Supplementary Material (ESI) for Chemical Communications This journal is © The Royal Society of Chemistry 2001 data_global _journal_coden_Cambridge 182 _publ_requested_journal 'Chemical Communications' loop_ _publ_author_name 'Gazeau, Stephanie' 'Marchon,J.C.' 'Pecaut, Jacques' _publ_contact_author_name 'Dr J C Marchon' _publ_contact_author_address ; Laboratoire de Chimie Inorganique et Biologique CEA-Grenoble DRFMC/SCIB Grenoble cedex 9 38054 FRANCE ; _publ_contact_author_email 'JCMARCHON@CEA.FR' _publ_section_title ; Nickel porphyrin nanotweezers ; data_NiPP8mono _database_code_CSD 167256 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C60.50 H74.75 N4.25 Ni O9' _chemical_formula_weight 1064.21 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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 P2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 16.8288(8) _cell_length_b 19.5869(9) _cell_length_c 20.0979(9) _cell_angle_alpha 90.00 _cell_angle_beta 110.3270(10) _cell_angle_gamma 90.00 _cell_volume 6212.2(5) _cell_formula_units_Z 4 _cell_measurement_temperature 193(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.08 _exptl_crystal_size_mid 0.4 _exptl_crystal_size_min 0.4 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.138 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2270 _exptl_absorpt_coefficient_mu 0.366 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 193(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 24730 _diffrn_reflns_av_R_equivalents 0.0490 _diffrn_reflns_av_sigmaI/netI 0.0903 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.66 _diffrn_reflns_theta_max 29.63 _reflns_number_total 17805 _reflns_number_gt 12196 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.1000P)^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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.017(13) _refine_ls_number_reflns 17805 _refine_ls_number_parameters 1392 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0954 _refine_ls_R_factor_gt 0.0637 _refine_ls_wR_factor_ref 0.1772 _refine_ls_wR_factor_gt 0.1649 _refine_ls_goodness_of_fit_ref 1.057 _refine_ls_restrained_S_all 1.057 _refine_ls_shift/su_max 0.124 _refine_ls_shift/su_mean 0.004 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 0.25714(4) 0.05691(4) 0.92544(4) 0.0244(2) Uani 1 1 d . . . O21 O 0.1778(3) 0.3069(3) 0.9998(3) 0.0539(15) Uani 1 1 d . . . O22 O 0.0481(3) 0.3255(2) 1.0061(3) 0.0400(13) Uani 1 1 d . . . O41 O 0.2000(3) -0.1215(3) 0.7371(4) 0.0632(16) Uani 1 1 d . . . O42 O 0.2934(3) -0.1648(3) 0.6923(3) 0.0559(16) Uani 1 1 d . . . O61 O 0.5925(3) 0.0684(3) 0.9396(3) 0.0577(16) Uani 1 1 d . . . O62 O 0.6532(2) -0.0295(3) 0.9190(3) 0.0448(14) Uani 1 1 d . . . O81 O 0.0220(2) -0.0357(2) 0.9900(3) 0.0319(11) Uani 1 1 d . . . O82 O -0.0558(2) -0.0175(2) 1.0611(3) 0.0358(12) Uani 1 1 d . . . N1 N 0.1774(2) 0.0952(2) 0.9626(3) 0.0211(12) Uani 1 1 d . . . N2 N 0.2009(2) 0.1016(2) 0.8356(3) 0.0232(12) Uani 1 1 d . . . N3 N 0.3363(3) 0.0161(3) 0.8880(3) 0.0273(13) Uani 1 1 d . . . N4 N 0.3152(3) 0.0151(3) 1.0151(3) 0.0261(12) Uani 1 1 d . . . C1 C 0.1590(3) 0.0718(3) 1.0200(3) 0.0214(14) Uani 1 1 d . . . C2 C 0.0909(3) 0.1127(3) 1.0291(4) 0.0260(15) Uani 1 1 d . . . H2 H 0.0649 0.1065 1.0637 0.031 Uiso 1 1 calc R . . C3 C 0.0729(3) 0.1606(3) 0.9788(4) 0.0291(16) Uani 1 1 d . . . H3 H 0.0322 0.1959 0.9725 0.035 Uiso 1 1 calc R . . C4 C 0.1239(3) 0.1505(3) 0.9360(4) 0.0208(14) Uani 1 1 d . . . C5 C 0.1162(3) 0.1845(3) 0.8748(4) 0.0246(15) Uani 1 1 d . . . C6 C 0.1495(3) 0.1576(3) 0.8251(4) 0.0260(15) Uani 1 1 d . . . C7 C 0.1250(4) 0.1781(3) 0.7532(4) 0.0343(17) Uani 1 1 d . . . H7 H 0.0918 0.2169 0.7324 0.041 Uiso 1 1 calc R . . C8 C 0.1577(4) 0.1321(3) 0.7199(4) 0.0341(17) Uani 1 1 d . . . H8 H 0.1502 0.1319 0.6708 0.041 Uiso 1 1 calc R . . C9 C 0.2057(3) 0.0837(3) 0.7716(4) 0.0259(15) Uani 1 1 d . . . C10 C 0.2567(3) 0.0328(3) 0.7593(4) 0.0280(16) Uani 1 1 d . . . C11 C 0.3229(3) 0.0040(3) 0.8171(4) 0.0312(17) Uani 1 1 d . . . C12 C 0.3905(3) -0.0358(3) 0.8101(4) 0.0336(17) Uani 1 1 d . . . H12 H 0.3947 -0.0530 0.7673 0.040 Uiso 1 1 calc R . . C13 C 0.4464(3) -0.0442(3) 0.8752(4) 0.0348(17) Uani 1 1 d . . . H13 H 0.4992 -0.0672 0.8870 0.042 Uiso 1 1 calc R . . C14 C 0.4132(3) -0.0129(3) 0.9243(4) 0.0279(16) Uani 1 1 d . . . C15 C 0.4474(3) -0.0162(3) 0.9977(4) 0.0351(18) Uani 1 1 d . . . C16 C 0.3971(3) -0.0070(3) 1.0395(4) 0.0326(16) Uani 1 1 d . . . C17 C 0.4185(4) -0.0325(4) 1.1105(4) 0.046(2) Uani 1 1 d . . . H17 H 0.4724 -0.0488 1.1401 0.055 Uiso 1 1 calc R . . C18 C 0.3465(4) -0.0290(4) 1.1274(5) 0.047(2) Uani 1 1 d . . . H18 H 0.3398 -0.0438 1.1702 0.057 Uiso 1 1 calc R . . C19 C 0.2835(3) 0.0016(3) 1.0675(4) 0.0346(18) Uani 1 1 d . . . C20 C 0.2046(3) 0.0225(3) 1.0697(4) 0.0272(15) Uani 1 1 d . . . C21 C 0.0577(3) 0.2450(3) 0.8508(4) 0.0262(15) Uani 1 1 d . . . H21 H 0.0018 0.2320 0.8149 0.031 Uiso 1 1 calc R . . C22 C 0.0861(4) 0.3137(3) 0.8369(4) 0.0290(15) Uani 1 1 d . . . C23 C 0.1781(4) 0.3290(4) 0.8544(5) 0.051(2) Uani 1 1 d . . . H23A H 0.2114 0.3035 0.8969 0.076 Uiso 1 1 calc R . . H23B H 0.1879 0.3781 0.8632 0.076 Uiso 1 1 calc R . . H23C H 0.1955 0.3156 0.8145 0.076 Uiso 1 1 calc R . . C24 C 0.0280(5) 0.3518(4) 0.7723(4) 0.051(2) Uani 1 1 d . . . H24A H -0.0311 0.3397 0.7645 0.076 Uiso 1 1 calc R . . H24B H 0.0419 0.3391 0.7305 0.076 Uiso 1 1 calc R . . H24C H 0.0357 0.4011 0.7803 0.076 Uiso 1 1 calc R . . C25 C 0.0507(4) 0.3052(3) 0.8957(4) 0.0352(18) Uani 1 1 d . . . H25 H -0.0086 0.3227 0.8829 0.042 Uiso 1 1 calc R . . C26 C 0.1006(4) 0.3119(3) 0.9723(4) 0.0370(18) Uani 1 1 d . . . C27 C 0.0834(4) 0.3277(4) 1.0849(4) 0.045(2) Uani 1 1 d . . . H27A H 0.1250 0.2905 1.1033 0.054 Uiso 1 1 calc R . . H27B H 0.1124 0.3718 1.1012 0.054 Uiso 1 1 calc R . . C28 C 0.0119(5) 0.3196(3) 1.1111(5) 0.046(2) Uani 1 1 d . A . H28A H -0.0265 0.3593 1.0953 0.055 Uiso 1 1 calc R . . H28B H 0.0344 0.3199 1.1637 0.055 Uiso 1 1 calc R . . C29 C -0.0391(5) 0.2542(4) 1.0858(6) 0.069(3) Uani 1 1 d . . . C30A C -0.1020(5) 0.2383(5) 1.1130(8) 0.040(4) Uani 0.71(2) 1 d P A -1 H30A H -0.1343 0.2800 1.1150 0.048 Uiso 0.71(2) 1 calc PR A -1 H30B H -0.0759 0.2204 1.1619 0.048 Uiso 0.71(2) 1 calc PR A -1 C30B C -0.1161(17) 0.2446(13) 1.042(3) 0.068(14) Uani 0.29(2) 1 d P A -2 H30C H -0.1143 0.2367 0.9942 0.082 Uiso 0.29(2) 1 calc PR A -2 H30D H -0.1490 0.2869 1.0404 0.082 Uiso 0.29(2) 1 calc PR A -2 C31 C -0.1671(4) 0.1802(4) 1.0626(6) 0.073(3) Uani 1 1 d . . . C32 C -0.1191(4) 0.1184(4) 1.0460(5) 0.050(2) Uani 1 1 d . A . H32A H -0.0967 0.1314 1.0083 0.059 Uiso 1 1 calc R . . H32B H -0.0704 0.1066 1.0889 0.059 Uiso 1 1 calc R . . C33 C -0.1753(3) 0.0565(4) 1.0221(4) 0.0403(18) Uani 1 1 d . . . H33A H -0.1949 0.0418 1.0610 0.048 Uiso 1 1 calc R A . H33B H -0.2260 0.0692 0.9811 0.048 Uiso 1 1 calc R . . C34 C -0.1315(4) -0.0024(4) 1.0014(4) 0.046(2) Uani 1 1 d . A . H34A H -0.1693 -0.0428 0.9894 0.055 Uiso 1 1 calc R . . H34B H -0.1166 0.0097 0.9594 0.055 Uiso 1 1 calc R . . C41 C 0.2524(3) 0.0170(3) 0.6854(4) 0.0263(15) Uani 1 1 d . . . H41 H 0.2896 0.0471 0.6687 0.032 Uiso 1 1 calc R . . C42 C 0.1727(3) -0.0041(3) 0.6269(4) 0.0368(18) Uani 1 1 d . . . C43 C 0.0913(4) -0.0158(4) 0.6445(5) 0.054(2) Uani 1 1 d . . . H43A H 0.0501 0.0202 0.6224 0.081 Uiso 1 1 calc R . . H43B H 0.1051 -0.0146 0.6960 0.081 Uiso 1 1 calc R . . H43C H 0.0670 -0.0603 0.6261 0.081 Uiso 1 1 calc R . . C44 C 0.1592(4) 0.0211(4) 0.5535(4) 0.050(2) Uani 1 1 d . . . H44A H 0.1116 0.0532 0.5390 0.075 Uiso 1 1 calc R . . H44B H 0.1465 -0.0177 0.5206 0.075 Uiso 1 1 calc R . . H44C H 0.2105 0.0441 0.5528 0.075 Uiso 1 1 calc R . . C45 C 0.2460(3) -0.0565(3) 0.6562(4) 0.0345(18) Uani 1 1 d . . . H45 H 0.2794 -0.0648 0.6244 0.041 Uiso 1 1 calc R . . C46 C 0.2410(4) -0.1152(4) 0.6996(4) 0.0416(18) Uani 1 1 d . . . C47 C 0.3037(6) -0.2251(4) 0.7350(6) 0.072(3) Uani 1 1 d . . . H47A H 0.2581 -0.2579 0.7107 0.086 Uiso 1 1 calc R . . H47B H 0.2978 -0.2128 0.7809 0.086 Uiso 1 1 calc R . . C48 C 0.3862(6) -0.2582(6) 0.7487(8) 0.104(4) Uani 1 1 d . . . H48A H 0.3885 -0.2769 0.7037 0.125 Uiso 1 1 calc R . . H48B H 0.3918 -0.2968 0.7818 0.125 Uiso 1 1 calc R . . C49 C 0.4576(8) -0.2109(10) 0.7792(12) 0.192(10) Uani 1 1 d . . . H49A H 0.4494 -0.1746 0.7432 0.230 Uiso 1 1 calc R . . H49B H 0.4471 -0.1891 0.8198 0.230 Uiso 1 1 calc R . . C50 C 0.5433(11) -0.2248(8) 0.8033(9) 0.142(6) Uani 1 1 d . . . H50A H 0.5566 -0.2444 0.7629 0.170 Uiso 1 1 calc R . . H50B H 0.5537 -0.2612 0.8395 0.170 Uiso 1 1 calc R . . C51 C 0.6048(8) -0.1708(6) 0.8337(9) 0.109(5) Uani 1 1 d . . . H51A H 0.6620 -0.1914 0.8528 0.131 Uiso 1 1 calc R . . H51B H 0.5925 -0.1501 0.8740 0.131 Uiso 1 1 calc R . . C52 C 0.6059(7) -0.1145(6) 0.7817(7) 0.100(4) Uani 1 1 d . . . H52A H 0.5498 -0.0919 0.7647 0.120 Uiso 1 1 calc R . . H52B H 0.6153 -0.1353 0.7401 0.120 Uiso 1 1 calc R . . C53 C 0.6788(5) -0.0571(5) 0.8162(6) 0.073(3) Uani 1 1 d . . . H53A H 0.7294 -0.0804 0.8491 0.087 Uiso 1 1 calc R . . H53B H 0.6951 -0.0371 0.7775 0.087 Uiso 1 1 calc R . . C54 C 0.6563(5) -0.0015(4) 0.8544(5) 0.058(2) Uani 1 1 d . . . H54A H 0.6992 0.0353 0.8644 0.070 Uiso 1 1 calc R . . H54B H 0.6005 0.0178 0.8258 0.070 Uiso 1 1 calc R . . C61 C 0.5367(4) -0.0446(4) 1.0370(5) 0.047(2) Uani 1 1 d . . . H61 H 0.5365 -0.0916 1.0564 0.056 Uiso 1 1 calc R . . C62 C 0.6044(4) 0.0004(5) 1.0847(5) 0.057(3) Uani 1 1 d . . . C63 C 0.5857(5) 0.0745(6) 1.0899(6) 0.078(3) Uani 1 1 d . . . H63A H 0.6360 0.0973 1.1225 0.118 Uiso 1 1 calc R . . H63B H 0.5386 0.0792 1.1076 0.118 Uiso 1 1 calc R . . H63C H 0.5701 0.0956 1.0428 0.118 Uiso 1 1 calc R . . C64 C 0.6578(4) -0.0314(7) 1.1535(5) 0.099(4) Uani 1 1 d . . . H64A H 0.7000 0.0017 1.1812 0.148 Uiso 1 1 calc R . . H64B H 0.6867 -0.0717 1.1439 0.148 Uiso 1 1 calc R . . H64C H 0.6217 -0.0451 1.1803 0.148 Uiso 1 1 calc R . . C65 C 0.6154(3) -0.0289(4) 1.0204(5) 0.053(2) Uani 1 1 d . . . H65 H 0.6562 -0.0679 1.0317 0.063 Uiso 1 1 calc R . . C66 C 0.6173(4) 0.0115(5) 0.9572(5) 0.049(2) Uani 1 1 d . . . C81 C 0.1775(3) -0.0021(3) 1.1275(4) 0.0270(15) Uani 1 1 d . . . H81 H 0.2044 0.0230 1.1732 0.032 Uiso 1 1 calc R . . C82 C 0.1634(4) -0.0765(3) 1.1373(4) 0.0315(16) Uani 1 1 d . . . C83 C 0.1705(4) -0.1272(3) 1.0834(4) 0.0406(18) Uani 1 1 d . . . H83A H 0.1482 -0.1068 1.0359 0.061 Uiso 1 1 calc R . . H83B H 0.1377 -0.1682 1.0848 0.061 Uiso 1 1 calc R . . H83C H 0.2301 -0.1396 1.0943 0.061 Uiso 1 1 calc R . . C84 C 0.1955(4) -0.1016(4) 1.2135(4) 0.046(2) Uani 1 1 d . . . H84A H 0.1886 -0.0654 1.2447 0.069 Uiso 1 1 calc R . . H84B H 0.2556 -0.1136 1.2272 0.069 Uiso 1 1 calc R . . H84C H 0.1631 -0.1419 1.2176 0.069 Uiso 1 1 calc R . . C85 C 0.0883(3) -0.0287(3) 1.1174(4) 0.0263(15) Uani 1 1 d . . . H85 H 0.0689 -0.0176 1.1578 0.032 Uiso 1 1 calc R . . C86 C 0.0181(3) -0.0297(3) 1.0468(4) 0.0247(15) Uani 1 1 d . . . Ni2 Ni 0.80668(4) 0.38347(3) 0.61303(4) 0.02115(19) Uani 1 1 d . . . O121 O 0.8330(3) 0.1943(2) 0.4509(3) 0.0436(14) Uani 1 1 d . . . O122 O 0.8955(2) 0.0923(2) 0.4845(3) 0.0381(12) Uani 1 1 d . . . O141 O 0.9137(3) 0.5890(2) 0.7776(3) 0.0449(13) Uani 1 1 d . . . O142 O 0.8836(2) 0.6960(2) 0.7399(3) 0.0379(12) Uani 1 1 d . . . O161 O 0.6217(3) 0.5449(2) 0.4091(3) 0.0438(13) Uani 1 1 d . B . O162 O 0.5836(2) 0.6493(2) 0.4333(3) 0.0367(12) Uani 1 1 d . B . O181 O 0.8450(3) 0.1929(2) 0.8169(3) 0.0438(14) Uani 1 1 d . . . O182 O 0.8383(2) 0.0805(2) 0.7947(3) 0.0372(12) Uani 1 1 d . . . N101 N 0.8319(3) 0.2883(2) 0.6244(3) 0.0223(12) Uani 1 1 d . . . N102 N 0.9159(2) 0.4022(2) 0.6098(3) 0.0199(11) Uani 1 1 d . . . N103 N 0.7826(2) 0.4782(2) 0.6038(3) 0.0213(12) Uani 1 1 d . . . N104 N 0.6962(2) 0.3655(2) 0.6141(3) 0.0241(12) Uani 1 1 d . . . C101 C 0.7914(3) 0.2390(3) 0.6510(4) 0.0268(15) Uani 1 1 d . . . C102 C 0.8331(3) 0.1747(3) 0.6512(4) 0.0299(16) Uani 1 1 d . . . H102 H 0.8188 0.1325 0.6674 0.036 Uiso 1 1 calc R . . C103 C 0.8942(3) 0.1841(3) 0.6253(4) 0.0292(16) Uani 1 1 d . . . H103 H 0.9312 0.1501 0.6188 0.035 Uiso 1 1 calc R . . C104 C 0.8944(3) 0.2551(3) 0.6089(4) 0.0260(15) Uani 1 1 d . . . C105 C 0.9536(3) 0.2860(3) 0.5847(4) 0.0264(15) Uani 1 1 d . . . C106 C 0.9667(3) 0.3558(3) 0.5899(4) 0.0242(15) Uani 1 1 d . . . C107 C 1.0422(3) 0.3901(3) 0.5893(4) 0.0297(16) Uani 1 1 d . . . H107 H 1.0856 0.3710 0.5751 0.036 Uiso 1 1 calc R . . C108 C 1.0400(3) 0.4542(3) 0.6128(4) 0.0316(16) Uani 1 1 d . . . H108 H 1.0830 0.4877 0.6205 0.038 Uiso 1 1 calc R . . C109 C 0.9606(3) 0.4625(3) 0.6239(3) 0.0207(13) Uani 1 1 d . . . C110 C 0.9262(3) 0.5245(3) 0.6338(3) 0.0213(13) Uani 1 1 d . . . C111 C 0.8403(3) 0.5317(3) 0.6174(4) 0.0242(14) Uani 1 1 d . . . C112 C 0.7938(3) 0.5955(3) 0.6033(4) 0.0306(16) Uani 1 1 d . . . H112 H 0.8177 0.6399 0.6115 0.037 Uiso 1 1 calc R . . C113 C 0.7118(3) 0.5807(3) 0.5770(4) 0.0284(15) Uani 1 1 d . . . H113 H 0.6669 0.6128 0.5606 0.034 Uiso 1 1 calc R . . C114 C 0.7026(3) 0.5087(3) 0.5774(4) 0.0247(15) Uani 1 1 d . . . C115 C 0.6276(3) 0.4734(3) 0.5631(4) 0.0287(16) Uani 1 1 d . . . C116 C 0.6254(3) 0.4073(3) 0.5877(4) 0.0283(16) Uani 1 1 d . . . C117 C 0.5539(3) 0.3743(3) 0.5973(4) 0.043(2) Uani 1 1 d . . . H117 H 0.4976 0.3912 0.5824 0.051 Uiso 1 1 calc R . . C118 C 0.5810(4) 0.3158(3) 0.6305(4) 0.044(2) Uani 1 1 d . . . H118 H 0.5480 0.2843 0.6458 0.052 Uiso 1 1 calc R . . C119 C 0.6691(3) 0.3085(3) 0.6393(4) 0.0278(16) Uani 1 1 d . . . C120 C 0.7155(3) 0.2479(3) 0.6624(4) 0.0258(15) Uani 1 1 d . . . C121 C 1.0121(3) 0.2445(3) 0.5595(4) 0.0275(16) Uani 1 1 d . . . H121 H 1.0689 0.2376 0.5970 0.033 Uiso 1 1 calc R . . C122 C 1.0162(3) 0.2513(3) 0.4866(4) 0.0325(17) Uani 1 1 d . . . C123 C 0.9565(4) 0.2990(3) 0.4340(4) 0.0429(19) Uani 1 1 d . . . H12A H 0.9022 0.3000 0.4418 0.064 Uiso 1 1 calc R . . H12B H 0.9475 0.2829 0.3857 0.064 Uiso 1 1 calc R . . H12C H 0.9809 0.3450 0.4402 0.064 Uiso 1 1 calc R . . C124 C 1.1012(4) 0.2490(4) 0.4771(5) 0.0432(19) Uani 1 1 d . . . H12D H 1.1393 0.2185 0.5126 0.065 Uiso 1 1 calc R . . H12E H 1.1256 0.2951 0.4830 0.065 Uiso 1 1 calc R . . H12F H 1.0940 0.2321 0.4295 0.065 Uiso 1 1 calc R . . C125 C 0.9847(3) 0.1845(3) 0.5072(4) 0.0281(15) Uani 1 1 d . . . H125 H 1.0273 0.1467 0.5175 0.034 Uiso 1 1 calc R . . C126 C 0.8965(4) 0.1606(3) 0.4782(4) 0.0288(15) Uani 1 1 d . . . C127 C 0.8119(4) 0.0585(4) 0.4630(5) 0.047(2) Uani 1 1 d . . . H12G H 0.7908 0.0495 0.4113 0.056 Uiso 1 1 calc R . . H12H H 0.7705 0.0881 0.4741 0.056 Uiso 1 1 calc R . . C128 C 0.8229(4) -0.0076(4) 0.5034(4) 0.0425(19) Uani 1 1 d . . . H12I H 0.8687 -0.0344 0.4955 0.051 Uiso 1 1 calc R . . H12J H 0.7699 -0.0344 0.4845 0.051 Uiso 1 1 calc R . . C129 C 0.8442(4) 0.0030(3) 0.5828(4) 0.0357(17) Uani 1 1 d . . . H12K H 0.8979 0.0289 0.6012 0.043 Uiso 1 1 calc R . . H12L H 0.7994 0.0318 0.5898 0.043 Uiso 1 1 calc R . . C130 C 0.8533(4) -0.0604(3) 0.6272(5) 0.042(2) Uani 1 1 d . . . H13A H 0.9030 -0.0866 0.6258 0.051 Uiso 1 1 calc R . . H13B H 0.8025 -0.0893 0.6061 0.051 Uiso 1 1 calc R . . C131 C 0.8639(4) -0.0459(4) 0.7039(5) 0.043(2) Uani 1 1 d . . . H13C H 0.8566 -0.0890 0.7268 0.051 Uiso 1 1 calc R . . H13D H 0.8186 -0.0142 0.7051 0.051 Uiso 1 1 calc R . . C132 C 0.9490(4) -0.0151(4) 0.7467(5) 0.049(2) Uani 1 1 d . . . H13E H 0.9582 0.0261 0.7218 0.058 Uiso 1 1 calc R . . H13F H 0.9941 -0.0483 0.7485 0.058 Uiso 1 1 calc R . . C133 C 0.9579(4) 0.0045(4) 0.8224(4) 0.0422(19) Uani 1 1 d . . . H133 H 0.9800 -0.0262 0.8610 0.051 Uiso 1 1 calc R . . C134 C 0.9296(3) 0.0757(3) 0.8323(4) 0.0401(19) Uani 1 1 d . . . H13G H 0.9429 0.0851 0.8834 0.048 Uiso 1 1 calc R . . H13H H 0.9597 0.1096 0.8132 0.048 Uiso 1 1 calc R . . C141 C 0.9825(3) 0.5862(3) 0.6490(4) 0.0254(14) Uani 1 1 d . . . H141 H 0.9913 0.6052 0.6059 0.031 Uiso 1 1 calc R . . C142 C 1.0592(3) 0.5940(3) 0.7161(4) 0.0308(16) Uani 1 1 d . . . C143 C 1.0805(4) 0.5393(3) 0.7714(4) 0.0362(17) Uani 1 1 d . . . H14A H 1.1311 0.5146 0.7712 0.054 Uiso 1 1 calc R . . H14B H 1.0328 0.5074 0.7611 0.054 Uiso 1 1 calc R . . H14C H 1.0914 0.5599 0.8181 0.054 Uiso 1 1 calc R . . C144 C 1.1369(4) 0.6297(4) 0.7099(4) 0.0406(19) Uani 1 1 d . . . H14D H 1.1832 0.5967 0.7185 0.061 Uiso 1 1 calc R . . H14E H 1.1546 0.6666 0.7450 0.061 Uiso 1 1 calc R . . H14F H 1.1228 0.6489 0.6621 0.061 Uiso 1 1 calc R . . C145 C 0.9827(3) 0.6405(3) 0.7033(4) 0.0305(16) Uani 1 1 d . . . H145 H 0.9913 0.6880 0.6888 0.037 Uiso 1 1 calc R . . C146 C 0.9256(3) 0.6362(3) 0.7452(4) 0.0294(16) Uani 1 1 d . . . C147 C 0.8154(4) 0.6955(4) 0.7707(5) 0.049(2) Uani 1 1 d . B . H14G H 0.8398 0.6967 0.8232 0.059 Uiso 1 1 calc R . . H14H H 0.7802 0.6539 0.7560 0.059 Uiso 1 1 calc R . . C148 C 0.7618(5) 0.7595(5) 0.7425(5) 0.060(3) Uani 1 1 d . . . C49A C 0.7205(9) 0.7417(8) 0.6591(8) 0.069(6) Uani 0.69(2) 1 d P B -1 H14I H 0.7657 0.7438 0.6381 0.082 Uiso 0.69(2) 1 calc PR B -1 H14J H 0.6994 0.6941 0.6542 0.082 Uiso 0.69(2) 1 calc PR B -1 C49B C 0.7317(10) 0.7921(10) 0.6735(11) 0.022(7) Uani 0.31(2) 1 d P B -2 H14K H 0.7373 0.8417 0.6834 0.026 Uiso 0.31(2) 1 calc PR B -2 H14L H 0.7744 0.7809 0.6515 0.026 Uiso 0.31(2) 1 calc PR B -2 C150 C 0.6540(6) 0.7844(9) 0.6197(7) 0.128(6) Uani 1 1 d . . . C151 C 0.6192(4) 0.7700(4) 0.5408(5) 0.050(2) Uani 1 1 d . B . H15A H 0.5912 0.7248 0.5331 0.060 Uiso 1 1 calc R . . H15B H 0.5753 0.8046 0.5176 0.060 Uiso 1 1 calc R . . C152 C 0.6834(4) 0.7706(4) 0.5057(5) 0.056(3) Uani 1 1 d . . . H15C H 0.7281 0.7372 0.5303 0.068 Uiso 1 1 calc R B . H15D H 0.7102 0.8163 0.5127 0.068 Uiso 1 1 calc R . . C153 C 0.6529(4) 0.7547(4) 0.4276(5) 0.046(2) Uani 1 1 d . B . H15E H 0.6915 0.7772 0.4067 0.055 Uiso 1 1 calc R . . H15F H 0.5961 0.7752 0.4052 0.055 Uiso 1 1 calc R . . C154 C 0.6474(4) 0.6789(3) 0.4084(5) 0.044(2) Uani 1 1 d . . . H15G H 0.6309 0.6731 0.3564 0.053 Uiso 1 1 calc R B . H15H H 0.7029 0.6565 0.4316 0.053 Uiso 1 1 calc R . . C161 C 0.5434(3) 0.5095(3) 0.5314(4) 0.0340(17) Uani 1 1 d . . . H161 H 0.5161 0.5208 0.5670 0.041 Uiso 1 1 calc R . . C162 C 0.4807(3) 0.4886(4) 0.4598(4) 0.0405(19) Uani 1 1 d . . . C163 C 0.5054(4) 0.4340(4) 0.4179(5) 0.053(2) Uani 1 1 d . . . H16A H 0.5661 0.4376 0.4258 0.079 Uiso 1 1 calc R . . H16B H 0.4729 0.4400 0.3673 0.079 Uiso 1 1 calc R . . H16C H 0.4932 0.3890 0.4332 0.079 Uiso 1 1 calc R . . C164 C 0.3862(4) 0.4880(5) 0.4534(5) 0.062(3) Uani 1 1 d . . . H16D H 0.3653 0.4409 0.4480 0.093 Uiso 1 1 calc R . . H16E H 0.3529 0.5147 0.4118 0.093 Uiso 1 1 calc R . . H16F H 0.3805 0.5080 0.4962 0.093 Uiso 1 1 calc R . . C165 C 0.5199(3) 0.5593(4) 0.4685(4) 0.0361(17) Uani 1 1 d . B . H165 H 0.4806 0.5966 0.4714 0.043 Uiso 1 1 calc R . . C166 C 0.5805(3) 0.5803(3) 0.4335(4) 0.0338(17) Uani 1 1 d . . . C181 C 0.6718(3) 0.1899(3) 0.6833(4) 0.0294(16) Uani 1 1 d . . . H181 H 0.6284 0.1674 0.6418 0.035 Uiso 1 1 calc R . . C182 C 0.6476(3) 0.1896(3) 0.7495(4) 0.0323(17) Uani 1 1 d . . . C183 C 0.6726(5) 0.2473(4) 0.8033(5) 0.056(2) Uani 1 1 d . . . H18A H 0.6509 0.2378 0.8417 0.084 Uiso 1 1 calc R . . H18B H 0.6485 0.2903 0.7800 0.084 Uiso 1 1 calc R . . H18C H 0.7345 0.2511 0.8229 0.084 Uiso 1 1 calc R . . C184 C 0.5619(4) 0.1583(4) 0.7415(5) 0.050(2) Uani 1 1 d . . . H18D H 0.5525 0.1611 0.7869 0.075 Uiso 1 1 calc R . . H18E H 0.5610 0.1104 0.7273 0.075 Uiso 1 1 calc R . . H18F H 0.5170 0.1834 0.7053 0.075 Uiso 1 1 calc R . . C185 C 0.7136(3) 0.1399(3) 0.7449(4) 0.0320(17) Uani 1 1 d . . . H185 H 0.6921 0.0921 0.7347 0.038 Uiso 1 1 calc R . . C186 C 0.8041(3) 0.1440(3) 0.7906(4) 0.0306(16) Uani 1 1 d . . . O201 O 0.661(3) 0.3317(14) 1.0455(18) 0.32(3) Uani 0.50 1 d P . . O202 O 0.3954(8) 0.2070(7) 0.9724(9) 0.097(5) Uani 0.50 1 d P . . O203 O 0.5297(7) 0.2535(7) 0.9249(11) 0.126(8) Uani 0.50 1 d P . . O204 O 0.3845(6) 0.1991(7) 0.8249(7) 0.072(4) Uani 0.50 1 d P . . N201 N 0.5927(15) 0.1544(10) 0.4489(18) 0.160(14) Uani 0.50 1 d P . . C201 C 0.6247(7) 0.2076(6) 0.4572(7) 0.029(2) Uani 0.50 1 d P . . C202 C 0.6636(7) 0.2743(6) 0.4592(8) 0.029(2) Uani 0.50 1 d P . . H20A H 0.7149 0.2775 0.5014 0.043 Uiso 0.50 1 calc PR . . H20B H 0.6235 0.3100 0.4609 0.043 Uiso 0.50 1 calc PR . . H20C H 0.6786 0.2804 0.4166 0.043 Uiso 0.50 1 calc PR . . 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 0.0193(3) 0.0281(4) 0.0266(6) 0.0012(4) 0.0089(3) 0.0048(3) O21 0.040(3) 0.060(3) 0.053(4) -0.002(3) 0.005(2) -0.002(2) O22 0.054(3) 0.037(3) 0.024(4) -0.003(2) 0.009(2) 0.013(2) O41 0.077(3) 0.058(3) 0.068(5) 0.004(3) 0.041(3) -0.006(3) O42 0.053(3) 0.040(3) 0.074(5) 0.003(3) 0.022(3) -0.001(2) O61 0.048(3) 0.058(4) 0.066(5) -0.005(3) 0.018(3) 0.006(2) O62 0.032(2) 0.058(3) 0.045(4) -0.001(3) 0.013(2) 0.006(2) O81 0.039(2) 0.032(2) 0.027(3) -0.004(2) 0.014(2) -0.0031(17) O82 0.027(2) 0.043(3) 0.037(4) -0.003(2) 0.0100(18) 0.0012(18) N1 0.022(2) 0.021(2) 0.023(4) 0.006(2) 0.0115(19) 0.0031(17) N2 0.022(2) 0.031(3) 0.019(4) -0.002(2) 0.0111(19) 0.0001(18) N3 0.021(2) 0.035(3) 0.026(4) 0.001(2) 0.008(2) 0.0087(19) N4 0.023(2) 0.044(3) 0.017(4) -0.002(2) 0.014(2) -0.001(2) C1 0.024(2) 0.024(3) 0.019(4) -0.001(2) 0.010(2) 0.000(2) C2 0.027(3) 0.026(3) 0.027(5) -0.002(3) 0.013(2) 0.004(2) C3 0.023(3) 0.019(3) 0.043(5) -0.004(3) 0.009(3) 0.003(2) C4 0.018(2) 0.017(3) 0.026(4) 0.000(3) 0.006(2) 0.003(2) C5 0.023(3) 0.021(3) 0.027(5) -0.001(3) 0.006(2) -0.002(2) C6 0.027(3) 0.031(3) 0.019(5) 0.010(3) 0.008(2) 0.003(2) C7 0.037(3) 0.030(3) 0.035(5) 0.008(3) 0.012(3) 0.008(3) C8 0.037(3) 0.042(4) 0.026(5) 0.004(3) 0.014(3) 0.008(3) C9 0.025(3) 0.030(3) 0.023(5) -0.004(3) 0.009(2) -0.002(2) C10 0.021(3) 0.029(3) 0.035(5) 0.000(3) 0.012(2) -0.004(2) C11 0.026(3) 0.032(3) 0.036(5) -0.002(3) 0.012(3) -0.004(2) C12 0.025(3) 0.046(4) 0.030(5) -0.014(3) 0.011(3) 0.002(2) C13 0.021(3) 0.047(4) 0.037(5) -0.003(3) 0.011(3) 0.010(2) C14 0.021(3) 0.038(3) 0.026(5) 0.001(3) 0.009(2) 0.004(2) C15 0.024(3) 0.040(4) 0.042(6) -0.001(3) 0.012(3) 0.007(2) C16 0.028(3) 0.049(4) 0.020(5) 0.007(3) 0.007(3) 0.008(3) C17 0.034(3) 0.074(5) 0.028(5) 0.012(4) 0.009(3) 0.025(3) C18 0.031(3) 0.057(5) 0.052(6) 0.014(4) 0.011(3) 0.015(3) C19 0.026(3) 0.032(3) 0.041(5) 0.006(3) 0.005(3) 0.002(2) C20 0.025(3) 0.030(3) 0.030(5) -0.002(3) 0.015(2) 0.004(2) C21 0.027(3) 0.023(3) 0.027(4) -0.001(3) 0.007(2) 0.002(2) C22 0.047(3) 0.020(3) 0.019(4) 0.002(3) 0.010(3) 0.003(2) C23 0.059(4) 0.042(4) 0.055(7) 0.003(4) 0.024(4) -0.020(3) C24 0.077(5) 0.035(4) 0.037(6) 0.020(4) 0.016(4) 0.005(3) C25 0.039(3) 0.024(3) 0.036(5) 0.006(3) 0.005(3) 0.006(2) C26 0.055(4) 0.018(3) 0.037(5) -0.001(3) 0.014(3) 0.004(3) C27 0.064(4) 0.034(4) 0.034(6) 0.000(3) 0.011(4) 0.004(3) C28 0.071(5) 0.030(4) 0.035(6) 0.004(3) 0.018(4) 0.003(3) C29 0.052(4) 0.034(4) 0.112(9) 0.002(5) 0.016(5) -0.002(3) C30A 0.042(5) 0.032(5) 0.050(11) 0.003(5) 0.019(5) 0.012(4) C30B 0.073(19) 0.024(13) 0.09(4) 0.011(16) 0.014(18) -0.011(12) C31 0.041(4) 0.037(4) 0.135(10) -0.006(5) 0.022(5) 0.007(3) C32 0.031(3) 0.041(4) 0.075(7) 0.005(4) 0.017(3) 0.007(3) C33 0.024(3) 0.044(4) 0.047(5) 0.008(4) 0.006(3) -0.002(3) C34 0.029(3) 0.056(5) 0.045(6) -0.003(4) 0.004(3) -0.003(3) C41 0.021(3) 0.035(3) 0.025(5) -0.006(3) 0.010(2) -0.003(2) C42 0.031(3) 0.039(4) 0.038(5) -0.015(3) 0.008(3) -0.001(3) C43 0.025(3) 0.064(5) 0.074(7) -0.032(5) 0.018(3) -0.011(3) C44 0.050(4) 0.072(5) 0.024(6) -0.009(4) 0.009(3) 0.013(4) C45 0.025(3) 0.047(4) 0.035(5) -0.007(3) 0.014(3) 0.005(3) C46 0.039(3) 0.046(4) 0.042(6) -0.011(4) 0.017(3) -0.008(3) C47 0.094(6) 0.046(5) 0.078(9) 0.008(5) 0.033(6) -0.006(5) C48 0.087(7) 0.078(8) 0.142(13) 0.035(8) 0.032(7) 0.020(6) C49 0.075(9) 0.171(17) 0.28(3) 0.005(17) 0.007(11) 0.029(10) C50 0.219(18) 0.133(14) 0.074(13) -0.024(9) 0.052(11) -0.034(13) C51 0.126(9) 0.074(8) 0.161(16) -0.025(9) 0.093(9) -0.007(7) C52 0.130(9) 0.092(8) 0.072(9) -0.014(8) 0.029(7) 0.056(8) C53 0.051(5) 0.107(8) 0.072(9) 0.011(6) 0.036(5) 0.014(5) C54 0.049(4) 0.063(5) 0.062(8) 0.004(5) 0.019(4) 0.002(4) C61 0.028(3) 0.061(5) 0.049(6) 0.007(4) 0.012(3) 0.017(3) C62 0.021(3) 0.108(7) 0.036(6) -0.025(5) 0.003(3) 0.003(3) C63 0.048(4) 0.113(9) 0.072(8) -0.045(6) 0.017(4) -0.030(5) C64 0.025(4) 0.201(13) 0.062(8) -0.013(8) 0.004(4) 0.021(5) C65 0.017(3) 0.073(5) 0.061(7) 0.005(5) 0.005(3) 0.008(3) C66 0.023(3) 0.079(6) 0.041(6) -0.003(5) 0.007(3) 0.004(3) C81 0.028(3) 0.027(3) 0.025(5) 0.003(3) 0.008(2) 0.006(2) C82 0.035(3) 0.034(3) 0.032(5) 0.010(3) 0.021(3) 0.010(2) C83 0.051(4) 0.031(4) 0.044(6) 0.002(3) 0.020(3) 0.009(3) C84 0.052(4) 0.047(5) 0.042(6) 0.018(4) 0.020(3) 0.013(3) C85 0.033(3) 0.024(3) 0.025(5) 0.006(3) 0.015(3) 0.007(2) C86 0.030(3) 0.017(3) 0.027(5) -0.004(3) 0.011(3) 0.001(2) Ni2 0.0194(3) 0.0182(3) 0.0262(5) 0.0005(3) 0.0083(3) -0.0005(3) O121 0.040(2) 0.035(3) 0.055(4) 0.003(2) 0.016(2) 0.005(2) O122 0.038(2) 0.027(2) 0.055(4) 0.000(2) 0.023(2) -0.0011(17) O141 0.053(3) 0.039(3) 0.052(4) 0.007(3) 0.029(2) 0.002(2) O142 0.045(2) 0.030(2) 0.044(4) -0.008(2) 0.022(2) -0.0011(18) O161 0.042(2) 0.042(3) 0.054(4) -0.003(3) 0.025(2) 0.002(2) O162 0.036(2) 0.034(2) 0.043(4) 0.006(2) 0.018(2) 0.0032(18) O181 0.039(2) 0.038(3) 0.048(4) -0.007(2) 0.008(2) -0.012(2) O182 0.029(2) 0.034(2) 0.045(4) 0.002(2) 0.0089(19) -0.0033(17) N101 0.025(2) 0.023(2) 0.023(4) -0.002(2) 0.013(2) -0.0043(18) N102 0.023(2) 0.022(2) 0.015(3) 0.004(2) 0.0074(18) 0.0004(17) N103 0.021(2) 0.018(2) 0.027(4) 0.000(2) 0.0111(19) -0.0006(17) N104 0.022(2) 0.022(3) 0.027(4) -0.002(2) 0.008(2) -0.0048(17) C101 0.030(3) 0.017(3) 0.032(5) -0.002(3) 0.008(3) -0.002(2) C102 0.040(3) 0.019(3) 0.033(5) 0.003(3) 0.015(3) 0.001(2) C103 0.039(3) 0.024(3) 0.031(5) 0.003(3) 0.020(3) 0.003(2) C104 0.027(3) 0.021(3) 0.029(5) -0.005(3) 0.009(2) 0.001(2) C105 0.023(3) 0.022(3) 0.033(5) 0.002(3) 0.008(2) 0.001(2) C106 0.025(3) 0.024(3) 0.025(5) -0.001(3) 0.010(2) -0.001(2) C107 0.029(3) 0.025(3) 0.042(5) -0.006(3) 0.021(3) -0.003(2) C108 0.021(3) 0.033(3) 0.040(5) 0.002(3) 0.010(3) -0.005(2) C109 0.024(2) 0.024(3) 0.013(4) 0.003(3) 0.005(2) -0.004(2) C110 0.025(2) 0.023(3) 0.014(4) 0.004(3) 0.005(2) -0.001(2) C111 0.030(3) 0.020(3) 0.022(4) -0.002(3) 0.008(2) -0.004(2) C112 0.035(3) 0.020(3) 0.033(5) -0.003(3) 0.007(3) -0.001(2) C113 0.036(3) 0.021(3) 0.032(5) 0.002(3) 0.016(3) 0.006(2) C114 0.025(3) 0.023(3) 0.029(5) 0.002(3) 0.012(2) 0.004(2) C115 0.025(3) 0.027(3) 0.036(5) 0.001(3) 0.012(3) 0.001(2) C116 0.019(2) 0.030(3) 0.033(5) 0.002(3) 0.006(2) 0.001(2) C117 0.024(3) 0.036(4) 0.069(6) 0.022(4) 0.018(3) 0.009(3) C118 0.030(3) 0.040(4) 0.068(7) 0.016(4) 0.026(3) -0.005(3) C119 0.029(3) 0.029(3) 0.029(5) -0.002(3) 0.015(3) -0.003(2) C120 0.025(3) 0.024(3) 0.027(5) 0.001(3) 0.006(2) -0.005(2) C121 0.025(3) 0.025(3) 0.032(5) -0.001(3) 0.011(3) 0.003(2) C122 0.034(3) 0.026(3) 0.042(6) -0.008(3) 0.018(3) 0.002(2) C123 0.061(4) 0.033(4) 0.042(6) 0.012(3) 0.027(4) 0.001(3) C124 0.051(4) 0.040(4) 0.051(6) -0.014(4) 0.033(3) -0.007(3) C125 0.033(3) 0.027(3) 0.032(5) 0.007(3) 0.021(3) 0.005(2) C126 0.037(3) 0.028(3) 0.029(5) 0.003(3) 0.019(3) 0.004(2) C127 0.038(3) 0.047(4) 0.057(6) 0.002(4) 0.020(3) -0.011(3) C128 0.047(4) 0.038(4) 0.050(6) -0.013(4) 0.026(3) -0.013(3) C129 0.037(3) 0.035(4) 0.036(5) -0.007(3) 0.013(3) -0.006(3) C130 0.048(4) 0.026(3) 0.056(7) -0.001(3) 0.022(4) -0.010(3) C131 0.050(4) 0.034(4) 0.046(6) 0.006(4) 0.020(3) -0.009(3) C132 0.044(4) 0.044(4) 0.064(7) 0.000(4) 0.026(4) 0.004(3) C133 0.052(4) 0.042(4) 0.027(5) 0.014(3) 0.008(3) 0.011(3) C134 0.029(3) 0.038(4) 0.045(5) 0.007(3) 0.001(3) -0.003(2) C141 0.032(3) 0.021(3) 0.021(4) 0.003(3) 0.005(2) -0.004(2) C142 0.032(3) 0.036(3) 0.026(5) -0.005(3) 0.011(3) -0.011(2) C143 0.043(3) 0.041(4) 0.020(5) 0.000(3) 0.006(3) 0.000(3) C144 0.038(3) 0.048(4) 0.036(5) -0.005(4) 0.014(3) -0.020(3) C145 0.036(3) 0.026(3) 0.030(5) -0.001(3) 0.013(3) -0.006(2) C146 0.034(3) 0.028(3) 0.024(5) -0.007(3) 0.007(3) -0.006(2) C147 0.050(4) 0.046(4) 0.060(7) -0.019(4) 0.031(4) -0.001(3) C148 0.055(4) 0.081(6) 0.046(7) 0.009(5) 0.019(4) 0.031(4) C49A 0.087(9) 0.057(11) 0.076(13) 0.017(8) 0.046(8) 0.030(7) C49B 0.027(9) 0.011(11) 0.029(15) -0.005(8) 0.012(8) -0.001(7) C150 0.050(5) 0.264(19) 0.071(11) -0.003(10) 0.023(5) 0.028(8) C151 0.030(3) 0.048(4) 0.067(7) -0.001(4) 0.010(4) 0.008(3) C152 0.039(4) 0.062(5) 0.074(8) -0.018(5) 0.028(4) -0.004(3) C153 0.033(3) 0.043(4) 0.063(7) 0.023(4) 0.017(3) 0.011(3) C154 0.030(3) 0.042(4) 0.063(6) 0.002(4) 0.020(3) -0.006(3) C161 0.025(3) 0.033(3) 0.046(5) 0.010(3) 0.016(3) 0.001(2) C162 0.020(3) 0.045(4) 0.051(6) 0.003(4) 0.005(3) -0.003(3) C163 0.038(4) 0.048(4) 0.063(7) -0.014(4) 0.006(4) -0.006(3) C164 0.032(3) 0.067(5) 0.081(8) 0.012(5) 0.014(4) -0.006(3) C165 0.026(3) 0.040(4) 0.043(5) 0.004(4) 0.012(3) 0.002(3) C166 0.028(3) 0.038(4) 0.031(5) 0.011(3) 0.005(3) 0.003(3) C181 0.027(3) 0.026(3) 0.030(5) 0.002(3) 0.004(3) -0.008(2) C182 0.035(3) 0.034(3) 0.033(5) 0.003(3) 0.018(3) -0.009(3) C183 0.055(4) 0.046(4) 0.076(8) -0.013(5) 0.035(4) -0.007(3) C184 0.033(3) 0.049(4) 0.073(7) 0.010(4) 0.025(3) -0.007(3) C185 0.028(3) 0.024(3) 0.046(5) 0.006(3) 0.015(3) -0.008(2) C186 0.035(3) 0.028(3) 0.030(5) 0.006(3) 0.014(3) -0.006(3) O201 0.70(7) 0.16(2) 0.25(4) 0.14(2) 0.35(4) 0.30(3) O202 0.100(9) 0.074(10) 0.090(13) -0.003(8) -0.002(8) 0.000(7) O203 0.052(7) 0.085(10) 0.26(2) -0.076(12) 0.075(10) -0.031(6) O204 0.041(5) 0.104(10) 0.087(11) -0.046(8) 0.044(6) -0.027(5) N201 0.19(2) 0.070(12) 0.33(4) 0.022(17) 0.23(3) -0.011(13) C201 0.035(4) 0.037(5) 0.023(7) 0.000(4) 0.022(4) 0.008(3) C202 0.035(4) 0.037(5) 0.023(7) 0.000(4) 0.022(4) 0.008(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 N1 1.903(5) . ? Ni1 N4 1.909(5) . ? Ni1 N3 1.917(5) . ? Ni1 N2 1.933(5) . ? O21 C26 1.226(7) . ? O22 C26 1.316(9) . ? O22 C27 1.487(9) . ? O41 C46 1.193(9) . ? O42 C46 1.353(9) . ? O42 C47 1.434(10) . ? O61 C66 1.199(9) . ? O62 C66 1.385(9) . ? O62 C54 1.428(10) . ? O81 C86 1.172(8) . ? O82 C86 1.391(7) . ? O82 C34 1.444(8) . ? N1 C1 1.372(8) . ? N1 C4 1.390(7) . ? N2 C9 1.361(8) . ? N2 C6 1.368(7) . ? N3 C14 1.369(7) . ? N3 C11 1.384(9) . ? N4 C19 1.361(9) . ? N4 C16 1.363(7) . ? C1 C20 1.409(8) . ? C1 C2 1.461(7) . ? C2 C3 1.334(9) . ? C3 C4 1.425(9) . ? C4 C5 1.364(9) . ? C5 C6 1.407(9) . ? C5 C21 1.509(8) . ? C6 C7 1.416(9) . ? C7 C8 1.349(9) . ? C8 C9 1.432(9) . ? C9 C10 1.394(8) . ? C10 C11 1.417(9) . ? C10 C41 1.493(10) . ? C11 C12 1.425(8) . ? C12 C13 1.330(10) . ? C13 C14 1.430(9) . ? C14 C15 1.387(10) . ? C15 C16 1.397(9) . ? C15 C61 1.538(8) . ? C16 C17 1.434(10) . ? C17 C18 1.369(10) . ? C18 C19 1.431(10) . ? C19 C20 1.405(8) . ? C20 C81 1.470(9) . ? C21 C22 1.487(8) . ? C21 C25 1.514(9) . ? C22 C23 1.495(9) . ? C22 C25 1.506(10) . ? C22 C24 1.523(9) . ? C25 C26 1.482(10) . ? C27 C28 1.480(11) . ? C28 C29 1.529(10) . ? C29 C30B 1.30(3) . ? C29 C30A 1.385(14) . ? C30A C31 1.659(14) . ? C30B C31 1.65(3) . ? C31 C32 1.555(10) . ? C32 C33 1.510(9) . ? C33 C34 1.504(10) . ? C41 C42 1.502(8) . ? C41 C45 1.544(9) . ? C42 C44 1.497(11) . ? C42 C43 1.546(9) . ? C42 C45 1.555(9) . ? C45 C46 1.463(11) . ? C47 C48 1.468(13) . ? C48 C49 1.471(19) . ? C49 C50 1.381(18) . ? C50 C51 1.458(17) . ? C51 C52 1.524(18) . ? C52 C53 1.630(15) . ? C53 C54 1.456(13) . ? C61 C62 1.495(11) . ? C61 C65 1.505(10) . ? C62 C65 1.483(12) . ? C62 C64 1.497(14) . ? C62 C63 1.497(13) . ? C65 C66 1.506(12) . ? C81 C82 1.500(8) . ? C81 C85 1.534(8) . ? C82 C83 1.505(10) . ? C82 C85 1.510(7) . ? C82 C84 1.518(10) . ? C85 C86 1.499(9) . ? Ni2 N103 1.894(4) . ? Ni2 N102 1.898(4) . ? Ni2 N104 1.900(4) . ? Ni2 N101 1.907(5) . ? O121 C126 1.212(7) . ? O122 C126 1.345(7) . ? O122 C127 1.477(7) . ? O141 C146 1.188(8) . ? O142 C146 1.353(7) . ? O142 C147 1.483(8) . ? O161 C166 1.200(8) . ? O162 C166 1.353(8) . ? O162 C154 1.453(8) . ? O181 C186 1.192(7) . ? O182 C186 1.359(7) . ? O182 C134 1.461(6) . ? N101 C104 1.361(7) . ? N101 C101 1.392(8) . ? N102 C109 1.376(7) . ? N102 C106 1.398(7) . ? N103 C111 1.389(7) . ? N103 C114 1.399(6) . ? N104 C119 1.367(8) . ? N104 C116 1.390(7) . ? C101 C120 1.385(8) . ? C101 C102 1.441(8) . ? C102 C103 1.317(9) . ? C103 C104 1.431(8) . ? C104 C105 1.390(8) . ? C105 C106 1.383(8) . ? C105 C121 1.493(8) . ? C106 C107 1.440(7) . ? C107 C108 1.345(8) . ? C108 C109 1.440(8) . ? C109 C110 1.388(8) . ? C110 C111 1.373(7) . ? C110 C141 1.501(7) . ? C111 C112 1.449(8) . ? C112 C113 1.327(8) . ? C113 C114 1.420(8) . ? C114 C115 1.380(7) . ? C115 C116 1.391(8) . ? C115 C161 1.512(8) . ? C116 C117 1.435(8) . ? C117 C118 1.324(9) . ? C118 C119 1.439(8) . ? C119 C120 1.407(8) . ? C120 C181 1.491(8) . ? C121 C122 1.497(10) . ? C121 C125 1.539(9) . ? C122 C123 1.504(10) . ? C122 C124 1.509(8) . ? C122 C125 1.522(9) . ? C125 C126 1.470(8) . ? C127 C128 1.504(10) . ? C128 C129 1.525(11) . ? C129 C130 1.505(10) . ? C130 C131 1.516(11) . ? C131 C132 1.515(9) . ? C132 C133 1.527(12) . ? C133 C134 1.508(10) . ? C141 C142 1.517(9) . ? C141 C145 1.523(9) . ? C142 C143 1.496(9) . ? C142 C145 1.524(8) . ? C142 C144 1.525(8) . ? C145 C146 1.484(9) . ? C147 C148 1.532(11) . ? C148 C49B 1.45(2) . ? C148 C49A 1.614(18) . ? C49A C150 1.402(17) . ? C49B C150 1.39(2) . ? C150 C151 1.514(15) . ? C151 C152 1.482(11) . ? C152 C153 1.504(12) . ? C153 C154 1.529(10) . ? C161 C162 1.515(10) . ? C161 C165 1.535(10) . ? C162 C163 1.506(11) . ? C162 C165 1.518(9) . ? C162 C164 1.551(8) . ? C165 C166 1.484(9) . ? C181 C182 1.520(10) . ? C181 C185 1.542(9) . ? C182 C185 1.503(9) . ? C182 C183 1.520(10) . ? C182 C184 1.524(8) . ? C185 C186 1.482(8) . ? N201 C201 1.16(2) . ? C201 C202 1.455(17) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Ni1 N4 89.9(2) . . ? N1 Ni1 N3 178.6(2) . . ? N4 Ni1 N3 89.7(2) . . ? N1 Ni1 N2 90.3(2) . . ? N4 Ni1 N2 178.2(2) . . ? N3 Ni1 N2 90.2(2) . . ? C26 O22 C27 117.7(5) . . ? C46 O42 C47 118.3(7) . . ? C66 O62 C54 116.3(6) . . ? C86 O82 C34 117.2(6) . . ? C1 N1 C4 106.2(5) . . ? C1 N1 Ni1 126.4(3) . . ? C4 N1 Ni1 127.3(4) . . ? C9 N2 C6 107.6(5) . . ? C9 N2 Ni1 126.6(4) . . ? C6 N2 Ni1 125.8(4) . . ? C14 N3 C11 105.3(5) . . ? C14 N3 Ni1 128.4(5) . . ? C11 N3 Ni1 126.1(4) . . ? C19 N4 C16 106.1(5) . . ? C19 N4 Ni1 127.2(4) . . ? C16 N4 Ni1 126.8(4) . . ? N1 C1 C20 126.8(5) . . ? N1 C1 C2 109.7(5) . . ? C20 C1 C2 123.0(6) . . ? C3 C2 C1 105.8(6) . . ? C2 C3 C4 109.4(5) . . ? C5 C4 N1 125.0(5) . . ? C5 C4 C3 126.0(5) . . ? N1 C4 C3 108.7(5) . . ? C4 C5 C6 121.4(5) . . ? C4 C5 C21 121.3(5) . . ? C6 C5 C21 116.3(6) . . ? N2 C6 C5 125.3(6) . . ? N2 C6 C7 109.3(6) . . ? C5 C6 C7 124.9(5) . . ? C8 C7 C6 107.0(6) . . ? C7 C8 C9 107.8(7) . . ? N2 C9 C10 126.4(6) . . ? N2 C9 C8 108.2(5) . . ? C10 C9 C8 124.9(7) . . ? C9 C10 C11 119.7(7) . . ? C9 C10 C41 120.4(6) . . ? C11 C10 C41 119.0(5) . . ? N3 C11 C10 125.2(6) . . ? N3 C11 C12 110.2(5) . . ? C10 C11 C12 124.3(7) . . ? C13 C12 C11 106.7(7) . . ? C12 C13 C14 108.2(5) . . ? N3 C14 C15 123.6(6) . . ? N3 C14 C13 109.5(6) . . ? C15 C14 C13 126.6(5) . . ? C14 C15 C16 121.3(5) . . ? C14 C15 C61 122.2(6) . . ? C16 C15 C61 115.2(7) . . ? N4 C16 C15 124.9(6) . . ? N4 C16 C17 110.1(5) . . ? C15 C16 C17 123.9(5) . . ? C18 C17 C16 106.9(6) . . ? C17 C18 C19 105.8(8) . . ? N4 C19 C20 126.5(6) . . ? N4 C19 C18 111.0(5) . . ? C20 C19 C18 121.9(7) . . ? C19 C20 C1 117.8(6) . . ? C19 C20 C81 119.0(6) . . ? C1 C20 C81 122.9(5) . . ? C22 C21 C5 123.7(5) . . ? C22 C21 C25 60.2(4) . . ? C5 C21 C25 126.8(5) . . ? C21 C22 C23 120.8(5) . . ? C21 C22 C25 60.8(4) . . ? C23 C22 C25 119.9(6) . . ? C21 C22 C24 116.8(5) . . ? C23 C22 C24 114.1(6) . . ? C25 C22 C24 114.3(6) . . ? C26 C25 C22 124.7(6) . . ? C26 C25 C21 123.7(5) . . ? C22 C25 C21 59.0(4) . . ? O21 C26 O22 125.5(7) . . ? O21 C26 C25 126.2(7) . . ? O22 C26 C25 108.3(6) . . ? C28 C27 O22 107.6(6) . . ? C27 C28 C29 113.8(7) . . ? C30B C29 C30A 61.0(19) . . ? C30B C29 C28 131.2(13) . . ? C30A C29 C28 118.3(9) . . ? C29 C30A C31 110.2(10) . . ? C29 C30B C31 115(3) . . ? C32 C31 C30A 112.5(6) . . ? C32 C31 C30B 100.8(14) . . ? C30A C31 C30B 48.6(15) . . ? C33 C32 C31 112.2(5) . . ? C34 C33 C32 113.0(5) . . ? O82 C34 C33 107.6(6) . . ? C10 C41 C42 123.8(5) . . ? C10 C41 C45 123.0(6) . . ? C42 C41 C45 61.4(4) . . ? C44 C42 C41 118.0(6) . . ? C44 C42 C43 115.5(6) . . ? C41 C42 C43 118.9(7) . . ? C44 C42 C45 114.8(6) . . ? C41 C42 C45 60.6(4) . . ? C43 C42 C45 117.7(6) . . ? C46 C45 C41 121.1(7) . . ? C46 C45 C42 122.9(6) . . ? C41 C45 C42 58.0(4) . . ? O41 C46 O42 122.4(8) . . ? O41 C46 C45 128.6(7) . . ? O42 C46 C45 109.0(6) . . ? O42 C47 C48 112.7(8) . . ? C47 C48 C49 112.5(11) . . ? C50 C49 C48 128.7(16) . . ? C49 C50 C51 120.5(16) . . ? C50 C51 C52 114.4(14) . . ? C51 C52 C53 113.2(10) . . ? C54 C53 C52 116.4(7) . . ? O62 C54 C53 107.0(8) . . ? C62 C61 C65 59.3(5) . . ? C62 C61 C15 120.5(7) . . ? C65 C61 C15 126.1(7) . . ? C65 C62 C61 60.7(5) . . ? C65 C62 C64 115.3(7) . . ? C61 C62 C64 115.2(9) . . ? C65 C62 C63 121.8(9) . . ? C61 C62 C63 118.9(6) . . ? C64 C62 C63 114.4(8) . . ? C62 C65 C61 60.0(5) . . ? C62 C65 C66 125.3(8) . . ? C61 C65 C66 125.0(6) . . ? O61 C66 O62 123.4(8) . . ? O61 C66 C65 129.0(8) . . ? O62 C66 C65 107.7(7) . . ? C20 C81 C82 121.9(6) . . ? C20 C81 C85 124.4(5) . . ? C82 C81 C85 59.7(4) . . ? C81 C82 C83 119.4(6) . . ? C81 C82 C85 61.3(4) . . ? C83 C82 C85 119.1(6) . . ? C81 C82 C84 115.4(6) . . ? C83 C82 C84 115.0(6) . . ? C85 C82 C84 116.1(6) . . ? C86 C85 C82 123.7(6) . . ? C86 C85 C81 122.9(6) . . ? C82 C85 C81 59.0(4) . . ? O81 C86 O82 125.1(6) . . ? O81 C86 C85 129.1(6) . . ? O82 C86 C85 105.6(6) . . ? N103 Ni2 N102 89.06(18) . . ? N103 Ni2 N104 90.37(18) . . ? N102 Ni2 N104 178.7(2) . . ? N103 Ni2 N101 178.9(2) . . ? N102 Ni2 N101 90.89(18) . . ? N104 Ni2 N101 89.71(18) . . ? C126 O122 C127 117.4(5) . . ? C146 O142 C147 114.9(5) . . ? C166 O162 C154 115.8(5) . . ? C186 O182 C134 116.0(5) . . ? C104 N101 C101 106.0(5) . . ? C104 N101 Ni2 126.6(4) . . ? C101 N101 Ni2 127.3(4) . . ? C109 N102 C106 105.9(4) . . ? C109 N102 Ni2 128.7(4) . . ? C106 N102 Ni2 125.4(4) . . ? C111 N103 C114 105.5(4) . . ? C111 N103 Ni2 127.5(3) . . ? C114 N103 Ni2 126.9(3) . . ? C119 N104 C116 105.7(4) . . ? C119 N104 Ni2 127.5(4) . . ? C116 N104 Ni2 126.8(4) . . ? C120 C101 N101 125.4(5) . . ? C120 C101 C102 125.9(5) . . ? N101 C101 C102 107.7(5) . . ? C103 C102 C101 108.9(5) . . ? C102 C103 C104 106.9(5) . . ? N101 C104 C105 125.2(5) . . ? N101 C104 C103 110.4(5) . . ? C105 C104 C103 124.3(5) . . ? C106 C105 C104 121.2(6) . . ? C106 C105 C121 117.2(5) . . ? C104 C105 C121 121.2(5) . . ? C105 C106 N102 124.5(5) . . ? C105 C106 C107 125.4(5) . . ? N102 C106 C107 109.1(5) . . ? C108 C107 C106 107.5(5) . . ? C107 C108 C109 107.5(5) . . ? N102 C109 C110 123.7(5) . . ? N102 C109 C108 109.9(5) . . ? C110 C109 C108 125.3(5) . . ? C111 C110 C109 120.8(5) . . ? C111 C110 C141 120.3(5) . . ? C109 C110 C141 117.9(5) . . ? C110 C111 N103 125.1(5) . . ? C110 C111 C112 125.9(5) . . ? N103 C111 C112 108.6(4) . . ? C113 C112 C111 107.8(5) . . ? C112 C113 C114 108.3(5) . . ? C115 C114 N103 123.8(5) . . ? C115 C114 C113 126.2(5) . . ? N103 C114 C113 109.5(4) . . ? C114 C115 C116 121.9(5) . . ? C114 C115 C161 120.6(5) . . ? C116 C115 C161 116.7(5) . . ? C115 C116 N104 123.9(5) . . ? C115 C116 C117 126.4(5) . . ? N104 C116 C117 109.3(5) . . ? C118 C117 C116 107.4(5) . . ? C117 C118 C119 107.9(5) . . ? N104 C119 C120 126.4(5) . . ? N104 C119 C118 109.5(5) . . ? C120 C119 C118 123.7(5) . . ? C101 C120 C119 119.3(6) . . ? C101 C120 C181 121.6(5) . . ? C119 C120 C181 117.7(5) . . ? C105 C121 C122 122.9(5) . . ? C105 C121 C125 124.9(5) . . ? C122 C121 C125 60.2(4) . . ? C121 C122 C123 119.7(6) . . ? C121 C122 C124 119.4(6) . . ? C123 C122 C124 111.1(7) . . ? C121 C122 C125 61.3(4) . . ? C123 C122 C125 120.9(5) . . ? C124 C122 C125 116.4(5) . . ? C126 C125 C122 124.4(5) . . ? C126 C125 C121 122.3(5) . . ? C122 C125 C121 58.5(4) . . ? O121 C126 O122 123.1(5) . . ? O121 C126 C125 128.1(5) . . ? O122 C126 C125 108.8(5) . . ? O122 C127 C128 107.6(5) . . ? C127 C128 C129 112.9(6) . . ? C130 C129 C128 116.6(6) . . ? C129 C130 C131 113.5(6) . . ? C130 C131 C132 113.9(6) . . ? C131 C132 C133 114.3(6) . . ? C134 C133 C132 116.0(6) . . ? O182 C134 C133 108.4(5) . . ? C110 C141 C142 123.0(5) . . ? C110 C141 C145 123.5(5) . . ? C142 C141 C145 60.2(4) . . ? C143 C142 C141 119.9(5) . . ? C143 C142 C145 121.6(6) . . ? C141 C142 C145 60.1(4) . . ? C143 C142 C144 113.5(5) . . ? C141 C142 C144 117.5(6) . . ? C145 C142 C144 114.2(5) . . ? C146 C145 C142 123.1(6) . . ? C146 C145 C141 121.7(5) . . ? C142 C145 C141 59.7(4) . . ? O141 C146 O142 122.3(6) . . ? O141 C146 C145 128.5(6) . . ? O142 C146 C145 109.2(6) . . ? O142 C147 C148 106.4(7) . . ? C49B C148 C147 132.8(11) . . ? C49B C148 C49A 38.7(8) . . ? C147 C148 C49A 101.1(8) . . ? C150 C49A C148 115.4(12) . . ? C150 C49B C148 128.4(15) . . ? C49B C150 C49A 43.2(9) . . ? C49B C150 C151 139.0(12) . . ? C49A C150 C151 115.1(12) . . ? C152 C151 C150 114.6(7) . . ? C151 C152 C153 117.0(6) . . ? C152 C153 C154 115.7(6) . . ? O162 C154 C153 106.8(6) . . ? C115 C161 C162 120.9(6) . . ? C115 C161 C165 125.5(5) . . ? C162 C161 C165 59.7(5) . . ? C163 C162 C161 119.2(5) . . ? C163 C162 C165 121.2(6) . . ? C161 C162 C165 60.8(4) . . ? C163 C162 C164 115.0(6) . . ? C161 C162 C164 116.0(7) . . ? C165 C162 C164 114.1(6) . . ? C166 C165 C162 122.7(6) . . ? C166 C165 C161 122.9(5) . . ? C162 C165 C161 59.5(4) . . ? O161 C166 O162 123.2(6) . . ? O161 C166 C165 128.6(6) . . ? O162 C166 C165 108.2(6) . . ? C120 C181 C182 123.9(6) . . ? C120 C181 C185 125.4(5) . . ? C182 C181 C185 58.8(4) . . ? C185 C182 C181 61.4(4) . . ? C185 C182 C183 119.8(5) . . ? C181 C182 C183 121.9(6) . . ? C185 C182 C184 115.2(5) . . ? C181 C182 C184 116.2(6) . . ? C183 C182 C184 113.0(6) . . ? C186 C185 C182 123.4(6) . . ? C186 C185 C181 123.1(5) . . ? C182 C185 C181 59.9(4) . . ? O181 C186 O182 122.8(5) . . ? O181 C186 C185 128.9(6) . . ? O182 C186 C185 108.2(5) . . ? N201 C201 C202 174(2) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A C133 H133 O81 0.95 2.44 3.255(10) 143.2 1_655 C85 H85 O141 1.00 2.42 3.133(8) 127.6 2_647 C41 H41 O161 1.00 2.51 3.345(8) 140.9 2_646 _diffrn_measured_fraction_theta_max 0.720 _diffrn_reflns_theta_full 29.63 _diffrn_measured_fraction_theta_full 0.720 _refine_diff_density_max 0.812 _refine_diff_density_min -0.655 _refine_diff_density_rms 0.138 data_ZnPP8 _database_code_CSD 167257 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C61.50 H73.50 Cl4.50 N4 O8 Zn' _chemical_formula_weight 1221.64 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' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Zn' 'Zn' 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' _cell_length_a 14.1554(17) _cell_length_b 14.795(3) _cell_length_c 16.406(3) _cell_angle_alpha 84.311(14) _cell_angle_beta 77.063(10) _cell_angle_gamma 65.296(10) _cell_volume 3042.2(8) _cell_formula_units_Z 2 _cell_measurement_temperature 193(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.08 _exptl_crystal_size_mid 0.4 _exptl_crystal_size_min 0.5 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.334 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1282 _exptl_absorpt_coefficient_mu 0.658 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 193(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12163 _diffrn_reflns_av_R_equivalents 0.0297 _diffrn_reflns_av_sigmaI/netI 0.0473 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.62 _diffrn_reflns_theta_max 29.07 _reflns_number_total 11286 _reflns_number_gt 9067 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.1000P)^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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.010(11) _refine_ls_number_reflns 11286 _refine_ls_number_parameters 1423 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0724 _refine_ls_R_factor_gt 0.0565 _refine_ls_wR_factor_ref 0.1518 _refine_ls_wR_factor_gt 0.1425 _refine_ls_goodness_of_fit_ref 1.096 _refine_ls_restrained_S_all 1.096 _refine_ls_shift/su_max 0.479 _refine_ls_shift/su_mean 0.031 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 0.47702(5) 0.72233(5) 0.49609(4) 0.02277(18) Uani 1 1 d . . . O21 O 0.7621(4) 0.4960(3) 0.2606(3) 0.0356(12) Uani 1 1 d . . . O22 O 0.8457(5) 0.3356(4) 0.2259(4) 0.0511(15) Uani 1 1 d . . . O41 O 0.2242(4) 0.6786(4) 0.3161(3) 0.0377(12) Uani 1 1 d . . . O42 O 0.0767(5) 0.6518(5) 0.3403(5) 0.070(2) Uani 1 1 d . . . O61 O 0.2299(4) 1.0829(3) 0.4245(3) 0.0307(11) Uani 1 1 d . . . O62 O 0.1662(4) 1.2189(3) 0.5020(3) 0.0403(13) Uani 1 1 d . . . O81 O 0.7564(4) 0.8917(4) 0.4100(3) 0.0387(12) Uani 1 1 d . . . O82 O 0.8977(5) 0.8810(5) 0.4556(5) 0.0620(19) Uani 1 1 d . . . N1 N 0.6288(4) 0.7029(4) 0.4964(3) 0.0218(13) Uani 1 1 d . . . N2 N 0.5341(4) 0.5810(4) 0.4516(3) 0.0217(13) Uani 1 1 d . . . N3 N 0.3250(4) 0.7404(4) 0.4991(3) 0.0185(12) Uani 1 1 d . . . N4 N 0.4203(5) 0.8634(4) 0.5380(3) 0.0245(14) Uani 1 1 d . . . C1 C 0.6570(6) 0.7667(5) 0.5300(4) 0.0260(15) Uani 1 1 d . . . C2 C 0.7682(6) 0.7170(5) 0.5331(5) 0.0331(18) Uani 1 1 d . . . H2A H 0.8082 0.7439 0.5541 0.040 Uiso 1 1 calc R . . C3 C 0.8052(5) 0.6256(5) 0.5008(4) 0.0294(16) Uani 1 1 d . . . H3A H 0.8759 0.5765 0.4951 0.035 Uiso 1 1 calc R . . C4 C 0.7202(6) 0.6157(5) 0.4768(4) 0.0254(15) Uani 1 1 d . . . C5 C 0.7249(6) 0.5309(5) 0.4441(4) 0.0275(16) Uani 1 1 d . . . C6 C 0.6392(6) 0.5125(5) 0.4368(4) 0.0254(16) Uani 1 1 d . . . C7 C 0.6435(6) 0.4183(5) 0.4186(5) 0.0305(17) Uani 1 1 d . . . H7A H 0.7054 0.3580 0.4083 0.037 Uiso 1 1 calc R . . C8 C 0.5439(6) 0.4308(5) 0.4185(4) 0.0276(16) Uani 1 1 d . . . H8A H 0.5227 0.3810 0.4072 0.033 Uiso 1 1 calc R . . C9 C 0.4748(6) 0.5336(5) 0.4388(4) 0.0239(15) Uani 1 1 d . . . C10 C 0.3640(6) 0.5742(5) 0.4505(4) 0.0226(15) Uani 1 1 d . . . C11 C 0.2958(6) 0.6676(5) 0.4827(4) 0.0243(15) Uani 1 1 d . . . C12 C 0.1808(6) 0.7070(5) 0.5063(4) 0.0264(16) Uani 1 1 d . . . H12A H 0.1388 0.6718 0.5036 0.032 Uiso 1 1 calc R . . C13 C 0.1441(6) 0.7995(5) 0.5319(4) 0.0294(16) Uani 1 1 d . . . H13A H 0.0717 0.8429 0.5501 0.035 Uiso 1 1 calc R . . C14 C 0.2350(6) 0.8216(5) 0.5268(4) 0.0236(15) Uani 1 1 d . . . C15 C 0.2301(6) 0.9131(5) 0.5505(4) 0.0231(15) Uani 1 1 d . . . C16 C 0.3165(6) 0.9280(4) 0.5608(4) 0.0217(14) Uani 1 1 d . . . C17 C 0.3095(6) 1.0142(5) 0.6000(4) 0.0246(16) Uani 1 1 d . . . H17A H 0.2463 1.0700 0.6211 0.029 Uiso 1 1 calc R . . C18 C 0.4084(6) 1.0010(4) 0.6011(4) 0.0265(16) Uani 1 1 d . . . H18A H 0.4284 1.0455 0.6236 0.032 Uiso 1 1 calc R . . C19 C 0.4796(6) 0.9066(4) 0.5620(4) 0.0228(15) Uani 1 1 d . . . C20 C 0.5901(6) 0.8638(5) 0.5557(4) 0.0259(16) Uani 1 1 d . . . C21 C 0.8359(5) 0.4469(5) 0.4222(4) 0.0264(15) Uani 1 1 d . . . H21A H 0.8581 0.4057 0.4723 0.032 Uiso 1 1 calc R . . C22 C 0.9278(6) 0.4557(5) 0.3615(5) 0.0325(18) Uani 1 1 d . . . C23 C 0.9127(7) 0.5499(5) 0.3089(5) 0.0398(18) Uani 1 1 d . . . H23A H 0.9806 0.5426 0.2726 0.060 Uiso 1 1 calc R . . H23B H 0.8873 0.6070 0.3459 0.060 Uiso 1 1 calc R . . H23C H 0.8605 0.5606 0.2746 0.060 Uiso 1 1 calc R . . C24 C 1.0352(6) 0.4048(7) 0.3838(6) 0.051(2) Uani 1 1 d . . . H24A H 1.0392 0.3450 0.4172 0.076 Uiso 1 1 calc R . . H24B H 1.0466 0.4501 0.4163 0.076 Uiso 1 1 calc R . . H24C H 1.0901 0.3859 0.3326 0.076 Uiso 1 1 calc R . . C25 C 0.8828(5) 0.3864(5) 0.3423(4) 0.0289(15) Uani 1 1 d . . . H25A H 0.9279 0.3148 0.3517 0.035 Uiso 1 1 calc R . . C26 C 0.8288(6) 0.4025(5) 0.2717(4) 0.0324(16) Uani 1 1 d . . . C27 C 0.7057(7) 0.5124(6) 0.1952(5) 0.0409(19) Uani 1 1 d . . . H27A H 0.6625 0.4728 0.2055 0.049 Uiso 1 1 calc R . . H27B H 0.7562 0.4916 0.1411 0.049 Uiso 1 1 calc R . . C28 C 0.6341(7) 0.6225(6) 0.1921(5) 0.046(2) Uani 1 1 d . . . H28A H 0.5806 0.6417 0.2450 0.055 Uiso 1 1 calc R . . H28B H 0.6771 0.6619 0.1866 0.055 Uiso 1 1 calc R . . C29 C 0.5789(7) 0.6451(6) 0.1198(5) 0.045(2) Uani 1 1 d . . . H29A H 0.5299 0.6114 0.1295 0.055 Uiso 1 1 calc R . . H29B H 0.6327 0.6166 0.0685 0.055 Uiso 1 1 calc R . . C30 C 0.5160(8) 0.7556(6) 0.1045(5) 0.050(2) Uani 1 1 d . . . H30A H 0.5654 0.7889 0.0947 0.061 Uiso 1 1 calc R . . H30B H 0.4891 0.7624 0.0524 0.061 Uiso 1 1 calc R . . C31 C 0.4231(7) 0.8106(6) 0.1731(6) 0.048(2) Uani 1 1 d . . . H31A H 0.4490 0.8041 0.2256 0.058 Uiso 1 1 calc R . . H31B H 0.3928 0.8821 0.1583 0.058 Uiso 1 1 calc R . . C32 C 0.3352(7) 0.7723(6) 0.1884(6) 0.051(2) Uani 1 1 d . . . H32A H 0.3662 0.7001 0.2010 0.062 Uiso 1 1 calc R . . H32B H 0.3075 0.7811 0.1365 0.062 Uiso 1 1 calc R . . C33 C 0.2412(8) 0.8256(6) 0.2612(6) 0.053(3) Uani 1 1 d . . . H33A H 0.2697 0.8264 0.3109 0.064 Uiso 1 1 calc R . . H33B H 0.2023 0.8954 0.2447 0.064 Uiso 1 1 calc R . . C34 C 0.1667(7) 0.7771(6) 0.2837(6) 0.049(2) Uani 1 1 d . . . H34A H 0.1049 0.8163 0.3268 0.059 Uiso 1 1 calc R . . H34B H 0.1407 0.7717 0.2340 0.059 Uiso 1 1 calc R . . C41 C 0.3152(6) 0.5051(5) 0.4348(4) 0.0303(16) Uani 1 1 d . . . H41A H 0.3112 0.4592 0.4832 0.036 Uiso 1 1 calc R . . C42 C 0.3396(6) 0.4547(5) 0.3512(5) 0.0336(18) Uani 1 1 d . . . C43 C 0.4035(6) 0.4814(5) 0.2741(5) 0.0383(18) Uani 1 1 d . . . H43A H 0.4733 0.4260 0.2595 0.057 Uiso 1 1 calc R . . H43B H 0.4127 0.5409 0.2848 0.057 Uiso 1 1 calc R . . H43C H 0.3662 0.4946 0.2277 0.057 Uiso 1 1 calc R . . C44 C 0.3525(7) 0.3483(6) 0.3559(7) 0.052(2) Uani 1 1 d . . . H44A H 0.4258 0.3051 0.3310 0.077 Uiso 1 1 calc R . . H44B H 0.3041 0.3412 0.3251 0.077 Uiso 1 1 calc R . . H44C H 0.3359 0.3292 0.4145 0.077 Uiso 1 1 calc R . . C45 C 0.2261(6) 0.5296(5) 0.3882(5) 0.0350(17) Uani 1 1 d . . . H45A H 0.1782 0.4957 0.4135 0.042 Uiso 1 1 calc R . . C46 C 0.1687(6) 0.6263(6) 0.3453(6) 0.044(2) Uani 1 1 d . . . C61 C 0.1199(5) 0.9950(5) 0.5750(4) 0.0262(15) Uani 1 1 d . . . H61A H 0.0859 0.9898 0.6347 0.031 Uiso 1 1 calc R . . C62 C 0.0400(5) 1.0407(5) 0.5188(4) 0.0259(16) Uani 1 1 d . . . C63 C 0.0680(6) 1.0093(5) 0.4287(4) 0.0345(17) Uani 1 1 d . . . H63A H 0.0294 0.9698 0.4219 0.052 Uiso 1 1 calc R . . H63B H 0.1445 0.9692 0.4131 0.052 Uiso 1 1 calc R . . H63C H 0.0482 1.0685 0.3927 0.052 Uiso 1 1 calc R . . C64 C -0.0739(6) 1.0680(6) 0.5602(5) 0.0412(19) Uani 1 1 d . . . H64A H -0.0998 1.0239 0.5404 0.062 Uiso 1 1 calc R . . H64B H -0.1165 1.1371 0.5464 0.062 Uiso 1 1 calc R . . H64C H -0.0799 1.0607 0.6209 0.062 Uiso 1 1 calc R . . C65 C 0.0915(5) 1.1047(4) 0.5447(4) 0.0260(15) Uani 1 1 d . . . H65A H 0.0423 1.1534 0.5894 0.031 Uiso 1 1 calc R . . C66 C 0.1641(6) 1.1413(5) 0.4901(4) 0.0300(16) Uani 1 1 d . . . C67 C 0.3033(7) 1.1195(5) 0.3715(5) 0.0369(17) Uani 1 1 d . . . H67A H 0.3446 1.1337 0.4060 0.044 Uiso 1 1 calc R . . H67B H 0.2632 1.1822 0.3438 0.044 Uiso 1 1 calc R . . C68 C 0.3782(7) 1.0425(6) 0.3058(5) 0.0393(19) Uani 1 1 d . . . H68A H 0.4232 0.9823 0.3335 0.047 Uiso 1 1 calc R . . H68B H 0.3364 1.0231 0.2756 0.047 Uiso 1 1 calc R . . C69 C 0.4481(7) 1.0828(6) 0.2442(5) 0.047(2) Uani 1 1 d . . . H69A H 0.4881 1.1031 0.2757 0.057 Uiso 1 1 calc R . . H69B H 0.4018 1.1434 0.2178 0.057 Uiso 1 1 calc R . . C70 C 0.5278(7) 1.0116(7) 0.1747(5) 0.048(2) Uani 1 1 d . . . H70A H 0.4876 0.9963 0.1399 0.057 Uiso 1 1 calc R . . H70B H 0.5682 1.0465 0.1386 0.057 Uiso 1 1 calc R . . C71 C 0.6076(7) 0.9125(7) 0.2041(5) 0.050(2) Uani 1 1 d . . . H71A H 0.5678 0.8753 0.2373 0.060 Uiso 1 1 calc R . . H71B H 0.6536 0.8722 0.1544 0.060 Uiso 1 1 calc R . . C72 C 0.6758(7) 0.9244(6) 0.2553(6) 0.048(2) Uani 1 1 d . . . H72A H 0.6298 0.9644 0.3052 0.058 Uiso 1 1 calc R . . H72B H 0.7152 0.9620 0.2222 0.058 Uiso 1 1 calc R . . C73 C 0.7558(7) 0.8258(6) 0.2842(6) 0.045(2) Uani 1 1 d . . . H73A H 0.8003 0.7845 0.2346 0.054 Uiso 1 1 calc R . . H73B H 0.7166 0.7892 0.3194 0.054 Uiso 1 1 calc R . . C74 C 0.8263(7) 0.8402(7) 0.3328(5) 0.048(2) Uani 1 1 d . . . H74A H 0.8808 0.7752 0.3460 0.058 Uiso 1 1 calc R . . H74B H 0.8625 0.8808 0.3003 0.058 Uiso 1 1 calc R . . C81 C 0.6316(5) 0.9268(5) 0.5896(4) 0.0275(15) Uani 1 1 d . . . H81A H 0.6234 0.9215 0.6519 0.033 Uiso 1 1 calc R . . C82 C 0.6201(6) 1.0292(5) 0.5573(5) 0.0330(17) Uani 1 1 d . . . C83 C 0.5726(7) 1.0726(6) 0.4802(5) 0.0407(18) Uani 1 1 d . . . H83A H 0.5910 1.0189 0.4412 0.061 Uiso 1 1 calc R . . H83B H 0.6010 1.1205 0.4528 0.061 Uiso 1 1 calc R . . H83C H 0.4952 1.1063 0.4970 0.061 Uiso 1 1 calc R . . C84 C 0.5964(8) 1.1071(6) 0.6213(6) 0.053(2) Uani 1 1 d . . . H84A H 0.5243 1.1583 0.6235 0.080 Uiso 1 1 calc R . . H84B H 0.6474 1.1377 0.6054 0.080 Uiso 1 1 calc R . . H84C H 0.6023 1.0755 0.6765 0.080 Uiso 1 1 calc R . . C85 C 0.7310(6) 0.9446(5) 0.5469(5) 0.0364(18) Uani 1 1 d . . . H85A H 0.7703 0.9492 0.5888 0.044 Uiso 1 1 calc R . . C86 C 0.8037(6) 0.9035(5) 0.4666(5) 0.0382(19) Uani 1 1 d . . . Zn2 Zn 0.19991(5) 0.71754(4) 0.73116(4) 0.02121(18) Uani 1 1 d . . . O121 O 0.2225(4) 0.3548(3) 0.7968(3) 0.0342(12) Uani 1 1 d . . . O122 O 0.3021(5) 0.2086(3) 0.7318(4) 0.0512(16) Uani 1 1 d . . . O141 O 0.5660(5) 0.5425(4) 0.8434(3) 0.0373(13) Uani 1 1 d . . . O142 O 0.7266(5) 0.5471(5) 0.8074(5) 0.066(2) Uani 1 1 d . . . O161 O 0.1460(4) 0.9376(3) 0.9765(3) 0.0342(11) Uani 1 1 d . . . O162 O 0.0573(4) 1.1002(4) 1.0026(4) 0.0454(14) Uani 1 1 d . . . O181 O -0.2047(4) 0.7739(4) 0.8947(3) 0.0400(12) Uani 1 1 d . . . O182 O -0.3498(5) 0.8030(4) 0.8482(5) 0.064(2) Uani 1 1 d . . . N101 N 0.0657(4) 0.7027(4) 0.7250(3) 0.0219(13) Uani 1 1 d . . . N102 N 0.2899(4) 0.5755(4) 0.6916(3) 0.0207(13) Uani 1 1 d . . . N103 N 0.3335(5) 0.7339(4) 0.7375(3) 0.0219(13) Uani 1 1 d . . . N104 N 0.1088(4) 0.8585(4) 0.7738(3) 0.0201(13) Uani 1 1 d . . . C101 C -0.0353(5) 0.7768(5) 0.7338(4) 0.0259(15) Uani 1 1 d . . . C102 C -0.1029(6) 0.7411(5) 0.7053(5) 0.0323(18) Uani 1 1 d . . . H10A H -0.1758 0.7779 0.7037 0.039 Uiso 1 1 calc R . . C103 C -0.0433(6) 0.6461(5) 0.6815(5) 0.0319(17) Uani 1 1 d . . . H10B H -0.0669 0.6034 0.6603 0.038 Uiso 1 1 calc R . . C104 C 0.0628(6) 0.6203(5) 0.6939(4) 0.0239(15) Uani 1 1 d . . . C105 C 0.1480(6) 0.5285(5) 0.6729(4) 0.0225(15) Uani 1 1 d . . . C106 C 0.2554(6) 0.5101(5) 0.6687(4) 0.0252(16) Uani 1 1 d . . . C107 C 0.3463(6) 0.4204(5) 0.6353(5) 0.0298(18) Uani 1 1 d . . . H10C H 0.3441 0.3632 0.6157 0.036 Uiso 1 1 calc R . . C108 C 0.4345(5) 0.4338(4) 0.6374(4) 0.0234(15) Uani 1 1 d . . . H10D H 0.5059 0.3883 0.6185 0.028 Uiso 1 1 calc R . . C109 C 0.4001(5) 0.5291(5) 0.6734(4) 0.0212(15) Uani 1 1 d . . . C110 C 0.4699(5) 0.5681(5) 0.6850(4) 0.0228(14) Uani 1 1 d . . . C111 C 0.4369(5) 0.6667(4) 0.7105(4) 0.0219(14) Uani 1 1 d . . . C112 C 0.5082(6) 0.7117(5) 0.7161(4) 0.0248(15) Uani 1 1 d . . . H11A H 0.5834 0.6823 0.7004 0.030 Uiso 1 1 calc R . . C113 C 0.4473(5) 0.8035(4) 0.7480(4) 0.0244(15) Uani 1 1 d . . . H11B H 0.4723 0.8506 0.7589 0.029 Uiso 1 1 calc R . . C114 C 0.3379(6) 0.8178(5) 0.7627(4) 0.0216(15) Uani 1 1 d . . . C115 C 0.2507(6) 0.9048(4) 0.7920(4) 0.0236(16) Uani 1 1 d . . . C116 C 0.1449(6) 0.9261(4) 0.7918(4) 0.0226(15) Uani 1 1 d . . . C117 C 0.0565(6) 1.0223(5) 0.8082(4) 0.0267(17) Uani 1 1 d . . . H11C H 0.0604 1.0816 0.8213 0.032 Uiso 1 1 calc R . . C118 C -0.0321(5) 1.0128(4) 0.8016(4) 0.0238(15) Uani 1 1 d . . . H11D H -0.1022 1.0633 0.8094 0.029 Uiso 1 1 calc R . . C119 C 0.0010(6) 0.9107(5) 0.7805(4) 0.0251(16) Uani 1 1 d . . . C120 C -0.0682(5) 0.8715(5) 0.7655(4) 0.0238(15) Uani 1 1 d . . . C121 C 0.1247(5) 0.4486(5) 0.6456(4) 0.0265(16) Uani 1 1 d . . . H12B H 0.1196 0.4551 0.5853 0.032 Uiso 1 1 calc R . . C122 C 0.0504(6) 0.4085(5) 0.6978(5) 0.0289(17) Uani 1 1 d . . . C123 C -0.0004(7) 0.4390(6) 0.7889(5) 0.0423(19) Uani 1 1 d . . . H12C H -0.0753 0.4840 0.7930 0.063 Uiso 1 1 calc R . . H12D H 0.0365 0.4730 0.8088 0.063 Uiso 1 1 calc R . . H12E H 0.0051 0.3796 0.8232 0.063 Uiso 1 1 calc R . . C124 C -0.0223(6) 0.3876(6) 0.6526(6) 0.045(2) Uani 1 1 d . . . H12F H -0.0957 0.4360 0.6703 0.068 Uiso 1 1 calc R . . H12G H -0.0181 0.3202 0.6667 0.068 Uiso 1 1 calc R . . H12H H 0.0005 0.3931 0.5921 0.068 Uiso 1 1 calc R . . C125 C 0.1695(5) 0.3383(5) 0.6753(4) 0.0285(15) Uani 1 1 d . . . H12I H 0.1849 0.2909 0.6298 0.034 Uiso 1 1 calc R . . C126 C 0.2371(6) 0.2944(5) 0.7361(4) 0.0300(15) Uani 1 1 d . . . C127 C 0.2939(7) 0.3122(5) 0.8558(5) 0.0407(19) Uani 1 1 d . . . H12J H 0.3686 0.2890 0.8253 0.049 Uiso 1 1 calc R . . H12K H 0.2832 0.2542 0.8849 0.049 Uiso 1 1 calc R . . C128 C 0.2715(8) 0.3901(6) 0.9192(5) 0.046(2) Uani 1 1 d . . . H12L H 0.2839 0.4471 0.8898 0.055 Uiso 1 1 calc R . . H12M H 0.1960 0.4147 0.9480 0.055 Uiso 1 1 calc R . . C129 C 0.3408(8) 0.3492(6) 0.9832(5) 0.050(2) Uani 1 1 d . . . H12N H 0.4155 0.3335 0.9552 0.061 Uiso 1 1 calc R . . H12O H 0.3365 0.2862 1.0062 0.061 Uiso 1 1 calc R . . C130 C 0.3097(9) 0.4214(7) 1.0560(5) 0.055(2) Uani 1 1 d . . . H13B H 0.2345 0.4378 1.0828 0.066 Uiso 1 1 calc R . . H13C H 0.3532 0.3865 1.0982 0.066 Uiso 1 1 calc R . . C131 C 0.3229(9) 0.5188(7) 1.0316(6) 0.059(3) Uani 1 1 d . . . H13D H 0.2761 0.5554 0.9919 0.071 Uiso 1 1 calc R . . H13E H 0.2981 0.5600 1.0823 0.071 Uiso 1 1 calc R . . C132 C 0.4301(9) 0.5080(7) 0.9939(6) 0.059(3) Uani 1 1 d . . . H13F H 0.4575 0.4626 0.9456 0.071 Uiso 1 1 calc R . . H13G H 0.4761 0.4768 1.0352 0.071 Uiso 1 1 calc R . . C133 C 0.4378(8) 0.6081(6) 0.9638(6) 0.051(2) Uani 1 1 d . . . H13H H 0.3879 0.6421 0.9258 0.061 Uiso 1 1 calc R . . H13I H 0.4165 0.6517 1.0127 0.061 Uiso 1 1 calc R . . C134 C 0.5450(8) 0.5932(6) 0.9204(5) 0.047(2) Uani 1 1 d . . . H13J H 0.5504 0.6580 0.9086 0.057 Uiso 1 1 calc R . . H13K H 0.5970 0.5526 0.9553 0.057 Uiso 1 1 calc R . . C141 C 0.5862(5) 0.5031(4) 0.6600(4) 0.0246(14) Uani 1 1 d . . . H14A H 0.6129 0.5045 0.5983 0.030 Uiso 1 1 calc R . . C142 C 0.6411(6) 0.4008(5) 0.6984(5) 0.0322(18) Uani 1 1 d . . . C143 C 0.5812(6) 0.3652(5) 0.7735(5) 0.0339(17) Uani 1 1 d . . . H14B H 0.5292 0.4224 0.8076 0.051 Uiso 1 1 calc R . . H14C H 0.6313 0.3196 0.8070 0.051 Uiso 1 1 calc R . . H14D H 0.5444 0.3305 0.7545 0.051 Uiso 1 1 calc R . . C144 C 0.7246(7) 0.3190(5) 0.6404(6) 0.044(2) Uani 1 1 d . . . H14E H 0.7530 0.2577 0.6726 0.065 Uiso 1 1 calc R . . H14F H 0.7823 0.3390 0.6136 0.065 Uiso 1 1 calc R . . H14G H 0.6927 0.3076 0.5974 0.065 Uiso 1 1 calc R . . C145 C 0.6714(6) 0.4859(5) 0.7091(5) 0.0310(16) Uani 1 1 d . . . H14H H 0.7403 0.4785 0.6713 0.037 Uiso 1 1 calc R . . C146 C 0.6585(6) 0.5285(5) 0.7901(5) 0.0354(19) Uani 1 1 d . . . C161 C 0.2734(5) 0.9864(4) 0.8181(4) 0.0217(14) Uani 1 1 d . . . H16A H 0.2900 1.0277 0.7697 0.026 Uiso 1 1 calc R . . C162 C 0.3348(6) 0.9760(4) 0.8854(4) 0.0264(16) Uani 1 1 d . . . C163 C 0.3718(6) 0.8819(5) 0.9383(4) 0.0313(16) Uani 1 1 d . . . H16B H 0.4490 0.8459 0.9217 0.047 Uiso 1 1 calc R . . H16C H 0.3371 0.8395 0.9298 0.047 Uiso 1 1 calc R . . H16D H 0.3531 0.8999 0.9975 0.047 Uiso 1 1 calc R . . C164 C 0.4122(6) 1.0244(5) 0.8690(5) 0.0340(17) Uani 1 1 d . . . H16E H 0.3857 1.0844 0.8348 0.051 Uiso 1 1 calc R . . H16F H 0.4813 0.9778 0.8392 0.051 Uiso 1 1 calc R . . H16G H 0.4199 1.0424 0.9223 0.051 Uiso 1 1 calc R . . C165 C 0.2168(5) 1.0467(4) 0.8983(4) 0.0250(15) Uani 1 1 d . . . H16H H 0.2050 1.1182 0.8904 0.030 Uiso 1 1 calc R . . C166 C 0.1334(5) 1.0318(5) 0.9634(4) 0.0284(15) Uani 1 1 d . . . C167 C 0.0616(7) 0.9219(6) 1.0369(5) 0.0396(19) Uani 1 1 d . . . H16I H -0.0073 0.9590 1.0194 0.047 Uiso 1 1 calc R . . H16J H 0.0561 0.9463 1.0925 0.047 Uiso 1 1 calc R . . C168 C 0.0871(7) 0.8122(6) 1.0415(5) 0.0388(19) Uani 1 1 d . . . H16K H 0.1584 0.7750 1.0548 0.047 Uiso 1 1 calc R . . H16L H 0.0877 0.7891 0.9867 0.047 Uiso 1 1 calc R . . C169 C 0.0048(7) 0.7928(6) 1.1083(5) 0.044(2) Uani 1 1 d . . . H16M H -0.0652 0.8270 1.0922 0.053 Uiso 1 1 calc R . . H16N H 0.0003 0.8222 1.1614 0.053 Uiso 1 1 calc R . . C170 C 0.0277(7) 0.6827(6) 1.1232(5) 0.047(2) Uani 1 1 d . . . H17B H -0.0235 0.6764 1.1731 0.057 Uiso 1 1 calc R . . H17C H 0.0997 0.6477 1.1356 0.057 Uiso 1 1 calc R . . C171 C 0.0209(8) 0.6308(6) 1.0492(6) 0.051(2) Uani 1 1 d . . . H17D H 0.0725 0.6364 0.9993 0.061 Uiso 1 1 calc R . . H17E H 0.0415 0.5592 1.0627 0.061 Uiso 1 1 calc R . . C172 C -0.0874(8) 0.6731(7) 1.0285(6) 0.054(2) Uani 1 1 d . . . H17F H -0.1388 0.6669 1.0783 0.065 Uiso 1 1 calc R . . H17G H -0.1083 0.7449 1.0158 0.065 Uiso 1 1 calc R . . C173 C -0.0947(8) 0.6238(6) 0.9560(6) 0.051(2) Uani 1 1 d . . . H17H H -0.0864 0.5551 0.9727 0.061 Uiso 1 1 calc R . . H17I H -0.0348 0.6191 0.9093 0.061 Uiso 1 1 calc R . . C174 C -0.1970(7) 0.6764(6) 0.9249(5) 0.044(2) Uani 1 1 d . . . H17J H -0.1977 0.6379 0.8792 0.053 Uiso 1 1 calc R . . H17K H -0.2581 0.6827 0.9708 0.053 Uiso 1 1 calc R . . C181 C -0.1844(5) 0.9442(5) 0.7771(5) 0.0290(16) Uani 1 1 d . . . H18B H -0.1987 0.9914 0.7289 0.035 Uiso 1 1 calc R . . C182 C -0.2523(6) 0.9926(5) 0.8600(5) 0.0324(17) Uani 1 1 d . . . C183 C -0.2093(7) 0.9603(6) 0.9400(5) 0.0430(19) Uani 1 1 d . . . H18C H -0.1947 1.0134 0.9585 0.064 Uiso 1 1 calc R . . H18D H -0.1435 0.8998 0.9294 0.064 Uiso 1 1 calc R . . H18E H -0.2618 0.9470 0.9835 0.064 Uiso 1 1 calc R . . C184 C -0.3268(6) 1.1012(5) 0.8592(6) 0.047(2) Uani 1 1 d . . . H18F H -0.3510 1.1175 0.8060 0.070 Uiso 1 1 calc R . . H18G H -0.2896 1.1422 0.8656 0.070 Uiso 1 1 calc R . . H18H H -0.3881 1.1143 0.9054 0.070 Uiso 1 1 calc R . . C185 C -0.2791(6) 0.9228(5) 0.8180(5) 0.0384(19) Uani 1 1 d . . . H18I H -0.3405 0.9601 0.7900 0.046 Uiso 1 1 calc R . . C186 C -0.2818(6) 0.8274(5) 0.8557(5) 0.0399(19) Uani 1 1 d . . . C201 C 0.8369(11) 0.2748(11) 0.9745(9) 0.107(5) Uani 1 1 d . . . H20A H 0.8798 0.2058 0.9925 0.128 Uiso 1 1 calc R . . Cl11 Cl 0.8469(3) 0.2744(2) 0.8667(2) 0.0879(9) Uani 1 1 d . . . Cl12 Cl 0.8898(5) 0.3552(4) 0.9997(3) 0.1404(18) Uani 1 1 d . . . Cl13 Cl 0.7085(4) 0.3090(7) 1.0273(4) 0.233(4) Uani 1 1 d . . . C202 C 0.7768(9) 0.1693(7) 0.2451(9) 0.084(4) Uani 1 1 d . . . H20B H 0.7927 0.2296 0.2322 0.101 Uiso 1 1 calc R . . Cl21 Cl 0.6447(3) 0.2059(3) 0.2561(2) 0.0949(10) Uani 1 1 d . . . Cl22 Cl 0.8148(4) 0.1180(4) 0.3420(4) 0.152(2) Uani 1 1 d . . . Cl23 Cl 0.8470(5) 0.0871(3) 0.1637(4) 0.207(3) Uani 1 1 d . . . C203 C 0.1232(7) 0.1950(7) 0.1366(5) 0.053(2) Uani 1 1 d . . . H20C H 0.0721 0.1933 0.1040 0.064 Uiso 1 1 calc R . . Cl31 Cl 0.1019(3) 0.3185(2) 0.1456(3) 0.1115(13) Uani 1 1 d . . . Cl32 Cl 0.0996(3) 0.1419(3) 0.2350(2) 0.1049(12) Uani 1 1 d . . . Cl33 Cl 0.2522(2) 0.1246(2) 0.08282(17) 0.0801(8) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.0198(4) 0.0220(3) 0.0259(4) -0.0039(3) -0.0018(3) -0.0086(3) O21 0.031(3) 0.034(2) 0.035(3) -0.007(2) -0.008(2) -0.005(2) O22 0.064(4) 0.036(3) 0.052(3) -0.014(2) -0.011(3) -0.017(3) O41 0.029(3) 0.035(3) 0.045(3) 0.000(2) -0.008(3) -0.009(2) O42 0.042(4) 0.059(4) 0.118(6) -0.006(4) -0.036(4) -0.018(3) O61 0.034(3) 0.032(2) 0.028(2) -0.0056(18) 0.002(2) -0.018(2) O62 0.049(4) 0.026(2) 0.042(3) -0.005(2) -0.004(3) -0.013(2) O81 0.024(3) 0.045(3) 0.045(3) -0.002(2) 0.003(3) -0.018(2) O82 0.031(4) 0.064(4) 0.096(5) -0.025(4) -0.006(4) -0.022(3) N1 0.017(3) 0.025(3) 0.026(3) -0.006(2) -0.005(3) -0.010(3) N2 0.015(3) 0.024(3) 0.025(3) -0.001(2) 0.003(3) -0.011(2) N3 0.019(3) 0.022(3) 0.021(3) -0.001(2) -0.003(2) -0.014(3) N4 0.028(4) 0.025(3) 0.021(3) -0.005(2) -0.003(3) -0.011(3) C1 0.028(4) 0.032(3) 0.024(3) 0.005(3) -0.004(3) -0.019(3) C2 0.029(4) 0.035(4) 0.047(4) 0.002(3) -0.013(4) -0.022(3) C3 0.015(4) 0.030(3) 0.039(4) -0.006(3) 0.001(3) -0.007(3) C4 0.024(4) 0.026(3) 0.027(3) 0.001(3) -0.006(3) -0.010(3) C5 0.030(5) 0.026(3) 0.025(3) 0.000(3) -0.004(3) -0.011(3) C6 0.024(4) 0.023(3) 0.027(3) -0.002(2) -0.005(3) -0.007(3) C7 0.025(4) 0.024(3) 0.037(4) -0.003(3) 0.003(4) -0.009(3) C8 0.023(4) 0.022(3) 0.037(4) -0.006(3) -0.002(3) -0.009(3) C9 0.019(4) 0.027(3) 0.026(3) -0.005(3) 0.008(3) -0.015(3) C10 0.022(4) 0.023(3) 0.026(3) -0.003(2) -0.001(3) -0.014(3) C11 0.024(4) 0.034(3) 0.021(3) 0.002(3) 0.001(3) -0.020(3) C12 0.023(4) 0.033(3) 0.031(4) 0.005(3) -0.002(3) -0.022(3) C13 0.026(4) 0.031(3) 0.028(3) -0.002(3) 0.000(3) -0.011(3) C14 0.030(4) 0.021(3) 0.025(3) -0.001(2) -0.009(3) -0.013(3) C15 0.025(4) 0.024(3) 0.017(3) -0.001(2) -0.002(3) -0.008(3) C16 0.027(4) 0.022(3) 0.020(3) 0.000(2) -0.004(3) -0.014(3) C17 0.028(4) 0.019(3) 0.023(3) -0.006(2) -0.001(3) -0.008(3) C18 0.031(4) 0.022(3) 0.029(3) -0.005(2) -0.007(3) -0.011(3) C19 0.025(4) 0.017(3) 0.024(3) -0.004(2) 0.000(3) -0.008(3) C20 0.030(4) 0.030(3) 0.027(3) 0.002(3) -0.007(3) -0.021(3) C21 0.021(4) 0.023(3) 0.035(3) 0.001(3) -0.004(3) -0.009(3) C22 0.022(4) 0.027(3) 0.046(4) -0.003(3) -0.009(4) -0.007(3) C23 0.042(5) 0.037(4) 0.045(4) 0.000(3) 0.003(4) -0.027(4) C24 0.021(4) 0.055(5) 0.071(6) -0.005(4) -0.006(4) -0.012(4) C25 0.022(4) 0.024(3) 0.039(4) -0.002(3) -0.005(3) -0.008(3) C26 0.030(4) 0.027(3) 0.037(4) -0.003(3) 0.001(3) -0.011(3) C27 0.040(5) 0.039(4) 0.042(4) -0.002(3) -0.013(4) -0.013(4) C28 0.051(6) 0.041(4) 0.040(4) -0.008(3) -0.017(4) -0.008(4) C29 0.049(5) 0.048(4) 0.041(4) 0.001(3) -0.021(4) -0.016(4) C30 0.063(6) 0.052(5) 0.042(4) 0.003(4) -0.016(4) -0.027(4) C31 0.054(6) 0.038(4) 0.054(5) 0.002(3) -0.021(4) -0.015(4) C32 0.055(6) 0.044(4) 0.052(5) -0.007(4) -0.007(5) -0.018(4) C33 0.060(7) 0.036(4) 0.054(5) -0.008(4) -0.016(5) -0.006(4) C34 0.048(5) 0.038(4) 0.054(5) -0.003(3) -0.025(4) -0.002(4) C41 0.028(5) 0.029(3) 0.034(4) -0.004(3) 0.000(3) -0.015(3) C42 0.031(4) 0.033(4) 0.044(4) -0.008(3) -0.013(4) -0.015(3) C43 0.037(5) 0.039(4) 0.041(4) -0.013(3) -0.005(4) -0.016(3) C44 0.042(5) 0.034(4) 0.088(7) -0.019(4) -0.004(5) -0.024(4) C45 0.021(4) 0.036(4) 0.052(4) -0.014(3) 0.001(4) -0.017(3) C46 0.029(5) 0.041(4) 0.058(5) -0.019(4) -0.019(4) -0.003(4) C61 0.023(4) 0.030(3) 0.019(3) -0.009(2) 0.002(3) -0.006(3) C62 0.018(4) 0.025(3) 0.030(4) -0.007(3) -0.001(3) -0.004(3) C63 0.034(4) 0.037(4) 0.034(4) -0.004(3) -0.011(3) -0.013(3) C64 0.023(4) 0.046(4) 0.051(5) -0.010(3) -0.002(4) -0.011(4) C65 0.018(4) 0.026(3) 0.028(3) -0.013(2) 0.004(3) -0.006(3) C66 0.027(4) 0.026(3) 0.032(3) -0.005(3) -0.007(3) -0.003(3) C67 0.039(5) 0.037(4) 0.038(4) 0.002(3) -0.002(4) -0.022(4) C68 0.041(5) 0.037(4) 0.042(4) -0.002(3) 0.004(4) -0.024(4) C69 0.052(6) 0.050(4) 0.044(5) 0.004(4) -0.007(4) -0.028(4) C70 0.031(5) 0.061(5) 0.044(5) -0.008(4) 0.006(4) -0.017(4) C71 0.050(6) 0.063(5) 0.038(4) -0.020(4) 0.005(4) -0.027(5) C72 0.043(6) 0.049(5) 0.053(5) -0.011(4) 0.005(4) -0.023(4) C73 0.038(6) 0.040(4) 0.051(5) -0.014(4) 0.010(4) -0.015(4) C74 0.030(5) 0.056(5) 0.049(5) -0.009(4) 0.009(4) -0.015(4) C81 0.022(4) 0.028(3) 0.035(4) -0.004(3) -0.003(3) -0.014(3) C82 0.032(5) 0.027(3) 0.044(4) -0.007(3) -0.003(4) -0.018(3) C83 0.035(5) 0.038(4) 0.051(5) 0.009(3) -0.005(4) -0.021(4) C84 0.057(6) 0.041(4) 0.068(6) -0.018(4) -0.011(5) -0.023(4) C85 0.032(5) 0.036(4) 0.051(4) -0.005(3) -0.012(4) -0.020(3) C86 0.029(5) 0.035(4) 0.056(5) 0.000(3) -0.007(4) -0.021(4) Zn2 0.0175(4) 0.0194(3) 0.0249(4) -0.0038(3) -0.0002(3) -0.0070(3) O121 0.041(3) 0.030(2) 0.033(3) -0.0051(19) -0.010(2) -0.014(2) O122 0.065(4) 0.024(2) 0.054(3) -0.008(2) -0.024(3) -0.001(3) O141 0.048(4) 0.038(3) 0.035(3) -0.004(2) -0.014(3) -0.023(3) O142 0.046(4) 0.053(3) 0.110(6) -0.024(3) -0.037(4) -0.016(3) O161 0.034(3) 0.035(2) 0.031(2) -0.0061(19) 0.008(2) -0.018(2) O162 0.034(3) 0.036(3) 0.057(3) -0.018(2) 0.010(3) -0.011(3) O181 0.038(3) 0.037(3) 0.052(3) -0.004(2) -0.004(3) -0.023(3) O182 0.026(3) 0.041(3) 0.129(6) -0.016(3) -0.015(4) -0.013(3) N101 0.015(3) 0.023(3) 0.027(3) -0.008(2) 0.003(3) -0.009(2) N102 0.016(3) 0.020(2) 0.026(3) -0.002(2) -0.002(3) -0.008(2) N103 0.023(3) 0.016(3) 0.026(3) -0.002(2) -0.005(3) -0.008(2) N104 0.017(3) 0.021(3) 0.024(3) -0.002(2) 0.001(3) -0.011(2) C101 0.018(4) 0.029(3) 0.027(3) -0.003(3) -0.002(3) -0.007(3) C102 0.025(4) 0.032(3) 0.043(4) -0.006(3) -0.010(4) -0.011(3) C103 0.023(4) 0.035(3) 0.040(4) -0.009(3) -0.013(3) -0.010(3) C104 0.022(4) 0.030(3) 0.028(3) 0.002(3) -0.006(3) -0.019(3) C105 0.020(4) 0.031(3) 0.025(3) -0.004(3) -0.004(3) -0.018(3) C106 0.024(4) 0.024(3) 0.023(3) -0.002(2) 0.000(3) -0.007(3) C107 0.032(5) 0.026(3) 0.029(4) -0.006(3) -0.004(4) -0.009(3) C108 0.015(4) 0.020(3) 0.033(3) -0.006(2) -0.002(3) -0.006(3) C109 0.015(4) 0.023(3) 0.023(3) -0.003(2) 0.000(3) -0.006(3) C110 0.021(4) 0.024(3) 0.024(3) 0.001(2) 0.000(3) -0.013(3) C111 0.019(4) 0.021(3) 0.027(3) 0.003(2) -0.003(3) -0.010(3) C112 0.013(4) 0.024(3) 0.034(4) 0.002(3) 0.004(3) -0.009(3) C113 0.022(4) 0.023(3) 0.027(3) 0.001(2) 0.000(3) -0.010(3) C114 0.019(4) 0.022(3) 0.023(3) -0.001(2) 0.002(3) -0.010(3) C115 0.034(5) 0.014(3) 0.022(3) 0.005(2) -0.007(3) -0.010(3) C116 0.027(4) 0.020(3) 0.020(3) 0.000(2) -0.003(3) -0.009(3) C117 0.027(4) 0.021(3) 0.030(4) -0.007(3) -0.006(3) -0.006(3) C118 0.016(4) 0.021(3) 0.029(3) -0.007(2) 0.001(3) -0.004(3) C119 0.021(4) 0.022(3) 0.027(3) -0.007(2) 0.002(3) -0.005(3) C120 0.016(4) 0.024(3) 0.029(3) -0.004(3) 0.000(3) -0.007(3) C121 0.025(4) 0.027(3) 0.027(3) -0.009(2) -0.002(3) -0.010(3) C122 0.020(4) 0.036(3) 0.037(4) -0.016(3) 0.005(3) -0.021(3) C123 0.034(5) 0.039(4) 0.047(4) -0.015(3) 0.013(4) -0.016(4) C124 0.026(4) 0.053(5) 0.061(5) -0.022(4) -0.001(4) -0.020(4) C125 0.024(4) 0.026(3) 0.033(3) -0.012(3) 0.004(3) -0.010(3) C126 0.029(4) 0.028(3) 0.037(4) -0.006(3) 0.000(3) -0.018(3) C127 0.049(5) 0.039(4) 0.040(4) -0.003(3) -0.016(4) -0.020(4) C128 0.061(6) 0.041(4) 0.041(4) -0.008(3) -0.013(4) -0.023(4) C129 0.069(7) 0.052(5) 0.044(5) 0.006(4) -0.022(5) -0.035(5) C130 0.070(7) 0.073(6) 0.037(4) 0.002(4) -0.015(5) -0.041(5) C131 0.073(8) 0.064(6) 0.046(5) -0.015(4) -0.008(5) -0.032(5) C132 0.059(7) 0.060(5) 0.048(5) -0.012(4) -0.001(5) -0.016(5) C133 0.066(7) 0.042(4) 0.043(5) -0.010(4) -0.007(5) -0.021(4) C134 0.069(7) 0.041(4) 0.041(4) -0.009(3) -0.014(5) -0.027(4) C141 0.020(4) 0.020(3) 0.032(3) -0.004(2) 0.002(3) -0.010(3) C142 0.031(5) 0.022(3) 0.043(4) -0.005(3) -0.011(4) -0.007(3) C143 0.034(4) 0.024(3) 0.045(4) -0.004(3) -0.013(4) -0.010(3) C144 0.031(5) 0.030(3) 0.065(5) -0.013(3) -0.004(4) -0.008(3) C145 0.015(4) 0.028(3) 0.050(4) -0.010(3) -0.001(3) -0.010(3) C146 0.029(5) 0.021(3) 0.058(5) -0.007(3) -0.017(4) -0.007(3) C161 0.019(4) 0.019(3) 0.026(3) -0.002(2) -0.002(3) -0.007(3) C162 0.025(4) 0.017(3) 0.033(4) -0.007(2) -0.002(3) -0.005(3) C163 0.026(4) 0.029(3) 0.031(4) 0.003(3) -0.011(3) -0.003(3) C164 0.026(4) 0.029(3) 0.049(4) -0.010(3) -0.001(4) -0.015(3) C165 0.023(4) 0.018(3) 0.030(3) -0.006(2) -0.005(3) -0.004(3) C166 0.020(4) 0.032(3) 0.032(3) -0.005(3) 0.004(3) -0.013(3) C167 0.037(5) 0.051(4) 0.033(4) -0.006(3) 0.009(4) -0.028(4) C168 0.040(5) 0.044(4) 0.035(4) 0.001(3) 0.002(4) -0.026(4) C169 0.052(6) 0.055(5) 0.031(4) 0.003(3) -0.002(4) -0.029(4) C170 0.043(6) 0.044(4) 0.042(4) 0.010(3) 0.005(4) -0.014(4) C171 0.053(6) 0.039(4) 0.066(6) 0.006(4) -0.012(5) -0.025(4) C172 0.059(6) 0.050(5) 0.052(5) -0.009(4) -0.006(5) -0.019(4) C173 0.067(7) 0.042(5) 0.052(5) 0.003(4) -0.017(5) -0.029(5) C174 0.049(6) 0.039(4) 0.051(5) -0.012(3) 0.010(4) -0.032(4) C181 0.019(4) 0.026(3) 0.040(4) -0.005(3) -0.007(3) -0.007(3) C182 0.015(4) 0.028(3) 0.050(5) -0.012(3) 0.009(4) -0.009(3) C183 0.044(5) 0.040(4) 0.041(4) -0.012(3) 0.003(4) -0.016(4) C184 0.024(5) 0.025(3) 0.080(6) -0.015(4) 0.004(4) -0.004(3) C185 0.025(4) 0.032(3) 0.055(5) -0.012(3) -0.006(4) -0.008(3) C186 0.021(4) 0.035(4) 0.055(5) -0.019(3) 0.006(4) -0.007(3) C201 0.079(10) 0.092(9) 0.103(10) 0.002(8) 0.002(8) -0.001(7) Cl11 0.102(3) 0.0747(18) 0.091(2) -0.0127(15) -0.0197(19) -0.0365(17) Cl12 0.209(5) 0.127(3) 0.082(2) -0.035(2) -0.010(3) -0.068(3) Cl13 0.077(4) 0.352(10) 0.168(5) 0.073(6) 0.031(4) -0.033(5) C202 0.055(7) 0.039(5) 0.149(12) -0.008(6) 0.000(8) -0.018(5) Cl21 0.058(2) 0.094(2) 0.103(2) -0.0070(18) 0.0093(18) -0.0136(17) Cl22 0.110(3) 0.179(5) 0.196(5) 0.090(4) -0.066(4) -0.090(3) Cl23 0.189(6) 0.093(3) 0.213(6) -0.044(3) 0.154(5) -0.024(3) C203 0.045(6) 0.066(6) 0.045(5) -0.004(4) -0.002(4) -0.020(5) Cl31 0.112(3) 0.0759(19) 0.142(3) -0.033(2) 0.036(3) -0.057(2) Cl32 0.085(3) 0.096(2) 0.078(2) 0.0191(17) 0.0199(18) -0.0052(18) Cl33 0.0642(19) 0.105(2) 0.0605(15) -0.0339(14) 0.0069(14) -0.0272(16) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 N4 2.027(5) . ? Zn1 N1 2.046(6) . ? Zn1 N2 2.046(5) . ? Zn1 N3 2.045(6) . ? O21 C26 1.332(8) . ? O21 C27 1.421(8) . ? O22 C26 1.213(8) . ? O41 C46 1.308(10) . ? O41 C34 1.454(9) . ? O42 C46 1.215(9) . ? O61 C66 1.355(8) . ? O61 C67 1.449(9) . ? O62 C66 1.198(8) . ? O81 C86 1.322(9) . ? O81 C74 1.472(10) . ? O82 C86 1.203(9) . ? N1 C1 1.369(8) . ? N1 C4 1.394(9) . ? N2 C9 1.357(9) . ? N2 C6 1.388(9) . ? N3 C14 1.357(9) . ? N3 C11 1.372(8) . ? N4 C16 1.365(9) . ? N4 C19 1.384(9) . ? C1 C20 1.393(10) . ? C1 C2 1.442(10) . ? C2 C3 1.345(10) . ? C3 C4 1.411(9) . ? C4 C5 1.383(9) . ? C5 C6 1.382(10) . ? C5 C21 1.532(10) . ? C6 C7 1.428(9) . ? C7 C8 1.343(10) . ? C8 C9 1.446(9) . ? C9 C10 1.400(10) . ? C10 C11 1.386(9) . ? C10 C41 1.518(9) . ? C11 C12 1.452(10) . ? C12 C13 1.319(9) . ? C13 C14 1.439(10) . ? C14 C15 1.415(9) . ? C15 C16 1.377(10) . ? C15 C61 1.517(9) . ? C16 C17 1.442(8) . ? C17 C18 1.334(9) . ? C18 C19 1.445(9) . ? C19 C20 1.405(10) . ? C20 C81 1.493(9) . ? C21 C22 1.496(11) . ? C21 C25 1.519(9) . ? C22 C24 1.501(10) . ? C22 C25 1.501(10) . ? C22 C23 1.525(10) . ? C25 C26 1.475(9) . ? C27 C28 1.519(10) . ? C28 C29 1.500(10) . ? C29 C30 1.527(11) . ? C30 C31 1.511(13) . ? C31 C32 1.534(13) . ? C32 C33 1.555(13) . ? C33 C34 1.473(13) . ? C41 C45 1.518(10) . ? C41 C42 1.527(10) . ? C42 C43 1.505(11) . ? C42 C44 1.504(10) . ? C42 C45 1.545(11) . ? C45 C46 1.512(11) . ? C61 C62 1.514(9) . ? C61 C65 1.558(9) . ? C62 C64 1.498(11) . ? C62 C63 1.509(9) . ? C62 C65 1.550(9) . ? C65 C66 1.452(10) . ? C67 C68 1.519(10) . ? C68 C69 1.510(12) . ? C69 C70 1.533(12) . ? C70 C71 1.542(12) . ? C71 C72 1.483(12) . ? C72 C73 1.536(12) . ? C73 C74 1.498(12) . ? C81 C82 1.508(9) . ? C81 C85 1.539(11) . ? C82 C83 1.524(10) . ? C82 C85 1.529(11) . ? C82 C84 1.518(10) . ? C85 C86 1.481(11) . ? Zn2 N102 2.030(5) . ? Zn2 N101 2.026(6) . ? Zn2 N104 2.034(5) . ? Zn2 N103 2.029(6) . ? O121 C126 1.328(8) . ? O121 C127 1.464(8) . ? O122 C126 1.214(8) . ? O141 C146 1.349(10) . ? O141 C134 1.443(9) . ? O142 C146 1.203(9) . ? O161 C166 1.331(8) . ? O161 C167 1.456(9) . ? O162 C166 1.228(8) . ? O181 C186 1.311(9) . ? O181 C174 1.445(9) . ? O182 C186 1.193(9) . ? N101 C101 1.377(8) . ? N101 C104 1.387(8) . ? N102 C106 1.366(9) . ? N102 C109 1.389(9) . ? N103 C114 1.378(8) . ? N103 C111 1.381(9) . ? N104 C119 1.376(9) . ? N104 C116 1.378(8) . ? C101 C120 1.394(9) . ? C101 C102 1.444(10) . ? C102 C103 1.346(10) . ? C103 C104 1.445(9) . ? C104 C105 1.398(10) . ? C105 C106 1.414(9) . ? C105 C121 1.485(9) . ? C106 C107 1.456(10) . ? C107 C108 1.351(10) . ? C108 C109 1.427(8) . ? C109 C110 1.389(10) . ? C110 C111 1.408(9) . ? C110 C141 1.502(10) . ? C111 C112 1.444(10) . ? C112 C113 1.351(9) . ? C113 C114 1.438(9) . ? C114 C115 1.393(9) . ? C115 C116 1.397(9) . ? C115 C161 1.495(9) . ? C116 C117 1.449(9) . ? C117 C118 1.348(9) . ? C118 C119 1.435(8) . ? C119 C120 1.402(10) . ? C120 C181 1.523(9) . ? C121 C122 1.486(10) . ? C121 C125 1.554(9) . ? C122 C123 1.528(10) . ? C122 C124 1.535(10) . ? C122 C125 1.546(10) . ? C125 C126 1.454(9) . ? C127 C128 1.515(10) . ? C128 C129 1.506(11) . ? C129 C130 1.545(12) . ? C130 C131 1.533(13) . ? C131 C132 1.452(14) . ? C132 C133 1.555(13) . ? C133 C134 1.458(13) . ? C141 C142 1.529(9) . ? C141 C145 1.518(9) . ? C142 C143 1.514(11) . ? C142 C145 1.526(10) . ? C142 C144 1.516(10) . ? C145 C146 1.468(10) . ? C161 C162 1.510(9) . ? C161 C165 1.528(8) . ? C162 C164 1.506(10) . ? C162 C165 1.535(9) . ? C162 C163 1.523(9) . ? C165 C166 1.479(10) . ? C167 C168 1.506(11) . ? C168 C169 1.512(11) . ? C169 C170 1.527(11) . ? C170 C171 1.540(12) . ? C171 C172 1.498(12) . ? C172 C173 1.500(12) . ? C173 C174 1.508(12) . ? C181 C182 1.524(10) . ? C181 C185 1.502(11) . ? C182 C184 1.509(9) . ? C182 C185 1.507(10) . ? C182 C183 1.519(11) . ? C185 C186 1.497(11) . ? C201 Cl13 1.711(15) . ? C201 Cl11 1.743(15) . ? C201 Cl12 1.768(17) . ? C202 Cl21 1.686(12) . ? C202 Cl23 1.722(13) . ? C202 Cl22 1.788(15) . ? C203 Cl33 1.752(9) . ? C203 Cl31 1.739(10) . ? C203 Cl32 1.749(9) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N4 Zn1 N1 90.6(2) . . ? N4 Zn1 N2 178.9(2) . . ? N1 Zn1 N2 89.6(2) . . ? N4 Zn1 N3 89.4(2) . . ? N1 Zn1 N3 178.4(2) . . ? N2 Zn1 N3 90.4(2) . . ? C26 O21 C27 116.2(5) . . ? C46 O41 C34 116.2(6) . . ? C66 O61 C67 115.9(5) . . ? C86 O81 C74 116.4(6) . . ? C1 N1 C4 106.8(5) . . ? C1 N1 Zn1 125.8(5) . . ? C4 N1 Zn1 126.4(4) . . ? C9 N2 C6 107.1(6) . . ? C9 N2 Zn1 126.0(5) . . ? C6 N2 Zn1 126.6(4) . . ? C14 N3 C11 107.9(6) . . ? C14 N3 Zn1 126.3(4) . . ? C11 N3 Zn1 125.3(4) . . ? C16 N4 C19 106.3(5) . . ? C16 N4 Zn1 127.3(5) . . ? C19 N4 Zn1 125.6(5) . . ? N1 C1 C20 125.8(6) . . ? N1 C1 C2 108.4(6) . . ? C20 C1 C2 125.9(6) . . ? C3 C2 C1 107.8(6) . . ? C2 C3 C4 107.8(6) . . ? C5 C4 N1 125.1(6) . . ? C5 C4 C3 125.6(6) . . ? N1 C4 C3 109.1(6) . . ? C4 C5 C6 126.2(7) . . ? C4 C5 C21 115.5(6) . . ? C6 C5 C21 118.0(6) . . ? C5 C6 N2 125.4(6) . . ? C5 C6 C7 125.5(6) . . ? N2 C6 C7 109.0(6) . . ? C8 C7 C6 107.3(6) . . ? C7 C8 C9 107.7(6) . . ? N2 C9 C10 126.0(6) . . ? N2 C9 C8 108.8(6) . . ? C10 C9 C8 125.0(6) . . ? C11 C10 C9 125.5(6) . . ? C11 C10 C41 117.9(6) . . ? C9 C10 C41 116.3(6) . . ? N3 C11 C10 126.1(6) . . ? N3 C11 C12 106.8(6) . . ? C10 C11 C12 127.0(6) . . ? C13 C12 C11 109.1(6) . . ? C12 C13 C14 106.6(6) . . ? N3 C14 C15 125.9(6) . . ? N3 C14 C13 109.4(5) . . ? C15 C14 C13 124.6(6) . . ? C16 C15 C14 124.4(6) . . ? C16 C15 C61 119.1(6) . . ? C14 C15 C61 116.1(6) . . ? N4 C16 C15 125.8(6) . . ? N4 C16 C17 109.9(6) . . ? C15 C16 C17 124.3(6) . . ? C18 C17 C16 107.2(6) . . ? C17 C18 C19 107.7(6) . . ? N4 C19 C20 126.3(6) . . ? N4 C19 C18 108.9(6) . . ? C20 C19 C18 124.6(6) . . ? C1 C20 C19 124.8(6) . . ? C1 C20 C81 120.5(6) . . ? C19 C20 C81 114.3(6) . . ? C5 C21 C22 125.0(6) . . ? C5 C21 C25 126.1(6) . . ? C22 C21 C25 59.7(5) . . ? C24 C22 C25 114.5(6) . . ? C24 C22 C21 117.4(7) . . ? C25 C22 C21 60.9(5) . . ? C24 C22 C23 114.1(7) . . ? C25 C22 C23 119.3(6) . . ? C21 C22 C23 120.5(6) . . ? C26 C25 C22 122.9(6) . . ? C26 C25 C21 124.7(6) . . ? C22 C25 C21 59.4(5) . . ? O22 C26 O21 122.4(6) . . ? O22 C26 C25 122.3(6) . . ? O21 C26 C25 115.2(5) . . ? O21 C27 C28 108.7(6) . . ? C29 C28 C27 110.8(6) . . ? C28 C29 C30 114.9(7) . . ? C31 C30 C29 116.5(7) . . ? C32 C31 C30 113.2(7) . . ? C31 C32 C33 113.7(7) . . ? C34 C33 C32 112.7(7) . . ? O41 C34 C33 107.2(7) . . ? C10 C41 C45 127.1(6) . . ? C10 C41 C42 123.9(7) . . ? C45 C41 C42 61.0(5) . . ? C43 C42 C44 114.9(7) . . ? C43 C42 C41 121.3(6) . . ? C44 C42 C41 116.0(7) . . ? C43 C42 C45 120.2(6) . . ? C44 C42 C45 113.8(7) . . ? C41 C42 C45 59.2(5) . . ? C46 C45 C41 127.8(6) . . ? C46 C45 C42 123.1(7) . . ? C41 C45 C42 59.8(4) . . ? O42 C46 O41 124.0(8) . . ? O42 C46 C45 120.4(9) . . ? O41 C46 C45 115.6(6) . . ? C62 C61 C15 125.6(5) . . ? C62 C61 C65 60.6(4) . . ? C15 C61 C65 122.7(6) . . ? C64 C62 C61 115.9(6) . . ? C64 C62 C63 114.8(6) . . ? C61 C62 C63 120.8(6) . . ? C64 C62 C65 115.0(6) . . ? C61 C62 C65 61.1(4) . . ? C63 C62 C65 118.8(6) . . ? C66 C65 C62 126.6(6) . . ? C66 C65 C61 125.5(6) . . ? C62 C65 C61 58.3(4) . . ? O62 C66 O61 121.3(7) . . ? O62 C66 C65 122.2(6) . . ? O61 C66 C65 116.5(5) . . ? O61 C67 C68 109.9(6) . . ? C69 C68 C67 111.1(6) . . ? C68 C69 C70 116.0(7) . . ? C71 C70 C69 115.8(7) . . ? C72 C71 C70 114.1(7) . . ? C71 C72 C73 114.1(7) . . ? C72 C73 C74 112.8(7) . . ? O81 C74 C73 106.0(7) . . ? C20 C81 C82 124.4(6) . . ? C20 C81 C85 125.2(6) . . ? C82 C81 C85 60.2(5) . . ? C81 C82 C83 121.1(6) . . ? C81 C82 C85 60.9(5) . . ? C83 C82 C85 119.4(7) . . ? C81 C82 C84 117.3(7) . . ? C83 C82 C84 113.4(7) . . ? C85 C82 C84 115.1(6) . . ? C86 C85 C82 126.1(7) . . ? C86 C85 C81 127.8(6) . . ? C82 C85 C81 58.9(5) . . ? O82 C86 O81 123.8(8) . . ? O82 C86 C85 122.2(7) . . ? O81 C86 C85 114.0(7) . . ? N102 Zn2 N101 90.8(2) . . ? N102 Zn2 N104 178.5(3) . . ? N101 Zn2 N104 88.9(2) . . ? N102 Zn2 N103 89.7(2) . . ? N101 Zn2 N103 179.4(2) . . ? N104 Zn2 N103 90.5(2) . . ? C126 O121 C127 115.2(5) . . ? C146 O141 C134 116.8(6) . . ? C166 O161 C167 115.7(6) . . ? C186 O181 C174 118.0(6) . . ? C101 N101 C104 106.8(5) . . ? C101 N101 Zn2 127.0(4) . . ? C104 N101 Zn2 125.0(4) . . ? C106 N102 C109 105.9(5) . . ? C106 N102 Zn2 127.1(4) . . ? C109 N102 Zn2 126.7(4) . . ? C114 N103 C111 107.0(6) . . ? C114 N103 Zn2 126.2(5) . . ? C111 N103 Zn2 126.6(4) . . ? C119 N104 C116 105.3(5) . . ? C119 N104 Zn2 127.8(4) . . ? C116 N104 Zn2 126.4(4) . . ? N101 C101 C120 125.7(6) . . ? N101 C101 C102 109.4(6) . . ? C120 C101 C102 124.8(6) . . ? C103 C102 C101 107.2(6) . . ? C102 C103 C104 108.0(6) . . ? C105 C104 N101 126.9(6) . . ? C105 C104 C103 124.4(6) . . ? N101 C104 C103 108.6(6) . . ? C104 C105 C106 124.2(6) . . ? C104 C105 C121 117.5(6) . . ? C106 C105 C121 118.1(6) . . ? N102 C106 C105 125.3(6) . . ? N102 C106 C107 109.6(6) . . ? C105 C106 C107 125.1(6) . . ? C108 C107 C106 107.1(6) . . ? C107 C108 C109 107.0(6) . . ? C110 C109 N102 126.6(6) . . ? C110 C109 C108 123.0(6) . . ? N102 C109 C108 110.4(6) . . ? C109 C110 C111 123.3(6) . . ? C109 C110 C141 116.5(6) . . ? C111 C110 C141 119.9(6) . . ? N103 C111 C110 126.4(6) . . ? N103 C111 C112 109.2(6) . . ? C110 C111 C112 124.4(6) . . ? C113 C112 C111 106.8(6) . . ? C112 C113 C114 108.2(6) . . ? N103 C114 C115 125.6(6) . . ? N103 C114 C113 108.7(6) . . ? C115 C114 C113 125.6(6) . . ? C114 C115 C116 125.9(6) . . ? C114 C115 C161 116.8(6) . . ? C116 C115 C161 117.0(6) . . ? C115 C116 N104 124.8(5) . . ? C115 C116 C117 125.8(6) . . ? N104 C116 C117 109.3(6) . . ? C118 C117 C116 108.0(6) . . ? C117 C118 C119 106.0(6) . . ? N104 C119 C120 125.0(6) . . ? N104 C119 C118 111.4(6) . . ? C120 C119 C118 123.5(6) . . ? C101 C120 C119 124.2(6) . . ? C101 C120 C181 120.2(6) . . ? C119 C120 C181 115.3(6) . . ? C122 C121 C105 124.0(6) . . ? C122 C121 C125 61.1(5) . . ? C105 C121 C125 125.2(6) . . ? C121 C122 C123 122.2(6) . . ? C121 C122 C124 116.5(6) . . ? C123 C122 C124 112.9(7) . . ? C121 C122 C125 61.6(4) . . ? C123 C122 C125 119.1(6) . . ? C124 C122 C125 115.4(6) . . ? C126 C125 C122 124.3(6) . . ? C126 C125 C121 127.7(5) . . ? C122 C125 C121 57.3(4) . . ? O122 C126 O121 122.4(6) . . ? O122 C126 C125 122.5(6) . . ? O121 C126 C125 115.1(6) . . ? O121 C127 C128 109.6(6) . . ? C129 C128 C127 111.8(7) . . ? C128 C129 C130 113.3(7) . . ? C131 C130 C129 115.4(8) . . ? C132 C131 C130 115.5(9) . . ? C131 C132 C133 113.5(8) . . ? C134 C133 C132 111.8(8) . . ? O141 C134 C133 107.0(7) . . ? C110 C141 C142 124.0(6) . . ? C110 C141 C145 126.6(6) . . ? C142 C141 C145 60.1(4) . . ? C143 C142 C145 119.0(6) . . ? C143 C142 C141 120.0(6) . . ? C145 C142 C141 59.6(4) . . ? C143 C142 C144 114.8(6) . . ? C145 C142 C144 114.6(7) . . ? C141 C142 C144 117.7(7) . . ? C146 C145 C142 124.3(7) . . ? C146 C145 C141 127.9(6) . . ? C142 C145 C141 60.3(4) . . ? O142 C146 O141 123.2(8) . . ? O142 C146 C145 122.1(9) . . ? O141 C146 C145 114.7(6) . . ? C115 C161 C162 124.4(5) . . ? C115 C161 C165 125.1(6) . . ? C162 C161 C165 60.7(4) . . ? C164 C162 C161 117.1(6) . . ? C164 C162 C165 116.2(5) . . ? C161 C162 C165 60.2(4) . . ? C164 C162 C163 111.9(6) . . ? C161 C162 C163 122.0(5) . . ? C165 C162 C163 120.5(6) . . ? C166 C165 C161 125.5(5) . . ? C166 C165 C162 123.6(6) . . ? C161 C165 C162 59.1(4) . . ? O162 C166 O161 121.6(7) . . ? O162 C166 C165 123.4(6) . . ? O161 C166 C165 115.0(6) . . ? O161 C167 C168 108.4(6) . . ? C167 C168 C169 109.6(7) . . ? C168 C169 C170 114.2(7) . . ? C169 C170 C171 114.3(7) . . ? C172 C171 C170 113.5(8) . . ? C173 C172 C171 114.0(8) . . ? C172 C173 C174 114.6(8) . . ? O181 C174 C173 108.4(7) . . ? C120 C181 C182 124.1(6) . . ? C120 C181 C185 126.8(6) . . ? C182 C181 C185 59.7(5) . . ? C184 C182 C181 118.1(7) . . ? C184 C182 C185 115.9(7) . . ? C181 C182 C185 59.4(5) . . ? C184 C182 C183 113.4(6) . . ? C181 C182 C183 120.2(6) . . ? C185 C182 C183 119.7(7) . . ? C186 C185 C182 124.4(7) . . ? C186 C185 C181 128.7(6) . . ? C182 C185 C181 60.8(5) . . ? O182 C186 O181 123.9(8) . . ? O182 C186 C185 120.5(7) . . ? O181 C186 C185 115.5(7) . . ? Cl13 C201 Cl11 111.7(9) . . ? Cl13 C201 Cl12 110.3(9) . . ? Cl11 C201 Cl12 110.0(9) . . ? Cl21 C202 Cl23 111.8(8) . . ? Cl21 C202 Cl22 109.1(8) . . ? Cl23 C202 Cl22 112.0(6) . . ? Cl33 C203 Cl31 111.4(5) . . ? Cl33 C203 Cl32 109.9(5) . . ? Cl31 C203 Cl32 111.0(5) . . ? _diffrn_measured_fraction_theta_max 0.678 _diffrn_reflns_theta_full 29.07 _diffrn_measured_fraction_theta_full 0.678 _refine_diff_density_max 0.913 _refine_diff_density_min -0.677 _refine_diff_density_rms 0.082