72 H66 109.5 . . ? H65 C72 H66 109.5 . . ? C71 C72 H67 109.5 . . ? H65 C72 H67 109.5 . . ? H66 C72 H67 109.5 . . ? C71 C73 H68 109.5 . . ? C71 C73 H69 109.5 . . ? H68 C73 H69 109.5 . . ? C71 C73 H70 109.5 . . ? H68 C73 H70 109.5 . . ? H69 C73 H70 109.5 . . ? C71 C74 H71 109.5 . . ? C71 C74 H72 109.5 . . ? H71 C74 H72 109.5 . . ? C71 C74 H73 109.5 . . ? H71 C74 H73 109.5 . . ? H72 C74 H73 109.5 . . ? C71 C75 H74 109.5 . . ? C71 C75 H75 109.5 . . ? H74 C75 H75 109.5 . . ? C71 C75 H76 109.5 . . ? H74 C75 H76 109.5 . . ? H75 C75 H76 109.5 . . ? C71 C76 H77 109.5 . . ? C71 C76 H78 109.5 . . ? H77 C76 H78 109.5 . . ? C71 C76 H79 109.5 . . ? H77 C76 H79 109.5 . . ? H78 C76 H79 109.5 . . ? C71 C77 H80 109.5 . . ? C71 C77 H81 109.5 . . ? H80 C77 H81 109.5 . . ? C71 C77 H82 109.5 . . ? H80 C77 H82 109.5 . . ? H81 C77 H82 109.5 . . ? C78 O5 Co1 127.4(6) . . ? O6 C78 O5 127.6(10) . . ? O6 C78 C79 118.9(14) . . ? O5 C78 C79 113.4(10) . . ? C78 C79 H83 109.5 . . ? C78 C79 H84 109.5 . . ? H83 C79 H84 109.5 . . ? C78 C79 H85 109.5 . . ? H83 C79 H85 109.5 . . ? H84 C79 H85 109.5 . . ? C80 O7 Co1 124.5(5) . . ? C80 O8 Co2 140.1(6) . . ? O8 C80 O7 127.9(8) . . ? O8 C80 C81 117.1(10) . . ? O7 C80 C81 115.0(7) . . ? C80 C81 H86 109.5 . . ? C80 C81 H87 109.5 . . ? H86 C81 H87 109.5 . . ? C80 C81 H88 109.5 . . ? H86 C81 H88 109.5 . . ? H87 C81 H88 109.5 . . ? C82 O9 Co3 135.5(7) . . ? O9 C82 O10 121.3(11) . . ? O9 C82 C83 122.0(10) . . ? O10 C82 C83 116.3(11) . . ? C82 C83 H89 109.5 . . ? C82 C83 H90 109.5 . . ? H89 C83 H90 109.5 . . ? C82 C83 H91 109.5 . . ? H89 C83 H91 109.5 . . ? H90 C83 H91 109.5 . . ? C84 O11 Co3 122.7(5) . . ? C84 O11 Co2 121.7(5) . . ? Co3 O11 Co2 95.3(2) . . ? O11 C84 H92 109.5 . . ? O11 C84 H93 109.5 . . ? H92 C84 H93 109.5 . . ? O11 C84 H94 109.5 . . ? H92 C84 H94 109.5 . . ? H93 C84 H94 109.5 . . ? C85 O12 H95 109.5 . . ? O12 C85 H96 109.5 . . ? O12 C85 H97 109.5 . . ? H96 C85 H97 109.5 . . ? O12 C85 H98 109.5 . . ? H96 C85 H98 109.5 . . ? H97 C85 H98 109.5 . . ? C86 O13 H99 109.5 . . ? O13 C86 H100 109.5 . . ? O13 C86 H101 109.5 . . ? H100 C86 H101 109.5 . . ? O13 C86 H102 109.5 . . ? H100 C86 H102 109.5 . . ? H101 C86 H102 109.5 . . ? C89 C88 H107 109.5 . . ? C89 C88 H108 109.5 . . ? H107 C88 H108 109.5 . . ? C89 C88 H109 109.5 . . ? H107 C88 H109 109.5 . . ? H108 C88 H109 109.5 . . ? O15 C89 C88 117.7(18) . . ? O15 C89 H110 107.9 . . ? C88 C89 H110 107.9 . . ? O15 C89 H111 107.9 . . ? C88 C89 H111 107.9 . . ? H110 C89 H111 107.2 . . ? C89 O15 C90 116.8(15) . . ? O15 C90 C91 113.3(16) . . ? O15 C90 H112 108.9 . . ? C91 C90 H112 108.9 . . ? O15 C90 H113 108.9 . . ? C91 C90 H113 108.9 . . ? H112 C90 H113 107.7 . . ? C90 C91 H114 109.5 . . ? C90 C91 H115 109.5 . . ? H114 C91 H115 109.5 . . ? C90 C91 H116 109.5 . . ? H114 C91 H116 109.5 . . ? H115 C91 H116 109.5 . . ? 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 O8 Co2 Co3 O3 -62.3(3) . . . . ? O11 Co2 Co3 O3 -138.2(3) . . . . ? N3 Co2 Co3 O3 112.4(3) . . . . ? N4 Co2 Co3 O3 28.0(3) . . . . ? O2 Co2 Co3 O3 -154.0(2) . . . . ? O8 Co2 Co3 O4 -172.4(3) . . . . ? O11 Co2 Co3 O4 111.6(3) . . . . ? N3 Co2 Co3 O4 2.3(3) . . . . ? O3 Co2 Co3 O4 -110.1(3) . . . . ? N4 Co2 Co3 O4 -82.1(3) . . . . ? O2 Co2 Co3 O4 95.9(3) . . . . ? O8 Co2 Co3 N6 115.9(3) . . . . ? O11 Co2 Co3 N6 40.0(3) . . . . ? N3 Co2 Co3 N6 -69.4(4) . . . . ? O3 Co2 Co3 N6 178.2(3) . . . . ? N4 Co2 Co3 N6 -153.8(3) . . . . ? O2 Co2 Co3 N6 24.2(3) . . . . ? O8 Co2 Co3 N5 6.2(4) . . . . ? O11 Co2 Co3 N5 -69.8(4) . . . . ? N3 Co2 Co3 N5 -179.1(4) . . . . ? O3 Co2 Co3 N5 68.5(4) . . . . ? N4 Co2 Co3 N5 96.5(3) . . . . ? O2 Co2 Co3 N5 -85.5(3) . . . . ? O8 Co2 Co3 O11 76.0(3) . . . . ? N3 Co2 Co3 O11 -109.4(4) . . . . ? O3 Co2 Co3 O11 138.2(3) . . . . ? N4 Co2 Co3 O11 166.2(3) . . . . ? O2 Co2 Co3 O11 -15.8(3) . . . . ? O8 Co2 Co3 O9 -109.5(3) . . . . ? O11 Co2 Co3 O9 174.6(3) . . . . ? N3 Co2 Co3 O9 65.2(4) . . . . ? O3 Co2 Co3 O9 -47.2(3) . . . . ? N4 Co2 Co3 O9 -19.2(3) . . . . ? O2 Co2 Co3 O9 158.8(3) . . . . ? O1 C1 C2 C3 175.7(8) . . . . ? C6 C1 C2 C3 1.0(13) . . . . ? O1 C1 C2 C11 1.7(14) . . . . ? C6 C1 C2 C11 -172.9(9) . . . . ? C1 C2 C3 C4 2.4(14) . . . . ? C11 C2 C3 C4 176.7(10) . . . . ? C2 C3 C4 C5 -2.4(15) . . . . ? C2 C3 C4 C7 178.0(9) . . . . ? C3 C4 C5 C6 -1.1(15) . . . . ? C7 C4 C5 C6 178.5(10) . . . . ? C4 C5 C6 C1 4.6(16) . . . . ? O1 C1 C6 C5 -179.4(8) . . . . ? C2 C1 C6 C5 -4.4(14) . . . . ? C2 C1 O1 Co1 27.8(11) . . . . ? C6 C1 O1 Co1 -157.5(7) . . . . ? O5 Co1 O1 C1 69.4(6) . . . . ? O2 Co1 O1 C1 157.2(6) . . . . ? N2 Co1 O1 C1 -144(7) . . . . ? N1 Co1 O1 C1 -27.1(6) . . . . ? O7 Co1 O1 C1 -110.9(6) . . . . ? C3 C4 C7 C8 7.7(15) . . . . ? C5 C4 C7 C8 -171.8(10) . . . . ? C3 C4 C7 C9 -116.1(11) . . . . ? C5 C4 C7 C9 64.4(13) . . . . ? C3 C4 C7 C10 128.3(10) . . . . ? C5 C4 C7 C10 -51.2(12) . . . . ? O1 Co1 N1 C15 -162.7(7) . . . . ? O5 Co1 N1 C15 109.4(7) . . . . ? O2 Co1 N1 C15 -33(4) . . . . ? N2 Co1 N1 C15 15.6(7) . . . . ? O7 Co1 N1 C15 -72.8(7) . . . . ? O1 Co1 N1 C11 3.6(8) . . . . ? O5 Co1 N1 C11 -84.3(8) . . . . ? O2 Co1 N1 C11 134(3) . . . . ? N2 Co1 N1 C11 -178.1(8) . . . . ? O7 Co1 N1 C11 93.5(8) . . . . ? C15 N1 C11 C12 -0.1(15) . . . . ? Co1 N1 C11 C12 -165.2(7) . . . . ? C15 N1 C11 C2 -174.9(9) . . . . ? Co1 N1 C11 C2 20.0(14) . . . . ? C1 C2 C11 N1 -26.8(15) . . . . ? C3 C2 C11 N1 159.2(9) . . . . ? C1 C2 C11 C12 158.9(10) . . . . ? C3 C2 C11 C12 -15.1(15) . . . . ? N1 C11 C12 C13 3.9(15) . . . . ? C2 C11 C12 C13 178.4(10) . . . . ? C11 C12 C13 C14 -6.1(17) . . . . ? C12 C13 C14 C15 4.5(17) . . . . ? C11 N1 C15 C14 -1.4(15) . . . . ? Co1 N1 C15 C14 165.4(8) . . . . ? C11 N1 C15 C16 176.8(9) . . . . ? Co1 N1 C15 C16 -16.4(10) . . . . ? C13 C14 C15 N1 -0.8(16) . . . . ? C13 C14 C15 C16 -178.9(10) . . . . ? O1 Co1 N2 C20 -75(8) . . . . ? O5 Co1 N2 C20 71.7(8) . . . . ? O2 Co1 N2 C20 -16.0(8) . . . . ? N1 Co1 N2 C20 168.1(8) . . . . ? O7 Co1 N2 C20 -108.0(8) . . . . ? O1 Co1 N2 C16 106(8) . . . . ? O5 Co1 N2 C16 -107.5(6) . . . . ? O2 Co1 N2 C16 164.8(6) . . . . ? N1 Co1 N2 C16 -11.1(6) . . . . ? O7 Co1 N2 C16 72.8(6) . . . . ? C20 N2 C16 C17 4.2(14) . . . . ? Co1 N2 C16 C17 -176.5(8) . . . . ? C20 N2 C16 C15 -174.3(8) . . . . ? Co1 N2 C16 C15 5.0(10) . . . . ? N1 C15 C16 N2 7.6(12) . . . . ? C14 C15 C16 N2 -174.2(9) . . . . ? N1 C15 C16 C17 -170.8(9) . . . . ? C14 C15 C16 C17 7.4(16) . . . . ? N2 C16 C17 C18 0.1(15) . . . . ? C15 C16 C17 C18 178.5(9) . . . . ? C16 C17 C18 C19 -1.1(16) . . . . ? C17 C18 C19 C20 -2.3(16) . . . . ? C16 N2 C20 C19 -7.5(14) . . . . ? Co1 N2 C20 C19 173.4(7) . . . . ? C16 N2 C20 C22 169.5(8) . . . . ? Co1 N2 C20 C22 -9.7(13) . . . . ? C18 C19 C20 N2 6.6(15) . . . . ? C18 C19 C20 C22 -170.2(9) . . . . ? O2 C21 C22 C23 -169.4(8) . . . . ? C26 C21 C22 C23 6.3(14) . . . . ? O2 C21 C22 C20 17.1(14) . . . . ? C26 C21 C22 C20 -167.2(9) . . . . ? N2 C20 C22 C23 -157.8(9) . . . . ? C19 C20 C22 C23 19.0(15) . . . . ? N2 C20 C22 C21 15.7(14) . . . . ? C19 C20 C22 C21 -167.5(10) . . . . ? C21 C22 C23 C24 1.0(15) . . . . ? C20 C22 C23 C24 174.6(9) . . . . ? C22 C23 C24 C25 -8.4(15) . . . . ? C22 C23 C24 C27 175.4(9) . . . . ? C23 C24 C25 C26 8.4(15) . . . . ? C27 C24 C25 C26 -175.3(9) . . . . ? C24 C25 C26 C21 -1.2(15) . . . . ? C24 C25 C26 C31 -170.1(9) . . . . ? O2 C21 C26 C25 169.6(9) . . . . ? C22 C21 C26 C25 -6.3(14) . . . . ? O2 C21 C26 C31 -21.4(13) . . . . ? C22 C21 C26 C31 162.7(9) . . . . ? C22 C21 O2 Co1 -52.3(11) . . . . ? C26 C21 O2 Co1 132.0(7) . . . . ? C22 C21 O2 Co2 132.0(8) . . . . ? C26 C21 O2 Co2 -43.7(10) . . . . ? O1 Co1 O2 C21 -136.6(6) . . . . ? O5 Co1 O2 C21 -49.2(6) . . . . ? N2 Co1 O2 C21 45.1(6) . . . . ? N1 Co1 O2 C21 93(3) . . . . ? O7 Co1 O2 C21 133.0(6) . . . . ? O1 Co1 O2 Co2 38.4(4) . . . . ? O5 Co1 O2 Co2 125.8(4) . . . . ? N2 Co1 O2 Co2 -139.9(4) . . . . ? N1 Co1 O2 Co2 -92(3) . . . . ? O7 Co1 O2 Co2 -52.0(4) . . . . ? O8 Co2 O2 C21 -155.3(6) . . . . ? O11 Co2 O2 C21 -59.6(6) . . . . ? N3 Co2 O2 C21 67.5(6) . . . . ? O3 Co2 O2 C21 -87.4(7) . . . . ? N4 Co2 O2 C21 128.1(6) . . . . ? Co3 Co2 O2 C21 -49.6(6) . . . . ? O8 Co2 O2 Co1 29.5(4) . . . . ? O11 Co2 O2 Co1 125.2(4) . . . . ? N3 Co2 O2 Co1 -107.7(4) . . . . ? O3 Co2 O2 Co1 97.4(6) . . . . ? N4 Co2 O2 Co1 -47.1(4) . . . . ? Co3 Co2 O2 Co1 135.2(3) . . . . ? C25 C24 C27 C29 162.0(10) . . . . ? C23 C24 C27 C29 -21.8(14) . . . . ? C25 C24 C27 C30 -76.6(13) . . . . ? C23 C24 C27 C30 99.6(11) . . . . ? C25 C24 C27 C28 43.4(13) . . . . ? C23 C24 C27 C28 -140.4(10) . . . . ? O8 Co2 N3 C35 68.5(7) . . . . ? O11 Co2 N3 C35 -151.7(5) . . . . ? O3 Co2 N3 C35 -59.2(7) . . . . ? N4 Co2 N3 C35 0.2(6) . . . . ? O2 Co2 N3 C35 134.3(6) . . . . ? Co3 Co2 N3 C35 -104.6(6) . . . . ? O8 Co2 N3 C31 -114.6(6) . . . . ? O11 Co2 N3 C31 25.2(7) . . . . ? O3 Co2 N3 C31 117.7(6) . . . . ? N4 Co2 N3 C31 177.1(6) . . . . ? O2 Co2 N3 C31 -48.8(6) . . . . ? Co3 Co2 N3 C31 72.3(6) . . . . ? C35 N3 C31 C32 1.8(11) . . . . ? Co2 N3 C31 C32 -175.0(6) . . . . ? C35 N3 C31 C26 -175.3(7) . . . . ? Co2 N3 C31 C26 7.8(10) . . . . ? C25 C26 C31 C32 35.2(13) . . . . ? C21 C26 C31 C32 -133.9(9) . . . . ? C25 C26 C31 N3 -147.7(9) . . . . ? C21 C26 C31 N3 43.2(12) . . . . ? N3 C31 C32 C33 0.7(13) . . . . ? C26 C31 C32 C33 177.7(8) . . . . ? C31 C32 C33 C34 -2.7(14) . . . . ? C32 C33 C34 C35 2.2(14) . . . . ? C31 N3 C35 C34 -2.3(12) . . . . ? Co2 N3 C35 C34 174.7(6) . . . . ? C31 N3 C35 C36 177.6(7) . . . . ? Co2 N3 C35 C36 -5.5(9) . . . . ? C33 C34 C35 N3 0.2(13) . . . . ? C33 C34 C35 C36 -179.6(8) . . . . ? O8 Co2 N4 C36 -130.9(5) . . . . ? O11 Co2 N4 C36 138.9(5) . . . . ? N3 Co2 N4 C36 5.5(5) . . . . ? O3 Co2 N4 C36 139.8(5) . . . . ? O2 Co2 N4 C36 -55.6(5) . . . . ? Co3 Co2 N4 C36 122.3(5) . . . . ? O8 Co2 N4 C40 46.4(6) . . . . ? O11 Co2 N4 C40 -43.7(8) . . . . ? N3 Co2 N4 C40 -177.1(6) . . . . ? O3 Co2 N4 C40 -42.8(6) . . . . ? O2 Co2 N4 C40 121.8(6) . . . . ? Co3 Co2 N4 C40 -60.3(6) . . . . ? C40 N4 C36 C37 -3.1(10) . . . . ? Co2 N4 C36 C37 174.4(5) . . . . ? C40 N4 C36 C35 172.5(7) . . . . ? Co2 N4 C36 C35 -10.1(8) . . . . ? N3 C35 C36 N4 10.3(10) . . . . ? C34 C35 C36 N4 -169.8(8) . . . . ? N3 C35 C36 C37 -174.4(7) . . . . ? C34 C35 C36 C37 5.5(12) . . . . ? N4 C36 C37 C38 0.5(11) . . . . ? C35 C36 C37 C38 -174.6(7) . . . . ? C36 C37 C38 C39 3.1(12) . . . . ? C37 C38 C39 C40 -4.2(12) . . . . ? C36 N4 C40 C39 2.0(11) . . . . ? Co2 N4 C40 C39 -175.2(5) . . . . ? C36 N4 C40 C42 -174.0(7) . . . . ? Co2 N4 C40 C42 8.8(10) . . . . ? C38 C39 C40 N4 1.7(12) . . . . ? C38 C39 C40 C42 177.7(7) . . . . ? O3 C41 C42 C43 -178.2(7) . . . . ? C46 C41 C42 C43 1.7(13) . . . . ? O3 C41 C42 C40 -1.1(13) . . . . ? C46 C41 C42 C40 178.8(8) . . . . ? N4 C40 C42 C43 -155.6(8) . . . . ? C39 C40 C42 C43 28.5(11) . . . . ? N4 C40 C42 C41 27.2(12) . . . . ? C39 C40 C42 C41 -148.7(8) . . . . ? C41 C42 C43 C44 -0.3(13) . . . . ? C40 C42 C43 C44 -177.5(8) . . . . ? C42 C43 C44 C45 -0.2(15) . . . . ? C42 C43 C44 C47 170.3(11) . . . . ? C42 C43 C44 C51 -164(2) . . . . ? C43 C44 C45 C46 -0.8(16) . . . . ? C47 C44 C45 C46 -171.1(11) . . . . ? C51 C44 C45 C46 164(2) . . . . ? O3 C41 C46 C45 177.4(8) . . . . ? C42 C41 C46 C45 -2.6(12) . . . . ? O3 C41 C46 C55 -7.5(14) . . . . ? C42 C41 C46 C55 172.5(8) . . . . ? C44 C45 C46 C41 2.2(15) . . . . ? C44 C45 C46 C55 -173.0(10) . . . . ? C46 C41 O3 Co3 -1.2(12) . . . . ? C42 C41 O3 Co3 178.8(5) . . . . ? C46 C41 O3 Co2 121.7(8) . . . . ? C42 C41 O3 Co2 -58.4(9) . . . . ? O4 Co3 O3 C41 -173.7(7) . . . . ? N6 Co3 O3 C41 113(3) . . . . ? N5 Co3 O3 C41 8.0(7) . . . . ? O11 Co3 O3 C41 103.2(7) . . . . ? O9 Co3 O3 C41 -85.1(7) . . . . ? Co2 Co3 O3 C41 131.3(7) . . . . ? O4 Co3 O3 Co2 54.9(2) . . . . ? N6 Co3 O3 Co2 -19(3) . . . . ? N5 Co3 O3 Co2 -123.4(3) . . . . ? O11 Co3 O3 Co2 -28.2(2) . . . . ? O9 Co3 O3 Co2 143.5(2) . . . . ? O8 Co2 O3 C41 -16.5(6) . . . . ? O11 Co2 O3 C41 -112.3(6) . . . . ? N3 Co2 O3 C41 127.8(6) . . . . ? N4 Co2 O3 C41 68.2(6) . . . . ? O2 Co2 O3 C41 -83.2(8) . . . . ? Co3 Co2 O3 C41 -138.9(7) . . . . ? O8 Co2 O3 Co3 122.4(2) . . . . ? O11 Co2 O3 Co3 26.67(18) . . . . ? N3 Co2 O3 Co3 -93.3(3) . . . . ? N4 Co2 O3 Co3 -152.8(2) . . . . ? O2 Co2 O3 Co3 55.8(5) . . . . ? C45 C44 C47 C50 -68.4(18) . . . . ? C43 C44 C47 C50 121.6(15) . . . . ? C51 C44 C47 C50 22(5) . . . . ? C45 C44 C47 C49 54.3(18) . . . . ? C43 C44 C47 C49 -115.6(15) . . . . ? C51 C44 C47 C49 145(6) . . . . ? C45 C44 C47 C48 174.0(13) . . . . ? C43 C44 C47 C48 4(2) . . . . ? C51 C44 C47 C48 -96(6) . . . . ? C45 C44 C51 C52 140(3) . . . . ? C43 C44 C51 C52 -56(4) . . . . ? C47 C44 C51 C52 37(5) . . . . ? C45 C44 C51 C53 -96(4) . . . . ? C43 C44 C51 C53 68(4) . . . . ? C47 C44 C51 C53 161(8) . . . . ? C45 C44 C51 C54 18(4) . . . . ? C43 C44 C51 C54 -178(3) . . . . ? C47 C44 C51 C54 -84(6) . . . . ? O3 Co3 N5 C55 -9.5(8) . . . . ? O4 Co3 N5 C55 -34(5) . . . . ? N6 Co3 N5 C55 174.6(8) . . . . ? O11 Co3 N5 C55 -93.7(8) . . . . ? O9 Co3 N5 C55 81.0(8) . . . . ? Co2 Co3 N5 C55 -52.0(8) . . . . ? O3 Co3 N5 C59 170.1(6) . . . . ? O4 Co3 N5 C59 145(4) . . . . ? N6 Co3 N5 C59 -5.8(7) . . . . ? O11 Co3 N5 C59 85.9(6) . . . . ? O9 Co3 N5 C59 -99.4(7) . . . . ? Co2 Co3 N5 C59 127.5(6) . . . . ? C59 N5 C55 C56 2.7(13) . . . . ? Co3 N5 C55 C56 -177.7(7) . . . . ? C59 N5 C55 C46 -175.2(8) . . . . ? Co3 N5 C55 C46 4.3(13) . . . . ? C41 C46 C55 N5 5.7(14) . . . . ? C45 C46 C55 N5 -179.4(8) . . . . ? C41 C46 C55 C56 -172.2(8) . . . . ? C45 C46 C55 C56 2.7(14) . . . . ? N5 C55 C56 C57 -2.1(15) . . . . ? C46 C55 C56 C57 175.8(11) . . . . ? C55 C56 C57 C58 0.6(19) . . . . ? C56 C57 C58 C59 0.3(17) . . . . ? C55 N5 C59 C58 -1.9(14) . . . . ? Co3 N5 C59 C58 178.4(7) . . . . ? C55 N5 C59 C60 -176.4(8) . . . . ? Co3 N5 C59 C60 4.0(10) . . . . ? C57 C58 C59 N5 0.3(15) . . . . ? C57 C58 C59 C60 174.4(10) . . . . ? O3 Co3 N6 C60 -98(3) . . . . ? O4 Co3 N6 C60 -171.5(6) . . . . ? N5 Co3 N6 C60 6.6(6) . . . . ? O11 Co3 N6 C60 -88.9(6) . . . . ? O9 Co3 N6 C60 99.4(6) . . . . ? Co2 Co3 N6 C60 -115.9(6) . . . . ? O3 Co3 N6 C64 81(3) . . . . ? O4 Co3 N6 C64 8.2(8) . . . . ? N5 Co3 N6 C64 -173.8(8) . . . . ? O11 Co3 N6 C64 90.7(7) . . . . ? O9 Co3 N6 C64 -80.9(8) . . . . ? Co2 Co3 N6 C64 63.8(8) . . . . ? C64 N6 C60 C61 -4.4(14) . . . . ? Co3 N6 C60 C61 175.3(8) . . . . ? C64 N6 C60 C59 174.5(8) . . . . ? Co3 N6 C60 C59 -5.8(10) . . . . ? N5 C59 C60 N6 1.1(12) . . . . ? C58 C59 C60 N6 -173.4(9) . . . . ? N5 C59 C60 C61 -180.0(9) . . . . ? C58 C59 C60 C61 5.5(16) . . . . ? N6 C60 C61 C62 -1.3(15) . . . . ? C59 C60 C61 C62 180.0(9) . . . . ? C60 C61 C62 C63 2.5(14) . . . . ? C61 C62 C63 C64 1.9(14) . . . . ? C60 N6 C64 C63 8.7(13) . . . . ? Co3 N6 C64 C63 -171.0(7) . . . . ? C60 N6 C64 C66 -171.7(8) . . . . ? Co3 N6 C64 C66 8.6(12) . . . . ? C62 C63 C64 N6 -7.5(14) . . . . ? C62 C63 C64 C66 172.9(8) . . . . ? O4 C65 C66 C67 -174.5(8) . . . . ? C70 C65 C66 C67 4.7(13) . . . . ? O4 C65 C66 C64 5.6(15) . . . . ? C70 C65 C66 C64 -175.2(8) . . . . ? N6 C64 C66 C67 161.3(8) . . . . ? C63 C64 C66 C67 -19.1(13) . . . . ? N6 C64 C66 C65 -18.9(13) . . . . ? C63 C64 C66 C65 160.7(10) . . . . ? C65 C66 C67 C68 -1.7(14) . . . . ? C64 C66 C67 C68 178.2(9) . . . . ? C66 C67 C68 C69 -2.3(14) . . . . ? C66 C67 C68 C71 179.4(10) . . . . ? C67 C68 C69 C70 3.2(15) . . . . ? C71 C68 C69 C70 -178.4(9) . . . . ? C68 C69 C70 C65 -0.1(15) . . . . ? O4 C65 C70 C69 175.2(9) . . . . ? C66 C65 C70 C69 -4.0(13) . . . . ? C70 C65 O4 Co3 -162.1(6) . . . . ? C66 C65 O4 Co3 17.0(12) . . . . ? O3 Co3 O4 C65 163.1(7) . . . . ? N6 Co3 O4 C65 -21.0(7) . . . . ? N5 Co3 O4 C65 -172(4) . . . . ? O11 Co3 O4 C65 -112.2(7) . . . . ? O9 Co3 O4 C65 72.7(7) . . . . ? Co2 Co3 O4 C65 -153.5(7) . . . . ? C67 C68 C71 C75 -113(2) . . . . ? C69 C68 C71 C75 69(2) . . . . ? C67 C68 C71 C74 65.7(17) . . . . ? C69 C68 C71 C74 -112.6(16) . . . . ? C67 C68 C71 C73 -54.1(18) . . . . ? C69 C68 C71 C73 127.6(17) . . . . ? C67 C68 C71 C77 125.5(17) . . . . ? C69 C68 C71 C77 -52.8(19) . . . . ? C67 C68 C71 C72 -168.7(14) . . . . ? C69 C68 C71 C72 13.0(18) . . . . ? C67 C68 C71 C76 10(2) . . . . ? C69 C68 C71 C76 -168.0(19) . . . . ? O1 Co1 O5 C78 -147.0(10) . . . . ? O2 Co1 O5 C78 124.9(10) . . . . ? N2 Co1 O5 C78 34.0(10) . . . . ? N1 Co1 O5 C78 -51.6(11) . . . . ? O7 Co1 O5 C78 -154(6) . . . . ? Co1 O5 C78 O6 6(2) . . . . ? Co1 O5 C78 C79 -169.4(8) . . . . ? O1 Co1 O7 C80 -43.2(8) . . . . ? O5 Co1 O7 C80 -36(7) . . . . ? O2 Co1 O7 C80 44.7(8) . . . . ? N2 Co1 O7 C80 135.7(8) . . . . ? N1 Co1 O7 C80 -138.8(8) . . . . ? O11 Co2 O8 C80 -63.1(10) . . . . ? N3 Co2 O8 C80 84.6(10) . . . . ? O3 Co2 O8 C80 -135.0(10) . . . . ? N4 Co2 O8 C80 149.4(10) . . . . ? O2 Co2 O8 C80 20.7(10) . . . . ? Co3 Co2 O8 C80 -101.7(10) . . . . ? Co2 O8 C80 O7 -31.4(17) . . . . ? Co2 O8 C80 C81 150.7(8) . . . . ? Co1 O7 C80 O8 -13.5(15) . . . . ? Co1 O7 C80 C81 164.5(6) . . . . ? O3 Co3 O9 C82 130.5(11) . . . . ? O4 Co3 O9 C82 -147.0(11) . . . . ? N6 Co3 O9 C82 -50.8(11) . . . . ? N5 Co3 O9 C82 36.6(11) . . . . ? O11 Co3 O9 C82 -175.3(14) . . . . ? Co2 Co3 O9 C82 162.6(10) . . . . ? Co3 O9 C82 O10 13.9(18) . . . . ? Co3 O9 C82 C83 -174.6(7) . . . . ? O3 Co3 O11 C84 -104.3(6) . . . . ? O4 Co3 O11 C84 172.5(6) . . . . ? N6 Co3 O11 C84 76.4(6) . . . . ? N5 Co3 O11 C84 -10.9(6) . . . . ? O9 Co3 O11 C84 -158.9(14) . . . . ? Co2 Co3 O11 C84 -133.3(7) . . . . ? O3 Co3 O11 Co2 29.1(2) . . . . ? O4 Co3 O11 Co2 -54.1(2) . . . . ? N6 Co3 O11 Co2 -150.2(3) . . . . ? N5 Co3 O11 Co2 122.4(3) . . . . ? O9 Co3 O11 Co2 -25.6(17) . . . . ? O8 Co2 O11 C84 22.1(6) . . . . ? N3 Co2 O11 C84 -129.3(6) . . . . ? O3 Co2 O11 C84 108.3(6) . . . . ? N4 Co2 O11 C84 109.2(7) . . . . ? O2 Co2 O11 C84 -59.2(6) . . . . ? Co3 Co2 O11 C84 134.0(7) . . . . ? O8 Co2 O11 Co3 -111.9(2) . . . . ? N3 Co2 O11 Co3 96.7(3) . . . . ? O3 Co2 O11 Co3 -25.69(19) . . . . ? N4 Co2 O11 Co3 -24.8(5) . . . . ? O2 Co2 O11 Co3 166.8(2) . . . . ? C88 C89 O15 C90 -175(2) . . . . ? C89 O15 C90 C91 164(2) . . . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 0.999 _refine_diff_density_min -0.609 _refine_diff_density_rms 0.102 _database_code_depnum_ccdc_archive 'CCDC 938303'