# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2005 data_global _journal_coden_Cambridge 182 loop_ _publ_author_name 'Jason Love' 'A. Blake' 'Gonzalo Givaja' 'M. Schroder' 'Claire Wilson' _publ_contact_author_name 'Jason Love' _publ_contact_author_address ; School of Chemistry University of Nottingham University Park Nottingham NG7 2RD UNITED KINGDOM ; _publ_contact_author_email JASON.LOVE@NOTTINGHAM.AC.UK _publ_requested_journal 'Chemical Communications' _publ_section_title ; Metal-directed ring expansion in Schiff-base polypyrollic macrocycles ; data_cdpyra _database_code_depnum_ccdc_archive 'CCDC 274152' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C49.25 H51.25 Cd2 Cl9.75 N8 O8' _chemical_formula_weight 1453.67 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' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 14.6804(13) _cell_length_b 20.348(2) _cell_length_c 25.125(2) _cell_angle_alpha 74.108(1) _cell_angle_beta 74.961(1) _cell_angle_gamma 70.241(1) _cell_volume 6677(2) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 19016 _cell_measurement_theta_min 2.15 _cell_measurement_theta_max 27.5 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.55 _exptl_crystal_size_mid 0.27 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.446 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2914 _exptl_absorpt_coefficient_mu 1.077 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.593 _exptl_absorpt_correction_T_max 1.00 _exptl_absorpt_process_details 'sadabs v2.05' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART1000 CCD area detector' _diffrn_measurement_method omega _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 58646 _diffrn_reflns_av_R_equivalents 0.038 _diffrn_reflns_av_sigmaI/netI 0.0549 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 1.50 _diffrn_reflns_theta_max 27.50 _reflns_number_total 29147 _reflns_number_gt 16646 _reflns_threshold_expression >2\s(I) _computing_data_collection 'Bruker SMART version 5.624 (Bruker, 2001)' _computing_cell_refinement 'Bruker SAINT version 6.36a (Bruker, 2000)' _computing_data_reduction 'Bruker SAINT; Bruker SHELXTL (Bruker, 2001)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material 'enCIFer (CCDC, 2003); PLATON (Spek, 2003)' _refine_special_details ; SQUEEZE used to account for poorly defined electron density corresponding to approximately 2 molecules of solvent per asymmetric unit. Disorder in 2 of the explicitly modelled CHCl3 molecules. Cl8 and CL9 modelled over two sites with occupancies 0.6 and 0.4. C5s molecule half occupied and Cl13 and Cl23 each 0.25 occupied and modelled with isotropic adps. ; _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^)+(0.0963P)^2^+22.9673P] 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 22782 _refine_ls_number_parameters 1358 _refine_ls_number_restraints 15 _refine_ls_R_factor_all 0.0828 _refine_ls_R_factor_gt 0.0587 _refine_ls_wR_factor_ref 0.1850 _refine_ls_wR_factor_gt 0.1690 _refine_ls_goodness_of_fit_ref 1.069 _refine_ls_restrained_S_all 1.070 _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 0.74246(3) 0.03570(2) 0.604141(19) 0.02685(13) Uani 1 1 d . . . Cd2 Cd 0.57840(3) 0.20601(2) 0.655930(19) 0.02574(12) Uani 1 1 d . . . O1 O 0.7875(5) 0.1193(3) 0.5181(2) 0.0585(17) Uani 1 1 d . . . O2 O 0.6872(4) 0.0604(3) 0.5218(2) 0.0368(11) Uani 1 1 d . . . O3 O 0.6653(3) -0.0053(2) 0.69944(18) 0.0295(10) Uani 1 1 d . . . O4 O 0.5736(3) 0.0892(2) 0.65180(16) 0.0231(9) Uani 1 1 d . . . O5 O 0.5522(4) 0.2236(3) 0.5654(2) 0.0495(14) Uani 1 1 d . . . O6 O 0.6193(4) 0.2959(3) 0.5792(2) 0.0421(12) Uani 1 1 d . . . O7 O 0.6602(3) 0.1327(2) 0.72998(19) 0.0330(11) Uani 1 1 d . . . O8 O 0.7498(3) 0.1249(2) 0.64684(19) 0.0313(10) Uani 1 1 d . . . N1 N 0.3836(4) 0.1629(3) 0.6263(2) 0.0288(12) Uani 1 1 d . . . H1B H 0.4471 0.1454 0.6269 0.035 Uiso 1 1 calc R . . N2 N 0.5409(4) -0.0006(3) 0.5846(2) 0.0329(13) Uani 1 1 d . . . H2A H 0.5815 0.0224 0.5612 0.040 Uiso 1 1 calc R . . N3 N 0.7463(4) -0.0839(3) 0.6065(2) 0.0303(12) Uani 1 1 d . . . N4 N 0.9030(4) -0.0337(3) 0.6040(2) 0.0305(12) Uani 1 1 d . . . N5 N 0.9359(4) 0.1163(3) 0.5764(2) 0.0336(13) Uani 1 1 d . . . H5A H 0.8778 0.1208 0.5986 0.040 Uiso 1 1 calc R . . N6 N 0.7764(4) 0.2707(3) 0.6325(2) 0.0326(13) Uani 1 1 d . . . H6A H 0.7326 0.2805 0.6112 0.039 Uiso 1 1 calc R . . N7 N 0.5784(4) 0.2877(3) 0.7086(2) 0.0287(12) Uani 1 1 d . . . N8 N 0.4208(4) 0.2421(3) 0.7046(2) 0.0271(12) Uani 1 1 d . . . C1 C 0.3384(5) 0.2491(3) 0.6905(3) 0.0288(14) Uani 1 1 d . . . H1A H 0.2826 0.2829 0.7064 0.035 Uiso 1 1 calc R . . C2 C 0.3191(5) 0.2137(4) 0.6548(3) 0.0319(15) Uani 1 1 d . . . C3 C 0.2271(5) 0.2275(5) 0.6423(3) 0.049(2) Uani 1 1 d . . . H3A H 0.1682 0.2610 0.6559 0.059 Uiso 1 1 calc R . . C4 C 0.2364(6) 0.1834(5) 0.6063(3) 0.050(2) Uani 1 1 d . . . H4A H 0.1851 0.1810 0.5911 0.060 Uiso 1 1 calc R . . C5 C 0.3344(5) 0.1437(4) 0.5969(3) 0.0364(17) Uani 1 1 d . . . C6 C 0.3880(5) 0.0919(4) 0.5580(3) 0.0410(18) Uani 1 1 d . . . C7 C 0.3099(6) 0.0776(5) 0.5347(4) 0.057(2) Uani 1 1 d . . . H7A H 0.3429 0.0431 0.5102 0.085 Uiso 1 1 calc R . . H7B H 0.2734 0.1223 0.5132 0.085 Uiso 1 1 calc R . . H7C H 0.2642 0.0583 0.5662 0.085 Uiso 1 1 calc R . . C8 C 0.4556(5) 0.1255(4) 0.5080(3) 0.0430(18) Uani 1 1 d . . . H8A H 0.5073 0.1329 0.5218 0.064 Uiso 1 1 calc R . . H8B H 0.4168 0.1714 0.4891 0.064 Uiso 1 1 calc R . . H8C H 0.4859 0.0935 0.4813 0.064 Uiso 1 1 calc R . . C9 C 0.4419(5) 0.0232(4) 0.5907(3) 0.0359(16) Uani 1 1 d . . . C10 C 0.4058(6) -0.0282(5) 0.6310(4) 0.050(2) Uani 1 1 d . . . H10A H 0.3382 -0.0260 0.6440 0.060 Uiso 1 1 calc R . . C11 C 0.4848(6) -0.0837(5) 0.6494(3) 0.0459(19) Uani 1 1 d . . . H11A H 0.4812 -0.1259 0.6769 0.055 Uiso 1 1 calc R . . C12 C 0.5697(5) -0.0655(4) 0.6199(3) 0.0353(16) Uani 1 1 d . . . C13 C 0.6671(5) -0.1048(4) 0.6263(3) 0.0368(16) Uani 1 1 d . . . H13A H 0.6761 -0.1523 0.6475 0.044 Uiso 1 1 calc R . . C14 C 0.8358(5) -0.1335(4) 0.6167(3) 0.0331(15) Uani 1 1 d . . . C15 C 0.8545(7) -0.2078(4) 0.6249(3) 0.048(2) Uani 1 1 d . . . H15A H 0.8041 -0.2258 0.6225 0.058 Uiso 1 1 calc R . . C16 C 0.9421(7) -0.2550(4) 0.6360(3) 0.054(2) Uani 1 1 d . . . H16A H 0.9520 -0.3048 0.6414 0.065 Uiso 1 1 calc R . . C17 C 1.0167(7) -0.2294(4) 0.6392(3) 0.055(2) Uani 1 1 d . . . H17A H 1.0775 -0.2619 0.6479 0.066 Uiso 1 1 calc R . . C18 C 1.0027(6) -0.1575(4) 0.6300(3) 0.0437(18) Uani 1 1 d . . . H18A H 1.0538 -0.1407 0.6330 0.052 Uiso 1 1 calc R . . C19 C 0.9156(5) -0.1085(4) 0.6163(3) 0.0346(16) Uani 1 1 d . . . C20 C 0.9824(5) -0.0133(4) 0.5758(3) 0.0303(15) Uani 1 1 d . . . H20A H 1.0371 -0.0503 0.5631 0.036 Uiso 1 1 calc R . . C21 C 0.9982(5) 0.0537(4) 0.5619(3) 0.0326(15) Uani 1 1 d . . . C22 C 1.0828(5) 0.0696(4) 0.5279(3) 0.0385(17) Uani 1 1 d . . . H22A H 1.1398 0.0365 0.5122 0.046 Uiso 1 1 calc R . . C23 C 1.0690(5) 0.1421(4) 0.5211(3) 0.0353(16) Uani 1 1 d . . . H23A H 1.1143 0.1678 0.4995 0.042 Uiso 1 1 calc R . . C24 C 0.9775(5) 0.1701(4) 0.5515(3) 0.0311(15) Uani 1 1 d . . . C25 C 0.9225(5) 0.2469(4) 0.5544(3) 0.0400(17) Uani 1 1 d . . . C26 C 0.9936(6) 0.2935(5) 0.5328(4) 0.051(2) Uani 1 1 d . . . H26A H 1.0254 0.2900 0.4938 0.076 Uiso 1 1 calc R . . H26B H 1.0439 0.2767 0.5565 0.076 Uiso 1 1 calc R . . H26C H 0.9567 0.3432 0.5344 0.076 Uiso 1 1 calc R . . C27 C 0.8456(6) 0.2716(5) 0.5158(3) 0.049(2) Uani 1 1 d . . . H27A H 0.8006 0.2419 0.5293 0.074 Uiso 1 1 calc R . . H27B H 0.8793 0.2672 0.4773 0.074 Uiso 1 1 calc R . . H27C H 0.8081 0.3215 0.5164 0.074 Uiso 1 1 calc R . . C28 C 0.8740(5) 0.2525(4) 0.6151(3) 0.0342(16) Uani 1 1 d . . . C29 C 0.9185(6) 0.2419(4) 0.6600(3) 0.0440(19) Uani 1 1 d . . . H29A H 0.9873 0.2286 0.6594 0.053 Uiso 1 1 calc R . . C30 C 0.8446(6) 0.2543(4) 0.7061(3) 0.0431(18) Uani 1 1 d . . . H30A H 0.8533 0.2512 0.7430 0.052 Uiso 1 1 calc R . . C31 C 0.7549(6) 0.2719(4) 0.6890(3) 0.0375(17) Uani 1 1 d . . . C32 C 0.6595(5) 0.2842(4) 0.7232(3) 0.0336(16) Uani 1 1 d . . . H32A H 0.6541 0.2903 0.7601 0.040 Uiso 1 1 calc R . . C33 C 0.4893(5) 0.3053(4) 0.7473(3) 0.0331(15) Uani 1 1 d . . . C34 C 0.4759(6) 0.3490(4) 0.7851(4) 0.047(2) Uani 1 1 d . . . H34A H 0.5267 0.3686 0.7840 0.057 Uiso 1 1 calc R . . C35 C 0.3907(6) 0.3633(5) 0.8233(4) 0.055(2) Uani 1 1 d . . . H35A H 0.3819 0.3943 0.8476 0.066 Uiso 1 1 calc R . . C36 C 0.3166(6) 0.3332(4) 0.8272(3) 0.047(2) Uani 1 1 d . . . H36A H 0.2593 0.3405 0.8557 0.056 Uiso 1 1 calc R . . C37 C 0.3280(5) 0.2924(4) 0.7886(3) 0.0356(16) Uani 1 1 d . . . H37A H 0.2773 0.2722 0.7906 0.043 Uiso 1 1 calc R . . C38 C 0.4125(5) 0.2802(3) 0.7470(3) 0.0288(14) Uani 1 1 d . . . C39 C 0.7341(5) 0.1053(4) 0.4955(3) 0.0324(15) Uani 1 1 d . . . C40 C 0.7232(6) 0.1379(6) 0.4361(4) 0.063(3) Uani 1 1 d . . . H40A H 0.7535 0.1770 0.4222 0.095 Uiso 1 1 calc R . . H40B H 0.6531 0.1564 0.4338 0.095 Uiso 1 1 calc R . . H40C H 0.7559 0.1017 0.4130 0.095 Uiso 1 1 calc R . . C41 C 0.5829(4) 0.0399(3) 0.6961(2) 0.0225(13) Uani 1 1 d U . . C42 C 0.4961(6) 0.0392(4) 0.7425(3) 0.0421(18) Uani 1 1 d . . . H42A H 0.5124 -0.0038 0.7717 0.063 Uiso 1 1 calc R . . H42B H 0.4405 0.0394 0.7276 0.063 Uiso 1 1 calc R . . H42C H 0.4781 0.0816 0.7586 0.063 Uiso 1 1 calc R . . C43 C 0.5879(6) 0.2744(4) 0.5473(3) 0.0424(18) Uani 1 1 d . . . C44 C 0.5985(9) 0.3099(6) 0.4851(4) 0.076(3) Uani 1 1 d . . . H44A H 0.5730 0.3618 0.4812 0.113 Uiso 1 1 calc R . . H44B H 0.5612 0.2935 0.4668 0.113 Uiso 1 1 calc R . . H44C H 0.6682 0.2971 0.4673 0.113 Uiso 1 1 calc R . . C45 C 0.7396(5) 0.1089(4) 0.7002(3) 0.0307(15) Uani 1 1 d . . . C46 C 0.8260(6) 0.0604(5) 0.7264(4) 0.051(2) Uani 1 1 d . . . H46A H 0.8073 0.0534 0.7675 0.076 Uiso 1 1 calc R . . H46B H 0.8806 0.0819 0.7136 0.076 Uiso 1 1 calc R . . H46C H 0.8467 0.0142 0.7152 0.076 Uiso 1 1 calc R . . Cd3 Cd 0.93490(3) 0.36465(2) 0.949093(18) 0.02099(12) Uani 1 1 d . . . Cd4 Cd 0.83896(3) 0.20718(2) 1.029910(19) 0.02304(12) Uani 1 1 d . . . N9 N 0.7559(4) 0.2706(3) 1.1523(2) 0.0264(11) Uani 1 1 d . . . H9A H 0.8120 0.2386 1.1435 0.032 Uiso 1 1 calc R . . N10 N 0.8510(4) 0.4212(3) 1.0810(2) 0.0260(12) Uani 1 1 d . . . H10B H 0.8491 0.3878 1.0656 0.031 Uiso 1 1 calc R . . N11 N 0.8836(4) 0.4831(3) 0.9523(2) 0.0237(11) Uani 1 1 d . . . N12 N 0.9813(4) 0.4277(3) 0.8539(2) 0.0218(11) Uani 1 1 d . . . N13 N 1.0883(3) 0.2760(2) 0.8442(2) 0.0216(11) Uani 1 1 d . . . H13B H 1.1032 0.2826 0.8737 0.026 Uiso 1 1 calc R . . N14 N 1.0104(4) 0.1211(3) 0.9193(2) 0.0249(11) Uani 1 1 d . . . H14A H 0.9864 0.1640 0.9270 0.030 Uiso 1 1 calc R . . N15 N 0.8109(4) 0.1178(3) 1.0009(2) 0.0282(12) Uani 1 1 d . . . N16 N 0.7093(4) 0.1729(3) 1.0985(2) 0.0262(12) Uani 1 1 d . . . O9 O 1.1044(3) 0.3098(2) 0.93962(19) 0.0304(10) Uani 1 1 d . . . O10 O 1.0250(3) 0.3240(2) 1.0235(2) 0.0354(11) Uani 1 1 d . . . O11 O 0.8165(3) 0.3669(2) 0.89774(18) 0.0266(9) Uani 1 1 d . . . O12 O 0.9056(3) 0.2612(2) 0.93377(17) 0.0217(9) Uani 1 1 d . . . O13 O 0.9193(4) 0.1629(3) 1.1153(2) 0.0384(12) Uani 1 1 d . . . O14 O 1.0034(4) 0.1651(2) 1.0299(2) 0.0379(11) Uani 1 1 d . . . O15 O 0.8089(3) 0.3306(2) 1.02699(17) 0.0229(9) Uani 1 1 d . . . O16 O 0.6914(3) 0.3035(2) 1.00698(19) 0.0285(10) Uani 1 1 d . . . C47 C 0.6467(5) 0.2176(3) 1.1273(3) 0.0276(14) Uani 1 1 d . . . H47A H 0.5802 0.2167 1.1350 0.033 Uiso 1 1 calc R . . C48 C 0.6657(5) 0.2689(4) 1.1492(3) 0.0303(14) Uani 1 1 d . . . C49 C 0.5972(6) 0.3271(4) 1.1677(4) 0.0461(19) Uani 1 1 d . . . H49A H 0.5278 0.3387 1.1710 0.055 Uiso 1 1 calc R . . C50 C 0.6471(6) 0.3660(4) 1.1809(4) 0.0453(19) Uani 1 1 d . . . H50A H 0.6185 0.4093 1.1942 0.054 Uiso 1 1 calc R . . C51 C 0.7453(5) 0.3300(3) 1.1712(3) 0.0311(15) Uani 1 1 d . . . C52 C 0.8311(5) 0.3493(4) 1.1792(3) 0.0334(15) Uani 1 1 d . . . C53 C 0.8110(6) 0.3613(4) 1.2391(3) 0.0461(19) Uani 1 1 d . . . H53A H 0.8665 0.3734 1.2449 0.069 Uiso 1 1 calc R . . H53B H 0.8031 0.3176 1.2661 0.069 Uiso 1 1 calc R . . H53C H 0.7507 0.4004 1.2448 0.069 Uiso 1 1 calc R . . C54 C 0.9287(5) 0.2905(4) 1.1694(3) 0.0403(18) Uani 1 1 d . . . H54A H 0.9824 0.3051 1.1747 0.060 Uiso 1 1 calc R . . H54B H 0.9418 0.2829 1.1309 0.060 Uiso 1 1 calc R . . H54C H 0.9242 0.2461 1.1962 0.060 Uiso 1 1 calc R . . C55 C 0.8400(5) 0.4167(3) 1.1369(3) 0.0261(14) Uani 1 1 d . . . C56 C 0.8456(5) 0.4803(3) 1.1445(3) 0.0312(15) Uani 1 1 d . . . H56A H 0.8396 0.4922 1.1795 0.037 Uiso 1 1 calc R . . C57 C 0.8615(5) 0.5235(3) 1.0914(3) 0.0292(14) Uani 1 1 d . . . H57A H 0.8684 0.5701 1.0836 0.035 Uiso 1 1 calc R . . C58 C 0.8655(5) 0.4857(3) 1.0517(3) 0.0257(14) Uani 1 1 d . . . C59 C 0.8786(4) 0.5122(3) 0.9937(3) 0.0233(13) Uani 1 1 d . . . H59A H 0.8848 0.5592 0.9825 0.028 Uiso 1 1 calc R . . C60 C 0.8857(5) 0.5289(3) 0.8977(3) 0.0250(13) Uani 1 1 d . . . C61 C 0.8338(5) 0.6017(3) 0.8921(3) 0.0318(15) Uani 1 1 d . . . H61A H 0.7952 0.6197 0.9246 0.038 Uiso 1 1 calc R . . C62 C 0.8380(5) 0.6471(3) 0.8405(3) 0.0363(16) Uani 1 1 d . . . H62A H 0.8024 0.6962 0.8376 0.044 Uiso 1 1 calc R . . C63 C 0.8933(5) 0.6226(3) 0.7929(3) 0.0337(16) Uani 1 1 d . . . H63A H 0.8977 0.6546 0.7574 0.040 Uiso 1 1 calc R . . C64 C 0.9426(5) 0.5502(3) 0.7974(3) 0.0310(15) Uani 1 1 d . . . H64A H 0.9817 0.5329 0.7648 0.037 Uiso 1 1 calc R . . C65 C 0.9353(4) 0.5025(3) 0.8494(3) 0.0230(13) Uani 1 1 d . . . C66 C 0.9906(5) 0.4013(3) 0.8113(3) 0.0251(13) Uani 1 1 d . . . H66A H 0.9649 0.4333 0.7797 0.030 Uiso 1 1 calc R . . C67 C 1.0353(5) 0.3288(3) 0.8065(3) 0.0277(14) Uani 1 1 d . . . C68 C 1.0301(5) 0.2974(3) 0.7653(3) 0.0342(16) Uani 1 1 d . . . H68A H 0.9994 0.3210 0.7335 0.041 Uiso 1 1 calc R . . C69 C 1.0784(6) 0.2242(4) 0.7792(3) 0.0364(16) Uani 1 1 d . . . H69A H 1.0856 0.1892 0.7587 0.044 Uiso 1 1 calc R . . C70 C 1.1138(5) 0.2123(3) 0.8284(3) 0.0263(14) Uani 1 1 d . . . C71 C 1.1691(5) 0.1426(3) 0.8608(3) 0.0286(14) Uani 1 1 d . . . C72 C 1.2568(5) 0.1057(4) 0.8201(3) 0.0401(18) Uani 1 1 d . . . H72A H 1.3010 0.1358 0.8038 0.060 Uiso 1 1 calc R . . H72B H 1.2329 0.0980 0.7900 0.060 Uiso 1 1 calc R . . H72C H 1.2925 0.0596 0.8406 0.060 Uiso 1 1 calc R . . C73 C 1.2060(5) 0.1529(4) 0.9092(3) 0.0322(15) Uani 1 1 d . . . H73A H 1.1498 0.1767 0.9350 0.048 Uiso 1 1 calc R . . H73B H 1.2514 0.1823 0.8937 0.048 Uiso 1 1 calc R . . H73C H 1.2404 0.1063 0.9296 0.048 Uiso 1 1 calc R . . C74 C 1.0993(5) 0.0969(3) 0.8868(3) 0.0275(14) Uani 1 1 d . . . C75 C 1.1116(5) 0.0271(3) 0.8845(3) 0.0326(15) Uani 1 1 d . . . H75A H 1.1667 -0.0030 0.8647 0.039 Uiso 1 1 calc R . . C76 C 1.0271(6) 0.0099(3) 0.9171(3) 0.0386(17) Uani 1 1 d . . . H76A H 1.0148 -0.0348 0.9238 0.046 Uiso 1 1 calc R . . C77 C 0.9639(5) 0.0688(3) 0.9383(3) 0.0265(14) Uani 1 1 d . . . C78 C 0.8754(5) 0.0691(3) 0.9746(3) 0.0289(14) Uani 1 1 d . . . H78A H 0.8582 0.0261 0.9819 0.035 Uiso 1 1 calc R . . C79 C 0.7225(4) 0.1013(3) 1.0328(3) 0.0255(14) Uani 1 1 d . . . C80 C 0.6809(5) 0.0604(3) 1.0140(3) 0.0346(16) Uani 1 1 d . . . H80A H 0.7091 0.0470 0.9785 0.042 Uiso 1 1 calc R . . C81 C 0.6007(5) 0.0398(4) 1.0460(3) 0.0388(17) Uani 1 1 d . . . H81A H 0.5731 0.0128 1.0325 0.047 Uiso 1 1 calc R . . C82 C 0.5602(5) 0.0580(4) 1.0975(3) 0.0380(17) Uani 1 1 d . . . H82A H 0.5072 0.0410 1.1208 0.046 Uiso 1 1 calc R . . C83 C 0.5961(5) 0.1006(3) 1.1152(3) 0.0321(15) Uani 1 1 d . . . H83A H 0.5663 0.1138 1.1506 0.039 Uiso 1 1 calc R . . C84 C 0.6760(5) 0.1253(3) 1.0824(3) 0.0309(15) Uani 1 1 d . . . C85 C 1.1033(4) 0.3021(3) 0.9909(3) 0.0246(14) Uani 1 1 d . . . C86 C 1.1982(6) 0.2667(4) 1.0120(4) 0.0447(19) Uani 1 1 d . . . H86A H 1.1859 0.2623 1.0528 0.067 Uiso 1 1 calc R . . H86B H 1.2439 0.2954 0.9939 0.067 Uiso 1 1 calc R . . H86C H 1.2270 0.2191 1.0030 0.067 Uiso 1 1 calc R . . C87 C 0.8408(5) 0.3003(3) 0.9044(3) 0.0274(14) Uani 1 1 d . . . C88 C 0.7930(6) 0.2655(4) 0.8788(3) 0.0400(17) Uani 1 1 d . . . H88A H 0.8421 0.2239 0.8656 0.060 Uiso 1 1 calc R . . H88B H 0.7655 0.2996 0.8469 0.060 Uiso 1 1 calc R . . H88C H 0.7402 0.2502 0.9070 0.060 Uiso 1 1 calc R . . C89 C 0.9997(5) 0.1522(3) 1.0815(3) 0.0307(15) Uani 1 1 d . . . C90 C 1.0927(6) 0.1217(5) 1.1053(4) 0.049(2) Uani 1 1 d . . . H90A H 1.1008 0.1570 1.1222 0.074 Uiso 1 1 calc R . . H90B H 1.1491 0.1094 1.0752 0.074 Uiso 1 1 calc R . . H90C H 1.0888 0.0786 1.1342 0.074 Uiso 1 1 calc R . . C91 C 0.7223(5) 0.3482(3) 1.0156(3) 0.0276(14) Uani 1 1 d . . . C92 C 0.6621(5) 0.4245(3) 1.0119(3) 0.0387(17) Uani 1 1 d . . . H92A H 0.5963 0.4298 1.0060 0.058 Uiso 1 1 calc R . . H92B H 0.6941 0.4545 0.9802 0.058 Uiso 1 1 calc R . . H92C H 0.6564 0.4392 1.0469 0.058 Uiso 1 1 calc R . . Cl1 Cl 0.3489(2) -0.02121(14) 1.12107(13) 0.0747(7) Uani 1 1 d . . . Cl2 Cl 0.3315(3) -0.16064(16) 1.13208(11) 0.0849(9) Uani 1 1 d . . . Cl3 Cl 0.5226(2) -0.13764(17) 1.11089(15) 0.0891(9) Uani 1 1 d . . . Cl4 Cl 0.84075(17) -0.16906(12) 0.76216(9) 0.0586(6) Uani 1 1 d . . . Cl5 Cl 0.69442(17) -0.15197(13) 0.86258(10) 0.0637(6) Uani 1 1 d . . . Cl6 Cl 0.6518(2) -0.19038(17) 0.77270(11) 0.0807(8) Uani 1 1 d . . . Cl7 Cl 0.6145(2) 0.60857(14) 1.02817(13) 0.0898(10) Uani 1 1 d . A . Cl8 Cl 0.5818(3) 0.7111(4) 0.9229(2) 0.0930(18) Uani 0.60 1 d P A 1 Cl9 Cl 0.5032(6) 0.7492(4) 1.0289(4) 0.111(3) Uani 0.60 1 d P A 1 Cl8' Cl 0.5710(5) 0.6422(8) 0.9304(3) 0.118(4) Uani 0.40 1 d P A 2 Cl9' Cl 0.5221(8) 0.7572(5) 0.9870(6) 0.113(4) Uani 0.40 1 d P A 2 Cl10 Cl 0.2936(4) 0.5621(2) 1.23475(15) 0.1199(13) Uani 1 1 d . . . Cl11 Cl 0.4467(2) 0.53670(17) 1.13713(16) 0.0959(10) Uani 1 1 d . . . Cl12 Cl 0.3221(3) 0.44298(17) 1.1841(2) 0.1285(16) Uani 1 1 d . . . C1S C 0.4002(7) -0.1125(5) 1.1437(4) 0.055(2) Uani 1 1 d . . . H1SA H 0.3981 -0.1221 1.1852 0.066 Uiso 1 1 calc R . . C2S C 0.7151(6) -0.1411(4) 0.7887(4) 0.055(2) Uani 1 1 d . . . H2SA H 0.6885 -0.0895 0.7718 0.066 Uiso 1 1 calc R . . C3S C 0.5295(6) 0.6787(5) 0.9935(4) 0.056(2) Uani 1 1 d . . . H3SA H 0.4688 0.6655 0.9953 0.067 Uiso 1 1 calc R A 1 C4S C 0.3307(7) 0.5283(5) 1.1721(4) 0.063(3) Uani 1 1 d . . . H4SA H 0.2832 0.5592 1.1467 0.076 Uiso 1 1 calc R . . Cl15 Cl 1.1447(5) 0.4442(3) 0.3279(2) 0.0799(16) Uani 0.50 1 d PD B . Cl14 Cl 1.0906(6) 0.5721(3) 0.3678(2) 0.094(2) Uani 0.50 1 d PD B . Cl13 Cl 1.0185(11) 0.4550(7) 0.4301(6) 0.112(5) Uiso 0.25 1 d PD B 1 Cl23 Cl 1.0652(18) 0.4529(12) 0.4495(7) 0.162(8) Uiso 0.25 1 d PD B 2 C5S C 1.108(2) 0.4839(6) 0.3828(6) 0.124(12) Uani 0.50 1 d PD . . H5SA H 1.1659 0.4644 0.4024 0.149 Uiso 0.50 1 calc PR B 1 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cd1 0.0255(3) 0.0308(3) 0.0243(2) -0.00941(19) 0.00046(18) -0.0089(2) Cd2 0.0262(3) 0.0256(2) 0.0247(2) -0.00902(19) -0.00067(18) -0.00658(19) O1 0.072(4) 0.066(4) 0.053(4) 0.020(3) -0.036(3) -0.047(3) O2 0.034(3) 0.041(3) 0.036(3) -0.004(2) -0.005(2) -0.017(2) O3 0.029(3) 0.024(2) 0.030(2) -0.0050(19) -0.0018(19) -0.005(2) O4 0.027(2) 0.025(2) 0.019(2) 0.0009(17) 0.0030(17) -0.0199(18) O5 0.068(4) 0.050(3) 0.039(3) 0.000(3) -0.014(3) -0.032(3) O6 0.035(3) 0.055(3) 0.039(3) -0.002(2) -0.003(2) -0.025(2) O7 0.027(3) 0.040(3) 0.032(3) -0.012(2) -0.003(2) -0.007(2) O8 0.035(3) 0.031(2) 0.030(3) -0.010(2) -0.006(2) -0.009(2) N1 0.021(3) 0.039(3) 0.030(3) -0.015(2) -0.002(2) -0.010(2) N2 0.031(3) 0.037(3) 0.034(3) -0.015(3) 0.002(2) -0.013(3) N3 0.038(3) 0.028(3) 0.024(3) -0.006(2) 0.006(2) -0.016(3) N4 0.029(3) 0.037(3) 0.026(3) -0.010(2) -0.006(2) -0.006(2) N5 0.021(3) 0.050(4) 0.032(3) -0.017(3) 0.003(2) -0.012(3) N6 0.024(3) 0.043(3) 0.037(3) -0.012(3) -0.001(2) -0.017(3) N7 0.028(3) 0.031(3) 0.031(3) -0.016(2) 0.005(2) -0.014(2) N8 0.035(3) 0.023(3) 0.024(3) -0.008(2) -0.001(2) -0.011(2) C1 0.025(3) 0.032(4) 0.030(3) -0.015(3) 0.002(3) -0.006(3) C2 0.025(3) 0.042(4) 0.032(4) -0.018(3) 0.000(3) -0.008(3) C3 0.021(4) 0.075(6) 0.054(5) -0.039(5) -0.002(3) 0.001(4) C4 0.030(4) 0.081(6) 0.052(5) -0.040(5) -0.012(4) -0.009(4) C5 0.020(3) 0.053(4) 0.040(4) -0.023(3) -0.004(3) -0.007(3) C6 0.032(4) 0.059(5) 0.041(4) -0.031(4) -0.003(3) -0.011(4) C7 0.035(4) 0.094(7) 0.064(6) -0.050(5) -0.007(4) -0.021(4) C8 0.034(4) 0.059(5) 0.036(4) -0.023(4) -0.001(3) -0.007(4) C9 0.023(4) 0.052(4) 0.041(4) -0.026(4) 0.006(3) -0.018(3) C10 0.027(4) 0.069(6) 0.061(5) -0.023(4) 0.007(4) -0.026(4) C11 0.045(5) 0.056(5) 0.043(4) -0.005(4) 0.004(4) -0.034(4) C12 0.037(4) 0.042(4) 0.034(4) -0.018(3) 0.000(3) -0.018(3) C13 0.043(4) 0.039(4) 0.031(4) -0.014(3) 0.002(3) -0.018(3) C14 0.038(4) 0.031(4) 0.022(3) -0.006(3) 0.003(3) -0.005(3) C15 0.064(6) 0.038(4) 0.035(4) -0.008(3) -0.002(4) -0.009(4) C16 0.071(6) 0.030(4) 0.042(5) -0.006(3) 0.001(4) 0.000(4) C17 0.053(5) 0.041(5) 0.043(5) -0.002(4) -0.004(4) 0.012(4) C18 0.034(4) 0.046(5) 0.041(4) -0.008(4) 0.003(3) -0.007(3) C19 0.037(4) 0.032(4) 0.026(4) -0.008(3) -0.001(3) 0.000(3) C20 0.021(3) 0.041(4) 0.027(3) -0.011(3) 0.002(3) -0.008(3) C21 0.030(4) 0.042(4) 0.030(4) -0.013(3) -0.004(3) -0.013(3) C22 0.022(4) 0.062(5) 0.034(4) -0.021(4) 0.005(3) -0.013(3) C23 0.028(4) 0.050(4) 0.029(4) -0.010(3) 0.003(3) -0.018(3) C24 0.028(4) 0.046(4) 0.022(3) -0.005(3) 0.001(3) -0.019(3) C25 0.036(4) 0.048(4) 0.038(4) -0.016(3) 0.002(3) -0.017(3) C26 0.041(5) 0.058(5) 0.054(5) -0.019(4) 0.015(4) -0.028(4) C27 0.051(5) 0.053(5) 0.036(4) -0.008(4) -0.003(4) -0.010(4) C28 0.029(4) 0.037(4) 0.044(4) -0.014(3) 0.004(3) -0.021(3) C29 0.029(4) 0.060(5) 0.048(5) -0.027(4) -0.002(3) -0.009(4) C30 0.041(4) 0.059(5) 0.038(4) -0.021(4) -0.004(3) -0.020(4) C31 0.047(4) 0.037(4) 0.037(4) -0.018(3) -0.007(3) -0.014(3) C32 0.037(4) 0.037(4) 0.034(4) -0.017(3) 0.004(3) -0.018(3) C33 0.031(4) 0.036(4) 0.031(4) -0.015(3) 0.011(3) -0.015(3) C34 0.036(4) 0.058(5) 0.062(5) -0.045(4) 0.004(4) -0.013(4) C35 0.046(5) 0.072(6) 0.065(6) -0.056(5) 0.004(4) -0.015(4) C36 0.041(4) 0.060(5) 0.046(5) -0.033(4) 0.008(4) -0.016(4) C37 0.037(4) 0.035(4) 0.039(4) -0.016(3) -0.004(3) -0.011(3) C38 0.029(4) 0.024(3) 0.036(4) -0.013(3) -0.002(3) -0.009(3) C39 0.029(4) 0.038(4) 0.025(3) -0.003(3) -0.001(3) -0.009(3) C40 0.042(5) 0.092(7) 0.044(5) 0.014(5) -0.006(4) -0.029(5) C41 0.025(3) 0.025(3) 0.018(3) -0.001(2) 0.010(2) -0.020(2) C42 0.042(4) 0.051(5) 0.026(4) -0.011(3) 0.006(3) -0.012(4) C43 0.048(5) 0.046(5) 0.033(4) -0.009(3) -0.008(3) -0.012(4) C44 0.101(9) 0.085(7) 0.043(5) 0.007(5) -0.021(5) -0.040(7) C45 0.029(4) 0.033(4) 0.034(4) -0.011(3) -0.003(3) -0.013(3) C46 0.037(4) 0.058(5) 0.052(5) -0.016(4) -0.015(4) 0.001(4) Cd3 0.0225(2) 0.0137(2) 0.0263(2) -0.00422(17) -0.00433(18) -0.00472(17) Cd4 0.0231(2) 0.0156(2) 0.0292(3) -0.00307(18) -0.00281(18) -0.00686(18) N9 0.025(3) 0.023(3) 0.028(3) -0.007(2) -0.001(2) -0.006(2) N10 0.038(3) 0.016(2) 0.030(3) -0.009(2) -0.008(2) -0.009(2) N11 0.023(3) 0.018(2) 0.030(3) -0.008(2) -0.010(2) -0.001(2) N12 0.019(3) 0.019(2) 0.024(3) -0.001(2) -0.001(2) -0.006(2) N13 0.019(3) 0.020(2) 0.027(3) -0.008(2) -0.001(2) -0.006(2) N14 0.026(3) 0.012(2) 0.033(3) -0.008(2) 0.004(2) -0.006(2) N15 0.036(3) 0.016(3) 0.033(3) -0.006(2) -0.012(2) -0.005(2) N16 0.031(3) 0.015(2) 0.028(3) 0.000(2) -0.003(2) -0.007(2) O9 0.034(3) 0.023(2) 0.034(3) -0.0087(19) -0.010(2) -0.0022(19) O10 0.025(3) 0.037(3) 0.036(3) -0.004(2) -0.002(2) -0.004(2) O11 0.028(2) 0.019(2) 0.032(2) -0.0011(18) -0.0048(19) -0.0102(18) O12 0.018(2) 0.016(2) 0.030(2) -0.0052(17) 0.0005(18) -0.0073(17) O13 0.031(3) 0.035(3) 0.053(3) -0.019(2) -0.006(2) -0.007(2) O14 0.039(3) 0.032(3) 0.041(3) -0.002(2) -0.014(2) -0.007(2) O15 0.029(2) 0.0124(19) 0.023(2) -0.0009(16) -0.0018(18) -0.0059(17) O16 0.029(2) 0.018(2) 0.036(3) -0.0049(19) -0.007(2) -0.0046(18) C47 0.020(3) 0.028(3) 0.036(4) 0.002(3) -0.001(3) -0.019(3) C48 0.026(4) 0.034(4) 0.032(4) -0.010(3) -0.003(3) -0.010(3) C49 0.028(4) 0.044(4) 0.067(5) -0.026(4) -0.004(4) -0.004(3) C50 0.039(4) 0.033(4) 0.065(5) -0.025(4) 0.000(4) -0.007(3) C51 0.039(4) 0.024(3) 0.028(3) -0.004(3) -0.004(3) -0.009(3) C52 0.040(4) 0.030(4) 0.033(4) -0.006(3) -0.008(3) -0.013(3) C53 0.062(5) 0.052(5) 0.033(4) -0.008(3) -0.010(4) -0.026(4) C54 0.040(4) 0.029(4) 0.056(5) 0.001(3) -0.023(4) -0.012(3) C55 0.028(3) 0.022(3) 0.028(3) -0.004(3) -0.006(3) -0.008(3) C56 0.035(4) 0.028(3) 0.034(4) -0.014(3) -0.007(3) -0.008(3) C57 0.034(4) 0.019(3) 0.036(4) -0.013(3) -0.005(3) -0.005(3) C58 0.022(3) 0.020(3) 0.035(4) -0.012(3) -0.008(3) 0.001(2) C59 0.018(3) 0.016(3) 0.036(4) -0.012(3) -0.004(3) -0.001(2) C60 0.028(3) 0.017(3) 0.030(3) -0.005(3) -0.008(3) -0.005(3) C61 0.045(4) 0.013(3) 0.033(4) -0.006(3) -0.009(3) 0.000(3) C62 0.040(4) 0.017(3) 0.047(4) -0.002(3) -0.012(3) -0.002(3) C63 0.043(4) 0.021(3) 0.034(4) 0.006(3) -0.009(3) -0.014(3) C64 0.033(4) 0.025(3) 0.031(4) -0.005(3) -0.006(3) -0.005(3) C65 0.020(3) 0.016(3) 0.032(3) -0.003(2) -0.002(3) -0.008(2) C66 0.026(3) 0.021(3) 0.024(3) -0.003(3) -0.002(3) -0.006(3) C67 0.038(4) 0.020(3) 0.024(3) -0.007(3) -0.002(3) -0.007(3) C68 0.042(4) 0.027(3) 0.030(4) -0.005(3) -0.002(3) -0.010(3) C69 0.050(5) 0.029(4) 0.030(4) -0.015(3) 0.003(3) -0.012(3) C70 0.026(3) 0.015(3) 0.030(3) -0.008(3) 0.011(3) -0.007(3) C71 0.023(3) 0.019(3) 0.037(4) -0.008(3) 0.006(3) -0.004(3) C72 0.033(4) 0.027(4) 0.051(5) -0.016(3) 0.009(3) -0.002(3) C73 0.020(3) 0.028(3) 0.045(4) -0.005(3) -0.002(3) -0.008(3) C74 0.033(4) 0.013(3) 0.032(4) 0.002(3) -0.008(3) -0.003(3) C75 0.042(4) 0.016(3) 0.032(4) -0.005(3) -0.002(3) -0.001(3) C76 0.057(5) 0.018(3) 0.042(4) -0.006(3) -0.006(4) -0.013(3) C77 0.034(4) 0.017(3) 0.027(3) 0.001(2) 0.000(3) -0.013(3) C78 0.032(4) 0.019(3) 0.038(4) -0.006(3) -0.001(3) -0.015(3) C79 0.019(3) 0.023(3) 0.035(4) 0.008(3) -0.005(3) -0.017(3) C80 0.042(4) 0.025(3) 0.041(4) -0.001(3) -0.015(3) -0.014(3) C81 0.034(4) 0.031(4) 0.058(5) 0.003(3) -0.013(4) -0.024(3) C82 0.034(4) 0.027(4) 0.052(5) 0.003(3) -0.010(3) -0.016(3) C83 0.025(3) 0.029(3) 0.036(4) 0.001(3) 0.004(3) -0.014(3) C84 0.033(4) 0.024(3) 0.035(4) -0.003(3) -0.016(3) -0.003(3) C85 0.022(3) 0.017(3) 0.036(4) -0.001(3) -0.008(3) -0.010(3) C86 0.043(5) 0.033(4) 0.063(5) -0.010(4) -0.030(4) -0.002(3) C87 0.035(4) 0.023(3) 0.023(3) -0.006(3) 0.001(3) -0.010(3) C88 0.051(5) 0.035(4) 0.045(4) -0.009(3) -0.017(4) -0.020(3) C89 0.023(4) 0.019(3) 0.056(5) -0.009(3) -0.011(3) -0.011(3) C90 0.031(4) 0.055(5) 0.060(5) -0.005(4) -0.020(4) -0.008(4) C91 0.034(4) 0.018(3) 0.027(3) -0.009(3) -0.010(3) 0.004(3) C92 0.031(4) 0.021(3) 0.058(5) -0.005(3) -0.008(3) -0.002(3) Cl1 0.0760(17) 0.0636(15) 0.101(2) -0.0247(14) -0.0216(15) -0.0303(13) Cl2 0.133(3) 0.0937(19) 0.0657(16) 0.0005(14) -0.0289(16) -0.086(2) Cl3 0.0680(18) 0.0823(19) 0.110(2) -0.0202(17) -0.0013(16) -0.0230(15) Cl4 0.0537(13) 0.0632(13) 0.0437(11) 0.0007(10) 0.0031(9) -0.0161(11) Cl5 0.0533(13) 0.0650(14) 0.0629(14) -0.0245(12) 0.0023(11) -0.0053(11) Cl6 0.0874(19) 0.105(2) 0.0587(15) 0.0146(14) -0.0343(14) -0.0491(17) Cl7 0.0722(17) 0.0504(14) 0.101(2) 0.0161(14) 0.0064(15) -0.0015(12) Cl8 0.038(2) 0.126(4) 0.072(3) 0.028(3) -0.012(2) -0.006(3) Cl9 0.082(4) 0.078(5) 0.199(8) -0.098(6) -0.053(6) 0.021(3) Cl8' 0.047(4) 0.232(13) 0.067(5) -0.065(7) -0.012(3) -0.003(6) Cl9' 0.082(7) 0.047(4) 0.210(13) 0.016(7) -0.073(9) -0.017(4) Cl10 0.175(4) 0.123(3) 0.074(2) -0.017(2) -0.011(2) -0.070(3) Cl11 0.0667(18) 0.085(2) 0.137(3) -0.0206(19) -0.0173(18) -0.0260(15) Cl12 0.080(2) 0.0627(18) 0.252(5) -0.042(2) -0.036(3) -0.0212(16) C1S 0.070(6) 0.075(6) 0.039(4) -0.009(4) -0.003(4) -0.052(5) C2S 0.049(5) 0.037(4) 0.060(5) 0.014(4) -0.017(4) -0.003(4) C3S 0.035(5) 0.070(6) 0.070(6) -0.029(5) -0.008(4) -0.014(4) C4S 0.051(5) 0.053(5) 0.088(7) -0.008(5) -0.039(5) -0.004(4) Cl15 0.103(4) 0.066(3) 0.076(3) -0.022(3) 0.004(3) -0.040(3) Cl14 0.167(6) 0.042(3) 0.072(3) -0.011(2) -0.048(4) -0.009(3) C5S 0.22(4) 0.064(15) 0.060(15) 0.014(12) -0.016(19) -0.040(19) _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 O2 2.283(5) . ? Cd1 N4 2.301(5) . ? Cd1 O8 2.391(4) . ? Cd1 N3 2.399(5) . ? Cd1 O3 2.418(4) . ? Cd1 O1 2.451(5) . ? Cd1 O4 2.473(4) . ? Cd1 C39 2.721(7) . ? Cd2 N8 2.294(5) . ? Cd2 O5 2.317(5) . ? Cd2 O7 2.357(5) . ? Cd2 O6 2.374(5) . ? Cd2 N7 2.393(5) . ? Cd2 O4 2.434(4) . ? Cd2 O8 2.491(5) . ? Cd2 C43 2.693(8) . ? O1 C39 1.220(9) . ? O2 C39 1.267(8) . ? O3 C41 1.255(8) . ? O4 C41 1.280(7) . ? O5 C43 1.239(9) . ? O6 C43 1.252(9) . ? O7 C45 1.231(8) . ? O8 C45 1.272(8) . ? N1 C5 1.358(8) . ? N1 C2 1.368(8) . ? N2 C9 1.349(9) . ? N2 C12 1.374(9) . ? N3 C13 1.303(9) . ? N3 C14 1.395(9) . ? N4 C20 1.331(8) . ? N4 C19 1.425(9) . ? N5 C24 1.357(9) . ? N5 C21 1.372(9) . ? N6 C28 1.337(9) . ? N6 C31 1.377(9) . ? N7 C32 1.308(9) . ? N7 C33 1.413(8) . ? N8 C1 1.299(8) . ? N8 C38 1.438(8) . ? C1 C2 1.423(9) . ? C2 C3 1.385(10) . ? C3 C4 1.392(11) . ? C4 C5 1.386(10) . ? C5 C6 1.514(9) . ? C6 C9 1.488(11) . ? C6 C8 1.541(11) . ? C6 C7 1.551(10) . ? C9 C10 1.385(11) . ? C10 C11 1.393(12) . ? C11 C12 1.386(10) . ? C12 C13 1.408(10) . ? C14 C15 1.408(10) . ? C14 C19 1.423(10) . ? C15 C16 1.363(12) . ? C16 C17 1.390(13) . ? C17 C18 1.370(12) . ? C18 C19 1.388(10) . ? C20 C21 1.395(10) . ? C21 C22 1.395(10) . ? C22 C23 1.389(11) . ? C23 C24 1.378(9) . ? C24 C25 1.509(10) . ? C25 C28 1.524(10) . ? C25 C26 1.541(10) . ? C25 C27 1.544(11) . ? C28 C29 1.380(10) . ? C29 C30 1.381(10) . ? C30 C31 1.391(11) . ? C31 C32 1.421(10) . ? C33 C38 1.390(9) . ? C33 C34 1.407(9) . ? C34 C35 1.361(11) . ? C35 C36 1.390(11) . ? C36 C37 1.385(10) . ? C37 C38 1.398(9) . ? C39 C40 1.486(10) . ? C41 C42 1.488(9) . ? C43 C44 1.524(11) . ? C45 C46 1.499(10) . ? Cd3 N11 2.286(5) . ? Cd3 O9 2.336(4) . ? Cd3 O10 2.372(5) . ? Cd3 O11 2.401(4) . ? Cd3 N12 2.429(5) . ? Cd3 O12 2.431(4) . ? Cd3 O15 2.444(4) . ? Cd3 C85 2.706(6) . ? Cd4 O14 2.272(5) . ? Cd4 N15 2.324(5) . ? Cd4 N16 2.370(5) . ? Cd4 O15 2.383(4) . ? Cd4 O16 2.455(4) . ? Cd4 O12 2.459(4) . ? Cd4 O13 2.518(5) . ? Cd4 C89 2.739(7) . ? N9 C48 1.359(8) . ? N9 C51 1.363(8) . ? N10 C55 1.353(8) . ? N10 C58 1.373(8) . ? N11 C59 1.308(8) . ? N11 C60 1.432(8) . ? N12 C66 1.282(8) . ? N12 C65 1.427(7) . ? N13 C70 1.363(7) . ? N13 C67 1.384(8) . ? N14 C74 1.358(8) . ? N14 C77 1.367(8) . ? N15 C78 1.309(8) . ? N15 C79 1.429(8) . ? N16 C47 1.283(8) . ? N16 C84 1.406(8) . ? O9 C85 1.251(8) . ? O10 C85 1.246(8) . ? O11 C87 1.252(7) . ? O12 C87 1.271(8) . ? O13 C89 1.253(8) . ? O14 C89 1.240(9) . ? O15 C91 1.285(8) . ? O16 C91 1.234(8) . ? C47 C48 1.435(9) . ? C48 C49 1.372(10) . ? C49 C50 1.392(11) . ? C50 C51 1.369(10) . ? C51 C52 1.514(10) . ? C52 C55 1.509(9) . ? C52 C53 1.528(10) . ? C52 C54 1.537(10) . ? C55 C56 1.390(9) . ? C56 C57 1.393(10) . ? C57 C58 1.396(9) . ? C58 C59 1.393(9) . ? C60 C65 1.386(9) . ? C60 C61 1.406(8) . ? C61 C62 1.372(10) . ? C62 C63 1.374(10) . ? C63 C64 1.392(9) . ? C64 C65 1.400(9) . ? C66 C67 1.421(8) . ? C67 C68 1.387(9) . ? C68 C69 1.404(10) . ? C69 C70 1.393(10) . ? C70 C71 1.506(9) . ? C71 C74 1.519(9) . ? C71 C72 1.533(9) . ? C71 C73 1.540(10) . ? C74 C75 1.383(9) . ? C75 C76 1.393(10) . ? C76 C77 1.386(9) . ? C77 C78 1.378(9) . ? C79 C84 1.388(9) . ? C79 C80 1.415(9) . ? C80 C81 1.365(10) . ? C81 C82 1.371(11) . ? C82 C83 1.368(10) . ? C83 C84 1.407(9) . ? C85 C86 1.495(9) . ? C87 C88 1.493(9) . ? C89 C90 1.502(9) . ? C91 C92 1.494(8) . ? Cl1 C1S 1.743(10) . ? Cl2 C1S 1.744(8) . ? Cl3 C1S 1.735(10) . ? Cl4 C2S 1.740(9) . ? Cl5 C2S 1.766(9) . ? Cl6 C2S 1.754(10) . ? Cl7 C3S 1.742(9) . ? Cl8 C3S 1.779(11) . ? Cl9 C3S 1.774(10) . ? Cl8' C3S 1.809(12) . ? Cl9' C3S 1.530(14) . ? Cl10 C4S 1.774(11) . ? Cl11 C4S 1.743(11) . ? Cl12 C4S 1.721(10) . ? Cl15 C5S 1.666(9) . ? Cl14 C5S 1.672(9) . ? Cl13 C5S 1.680(10) . ? Cl23 C5S 1.657(10) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Cd1 N4 115.85(18) . . ? O2 Cd1 O8 123.78(16) . . ? N4 Cd1 O8 97.10(17) . . ? O2 Cd1 N3 83.45(18) . . ? N4 Cd1 N3 73.0(2) . . ? O8 Cd1 N3 152.07(17) . . ? O2 Cd1 O3 129.48(16) . . ? N4 Cd1 O3 101.23(17) . . ? O8 Cd1 O3 81.00(15) . . ? N3 Cd1 O3 75.69(16) . . ? O2 Cd1 O1 54.21(17) . . ? N4 Cd1 O1 92.9(2) . . ? O8 Cd1 O1 81.57(18) . . ? N3 Cd1 O1 124.1(2) . . ? O3 Cd1 O1 158.76(19) . . ? O2 Cd1 O4 90.10(15) . . ? N4 Cd1 O4 152.85(16) . . ? O8 Cd1 O4 72.59(14) . . ? N3 Cd1 O4 104.20(16) . . ? O3 Cd1 O4 53.02(14) . . ? O1 Cd1 O4 109.77(18) . . ? O2 Cd1 C39 27.59(19) . . ? N4 Cd1 C39 105.8(2) . . ? O8 Cd1 C39 102.80(19) . . ? N3 Cd1 C39 105.0(2) . . ? O3 Cd1 C39 151.92(18) . . ? O1 Cd1 C39 26.62(19) . . ? O4 Cd1 C39 101.02(17) . . ? N8 Cd2 O5 101.9(2) . . ? N8 Cd2 O7 100.62(17) . . ? O5 Cd2 O7 148.79(18) . . ? N8 Cd2 O6 112.81(18) . . ? O5 Cd2 O6 55.02(18) . . ? O7 Cd2 O6 132.03(17) . . ? N8 Cd2 N7 73.40(18) . . ? O5 Cd2 N7 131.50(19) . . ? O7 Cd2 N7 75.89(18) . . ? O6 Cd2 N7 81.71(18) . . ? N8 Cd2 O4 96.63(16) . . ? O5 Cd2 O4 77.32(16) . . ? O7 Cd2 O4 78.89(15) . . ? O6 Cd2 O4 127.26(16) . . ? N7 Cd2 O4 150.44(16) . . ? N8 Cd2 O8 152.32(17) . . ? O5 Cd2 O8 99.74(18) . . ? O7 Cd2 O8 53.23(15) . . ? O6 Cd2 O8 93.72(16) . . ? N7 Cd2 O8 104.28(17) . . ? O4 Cd2 O8 71.56(14) . . ? N8 Cd2 C43 109.8(2) . . ? O5 Cd2 C43 27.3(2) . . ? O7 Cd2 C43 149.1(2) . . ? O6 Cd2 C43 27.7(2) . . ? N7 Cd2 C43 107.3(2) . . ? O4 Cd2 C43 102.30(19) . . ? O8 Cd2 C43 97.3(2) . . ? C39 O1 Cd1 89.1(4) . . ? C39 O2 Cd1 95.8(4) . . ? C41 O3 Cd1 95.4(3) . . ? C41 O4 Cd2 117.8(4) . . ? C41 O4 Cd1 92.2(3) . . ? Cd2 O4 Cd1 102.80(14) . . ? C43 O5 Cd2 93.5(4) . . ? C43 O6 Cd2 90.5(5) . . ? C45 O7 Cd2 96.6(4) . . ? C45 O8 Cd1 115.2(4) . . ? C45 O8 Cd2 89.3(4) . . ? Cd1 O8 Cd2 103.51(17) . . ? C5 N1 C2 109.3(5) . . ? C9 N2 C12 110.7(6) . . ? C13 N3 C14 117.5(6) . . ? C13 N3 Cd1 120.8(5) . . ? C14 N3 Cd1 112.5(4) . . ? C20 N4 C19 115.6(6) . . ? C20 N4 Cd1 125.5(5) . . ? C19 N4 Cd1 114.4(4) . . ? C24 N5 C21 109.7(6) . . ? C28 N6 C31 109.5(6) . . ? C32 N7 C33 117.7(6) . . ? C32 N7 Cd2 120.4(4) . . ? C33 N7 Cd2 112.0(4) . . ? C1 N8 C38 115.3(5) . . ? C1 N8 Cd2 128.7(4) . . ? C38 N8 Cd2 113.4(4) . . ? N8 C1 C2 129.7(6) . . ? N1 C2 C3 107.6(6) . . ? N1 C2 C1 128.6(6) . . ? C3 C2 C1 123.7(6) . . ? C2 C3 C4 107.6(6) . . ? C5 C4 C3 107.3(6) . . ? N1 C5 C4 108.1(6) . . ? N1 C5 C6 121.3(6) . . ? C4 C5 C6 130.4(6) . . ? C9 C6 C5 109.3(6) . . ? C9 C6 C8 113.1(6) . . ? C5 C6 C8 109.7(6) . . ? C9 C6 C7 108.3(7) . . ? C5 C6 C7 108.0(6) . . ? C8 C6 C7 108.3(6) . . ? N2 C9 C10 106.6(7) . . ? N2 C9 C6 123.7(7) . . ? C10 C9 C6 129.7(7) . . ? C9 C10 C11 108.8(7) . . ? C12 C11 C10 106.8(7) . . ? N2 C12 C11 107.1(7) . . ? N2 C12 C13 126.2(6) . . ? C11 C12 C13 126.7(7) . . ? N3 C13 C12 127.9(7) . . ? N3 C14 C15 124.1(7) . . ? N3 C14 C19 119.0(6) . . ? C15 C14 C19 116.9(7) . . ? C16 C15 C14 122.7(9) . . ? C15 C16 C17 119.3(8) . . ? C18 C17 C16 120.0(8) . . ? C17 C18 C19 121.5(8) . . ? C18 C19 C14 119.2(7) . . ? C18 C19 N4 121.5(7) . . ? C14 C19 N4 119.3(6) . . ? N4 C20 C21 130.3(6) . . ? N5 C21 C22 106.6(6) . . ? N5 C21 C20 128.6(6) . . ? C22 C21 C20 124.8(7) . . ? C23 C22 C21 108.0(6) . . ? C24 C23 C22 107.5(6) . . ? N5 C24 C23 108.2(6) . . ? N5 C24 C25 122.3(6) . . ? C23 C24 C25 129.3(6) . . ? C24 C25 C28 109.8(6) . . ? C24 C25 C26 110.4(6) . . ? C28 C25 C26 108.9(6) . . ? C24 C25 C27 106.7(6) . . ? C28 C25 C27 111.7(6) . . ? C26 C25 C27 109.4(7) . . ? N6 C28 C29 108.8(6) . . ? N6 C28 C25 122.9(6) . . ? C29 C28 C25 128.3(6) . . ? C28 C29 C30 107.3(7) . . ? C29 C30 C31 107.8(7) . . ? N6 C31 C30 106.7(6) . . ? N6 C31 C32 125.8(6) . . ? C30 C31 C32 127.4(7) . . ? N7 C32 C31 126.2(6) . . ? C38 C33 C34 119.3(6) . . ? C38 C33 N7 119.1(6) . . ? C34 C33 N7 121.5(6) . . ? C35 C34 C33 120.6(7) . . ? C34 C35 C36 120.9(7) . . ? C37 C36 C35 118.5(7) . . ? C36 C37 C38 121.6(7) . . ? C33 C38 C37 118.6(6) . . ? C33 C38 N8 120.1(6) . . ? C37 C38 N8 121.2(6) . . ? O1 C39 O2 120.8(6) . . ? O1 C39 C40 122.2(7) . . ? O2 C39 C40 116.9(7) . . ? O1 C39 Cd1 64.2(4) . . ? O2 C39 Cd1 56.6(3) . . ? C40 C39 Cd1 173.5(6) . . ? O3 C41 O4 119.0(5) . . ? O3 C41 C42 122.3(6) . . ? O4 C41 C42 118.7(6) . . ? O5 C43 O6 121.0(7) . . ? O5 C43 C44 120.4(7) . . ? O6 C43 C44 118.5(8) . . ? O5 C43 Cd2 59.2(4) . . ? O6 C43 Cd2 61.8(4) . . ? C44 C43 Cd2 176.9(7) . . ? O7 C45 O8 120.7(6) . . ? O7 C45 C46 120.5(6) . . ? O8 C45 C46 118.8(6) . . ? N11 Cd3 O9 116.18(17) . . ? N11 Cd3 O10 97.15(17) . . ? O9 Cd3 O10 54.91(15) . . ? N11 Cd3 O11 97.82(16) . . ? O9 Cd3 O11 131.39(15) . . ? O10 Cd3 O11 156.25(15) . . ? N11 Cd3 N12 73.82(17) . . ? O9 Cd3 N12 82.76(16) . . ? O10 Cd3 N12 127.91(17) . . ? O11 Cd3 N12 74.23(15) . . ? N11 Cd3 O12 150.32(16) . . ? O9 Cd3 O12 92.06(14) . . ? O10 Cd3 O12 107.14(15) . . ? O11 Cd3 O12 53.94(14) . . ? N12 Cd3 O12 102.75(15) . . ? N11 Cd3 O15 96.08(16) . . ? O9 Cd3 O15 125.98(15) . . ? O10 Cd3 O15 80.38(15) . . ? O11 Cd3 O15 79.79(14) . . ? N12 Cd3 O15 150.31(15) . . ? O12 Cd3 O15 72.11(13) . . ? N11 Cd3 C85 108.83(17) . . ? O9 Cd3 C85 27.50(17) . . ? O10 Cd3 C85 27.41(17) . . ? O11 Cd3 C85 152.46(16) . . ? N12 Cd3 C85 106.16(18) . . ? O12 Cd3 C85 100.48(15) . . ? O15 Cd3 C85 103.52(17) . . ? O14 Cd4 N15 101.92(18) . . ? O14 Cd4 N16 128.36(18) . . ? N15 Cd4 N16 73.96(19) . . ? O14 Cd4 O15 101.33(16) . . ? N15 Cd4 O15 149.83(16) . . ? N16 Cd4 O15 105.55(16) . . ? O14 Cd4 O16 151.62(16) . . ? N15 Cd4 O16 98.30(16) . . ? N16 Cd4 O16 76.42(16) . . ? O15 Cd4 O16 53.75(14) . . ? O14 Cd4 O12 78.75(16) . . ? N15 Cd4 O12 93.38(16) . . ? N16 Cd4 O12 151.45(16) . . ? O15 Cd4 O12 72.65(13) . . ? O16 Cd4 O12 80.38(14) . . ? O14 Cd4 O13 53.77(17) . . ? N15 Cd4 O13 113.72(17) . . ? N16 Cd4 O13 80.21(17) . . ? O15 Cd4 O13 95.52(14) . . ? O16 Cd4 O13 132.85(15) . . ? O12 Cd4 O13 128.22(15) . . ? O14 Cd4 C89 26.61(19) . . ? N15 Cd4 C89 110.10(18) . . ? N16 Cd4 C89 105.0(2) . . ? O15 Cd4 C89 99.27(16) . . ? O16 Cd4 C89 150.92(17) . . ? O12 Cd4 C89 103.41(18) . . ? O13 Cd4 C89 27.16(19) . . ? C48 N9 C51 108.9(5) . . ? C55 N10 C58 110.1(5) . . ? C59 N11 C60 115.9(5) . . ? C59 N11 Cd3 128.3(4) . . ? C60 N11 Cd3 113.1(4) . . ? C66 N12 C65 117.5(5) . . ? C66 N12 Cd3 120.9(4) . . ? C65 N12 Cd3 110.0(4) . . ? C70 N13 C67 109.4(5) . . ? C74 N14 C77 109.9(5) . . ? C78 N15 C79 116.6(5) . . ? C78 N15 Cd4 127.8(4) . . ? C79 N15 Cd4 111.7(4) . . ? C47 N16 C84 118.6(6) . . ? C47 N16 Cd4 119.9(4) . . ? C84 N16 Cd4 112.0(4) . . ? C85 O9 Cd3 93.0(4) . . ? C85 O10 Cd3 91.4(4) . . ? C87 O11 Cd3 93.6(4) . . ? C87 O12 Cd3 91.8(3) . . ? C87 O12 Cd4 114.5(4) . . ? Cd3 O12 Cd4 101.70(15) . . ? C89 O13 Cd4 86.3(4) . . ? C89 O14 Cd4 98.2(4) . . ? C91 O15 Cd4 93.8(3) . . ? C91 O15 Cd3 115.6(4) . . ? Cd4 O15 Cd3 103.53(15) . . ? C91 O16 Cd4 91.7(4) . . ? N16 C47 C48 127.4(6) . . ? N9 C48 C49 107.7(6) . . ? N9 C48 C47 125.8(6) . . ? C49 C48 C47 126.4(6) . . ? C48 C49 C50 108.0(7) . . ? C51 C50 C49 107.0(6) . . ? N9 C51 C50 108.4(6) . . ? N9 C51 C52 123.3(6) . . ? C50 C51 C52 128.4(6) . . ? C55 C52 C51 108.1(5) . . ? C55 C52 C53 110.4(6) . . ? C51 C52 C53 108.8(6) . . ? C55 C52 C54 108.2(6) . . ? C51 C52 C54 111.9(5) . . ? C53 C52 C54 109.4(6) . . ? N10 C55 C56 107.8(6) . . ? N10 C55 C52 121.7(5) . . ? C56 C55 C52 130.3(6) . . ? C55 C56 C57 107.6(6) . . ? C56 C57 C58 107.5(6) . . ? N10 C58 C59 128.7(5) . . ? N10 C58 C57 107.0(6) . . ? C59 C58 C57 124.3(6) . . ? N11 C59 C58 130.7(6) . . ? C65 C60 C61 118.7(6) . . ? C65 C60 N11 121.4(5) . . ? C61 C60 N11 119.8(6) . . ? C62 C61 C60 120.8(6) . . ? C61 C62 C63 120.9(6) . . ? C62 C63 C64 118.9(6) . . ? C63 C64 C65 121.0(6) . . ? C60 C65 C64 119.3(5) . . ? C60 C65 N12 119.4(5) . . ? C64 C65 N12 121.3(5) . . ? N12 C66 C67 126.6(6) . . ? N13 C67 C68 107.6(5) . . ? N13 C67 C66 125.6(6) . . ? C68 C67 C66 126.7(6) . . ? C67 C68 C69 107.5(6) . . ? C70 C69 C68 107.5(6) . . ? N13 C70 C69 108.0(5) . . ? N13 C70 C71 123.9(6) . . ? C69 C70 C71 128.1(6) . . ? C70 C71 C74 108.2(5) . . ? C70 C71 C72 108.7(5) . . ? C74 C71 C72 110.5(5) . . ? C70 C71 C73 112.2(5) . . ? C74 C71 C73 107.6(5) . . ? C72 C71 C73 109.7(6) . . ? N14 C74 C75 108.4(6) . . ? N14 C74 C71 122.0(5) . . ? C75 C74 C71 129.6(6) . . ? C74 C75 C76 106.4(6) . . ? C77 C76 C75 108.9(6) . . ? N14 C77 C78 129.3(6) . . ? N14 C77 C76 106.4(6) . . ? C78 C77 C76 124.1(6) . . ? N15 C78 C77 131.8(6) . . ? C84 C79 C80 118.9(6) . . ? C84 C79 N15 120.8(6) . . ? C80 C79 N15 120.3(6) . . ? C81 C80 C79 121.0(7) . . ? C80 C81 C82 120.0(7) . . ? C83 C82 C81 120.0(7) . . ? C82 C83 C84 121.6(7) . . ? C79 C84 N16 119.8(6) . . ? C79 C84 C83 118.1(6) . . ? N16 C84 C83 122.0(6) . . ? O10 C85 O9 120.7(6) . . ? O10 C85 C86 120.9(6) . . ? O9 C85 C86 118.3(6) . . ? O10 C85 Cd3 61.2(3) . . ? O9 C85 Cd3 59.6(3) . . ? C86 C85 Cd3 177.9(5) . . ? O11 C87 O12 120.6(6) . . ? O11 C87 C88 120.7(6) . . ? O12 C87 C88 118.7(6) . . ? O14 C89 O13 121.7(6) . . ? O14 C89 C90 120.4(7) . . ? O13 C89 C90 117.9(7) . . ? O14 C89 Cd4 55.2(3) . . ? O13 C89 Cd4 66.5(4) . . ? C90 C89 Cd4 175.6(6) . . ? O16 C91 O15 120.5(5) . . ? O16 C91 C92 121.6(6) . . ? O15 C91 C92 117.9(6) . . ? Cl3 C1S Cl1 109.7(5) . . ? Cl3 C1S Cl2 112.3(5) . . ? Cl1 C1S Cl2 110.6(5) . . ? Cl4 C2S Cl6 111.3(5) . . ? Cl4 C2S Cl5 110.2(5) . . ? Cl6 C2S Cl5 108.2(5) . . ? Cl9' C3S Cl7 123.3(7) . . ? Cl7 C3S Cl9 104.4(5) . . ? Cl7 C3S Cl8 112.2(5) . . ? Cl9 C3S Cl8 105.1(7) . . ? Cl9' C3S Cl8' 117.5(9) . . ? Cl7 C3S Cl8' 91.9(5) . . ? Cl9 C3S Cl8' 151.6(8) . . ? Cl12 C4S Cl11 113.4(5) . . ? Cl12 C4S Cl10 112.0(6) . . ? Cl11 C4S Cl10 110.8(5) . . ? Cl23 C5S Cl15 129.5(10) . . ? Cl23 C5S Cl14 113.2(10) . . ? Cl15 C5S Cl14 116.1(8) . . ? Cl15 C5S Cl13 111.5(10) . . ? Cl14 C5S Cl13 115.6(11) . . ? _diffrn_measured_fraction_theta_max 0.968 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.968 _refine_diff_density_max 1.989 _refine_diff_density_min -1.104 _refine_diff_density_rms 0.138 data_znbzpr _database_code_depnum_ccdc_archive 'CCDC 274153' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C78 H88 Cl15 N12 O13 Zn3' _chemical_formula_weight 2129.46 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.124(2) _cell_length_b 14.423(2) _cell_length_c 27.710(4) _cell_angle_alpha 87.110(2) _cell_angle_beta 81.228(2) _cell_angle_gamma 80.730(2) _cell_volume 4724(2) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 4249 _cell_measurement_theta_min 2.3 _cell_measurement_theta_max 22.55 _exptl_crystal_description column _exptl_crystal_colour yellow _exptl_crystal_size_max 0.68 _exptl_crystal_size_mid 0.31 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.497 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2178 _exptl_absorpt_coefficient_mu 1.243 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.637 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details 'Bruker SADABS v2.03' _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 SMART APEX CCD area detector' _diffrn_measurement_method omega _diffrn_detector_area_resol_mean ? _diffrn_standards_number . _diffrn_standards_interval_count . _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 28736 _diffrn_reflns_av_R_equivalents 0.068 _diffrn_reflns_av_sigmaI/netI 0.1074 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 2.09 _diffrn_reflns_theta_max 23.26 _reflns_number_total 13539 _reflns_number_gt 7629 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART version 5.625 (Bruker, 2001)' _computing_cell_refinement 'Bruker SAINT version 6.36a (Bruker, 2000)' _computing_data_reduction 'Bruker SAINT; Bruker SHELXTL (Bruker, 2001)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material 'enCIFer (CCDC, 2003); PLATON (Spek, 2003)' _refine_special_details ; Weak dataset, 0.9 \%A limit applied. One CHCl3 disordered about C-H axis, modelled over 3 sites with occupancies 0.3, 0.35 and 0.35, and isotropic adps. ; _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^)+(0.1249P)^2^+13.7384P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 13537 _refine_ls_number_parameters 1094 _refine_ls_number_restraints 36 _refine_ls_R_factor_all 0.1449 _refine_ls_R_factor_gt 0.0788 _refine_ls_wR_factor_ref 0.2445 _refine_ls_wR_factor_gt 0.1990 _refine_ls_goodness_of_fit_ref 1.024 _refine_ls_restrained_S_all 1.050 _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 Zn1 Zn 1.21835(10) 0.44336(8) 0.26148(4) 0.0362(3) Uani 1 1 d . . . Zn2 Zn 0.88563(9) 0.91361(8) 0.39231(4) 0.0325(3) Uani 1 1 d . . . Zn3 Zn 1.23786(9) 0.92737(8) 0.07331(4) 0.0314(3) Uani 1 1 d . . . N1 N 1.1691(7) 0.3707(6) 0.2098(3) 0.0358(19) Uani 1 1 d . . . N2 N 1.1183(6) 0.3684(5) 0.3077(3) 0.0323(19) Uani 1 1 d . . . N3 N 1.1575(7) 0.5147(5) 0.3760(3) 0.0348(19) Uani 1 1 d . . . H3A H 1.2136 0.5125 0.3516 0.042 Uiso 1 1 calc R . . N4 N 1.0639(7) 0.7720(5) 0.4502(3) 0.036(2) Uani 1 1 d . . . H4A H 1.0267 0.7716 0.4253 0.043 Uiso 1 1 calc R . . N5 N 0.8643(6) 0.9262(5) 0.4661(3) 0.0321(19) Uani 1 1 d . . . N6 N 0.7535(7) 1.0184(6) 0.3955(3) 0.036(2) Uani 1 1 d . . . N7 N 0.7993(6) 1.0027(5) 0.2849(2) 0.0275(17) Uani 1 1 d . . . H7A H 0.8201 0.9461 0.2969 0.033 Uiso 1 1 calc R . . N8 N 0.9699(6) 1.0038(5) 0.1226(2) 0.0265(17) Uani 1 1 d . . . H8A H 1.0343 0.9802 0.1327 0.032 Uiso 1 1 calc R . . N9 N 1.1543(6) 1.0362(5) 0.0373(2) 0.0251(17) Uani 1 1 d . . . N10 N 1.3516(6) 0.9227(5) 0.0096(3) 0.0289(18) Uani 1 1 d . . . N11 N 1.4276(6) 0.7373(5) 0.0597(3) 0.0307(18) Uani 1 1 d . . . H11A H 1.3790 0.7710 0.0815 0.037 Uiso 1 1 calc R . . N12 N 1.3143(7) 0.4929(6) 0.1489(3) 0.037(2) Uani 1 1 d . . . H12A H 1.3405 0.4805 0.1768 0.044 Uiso 1 1 calc R . . C1 C 1.1157(8) 0.2958(7) 0.2313(3) 0.036(2) Uani 1 1 d . . . C2 C 1.0922(8) 0.2224(7) 0.2051(4) 0.042(3) Uani 1 1 d . . . H2A H 1.1086 0.2232 0.1704 0.050 Uiso 1 1 calc R . . C3 C 1.0457(8) 0.1499(8) 0.2293(4) 0.044(3) Uani 1 1 d . . . H3B H 1.0291 0.1010 0.2112 0.052 Uiso 1 1 calc R . . C4 C 1.0225(9) 0.1465(8) 0.2794(4) 0.047(3) Uani 1 1 d . . . H4B H 0.9889 0.0961 0.2957 0.056 Uiso 1 1 calc R . . C5 C 1.0480(8) 0.2162(7) 0.3061(4) 0.038(2) Uani 1 1 d . . . H5A H 1.0352 0.2123 0.3408 0.046 Uiso 1 1 calc R . . C6 C 1.0923(8) 0.2925(7) 0.2824(3) 0.033(2) Uani 1 1 d . . . C7 C 1.0609(8) 0.3878(7) 0.3508(3) 0.039(2) Uani 1 1 d . . . H7B H 1.0031 0.3513 0.3622 0.047 Uiso 1 1 calc R . . C8 C 1.0757(8) 0.4567(7) 0.3818(3) 0.036(2) Uani 1 1 d . . . C9 C 1.0048(8) 0.4832(7) 0.4250(3) 0.037(2) Uani 1 1 d . . . H9A H 0.9408 0.4555 0.4389 0.045 Uiso 1 1 calc R . . C10 C 1.0433(8) 0.5567(7) 0.4442(3) 0.036(2) Uani 1 1 d . . . H10A H 1.0101 0.5884 0.4734 0.044 Uiso 1 1 calc R . . C11 C 1.1386(8) 0.5758(6) 0.4135(3) 0.035(2) Uani 1 1 d . . . C12 C 1.2175(8) 0.6447(7) 0.4170(3) 0.034(2) Uani 1 1 d . . . C13 C 1.2427(9) 0.6970(7) 0.3679(3) 0.043(3) Uani 1 1 d . . . H13A H 1.1718 0.7299 0.3582 0.065 Uiso 1 1 calc R . . H13B H 1.2795 0.6517 0.3429 0.065 Uiso 1 1 calc R . . H13C H 1.2928 0.7426 0.3711 0.065 Uiso 1 1 calc R . . C14 C 1.3286(9) 0.5911(8) 0.4315(4) 0.052(3) Uani 1 1 d . . . H14A H 1.3127 0.5583 0.4631 0.078 Uiso 1 1 calc R . . H14B H 1.3803 0.6357 0.4342 0.078 Uiso 1 1 calc R . . H14C H 1.3634 0.5453 0.4066 0.078 Uiso 1 1 calc R . . C15 C 1.1625(8) 0.7149(7) 0.4553(3) 0.035(2) Uani 1 1 d . . . C16 C 1.1961(9) 0.7366(7) 0.4983(3) 0.043(3) Uani 1 1 d . . . H16A H 1.2621 0.7078 0.5111 0.052 Uiso 1 1 calc R . . C17 C 1.1144(9) 0.8095(7) 0.5197(3) 0.041(3) Uani 1 1 d . . . H17A H 1.0814 0.7893 0.5527 0.049 Uiso 1 1 calc R . . H17B H 1.1499 0.8657 0.5230 0.049 Uiso 1 1 calc R . . C18 C 1.0298(8) 0.8311(7) 0.4898(3) 0.035(2) Uani 1 1 d . . . C19 C 0.9335(8) 0.8983(7) 0.4970(3) 0.036(2) Uani 1 1 d . . . H19A H 0.9166 0.9269 0.5280 0.043 Uiso 1 1 calc R . . C20 C 0.7635(9) 0.9869(7) 0.4814(3) 0.037(2) Uani 1 1 d . . . C21 C 0.7135(10) 0.9998(8) 0.5307(3) 0.050(3) Uani 1 1 d . . . H21A H 0.7495 0.9664 0.5559 0.060 Uiso 1 1 calc R . . C22 C 0.6158(10) 1.0585(9) 0.5425(4) 0.064(4) Uani 1 1 d . . . H22A H 0.5870 1.0689 0.5760 0.077 Uiso 1 1 calc R . . C23 C 0.5564(9) 1.1039(8) 0.5069(4) 0.050(3) Uani 1 1 d . . . H23A H 0.4857 1.1427 0.5156 0.060 Uiso 1 1 calc R . . C24 C 0.6025(9) 1.0916(7) 0.4584(4) 0.045(3) Uani 1 1 d . . . H24A H 0.5633 1.1230 0.4335 0.055 Uiso 1 1 calc R . . C25 C 0.7043(8) 1.0343(7) 0.4455(3) 0.035(2) Uani 1 1 d . . . C26 C 0.7280(8) 1.0847(7) 0.3634(3) 0.035(2) Uani 1 1 d . . . H26A H 0.6878 1.1426 0.3760 0.042 Uiso 1 1 calc R . . C27 C 0.7535(8) 1.0800(7) 0.3119(3) 0.032(2) Uani 1 1 d . . . C28 C 0.7333(9) 1.1544(7) 0.2791(3) 0.042(3) Uani 1 1 d . . . H28A H 0.7005 1.2171 0.2871 0.050 Uiso 1 1 calc R . . C29 C 0.7697(8) 1.1207(7) 0.2326(3) 0.035(2) Uani 1 1 d . . . H29A H 0.7684 1.1568 0.2030 0.043 Uiso 1 1 calc R . . C30 C 0.8075(8) 1.0274(7) 0.2366(3) 0.030(2) Uani 1 1 d . . . C31 C 0.8505(8) 0.9525(7) 0.1983(3) 0.030(2) Uani 1 1 d . . . C32 C 0.9572(8) 0.8909(7) 0.2098(4) 0.042(3) Uani 1 1 d . . . H32A H 1.0164 0.9297 0.2103 0.062 Uiso 1 1 calc R . . H32B H 0.9824 0.8434 0.1847 0.062 Uiso 1 1 calc R . . H32C H 0.9419 0.8597 0.2418 0.062 Uiso 1 1 calc R . . C33 C 0.7586(9) 0.8903(7) 0.1984(3) 0.047(3) Uani 1 1 d . . . H33A H 0.7460 0.8581 0.2303 0.070 Uiso 1 1 calc R . . H33B H 0.7831 0.8436 0.1729 0.070 Uiso 1 1 calc R . . H33C H 0.6882 0.9295 0.1920 0.070 Uiso 1 1 calc R . . C34 C 0.8677(7) 1.0009(7) 0.1484(3) 0.029(2) Uani 1 1 d . . . C35 C 0.7868(8) 1.0441(7) 0.1202(3) 0.036(2) Uani 1 1 d . . . H35A H 0.7072 1.0512 0.1293 0.043 Uiso 1 1 calc R . . C36 C 0.8444(8) 1.0749(6) 0.0761(3) 0.033(2) Uani 1 1 d . . . H36A H 0.8109 1.1072 0.0499 0.039 Uiso 1 1 calc R . . C37 C 0.9600(8) 1.0495(7) 0.0777(3) 0.031(2) Uani 1 1 d . . . C38 C 1.0469(8) 1.0656(6) 0.0399(3) 0.031(2) Uani 1 1 d . . . H38A H 1.0239 1.1028 0.0128 0.037 Uiso 1 1 calc R . . C39 C 1.2291(8) 1.0678(7) -0.0030(3) 0.031(2) Uani 1 1 d . . . C40 C 1.2042(8) 1.1537(7) -0.0278(3) 0.035(2) Uani 1 1 d . . . H40A H 1.1347 1.1936 -0.0182 0.042 Uiso 1 1 calc R . . C41 C 1.2801(9) 1.1805(8) -0.0660(4) 0.043(3) Uani 1 1 d . . . H41A H 1.2629 1.2384 -0.0832 0.051 Uiso 1 1 calc R . . C42 C 1.3804(8) 1.1231(7) -0.0791(3) 0.036(2) Uani 1 1 d . . . H42A H 1.4324 1.1419 -0.1055 0.043 Uiso 1 1 calc R . . C43 C 1.4076(8) 1.0397(7) -0.0552(3) 0.032(2) Uani 1 1 d . . . H43A H 1.4787 1.0019 -0.0646 0.039 Uiso 1 1 calc R . . C44 C 1.3321(8) 1.0094(7) -0.0170(3) 0.030(2) Uani 1 1 d . . . C45 C 1.4226(9) 0.8538(7) -0.0095(3) 0.038(2) Uani 1 1 d . . . H45A H 1.4542 0.8629 -0.0426 0.045 Uiso 1 1 calc R . . C46 C 1.4594(8) 0.7665(7) 0.0123(3) 0.034(2) Uani 1 1 d . . . C47 C 1.5356(10) 0.6936(8) -0.0088(4) 0.059(3) Uani 1 1 d . . . H47A H 1.5723 0.6927 -0.0416 0.071 Uiso 1 1 calc R . . C48 C 1.5503(10) 0.6210(8) 0.0260(4) 0.057(3) Uani 1 1 d . . . H48A H 1.5990 0.5626 0.0214 0.068 Uiso 1 1 calc R . . C49 C 1.4811(8) 0.6502(7) 0.0681(3) 0.034(2) Uani 1 1 d . . . C50 C 1.4561(8) 0.5972(7) 0.1159(3) 0.034(2) Uani 1 1 d . . . C51 C 1.4263(10) 0.6652(8) 0.1596(3) 0.050(3) Uani 1 1 d . . . H51A H 1.3608 0.7122 0.1544 0.075 Uiso 1 1 calc R . . H51B H 1.4909 0.6970 0.1618 0.075 Uiso 1 1 calc R . . H51C H 1.4084 0.6293 0.1900 0.075 Uiso 1 1 calc R . . C52 C 1.5580(9) 0.5236(9) 0.1234(4) 0.060(3) Uani 1 1 d . . . H52A H 1.5756 0.4808 0.0959 0.091 Uiso 1 1 calc R . . H52B H 1.5406 0.4877 0.1538 0.091 Uiso 1 1 calc R . . H52C H 1.6232 0.5548 0.1253 0.091 Uiso 1 1 calc R . . C53 C 1.3562(8) 0.5498(7) 0.1127(3) 0.036(2) Uani 1 1 d . . . C54 C 1.2914(9) 0.5511(8) 0.0750(4) 0.048(3) Uani 1 1 d . . . H54A H 1.3005 0.5857 0.0449 0.058 Uiso 1 1 calc R . . C55 C 1.2118(9) 0.4933(8) 0.0894(3) 0.046(3) Uani 1 1 d . . . H55A H 1.1569 0.4801 0.0706 0.055 Uiso 1 1 calc R . . C56 C 1.2254(9) 0.4574(7) 0.1358(3) 0.037(2) Uani 1 1 d . . . C57 C 1.1616(8) 0.3951(7) 0.1642(4) 0.039(2) Uani 1 1 d . . . H57A H 1.1090 0.3688 0.1490 0.047 Uiso 1 1 calc R . . O1 O 1.3844(6) 0.4106(5) 0.2407(3) 0.053(2) Uani 1 1 d . . . O2 O 1.3805(7) 0.4438(6) 0.3176(3) 0.067(2) Uani 1 1 d . . . C58 C 1.4325(9) 0.4243(9) 0.2770(4) 0.051(3) Uani 1 1 d . . . C59 C 1.5590(10) 0.4193(12) 0.2663(5) 0.088(5) Uani 1 1 d . . . H59A H 1.5880 0.4317 0.2961 0.132 Uiso 1 1 calc R . . H59B H 1.5779 0.4664 0.2410 0.132 Uiso 1 1 calc R . . H59C H 1.5935 0.3565 0.2550 0.132 Uiso 1 1 calc R . . O3 O 1.2148(7) 0.5743(5) 0.2674(2) 0.052(2) Uani 1 1 d . . . O4 O 1.0816(8) 0.6097(7) 0.2216(4) 0.091(3) Uani 1 1 d . . . C60 C 1.1483(8) 0.6315(9) 0.2450(4) 0.045(3) Uani 1 1 d . . . C61 C 1.1660(9) 0.7343(7) 0.2446(4) 0.048(3) Uani 1 1 d . . . H61A H 1.1110 0.7732 0.2266 0.073 Uiso 1 1 calc R . . H61B H 1.2427 0.7400 0.2287 0.073 Uiso 1 1 calc R . . H61C H 1.1557 0.7556 0.2783 0.073 Uiso 1 1 calc R . . O5 O 0.8928(5) 0.7770(5) 0.3875(2) 0.0390(17) Uani 1 1 d . . . O6 O 0.8183(5) 0.8157(5) 0.3202(2) 0.0405(17) Uani 1 1 d . . . C62 C 0.8603(8) 0.7549(7) 0.3483(3) 0.033(2) Uani 1 1 d . . . C63 C 0.8762(10) 0.6524(7) 0.3378(4) 0.052(3) Uani 1 1 d . . . H63A H 0.8479 0.6441 0.3073 0.079 Uiso 1 1 calc R . . H63B H 0.8343 0.6195 0.3646 0.079 Uiso 1 1 calc R . . H63C H 0.9567 0.6263 0.3347 0.079 Uiso 1 1 calc R . . O7 O 1.0266(5) 0.9223(5) 0.3523(2) 0.0396(17) Uani 1 1 d . . . O8 O 1.0428(6) 1.0426(5) 0.3962(2) 0.051(2) Uani 1 1 d . . . C64 C 1.0831(8) 0.9824(8) 0.3656(3) 0.038(2) Uani 1 1 d . . . C65 C 1.2060(9) 0.9719(9) 0.3424(4) 0.058(3) Uani 1 1 d . . . H65A H 1.2425 1.0198 0.3549 0.088 Uiso 1 1 calc R . . H65B H 1.2104 0.9800 0.3069 0.088 Uiso 1 1 calc R . . H65C H 1.2447 0.9093 0.3504 0.088 Uiso 1 1 calc R . . O9 O 1.1892(6) 0.9932(5) 0.1491(3) 0.0514(19) Uani 1 1 d . . . O10 O 1.3526(5) 0.9100(5) 0.1231(2) 0.0486(19) Uani 1 1 d . . . C66 C 1.2830(9) 0.9543(7) 0.1568(3) 0.037(2) Uani 1 1 d . . . C67 C 1.3199(10) 0.9540(9) 0.2065(4) 0.060(3) Uani 1 1 d . . . H67A H 1.2882 1.0138 0.2222 0.089 Uiso 1 1 calc R . . H67B H 1.4026 0.9458 0.2028 0.089 Uiso 1 1 calc R . . H67C H 1.2930 0.9022 0.2268 0.089 Uiso 1 1 calc R . . O11 O 1.1663(6) 0.8207(5) 0.0990(2) 0.0418(17) Uani 1 1 d . . . O12 O 1.1168(6) 0.8044(5) 0.0273(2) 0.051(2) Uani 1 1 d . . . C68 C 1.1119(8) 0.7835(7) 0.0716(3) 0.033(2) Uani 1 1 d . . . C69 C 1.0374(9) 0.7168(8) 0.0948(4) 0.045(3) Uani 1 1 d . . . H69A H 1.0001 0.6932 0.0700 0.067 Uiso 1 1 calc R . . H69B H 0.9801 0.7490 0.1198 0.067 Uiso 1 1 calc R . . H69C H 1.0826 0.6640 0.1100 0.067 Uiso 1 1 calc R . . Cl1 Cl 0.6428(5) 1.5074(4) 0.4321(2) 0.1311(18) Uani 1 1 d . . . Cl2 Cl 0.7452(4) 1.3609(4) 0.36604(17) 0.1272(18) Uani 1 1 d . . . Cl3 Cl 0.5350(4) 1.3486(3) 0.4224(2) 0.1180(16) Uani 1 1 d . . . C1A C 0.6162(13) 1.4248(12) 0.3938(6) 0.093(5) Uani 1 1 d . . . H1AA H 0.5764 1.4588 0.3675 0.112 Uiso 1 1 calc R . . Cl4 Cl 0.5261(3) 0.9288(3) 0.31527(12) 0.0750(10) Uani 1 1 d . . . Cl5 Cl 0.4945(3) 0.7564(3) 0.27627(13) 0.0796(11) Uani 1 1 d . . . Cl6 Cl 0.5551(3) 0.7566(3) 0.37288(12) 0.0836(11) Uani 1 1 d . . . C2A C 0.5693(9) 0.8081(9) 0.3149(4) 0.055(3) Uani 1 1 d . . . H2AA H 0.6512 0.7963 0.3009 0.066 Uiso 1 1 calc R . . Cl7 Cl 0.8641(3) 0.4491(3) 0.23691(15) 0.0939(13) Uani 1 1 d . . . Cl8 Cl 0.7368(3) 0.6296(3) 0.22085(14) 0.0866(12) Uani 1 1 d . . . Cl9 Cl 0.8806(3) 0.5343(3) 0.14086(13) 0.0836(11) Uani 1 1 d . . . C3A C 0.8647(9) 0.5551(9) 0.2037(4) 0.060(3) Uani 1 1 d . . . H3AA H 0.9287 0.5857 0.2107 0.071 Uiso 1 1 calc R . . Cl13 Cl 1.4783(4) 0.1510(4) 0.21862(16) 0.1265(18) Uani 1 1 d . . . Cl14 Cl 1.5614(4) 0.2619(3) 0.13811(16) 0.1006(13) Uani 1 1 d . . . Cl15 Cl 1.3640(3) 0.1767(3) 0.13433(13) 0.0827(11) Uani 1 1 d . . . C5A C 1.4426(14) 0.2278(11) 0.1715(5) 0.086(5) Uani 1 1 d . . . H5AA H 1.3939 0.2851 0.1862 0.103 Uiso 1 1 calc R . . O1S O 0.3285(7) 1.2356(6) 0.4356(3) 0.070(2) Uani 1 1 d . . . C1S C 0.2474(12) 1.3007(10) 0.4666(5) 0.078(4) Uani 1 1 d . . . H1SA H 0.1712 1.2830 0.4690 0.094 Uiso 1 1 calc R . . H1SB H 0.2447 1.3651 0.4522 0.094 Uiso 1 1 calc R . . C2S C 0.2813(12) 1.2984(12) 0.5160(5) 0.097(5) Uani 1 1 d . . . H2SA H 0.2254 1.3409 0.5372 0.145 Uiso 1 1 calc R . . H2SB H 0.3555 1.3186 0.5135 0.145 Uiso 1 1 calc R . . H2SC H 0.2855 1.2343 0.5298 0.145 Uiso 1 1 calc R . . C3S C 0.3018(12) 1.2337(11) 0.3876(4) 0.077(4) Uani 1 1 d . . . H3SA H 0.2897 1.2984 0.3736 0.092 Uiso 1 1 calc R . . H3SB H 0.2314 1.2067 0.3884 0.092 Uiso 1 1 calc R . . C4S C 0.3966(13) 1.1755(11) 0.3566(5) 0.091(5) Uani 1 1 d . . . H4SA H 0.3785 1.1744 0.3234 0.137 Uiso 1 1 calc R . . H4SB H 0.4075 1.1113 0.3703 0.137 Uiso 1 1 calc R . . H4SC H 0.4659 1.2027 0.3557 0.137 Uiso 1 1 calc R . . C4A C 0.8950(5) 1.3280(7) 0.0560(3) 0.073(4) Uiso 1 1 d D . . Cl10 Cl 0.8746(13) 1.2925(8) 0.1186(3) 0.070(3) Uiso 0.30 1 d PD A 1 Cl12 Cl 1.0377(6) 1.3378(8) 0.0473(4) 0.056(3) Uiso 0.30 1 d PD A 1 Cl11 Cl 0.8058(11) 1.4266(7) 0.0409(4) 0.071(3) Uiso 0.30 1 d PD A 1 ClD Cl 0.7538(7) 1.3610(9) 0.0579(4) 0.094(3) Uiso 0.35 1 d PD A 2 ClE Cl 0.9759(11) 1.4074(9) 0.0229(5) 0.119(4) Uiso 0.35 1 d PD A 2 ClF Cl 0.9640(11) 1.2781(8) 0.1022(4) 0.101(4) Uiso 0.35 1 d PD A 2 ClA Cl 0.8125(9) 1.3161(7) 0.1140(3) 0.068(3) Uiso 0.35 1 d PD A 3 ClB Cl 0.8560(10) 1.4443(5) 0.0342(3) 0.065(3) Uiso 0.35 1 d PD A 3 ClC Cl 1.0341(6) 1.3053(8) 0.0649(4) 0.065(3) Uiso 0.35 1 d PD A 3 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.0420(7) 0.0435(7) 0.0250(6) -0.0021(5) -0.0003(5) -0.0162(6) Zn2 0.0346(7) 0.0433(7) 0.0177(5) -0.0035(5) -0.0027(5) -0.0010(5) Zn3 0.0318(7) 0.0442(7) 0.0171(5) 0.0012(5) -0.0013(4) -0.0054(5) N1 0.038(5) 0.046(5) 0.026(4) 0.003(4) -0.005(4) -0.011(4) N2 0.031(5) 0.042(5) 0.024(4) 0.000(4) -0.004(4) -0.008(4) N3 0.035(5) 0.048(5) 0.022(4) 0.003(4) -0.003(3) -0.010(4) N4 0.041(5) 0.045(5) 0.019(4) -0.005(4) -0.007(4) 0.001(4) N5 0.034(5) 0.038(5) 0.021(4) 0.001(3) -0.005(4) 0.004(4) N6 0.038(5) 0.056(6) 0.017(4) -0.007(4) -0.006(4) -0.010(4) N7 0.026(4) 0.037(5) 0.019(4) -0.001(3) -0.005(3) 0.000(4) N8 0.025(4) 0.035(4) 0.017(4) 0.000(3) -0.004(3) 0.002(3) N9 0.026(5) 0.034(4) 0.014(4) 0.001(3) 0.004(3) -0.008(4) N10 0.020(4) 0.033(5) 0.034(4) -0.002(4) -0.007(3) -0.003(4) N11 0.029(4) 0.038(5) 0.023(4) -0.001(3) 0.001(3) -0.001(4) N12 0.043(5) 0.048(5) 0.020(4) 0.000(4) -0.004(4) -0.011(4) C1 0.033(6) 0.040(6) 0.036(6) 0.000(5) -0.003(4) -0.007(5) C2 0.038(6) 0.051(7) 0.040(6) -0.007(5) -0.001(5) -0.021(5) C3 0.038(6) 0.053(7) 0.045(6) -0.012(5) -0.002(5) -0.022(5) C4 0.045(7) 0.047(7) 0.052(7) 0.001(5) -0.005(5) -0.020(5) C5 0.041(6) 0.038(6) 0.035(6) 0.001(5) 0.000(5) -0.012(5) C6 0.027(5) 0.036(6) 0.035(6) -0.002(4) -0.001(4) -0.009(4) C7 0.041(6) 0.043(6) 0.034(6) 0.000(5) -0.002(5) -0.011(5) C8 0.036(6) 0.049(6) 0.023(5) 0.005(5) -0.003(4) -0.011(5) C9 0.037(6) 0.046(6) 0.027(5) 0.003(5) 0.001(4) -0.009(5) C10 0.035(6) 0.051(7) 0.021(5) 0.000(5) 0.006(4) -0.010(5) C11 0.043(6) 0.032(6) 0.028(5) 0.002(4) -0.009(5) 0.003(5) C12 0.034(6) 0.047(6) 0.024(5) 0.001(4) -0.011(4) -0.008(5) C13 0.047(7) 0.047(7) 0.037(6) -0.007(5) 0.002(5) -0.016(5) C14 0.045(7) 0.063(8) 0.046(7) -0.010(6) -0.006(5) -0.002(6) C15 0.030(6) 0.048(6) 0.024(5) 0.004(4) -0.005(4) -0.002(5) C16 0.049(7) 0.046(7) 0.036(6) -0.008(5) -0.021(5) 0.003(5) C17 0.054(7) 0.040(6) 0.033(6) 0.005(5) -0.013(5) -0.013(5) C18 0.036(6) 0.048(6) 0.021(5) -0.006(4) -0.006(4) -0.002(5) C19 0.043(6) 0.035(6) 0.028(5) -0.009(4) -0.001(5) -0.001(5) C20 0.049(7) 0.033(6) 0.024(5) -0.008(4) 0.003(5) 0.000(5) C21 0.063(8) 0.066(8) 0.013(5) 0.005(5) 0.002(5) 0.006(6) C22 0.067(9) 0.090(10) 0.020(6) 0.003(6) 0.010(5) 0.019(7) C23 0.044(7) 0.059(7) 0.033(6) -0.003(5) 0.007(5) 0.017(6) C24 0.045(7) 0.055(7) 0.031(6) 0.002(5) -0.003(5) 0.005(6) C25 0.031(6) 0.052(7) 0.022(5) -0.007(4) 0.002(4) -0.004(5) C26 0.033(6) 0.046(6) 0.024(5) -0.003(5) -0.006(4) 0.003(5) C27 0.029(6) 0.038(6) 0.025(5) -0.001(4) -0.003(4) 0.008(4) C28 0.047(7) 0.043(6) 0.031(6) -0.004(5) -0.007(5) 0.008(5) C29 0.041(6) 0.043(6) 0.018(5) 0.003(4) 0.000(4) 0.000(5) C30 0.030(5) 0.040(6) 0.018(5) 0.004(4) -0.005(4) -0.002(4) C31 0.034(6) 0.041(6) 0.013(4) -0.004(4) 0.004(4) -0.005(5) C32 0.042(6) 0.042(6) 0.036(6) 0.010(5) 0.001(5) 0.001(5) C33 0.067(8) 0.055(7) 0.022(5) 0.004(5) 0.000(5) -0.030(6) C34 0.024(5) 0.047(6) 0.017(5) -0.009(4) 0.004(4) -0.007(4) C35 0.028(6) 0.056(7) 0.026(5) -0.005(5) -0.010(4) -0.007(5) C36 0.036(6) 0.037(6) 0.024(5) 0.003(4) -0.007(4) -0.004(5) C37 0.030(6) 0.040(6) 0.021(5) -0.001(4) -0.003(4) -0.005(4) C38 0.035(6) 0.036(6) 0.021(5) -0.003(4) 0.001(4) -0.007(5) C39 0.034(6) 0.039(6) 0.022(5) 0.000(4) -0.006(4) -0.011(5) C40 0.027(6) 0.042(6) 0.034(5) -0.003(5) 0.005(4) -0.003(5) C41 0.039(7) 0.053(7) 0.037(6) 0.009(5) -0.005(5) -0.015(6) C42 0.035(6) 0.046(6) 0.025(5) 0.007(5) 0.006(4) -0.016(5) C43 0.021(5) 0.045(6) 0.032(5) -0.002(5) 0.000(4) -0.013(4) C44 0.029(6) 0.040(6) 0.022(5) 0.001(4) -0.008(4) -0.005(5) C45 0.042(6) 0.046(7) 0.028(5) 0.005(5) -0.007(5) -0.017(5) C46 0.039(6) 0.043(6) 0.021(5) -0.007(4) 0.002(4) -0.010(5) C47 0.075(9) 0.049(7) 0.043(7) 0.003(6) 0.007(6) 0.005(6) C48 0.077(9) 0.040(7) 0.038(6) 0.006(5) 0.013(6) 0.010(6) C49 0.035(6) 0.040(6) 0.023(5) 0.002(4) 0.002(4) -0.003(5) C50 0.033(6) 0.044(6) 0.022(5) 0.006(4) -0.002(4) -0.004(5) C51 0.071(8) 0.059(7) 0.024(5) 0.000(5) -0.006(5) -0.023(6) C52 0.038(7) 0.076(9) 0.067(8) 0.021(7) -0.012(6) -0.010(6) C53 0.035(6) 0.044(6) 0.029(5) -0.003(5) 0.000(4) -0.006(5) C54 0.063(8) 0.052(7) 0.036(6) 0.010(5) -0.015(5) -0.023(6) C55 0.047(7) 0.067(8) 0.030(6) -0.002(5) -0.011(5) -0.022(6) C56 0.048(7) 0.043(6) 0.026(5) 0.000(4) -0.009(5) -0.017(5) C57 0.036(6) 0.047(6) 0.037(6) -0.003(5) -0.006(5) -0.013(5) O1 0.045(5) 0.074(6) 0.041(4) -0.004(4) -0.013(4) -0.010(4) O2 0.069(6) 0.093(7) 0.032(5) 0.008(4) -0.002(4) -0.001(5) C58 0.040(7) 0.077(9) 0.038(7) 0.007(6) -0.012(6) -0.011(6) C59 0.043(8) 0.149(15) 0.077(10) -0.002(9) -0.027(7) -0.011(9) O3 0.068(5) 0.052(5) 0.039(4) 0.009(4) -0.020(4) -0.010(4) O4 0.057(6) 0.099(8) 0.130(9) -0.030(6) -0.041(6) -0.018(5) C60 0.023(6) 0.082(9) 0.029(6) -0.012(6) 0.003(5) -0.003(6) C61 0.045(7) 0.039(7) 0.061(7) -0.005(5) -0.017(6) 0.003(5) O5 0.042(4) 0.054(4) 0.022(3) -0.009(3) -0.008(3) -0.006(3) O6 0.035(4) 0.048(4) 0.039(4) 0.008(3) -0.010(3) -0.006(3) C62 0.026(6) 0.036(6) 0.038(6) 0.000(5) -0.003(5) -0.010(5) C63 0.069(8) 0.052(7) 0.038(6) -0.008(5) -0.020(6) 0.002(6) O7 0.037(4) 0.057(5) 0.024(3) -0.009(3) 0.005(3) -0.009(4) O8 0.066(5) 0.064(5) 0.024(4) -0.012(4) -0.003(4) -0.009(4) C64 0.037(6) 0.055(7) 0.022(5) 0.012(5) -0.006(5) -0.010(5) C65 0.049(8) 0.071(8) 0.055(7) -0.005(6) 0.000(6) -0.015(6) O9 0.035(5) 0.060(5) 0.061(5) -0.017(4) -0.015(4) 0.000(4) O10 0.026(4) 0.088(6) 0.032(4) -0.018(4) -0.002(3) -0.006(4) C66 0.041(7) 0.051(7) 0.020(5) 0.003(5) -0.002(5) -0.016(5) C67 0.071(9) 0.079(9) 0.032(6) -0.010(6) -0.016(6) -0.010(7) O11 0.059(5) 0.049(4) 0.024(3) 0.002(3) -0.008(3) -0.025(4) O12 0.063(5) 0.069(5) 0.028(4) 0.007(4) -0.014(3) -0.025(4) C68 0.035(6) 0.036(6) 0.027(6) 0.001(4) 0.000(4) -0.003(5) C69 0.042(6) 0.055(7) 0.036(6) 0.000(5) 0.001(5) -0.011(5) Cl1 0.140(5) 0.110(4) 0.153(5) -0.021(3) -0.045(4) -0.024(3) Cl2 0.089(3) 0.199(5) 0.090(3) -0.025(3) -0.018(3) -0.001(3) Cl3 0.094(3) 0.107(3) 0.150(4) 0.023(3) -0.009(3) -0.020(3) C1A 0.078(11) 0.127(14) 0.076(10) -0.016(9) -0.002(8) -0.026(10) Cl4 0.061(2) 0.086(3) 0.071(2) -0.0096(18) 0.0086(17) -0.0054(18) Cl5 0.055(2) 0.115(3) 0.072(2) -0.026(2) -0.0162(17) -0.008(2) Cl6 0.070(2) 0.132(3) 0.0458(18) 0.0200(19) 0.0013(16) -0.023(2) C2A 0.036(7) 0.100(10) 0.030(6) -0.001(6) 0.004(5) -0.020(6) Cl7 0.058(2) 0.106(3) 0.108(3) 0.032(2) -0.007(2) -0.002(2) Cl8 0.076(2) 0.092(3) 0.093(3) -0.036(2) -0.030(2) 0.012(2) Cl9 0.070(2) 0.111(3) 0.070(2) -0.014(2) 0.0021(18) -0.024(2) C3A 0.035(7) 0.073(9) 0.075(8) -0.010(7) -0.017(6) -0.009(6) Cl13 0.136(4) 0.176(5) 0.081(3) 0.031(3) -0.038(3) -0.053(4) Cl14 0.094(3) 0.109(3) 0.097(3) -0.004(2) 0.006(2) -0.029(3) Cl15 0.079(3) 0.106(3) 0.064(2) -0.011(2) -0.0020(18) -0.021(2) C5A 0.115(13) 0.083(11) 0.062(9) 0.004(8) -0.001(8) -0.033(9) O1S 0.063(6) 0.087(6) 0.058(5) 0.008(5) -0.013(4) -0.006(5) C1S 0.069(10) 0.067(9) 0.088(11) -0.006(8) 0.005(8) 0.011(7) C2S 0.072(10) 0.147(16) 0.065(10) -0.020(10) 0.003(8) -0.005(10) C3S 0.084(11) 0.100(11) 0.051(8) 0.014(8) -0.028(7) -0.014(9) C4S 0.103(12) 0.115(13) 0.054(9) -0.008(8) -0.018(8) -0.001(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 O3 1.897(7) . ? Zn1 O1 1.993(7) . ? Zn1 N2 2.022(7) . ? Zn1 N1 2.028(8) . ? Zn2 O7 1.909(6) . ? Zn2 O5 1.969(7) . ? Zn2 N6 2.012(8) . ? Zn2 N5 2.036(7) . ? Zn3 O11 1.938(6) . ? Zn3 N9 2.030(7) . ? Zn3 N10 2.064(7) . ? Zn3 O10 2.084(6) . ? Zn3 O9 2.303(7) . ? Zn3 C66 2.520(9) . ? N1 C57 1.307(12) . ? N1 C1 1.409(12) . ? N2 C7 1.305(12) . ? N2 C6 1.430(12) . ? N3 C11 1.367(11) . ? N3 C8 1.383(12) . ? N4 C15 1.360(12) . ? N4 C18 1.393(11) . ? N5 C19 1.293(11) . ? N5 C20 1.405(12) . ? N6 C26 1.305(11) . ? N6 C25 1.437(11) . ? N7 C30 1.362(10) . ? N7 C27 1.365(11) . ? N8 C34 1.338(11) . ? N8 C37 1.393(11) . ? N9 C38 1.296(11) . ? N9 C39 1.432(11) . ? N10 C45 1.285(12) . ? N10 C44 1.426(11) . ? N11 C49 1.345(11) . ? N11 C46 1.376(11) . ? N12 C53 1.355(12) . ? N12 C56 1.368(12) . ? C1 C2 1.402(13) . ? C1 C6 1.402(13) . ? C2 C3 1.365(13) . ? C3 C4 1.375(14) . ? C4 C5 1.378(14) . ? C5 C6 1.394(13) . ? C7 C8 1.396(13) . ? C8 C9 1.395(13) . ? C9 C10 1.384(13) . ? C10 C11 1.384(13) . ? C11 C12 1.502(13) . ? C12 C15 1.506(13) . ? C12 C13 1.537(13) . ? C12 C14 1.540(13) . ? C15 C16 1.383(12) . ? C16 C17 1.409(14) . ? C17 C18 1.404(13) . ? C18 C19 1.388(13) . ? C20 C25 1.402(13) . ? C20 C21 1.417(13) . ? C21 C22 1.346(15) . ? C22 C23 1.387(14) . ? C23 C24 1.385(13) . ? C24 C25 1.378(13) . ? C26 C27 1.417(12) . ? C27 C28 1.387(13) . ? C28 C29 1.381(13) . ? C29 C30 1.356(13) . ? C30 C31 1.525(12) . ? C31 C32 1.514(13) . ? C31 C34 1.518(12) . ? C31 C33 1.540(13) . ? C34 C35 1.394(12) . ? C35 C36 1.403(13) . ? C36 C37 1.398(13) . ? C37 C38 1.406(12) . ? C39 C40 1.398(13) . ? C39 C44 1.401(13) . ? C40 C41 1.377(13) . ? C41 C42 1.366(13) . ? C42 C43 1.362(13) . ? C43 C44 1.391(12) . ? C45 C46 1.404(13) . ? C46 C47 1.374(14) . ? C47 C48 1.395(14) . ? C48 C49 1.371(13) . ? C49 C50 1.510(12) . ? C50 C53 1.500(13) . ? C50 C52 1.526(14) . ? C50 C51 1.559(13) . ? C53 C54 1.397(13) . ? C54 C55 1.377(14) . ? C55 C56 1.387(13) . ? C56 C57 1.412(13) . ? O1 C58 1.275(12) . ? O2 C58 1.224(13) . ? C58 C59 1.508(16) . ? O3 C60 1.267(12) . ? O4 C60 1.198(12) . ? C60 C61 1.532(15) . ? O5 C62 1.281(11) . ? O6 C62 1.244(11) . ? C62 C63 1.498(14) . ? O7 C64 1.287(12) . ? O8 C64 1.233(12) . ? C64 C65 1.518(14) . ? O9 C66 1.229(11) . ? O10 C66 1.280(12) . ? C66 C67 1.512(13) . ? O11 C68 1.269(11) . ? O12 C68 1.243(11) . ? C68 C69 1.483(13) . ? Cl1 C1A 1.733(15) . ? Cl2 C1A 1.768(16) . ? Cl3 C1A 1.681(16) . ? Cl4 C2A 1.736(13) . ? Cl5 C2A 1.765(11) . ? Cl6 C2A 1.732(11) . ? Cl7 C3A 1.745(13) . ? Cl8 C3A 1.753(12) . ? Cl9 C3A 1.759(12) . ? Cl13 C5A 1.730(14) . ? Cl14 C5A 1.716(15) . ? Cl15 C5A 1.764(15) . ? O1S C3S 1.421(13) . ? O1S C1S 1.453(14) . ? C1S C2S 1.485(18) . ? C3S C4S 1.490(19) . ? C4A ClD 1.695(8) . ? C4A ClF 1.701(8) . ? C4A Cl11 1.717(8) . ? C4A ClC 1.718(8) . ? C4A Cl12 1.738(8) . ? C4A ClE 1.760(8) . ? C4A ClB 1.770(8) . ? C4A ClA 1.773(8) . ? C4A Cl10 1.776(8) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O3 Zn1 O1 97.0(3) . . ? O3 Zn1 N2 122.6(3) . . ? O1 Zn1 N2 127.0(3) . . ? O3 Zn1 N1 130.8(3) . . ? O1 Zn1 N1 97.1(3) . . ? N2 Zn1 N1 83.1(3) . . ? O7 Zn2 O5 96.6(3) . . ? O7 Zn2 N6 122.3(3) . . ? O5 Zn2 N6 130.7(3) . . ? O7 Zn2 N5 122.1(3) . . ? O5 Zn2 N5 100.6(3) . . ? N6 Zn2 N5 84.3(3) . . ? O11 Zn3 N9 121.6(3) . . ? O11 Zn3 N10 122.8(3) . . ? N9 Zn3 N10 82.6(3) . . ? O11 Zn3 O10 94.2(3) . . ? N9 Zn3 O10 136.9(3) . . ? N10 Zn3 O10 98.5(3) . . ? O11 Zn3 O9 88.8(3) . . ? N9 Zn3 O9 95.2(3) . . ? N10 Zn3 O9 144.2(3) . . ? O10 Zn3 O9 59.5(3) . . ? O11 Zn3 C66 90.3(3) . . ? N9 Zn3 C66 118.7(3) . . ? N10 Zn3 C66 124.9(3) . . ? O10 Zn3 C66 30.4(3) . . ? O9 Zn3 C66 29.1(3) . . ? C57 N1 C1 119.1(8) . . ? C57 N1 Zn1 128.6(7) . . ? C1 N1 Zn1 110.8(6) . . ? C7 N2 C6 117.9(8) . . ? C7 N2 Zn1 131.0(7) . . ? C6 N2 Zn1 109.6(6) . . ? C11 N3 C8 110.2(8) . . ? C15 N4 C18 110.8(8) . . ? C19 N5 C20 119.5(8) . . ? C19 N5 Zn2 130.1(7) . . ? C20 N5 Zn2 109.6(5) . . ? C26 N6 C25 117.2(8) . . ? C26 N6 Zn2 130.1(6) . . ? C25 N6 Zn2 109.8(6) . . ? C30 N7 C27 109.2(7) . . ? C34 N8 C37 110.4(7) . . ? C38 N9 C39 118.7(7) . . ? C38 N9 Zn3 129.9(6) . . ? C39 N9 Zn3 109.9(6) . . ? C45 N10 C44 120.1(8) . . ? C45 N10 Zn3 130.1(7) . . ? C44 N10 Zn3 109.3(6) . . ? C49 N11 C46 110.5(8) . . ? C53 N12 C56 110.2(8) . . ? C2 C1 C6 119.0(9) . . ? C2 C1 N1 124.2(9) . . ? C6 C1 N1 116.7(8) . . ? C3 C2 C1 120.1(9) . . ? C2 C3 C4 121.1(10) . . ? C3 C4 C5 120.0(10) . . ? C4 C5 C6 120.2(9) . . ? C5 C6 C1 119.6(9) . . ? C5 C6 N2 123.2(8) . . ? C1 C6 N2 117.1(8) . . ? N2 C7 C8 126.7(9) . . ? N3 C8 C9 106.0(8) . . ? N3 C8 C7 128.6(9) . . ? C9 C8 C7 125.3(9) . . ? C10 C9 C8 108.5(9) . . ? C11 C10 C9 108.0(8) . . ? N3 C11 C10 107.3(8) . . ? N3 C11 C12 121.2(8) . . ? C10 C11 C12 131.5(9) . . ? C11 C12 C15 108.6(8) . . ? C11 C12 C13 110.7(7) . . ? C15 C12 C13 109.1(8) . . ? C11 C12 C14 108.9(8) . . ? C15 C12 C14 110.1(8) . . ? C13 C12 C14 109.4(8) . . ? N4 C15 C16 108.0(8) . . ? N4 C15 C12 121.1(8) . . ? C16 C15 C12 130.9(9) . . ? C15 C16 C17 107.4(9) . . ? C18 C17 C16 108.4(8) . . ? C19 C18 N4 126.8(8) . . ? C19 C18 C17 127.8(9) . . ? N4 C18 C17 105.4(8) . . ? N5 C19 C18 127.0(9) . . ? C25 C20 N5 118.2(8) . . ? C25 C20 C21 117.1(9) . . ? N5 C20 C21 124.6(9) . . ? C22 C21 C20 121.3(10) . . ? C21 C22 C23 121.3(10) . . ? C24 C23 C22 118.6(10) . . ? C25 C24 C23 121.0(9) . . ? C24 C25 C20 120.6(8) . . ? C24 C25 N6 122.5(9) . . ? C20 C25 N6 116.8(8) . . ? N6 C26 C27 127.2(9) . . ? N7 C27 C28 107.0(8) . . ? N7 C27 C26 127.5(8) . . ? C28 C27 C26 125.5(9) . . ? C29 C28 C27 107.5(9) . . ? C30 C29 C28 108.2(8) . . ? C29 C30 N7 108.1(8) . . ? C29 C30 C31 132.0(8) . . ? N7 C30 C31 119.8(8) . . ? C32 C31 C34 112.1(7) . . ? C32 C31 C30 111.4(7) . . ? C34 C31 C30 108.6(7) . . ? C32 C31 C33 108.5(8) . . ? C34 C31 C33 107.9(7) . . ? C30 C31 C33 108.2(8) . . ? N8 C34 C35 108.1(8) . . ? N8 C34 C31 122.8(8) . . ? C35 C34 C31 129.0(8) . . ? C34 C35 C36 107.6(8) . . ? C37 C36 C35 107.4(8) . . ? N8 C37 C36 106.5(8) . . ? N8 C37 C38 128.1(8) . . ? C36 C37 C38 125.4(8) . . ? N9 C38 C37 128.2(9) . . ? C40 C39 C44 119.7(8) . . ? C40 C39 N9 122.9(8) . . ? C44 C39 N9 117.4(8) . . ? C41 C40 C39 120.1(9) . . ? C42 C41 C40 119.5(10) . . ? C43 C42 C41 121.7(9) . . ? C42 C43 C44 120.4(9) . . ? C43 C44 C39 118.6(9) . . ? C43 C44 N10 124.7(8) . . ? C39 C44 N10 116.7(8) . . ? N10 C45 C46 128.2(9) . . ? C47 C46 N11 105.9(9) . . ? C47 C46 C45 127.4(9) . . ? N11 C46 C45 126.8(9) . . ? C46 C47 C48 108.7(10) . . ? C49 C48 C47 106.9(10) . . ? N11 C49 C48 108.0(8) . . ? N11 C49 C50 122.2(8) . . ? C48 C49 C50 129.6(9) . . ? C53 C50 C49 107.2(8) . . ? C53 C50 C52 109.8(9) . . ? C49 C50 C52 109.6(8) . . ? C53 C50 C51 108.9(8) . . ? C49 C50 C51 111.2(8) . . ? C52 C50 C51 110.1(8) . . ? N12 C53 C54 107.2(8) . . ? N12 C53 C50 122.5(8) . . ? C54 C53 C50 130.3(9) . . ? C55 C54 C53 107.5(9) . . ? C54 C55 C56 108.3(9) . . ? N12 C56 C55 106.8(8) . . ? N12 C56 C57 126.1(8) . . ? C55 C56 C57 127.1(9) . . ? N1 C57 C56 125.1(9) . . ? C58 O1 Zn1 107.2(7) . . ? O2 C58 O1 123.1(10) . . ? O2 C58 C59 121.4(11) . . ? O1 C58 C59 115.5(10) . . ? C60 O3 Zn1 119.2(7) . . ? O4 C60 O3 124.9(12) . . ? O4 C60 C61 119.6(11) . . ? O3 C60 C61 115.2(9) . . ? C62 O5 Zn2 112.4(6) . . ? O6 C62 O5 121.6(9) . . ? O6 C62 C63 121.5(9) . . ? O5 C62 C63 116.9(9) . . ? C64 O7 Zn2 115.4(6) . . ? O8 C64 O7 123.4(9) . . ? O8 C64 C65 121.5(10) . . ? O7 C64 C65 115.1(9) . . ? C66 O9 Zn3 85.3(6) . . ? C66 O10 Zn3 93.9(6) . . ? O9 C66 O10 121.1(9) . . ? O9 C66 C67 121.8(10) . . ? O10 C66 C67 117.1(10) . . ? O9 C66 Zn3 65.6(5) . . ? O10 C66 Zn3 55.6(5) . . ? C67 C66 Zn3 170.6(8) . . ? C68 O11 Zn3 118.2(6) . . ? O12 C68 O11 121.8(9) . . ? O12 C68 C69 120.8(9) . . ? O11 C68 C69 117.3(8) . . ? Cl3 C1A Cl1 113.6(9) . . ? Cl3 C1A Cl2 108.8(10) . . ? Cl1 C1A Cl2 109.8(8) . . ? Cl6 C2A Cl4 112.6(6) . . ? Cl6 C2A Cl5 111.0(7) . . ? Cl4 C2A Cl5 109.7(6) . . ? Cl7 C3A Cl8 109.5(7) . . ? Cl7 C3A Cl9 109.8(7) . . ? Cl8 C3A Cl9 109.2(6) . . ? Cl14 C5A Cl13 110.5(9) . . ? Cl14 C5A Cl15 111.5(8) . . ? Cl13 C5A Cl15 110.6(8) . . ? C3S O1S C1S 112.9(10) . . ? O1S C1S C2S 109.4(11) . . ? O1S C3S C4S 109.3(11) . . ? ClD C4A ClF 127.3(8) . . ? ClD C4A Cl11 43.1(6) . . ? ClF C4A Cl11 142.1(10) . . ? ClD C4A ClC 168.8(9) . . ? ClF C4A ClC 45.4(6) . . ? Cl11 C4A ClC 134.6(8) . . ? ClD C4A Cl12 158.5(8) . . ? ClF C4A Cl12 66.5(6) . . ? Cl11 C4A Cl12 115.5(8) . . ? ClC C4A Cl12 22.0(4) . . ? ClD C4A ClE 113.6(7) . . ? ClF C4A ClE 108.6(8) . . ? Cl11 C4A ClE 71.1(7) . . ? ClC C4A ClE 67.8(6) . . ? Cl12 C4A ClE 46.0(6) . . ? ClD C4A ClB 66.0(6) . . ? ClF C4A ClB 135.1(9) . . ? Cl11 C4A ClB 22.9(5) . . ? ClC C4A ClB 112.3(7) . . ? Cl12 C4A ClB 92.6(7) . . ? ClE C4A ClB 48.7(6) . . ? ClD C4A ClA 64.5(6) . . ? ClF C4A ClA 62.9(6) . . ? Cl11 C4A ClA 92.2(7) . . ? ClC C4A ClA 106.9(7) . . ? Cl12 C4A ClA 124.4(8) . . ? ClE C4A ClA 139.7(10) . . ? ClB C4A ClA 107.1(7) . . ? ClD C4A Cl10 90.5(7) . . ? ClF C4A Cl10 36.8(5) . . ? Cl11 C4A Cl10 115.0(8) . . ? ClC C4A Cl10 81.5(7) . . ? Cl12 C4A Cl10 100.9(7) . . ? ClE C4A Cl10 132.9(9) . . ? ClB C4A Cl10 124.0(8) . . ? ClA C4A Cl10 26.1(4) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 23.26 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.238 _refine_diff_density_min -1.077 _refine_diff_density_rms 0.119