# Electronic Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_mo_becky_lcrownfe_0m _audit_update_record ; 2013-10-06 # Formatted by publCIF ; _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C100 H80 Fe2 N12 O6 S4, 4(Cl O4), 4(C H Cl3), 2(C2 H3 N)' _chemical_formula_sum 'C108 H90 Cl16 Fe2 N14 O22 S4' _chemical_formula_weight 2743.08 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' Fe Fe 0.3463 0.8444 '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 ' _symmetry_space_group_name_Hall -P1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.7211(6) _cell_length_b 13.4503(8) _cell_length_c 21.2922(12) _cell_angle_alpha 104.0930(10) _cell_angle_beta 96.2950(10) _cell_angle_gamma 110.1670(10) _cell_volume 2986.2(3) _cell_formula_units_Z 1 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 5847 _cell_measurement_theta_min 2.76 _cell_measurement_theta_max 22.82 _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.525 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1400 _exptl_absorpt_coefficient_mu 0.745 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7071 _exptl_absorpt_correction_T_max 0.9780 _exptl_absorpt_process_details sadabs _exptl_special_details ? _diffrn_ambient_temperature 150(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 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 55213 _diffrn_reflns_av_R_equivalents 0.0774 _diffrn_reflns_av_sigmaI/netI 0.0895 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 1.69 _diffrn_reflns_theta_max 28.72 _reflns_number_total 14883 _reflns_number_gt 8603 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^)+(0.0641P)^2^+2.8371P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 14883 _refine_ls_number_parameters 751 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1243 _refine_ls_R_factor_gt 0.0596 _refine_ls_wR_factor_ref 0.1594 _refine_ls_wR_factor_gt 0.1324 _refine_ls_goodness_of_fit_ref 1.016 _refine_ls_restrained_S_all 1.016 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C50 C 0.6561(3) 0.3260(3) -0.16094(18) 0.0244(8) Uani 1 1 d . . . Fe1 Fe 0.50862(4) 0.74824(4) 0.30576(2) 0.01834(12) Uani 1 1 d . . . S1 S 0.75374(9) 0.79009(8) 0.16226(5) 0.0310(2) Uani 1 1 d . . . S2 S 0.21566(9) 0.47202(8) 0.14864(5) 0.0346(3) Uani 1 1 d . . . Cl1 Cl 0.31810(9) 0.61901(8) 0.55237(5) 0.0315(2) Uani 1 1 d . . . Cl2 Cl 0.98017(9) 0.16639(8) 0.17614(5) 0.0359(2) Uani 1 1 d . . . Cl3 Cl 0.92631(16) 0.64311(15) 0.30110(11) 0.1035(7) Uani 1 1 d . . . Cl4 Cl 0.90517(15) 0.41488(14) 0.26937(7) 0.0753(4) Uani 1 1 d . . . Cl5 Cl 1.03321(12) 0.56713(11) 0.39901(7) 0.0590(4) Uani 1 1 d . . . Cl6 Cl 0.90286(16) 0.13643(16) 0.76898(12) 0.1089(8) Uani 1 1 d . . . Cl7 Cl 0.74667(13) -0.09458(13) 0.70296(9) 0.0745(4) Uani 1 1 d . . . Cl8 Cl 0.97816(13) 0.00780(16) 0.66735(7) 0.0813(5) Uani 1 1 d . . . N1 N 0.4209(3) 0.8257(2) 0.36097(15) 0.0246(7) Uani 1 1 d . . . N2 N 0.5841(3) 0.8933(2) 0.29777(14) 0.0218(6) Uani 1 1 d . . . N3 N 0.6218(3) 0.7208(2) 0.24313(14) 0.0204(6) Uani 1 1 d . . . N4 N 0.6286(3) 0.7741(2) 0.38605(14) 0.0209(6) Uani 1 1 d . . . N5 N 0.4314(3) 0.6132(2) 0.32511(14) 0.0196(6) Uani 1 1 d . . . N6 N 0.3682(3) 0.6639(2) 0.22395(14) 0.0198(6) Uani 1 1 d . . . N7 N 0.9011(4) 0.1251(3) 0.4516(2) 0.0481(10) Uani 1 1 d . . . O1 O 0.5986(2) 0.30492(18) 0.04920(12) 0.0233(5) Uani 1 1 d . . . O2 O 0.8380(2) 0.4598(2) 0.05038(14) 0.0359(7) Uani 1 1 d . . . O3 O 0.8307(3) 0.6601(2) 0.03643(15) 0.0403(7) Uani 1 1 d . . . O4 O 0.2643(3) 0.6485(2) 0.60767(14) 0.0400(7) Uani 1 1 d . . . O5 O 0.4474(3) 0.6859(3) 0.56893(19) 0.0690(11) Uani 1 1 d . . . O6 O 0.3042(4) 0.5068(3) 0.5397(2) 0.0742(12) Uani 1 1 d . . . O7 O 0.2612(4) 0.6362(4) 0.49661(19) 0.0854(14) Uani 1 1 d . . . O8 O 1.0165(3) 0.1994(3) 0.24715(14) 0.0494(8) Uani 1 1 d . . . O9 O 0.8714(4) 0.1872(3) 0.15930(19) 0.0681(11) Uani 1 1 d . . . O10 O 0.9499(3) 0.0493(2) 0.15020(15) 0.0481(8) Uani 1 1 d . . . O11 O 1.0795(4) 0.2264(3) 0.15083(19) 0.0804(14) Uani 1 1 d . . . C1 C 0.3323(4) 0.7815(4) 0.3925(2) 0.0349(10) Uani 1 1 d . . . H1 H 0.3009 0.7035 0.3853 0.042 Uiso 1 1 calc R . . C2 C 0.2851(5) 0.8450(4) 0.4349(2) 0.0460(12) Uani 1 1 d . . . H2 H 0.2221 0.8108 0.4561 0.055 Uiso 1 1 calc R . . C3 C 0.3299(5) 0.9577(4) 0.4460(2) 0.0519(13) Uani 1 1 d . . . H3 H 0.2994 1.0028 0.4754 0.062 Uiso 1 1 calc R . . C4 C 0.4205(4) 1.0045(4) 0.4134(2) 0.0410(11) Uani 1 1 d . . . H4 H 0.4525 1.0824 0.4202 0.049 Uiso 1 1 calc R . . C5 C 0.4640(4) 0.9379(3) 0.37122(18) 0.0271(8) Uani 1 1 d . . . C6 C 0.5576(3) 0.9769(3) 0.33347(17) 0.0245(8) Uani 1 1 d . . . C7 C 0.6151(4) 1.0840(3) 0.3305(2) 0.0342(10) Uani 1 1 d . . . H7 H 0.5966 1.1427 0.3560 0.041 Uiso 1 1 calc R . . C8 C 0.6994(4) 1.1048(3) 0.2904(2) 0.0367(10) Uani 1 1 d . . . H8 H 0.7379 1.1778 0.2875 0.044 Uiso 1 1 calc R . . C9 C 0.7281(4) 1.0183(3) 0.2541(2) 0.0333(9) Uani 1 1 d . . . H9 H 0.7870 1.0315 0.2267 0.040 Uiso 1 1 calc R . . C10 C 0.6686(3) 0.9131(3) 0.25906(18) 0.0243(8) Uani 1 1 d . . . C11 C 0.6812(3) 0.8110(3) 0.22628(17) 0.0232(8) Uani 1 1 d . . . C12 C 0.7008(4) 0.6514(3) 0.15609(19) 0.0301(9) Uani 1 1 d . . . H12 H 0.7162 0.5973 0.1241 0.036 Uiso 1 1 calc R . . C13 C 0.6338(3) 0.6288(3) 0.20295(18) 0.0234(8) Uani 1 1 d . . . C14 C 0.5812(3) 0.5172(3) 0.21072(17) 0.0222(7) Uani 1 1 d . . . C15 C 0.5965(3) 0.4998(3) 0.27220(18) 0.0260(8) Uani 1 1 d . . . H15 H 0.6387 0.5610 0.3110 0.031 Uiso 1 1 calc R . . C16 C 0.5500(4) 0.3929(3) 0.27677(18) 0.0297(9) Uani 1 1 d . . . H16 H 0.5567 0.3810 0.3190 0.036 Uiso 1 1 calc R . . C17 C 0.4935(4) 0.3031(3) 0.21985(18) 0.0291(9) Uani 1 1 d . . . H17 H 0.4622 0.2299 0.2234 0.035 Uiso 1 1 calc R . . C18 C 0.4820(3) 0.3188(3) 0.15775(17) 0.0235(8) Uani 1 1 d . . . C19 C 0.5240(3) 0.4272(3) 0.15379(17) 0.0233(8) Uani 1 1 d . . . H19 H 0.5134 0.4396 0.1118 0.028 Uiso 1 1 calc R . . C20 C 0.4269(3) 0.2225(3) 0.09623(17) 0.0226(8) Uani 1 1 d . . . C21 C 0.3154(3) 0.1356(3) 0.09069(19) 0.0265(8) Uani 1 1 d . . . H21 H 0.2738 0.1386 0.1266 0.032 Uiso 1 1 calc R . . C22 C 0.2632(3) 0.0448(3) 0.03415(19) 0.0275(8) Uani 1 1 d . . . C23 C 0.3238(3) 0.0423(3) -0.01844(18) 0.0262(8) Uani 1 1 d . . . H23 H 0.2881 -0.0191 -0.0576 0.031 Uiso 1 1 calc R . . C24 C 0.4359(3) 0.1279(3) -0.01518(17) 0.0222(7) Uani 1 1 d . . . C25 C 0.4876(3) 0.2177(3) 0.04313(17) 0.0215(7) Uani 1 1 d . . . C26 C 0.1433(4) -0.0489(3) 0.0299(2) 0.0409(11) Uani 1 1 d . . . H26A H 0.0985 -0.0837 -0.0164 0.061 Uiso 1 1 calc R . . H26B H 0.0918 -0.0197 0.0562 0.061 Uiso 1 1 calc R . . H26C H 0.1615 -0.1042 0.0472 0.061 Uiso 1 1 calc R . . C27 C 0.4967(3) 0.1252(3) -0.07304(17) 0.0218(7) Uani 1 1 d . . . C28 C 0.5088(4) 0.0294(3) -0.10846(18) 0.0272(8) Uani 1 1 d . . . H28 H 0.4778 -0.0362 -0.0956 0.033 Uiso 1 1 calc R . . C29 C 0.5656(4) 0.0280(3) -0.16236(19) 0.0317(9) Uani 1 1 d . . . H29 H 0.5723 -0.0384 -0.1865 0.038 Uiso 1 1 calc R . . C30 C 0.6127(4) 0.1237(3) -0.18108(18) 0.0276(8) Uani 1 1 d . . . H30 H 0.6530 0.1233 -0.2174 0.033 Uiso 1 1 calc R . . C31 C 0.6005(3) 0.2200(3) -0.14638(17) 0.0233(8) Uani 1 1 d . . . C32 C 0.5424(3) 0.2203(3) -0.09280(17) 0.0227(8) Uani 1 1 d . . . H32 H 0.5338 0.2863 -0.0694 0.027 Uiso 1 1 calc R . . C33 C 0.7097(4) 0.2829(3) 0.0591(2) 0.0338(9) Uani 1 1 d . . . H33A H 0.7235 0.2464 0.0159 0.041 Uiso 1 1 calc R . . H33B H 0.7014 0.2326 0.0869 0.041 Uiso 1 1 calc R . . C34 C 0.8171(4) 0.3910(4) 0.0925(2) 0.0390(10) Uani 1 1 d . . . H34A H 0.7997 0.4296 0.1340 0.047 Uiso 1 1 calc R . . H34B H 0.8928 0.3766 0.1042 0.047 Uiso 1 1 calc R . . C35 C 0.9358(4) 0.5651(3) 0.0834(2) 0.0373(10) Uani 1 1 d . . . H35A H 1.0159 0.5558 0.0904 0.045 Uiso 1 1 calc R . . H35B H 0.9206 0.5966 0.1273 0.045 Uiso 1 1 calc R . . C36 C 0.9426(4) 0.6433(3) 0.0428(2) 0.0370(10) Uani 1 1 d . . . H36A H 1.0133 0.7150 0.0648 0.044 Uiso 1 1 calc R . . H36B H 0.9558 0.6114 -0.0016 0.044 Uiso 1 1 calc R . . C37 C 0.8351(4) 0.7473(3) 0.0085(2) 0.0417(11) Uani 1 1 d . . . H37A H 0.8875 0.8191 0.0409 0.062 Uiso 1 1 calc R . . H37B H 0.7508 0.7449 -0.0034 0.062 Uiso 1 1 calc R . . H37C H 0.8699 0.7377 -0.0313 0.062 Uiso 1 1 calc R . . C38 C 0.7399(3) 0.8578(3) 0.41199(18) 0.0263(8) Uani 1 1 d . . . H38 H 0.7684 0.9108 0.3889 0.032 Uiso 1 1 calc R . . C39 C 0.8148(4) 0.8708(3) 0.4704(2) 0.0326(9) Uani 1 1 d . . . H39 H 0.8945 0.9296 0.4861 0.039 Uiso 1 1 calc R . . C40 C 0.7724(4) 0.7969(3) 0.5059(2) 0.0329(9) Uani 1 1 d . . . H40 H 0.8208 0.8063 0.5473 0.039 Uiso 1 1 calc R . . C41 C 0.6586(4) 0.7092(3) 0.48020(18) 0.0291(8) Uani 1 1 d . . . H41 H 0.6279 0.6572 0.5036 0.035 Uiso 1 1 calc R . . C42 C 0.5902(3) 0.6982(3) 0.41995(17) 0.0233(8) Uani 1 1 d . . . C43 C 0.4743(3) 0.6036(3) 0.38376(17) 0.0230(8) Uani 1 1 d . . . C44 C 0.4151(4) 0.5099(3) 0.40228(19) 0.0303(9) Uani 1 1 d . . . H44 H 0.4455 0.5036 0.4438 0.036 Uiso 1 1 calc R . . C45 C 0.3106(4) 0.4256(3) 0.3590(2) 0.0346(10) Uani 1 1 d . . . H45 H 0.2695 0.3605 0.3706 0.042 Uiso 1 1 calc R . . C46 C 0.2656(4) 0.4354(3) 0.2991(2) 0.0299(9) Uani 1 1 d . . . H46 H 0.1932 0.3785 0.2696 0.036 Uiso 1 1 calc R . . C47 C 0.3293(3) 0.5310(3) 0.28325(17) 0.0222(7) Uani 1 1 d . . . C48 C 0.3034(3) 0.5608(3) 0.22392(18) 0.0237(8) Uani 1 1 d . . . C49 C 0.2657(4) 0.5777(3) 0.1147(2) 0.0325(9) Uani 1 1 d . . . H49 H 0.2420 0.5703 0.0692 0.039 Uiso 1 1 calc R . . C51 C 0.9105(5) 0.5307(4) 0.3320(3) 0.0558(14) Uani 1 1 d . . . H51 H 0.8307 0.5099 0.3478 0.067 Uiso 1 1 calc R . . C52 C 0.9010(4) 0.0048(4) 0.7319(2) 0.0481(12) Uani 1 1 d . . . H52 H 0.9451 -0.0171 0.7657 0.058 Uiso 1 1 calc R . . C53 C 0.9402(4) 0.2038(4) 0.4384(2) 0.0377(10) Uani 1 1 d . . . C54 C 0.9929(5) 0.3048(4) 0.4205(3) 0.0548(14) Uani 1 1 d . . . H54A H 1.0693 0.3554 0.4531 0.082 Uiso 1 1 calc R . . H54B H 0.9329 0.3405 0.4198 0.082 Uiso 1 1 calc R . . H54C H 1.0122 0.2868 0.3766 0.082 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C50 0.0247(19) 0.0269(19) 0.0254(19) 0.0133(15) 0.0049(15) 0.0108(15) Fe1 0.0213(3) 0.0145(2) 0.0193(3) 0.00651(19) 0.00593(19) 0.00538(19) S1 0.0315(5) 0.0319(5) 0.0349(6) 0.0160(4) 0.0184(4) 0.0111(4) S2 0.0330(5) 0.0265(5) 0.0305(5) 0.0113(4) -0.0061(4) -0.0030(4) Cl1 0.0414(6) 0.0301(5) 0.0294(5) 0.0130(4) 0.0085(4) 0.0183(4) Cl2 0.0363(6) 0.0284(5) 0.0340(5) 0.0127(4) 0.0049(4) 0.0004(4) Cl3 0.0696(11) 0.0856(12) 0.1606(19) 0.0917(13) -0.0057(11) 0.0078(9) Cl4 0.0791(11) 0.0903(11) 0.0530(8) 0.0251(8) 0.0103(7) 0.0271(9) Cl5 0.0552(8) 0.0489(7) 0.0619(8) 0.0245(6) -0.0029(6) 0.0060(6) Cl6 0.0609(10) 0.0837(12) 0.1589(19) -0.0143(12) 0.0306(11) 0.0328(9) Cl7 0.0474(8) 0.0760(10) 0.1006(12) 0.0421(9) 0.0179(8) 0.0133(7) Cl8 0.0528(8) 0.1216(14) 0.0482(8) 0.0128(8) 0.0183(6) 0.0146(8) N1 0.0310(17) 0.0235(15) 0.0254(16) 0.0112(13) 0.0091(13) 0.0142(13) N2 0.0252(16) 0.0174(14) 0.0227(16) 0.0071(12) 0.0044(12) 0.0075(12) N3 0.0198(15) 0.0199(14) 0.0223(15) 0.0072(12) 0.0063(12) 0.0076(12) N4 0.0255(15) 0.0167(14) 0.0208(15) 0.0060(12) 0.0060(12) 0.0081(12) N5 0.0213(15) 0.0177(14) 0.0194(15) 0.0065(11) 0.0062(12) 0.0060(11) N6 0.0207(15) 0.0202(14) 0.0218(15) 0.0104(12) 0.0063(12) 0.0085(12) N7 0.046(2) 0.040(2) 0.054(3) 0.0127(19) 0.0133(19) 0.0110(18) O1 0.0255(13) 0.0168(12) 0.0258(13) 0.0063(10) 0.0055(10) 0.0059(10) O2 0.0318(15) 0.0293(15) 0.0406(17) 0.0178(13) 0.0018(12) 0.0014(12) O3 0.0335(16) 0.0458(18) 0.0513(19) 0.0316(15) 0.0155(14) 0.0134(13) O4 0.0452(18) 0.0358(16) 0.0384(17) 0.0074(13) 0.0167(14) 0.0151(14) O5 0.046(2) 0.079(3) 0.078(3) 0.025(2) 0.0278(19) 0.0144(19) O6 0.115(3) 0.0342(19) 0.089(3) 0.0184(19) 0.046(3) 0.041(2) O7 0.112(4) 0.146(4) 0.048(2) 0.058(3) 0.024(2) 0.088(3) O8 0.057(2) 0.0446(18) 0.0309(17) 0.0115(14) 0.0002(14) 0.0029(15) O9 0.069(3) 0.053(2) 0.072(3) 0.0038(19) -0.019(2) 0.0313(19) O10 0.059(2) 0.0319(16) 0.0435(19) 0.0075(14) 0.0032(15) 0.0101(15) O11 0.083(3) 0.063(2) 0.073(3) 0.028(2) 0.041(2) -0.011(2) C1 0.045(2) 0.036(2) 0.038(2) 0.0190(19) 0.0219(19) 0.0229(19) C2 0.060(3) 0.047(3) 0.050(3) 0.021(2) 0.035(2) 0.032(2) C3 0.076(4) 0.051(3) 0.050(3) 0.016(2) 0.037(3) 0.041(3) C4 0.061(3) 0.034(2) 0.037(2) 0.0110(19) 0.017(2) 0.027(2) C5 0.040(2) 0.0238(19) 0.0243(19) 0.0076(15) 0.0083(16) 0.0198(17) C6 0.033(2) 0.0180(17) 0.0214(18) 0.0078(14) 0.0009(15) 0.0095(15) C7 0.049(3) 0.0167(18) 0.034(2) 0.0039(16) 0.0029(19) 0.0130(17) C8 0.042(2) 0.0183(19) 0.043(3) 0.0126(17) 0.0041(19) 0.0033(17) C9 0.030(2) 0.026(2) 0.040(2) 0.0157(18) 0.0080(17) 0.0023(16) C10 0.0244(19) 0.0199(17) 0.027(2) 0.0104(15) 0.0051(15) 0.0048(14) C11 0.0230(18) 0.0207(17) 0.0232(18) 0.0083(14) 0.0055(14) 0.0040(14) C12 0.033(2) 0.028(2) 0.031(2) 0.0072(16) 0.0112(17) 0.0140(17) C13 0.0241(18) 0.0205(17) 0.0267(19) 0.0059(14) 0.0085(15) 0.0100(14) C14 0.0239(18) 0.0197(17) 0.0254(19) 0.0063(14) 0.0088(14) 0.0104(14) C15 0.031(2) 0.0260(19) 0.0203(18) 0.0043(15) 0.0018(15) 0.0135(16) C16 0.044(2) 0.034(2) 0.0189(19) 0.0122(16) 0.0089(17) 0.0211(18) C17 0.043(2) 0.0239(19) 0.026(2) 0.0122(16) 0.0100(17) 0.0156(17) C18 0.0295(19) 0.0211(18) 0.0241(19) 0.0080(14) 0.0080(15) 0.0134(15) C19 0.030(2) 0.0263(19) 0.0201(18) 0.0098(15) 0.0088(15) 0.0161(15) C20 0.031(2) 0.0205(17) 0.0196(18) 0.0080(14) 0.0059(15) 0.0125(15) C21 0.031(2) 0.0270(19) 0.028(2) 0.0148(16) 0.0105(16) 0.0132(16) C22 0.0263(19) 0.0223(18) 0.034(2) 0.0128(16) 0.0054(16) 0.0069(15) C23 0.031(2) 0.0201(18) 0.0242(19) 0.0072(15) 0.0031(15) 0.0060(15) C24 0.0290(19) 0.0195(17) 0.0219(18) 0.0101(14) 0.0069(15) 0.0108(14) C25 0.0250(18) 0.0165(16) 0.0234(18) 0.0087(14) 0.0047(14) 0.0070(14) C26 0.036(2) 0.032(2) 0.047(3) 0.013(2) 0.013(2) 0.0015(18) C27 0.0263(19) 0.0199(17) 0.0182(17) 0.0067(14) 0.0013(14) 0.0082(14) C28 0.041(2) 0.0177(17) 0.026(2) 0.0089(15) 0.0080(16) 0.0129(16) C29 0.045(2) 0.027(2) 0.028(2) 0.0057(16) 0.0065(18) 0.0215(18) C30 0.036(2) 0.029(2) 0.0215(19) 0.0096(15) 0.0087(16) 0.0159(17) C31 0.0258(19) 0.0230(18) 0.0213(18) 0.0097(14) 0.0006(14) 0.0090(15) C32 0.0264(19) 0.0176(17) 0.0215(18) 0.0050(14) 0.0010(14) 0.0072(14) C33 0.028(2) 0.027(2) 0.048(3) 0.0157(18) 0.0006(18) 0.0124(16) C34 0.033(2) 0.042(2) 0.039(2) 0.020(2) -0.0011(18) 0.0096(19) C35 0.028(2) 0.032(2) 0.046(3) 0.0094(19) -0.0002(18) 0.0093(17) C36 0.027(2) 0.029(2) 0.051(3) 0.0096(19) 0.0131(19) 0.0071(17) C37 0.051(3) 0.035(2) 0.042(3) 0.021(2) 0.016(2) 0.013(2) C38 0.0277(19) 0.0218(18) 0.026(2) 0.0053(15) 0.0066(15) 0.0067(15) C39 0.028(2) 0.030(2) 0.033(2) 0.0037(17) -0.0003(17) 0.0086(16) C40 0.035(2) 0.033(2) 0.029(2) 0.0066(17) -0.0051(17) 0.0158(18) C41 0.038(2) 0.027(2) 0.026(2) 0.0102(16) 0.0058(17) 0.0165(17) C42 0.0284(19) 0.0195(17) 0.0231(19) 0.0062(14) 0.0087(15) 0.0099(15) C43 0.0285(19) 0.0209(17) 0.0219(18) 0.0080(14) 0.0082(15) 0.0102(15) C44 0.036(2) 0.027(2) 0.029(2) 0.0160(16) 0.0089(17) 0.0089(16) C45 0.043(2) 0.0226(19) 0.037(2) 0.0188(17) 0.0099(19) 0.0047(17) C46 0.027(2) 0.0211(18) 0.035(2) 0.0115(16) 0.0028(16) 0.0006(15) C47 0.0230(18) 0.0181(17) 0.0253(19) 0.0092(14) 0.0058(14) 0.0056(14) C48 0.0218(18) 0.0218(18) 0.0272(19) 0.0120(15) 0.0026(15) 0.0056(14) C49 0.030(2) 0.029(2) 0.031(2) 0.0141(17) -0.0006(17) 0.0021(16) C51 0.044(3) 0.053(3) 0.069(4) 0.035(3) 0.002(2) 0.008(2) C52 0.041(3) 0.064(3) 0.049(3) 0.024(2) 0.011(2) 0.026(2) C53 0.030(2) 0.041(3) 0.043(3) 0.013(2) 0.0110(19) 0.0137(19) C54 0.049(3) 0.055(3) 0.081(4) 0.044(3) 0.021(3) 0.026(2) _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 C50 C49 1.359(5) 2_665 ? C50 N6 1.389(4) 2_665 ? C50 C31 1.474(5) . ? Fe1 N5 1.897(3) . ? Fe1 N2 1.904(3) . ? Fe1 N4 1.966(3) . ? Fe1 N1 1.983(3) . ? Fe1 N6 2.038(3) . ? Fe1 N3 2.040(3) . ? S1 C11 1.700(4) . ? S1 C12 1.716(4) . ? S2 C49 1.704(4) . ? S2 C48 1.707(4) . ? Cl1 O7 1.405(4) . ? Cl1 O6 1.414(3) . ? Cl1 O5 1.421(4) . ? Cl1 O4 1.432(3) . ? Cl2 O11 1.414(3) . ? Cl2 O9 1.424(4) . ? Cl2 O10 1.435(3) . ? Cl2 O8 1.437(3) . ? Cl3 C51 1.752(5) . ? Cl4 C51 1.764(6) . ? Cl5 C51 1.752(5) . ? Cl6 C52 1.746(5) . ? Cl7 C52 1.768(5) . ? Cl8 C52 1.727(5) . ? N1 C1 1.342(5) . ? N1 C5 1.368(5) . ? N2 C6 1.346(5) . ? N2 C10 1.354(4) . ? N3 C11 1.330(4) . ? N3 C13 1.383(4) . ? N4 C38 1.342(4) . ? N4 C42 1.371(4) . ? N5 C43 1.347(4) . ? N5 C47 1.350(4) . ? N6 C48 1.331(4) . ? N6 C50 1.389(4) 2_665 ? N7 C53 1.117(5) . ? O1 C25 1.386(4) . ? O1 C33 1.437(5) . ? O2 C34 1.421(5) . ? O2 C35 1.426(4) . ? O3 C36 1.405(5) . ? O3 C37 1.427(5) . ? C1 C2 1.383(6) . ? C1 H1 0.9500 . ? C2 C3 1.371(6) . ? C2 H2 0.9500 . ? C3 C4 1.384(6) . ? C3 H3 0.9500 . ? C4 C5 1.377(5) . ? C4 H4 0.9500 . ? C5 C6 1.459(5) . ? C6 C7 1.385(5) . ? C7 C8 1.376(6) . ? C7 H7 0.9500 . ? C8 C9 1.399(6) . ? C8 H8 0.9500 . ? C9 C10 1.382(5) . ? C9 H9 0.9500 . ? C10 C11 1.447(5) . ? C12 C13 1.364(5) . ? C12 H12 0.9500 . ? C13 C14 1.471(5) . ? C14 C15 1.389(5) . ? C14 C19 1.390(5) . ? C15 C16 1.383(5) . ? C15 H15 0.9500 . ? C16 C17 1.388(5) . ? C16 H16 0.9500 . ? C17 C18 1.388(5) . ? C17 H17 0.9500 . ? C18 C19 1.396(5) . ? C18 C20 1.491(5) . ? C19 H19 0.9500 . ? C20 C21 1.391(5) . ? C20 C25 1.400(5) . ? C21 C22 1.386(5) . ? C21 H21 0.9500 . ? C22 C23 1.390(5) . ? C22 C26 1.506(5) . ? C23 C24 1.398(5) . ? C23 H23 0.9500 . ? C24 C25 1.403(5) . ? C24 C27 1.488(5) . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 C28 1.388(5) . ? C27 C32 1.392(5) . ? C28 C29 1.388(5) . ? C28 H28 0.9500 . ? C29 C30 1.389(5) . ? C29 H29 0.9500 . ? C30 C31 1.388(5) . ? C30 H30 0.9500 . ? C31 C32 1.391(5) . ? C32 H32 0.9500 . ? C33 C34 1.498(5) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? C35 C36 1.502(6) . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? C36 H36A 0.9900 . ? C36 H36B 0.9900 . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C38 C39 1.378(5) . ? C38 H38 0.9500 . ? C39 C40 1.383(6) . ? C39 H39 0.9500 . ? C40 C41 1.383(5) . ? C40 H40 0.9500 . ? C41 C42 1.383(5) . ? C41 H41 0.9500 . ? C42 C43 1.469(5) . ? C43 C44 1.388(5) . ? C44 C45 1.386(5) . ? C44 H44 0.9500 . ? C45 C46 1.379(6) . ? C45 H45 0.9500 . ? C46 C47 1.390(5) . ? C46 H46 0.9500 . ? C47 C48 1.447(5) . ? C49 C50 1.359(5) 2_665 ? C49 H49 0.9500 . ? C51 H51 1.0000 . ? C52 H52 1.0000 . ? C53 C54 1.448(6) . ? C54 H54A 0.9800 . ? C54 H54B 0.9800 . ? C54 H54C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C49 C50 N6 113.9(3) 2_665 2_665 ? C49 C50 C31 123.8(3) 2_665 . ? N6 C50 C31 122.3(3) 2_665 . ? N5 Fe1 N2 172.35(12) . . ? N5 Fe1 N4 80.50(12) . . ? N2 Fe1 N4 95.46(12) . . ? N5 Fe1 N1 93.30(12) . . ? N2 Fe1 N1 80.12(12) . . ? N4 Fe1 N1 89.65(12) . . ? N5 Fe1 N6 79.70(12) . . ? N2 Fe1 N6 104.95(12) . . ? N4 Fe1 N6 159.12(12) . . ? N1 Fe1 N6 98.03(12) . . ? N5 Fe1 N3 106.64(12) . . ? N2 Fe1 N3 80.03(12) . . ? N4 Fe1 N3 94.28(12) . . ? N1 Fe1 N3 160.04(12) . . ? N6 Fe1 N3 85.12(11) . . ? C11 S1 C12 89.08(18) . . ? C49 S2 C48 89.35(18) . . ? O7 Cl1 O6 111.1(3) . . ? O7 Cl1 O5 109.7(3) . . ? O6 Cl1 O5 108.0(3) . . ? O7 Cl1 O4 110.1(2) . . ? O6 Cl1 O4 109.0(2) . . ? O5 Cl1 O4 108.9(2) . . ? O11 Cl2 O9 111.7(3) . . ? O11 Cl2 O10 110.3(2) . . ? O9 Cl2 O10 108.3(2) . . ? O11 Cl2 O8 109.1(2) . . ? O9 Cl2 O8 108.3(2) . . ? O10 Cl2 O8 109.15(19) . . ? C1 N1 C5 117.9(3) . . ? C1 N1 Fe1 127.2(3) . . ? C5 N1 Fe1 114.7(2) . . ? C6 N2 C10 120.4(3) . . ? C6 N2 Fe1 119.5(2) . . ? C10 N2 Fe1 120.0(2) . . ? C11 N3 C13 110.4(3) . . ? C11 N3 Fe1 111.7(2) . . ? C13 N3 Fe1 136.1(2) . . ? C38 N4 C42 117.2(3) . . ? C38 N4 Fe1 128.0(2) . . ? C42 N4 Fe1 114.8(2) . . ? C43 N5 C47 120.1(3) . . ? C43 N5 Fe1 118.9(2) . . ? C47 N5 Fe1 120.8(2) . . ? C48 N6 C50 110.1(3) . 2_665 ? C48 N6 Fe1 111.7(2) . . ? C50 N6 Fe1 135.2(2) 2_665 . ? C25 O1 C33 116.2(3) . . ? C34 O2 C35 110.9(3) . . ? C36 O3 C37 113.3(3) . . ? N1 C1 C2 122.6(4) . . ? N1 C1 H1 118.7 . . ? C2 C1 H1 118.7 . . ? C3 C2 C1 119.4(4) . . ? C3 C2 H2 120.3 . . ? C1 C2 H2 120.3 . . ? C2 C3 C4 118.7(4) . . ? C2 C3 H3 120.6 . . ? C4 C3 H3 120.6 . . ? C5 C4 C3 119.8(4) . . ? C5 C4 H4 120.1 . . ? C3 C4 H4 120.1 . . ? N1 C5 C4 121.5(4) . . ? N1 C5 C6 113.5(3) . . ? C4 C5 C6 125.0(4) . . ? N2 C6 C7 120.5(3) . . ? N2 C6 C5 111.7(3) . . ? C7 C6 C5 127.7(4) . . ? C8 C7 C6 119.6(4) . . ? C8 C7 H7 120.2 . . ? C6 C7 H7 120.2 . . ? C7 C8 C9 119.8(4) . . ? C7 C8 H8 120.1 . . ? C9 C8 H8 120.1 . . ? C10 C9 C8 118.2(4) . . ? C10 C9 H9 120.9 . . ? C8 C9 H9 120.9 . . ? N2 C10 C9 121.4(3) . . ? N2 C10 C11 110.0(3) . . ? C9 C10 C11 128.6(3) . . ? N3 C11 C10 117.9(3) . . ? N3 C11 S1 115.3(3) . . ? C10 C11 S1 126.5(3) . . ? C13 C12 S1 111.4(3) . . ? C13 C12 H12 124.3 . . ? S1 C12 H12 124.3 . . ? C12 C13 N3 113.7(3) . . ? C12 C13 C14 123.0(3) . . ? N3 C13 C14 123.2(3) . . ? C15 C14 C19 120.0(3) . . ? C15 C14 C13 121.7(3) . . ? C19 C14 C13 118.0(3) . . ? C16 C15 C14 119.7(3) . . ? C16 C15 H15 120.1 . . ? C14 C15 H15 120.1 . . ? C15 C16 C17 120.1(3) . . ? C15 C16 H16 119.9 . . ? C17 C16 H16 119.9 . . ? C16 C17 C18 120.8(3) . . ? C16 C17 H17 119.6 . . ? C18 C17 H17 119.6 . . ? C17 C18 C19 118.6(3) . . ? C17 C18 C20 121.1(3) . . ? C19 C18 C20 120.3(3) . . ? C14 C19 C18 120.5(3) . . ? C14 C19 H19 119.7 . . ? C18 C19 H19 119.7 . . ? C21 C20 C25 118.9(3) . . ? C21 C20 C18 120.8(3) . . ? C25 C20 C18 120.3(3) . . ? C22 C21 C20 121.7(3) . . ? C22 C21 H21 119.1 . . ? C20 C21 H21 119.1 . . ? C21 C22 C23 118.6(3) . . ? C21 C22 C26 120.6(3) . . ? C23 C22 C26 120.8(3) . . ? C22 C23 C24 121.7(3) . . ? C22 C23 H23 119.2 . . ? C24 C23 H23 119.2 . . ? C23 C24 C25 118.4(3) . . ? C23 C24 C27 120.6(3) . . ? C25 C24 C27 120.9(3) . . ? O1 C25 C20 118.3(3) . . ? O1 C25 C24 121.0(3) . . ? C20 C25 C24 120.7(3) . . ? C22 C26 H26A 109.5 . . ? C22 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C22 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C28 C27 C32 118.6(3) . . ? C28 C27 C24 121.5(3) . . ? C32 C27 C24 119.9(3) . . ? C29 C28 C27 120.9(3) . . ? C29 C28 H28 119.6 . . ? C27 C28 H28 119.6 . . ? C28 C29 C30 120.1(3) . . ? C28 C29 H29 120.0 . . ? C30 C29 H29 120.0 . . ? C31 C30 C29 119.6(3) . . ? C31 C30 H30 120.2 . . ? C29 C30 H30 120.2 . . ? C30 C31 C32 119.9(3) . . ? C30 C31 C50 122.1(3) . . ? C32 C31 C50 117.9(3) . . ? C31 C32 C27 120.9(3) . . ? C31 C32 H32 119.6 . . ? C27 C32 H32 119.6 . . ? O1 C33 C34 108.4(3) . . ? O1 C33 H33A 110.0 . . ? C34 C33 H33A 110.0 . . ? O1 C33 H33B 110.0 . . ? C34 C33 H33B 110.0 . . ? H33A C33 H33B 108.4 . . ? O2 C34 C33 110.7(3) . . ? O2 C34 H34A 109.5 . . ? C33 C34 H34A 109.5 . . ? O2 C34 H34B 109.5 . . ? C33 C34 H34B 109.5 . . ? H34A C34 H34B 108.1 . . ? O2 C35 C36 110.2(3) . . ? O2 C35 H35A 109.6 . . ? C36 C35 H35A 109.6 . . ? O2 C35 H35B 109.6 . . ? C36 C35 H35B 109.6 . . ? H35A C35 H35B 108.1 . . ? O3 C36 C35 108.8(3) . . ? O3 C36 H36A 109.9 . . ? C35 C36 H36A 109.9 . . ? O3 C36 H36B 109.9 . . ? C35 C36 H36B 109.9 . . ? H36A C36 H36B 108.3 . . ? O3 C37 H37A 109.5 . . ? O3 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? O3 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? N4 C38 C39 123.3(4) . . ? N4 C38 H38 118.4 . . ? C39 C38 H38 118.4 . . ? C38 C39 C40 119.0(4) . . ? C38 C39 H39 120.5 . . ? C40 C39 H39 120.5 . . ? C39 C40 C41 119.1(4) . . ? C39 C40 H40 120.5 . . ? C41 C40 H40 120.5 . . ? C42 C41 C40 119.0(4) . . ? C42 C41 H41 120.5 . . ? C40 C41 H41 120.5 . . ? N4 C42 C41 122.3(3) . . ? N4 C42 C43 112.8(3) . . ? C41 C42 C43 124.9(3) . . ? N5 C43 C44 121.0(3) . . ? N5 C43 C42 111.6(3) . . ? C44 C43 C42 127.2(3) . . ? C45 C44 C43 118.6(4) . . ? C45 C44 H44 120.7 . . ? C43 C44 H44 120.7 . . ? C46 C45 C44 120.7(3) . . ? C46 C45 H45 119.7 . . ? C44 C45 H45 119.7 . . ? C45 C46 C47 118.0(3) . . ? C45 C46 H46 121.0 . . ? C47 C46 H46 121.0 . . ? N5 C47 C46 121.6(3) . . ? N5 C47 C48 109.3(3) . . ? C46 C47 C48 129.1(3) . . ? N6 C48 C47 117.7(3) . . ? N6 C48 S2 115.0(3) . . ? C47 C48 S2 126.5(3) . . ? C50 C49 S2 111.6(3) 2_665 . ? C50 C49 H49 124.2 2_665 . ? S2 C49 H49 124.2 . . ? Cl5 C51 Cl3 110.7(3) . . ? Cl5 C51 Cl4 109.9(3) . . ? Cl3 C51 Cl4 110.7(3) . . ? Cl5 C51 H51 108.5 . . ? Cl3 C51 H51 108.5 . . ? Cl4 C51 H51 108.5 . . ? Cl8 C52 Cl6 110.1(3) . . ? Cl8 C52 Cl7 110.2(3) . . ? Cl6 C52 Cl7 110.8(3) . . ? Cl8 C52 H52 108.5 . . ? Cl6 C52 H52 108.5 . . ? Cl7 C52 H52 108.5 . . ? N7 C53 C54 178.6(5) . . ? C53 C54 H54A 109.5 . . ? C53 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? C53 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.962 _diffrn_reflns_theta_full 28.72 _diffrn_measured_fraction_theta_full 0.962 _refine_diff_density_max 1.518 _refine_diff_density_min -1.128 _refine_diff_density_rms 0.089 _database_code_depnum_ccdc_archive 'CCDC 958173' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_mo_chris_nh2cdbf4_0m _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C90 H63 Cd2 N14 S4, 5(Cl O4), 0.86(C H3 N O2), 4(C H2 Cl2), H2O ' _chemical_formula_sum 'C94.86 H75.57 Cd2 Cl13 F0 N14.86 O22.71 S4' _chemical_formula_weight 2600.83 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' F F 0.0171 0.0103 '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' Cd Cd -0.8075 1.2024 '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 ' _symmetry_space_group_name_Hall -P1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.8209(7) _cell_length_b 18.3351(9) _cell_length_c 21.5994(10) _cell_angle_alpha 95.0080(10) _cell_angle_beta 92.1730(10) _cell_angle_gamma 107.4850(10) _cell_volume 5188.8(4) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 9833 _cell_measurement_theta_min 2.34 _cell_measurement_theta_max 29.46 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.665 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2622.8 _exptl_absorpt_coefficient_mu 0.905 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7136 _exptl_absorpt_correction_T_max 0.9150 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 118786 _diffrn_reflns_av_R_equivalents 0.0580 _diffrn_reflns_av_sigmaI/netI 0.0677 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 1.43 _diffrn_reflns_theta_max 30.51 _reflns_number_total 31560 _reflns_number_gt 20025 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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. Restraints used in LS refinement sadi c1a cl2a c1r cl1r c1a cl2a c1r cl2r sadi cl2a cl1a cl1r cl2r DELU 0.01 C1S N1S O1S O2S C1R C93 SIMU 0.04 C1S N1S O2S O1S C1R C93 ; _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^)+(0.0854P)^2^+6.6062P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 31560 _refine_ls_number_parameters 1401 _refine_ls_number_restraints 52 _refine_ls_R_factor_all 0.1070 _refine_ls_R_factor_gt 0.0588 _refine_ls_wR_factor_ref 0.1784 _refine_ls_wR_factor_gt 0.1514 _refine_ls_goodness_of_fit_ref 1.045 _refine_ls_restrained_S_all 1.046 _refine_ls_shift/su_max 0.004 _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 Cd1 Cd 0.29790(2) -0.300267(16) 0.043267(12) 0.02437(7) Uani 1 1 d . . . Cd2 Cd 0.19465(2) 0.319824(16) 0.465441(12) 0.02267(7) Uani 1 1 d . . . S1 S 0.31584(9) 0.30614(7) 0.26264(4) 0.0324(2) Uani 1 1 d . . . S2 S 0.37197(9) -0.03227(6) 0.03288(5) 0.0337(2) Uani 1 1 d . . . S3 S 0.13368(9) 0.05399(6) 0.48920(5) 0.0344(2) Uani 1 1 d . . . S4 S 0.15240(9) -0.33080(7) 0.23818(5) 0.0356(3) Uani 1 1 d . . . Cl1 Cl 0.36411(8) 0.61961(6) 0.38330(5) 0.0350(2) Uani 1 1 d . . . Cl2 Cl 0.14663(8) 0.38254(6) 0.10743(5) 0.0302(2) Uani 1 1 d . . . Cl3 Cl 0.48228(10) 0.16853(7) 0.15959(5) 0.0411(3) Uani 1 1 d . . . Cl4 Cl 0.87756(9) 0.58254(7) 0.29423(5) 0.0405(3) Uani 1 1 d . . . Cl5 Cl 0.71642(14) 0.02080(10) 0.32633(10) 0.0736(5) Uani 1 1 d . . . Cl6 Cl 0.93730(11) 0.14457(8) 0.56044(7) 0.0548(3) Uani 1 1 d . . . Cl7 Cl 0.8910(2) 0.11121(11) 0.68636(8) 0.1046(8) Uani 1 1 d . . . Cl8 Cl 0.60594(12) 0.22951(11) 0.35644(7) 0.0656(4) Uani 1 1 d . . . Cl9 Cl 0.78272(15) 0.33238(13) 0.30565(10) 0.1030(8) Uani 1 1 d . . . N1 N 0.0526(3) 0.3624(2) 0.48910(14) 0.0264(7) Uani 1 1 d . . . N2 N 0.1452(2) 0.37631(18) 0.38322(14) 0.0220(6) Uani 1 1 d . . . N3 N 0.2883(2) 0.30132(18) 0.37877(14) 0.0224(6) Uani 1 1 d . . . N4 N 0.4618(3) 0.03029(19) 0.31931(15) 0.0298(7) Uani 1 1 d . . . H4A H 0.5105 0.0138 0.3007 0.045 Uiso 1 1 calc R . . H4B H 0.4911 0.0771 0.3411 0.045 Uiso 1 1 calc R . . H4C H 0.4155 0.0342 0.2897 0.045 Uiso 1 1 calc R . . N5 N 0.3627(3) -0.16618(19) 0.06205(14) 0.0250(7) Uani 1 1 d . . . N6 N 0.2575(2) -0.24743(19) -0.04312(14) 0.0245(7) Uani 1 1 d . . . N7 N 0.1837(3) -0.3947(2) -0.02629(15) 0.0296(7) Uani 1 1 d . . . N8 N 0.3091(3) 0.4184(2) 0.53270(15) 0.0285(7) Uani 1 1 d . . . N9 N 0.2367(2) 0.27290(19) 0.55503(14) 0.0231(6) Uani 1 1 d . . . N10 N 0.1284(2) 0.18235(18) 0.45401(14) 0.0232(6) Uani 1 1 d . . . N11 N 0.0501(4) -0.0232(2) 0.20305(17) 0.0526(12) Uani 1 1 d . . . H11A H 0.0339 -0.0056 0.2391 0.063 Uiso 1 1 calc R . . H11B H 0.0420 -0.0727 0.1949 0.063 Uiso 1 1 calc R . . N12 N 0.1993(2) -0.29965(18) 0.12860(14) 0.0227(6) Uani 1 1 d . . . N13 N 0.3429(2) -0.37105(18) 0.11638(14) 0.0236(6) Uani 1 1 d . . . N14 N 0.4410(3) -0.3357(2) 0.01410(15) 0.0308(7) Uani 1 1 d . . . O1 O 0.4567(3) 0.6583(2) 0.3577(2) 0.0553(10) Uani 1 1 d . . . O2 O 0.2837(3) 0.6444(3) 0.35717(17) 0.0553(10) Uani 1 1 d . . . O3 O 0.3716(3) 0.6390(2) 0.44942(15) 0.0566(10) Uani 1 1 d . . . O4 O 0.3419(3) 0.5387(2) 0.36886(17) 0.0548(10) Uani 1 1 d . . . O5 O 0.1465(3) 0.3732(2) 0.04065(14) 0.0487(9) Uani 1 1 d . . . O6 O 0.2352(3) 0.3676(2) 0.13396(15) 0.0427(8) Uani 1 1 d . . . O7 O 0.1487(3) 0.45977(18) 0.12791(16) 0.0409(8) Uani 1 1 d . . . O8 O 0.0573(3) 0.3295(2) 0.12729(18) 0.0489(9) Uani 1 1 d . . . O9 O 0.5541(4) 0.2423(2) 0.1709(2) 0.0900(18) Uani 1 1 d . . . O10 O 0.3817(4) 0.1676(3) 0.1699(2) 0.0819(16) Uani 1 1 d . . . O11 O 0.5095(3) 0.1204(2) 0.20244(18) 0.0614(11) Uani 1 1 d . . . O12 O 0.4863(3) 0.1391(2) 0.09699(16) 0.0504(9) Uani 1 1 d . . . O13 O 0.9229(3) 0.5361(3) 0.25684(18) 0.0622(11) Uani 1 1 d . . . O14 O 0.8490(3) 0.5460(2) 0.35082(19) 0.0604(11) Uani 1 1 d . . . O15 O 0.7886(4) 0.5885(3) 0.2621(2) 0.0812(15) Uani 1 1 d . . . O16 O 0.9497(3) 0.6562(2) 0.30933(17) 0.0595(11) Uani 1 1 d . . . O17 O 0.6478(5) 0.0255(4) 0.2750(3) 0.115(2) Uani 1 1 d . . . O18 O 0.6539(5) -0.0114(5) 0.3743(3) 0.140(3) Uani 1 1 d . . . O19 O 0.7807(6) 0.0907(4) 0.3476(6) 0.211(5) Uani 1 1 d . . . O20 O 0.7746(7) -0.0283(4) 0.3048(3) 0.148(3) Uani 1 1 d . . . C1 C 0.0054(3) 0.3505(3) 0.54172(19) 0.0331(9) Uani 1 1 d . . . H1 H 0.0325 0.3268 0.5726 0.040 Uiso 1 1 calc R . . C2 C -0.0814(4) 0.3713(3) 0.5535(2) 0.0389(10) Uani 1 1 d . . . H2 H -0.1128 0.3625 0.5916 0.047 Uiso 1 1 calc R . . C3 C -0.1202(4) 0.4048(3) 0.5086(2) 0.0392(10) Uani 1 1 d . . . H3 H -0.1807 0.4182 0.5148 0.047 Uiso 1 1 calc R . . C4 C -0.0714(3) 0.4192(3) 0.4541(2) 0.0350(9) Uani 1 1 d . . . H4 H -0.0968 0.4437 0.4231 0.042 Uiso 1 1 calc R . . C5 C 0.0152(3) 0.3972(2) 0.44558(17) 0.0253(8) Uani 1 1 d . . . C6 C 0.0707(3) 0.4086(2) 0.38784(17) 0.0241(7) Uani 1 1 d . . . C7 C 0.0452(3) 0.4469(2) 0.33966(19) 0.0299(8) Uani 1 1 d . . . H7 H -0.0065 0.4710 0.3439 0.036 Uiso 1 1 calc R . . C8 C 0.0965(3) 0.4493(3) 0.28565(19) 0.0316(9) Uani 1 1 d . . . H8 H 0.0806 0.4756 0.2526 0.038 Uiso 1 1 calc R . . C9 C 0.1714(3) 0.4130(2) 0.28007(18) 0.0283(8) Uani 1 1 d . . . H9 H 0.2063 0.4128 0.2430 0.034 Uiso 1 1 calc R . . C10 C 0.1936(3) 0.3770(2) 0.33046(16) 0.0227(7) Uani 1 1 d . . . C11 C 0.2657(3) 0.3323(2) 0.32923(16) 0.0236(7) Uani 1 1 d . . . C12 C 0.3686(3) 0.2507(3) 0.30295(18) 0.0319(9) Uani 1 1 d . . . H12 H 0.4087 0.2213 0.2854 0.038 Uiso 1 1 calc R . . C13 C 0.3461(3) 0.2538(2) 0.36408(17) 0.0231(7) Uani 1 1 d . . . C14 C 0.3753(3) 0.2088(2) 0.41100(17) 0.0226(7) Uani 1 1 d . . . C15 C 0.4136(3) 0.2408(2) 0.47087(18) 0.0259(8) Uani 1 1 d . . . H15 H 0.4211 0.2934 0.4830 0.031 Uiso 1 1 calc R . . C16 C 0.4408(3) 0.1969(2) 0.51284(18) 0.0287(8) Uani 1 1 d . . . H16 H 0.4663 0.2193 0.5538 0.034 Uiso 1 1 calc R . . C17 C 0.4312(3) 0.1203(2) 0.49576(18) 0.0264(8) Uani 1 1 d . . . H17 H 0.4504 0.0907 0.5251 0.032 Uiso 1 1 calc R . . C18 C 0.3937(3) 0.0862(2) 0.43586(17) 0.0235(7) Uani 1 1 d . . . C19 C 0.3639(3) 0.1309(2) 0.39414(17) 0.0242(7) Uani 1 1 d . . . H19 H 0.3355 0.1081 0.3537 0.029 Uiso 1 1 calc R . . C20 C 0.3817(3) 0.0037(2) 0.41873(17) 0.0256(8) Uani 1 1 d . . . C21 C 0.4108(3) -0.0249(2) 0.36195(17) 0.0246(8) Uani 1 1 d . . . C22 C 0.3964(3) -0.1026(2) 0.34661(17) 0.0252(8) Uani 1 1 d . . . C23 C 0.3555(3) -0.1531(2) 0.39026(19) 0.0296(8) Uani 1 1 d . . . H23 H 0.3451 -0.2066 0.3804 0.035 Uiso 1 1 calc R . . C24 C 0.3296(3) -0.1270(3) 0.44807(19) 0.0310(9) Uani 1 1 d . . . C25 C 0.3412(3) -0.0497(2) 0.46096(18) 0.0291(8) Uani 1 1 d . . . H25 H 0.3211 -0.0321 0.4996 0.035 Uiso 1 1 calc R . . C26 C 0.2878(4) -0.1840(3) 0.4955(2) 0.0386(10) Uani 1 1 d . . . H26A H 0.2901 -0.1557 0.5364 0.058 Uiso 1 1 calc R . . H26B H 0.3291 -0.2188 0.4979 0.058 Uiso 1 1 calc R . . H26C H 0.2173 -0.2138 0.4824 0.058 Uiso 1 1 calc R . . C27 C 0.4246(3) -0.1348(2) 0.28661(18) 0.0262(8) Uani 1 1 d . . . C28 C 0.4762(3) -0.1894(2) 0.28646(19) 0.0322(9) Uani 1 1 d . . . H28 H 0.4953 -0.2047 0.3248 0.039 Uiso 1 1 calc R . . C29 C 0.4998(4) -0.2217(2) 0.2306(2) 0.0337(9) Uani 1 1 d . . . H29 H 0.5330 -0.2601 0.2310 0.040 Uiso 1 1 calc R . . C30 C 0.4754(3) -0.1985(2) 0.17485(19) 0.0301(9) Uani 1 1 d . . . H30 H 0.4937 -0.2198 0.1370 0.036 Uiso 1 1 calc R . . C31 C 0.4243(3) -0.1438(2) 0.17356(17) 0.0253(8) Uani 1 1 d . . . C32 C 0.3978(3) -0.1132(2) 0.22966(18) 0.0267(8) Uani 1 1 d . . . H32 H 0.3610 -0.0770 0.2290 0.032 Uiso 1 1 calc R . . C33 C 0.3991(3) -0.1163(2) 0.11507(18) 0.0271(8) Uani 1 1 d . . . C34 C 0.4097(3) -0.0409(2) 0.1073(2) 0.0335(9) Uani 1 1 d . . . H34 H 0.4345 0.0007 0.1390 0.040 Uiso 1 1 calc R . . C35 C 0.3442(3) -0.1293(2) 0.01507(18) 0.0261(8) Uani 1 1 d . . . C36 C 0.2932(3) -0.1716(2) -0.04438(17) 0.0262(8) Uani 1 1 d . . . C37 C 0.2779(3) -0.1359(3) -0.09633(19) 0.0328(9) Uani 1 1 d . . . H37 H 0.3056 -0.0818 -0.0970 0.039 Uiso 1 1 calc R . . C38 C 0.2208(4) -0.1820(3) -0.1471(2) 0.0372(10) Uani 1 1 d . . . H38 H 0.2093 -0.1598 -0.1836 0.045 Uiso 1 1 calc R . . C39 C 0.1803(3) -0.2607(3) -0.14493(18) 0.0330(9) Uani 1 1 d . . . H39 H 0.1391 -0.2923 -0.1792 0.040 Uiso 1 1 calc R . . C40 C 0.2011(3) -0.2925(2) -0.09165(16) 0.0261(8) Uani 1 1 d . . . C41 C 0.1591(3) -0.3752(2) -0.08223(17) 0.0268(8) Uani 1 1 d . . . C42 C 0.0976(3) -0.4293(3) -0.12738(19) 0.0342(9) Uani 1 1 d . . . H42 H 0.0819 -0.4148 -0.1668 0.041 Uiso 1 1 calc R . . C43 C 0.0592(4) -0.5053(3) -0.1143(2) 0.0412(11) Uani 1 1 d . . . H43 H 0.0163 -0.5431 -0.1445 0.049 Uiso 1 1 calc R . . C44 C 0.0839(4) -0.5246(3) -0.0576(2) 0.0411(11) Uani 1 1 d . . . H44 H 0.0584 -0.5762 -0.0479 0.049 Uiso 1 1 calc R . . C45 C 0.1466(4) -0.4681(3) -0.0144(2) 0.0382(10) Uani 1 1 d . . . H45 H 0.1638 -0.4820 0.0250 0.046 Uiso 1 1 calc R . . C46 C 0.3441(4) 0.4906(3) 0.5182(2) 0.0404(11) Uani 1 1 d . . . H46 H 0.3263 0.5019 0.4780 0.049 Uiso 1 1 calc R . . C47 C 0.4051(5) 0.5492(3) 0.5594(2) 0.0534(14) Uani 1 1 d . . . H47 H 0.4294 0.6000 0.5477 0.064 Uiso 1 1 calc R . . C48 C 0.4306(5) 0.5333(3) 0.6180(2) 0.0539(15) Uani 1 1 d . . . H48 H 0.4724 0.5729 0.6474 0.065 Uiso 1 1 calc R . . C49 C 0.3943(4) 0.4590(3) 0.6332(2) 0.0408(11) Uani 1 1 d . . . H49 H 0.4111 0.4465 0.6731 0.049 Uiso 1 1 calc R . . C50 C 0.3333(3) 0.4029(2) 0.58961(17) 0.0254(8) Uani 1 1 d . . . C51 C 0.2910(3) 0.3211(2) 0.60291(17) 0.0244(8) Uani 1 1 d . . . C52 C 0.3090(3) 0.2940(3) 0.65907(19) 0.0345(9) Uani 1 1 d . . . H52 H 0.3461 0.3285 0.6932 0.041 Uiso 1 1 calc R . . C53 C 0.2722(4) 0.2161(3) 0.6645(2) 0.0394(11) Uani 1 1 d . . . H53 H 0.2832 0.1967 0.7027 0.047 Uiso 1 1 calc R . . C54 C 0.2193(3) 0.1665(3) 0.6143(2) 0.0339(9) Uani 1 1 d . . . H54 H 0.1945 0.1127 0.6170 0.041 Uiso 1 1 calc R . . C55 C 0.2035(3) 0.1973(2) 0.56007(18) 0.0255(8) Uani 1 1 d . . . C56 C 0.1537(3) 0.1511(2) 0.50206(18) 0.0264(8) Uani 1 1 d . . . C57 C 0.0874(4) 0.0553(3) 0.4151(2) 0.0357(10) Uani 1 1 d . . . H57 H 0.0621 0.0110 0.3859 0.043 Uiso 1 1 calc R . . C58 C 0.0915(3) 0.1284(2) 0.40324(18) 0.0264(8) Uani 1 1 d . . . C59 C 0.0633(3) 0.1507(2) 0.34349(19) 0.0281(8) Uani 1 1 d . . . C60 C 0.0081(3) 0.2027(2) 0.3399(2) 0.0308(9) Uani 1 1 d . . . H60 H -0.0141 0.2235 0.3766 0.037 Uiso 1 1 calc R . . C61 C -0.0140(3) 0.2238(3) 0.2821(2) 0.0334(9) Uani 1 1 d . . . H61 H -0.0503 0.2601 0.2795 0.040 Uiso 1 1 calc R . . C62 C 0.0160(3) 0.1927(2) 0.2281(2) 0.0329(9) Uani 1 1 d . . . H62 H 0.0001 0.2079 0.1890 0.040 Uiso 1 1 calc R . . C63 C 0.0697(3) 0.1389(2) 0.23046(18) 0.0291(8) Uani 1 1 d . . . C64 C 0.0939(3) 0.1197(2) 0.28890(19) 0.0303(9) Uani 1 1 d . . . H64 H 0.1320 0.0846 0.2917 0.036 Uiso 1 1 calc R . . C65 C 0.1022(3) 0.1069(2) 0.17147(18) 0.0281(8) Uani 1 1 d . . . C66 C 0.1420(3) 0.1569(2) 0.1271(2) 0.0318(9) Uani 1 1 d . . . H66 H 0.1506 0.2102 0.1361 0.038 Uiso 1 1 calc R . . C67 C 0.1694(3) 0.1306(2) 0.0704(2) 0.0316(9) Uani 1 1 d . . . C68 C 0.1550(3) 0.0524(2) 0.05772(19) 0.0295(8) Uani 1 1 d . . . H68 H 0.1728 0.0339 0.0187 0.035 Uiso 1 1 calc R . . C69 C 0.1153(3) 0.0000(2) 0.10017(18) 0.0281(8) Uani 1 1 d . . . C70 C 0.0896(4) 0.0281(2) 0.15789(19) 0.0329(9) Uani 1 1 d . . . C71 C 0.2152(4) 0.1862(3) 0.0227(2) 0.0440(12) Uani 1 1 d . . . H71A H 0.2893 0.1975 0.0253 0.066 Uiso 1 1 calc R . . H71B H 0.1980 0.2340 0.0315 0.066 Uiso 1 1 calc R . . H71C H 0.1876 0.1626 -0.0193 0.066 Uiso 1 1 calc R . . C72 C 0.0971(3) -0.0832(2) 0.08152(17) 0.0272(8) Uani 1 1 d . . . C73 C 0.0568(3) -0.1141(2) 0.02071(18) 0.0302(9) Uani 1 1 d . . . H73 H 0.0393 -0.0818 -0.0069 0.036 Uiso 1 1 calc R . . C74 C 0.0422(3) -0.1909(2) 0.00039(19) 0.0311(9) Uani 1 1 d . . . H74 H 0.0153 -0.2107 -0.0409 0.037 Uiso 1 1 calc R . . C75 C 0.0668(3) -0.2389(2) 0.04058(18) 0.0278(8) Uani 1 1 d . . . H75 H 0.0570 -0.2914 0.0267 0.033 Uiso 1 1 calc R . . C76 C 0.1059(3) -0.2099(2) 0.10096(18) 0.0254(8) Uani 1 1 d . . . C77 C 0.1222(3) -0.1327(2) 0.12104(18) 0.0282(8) Uani 1 1 d . . . H77 H 0.1507 -0.1132 0.1621 0.034 Uiso 1 1 calc R . . C78 C 0.1322(3) -0.2603(2) 0.14452(17) 0.0255(8) Uani 1 1 d . . . C79 C 0.0967(4) -0.2726(3) 0.20204(19) 0.0341(10) Uani 1 1 d . . . H79 H 0.0476 -0.2516 0.2197 0.041 Uiso 1 1 calc R . . C80 C 0.2186(3) -0.3377(2) 0.17375(16) 0.0241(7) Uani 1 1 d . . . C81 C 0.2951(3) -0.3786(2) 0.16923(16) 0.0223(7) Uani 1 1 d . . . C82 C 0.3200(3) -0.4188(2) 0.21542(18) 0.0283(8) Uani 1 1 d . . . H82 H 0.2851 -0.4241 0.2526 0.034 Uiso 1 1 calc R . . C83 C 0.3972(4) -0.4513(3) 0.2059(2) 0.0356(10) Uani 1 1 d . . . H83 H 0.4156 -0.4798 0.2365 0.043 Uiso 1 1 calc R . . C84 C 0.4479(4) -0.4421(3) 0.1514(2) 0.0348(10) Uani 1 1 d . . . H84 H 0.5012 -0.4640 0.1445 0.042 Uiso 1 1 calc R . . C85 C 0.4197(3) -0.4006(2) 0.10722(18) 0.0274(8) Uani 1 1 d . . . C86 C 0.4727(3) -0.3827(2) 0.04912(19) 0.0290(8) Uani 1 1 d . . . C87 C 0.5510(4) -0.4104(3) 0.0316(2) 0.0407(11) Uani 1 1 d . . . H87 H 0.5728 -0.4433 0.0567 0.049 Uiso 1 1 calc R . . C88 C 0.5980(4) -0.3900(3) -0.0227(2) 0.0447(12) Uani 1 1 d . . . H88 H 0.6517 -0.4092 -0.0352 0.054 Uiso 1 1 calc R . . C89 C 0.5664(4) -0.3424(3) -0.0579(2) 0.0444(12) Uani 1 1 d . . . H89 H 0.5978 -0.3273 -0.0951 0.053 Uiso 1 1 calc R . . C90 C 0.4874(4) -0.3167(3) -0.0382(2) 0.0409(11) Uani 1 1 d . . . H90 H 0.4648 -0.2840 -0.0630 0.049 Uiso 1 1 calc R . . C91 C 0.9123(5) 0.1782(3) 0.6347(3) 0.0600(15) Uani 1 1 d . . . H91A H 0.9707 0.2228 0.6514 0.072 Uiso 1 1 calc R . . H91B H 0.8520 0.1964 0.6309 0.072 Uiso 1 1 calc R . . C92 C 0.7019(5) 0.2377(4) 0.3040(3) 0.0665(18) Uani 1 1 d . . . H92A H 0.7427 0.2038 0.3144 0.080 Uiso 1 1 calc R . . H92B H 0.6701 0.2200 0.2613 0.080 Uiso 1 1 calc R . . C1A C 0.3459(6) 0.5692(4) 0.8127(3) 0.097(3) Uani 1 1 d D . . H1A1 H 0.2906 0.5425 0.7806 0.116 Uiso 1 1 calc R . . H1A2 H 0.3401 0.6212 0.8238 0.116 Uiso 1 1 calc R . . Cl2A Cl 0.32552(17) 0.52003(14) 0.87799(12) 0.0985(7) Uani 1 1 d D . . Cl1A Cl 0.45210(18) 0.57875(15) 0.78200(10) 0.0976(7) Uani 1 1 d D . . C93 C 0.7196(6) 0.9309(5) 0.1477(4) 0.071(2) Uani 0.857(3) 1 d P . . H93A H 0.6859 0.9549 0.1796 0.086 Uiso 0.857(3) 1 calc PR A 1 H93B H 0.7273 0.8834 0.1629 0.086 Uiso 0.857(3) 1 calc PR A 1 Cl10 Cl 0.64360(14) 0.90714(12) 0.07872(9) 0.0658(6) Uani 0.857(3) 1 d P A 1 Cl11 Cl 0.83730(17) 0.99277(16) 0.13865(15) 0.0992(9) Uani 0.857(3) 1 d P A 1 O1S O 0.8764(4) 0.7968(3) 0.2065(3) 0.0596(14) Uani 0.857(3) 1 d PU A 1 N1S N 0.8004(7) 0.7382(7) 0.1637(4) 0.113(3) Uani 0.857(3) 1 d PU A 1 O2S O 0.6994(6) 0.7175(5) 0.1527(5) 0.111(3) Uani 0.857(3) 1 d PU A 1 C1S C 0.8248(8) 0.6876(7) 0.1231(6) 0.128(4) Uani 0.857(3) 1 d PU A 1 H1S1 H 0.8287 0.6433 0.1443 0.191 Uiso 0.857(3) 1 calc PR A 1 H1S2 H 0.8908 0.7124 0.1071 0.191 Uiso 0.857(3) 1 calc PR A 1 H1S3 H 0.7727 0.6703 0.0885 0.191 Uiso 0.857(3) 1 calc PR A 1 Cl2R Cl 0.6749(9) 0.6892(8) 0.1655(6) 0.054(3) Uani 0.143(3) 1 d PD A 2 Cl1R Cl 0.8691(12) 0.7986(9) 0.1686(9) 0.091(6) Uani 0.143(3) 1 d PD A 2 C1R C 0.7419(17) 0.7820(16) 0.1658(10) 0.114(15) Uani 0.143(3) 1 d PDU A 2 H1R1 H 0.7250 0.8115 0.2022 0.136 Uiso 0.143(3) 1 calc PR A 2 H1R2 H 0.7210 0.8014 0.1278 0.136 Uiso 0.143(3) 1 calc PR A 2 O1X O 0.2928(3) 0.0366(2) 0.24250(15) 0.0433(8) Uani 1 1 d . . . H1Z H 0.2284 0.0184 0.2375 0.052 Uiso 1 1 d R . . H2Z H 0.2850 0.0682 0.2177 0.052 Uiso 1 1 d R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cd1 0.03311(16) 0.02204(15) 0.01859(12) 0.00543(10) 0.00005(10) 0.00864(12) Cd2 0.02922(15) 0.02144(14) 0.01904(12) 0.00395(10) 0.00153(10) 0.00975(11) S1 0.0410(6) 0.0411(6) 0.0219(4) 0.0085(4) 0.0091(4) 0.0206(5) S2 0.0459(6) 0.0224(5) 0.0331(5) 0.0085(4) 0.0005(4) 0.0095(5) S3 0.0452(6) 0.0202(5) 0.0375(5) 0.0070(4) 0.0021(5) 0.0086(5) S4 0.0464(6) 0.0462(7) 0.0258(5) 0.0130(4) 0.0121(4) 0.0280(5) Cl1 0.0391(6) 0.0291(5) 0.0321(5) 0.0068(4) -0.0013(4) 0.0026(4) Cl2 0.0350(5) 0.0249(5) 0.0308(4) 0.0053(4) 0.0026(4) 0.0088(4) Cl3 0.0511(7) 0.0335(6) 0.0341(5) 0.0028(4) -0.0001(5) 0.0064(5) Cl4 0.0411(6) 0.0411(7) 0.0400(6) -0.0030(5) -0.0019(5) 0.0160(5) Cl5 0.0644(10) 0.0615(10) 0.0999(13) 0.0222(9) 0.0191(9) 0.0210(9) Cl6 0.0545(8) 0.0517(8) 0.0612(8) 0.0122(6) 0.0165(6) 0.0175(7) Cl7 0.207(3) 0.0528(10) 0.0582(10) 0.0122(8) 0.0341(13) 0.0413(13) Cl8 0.0546(9) 0.0857(12) 0.0592(8) 0.0165(8) 0.0170(7) 0.0212(8) Cl9 0.0736(12) 0.0953(15) 0.1003(14) -0.0378(12) 0.0325(11) -0.0236(11) N1 0.0287(17) 0.0275(18) 0.0234(15) 0.0009(13) 0.0023(12) 0.0096(14) N2 0.0243(16) 0.0183(15) 0.0228(14) 0.0016(12) -0.0001(12) 0.0059(13) N3 0.0246(16) 0.0219(16) 0.0213(14) 0.0023(12) 0.0018(11) 0.0081(13) N4 0.038(2) 0.0240(18) 0.0254(15) 0.0036(13) 0.0053(14) 0.0066(15) N5 0.0307(17) 0.0235(17) 0.0213(14) 0.0055(12) 0.0000(12) 0.0083(14) N6 0.0284(17) 0.0229(17) 0.0231(14) 0.0040(12) 0.0015(12) 0.0087(14) N7 0.038(2) 0.0277(19) 0.0216(15) 0.0052(13) -0.0001(13) 0.0080(15) N8 0.0342(19) 0.0233(17) 0.0263(15) 0.0044(13) 0.0008(13) 0.0057(14) N9 0.0239(16) 0.0249(17) 0.0219(14) 0.0043(12) 0.0032(12) 0.0091(13) N10 0.0218(16) 0.0203(16) 0.0268(15) 0.0041(12) 0.0018(12) 0.0050(13) N11 0.111(4) 0.029(2) 0.0259(18) 0.0077(16) 0.012(2) 0.031(2) N12 0.0255(16) 0.0206(16) 0.0229(14) 0.0019(12) -0.0001(12) 0.0087(13) N13 0.0300(17) 0.0204(16) 0.0216(14) 0.0034(12) 0.0030(12) 0.0090(13) N14 0.0314(19) 0.033(2) 0.0274(16) 0.0086(14) 0.0059(13) 0.0070(15) O1 0.040(2) 0.046(2) 0.079(3) 0.022(2) 0.0175(18) 0.0061(17) O2 0.050(2) 0.078(3) 0.047(2) 0.0016(19) -0.0002(17) 0.034(2) O3 0.084(3) 0.043(2) 0.0297(16) 0.0034(15) -0.0076(17) 0.002(2) O4 0.077(3) 0.0264(18) 0.051(2) 0.0013(15) -0.0091(19) 0.0024(18) O5 0.074(3) 0.047(2) 0.0272(15) 0.0023(14) -0.0037(16) 0.0233(19) O6 0.0425(19) 0.056(2) 0.0382(17) 0.0089(15) 0.0035(14) 0.0275(17) O7 0.049(2) 0.0249(16) 0.0470(18) -0.0011(14) -0.0016(15) 0.0112(15) O8 0.043(2) 0.0330(19) 0.070(2) 0.0149(17) 0.0188(17) 0.0061(16) O9 0.136(5) 0.031(2) 0.073(3) 0.012(2) -0.037(3) -0.017(3) O10 0.073(3) 0.145(5) 0.051(2) 0.015(3) 0.013(2) 0.067(3) O11 0.080(3) 0.044(2) 0.052(2) 0.0208(18) -0.012(2) 0.006(2) O12 0.069(3) 0.042(2) 0.0375(17) 0.0037(15) 0.0146(17) 0.0111(18) O13 0.075(3) 0.077(3) 0.053(2) 0.001(2) 0.013(2) 0.051(2) O14 0.059(3) 0.058(3) 0.057(2) 0.015(2) 0.0199(19) 0.003(2) O15 0.070(3) 0.087(4) 0.094(4) -0.009(3) -0.031(3) 0.044(3) O16 0.071(3) 0.046(2) 0.044(2) 0.0001(17) 0.0082(18) -0.007(2) O17 0.102(4) 0.192(7) 0.093(4) 0.050(4) 0.029(3) 0.096(5) O18 0.123(5) 0.193(8) 0.074(4) 0.030(4) 0.024(4) -0.002(5) O19 0.086(5) 0.093(6) 0.409(16) -0.023(8) -0.002(7) -0.024(4) O20 0.221(8) 0.159(7) 0.139(6) 0.065(5) 0.045(6) 0.153(7) C1 0.039(2) 0.031(2) 0.0287(19) 0.0022(17) 0.0102(17) 0.0093(19) C2 0.043(3) 0.036(3) 0.039(2) -0.0003(19) 0.0159(19) 0.012(2) C3 0.033(2) 0.038(3) 0.049(3) -0.002(2) 0.010(2) 0.016(2) C4 0.032(2) 0.034(2) 0.041(2) 0.0047(19) 0.0021(18) 0.0145(19) C5 0.029(2) 0.0200(19) 0.0265(17) -0.0028(14) 0.0011(14) 0.0082(16) C6 0.028(2) 0.0190(18) 0.0240(17) 0.0008(14) -0.0007(14) 0.0059(15) C7 0.032(2) 0.028(2) 0.034(2) 0.0045(17) -0.0028(16) 0.0143(18) C8 0.036(2) 0.030(2) 0.0306(19) 0.0090(17) -0.0039(16) 0.0120(19) C9 0.032(2) 0.028(2) 0.0243(17) 0.0075(15) -0.0002(15) 0.0073(17) C10 0.0254(19) 0.0197(18) 0.0221(16) 0.0054(14) 0.0018(13) 0.0048(15) C11 0.0272(19) 0.0206(19) 0.0223(16) 0.0018(14) 0.0035(14) 0.0059(15) C12 0.037(2) 0.038(2) 0.0272(18) 0.0055(17) 0.0077(16) 0.020(2) C13 0.0225(18) 0.0233(19) 0.0237(16) 0.0013(14) 0.0021(13) 0.0076(15) C14 0.0219(18) 0.0242(19) 0.0235(16) 0.0036(14) 0.0039(13) 0.0088(15) C15 0.026(2) 0.0219(19) 0.0285(18) -0.0010(15) 0.0015(15) 0.0072(16) C16 0.030(2) 0.031(2) 0.0240(17) -0.0013(15) -0.0021(15) 0.0090(17) C17 0.026(2) 0.026(2) 0.0269(18) 0.0041(15) -0.0013(14) 0.0070(16) C18 0.0236(18) 0.0211(19) 0.0251(17) 0.0021(14) 0.0020(14) 0.0057(15) C19 0.0274(19) 0.024(2) 0.0230(16) 0.0020(14) 0.0013(14) 0.0106(16) C20 0.027(2) 0.025(2) 0.0237(17) 0.0043(15) -0.0026(14) 0.0065(16) C21 0.0274(19) 0.0226(19) 0.0250(17) 0.0075(14) -0.0004(14) 0.0084(16) C22 0.027(2) 0.0216(19) 0.0262(17) 0.0013(14) -0.0036(14) 0.0081(16) C23 0.033(2) 0.024(2) 0.0313(19) 0.0032(16) -0.0032(16) 0.0092(17) C24 0.031(2) 0.030(2) 0.0310(19) 0.0093(17) -0.0008(16) 0.0072(18) C25 0.030(2) 0.031(2) 0.0267(18) 0.0057(16) 0.0010(15) 0.0086(17) C26 0.048(3) 0.031(2) 0.037(2) 0.0128(19) 0.004(2) 0.010(2) C27 0.029(2) 0.0213(19) 0.0270(18) 0.0004(15) -0.0033(15) 0.0063(16) C28 0.043(2) 0.029(2) 0.0260(18) 0.0032(16) -0.0057(17) 0.0144(19) C29 0.042(3) 0.024(2) 0.039(2) 0.0010(17) -0.0026(18) 0.0171(19) C30 0.036(2) 0.024(2) 0.0305(19) -0.0013(16) -0.0009(16) 0.0116(18) C31 0.027(2) 0.0198(19) 0.0266(17) -0.0006(14) -0.0028(14) 0.0047(15) C32 0.030(2) 0.0209(19) 0.0303(18) 0.0017(15) -0.0064(15) 0.0102(16) C33 0.031(2) 0.023(2) 0.0269(18) 0.0015(15) -0.0028(15) 0.0079(16) C34 0.043(3) 0.023(2) 0.032(2) 0.0017(16) 0.0002(18) 0.0070(18) C35 0.028(2) 0.024(2) 0.0265(17) 0.0069(15) 0.0028(14) 0.0072(16) C36 0.027(2) 0.028(2) 0.0243(17) 0.0075(15) 0.0023(14) 0.0084(16) C37 0.039(2) 0.029(2) 0.032(2) 0.0130(17) 0.0028(17) 0.0100(19) C38 0.043(3) 0.042(3) 0.029(2) 0.0176(19) -0.0016(18) 0.014(2) C39 0.035(2) 0.040(3) 0.0234(18) 0.0076(17) -0.0029(16) 0.0105(19) C40 0.029(2) 0.032(2) 0.0198(16) 0.0055(15) 0.0033(14) 0.0118(17) C41 0.030(2) 0.031(2) 0.0229(17) 0.0032(15) 0.0024(14) 0.0130(17) C42 0.039(2) 0.034(2) 0.0266(19) 0.0012(17) -0.0059(17) 0.0091(19) C43 0.041(3) 0.034(3) 0.041(2) -0.003(2) -0.009(2) 0.003(2) C44 0.049(3) 0.028(2) 0.039(2) 0.0026(19) 0.000(2) 0.002(2) C45 0.050(3) 0.031(2) 0.028(2) 0.0059(17) 0.0017(18) 0.004(2) C46 0.054(3) 0.029(2) 0.033(2) 0.0081(18) -0.004(2) 0.005(2) C47 0.071(4) 0.025(2) 0.049(3) 0.010(2) -0.006(3) -0.009(2) C48 0.068(4) 0.033(3) 0.043(3) 0.002(2) -0.014(2) -0.009(3) C49 0.047(3) 0.037(3) 0.031(2) 0.0047(19) -0.0086(19) 0.004(2) C50 0.028(2) 0.026(2) 0.0229(16) 0.0036(15) 0.0023(14) 0.0082(16) C51 0.0270(19) 0.027(2) 0.0220(16) 0.0026(14) 0.0020(14) 0.0117(16) C52 0.041(2) 0.036(2) 0.0266(19) 0.0040(17) -0.0070(17) 0.013(2) C53 0.049(3) 0.038(3) 0.033(2) 0.0147(19) -0.0046(19) 0.013(2) C54 0.038(2) 0.028(2) 0.037(2) 0.0110(18) -0.0021(18) 0.0091(19) C55 0.026(2) 0.023(2) 0.0290(18) 0.0067(15) 0.0045(15) 0.0088(16) C56 0.027(2) 0.024(2) 0.0297(18) 0.0064(15) 0.0058(15) 0.0080(16) C57 0.045(3) 0.023(2) 0.036(2) 0.0016(17) -0.0015(19) 0.0077(19) C58 0.026(2) 0.0215(19) 0.0292(18) -0.0015(15) 0.0005(15) 0.0053(16) C59 0.026(2) 0.024(2) 0.033(2) 0.0013(16) -0.0037(15) 0.0066(16) C60 0.025(2) 0.024(2) 0.041(2) -0.0013(17) -0.0009(16) 0.0054(17) C61 0.030(2) 0.028(2) 0.045(2) 0.0038(18) -0.0030(18) 0.0145(18) C62 0.035(2) 0.027(2) 0.036(2) 0.0024(17) -0.0060(17) 0.0103(18) C63 0.036(2) 0.023(2) 0.0280(18) -0.0003(15) -0.0057(16) 0.0105(17) C64 0.037(2) 0.022(2) 0.032(2) -0.0002(16) -0.0038(16) 0.0112(18) C65 0.034(2) 0.024(2) 0.0288(18) -0.0008(15) -0.0055(15) 0.0147(17) C66 0.031(2) 0.021(2) 0.041(2) 0.0011(17) -0.0087(17) 0.0078(17) C67 0.031(2) 0.025(2) 0.039(2) 0.0034(17) -0.0036(17) 0.0087(17) C68 0.029(2) 0.028(2) 0.0324(19) 0.0056(16) -0.0029(16) 0.0102(17) C69 0.035(2) 0.024(2) 0.0269(18) 0.0007(15) -0.0067(15) 0.0130(17) C70 0.047(3) 0.026(2) 0.0285(19) 0.0081(16) -0.0046(17) 0.0151(19) C71 0.050(3) 0.025(2) 0.057(3) 0.007(2) 0.015(2) 0.010(2) C72 0.038(2) 0.0183(19) 0.0251(17) 0.0005(14) -0.0035(15) 0.0097(17) C73 0.035(2) 0.028(2) 0.0278(18) 0.0015(16) -0.0068(16) 0.0128(18) C74 0.035(2) 0.027(2) 0.0279(19) -0.0006(16) -0.0078(16) 0.0071(18) C75 0.031(2) 0.022(2) 0.0303(19) 0.0017(15) 0.0004(15) 0.0093(17) C76 0.027(2) 0.0218(19) 0.0289(18) 0.0035(15) -0.0009(14) 0.0098(16) C77 0.037(2) 0.024(2) 0.0237(17) -0.0018(15) -0.0054(15) 0.0123(17) C78 0.030(2) 0.023(2) 0.0258(17) 0.0019(15) -0.0006(15) 0.0113(16) C79 0.043(3) 0.038(3) 0.030(2) 0.0073(18) 0.0081(18) 0.024(2) C80 0.030(2) 0.0235(19) 0.0188(15) 0.0036(14) 0.0010(14) 0.0085(16) C81 0.0252(19) 0.0203(18) 0.0211(16) 0.0042(14) 0.0001(13) 0.0058(15) C82 0.035(2) 0.029(2) 0.0241(17) 0.0094(15) 0.0018(15) 0.0116(18) C83 0.042(3) 0.038(3) 0.036(2) 0.0154(19) 0.0030(18) 0.022(2) C84 0.043(3) 0.035(2) 0.037(2) 0.0122(18) 0.0077(18) 0.023(2) C85 0.033(2) 0.023(2) 0.0278(18) 0.0037(15) 0.0049(15) 0.0110(17) C86 0.032(2) 0.025(2) 0.0307(19) 0.0038(16) 0.0069(16) 0.0085(17) C87 0.040(3) 0.046(3) 0.043(2) 0.006(2) 0.013(2) 0.021(2) C88 0.036(3) 0.051(3) 0.045(3) 0.000(2) 0.018(2) 0.011(2) C89 0.035(3) 0.055(3) 0.037(2) 0.007(2) 0.0098(19) 0.003(2) C90 0.039(3) 0.050(3) 0.033(2) 0.015(2) 0.0085(18) 0.008(2) C91 0.074(4) 0.045(3) 0.056(3) -0.001(3) 0.005(3) 0.012(3) C92 0.052(4) 0.069(4) 0.069(4) -0.012(3) 0.007(3) 0.007(3) C1A 0.108(6) 0.071(5) 0.066(4) 0.007(4) -0.004(4) -0.039(5) Cl2A 0.0817(14) 0.1046(17) 0.1203(18) 0.0210(14) 0.0002(12) 0.0430(13) Cl1A 0.0946(15) 0.1268(19) 0.0779(12) 0.0130(12) 0.0208(11) 0.0411(14) C93 0.069(5) 0.061(5) 0.087(6) 0.027(4) 0.007(4) 0.018(4) Cl10 0.0616(11) 0.0788(14) 0.0674(11) 0.0355(10) 0.0241(9) 0.0269(10) Cl11 0.0588(13) 0.0925(18) 0.150(2) 0.0484(17) -0.0045(14) 0.0200(12) O1S 0.042(3) 0.045(3) 0.098(4) 0.030(3) 0.019(3) 0.015(2) N1S 0.092(5) 0.160(9) 0.081(6) 0.009(5) 0.020(4) 0.028(6) O2S 0.051(4) 0.083(6) 0.203(9) 0.030(6) 0.006(5) 0.024(4) C1S 0.079(7) 0.139(11) 0.161(12) -0.015(8) 0.019(7) 0.035(7) Cl2R 0.027(5) 0.056(8) 0.065(6) -0.010(5) 0.010(4) -0.005(5) Cl1R 0.086(10) 0.054(8) 0.107(13) 0.034(9) -0.013(9) -0.020(7) C1R 0.110(17) 0.120(17) 0.117(17) 0.004(10) 0.012(10) 0.045(10) O1X 0.0382(18) 0.050(2) 0.0463(18) 0.0074(16) -0.0046(14) 0.0201(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 Cd1 N6 2.301(3) . ? Cd1 N13 2.309(3) . ? Cd1 N12 2.335(3) . ? Cd1 N7 2.339(3) . ? Cd1 N5 2.342(3) . ? Cd1 N14 2.351(4) . ? Cd2 N9 2.308(3) . ? Cd2 N2 2.313(3) . ? Cd2 N8 2.352(3) . ? Cd2 N3 2.373(3) . ? Cd2 N1 2.378(3) . ? Cd2 N10 2.396(3) . ? S1 C12 1.695(4) . ? S1 C11 1.713(4) . ? S2 C34 1.707(4) . ? S2 C35 1.709(4) . ? S3 C57 1.705(5) . ? S3 C56 1.713(4) . ? S4 C80 1.711(4) . ? S4 C79 1.714(4) . ? Cl1 O1 1.423(4) . ? Cl1 O4 1.426(4) . ? Cl1 O3 1.433(3) . ? Cl1 O2 1.436(4) . ? Cl2 O8 1.430(3) . ? Cl2 O7 1.438(3) . ? Cl2 O5 1.437(3) . ? Cl2 O6 1.441(3) . ? Cl3 O9 1.411(4) . ? Cl3 O10 1.412(4) . ? Cl3 O12 1.421(3) . ? Cl3 O11 1.447(4) . ? Cl4 O13 1.418(4) . ? Cl4 O16 1.419(4) . ? Cl4 O15 1.427(4) . ? Cl4 O14 1.456(4) . ? Cl5 O19 1.350(7) . ? Cl5 O18 1.428(6) . ? Cl5 O20 1.437(6) . ? Cl5 O17 1.458(6) . ? Cl6 C91 1.753(6) . ? Cl7 C91 1.699(6) . ? Cl8 C92 1.758(6) . ? Cl9 C92 1.756(7) . ? N1 C1 1.333(5) . ? N1 C5 1.351(5) . ? N2 C6 1.334(5) . ? N2 C10 1.343(4) . ? N3 C11 1.324(5) . ? N3 C13 1.373(5) . ? N4 C21 1.468(5) . ? N4 H4A 0.9100 . ? N4 H4B 0.9100 . ? N4 H4C 0.9100 . ? N5 C35 1.325(5) . ? N5 C33 1.378(5) . ? N6 C36 1.332(5) . ? N6 C40 1.338(5) . ? N7 C45 1.340(6) . ? N7 C41 1.349(5) . ? N8 C46 1.336(6) . ? N8 C50 1.338(5) . ? N9 C55 1.339(5) . ? N9 C51 1.341(5) . ? N10 C56 1.313(5) . ? N10 C58 1.381(5) . ? N11 C70 1.424(6) . ? N11 H11A 0.8800 . ? N11 H11B 0.8800 . ? N12 C80 1.312(5) . ? N12 C78 1.371(5) . ? N13 C81 1.337(4) . ? N13 C85 1.342(5) . ? N14 C90 1.342(5) . ? N14 C86 1.349(5) . ? C1 C2 1.389(6) . ? C1 H1 0.9500 . ? C2 C3 1.366(7) . ? C2 H2 0.9500 . ? C3 C4 1.385(6) . ? C3 H3 0.9500 . ? C4 C5 1.387(6) . ? C4 H4 0.9500 . ? C5 C6 1.487(5) . ? C6 C7 1.397(5) . ? C7 C8 1.385(6) . ? C7 H7 0.9500 . ? C8 C9 1.393(6) . ? C8 H8 0.9500 . ? C9 C10 1.391(5) . ? C9 H9 0.9500 . ? C10 C11 1.467(5) . ? C12 C13 1.368(5) . ? C12 H12 0.9500 . ? C13 C14 1.479(5) . ? C14 C15 1.388(5) . ? C14 C19 1.403(5) . ? C15 C16 1.376(6) . ? C15 H15 0.9500 . ? C16 C17 1.386(6) . ? C16 H16 0.9500 . ? C17 C18 1.395(5) . ? C17 H17 0.9500 . ? C18 C19 1.398(5) . ? C18 C20 1.484(5) . ? C19 H19 0.9500 . ? C20 C25 1.403(5) . ? C20 C21 1.411(5) . ? C21 C22 1.385(5) . ? C22 C23 1.395(6) . ? C22 C27 1.491(5) . ? C23 C24 1.396(6) . ? C23 H23 0.9500 . ? C24 C25 1.380(6) . ? C24 C26 1.530(6) . ? C25 H25 0.9500 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 C28 1.393(6) . ? C27 C32 1.395(5) . ? C28 C29 1.390(6) . ? C28 H28 0.9500 . ? C29 C30 1.375(6) . ? C29 H29 0.9500 . ? C30 C31 1.390(6) . ? C30 H30 0.9500 . ? C31 C32 1.399(5) . ? C31 C33 1.468(5) . ? C32 H32 0.9500 . ? C33 C34 1.371(6) . ? C34 H34 0.9500 . ? C35 C36 1.475(5) . ? C36 C37 1.388(5) . ? C37 C38 1.383(6) . ? C37 H37 0.9500 . ? C38 C39 1.386(6) . ? C38 H38 0.9500 . ? C39 C40 1.393(5) . ? C39 H39 0.9500 . ? C40 C41 1.487(6) . ? C41 C42 1.385(6) . ? C42 C43 1.391(7) . ? C42 H42 0.9500 . ? C43 C44 1.363(7) . ? C43 H43 0.9500 . ? C44 C45 1.389(6) . ? C44 H44 0.9500 . ? C45 H45 0.9500 . ? C46 C47 1.375(7) . ? C46 H46 0.9500 . ? C47 C48 1.380(7) . ? C47 H47 0.9500 . ? C48 C49 1.376(7) . ? C48 H48 0.9500 . ? C49 C50 1.380(6) . ? C49 H49 0.9500 . ? C50 C51 1.495(6) . ? C51 C52 1.392(5) . ? C52 C53 1.382(6) . ? C52 H52 0.9500 . ? C53 C54 1.380(6) . ? C53 H53 0.9500 . ? C54 C55 1.383(5) . ? C54 H54 0.9500 . ? C55 C56 1.469(6) . ? C57 C58 1.373(6) . ? C57 H57 0.9500 . ? C58 C59 1.461(6) . ? C59 C60 1.395(6) . ? C59 C64 1.399(6) . ? C60 C61 1.389(6) . ? C60 H60 0.9500 . ? C61 C62 1.387(6) . ? C61 H61 0.9500 . ? C62 C63 1.404(6) . ? C62 H62 0.9500 . ? C63 C64 1.395(6) . ? C63 C65 1.496(6) . ? C64 H64 0.9500 . ? C65 C66 1.396(6) . ? C65 C70 1.405(6) . ? C66 C67 1.384(6) . ? C66 H66 0.9500 . ? C67 C68 1.388(6) . ? C67 C71 1.532(6) . ? C68 C69 1.392(6) . ? C68 H68 0.9500 . ? C69 C70 1.407(6) . ? C69 C72 1.486(5) . ? C71 H71A 0.9800 . ? C71 H71B 0.9800 . ? C71 H71C 0.9800 . ? C72 C77 1.405(5) . ? C72 C73 1.407(5) . ? C73 C74 1.391(6) . ? C73 H73 0.9500 . ? C74 C75 1.391(6) . ? C74 H74 0.9500 . ? C75 C76 1.389(5) . ? C75 H75 0.9500 . ? C76 C77 1.391(5) . ? C76 C78 1.484(5) . ? C77 H77 0.9500 . ? C78 C79 1.365(5) . ? C79 H79 0.9500 . ? C80 C81 1.469(5) . ? C81 C82 1.383(5) . ? C82 C83 1.383(6) . ? C82 H82 0.9500 . ? C83 C84 1.389(6) . ? C83 H83 0.9500 . ? C84 C85 1.385(6) . ? C84 H84 0.9500 . ? C85 C86 1.489(5) . ? C86 C87 1.379(6) . ? C87 C88 1.389(6) . ? C87 H87 0.9500 . ? C88 C89 1.361(7) . ? C88 H88 0.9500 . ? C89 C90 1.380(7) . ? C89 H89 0.9500 . ? C90 H90 0.9500 . ? C91 H91A 0.9900 . ? C91 H91B 0.9900 . ? C92 H92A 0.9900 . ? C92 H92B 0.9900 . ? C1A Cl1A 1.601(9) . ? C1A Cl2A 1.727(7) . ? C1A H1A1 0.9900 . ? C1A H1A2 0.9900 . ? C93 Cl11 1.710(8) . ? C93 Cl10 1.735(9) . ? C93 H93A 0.9900 . ? C93 H93B 0.9900 . ? O1S N1S 1.479(11) . ? N1S O2S 1.338(12) . ? N1S C1S 1.346(13) . ? C1S H1S1 0.9800 . ? C1S H1S2 0.9800 . ? C1S H1S3 0.9800 . ? Cl2R C1R 1.68(2) . ? Cl1R C1R 1.69(2) . ? C1R H1R1 0.9900 . ? C1R H1R2 0.9900 . ? O1X H1Z 0.8500 . ? O1X H2Z 0.8500 . ? 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 N6 Cd1 N13 169.09(11) . . ? N6 Cd1 N12 117.50(11) . . ? N13 Cd1 N12 70.95(11) . . ? N6 Cd1 N7 69.58(12) . . ? N13 Cd1 N7 102.84(12) . . ? N12 Cd1 N7 100.84(11) . . ? N6 Cd1 N5 71.45(11) . . ? N13 Cd1 N5 117.04(11) . . ? N12 Cd1 N5 88.73(11) . . ? N7 Cd1 N5 139.89(11) . . ? N6 Cd1 N14 102.47(11) . . ? N13 Cd1 N14 69.68(11) . . ? N12 Cd1 N14 139.98(11) . . ? N7 Cd1 N14 94.55(12) . . ? N5 Cd1 N14 102.78(12) . . ? N9 Cd2 N2 173.25(11) . . ? N9 Cd2 N8 69.25(11) . . ? N2 Cd2 N8 107.30(11) . . ? N9 Cd2 N3 115.10(11) . . ? N2 Cd2 N3 71.17(11) . . ? N8 Cd2 N3 105.05(11) . . ? N9 Cd2 N1 105.06(11) . . ? N2 Cd2 N1 69.00(11) . . ? N8 Cd2 N1 93.69(12) . . ? N3 Cd2 N1 139.46(11) . . ? N9 Cd2 N10 70.54(11) . . ? N2 Cd2 N10 113.56(11) . . ? N8 Cd2 N10 138.89(11) . . ? N3 Cd2 N10 84.47(11) . . ? N1 Cd2 N10 104.62(11) . . ? C12 S1 C11 89.68(19) . . ? C34 S2 C35 90.0(2) . . ? C57 S3 C56 89.4(2) . . ? C80 S4 C79 89.42(19) . . ? O1 Cl1 O4 109.6(2) . . ? O1 Cl1 O3 110.2(3) . . ? O4 Cl1 O3 110.4(2) . . ? O1 Cl1 O2 109.0(2) . . ? O4 Cl1 O2 109.8(2) . . ? O3 Cl1 O2 107.9(2) . . ? O8 Cl2 O7 109.5(2) . . ? O8 Cl2 O5 109.8(2) . . ? O7 Cl2 O5 109.5(2) . . ? O8 Cl2 O6 109.2(2) . . ? O7 Cl2 O6 109.7(2) . . ? O5 Cl2 O6 109.1(2) . . ? O9 Cl3 O10 113.7(4) . . ? O9 Cl3 O12 108.8(3) . . ? O10 Cl3 O12 109.1(3) . . ? O9 Cl3 O11 107.5(3) . . ? O10 Cl3 O11 107.2(3) . . ? O12 Cl3 O11 110.5(2) . . ? O13 Cl4 O16 108.7(3) . . ? O13 Cl4 O15 110.4(3) . . ? O16 Cl4 O15 110.8(3) . . ? O13 Cl4 O14 108.0(3) . . ? O16 Cl4 O14 109.9(2) . . ? O15 Cl4 O14 109.0(3) . . ? O19 Cl5 O18 110.3(6) . . ? O19 Cl5 O20 109.0(6) . . ? O18 Cl5 O20 110.8(5) . . ? O19 Cl5 O17 111.6(6) . . ? O18 Cl5 O17 106.5(4) . . ? O20 Cl5 O17 108.6(4) . . ? C1 N1 C5 118.6(4) . . ? C1 N1 Cd2 123.4(3) . . ? C5 N1 Cd2 118.0(2) . . ? C6 N2 C10 120.1(3) . . ? C6 N2 Cd2 121.2(2) . . ? C10 N2 Cd2 118.8(2) . . ? C11 N3 C13 111.3(3) . . ? C11 N3 Cd2 113.3(2) . . ? C13 N3 Cd2 134.0(2) . . ? C21 N4 H4A 109.5 . . ? C21 N4 H4B 109.5 . . ? H4A N4 H4B 109.5 . . ? C21 N4 H4C 109.5 . . ? H4A N4 H4C 109.5 . . ? H4B N4 H4C 109.5 . . ? C35 N5 C33 111.2(3) . . ? C35 N5 Cd1 113.9(3) . . ? C33 N5 Cd1 133.5(2) . . ? C36 N6 C40 120.9(3) . . ? C36 N6 Cd1 118.8(2) . . ? C40 N6 Cd1 120.3(3) . . ? C45 N7 C41 118.8(4) . . ? C45 N7 Cd1 122.8(3) . . ? C41 N7 Cd1 118.3(3) . . ? C46 N8 C50 118.8(4) . . ? C46 N8 Cd2 122.4(3) . . ? C50 N8 Cd2 118.5(3) . . ? C55 N9 C51 119.8(3) . . ? C55 N9 Cd2 119.8(3) . . ? C51 N9 Cd2 120.4(3) . . ? C56 N10 C58 111.5(3) . . ? C56 N10 Cd2 113.0(3) . . ? C58 N10 Cd2 133.3(2) . . ? C70 N11 H11A 120.0 . . ? C70 N11 H11B 120.0 . . ? H11A N11 H11B 120.0 . . ? C80 N12 C78 112.2(3) . . ? C80 N12 Cd1 114.7(2) . . ? C78 N12 Cd1 132.7(2) . . ? C81 N13 C85 120.6(3) . . ? C81 N13 Cd1 119.1(3) . . ? C85 N13 Cd1 120.2(2) . . ? C90 N14 C86 118.4(4) . . ? C90 N14 Cd1 123.2(3) . . ? C86 N14 Cd1 118.1(3) . . ? N1 C1 C2 123.0(4) . . ? N1 C1 H1 118.5 . . ? C2 C1 H1 118.5 . . ? C3 C2 C1 118.1(4) . . ? C3 C2 H2 120.9 . . ? C1 C2 H2 120.9 . . ? C2 C3 C4 120.0(4) . . ? C2 C3 H3 120.0 . . ? C4 C3 H3 120.0 . . ? C3 C4 C5 118.7(4) . . ? C3 C4 H4 120.6 . . ? C5 C4 H4 120.6 . . ? N1 C5 C4 121.5(4) . . ? N1 C5 C6 116.1(3) . . ? C4 C5 C6 122.4(4) . . ? N2 C6 C7 121.1(4) . . ? N2 C6 C5 115.5(3) . . ? C7 C6 C5 123.4(4) . . ? C8 C7 C6 119.0(4) . . ? C8 C7 H7 120.5 . . ? C6 C7 H7 120.5 . . ? C7 C8 C9 119.7(4) . . ? C7 C8 H8 120.2 . . ? C9 C8 H8 120.2 . . ? C10 C9 C8 117.9(4) . . ? C10 C9 H9 121.0 . . ? C8 C9 H9 121.0 . . ? N2 C10 C9 122.1(4) . . ? N2 C10 C11 114.3(3) . . ? C9 C10 C11 123.5(3) . . ? N3 C11 C10 122.0(3) . . ? N3 C11 S1 114.0(3) . . ? C10 C11 S1 123.5(3) . . ? C13 C12 S1 111.3(3) . . ? C13 C12 H12 124.3 . . ? S1 C12 H12 124.3 . . ? C12 C13 N3 113.7(3) . . ? C12 C13 C14 125.1(3) . . ? N3 C13 C14 121.2(3) . . ? C15 C14 C19 118.9(3) . . ? C15 C14 C13 122.5(4) . . ? C19 C14 C13 118.6(3) . . ? C16 C15 C14 120.5(4) . . ? C16 C15 H15 119.8 . . ? C14 C15 H15 119.8 . . ? C15 C16 C17 120.5(4) . . ? C15 C16 H16 119.7 . . ? C17 C16 H16 119.7 . . ? C16 C17 C18 120.7(4) . . ? C16 C17 H17 119.7 . . ? C18 C17 H17 119.7 . . ? C17 C18 C19 118.3(4) . . ? C17 C18 C20 120.0(3) . . ? C19 C18 C20 121.6(3) . . ? C18 C19 C14 121.1(3) . . ? C18 C19 H19 119.5 . . ? C14 C19 H19 119.5 . . ? C25 C20 C21 117.1(4) . . ? C25 C20 C18 119.3(3) . . ? C21 C20 C18 123.6(3) . . ? C22 C21 C20 122.2(3) . . ? C22 C21 N4 119.4(3) . . ? C20 C21 N4 118.3(3) . . ? C21 C22 C23 118.2(4) . . ? C21 C22 C27 123.5(3) . . ? C23 C22 C27 118.2(4) . . ? C22 C23 C24 121.5(4) . . ? C22 C23 H23 119.2 . . ? C24 C23 H23 119.2 . . ? C25 C24 C23 118.8(4) . . ? C25 C24 C26 121.2(4) . . ? C23 C24 C26 120.0(4) . . ? C24 C25 C20 122.0(4) . . ? C24 C25 H25 119.0 . . ? C20 C25 H25 119.0 . . ? C24 C26 H26A 109.5 . . ? C24 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C24 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C28 C27 C32 118.5(4) . . ? C28 C27 C22 120.0(3) . . ? C32 C27 C22 121.5(4) . . ? C29 C28 C27 120.5(4) . . ? C29 C28 H28 119.8 . . ? C27 C28 H28 119.8 . . ? C30 C29 C28 120.5(4) . . ? C30 C29 H29 119.7 . . ? C28 C29 H29 119.7 . . ? C29 C30 C31 120.3(4) . . ? C29 C30 H30 119.9 . . ? C31 C30 H30 119.9 . . ? C30 C31 C32 119.1(4) . . ? C30 C31 C33 121.8(4) . . ? C32 C31 C33 119.1(4) . . ? C27 C32 C31 121.1(4) . . ? C27 C32 H32 119.4 . . ? C31 C32 H32 119.4 . . ? C34 C33 N5 114.0(3) . . ? C34 C33 C31 124.7(4) . . ? N5 C33 C31 121.3(3) . . ? C33 C34 S2 110.6(3) . . ? C33 C34 H34 124.7 . . ? S2 C34 H34 124.7 . . ? N5 C35 C36 121.2(4) . . ? N5 C35 S2 114.1(3) . . ? C36 C35 S2 124.3(3) . . ? N6 C36 C37 122.3(4) . . ? N6 C36 C35 114.1(3) . . ? C37 C36 C35 123.5(4) . . ? C38 C37 C36 117.3(4) . . ? C38 C37 H37 121.3 . . ? C36 C37 H37 121.3 . . ? C37 C38 C39 120.4(4) . . ? C37 C38 H38 119.8 . . ? C39 C38 H38 119.8 . . ? C38 C39 C40 118.8(4) . . ? C38 C39 H39 120.6 . . ? C40 C39 H39 120.6 . . ? N6 C40 C39 120.2(4) . . ? N6 C40 C41 115.4(3) . . ? C39 C40 C41 124.3(4) . . ? N7 C41 C42 121.5(4) . . ? N7 C41 C40 115.8(3) . . ? C42 C41 C40 122.7(4) . . ? C41 C42 C43 119.2(4) . . ? C41 C42 H42 120.4 . . ? C43 C42 H42 120.4 . . ? C44 C43 C42 119.1(4) . . ? C44 C43 H43 120.4 . . ? C42 C43 H43 120.4 . . ? C43 C44 C45 119.2(4) . . ? C43 C44 H44 120.4 . . ? C45 C44 H44 120.4 . . ? N7 C45 C44 122.2(4) . . ? N7 C45 H45 118.9 . . ? C44 C45 H45 118.9 . . ? N8 C46 C47 122.2(4) . . ? N8 C46 H46 118.9 . . ? C47 C46 H46 118.9 . . ? C46 C47 C48 119.1(5) . . ? C46 C47 H47 120.5 . . ? C48 C47 H47 120.5 . . ? C49 C48 C47 118.8(5) . . ? C49 C48 H48 120.6 . . ? C47 C48 H48 120.6 . . ? C48 C49 C50 119.2(4) . . ? C48 C49 H49 120.4 . . ? C50 C49 H49 120.4 . . ? N8 C50 C49 121.9(4) . . ? N8 C50 C51 116.0(3) . . ? C49 C50 C51 122.1(4) . . ? N9 C51 C52 120.7(4) . . ? N9 C51 C50 115.0(3) . . ? C52 C51 C50 124.2(4) . . ? C53 C52 C51 119.2(4) . . ? C53 C52 H52 120.4 . . ? C51 C52 H52 120.4 . . ? C54 C53 C52 119.8(4) . . ? C54 C53 H53 120.1 . . ? C52 C53 H53 120.1 . . ? C53 C54 C55 118.2(4) . . ? C53 C54 H54 120.9 . . ? C55 C54 H54 120.9 . . ? N9 C55 C54 122.3(4) . . ? N9 C55 C56 113.6(3) . . ? C54 C55 C56 124.0(4) . . ? N10 C56 C55 122.2(4) . . ? N10 C56 S3 114.6(3) . . ? C55 C56 S3 123.0(3) . . ? C58 C57 S3 111.3(3) . . ? C58 C57 H57 124.4 . . ? S3 C57 H57 124.4 . . ? C57 C58 N10 113.2(4) . . ? C57 C58 C59 125.6(4) . . ? N10 C58 C59 121.2(3) . . ? C60 C59 C64 119.6(4) . . ? C60 C59 C58 121.5(4) . . ? C64 C59 C58 118.9(4) . . ? C61 C60 C59 119.2(4) . . ? C61 C60 H60 120.4 . . ? C59 C60 H60 120.4 . . ? C62 C61 C60 121.0(4) . . ? C62 C61 H61 119.5 . . ? C60 C61 H61 119.5 . . ? C61 C62 C63 120.7(4) . . ? C61 C62 H62 119.6 . . ? C63 C62 H62 119.6 . . ? C64 C63 C62 117.8(4) . . ? C64 C63 C65 122.6(4) . . ? C62 C63 C65 119.6(4) . . ? C63 C64 C59 121.6(4) . . ? C63 C64 H64 119.2 . . ? C59 C64 H64 119.2 . . ? C66 C65 C70 118.9(4) . . ? C66 C65 C63 118.6(4) . . ? C70 C65 C63 122.4(4) . . ? C67 C66 C65 121.6(4) . . ? C67 C66 H66 119.2 . . ? C65 C66 H66 119.2 . . ? C66 C67 C68 118.5(4) . . ? C66 C67 C71 121.1(4) . . ? C68 C67 C71 120.4(4) . . ? C67 C68 C69 122.3(4) . . ? C67 C68 H68 118.8 . . ? C69 C68 H68 118.8 . . ? C68 C69 C70 118.3(4) . . ? C68 C69 C72 118.8(4) . . ? C70 C69 C72 122.8(4) . . ? C65 C70 C69 120.4(4) . . ? C65 C70 N11 119.4(4) . . ? C69 C70 N11 120.1(4) . . ? C67 C71 H71A 109.5 . . ? C67 C71 H71B 109.5 . . ? H71A C71 H71B 109.5 . . ? C67 C71 H71C 109.5 . . ? H71A C71 H71C 109.5 . . ? H71B C71 H71C 109.5 . . ? C77 C72 C73 117.7(4) . . ? C77 C72 C69 123.1(3) . . ? C73 C72 C69 119.1(3) . . ? C74 C73 C72 121.2(4) . . ? C74 C73 H73 119.4 . . ? C72 C73 H73 119.4 . . ? C73 C74 C75 119.9(4) . . ? C73 C74 H74 120.0 . . ? C75 C74 H74 120.0 . . ? C76 C75 C74 119.9(4) . . ? C76 C75 H75 120.1 . . ? C74 C75 H75 120.1 . . ? C75 C76 C77 120.2(4) . . ? C75 C76 C78 120.6(4) . . ? C77 C76 C78 119.2(3) . . ? C76 C77 C72 121.0(4) . . ? C76 C77 H77 119.5 . . ? C72 C77 H77 119.5 . . ? C79 C78 N12 113.4(3) . . ? C79 C78 C76 126.5(4) . . ? N12 C78 C76 120.1(3) . . ? C78 C79 S4 110.9(3) . . ? C78 C79 H79 124.6 . . ? S4 C79 H79 124.6 . . ? N12 C80 C81 121.7(3) . . ? N12 C80 S4 114.0(3) . . ? C81 C80 S4 124.2(3) . . ? N13 C81 C82 121.9(4) . . ? N13 C81 C80 113.5(3) . . ? C82 C81 C80 124.5(3) . . ? C81 C82 C83 118.1(4) . . ? C81 C82 H82 121.0 . . ? C83 C82 H82 121.0 . . ? C82 C83 C84 119.8(4) . . ? C82 C83 H83 120.1 . . ? C84 C83 H83 120.1 . . ? C85 C84 C83 119.2(4) . . ? C85 C84 H84 120.4 . . ? C83 C84 H84 120.4 . . ? N13 C85 C84 120.4(4) . . ? N13 C85 C86 115.6(3) . . ? C84 C85 C86 123.9(4) . . ? N14 C86 C87 120.8(4) . . ? N14 C86 C85 116.0(4) . . ? C87 C86 C85 123.1(4) . . ? C86 C87 C88 119.8(5) . . ? C86 C87 H87 120.1 . . ? C88 C87 H87 120.1 . . ? C89 C88 C87 119.4(5) . . ? C89 C88 H88 120.3 . . ? C87 C88 H88 120.3 . . ? C88 C89 C90 118.2(4) . . ? C88 C89 H89 120.9 . . ? C90 C89 H89 120.9 . . ? N14 C90 C89 123.3(5) . . ? N14 C90 H90 118.3 . . ? C89 C90 H90 118.3 . . ? Cl7 C91 Cl6 113.9(3) . . ? Cl7 C91 H91A 108.8 . . ? Cl6 C91 H91A 108.8 . . ? Cl7 C91 H91B 108.8 . . ? Cl6 C91 H91B 108.8 . . ? H91A C91 H91B 107.7 . . ? Cl9 C92 Cl8 112.4(4) . . ? Cl9 C92 H92A 109.1 . . ? Cl8 C92 H92A 109.1 . . ? Cl9 C92 H92B 109.1 . . ? Cl8 C92 H92B 109.1 . . ? H92A C92 H92B 107.9 . . ? Cl1A C1A Cl2A 117.0(6) . . ? Cl1A C1A H1A1 108.1 . . ? Cl2A C1A H1A1 108.1 . . ? Cl1A C1A H1A2 108.1 . . ? Cl2A C1A H1A2 108.1 . . ? H1A1 C1A H1A2 107.3 . . ? Cl11 C93 Cl10 112.1(5) . . ? Cl11 C93 H93A 109.2 . . ? Cl10 C93 H93A 109.2 . . ? Cl11 C93 H93B 109.2 . . ? Cl10 C93 H93B 109.2 . . ? H93A C93 H93B 107.9 . . ? O2S N1S C1S 101.3(10) . . ? O2S N1S O1S 135.6(9) . . ? C1S N1S O1S 123.1(9) . . ? Cl2R C1R Cl1R 114(2) . . ? Cl2R C1R H1R1 108.7 . . ? Cl1R C1R H1R1 108.7 . . ? Cl2R C1R H1R2 108.7 . . ? Cl1R C1R H1R2 108.7 . . ? H1R1 C1R H1R2 107.6 . . ? H1Z O1X H2Z 84.0 . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 30.51 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.888 _refine_diff_density_min -1.980 _refine_diff_density_rms 0.123 _database_code_depnum_ccdc_archive 'CCDC 958174' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_added_by_encifer _audit_update_record ; 2013-10-06 # Formatted by publCIF ; _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C98 H92 Cd2 Cl10 N13 O30 S4' _chemical_formula_weight 2639.39 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' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 13.3018(3) _cell_length_b 20.7598(4) _cell_length_c 44.2313(9) _cell_angle_alpha 90.00 _cell_angle_beta 91.2640(10) _cell_angle_gamma 90.00 _cell_volume 12211.2(4) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 9928 _cell_measurement_theta_min 2.40 _cell_measurement_theta_max 22.99 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.436 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5364 _exptl_absorpt_coefficient_mu 0.710 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7178 _exptl_absorpt_correction_T_max 0.9520 _exptl_absorpt_process_details sadabs _exptl_special_details ? _diffrn_ambient_temperature 150(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 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 104867 _diffrn_reflns_av_R_equivalents 0.0686 _diffrn_reflns_av_sigmaI/netI 0.0556 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -52 _diffrn_reflns_limit_l_max 52 _diffrn_reflns_theta_min 1.35 _diffrn_reflns_theta_max 25.00 _reflns_number_total 21329 _reflns_number_gt 13700 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^)+(0.2000P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 21329 _refine_ls_number_parameters 1304 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.1708 _refine_ls_R_factor_gt 0.1218 _refine_ls_wR_factor_ref 0.4018 _refine_ls_wR_factor_gt 0.3489 _refine_ls_goodness_of_fit_ref 1.516 _refine_ls_restrained_S_all 1.517 _refine_ls_shift/su_max 0.003 _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 Cd1 Cd 0.66994(5) 0.39956(4) 0.642985(17) 0.0411(3) Uani 1 1 d . . . Cl1 Cl 0.8225(2) 0.42675(18) 0.44810(8) 0.0696(9) Uani 1 1 d . . . S1 S 0.6598(2) 0.5380(2) 0.38631(9) 0.0761(11) Uani 1 1 d . . . O1 O 0.4566(5) -0.1403(4) 0.47818(19) 0.058(2) Uani 1 1 d . . . N1 N 0.2863(8) 0.7022(5) 0.3374(2) 0.055(2) Uani 1 1 d . . . C1 C 0.1905(10) 0.7190(7) 0.3337(3) 0.069(4) Uani 1 1 d . . . H1 H 0.1401 0.6933 0.3427 0.083 Uiso 1 1 calc R . . Cd2 Cd 0.86586(5) -0.11301(4) 0.607127(17) 0.0424(3) Uani 1 1 d . . . Cl2 Cl 0.5831(2) 0.93578(19) 0.30855(8) 0.0681(9) Uani 1 1 d . . . S2 S 0.8331(2) 0.43776(16) 0.55086(7) 0.0554(8) Uani 1 1 d . . . N2 N 0.4731(7) 0.6568(5) 0.3442(2) 0.051(2) Uani 1 1 d . . . C2 C 0.1622(16) 0.7722(8) 0.3175(4) 0.095(6) Uani 1 1 d . . . H2 H 0.0930 0.7820 0.3142 0.114 Uiso 1 1 calc R . . Cl3 Cl 0.7650(3) 0.0816(2) 0.44102(11) 0.0922(12) Uiso 1 1 d . . . S3 S 0.1047(2) 0.05282(16) 0.49517(6) 0.0536(7) Uani 1 1 d . . . O3 O 0.4928(11) -0.2937(7) 0.5776(3) 0.130(5) Uiso 1 1 d . . . N3 N 0.4739(6) 0.5428(5) 0.3720(2) 0.050(2) Uani 1 1 d . . . C3 C 0.2341(17) 0.8105(9) 0.3063(4) 0.099(6) Uani 1 1 d . . . H3 H 0.2153 0.8490 0.2961 0.118 Uiso 1 1 calc R . . Cl4 Cl 0.8784(3) 0.4130(2) 0.27217(11) 0.0950(13) Uani 1 1 d . . . S4 S 0.5181(2) -0.06706(18) 0.61666(7) 0.0614(8) Uani 1 1 d . . . O4 O 0.9254(8) 0.4333(7) 0.4459(4) 0.124(5) Uani 1 1 d . . . N4 N 0.4472(6) 0.3550(5) 0.47914(18) 0.045(2) Uani 1 1 d . . . H4A H 0.4756 0.3245 0.4914 0.068 Uiso 1 1 calc R . . H4B H 0.4867 0.3907 0.4792 0.068 Uiso 1 1 calc R . . H4C H 0.4411 0.3394 0.4600 0.068 Uiso 1 1 calc R . . C4 C 0.3386(16) 0.7942(7) 0.3095(3) 0.096(6) Uani 1 1 d . . . H4 H 0.3904 0.8200 0.3014 0.116 Uiso 1 1 calc R . . Cl5 Cl 0.0053(3) 0.39207(19) 0.14804(9) 0.0772(10) Uani 1 1 d . . . O5 O 0.8178(11) 0.3846(7) 0.4749(3) 0.134(6) Uani 1 1 d . . . N5 N 0.7146(8) 0.4490(5) 0.6894(2) 0.057(3) Uani 1 1 d . . . C5 C 0.3590(12) 0.7355(6) 0.3260(3) 0.066(4) Uani 1 1 d . . . Cl6 Cl 0.0582(4) 0.3708(3) 0.21049(11) 0.1098(16) Uani 1 1 d . . . O6 O 0.7590(8) 0.4771(6) 0.4564(4) 0.142(6) Uani 1 1 d . . . N6 N 0.8230(6) 0.4511(4) 0.6397(2) 0.047(2) Uani 1 1 d . . . C6 C 0.4634(10) 0.7140(7) 0.3311(3) 0.066(3) Uani 1 1 d . . . Cl7 Cl 0.5296(10) 0.4293(6) 0.3159(2) 0.136(4) Uani 0.50 1 d PD . . O7 O 0.7833(10) 0.3862(6) 0.4248(3) 0.118(5) Uani 1 1 d . . . N7 N 0.7217(6) 0.3961(4) 0.59241(18) 0.0373(19) Uani 1 1 d . . . C7 C 0.5511(14) 0.7506(8) 0.3240(4) 0.093(5) Uani 1 1 d . . . H7 H 0.5457 0.7913 0.3143 0.112 Uiso 1 1 calc R . . Cl8 Cl 0.6167(7) 0.5271(7) 0.2832(3) 0.135(4) Uani 0.50 1 d PD . . O8 O 0.5281(8) 0.9108(6) 0.3329(2) 0.094(3) Uani 1 1 d . . . N8 N 0.0903(7) 0.2168(4) 0.3724(2) 0.049(2) Uani 1 1 d . . . C8 C 0.6394(13) 0.7258(10) 0.3314(6) 0.130(8) Uani 1 1 d . . . H8 H 0.6984 0.7485 0.3261 0.156 Uiso 1 1 calc R . . Cl9 Cl 0.8423(8) 0.2356(6) 0.5554(3) 0.228(4) Uiso 1 1 d . . . O9 O 0.5166(9) 0.9296(10) 0.2835(3) 0.146(6) Uani 1 1 d . . . N9 N 0.0418(6) 0.1701(4) 0.4271(2) 0.046(2) Uani 1 1 d . . . C9 C 0.6495(12) 0.6669(9) 0.3468(5) 0.103(6) Uani 1 1 d . . . H9 H 0.7133 0.6516 0.3537 0.123 Uiso 1 1 calc R . . Cl10 Cl 0.9939(4) 0.1286(3) 0.55996(15) 0.1293(18) Uiso 1 1 d . . . O10 O 0.6011(9) 0.9997(7) 0.3140(3) 0.121(4) Uani 1 1 d . . . N10 N 0.1291(6) 0.0555(4) 0.43790(19) 0.042(2) Uani 1 1 d . . . C10 C 0.5631(8) 0.6325(6) 0.3516(3) 0.057(3) Uani 1 1 d . . . Cl11 Cl 0.0855(5) 0.3166(4) 0.62348(18) 0.152(2) Uiso 1 1 d D . . O11 O 0.6712(9) 0.9030(7) 0.3043(3) 0.121(5) Uani 1 1 d . . . N11 N 0.9942(7) -0.0714(5) 0.6393(2) 0.052(2) Uani 1 1 d . . . C11 C 0.5585(7) 0.5740(6) 0.3676(3) 0.055(3) Uani 1 1 d . . . O12 O 0.7012(15) 0.0504(10) 0.4251(5) 0.187(7) Uiso 1 1 d . . . N12 N 0.7980(6) -0.0682(4) 0.64995(19) 0.044(2) Uani 1 1 d . . . C12 C 0.5810(8) 0.4807(7) 0.4002(3) 0.062(3) Uani 1 1 d . . . H12 H 0.6021 0.4466 0.4132 0.075 Uiso 1 1 calc R . . O13 O 0.7879(10) 0.1448(7) 0.4270(3) 0.124(4) Uiso 1 1 d . . . N13 N 0.6876(6) -0.1123(4) 0.60238(19) 0.042(2) Uani 1 1 d . . . C13 C 0.4844(8) 0.4898(6) 0.3904(2) 0.048(3) Uani 1 1 d . . . O14 O 0.8491(9) 0.0407(6) 0.4448(3) 0.111(4) Uiso 1 1 d . . . C14 C 0.3966(8) 0.4520(5) 0.3979(3) 0.048(3) Uani 1 1 d . . . O15 O 0.728(2) 0.1048(13) 0.4686(7) 0.245(11) Uiso 1 1 d . . . C15 C 0.3269(8) 0.4311(5) 0.3766(3) 0.051(3) Uani 1 1 d . . . H15 H 0.3352 0.4416 0.3559 0.061 Uiso 1 1 calc R . . O16 O 0.8010(10) 0.4028(7) 0.2532(3) 0.114(4) Uani 1 1 d . . . C16 C 0.2445(9) 0.3947(6) 0.3852(3) 0.058(3) Uani 1 1 d . . . H16 H 0.1997 0.3782 0.3700 0.069 Uiso 1 1 calc R . . O17 O 0.9296(11) 0.4713(7) 0.2606(3) 0.136(5) Uani 1 1 d . . . C17 C 0.2267(8) 0.3825(5) 0.4147(3) 0.049(3) Uani 1 1 d . . . H17 H 0.1673 0.3600 0.4199 0.058 Uiso 1 1 calc R . . O18 O 0.8386(9) 0.4246(7) 0.3036(2) 0.113(4) Uani 1 1 d . . . C18 C 0.2956(7) 0.4027(5) 0.4381(2) 0.044(3) Uani 1 1 d . . . O19 O 0.9484(10) 0.3752(9) 0.2702(5) 0.175(9) Uani 1 1 d . . . C19 C 0.3791(7) 0.4377(5) 0.4283(2) 0.040(2) Uani 1 1 d . . . H19 H 0.4264 0.4525 0.4431 0.048 Uiso 1 1 calc R . . O20 O -0.0159(12) 0.3201(8) 0.6126(4) 0.145(5) Uiso 1 1 d D . . C20 C 0.6578(11) 0.4518(8) 0.7123(3) 0.077(4) Uani 1 1 d . . . H20 H 0.5959 0.4290 0.7111 0.093 Uiso 1 1 calc R . . C21 C 0.6794(14) 0.4852(9) 0.7388(4) 0.094(5) Uani 1 1 d . . . H21 H 0.6316 0.4870 0.7544 0.112 Uiso 1 1 calc R . . C22 C 0.7686(15) 0.5154(9) 0.7422(4) 0.097(5) Uani 1 1 d . . . H22 H 0.7865 0.5373 0.7603 0.117 Uiso 1 1 calc R . . O23 O 0.1430(15) 0.3736(11) 0.6118(5) 0.191(8) Uiso 1 1 d D . . C23 C 0.8326(12) 0.5130(8) 0.7183(3) 0.083(4) Uani 1 1 d . . . H23 H 0.8955 0.5346 0.7196 0.099 Uiso 1 1 calc R . . O24 O 0.5644(7) 0.4634(5) 0.4833(2) 0.084(3) Uani 1 1 d . . . C24 C 0.8052(10) 0.4779(7) 0.6909(3) 0.067(4) Uani 1 1 d . . . O25 O 0.8306(14) 0.3406(10) 0.7453(4) 0.177(7) Uiso 1 1 d . . . C25 C 0.8674(8) 0.4772(6) 0.6639(2) 0.050(3) Uani 1 1 d . . . O26 O 0.5178(18) -0.1829(12) 0.6864(6) 0.108(7) Uiso 0.50 1 d P . . C26 C 0.9623(10) 0.5040(7) 0.6621(4) 0.071(4) Uani 1 1 d . . . H26 H 0.9943 0.5218 0.6797 0.085 Uiso 1 1 calc R . . O27 O 0.3038(11) 0.3368(8) 0.3027(4) 0.142(5) Uiso 1 1 d . . . C27 C 1.0089(9) 0.5048(7) 0.6356(4) 0.077(4) Uani 1 1 d . . . H27 H 1.0743 0.5228 0.6345 0.093 Uiso 1 1 calc R . . C28 C 0.9635(9) 0.4798(6) 0.6098(4) 0.069(4) Uani 1 1 d . . . H28 H 0.9959 0.4803 0.5909 0.083 Uiso 1 1 calc R . . C29 C 0.8688(7) 0.4540(6) 0.6128(3) 0.046(3) Uani 1 1 d . . . C30 C 0.8077(7) 0.4270(6) 0.5881(2) 0.046(3) Uani 1 1 d . . . C31 C 0.7224(8) 0.4012(6) 0.5409(2) 0.047(3) Uani 1 1 d . . . H31 H 0.6982 0.3960 0.5206 0.056 Uiso 1 1 calc R . . C32 C 0.6734(7) 0.3804(5) 0.5655(2) 0.038(2) Uani 1 1 d . . . C33 C 0.5752(7) 0.3499(5) 0.5656(2) 0.039(2) Uani 1 1 d . . . C34 C 0.5029(7) 0.3693(5) 0.5446(2) 0.040(2) Uani 1 1 d . . . H34 H 0.5182 0.4027 0.5308 0.048 Uiso 1 1 calc R . . C35 C 0.4063(7) 0.3405(5) 0.5433(2) 0.036(2) Uani 1 1 d . . . C36 C 0.3867(8) 0.2936(6) 0.5655(2) 0.050(3) Uani 1 1 d . . . H36 H 0.3216 0.2749 0.5661 0.059 Uiso 1 1 calc R . . C37 C 0.4558(9) 0.2748(6) 0.5857(3) 0.052(3) Uani 1 1 d . . . H37 H 0.4397 0.2419 0.5997 0.062 Uiso 1 1 calc R . . C38 C 0.5493(8) 0.3014(5) 0.5867(2) 0.045(2) Uani 1 1 d . . . H38 H 0.5973 0.2876 0.6016 0.054 Uiso 1 1 calc R . . C39 C 0.3308(7) 0.3626(5) 0.5216(2) 0.040(2) Uani 1 1 d . . . C40 C 0.2320(8) 0.3748(5) 0.5299(3) 0.047(3) Uani 1 1 d . . . H40 H 0.2168 0.3708 0.5507 0.057 Uiso 1 1 calc R . . C41 C 0.1547(8) 0.3925(6) 0.5102(3) 0.055(3) Uani 1 1 d . . . C42 C 0.1785(7) 0.4024(5) 0.4804(3) 0.045(3) Uani 1 1 d . . . H42 H 0.1277 0.4171 0.4666 0.054 Uiso 1 1 calc R . . C43 C 0.2767(8) 0.3912(5) 0.4696(2) 0.042(2) Uani 1 1 d . . . C44 C 0.3506(7) 0.3712(5) 0.4899(2) 0.041(2) Uani 1 1 d . . . C45 C 0.0530(8) 0.4051(7) 0.5213(3) 0.071(4) Uani 1 1 d . . . H45A H 0.0561 0.4391 0.5367 0.107 Uiso 1 1 calc R . . H45B H 0.0259 0.3657 0.5302 0.107 Uiso 1 1 calc R . . H45C H 0.0092 0.4190 0.5044 0.107 Uiso 1 1 calc R . . C46 C 0.1076(9) 0.2332(6) 0.3452(3) 0.060(3) Uani 1 1 d . . . H46 H 0.1542 0.2082 0.3342 0.072 Uiso 1 1 calc R . . C47 C 0.0611(12) 0.2865(8) 0.3304(4) 0.081(4) Uani 1 1 d . . . H47 H 0.0788 0.2996 0.3106 0.098 Uiso 1 1 calc R . . C48 C -0.0114(12) 0.3180(7) 0.3466(3) 0.080(4) Uani 1 1 d . . . H48 H -0.0495 0.3514 0.3372 0.096 Uiso 1 1 calc R . . C49 C -0.0300(11) 0.3019(7) 0.3764(4) 0.075(4) Uani 1 1 d . . . H49 H -0.0769 0.3256 0.3878 0.090 Uiso 1 1 calc R . . C50 C 0.0232(9) 0.2491(6) 0.3893(3) 0.060(3) Uani 1 1 d . . . C51 C 0.0052(8) 0.2296(6) 0.4199(3) 0.053(3) Uani 1 1 d . . . C52 C -0.0421(11) 0.2652(7) 0.4421(4) 0.082(5) Uani 1 1 d . . . H52 H -0.0668 0.3070 0.4372 0.098 Uiso 1 1 calc R . . C53 C -0.0538(13) 0.2428(8) 0.4700(3) 0.084(4) Uani 1 1 d . . . H53 H -0.0868 0.2683 0.4846 0.101 Uiso 1 1 calc R . . C54 C -0.0163(9) 0.1792(7) 0.4781(3) 0.063(3) Uani 1 1 d . . . H54 H -0.0253 0.1609 0.4975 0.076 Uiso 1 1 calc R . . C55 C 0.0335(8) 0.1472(6) 0.4553(3) 0.050(3) Uani 1 1 d . . . C56 C 0.0838(8) 0.0866(6) 0.4602(3) 0.048(3) Uani 1 1 d . . . C57 C 0.1759(9) -0.0046(6) 0.4796(3) 0.056(3) Uani 1 1 d . . . H57 H 0.2077 -0.0383 0.4908 0.067 Uiso 1 1 calc R . . C58 C 0.1826(8) 0.0030(5) 0.4488(2) 0.044(2) Uani 1 1 d . . . C59 C 0.2403(8) -0.0360(5) 0.4284(2) 0.045(2) Uani 1 1 d . . . C60 C 0.3398(7) -0.0540(5) 0.4376(2) 0.041(2) Uani 1 1 d . . . H60 H 0.3651 -0.0412 0.4569 0.050 Uiso 1 1 calc R . . C61 C 0.3996(7) -0.0896(5) 0.4189(2) 0.043(2) Uani 1 1 d . . . C62 C 0.3633(9) -0.1084(5) 0.3906(2) 0.049(3) Uani 1 1 d . . . H62 H 0.4041 -0.1325 0.3773 0.059 Uiso 1 1 calc R . . C63 C 0.2663(9) -0.0911(6) 0.3822(3) 0.054(3) Uani 1 1 d . . . H63 H 0.2401 -0.1051 0.3632 0.065 Uiso 1 1 calc R . . C64 C 0.2063(8) -0.0545(6) 0.4004(2) 0.050(3) Uani 1 1 d . . . H64 H 0.1410 -0.0420 0.3935 0.060 Uiso 1 1 calc R . . C65 C 0.5064(8) -0.1052(5) 0.4284(3) 0.046(3) Uani 1 1 d . . . C66 C 0.5834(9) -0.0958(6) 0.4072(3) 0.061(3) Uani 1 1 d . . . H66 H 0.5660 -0.0820 0.3873 0.074 Uiso 1 1 calc R . . C67 C 0.6811(9) -0.1062(6) 0.4148(3) 0.059(3) Uani 1 1 d . . . C68 C 0.7061(9) -0.1253(6) 0.4437(3) 0.059(3) Uani 1 1 d . . . H68 H 0.7751 -0.1311 0.4491 0.070 Uiso 1 1 calc R . . C69 C 0.6338(8) -0.1367(5) 0.4657(2) 0.046(3) Uani 1 1 d . . . C70 C 0.5331(7) -0.1269(5) 0.4570(2) 0.042(2) Uani 1 1 d . . . C71 C 0.7620(11) -0.0962(9) 0.3909(3) 0.093(5) Uani 1 1 d . . . H71A H 0.7928 -0.1377 0.3860 0.139 Uiso 1 1 calc R . . H71B H 0.8138 -0.0668 0.3988 0.139 Uiso 1 1 calc R . . H71C H 0.7309 -0.0777 0.3725 0.139 Uiso 1 1 calc R . . C72 C 0.4185(14) -0.1985(10) 0.4737(5) 0.108(6) Uiso 1 1 d . . . H72A H 0.4735 -0.2305 0.4731 0.130 Uiso 1 1 calc R . . H72B H 0.3814 -0.1997 0.4541 0.130 Uiso 1 1 calc R . . C73 C 0.341(2) -0.2169(16) 0.5017(7) 0.182(11) Uiso 1 1 d . . . H73A H 0.3080 -0.1785 0.5103 0.219 Uiso 1 1 calc R . . H73B H 0.2890 -0.2490 0.4954 0.219 Uiso 1 1 calc R . . C75 C 0.401(2) -0.2568(14) 0.5750(7) 0.164(10) Uiso 1 1 d . . . H75A H 0.3587 -0.2681 0.5924 0.197 Uiso 1 1 calc R . . H75B H 0.4187 -0.2107 0.5771 0.197 Uiso 1 1 calc R . . C76 C 0.5304(16) -0.2804(11) 0.6112(5) 0.128(7) Uiso 1 1 d . . . H76A H 0.4936 -0.3081 0.6250 0.193 Uiso 1 1 calc R . . H76B H 0.5185 -0.2351 0.6163 0.193 Uiso 1 1 calc R . . H76C H 0.6025 -0.2897 0.6130 0.193 Uiso 1 1 calc R . . C77 C 1.0916(8) -0.0766(7) 0.6338(3) 0.065(3) Uani 1 1 d . . . H77 H 1.1104 -0.0913 0.6144 0.078 Uiso 1 1 calc R . . C78 C 1.1657(10) -0.0623(9) 0.6542(4) 0.085(5) Uani 1 1 d . . . H78 H 1.2338 -0.0629 0.6481 0.102 Uiso 1 1 calc R . . C79 C 1.1447(12) -0.0475(9) 0.6821(4) 0.096(5) Uani 1 1 d . . . H79 H 1.1972 -0.0422 0.6968 0.115 Uiso 1 1 calc R . . C80 C 1.0423(10) -0.0396(8) 0.6903(3) 0.076(4) Uani 1 1 d . . . H80 H 1.0240 -0.0259 0.7099 0.091 Uiso 1 1 calc R . . C81 C 0.9687(9) -0.0534(6) 0.6670(3) 0.054(3) Uani 1 1 d . . . C82 C 0.8606(9) -0.0449(6) 0.6719(2) 0.051(3) Uani 1 1 d . . . C83 C 0.8213(10) -0.0138(7) 0.6959(3) 0.070(4) Uani 1 1 d . . . H83 H 0.8641 0.0031 0.7115 0.084 Uiso 1 1 calc R . . C84 C 0.7138(11) -0.0069(10) 0.6975(3) 0.093(5) Uani 1 1 d . . . H84 H 0.6854 0.0157 0.7139 0.111 Uiso 1 1 calc R . . C85 C 0.6538(10) -0.0323(7) 0.6759(3) 0.067(4) Uani 1 1 d . . . H85 H 0.5827 -0.0318 0.6777 0.081 Uiso 1 1 calc R . . C86 C 0.6987(8) -0.0594(6) 0.6509(3) 0.050(3) Uani 1 1 d . . . C87 C 0.6425(7) -0.0827(6) 0.6243(2) 0.044(2) Uani 1 1 d . . . C88 C 0.5284(8) -0.1019(6) 0.5816(3) 0.055(3) Uani 1 1 d . . . H88 H 0.4753 -0.1052 0.5670 0.066 Uiso 1 1 calc R . . C89 C 0.6232(8) -0.1241(5) 0.5779(3) 0.045(2) Uani 1 1 d . . . C90 C 0.6613(7) -0.1547(5) 0.5504(2) 0.039(2) Uani 1 1 d . . . C91 C 0.6297(7) -0.1340(5) 0.5222(3) 0.045(3) Uani 1 1 d . . . H91 H 0.5818 -0.1001 0.5207 0.054 Uiso 1 1 calc R . . C92 C 0.6652(7) -0.1606(5) 0.4959(2) 0.044(2) Uani 1 1 d . . . C93 C 0.7378(7) -0.2095(5) 0.4989(2) 0.047(3) Uani 1 1 d . . . H93 H 0.7653 -0.2279 0.4812 0.056 Uiso 1 1 calc R . . C94 C 0.7699(8) -0.2313(5) 0.5268(3) 0.046(3) Uani 1 1 d . . . H94 H 0.8191 -0.2644 0.5283 0.055 Uiso 1 1 calc R . . C95 C 0.7308(7) -0.2053(5) 0.5527(3) 0.044(3) Uani 1 1 d . . . H95 H 0.7508 -0.2216 0.5720 0.053 Uiso 1 1 calc R . . C96 C 0.0974(10) 0.3656(8) 0.1750(3) 0.080(4) Uani 1 1 d . . . H96A H 0.1151 0.3203 0.1706 0.095 Uiso 1 1 calc R . . H96B H 0.1589 0.3920 0.1729 0.095 Uiso 1 1 calc R . . C98 C 0.9390(19) 0.1953(14) 0.5771(6) 0.160(9) Uiso 1 1 d . . . H98A H 0.9927 0.2268 0.5820 0.192 Uiso 1 1 calc R . . H98B H 0.9101 0.1811 0.5964 0.192 Uiso 1 1 calc R . . O22 O 0.069(2) 0.2926(15) 0.6549(7) 0.278(13) Uiso 1 1 d D . . O21 O 0.145(2) 0.2682(15) 0.6035(7) 0.284(13) Uiso 1 1 d D . . C97 C 0.596(2) 0.4346(13) 0.2851(6) 0.165(10) Uiso 1 1 d D . . H97A H 0.5576 0.4186 0.2671 0.198 Uiso 1 1 calc R . . H97B H 0.6601 0.4109 0.2871 0.198 Uiso 1 1 calc R . . O28 O 0.7176(11) 0.3599(8) 0.3565(4) 0.141(5) Uiso 1 1 d . . . O29 O 0.5724(13) 0.0291(9) 0.4881(4) 0.076(5) Uiso 0.50 1 d P . . O30 O 0.4886(17) -0.1828(12) 0.7498(6) 0.103(7) Uiso 0.50 1 d P . . O2 O 0.4128(11) -0.2425(8) 0.5205(4) 0.133(5) Uiso 1 1 d . . . C74 C 0.342(2) -0.2642(15) 0.5482(7) 0.165(10) Uiso 1 1 d . . . H74A H 0.2810 -0.2366 0.5489 0.198 Uiso 1 1 calc R . . H74B H 0.3200 -0.3095 0.5457 0.198 Uiso 1 1 calc R . . O31 O 0.901(2) -0.1760(14) 0.7323(7) 0.128(9) Uiso 0.50 1 d P . . O32 O 0.7483(16) 0.2249(12) 0.3478(5) 0.099(7) Uiso 0.50 1 d P . . O33 O 0.790(2) 0.2240(16) 0.3083(7) 0.140(10) Uiso 0.50 1 d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cd1 0.0451(4) 0.0483(5) 0.0296(4) 0.0009(3) -0.0070(3) 0.0025(3) Cl1 0.0581(17) 0.075(2) 0.075(2) -0.0126(19) -0.0098(15) 0.0218(15) S1 0.0426(15) 0.105(3) 0.080(3) 0.012(2) -0.0034(15) 0.0092(16) O1 0.051(4) 0.060(5) 0.061(5) 0.015(4) -0.010(4) -0.007(4) N1 0.077(6) 0.046(6) 0.041(6) 0.001(5) -0.001(5) 0.013(5) C1 0.069(8) 0.065(9) 0.073(9) 0.004(7) -0.019(7) 0.019(7) Cd2 0.0469(4) 0.0452(5) 0.0345(5) -0.0018(3) -0.0113(3) 0.0053(3) Cl2 0.0583(17) 0.089(3) 0.057(2) 0.0095(18) 0.0064(14) 0.0032(16) S2 0.0473(14) 0.071(2) 0.0484(18) 0.0073(15) 0.0108(12) 0.0057(13) N2 0.059(5) 0.055(6) 0.041(5) -0.003(5) 0.006(4) -0.009(4) C2 0.148(16) 0.061(10) 0.074(11) -0.002(9) -0.033(11) 0.041(11) S3 0.0633(16) 0.0619(19) 0.0356(15) 0.0047(14) -0.0015(12) -0.0059(14) N3 0.053(5) 0.061(6) 0.037(5) -0.006(5) -0.002(4) 0.001(4) C3 0.162(17) 0.066(11) 0.065(10) 0.001(9) -0.044(11) 0.047(12) Cl4 0.091(3) 0.104(3) 0.089(3) 0.014(3) -0.041(2) -0.007(2) S4 0.0479(15) 0.084(2) 0.0522(19) -0.0040(17) -0.0016(13) 0.0103(14) O4 0.069(7) 0.131(11) 0.172(14) 0.022(10) 0.015(7) -0.007(7) N4 0.040(4) 0.068(6) 0.027(4) 0.008(4) -0.006(3) 0.011(4) C4 0.185(18) 0.051(9) 0.051(9) 0.014(7) -0.041(10) 0.012(10) Cl5 0.070(2) 0.091(3) 0.070(2) -0.0009(19) -0.0073(17) 0.0091(17) O5 0.142(11) 0.142(13) 0.122(11) 0.044(9) 0.065(9) 0.030(9) N5 0.076(6) 0.060(6) 0.033(5) -0.012(5) -0.018(5) 0.004(5) C5 0.119(11) 0.051(8) 0.029(6) 0.000(6) -0.008(7) -0.002(7) Cl6 0.108(3) 0.141(4) 0.080(3) 0.000(3) -0.013(2) -0.040(3) O6 0.085(8) 0.097(9) 0.245(18) -0.060(11) 0.048(9) -0.009(6) N6 0.043(4) 0.041(5) 0.056(6) -0.009(4) -0.014(4) 0.005(4) C6 0.079(8) 0.061(9) 0.058(8) 0.005(7) -0.001(7) -0.007(7) Cl7 0.201(11) 0.138(9) 0.072(6) -0.003(6) 0.080(7) 0.038(8) O7 0.112(9) 0.118(11) 0.123(11) -0.037(8) -0.037(8) 0.038(7) N7 0.035(4) 0.042(5) 0.035(5) -0.005(4) -0.004(3) 0.004(3) C7 0.132(15) 0.063(10) 0.086(12) 0.025(9) 0.024(10) -0.017(10) Cl8 0.078(5) 0.181(12) 0.145(10) -0.046(9) 0.012(5) -0.010(6) O8 0.111(8) 0.105(8) 0.068(7) 0.026(6) 0.036(6) -0.004(6) N8 0.061(5) 0.036(5) 0.049(6) -0.001(4) -0.014(4) 0.010(4) C8 0.067(10) 0.100(15) 0.22(3) 0.048(16) 0.017(12) -0.014(9) O9 0.095(8) 0.28(2) 0.064(8) 0.015(10) -0.021(6) -0.037(10) N9 0.041(4) 0.042(5) 0.055(6) -0.004(4) -0.016(4) -0.003(4) C9 0.077(10) 0.090(13) 0.142(17) 0.022(12) 0.027(10) -0.008(8) O10 0.103(9) 0.109(11) 0.150(13) -0.029(9) 0.024(8) -0.011(7) N10 0.043(4) 0.048(5) 0.035(5) -0.002(4) -0.010(4) 0.005(4) C10 0.049(6) 0.063(8) 0.058(8) 0.001(6) 0.003(5) -0.002(5) O11 0.080(8) 0.162(13) 0.122(11) -0.008(9) 0.020(7) 0.013(7) N11 0.055(5) 0.058(6) 0.043(6) -0.003(5) -0.011(4) 0.009(4) C11 0.038(5) 0.079(9) 0.046(7) 0.000(6) -0.006(5) 0.002(5) N12 0.052(5) 0.047(5) 0.033(5) 0.002(4) -0.007(4) 0.006(4) C12 0.050(6) 0.093(10) 0.044(7) 0.012(7) -0.003(5) 0.009(6) N13 0.044(4) 0.046(5) 0.035(5) 0.003(4) -0.008(4) -0.001(4) C13 0.050(6) 0.057(7) 0.036(6) -0.002(5) -0.011(5) 0.017(5) C14 0.049(6) 0.044(6) 0.050(7) -0.001(5) -0.016(5) 0.010(5) C15 0.066(7) 0.048(7) 0.038(6) 0.004(5) -0.021(5) 0.006(5) O16 0.125(10) 0.155(12) 0.062(7) -0.011(7) -0.029(7) -0.003(8) C16 0.072(8) 0.054(8) 0.046(7) -0.007(6) -0.025(6) 0.004(6) O17 0.153(11) 0.104(10) 0.149(12) 0.057(9) -0.055(9) -0.051(9) C17 0.041(5) 0.045(6) 0.059(8) 0.005(5) -0.015(5) -0.004(4) O18 0.122(9) 0.159(12) 0.055(7) -0.012(7) -0.009(6) -0.001(8) C18 0.038(5) 0.050(7) 0.042(6) -0.003(5) -0.011(4) 0.017(4) O19 0.078(8) 0.182(16) 0.27(2) -0.117(15) 0.073(10) -0.022(9) C19 0.043(5) 0.042(6) 0.034(6) -0.004(5) -0.020(4) 0.003(4) C20 0.098(10) 0.094(11) 0.040(8) -0.011(7) 0.000(7) -0.020(8) C21 0.119(13) 0.108(14) 0.054(9) -0.021(9) 0.006(9) 0.004(11) C22 0.129(14) 0.099(13) 0.063(11) -0.013(9) -0.023(10) -0.013(11) C23 0.094(10) 0.099(12) 0.053(9) -0.019(8) -0.023(8) -0.001(9) O24 0.082(6) 0.099(8) 0.071(6) 0.018(6) -0.013(5) 0.001(5) C24 0.078(8) 0.070(9) 0.052(8) 0.005(7) -0.032(7) -0.003(7) C25 0.051(6) 0.057(7) 0.041(6) -0.007(5) -0.021(5) 0.003(5) C26 0.062(7) 0.069(9) 0.080(10) -0.005(8) -0.017(7) -0.012(6) C27 0.043(6) 0.081(10) 0.107(13) -0.006(9) -0.012(7) -0.021(6) C28 0.056(7) 0.056(8) 0.095(11) 0.006(8) -0.001(7) -0.009(6) C29 0.038(5) 0.053(7) 0.048(7) 0.001(5) -0.004(5) 0.007(4) C30 0.037(5) 0.061(7) 0.040(6) 0.000(5) -0.004(4) 0.013(5) C31 0.055(6) 0.061(7) 0.025(5) 0.000(5) 0.003(5) 0.014(5) C32 0.041(5) 0.044(6) 0.028(5) -0.003(4) -0.002(4) 0.009(4) C33 0.057(6) 0.032(5) 0.029(5) -0.007(4) -0.009(4) 0.004(4) C34 0.057(6) 0.037(6) 0.027(5) -0.005(4) 0.000(4) 0.008(5) C35 0.042(5) 0.034(5) 0.030(5) -0.007(4) 0.001(4) 0.000(4) C36 0.058(6) 0.048(7) 0.043(6) -0.011(5) -0.002(5) -0.001(5) C37 0.072(7) 0.043(7) 0.041(6) -0.003(5) -0.001(6) -0.004(5) C38 0.060(6) 0.038(6) 0.037(6) 0.001(5) -0.010(5) -0.005(5) C39 0.046(5) 0.034(5) 0.039(6) -0.010(5) -0.007(4) -0.004(4) C40 0.051(6) 0.050(7) 0.042(6) -0.012(5) 0.006(5) -0.006(5) C41 0.049(6) 0.048(7) 0.067(9) -0.004(6) 0.000(6) 0.001(5) C42 0.037(5) 0.051(7) 0.045(7) 0.007(5) -0.013(4) 0.004(4) C43 0.052(6) 0.041(6) 0.032(6) 0.000(5) -0.018(4) 0.007(4) C44 0.035(5) 0.041(6) 0.047(7) -0.007(5) -0.003(4) 0.001(4) C45 0.043(6) 0.084(10) 0.088(11) 0.000(8) 0.008(6) 0.012(6) C46 0.078(8) 0.043(7) 0.057(8) 0.016(6) -0.012(6) 0.008(6) C47 0.093(10) 0.075(10) 0.074(10) 0.013(8) -0.028(8) -0.020(8) C48 0.115(12) 0.065(9) 0.058(9) 0.010(7) -0.024(8) 0.026(8) C49 0.091(9) 0.055(8) 0.079(10) -0.002(7) -0.032(8) 0.019(7) C50 0.058(7) 0.048(7) 0.071(9) -0.001(6) -0.032(6) 0.000(5) C51 0.049(6) 0.055(7) 0.055(8) -0.003(6) -0.015(5) 0.013(5) C52 0.100(10) 0.055(8) 0.090(12) -0.025(8) -0.016(9) 0.036(8) C53 0.116(12) 0.090(12) 0.047(8) -0.007(8) -0.011(8) 0.020(9) C54 0.066(7) 0.077(9) 0.046(7) -0.011(7) -0.006(6) 0.012(6) C55 0.052(6) 0.047(7) 0.049(7) -0.004(6) -0.012(5) 0.004(5) C56 0.047(5) 0.056(7) 0.039(6) 0.006(5) -0.011(5) -0.005(5) C57 0.078(8) 0.048(7) 0.041(7) 0.002(5) -0.001(6) -0.005(6) C58 0.054(6) 0.041(6) 0.037(6) 0.000(5) -0.005(5) -0.004(5) C59 0.054(6) 0.040(6) 0.039(6) 0.005(5) -0.015(5) -0.010(5) C60 0.056(6) 0.033(5) 0.035(6) 0.012(5) -0.014(5) -0.001(4) C61 0.048(5) 0.046(6) 0.034(6) 0.007(5) -0.011(4) 0.001(5) C62 0.077(7) 0.043(6) 0.028(6) -0.004(5) -0.008(5) 0.003(5) C63 0.076(7) 0.048(7) 0.037(6) -0.010(5) -0.019(6) 0.004(6) C64 0.060(6) 0.052(7) 0.038(6) 0.002(5) -0.017(5) 0.003(5) C65 0.055(6) 0.034(6) 0.049(7) 0.005(5) -0.008(5) -0.002(4) C66 0.073(8) 0.070(9) 0.042(7) 0.010(6) 0.001(6) 0.008(6) C67 0.061(7) 0.058(8) 0.059(8) 0.012(6) -0.004(6) 0.000(5) C68 0.054(6) 0.057(8) 0.065(8) 0.000(6) -0.002(6) -0.003(5) C69 0.051(6) 0.048(6) 0.038(6) 0.003(5) -0.014(5) 0.004(5) C70 0.052(6) 0.038(6) 0.035(6) 0.004(5) -0.006(5) -0.002(4) C71 0.080(9) 0.136(16) 0.063(10) 0.033(10) 0.015(8) 0.025(9) C77 0.051(7) 0.079(9) 0.064(9) -0.017(7) -0.009(6) -0.013(6) C78 0.064(8) 0.112(14) 0.079(11) -0.027(10) -0.025(7) 0.000(8) C79 0.088(11) 0.102(13) 0.095(13) -0.025(11) -0.046(9) 0.003(9) C80 0.073(8) 0.091(11) 0.063(9) -0.017(8) -0.014(7) -0.003(7) C81 0.070(7) 0.057(7) 0.034(6) -0.005(5) -0.021(5) -0.004(6) C82 0.069(7) 0.047(7) 0.036(6) -0.005(5) -0.012(5) -0.001(5) C83 0.081(9) 0.086(10) 0.043(7) -0.002(7) -0.008(6) -0.002(7) C84 0.093(10) 0.156(17) 0.029(7) -0.026(9) -0.006(7) 0.019(10) C85 0.063(7) 0.089(10) 0.051(8) -0.018(7) 0.009(6) -0.003(7) C86 0.060(6) 0.049(7) 0.041(6) 0.001(5) -0.001(5) 0.004(5) C87 0.044(5) 0.056(7) 0.033(6) 0.001(5) 0.002(4) -0.004(5) C88 0.041(5) 0.071(8) 0.051(7) -0.011(6) -0.007(5) 0.006(5) C89 0.049(6) 0.044(6) 0.042(6) 0.004(5) -0.007(5) -0.005(5) C90 0.037(5) 0.038(6) 0.042(6) 0.001(5) -0.017(4) -0.002(4) C91 0.035(5) 0.046(6) 0.054(7) 0.005(5) -0.007(5) -0.005(4) C92 0.046(5) 0.040(6) 0.044(6) 0.004(5) -0.011(5) -0.003(4) C93 0.049(5) 0.047(6) 0.044(6) -0.013(5) -0.013(5) -0.012(5) C94 0.057(6) 0.029(5) 0.052(7) -0.009(5) -0.024(5) 0.010(4) C95 0.050(5) 0.037(6) 0.045(6) 0.006(5) -0.021(5) -0.006(4) C96 0.068(8) 0.095(11) 0.076(10) 0.001(9) 0.006(7) -0.002(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cd1 N6 2.308(9) . ? Cd1 N2 2.315(9) 3_666 ? Cd1 N3 2.340(9) 3_666 ? Cd1 N1 2.352(10) 3_666 ? Cd1 N7 2.356(8) . ? Cd1 N5 2.361(9) . ? Cl1 O4 1.382(11) . ? Cl1 O6 1.397(12) . ? Cl1 O7 1.419(13) . ? Cl1 O5 1.476(13) . ? S1 C12 1.709(14) . ? S1 C11 1.734(11) . ? O1 C72 1.32(2) . ? O1 C70 1.424(13) . ? N1 C5 1.298(17) . ? N1 C1 1.328(15) . ? N1 Cd1 2.352(9) 3_666 ? C1 C2 1.37(2) . ? Cd2 N9 2.299(9) 3_656 ? Cd2 N12 2.312(9) . ? Cd2 N10 2.324(9) 3_656 ? Cd2 N11 2.361(9) . ? Cd2 N13 2.376(8) . ? Cd2 N8 2.404(9) 3_656 ? Cl2 O10 1.368(13) . ? Cl2 O11 1.371(12) . ? Cl2 O9 1.410(12) . ? Cl2 O8 1.414(9) . ? S2 C30 1.706(11) . ? S2 C31 1.707(12) . ? N2 C6 1.323(16) . ? N2 C10 1.334(14) . ? N2 Cd1 2.315(9) 3_666 ? C2 C3 1.35(3) . ? Cl3 O12 1.27(2) . ? Cl3 O14 1.411(13) . ? Cl3 O15 1.41(3) . ? Cl3 O13 1.486(15) . ? S3 C57 1.678(13) . ? S3 C56 1.713(11) . ? O3 C75 1.44(3) . ? O3 C76 1.58(2) . ? N3 C11 1.315(14) . ? N3 C13 1.372(14) . ? N3 Cd1 2.340(9) 3_666 ? C3 C4 1.43(3) . ? Cl4 O19 1.221(16) . ? Cl4 O16 1.330(12) . ? Cl4 O17 1.487(13) . ? Cl4 O18 1.517(12) . ? S4 C87 1.712(10) . ? S4 C88 1.719(12) . ? N4 C44 1.421(12) . ? C4 C5 1.442(18) . ? Cl5 C96 1.777(15) . ? N5 C20 1.279(16) . ? N5 C24 1.346(16) . ? C5 C6 1.471(19) . ? Cl6 C96 1.669(15) . ? N6 C25 1.327(13) . ? N6 C29 1.350(14) . ? C6 C7 1.43(2) . ? Cl7 C97 1.64(2) . ? N7 C30 1.328(13) . ? N7 C32 1.378(12) . ? C7 C8 1.32(2) . ? Cl8 C97 1.94(3) . ? N8 C46 1.277(15) . ? N8 C50 1.352(16) . ? N8 Cd2 2.404(9) 3_656 ? C8 C9 1.40(3) . ? Cl9 C98 1.80(3) . ? N9 C55 1.341(14) . ? N9 C51 1.362(14) . ? N9 Cd2 2.299(9) 3_656 ? C9 C10 1.373(19) . ? Cl10 C98 1.75(3) . ? N10 C56 1.335(14) . ? N10 C58 1.384(13) . ? N10 Cd2 2.324(9) 3_656 ? C10 C11 1.408(17) . ? Cl11 O20 1.423(15) . ? Cl11 O22 1.50(3) . ? Cl11 O23 1.51(2) . ? Cl11 O21 1.57(3) . ? N11 C77 1.327(14) . ? N11 C81 1.336(14) . ? N12 C86 1.335(13) . ? N12 C82 1.353(13) . ? C12 C13 1.362(14) . ? N13 C87 1.306(14) . ? N13 C89 1.389(13) . ? C13 C14 1.452(16) . ? C14 C15 1.376(14) . ? C14 C19 1.400(15) . ? C15 C16 1.391(17) . ? C16 C17 1.356(17) . ? C17 C18 1.429(14) . ? C18 C19 1.404(15) . ? C18 C43 1.444(15) . ? C20 C21 1.38(2) . ? C21 C22 1.35(2) . ? C22 C23 1.37(2) . ? C23 C24 1.453(18) . ? C24 C25 1.465(18) . ? C25 C26 1.383(17) . ? C26 C27 1.34(2) . ? C27 C28 1.38(2) . ? C28 C29 1.376(15) . ? C29 C30 1.460(15) . ? C31 C32 1.353(14) . ? C32 C33 1.452(14) . ? C33 C34 1.381(13) . ? C33 C38 1.421(14) . ? C34 C35 1.418(14) . ? C35 C36 1.412(15) . ? C35 C39 1.448(13) . ? C36 C37 1.324(15) . ? C37 C38 1.361(15) . ? C39 C40 1.395(14) . ? C39 C44 1.443(15) . ? C40 C41 1.384(16) . ? C41 C42 1.379(17) . ? C41 C45 1.473(16) . ? C42 C43 1.419(15) . ? C43 C44 1.380(14) . ? C46 C47 1.421(18) . ? C47 C48 1.38(2) . ? C48 C49 1.39(2) . ? C49 C50 1.418(17) . ? C50 C51 1.441(18) . ? C51 C52 1.391(17) . ? C52 C53 1.33(2) . ? C53 C54 1.45(2) . ? C54 C55 1.388(16) . ? C55 C56 1.440(16) . ? C57 C58 1.376(15) . ? C58 C59 1.448(15) . ? C59 C64 1.363(14) . ? C59 C60 1.426(14) . ? C60 C61 1.377(15) . ? C61 C62 1.388(14) . ? C61 C65 1.508(14) . ? C62 C63 1.382(16) . ? C63 C64 1.376(16) . ? C65 C70 1.383(15) . ? C65 C66 1.417(17) . ? C66 C67 1.353(17) . ? C67 C68 1.373(18) . ? C67 C71 1.540(19) . ? C68 C69 1.403(16) . ? C69 C70 1.400(14) . ? C69 C92 1.475(14) . ? C72 C73 1.67(3) . ? C73 O2 1.37(3) . ? C75 C74 1.42(3) . ? C77 C78 1.355(17) . ? C78 C79 1.31(2) . ? C79 C80 1.43(2) . ? C80 C81 1.432(16) . ? C81 C82 1.469(16) . ? C82 C83 1.360(17) . ? C83 C84 1.440(19) . ? C84 C85 1.340(19) . ? C85 C86 1.388(16) . ? C86 C87 1.462(15) . ? C88 C89 1.356(15) . ? C89 C90 1.470(15) . ? C90 C91 1.378(14) . ? C90 C95 1.403(14) . ? C91 C92 1.380(15) . ? C92 C93 1.406(15) . ? C93 C94 1.374(15) . ? C94 C95 1.377(15) . ? O2 C74 1.63(3) . ? 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 N6 Cd1 N2 168.7(3) . 3_666 ? N6 Cd1 N3 117.5(3) . 3_666 ? N2 Cd1 N3 69.9(3) 3_666 3_666 ? N6 Cd1 N1 103.2(3) . 3_666 ? N2 Cd1 N1 69.7(4) 3_666 3_666 ? N3 Cd1 N1 139.3(4) 3_666 3_666 ? N6 Cd1 N7 71.2(3) . . ? N2 Cd1 N7 118.5(3) 3_666 . ? N3 Cd1 N7 90.0(3) 3_666 . ? N1 Cd1 N7 104.4(3) 3_666 . ? N6 Cd1 N5 69.3(4) . . ? N2 Cd1 N5 101.5(3) 3_666 . ? N3 Cd1 N5 102.3(3) 3_666 . ? N1 Cd1 N5 90.8(3) 3_666 . ? N7 Cd1 N5 140.0(3) . . ? O4 Cl1 O6 123.5(8) . . ? O4 Cl1 O7 110.7(9) . . ? O6 Cl1 O7 114.8(8) . . ? O4 Cl1 O5 100.1(8) . . ? O6 Cl1 O5 101.3(9) . . ? O7 Cl1 O5 102.1(10) . . ? C12 S1 C11 89.7(6) . . ? C72 O1 C70 110.9(11) . . ? C5 N1 C1 122.3(12) . . ? C5 N1 Cd1 116.1(8) . 3_666 ? C1 N1 Cd1 120.7(9) . 3_666 ? N1 C1 C2 122.0(16) . . ? N9 Cd2 N12 166.1(3) 3_656 . ? N9 Cd2 N10 71.0(3) 3_656 3_656 ? N12 Cd2 N10 121.0(3) . 3_656 ? N9 Cd2 N11 101.3(3) 3_656 . ? N12 Cd2 N11 69.5(3) . . ? N10 Cd2 N11 107.1(3) 3_656 . ? N9 Cd2 N13 119.5(3) 3_656 . ? N12 Cd2 N13 70.3(3) . . ? N10 Cd2 N13 88.2(3) 3_656 . ? N11 Cd2 N13 139.3(3) . . ? N9 Cd2 N8 69.9(3) 3_656 3_656 ? N12 Cd2 N8 98.6(3) . 3_656 ? N10 Cd2 N8 140.5(3) 3_656 3_656 ? N11 Cd2 N8 86.3(3) . 3_656 ? N13 Cd2 N8 105.8(3) . 3_656 ? O10 Cl2 O11 111.0(8) . . ? O10 Cl2 O9 109.3(11) . . ? O11 Cl2 O9 111.8(10) . . ? O10 Cl2 O8 108.2(8) . . ? O11 Cl2 O8 112.3(8) . . ? O9 Cl2 O8 104.0(8) . . ? C30 S2 C31 90.2(5) . . ? C6 N2 C10 121.7(10) . . ? C6 N2 Cd1 119.2(8) . 3_666 ? C10 N2 Cd1 119.1(8) . 3_666 ? C3 C2 C1 118.7(18) . . ? O12 Cl3 O14 106.1(11) . . ? O12 Cl3 O15 114.3(15) . . ? O14 Cl3 O15 113.2(13) . . ? O12 Cl3 O13 111.2(11) . . ? O14 Cl3 O13 114.3(8) . . ? O15 Cl3 O13 98.0(13) . . ? C57 S3 C56 90.2(6) . . ? C75 O3 C76 103.4(17) . . ? C11 N3 C13 114.0(9) . . ? C11 N3 Cd1 113.8(8) . 3_666 ? C13 N3 Cd1 130.4(7) . 3_666 ? C2 C3 C4 121.3(15) . . ? O19 Cl4 O16 115.7(11) . . ? O19 Cl4 O17 98.2(11) . . ? O16 Cl4 O17 105.4(8) . . ? O19 Cl4 O18 116.7(12) . . ? O16 Cl4 O18 108.7(8) . . ? O17 Cl4 O18 111.0(10) . . ? C87 S4 C88 90.2(5) . . ? C3 C4 C5 114.9(17) . . ? C20 N5 C24 119.1(11) . . ? C20 N5 Cd1 124.5(9) . . ? C24 N5 Cd1 116.3(8) . . ? N1 C5 C4 120.8(15) . . ? N1 C5 C6 119.2(11) . . ? C4 C5 C6 120.0(14) . . ? C25 N6 C29 119.4(10) . . ? C25 N6 Cd1 121.1(8) . . ? C29 N6 Cd1 119.5(7) . . ? N2 C6 C7 119.9(13) . . ? N2 C6 C5 114.9(11) . . ? C7 C6 C5 125.1(14) . . ? C30 N7 C32 112.2(9) . . ? C30 N7 Cd1 113.0(7) . . ? C32 N7 Cd1 133.3(6) . . ? C8 C7 C6 117.6(15) . . ? C46 N8 C50 121.5(10) . . ? C46 N8 Cd2 123.1(8) . 3_656 ? C50 N8 Cd2 113.2(8) . 3_656 ? C7 C8 C9 122.4(15) . . ? C55 N9 C51 120.1(10) . . ? C55 N9 Cd2 119.0(7) . 3_656 ? C51 N9 Cd2 120.6(8) . 3_656 ? C10 C9 C8 117.1(16) . . ? C56 N10 C58 111.0(9) . . ? C56 N10 Cd2 114.1(7) . 3_656 ? C58 N10 Cd2 132.8(7) . 3_656 ? N2 C10 C9 121.0(13) . . ? N2 C10 C11 113.7(10) . . ? C9 C10 C11 124.9(12) . . ? O20 Cl11 O22 100.0(14) . . ? O20 Cl11 O23 109.2(12) . . ? O22 Cl11 O23 131.7(16) . . ? O20 Cl11 O21 109.3(15) . . ? O22 Cl11 O21 113.3(18) . . ? O23 Cl11 O21 92.4(15) . . ? C77 N11 C81 117.3(10) . . ? C77 N11 Cd2 123.8(8) . . ? C81 N11 Cd2 117.5(7) . . ? N3 C11 C10 123.1(10) . . ? N3 C11 S1 112.1(9) . . ? C10 C11 S1 124.7(8) . . ? C86 N12 C82 121.5(10) . . ? C86 N12 Cd2 119.0(7) . . ? C82 N12 Cd2 119.0(7) . . ? C13 C12 S1 111.7(10) . . ? C87 N13 C89 112.2(9) . . ? C87 N13 Cd2 114.3(7) . . ? C89 N13 Cd2 131.7(7) . . ? C12 C13 N3 112.5(11) . . ? C12 C13 C14 127.6(11) . . ? N3 C13 C14 119.9(9) . . ? C15 C14 C19 117.7(10) . . ? C15 C14 C13 123.1(11) . . ? C19 C14 C13 119.1(9) . . ? C14 C15 C16 120.5(11) . . ? C17 C16 C15 121.3(10) . . ? C16 C17 C18 121.2(10) . . ? C19 C18 C17 115.3(10) . . ? C19 C18 C43 122.7(9) . . ? C17 C18 C43 121.9(10) . . ? C14 C19 C18 123.8(9) . . ? N5 C20 C21 125.2(15) . . ? C22 C21 C20 119.5(16) . . ? C21 C22 C23 117.2(15) . . ? C22 C23 C24 120.8(15) . . ? N5 C24 C23 118.1(13) . . ? N5 C24 C25 118.6(11) . . ? C23 C24 C25 123.1(13) . . ? N6 C25 C26 120.6(12) . . ? N6 C25 C24 114.2(10) . . ? C26 C25 C24 125.1(11) . . ? C27 C26 C25 119.7(13) . . ? C26 C27 C28 121.2(12) . . ? C29 C28 C27 116.7(14) . . ? N6 C29 C28 122.4(11) . . ? N6 C29 C30 112.8(9) . . ? C28 C29 C30 124.9(11) . . ? N7 C30 C29 123.1(10) . . ? N7 C30 S2 113.0(8) . . ? C29 C30 S2 123.6(8) . . ? C32 C31 S2 111.1(8) . . ? C31 C32 N7 113.4(9) . . ? C31 C32 C33 126.1(9) . . ? N7 C32 C33 120.3(9) . . ? C34 C33 C38 118.2(9) . . ? C34 C33 C32 119.0(9) . . ? C38 C33 C32 122.8(9) . . ? C33 C34 C35 121.5(10) . . ? C36 C35 C34 116.2(9) . . ? C36 C35 C39 123.0(9) . . ? C34 C35 C39 120.6(9) . . ? C37 C36 C35 122.4(10) . . ? C36 C37 C38 121.5(11) . . ? C37 C38 C33 120.0(10) . . ? C40 C39 C44 115.3(9) . . ? C40 C39 C35 121.7(10) . . ? C44 C39 C35 123.0(8) . . ? C41 C40 C39 124.9(11) . . ? C42 C41 C40 117.3(10) . . ? C42 C41 C45 121.6(11) . . ? C40 C41 C45 120.9(12) . . ? C41 C42 C43 122.0(9) . . ? C44 C43 C42 118.6(10) . . ? C44 C43 C18 122.8(9) . . ? C42 C43 C18 118.6(8) . . ? C43 C44 N4 119.4(10) . . ? C43 C44 C39 121.7(9) . . ? N4 C44 C39 118.8(8) . . ? N8 C46 C47 123.8(14) . . ? C48 C47 C46 115.5(15) . . ? C47 C48 C49 121.5(13) . . ? C48 C49 C50 118.1(14) . . ? N8 C50 C49 119.4(13) . . ? N8 C50 C51 120.4(10) . . ? C49 C50 C51 120.3(13) . . ? N9 C51 C52 118.9(12) . . ? N9 C51 C50 114.0(10) . . ? C52 C51 C50 127.1(12) . . ? C53 C52 C51 122.1(14) . . ? C52 C53 C54 120.0(14) . . ? C55 C54 C53 115.0(12) . . ? N9 C55 C54 123.7(11) . . ? N9 C55 C56 113.9(10) . . ? C54 C55 C56 122.4(11) . . ? N10 C56 C55 121.6(10) . . ? N10 C56 S3 113.8(8) . . ? C55 C56 S3 124.1(9) . . ? C58 C57 S3 112.0(9) . . ? C57 C58 N10 113.1(10) . . ? C57 C58 C59 127.0(10) . . ? N10 C58 C59 119.9(9) . . ? C64 C59 C60 118.3(11) . . ? C64 C59 C58 123.7(10) . . ? C60 C59 C58 117.9(9) . . ? C61 C60 C59 120.9(9) . . ? C60 C61 C62 120.0(10) . . ? C60 C61 C65 120.0(9) . . ? C62 C61 C65 119.9(10) . . ? C63 C62 C61 118.2(11) . . ? C64 C63 C62 122.5(10) . . ? C59 C64 C63 120.0(10) . . ? C70 C65 C66 118.4(10) . . ? C70 C65 C61 123.2(10) . . ? C66 C65 C61 118.4(10) . . ? C67 C66 C65 121.3(12) . . ? C66 C67 C68 119.2(12) . . ? C66 C67 C71 119.3(12) . . ? C68 C67 C71 121.4(11) . . ? C67 C68 C69 122.6(11) . . ? C70 C69 C68 116.9(10) . . ? C70 C69 C92 123.2(10) . . ? C68 C69 C92 119.9(9) . . ? C65 C70 C69 121.5(10) . . ? C65 C70 O1 119.4(9) . . ? C69 C70 O1 119.0(9) . . ? O1 C72 C73 109.9(18) . . ? O2 C73 C72 96(2) . . ? C74 C75 O3 118(3) . . ? N11 C77 C78 124.1(13) . . ? C79 C78 C77 120.8(15) . . ? C78 C79 C80 119.4(13) . . ? C79 C80 C81 115.9(13) . . ? N11 C81 C80 122.2(11) . . ? N11 C81 C82 115.9(9) . . ? C80 C81 C82 121.8(11) . . ? N12 C82 C83 119.3(11) . . ? N12 C82 C81 116.2(10) . . ? C83 C82 C81 124.4(11) . . ? C82 C83 C84 119.0(12) . . ? C85 C84 C83 120.1(13) . . ? C84 C85 C86 117.9(12) . . ? N12 C86 C85 121.6(11) . . ? N12 C86 C87 114.7(10) . . ? C85 C86 C87 123.6(11) . . ? N13 C87 C86 121.2(9) . . ? N13 C87 S4 113.6(8) . . ? C86 C87 S4 124.9(8) . . ? C89 C88 S4 110.2(8) . . ? C88 C89 N13 113.8(10) . . ? C88 C89 C90 125.9(10) . . ? N13 C89 C90 120.2(9) . . ? C91 C90 C95 119.1(10) . . ? C91 C90 C89 120.7(9) . . ? C95 C90 C89 120.2(9) . . ? C90 C91 C92 122.4(10) . . ? C91 C92 C93 117.2(10) . . ? C91 C92 C69 122.0(10) . . ? C93 C92 C69 120.7(10) . . ? C94 C93 C92 121.5(10) . . ? C93 C94 C95 120.1(10) . . ? C94 C95 C90 119.6(9) . . ? Cl6 C96 Cl5 112.7(8) . . ? Cl10 C98 Cl9 116.1(16) . . ? Cl7 C97 Cl8 100.5(14) . . ? C73 O2 C74 98.9(19) . . ? C75 C74 O2 106(2) . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 2.368 _refine_diff_density_min -1.571 _refine_diff_density_rms 0.242 _database_code_depnum_ccdc_archive 'CCDC 958175'