Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2001 data_global _journal_coden_Cambridge 182 loop_ _publ_author_name 'Baylies, C. J.' 'Harding, L. P.' 'Jeffrey, John C.' 'Paul, Rowena L.' 'Rice, C. R.' 'Ward, Mike' _publ_contact_author 'Dr. Craig Rice' _publ_contact_author_address ; Dr. Craig Rice Department of Chemistry and Biological Sciences University of Huddersfield Huddersfield HD1 3DH UNITED KINGDOM ; _publ_contact_author_fax '01484 472182' _publ_contact_author_email c.r.rice@hud.ac.uk _publ_contact_letter ; This CIF file contains details of the two crystal structures in the paper Pyridyl-thiazole multidentate ligands: metal-specific recognition of a combination of ligands from a mixture ' by Craig Rice, et al, submitted to Chemical Communications for publication. ; #======================================================== data_zinc _database_code_CSD 163221 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C54 H38 Cl4 N14 O20 S4 Zn2' _chemical_formula_weight 1603.76 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 '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 P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.2805(18) _cell_length_b 12.5562(18) _cell_length_c 21.182(3) _cell_angle_alpha 90.258(2) _cell_angle_beta 103.166(2) _cell_angle_gamma 100.171(2) _cell_volume 3127.0(8) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.6 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.703 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1624 _exptl_absorpt_coefficient_mu 1.160 _exptl_absorpt_correction_type 'Empirical, pseudo-azimuthal scan (SADABS)' _exptl_absorpt_correction_T_min 0.50 _exptl_absorpt_correction_T_max 0.78 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'Siemens SMART Area Detector' _diffrn_measurement_method '\w rotation with narrow frames (0.3 degrees)' _diffrn_detector_area_resol_mean ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 32976 _diffrn_reflns_av_R_equivalents 0.0371 _diffrn_reflns_av_sigmaI/netI 0.0618 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.65 _diffrn_reflns_theta_max 27.51 _reflns_number_total 14215 _reflns_number_gt 9532 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0634P)^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 14215 _refine_ls_number_parameters 928 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0637 _refine_ls_R_factor_gt 0.0432 _refine_ls_wR_factor_ref 0.1203 _refine_ls_wR_factor_gt 0.1152 _refine_ls_goodness_of_fit_ref 0.958 _refine_ls_restrained_S_all 0.958 _refine_ls_shift/su_max 0.026 _refine_ls_shift/su_mean 0.002 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zn1 Zn 0.24629(3) 0.33151(3) 0.843822(17) 0.02887(10) Uani 1 1 d . . . Zn2 Zn 0.19485(3) 0.13115(3) 0.653029(17) 0.02903(10) Uani 1 1 d . . . Cl1 Cl 0.81822(7) 0.32931(6) 0.09800(4) 0.03394(18) Uani 1 1 d . . . Cl2 Cl 0.29033(10) 0.05377(9) 0.08941(5) 0.0565(3) Uani 1 1 d . . . Cl3 Cl 0.23902(9) 0.78375(9) 0.55673(5) 0.0564(3) Uani 1 1 d . . . Cl4 Cl 0.26809(7) 0.46394(7) 0.36029(4) 0.0378(2) Uani 1 1 d . . . S103 S 0.41653(7) 0.06465(7) 0.93888(4) 0.0376(2) Uani 1 1 d . . . S113 S 0.03525(6) 0.53559(6) 0.71440(4) 0.03041(18) Uani 1 1 d . . . S203 S 0.32956(7) -0.11745(7) 0.78447(4) 0.0351(2) Uani 1 1 d . . . S213 S 0.03371(8) 0.40084(8) 0.55656(4) 0.0412(2) Uani 1 1 d . . . N101 N 0.3402(2) 0.2266(2) 0.88840(11) 0.0263(5) Uani 1 1 d . . . N251 N 0.1384(2) 0.12436(19) 0.81701(11) 0.0247(5) Uani 1 1 d . . . N141 N 0.30423(19) 0.39035(19) 0.74199(11) 0.0239(5) Uani 1 1 d . . . N111 N 0.1361(2) 0.41635(19) 0.79430(11) 0.0249(5) Uani 1 1 d . . . N121 N 0.1098(2) 0.3117(2) 0.89728(12) 0.0283(6) Uani 1 1 d . . . N131 N 0.4048(2) 0.4369(2) 0.88833(12) 0.0289(6) Uani 1 1 d . . . N241 N 0.0307(2) 0.19549(19) 0.69886(11) 0.0244(5) Uani 1 1 d . . . N201 N 0.2345(2) 0.00839(19) 0.70650(12) 0.0254(5) Uani 1 1 d . . . N207 N 0.37631(19) 0.19235(19) 0.73915(11) 0.0232(5) Uani 1 1 d . . . N211 N 0.1436(2) 0.25950(19) 0.60824(11) 0.0253(5) Uani 1 1 d . . . N221 N 0.0488(2) 0.0031(2) 0.61701(12) 0.0278(6) Uani 1 1 d . . . N231 N 0.3134(2) 0.1698(2) 0.59203(12) 0.0307(6) Uani 1 1 d . . . N400 N 0.7139(3) 0.6066(3) 0.81222(16) 0.0478(8) Uani 1 1 d . . . O3 O 0.7829(2) 0.3279(2) 0.15809(11) 0.0520(7) Uani 1 1 d . . . O11 O 0.9331(2) 0.3126(2) 0.10949(15) 0.0656(8) Uani 1 1 d . . . O12 O 0.7458(2) 0.24460(19) 0.05425(12) 0.0477(6) Uani 1 1 d . . . O13 O 0.8092(2) 0.43210(19) 0.07039(11) 0.0434(6) Uani 1 1 d . . . O21 O 0.2968(3) -0.0420(2) 0.05653(15) 0.0739(9) Uani 1 1 d . . . O22 O 0.2679(3) 0.0354(3) 0.15059(15) 0.0937(12) Uani 1 1 d . . . O23A O 0.2728(12) 0.1411(7) 0.0566(6) 0.125(6) Uani 0.50 1 d P . . O23B O 0.1933(12) 0.0867(13) 0.0540(6) 0.182(8) Uani 0.50 1 d P . . O24 O 0.4124(4) 0.1095(3) 0.1073(2) 0.1277(16) Uani 1 1 d . . . O31A O 0.2928(17) 0.7014(11) 0.5440(8) 0.139(8) Uani 0.50 1 d P . . O31B O 0.2696(18) 0.7107(14) 0.5237(8) 0.157(7) Uani 0.50 1 d P . . O32A O 0.2432(17) 0.8412(10) 0.5018(4) 0.213(9) Uani 0.50 1 d P . . O32B O 0.1599(9) 0.8315(9) 0.5259(5) 0.134(4) Uani 0.50 1 d P . . O33 O 0.1463(3) 0.7199(4) 0.5853(2) 0.1198(15) Uani 1 1 d . . . O34A O 0.3026(11) 0.8648(10) 0.6060(6) 0.130(7) Uani 0.50 1 d P . . O34B O 0.3102(11) 0.8115(9) 0.6118(5) 0.097(4) Uani 0.50 1 d P . . O401 O 0.6170(2) 0.6107(3) 0.78425(14) 0.0648(8) Uani 1 1 d . . . O402 O 0.7460(2) 0.5231(2) 0.83177(14) 0.0590(7) Uani 1 1 d . . . O42 O 0.29538(19) 0.55856(19) 0.32593(12) 0.0430(6) Uani 1 1 d . . . O41 O 0.1945(2) 0.3831(2) 0.31270(16) 0.0681(9) Uani 1 1 d . . . O43 O 0.3671(2) 0.4209(2) 0.38871(13) 0.0607(8) Uani 1 1 d . . . O44 O 0.2064(3) 0.4845(3) 0.40582(15) 0.0862(11) Uani 1 1 d . . . C102 C 0.3093(3) 0.1212(3) 0.89341(14) 0.0276(7) Uani 1 1 d . . . C104 C 0.5034(3) 0.1887(3) 0.95226(15) 0.0363(8) Uani 1 1 d . . . H104 H 0.5794 0.2019 0.9776 0.044 Uiso 1 1 calc R . . C105 C 0.4492(2) 0.2656(3) 0.92187(14) 0.0287(7) Uani 1 1 d . . . C112 C 0.1482(2) 0.4730(2) 0.74383(14) 0.0254(6) Uani 1 1 d . . . C114 C -0.0291(3) 0.4830(2) 0.77385(15) 0.0310(7) Uani 1 1 d . . . H114 H -0.1008 0.4950 0.7790 0.037 Uiso 1 1 calc R . . C115 C 0.0372(2) 0.4212(2) 0.81288(14) 0.0270(6) Uani 1 1 d . . . C122 C 0.0206(3) 0.3584(2) 0.86924(14) 0.0290(7) Uani 1 1 d . . . C123 C -0.0791(3) 0.3441(3) 0.89127(17) 0.0421(9) Uani 1 1 d . . . H123 H -0.1399 0.3793 0.8715 0.050 Uiso 1 1 calc R . . C124 C -0.0879(3) 0.2781(4) 0.94221(19) 0.0532(10) Uani 1 1 d . . . H124 H -0.1559 0.2658 0.9574 0.064 Uiso 1 1 calc R . . C125 C 0.0022(3) 0.2302(3) 0.97100(17) 0.0481(10) Uani 1 1 d . . . H125 H -0.0025 0.1848 1.0064 0.058 Uiso 1 1 calc R . . C126 C 0.0994(3) 0.2493(3) 0.94753(15) 0.0366(8) Uani 1 1 d . . . H126 H 0.1619 0.2167 0.9678 0.044 Uiso 1 1 calc R . . C132 C 0.4861(2) 0.3838(3) 0.92089(14) 0.0297(7) Uani 1 1 d . . . C133 C 0.5937(3) 0.4368(3) 0.95126(15) 0.0383(8) Uani 1 1 d . . . H133 H 0.6491 0.3976 0.9735 0.046 Uiso 1 1 calc R . . C134 C 0.6193(3) 0.5483(3) 0.94864(17) 0.0458(9) Uani 1 1 d . . . H134 H 0.6925 0.5870 0.9696 0.055 Uiso 1 1 calc R . . C135 C 0.5369(3) 0.6029(3) 0.91511(17) 0.0442(9) Uani 1 1 d . . . H135 H 0.5528 0.6794 0.9125 0.053 Uiso 1 1 calc R . . C136 C 0.4305(3) 0.5437(3) 0.88542(16) 0.0352(7) Uani 1 1 d . . . H136 H 0.3742 0.5811 0.8622 0.042 Uiso 1 1 calc R . . C142 C 0.3984(2) 0.3812(2) 0.72233(14) 0.0251(6) Uani 1 1 d . . . C143 C 0.4419(3) 0.4523(3) 0.68037(15) 0.0314(7) Uani 1 1 d . . . H143 H 0.5105 0.4453 0.6686 0.038 Uiso 1 1 calc R . . C144 C 0.3841(3) 0.5327(3) 0.65625(16) 0.0373(8) Uani 1 1 d . . . H144 H 0.4118 0.5812 0.6268 0.045 Uiso 1 1 calc R . . C145 C 0.2848(3) 0.5434(3) 0.67484(15) 0.0327(7) Uani 1 1 d . . . H145 H 0.2432 0.5982 0.6583 0.039 Uiso 1 1 calc R . . C146 C 0.2490(2) 0.4710(2) 0.71833(14) 0.0259(6) Uani 1 1 d . . . C202 C 0.3285(2) 0.0046(2) 0.74895(14) 0.0258(6) Uani 1 1 d . . . C204 C 0.1947(3) -0.1639(3) 0.73904(15) 0.0335(7) Uani 1 1 d . . . H204 H 0.1518 -0.2340 0.7415 0.040 Uiso 1 1 calc R . . C205 C 0.1577(3) -0.0873(2) 0.69927(14) 0.0274(7) Uani 1 1 d . . . C206 C 0.4166(2) 0.1044(2) 0.76287(14) 0.0261(6) Uani 1 1 d . . . C208 C 0.4498(2) 0.2869(2) 0.74670(14) 0.0248(6) Uani 1 1 d . . . C209 C 0.5650(3) 0.2950(3) 0.77704(15) 0.0317(7) Uani 1 1 d . . . H209 H 0.6159 0.3623 0.7803 0.038 Uiso 1 1 calc R . . C210 C 0.6028(3) 0.2045(3) 0.80186(16) 0.0356(8) Uani 1 1 d . . . H210 H 0.6803 0.2089 0.8236 0.043 Uiso 1 1 calc R . . C211 C 0.5284(3) 0.1064(3) 0.79533(15) 0.0317(7) Uani 1 1 d . . . H211 H 0.5532 0.0427 0.8125 0.038 Uiso 1 1 calc R . . C212 C 0.0519(3) 0.2992(2) 0.60949(14) 0.0274(7) Uani 1 1 d . . . C214 C 0.1552(3) 0.3870(3) 0.53269(16) 0.0409(8) Uani 1 1 d . . . H214 H 0.1851 0.4293 0.5014 0.049 Uiso 1 1 calc R . . C215 C 0.2021(3) 0.3077(3) 0.56472(14) 0.0300(7) Uani 1 1 d . . . C222 C 0.0504(3) -0.0874(2) 0.65110(14) 0.0270(6) Uani 1 1 d . . . C223 C -0.0425(3) -0.1709(3) 0.64181(16) 0.0355(8) Uani 1 1 d . . . H223 H -0.0389 -0.2342 0.6660 0.043 Uiso 1 1 calc R . . C224 C -0.1400(3) -0.1608(3) 0.59709(17) 0.0429(9) Uani 1 1 d . . . H224 H -0.2049 -0.2170 0.5904 0.051 Uiso 1 1 calc R . . C225 C -0.1435(3) -0.0689(3) 0.56194(17) 0.0412(8) Uani 1 1 d . . . H225 H -0.2105 -0.0605 0.5310 0.049 Uiso 1 1 calc R . . C226 C -0.0467(3) 0.0112(3) 0.57295(15) 0.0335(7) Uani 1 1 d . . . H226 H -0.0481 0.0741 0.5483 0.040 Uiso 1 1 calc R . . C232 C 0.3035(3) 0.2629(3) 0.56008(14) 0.0325(7) Uani 1 1 d . . . C233 C 0.3828(3) 0.3097(3) 0.52693(17) 0.0451(9) Uani 1 1 d . . . H233 H 0.3746 0.3748 0.5051 0.054 Uiso 1 1 calc R . . C234 C 0.4741(3) 0.2603(4) 0.52603(19) 0.0574(11) Uani 1 1 d . . . H234 H 0.5300 0.2914 0.5037 0.069 Uiso 1 1 calc R . . C235 C 0.4840(3) 0.1659(4) 0.55738(19) 0.0550(11) Uani 1 1 d . . . H235 H 0.5462 0.1308 0.5568 0.066 Uiso 1 1 calc R . . C236 C 0.4017(3) 0.1228(3) 0.58990(16) 0.0398(8) Uani 1 1 d . . . H236 H 0.4084 0.0573 0.6115 0.048 Uiso 1 1 calc R . . C242 C -0.0204(2) 0.2557(2) 0.65273(14) 0.0259(6) Uani 1 1 d . . . C243 C -0.1316(3) 0.2715(3) 0.64538(15) 0.0319(7) Uani 1 1 d . . . H243 H -0.1639 0.3162 0.6129 0.038 Uiso 1 1 calc R . . C244 C -0.1935(3) 0.2200(3) 0.68699(17) 0.0375(8) Uani 1 1 d . . . H244 H -0.2704 0.2276 0.6830 0.045 Uiso 1 1 calc R . . C245 C -0.1434(3) 0.1575(3) 0.73420(16) 0.0321(7) Uani 1 1 d . . . H245 H -0.1851 0.1216 0.7630 0.039 Uiso 1 1 calc R . . C246 C -0.0300(2) 0.1477(2) 0.73915(14) 0.0243(6) Uani 1 1 d . . . C252 C 0.1943(3) 0.0673(2) 0.86315(14) 0.0271(6) Uani 1 1 d . . . C253 C 0.1451(3) -0.0300(3) 0.88392(16) 0.0380(8) Uani 1 1 d . . . H253 H 0.1878 -0.0681 0.9163 0.046 Uiso 1 1 calc R . . C254 C 0.0322(3) -0.0699(3) 0.85622(17) 0.0425(9) Uani 1 1 d . . . H254 H -0.0046 -0.1361 0.8695 0.051 Uiso 1 1 calc R . . C255 C -0.0266(3) -0.0129(3) 0.80921(16) 0.0361(8) Uani 1 1 d . . . H255 H -0.1045 -0.0393 0.7898 0.043 Uiso 1 1 calc R . . C256 C 0.0287(2) 0.0837(2) 0.79014(14) 0.0259(6) Uani 1 1 d . . . C403 C 0.7991(4) 0.7094(3) 0.8253(3) 0.0744(15) Uani 1 1 d . . . O703 O 0.5868(3) 0.9928(3) 0.68076(19) 0.0909(11) Uani 1 1 d . . . N701 N 0.6145(5) 0.9092(4) 0.6749(3) 0.115(2) Uani 1 1 d . . . C704 C 0.7304(5) 0.9069(4) 0.6962(3) 0.0833(16) Uani 1 1 d . . . O702 O 0.5621(5) 0.8057(4) 0.6906(4) 0.080(2) Uani 0.50 1 d P . . O705 O 0.6077(8) 0.9156(9) 0.6030(5) 0.141(4) Uani 0.50 1 d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.02524(18) 0.0300(2) 0.0321(2) 0.00846(16) 0.00534(15) 0.00850(15) Zn2 0.0305(2) 0.0255(2) 0.0313(2) 0.01091(15) 0.00674(15) 0.00618(15) Cl1 0.0350(4) 0.0299(4) 0.0336(4) -0.0018(3) -0.0018(3) 0.0097(3) Cl2 0.0802(7) 0.0560(6) 0.0494(6) 0.0172(5) 0.0299(5) 0.0352(6) Cl3 0.0510(6) 0.0661(7) 0.0536(6) -0.0037(5) 0.0030(5) 0.0269(5) Cl4 0.0333(4) 0.0420(5) 0.0455(5) 0.0214(4) 0.0197(4) 0.0125(4) S103 0.0384(5) 0.0410(5) 0.0347(4) 0.0146(4) 0.0038(4) 0.0169(4) S113 0.0300(4) 0.0252(4) 0.0363(4) 0.0066(3) 0.0050(3) 0.0089(3) S203 0.0398(5) 0.0266(4) 0.0366(4) 0.0098(3) 0.0015(4) 0.0093(4) S213 0.0463(5) 0.0440(5) 0.0384(5) 0.0221(4) 0.0102(4) 0.0206(4) N101 0.0254(13) 0.0317(15) 0.0220(12) 0.0059(11) 0.0040(10) 0.0078(11) N251 0.0275(13) 0.0246(13) 0.0240(12) 0.0055(10) 0.0086(10) 0.0064(10) N141 0.0246(12) 0.0214(13) 0.0248(12) 0.0040(10) 0.0044(10) 0.0032(10) N111 0.0249(12) 0.0223(13) 0.0275(13) 0.0021(11) 0.0065(10) 0.0040(10) N121 0.0297(13) 0.0270(14) 0.0290(13) 0.0017(11) 0.0083(11) 0.0060(11) N131 0.0296(13) 0.0306(15) 0.0265(13) -0.0010(11) 0.0085(11) 0.0032(11) N241 0.0266(13) 0.0221(13) 0.0245(12) 0.0029(10) 0.0052(10) 0.0053(10) N201 0.0257(13) 0.0236(13) 0.0271(13) 0.0034(10) 0.0050(10) 0.0066(10) N207 0.0244(12) 0.0242(13) 0.0223(12) 0.0054(10) 0.0070(10) 0.0052(10) N211 0.0273(13) 0.0261(14) 0.0221(12) 0.0061(10) 0.0051(10) 0.0044(11) N221 0.0310(14) 0.0235(14) 0.0281(13) 0.0002(11) 0.0059(11) 0.0040(11) N231 0.0309(14) 0.0366(16) 0.0260(13) 0.0052(12) 0.0077(11) 0.0082(12) N400 0.0426(19) 0.053(2) 0.0490(19) -0.0103(16) 0.0159(15) 0.0049(16) O3 0.082(2) 0.0426(15) 0.0337(13) 0.0109(12) 0.0132(13) 0.0167(14) O11 0.0354(14) 0.0617(19) 0.091(2) -0.0158(16) -0.0100(14) 0.0198(13) O12 0.0475(15) 0.0369(14) 0.0483(15) -0.0099(12) -0.0064(12) 0.0031(11) O13 0.0491(15) 0.0350(14) 0.0412(14) 0.0117(11) 0.0019(11) 0.0056(11) O21 0.100(2) 0.0533(19) 0.074(2) -0.0052(16) 0.0290(19) 0.0166(17) O22 0.101(3) 0.153(4) 0.059(2) 0.036(2) 0.0395(19) 0.081(3) O23A 0.270(17) 0.049(5) 0.056(5) 0.026(4) 0.006(9) 0.070(7) O23B 0.243(15) 0.32(2) 0.055(5) 0.048(11) 0.014(9) 0.269(15) O24 0.128(4) 0.089(3) 0.154(4) 0.006(3) 0.039(3) -0.019(3) O31A 0.215(16) 0.102(9) 0.197(15) 0.119(11) 0.165(13) 0.130(11) O31B 0.148(11) 0.193(17) 0.145(12) -0.091(11) 0.060(9) 0.041(12) O32A 0.50(3) 0.148(10) 0.066(6) 0.063(6) 0.084(10) 0.222(15) O32B 0.154(8) 0.159(9) 0.101(7) 0.032(7) -0.028(6) 0.135(8) O33 0.089(3) 0.145(4) 0.127(4) -0.021(3) 0.029(3) 0.022(3) O34A 0.133(9) 0.115(10) 0.135(10) -0.089(8) 0.098(8) -0.077(8) O34B 0.104(7) 0.111(10) 0.046(4) -0.008(5) -0.028(4) -0.003(7) O401 0.0371(15) 0.094(2) 0.0578(18) -0.0053(16) 0.0062(13) 0.0035(15) O402 0.0666(19) 0.0458(17) 0.071(2) 0.0017(15) 0.0290(15) 0.0107(14) O42 0.0388(13) 0.0410(14) 0.0562(16) 0.0249(12) 0.0206(12) 0.0130(11) O41 0.0569(18) 0.0451(17) 0.092(2) 0.0076(16) 0.0054(16) -0.0030(14) O43 0.0433(15) 0.077(2) 0.0687(19) 0.0448(16) 0.0156(13) 0.0261(14) O44 0.110(3) 0.116(3) 0.071(2) 0.053(2) 0.065(2) 0.065(2) C102 0.0325(16) 0.0324(18) 0.0208(14) 0.0083(13) 0.0079(12) 0.0110(14) C104 0.0297(17) 0.047(2) 0.0314(17) 0.0082(15) 0.0029(14) 0.0113(15) C105 0.0240(15) 0.0406(19) 0.0221(15) 0.0035(13) 0.0059(12) 0.0067(14) C112 0.0272(15) 0.0208(15) 0.0278(15) 0.0033(12) 0.0053(12) 0.0045(12) C114 0.0291(16) 0.0253(17) 0.0396(18) 0.0022(14) 0.0081(14) 0.0074(13) C115 0.0245(15) 0.0244(16) 0.0315(16) -0.0023(13) 0.0065(13) 0.0032(12) C122 0.0288(16) 0.0276(17) 0.0301(16) -0.0019(13) 0.0078(13) 0.0025(13) C123 0.0326(18) 0.055(2) 0.043(2) 0.0093(18) 0.0149(16) 0.0128(17) C124 0.042(2) 0.075(3) 0.049(2) 0.013(2) 0.0259(18) 0.008(2) C125 0.052(2) 0.060(3) 0.037(2) 0.0178(18) 0.0197(17) 0.010(2) C126 0.0424(19) 0.039(2) 0.0298(17) 0.0070(15) 0.0092(15) 0.0111(16) C132 0.0275(16) 0.0406(19) 0.0212(15) 0.0005(13) 0.0070(12) 0.0045(14) C133 0.0298(17) 0.053(2) 0.0301(17) -0.0001(16) 0.0080(14) 0.0014(16) C134 0.0356(19) 0.057(3) 0.038(2) -0.0095(18) 0.0106(16) -0.0115(18) C135 0.054(2) 0.036(2) 0.043(2) -0.0074(16) 0.0240(18) -0.0083(17) C136 0.0399(19) 0.0318(19) 0.0354(18) -0.0006(14) 0.0148(15) 0.0030(15) C142 0.0227(14) 0.0236(16) 0.0270(15) 0.0049(12) 0.0044(12) 0.0004(12) C143 0.0257(15) 0.0325(18) 0.0373(18) 0.0108(14) 0.0125(14) 0.0017(13) C144 0.0347(18) 0.0347(19) 0.0409(19) 0.0140(15) 0.0111(15) -0.0017(15) C145 0.0333(17) 0.0291(18) 0.0356(18) 0.0105(14) 0.0078(14) 0.0054(14) C146 0.0254(15) 0.0224(16) 0.0276(15) 0.0042(12) 0.0028(12) 0.0026(12) C202 0.0300(16) 0.0227(16) 0.0272(15) 0.0041(12) 0.0088(13) 0.0083(12) C204 0.0373(18) 0.0244(17) 0.0357(18) 0.0052(14) 0.0042(14) 0.0031(14) C205 0.0307(16) 0.0228(16) 0.0293(16) 0.0009(13) 0.0095(13) 0.0029(13) C206 0.0281(15) 0.0303(17) 0.0231(15) 0.0057(13) 0.0091(12) 0.0094(13) C208 0.0244(15) 0.0278(16) 0.0252(15) 0.0037(12) 0.0107(12) 0.0058(12) C209 0.0254(16) 0.0334(18) 0.0350(17) 0.0028(14) 0.0067(13) 0.0020(13) C210 0.0209(15) 0.045(2) 0.0395(19) 0.0042(16) 0.0023(14) 0.0074(14) C211 0.0285(16) 0.0352(19) 0.0325(17) 0.0082(14) 0.0052(13) 0.0112(14) C212 0.0304(16) 0.0244(16) 0.0261(15) 0.0058(13) 0.0016(13) 0.0080(13) C214 0.048(2) 0.045(2) 0.0333(18) 0.0202(16) 0.0134(16) 0.0121(17) C215 0.0355(17) 0.0315(18) 0.0237(15) 0.0084(13) 0.0091(13) 0.0050(14) C222 0.0325(16) 0.0244(16) 0.0250(15) 0.0002(12) 0.0066(13) 0.0076(13) C223 0.0380(18) 0.0264(17) 0.0392(19) 0.0049(14) 0.0063(15) 0.0017(14) C224 0.0363(19) 0.036(2) 0.049(2) -0.0030(17) 0.0033(16) -0.0057(16) C225 0.0371(19) 0.041(2) 0.0380(19) -0.0042(16) -0.0043(15) 0.0052(16) C226 0.0384(18) 0.0327(18) 0.0281(16) 0.0026(14) 0.0032(14) 0.0092(15) C232 0.0365(18) 0.0379(19) 0.0221(15) 0.0072(14) 0.0081(13) 0.0027(15) C233 0.047(2) 0.056(2) 0.0363(19) 0.0140(17) 0.0197(17) 0.0073(18) C234 0.045(2) 0.084(3) 0.050(2) 0.013(2) 0.0264(19) 0.007(2) C235 0.043(2) 0.081(3) 0.049(2) 0.007(2) 0.0179(18) 0.024(2) C236 0.0388(19) 0.051(2) 0.0356(19) 0.0068(16) 0.0127(15) 0.0176(17) C242 0.0318(16) 0.0204(15) 0.0250(15) 0.0020(12) 0.0052(12) 0.0049(12) C243 0.0299(16) 0.0310(18) 0.0350(17) 0.0060(14) 0.0028(14) 0.0119(14) C244 0.0302(17) 0.038(2) 0.047(2) 0.0042(16) 0.0094(15) 0.0121(15) C245 0.0311(17) 0.0295(18) 0.0382(18) 0.0030(14) 0.0128(14) 0.0060(14) C246 0.0250(15) 0.0217(15) 0.0251(15) 0.0002(12) 0.0049(12) 0.0028(12) C252 0.0305(16) 0.0265(16) 0.0270(15) 0.0056(13) 0.0098(13) 0.0087(13) C253 0.047(2) 0.0313(19) 0.0371(19) 0.0163(15) 0.0089(16) 0.0108(16) C254 0.046(2) 0.0305(19) 0.047(2) 0.0157(16) 0.0105(17) -0.0028(16) C255 0.0313(17) 0.0340(19) 0.0390(19) 0.0076(15) 0.0068(14) -0.0027(14) C256 0.0286(15) 0.0271(16) 0.0249(15) 0.0034(12) 0.0112(12) 0.0067(13) C403 0.045(2) 0.038(2) 0.125(4) -0.017(3) 0.003(3) -0.0100(19) O703 0.098(3) 0.067(2) 0.102(3) -0.010(2) -0.003(2) 0.034(2) N701 0.104(4) 0.082(4) 0.183(6) -0.035(4) 0.083(4) 0.019(3) C704 0.070(3) 0.077(4) 0.101(4) -0.018(3) 0.021(3) 0.009(3) O702 0.069(4) 0.027(3) 0.132(6) 0.017(3) 0.005(4) 0.004(3) O705 0.113(7) 0.205(11) 0.119(8) 0.009(7) 0.046(6) 0.045(7) _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 N111 1.984(2) . ? Zn1 N101 2.002(2) . ? Zn1 N131 2.161(3) . ? Zn1 N121 2.208(2) . ? Zn1 N141 2.496(2) . ? Zn2 N201 1.981(2) . ? Zn2 N211 1.998(2) . ? Zn2 N231 2.153(3) . ? Zn2 N221 2.175(2) . ? Cl1 O11 1.428(3) . ? Cl1 O13 1.431(2) . ? Cl1 O3 1.435(3) . ? Cl1 O12 1.436(2) . ? Cl2 O23A 1.325(8) . ? Cl2 O23B 1.386(9) . ? Cl2 O22 1.397(3) . ? Cl2 O21 1.410(3) . ? Cl2 O24 1.500(4) . ? Cl3 O32B 1.284(6) . ? Cl3 O34B 1.293(9) . ? Cl3 O31B 1.307(14) . ? Cl3 O31A 1.378(12) . ? Cl3 O32A 1.379(9) . ? Cl3 O34A 1.440(11) . ? Cl3 O33 1.517(5) . ? Cl4 O44 1.404(3) . ? Cl4 O42 1.425(2) . ? Cl4 O43 1.426(2) . ? Cl4 O41 1.455(3) . ? S103 C104 1.708(4) . ? S103 C102 1.710(3) . ? S113 C114 1.709(3) . ? S113 C112 1.710(3) . ? S203 C202 1.711(3) . ? S203 C204 1.714(3) . ? S213 C212 1.714(3) . ? S213 C214 1.716(4) . ? N101 C102 1.323(4) . ? N101 C105 1.366(4) . ? N251 C256 1.343(4) . ? N251 C252 1.347(4) . ? N141 C142 1.338(4) . ? N141 C146 1.353(4) . ? N111 C112 1.309(4) . ? N111 C115 1.370(4) . ? N121 C126 1.341(4) . ? N121 C122 1.352(4) . ? N131 C136 1.328(4) . ? N131 C132 1.357(4) . ? N241 C246 1.334(4) . ? N241 C242 1.348(4) . ? N201 C202 1.300(4) . ? N201 C205 1.375(4) . ? N207 C206 1.342(4) . ? N207 C208 1.344(4) . ? N211 C212 1.315(4) . ? N211 C215 1.373(4) . ? N221 C226 1.342(4) . ? N221 C222 1.350(4) . ? N231 C236 1.331(4) . ? N231 C232 1.364(4) . ? N400 O401 1.212(4) . ? N400 O402 1.226(4) . ? N400 C403 1.492(5) . ? O23A O23B 1.078(19) . ? O31B O32A 1.770(19) . ? O32A O32B 1.233(17) . ? O34A O34B 0.701(19) . ? C102 C252 1.453(4) . ? C104 C105 1.352(4) . ? C105 C132 1.476(4) . ? C112 C146 1.463(4) . ? C114 C115 1.368(4) . ? C115 C122 1.466(4) . ? C122 C123 1.390(4) . ? C123 C124 1.376(5) . ? C124 C125 1.375(5) . ? C125 C126 1.379(5) . ? C132 C133 1.379(4) . ? C133 C134 1.384(5) . ? C134 C135 1.385(5) . ? C135 C136 1.390(5) . ? C142 C143 1.387(4) . ? C142 C208 1.479(4) . ? C143 C144 1.370(4) . ? C144 C145 1.391(5) . ? C145 C146 1.385(4) . ? C202 C206 1.484(4) . ? C204 C205 1.352(4) . ? C205 C222 1.471(4) . ? C206 C211 1.385(4) . ? C208 C209 1.399(4) . ? C209 C210 1.365(4) . ? C210 C211 1.383(4) . ? C212 C242 1.459(4) . ? C214 C215 1.347(4) . ? C215 C232 1.477(4) . ? C222 C223 1.383(4) . ? C223 C224 1.373(5) . ? C224 C225 1.378(5) . ? C225 C226 1.389(5) . ? C232 C233 1.378(4) . ? C233 C234 1.377(5) . ? C234 C235 1.371(6) . ? C235 C236 1.385(5) . ? C242 C243 1.387(4) . ? C243 C244 1.383(4) . ? C244 C245 1.375(4) . ? C245 C246 1.400(4) . ? C246 C256 1.480(4) . ? C252 C253 1.384(4) . ? C253 C254 1.378(5) . ? C254 C255 1.373(5) . ? C255 C256 1.391(4) . ? O703 N701 1.173(5) . ? N701 C704 1.397(7) . ? N701 O702 1.420(7) . ? N701 O705 1.510(11) . ? 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 N111 Zn1 N101 171.54(10) . . ? N111 Zn1 N131 110.54(10) . . ? N101 Zn1 N131 77.88(10) . . ? N111 Zn1 N121 76.62(10) . . ? N101 Zn1 N121 100.50(10) . . ? N131 Zn1 N121 117.38(9) . . ? N111 Zn1 N141 70.56(9) . . ? N101 Zn1 N141 110.83(9) . . ? N131 Zn1 N141 82.31(8) . . ? N121 Zn1 N141 146.23(9) . . ? N201 Zn2 N211 172.15(10) . . ? N201 Zn2 N231 109.03(10) . . ? N211 Zn2 N231 78.32(10) . . ? N201 Zn2 N221 77.39(10) . . ? N211 Zn2 N221 102.01(10) . . ? N231 Zn2 N221 116.91(10) . . ? O11 Cl1 O13 110.10(17) . . ? O11 Cl1 O3 109.80(18) . . ? O13 Cl1 O3 108.57(15) . . ? O11 Cl1 O12 109.29(16) . . ? O13 Cl1 O12 109.60(14) . . ? O3 Cl1 O12 109.46(16) . . ? O23A Cl2 O23B 46.8(7) . . ? O23A Cl2 O22 124.1(6) . . ? O23B Cl2 O22 103.9(6) . . ? O23A Cl2 O21 120.1(6) . . ? O23B Cl2 O21 105.0(6) . . ? O22 Cl2 O21 112.8(2) . . ? O23A Cl2 O24 85.0(6) . . ? O23B Cl2 O24 131.7(7) . . ? O22 Cl2 O24 101.3(3) . . ? O21 Cl2 O24 102.1(2) . . ? O32B Cl3 O34B 129.2(8) . . ? O32B Cl3 O31B 116.8(10) . . ? O34B Cl3 O31B 112.4(11) . . ? O32B Cl3 O31A 137.1(9) . . ? O34B Cl3 O31A 93.0(10) . . ? O31B Cl3 O31A 20.6(13) . . ? O32B Cl3 O32A 55.0(7) . . ? O34B Cl3 O32A 122.6(10) . . ? O31B Cl3 O32A 82.4(9) . . ? O31A Cl3 O32A 99.0(7) . . ? O32B Cl3 O34A 102.2(8) . . ? O34B Cl3 O34A 29.1(8) . . ? O31B Cl3 O34A 132.4(11) . . ? O31A Cl3 O34A 116.9(11) . . ? O32A Cl3 O34A 100.2(8) . . ? O32B Cl3 O33 84.9(6) . . ? O34B Cl3 O33 95.5(6) . . ? O31B Cl3 O33 104.0(9) . . ? O31A Cl3 O33 99.9(6) . . ? O32A Cl3 O33 136.1(9) . . ? O34A Cl3 O33 105.8(5) . . ? O44 Cl4 O42 110.74(18) . . ? O44 Cl4 O43 112.61(18) . . ? O42 Cl4 O43 111.50(15) . . ? O44 Cl4 O41 107.5(2) . . ? O42 Cl4 O41 106.73(16) . . ? O43 Cl4 O41 107.43(18) . . ? C104 S103 C102 90.37(15) . . ? C114 S113 C112 90.36(15) . . ? C202 S203 C204 89.67(15) . . ? C212 S213 C214 90.51(15) . . ? C102 N101 C105 112.8(3) . . ? C102 N101 Zn1 128.5(2) . . ? C105 N101 Zn1 118.6(2) . . ? C256 N251 C252 117.5(3) . . ? C142 N141 C146 117.8(2) . . ? C142 N141 Zn1 129.76(18) . . ? C146 N141 Zn1 108.43(18) . . ? C112 N111 C115 113.5(2) . . ? C112 N111 Zn1 126.3(2) . . ? C115 N111 Zn1 120.2(2) . . ? C126 N121 C122 117.9(3) . . ? C126 N121 Zn1 127.9(2) . . ? C122 N121 Zn1 113.60(19) . . ? C136 N131 C132 118.5(3) . . ? C136 N131 Zn1 127.6(2) . . ? C132 N131 Zn1 113.8(2) . . ? C246 N241 C242 117.7(2) . . ? C202 N201 C205 112.8(3) . . ? C202 N201 Zn2 127.9(2) . . ? C205 N201 Zn2 119.27(19) . . ? C206 N207 C208 117.6(2) . . ? C212 N211 C215 113.3(3) . . ? C212 N211 Zn2 128.2(2) . . ? C215 N211 Zn2 118.1(2) . . ? C226 N221 C222 118.2(3) . . ? C226 N221 Zn2 127.1(2) . . ? C222 N221 Zn2 113.84(19) . . ? C236 N231 C232 118.3(3) . . ? C236 N231 Zn2 127.4(2) . . ? C232 N231 Zn2 113.5(2) . . ? O401 N400 O402 124.0(3) . . ? O401 N400 C403 118.5(4) . . ? O402 N400 C403 117.6(3) . . ? O23B O23A Cl2 69.6(7) . . ? O23A O23B Cl2 63.6(8) . . ? Cl3 O31B O32A 50.5(6) . . ? O32B O32A Cl3 58.6(6) . . ? O32B O32A O31B 92.9(12) . . ? Cl3 O32A O31B 47.0(6) . . ? O32A O32B Cl3 66.4(6) . . ? O34B O34A Cl3 63.8(13) . . ? O34A O34B Cl3 87.2(17) . . ? N101 C102 C252 120.1(3) . . ? N101 C102 S103 112.4(2) . . ? C252 C102 S103 127.6(2) . . ? C105 C104 S103 110.7(2) . . ? C104 C105 N101 113.8(3) . . ? C104 C105 C132 131.0(3) . . ? N101 C105 C132 115.2(3) . . ? N111 C112 C146 118.4(3) . . ? N111 C112 S113 112.7(2) . . ? C146 C112 S113 128.9(2) . . ? C115 C114 S113 110.5(2) . . ? C114 C115 N111 112.9(3) . . ? C114 C115 C122 132.0(3) . . ? N111 C115 C122 115.1(3) . . ? N121 C122 C123 122.1(3) . . ? N121 C122 C115 114.2(3) . . ? C123 C122 C115 123.6(3) . . ? C124 C123 C122 118.7(3) . . ? C125 C124 C123 119.7(3) . . ? C124 C125 C126 118.7(3) . . ? N121 C126 C125 122.9(3) . . ? N131 C132 C133 122.4(3) . . ? N131 C132 C105 114.5(3) . . ? C133 C132 C105 123.1(3) . . ? C132 C133 C134 118.7(3) . . ? C133 C134 C135 119.2(3) . . ? C134 C135 C136 118.8(3) . . ? N131 C136 C135 122.4(3) . . ? N141 C142 C143 122.6(3) . . ? N141 C142 C208 114.7(2) . . ? C143 C142 C208 122.7(3) . . ? C144 C143 C142 118.9(3) . . ? C143 C144 C145 120.0(3) . . ? C146 C145 C144 117.4(3) . . ? N141 C146 C145 123.3(3) . . ? N141 C146 C112 112.5(2) . . ? C145 C146 C112 124.2(3) . . ? N201 C202 C206 117.9(3) . . ? N201 C202 S203 113.4(2) . . ? C206 C202 S203 128.6(2) . . ? C205 C204 S203 110.8(2) . . ? C204 C205 N201 113.3(3) . . ? C204 C205 C222 131.9(3) . . ? N201 C205 C222 114.8(3) . . ? N207 C206 C211 123.7(3) . . ? N207 C206 C202 112.4(2) . . ? C211 C206 C202 123.9(3) . . ? N207 C208 C209 122.1(3) . . ? N207 C208 C142 114.6(2) . . ? C209 C208 C142 123.2(3) . . ? C210 C209 C208 118.8(3) . . ? C209 C210 C211 120.1(3) . . ? C210 C211 C206 117.6(3) . . ? N211 C212 C242 120.0(3) . . ? N211 C212 S213 112.1(2) . . ? C242 C212 S213 127.9(2) . . ? C215 C214 S213 110.4(2) . . ? C214 C215 N211 113.7(3) . . ? C214 C215 C232 131.2(3) . . ? N211 C215 C232 115.1(3) . . ? N221 C222 C223 122.1(3) . . ? N221 C222 C205 114.1(3) . . ? C223 C222 C205 123.8(3) . . ? C224 C223 C222 119.0(3) . . ? C223 C224 C225 119.8(3) . . ? C224 C225 C226 118.3(3) . . ? N221 C226 C225 122.6(3) . . ? N231 C232 C233 121.9(3) . . ? N231 C232 C215 114.1(3) . . ? C233 C232 C215 124.0(3) . . ? C234 C233 C232 118.7(4) . . ? C235 C234 C233 119.8(4) . . ? C234 C235 C236 118.8(4) . . ? N231 C236 C235 122.4(3) . . ? N241 C242 C243 123.8(3) . . ? N241 C242 C212 112.9(3) . . ? C243 C242 C212 123.3(3) . . ? C244 C243 C242 117.6(3) . . ? C245 C244 C243 119.7(3) . . ? C244 C245 C246 119.0(3) . . ? N241 C246 C245 122.2(3) . . ? N241 C246 C256 116.7(2) . . ? C245 C246 C256 121.1(3) . . ? N251 C252 C253 123.7(3) . . ? N251 C252 C102 113.9(3) . . ? C253 C252 C102 122.2(3) . . ? C254 C253 C252 118.0(3) . . ? C255 C254 C253 119.3(3) . . ? C254 C255 C256 119.6(3) . . ? N251 C256 C255 121.9(3) . . ? N251 C256 C246 116.2(3) . . ? C255 C256 C246 121.9(3) . . ? O703 N701 C704 116.5(5) . . ? O703 N701 O702 127.8(5) . . ? C704 N701 O702 102.9(5) . . ? O703 N701 O705 95.3(7) . . ? C704 N701 O705 98.8(5) . . ? O702 N701 O705 111.7(7) . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 27.51 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 0.829 _refine_diff_density_min -0.733 _refine_diff_density_rms 0.079 #=END data_nickel _database_code_CSD 163222 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C54 H40 Cl4 N14 Ni2 O21 S4' _chemical_formula_weight 1608.46 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' 'S' 'S' 0.1246 0.1234 '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' 'Ni' 'Ni' 0.3393 1.1124 '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 13.8523(9) _cell_length_b 15.0576(10) _cell_length_c 16.8639(11) _cell_angle_alpha 74.4310(10) _cell_angle_beta 68.2440(10) _cell_angle_gamma 84.9940(10) _cell_volume 3146.8(4) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description rod _exptl_crystal_colour green _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.698 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1636 _exptl_absorpt_coefficient_mu 0.990 _exptl_absorpt_correction_type 'Empirical, pseudo-azimuthal scan (SADABS)' _exptl_absorpt_correction_T_min 0.78 _exptl_absorpt_correction_T_max 0.86 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'Siemens SMART Area Detector' _diffrn_measurement_method '\w rotation with narrow frames (0.3 degrees)' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 33084 _diffrn_reflns_av_R_equivalents 0.0225 _diffrn_reflns_av_sigmaI/netI 0.0406 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.58 _diffrn_reflns_theta_max 27.52 _reflns_number_total 14308 _reflns_number_gt 10137 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1024P)^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 14308 _refine_ls_number_parameters 1000 _refine_ls_number_restraints 89 _refine_ls_R_factor_all 0.0696 _refine_ls_R_factor_gt 0.0497 _refine_ls_wR_factor_ref 0.1554 _refine_ls_wR_factor_gt 0.1458 _refine_ls_goodness_of_fit_ref 1.004 _refine_ls_restrained_S_all 1.011 _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 Ni1 Ni 0.26653(3) 0.15679(3) 0.22426(2) 0.02944(11) Uani 1 1 d . . . Ni2 Ni 0.45836(3) 0.35905(3) 0.30651(2) 0.02896(11) Uani 1 1 d . . . S103 S 0.05401(7) 0.38416(7) 0.17603(7) 0.0485(2) Uani 1 1 d . . . S113 S 0.46542(7) -0.08461(6) 0.26093(6) 0.0406(2) Uani 1 1 d . . . S203 S 0.21995(7) 0.57426(6) 0.29632(7) 0.0496(2) Uani 1 1 d . . . S214 S 0.71502(7) 0.15915(7) 0.29248(7) 0.0507(2) Uani 1 1 d . . . Cl1 Cl 0.42196(8) 0.76389(6) 0.12709(7) 0.0533(2) Uani 1 1 d . . . Cl2 Cl 0.70001(9) 0.86558(7) 0.33300(8) 0.0614(3) Uani 1 1 d . . . Cl3 Cl 0.80092(7) 0.26970(7) 0.44055(7) 0.0522(2) Uani 1 1 d . . . Cl4 Cl 0.07851(8) 0.63405(8) 0.04748(8) 0.0622(3) Uani 1 1 d . . . O11 O 0.4282(3) 0.7348(2) 0.2129(2) 0.0657(8) Uani 1 1 d . . . O12 O 0.3691(4) 0.8465(3) 0.1183(3) 0.1239(19) Uani 1 1 d . . . O13 O 0.5280(3) 0.7765(3) 0.0638(3) 0.1030(13) Uani 1 1 d . . . O14 O 0.3773(3) 0.6923(2) 0.1114(2) 0.0714(9) Uani 1 1 d . . . O21 O 0.6949(3) 0.8083(3) 0.2796(3) 0.1000(13) Uani 1 1 d . . . O22 O 0.6033(3) 0.8571(3) 0.4082(2) 0.0877(11) Uani 1 1 d . . . O23 O 0.6995(4) 0.9557(3) 0.2819(4) 0.138(2) Uani 1 1 d . . . O24 O 0.7809(5) 0.8427(5) 0.3598(4) 0.177(3) Uani 1 1 d . . . O31A O 0.7106(7) 0.2188(8) 0.4696(8) 0.077(3) Uani 0.50 1 d P . . O31B O 0.7542(13) 0.1759(10) 0.4787(8) 0.147(6) Uani 0.50 1 d P . . O32 O 0.8850(2) 0.2486(3) 0.3741(3) 0.0925(13) Uani 1 1 d . . . O33 O 0.8301(3) 0.2876(2) 0.5081(2) 0.0667(8) Uani 1 1 d . . . O34A O 0.7842(10) 0.3599(6) 0.3840(7) 0.099(4) Uani 0.50 1 d P . . O34B O 0.7293(9) 0.3270(12) 0.4265(11) 0.153(7) Uani 0.50 1 d P . . O41A O -0.0043(13) 0.5850(12) 0.0703(11) 0.087(6) Uani 0.50 1 d P . . O41B O 0.0151(14) 0.5607(10) 0.0473(10) 0.074(5) Uani 0.50 1 d P . . O42 O 0.1004(3) 0.6246(3) 0.1262(3) 0.1108(16) Uani 1 1 d . . . O43A O 0.0772(9) 0.7225(7) -0.0125(12) 0.181(8) Uani 0.50 1 d P . . O43B O 0.0073(6) 0.7120(5) 0.0495(5) 0.072(2) Uani 0.50 1 d P . . O44A O 0.1643(9) 0.6451(10) -0.0149(10) 0.128(6) Uani 0.50 1 d P . . O44B O 0.1741(9) 0.5979(10) -0.0149(6) 0.099(5) Uani 0.50 1 d P . . N101 N 0.1851(2) 0.25768(18) 0.18083(17) 0.0329(6) Uani 1 1 d . . . N111 N 0.3337(2) 0.04197(17) 0.26244(17) 0.0321(6) Uani 1 1 d . . . N121 N 0.2736(2) 0.13167(18) 0.10343(17) 0.0349(6) Uani 1 1 d . . . N131 N 0.1377(2) 0.0647(2) 0.3046(2) 0.0451(7) Uani 1 1 d . . . N141 N 0.44441(19) 0.18846(17) 0.16792(16) 0.0285(5) Uani 1 1 d . . . N151 N 0.2115(2) 0.24411(17) 0.32709(17) 0.0322(6) Uani 1 1 d . . . N201 N 0.3433(2) 0.44665(18) 0.32539(18) 0.0336(6) Uani 1 1 d . . . N211 N 0.5862(2) 0.28768(19) 0.28580(17) 0.0335(6) Uani 1 1 d . . . N221 N 0.5790(2) 0.46267(19) 0.23146(17) 0.0337(6) Uani 1 1 d . . . N231 N 0.4391(2) 0.3795(2) 0.43210(18) 0.0383(6) Uani 1 1 d . . . N241 N 0.40338(18) 0.38636(17) 0.18480(17) 0.0294(5) Uani 1 1 d . . . N251 N 0.4077(2) 0.20677(17) 0.36948(16) 0.0304(5) Uani 1 1 d . . . C102 C 0.1302(2) 0.3139(2) 0.2267(2) 0.0356(7) Uani 1 1 d . . . C104 C 0.0971(3) 0.3308(3) 0.0917(3) 0.0469(9) Uani 1 1 d . . . H104 H 0.0763 0.3462 0.0420 0.056 Uiso 1 1 calc R . . C105 C 0.1660(3) 0.2625(2) 0.1056(2) 0.0382(7) Uani 1 1 d . . . C112 C 0.4341(2) 0.0290(2) 0.2334(2) 0.0324(7) Uani 1 1 d . . . C114 C 0.3369(3) -0.1134(2) 0.3130(2) 0.0415(8) Uani 1 1 d . . . H114 H 0.3105 -0.1744 0.3423 0.050 Uiso 1 1 calc R . . C115 C 0.2771(3) -0.0370(2) 0.3070(2) 0.0373(7) Uani 1 1 d . . . C122 C 0.2171(3) 0.1908(2) 0.0615(2) 0.0386(7) Uani 1 1 d . . . C123 C 0.2067(3) 0.1786(3) -0.0146(3) 0.0498(9) Uani 1 1 d . . . H123 H 0.1658 0.2195 -0.0424 0.060 Uiso 1 1 calc R . . C124 C 0.2572(4) 0.1064(3) -0.0480(3) 0.0611(11) Uani 1 1 d . . . H124 H 0.2515 0.0970 -0.0997 0.073 Uiso 1 1 calc R . . C125 C 0.3158(4) 0.0476(3) -0.0065(3) 0.0568(10) Uani 1 1 d . . . H125 H 0.3514 -0.0022 -0.0294 0.068 Uiso 1 1 calc R . . C126 C 0.3220(3) 0.0621(2) 0.0693(2) 0.0431(8) Uani 1 1 d . . . H126 H 0.3621 0.0212 0.0981 0.052 Uiso 1 1 calc R . . C132 C 0.1645(3) -0.0233(3) 0.3339(3) 0.0535(11) Uani 1 1 d . . . C133 C 0.0915(4) -0.0937(3) 0.3792(5) 0.110(3) Uani 1 1 d . . . H133 H 0.1117 -0.1546 0.4008 0.132 Uiso 1 1 calc R . . C134 C -0.0121(4) -0.0732(4) 0.3925(7) 0.187(5) Uani 1 1 d . . . H134 H -0.0634 -0.1209 0.4182 0.224 Uiso 1 1 calc R . . C135 C -0.0402(4) 0.0187(4) 0.3677(6) 0.157(4) Uani 1 1 d . . . H135 H -0.1112 0.0349 0.3809 0.189 Uiso 1 1 calc R . . C136 C 0.0355(3) 0.0841(3) 0.3244(4) 0.0795(17) Uani 1 1 d . . . H136 H 0.0160 0.1463 0.3073 0.095 Uiso 1 1 calc R . . C142 C 0.5002(2) 0.1103(2) 0.18014(19) 0.0294(6) Uani 1 1 d . . . C143 C 0.6084(2) 0.1092(2) 0.1464(2) 0.0360(7) Uani 1 1 d . . . H143 H 0.6449 0.0536 0.1572 0.043 Uiso 1 1 calc R . . C144 C 0.6613(3) 0.1908(2) 0.0969(2) 0.0403(8) Uani 1 1 d . . . H144 H 0.7351 0.1919 0.0722 0.048 Uiso 1 1 calc R . . C145 C 0.6068(3) 0.2709(2) 0.0835(2) 0.0378(7) Uani 1 1 d . . . H145 H 0.6421 0.3277 0.0492 0.045 Uiso 1 1 calc R . . C146 C 0.4984(2) 0.2668(2) 0.12139(19) 0.0299(6) Uani 1 1 d . . . C152 C 0.1397(2) 0.3070(2) 0.3113(2) 0.0344(7) Uani 1 1 d . . . C153 C 0.0804(3) 0.3563(2) 0.3712(2) 0.0426(8) Uani 1 1 d . . . H153 H 0.0303 0.3992 0.3585 0.051 Uiso 1 1 calc R . . C154 C 0.0962(3) 0.3411(3) 0.4492(3) 0.0486(9) Uani 1 1 d . . . H154 H 0.0560 0.3733 0.4917 0.058 Uiso 1 1 calc R . . C155 C 0.1704(3) 0.2790(2) 0.4670(2) 0.0417(8) Uani 1 1 d . . . H155 H 0.1824 0.2686 0.5207 0.050 Uiso 1 1 calc R . . C156 C 0.2273(2) 0.2322(2) 0.4024(2) 0.0338(7) Uani 1 1 d . . . C202 C 0.3036(2) 0.4888(2) 0.2651(2) 0.0343(7) Uani 1 1 d . . . C204 C 0.2420(3) 0.5526(3) 0.3920(3) 0.0525(10) Uani 1 1 d . . . H204 H 0.2101 0.5846 0.4364 0.063 Uiso 1 1 calc R . . C205 C 0.3123(3) 0.4822(2) 0.3971(2) 0.0415(8) Uani 1 1 d . . . C212 C 0.6818(2) 0.3289(2) 0.2425(2) 0.0371(7) Uani 1 1 d . . . C213 C 0.7606(3) 0.2688(3) 0.2390(3) 0.0493(9) Uani 1 1 d . . . H213 H 0.8322 0.2855 0.2103 0.059 Uiso 1 1 calc R . . C215 C 0.5902(3) 0.1986(2) 0.3176(2) 0.0368(7) Uani 1 1 d . . . C222 C 0.6777(2) 0.4295(2) 0.2123(2) 0.0371(7) Uani 1 1 d . . . C223 C 0.7636(3) 0.4876(3) 0.1710(3) 0.0481(9) Uani 1 1 d . . . H223 H 0.8315 0.4629 0.1580 0.058 Uiso 1 1 calc R . . C224 C 0.7503(3) 0.5808(3) 0.1488(3) 0.0510(9) Uani 1 1 d . . . H224 H 0.8091 0.6211 0.1208 0.061 Uiso 1 1 calc R . . C225 C 0.6506(3) 0.6164(3) 0.1671(2) 0.0455(8) Uani 1 1 d . . . H225 H 0.6396 0.6810 0.1525 0.055 Uiso 1 1 calc R . . C226 C 0.5675(3) 0.5540(2) 0.2078(2) 0.0383(7) Uani 1 1 d . . . H226 H 0.4991 0.5774 0.2193 0.046 Uiso 1 1 calc R . . C232 C 0.3637(3) 0.4417(2) 0.4595(2) 0.0418(8) Uani 1 1 d . . . C233 C 0.3419(4) 0.4641(3) 0.5383(3) 0.0588(11) Uani 1 1 d . . . H233 H 0.2899 0.5078 0.5559 0.071 Uiso 1 1 calc R . . C234 C 0.3970(4) 0.4219(4) 0.5912(3) 0.0700(14) Uani 1 1 d . . . H234 H 0.3833 0.4362 0.6459 0.084 Uiso 1 1 calc R . . C235 C 0.4714(4) 0.3593(3) 0.5647(3) 0.0629(12) Uani 1 1 d . . . H235 H 0.5099 0.3299 0.6006 0.075 Uiso 1 1 calc R . . C236 C 0.4902(3) 0.3392(3) 0.4846(2) 0.0482(9) Uani 1 1 d . . . H236 H 0.5414 0.2950 0.4669 0.058 Uiso 1 1 calc R . . C242 C 0.3368(2) 0.4586(2) 0.1839(2) 0.0327(7) Uani 1 1 d . . . C243 C 0.3051(3) 0.4973(2) 0.1143(2) 0.0387(8) Uani 1 1 d . . . H243 H 0.2594 0.5482 0.1160 0.046 Uiso 1 1 calc R . . C244 C 0.3407(3) 0.4610(2) 0.0417(2) 0.0440(8) Uani 1 1 d . . . H244 H 0.3204 0.4869 -0.0076 0.053 Uiso 1 1 calc R . . C245 C 0.4055(3) 0.3876(2) 0.0416(2) 0.0412(8) Uani 1 1 d . . . H245 H 0.4305 0.3616 -0.0077 0.049 Uiso 1 1 calc R . . C246 C 0.4348(2) 0.3509(2) 0.1144(2) 0.0302(6) Uani 1 1 d . . . C252 C 0.4903(3) 0.1496(2) 0.3672(2) 0.0347(7) Uani 1 1 d . . . C253 C 0.4797(3) 0.0558(2) 0.4059(2) 0.0404(8) Uani 1 1 d . . . H253 H 0.5391 0.0180 0.4019 0.048 Uiso 1 1 calc R . . C254 C 0.3808(3) 0.0185(2) 0.4505(2) 0.0448(9) Uani 1 1 d . . . H254 H 0.3708 -0.0454 0.4789 0.054 Uiso 1 1 calc R . . C255 C 0.2969(3) 0.0752(2) 0.4533(2) 0.0423(8) Uani 1 1 d . . . H255 H 0.2282 0.0506 0.4839 0.051 Uiso 1 1 calc R . . C256 C 0.3131(3) 0.1688(2) 0.4111(2) 0.0333(7) Uani 1 1 d . . . O910 O 0.0569(4) 0.4432(4) 0.6174(3) 0.1058(14) Uani 1 1 d . . . O902 O 0.1150(5) 0.3403(6) 0.7203(5) 0.185(3) Uani 1 1 d . . . N911 N 0.0460(11) 0.3641(10) 0.6607(7) 0.093(5) Uani 0.50 1 d P . . N901 N 0.0784(8) 0.4192(11) 0.6769(6) 0.092(4) Uani 0.50 1 d P . . C912 C -0.0025(7) 0.3074(7) 0.6650(7) 0.058(3) Uani 0.50 1 d P . . C900 C 0.1006(8) 0.4866(7) 0.6990(7) 0.072(3) Uani 0.50 1 d P . . O702 O -0.0229(17) 0.9991(13) 0.8617(12) 0.314(12) Uani 0.50 1 d PDU . . N701 N 0.0420(10) 0.9324(8) 0.8526(9) 0.154(5) Uani 0.50 1 d PDU . . C700 C 0.088(3) 0.961(4) 0.905(4) 0.242(14) Uani 0.50 1 d PDU . . O703 O 0.0580(6) 0.8725(7) 0.8314(7) 0.127(3) Uani 0.50 1 d PDU . . O603 O 0.8583(14) 0.178(2) 0.863(3) 0.367(16) Uani 0.50 1 d PDU . . C600 C 1.022(3) 0.085(4) 0.865(2) 0.38(3) Uani 0.50 1 d PDU . . N601 N 0.918(4) 0.111(3) 0.857(3) 0.52(3) Uani 0.50 1 d PDU . . O602 O 0.915(4) 0.129(2) 0.926(3) 0.59(3) Uani 0.50 1 d PDU . . O650 O 0.877(2) 0.1948(18) 0.769(3) 0.358(15) Uani 0.50 1 d PU . . O750 O 0.123(2) 0.941(2) 0.895(2) 0.201(8) Uani 0.50 1 d PU . . 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 0.0312(2) 0.0250(2) 0.0285(2) -0.00424(16) -0.00965(16) 0.00521(15) Ni2 0.0302(2) 0.0283(2) 0.0278(2) -0.00710(16) -0.01018(16) 0.00193(15) S103 0.0380(4) 0.0424(5) 0.0574(6) -0.0025(4) -0.0186(4) 0.0136(4) S113 0.0407(4) 0.0290(4) 0.0540(5) -0.0128(4) -0.0200(4) 0.0118(3) S203 0.0401(5) 0.0323(4) 0.0645(6) -0.0131(4) -0.0072(4) 0.0106(4) S214 0.0427(5) 0.0479(5) 0.0702(7) -0.0152(5) -0.0333(5) 0.0155(4) Cl1 0.0710(6) 0.0367(5) 0.0527(5) -0.0127(4) -0.0214(5) -0.0027(4) Cl2 0.0811(7) 0.0440(5) 0.0669(7) -0.0122(5) -0.0406(6) 0.0181(5) Cl3 0.0420(5) 0.0625(6) 0.0553(5) -0.0305(5) -0.0107(4) 0.0023(4) Cl4 0.0496(6) 0.0629(7) 0.0797(7) -0.0125(6) -0.0344(6) 0.0033(5) O11 0.093(2) 0.0507(17) 0.070(2) -0.0302(15) -0.0411(18) 0.0191(16) O12 0.206(5) 0.076(3) 0.152(4) -0.055(3) -0.132(4) 0.076(3) O13 0.087(3) 0.111(3) 0.088(3) -0.019(2) -0.003(2) -0.039(2) O14 0.093(2) 0.062(2) 0.0582(18) -0.0200(16) -0.0175(17) -0.0280(17) O21 0.109(3) 0.127(4) 0.086(3) -0.056(3) -0.048(2) 0.033(3) O22 0.107(3) 0.076(2) 0.066(2) -0.0186(19) -0.015(2) 0.003(2) O23 0.131(4) 0.059(3) 0.169(5) 0.017(3) -0.028(4) 0.015(3) O24 0.160(5) 0.296(8) 0.161(5) -0.139(6) -0.129(4) 0.147(5) O31A 0.054(4) 0.091(8) 0.080(6) -0.001(6) -0.026(4) -0.021(4) O31B 0.242(18) 0.119(11) 0.066(6) -0.025(7) -0.012(10) -0.119(11) O32 0.0491(18) 0.149(4) 0.098(3) -0.080(3) -0.0180(18) 0.022(2) O33 0.101(2) 0.0517(17) 0.0596(18) -0.0247(15) -0.0355(17) 0.0015(16) O34A 0.182(12) 0.043(4) 0.076(6) -0.002(4) -0.061(7) 0.011(6) O34B 0.099(8) 0.220(19) 0.218(17) -0.152(15) -0.105(10) 0.127(11) O41A 0.053(5) 0.137(15) 0.064(6) 0.005(7) -0.022(4) -0.050(8) O41B 0.094(10) 0.052(5) 0.095(11) 0.012(6) -0.071(9) -0.019(5) O42 0.106(3) 0.155(4) 0.134(4) -0.092(3) -0.093(3) 0.076(3) O43A 0.103(8) 0.092(7) 0.33(2) 0.073(10) -0.142(11) -0.035(7) O43B 0.082(5) 0.061(4) 0.096(5) -0.023(4) -0.061(4) 0.028(4) O44A 0.046(5) 0.120(10) 0.167(12) -0.039(8) 0.025(6) -0.011(6) O44B 0.059(5) 0.192(14) 0.047(4) -0.030(6) -0.029(4) 0.030(7) N101 0.0317(13) 0.0288(13) 0.0343(14) -0.0016(11) -0.0129(11) 0.0030(11) N111 0.0342(13) 0.0285(13) 0.0308(13) -0.0070(11) -0.0097(11) 0.0047(11) N121 0.0401(14) 0.0325(14) 0.0315(14) -0.0058(11) -0.0133(12) -0.0018(11) N131 0.0330(14) 0.0311(15) 0.0524(18) 0.0025(13) -0.0041(13) 0.0037(12) N141 0.0318(13) 0.0287(13) 0.0267(12) -0.0100(10) -0.0111(10) 0.0042(10) N151 0.0320(13) 0.0270(13) 0.0306(13) -0.0060(11) -0.0050(11) 0.0037(10) N201 0.0332(13) 0.0285(13) 0.0357(14) -0.0125(11) -0.0048(11) -0.0028(11) N211 0.0341(14) 0.0347(14) 0.0316(14) -0.0069(11) -0.0140(11) 0.0052(11) N221 0.0332(13) 0.0396(15) 0.0286(13) -0.0057(12) -0.0136(11) 0.0003(11) N231 0.0440(15) 0.0390(15) 0.0300(14) -0.0076(12) -0.0095(12) -0.0109(12) N241 0.0279(12) 0.0263(13) 0.0326(13) -0.0052(11) -0.0112(11) 0.0001(10) N251 0.0394(14) 0.0285(13) 0.0249(12) -0.0064(10) -0.0142(11) 0.0021(11) C102 0.0310(15) 0.0257(15) 0.0423(18) -0.0007(14) -0.0106(14) 0.0031(12) C104 0.0437(19) 0.048(2) 0.046(2) 0.0006(17) -0.0229(17) 0.0045(16) C105 0.0359(17) 0.0373(18) 0.0374(17) 0.0023(14) -0.0162(14) -0.0034(14) C112 0.0377(16) 0.0299(15) 0.0323(16) -0.0110(13) -0.0155(13) 0.0099(13) C114 0.0417(18) 0.0288(17) 0.047(2) -0.0064(15) -0.0123(16) 0.0062(14) C115 0.0405(17) 0.0272(16) 0.0354(17) -0.0036(14) -0.0076(14) 0.0039(13) C122 0.0433(18) 0.0370(18) 0.0328(17) -0.0013(14) -0.0142(14) -0.0068(14) C123 0.064(2) 0.046(2) 0.044(2) -0.0013(17) -0.0292(19) -0.0076(18) C124 0.092(3) 0.056(3) 0.045(2) -0.014(2) -0.033(2) -0.005(2) C125 0.078(3) 0.052(2) 0.048(2) -0.024(2) -0.023(2) 0.004(2) C126 0.053(2) 0.0395(19) 0.0395(19) -0.0145(16) -0.0170(16) 0.0020(16) C132 0.0369(18) 0.0348(19) 0.063(2) 0.0075(18) -0.0038(17) 0.0064(15) C133 0.045(2) 0.043(3) 0.164(6) 0.041(3) 0.004(3) -0.001(2) C134 0.045(3) 0.064(4) 0.299(11) 0.086(5) 0.016(4) 0.000(3) C135 0.036(2) 0.073(4) 0.235(9) 0.067(5) 0.019(4) 0.006(2) C136 0.038(2) 0.043(2) 0.107(4) 0.015(2) 0.005(2) 0.0078(18) C142 0.0323(15) 0.0322(16) 0.0281(15) -0.0124(13) -0.0139(12) 0.0059(12) C143 0.0350(16) 0.0383(18) 0.0394(17) -0.0167(15) -0.0156(14) 0.0083(14) C144 0.0310(16) 0.047(2) 0.0434(19) -0.0156(16) -0.0113(14) 0.0039(14) C145 0.0365(17) 0.0398(18) 0.0380(17) -0.0129(15) -0.0121(14) -0.0005(14) C146 0.0345(15) 0.0325(16) 0.0260(14) -0.0103(13) -0.0129(12) 0.0021(13) C152 0.0281(15) 0.0262(15) 0.0417(18) -0.0064(13) -0.0064(13) 0.0011(12) C153 0.0323(16) 0.0362(18) 0.054(2) -0.0170(16) -0.0067(15) 0.0051(14) C154 0.0390(18) 0.046(2) 0.056(2) -0.0280(19) -0.0018(17) -0.0002(16) C155 0.0398(18) 0.0405(19) 0.0401(18) -0.0174(16) -0.0027(15) -0.0054(15) C156 0.0346(16) 0.0283(15) 0.0326(16) -0.0083(13) -0.0041(13) -0.0040(13) C202 0.0259(14) 0.0259(15) 0.0455(18) -0.0074(14) -0.0082(13) 0.0022(12) C204 0.048(2) 0.0363(19) 0.059(2) -0.0234(18) 0.0055(18) -0.0002(16) C205 0.0415(18) 0.0361(18) 0.0381(18) -0.0161(15) 0.0022(15) -0.0087(14) C212 0.0312(16) 0.0467(19) 0.0363(17) -0.0108(15) -0.0156(14) 0.0017(14) C213 0.0370(18) 0.055(2) 0.063(2) -0.018(2) -0.0251(18) 0.0077(16) C215 0.0429(18) 0.0381(18) 0.0388(17) -0.0123(15) -0.0257(15) 0.0103(14) C222 0.0310(16) 0.047(2) 0.0354(17) -0.0111(15) -0.0147(14) 0.0026(14) C223 0.0320(17) 0.058(2) 0.049(2) -0.0058(18) -0.0131(16) -0.0019(16) C224 0.0410(19) 0.056(2) 0.047(2) 0.0004(18) -0.0123(17) -0.0122(17) C225 0.049(2) 0.040(2) 0.042(2) 0.0028(16) -0.0176(17) -0.0091(16) C226 0.0396(17) 0.0394(18) 0.0340(17) -0.0030(14) -0.0153(14) -0.0022(14) C232 0.0466(19) 0.0394(19) 0.0331(17) -0.0116(15) -0.0024(15) -0.0139(15) C233 0.069(3) 0.059(3) 0.040(2) -0.022(2) 0.0005(19) -0.022(2) C234 0.093(4) 0.081(3) 0.035(2) -0.020(2) -0.010(2) -0.036(3) C235 0.082(3) 0.071(3) 0.038(2) 0.000(2) -0.027(2) -0.030(3) C236 0.061(2) 0.050(2) 0.0358(18) -0.0032(17) -0.0204(17) -0.0196(18) C242 0.0279(14) 0.0235(14) 0.0440(18) -0.0034(13) -0.0135(13) -0.0006(12) C243 0.0352(16) 0.0279(16) 0.054(2) -0.0016(15) -0.0233(16) 0.0020(13) C244 0.053(2) 0.0375(19) 0.047(2) 0.0004(16) -0.0322(18) -0.0013(16) C245 0.053(2) 0.0376(18) 0.0380(18) -0.0066(15) -0.0236(16) -0.0021(15) C246 0.0316(15) 0.0278(15) 0.0292(15) -0.0029(12) -0.0112(12) -0.0030(12) C252 0.0486(18) 0.0317(16) 0.0294(15) -0.0085(13) -0.0217(14) 0.0078(14) C253 0.058(2) 0.0326(17) 0.0379(18) -0.0080(14) -0.0286(17) 0.0084(15) C254 0.073(3) 0.0288(17) 0.0345(18) -0.0018(14) -0.0257(18) 0.0006(17) C255 0.054(2) 0.0311(17) 0.0353(17) -0.0023(14) -0.0115(16) -0.0058(15) C256 0.0460(18) 0.0301(16) 0.0233(14) -0.0067(12) -0.0119(13) 0.0009(13) O910 0.107(3) 0.114(4) 0.105(3) -0.045(3) -0.042(3) 0.032(3) O902 0.153(6) 0.228(8) 0.145(5) -0.040(5) -0.033(5) 0.027(5) N911 0.102(10) 0.109(10) 0.042(5) -0.023(7) -0.009(6) 0.066(9) N901 0.072(6) 0.140(12) 0.045(5) -0.021(6) -0.018(4) 0.070(8) C912 0.050(5) 0.064(6) 0.066(6) -0.039(5) -0.011(4) -0.005(4) C900 0.082(7) 0.061(6) 0.072(6) -0.033(5) -0.020(5) 0.011(5) O702 0.274(16) 0.226(15) 0.181(15) 0.066(11) 0.089(11) 0.193(15) N701 0.106(8) 0.079(7) 0.131(11) 0.041(6) 0.063(5) 0.048(6) C700 0.19(2) 0.18(4) 0.27(3) -0.13(3) 0.066(16) 0.007(18) O703 0.043(4) 0.115(7) 0.147(8) 0.015(6) 0.014(4) 0.023(4) O603 0.114(11) 0.40(3) 0.68(4) -0.42(3) -0.05(2) -0.027(15) C600 0.31(4) 0.58(7) 0.111(18) 0.11(3) -0.06(2) 0.04(4) N601 0.41(5) 0.56(6) 0.70(6) -0.29(4) -0.28(6) 0.20(5) O602 0.77(6) 0.32(3) 0.87(7) -0.47(4) -0.35(4) 0.33(3) O650 0.23(2) 0.28(2) 0.75(4) -0.36(3) -0.26(3) 0.164(19) O750 0.23(2) 0.108(11) 0.21(2) -0.076(12) 0.000(19) 0.031(14) _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 N111 1.958(3) . ? Ni1 N101 1.958(2) . ? Ni1 N121 2.136(3) . ? Ni1 N131 2.139(3) . ? Ni1 N151 2.321(3) . ? Ni1 N141 2.330(3) . ? Ni2 N211 1.955(2) . ? Ni2 N201 1.965(3) . ? Ni2 N231 2.137(3) . ? Ni2 N221 2.158(3) . ? Ni2 N251 2.302(3) . ? Ni2 N241 2.369(3) . ? S103 C104 1.710(4) . ? S103 C102 1.718(3) . ? S113 C114 1.703(4) . ? S113 C112 1.711(3) . ? S203 C204 1.693(5) . ? S203 C202 1.711(3) . ? S214 C213 1.703(4) . ? S214 C215 1.714(3) . ? Cl1 O12 1.389(3) . ? Cl1 O14 1.417(3) . ? Cl1 O11 1.427(3) . ? Cl1 O13 1.453(4) . ? Cl2 O24 1.343(4) . ? Cl2 O23 1.399(4) . ? Cl2 O21 1.427(4) . ? Cl2 O22 1.450(4) . ? Cl3 O34B 1.304(10) . ? Cl3 O32 1.369(3) . ? Cl3 O31A 1.380(10) . ? Cl3 O33 1.434(3) . ? Cl3 O34A 1.490(9) . ? Cl3 O31B 1.480(12) . ? Cl4 O44A 1.249(12) . ? Cl4 O41A 1.296(15) . ? Cl4 O43A 1.443(10) . ? Cl4 O42 1.436(4) . ? Cl4 O43B 1.465(6) . ? Cl4 O41B 1.471(16) . ? Cl4 O44B 1.518(11) . ? O31A O31B 0.868(18) . ? O31A O34B 1.60(2) . ? O34A O34B 0.899(17) . ? O41A O41B 0.58(3) . ? O43A O43B 1.115(16) . ? O43A O44A 1.599(17) . ? O44A O44B 0.711(19) . ? N101 C102 1.303(4) . ? N101 C105 1.370(4) . ? N111 C112 1.308(4) . ? N111 C115 1.356(4) . ? N121 C126 1.338(4) . ? N121 C122 1.362(4) . ? N131 C136 1.353(5) . ? N131 C132 1.355(4) . ? N141 C146 1.337(4) . ? N141 C142 1.362(4) . ? N151 C156 1.331(4) . ? N151 C152 1.362(4) . ? N201 C202 1.322(4) . ? N201 C205 1.362(4) . ? N211 C215 1.309(4) . ? N211 C212 1.363(4) . ? N221 C226 1.338(4) . ? N221 C222 1.365(4) . ? N231 C236 1.324(5) . ? N231 C232 1.373(5) . ? N241 C246 1.342(4) . ? N241 C242 1.363(4) . ? N251 C256 1.331(4) . ? N251 C252 1.366(4) . ? C102 C152 1.456(5) . ? C104 C105 1.373(5) . ? C105 C122 1.460(5) . ? C112 C142 1.463(5) . ? C114 C115 1.361(4) . ? C115 C132 1.467(5) . ? C122 C123 1.403(5) . ? C123 C124 1.377(6) . ? C124 C125 1.378(6) . ? C125 C126 1.388(5) . ? C132 C133 1.382(6) . ? C133 C134 1.388(7) . ? C134 C135 1.398(8) . ? C135 C136 1.351(7) . ? C142 C143 1.392(4) . ? C143 C144 1.377(5) . ? C144 C145 1.378(5) . ? C145 C146 1.396(4) . ? C146 C246 1.483(4) . ? C152 C153 1.388(4) . ? C153 C154 1.369(6) . ? C154 C155 1.389(5) . ? C155 C156 1.409(4) . ? C156 C256 1.483(4) . ? C202 C242 1.458(5) . ? C204 C205 1.382(5) . ? C205 C232 1.457(5) . ? C212 C213 1.351(5) . ? C212 C222 1.465(5) . ? C215 C252 1.465(5) . ? C222 C223 1.380(5) . ? C223 C224 1.367(5) . ? C224 C225 1.391(5) . ? C225 C226 1.392(5) . ? C232 C233 1.378(5) . ? C233 C234 1.378(7) . ? C234 C235 1.365(7) . ? C235 C236 1.390(5) . ? C242 C243 1.372(5) . ? C243 C244 1.380(5) . ? C244 C245 1.362(5) . ? C245 C246 1.393(4) . ? C252 C253 1.383(5) . ? C253 C254 1.379(5) . ? C254 C255 1.375(5) . ? C255 C256 1.394(5) . ? O910 N901 1.111(11) . ? O910 N911 1.208(13) . ? O902 N901 1.380(13) . ? O902 N911 1.586(15) . ? N911 N901 1.116(19) . ? N911 C912 1.103(17) . ? N901 C900 1.267(18) . ? O702 N701 1.290(12) . ? O702 O750 2.33(3) . ? N701 O703 1.034(13) . ? N701 C700 1.43(2) . ? C700 O750 0.54(5) . ? O703 O750 2.12(3) . ? O603 N601 1.25(2) . ? O603 O650 1.46(5) . ? C600 N601 1.51(2) . ? N601 O602 1.25(2) . ? 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 N111 Ni1 N101 169.78(11) . . ? N111 Ni1 N121 95.63(10) . . ? N101 Ni1 N121 77.21(11) . . ? N111 Ni1 N131 77.04(11) . . ? N101 Ni1 N131 96.05(11) . . ? N121 Ni1 N131 94.34(12) . . ? N111 Ni1 N151 113.42(10) . . ? N101 Ni1 N151 73.54(10) . . ? N121 Ni1 N151 150.75(10) . . ? N131 Ni1 N151 89.12(11) . . ? N111 Ni1 N141 73.37(10) . . ? N101 Ni1 N141 113.70(10) . . ? N121 Ni1 N141 91.60(9) . . ? N131 Ni1 N141 150.24(10) . . ? N151 Ni1 N141 99.68(9) . . ? N211 Ni2 N201 171.15(11) . . ? N211 Ni2 N231 99.45(11) . . ? N201 Ni2 N231 77.26(11) . . ? N211 Ni2 N221 76.56(11) . . ? N201 Ni2 N221 95.45(10) . . ? N231 Ni2 N221 95.20(10) . . ? N211 Ni2 N251 73.76(10) . . ? N201 Ni2 N251 114.28(10) . . ? N231 Ni2 N251 91.24(10) . . ? N221 Ni2 N251 150.27(10) . . ? N211 Ni2 N241 110.65(10) . . ? N201 Ni2 N241 72.65(10) . . ? N231 Ni2 N241 149.83(10) . . ? N221 Ni2 N241 89.90(9) . . ? N251 Ni2 N241 98.93(9) . . ? C104 S103 C102 90.22(17) . . ? C114 S113 C112 90.04(16) . . ? C204 S203 C202 90.40(17) . . ? C213 S214 C215 89.80(17) . . ? O12 Cl1 O14 113.6(3) . . ? O12 Cl1 O11 110.2(2) . . ? O14 Cl1 O11 109.54(19) . . ? O12 Cl1 O13 110.0(3) . . ? O14 Cl1 O13 106.4(2) . . ? O11 Cl1 O13 106.9(2) . . ? O24 Cl2 O23 116.8(5) . . ? O24 Cl2 O21 110.8(3) . . ? O23 Cl2 O21 104.6(3) . . ? O24 Cl2 O22 110.6(3) . . ? O23 Cl2 O22 104.3(3) . . ? O21 Cl2 O22 109.3(3) . . ? O34B Cl3 O32 123.3(8) . . ? O34B Cl3 O31A 72.9(9) . . ? O32 Cl3 O31A 118.0(6) . . ? O34B Cl3 O33 109.9(6) . . ? O32 Cl3 O33 111.8(2) . . ? O31A Cl3 O33 115.9(5) . . ? O34B Cl3 O34A 36.8(8) . . ? O32 Cl3 O34A 93.7(5) . . ? O31A Cl3 O34A 106.3(6) . . ? O33 Cl3 O34A 108.2(5) . . ? O34B Cl3 O31B 108.0(10) . . ? O32 Cl3 O31B 96.7(6) . . ? O31A Cl3 O31B 35.1(7) . . ? O33 Cl3 O31B 104.6(5) . . ? O34A Cl3 O31B 138.8(8) . . ? O44A Cl4 O41A 134.8(10) . . ? O44A Cl4 O43A 72.5(9) . . ? O41A Cl4 O43A 112.6(9) . . ? O44A Cl4 O42 106.3(8) . . ? O41A Cl4 O42 106.8(8) . . ? O43A Cl4 O42 122.4(7) . . ? O44A Cl4 O43B 117.2(7) . . ? O41A Cl4 O43B 84.5(9) . . ? O43A Cl4 O43B 45.1(6) . . ? O42 Cl4 O43B 102.1(3) . . ? O44A Cl4 O41B 112.3(9) . . ? O41A Cl4 O41B 23.2(11) . . ? O43A Cl4 O41B 115.8(7) . . ? O42 Cl4 O41B 116.9(6) . . ? O43B Cl4 O41B 102.0(7) . . ? O44A Cl4 O44B 27.7(9) . . ? O41A Cl4 O44B 112.8(9) . . ? O43A Cl4 O44B 96.5(9) . . ? O42 Cl4 O44B 105.1(3) . . ? O43B Cl4 O44B 141.2(6) . . ? O41B Cl4 O44B 89.8(8) . . ? O31B O31A Cl3 78.7(13) . . ? O31B O31A O34B 130.0(16) . . ? Cl3 O31A O34B 51.3(5) . . ? O31A O31B Cl3 66.2(12) . . ? O34B O34A Cl3 60.3(9) . . ? O34A O34B Cl3 82.9(10) . . ? O34A O34B O31A 132.0(14) . . ? Cl3 O34B O31A 55.7(7) . . ? O41B O41A Cl4 96(3) . . ? O41A O41B Cl4 61(3) . . ? O43B O43A Cl4 68.5(8) . . ? O43B O43A O44A 116.2(11) . . ? Cl4 O43A O44A 48.1(6) . . ? O43A O43B Cl4 66.4(6) . . ? O44B O44A Cl4 98(2) . . ? O44B O44A O43A 143(2) . . ? Cl4 O44A O43A 59.4(7) . . ? O44A O44B Cl4 54.6(15) . . ? C102 N101 C105 114.3(3) . . ? C102 N101 Ni1 124.0(2) . . ? C105 N101 Ni1 120.6(2) . . ? C112 N111 C115 113.6(3) . . ? C112 N111 Ni1 124.4(2) . . ? C115 N111 Ni1 120.6(2) . . ? C126 N121 C122 118.6(3) . . ? C126 N121 Ni1 126.6(2) . . ? C122 N121 Ni1 114.6(2) . . ? C136 N131 C132 118.2(3) . . ? C136 N131 Ni1 127.2(3) . . ? C132 N131 Ni1 114.4(2) . . ? C146 N141 C142 116.9(3) . . ? C146 N141 Ni1 131.3(2) . . ? C142 N141 Ni1 111.6(2) . . ? C156 N151 C152 117.8(3) . . ? C156 N151 Ni1 129.9(2) . . ? C152 N151 Ni1 111.3(2) . . ? C202 N201 C205 113.8(3) . . ? C202 N201 Ni2 124.4(2) . . ? C205 N201 Ni2 120.6(2) . . ? C215 N211 C212 113.2(3) . . ? C215 N211 Ni2 124.7(2) . . ? C212 N211 Ni2 121.9(2) . . ? C226 N221 C222 117.9(3) . . ? C226 N221 Ni2 127.5(2) . . ? C222 N221 Ni2 114.5(2) . . ? C236 N231 C232 118.2(3) . . ? C236 N231 Ni2 127.6(3) . . ? C232 N231 Ni2 114.2(2) . . ? C246 N241 C242 116.6(3) . . ? C246 N241 Ni2 131.4(2) . . ? C242 N241 Ni2 111.5(2) . . ? C256 N251 C252 117.3(3) . . ? C256 N251 Ni2 130.3(2) . . ? C252 N251 Ni2 112.3(2) . . ? N101 C102 C152 117.3(3) . . ? N101 C102 S103 112.4(3) . . ? C152 C102 S103 130.3(2) . . ? C105 C104 S103 110.8(3) . . ? N101 C105 C104 112.2(3) . . ? N101 C105 C122 113.6(3) . . ? C104 C105 C122 134.0(3) . . ? N111 C112 C142 116.9(3) . . ? N111 C112 S113 112.5(2) . . ? C142 C112 S113 130.5(2) . . ? C115 C114 S113 110.7(3) . . ? N111 C115 C114 113.1(3) . . ? N111 C115 C132 113.6(3) . . ? C114 C115 C132 133.2(3) . . ? N121 C122 C123 121.5(3) . . ? N121 C122 C105 113.8(3) . . ? C123 C122 C105 124.6(3) . . ? C124 C123 C122 118.6(4) . . ? C123 C124 C125 119.9(4) . . ? C124 C125 C126 118.9(4) . . ? N121 C126 C125 122.4(4) . . ? N131 C132 C133 122.2(4) . . ? N131 C132 C115 113.7(3) . . ? C133 C132 C115 124.0(3) . . ? C132 C133 C134 118.3(4) . . ? C133 C134 C135 119.2(5) . . ? C136 C135 C134 118.9(5) . . ? C135 C136 N131 122.8(4) . . ? N141 C142 C143 123.1(3) . . ? N141 C142 C112 112.5(3) . . ? C143 C142 C112 124.4(3) . . ? C144 C143 C142 118.4(3) . . ? C143 C144 C145 119.8(3) . . ? C144 C145 C146 118.5(3) . . ? N141 C146 C145 123.4(3) . . ? N141 C146 C246 115.0(3) . . ? C145 C146 C246 121.5(3) . . ? N151 C152 C153 123.1(3) . . ? N151 C152 C102 112.5(3) . . ? C153 C152 C102 124.5(3) . . ? C154 C153 C152 118.0(3) . . ? C153 C154 C155 120.8(3) . . ? C154 C155 C156 117.5(3) . . ? N151 C156 C155 122.8(3) . . ? N151 C156 C256 114.5(3) . . ? C155 C156 C256 122.6(3) . . ? N201 C202 C242 117.6(3) . . ? N201 C202 S203 112.4(2) . . ? C242 C202 S203 130.0(3) . . ? C205 C204 S203 111.4(3) . . ? N201 C205 C204 112.0(4) . . ? N201 C205 C232 113.8(3) . . ? C204 C205 C232 134.1(3) . . ? C213 C212 N211 113.2(3) . . ? C213 C212 C222 133.4(3) . . ? N211 C212 C222 113.4(3) . . ? C212 C213 S214 111.2(3) . . ? N211 C215 C252 116.5(3) . . ? N211 C215 S214 112.6(3) . . ? C252 C215 S214 130.9(3) . . ? N221 C222 C223 121.6(3) . . ? N221 C222 C212 113.6(3) . . ? C223 C222 C212 124.8(3) . . ? C224 C223 C222 119.7(3) . . ? C223 C224 C225 119.9(3) . . ? C226 C225 C224 117.5(3) . . ? N221 C226 C225 123.4(3) . . ? N231 C232 C233 121.9(4) . . ? N231 C232 C205 113.9(3) . . ? C233 C232 C205 124.1(4) . . ? C234 C233 C232 118.7(4) . . ? C235 C234 C233 119.7(4) . . ? C234 C235 C236 119.3(4) . . ? N231 C236 C235 122.2(4) . . ? N241 C242 C243 123.4(3) . . ? N241 C242 C202 112.2(3) . . ? C243 C242 C202 124.5(3) . . ? C242 C243 C244 118.8(3) . . ? C245 C244 C243 119.1(3) . . ? C244 C245 C246 119.5(3) . . ? N241 C246 C245 122.6(3) . . ? N241 C246 C146 115.2(3) . . ? C245 C246 C146 122.1(3) . . ? N251 C252 C253 123.3(3) . . ? N251 C252 C215 112.3(3) . . ? C253 C252 C215 124.4(3) . . ? C254 C253 C252 118.3(3) . . ? C255 C254 C253 119.1(3) . . ? C254 C255 C256 119.6(3) . . ? N251 C256 C255 122.4(3) . . ? N251 C256 C156 114.6(3) . . ? C255 C256 C156 122.8(3) . . ? N901 O910 N911 57.3(10) . . ? N901 O902 N911 43.5(8) . . ? N901 N911 C912 162.9(14) . . ? N901 N911 O910 57.0(10) . . ? C912 N911 O910 131.2(15) . . ? N901 N911 O902 58.4(11) . . ? C912 N911 O902 116.4(11) . . ? O910 N911 O902 112.4(14) . . ? N911 N901 O910 65.7(10) . . ? N911 N901 C900 170.8(12) . . ? O910 N901 C900 111.2(14) . . ? N911 N901 O902 78.1(13) . . ? O910 N901 O902 138.4(15) . . ? C900 N901 O902 107.6(11) . . ? N701 O702 O750 39.4(14) . . ? O702 N701 O703 143(3) . . ? O702 N701 C700 90(2) . . ? O703 N701 C700 126(2) . . ? O750 C700 N701 94(4) . . ? O750 O703 N701 44.8(12) . . ? N601 O603 O650 89(3) . . ? O603 N601 O602 76(3) . . ? O603 N601 C600 137(5) . . ? O602 N601 C600 73(3) . . ? O703 O750 C700 92(5) . . ? O703 O750 O702 59.3(10) . . ? C700 O750 O702 36(5) . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 27.52 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 0.868 _refine_diff_density_min -0.605 _refine_diff_density_rms 0.087 #=END