# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 ####################################################################### # # 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_aja0804 _database_code_depnum_ccdc_archive 'CCDC 844367' #TrackingRef '- aja0804_5.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common aja0804 _chemical_melting_point ? _chemical_formula_moiety '2(C34 H30 N8 O2 S2 Zn), C2 H3 N, 4(Cl O4)' _chemical_formula_sum 'C70 H63 Cl4 N17 O20 S4 Zn2' _chemical_formula_weight 1863.23 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' 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 10.46660(10) _cell_length_b 42.1309(4) _cell_length_c 17.5050(2) _cell_angle_alpha 90 _cell_angle_beta 91.2101(4) _cell_angle_gamma 90 _cell_volume 7717.41(14) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 100471 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.485 _exptl_crystal_description rectangle _exptl_crystal_colour colourless _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.4 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.604 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3816 _exptl_absorpt_coefficient_mu 0.953 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.658 _exptl_absorpt_correction_T_max 0.867 _exptl_absorpt_process_details 'Sortav (Blessing, 1995)' _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 KappaCCD _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean 9 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 37445 _diffrn_reflns_av_R_equivalents 0.1463 _diffrn_reflns_av_sigmaI/netI 0.1213 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -54 _diffrn_reflns_limit_k_max 54 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.96 _diffrn_reflns_theta_max 27.48 _reflns_number_total 17709 _reflns_number_gt 9711 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1986)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _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^)+(0.1183P)^2^+18.9093P] 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 14469 _refine_ls_number_parameters 1055 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1262 _refine_ls_R_factor_gt 0.0800 _refine_ls_wR_factor_ref 0.2425 _refine_ls_wR_factor_gt 0.2002 _refine_ls_goodness_of_fit_ref 1.055 _refine_ls_restrained_S_all 1.055 _refine_ls_shift/su_max 0.016 _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 C1 C 0.5566(6) 0.07965(16) 0.8636(4) 0.0280(15) Uani 1 1 d . . . H1A H 0.5316 0.0971 0.8287 0.034 Uiso 1 1 calc R . . H1B H 0.6089 0.0888 0.9060 0.034 Uiso 1 1 calc R . . C2 C 0.4368(6) 0.06460(15) 0.8960(4) 0.0236(13) Uani 1 1 d . . . C3 C 0.3762(6) 0.07785(16) 0.9577(4) 0.0305(15) Uani 1 1 d . . . H3 H 0.4108 0.0960 0.9827 0.037 Uiso 1 1 calc R . . C4 C 0.2649(7) 0.06426(17) 0.9821(4) 0.0354(17) Uani 1 1 d . . . H4 H 0.2199 0.0735 1.0231 0.042 Uiso 1 1 calc R . . C5 C 0.2187(6) 0.03707(16) 0.9470(4) 0.0299(15) Uani 1 1 d . . . H5 H 0.1432 0.0269 0.9638 0.036 Uiso 1 1 calc R . . C6 C 0.2861(5) 0.02531(15) 0.8868(3) 0.0218(13) Uani 1 1 d . . . C7 C 0.2988(5) -0.03057(14) 0.8537(3) 0.0208(13) Uani 1 1 d . . . C8 C 0.1649(5) -0.05254(16) 0.7461(4) 0.0241(14) Uani 1 1 d . . . C9 C 0.1645(5) -0.07991(14) 0.6925(4) 0.0213(13) Uani 1 1 d . . . C10 C 0.0473(6) -0.09029(18) 0.6608(4) 0.0325(16) Uani 1 1 d . . . H10 H -0.0305 -0.0808 0.6762 0.039 Uiso 1 1 calc R . . C11 C 0.0461(7) -0.11412(17) 0.6078(4) 0.0356(17) Uani 1 1 d . . . H11 H -0.0327 -0.1212 0.5859 0.043 Uiso 1 1 calc R . . C12 C 0.1588(7) -0.12780(16) 0.5861(4) 0.0333(16) Uani 1 1 d . . . H12 H 0.1569 -0.1442 0.5487 0.040 Uiso 1 1 calc R . . C13 C 0.2744(7) -0.11837(16) 0.6172(4) 0.0321(16) Uani 1 1 d . . . H13 H 0.3513 -0.1282 0.6017 0.038 Uiso 1 1 calc R . . C14 C 0.2775(5) -0.09435(15) 0.6716(4) 0.0240(14) Uani 1 1 d . . . H14 H 0.3565 -0.0879 0.6942 0.029 Uiso 1 1 calc R . . C15 C 0.7100(5) 0.07037(16) 0.7627(4) 0.0279(15) Uani 1 1 d . . . H15A H 0.7768 0.0550 0.7482 0.033 Uiso 1 1 calc R . . H15B H 0.7529 0.0898 0.7822 0.033 Uiso 1 1 calc R . . C16 C 0.6296(5) 0.07857(15) 0.6936(4) 0.0240(13) Uani 1 1 d . . . C17 C 0.6655(6) 0.10288(16) 0.6439(4) 0.0294(15) Uani 1 1 d . . . H17 H 0.7412 0.1148 0.6535 0.035 Uiso 1 1 calc R . . C18 C 0.5891(6) 0.10908(18) 0.5811(4) 0.0373(17) Uani 1 1 d . . . H18 H 0.6123 0.1252 0.5461 0.045 Uiso 1 1 calc R . . C19 C 0.4785(6) 0.09191(16) 0.5690(4) 0.0303(15) Uani 1 1 d . . . H19 H 0.4254 0.0957 0.5253 0.036 Uiso 1 1 calc R . . C20 C 0.4467(5) 0.06893(14) 0.6221(4) 0.0215(13) Uani 1 1 d . . . C21 C 0.2853(5) 0.02510(15) 0.6328(3) 0.0223(13) Uani 1 1 d . . . C22 C 0.0716(5) 0.03770(15) 0.5781(3) 0.0223(13) Uani 1 1 d . . . C23 C -0.0629(5) 0.02509(15) 0.5704(4) 0.0234(13) Uani 1 1 d . . . C24 C -0.1017(6) -0.00408(18) 0.6002(4) 0.0343(17) Uani 1 1 d . . . H24 H -0.0434 -0.0171 0.6282 0.041 Uiso 1 1 calc R . . C25 C -0.2268(6) -0.0135(2) 0.5879(4) 0.0401(18) Uani 1 1 d . . . H25 H -0.2538 -0.0334 0.6077 0.048 Uiso 1 1 calc R . . C26 C -0.3139(6) 0.00502(18) 0.5477(4) 0.0336(17) Uani 1 1 d . . . H26 H -0.3994 -0.0021 0.5401 0.040 Uiso 1 1 calc R . . C27 C -0.2761(6) 0.03401(17) 0.5184(4) 0.0301(16) Uani 1 1 d . . . H27 H -0.3359 0.0468 0.4908 0.036 Uiso 1 1 calc R . . C28 C -0.1494(6) 0.04466(17) 0.5294(4) 0.0308(15) Uani 1 1 d . . . H28 H -0.1229 0.0645 0.5096 0.037 Uiso 1 1 calc R . . C29 C 0.7087(6) 0.03590(15) 0.8747(4) 0.0274(14) Uani 1 1 d . . . H29A H 0.6627 0.0331 0.9231 0.033 Uiso 1 1 calc R . . H29B H 0.7920 0.0461 0.8868 0.033 Uiso 1 1 calc R . . C30 C 0.7308(5) 0.00394(16) 0.8389(3) 0.0244(14) Uani 1 1 d . . . C31 C 0.8330(5) -0.01514(16) 0.8604(4) 0.0256(14) Uani 1 1 d . . . H31 H 0.8966 -0.0073 0.8950 0.031 Uiso 1 1 calc R . . C32 C 0.8426(6) -0.04545(16) 0.8315(4) 0.0267(14) Uani 1 1 d . . . H32 H 0.9141 -0.0584 0.8445 0.032 Uiso 1 1 calc R . . C33 C 0.7458(5) -0.05684(15) 0.7830(4) 0.0242(13) Uani 1 1 d . . . H33 H 0.7475 -0.0780 0.7646 0.029 Uiso 1 1 calc R . . C34 C 0.6464(6) -0.03637(15) 0.7620(4) 0.0256(14) Uani 1 1 d . . . H34 H 0.5822 -0.0437 0.7271 0.031 Uiso 1 1 calc R . . C35 C 0.0478(6) 0.17276(18) 0.7794(4) 0.0355(17) Uani 1 1 d . . . H35A H -0.0215 0.1876 0.7643 0.043 Uiso 1 1 calc R . . H35B H 0.0080 0.1529 0.7973 0.043 Uiso 1 1 calc R . . C36 C 0.1280(6) 0.16578(16) 0.7115(4) 0.0263(14) Uani 1 1 d . . . C37 C 0.0868(6) 0.14376(16) 0.6579(4) 0.0317(15) Uani 1 1 d . . . H37 H 0.0095 0.1323 0.6644 0.038 Uiso 1 1 calc R . . C38 C 0.1608(6) 0.13879(16) 0.5944(4) 0.0317(15) Uani 1 1 d . . . H38 H 0.1349 0.1238 0.5566 0.038 Uiso 1 1 calc R . . C39 C 0.2727(6) 0.15573(15) 0.5864(4) 0.0313(15) Uani 1 1 d . . . H39 H 0.3249 0.1524 0.5433 0.038 Uiso 1 1 calc R . . C40 C 0.3074(6) 0.17752(15) 0.6418(4) 0.0259(14) Uani 1 1 d . . . C41 C 0.4638(6) 0.22148(16) 0.6592(4) 0.0289(15) Uani 1 1 d . . . C42 C 0.6757(6) 0.21208(17) 0.6030(4) 0.0332(16) Uani 1 1 d . . . C43 C 0.8041(6) 0.22658(16) 0.5988(4) 0.0272(14) Uani 1 1 d . . . C44 C 0.9034(6) 0.20794(18) 0.5748(4) 0.0356(17) Uani 1 1 d . . . H44 H 0.8879 0.1863 0.5624 0.043 Uiso 1 1 calc R . . C45 C 1.0259(7) 0.2202(2) 0.5682(5) 0.047(2) Uani 1 1 d . . . H45 H 1.0941 0.2068 0.5532 0.056 Uiso 1 1 calc R . . C46 C 1.0477(7) 0.2515(2) 0.5834(4) 0.044(2) Uani 1 1 d . . . H46 H 1.1315 0.2599 0.5789 0.052 Uiso 1 1 calc R . . C47 C 0.9492(8) 0.2712(2) 0.6053(5) 0.052(2) Uani 1 1 d . . . H47 H 0.9653 0.2930 0.6151 0.062 Uiso 1 1 calc R . . C48 C 0.8273(7) 0.2590(2) 0.6129(5) 0.046(2) Uani 1 1 d . . . H48 H 0.7595 0.2725 0.6277 0.055 Uiso 1 1 calc R . . C49 C 0.2048(7) 0.16262(16) 0.8832(4) 0.0340(16) Uani 1 1 d . . . H49A H 0.2345 0.1465 0.8465 0.041 Uiso 1 1 calc R . . H49B H 0.1533 0.1518 0.9222 0.041 Uiso 1 1 calc R . . C50 C 0.3191(6) 0.17901(16) 0.9213(4) 0.0292(15) Uani 1 1 d . . . C51 C 0.3723(7) 0.16835(17) 0.9898(4) 0.0392(18) Uani 1 1 d . . . H51 H 0.3359 0.1509 1.0158 0.047 Uiso 1 1 calc R . . C52 C 0.4794(8) 0.1836(2) 1.0199(4) 0.047(2) Uani 1 1 d . . . H52 H 0.5183 0.1763 1.0661 0.057 Uiso 1 1 calc R . . C53 C 0.5286(8) 0.20920(19) 0.9826(4) 0.0428(19) Uani 1 1 d . . . H53 H 0.6030 0.2196 1.0020 0.051 Uiso 1 1 calc R . . C54 C 0.4683(6) 0.21967(15) 0.9163(4) 0.0276(14) Uani 1 1 d . . . C55 C 0.4588(6) 0.27534(15) 0.8900(4) 0.0263(14) Uani 1 1 d . . . C56 C 0.5875(6) 0.29846(15) 0.7850(4) 0.0256(14) Uani 1 1 d . . . C57 C 0.5973(5) 0.32748(14) 0.7374(4) 0.0225(13) Uani 1 1 d . . . C58 C 0.4921(6) 0.34681(16) 0.7219(4) 0.0281(15) Uani 1 1 d . . . H58 H 0.4128 0.3429 0.7457 0.034 Uiso 1 1 calc R . . C59 C 0.5051(7) 0.37202(16) 0.6708(4) 0.0318(16) Uani 1 1 d . . . H59 H 0.4343 0.3855 0.6599 0.038 Uiso 1 1 calc R . . C60 C 0.6200(7) 0.37746(16) 0.6361(4) 0.0346(16) Uani 1 1 d . . . H60 H 0.6278 0.3945 0.6010 0.042 Uiso 1 1 calc R . . C61 C 0.7247(6) 0.35802(18) 0.6525(4) 0.0337(16) Uani 1 1 d . . . H61 H 0.8041 0.3620 0.6289 0.040 Uiso 1 1 calc R . . C62 C 0.7138(6) 0.33306(17) 0.7025(4) 0.0316(15) Uani 1 1 d . . . H62 H 0.7851 0.3197 0.7133 0.038 Uiso 1 1 calc R . . C63 C 0.0482(7) 0.20595(17) 0.8939(4) 0.0351(16) Uani 1 1 d . . . H63A H 0.0912 0.2072 0.9447 0.042 Uiso 1 1 calc R . . H63B H -0.0358 0.1956 0.9003 0.042 Uiso 1 1 calc R . . C64 C 0.0284(6) 0.23908(17) 0.8626(4) 0.0295(15) Uani 1 1 d . . . C65 C -0.0716(6) 0.25848(19) 0.8837(4) 0.0384(18) Uani 1 1 d . . . H65 H -0.1369 0.2501 0.9148 0.046 Uiso 1 1 calc R . . C66 C -0.0782(7) 0.28996(19) 0.8601(4) 0.0416(19) Uani 1 1 d . . . H66 H -0.1457 0.3034 0.8757 0.050 Uiso 1 1 calc R . . C67 C 0.0162(7) 0.30094(19) 0.8135(4) 0.0426(19) Uani 1 1 d . . . H67 H 0.0154 0.3223 0.7960 0.051 Uiso 1 1 calc R . . C68 C 0.1123(7) 0.28034(17) 0.7926(4) 0.0343(16) Uani 1 1 d . . . H68 H 0.1769 0.2881 0.7601 0.041 Uiso 1 1 calc R . . C69 C 1.1192(10) -0.1038(3) 1.0196(6) 0.079(3) Uani 1 1 d . . . H69A H 1.2114 -0.1075 1.0163 0.118 Uiso 1 1 calc R . . H69B H 1.0729 -0.1200 0.9899 0.118 Uiso 1 1 calc R . . H69C H 1.0940 -0.1049 1.0731 0.118 Uiso 1 1 calc R . . C70 C 1.0890(8) -0.0729(3) 0.9893(5) 0.053(2) Uani 1 1 d . . . N1 N 0.6329(5) 0.05672(13) 0.8225(3) 0.0255(12) Uani 1 1 d . . . N2 N 0.3929(5) 0.03873(12) 0.8607(3) 0.0216(11) Uani 1 1 d . . . N3 N 0.5204(4) 0.06206(12) 0.6835(3) 0.0204(11) Uani 1 1 d . . . N4 N 0.6385(4) -0.00691(12) 0.7893(3) 0.0223(11) Uani 1 1 d . . . N5 N 0.2411(4) -0.00221(12) 0.8474(3) 0.0196(11) Uani 1 1 d . . . H5A H 0.1727 -0.0005 0.8176 0.023 Uiso 1 1 calc R . . N6 N 0.2564(5) -0.05391(12) 0.8055(3) 0.0238(11) Uani 1 1 d . . . H6 H 0.2919 -0.0726 0.8128 0.029 Uiso 1 1 calc R . . N7 N 0.3267(4) 0.05373(13) 0.6107(3) 0.0235(11) Uani 1 1 d . . . H7 H 0.2699 0.0650 0.5848 0.028 Uiso 1 1 calc R . . N8 N 0.1597(4) 0.01883(12) 0.6184(3) 0.0190(10) Uani 1 1 d . . . H8 H 0.1306 0.0008 0.6366 0.023 Uiso 1 1 calc R . . N9 N 0.1258(5) 0.18695(12) 0.8426(3) 0.0259(12) Uani 1 1 d . . . N10 N 0.2364(5) 0.18226(13) 0.7045(3) 0.0275(12) Uani 1 1 d . . . N11 N 0.3658(5) 0.20492(12) 0.8851(3) 0.0246(12) Uani 1 1 d . . . N12 N 0.1190(5) 0.24986(13) 0.8159(3) 0.0286(12) Uani 1 1 d . . . N13 N 0.4261(5) 0.19247(12) 0.6372(3) 0.0254(12) Uani 1 1 d . . . H13A H 0.4861 0.1809 0.6165 0.030 Uiso 1 1 calc R . . N14 N 0.5884(5) 0.22893(13) 0.6459(3) 0.0273(12) Uani 1 1 d . . . H14A H 0.6169 0.2466 0.6672 0.033 Uiso 1 1 calc R . . N15 N 0.5122(5) 0.24688(12) 0.8777(3) 0.0257(12) Uani 1 1 d . . . H15 H 0.5751 0.2452 0.8454 0.031 Uiso 1 1 calc R . . N16 N 0.5018(5) 0.30007(12) 0.8444(3) 0.0258(12) Uani 1 1 d . . . H16 H 0.4709 0.3190 0.8545 0.031 Uiso 1 1 calc R . . N17 N 1.0692(7) -0.0488(3) 0.9672(5) 0.071(3) Uani 1 1 d . . . O1 O 0.0927(4) -0.02986(10) 0.7392(2) 0.0256(10) Uani 1 1 d . . . O2 O 0.1028(4) 0.06286(11) 0.5491(3) 0.0294(10) Uani 1 1 d . . . O3 O 0.6473(4) 0.18739(12) 0.5702(3) 0.0410(13) Uani 1 1 d . . . O4 O 0.6516(4) 0.27472(11) 0.7734(3) 0.0292(10) Uani 1 1 d . . . O5 O 0.0356(6) 0.09518(14) 0.8256(3) 0.0599(17) Uani 1 1 d . . . O6 O -0.0114(4) 0.07658(13) 0.7038(3) 0.0416(13) Uani 1 1 d . . . O7 O 0.0258(5) 0.04081(12) 0.8033(3) 0.0492(15) Uani 1 1 d . . . O8 O 0.1947(5) 0.07058(15) 0.7574(3) 0.0554(16) Uani 1 1 d . . . O9 O 0.7073(7) 0.20206(14) 0.8237(4) 0.080(2) Uani 1 1 d . . . O10 O 0.7393(8) 0.1495(2) 0.8516(6) 0.115(3) Uani 1 1 d . . . O11 O 0.7511(6) 0.1657(2) 0.7300(5) 0.099(3) Uani 1 1 d . . . O12 O 0.5541(6) 0.16455(19) 0.7907(4) 0.085(2) Uani 1 1 d . . . O13 O 0.7419(5) -0.12710(13) 0.6792(3) 0.0426(13) Uani 1 1 d . . . O14 O 0.5816(4) -0.13945(11) 0.5873(3) 0.0338(11) Uani 1 1 d . . . O15 O 0.5860(4) -0.08901(12) 0.6433(3) 0.0442(13) Uani 1 1 d . . . O16 O 0.7437(4) -0.10353(13) 0.5581(3) 0.0427(13) Uani 1 1 d . . . O17 O 0.7961(5) -0.12039(12) 0.8958(3) 0.0491(14) Uani 1 1 d . . . O18 O 0.9693(6) -0.1354(2) 0.8229(4) 0.087(2) Uani 1 1 d . . . O19 O 0.9384(6) -0.15878(14) 0.9414(3) 0.0602(17) Uani 1 1 d . . . O20 O 0.7989(5) -0.17064(14) 0.8399(3) 0.0541(16) Uani 1 1 d . . . S1 S 0.42000(15) -0.03789(4) 0.91472(10) 0.0293(4) Uani 1 1 d . . . S2 S 0.37508(13) -0.00393(4) 0.67324(9) 0.0207(3) Uani 1 1 d . . . S3 S 0.37245(14) 0.24954(4) 0.70011(10) 0.0256(4) Uani 1 1 d . . . S4 S 0.34540(18) 0.28129(5) 0.95271(11) 0.0389(5) Uani 1 1 d . . . Cl1 Cl 0.06209(14) 0.07079(4) 0.77296(9) 0.0268(3) Uani 1 1 d . . . Cl2 Cl 0.68626(17) 0.17038(5) 0.80121(12) 0.0437(5) Uani 1 1 d . . . Cl3 Cl 0.66409(14) -0.11482(4) 0.61793(9) 0.0270(3) Uani 1 1 d . . . Cl4 Cl 0.87619(16) -0.14600(5) 0.87381(10) 0.0374(4) Uani 1 1 d . . . Zn1 Zn 0.49530(6) 0.025312(17) 0.76551(4) 0.01955(18) Uani 1 1 d . . . Zn2 Zn 0.26088(7) 0.218345(17) 0.78910(4) 0.02366(19) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.033(3) 0.028(4) 0.023(4) -0.015(3) 0.003(3) -0.003(3) C2 0.029(3) 0.023(3) 0.018(4) -0.002(2) -0.007(3) 0.002(3) C3 0.041(4) 0.029(4) 0.021(4) -0.008(3) -0.001(3) 0.005(3) C4 0.049(4) 0.041(4) 0.017(4) -0.005(3) 0.008(3) 0.016(3) C5 0.037(3) 0.030(4) 0.023(4) -0.002(3) 0.006(3) 0.008(3) C6 0.025(3) 0.027(4) 0.013(3) 0.002(2) -0.002(2) 0.005(3) C7 0.022(3) 0.021(3) 0.020(3) 0.005(2) 0.002(2) -0.006(2) C8 0.021(3) 0.031(4) 0.020(4) 0.005(3) 0.002(2) -0.005(3) C9 0.024(3) 0.015(3) 0.025(4) 0.009(2) 0.005(2) 0.001(2) C10 0.027(3) 0.046(5) 0.024(4) -0.001(3) 0.001(3) 0.002(3) C11 0.038(4) 0.039(4) 0.029(4) -0.006(3) -0.001(3) -0.010(3) C12 0.049(4) 0.028(4) 0.023(4) -0.007(3) 0.003(3) 0.004(3) C13 0.038(3) 0.030(4) 0.028(4) -0.001(3) 0.004(3) 0.013(3) C14 0.020(3) 0.028(4) 0.025(4) 0.007(3) 0.002(2) 0.000(3) C15 0.021(3) 0.033(4) 0.030(4) -0.010(3) 0.000(3) 0.000(3) C16 0.026(3) 0.020(3) 0.026(4) -0.007(2) 0.004(3) 0.003(3) C17 0.033(3) 0.024(4) 0.031(4) -0.005(3) 0.011(3) -0.007(3) C18 0.034(3) 0.037(4) 0.040(5) 0.009(3) 0.000(3) -0.006(3) C19 0.028(3) 0.039(4) 0.024(4) 0.013(3) 0.000(3) -0.002(3) C20 0.022(3) 0.019(3) 0.024(4) -0.001(2) 0.007(2) -0.002(2) C21 0.024(3) 0.035(4) 0.007(3) -0.006(2) 0.007(2) 0.005(3) C22 0.024(3) 0.026(4) 0.018(4) 0.000(2) 0.002(2) 0.002(3) C23 0.020(3) 0.031(4) 0.020(4) 0.002(3) -0.001(2) 0.000(3) C24 0.027(3) 0.057(5) 0.018(4) 0.011(3) -0.004(3) -0.009(3) C25 0.035(4) 0.053(5) 0.032(5) 0.006(3) -0.004(3) -0.016(4) C26 0.022(3) 0.049(5) 0.030(4) -0.014(3) 0.005(3) -0.010(3) C27 0.023(3) 0.038(4) 0.029(4) -0.011(3) -0.007(3) 0.012(3) C28 0.028(3) 0.033(4) 0.031(4) -0.003(3) -0.003(3) 0.006(3) C29 0.031(3) 0.028(4) 0.023(4) -0.005(3) -0.007(3) -0.001(3) C30 0.019(3) 0.043(4) 0.012(3) -0.004(3) 0.003(2) -0.003(3) C31 0.021(3) 0.036(4) 0.019(4) 0.005(3) -0.004(2) -0.001(3) C32 0.025(3) 0.031(4) 0.024(4) 0.008(3) 0.002(3) 0.005(3) C33 0.028(3) 0.024(4) 0.021(4) 0.002(2) 0.008(3) 0.002(3) C34 0.028(3) 0.027(4) 0.022(4) -0.007(3) -0.003(3) -0.003(3) C35 0.030(3) 0.037(4) 0.040(5) -0.001(3) 0.004(3) -0.011(3) C36 0.028(3) 0.027(4) 0.024(4) 0.006(3) 0.004(3) -0.003(3) C37 0.039(3) 0.030(4) 0.026(4) 0.001(3) 0.005(3) -0.012(3) C38 0.040(4) 0.020(4) 0.035(4) -0.007(3) 0.002(3) 0.000(3) C39 0.034(3) 0.022(4) 0.039(4) -0.006(3) 0.000(3) 0.002(3) C40 0.025(3) 0.019(3) 0.033(4) 0.000(3) 0.000(3) 0.004(3) C41 0.024(3) 0.032(4) 0.031(4) 0.003(3) 0.000(3) -0.005(3) C42 0.028(3) 0.035(4) 0.037(5) -0.008(3) 0.008(3) -0.004(3) C43 0.023(3) 0.030(4) 0.029(4) 0.000(3) 0.006(3) -0.004(3) C44 0.031(3) 0.038(4) 0.038(5) 0.001(3) 0.003(3) -0.006(3) C45 0.027(3) 0.064(6) 0.049(5) 0.009(4) 0.004(3) 0.016(4) C46 0.040(4) 0.066(6) 0.025(4) 0.012(4) 0.005(3) -0.018(4) C47 0.051(5) 0.052(5) 0.054(6) -0.010(4) 0.022(4) -0.023(4) C48 0.043(4) 0.050(5) 0.046(5) -0.012(4) 0.020(4) -0.021(4) C49 0.048(4) 0.020(4) 0.034(4) 0.007(3) 0.006(3) -0.005(3) C50 0.043(4) 0.029(4) 0.017(4) 0.006(3) 0.009(3) 0.012(3) C51 0.053(4) 0.022(4) 0.043(5) 0.011(3) 0.009(4) 0.004(3) C52 0.062(5) 0.049(5) 0.030(5) 0.016(4) -0.014(4) -0.001(4) C53 0.052(4) 0.045(5) 0.031(5) 0.005(3) -0.009(4) -0.005(4) C54 0.040(3) 0.026(4) 0.017(4) 0.001(2) 0.003(3) 0.006(3) C55 0.033(3) 0.024(4) 0.022(4) -0.001(2) -0.003(3) -0.003(3) C56 0.027(3) 0.021(4) 0.029(4) -0.005(3) 0.003(3) -0.004(3) C57 0.022(3) 0.017(3) 0.028(4) -0.002(2) -0.003(3) -0.003(3) C58 0.032(3) 0.025(4) 0.027(4) -0.009(3) 0.001(3) -0.003(3) C59 0.045(4) 0.026(4) 0.025(4) -0.009(3) -0.007(3) 0.010(3) C60 0.053(4) 0.024(4) 0.026(4) -0.002(3) -0.003(3) -0.003(3) C61 0.032(3) 0.044(5) 0.025(4) -0.002(3) 0.000(3) -0.001(3) C62 0.031(3) 0.034(4) 0.030(4) 0.002(3) 0.000(3) -0.003(3) C63 0.039(4) 0.032(4) 0.034(5) 0.005(3) 0.016(3) 0.002(3) C64 0.031(3) 0.039(4) 0.018(4) -0.001(3) 0.000(3) -0.003(3) C65 0.029(3) 0.056(5) 0.030(4) -0.005(3) 0.002(3) 0.001(3) C66 0.043(4) 0.043(5) 0.039(5) -0.004(3) 0.006(3) 0.020(4) C67 0.057(5) 0.041(5) 0.030(5) 0.000(3) 0.003(4) 0.016(4) C68 0.042(4) 0.038(4) 0.023(4) 0.004(3) 0.003(3) 0.006(3) C69 0.071(6) 0.112(10) 0.053(7) -0.046(7) 0.001(5) -0.015(7) C70 0.035(4) 0.102(9) 0.023(5) -0.003(5) 0.000(3) -0.019(5) N1 0.027(2) 0.030(3) 0.019(3) 0.002(2) 0.001(2) -0.008(2) N2 0.028(2) 0.030(3) 0.008(3) -0.003(2) 0.001(2) 0.006(2) N3 0.020(2) 0.021(3) 0.021(3) 0.000(2) 0.002(2) -0.007(2) N4 0.021(2) 0.027(3) 0.019(3) 0.001(2) -0.005(2) -0.002(2) N5 0.026(2) 0.021(3) 0.012(3) 0.0019(19) 0.004(2) 0.001(2) N6 0.029(3) 0.016(3) 0.026(3) 0.002(2) -0.004(2) -0.003(2) N7 0.018(2) 0.034(3) 0.018(3) 0.006(2) -0.0006(19) 0.000(2) N8 0.020(2) 0.018(3) 0.019(3) 0.0060(19) -0.001(2) 0.000(2) N9 0.030(3) 0.020(3) 0.028(3) 0.003(2) 0.011(2) -0.002(2) N10 0.030(3) 0.026(3) 0.027(3) -0.002(2) 0.001(2) -0.009(2) N11 0.034(3) 0.016(3) 0.024(3) 0.006(2) 0.005(2) 0.005(2) N12 0.033(3) 0.028(3) 0.024(3) 0.007(2) -0.001(2) 0.000(2) N13 0.028(3) 0.021(3) 0.028(3) -0.010(2) 0.004(2) -0.002(2) N14 0.025(2) 0.026(3) 0.030(3) -0.008(2) 0.006(2) -0.004(2) N15 0.032(3) 0.024(3) 0.022(3) 0.008(2) 0.003(2) -0.003(2) N16 0.034(3) 0.014(3) 0.030(3) -0.003(2) 0.007(2) -0.003(2) N17 0.043(4) 0.125(9) 0.044(5) 0.028(5) -0.008(3) -0.025(5) O1 0.0215(19) 0.030(3) 0.025(3) -0.0015(18) 0.0015(18) 0.0037(19) O2 0.023(2) 0.027(3) 0.037(3) 0.015(2) -0.0031(19) -0.0036(19) O3 0.033(2) 0.032(3) 0.058(4) -0.020(2) 0.008(2) -0.006(2) O4 0.028(2) 0.027(3) 0.033(3) -0.0027(19) 0.0068(19) 0.005(2) O5 0.073(4) 0.048(4) 0.058(4) -0.025(3) -0.005(3) 0.014(3) O6 0.039(3) 0.055(3) 0.031(3) 0.009(2) -0.008(2) -0.004(2) O7 0.047(3) 0.038(3) 0.062(4) 0.026(3) -0.003(3) 0.001(3) O8 0.029(2) 0.079(4) 0.058(4) 0.014(3) 0.004(2) 0.006(3) O9 0.117(6) 0.029(4) 0.097(6) -0.010(3) 0.043(5) -0.009(4) O10 0.093(5) 0.086(6) 0.166(9) 0.071(6) -0.018(6) 0.003(5) O11 0.069(4) 0.137(8) 0.093(6) -0.070(5) 0.024(4) -0.008(5) O12 0.044(3) 0.111(6) 0.100(6) -0.019(5) 0.003(4) 0.011(4) O13 0.042(3) 0.057(4) 0.029(3) 0.012(2) -0.004(2) 0.002(3) O14 0.034(2) 0.028(3) 0.039(3) -0.001(2) 0.004(2) -0.009(2) O15 0.037(3) 0.040(3) 0.055(4) -0.026(3) 0.004(2) 0.003(2) O16 0.035(2) 0.064(4) 0.029(3) 0.016(2) 0.006(2) -0.015(3) O17 0.051(3) 0.024(3) 0.073(4) -0.005(3) 0.007(3) 0.007(2) O18 0.044(3) 0.158(8) 0.060(5) 0.002(5) 0.015(3) -0.014(4) O19 0.086(4) 0.054(4) 0.039(4) -0.003(3) -0.028(3) 0.019(3) O20 0.061(3) 0.053(4) 0.048(4) -0.028(3) -0.012(3) 0.008(3) S1 0.0338(8) 0.0299(9) 0.0239(10) -0.0007(7) -0.0080(7) 0.0020(7) S2 0.0198(6) 0.0216(8) 0.0206(9) -0.0033(6) -0.0023(6) 0.0007(6) S3 0.0278(7) 0.0193(8) 0.0297(10) 0.0033(6) 0.0038(6) -0.0019(6) S4 0.0500(10) 0.0345(11) 0.0330(12) -0.0012(8) 0.0162(8) -0.0015(9) Cl1 0.0265(7) 0.0276(9) 0.0263(9) 0.0013(6) 0.0030(6) 0.0027(7) Cl2 0.0402(9) 0.0340(11) 0.0565(14) -0.0060(8) -0.0058(9) 0.0084(8) Cl3 0.0283(7) 0.0316(9) 0.0213(9) -0.0018(6) 0.0026(6) -0.0025(7) Cl4 0.0371(8) 0.0442(11) 0.0309(11) -0.0062(7) -0.0026(7) 0.0073(8) Zn1 0.0200(3) 0.0216(4) 0.0170(4) -0.0035(3) -0.0009(3) -0.0017(3) Zn2 0.0292(4) 0.0208(4) 0.0211(4) 0.0027(3) 0.0037(3) -0.0029(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.454(8) . ? C1 C2 1.525(9) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 N2 1.330(8) . ? C2 C3 1.381(9) . ? C3 C4 1.374(10) . ? C3 H3 0.9500 . ? C4 C5 1.383(10) . ? C4 H4 0.9500 . ? C5 C6 1.372(9) . ? C5 H5 0.9500 . ? C6 N2 1.342(8) . ? C6 N5 1.425(8) . ? C7 N5 1.342(8) . ? C7 N6 1.364(8) . ? C7 S1 1.670(6) . ? C8 O1 1.222(7) . ? C8 N6 1.400(7) . ? C8 C9 1.487(9) . ? C9 C14 1.386(8) . ? C9 C10 1.406(8) . ? C10 C11 1.368(9) . ? C10 H10 0.9500 . ? C11 C12 1.374(10) . ? C11 H11 0.9500 . ? C12 C13 1.375(9) . ? C12 H12 0.9500 . ? C13 C14 1.389(9) . ? C13 H13 0.9500 . ? C14 H14 0.9500 . ? C15 N1 1.454(8) . ? C15 C16 1.498(9) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 N3 1.346(7) . ? C16 C17 1.401(9) . ? C17 C18 1.370(10) . ? C17 H17 0.9500 . ? C18 C19 1.377(9) . ? C18 H18 0.9500 . ? C19 C20 1.388(8) . ? C19 H19 0.9500 . ? C20 N3 1.343(8) . ? C20 N7 1.420(7) . ? C21 N7 1.342(8) . ? C21 N8 1.359(7) . ? C21 S2 1.689(6) . ? C22 O2 1.223(7) . ? C22 N8 1.398(7) . ? C22 C23 1.508(8) . ? C23 C24 1.398(9) . ? C23 C28 1.410(9) . ? C24 C25 1.381(9) . ? C24 H24 0.9500 . ? C25 C26 1.382(10) . ? C25 H25 0.9500 . ? C26 C27 1.385(10) . ? C26 H26 0.9500 . ? C27 C28 1.409(9) . ? C27 H27 0.9500 . ? C28 H28 0.9500 . ? C29 N1 1.485(8) . ? C29 C30 1.506(9) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C30 N4 1.365(7) . ? C30 C31 1.384(8) . ? C31 C32 1.378(9) . ? C31 H31 0.9500 . ? C32 C33 1.394(9) . ? C32 H32 0.9500 . ? C33 C34 1.394(9) . ? C33 H33 0.9500 . ? C34 N4 1.333(8) . ? C34 H34 0.9500 . ? C35 N9 1.487(9) . ? C35 C36 1.499(9) . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? C36 N10 1.337(8) . ? C36 C37 1.382(9) . ? C37 C38 1.384(9) . ? C37 H37 0.9500 . ? C38 C39 1.381(9) . ? C38 H38 0.9500 . ? C39 C40 1.379(9) . ? C39 H39 0.9500 . ? C40 N10 1.353(8) . ? C40 N13 1.397(8) . ? C41 N13 1.338(8) . ? C41 N14 1.367(8) . ? C41 S3 1.689(7) . ? C42 O3 1.221(8) . ? C42 N14 1.390(8) . ? C42 C43 1.480(9) . ? C43 C44 1.376(9) . ? C43 C48 1.409(10) . ? C44 C45 1.389(10) . ? C44 H44 0.9500 . ? C45 C46 1.365(12) . ? C45 H45 0.9500 . ? C46 C47 1.383(12) . ? C46 H46 0.9500 . ? C47 C48 1.384(10) . ? C47 H47 0.9500 . ? C48 H48 0.9500 . ? C49 N9 1.489(8) . ? C49 C50 1.523(10) . ? C49 H49A 0.9900 . ? C49 H49B 0.9900 . ? C50 N11 1.359(8) . ? C50 C51 1.387(9) . ? C51 C52 1.385(11) . ? C51 H51 0.9500 . ? C52 C53 1.367(11) . ? C52 H52 0.9500 . ? C53 C54 1.383(9) . ? C53 H53 0.9500 . ? C54 N11 1.346(8) . ? C54 N15 1.412(8) . ? C55 N15 1.342(8) . ? C55 N16 1.393(8) . ? C55 S4 1.652(7) . ? C56 O4 1.224(7) . ? C56 N16 1.390(8) . ? C56 C57 1.485(9) . ? C57 C58 1.391(9) . ? C57 C62 1.396(8) . ? C58 C59 1.397(9) . ? C58 H58 0.9500 . ? C59 C60 1.378(10) . ? C59 H59 0.9500 . ? C60 C61 1.393(10) . ? C60 H60 0.9500 . ? C61 C62 1.375(10) . ? C61 H61 0.9500 . ? C62 H62 0.9500 . ? C63 N9 1.463(8) . ? C63 C64 1.513(10) . ? C63 H63A 0.9900 . ? C63 H63B 0.9900 . ? C64 N12 1.344(8) . ? C64 C65 1.384(10) . ? C65 C66 1.390(11) . ? C65 H65 0.9500 . ? C66 C67 1.375(11) . ? C66 H66 0.9500 . ? C67 C68 1.384(10) . ? C67 H67 0.9500 . ? C68 N12 1.349(9) . ? C68 H68 0.9500 . ? C69 C70 1.439(16) . ? C69 H69A 0.9800 . ? C69 H69B 0.9800 . ? C69 H69C 0.9800 . ? C70 N17 1.105(13) . ? N1 Zn1 2.181(5) . ? N2 Zn1 2.078(5) . ? N3 Zn1 2.131(5) . ? N4 Zn1 2.058(5) . ? N5 H5A 0.8800 . ? N6 H6 0.8800 . ? N7 H7 0.8800 . ? N8 H8 0.8800 . ? N9 Zn2 2.163(5) . ? N10 Zn2 2.134(5) . ? N11 Zn2 2.066(5) . ? N12 Zn2 2.054(5) . ? N13 H13A 0.8800 . ? N14 H14A 0.8800 . ? N15 H15 0.8800 . ? N16 H16 0.8800 . ? O5 Cl1 1.412(5) . ? O6 Cl1 1.441(5) . ? O7 Cl1 1.425(5) . ? O8 Cl1 1.420(5) . ? O9 Cl2 1.408(6) . ? O10 Cl2 1.356(7) . ? O11 Cl2 1.446(7) . ? O12 Cl2 1.413(6) . ? O13 Cl3 1.430(5) . ? O14 Cl3 1.446(5) . ? O15 Cl3 1.436(5) . ? O16 Cl3 1.432(5) . ? O17 Cl4 1.424(5) . ? O18 Cl4 1.407(6) . ? O19 Cl4 1.443(5) . ? O20 Cl4 1.437(5) . ? S2 Zn1 2.3716(15) . ? S3 Zn2 2.3653(17) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 C2 111.8(5) . . ? N1 C1 H1A 109.3 . . ? C2 C1 H1A 109.3 . . ? N1 C1 H1B 109.3 . . ? C2 C1 H1B 109.3 . . ? H1A C1 H1B 107.9 . . ? N2 C2 C3 122.3(6) . . ? N2 C2 C1 116.5(6) . . ? C3 C2 C1 121.1(6) . . ? C4 C3 C2 118.8(6) . . ? C4 C3 H3 120.6 . . ? C2 C3 H3 120.6 . . ? C3 C4 C5 119.8(6) . . ? C3 C4 H4 120.1 . . ? C5 C4 H4 120.1 . . ? C6 C5 C4 117.4(7) . . ? C6 C5 H5 121.3 . . ? C4 C5 H5 121.3 . . ? N2 C6 C5 123.7(6) . . ? N2 C6 N5 116.5(5) . . ? C5 C6 N5 119.7(6) . . ? N5 C7 N6 116.8(5) . . ? N5 C7 S1 123.5(5) . . ? N6 C7 S1 119.7(5) . . ? O1 C8 N6 121.1(6) . . ? O1 C8 C9 123.4(5) . . ? N6 C8 C9 115.4(5) . . ? C14 C9 C10 120.1(6) . . ? C14 C9 C8 121.1(5) . . ? C10 C9 C8 118.7(5) . . ? C11 C10 C9 119.4(6) . . ? C11 C10 H10 120.3 . . ? C9 C10 H10 120.3 . . ? C10 C11 C12 120.0(6) . . ? C10 C11 H11 120.0 . . ? C12 C11 H11 120.0 . . ? C13 C12 C11 121.5(6) . . ? C13 C12 H12 119.3 . . ? C11 C12 H12 119.3 . . ? C12 C13 C14 119.3(6) . . ? C12 C13 H13 120.3 . . ? C14 C13 H13 120.3 . . ? C9 C14 C13 119.6(6) . . ? C9 C14 H14 120.2 . . ? C13 C14 H14 120.2 . . ? N1 C15 C16 111.2(5) . . ? N1 C15 H15A 109.4 . . ? C16 C15 H15A 109.4 . . ? N1 C15 H15B 109.4 . . ? C16 C15 H15B 109.4 . . ? H15A C15 H15B 108.0 . . ? N3 C16 C17 122.3(6) . . ? N3 C16 C15 116.6(6) . . ? C17 C16 C15 121.1(6) . . ? C18 C17 C16 118.5(6) . . ? C18 C17 H17 120.7 . . ? C16 C17 H17 120.7 . . ? C17 C18 C19 119.9(7) . . ? C17 C18 H18 120.1 . . ? C19 C18 H18 120.1 . . ? C18 C19 C20 118.4(6) . . ? C18 C19 H19 120.8 . . ? C20 C19 H19 120.8 . . ? N3 C20 C19 123.0(5) . . ? N3 C20 N7 120.4(5) . . ? C19 C20 N7 116.5(5) . . ? N7 C21 N8 116.0(5) . . ? N7 C21 S2 126.3(4) . . ? N8 C21 S2 117.7(5) . . ? O2 C22 N8 121.6(5) . . ? O2 C22 C23 121.7(5) . . ? N8 C22 C23 116.7(5) . . ? C24 C23 C28 121.0(6) . . ? C24 C23 C22 123.7(5) . . ? C28 C23 C22 115.3(6) . . ? C25 C24 C23 118.5(6) . . ? C25 C24 H24 120.7 . . ? C23 C24 H24 120.7 . . ? C24 C25 C26 121.9(7) . . ? C24 C25 H25 119.0 . . ? C26 C25 H25 119.0 . . ? C25 C26 C27 119.8(6) . . ? C25 C26 H26 120.1 . . ? C27 C26 H26 120.1 . . ? C26 C27 C28 120.4(6) . . ? C26 C27 H27 119.8 . . ? C28 C27 H27 119.8 . . ? C27 C28 C23 118.4(7) . . ? C27 C28 H28 120.8 . . ? C23 C28 H28 120.8 . . ? N1 C29 C30 110.9(5) . . ? N1 C29 H29A 109.5 . . ? C30 C29 H29A 109.5 . . ? N1 C29 H29B 109.5 . . ? C30 C29 H29B 109.5 . . ? H29A C29 H29B 108.1 . . ? N4 C30 C31 120.8(6) . . ? N4 C30 C29 116.9(5) . . ? C31 C30 C29 122.1(5) . . ? C32 C31 C30 120.0(6) . . ? C32 C31 H31 120.0 . . ? C30 C31 H31 120.0 . . ? C31 C32 C33 119.0(6) . . ? C31 C32 H32 120.5 . . ? C33 C32 H32 120.5 . . ? C32 C33 C34 118.4(6) . . ? C32 C33 H33 120.8 . . ? C34 C33 H33 120.8 . . ? N4 C34 C33 122.2(6) . . ? N4 C34 H34 118.9 . . ? C33 C34 H34 118.9 . . ? N9 C35 C36 111.2(5) . . ? N9 C35 H35A 109.4 . . ? C36 C35 H35A 109.4 . . ? N9 C35 H35B 109.4 . . ? C36 C35 H35B 109.4 . . ? H35A C35 H35B 108.0 . . ? N10 C36 C37 122.7(6) . . ? N10 C36 C35 117.4(6) . . ? C37 C36 C35 119.8(6) . . ? C36 C37 C38 118.3(6) . . ? C36 C37 H37 120.8 . . ? C38 C37 H37 120.8 . . ? C39 C38 C37 119.6(6) . . ? C39 C38 H38 120.2 . . ? C37 C38 H38 120.2 . . ? C40 C39 C38 118.9(7) . . ? C40 C39 H39 120.6 . . ? C38 C39 H39 120.6 . . ? N10 C40 C39 121.9(6) . . ? N10 C40 N13 119.0(6) . . ? C39 C40 N13 118.7(6) . . ? N13 C41 N14 115.9(6) . . ? N13 C41 S3 126.6(5) . . ? N14 C41 S3 117.5(5) . . ? O3 C42 N14 122.2(6) . . ? O3 C42 C43 122.8(6) . . ? N14 C42 C43 115.1(6) . . ? C44 C43 C48 118.6(6) . . ? C44 C43 C42 118.2(6) . . ? C48 C43 C42 123.1(6) . . ? C43 C44 C45 121.2(7) . . ? C43 C44 H44 119.4 . . ? C45 C44 H44 119.4 . . ? C46 C45 C44 119.6(7) . . ? C46 C45 H45 120.2 . . ? C44 C45 H45 120.2 . . ? C45 C46 C47 120.7(7) . . ? C45 C46 H46 119.6 . . ? C47 C46 H46 119.6 . . ? C46 C47 C48 120.0(8) . . ? C46 C47 H47 120.0 . . ? C48 C47 H47 120.0 . . ? C47 C48 C43 119.8(8) . . ? C47 C48 H48 120.1 . . ? C43 C48 H48 120.1 . . ? N9 C49 C50 108.7(5) . . ? N9 C49 H49A 110.0 . . ? C50 C49 H49A 110.0 . . ? N9 C49 H49B 110.0 . . ? C50 C49 H49B 110.0 . . ? H49A C49 H49B 108.3 . . ? N11 C50 C51 121.5(7) . . ? N11 C50 C49 116.5(6) . . ? C51 C50 C49 122.0(6) . . ? C52 C51 C50 119.0(7) . . ? C52 C51 H51 120.5 . . ? C50 C51 H51 120.5 . . ? C53 C52 C51 119.7(7) . . ? C53 C52 H52 120.1 . . ? C51 C52 H52 120.1 . . ? C52 C53 C54 118.8(7) . . ? C52 C53 H53 120.6 . . ? C54 C53 H53 120.6 . . ? N11 C54 C53 122.7(6) . . ? N11 C54 N15 116.5(5) . . ? C53 C54 N15 120.9(6) . . ? N15 C55 N16 115.8(6) . . ? N15 C55 S4 123.3(5) . . ? N16 C55 S4 120.8(5) . . ? O4 C56 N16 122.0(6) . . ? O4 C56 C57 122.3(6) . . ? N16 C56 C57 115.7(5) . . ? C58 C57 C62 120.8(6) . . ? C58 C57 C56 121.9(5) . . ? C62 C57 C56 117.1(5) . . ? C57 C58 C59 118.8(6) . . ? C57 C58 H58 120.6 . . ? C59 C58 H58 120.6 . . ? C60 C59 C58 120.4(6) . . ? C60 C59 H59 119.8 . . ? C58 C59 H59 119.8 . . ? C59 C60 C61 120.1(7) . . ? C59 C60 H60 119.9 . . ? C61 C60 H60 119.9 . . ? C62 C61 C60 120.3(6) . . ? C62 C61 H61 119.8 . . ? C60 C61 H61 119.8 . . ? C61 C62 C57 119.5(6) . . ? C61 C62 H62 120.2 . . ? C57 C62 H62 120.2 . . ? N9 C63 C64 110.8(5) . . ? N9 C63 H63A 109.5 . . ? C64 C63 H63A 109.5 . . ? N9 C63 H63B 109.5 . . ? C64 C63 H63B 109.5 . . ? H63A C63 H63B 108.1 . . ? N12 C64 C65 120.7(7) . . ? N12 C64 C63 116.0(6) . . ? C65 C64 C63 123.1(6) . . ? C64 C65 C66 121.1(7) . . ? C64 C65 H65 119.4 . . ? C66 C65 H65 119.4 . . ? C67 C66 C65 117.7(7) . . ? C67 C66 H66 121.1 . . ? C65 C66 H66 121.1 . . ? C66 C67 C68 118.8(7) . . ? C66 C67 H67 120.6 . . ? C68 C67 H67 120.6 . . ? N12 C68 C67 123.4(7) . . ? N12 C68 H68 118.3 . . ? C67 C68 H68 118.3 . . ? C70 C69 H69A 109.5 . . ? C70 C69 H69B 109.5 . . ? H69A C69 H69B 109.5 . . ? C70 C69 H69C 109.5 . . ? H69A C69 H69C 109.5 . . ? H69B C69 H69C 109.5 . . ? N17 C70 C69 177.7(10) . . ? C1 N1 C15 114.4(5) . . ? C1 N1 C29 112.3(5) . . ? C15 N1 C29 112.3(5) . . ? C1 N1 Zn1 105.4(3) . . ? C15 N1 Zn1 106.4(4) . . ? C29 N1 Zn1 105.2(4) . . ? C2 N2 C6 117.9(5) . . ? C2 N2 Zn1 114.7(4) . . ? C6 N2 Zn1 127.3(4) . . ? C20 N3 C16 117.8(5) . . ? C20 N3 Zn1 128.3(4) . . ? C16 N3 Zn1 113.8(4) . . ? C34 N4 C30 119.4(5) . . ? C34 N4 Zn1 126.3(4) . . ? C30 N4 Zn1 114.2(4) . . ? C7 N5 C6 122.7(5) . . ? C7 N5 H5A 118.6 . . ? C6 N5 H5A 118.6 . . ? C7 N6 C8 129.7(5) . . ? C7 N6 H6 115.2 . . ? C8 N6 H6 115.2 . . ? C21 N7 C20 130.9(5) . . ? C21 N7 H7 114.5 . . ? C20 N7 H7 114.5 . . ? C21 N8 C22 127.5(5) . . ? C21 N8 H8 116.3 . . ? C22 N8 H8 116.3 . . ? C63 N9 C35 112.0(5) . . ? C63 N9 C49 113.2(5) . . ? C35 N9 C49 111.7(5) . . ? C63 N9 Zn2 107.9(4) . . ? C35 N9 Zn2 106.1(4) . . ? C49 N9 Zn2 105.4(4) . . ? C36 N10 C40 118.6(5) . . ? C36 N10 Zn2 113.4(4) . . ? C40 N10 Zn2 127.4(4) . . ? C54 N11 C50 118.2(6) . . ? C54 N11 Zn2 127.5(4) . . ? C50 N11 Zn2 114.2(4) . . ? C64 N12 C68 118.2(6) . . ? C64 N12 Zn2 116.3(4) . . ? C68 N12 Zn2 125.4(5) . . ? C41 N13 C40 130.7(6) . . ? C41 N13 H13A 114.7 . . ? C40 N13 H13A 114.7 . . ? C41 N14 C42 127.9(6) . . ? C41 N14 H14A 116.0 . . ? C42 N14 H14A 116.0 . . ? C55 N15 C54 120.5(5) . . ? C55 N15 H15 119.7 . . ? C54 N15 H15 119.7 . . ? C56 N16 C55 127.9(5) . . ? C56 N16 H16 116.1 . . ? C55 N16 H16 116.1 . . ? C21 S2 Zn1 101.1(2) . . ? C41 S3 Zn2 100.5(2) . . ? O5 Cl1 O8 109.7(4) . . ? O5 Cl1 O7 110.1(4) . . ? O8 Cl1 O7 109.6(3) . . ? O5 Cl1 O6 108.5(3) . . ? O8 Cl1 O6 110.3(3) . . ? O7 Cl1 O6 108.7(3) . . ? O10 Cl2 O9 112.0(6) . . ? O10 Cl2 O12 111.0(5) . . ? O9 Cl2 O12 110.4(5) . . ? O10 Cl2 O11 106.2(6) . . ? O9 Cl2 O11 107.2(5) . . ? O12 Cl2 O11 109.9(4) . . ? O13 Cl3 O16 109.8(3) . . ? O13 Cl3 O15 111.1(3) . . ? O16 Cl3 O15 108.5(3) . . ? O13 Cl3 O14 110.2(3) . . ? O16 Cl3 O14 108.6(3) . . ? O15 Cl3 O14 108.6(3) . . ? O18 Cl4 O17 110.6(4) . . ? O18 Cl4 O20 111.0(4) . . ? O17 Cl4 O20 109.2(3) . . ? O18 Cl4 O19 109.3(4) . . ? O17 Cl4 O19 108.6(4) . . ? O20 Cl4 O19 108.1(4) . . ? N4 Zn1 N2 113.8(2) . . ? N4 Zn1 N3 121.05(19) . . ? N2 Zn1 N3 114.5(2) . . ? N4 Zn1 N1 80.6(2) . . ? N2 Zn1 N1 79.3(2) . . ? N3 Zn1 N1 77.16(19) . . ? N4 Zn1 S2 99.70(14) . . ? N2 Zn1 S2 114.35(14) . . ? N3 Zn1 S2 89.42(13) . . ? N1 Zn1 S2 164.19(15) . . ? N12 Zn2 N11 111.5(2) . . ? N12 Zn2 N10 122.8(2) . . ? N11 Zn2 N10 115.0(2) . . ? N12 Zn2 N9 79.3(2) . . ? N11 Zn2 N9 79.8(2) . . ? N10 Zn2 N9 78.1(2) . . ? N12 Zn2 S3 99.24(16) . . ? N11 Zn2 S3 115.22(15) . . ? N10 Zn2 S3 89.58(15) . . ? N9 Zn2 S3 163.92(15) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 C1 C2 N2 -24.9(8) . . . . ? N1 C1 C2 C3 156.6(6) . . . . ? N2 C2 C3 C4 -1.7(10) . . . . ? C1 C2 C3 C4 176.7(6) . . . . ? C2 C3 C4 C5 2.6(10) . . . . ? C3 C4 C5 C6 -1.7(10) . . . . ? C4 C5 C6 N2 -0.2(9) . . . . ? C4 C5 C6 N5 -178.5(6) . . . . ? O1 C8 C9 C14 141.8(6) . . . . ? N6 C8 C9 C14 -37.0(8) . . . . ? O1 C8 C9 C10 -35.8(9) . . . . ? N6 C8 C9 C10 145.4(6) . . . . ? C14 C9 C10 C11 -1.8(10) . . . . ? C8 C9 C10 C11 175.9(6) . . . . ? C9 C10 C11 C12 0.3(11) . . . . ? C10 C11 C12 C13 0.8(11) . . . . ? C11 C12 C13 C14 -0.3(11) . . . . ? C10 C9 C14 C13 2.2(9) . . . . ? C8 C9 C14 C13 -175.4(6) . . . . ? C12 C13 C14 C9 -1.1(10) . . . . ? N1 C15 C16 N3 -25.3(8) . . . . ? N1 C15 C16 C17 152.9(6) . . . . ? N3 C16 C17 C18 -2.8(9) . . . . ? C15 C16 C17 C18 179.2(6) . . . . ? C16 C17 C18 C19 1.2(10) . . . . ? C17 C18 C19 C20 1.0(11) . . . . ? C18 C19 C20 N3 -1.9(10) . . . . ? C18 C19 C20 N7 174.8(6) . . . . ? O2 C22 C23 C24 177.5(6) . . . . ? N8 C22 C23 C24 -0.9(9) . . . . ? O2 C22 C23 C28 -1.5(9) . . . . ? N8 C22 C23 C28 -179.9(6) . . . . ? C28 C23 C24 C25 0.6(11) . . . . ? C22 C23 C24 C25 -178.4(7) . . . . ? C23 C24 C25 C26 -0.3(12) . . . . ? C24 C25 C26 C27 0.0(11) . . . . ? C25 C26 C27 C28 0.1(10) . . . . ? C26 C27 C28 C23 0.2(10) . . . . ? C24 C23 C28 C27 -0.5(10) . . . . ? C22 C23 C28 C27 178.5(6) . . . . ? N1 C29 C30 N4 -30.6(8) . . . . ? N1 C29 C30 C31 155.7(6) . . . . ? N4 C30 C31 C32 0.2(9) . . . . ? C29 C30 C31 C32 173.6(6) . . . . ? C30 C31 C32 C33 -2.4(9) . . . . ? C31 C32 C33 C34 3.6(9) . . . . ? C32 C33 C34 N4 -2.8(9) . . . . ? N9 C35 C36 N10 -23.2(9) . . . . ? N9 C35 C36 C37 158.8(6) . . . . ? N10 C36 C37 C38 -0.3(10) . . . . ? C35 C36 C37 C38 177.6(6) . . . . ? C36 C37 C38 C39 0.0(10) . . . . ? C37 C38 C39 C40 -0.6(10) . . . . ? C38 C39 C40 N10 1.4(10) . . . . ? C38 C39 C40 N13 174.1(6) . . . . ? O3 C42 C43 C44 -17.4(11) . . . . ? N14 C42 C43 C44 163.7(6) . . . . ? O3 C42 C43 C48 157.8(8) . . . . ? N14 C42 C43 C48 -21.1(10) . . . . ? C48 C43 C44 C45 3.4(11) . . . . ? C42 C43 C44 C45 178.8(7) . . . . ? C43 C44 C45 C46 -2.2(12) . . . . ? C44 C45 C46 C47 0.0(12) . . . . ? C45 C46 C47 C48 0.9(13) . . . . ? C46 C47 C48 C43 0.4(13) . . . . ? C44 C43 C48 C47 -2.4(12) . . . . ? C42 C43 C48 C47 -177.6(8) . . . . ? N9 C49 C50 N11 -32.1(8) . . . . ? N9 C49 C50 C51 147.2(6) . . . . ? N11 C50 C51 C52 -3.2(11) . . . . ? C49 C50 C51 C52 177.5(7) . . . . ? C50 C51 C52 C53 1.6(12) . . . . ? C51 C52 C53 C54 1.3(12) . . . . ? C52 C53 C54 N11 -2.7(11) . . . . ? C52 C53 C54 N15 177.1(7) . . . . ? O4 C56 C57 C58 146.4(6) . . . . ? N16 C56 C57 C58 -34.3(8) . . . . ? O4 C56 C57 C62 -27.7(9) . . . . ? N16 C56 C57 C62 151.6(6) . . . . ? C62 C57 C58 C59 -0.1(9) . . . . ? C56 C57 C58 C59 -174.0(6) . . . . ? C57 C58 C59 C60 0.4(9) . . . . ? C58 C59 C60 C61 -0.8(10) . . . . ? C59 C60 C61 C62 0.8(10) . . . . ? C60 C61 C62 C57 -0.5(10) . . . . ? C58 C57 C62 C61 0.2(10) . . . . ? C56 C57 C62 C61 174.3(6) . . . . ? N9 C63 C64 N12 -26.2(8) . . . . ? N9 C63 C64 C65 158.0(6) . . . . ? N12 C64 C65 C66 -2.9(10) . . . . ? C63 C64 C65 C66 172.7(7) . . . . ? C64 C65 C66 C67 1.7(11) . . . . ? C65 C66 C67 C68 0.0(11) . . . . ? C66 C67 C68 N12 -0.4(11) . . . . ? C2 C1 N1 C15 152.7(5) . . . . ? C2 C1 N1 C29 -77.8(6) . . . . ? C2 C1 N1 Zn1 36.3(6) . . . . ? C16 C15 N1 C1 -75.9(6) . . . . ? C16 C15 N1 C29 154.7(5) . . . . ? C16 C15 N1 Zn1 40.1(6) . . . . ? C30 C29 N1 C1 151.1(5) . . . . ? C30 C29 N1 C15 -78.4(6) . . . . ? C30 C29 N1 Zn1 36.9(6) . . . . ? C3 C2 N2 C6 -0.2(9) . . . . ? C1 C2 N2 C6 -178.7(5) . . . . ? C3 C2 N2 Zn1 176.4(5) . . . . ? C1 C2 N2 Zn1 -2.1(7) . . . . ? C5 C6 N2 C2 1.2(9) . . . . ? N5 C6 N2 C2 179.5(5) . . . . ? C5 C6 N2 Zn1 -174.9(5) . . . . ? N5 C6 N2 Zn1 3.4(7) . . . . ? C19 C20 N3 C16 0.4(9) . . . . ? N7 C20 N3 C16 -176.1(5) . . . . ? C19 C20 N3 Zn1 -174.5(5) . . . . ? N7 C20 N3 Zn1 9.0(8) . . . . ? C17 C16 N3 C20 1.9(9) . . . . ? C15 C16 N3 C20 -179.9(5) . . . . ? C17 C16 N3 Zn1 177.6(5) . . . . ? C15 C16 N3 Zn1 -4.3(7) . . . . ? C33 C34 N4 C30 0.7(9) . . . . ? C33 C34 N4 Zn1 -178.3(4) . . . . ? C31 C30 N4 C34 0.7(9) . . . . ? C29 C30 N4 C34 -173.1(6) . . . . ? C31 C30 N4 Zn1 179.8(4) . . . . ? C29 C30 N4 Zn1 6.0(7) . . . . ? N6 C7 N5 C6 -171.7(5) . . . . ? S1 C7 N5 C6 6.4(8) . . . . ? N2 C6 N5 C7 73.4(7) . . . . ? C5 C6 N5 C7 -108.2(7) . . . . ? N5 C7 N6 C8 4.1(9) . . . . ? S1 C7 N6 C8 -174.2(5) . . . . ? O1 C8 N6 C7 -13.6(10) . . . . ? C9 C8 N6 C7 165.2(6) . . . . ? N8 C21 N7 C20 174.2(6) . . . . ? S2 C21 N7 C20 -8.3(10) . . . . ? N3 C20 N7 C21 -28.3(10) . . . . ? C19 C20 N7 C21 154.9(6) . . . . ? N7 C21 N8 C22 5.4(9) . . . . ? S2 C21 N8 C22 -172.3(5) . . . . ? O2 C22 N8 C21 1.6(10) . . . . ? C23 C22 N8 C21 -179.9(6) . . . . ? C64 C63 N9 C35 -83.3(7) . . . . ? C64 C63 N9 C49 149.4(5) . . . . ? C64 C63 N9 Zn2 33.1(6) . . . . ? C36 C35 N9 C63 155.6(6) . . . . ? C36 C35 N9 C49 -76.3(7) . . . . ? C36 C35 N9 Zn2 38.0(6) . . . . ? C50 C49 N9 C63 -76.6(7) . . . . ? C50 C49 N9 C35 156.0(5) . . . . ? C50 C49 N9 Zn2 41.2(6) . . . . ? C37 C36 N10 C40 1.1(10) . . . . ? C35 C36 N10 C40 -176.8(6) . . . . ? C37 C36 N10 Zn2 172.7(5) . . . . ? C35 C36 N10 Zn2 -5.2(7) . . . . ? C39 C40 N10 C36 -1.6(9) . . . . ? N13 C40 N10 C36 -174.4(6) . . . . ? C39 C40 N10 Zn2 -171.9(5) . . . . ? N13 C40 N10 Zn2 15.4(8) . . . . ? C53 C54 N11 C50 1.1(10) . . . . ? N15 C54 N11 C50 -178.7(5) . . . . ? C53 C54 N11 Zn2 177.4(5) . . . . ? N15 C54 N11 Zn2 -2.3(8) . . . . ? C51 C50 N11 C54 1.9(9) . . . . ? C49 C50 N11 C54 -178.8(6) . . . . ? C51 C50 N11 Zn2 -174.9(5) . . . . ? C49 C50 N11 Zn2 4.4(7) . . . . ? C65 C64 N12 C68 2.4(9) . . . . ? C63 C64 N12 C68 -173.5(6) . . . . ? C65 C64 N12 Zn2 -179.7(5) . . . . ? C63 C64 N12 Zn2 4.4(7) . . . . ? C67 C68 N12 C64 -0.8(10) . . . . ? C67 C68 N12 Zn2 -178.5(5) . . . . ? N14 C41 N13 C40 -179.6(6) . . . . ? S3 C41 N13 C40 -0.5(11) . . . . ? N10 C40 N13 C41 -38.3(10) . . . . ? C39 C40 N13 C41 148.7(7) . . . . ? N13 C41 N14 C42 10.1(10) . . . . ? S3 C41 N14 C42 -169.1(6) . . . . ? O3 C42 N14 C41 0.5(12) . . . . ? C43 C42 N14 C41 179.5(6) . . . . ? N16 C55 N15 C54 -174.8(5) . . . . ? S4 C55 N15 C54 3.2(8) . . . . ? N11 C54 N15 C55 84.0(7) . . . . ? C53 C54 N15 C55 -95.7(8) . . . . ? O4 C56 N16 C55 -11.6(10) . . . . ? C57 C56 N16 C55 169.1(6) . . . . ? N15 C55 N16 C56 4.0(9) . . . . ? S4 C55 N16 C56 -174.0(5) . . . . ? N7 C21 S2 Zn1 45.5(6) . . . . ? N8 C21 S2 Zn1 -137.0(4) . . . . ? N13 C41 S3 Zn2 43.5(6) . . . . ? N14 C41 S3 Zn2 -137.4(5) . . . . ? C34 N4 Zn1 N2 117.4(5) . . . . ? C30 N4 Zn1 N2 -61.6(5) . . . . ? C34 N4 Zn1 N3 -100.0(5) . . . . ? C30 N4 Zn1 N3 81.0(5) . . . . ? C34 N4 Zn1 N1 -168.8(6) . . . . ? C30 N4 Zn1 N1 12.2(4) . . . . ? C34 N4 Zn1 S2 -4.8(5) . . . . ? C30 N4 Zn1 S2 176.2(4) . . . . ? C2 N2 Zn1 N4 92.5(4) . . . . ? C6 N2 Zn1 N4 -91.3(5) . . . . ? C2 N2 Zn1 N3 -52.6(4) . . . . ? C6 N2 Zn1 N3 123.5(5) . . . . ? C2 N2 Zn1 N1 17.8(4) . . . . ? C6 N2 Zn1 N1 -166.0(5) . . . . ? C2 N2 Zn1 S2 -153.9(4) . . . . ? C6 N2 Zn1 S2 22.3(5) . . . . ? C20 N3 Zn1 N4 125.3(5) . . . . ? C16 N3 Zn1 N4 -49.8(5) . . . . ? C20 N3 Zn1 N2 -92.4(5) . . . . ? C16 N3 Zn1 N2 92.6(4) . . . . ? C20 N3 Zn1 N1 -164.1(5) . . . . ? C16 N3 Zn1 N1 20.8(4) . . . . ? C20 N3 Zn1 S2 24.3(5) . . . . ? C16 N3 Zn1 S2 -150.8(4) . . . . ? C1 N1 Zn1 N4 -145.8(4) . . . . ? C15 N1 Zn1 N4 92.4(4) . . . . ? C29 N1 Zn1 N4 -26.9(4) . . . . ? C1 N1 Zn1 N2 -29.3(4) . . . . ? C15 N1 Zn1 N2 -151.1(4) . . . . ? C29 N1 Zn1 N2 89.6(4) . . . . ? C1 N1 Zn1 N3 89.2(4) . . . . ? C15 N1 Zn1 N3 -32.6(4) . . . . ? C29 N1 Zn1 N3 -151.9(4) . . . . ? C1 N1 Zn1 S2 121.7(5) . . . . ? C15 N1 Zn1 S2 -0.1(8) . . . . ? C29 N1 Zn1 S2 -119.4(5) . . . . ? C21 S2 Zn1 N4 -163.3(2) . . . . ? C21 S2 Zn1 N2 75.0(3) . . . . ? C21 S2 Zn1 N3 -41.9(2) . . . . ? C21 S2 Zn1 N1 -73.5(6) . . . . ? C64 N12 Zn2 N11 -63.0(5) . . . . ? C68 N12 Zn2 N11 114.8(5) . . . . ? C64 N12 Zn2 N10 79.7(5) . . . . ? C68 N12 Zn2 N10 -102.6(6) . . . . ? C64 N12 Zn2 N9 11.4(5) . . . . ? C68 N12 Zn2 N9 -170.8(6) . . . . ? C64 N12 Zn2 S3 175.2(4) . . . . ? C68 N12 Zn2 S3 -7.1(6) . . . . ? C54 N11 Zn2 N12 -86.9(5) . . . . ? C50 N11 Zn2 N12 89.6(5) . . . . ? C54 N11 Zn2 N10 127.4(5) . . . . ? C50 N11 Zn2 N10 -56.1(5) . . . . ? C54 N11 Zn2 N9 -161.0(6) . . . . ? C50 N11 Zn2 N9 15.5(4) . . . . ? C54 N11 Zn2 S3 25.2(6) . . . . ? C50 N11 Zn2 S3 -158.3(4) . . . . ? C36 N10 Zn2 N12 -47.7(5) . . . . ? C40 N10 Zn2 N12 123.0(5) . . . . ? C36 N10 Zn2 N11 93.7(5) . . . . ? C40 N10 Zn2 N11 -95.6(5) . . . . ? C36 N10 Zn2 N9 21.1(4) . . . . ? C40 N10 Zn2 N9 -168.2(6) . . . . ? C36 N10 Zn2 S3 -148.5(4) . . . . ? C40 N10 Zn2 S3 22.2(5) . . . . ? C63 N9 Zn2 N12 -24.5(4) . . . . ? C35 N9 Zn2 N12 95.7(4) . . . . ? C49 N9 Zn2 N12 -145.7(4) . . . . ? C63 N9 Zn2 N11 89.9(4) . . . . ? C35 N9 Zn2 N11 -150.0(4) . . . . ? C49 N9 Zn2 N11 -31.4(4) . . . . ? C63 N9 Zn2 N10 -151.6(5) . . . . ? C35 N9 Zn2 N10 -31.5(4) . . . . ? C49 N9 Zn2 N10 87.1(4) . . . . ? C63 N9 Zn2 S3 -110.7(6) . . . . ? C35 N9 Zn2 S3 9.5(8) . . . . ? C49 N9 Zn2 S3 128.1(5) . . . . ? C41 S3 Zn2 N12 -165.2(3) . . . . ? C41 S3 Zn2 N11 75.7(3) . . . . ? C41 S3 Zn2 N10 -42.0(3) . . . . ? C41 S3 Zn2 N9 -81.9(6) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.016 _refine_diff_density_min -0.818 _refine_diff_density_rms 0.147 data_aja0815a _database_code_depnum_ccdc_archive 'CCDC 844368' #TrackingRef '- aja0815b_3.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C36 H33 Cl2 N9 Ni O10 S2, 0.5(C3 H6 O), 0.5(H2 O)' _chemical_formula_sum 'C37.50 H37 Cl2 N9 Ni O11 S2' _chemical_formula_weight 983.49 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 '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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 12.6653(6) _cell_length_b 18.0877(9) _cell_length_c 18.8600(10) _cell_angle_alpha 90.00 _cell_angle_beta 96.484(3) _cell_angle_gamma 90.00 _cell_volume 4292.9(4) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 3687 _cell_measurement_theta_min 2.45 _cell_measurement_theta_max 20.81 _exptl_crystal_description needle _exptl_crystal_colour colourless _exptl_crystal_size_max 0.42 _exptl_crystal_size_mid 0.03 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.522 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2028 _exptl_absorpt_coefficient_mu 0.743 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.7454 _exptl_absorpt_correction_T_max 0.9853 _exptl_absorpt_process_details Denzo/scalepack _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 'Nonius KappaCCD' _diffrn_measurement_method 'CCD scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8397 _diffrn_reflns_av_R_equivalents 0.0624 _diffrn_reflns_av_sigmaI/netI 0.0763 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.45 _diffrn_reflns_theta_max 20.81 _reflns_number_total 4431 _reflns_number_gt 3687 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'cOLLECT,Nonius BV, 1997-2001' _computing_cell_refinement DENZO/SCALEPACK _computing_data_reduction DENZO/SCALEPACK _computing_structure_solution SHELXs-97 _computing_structure_refinement SHELXL-97 _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^)+(0.0379P)^2^+35.4450P] 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 4431 _refine_ls_number_parameters 497 _refine_ls_number_restraints 24 _refine_ls_R_factor_all 0.1188 _refine_ls_R_factor_gt 0.0941 _refine_ls_wR_factor_ref 0.1865 _refine_ls_wR_factor_gt 0.1777 _refine_ls_goodness_of_fit_ref 1.257 _refine_ls_restrained_S_all 1.256 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group N1 N 0.3697(6) -0.2727(4) -0.4181(4) 0.023(2) Uani 1 1 d . . . C1 C 0.4638(3) -0.3140(2) -0.4361(2) 0.025(3) Uani 1 1 d . . . H1A H 0.5115 -0.3240 -0.3918 0.030 Uiso 1 1 calc R . . H1B H 0.4407 -0.3621 -0.4574 0.030 Uiso 1 1 calc R . . N2 N 0.4752(3) -0.2097(2) -0.5159(2) 0.025(2) Uani 1 1 d R . . C2 C 0.5227(3) -0.2735(2) -0.4860(2) 0.024(3) Uani 1 1 d R . . C3 C 0.6206(3) -0.2963(2) -0.5048(2) 0.025(3) Uani 1 1 d R . . H3 H 0.6530 -0.3399 -0.4844 0.030 Uiso 1 1 calc R . . C4 C 0.6710(3) -0.2553(2) -0.5535(2) 0.032(3) Uani 1 1 d R . . H4 H 0.7379 -0.2709 -0.5664 0.038 Uiso 1 1 calc R . . C5 C 0.6236(3) -0.1915(2) -0.5834(2) 0.027(3) Uani 1 1 d R . . H5 H 0.6580 -0.1635 -0.6166 0.033 Uiso 1 1 calc R . . C6 C 0.5257(3) -0.1687(2) -0.5645(2) 0.024(3) Uani 1 1 d R . . C7 C 0.4480(8) -0.0928(6) -0.6589(5) 0.025(3) Uani 1 1 d . . . C8 C 0.3859(3) 0.0338(2) -0.6287(2) 0.026(3) Uani 1 1 d . . . C9 C 0.3504(3) 0.1049(2) -0.6624(2) 0.026(3) Uani 1 1 d R . . C10 C 0.3819(3) 0.1268(2) -0.7274(2) 0.028(3) Uani 1 1 d R . . H10 H 0.4218 0.0940 -0.7534 0.034 Uiso 1 1 calc R . . C11 C 0.3549(3) 0.1966(2) -0.7546(2) 0.031(3) Uani 1 1 d R . . H11 H 0.3764 0.2115 -0.7990 0.037 Uiso 1 1 calc R . . C12 C 0.2964(3) 0.2445(2) -0.7166(2) 0.041(3) Uani 1 1 d R . . H12 H 0.2780 0.2922 -0.7351 0.049 Uiso 1 1 calc R . . C13 C 0.2650(3) 0.2226(2) -0.6515(2) 0.042(3) Uani 1 1 d R . . H13 H 0.2250 0.2554 -0.6256 0.051 Uiso 1 1 calc R . . C14 C 0.2920(3) 0.1529(2) -0.6244(2) 0.034(3) Uani 1 1 d R . . H14 H 0.2705 0.1379 -0.5799 0.041 Uiso 1 1 calc R . . C15 C 0.4052(9) -0.2141(6) -0.3657(5) 0.033(3) Uani 1 1 d . . . H15A H 0.3967 -0.2329 -0.3174 0.039 Uiso 1 1 calc R . . H15B H 0.4820 -0.2055 -0.3677 0.039 Uiso 1 1 calc R . . N3 N 0.4771(6) -0.1044(4) -0.5893(4) 0.025(2) Uani 1 1 d . . . H3A H 0.4648 -0.0698 -0.5585 0.030 Uiso 1 1 calc R . . N4 N 0.4042(3) -0.0233(2) -0.6743(2) 0.024(2) Uani 1 1 d U . . H4A H 0.3855 -0.0144 -0.7198 0.029 Uiso 1 1 calc R . . N5 N 0.2965(3) -0.1273(2) -0.4417(2) 0.024(2) Uani 1 1 d R . . C16 C 0.3501(3) -0.1426(2) -0.3749(2) 0.025(3) Uani 1 1 d R . . C17 C 0.3553(3) -0.0895(2) -0.3213(2) 0.030(3) Uani 1 1 d R . . H17 H 0.3920 -0.0999 -0.2757 0.036 Uiso 1 1 calc R . . C18 C 0.3069(3) -0.0211(2) -0.3346(2) 0.031(3) Uani 1 1 d R . . H18 H 0.3105 0.0151 -0.2980 0.038 Uiso 1 1 calc R . . C19 C 0.2533(3) -0.0059(2) -0.4014(2) 0.029(3) Uani 1 1 d R . . H19 H 0.2202 0.0409 -0.4104 0.035 Uiso 1 1 calc R . . C20 C 0.2481(3) -0.0589(2) -0.4550(2) 0.029(3) Uani 1 1 d R . . C21 C 0.1678(8) -0.0764(6) -0.5820(5) 0.026(3) Uani 1 1 d . . . C22 C 0.0431(3) 0.0254(2) -0.6223(2) 0.031(3) Uani 1 1 d . . . C23 C -0.0283(3) 0.0530(2) -0.6842(2) 0.030(3) Uani 1 1 d R . . C24 C -0.0665(3) 0.0087(2) -0.7416(2) 0.031(3) Uani 1 1 d R . . H24 H -0.0443 -0.0414 -0.7434 0.037 Uiso 1 1 calc R . . C25 C -0.1372(3) 0.0376(2) -0.7964(2) 0.037(3) Uani 1 1 d R . . H25 H -0.1633 0.0073 -0.8356 0.044 Uiso 1 1 calc R . . C26 C -0.1696(3) 0.1108(2) -0.7937(2) 0.037(3) Uani 1 1 d R . . H26 H -0.2179 0.1306 -0.8311 0.045 Uiso 1 1 calc R . . C27 C -0.1314(3) 0.1552(2) -0.7363(2) 0.038(3) Uani 1 1 d R . . H27 H -0.1536 0.2053 -0.7345 0.045 Uiso 1 1 calc R . . C28 C -0.0607(3) 0.1263(2) -0.6815(2) 0.035(3) Uani 1 1 d R . . H28 H -0.0346 0.1566 -0.6423 0.042 Uiso 1 1 calc R . . C29 C 0.2934(8) -0.3231(6) -0.3918(5) 0.028(3) Uani 1 1 d . . . H29A H 0.3068 -0.3252 -0.3391 0.033 Uiso 1 1 calc R . . H29B H 0.3052 -0.3732 -0.4103 0.033 Uiso 1 1 calc R . . N6 N 0.1821(6) -0.0444(5) -0.5172(4) 0.029(2) Uani 1 1 d . . . H6 H 0.1407 -0.0059 -0.5136 0.034 Uiso 1 1 calc R . . N7 N 0.1019(3) -0.0390(2) -0.6316(2) 0.032(2) Uani 1 1 d . . . H7 H 0.0953 -0.0575 -0.6751 0.038 Uiso 1 1 calc R . . N8 N 0.1613(3) -0.2546(2) -0.4704(2) 0.025(2) Uani 1 1 d R . . C30 C 0.1798(3) -0.3020(2) -0.4123(2) 0.029(3) Uani 1 1 d R . . C31 C 0.0950(3) -0.3303(2) -0.3802(2) 0.033(3) Uani 1 1 d R . . H31 H 0.1077 -0.3626 -0.3404 0.040 Uiso 1 1 calc R . . C32 C -0.0085(3) -0.3111(2) -0.4061(2) 0.040(3) Uani 1 1 d R . . H32 H -0.0665 -0.3304 -0.3841 0.048 Uiso 1 1 calc R . . C33 C -0.0271(3) -0.2637(2) -0.4642(2) 0.043(3) Uani 1 1 d R . . H33 H -0.0978 -0.2506 -0.4819 0.052 Uiso 1 1 calc R . . C34 C 0.0578(3) -0.2355(2) -0.4963(2) 0.035(3) Uani 1 1 d R . . H34 H 0.0451 -0.2031 -0.5360 0.042 Uiso 1 1 calc R . . C35 C 0.3464(8) -0.3318(6) -0.6245(7) 0.030(3) Uani 1 1 d . . . C36 C 0.3972(10) -0.3595(7) -0.6846(7) 0.050(3) Uani 1 1 d . . . H36A H 0.4222 -0.3178 -0.7114 0.075 Uiso 1 1 calc R . . H36B H 0.3460 -0.3886 -0.7159 0.075 Uiso 1 1 calc R . . H36C H 0.4578 -0.3908 -0.6670 0.075 Uiso 1 1 calc R . . C37 C 0.0565(12) -0.4109(12) -0.5799(10) 0.041(6) Uani 0.50 1 d PDU . . H37A H 0.1056 -0.4190 -0.6158 0.062 Uiso 0.50 1 calc PR . . H37B H 0.0873 -0.4313 -0.5340 0.062 Uiso 0.50 1 calc PR . . H37C H 0.0444 -0.3578 -0.5748 0.062 Uiso 0.50 1 calc PR . . C38 C -0.0487(11) -0.4493(10) -0.6034(9) 0.033(6) Uani 0.50 1 d PDU . . C39 C -0.1311(15) -0.4384(14) -0.5500(10) 0.115(16) Uani 0.50 1 d PD . . H39A H -0.1972 -0.4640 -0.5675 0.173 Uiso 0.50 1 calc PR . . H39B H -0.1454 -0.3855 -0.5450 0.173 Uiso 0.50 1 calc PR . . H39C H -0.1031 -0.4588 -0.5035 0.173 Uiso 0.50 1 calc PR . . O1 O 0.4029(6) 0.0268(4) -0.5634(4) 0.038(2) Uani 1 1 d . . . O2 O 0.0532(6) 0.0586(4) -0.5647(4) 0.048(2) Uani 1 1 d . . . O3 O 0.2717(7) 0.0057(5) -0.8145(5) 0.070(3) Uani 1 1 d . . . O4 O 0.2493(7) -0.1034(5) -0.8813(4) 0.061(3) Uani 1 1 d . . . O5 O 0.1405(8) -0.0795(6) -0.7902(6) 0.090(3) Uani 1 1 d . . . O6 O 0.1211(9) -0.0092(6) -0.8970(6) 0.105(4) Uani 1 1 d . . . O7 O -0.1064(6) -0.1483(4) -0.6100(4) 0.046(2) Uani 1 1 d . . . O8 O -0.0364(6) -0.1726(4) -0.7169(4) 0.038(2) Uani 1 1 d . . . O9 O -0.1178(7) -0.2676(4) -0.6581(5) 0.062(3) Uani 1 1 d . . . O10 O -0.2193(6) -0.1708(5) -0.7131(4) 0.062(3) Uani 1 1 d . . . O11 O 0.405(2) -0.4935(12) -0.4617(11) 0.108(8) Uani 0.50 1 d P . . O12 O -0.0695(11) -0.4821(8) -0.6602(7) 0.053(5) Uani 0.50 1 d PD . . Ni1 Ni 0.30073(10) -0.21715(7) -0.50760(7) 0.0217(4) Uani 1 1 d . . . N9 N 0.3110(7) -0.3071(5) -0.5760(5) 0.030(2) Uani 1 1 d . . . S1 S 0.4605(2) -0.15130(16) -0.72353(15) 0.0362(8) Uani 1 1 d . . . S2 S 0.2231(2) -0.15423(14) -0.60905(13) 0.0258(7) Uani 1 1 d . . . Cl1 Cl 0.1963(3) -0.04670(17) -0.84592(18) 0.0542(10) Uani 1 1 d . . . Cl2 Cl -0.1195(2) -0.19013(15) -0.67439(14) 0.0315(7) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 N1 0.012(5) 0.023(5) 0.036(5) 0.006(4) 0.008(4) 0.003(4) C1 0.032(7) 0.016(6) 0.027(6) 0.006(5) 0.002(5) -0.006(5) N2 0.018(5) 0.025(5) 0.031(5) 0.000(4) -0.005(4) 0.001(4) C2 0.020(6) 0.027(7) 0.024(6) -0.005(5) -0.004(5) 0.012(5) C3 0.034(7) 0.020(6) 0.023(6) 0.001(5) 0.009(5) 0.001(5) C4 0.023(6) 0.036(7) 0.034(7) -0.010(6) -0.006(5) 0.012(6) C5 0.027(7) 0.025(7) 0.030(6) -0.004(5) 0.003(5) -0.004(5) C6 0.030(7) 0.014(6) 0.028(6) -0.004(5) 0.003(5) -0.007(5) C7 0.029(6) 0.022(7) 0.025(7) 0.006(5) 0.009(5) -0.012(5) C8 0.032(7) 0.023(7) 0.023(7) 0.011(6) 0.008(5) 0.000(5) C9 0.026(6) 0.022(7) 0.027(7) 0.008(6) -0.012(5) -0.003(5) C10 0.029(7) 0.020(7) 0.033(7) -0.002(5) -0.013(5) -0.003(5) C11 0.035(7) 0.026(7) 0.029(7) 0.003(6) -0.007(5) -0.002(6) C12 0.050(8) 0.022(7) 0.045(8) 0.013(6) -0.018(7) -0.003(6) C13 0.054(8) 0.021(7) 0.049(8) -0.001(6) -0.006(6) 0.013(6) C14 0.039(7) 0.021(7) 0.042(7) 0.002(6) 0.002(6) 0.002(6) C15 0.043(7) 0.026(7) 0.027(6) 0.003(6) -0.004(5) -0.002(6) N3 0.040(6) 0.008(5) 0.029(6) 0.004(4) 0.013(4) -0.004(4) N4 0.034(4) 0.017(4) 0.021(4) 0.000(3) 0.001(3) -0.005(3) N5 0.022(5) 0.032(6) 0.019(5) -0.005(4) 0.005(4) -0.005(4) C16 0.018(6) 0.028(7) 0.030(7) 0.004(6) 0.008(5) -0.002(5) C17 0.018(6) 0.042(8) 0.029(7) -0.007(6) -0.001(5) 0.004(6) C18 0.023(6) 0.040(8) 0.031(7) -0.020(6) 0.002(5) -0.005(6) C19 0.026(6) 0.023(7) 0.038(7) -0.009(6) 0.005(6) 0.005(5) C20 0.034(7) 0.018(7) 0.036(7) 0.003(6) 0.015(6) 0.000(6) C21 0.024(6) 0.036(7) 0.018(7) -0.008(6) -0.004(5) 0.000(5) C22 0.031(7) 0.039(8) 0.024(7) 0.001(6) 0.004(6) 0.007(6) C23 0.028(6) 0.026(7) 0.036(7) 0.015(6) 0.007(6) 0.004(6) C24 0.032(7) 0.026(7) 0.033(7) 0.001(6) 0.001(6) 0.007(5) C25 0.041(7) 0.039(8) 0.029(7) 0.005(6) -0.003(6) -0.007(6) C26 0.039(7) 0.036(8) 0.037(7) 0.014(6) 0.006(6) 0.015(6) C27 0.039(7) 0.029(7) 0.046(8) 0.007(6) 0.010(6) 0.015(6) C28 0.031(7) 0.038(8) 0.037(7) 0.008(6) 0.010(6) 0.011(6) C29 0.035(7) 0.027(7) 0.022(6) 0.003(5) 0.007(5) 0.003(6) N6 0.034(6) 0.027(5) 0.024(6) 0.003(4) -0.002(5) 0.013(4) N7 0.036(6) 0.038(6) 0.018(5) -0.001(4) -0.008(4) 0.013(5) N8 0.031(6) 0.023(5) 0.021(5) -0.001(4) 0.000(4) -0.005(4) C30 0.034(7) 0.029(7) 0.023(7) -0.020(6) -0.002(5) -0.004(6) C31 0.042(8) 0.031(7) 0.028(7) 0.004(5) 0.010(6) -0.007(6) C32 0.018(7) 0.061(9) 0.043(8) -0.006(7) 0.006(6) -0.007(6) C33 0.025(7) 0.072(9) 0.032(7) 0.012(7) 0.001(6) 0.002(7) C34 0.023(7) 0.040(8) 0.038(7) 0.001(6) -0.011(6) -0.003(6) C35 0.017(6) 0.022(7) 0.050(9) 0.008(6) 0.000(6) 0.006(5) C36 0.048(8) 0.046(8) 0.057(9) -0.007(7) 0.011(7) 0.008(7) C37 0.044(7) 0.042(7) 0.039(7) -0.004(5) 0.007(5) 0.000(5) C38 0.037(7) 0.027(7) 0.033(7) 0.005(5) 0.000(5) 0.004(5) C39 0.14(3) 0.06(2) 0.13(3) 0.04(2) -0.09(3) -0.03(2) O1 0.061(5) 0.031(5) 0.023(5) 0.001(4) 0.008(4) 0.010(4) O2 0.060(6) 0.043(5) 0.037(5) -0.004(4) -0.008(4) 0.017(4) O3 0.074(7) 0.042(5) 0.086(7) -0.015(5) -0.032(5) -0.012(5) O4 0.072(6) 0.049(6) 0.059(6) -0.024(5) -0.004(5) 0.000(5) O5 0.088(8) 0.082(8) 0.109(9) 0.028(7) 0.056(7) 0.002(6) O6 0.104(9) 0.076(7) 0.115(9) -0.022(7) -0.081(7) 0.028(6) O7 0.054(5) 0.050(5) 0.033(5) -0.018(4) -0.003(4) 0.014(4) O8 0.036(5) 0.033(5) 0.049(5) -0.002(4) 0.019(4) -0.004(4) O9 0.089(7) 0.021(5) 0.082(7) 0.003(4) 0.033(5) -0.013(5) O10 0.024(5) 0.123(8) 0.037(5) 0.004(5) -0.009(4) 0.017(5) O11 0.19(3) 0.072(15) 0.064(14) -0.010(12) 0.027(15) -0.015(16) O12 0.061(12) 0.043(11) 0.053(11) 0.010(9) -0.008(9) 0.026(9) Ni1 0.0259(8) 0.0175(8) 0.0208(8) 0.0024(6) -0.0014(6) 0.0028(6) N9 0.027(6) 0.032(6) 0.031(6) -0.004(5) 0.003(5) 0.006(5) S1 0.0474(19) 0.0327(18) 0.0276(17) -0.0061(14) 0.0006(14) 0.0036(15) S2 0.0353(17) 0.0221(16) 0.0189(15) 0.0009(12) -0.0024(12) 0.0062(13) Cl1 0.059(2) 0.036(2) 0.062(2) -0.0115(18) -0.0175(19) 0.0026(18) Cl2 0.0332(18) 0.0321(18) 0.0291(17) -0.0032(14) 0.0029(14) -0.0012(13) _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 N1 C29 1.455(12) . ? N1 C1 1.478(8) . ? N1 C15 1.483(12) . ? N1 Ni1 2.072(8) . ? C1 C2 1.4616 . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? N2 C2 1.3900 . ? N2 C6 1.3900 . ? N2 Ni1 2.237(4) . ? C2 C3 1.3900 . ? C3 C4 1.3900 . ? C3 H3 0.9500 . ? C4 C5 1.3900 . ? C4 H4 0.9500 . ? C5 C6 1.3900 . ? C5 H5 0.9500 . ? C6 N3 1.373(9) . ? C7 N3 1.340(12) . ? C7 N4 1.392(11) . ? C7 S1 1.635(11) . ? C8 O1 1.233(8) . ? C8 N4 1.379(6) . ? C8 C9 1.4821 . ? C9 C10 1.3900 . ? C9 C14 1.3900 . ? C10 C11 1.3900 . ? C10 H10 0.9500 . ? C11 C12 1.3900 . ? C11 H11 0.9500 . ? C12 C13 1.3900 . ? C12 H12 0.9500 . ? C13 C14 1.3900 . ? C13 H13 0.9500 . ? C14 H14 0.9500 . ? C15 C16 1.471(11) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? N3 H3A 0.8800 . ? N4 H4A 0.8800 . ? N5 C16 1.3900 . ? N5 C20 1.3900 . ? N5 Ni1 2.050(4) . ? C16 C17 1.3900 . ? C17 C18 1.3900 . ? C17 H17 0.9500 . ? C18 C19 1.3900 . ? C18 H18 0.9500 . ? C19 C20 1.3900 . ? C19 H19 0.9500 . ? C20 N6 1.388(9) . ? C21 N6 1.346(12) . ? C21 N7 1.362(10) . ? C21 S2 1.676(11) . ? C22 O2 1.236(9) . ? C22 N7 1.404(6) . ? C22 C23 1.4802 . ? C23 C24 1.3900 . ? C23 C28 1.3900 . ? C24 C25 1.3900 . ? C24 H24 0.9500 . ? C25 C26 1.3900 . ? C25 H25 0.9500 . ? C26 C27 1.3900 . ? C26 H26 0.9500 . ? C27 C28 1.3900 . ? C27 H27 0.9500 . ? C28 H28 0.9500 . ? C29 C30 1.496(10) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? N6 H6 0.8800 . ? N7 H7 0.8800 . ? N8 C30 1.3900 . ? N8 C34 1.3900 . ? N8 Ni1 2.086(4) . ? C30 C31 1.3900 . ? C31 C32 1.3900 . ? C31 H31 0.9500 . ? C32 C33 1.3900 . ? C32 H32 0.9500 . ? C33 C34 1.3900 . ? C33 H33 0.9500 . ? C34 H34 0.9500 . ? C35 N9 1.152(13) . ? C35 C36 1.454(17) . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 C38 1.523(8) . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C38 O12 1.227(8) . ? C38 C39 1.544(8) . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? O3 Cl1 1.427(8) . ? O4 Cl1 1.431(9) . ? O5 Cl1 1.457(10) . ? O6 Cl1 1.445(9) . ? O7 Cl2 1.424(7) . ? O8 Cl2 1.429(7) . ? O9 Cl2 1.435(8) . ? O10 Cl2 1.430(7) . ? Ni1 N9 2.090(10) . ? Ni1 S2 2.345(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 C29 N1 C1 110.3(7) . . ? C29 N1 C15 112.5(8) . . ? C1 N1 C15 108.9(7) . . ? C29 N1 Ni1 110.2(6) . . ? C1 N1 Ni1 109.5(5) . . ? C15 N1 Ni1 105.3(6) . . ? C2 C1 N1 112.2(3) . . ? C2 C1 H1A 109.2 . . ? N1 C1 H1A 109.2 . . ? C2 C1 H1B 109.2 . . ? N1 C1 H1B 109.2 . . ? H1A C1 H1B 107.9 . . ? C2 N2 C6 120.0 . . ? C2 N2 Ni1 107.89(10) . . ? C6 N2 Ni1 127.55(10) . . ? N2 C2 C3 120.0 . . ? N2 C2 C1 116.6 . . ? C3 C2 C1 123.4 . . ? C4 C3 C2 120.0 . . ? C4 C3 H3 120.0 . . ? C2 C3 H3 120.0 . . ? C3 C4 C5 120.0 . . ? C3 C4 H4 120.0 . . ? C5 C4 H4 120.0 . . ? C6 C5 C4 120.0 . . ? C6 C5 H5 120.0 . . ? C4 C5 H5 120.0 . . ? N3 C6 C5 122.9(4) . . ? N3 C6 N2 117.0(4) . . ? C5 C6 N2 120.0 . . ? N3 C7 N4 113.9(8) . . ? N3 C7 S1 126.2(8) . . ? N4 C7 S1 120.0(7) . . ? O1 C8 N4 121.5(5) . . ? O1 C8 C9 121.8(4) . . ? N4 C8 C9 116.6(2) . . ? C10 C9 C14 120.0 . . ? C10 C9 C8 121.4 . . ? C14 C9 C8 118.3 . . ? C11 C10 C9 120.0 . . ? C11 C10 H10 120.0 . . ? C9 C10 H10 120.0 . . ? C10 C11 C12 120.0 . . ? C10 C11 H11 120.0 . . ? C12 C11 H11 120.0 . . ? C13 C12 C11 120.0 . . ? C13 C12 H12 120.0 . . ? C11 C12 H12 120.0 . . ? C14 C13 C12 120.0 . . ? C14 C13 H13 120.0 . . ? C12 C13 H13 120.0 . . ? C13 C14 C9 120.0 . . ? C13 C14 H14 120.0 . . ? C9 C14 H14 120.0 . . ? C16 C15 N1 116.5(7) . . ? C16 C15 H15A 108.2 . . ? N1 C15 H15A 108.2 . . ? C16 C15 H15B 108.2 . . ? N1 C15 H15B 108.2 . . ? H15A C15 H15B 107.3 . . ? C7 N3 C6 121.9(8) . . ? C7 N3 H3A 119.0 . . ? C6 N3 H3A 119.0 . . ? C8 N4 C7 129.6(5) . . ? C8 N4 H4A 115.2 . . ? C7 N4 H4A 115.2 . . ? C16 N5 C20 120.0 . . ? C16 N5 Ni1 110.39(11) . . ? C20 N5 Ni1 129.60(11) . . ? N5 C16 C17 120.0 . . ? N5 C16 C15 117.3(4) . . ? C17 C16 C15 122.6(4) . . ? C16 C17 C18 120.0 . . ? C16 C17 H17 120.0 . . ? C18 C17 H17 120.0 . . ? C19 C18 C17 120.0 . . ? C19 C18 H18 120.0 . . ? C17 C18 H18 120.0 . . ? C18 C19 C20 120.0 . . ? C18 C19 H19 120.0 . . ? C20 C19 H19 120.0 . . ? N6 C20 C19 117.3(4) . . ? N6 C20 N5 122.1(4) . . ? C19 C20 N5 120.0 . . ? N6 C21 N7 114.7(8) . . ? N6 C21 S2 128.3(8) . . ? N7 C21 S2 116.9(7) . . ? O2 C22 N7 120.7(5) . . ? O2 C22 C23 121.5(4) . . ? N7 C22 C23 117.9(2) . . ? C24 C23 C28 120.0 . . ? C24 C23 C22 123.1 . . ? C28 C23 C22 116.8 . . ? C23 C24 C25 120.0 . . ? C23 C24 H24 120.0 . . ? C25 C24 H24 120.0 . . ? C26 C25 C24 120.0 . . ? C26 C25 H25 120.0 . . ? C24 C25 H25 120.0 . . ? C27 C26 C25 120.0 . . ? C27 C26 H26 120.0 . . ? C25 C26 H26 120.0 . . ? C26 C27 C28 120.0 . . ? C26 C27 H27 120.0 . . ? C28 C27 H27 120.0 . . ? C23 C28 C27 120.0 . . ? C23 C28 H28 120.0 . . ? C27 C28 H28 120.0 . . ? N1 C29 C30 114.1(7) . . ? N1 C29 H29A 108.7 . . ? C30 C29 H29A 108.7 . . ? N1 C29 H29B 108.7 . . ? C30 C29 H29B 108.7 . . ? H29A C29 H29B 107.6 . . ? C21 N6 C20 133.9(8) . . ? C21 N6 H6 113.1 . . ? C20 N6 H6 113.1 . . ? C21 N7 C22 128.2(5) . . ? C21 N7 H7 115.9 . . ? C22 N7 H7 115.9 . . ? C30 N8 C34 120.0 . . ? C30 N8 Ni1 113.02(11) . . ? C34 N8 Ni1 126.96(11) . . ? N8 C30 C31 120.0 . . ? N8 C30 C29 115.7(4) . . ? C31 C30 C29 124.2(4) . . ? C32 C31 C30 120.0 . . ? C32 C31 H31 120.0 . . ? C30 C31 H31 120.0 . . ? C31 C32 C33 120.0 . . ? C31 C32 H32 120.0 . . ? C33 C32 H32 120.0 . . ? C32 C33 C34 120.0 . . ? C32 C33 H33 120.0 . . ? C34 C33 H33 120.0 . . ? C33 C34 N8 120.0 . . ? C33 C34 H34 120.0 . . ? N8 C34 H34 120.0 . . ? N9 C35 C36 176.1(12) . . ? C35 C36 H36A 109.5 . . ? C35 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C35 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C38 C37 H37A 109.5 . . ? C38 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C38 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? O12 C38 C37 124.7(8) . . ? O12 C38 C39 122.5(8) . . ? C37 C38 C39 112.7(7) . . ? C38 C39 H39A 109.5 . . ? C38 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C38 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? N5 Ni1 N1 85.9(3) . . ? N5 Ni1 N8 88.46(15) . . ? N1 Ni1 N8 82.2(2) . . ? N5 Ni1 N9 177.6(3) . . ? N1 Ni1 N9 94.4(3) . . ? N8 Ni1 N9 94.0(3) . . ? N5 Ni1 N2 95.06(14) . . ? N1 Ni1 N2 75.9(2) . . ? N8 Ni1 N2 157.47(16) . . ? N9 Ni1 N2 82.7(3) . . ? N5 Ni1 S2 94.16(13) . . ? N1 Ni1 S2 179.8(3) . . ? N8 Ni1 S2 98.02(14) . . ? N9 Ni1 S2 85.6(2) . . ? N2 Ni1 S2 103.90(13) . . ? C35 N9 Ni1 148.1(9) . . ? C21 S2 Ni1 108.1(4) . . ? O3 Cl1 O4 110.0(6) . . ? O3 Cl1 O6 108.9(6) . . ? O4 Cl1 O6 109.6(6) . . ? O3 Cl1 O5 109.2(7) . . ? O4 Cl1 O5 109.6(6) . . ? O6 Cl1 O5 109.6(7) . . ? O7 Cl2 O8 109.8(5) . . ? O7 Cl2 O10 108.5(5) . . ? O8 Cl2 O10 108.9(5) . . ? O7 Cl2 O9 109.8(5) . . ? O8 Cl2 O9 110.0(5) . . ? O10 Cl2 O9 109.9(6) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C29 N1 C1 C2 158.6(5) . . . . ? C15 N1 C1 C2 -77.5(6) . . . . ? Ni1 N1 C1 C2 37.1(5) . . . . ? C6 N2 C2 C3 0.0 . . . . ? Ni1 N2 C2 C3 157.81(10) . . . . ? C6 N2 C2 C1 -179.2 . . . . ? Ni1 N2 C2 C1 -21.38(10) . . . . ? N1 C1 C2 N2 -8.6(4) . . . . ? N1 C1 C2 C3 172.2(4) . . . . ? N2 C2 C3 C4 0.0 . . . . ? C1 C2 C3 C4 179.1 . . . . ? C2 C3 C4 C5 0.0 . . . . ? C3 C4 C5 C6 0.0 . . . . ? C4 C5 C6 N3 176.6(4) . . . . ? C4 C5 C6 N2 0.0 . . . . ? C2 N2 C6 N3 -176.8(4) . . . . ? Ni1 N2 C6 N3 30.2(4) . . . . ? C2 N2 C6 C5 0.0 . . . . ? Ni1 N2 C6 C5 -153.04(12) . . . . ? O1 C8 C9 C10 146.1(5) . . . . ? N4 C8 C9 C10 -30.7(2) . . . . ? O1 C8 C9 C14 -28.4(5) . . . . ? N4 C8 C9 C14 154.8(2) . . . . ? C14 C9 C10 C11 0.0 . . . . ? C8 C9 C10 C11 -174.4 . . . . ? C9 C10 C11 C12 0.0 . . . . ? C10 C11 C12 C13 0.0 . . . . ? C11 C12 C13 C14 0.0 . . . . ? C12 C13 C14 C9 0.0 . . . . ? C10 C9 C14 C13 0.0 . . . . ? C8 C9 C14 C13 174.6 . . . . ? C29 N1 C15 C16 -96.6(9) . . . . ? C1 N1 C15 C16 140.8(7) . . . . ? Ni1 N1 C15 C16 23.5(10) . . . . ? N4 C7 N3 C6 -177.3(6) . . . . ? S1 C7 N3 C6 2.2(13) . . . . ? C5 C6 N3 C7 61.9(9) . . . . ? N2 C6 N3 C7 -121.4(7) . . . . ? O1 C8 N4 C7 -4.2(9) . . . . ? C9 C8 N4 C7 172.6(6) . . . . ? N3 C7 N4 C8 -0.9(11) . . . . ? S1 C7 N4 C8 179.6(4) . . . . ? C20 N5 C16 C17 0.0 . . . . ? Ni1 N5 C16 C17 -178.79(11) . . . . ? C20 N5 C16 C15 -176.3(5) . . . . ? Ni1 N5 C16 C15 4.9(5) . . . . ? N1 C15 C16 N5 -20.2(10) . . . . ? N1 C15 C16 C17 163.6(6) . . . . ? N5 C16 C17 C18 0.0 . . . . ? C15 C16 C17 C18 176.1(5) . . . . ? C16 C17 C18 C19 0.0 . . . . ? C17 C18 C19 C20 0.0 . . . . ? C18 C19 C20 N6 171.7(4) . . . . ? C18 C19 C20 N5 0.0 . . . . ? C16 N5 C20 N6 -171.3(4) . . . . ? Ni1 N5 C20 N6 7.2(4) . . . . ? C16 N5 C20 C19 0.0 . . . . ? Ni1 N5 C20 C19 178.53(13) . . . . ? O2 C22 C23 C24 -160.4(5) . . . . ? N7 C22 C23 C24 21.5(3) . . . . ? O2 C22 C23 C28 16.7(5) . . . . ? N7 C22 C23 C28 -161.3(3) . . . . ? C28 C23 C24 C25 0.0 . . . . ? C22 C23 C24 C25 177.0 . . . . ? C23 C24 C25 C26 0.0 . . . . ? C24 C25 C26 C27 0.0 . . . . ? C25 C26 C27 C28 0.0 . . . . ? C24 C23 C28 C27 0.0 . . . . ? C22 C23 C28 C27 -177.2 . . . . ? C26 C27 C28 C23 0.0 . . . . ? C1 N1 C29 C30 -145.3(6) . . . . ? C15 N1 C29 C30 93.0(9) . . . . ? Ni1 N1 C29 C30 -24.3(9) . . . . ? N7 C21 N6 C20 -172.9(8) . . . . ? S2 C21 N6 C20 5.3(17) . . . . ? C19 C20 N6 C21 169.5(9) . . . . ? N5 C20 N6 C21 -18.9(12) . . . . ? N6 C21 N7 C22 -4.2(12) . . . . ? S2 C21 N7 C22 177.4(4) . . . . ? O2 C22 N7 C21 5.5(10) . . . . ? C23 C22 N7 C21 -176.4(6) . . . . ? C34 N8 C30 C31 0.0 . . . . ? Ni1 N8 C30 C31 178.31(11) . . . . ? C34 N8 C30 C29 176.1(5) . . . . ? Ni1 N8 C30 C29 -5.6(4) . . . . ? N1 C29 C30 N8 20.3(9) . . . . ? N1 C29 C30 C31 -163.9(5) . . . . ? N8 C30 C31 C32 0.0 . . . . ? C29 C30 C31 C32 -175.7(5) . . . . ? C30 C31 C32 C33 0.0 . . . . ? C31 C32 C33 C34 0.0 . . . . ? C32 C33 C34 N8 0.0 . . . . ? C30 N8 C34 C33 0.0 . . . . ? Ni1 N8 C34 C33 -178.06(13) . . . . ? C16 N5 Ni1 N1 6.9(2) . . . . ? C20 N5 Ni1 N1 -171.8(2) . . . . ? C16 N5 Ni1 N8 89.11(12) . . . . ? C20 N5 Ni1 N8 -89.53(14) . . . . ? C16 N5 Ni1 N9 -89(6) . . . . ? C20 N5 Ni1 N9 93(6) . . . . ? C16 N5 Ni1 N2 -68.59(12) . . . . ? C20 N5 Ni1 N2 112.77(13) . . . . ? C16 N5 Ni1 S2 -172.97(8) . . . . ? C20 N5 Ni1 S2 8.39(13) . . . . ? C29 N1 Ni1 N5 105.6(6) . . . . ? C1 N1 Ni1 N5 -133.0(4) . . . . ? C15 N1 Ni1 N5 -16.1(6) . . . . ? C29 N1 Ni1 N8 16.6(6) . . . . ? C1 N1 Ni1 N8 138.0(5) . . . . ? C15 N1 Ni1 N8 -105.1(6) . . . . ? C29 N1 Ni1 N9 -76.8(7) . . . . ? C1 N1 Ni1 N9 44.6(5) . . . . ? C15 N1 Ni1 N9 161.5(6) . . . . ? C29 N1 Ni1 N2 -158.2(6) . . . . ? C1 N1 Ni1 N2 -36.7(4) . . . . ? C15 N1 Ni1 N2 80.2(6) . . . . ? C29 N1 Ni1 S2 -155(100) . . . . ? C1 N1 Ni1 S2 -34(84) . . . . ? C15 N1 Ni1 S2 83(84) . . . . ? C30 N8 Ni1 N5 -92.21(12) . . . . ? C34 N8 Ni1 N5 85.97(14) . . . . ? C30 N8 Ni1 N1 -6.2(2) . . . . ? C34 N8 Ni1 N1 172.0(2) . . . . ? C30 N8 Ni1 N9 87.7(2) . . . . ? C34 N8 Ni1 N9 -94.1(2) . . . . ? C30 N8 Ni1 N2 7.3(4) . . . . ? C34 N8 Ni1 N2 -174.5(3) . . . . ? C30 N8 Ni1 S2 173.81(7) . . . . ? C34 N8 Ni1 S2 -8.01(12) . . . . ? C2 N2 Ni1 N5 116.64(11) . . . . ? C6 N2 Ni1 N5 -87.73(14) . . . . ? C2 N2 Ni1 N1 32.2(2) . . . . ? C6 N2 Ni1 N1 -172.2(2) . . . . ? C2 N2 Ni1 N8 18.4(4) . . . . ? C6 N2 Ni1 N8 174.0(3) . . . . ? C2 N2 Ni1 N9 -64.2(2) . . . . ? C6 N2 Ni1 N9 91.4(3) . . . . ? C2 N2 Ni1 S2 -147.80(7) . . . . ? C6 N2 Ni1 S2 7.83(13) . . . . ? C36 C35 N9 Ni1 26(18) . . . . ? N5 Ni1 N9 C35 -20(7) . . . . ? N1 Ni1 N9 C35 -115.6(15) . . . . ? N8 Ni1 N9 C35 162.0(15) . . . . ? N2 Ni1 N9 C35 -40.4(15) . . . . ? S2 Ni1 N9 C35 64.2(15) . . . . ? N6 C21 S2 Ni1 13.8(11) . . . . ? N7 C21 S2 Ni1 -168.1(6) . . . . ? N5 Ni1 S2 C21 -15.8(4) . . . . ? N1 Ni1 S2 C21 -115(84) . . . . ? N8 Ni1 S2 C21 73.2(4) . . . . ? N9 Ni1 S2 C21 166.6(5) . . . . ? N2 Ni1 S2 C21 -112.0(4) . . . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 20.81 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 0.886 _refine_diff_density_min -0.390 _refine_diff_density_rms 0.094 data_aja0816 _database_code_depnum_ccdc_archive 'CCDC 844369' #TrackingRef '- aja0816_4.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C34 H30 Cu N8 O2 S2, 2(Cl O4)' _chemical_formula_sum 'C34 H30 Cl2 Cu N8 O10 S2' _chemical_formula_weight 909.22 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' S S 0.1246 0.1234 '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' Cu Cu 0.3201 1.2651 '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 Monoclinic _symmetry_space_group_name_H-M P21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 13.9290(3) _cell_length_b 11.8320(2) _cell_length_c 22.3070(5) _cell_angle_alpha 90.00 _cell_angle_beta 91.2240(10) _cell_angle_gamma 90.00 _cell_volume 3675.53(13) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 5895 _cell_measurement_theta_min 2.92 _cell_measurement_theta_max 27.45 _exptl_crystal_description needle _exptl_crystal_colour colourless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.643 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1860 _exptl_absorpt_coefficient_mu 0.924 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.8367 _exptl_absorpt_correction_T_max 0.9133 _exptl_absorpt_process_details Denzo/Scalepack _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 'Nonius KappaCCD' _diffrn_measurement_method 'CCD scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 29591 _diffrn_reflns_av_R_equivalents 0.1136 _diffrn_reflns_av_sigmaI/netI 0.0898 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 2.92 _diffrn_reflns_theta_max 27.45 _reflns_number_total 8371 _reflns_number_gt 5895 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'cOLLECT,Nonius BV, 1997-2001' _computing_cell_refinement DENZO/SCALEPACK _computing_data_reduction DENZO/SCALEPACK _computing_structure_solution SHELXs-97 _computing_structure_refinement SHELXL-97 _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^)+(0.0413P)^2^+2.8090P] 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 8371 _refine_ls_number_parameters 514 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0875 _refine_ls_R_factor_gt 0.0539 _refine_ls_wR_factor_ref 0.1280 _refine_ls_wR_factor_gt 0.1147 _refine_ls_goodness_of_fit_ref 1.032 _refine_ls_restrained_S_all 1.032 _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 C1 C 0.1797(2) 0.2356(3) 1.03333(14) 0.0267(7) Uani 1 1 d . . . H1A H 0.2228 0.1691 1.0340 0.032 Uiso 1 1 calc R . . H1B H 0.1212 0.2162 1.0556 0.032 Uiso 1 1 calc R . . C2 C 0.2295(2) 0.3349(3) 1.06267(14) 0.0222(7) Uani 1 1 d . . . C3 C 0.2288(3) 0.3527(3) 1.12352(15) 0.0294(8) Uani 1 1 d . . . H3 H 0.1963 0.3021 1.1492 0.035 Uiso 1 1 calc R . . C4 C 0.2767(3) 0.4463(3) 1.14658(15) 0.0320(8) Uani 1 1 d . . . H4 H 0.2770 0.4609 1.1885 0.038 Uiso 1 1 calc R . . C5 C 0.3237(3) 0.5180(3) 1.10871(14) 0.0282(8) Uani 1 1 d . . . H5A H 0.3566 0.5826 1.1239 0.034 Uiso 1 1 calc R . . C6 C 0.3221(2) 0.4942(3) 1.04772(14) 0.0216(7) Uani 1 1 d . . . C7 C 0.4051(2) 0.5555(3) 0.95614(14) 0.0212(7) Uani 1 1 d . . . C8 C 0.4815(2) 0.7457(3) 0.96129(15) 0.0225(7) Uani 1 1 d . . . C9 C 0.5432(2) 0.8226(3) 0.92674(15) 0.0255(7) Uani 1 1 d . . . C10 C 0.5663(3) 0.8065(3) 0.86733(16) 0.0361(9) Uani 1 1 d . . . H10 H 0.5411 0.7432 0.8460 0.043 Uiso 1 1 calc R . . C11 C 0.6261(3) 0.8819(3) 0.83862(18) 0.0413(10) Uani 1 1 d . . . H11 H 0.6423 0.8692 0.7980 0.050 Uiso 1 1 calc R . . C12 C 0.6620(3) 0.9750(3) 0.86855(17) 0.0351(9) Uani 1 1 d . . . H12 H 0.7021 1.0273 0.8486 0.042 Uiso 1 1 calc R . . C13 C 0.6391(3) 0.9916(3) 0.92801(18) 0.0338(9) Uani 1 1 d . . . H13 H 0.6638 1.0556 0.9489 0.041 Uiso 1 1 calc R . . C14 C 0.5811(2) 0.9164(3) 0.95714(16) 0.0283(8) Uani 1 1 d . . . H14 H 0.5667 0.9282 0.9981 0.034 Uiso 1 1 calc R . . C15 C 0.0701(2) 0.3432(3) 0.96783(14) 0.0252(7) Uani 1 1 d . . . H15A H 0.0733 0.3953 1.0025 0.030 Uiso 1 1 calc R . . H15B H 0.0098 0.2992 0.9702 0.030 Uiso 1 1 calc R . . C16 C 0.0696(2) 0.4100(3) 0.91091(14) 0.0242(7) Uani 1 1 d . . . C17 C -0.0141(3) 0.4555(3) 0.88655(16) 0.0339(8) Uani 1 1 d . . . H17 H -0.0742 0.4415 0.9045 0.041 Uiso 1 1 calc R . . C18 C -0.0088(3) 0.5217(3) 0.83581(17) 0.0391(9) Uani 1 1 d . . . H18 H -0.0650 0.5551 0.8186 0.047 Uiso 1 1 calc R . . C19 C 0.0797(3) 0.5385(3) 0.81034(16) 0.0341(8) Uani 1 1 d . . . H19 H 0.0854 0.5839 0.7755 0.041 Uiso 1 1 calc R . . C20 C 0.1594(2) 0.4885(3) 0.83642(14) 0.0246(7) Uani 1 1 d . . . C21 C 0.2918(3) 0.4220(3) 0.77793(14) 0.0295(8) Uani 1 1 d . . . C22 C 0.4294(3) 0.5491(3) 0.75689(16) 0.0331(8) Uani 1 1 d . . . C23 C 0.5001(3) 0.5709(4) 0.70913(16) 0.0394(9) Uani 1 1 d . . . C24 C 0.5500(3) 0.6734(5) 0.7123(2) 0.0621(14) Uani 1 1 d . . . H24 H 0.5405 0.7232 0.7451 0.075 Uiso 1 1 calc R . . C25 C 0.6138(3) 0.7026(5) 0.6676(2) 0.0697(16) Uani 1 1 d . . . H25 H 0.6485 0.7716 0.6702 0.084 Uiso 1 1 calc R . . C26 C 0.6262(3) 0.6322(5) 0.6203(3) 0.0725(18) Uani 1 1 d . . . H26 H 0.6694 0.6529 0.5898 0.087 Uiso 1 1 calc R . . C27 C 0.5772(4) 0.5313(5) 0.6158(2) 0.0687(17) Uani 1 1 d . . . H27 H 0.5860 0.4836 0.5820 0.082 Uiso 1 1 calc R . . C28 C 0.5147(3) 0.4991(4) 0.66060(18) 0.0480(11) Uani 1 1 d . . . H28 H 0.4822 0.4286 0.6581 0.058 Uiso 1 1 calc R . . C29 C 0.1366(3) 0.1633(3) 0.93272(16) 0.0297(8) Uani 1 1 d . . . H29A H 0.0948 0.1834 0.8979 0.036 Uiso 1 1 calc R . . H29B H 0.1034 0.1048 0.9563 0.036 Uiso 1 1 calc R . . C30 C 0.2301(2) 0.1169(3) 0.91100(14) 0.0262(7) Uani 1 1 d . . . C31 C 0.2411(3) 0.0060(3) 0.89333(16) 0.0328(8) Uani 1 1 d . . . H31 H 0.1902 -0.0466 0.8980 0.039 Uiso 1 1 calc R . . C32 C 0.3262(3) -0.0279(3) 0.86897(16) 0.0366(9) Uani 1 1 d . . . H32 H 0.3349 -0.1041 0.8568 0.044 Uiso 1 1 calc R . . C33 C 0.3988(3) 0.0503(3) 0.86248(15) 0.0321(8) Uani 1 1 d . . . H33 H 0.4580 0.0291 0.8452 0.039 Uiso 1 1 calc R . . C34 C 0.3842(2) 0.1597(3) 0.88144(14) 0.0264(7) Uani 1 1 d . . . H34 H 0.4344 0.2133 0.8772 0.032 Uiso 1 1 calc R . . N1 N 0.15337(19) 0.2651(2) 0.97059(11) 0.0231(6) Uani 1 1 d . . . N2 N 0.27606(19) 0.4038(2) 1.02481(11) 0.0207(6) Uani 1 1 d . . . N3 N 0.36790(19) 0.5706(2) 1.00985(11) 0.0231(6) Uani 1 1 d . . . H3A H 0.3728 0.6399 1.0239 0.028 Uiso 1 1 calc R . . N4 N 0.45361(19) 0.6454(2) 0.93232(12) 0.0228(6) Uani 1 1 d . . . H4A H 0.4690 0.6394 0.8944 0.027 Uiso 1 1 calc R . . N5 N 0.15593(19) 0.4264(2) 0.88612(11) 0.0217(6) Uani 1 1 d . . . N6 N 0.2504(2) 0.5037(2) 0.81086(12) 0.0255(6) Uani 1 1 d . . . H6 H 0.2810 0.5680 0.8166 0.031 Uiso 1 1 calc R . . N7 N 0.3783(2) 0.4499(3) 0.75233(13) 0.0334(7) Uani 1 1 d . . . H7 H 0.4040 0.3970 0.7301 0.040 Uiso 1 1 calc R . . N8 N 0.30180(19) 0.1931(2) 0.90557(11) 0.0225(6) Uani 1 1 d . . . S1 S 0.40589(6) 0.43623(6) 0.91439(4) 0.02273(18) Uani 1 1 d . . . S2 S 0.24333(8) 0.29592(8) 0.76449(4) 0.0383(2) Uani 1 1 d . . . O1 O 0.45746(17) 0.76537(18) 1.01235(10) 0.0309(6) Uani 1 1 d . . . O2 O 0.41442(18) 0.6190(2) 0.79643(11) 0.0359(6) Uani 1 1 d . . . O3 O 0.6635(2) 0.1545(2) 0.75801(12) 0.0496(8) Uani 1 1 d . . . O4 O 0.5292(3) 0.2622(3) 0.7366(2) 0.0877(13) Uani 1 1 d . . . O5 O 0.5919(3) 0.2505(3) 0.83566(14) 0.0727(11) Uani 1 1 d . . . O6 O 0.6738(2) 0.3509(2) 0.76239(13) 0.0603(9) Uani 1 1 d . . . O7 O 0.2271(2) 0.6999(2) 0.90424(12) 0.0529(8) Uani 1 1 d . . . O8 O 0.14683(19) 0.6217(2) 0.98586(12) 0.0432(7) Uani 1 1 d . . . O9 O 0.0909(2) 0.7898(3) 0.94251(16) 0.0678(10) Uani 1 1 d . . . O10 O 0.2361(2) 0.7881(3) 0.99606(13) 0.0573(8) Uani 1 1 d . . . Cu1 Cu 0.26826(3) 0.34787(3) 0.938821(16) 0.02015(11) Uani 1 1 d . . . Cl1 Cl 0.61402(7) 0.25588(7) 0.77324(4) 0.0362(2) Uani 1 1 d . . . Cl2 Cl 0.17449(6) 0.72494(7) 0.95693(4) 0.0317(2) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0251(19) 0.0274(17) 0.0275(17) 0.0063(14) 0.0027(14) -0.0045(15) C2 0.0165(17) 0.0231(16) 0.0270(16) 0.0054(13) 0.0008(12) 0.0026(13) C3 0.029(2) 0.0336(19) 0.0257(17) 0.0044(15) 0.0063(14) -0.0006(16) C4 0.031(2) 0.043(2) 0.0226(17) 0.0005(16) 0.0044(14) -0.0007(17) C5 0.028(2) 0.0324(19) 0.0240(17) -0.0064(15) 0.0009(14) -0.0056(15) C6 0.0179(17) 0.0233(16) 0.0237(16) 0.0015(13) 0.0008(13) 0.0012(13) C7 0.0141(17) 0.0230(16) 0.0264(16) 0.0039(14) -0.0005(12) -0.0023(13) C8 0.0171(17) 0.0195(16) 0.0307(18) 0.0016(14) -0.0037(13) -0.0010(13) C9 0.0215(19) 0.0194(16) 0.0354(19) 0.0026(14) -0.0018(14) 0.0006(14) C10 0.044(2) 0.0250(18) 0.039(2) -0.0005(16) 0.0081(17) -0.0119(17) C11 0.047(3) 0.032(2) 0.045(2) 0.0007(18) 0.0142(19) -0.0061(18) C12 0.029(2) 0.0284(19) 0.048(2) 0.0142(17) -0.0017(17) -0.0061(16) C13 0.026(2) 0.0235(17) 0.051(2) 0.0031(17) -0.0109(17) -0.0086(15) C14 0.028(2) 0.0233(17) 0.0339(19) 0.0014(15) -0.0051(14) -0.0036(15) C15 0.0190(18) 0.0300(18) 0.0269(17) -0.0001(14) 0.0030(13) -0.0017(14) C16 0.0187(18) 0.0242(17) 0.0296(17) -0.0006(14) -0.0005(13) -0.0028(14) C17 0.023(2) 0.042(2) 0.037(2) -0.0006(17) -0.0008(15) 0.0015(16) C18 0.028(2) 0.051(2) 0.038(2) 0.0033(18) -0.0086(16) 0.0121(18) C19 0.034(2) 0.039(2) 0.0288(19) 0.0081(16) -0.0066(15) 0.0029(17) C20 0.027(2) 0.0232(17) 0.0235(17) -0.0006(14) -0.0033(14) -0.0005(14) C21 0.031(2) 0.035(2) 0.0225(17) 0.0047(15) 0.0012(14) 0.0004(16) C22 0.031(2) 0.041(2) 0.0266(18) 0.0105(17) -0.0022(15) -0.0013(17) C23 0.027(2) 0.060(3) 0.031(2) 0.0172(18) 0.0018(16) 0.0031(19) C24 0.055(3) 0.090(4) 0.042(2) 0.020(2) -0.004(2) -0.032(3) C25 0.043(3) 0.105(4) 0.061(3) 0.039(3) -0.002(2) -0.018(3) C26 0.034(3) 0.103(4) 0.082(4) 0.065(3) 0.028(3) 0.033(3) C27 0.070(4) 0.073(4) 0.064(3) 0.032(3) 0.039(3) 0.046(3) C28 0.047(3) 0.056(3) 0.041(2) 0.022(2) 0.0161(19) 0.025(2) C29 0.027(2) 0.0261(18) 0.0363(19) 0.0000(15) 0.0012(15) -0.0101(15) C30 0.030(2) 0.0252(17) 0.0236(17) 0.0036(14) -0.0038(14) -0.0091(15) C31 0.037(2) 0.0200(17) 0.041(2) 0.0034(16) -0.0070(16) -0.0068(16) C32 0.046(3) 0.0245(18) 0.038(2) -0.0050(16) -0.0125(18) 0.0074(18) C33 0.034(2) 0.0324(19) 0.0298(19) -0.0027(16) -0.0029(15) 0.0068(17) C34 0.029(2) 0.0277(18) 0.0223(16) 0.0007(14) -0.0021(14) 0.0022(15) N1 0.0220(15) 0.0229(14) 0.0243(14) 0.0024(11) -0.0012(11) -0.0038(12) N2 0.0203(15) 0.0192(13) 0.0226(13) 0.0000(11) 0.0007(11) -0.0012(11) N3 0.0272(16) 0.0182(13) 0.0240(14) -0.0007(11) 0.0021(11) -0.0058(12) N4 0.0244(15) 0.0223(13) 0.0217(13) -0.0009(11) 0.0004(11) -0.0037(12) N5 0.0179(15) 0.0217(13) 0.0254(14) -0.0013(11) -0.0008(11) -0.0016(11) N6 0.0273(17) 0.0232(14) 0.0258(14) 0.0035(12) 0.0000(12) -0.0035(12) N7 0.0363(19) 0.0360(17) 0.0280(16) -0.0030(13) 0.0070(13) -0.0030(14) N8 0.0245(16) 0.0213(13) 0.0216(13) 0.0004(11) -0.0012(11) -0.0013(12) S1 0.0208(5) 0.0209(4) 0.0266(4) -0.0023(3) 0.0038(3) -0.0042(3) S2 0.0472(6) 0.0323(5) 0.0354(5) -0.0045(4) 0.0047(4) -0.0068(4) O1 0.0376(15) 0.0253(12) 0.0298(13) -0.0026(10) 0.0043(11) -0.0071(11) O2 0.0385(16) 0.0376(14) 0.0315(14) 0.0032(12) 0.0005(11) -0.0096(12) O3 0.063(2) 0.0500(17) 0.0353(15) -0.0051(13) -0.0037(13) 0.0188(15) O4 0.065(2) 0.0481(19) 0.148(4) -0.026(2) -0.053(2) 0.0163(18) O5 0.102(3) 0.064(2) 0.0543(19) -0.0267(16) 0.0493(18) -0.0362(19) O6 0.077(2) 0.0570(19) 0.0467(18) 0.0020(15) 0.0069(16) -0.0298(17) O7 0.063(2) 0.0559(18) 0.0408(16) -0.0074(14) 0.0219(14) -0.0148(16) O8 0.0353(16) 0.0350(14) 0.0599(18) 0.0166(13) 0.0145(13) 0.0024(12) O9 0.0326(18) 0.063(2) 0.108(3) 0.046(2) 0.0089(17) 0.0123(15) O10 0.061(2) 0.0587(19) 0.0518(18) -0.0205(15) -0.0005(15) -0.0156(16) Cu1 0.0185(2) 0.0196(2) 0.0224(2) 0.00119(15) 0.00111(15) -0.00376(16) Cl1 0.0363(5) 0.0346(5) 0.0377(5) -0.0096(4) 0.0054(4) -0.0042(4) Cl2 0.0270(5) 0.0320(5) 0.0362(5) 0.0026(4) 0.0054(4) -0.0028(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.481(4) . ? C1 C2 1.507(4) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 N2 1.350(4) . ? C2 C3 1.374(5) . ? C3 C4 1.386(5) . ? C3 H3 0.9500 . ? C4 C5 1.373(5) . ? C4 H4 0.9500 . ? C5 C6 1.389(4) . ? C5 H5A 0.9500 . ? C6 N2 1.343(4) . ? C6 N3 1.400(4) . ? C7 N3 1.328(4) . ? C7 N4 1.373(4) . ? C7 S1 1.691(3) . ? C8 O1 1.216(4) . ? C8 N4 1.403(4) . ? C8 C9 1.479(4) . ? C9 C10 1.384(5) . ? C9 C14 1.398(5) . ? C10 C11 1.386(5) . ? C10 H10 0.9500 . ? C11 C12 1.377(5) . ? C11 H11 0.9500 . ? C12 C13 1.385(5) . ? C12 H12 0.9500 . ? C13 C14 1.375(5) . ? C13 H13 0.9500 . ? C14 H14 0.9500 . ? C15 N1 1.483(4) . ? C15 C16 1.496(4) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 N5 1.348(4) . ? C16 C17 1.385(5) . ? C17 C18 1.379(5) . ? C17 H17 0.9500 . ? C18 C19 1.382(5) . ? C18 H18 0.9500 . ? C19 C20 1.376(5) . ? C19 H19 0.9500 . ? C20 N5 1.331(4) . ? C20 N6 1.413(4) . ? C21 N6 1.350(4) . ? C21 N7 1.383(4) . ? C21 S2 1.663(4) . ? C22 O2 1.230(4) . ? C22 N7 1.376(5) . ? C22 C23 1.488(5) . ? C23 C28 1.394(6) . ? C23 C24 1.400(6) . ? C24 C25 1.393(6) . ? C24 H24 0.9500 . ? C25 C26 1.359(8) . ? C25 H25 0.9500 . ? C26 C27 1.378(8) . ? C26 H26 0.9500 . ? C27 C28 1.393(6) . ? C27 H27 0.9500 . ? C28 H28 0.9500 . ? C29 N1 1.487(4) . ? C29 C30 1.503(5) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C30 N8 1.352(4) . ? C30 C31 1.380(5) . ? C31 C32 1.374(5) . ? C31 H31 0.9500 . ? C32 C33 1.382(5) . ? C32 H32 0.9500 . ? C33 C34 1.378(5) . ? C33 H33 0.9500 . ? C34 N8 1.337(4) . ? C34 H34 0.9500 . ? N1 Cu1 2.018(3) . ? N2 Cu1 2.030(2) . ? N3 H3A 0.8800 . ? N4 H4A 0.8800 . ? N5 Cu1 2.148(3) . ? N6 H6 0.8800 . ? N7 H7 0.8800 . ? N8 Cu1 2.034(3) . ? S1 Cu1 2.2605(9) . ? O3 Cl1 1.428(3) . ? O4 Cl1 1.424(3) . ? O5 Cl1 1.434(3) . ? O6 Cl1 1.423(3) . ? O7 Cl2 1.429(3) . ? O8 Cl2 1.438(2) . ? O9 Cl2 1.425(3) . ? O10 Cl2 1.423(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 N1 C1 C2 109.2(2) . . ? N1 C1 H1A 109.8 . . ? C2 C1 H1A 109.8 . . ? N1 C1 H1B 109.8 . . ? C2 C1 H1B 109.8 . . ? H1A C1 H1B 108.3 . . ? N2 C2 C3 122.7(3) . . ? N2 C2 C1 115.0(3) . . ? C3 C2 C1 122.4(3) . . ? C2 C3 C4 118.4(3) . . ? C2 C3 H3 120.8 . . ? C4 C3 H3 120.8 . . ? C5 C4 C3 119.8(3) . . ? C5 C4 H4 120.1 . . ? C3 C4 H4 120.1 . . ? C4 C5 C6 118.6(3) . . ? C4 C5 H5A 120.7 . . ? C6 C5 H5A 120.7 . . ? N2 C6 C5 122.1(3) . . ? N2 C6 N3 120.3(3) . . ? C5 C6 N3 117.5(3) . . ? N3 C7 N4 116.7(3) . . ? N3 C7 S1 128.1(2) . . ? N4 C7 S1 115.1(2) . . ? O1 C8 N4 120.9(3) . . ? O1 C8 C9 123.0(3) . . ? N4 C8 C9 116.0(3) . . ? C10 C9 C14 118.7(3) . . ? C10 C9 C8 124.4(3) . . ? C14 C9 C8 116.9(3) . . ? C9 C10 C11 120.6(3) . . ? C9 C10 H10 119.7 . . ? C11 C10 H10 119.7 . . ? C12 C11 C10 120.4(4) . . ? C12 C11 H11 119.8 . . ? C10 C11 H11 119.8 . . ? C11 C12 C13 119.3(3) . . ? C11 C12 H12 120.4 . . ? C13 C12 H12 120.4 . . ? C14 C13 C12 120.7(3) . . ? C14 C13 H13 119.6 . . ? C12 C13 H13 119.6 . . ? C13 C14 C9 120.3(3) . . ? C13 C14 H14 119.9 . . ? C9 C14 H14 119.9 . . ? N1 C15 C16 110.7(3) . . ? N1 C15 H15A 109.5 . . ? C16 C15 H15A 109.5 . . ? N1 C15 H15B 109.5 . . ? C16 C15 H15B 109.5 . . ? H15A C15 H15B 108.1 . . ? N5 C16 C17 122.3(3) . . ? N5 C16 C15 115.9(3) . . ? C17 C16 C15 121.8(3) . . ? C18 C17 C16 118.9(3) . . ? C18 C17 H17 120.6 . . ? C16 C17 H17 120.6 . . ? C17 C18 C19 118.9(3) . . ? C17 C18 H18 120.5 . . ? C19 C18 H18 120.5 . . ? C20 C19 C18 118.8(3) . . ? C20 C19 H19 120.6 . . ? C18 C19 H19 120.6 . . ? N5 C20 C19 123.1(3) . . ? N5 C20 N6 117.1(3) . . ? C19 C20 N6 119.8(3) . . ? N6 C21 N7 116.1(3) . . ? N6 C21 S2 124.3(3) . . ? N7 C21 S2 119.6(3) . . ? O2 C22 N7 122.0(3) . . ? O2 C22 C23 121.5(3) . . ? N7 C22 C23 116.4(3) . . ? C28 C23 C24 119.2(4) . . ? C28 C23 C22 124.1(4) . . ? C24 C23 C22 116.7(4) . . ? C25 C24 C23 120.1(5) . . ? C25 C24 H24 120.0 . . ? C23 C24 H24 120.0 . . ? C26 C25 C24 119.9(5) . . ? C26 C25 H25 120.1 . . ? C24 C25 H25 120.1 . . ? C25 C26 C27 121.2(4) . . ? C25 C26 H26 119.4 . . ? C27 C26 H26 119.4 . . ? C26 C27 C28 120.0(5) . . ? C26 C27 H27 120.0 . . ? C28 C27 H27 120.0 . . ? C27 C28 C23 119.6(5) . . ? C27 C28 H28 120.2 . . ? C23 C28 H28 120.2 . . ? N1 C29 C30 110.6(3) . . ? N1 C29 H29A 109.5 . . ? C30 C29 H29A 109.5 . . ? N1 C29 H29B 109.5 . . ? C30 C29 H29B 109.5 . . ? H29A C29 H29B 108.1 . . ? N8 C30 C31 121.4(3) . . ? N8 C30 C29 115.6(3) . . ? C31 C30 C29 122.8(3) . . ? C32 C31 C30 119.5(3) . . ? C32 C31 H31 120.2 . . ? C30 C31 H31 120.2 . . ? C31 C32 C33 119.1(3) . . ? C31 C32 H32 120.5 . . ? C33 C32 H32 120.5 . . ? C34 C33 C32 118.9(3) . . ? C34 C33 H33 120.5 . . ? C32 C33 H33 120.5 . . ? N8 C34 C33 122.3(3) . . ? N8 C34 H34 118.8 . . ? C33 C34 H34 118.8 . . ? C1 N1 C15 111.3(3) . . ? C1 N1 C29 112.2(2) . . ? C15 N1 C29 111.6(3) . . ? C1 N1 Cu1 105.33(19) . . ? C15 N1 Cu1 107.98(19) . . ? C29 N1 Cu1 108.04(19) . . ? C6 N2 C2 118.4(3) . . ? C6 N2 Cu1 129.4(2) . . ? C2 N2 Cu1 112.2(2) . . ? C7 N3 C6 130.4(3) . . ? C7 N3 H3A 114.8 . . ? C6 N3 H3A 114.8 . . ? C7 N4 C8 127.7(3) . . ? C7 N4 H4A 116.2 . . ? C8 N4 H4A 116.2 . . ? C20 N5 C16 118.0(3) . . ? C20 N5 Cu1 130.9(2) . . ? C16 N5 Cu1 111.0(2) . . ? C21 N6 C20 121.7(3) . . ? C21 N6 H6 119.1 . . ? C20 N6 H6 119.1 . . ? C22 N7 C21 128.8(3) . . ? C22 N7 H7 115.6 . . ? C21 N7 H7 115.6 . . ? C34 N8 C30 118.8(3) . . ? C34 N8 Cu1 128.2(2) . . ? C30 N8 Cu1 113.0(2) . . ? C7 S1 Cu1 103.75(11) . . ? N1 Cu1 N2 81.55(10) . . ? N1 Cu1 N8 83.17(11) . . ? N2 Cu1 N8 129.04(10) . . ? N1 Cu1 N5 80.11(10) . . ? N2 Cu1 N5 113.57(10) . . ? N8 Cu1 N5 111.11(10) . . ? N1 Cu1 S1 172.88(8) . . ? N2 Cu1 S1 92.79(8) . . ? N8 Cu1 S1 97.24(8) . . ? N5 Cu1 S1 106.23(7) . . ? O6 Cl1 O4 110.1(2) . . ? O6 Cl1 O3 109.62(19) . . ? O4 Cl1 O3 107.85(18) . . ? O6 Cl1 O5 109.81(18) . . ? O4 Cl1 O5 111.5(3) . . ? O3 Cl1 O5 107.96(19) . . ? O10 Cl2 O9 109.5(2) . . ? O10 Cl2 O7 107.47(18) . . ? O9 Cl2 O7 110.9(2) . . ? O10 Cl2 O8 109.55(18) . . ? O9 Cl2 O8 109.47(17) . . ? O7 Cl2 O8 109.90(17) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 C1 C2 N2 -27.4(4) . . . . ? N1 C1 C2 C3 153.6(3) . . . . ? N2 C2 C3 C4 1.0(5) . . . . ? C1 C2 C3 C4 180.0(3) . . . . ? C2 C3 C4 C5 -0.4(5) . . . . ? C3 C4 C5 C6 -0.2(5) . . . . ? C4 C5 C6 N2 0.2(5) . . . . ? C4 C5 C6 N3 177.9(3) . . . . ? O1 C8 C9 C10 -175.4(3) . . . . ? N4 C8 C9 C10 6.3(5) . . . . ? O1 C8 C9 C14 5.6(5) . . . . ? N4 C8 C9 C14 -172.6(3) . . . . ? C14 C9 C10 C11 0.1(5) . . . . ? C8 C9 C10 C11 -178.9(3) . . . . ? C9 C10 C11 C12 -1.1(6) . . . . ? C10 C11 C12 C13 1.1(6) . . . . ? C11 C12 C13 C14 -0.1(6) . . . . ? C12 C13 C14 C9 -0.9(5) . . . . ? C10 C9 C14 C13 0.9(5) . . . . ? C8 C9 C14 C13 179.9(3) . . . . ? N1 C15 C16 N5 -26.8(4) . . . . ? N1 C15 C16 C17 155.5(3) . . . . ? N5 C16 C17 C18 -1.2(5) . . . . ? C15 C16 C17 C18 176.4(3) . . . . ? C16 C17 C18 C19 1.2(6) . . . . ? C17 C18 C19 C20 0.2(6) . . . . ? C18 C19 C20 N5 -1.7(5) . . . . ? C18 C19 C20 N6 179.4(3) . . . . ? O2 C22 C23 C28 -174.7(4) . . . . ? N7 C22 C23 C28 1.7(5) . . . . ? O2 C22 C23 C24 1.5(5) . . . . ? N7 C22 C23 C24 177.9(4) . . . . ? C28 C23 C24 C25 -0.3(7) . . . . ? C22 C23 C24 C25 -176.7(4) . . . . ? C23 C24 C25 C26 1.1(7) . . . . ? C24 C25 C26 C27 -0.5(7) . . . . ? C25 C26 C27 C28 -0.9(7) . . . . ? C26 C27 C28 C23 1.7(6) . . . . ? C24 C23 C28 C27 -1.1(6) . . . . ? C22 C23 C28 C27 175.0(4) . . . . ? N1 C29 C30 N8 -27.5(4) . . . . ? N1 C29 C30 C31 157.1(3) . . . . ? N8 C30 C31 C32 -0.8(5) . . . . ? C29 C30 C31 C32 174.2(3) . . . . ? C30 C31 C32 C33 -0.3(5) . . . . ? C31 C32 C33 C34 0.9(5) . . . . ? C32 C33 C34 N8 -0.4(5) . . . . ? C2 C1 N1 C15 -74.5(3) . . . . ? C2 C1 N1 C29 159.6(3) . . . . ? C2 C1 N1 Cu1 42.2(3) . . . . ? C16 C15 N1 C1 155.8(3) . . . . ? C16 C15 N1 C29 -77.9(3) . . . . ? C16 C15 N1 Cu1 40.7(3) . . . . ? C30 C29 N1 C1 -82.5(3) . . . . ? C30 C29 N1 C15 151.8(3) . . . . ? C30 C29 N1 Cu1 33.2(3) . . . . ? C5 C6 N2 C2 0.4(5) . . . . ? N3 C6 N2 C2 -177.2(3) . . . . ? C5 C6 N2 Cu1 -177.1(2) . . . . ? N3 C6 N2 Cu1 5.2(4) . . . . ? C3 C2 N2 C6 -1.0(5) . . . . ? C1 C2 N2 C6 180.0(3) . . . . ? C3 C2 N2 Cu1 176.9(3) . . . . ? C1 C2 N2 Cu1 -2.1(3) . . . . ? N4 C7 N3 C6 -174.1(3) . . . . ? S1 C7 N3 C6 2.2(5) . . . . ? N2 C6 N3 C7 -26.9(5) . . . . ? C5 C6 N3 C7 155.3(3) . . . . ? N3 C7 N4 C8 10.6(5) . . . . ? S1 C7 N4 C8 -166.1(3) . . . . ? O1 C8 N4 C7 -5.4(5) . . . . ? C9 C8 N4 C7 173.0(3) . . . . ? C19 C20 N5 C16 1.7(5) . . . . ? N6 C20 N5 C16 -179.4(3) . . . . ? C19 C20 N5 Cu1 -175.8(2) . . . . ? N6 C20 N5 Cu1 3.1(4) . . . . ? C17 C16 N5 C20 -0.2(5) . . . . ? C15 C16 N5 C20 -177.9(3) . . . . ? C17 C16 N5 Cu1 177.8(3) . . . . ? C15 C16 N5 Cu1 0.1(3) . . . . ? N7 C21 N6 C20 176.1(3) . . . . ? S2 C21 N6 C20 -1.0(4) . . . . ? N5 C20 N6 C21 78.0(4) . . . . ? C19 C20 N6 C21 -103.0(4) . . . . ? O2 C22 N7 C21 17.1(6) . . . . ? C23 C22 N7 C21 -159.3(3) . . . . ? N6 C21 N7 C22 1.7(5) . . . . ? S2 C21 N7 C22 179.0(3) . . . . ? C33 C34 N8 C30 -0.7(5) . . . . ? C33 C34 N8 Cu1 177.5(2) . . . . ? C31 C30 N8 C34 1.3(5) . . . . ? C29 C30 N8 C34 -174.1(3) . . . . ? C31 C30 N8 Cu1 -177.2(3) . . . . ? C29 C30 N8 Cu1 7.4(3) . . . . ? N3 C7 S1 Cu1 31.6(3) . . . . ? N4 C7 S1 Cu1 -152.1(2) . . . . ? C1 N1 Cu1 N2 -34.7(2) . . . . ? C15 N1 Cu1 N2 84.4(2) . . . . ? C29 N1 Cu1 N2 -154.8(2) . . . . ? C1 N1 Cu1 N8 96.6(2) . . . . ? C15 N1 Cu1 N8 -144.4(2) . . . . ? C29 N1 Cu1 N8 -23.6(2) . . . . ? C1 N1 Cu1 N5 -150.5(2) . . . . ? C15 N1 Cu1 N5 -31.50(19) . . . . ? C29 N1 Cu1 N5 89.3(2) . . . . ? C1 N1 Cu1 S1 2.8(8) . . . . ? C15 N1 Cu1 S1 121.9(6) . . . . ? C29 N1 Cu1 S1 -117.3(6) . . . . ? C6 N2 Cu1 N1 -161.0(3) . . . . ? C2 N2 Cu1 N1 21.4(2) . . . . ? C6 N2 Cu1 N8 125.0(3) . . . . ? C2 N2 Cu1 N8 -52.6(3) . . . . ? C6 N2 Cu1 N5 -85.7(3) . . . . ? C2 N2 Cu1 N5 96.7(2) . . . . ? C6 N2 Cu1 S1 23.4(3) . . . . ? C2 N2 Cu1 S1 -154.3(2) . . . . ? C34 N8 Cu1 N1 -168.8(3) . . . . ? C30 N8 Cu1 N1 9.5(2) . . . . ? C34 N8 Cu1 N2 -95.5(3) . . . . ? C30 N8 Cu1 N2 82.8(2) . . . . ? C34 N8 Cu1 N5 114.6(3) . . . . ? C30 N8 Cu1 N5 -67.1(2) . . . . ? C34 N8 Cu1 S1 4.1(3) . . . . ? C30 N8 Cu1 S1 -177.6(2) . . . . ? C20 N5 Cu1 N1 -164.1(3) . . . . ? C16 N5 Cu1 N1 18.2(2) . . . . ? C20 N5 Cu1 N2 119.7(3) . . . . ? C16 N5 Cu1 N2 -57.9(2) . . . . ? C20 N5 Cu1 N8 -85.5(3) . . . . ? C16 N5 Cu1 N8 96.9(2) . . . . ? C20 N5 Cu1 S1 19.2(3) . . . . ? C16 N5 Cu1 S1 -158.44(19) . . . . ? C7 S1 Cu1 N1 -71.2(7) . . . . ? C7 S1 Cu1 N2 -34.11(13) . . . . ? C7 S1 Cu1 N8 -164.04(13) . . . . ? C7 S1 Cu1 N5 81.43(13) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.45 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.555 _refine_diff_density_min -0.698 _refine_diff_density_rms 0.096 data_aja0817 _database_code_depnum_ccdc_archive 'CCDC 844370' #TrackingRef '- aja0817_6.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C34 H30 Cd N9 O2 S2, C2 H3 N, 2(Cl O4)' _chemical_formula_sum 'C36 H33 Cd Cl2 N9 O10 S2' _chemical_formula_weight 999.13 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' S S 0.1246 0.1234 '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 Monoclinic _symmetry_space_group_name_H-M P21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 16.4240(3) _cell_length_b 10.8230(2) _cell_length_c 22.9750(6) _cell_angle_alpha 90.00 _cell_angle_beta 97.7600(10) _cell_angle_gamma 90.00 _cell_volume 4046.57(15) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 48.4 _cell_measurement_theta_min 2.99 _cell_measurement_theta_max 27.48 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.640 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2024 _exptl_absorpt_coefficient_mu 0.844 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.8494 _exptl_absorpt_correction_T_max 0.8494 _exptl_absorpt_process_details Denzo/Scalepack _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 'Nonius KappaCCD' _diffrn_measurement_method 'CCD scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 32603 _diffrn_reflns_av_R_equivalents 0.1183 _diffrn_reflns_av_sigmaI/netI 0.1332 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 2.99 _diffrn_reflns_theta_max 27.48 _reflns_number_total 9235 _reflns_number_gt 4804 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'cOLLECT,Nonius BV, 1997-2001' _computing_cell_refinement DENZO/SCALEPACK _computing_data_reduction DENZO/SCALEPACK _computing_structure_solution SHELXs-97 _computing_structure_refinement SHELXL-97 _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^)+(0.0617P)^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 SHELXL _refine_ls_extinction_coef 0.0010(2) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 9235 _refine_ls_number_parameters 543 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1457 _refine_ls_R_factor_gt 0.0598 _refine_ls_wR_factor_ref 0.1465 _refine_ls_wR_factor_gt 0.1186 _refine_ls_goodness_of_fit_ref 0.994 _refine_ls_restrained_S_all 0.994 _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 C1 C 0.2443(3) 0.1680(6) 0.8063(2) 0.0662(17) Uani 1 1 d . . . H1A H 0.2562 0.2297 0.7780 0.079 Uiso 1 1 calc R . . H1B H 0.1991 0.1178 0.7878 0.079 Uiso 1 1 calc R . . C2 C 0.3191(3) 0.0865(5) 0.8213(2) 0.0423(13) Uani 1 1 d . . . C3 C 0.3676(3) 0.0564(5) 0.7789(2) 0.0418(12) Uani 1 1 d . . . H3 H 0.3565 0.0892 0.7413 0.050 Uiso 1 1 calc R . . C4 C 0.4330(3) -0.0231(5) 0.7931(2) 0.0401(12) Uani 1 1 d . . . H4 H 0.4671 -0.0436 0.7654 0.048 Uiso 1 1 calc R . . C5 C 0.4468(3) -0.0711(4) 0.8487(2) 0.0373(12) Uani 1 1 d . . . H5 H 0.4904 -0.1248 0.8594 0.045 Uiso 1 1 calc R . . C6 C 0.3951(3) -0.0387(4) 0.88837(19) 0.0335(11) Uani 1 1 d . . . C7 C 0.4028(2) -0.0571(4) 0.99708(19) 0.0304(11) Uani 1 1 d . . . C8 C 0.4520(3) -0.2614(5) 1.0364(2) 0.0390(12) Uani 1 1 d . . . C9 C 0.4842(3) -0.3275(5) 1.0914(2) 0.0414(12) Uani 1 1 d . . . C10 C 0.5036(3) -0.2714(5) 1.1454(2) 0.0449(13) Uani 1 1 d . . . H10 H 0.4936 -0.1874 1.1495 0.054 Uiso 1 1 calc R . . C11 C 0.5379(3) -0.3402(6) 1.1935(2) 0.0522(14) Uani 1 1 d . . . H11 H 0.5503 -0.3022 1.2299 0.063 Uiso 1 1 calc R . . C12 C 0.5535(3) -0.4636(6) 1.1877(2) 0.0610(16) Uani 1 1 d . . . H12 H 0.5776 -0.5086 1.2200 0.073 Uiso 1 1 calc R . . C13 C 0.5335(4) -0.5215(6) 1.1338(3) 0.0731(18) Uani 1 1 d . . . H13 H 0.5438 -0.6054 1.1299 0.088 Uiso 1 1 calc R . . C14 C 0.4981(4) -0.4538(5) 1.0860(2) 0.0609(16) Uani 1 1 d . . . H14 H 0.4835 -0.4927 1.0500 0.073 Uiso 1 1 calc R . . C15 C 0.1296(4) 0.2589(6) 0.8476(3) 0.075(2) Uani 1 1 d . . . H15A H 0.1156 0.2923 0.8084 0.090 Uiso 1 1 calc R . . H15B H 0.1177 0.3218 0.8753 0.090 Uiso 1 1 calc R . . C16 C 0.0771(3) 0.1484(7) 0.8542(3) 0.0694(19) Uani 1 1 d . . . C17 C 0.0086(4) 0.1266(9) 0.8123(3) 0.100(3) Uani 1 1 d . . . H17 H -0.0035 0.1773 0.7796 0.120 Uiso 1 1 calc R . . C18 C -0.0405(4) 0.0260(10) 0.8214(4) 0.104(3) Uani 1 1 d . . . H18 H -0.0857 0.0072 0.7940 0.125 Uiso 1 1 calc R . . C19 C -0.0231(4) -0.0448(8) 0.8702(3) 0.095(3) Uani 1 1 d . . . H19 H -0.0568 -0.1112 0.8765 0.114 Uiso 1 1 calc R . . C20 C 0.0459(3) -0.0174(7) 0.9109(3) 0.0658(19) Uani 1 1 d . . . C21 C 0.1116(3) -0.0905(6) 1.0093(3) 0.0564(16) Uani 1 1 d . . . C22 C 0.0448(4) -0.2810(7) 1.0450(4) 0.084(2) Uani 1 1 d . . . C23 C 0.0539(4) -0.3776(6) 1.0929(4) 0.078(2) Uani 1 1 d . . . C24 C 0.0003(5) -0.4798(7) 1.0811(4) 0.109(3) Uani 1 1 d . . . H24 H -0.0364 -0.4844 1.0466 0.131 Uiso 1 1 calc R . . C25 C 0.0048(7) -0.5732(8) 1.1232(5) 0.139(5) Uani 1 1 d . . . H25 H -0.0294 -0.6418 1.1171 0.166 Uiso 1 1 calc R . . C26 C 0.0587(8) -0.5641(8) 1.1730(5) 0.141(5) Uani 1 1 d . . . H26 H 0.0614 -0.6273 1.2006 0.169 Uiso 1 1 calc R . . C27 C 0.1092(5) -0.4642(7) 1.1836(4) 0.110(3) Uani 1 1 d . . . H27 H 0.1460 -0.4609 1.2181 0.132 Uiso 1 1 calc R . . C28 C 0.1065(5) -0.3670(7) 1.1436(4) 0.094(3) Uani 1 1 d . . . H28 H 0.1395 -0.2975 1.1513 0.113 Uiso 1 1 calc R . . C29 C 0.2692(4) 0.3412(6) 0.8731(2) 0.0629(16) Uani 1 1 d . . . H29A H 0.2538 0.4050 0.8440 0.075 Uiso 1 1 calc R . . H29B H 0.3265 0.3209 0.8719 0.075 Uiso 1 1 calc R . . C30 C 0.2601(3) 0.3908(6) 0.9326(3) 0.0602(16) Uani 1 1 d . . . C31 C 0.2717(4) 0.5133(6) 0.9473(3) 0.084(2) Uani 1 1 d . . . H31 H 0.2860 0.5688 0.9194 0.100 Uiso 1 1 calc R . . C32 C 0.2626(4) 0.5541(7) 1.0022(4) 0.094(2) Uani 1 1 d . . . H32 H 0.2705 0.6370 1.0121 0.112 Uiso 1 1 calc R . . C33 C 0.2414(4) 0.4702(7) 1.0427(3) 0.086(2) Uani 1 1 d . . . H33 H 0.2346 0.4953 1.0805 0.104 Uiso 1 1 calc R . . C34 C 0.2307(4) 0.3490(6) 1.0261(3) 0.0749(18) Uani 1 1 d . . . H34 H 0.2167 0.2925 1.0536 0.090 Uiso 1 1 calc R . . C35 C 0.2549(4) 0.1964(6) 1.1770(3) 0.084(2) Uani 1 1 d . . . H35A H 0.2487 0.1237 1.1528 0.126 Uiso 1 1 calc R . . H35B H 0.2204 0.2610 1.1588 0.126 Uiso 1 1 calc R . . H35C H 0.2394 0.1779 1.2149 0.126 Uiso 1 1 calc R . . C36 C 0.3417(5) 0.2372(7) 1.1840(3) 0.084(2) Uani 1 1 d . . . N1 N 0.2187(3) 0.2307(5) 0.85756(18) 0.0555(13) Uani 1 1 d . . . N2 N 0.3321(2) 0.0398(4) 0.87617(16) 0.0373(9) Uani 1 1 d . . . N3 N 0.4052(2) -0.1000(3) 0.94334(15) 0.0334(9) Uani 1 1 d . . . H3A H 0.4145 -0.1780 0.9415 0.040 Uiso 1 1 calc R . . N4 N 0.4229(2) -0.1424(3) 1.04201(16) 0.0340(9) Uani 1 1 d . . . H4A H 0.4167 -0.1189 1.0769 0.041 Uiso 1 1 calc R . . N5 N 0.0960(2) 0.0774(5) 0.9016(2) 0.0604(14) Uani 1 1 d . . . N6 N 0.0595(3) -0.0935(5) 0.9603(2) 0.0635(14) Uani 1 1 d . . . H6 H 0.0269 -0.1559 0.9583 0.076 Uiso 1 1 calc R . . N7 N 0.1043(3) -0.1898(4) 1.0475(2) 0.0659(14) Uani 1 1 d . . . H7 H 0.1426 -0.1948 1.0769 0.079 Uiso 1 1 calc R . . N8 N 0.2394(3) 0.3078(4) 0.9722(2) 0.0540(12) Uani 1 1 d . . . N9 N 0.4083(4) 0.2532(5) 1.1924(3) 0.0888(19) Uani 1 1 d . . . S1 S 0.38250(7) 0.08937(11) 1.01487(5) 0.0372(3) Uani 1 1 d . . . S2 S 0.18376(9) 0.01242(15) 1.03289(6) 0.0615(4) Uani 1 1 d . . . O1 O 0.4531(2) -0.3093(3) 0.98797(14) 0.0511(9) Uani 1 1 d . . . O2 O -0.0112(3) -0.2807(4) 1.0028(2) 0.0960(17) Uani 1 1 d . . . O3 O 0.2824(2) -0.2558(3) 0.84228(15) 0.0613(10) Uani 1 1 d . . . O4 O 0.1796(3) -0.1073(5) 0.81344(17) 0.0896(15) Uani 1 1 d . . . O5 O 0.21872(19) -0.1532(4) 0.91371(14) 0.0538(10) Uani 1 1 d . . . O6 O 0.1456(3) -0.2969(5) 0.8512(2) 0.130(2) Uani 1 1 d . . . O7 O 0.2769(3) -0.2421(4) 1.11415(19) 0.0809(13) Uani 1 1 d . . . O8 O 0.2291(2) -0.1186(4) 1.18476(19) 0.0807(13) Uani 1 1 d . . . O9 O 0.3570(2) -0.0758(3) 1.15470(16) 0.0602(10) Uani 1 1 d . . . O10 O 0.3403(3) -0.2524(5) 1.2119(2) 0.1085(17) Uani 1 1 d . . . Cd1 Cd 0.238852(19) 0.09807(4) 0.941219(14) 0.03976(16) Uani 1 1 d . . . Cl1 Cl 0.20642(8) -0.20419(16) 0.85482(6) 0.0633(5) Uani 1 1 d . . . Cl2 Cl 0.30087(9) -0.17287(15) 1.16664(7) 0.0642(4) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.073(4) 0.086(5) 0.039(3) 0.020(3) 0.006(3) 0.029(3) C2 0.045(3) 0.049(4) 0.033(3) 0.002(3) 0.006(2) 0.006(2) C3 0.049(3) 0.046(3) 0.030(3) 0.003(2) 0.007(2) 0.000(3) C4 0.044(3) 0.045(3) 0.033(3) -0.007(2) 0.012(2) -0.005(3) C5 0.038(3) 0.040(3) 0.035(3) -0.002(2) 0.007(2) -0.003(2) C6 0.042(3) 0.028(3) 0.030(3) -0.002(2) 0.004(2) -0.006(2) C7 0.027(2) 0.037(3) 0.029(3) -0.001(2) 0.0073(18) -0.006(2) C8 0.049(3) 0.026(3) 0.044(3) 0.000(3) 0.014(2) -0.009(2) C9 0.053(3) 0.038(4) 0.034(3) 0.006(3) 0.011(2) 0.003(2) C10 0.054(3) 0.042(3) 0.040(3) 0.001(3) 0.009(2) -0.004(3) C11 0.070(3) 0.055(4) 0.033(3) 0.005(3) 0.012(3) 0.003(3) C12 0.082(4) 0.054(4) 0.046(4) 0.020(3) 0.007(3) 0.004(3) C13 0.136(6) 0.033(4) 0.052(4) 0.013(3) 0.019(4) 0.007(4) C14 0.110(5) 0.036(4) 0.039(3) 0.009(3) 0.017(3) 0.001(3) C15 0.065(4) 0.096(6) 0.062(4) 0.015(4) 0.002(3) 0.044(4) C16 0.047(3) 0.107(6) 0.053(4) -0.009(4) 0.001(3) 0.035(4) C17 0.058(4) 0.160(9) 0.079(5) -0.039(5) -0.001(4) 0.046(5) C18 0.043(4) 0.182(10) 0.082(6) -0.066(6) -0.013(4) 0.028(5) C19 0.045(4) 0.155(8) 0.085(5) -0.056(6) 0.011(4) 0.000(4) C20 0.030(3) 0.106(6) 0.064(4) -0.042(4) 0.015(3) -0.001(3) C21 0.056(3) 0.068(4) 0.052(4) -0.024(3) 0.032(3) -0.019(3) C22 0.072(5) 0.075(5) 0.120(6) -0.057(5) 0.061(4) -0.044(4) C23 0.091(5) 0.050(5) 0.112(6) -0.032(4) 0.080(5) -0.038(4) C24 0.127(6) 0.085(6) 0.140(7) -0.066(6) 0.104(5) -0.063(5) C25 0.202(11) 0.068(6) 0.182(10) -0.060(7) 0.159(9) -0.085(7) C26 0.227(12) 0.071(6) 0.161(10) -0.057(7) 0.157(9) -0.059(7) C27 0.172(8) 0.062(5) 0.120(7) -0.024(5) 0.102(6) -0.051(5) C28 0.133(6) 0.068(5) 0.098(6) -0.035(5) 0.071(5) -0.048(5) C29 0.075(4) 0.060(4) 0.059(4) 0.023(3) 0.027(3) 0.018(3) C30 0.065(4) 0.046(4) 0.075(4) 0.011(4) 0.028(3) 0.017(3) C31 0.101(5) 0.050(5) 0.113(6) 0.015(4) 0.061(4) 0.010(4) C32 0.122(6) 0.044(4) 0.129(7) -0.014(5) 0.066(5) -0.010(4) C33 0.120(6) 0.054(5) 0.095(5) -0.024(4) 0.049(4) -0.011(4) C34 0.116(5) 0.055(5) 0.061(4) -0.002(4) 0.037(4) -0.001(4) C35 0.092(5) 0.106(6) 0.057(4) -0.012(4) 0.017(3) 0.007(4) C36 0.082(5) 0.122(7) 0.051(4) -0.015(4) 0.018(4) 0.028(5) N1 0.064(3) 0.067(4) 0.038(3) 0.010(2) 0.016(2) 0.029(3) N2 0.042(2) 0.041(3) 0.028(2) -0.0024(19) 0.0024(17) 0.003(2) N3 0.042(2) 0.028(2) 0.028(2) -0.0021(19) 0.0008(16) -0.0009(17) N4 0.046(2) 0.030(2) 0.027(2) -0.0001(18) 0.0067(16) -0.0036(19) N5 0.034(2) 0.092(4) 0.057(3) -0.012(3) 0.011(2) 0.017(3) N6 0.045(3) 0.083(4) 0.067(4) -0.027(3) 0.025(3) -0.020(3) N7 0.071(3) 0.065(4) 0.070(3) -0.027(3) 0.039(3) -0.031(3) N8 0.067(3) 0.049(3) 0.051(3) 0.001(3) 0.025(2) 0.009(2) N9 0.077(4) 0.078(4) 0.119(5) -0.024(4) 0.038(4) -0.010(3) S1 0.0452(7) 0.0323(8) 0.0341(7) -0.0012(6) 0.0052(5) -0.0024(6) S2 0.0776(10) 0.0707(12) 0.0408(8) -0.0157(8) 0.0244(7) -0.0376(8) O1 0.089(3) 0.029(2) 0.034(2) -0.0023(17) 0.0039(17) 0.0015(18) O2 0.069(3) 0.087(4) 0.142(4) -0.053(3) 0.047(3) -0.041(3) O3 0.070(2) 0.061(3) 0.058(2) -0.018(2) 0.0235(19) -0.004(2) O4 0.078(3) 0.138(5) 0.045(3) -0.005(3) -0.020(2) 0.018(3) O5 0.053(2) 0.076(3) 0.0332(19) -0.0127(19) 0.0095(15) -0.0099(19) O6 0.110(4) 0.190(6) 0.100(4) -0.068(4) 0.045(3) -0.107(4) O7 0.102(3) 0.063(3) 0.089(3) -0.022(3) 0.055(3) -0.030(2) O8 0.078(3) 0.083(3) 0.093(3) -0.011(3) 0.051(2) 0.002(2) O9 0.069(2) 0.059(3) 0.058(2) -0.004(2) 0.0286(19) -0.008(2) O10 0.130(4) 0.117(4) 0.089(3) 0.058(3) 0.052(3) 0.034(3) Cd1 0.0379(2) 0.0478(3) 0.0347(2) 0.00091(18) 0.00882(15) 0.00194(17) Cl1 0.0506(8) 0.0945(13) 0.0470(9) -0.0263(9) 0.0139(6) -0.0285(8) Cl2 0.0786(10) 0.0605(11) 0.0620(10) 0.0044(9) 0.0403(8) 0.0023(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 C1 N1 1.470(6) . ? C1 C2 1.513(7) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 N2 1.349(6) . ? C2 C3 1.378(6) . ? C3 C4 1.380(6) . ? C3 H3 0.9300 . ? C4 C5 1.370(6) . ? C4 H4 0.9300 . ? C5 C6 1.372(6) . ? C5 H5 0.9300 . ? C6 N2 1.338(6) . ? C6 N3 1.417(5) . ? C7 N3 1.325(5) . ? C7 N4 1.392(5) . ? C7 S1 1.681(5) . ? C8 O1 1.231(5) . ? C8 N4 1.385(6) . ? C8 C9 1.485(7) . ? C9 C10 1.378(6) . ? C9 C14 1.395(7) . ? C10 C11 1.388(7) . ? C10 H10 0.9300 . ? C11 C12 1.370(8) . ? C11 H11 0.9300 . ? C12 C13 1.387(8) . ? C12 H12 0.9300 . ? C13 C14 1.383(7) . ? C13 H13 0.9300 . ? C14 H14 0.9300 . ? C15 N1 1.482(7) . ? C15 C16 1.494(9) . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 N5 1.334(7) . ? C16 C17 1.399(9) . ? C17 C18 1.388(12) . ? C17 H17 0.9300 . ? C18 C19 1.355(11) . ? C18 H18 0.9300 . ? C19 C20 1.400(8) . ? C19 H19 0.9300 . ? C20 N5 1.351(8) . ? C20 N6 1.396(8) . ? C21 N6 1.320(7) . ? C21 N7 1.403(7) . ? C21 S2 1.663(5) . ? C22 O2 1.242(8) . ? C22 N7 1.385(7) . ? C22 C23 1.511(10) . ? C23 C28 1.359(10) . ? C23 C24 1.416(8) . ? C24 C25 1.395(12) . ? C24 H24 0.9300 . ? C25 C26 1.352(14) . ? C25 H25 0.9300 . ? C26 C27 1.365(10) . ? C26 H26 0.9300 . ? C27 C28 1.394(10) . ? C27 H27 0.9300 . ? C28 H28 0.9300 . ? C29 N1 1.472(7) . ? C29 C30 1.496(8) . ? C29 H29A 0.9700 . ? C29 H29B 0.9700 . ? C30 N8 1.353(7) . ? C30 C31 1.375(8) . ? C31 C32 1.364(9) . ? C31 H31 0.9300 . ? C32 C33 1.380(9) . ? C32 H32 0.9300 . ? C33 C34 1.370(9) . ? C33 H33 0.9300 . ? C34 N8 1.344(7) . ? C34 H34 0.9300 . ? C35 C36 1.480(10) . ? C35 H35A 0.9600 . ? C35 H35B 0.9600 . ? C35 H35C 0.9600 . ? C36 N9 1.100(8) . ? N1 Cd1 2.386(4) . ? N2 Cd1 2.365(4) . ? N3 H3A 0.8600 . ? N4 H4A 0.8600 . ? N5 Cd1 2.409(4) . ? N6 H6 0.8600 . ? N7 H7 0.8600 . ? N8 Cd1 2.378(5) . ? S1 Cd1 2.7130(12) . ? S2 Cd1 2.5746(14) . ? O3 Cl1 1.431(4) . ? O4 Cl1 1.444(4) . ? O5 Cl1 1.450(3) . ? O6 Cl1 1.410(4) . ? O7 Cl2 1.429(4) . ? O8 Cl2 1.429(4) . ? O9 Cl2 1.448(4) . ? O10 Cl2 1.435(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 C2 113.4(4) . . ? N1 C1 H1A 108.9 . . ? C2 C1 H1A 108.9 . . ? N1 C1 H1B 108.9 . . ? C2 C1 H1B 108.9 . . ? H1A C1 H1B 107.7 . . ? N2 C2 C3 122.5(4) . . ? N2 C2 C1 117.0(4) . . ? C3 C2 C1 120.4(4) . . ? C2 C3 C4 119.2(4) . . ? C2 C3 H3 120.4 . . ? C4 C3 H3 120.4 . . ? C5 C4 C3 118.8(4) . . ? C5 C4 H4 120.6 . . ? C3 C4 H4 120.6 . . ? C4 C5 C6 118.9(4) . . ? C4 C5 H5 120.5 . . ? C6 C5 H5 120.5 . . ? N2 C6 C5 123.6(4) . . ? N2 C6 N3 118.6(4) . . ? C5 C6 N3 117.6(4) . . ? N3 C7 N4 115.1(4) . . ? N3 C7 S1 126.1(4) . . ? N4 C7 S1 118.7(3) . . ? O1 C8 N4 121.5(4) . . ? O1 C8 C9 121.3(5) . . ? N4 C8 C9 117.2(4) . . ? C10 C9 C14 119.5(5) . . ? C10 C9 C8 124.4(5) . . ? C14 C9 C8 116.1(4) . . ? C9 C10 C11 120.0(5) . . ? C9 C10 H10 120.0 . . ? C11 C10 H10 120.0 . . ? C12 C11 C10 120.5(5) . . ? C12 C11 H11 119.8 . . ? C10 C11 H11 119.8 . . ? C11 C12 C13 120.2(5) . . ? C11 C12 H12 119.9 . . ? C13 C12 H12 119.9 . . ? C14 C13 C12 119.6(6) . . ? C14 C13 H13 120.2 . . ? C12 C13 H13 120.2 . . ? C13 C14 C9 120.3(5) . . ? C13 C14 H14 119.8 . . ? C9 C14 H14 119.8 . . ? N1 C15 C16 113.0(5) . . ? N1 C15 H15A 109.0 . . ? C16 C15 H15A 109.0 . . ? N1 C15 H15B 109.0 . . ? C16 C15 H15B 109.0 . . ? H15A C15 H15B 107.8 . . ? N5 C16 C17 122.8(7) . . ? N5 C16 C15 118.0(5) . . ? C17 C16 C15 119.1(7) . . ? C18 C17 C16 117.2(8) . . ? C18 C17 H17 121.4 . . ? C16 C17 H17 121.4 . . ? C19 C18 C17 120.5(7) . . ? C19 C18 H18 119.8 . . ? C17 C18 H18 119.8 . . ? C18 C19 C20 119.5(8) . . ? C18 C19 H19 120.2 . . ? C20 C19 H19 120.2 . . ? N5 C20 N6 122.8(5) . . ? N5 C20 C19 120.8(7) . . ? N6 C20 C19 116.4(7) . . ? N6 C21 N7 114.5(5) . . ? N6 C21 S2 130.2(5) . . ? N7 C21 S2 115.3(4) . . ? O2 C22 N7 118.3(8) . . ? O2 C22 C23 124.0(6) . . ? N7 C22 C23 117.6(7) . . ? C28 C23 C24 122.5(8) . . ? C28 C23 C22 123.7(6) . . ? C24 C23 C22 113.8(8) . . ? C25 C24 C23 117.4(9) . . ? C25 C24 H24 121.3 . . ? C23 C24 H24 121.3 . . ? C26 C25 C24 120.1(8) . . ? C26 C25 H25 120.0 . . ? C24 C25 H25 119.9 . . ? C25 C26 C27 121.5(11) . . ? C25 C26 H26 119.3 . . ? C27 C26 H26 119.3 . . ? C26 C27 C28 121.0(10) . . ? C26 C27 H27 119.5 . . ? C28 C27 H27 119.5 . . ? C23 C28 C27 117.5(7) . . ? C23 C28 H28 121.3 . . ? C27 C28 H28 121.3 . . ? N1 C29 C30 112.9(5) . . ? N1 C29 H29A 109.0 . . ? C30 C29 H29A 109.0 . . ? N1 C29 H29B 109.0 . . ? C30 C29 H29B 109.0 . . ? H29A C29 H29B 107.8 . . ? N8 C30 C31 121.1(6) . . ? N8 C30 C29 116.2(5) . . ? C31 C30 C29 122.7(6) . . ? C32 C31 C30 120.6(6) . . ? C32 C31 H31 119.7 . . ? C30 C31 H31 119.7 . . ? C31 C32 C33 118.7(7) . . ? C31 C32 H32 120.6 . . ? C33 C32 H32 120.6 . . ? C34 C33 C32 118.5(6) . . ? C34 C33 H33 120.8 . . ? C32 C33 H33 120.8 . . ? N8 C34 C33 123.3(6) . . ? N8 C34 H34 118.4 . . ? C33 C34 H34 118.4 . . ? C36 C35 H35A 109.5 . . ? C36 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C36 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? N9 C36 C35 170.9(9) . . ? C1 N1 C29 110.9(5) . . ? C1 N1 C15 110.8(4) . . ? C29 N1 C15 112.5(5) . . ? C1 N1 Cd1 110.2(3) . . ? C29 N1 Cd1 106.3(3) . . ? C15 N1 Cd1 106.0(3) . . ? C6 N2 C2 117.0(4) . . ? C6 N2 Cd1 125.8(3) . . ? C2 N2 Cd1 117.1(3) . . ? C7 N3 C6 130.7(4) . . ? C7 N3 H3A 114.7 . . ? C6 N3 H3A 114.7 . . ? C8 N4 C7 126.8(4) . . ? C8 N4 H4A 116.6 . . ? C7 N4 H4A 116.6 . . ? C16 N5 C20 119.1(5) . . ? C16 N5 Cd1 111.2(4) . . ? C20 N5 Cd1 126.5(4) . . ? C21 N6 C20 134.0(5) . . ? C21 N6 H6 113.0 . . ? C20 N6 H6 113.0 . . ? C22 N7 C21 129.8(6) . . ? C22 N7 H7 115.1 . . ? C21 N7 H7 115.1 . . ? C34 N8 C30 117.8(5) . . ? C34 N8 Cd1 126.6(4) . . ? C30 N8 Cd1 115.1(4) . . ? C7 S1 Cd1 93.75(14) . . ? C21 S2 Cd1 106.7(2) . . ? N2 Cd1 N8 117.83(15) . . ? N2 Cd1 N1 71.50(13) . . ? N8 Cd1 N1 70.20(16) . . ? N2 Cd1 N5 114.63(14) . . ? N8 Cd1 N5 99.55(16) . . ? N1 Cd1 N5 74.29(17) . . ? N2 Cd1 S2 138.58(11) . . ? N8 Cd1 S2 94.97(12) . . ? N1 Cd1 S2 148.19(10) . . ? N5 Cd1 S2 81.03(13) . . ? N2 Cd1 S1 78.59(9) . . ? N8 Cd1 S1 83.04(11) . . ? N1 Cd1 S1 122.53(12) . . ? N5 Cd1 S1 162.33(13) . . ? S2 Cd1 S1 81.33(4) . . ? O6 Cl1 O3 109.9(3) . . ? O6 Cl1 O4 109.2(3) . . ? O3 Cl1 O4 110.3(3) . . ? O6 Cl1 O5 109.5(2) . . ? O3 Cl1 O5 108.7(2) . . ? O4 Cl1 O5 109.2(3) . . ? O8 Cl2 O7 108.5(3) . . ? O8 Cl2 O10 110.2(3) . . ? O7 Cl2 O10 110.1(3) . . ? O8 Cl2 O9 109.2(2) . . ? O7 Cl2 O9 109.3(2) . . ? O10 Cl2 O9 109.6(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 C1 C2 N2 26.8(7) . . . . ? N1 C1 C2 C3 -157.2(5) . . . . ? N2 C2 C3 C4 -1.0(8) . . . . ? C1 C2 C3 C4 -176.7(5) . . . . ? C2 C3 C4 C5 1.0(7) . . . . ? C3 C4 C5 C6 0.1(7) . . . . ? C4 C5 C6 N2 -1.3(7) . . . . ? C4 C5 C6 N3 173.3(4) . . . . ? O1 C8 C9 C10 163.5(5) . . . . ? N4 C8 C9 C10 -14.7(7) . . . . ? O1 C8 C9 C14 -13.8(7) . . . . ? N4 C8 C9 C14 168.0(4) . . . . ? C14 C9 C10 C11 1.1(7) . . . . ? C8 C9 C10 C11 -176.2(4) . . . . ? C9 C10 C11 C12 0.7(8) . . . . ? C10 C11 C12 C13 -1.4(8) . . . . ? C11 C12 C13 C14 0.4(9) . . . . ? C12 C13 C14 C9 1.4(9) . . . . ? C10 C9 C14 C13 -2.1(8) . . . . ? C8 C9 C14 C13 175.4(5) . . . . ? N1 C15 C16 N5 47.9(7) . . . . ? N1 C15 C16 C17 -134.8(5) . . . . ? N5 C16 C17 C18 -0.1(9) . . . . ? C15 C16 C17 C18 -177.2(6) . . . . ? C16 C17 C18 C19 1.8(10) . . . . ? C17 C18 C19 C20 -1.2(11) . . . . ? C18 C19 C20 N5 -1.2(9) . . . . ? C18 C19 C20 N6 179.4(6) . . . . ? O2 C22 C23 C28 -168.8(6) . . . . ? N7 C22 C23 C28 13.5(9) . . . . ? O2 C22 C23 C24 9.4(9) . . . . ? N7 C22 C23 C24 -168.3(5) . . . . ? C28 C23 C24 C25 -1.8(10) . . . . ? C22 C23 C24 C25 -180.0(6) . . . . ? C23 C24 C25 C26 0.0(12) . . . . ? C24 C25 C26 C27 0.6(15) . . . . ? C25 C26 C27 C28 0.5(13) . . . . ? C24 C23 C28 C27 2.8(10) . . . . ? C22 C23 C28 C27 -179.2(6) . . . . ? C26 C27 C28 C23 -2.2(11) . . . . ? N1 C29 C30 N8 27.5(7) . . . . ? N1 C29 C30 C31 -152.6(5) . . . . ? N8 C30 C31 C32 -0.1(10) . . . . ? C29 C30 C31 C32 180.0(6) . . . . ? C30 C31 C32 C33 0.0(11) . . . . ? C31 C32 C33 C34 0.2(11) . . . . ? C32 C33 C34 N8 -0.3(10) . . . . ? C2 C1 N1 C29 80.8(6) . . . . ? C2 C1 N1 C15 -153.6(5) . . . . ? C2 C1 N1 Cd1 -36.7(6) . . . . ? C30 C29 N1 C1 -166.0(4) . . . . ? C30 C29 N1 C15 69.3(6) . . . . ? C30 C29 N1 Cd1 -46.3(5) . . . . ? C16 C15 N1 C1 76.9(6) . . . . ? C16 C15 N1 C29 -158.4(5) . . . . ? C16 C15 N1 Cd1 -42.6(6) . . . . ? C5 C6 N2 C2 1.3(7) . . . . ? N3 C6 N2 C2 -173.2(4) . . . . ? C5 C6 N2 Cd1 178.9(3) . . . . ? N3 C6 N2 Cd1 4.4(6) . . . . ? C3 C2 N2 C6 -0.1(7) . . . . ? C1 C2 N2 C6 175.7(4) . . . . ? C3 C2 N2 Cd1 -178.0(4) . . . . ? C1 C2 N2 Cd1 -2.1(6) . . . . ? N4 C7 N3 C6 -174.4(4) . . . . ? S1 C7 N3 C6 2.4(6) . . . . ? N2 C6 N3 C7 -46.4(6) . . . . ? C5 C6 N3 C7 138.8(4) . . . . ? O1 C8 N4 C7 -9.5(7) . . . . ? C9 C8 N4 C7 168.7(4) . . . . ? N3 C7 N4 C8 6.4(6) . . . . ? S1 C7 N4 C8 -170.7(3) . . . . ? C17 C16 N5 C20 -2.3(8) . . . . ? C15 C16 N5 C20 174.9(5) . . . . ? C17 C16 N5 Cd1 158.9(5) . . . . ? C15 C16 N5 Cd1 -23.9(6) . . . . ? N6 C20 N5 C16 -177.7(5) . . . . ? C19 C20 N5 C16 2.9(8) . . . . ? N6 C20 N5 Cd1 24.2(7) . . . . ? C19 C20 N5 Cd1 -155.1(4) . . . . ? N7 C21 N6 C20 -178.9(5) . . . . ? S2 C21 N6 C20 1.5(9) . . . . ? N5 C20 N6 C21 7.9(9) . . . . ? C19 C20 N6 C21 -172.7(6) . . . . ? O2 C22 N7 C21 1.7(9) . . . . ? C23 C22 N7 C21 179.5(5) . . . . ? N6 C21 N7 C22 -9.0(8) . . . . ? S2 C21 N7 C22 170.6(5) . . . . ? C33 C34 N8 C30 0.2(9) . . . . ? C33 C34 N8 Cd1 171.9(5) . . . . ? C31 C30 N8 C34 0.0(8) . . . . ? C29 C30 N8 C34 179.9(5) . . . . ? C31 C30 N8 Cd1 -172.6(5) . . . . ? C29 C30 N8 Cd1 7.3(6) . . . . ? N3 C7 S1 Cd1 54.0(4) . . . . ? N4 C7 S1 Cd1 -129.3(3) . . . . ? N6 C21 S2 Cd1 -32.5(6) . . . . ? N7 C21 S2 Cd1 147.9(3) . . . . ? C6 N2 Cd1 N8 114.6(4) . . . . ? C2 N2 Cd1 N8 -67.8(4) . . . . ? C6 N2 Cd1 N1 169.1(4) . . . . ? C2 N2 Cd1 N1 -13.3(3) . . . . ? C6 N2 Cd1 N5 -128.8(4) . . . . ? C2 N2 Cd1 N5 48.9(4) . . . . ? C6 N2 Cd1 S2 -23.7(4) . . . . ? C2 N2 Cd1 S2 153.9(3) . . . . ? C6 N2 Cd1 S1 38.9(3) . . . . ? C2 N2 Cd1 S1 -143.5(3) . . . . ? C34 N8 Cd1 N2 -141.0(5) . . . . ? C30 N8 Cd1 N2 30.8(4) . . . . ? C34 N8 Cd1 N1 163.8(5) . . . . ? C30 N8 Cd1 N1 -24.3(4) . . . . ? C34 N8 Cd1 N5 94.4(5) . . . . ? C30 N8 Cd1 N5 -93.7(4) . . . . ? C34 N8 Cd1 S2 12.7(5) . . . . ? C30 N8 Cd1 S2 -175.4(4) . . . . ? C34 N8 Cd1 S1 -67.9(5) . . . . ? C30 N8 Cd1 S1 104.0(4) . . . . ? C1 N1 Cd1 N2 26.0(3) . . . . ? C29 N1 Cd1 N2 -94.2(3) . . . . ? C15 N1 Cd1 N2 145.9(4) . . . . ? C1 N1 Cd1 N8 156.1(4) . . . . ? C29 N1 Cd1 N8 35.8(3) . . . . ? C15 N1 Cd1 N8 -84.1(4) . . . . ? C1 N1 Cd1 N5 -97.4(4) . . . . ? C29 N1 Cd1 N5 142.4(3) . . . . ? C15 N1 Cd1 N5 22.5(4) . . . . ? C1 N1 Cd1 S2 -137.9(3) . . . . ? C29 N1 Cd1 S2 101.9(3) . . . . ? C15 N1 Cd1 S2 -18.0(5) . . . . ? C1 N1 Cd1 S1 88.6(4) . . . . ? C29 N1 Cd1 S1 -31.7(3) . . . . ? C15 N1 Cd1 S1 -151.6(3) . . . . ? C16 N5 Cd1 N2 -60.8(4) . . . . ? C20 N5 Cd1 N2 98.7(4) . . . . ? C16 N5 Cd1 N8 65.9(4) . . . . ? C20 N5 Cd1 N8 -134.6(4) . . . . ? C16 N5 Cd1 N1 -0.3(4) . . . . ? C20 N5 Cd1 N1 159.2(5) . . . . ? C16 N5 Cd1 S2 159.5(4) . . . . ? C20 N5 Cd1 S2 -41.0(4) . . . . ? C16 N5 Cd1 S1 163.0(3) . . . . ? C20 N5 Cd1 S1 -37.5(7) . . . . ? C21 S2 Cd1 N2 -80.3(3) . . . . ? C21 S2 Cd1 N8 136.0(2) . . . . ? C21 S2 Cd1 N1 76.3(3) . . . . ? C21 S2 Cd1 N5 37.1(3) . . . . ? C21 S2 Cd1 S1 -141.9(2) . . . . ? C7 S1 Cd1 N2 -55.18(18) . . . . ? C7 S1 Cd1 N8 -175.47(19) . . . . ? C7 S1 Cd1 N1 -114.3(2) . . . . ? C7 S1 Cd1 N5 84.9(4) . . . . ? C7 S1 Cd1 S2 88.40(16) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.823 _refine_diff_density_min -0.735 _refine_diff_density_rms 0.123 data_aja0820t _database_code_depnum_ccdc_archive 'CCDC 844371' #TrackingRef '- aja0820t_2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C34 H30 Co N8 O2 S2, 2(cl O4)' _chemical_formula_sum 'C34 H30 Cl2 Co N8 O10 S2' _chemical_formula_weight 904.61 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' Co Co 0.3494 0.9721 '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 Monoclinic _symmetry_space_group_name_H-M P21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 14.0690(6) _cell_length_b 11.8060(4) _cell_length_c 22.1260(9) _cell_angle_alpha 90.00 _cell_angle_beta 90.400(10) _cell_angle_gamma 90.00 _cell_volume 3675.0(2) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 4307 _cell_measurement_theta_min 2.90 _cell_measurement_theta_max 27.54 _exptl_crystal_description plate _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 1.635 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1852 _exptl_absorpt_coefficient_mu 0.797 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.7411 _exptl_absorpt_correction_T_max 0.9246 _exptl_absorpt_process_details Denzo/Scalepack _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_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method 'CCD scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 23933 _diffrn_reflns_av_R_equivalents 0.1589 _diffrn_reflns_av_sigmaI/netI 0.1559 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 2.90 _diffrn_reflns_theta_max 27.54 _reflns_number_total 7889 _reflns_number_gt 4307 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'cOLLECT,Nonius BV, 1997-2001' _computing_cell_refinement DENZO/SCALEPACK _computing_data_reduction DENZO/SCALEPACK _computing_structure_solution SHELXs-97 _computing_structure_refinement SHELXL-97 _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^)+(0.0750P)^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 7889 _refine_ls_number_parameters 514 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1564 _refine_ls_R_factor_gt 0.0782 _refine_ls_wR_factor_ref 0.1912 _refine_ls_wR_factor_gt 0.1604 _refine_ls_goodness_of_fit_ref 1.019 _refine_ls_restrained_S_all 1.019 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.1778(4) 0.2335(4) -0.0292(2) 0.0325(13) Uani 1 1 d . . . H1A H 0.1205 0.2148 -0.0534 0.039 Uiso 1 1 calc R . . H1B H 0.2196 0.1660 -0.0284 0.039 Uiso 1 1 calc R . . C2 C 0.2295(4) 0.3316(4) -0.0579(2) 0.0286(12) Uani 1 1 d . . . C3 C 0.2272(4) 0.3487(5) -0.1193(2) 0.0365(13) Uani 1 1 d . . . H3 H 0.1931 0.2984 -0.1450 0.044 Uiso 1 1 calc R . . C4 C 0.2756(4) 0.4407(5) -0.1431(2) 0.0386(14) Uani 1 1 d . . . H4 H 0.2764 0.4532 -0.1855 0.046 Uiso 1 1 calc R . . C5 C 0.3219(4) 0.5128(4) -0.1051(2) 0.0339(13) Uani 1 1 d . . . H5 H 0.3526 0.5786 -0.1202 0.041 Uiso 1 1 calc R . . C6 C 0.3232(3) 0.4879(4) -0.0437(2) 0.0293(12) Uani 1 1 d . . . C7 C 0.4095(4) 0.5552(4) 0.0474(2) 0.0292(12) Uani 1 1 d . . . C8 C 0.4851(4) 0.7451(4) 0.0393(2) 0.0334(13) Uani 1 1 d . . . C9 C 0.5461(4) 0.8231(4) 0.0742(2) 0.0314(13) Uani 1 1 d . . . C10 C 0.5806(4) 0.9183(5) 0.0429(3) 0.0409(14) Uani 1 1 d . . . H10 H 0.5640 0.9299 0.0017 0.049 Uiso 1 1 calc R . . C11 C 0.6386(4) 0.9946(5) 0.0724(3) 0.0464(16) Uani 1 1 d . . . H11 H 0.6622 1.0588 0.0515 0.056 Uiso 1 1 calc R . . C12 C 0.6624(4) 0.9782(5) 0.1320(3) 0.0465(16) Uani 1 1 d . . . H12 H 0.7015 1.0319 0.1522 0.056 Uiso 1 1 calc R . . C13 C 0.6307(5) 0.8862(5) 0.1624(3) 0.0543(17) Uani 1 1 d . . . H13 H 0.6488 0.8753 0.2035 0.065 Uiso 1 1 calc R . . C14 C 0.5718(4) 0.8075(5) 0.1340(3) 0.0486(16) Uani 1 1 d . . . H14 H 0.5493 0.7435 0.1556 0.058 Uiso 1 1 calc R . . C15 C 0.0679(4) 0.3402(4) 0.0339(2) 0.0325(13) Uani 1 1 d . . . H15A H 0.0083 0.2956 0.0322 0.039 Uiso 1 1 calc R . . H15B H 0.0694 0.3902 -0.0020 0.039 Uiso 1 1 calc R . . C16 C 0.0691(4) 0.4105(4) 0.0898(2) 0.0270(12) Uani 1 1 d . . . C17 C -0.0127(4) 0.4601(4) 0.1125(2) 0.0365(13) Uani 1 1 d . . . H17 H -0.0727 0.4455 0.0941 0.044 Uiso 1 1 calc R . . C18 C -0.0060(4) 0.5312(5) 0.1622(3) 0.0466(16) Uani 1 1 d . . . H18 H -0.0610 0.5672 0.1778 0.056 Uiso 1 1 calc R . . C19 C 0.0822(4) 0.5487(5) 0.1887(2) 0.0402(14) Uani 1 1 d . . . H19 H 0.0892 0.5963 0.2231 0.048 Uiso 1 1 calc R . . C20 C 0.1593(4) 0.4953(4) 0.1640(2) 0.0313(12) Uani 1 1 d . . . C21 C 0.2949(4) 0.4275(5) 0.2216(2) 0.0389(14) Uani 1 1 d . . . C22 C 0.4274(4) 0.5619(6) 0.2448(2) 0.0402(15) Uani 1 1 d . . . C23 C 0.5013(5) 0.5830(6) 0.2913(3) 0.0550(18) Uani 1 1 d . . . C24 C 0.5467(5) 0.6856(8) 0.2880(3) 0.079(2) Uani 1 1 d . . . H24 H 0.5316 0.7358 0.2557 0.095 Uiso 1 1 calc R . . C25 C 0.6134(6) 0.7175(10) 0.3303(4) 0.100(3) Uani 1 1 d . . . H25 H 0.6464 0.7875 0.3273 0.120 Uiso 1 1 calc R . . C26 C 0.6307(6) 0.6427(10) 0.3780(5) 0.108(4) Uani 1 1 d . . . H26 H 0.6748 0.6644 0.4085 0.130 Uiso 1 1 calc R . . C27 C 0.5866(6) 0.5385(9) 0.3827(4) 0.102(4) Uani 1 1 d . . . H27 H 0.6005 0.4890 0.4155 0.122 Uiso 1 1 calc R . . C28 C 0.5210(5) 0.5080(7) 0.3378(3) 0.075(2) Uani 1 1 d . . . H28 H 0.4902 0.4365 0.3392 0.090 Uiso 1 1 calc R . . C29 C 0.1359(4) 0.1616(4) 0.0706(2) 0.0344(13) Uani 1 1 d . . . H29A H 0.1011 0.1034 0.0470 0.041 Uiso 1 1 calc R . . H29B H 0.0970 0.1817 0.1061 0.041 Uiso 1 1 calc R . . C30 C 0.2294(4) 0.1141(5) 0.0915(2) 0.0326(13) Uani 1 1 d . . . C31 C 0.2396(4) 0.0042(5) 0.1093(2) 0.0389(14) Uani 1 1 d . . . H31 H 0.1880 -0.0473 0.1059 0.047 Uiso 1 1 calc R . . C32 C 0.3259(5) -0.0311(5) 0.1323(2) 0.0449(16) Uani 1 1 d . . . H32 H 0.3345 -0.1074 0.1448 0.054 Uiso 1 1 calc R . . C33 C 0.3993(4) 0.0448(5) 0.1371(2) 0.0378(14) Uani 1 1 d . . . H33 H 0.4591 0.0226 0.1533 0.045 Uiso 1 1 calc R . . C34 C 0.3838(4) 0.1552(5) 0.1176(2) 0.0328(13) Uani 1 1 d . . . H34 H 0.4345 0.2082 0.1206 0.039 Uiso 1 1 calc R . . N1 N 0.1501(3) 0.2629(3) 0.03277(18) 0.0292(10) Uani 1 1 d . . . N2 N 0.2769(3) 0.4004(3) -0.01980(17) 0.0257(9) Uani 1 1 d . . . N3 N 0.3709(3) 0.5664(3) -0.00672(17) 0.0289(10) Uani 1 1 d . . . H3A H 0.3759 0.6347 -0.0223 0.035 Uiso 1 1 calc R . . N4 N 0.4582(3) 0.6464(3) 0.06931(18) 0.0301(10) Uani 1 1 d . . . H4A H 0.4749 0.6425 0.1077 0.036 Uiso 1 1 calc R . . N5 N 0.1552(3) 0.4281(3) 0.11471(17) 0.0250(9) Uani 1 1 d . . . N6 N 0.2505(3) 0.5116(4) 0.18991(18) 0.0328(10) Uani 1 1 d . . . H6 H 0.2792 0.5773 0.1855 0.039 Uiso 1 1 calc R . . N7 N 0.3812(3) 0.4596(4) 0.2475(2) 0.0450(13) Uani 1 1 d . . . H7 H 0.4103 0.4067 0.2686 0.054 Uiso 1 1 calc R . . N8 N 0.3001(3) 0.1901(3) 0.09478(17) 0.0280(10) Uani 1 1 d . . . O1 O 0.4596(3) 0.7627(3) -0.01228(16) 0.0409(10) Uani 1 1 d . . . O2 O 0.4083(3) 0.6332(3) 0.20607(17) 0.0475(11) Uani 1 1 d . . . O3 O 0.2327(3) 0.6982(4) 0.09695(18) 0.0621(13) Uani 1 1 d . . . O4 O 0.1516(3) 0.6183(3) 0.01458(19) 0.0525(11) Uani 1 1 d . . . O5 O 0.0961(3) 0.7869(4) 0.0584(2) 0.0751(15) Uani 1 1 d . . . O6 O 0.2393(3) 0.7847(4) 0.0040(2) 0.0710(14) Uani 1 1 d . . . O7 O 0.5921(4) 0.2538(4) 0.16253(18) 0.0712(14) Uani 1 1 d . . . O8 O 0.5262(3) 0.2680(4) 0.2604(2) 0.0818(17) Uani 1 1 d . . . O9 O 0.6623(4) 0.1632(4) 0.24398(18) 0.0659(14) Uani 1 1 d . . . O10 O 0.6675(4) 0.3607(4) 0.23700(18) 0.0696(14) Uani 1 1 d . . . S1 S 0.41379(9) 0.43792(11) 0.09146(6) 0.0317(3) Uani 1 1 d . . . S2 S 0.25303(12) 0.30036(14) 0.23113(7) 0.0497(4) Uani 1 1 d . . . Co1 Co 0.26836(5) 0.35368(6) 0.07093(3) 0.0262(2) Uani 1 1 d . . . Cl1 Cl 0.17906(10) 0.72290(12) 0.04346(6) 0.0411(4) Uani 1 1 d . . . Cl2 Cl 0.61245(11) 0.26225(12) 0.22602(6) 0.0433(4) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.032(3) 0.029(3) 0.036(3) -0.006(2) -0.009(2) -0.004(2) C2 0.027(3) 0.029(3) 0.029(3) -0.004(2) 0.000(2) 0.004(2) C3 0.034(3) 0.042(3) 0.033(3) -0.007(3) -0.008(3) -0.005(3) C4 0.048(4) 0.045(4) 0.023(3) 0.000(2) -0.005(3) -0.005(3) C5 0.042(3) 0.033(3) 0.027(3) 0.006(2) -0.004(3) -0.003(3) C6 0.022(3) 0.037(3) 0.028(3) -0.004(2) -0.001(2) 0.004(2) C7 0.026(3) 0.029(3) 0.033(3) -0.006(2) 0.003(2) -0.003(2) C8 0.032(3) 0.029(3) 0.039(3) 0.001(3) 0.004(3) -0.003(2) C9 0.024(3) 0.025(3) 0.045(3) -0.008(2) -0.004(2) -0.002(2) C10 0.038(3) 0.039(4) 0.046(3) -0.007(3) 0.008(3) -0.006(3) C11 0.033(3) 0.041(4) 0.066(4) -0.005(3) 0.016(3) -0.009(3) C12 0.034(3) 0.038(4) 0.067(4) -0.018(3) -0.004(3) -0.008(3) C13 0.061(4) 0.040(4) 0.061(4) -0.003(3) -0.026(3) -0.002(3) C14 0.058(4) 0.038(4) 0.049(4) 0.006(3) -0.016(3) -0.011(3) C15 0.022(3) 0.038(3) 0.037(3) -0.001(2) -0.005(2) -0.004(2) C16 0.027(3) 0.027(3) 0.027(3) -0.001(2) -0.003(2) -0.004(2) C17 0.026(3) 0.043(4) 0.040(3) 0.002(3) -0.003(3) 0.002(3) C18 0.041(4) 0.060(4) 0.039(3) -0.006(3) 0.003(3) 0.013(3) C19 0.041(4) 0.043(4) 0.037(3) -0.011(3) -0.004(3) 0.003(3) C20 0.030(3) 0.036(3) 0.027(3) 0.001(2) -0.003(2) -0.001(2) C21 0.043(4) 0.057(4) 0.016(3) -0.007(3) -0.003(2) 0.005(3) C22 0.034(3) 0.061(4) 0.026(3) -0.015(3) -0.008(3) 0.002(3) C23 0.039(4) 0.073(5) 0.053(4) -0.036(4) -0.010(3) 0.001(4) C24 0.061(5) 0.129(7) 0.048(4) -0.034(4) -0.006(4) -0.023(5) C25 0.056(5) 0.152(9) 0.092(7) -0.076(7) -0.015(5) -0.008(6) C26 0.050(5) 0.158(10) 0.115(8) -0.108(8) -0.041(5) 0.053(6) C27 0.090(7) 0.117(8) 0.098(6) -0.065(6) -0.062(5) 0.062(6) C28 0.066(5) 0.090(6) 0.068(5) -0.033(4) -0.030(4) 0.043(4) C29 0.037(3) 0.030(3) 0.037(3) -0.001(2) -0.006(3) -0.010(3) C30 0.039(3) 0.031(3) 0.028(3) -0.005(2) 0.004(3) -0.008(3) C31 0.049(4) 0.028(3) 0.040(3) -0.005(2) 0.005(3) -0.004(3) C32 0.066(5) 0.036(4) 0.033(3) 0.006(3) 0.010(3) 0.008(3) C33 0.039(3) 0.047(4) 0.028(3) 0.004(3) 0.001(3) 0.007(3) C34 0.036(3) 0.039(3) 0.024(3) 0.002(2) 0.003(2) -0.002(3) N1 0.027(2) 0.029(3) 0.031(2) -0.0037(19) -0.0022(19) -0.0048(19) N2 0.024(2) 0.029(2) 0.024(2) 0.0006(18) -0.0031(18) -0.0021(19) N3 0.033(3) 0.027(2) 0.027(2) 0.0063(18) -0.006(2) -0.0051(19) N4 0.036(3) 0.026(2) 0.028(2) 0.0011(19) -0.0087(19) -0.006(2) N5 0.023(2) 0.027(2) 0.025(2) 0.0005(18) -0.0023(18) -0.0017(18) N6 0.033(3) 0.033(3) 0.033(2) -0.006(2) -0.006(2) -0.005(2) N7 0.039(3) 0.058(3) 0.037(3) 0.001(2) -0.009(2) 0.003(3) N8 0.028(2) 0.033(3) 0.023(2) 0.0007(18) -0.0008(19) -0.001(2) O1 0.050(3) 0.039(2) 0.033(2) 0.0064(17) -0.0071(19) -0.0106(19) O2 0.050(3) 0.054(3) 0.038(2) -0.009(2) -0.002(2) -0.011(2) O3 0.070(3) 0.068(3) 0.048(3) 0.011(2) -0.027(2) -0.013(2) O4 0.042(3) 0.046(3) 0.069(3) -0.014(2) -0.013(2) -0.003(2) O5 0.039(3) 0.070(3) 0.116(4) -0.045(3) -0.020(3) 0.016(2) O6 0.079(4) 0.076(3) 0.058(3) 0.021(2) -0.006(3) -0.024(3) O7 0.102(4) 0.064(3) 0.047(3) 0.018(2) -0.045(3) -0.025(3) O8 0.063(3) 0.059(3) 0.124(5) 0.023(3) 0.038(3) 0.012(3) O9 0.083(4) 0.075(3) 0.040(2) 0.012(2) -0.002(2) 0.028(3) O10 0.091(4) 0.071(3) 0.047(3) -0.003(2) -0.007(3) -0.036(3) S1 0.0283(7) 0.0307(8) 0.0361(8) 0.0017(6) -0.0061(6) -0.0041(6) S2 0.0581(11) 0.0450(10) 0.0459(9) 0.0064(7) -0.0091(8) -0.0016(8) Co1 0.0244(4) 0.0284(4) 0.0258(4) -0.0030(3) -0.0034(3) -0.0035(3) Cl1 0.0368(8) 0.0401(9) 0.0463(9) 0.0011(7) -0.0106(7) -0.0039(7) Cl2 0.0458(9) 0.0450(9) 0.0389(8) 0.0092(7) -0.0099(7) -0.0028(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.470(6) . ? C1 C2 1.510(7) . ? C2 N2 1.344(6) . ? C2 C3 1.375(7) . ? C3 C4 1.388(7) . ? C4 C5 1.359(7) . ? C5 C6 1.391(7) . ? C6 N2 1.332(6) . ? C6 N3 1.403(6) . ? C7 N3 1.319(6) . ? C7 N4 1.364(6) . ? C7 S1 1.693(5) . ? C8 O1 1.212(6) . ? C8 N4 1.395(6) . ? C8 C9 1.472(7) . ? C9 C14 1.382(7) . ? C9 C10 1.409(7) . ? C10 C11 1.377(8) . ? C11 C12 1.373(8) . ? C12 C13 1.354(8) . ? C13 C14 1.392(8) . ? C15 N1 1.474(6) . ? C15 C16 1.489(7) . ? C16 N5 1.343(6) . ? C16 C17 1.388(7) . ? C17 C18 1.386(7) . ? C18 C19 1.385(8) . ? C19 C20 1.371(7) . ? C20 N5 1.349(6) . ? C20 N6 1.415(6) . ? C21 N6 1.364(7) . ? C21 N7 1.392(7) . ? C21 S2 1.627(6) . ? C22 O2 1.230(7) . ? C22 N7 1.374(7) . ? C22 C23 1.478(8) . ? C23 C24 1.372(9) . ? C23 C28 1.384(10) . ? C24 C25 1.375(10) . ? C25 C26 1.396(14) . ? C26 C27 1.382(13) . ? C27 C28 1.399(10) . ? C29 N1 1.474(6) . ? C29 C30 1.500(7) . ? C30 N8 1.340(6) . ? C30 C31 1.363(7) . ? C31 C32 1.378(8) . ? C32 C33 1.370(8) . ? C33 C34 1.389(7) . ? C34 N8 1.343(6) . ? N1 Co1 2.147(4) . ? N2 Co1 2.086(4) . ? N5 Co1 2.065(4) . ? N8 Co1 2.051(4) . ? O3 Cl1 1.429(4) . ? O4 Cl1 1.442(4) . ? O5 Cl1 1.432(4) . ? O6 Cl1 1.422(4) . ? O7 Cl2 1.435(4) . ? O8 Cl2 1.439(4) . ? O9 Cl2 1.419(4) . ? O10 Cl2 1.417(4) . ? S1 Co1 2.3170(14) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 C2 110.0(4) . . ? N2 C2 C3 122.6(5) . . ? N2 C2 C1 116.0(4) . . ? C3 C2 C1 121.3(4) . . ? C2 C3 C4 118.8(5) . . ? C5 C4 C3 119.3(5) . . ? C4 C5 C6 118.4(5) . . ? N2 C6 C5 123.3(5) . . ? N2 C6 N3 120.9(4) . . ? C5 C6 N3 115.7(5) . . ? N3 C7 N4 116.5(4) . . ? N3 C7 S1 128.1(4) . . ? N4 C7 S1 115.2(4) . . ? O1 C8 N4 120.7(5) . . ? O1 C8 C9 123.7(5) . . ? N4 C8 C9 115.6(5) . . ? C14 C9 C10 119.2(5) . . ? C14 C9 C8 124.5(5) . . ? C10 C9 C8 116.3(5) . . ? C11 C10 C9 119.6(6) . . ? C12 C11 C10 120.2(6) . . ? C13 C12 C11 120.8(6) . . ? C12 C13 C14 120.5(6) . . ? C9 C14 C13 119.7(6) . . ? N1 C15 C16 110.8(4) . . ? N5 C16 C17 122.3(4) . . ? N5 C16 C15 115.6(4) . . ? C17 C16 C15 122.0(5) . . ? C18 C17 C16 119.4(5) . . ? C19 C18 C17 118.8(5) . . ? C20 C19 C18 118.1(5) . . ? N5 C20 C19 124.3(5) . . ? N5 C20 N6 116.2(4) . . ? C19 C20 N6 119.5(5) . . ? N6 C21 N7 114.1(5) . . ? N6 C21 S2 125.0(4) . . ? N7 C21 S2 120.9(4) . . ? O2 C22 N7 122.1(5) . . ? O2 C22 C23 121.2(6) . . ? N7 C22 C23 116.7(6) . . ? C24 C23 C28 120.9(7) . . ? C24 C23 C22 115.9(7) . . ? C28 C23 C22 123.1(7) . . ? C23 C24 C25 121.5(9) . . ? C24 C25 C26 117.1(10) . . ? C27 C26 C25 123.1(8) . . ? C26 C27 C28 118.0(9) . . ? C23 C28 C27 119.5(9) . . ? N1 C29 C30 110.9(4) . . ? N8 C30 C31 123.0(5) . . ? N8 C30 C29 114.5(5) . . ? C31 C30 C29 122.4(5) . . ? C30 C31 C32 119.0(5) . . ? C33 C32 C31 119.5(5) . . ? C32 C33 C34 118.3(5) . . ? N8 C34 C33 122.6(5) . . ? C1 N1 C15 112.1(4) . . ? C1 N1 C29 112.0(4) . . ? C15 N1 C29 112.6(4) . . ? C1 N1 Co1 106.0(3) . . ? C15 N1 Co1 106.9(3) . . ? C29 N1 Co1 106.8(3) . . ? C6 N2 C2 117.5(4) . . ? C6 N2 Co1 128.2(3) . . ? C2 N2 Co1 114.3(3) . . ? C7 N3 C6 130.9(4) . . ? C7 N4 C8 129.0(4) . . ? C16 N5 C20 117.1(4) . . ? C16 N5 Co1 116.0(3) . . ? C20 N5 Co1 126.9(3) . . ? C21 N6 C20 121.3(4) . . ? C22 N7 C21 129.3(5) . . ? C30 N8 C34 117.6(5) . . ? C30 N8 Co1 117.2(4) . . ? C34 N8 Co1 125.0(4) . . ? C7 S1 Co1 102.14(18) . . ? N8 Co1 N5 116.53(16) . . ? N8 Co1 N2 118.88(16) . . ? N5 Co1 N2 112.89(15) . . ? N8 Co1 N1 78.33(16) . . ? N5 Co1 N1 78.39(15) . . ? N2 Co1 N1 78.67(15) . . ? N8 Co1 S1 99.42(12) . . ? N5 Co1 S1 114.08(12) . . ? N2 Co1 S1 91.04(12) . . ? N1 Co1 S1 166.45(11) . . ? O6 Cl1 O3 107.4(3) . . ? O6 Cl1 O5 111.2(3) . . ? O3 Cl1 O5 110.1(3) . . ? O6 Cl1 O4 109.0(3) . . ? O3 Cl1 O4 109.3(3) . . ? O5 Cl1 O4 109.8(3) . . ? O10 Cl2 O9 111.1(3) . . ? O10 Cl2 O7 109.3(3) . . ? O9 Cl2 O7 108.2(3) . . ? O10 Cl2 O8 109.4(3) . . ? O9 Cl2 O8 107.9(3) . . ? O7 Cl2 O8 111.0(3) . . ? _diffrn_measured_fraction_theta_max 0.931 _diffrn_reflns_theta_full 27.54 _diffrn_measured_fraction_theta_full 0.931 _refine_diff_density_max 0.485 _refine_diff_density_min -0.651 _refine_diff_density_rms 0.107 data_aja0832 _database_code_depnum_ccdc_archive 'CCDC 844372' #TrackingRef '- aja0832_L1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C34 H30 N8 O2 S2' _chemical_formula_sum 'C34 H30 N8 O2 S2' _chemical_formula_weight 646.78 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' _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 5.7870(10) _cell_length_b 15.603(2) _cell_length_c 17.042(4) _cell_angle_alpha 97.285(5) _cell_angle_beta 96.425(6) _cell_angle_gamma 91.148(7) _cell_volume 1515.9(5) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 1394 _cell_measurement_theta_min 3.64 _cell_measurement_theta_max 19.76 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.417 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 676 _exptl_absorpt_coefficient_mu 0.224 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.9651 _exptl_absorpt_correction_T_max 0.9867 _exptl_absorpt_process_details Denzo/scalepack _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 'Nonius KappaCCD' _diffrn_measurement_method 'CCD scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4216 _diffrn_reflns_av_R_equivalents 0.1388 _diffrn_reflns_av_sigmaI/netI 0.2118 _diffrn_reflns_limit_h_min -5 _diffrn_reflns_limit_h_max 5 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.64 _diffrn_reflns_theta_max 19.76 _reflns_number_total 2516 _reflns_number_gt 1394 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'cOLLECT,Nonius BV, 1997-2001' _computing_cell_refinement DENZO/SCALEPACK _computing_data_reduction DENZO/SCALEPACK _computing_structure_solution SHELXs-97 _computing_structure_refinement SHELXL-97 _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^)+(0.0000P)^2^+3.2506P] 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 2516 _refine_ls_number_parameters 195 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1731 _refine_ls_R_factor_gt 0.0916 _refine_ls_wR_factor_ref 0.1978 _refine_ls_wR_factor_gt 0.1638 _refine_ls_goodness_of_fit_ref 1.012 _refine_ls_restrained_S_all 1.012 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.0347(17) 1.2099(5) 0.2639(6) 0.031(2) Uiso 1 1 d . . . H1A H -0.1316 1.1913 0.2530 0.037 Uiso 1 1 calc R . . H1B H 0.0584 1.2436 0.3176 0.037 Uiso 1 1 calc R . . C2 C 0.1790(17) 1.1312(6) 0.2640(6) 0.029(2) Uiso 1 1 d . . . C3 C 0.3669(17) 1.1175(6) 0.2220(6) 0.034(3) Uiso 1 1 d . . . H3 H 0.4109 1.1583 0.1890 0.041 Uiso 1 1 calc R . . C4 C 0.4920(18) 1.0429(6) 0.2284(6) 0.040(3) Uiso 1 1 d . . . H4 H 0.6259 1.0330 0.2014 0.048 Uiso 1 1 calc R . . C5 C 0.4180(18) 0.9837(6) 0.2745(6) 0.039(3) Uiso 1 1 d . . . H5 H 0.5010 0.9326 0.2809 0.046 Uiso 1 1 calc R . . C6 C 0.2218(18) 1.0005(6) 0.3109(6) 0.036(3) Uiso 1 1 d . . . C7 C 0.1204(17) 0.8613(6) 0.3612(6) 0.037(3) Uiso 1 1 d . . . C8 C -0.1946(18) 0.8724(6) 0.4514(6) 0.044(3) Uiso 1 1 d . . . C9 C -0.3325(17) 0.8196(6) 0.4976(6) 0.033(3) Uiso 1 1 d . . . C10 C -0.3011(18) 0.7325(6) 0.5026(6) 0.044(3) Uiso 1 1 d . . . H10 H -0.1817 0.7032 0.4772 0.052 Uiso 1 1 calc R . . C11 C -0.4455(18) 0.6885(6) 0.5450(6) 0.042(3) Uiso 1 1 d . . . H11 H -0.4234 0.6290 0.5491 0.050 Uiso 1 1 calc R . . C12 C -0.6174(18) 0.7298(6) 0.5804(6) 0.038(3) Uiso 1 1 d . . . H12 H -0.7152 0.6981 0.6085 0.045 Uiso 1 1 calc R . . C13 C -0.6557(18) 0.8169(6) 0.5771(6) 0.044(3) Uiso 1 1 d . . . H13 H -0.7755 0.8453 0.6031 0.052 Uiso 1 1 calc R . . C14 C -0.5108(18) 0.8616(7) 0.5340(6) 0.048(3) Uiso 1 1 d . . . H14 H -0.5345 0.9209 0.5296 0.057 Uiso 1 1 calc R . . C15 C -0.1091(17) 1.2982(6) 0.1582(6) 0.034(3) Uiso 1 1 d . . . H15A H -0.0544 1.3460 0.1311 0.041 Uiso 1 1 calc R . . H15B H -0.2209 1.3220 0.1945 0.041 Uiso 1 1 calc R . . C16 C -0.2326(17) 1.2302(6) 0.0968(5) 0.029(2) Uiso 1 1 d . . . C17 C -0.1402(18) 1.1508(6) 0.0753(6) 0.038(3) Uiso 1 1 d . . . H17 H 0.0047 1.1361 0.1013 0.045 Uiso 1 1 calc R . . C18 C -0.2588(18) 1.0935(6) 0.0162(6) 0.040(3) Uiso 1 1 d . . . H18 H -0.1965 1.0389 0.0008 0.048 Uiso 1 1 calc R . . C19 C -0.4675(18) 1.1156(6) -0.0204(6) 0.040(3) Uiso 1 1 d . . . H19 H -0.5550 1.0768 -0.0610 0.047 Uiso 1 1 calc R . . C20 C -0.5461(17) 1.1971(6) 0.0042(6) 0.033(3) Uiso 1 1 d . . . C21 C -0.9028(18) 1.2016(6) -0.0925(6) 0.040(3) Uiso 1 1 d . . . C22 C -1.1361(16) 1.3371(5) -0.0735(6) 0.025(2) Uiso 1 1 d . . . C23 C -1.3452(17) 1.3764(6) -0.1088(6) 0.034(3) Uiso 1 1 d . . . C24 C -1.5187(17) 1.3318(6) -0.1608(6) 0.037(3) Uiso 1 1 d . . . H24 H -1.5052 1.2718 -0.1773 0.045 Uiso 1 1 calc R . . C25 C -1.7135(17) 1.3741(6) -0.1890(6) 0.035(3) Uiso 1 1 d . . . H25 H -1.8314 1.3436 -0.2259 0.042 Uiso 1 1 calc R . . C26 C -1.7347(18) 1.4608(6) -0.1631(6) 0.039(3) Uiso 1 1 d . . . H26 H -1.8705 1.4894 -0.1808 0.046 Uiso 1 1 calc R . . C27 C -1.5627(18) 1.5058(6) -0.1123(6) 0.041(3) Uiso 1 1 d . . . H27 H -1.5782 1.5657 -0.0958 0.049 Uiso 1 1 calc R . . C28 C -1.3642(18) 1.4646(6) -0.0845(6) 0.038(3) Uiso 1 1 d . . . H28 H -1.2436 1.4961 -0.0495 0.045 Uiso 1 1 calc R . . C29 C 0.2676(18) 1.3316(6) 0.2372(6) 0.041(3) Uiso 1 1 d . . . H29A H 0.3316 1.3533 0.1916 0.049 Uiso 1 1 calc R . . H29B H 0.3950 1.3029 0.2663 0.049 Uiso 1 1 calc R . . C30 C 0.2020(18) 1.4107(6) 0.2931(6) 0.039(3) Uiso 1 1 d . . . C31 C 0.344(2) 1.4840(6) 0.3051(7) 0.052(3) Uiso 1 1 d . . . H31 H 0.4744 1.4867 0.2761 0.063 Uiso 1 1 calc R . . C32 C 0.299(2) 1.5531(7) 0.3589(7) 0.061(3) Uiso 1 1 d . . . H32 H 0.3975 1.6038 0.3682 0.073 Uiso 1 1 calc R . . C33 C 0.109(2) 1.5464(7) 0.3984(7) 0.055(3) Uiso 1 1 d . . . H33 H 0.0746 1.5917 0.4378 0.066 Uiso 1 1 calc R . . C34 C -0.031(2) 1.4745(7) 0.3809(7) 0.055(3) Uiso 1 1 d . . . H34 H -0.1678 1.4727 0.4067 0.066 Uiso 1 1 calc R . . N1 N 0.0888(13) 1.2663(4) 0.2052(4) 0.029(2) Uiso 1 1 d . . . N2 N 0.1041(13) 1.0728(5) 0.3068(4) 0.032(2) Uiso 1 1 d . . . N3 N 0.1130(13) 0.9444(5) 0.3574(5) 0.035(2) Uiso 1 1 d . . . H3A H 0.0226 0.9714 0.3900 0.042 Uiso 1 1 calc R . . N4 N -0.0341(14) 0.8304(5) 0.4077(5) 0.039(2) Uiso 1 1 d . . . H4A H -0.0297 0.7744 0.4099 0.046 Uiso 1 1 calc R . . N5 N -0.4350(13) 1.2534(4) 0.0623(4) 0.030(2) Uiso 1 1 d . . . N6 N -0.7534(13) 1.2312(5) -0.0301(5) 0.033(2) Uiso 1 1 d . . . H6 H -0.7889 1.2813 -0.0053 0.040 Uiso 1 1 calc R . . N7 N -1.0858(14) 1.2557(5) -0.1090(5) 0.040(2) Uiso 1 1 d . . . H7 H -1.1880 1.2343 -0.1492 0.048 Uiso 1 1 calc R . . N8 N 0.0112(15) 1.4038(5) 0.3285(5) 0.042(2) Uiso 1 1 d . . . O1 O -0.2230(12) 0.9511(4) 0.4514(4) 0.0472(19) Uiso 1 1 d . . . O2 O -1.0107(11) 1.3700(4) -0.0136(4) 0.0392(18) Uiso 1 1 d . . . S1 S 0.2885(5) 0.78888(17) 0.31601(17) 0.0501(9) Uani 1 1 d . . . S2 S -0.8984(6) 1.10934(19) -0.1538(2) 0.0686(12) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 S1 0.062(2) 0.0425(17) 0.048(2) 0.0060(14) 0.0157(16) 0.0129(15) S2 0.068(2) 0.0492(19) 0.074(3) -0.0250(16) -0.0247(19) 0.0270(17) _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 C1 N1 1.469(11) . ? C1 C2 1.499(12) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 N2 1.330(11) . ? C2 C3 1.374(12) . ? C3 C4 1.392(12) . ? C3 H3 0.9500 . ? C4 C5 1.378(13) . ? C4 H4 0.9500 . ? C5 C6 1.368(13) . ? C5 H5 0.9500 . ? C6 N2 1.336(11) . ? C6 N3 1.433(11) . ? C7 N3 1.308(11) . ? C7 N4 1.378(12) . ? C7 S1 1.675(10) . ? C8 O1 1.241(11) . ? C8 N4 1.379(12) . ? C8 C9 1.488(14) . ? C9 C10 1.386(13) . ? C9 C14 1.395(13) . ? C10 C11 1.389(13) . ? C10 H10 0.9500 . ? C11 C12 1.353(13) . ? C11 H11 0.9500 . ? C12 C13 1.389(13) . ? C12 H12 0.9500 . ? C13 C14 1.405(13) . ? C13 H13 0.9500 . ? C14 H14 0.9500 . ? C15 N1 1.455(11) . ? C15 C16 1.501(12) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 N5 1.329(11) . ? C16 C17 1.382(12) . ? C17 C18 1.370(13) . ? C17 H17 0.9500 . ? C18 C19 1.367(13) . ? C18 H18 0.9500 . ? C19 C20 1.390(12) . ? C19 H19 0.9500 . ? C20 N5 1.334(11) . ? C20 N6 1.418(11) . ? C21 N6 1.322(11) . ? C21 N7 1.394(12) . ? C21 S2 1.670(10) . ? C22 O2 1.232(10) . ? C22 N7 1.388(11) . ? C22 C23 1.470(13) . ? C23 C24 1.376(12) . ? C23 C28 1.397(12) . ? C24 C25 1.388(13) . ? C24 H24 0.9500 . ? C25 C26 1.382(12) . ? C25 H25 0.9500 . ? C26 C27 1.363(13) . ? C26 H26 0.9500 . ? C27 C28 1.393(13) . ? C27 H27 0.9500 . ? C28 H28 0.9500 . ? C29 N1 1.448(11) . ? C29 C30 1.541(13) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C30 N8 1.325(12) . ? C30 C31 1.376(13) . ? C31 C32 1.373(14) . ? C31 H31 0.9500 . ? C32 C33 1.365(15) . ? C32 H32 0.9500 . ? C33 C34 1.351(13) . ? C33 H33 0.9500 . ? C34 N8 1.372(12) . ? C34 H34 0.9500 . ? N3 H3A 0.8800 . ? N4 H4A 0.8800 . ? N6 H6 0.8800 . ? N7 H7 0.8800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 C2 113.9(8) . . ? N1 C1 H1A 108.8 . . ? C2 C1 H1A 108.8 . . ? N1 C1 H1B 108.8 . . ? C2 C1 H1B 108.8 . . ? H1A C1 H1B 107.7 . . ? N2 C2 C3 121.9(9) . . ? N2 C2 C1 113.9(8) . . ? C3 C2 C1 124.1(8) . . ? C2 C3 C4 119.1(9) . . ? C2 C3 H3 120.5 . . ? C4 C3 H3 120.5 . . ? C5 C4 C3 118.8(10) . . ? C5 C4 H4 120.6 . . ? C3 C4 H4 120.6 . . ? C6 C5 C4 118.1(10) . . ? C6 C5 H5 120.9 . . ? C4 C5 H5 120.9 . . ? N2 C6 C5 123.4(9) . . ? N2 C6 N3 110.8(9) . . ? C5 C6 N3 125.8(9) . . ? N3 C7 N4 114.6(9) . . ? N3 C7 S1 128.4(8) . . ? N4 C7 S1 116.9(7) . . ? O1 C8 N4 120.9(9) . . ? O1 C8 C9 121.7(10) . . ? N4 C8 C9 117.3(9) . . ? C10 C9 C14 119.7(9) . . ? C10 C9 C8 124.2(9) . . ? C14 C9 C8 116.1(9) . . ? C9 C10 C11 119.5(10) . . ? C9 C10 H10 120.3 . . ? C11 C10 H10 120.3 . . ? C12 C11 C10 120.5(10) . . ? C12 C11 H11 119.7 . . ? C10 C11 H11 119.7 . . ? C11 C12 C13 122.2(9) . . ? C11 C12 H12 118.9 . . ? C13 C12 H12 118.9 . . ? C12 C13 C14 117.5(10) . . ? C12 C13 H13 121.2 . . ? C14 C13 H13 121.2 . . ? C9 C14 C13 120.7(10) . . ? C9 C14 H14 119.7 . . ? C13 C14 H14 119.7 . . ? N1 C15 C16 113.5(7) . . ? N1 C15 H15A 108.9 . . ? C16 C15 H15A 108.9 . . ? N1 C15 H15B 108.9 . . ? C16 C15 H15B 108.9 . . ? H15A C15 H15B 107.7 . . ? N5 C16 C17 122.3(8) . . ? N5 C16 C15 114.7(8) . . ? C17 C16 C15 123.0(9) . . ? C18 C17 C16 119.6(10) . . ? C18 C17 H17 120.2 . . ? C16 C17 H17 120.2 . . ? C19 C18 C17 119.5(10) . . ? C19 C18 H18 120.2 . . ? C17 C18 H18 120.2 . . ? C18 C19 C20 117.1(10) . . ? C18 C19 H19 121.5 . . ? C20 C19 H19 121.5 . . ? N5 C20 C19 124.4(9) . . ? N5 C20 N6 111.5(8) . . ? C19 C20 N6 124.1(9) . . ? N6 C21 N7 114.8(8) . . ? N6 C21 S2 128.6(8) . . ? N7 C21 S2 116.6(8) . . ? O2 C22 N7 118.7(9) . . ? O2 C22 C23 124.6(8) . . ? N7 C22 C23 116.6(8) . . ? C24 C23 C28 120.0(9) . . ? C24 C23 C22 124.5(8) . . ? C28 C23 C22 115.5(8) . . ? C23 C24 C25 120.2(9) . . ? C23 C24 H24 119.9 . . ? C25 C24 H24 119.9 . . ? C26 C25 C24 119.6(9) . . ? C26 C25 H25 120.2 . . ? C24 C25 H25 120.2 . . ? C27 C26 C25 120.6(10) . . ? C27 C26 H26 119.7 . . ? C25 C26 H26 119.7 . . ? C26 C27 C28 120.5(9) . . ? C26 C27 H27 119.8 . . ? C28 C27 H27 119.8 . . ? C27 C28 C23 119.0(9) . . ? C27 C28 H28 120.5 . . ? C23 C28 H28 120.5 . . ? N1 C29 C30 118.7(8) . . ? N1 C29 H29A 107.6 . . ? C30 C29 H29A 107.6 . . ? N1 C29 H29B 107.6 . . ? C30 C29 H29B 107.6 . . ? H29A C29 H29B 107.1 . . ? N8 C30 C31 123.1(9) . . ? N8 C30 C29 117.7(8) . . ? C31 C30 C29 119.1(9) . . ? C32 C31 C30 120.4(11) . . ? C32 C31 H31 119.8 . . ? C30 C31 H31 119.8 . . ? C33 C32 C31 117.6(11) . . ? C33 C32 H32 121.2 . . ? C31 C32 H32 121.2 . . ? C34 C33 C32 119.1(11) . . ? C34 C33 H33 120.5 . . ? C32 C33 H33 120.5 . . ? C33 C34 N8 124.6(11) . . ? C33 C34 H34 117.7 . . ? N8 C34 H34 117.7 . . ? C29 N1 C15 114.4(7) . . ? C29 N1 C1 112.6(8) . . ? C15 N1 C1 116.4(7) . . ? C2 N2 C6 118.5(8) . . ? C7 N3 C6 133.2(9) . . ? C7 N3 H3A 113.4 . . ? C6 N3 H3A 113.4 . . ? C7 N4 C8 130.9(8) . . ? C7 N4 H4A 114.5 . . ? C8 N4 H4A 114.5 . . ? C16 N5 C20 117.1(8) . . ? C21 N6 C20 131.8(8) . . ? C21 N6 H6 114.1 . . ? C20 N6 H6 114.1 . . ? C22 N7 C21 131.7(9) . . ? C22 N7 H7 114.2 . . ? C21 N7 H7 114.2 . . ? C30 N8 C34 115.0(8) . . ? _diffrn_measured_fraction_theta_max 0.916 _diffrn_reflns_theta_full 19.76 _diffrn_measured_fraction_theta_full 0.916 _refine_diff_density_max 0.311 _refine_diff_density_min -0.261 _refine_diff_density_rms 0.060 data_aja0942 _database_code_depnum_ccdc_archive 'CCDC 844373' #TrackingRef '- aja0942.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C34 H30 Mn N8 O2 S2, 2(Cl O4), 2(H2 O)' _chemical_formula_sum 'C34 H34 Cl2 Mn N8 O12 S2' _chemical_formula_weight 936.65 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' Mn Mn 0.3368 0.7283 '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 Monoclinic _symmetry_space_group_name_H-M P21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 14.846(3) _cell_length_b 11.049(3) _cell_length_c 23.882(6) _cell_angle_alpha 90.00 _cell_angle_beta 97.313(9) _cell_angle_gamma 90.00 _cell_volume 3885.6(16) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 2541 _cell_measurement_theta_min 2.98 _cell_measurement_theta_max 19.30 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.601 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1924 _exptl_absorpt_coefficient_mu 0.659 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.9076 _exptl_absorpt_correction_T_max 0.9371 _exptl_absorpt_process_details Denzo/Scalepack _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 'Nonius KappaCCD' _diffrn_measurement_method 'CCD scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4391 _diffrn_reflns_av_R_equivalents 0.0838 _diffrn_reflns_av_sigmaI/netI 0.1245 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.98 _diffrn_reflns_theta_max 19.30 _reflns_number_total 2818 _reflns_number_gt 2541 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'cOLLECT,Nonius BV, 1997-2001' _computing_cell_refinement DENZO/SCALEPACK _computing_data_reduction DENZO/SCALEPACK _computing_structure_solution SHELXs-97 _computing_structure_refinement SHELXL-97 _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. Only poor quality crystals could be obtained despite numerous attempts to grow better crystals. The crystals were twinned and the resultant weak data did not allow full anisotropic refinement leading to the lower precision in the determined parameters. Geometrical constraints were applied and specifically, the rings were made into regular hexagons, ; _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^)+(0.0001P)^2^+486.6085P] 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 2818 _refine_ls_number_parameters 232 _refine_ls_number_restraints 94 _refine_ls_R_factor_all 0.2603 _refine_ls_R_factor_gt 0.2481 _refine_ls_wR_factor_ref 0.5138 _refine_ls_wR_factor_gt 0.5043 _refine_ls_goodness_of_fit_ref 1.239 _refine_ls_restrained_S_all 1.220 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.872(2) 0.770(4) 0.1733(16) 0.033(10) Uiso 1 1 d . . . H1A H 0.8820 0.8041 0.2120 0.040 Uiso 1 1 calc R . . H1B H 0.8854 0.8341 0.1465 0.040 Uiso 1 1 calc R . . N1 N 0.7784(10) 0.7309(13) 0.1602(6) 0.046(10) Uiso 1 1 d . . . N2 N 0.9120(10) 0.5836(13) 0.1231(6) 0.037(9) Uiso 1 1 d R . . C2 C 0.9318(10) 0.6616(13) 0.1686(6) 0.036(11) Uiso 1 1 d R . . C3 C 1.0139(10) 0.6516(13) 0.2033(6) 0.041(11) Uiso 1 1 d R . . H3 H 1.0274 0.7050 0.2344 0.049 Uiso 1 1 calc R . . C4 C 1.0762(10) 0.5637(13) 0.1925(6) 0.027(10) Uiso 1 1 d R . . H4 H 1.1324 0.5569 0.2162 0.033 Uiso 1 1 calc R . . C5 C 1.0565(10) 0.4857(13) 0.1470(6) 0.057(13) Uiso 1 1 d R . . H5 H 1.0991 0.4256 0.1396 0.069 Uiso 1 1 calc R . . C6 C 0.9743(10) 0.4956(13) 0.1123(6) 0.029(10) Uiso 1 1 d R . . C7 C 0.902(2) 0.438(2) 0.0185(16) 0.036(11) Uiso 1 1 d D . . C8 C 0.946(3) 0.252(4) -0.0154(18) 0.041(11) Uiso 1 1 d . . . N3 N 0.9604(18) 0.426(3) 0.0693(11) 0.023(7) Uiso 1 1 d . . . H3A H 0.9930 0.3596 0.0720 0.027 Uiso 1 1 calc R . . N4 N 0.8972(11) 0.3569(15) -0.0196(7) 0.021(7) Uiso 1 1 d . . . H4A H 0.8599 0.3695 -0.0507 0.026 Uiso 1 1 calc R . . C9 C 0.9342(11) 0.1610(15) -0.0663(7) 0.033(10) Uiso 1 1 d R . . C10 C 0.8624(11) 0.1782(15) -0.1088(7) 0.074(16) Uiso 1 1 d R . . H10 H 0.8222 0.2447 -0.1069 0.089 Uiso 1 1 calc R . . C11 C 0.8492(11) 0.0983(15) -0.1539(7) 0.097(19) Uiso 1 1 d R . . H11 H 0.8000 0.1101 -0.1830 0.116 Uiso 1 1 calc R . . C12 C 0.9078(11) 0.0011(15) -0.1566(7) 0.083(17) Uiso 1 1 d R . . H12 H 0.8988 -0.0536 -0.1875 0.100 Uiso 1 1 calc R . . C13 C 0.9796(11) -0.0162(15) -0.1141(7) 0.078(16) Uiso 1 1 d R . . H13 H 1.0197 -0.0826 -0.1159 0.094 Uiso 1 1 calc R . . C14 C 0.9928(11) 0.0638(15) -0.0689(7) 0.055(13) Uiso 1 1 d R . . H14 H 1.0420 0.0520 -0.0399 0.066 Uiso 1 1 calc R . . C15 C 0.7430(10) 0.6653(13) 0.2081(6) 0.046(12) Uiso 1 1 d . . . H15A H 0.7918 0.6138 0.2276 0.056 Uiso 1 1 calc R . . H15B H 0.7256 0.7251 0.2356 0.056 Uiso 1 1 calc R . . N5 N 0.6544(10) 0.5383(13) 0.1349(6) 0.011(7) Uiso 1 1 d R . . C16 C 0.6646(10) 0.5900(13) 0.1883(6) 0.038(11) Uiso 1 1 d R . . C17 C 0.6023(10) 0.5644(13) 0.2254(6) 0.049(12) Uiso 1 1 d R . . H17 H 0.6093 0.5998 0.2620 0.059 Uiso 1 1 calc R . . C18 C 0.5299(10) 0.4873(13) 0.2091(6) 0.060(14) Uiso 1 1 d R . . H18 H 0.4873 0.4698 0.2345 0.072 Uiso 1 1 calc R . . C19 C 0.5197(10) 0.4357(13) 0.1557(6) 0.041(11) Uiso 1 1 d R . . H19 H 0.4702 0.3829 0.1445 0.049 Uiso 1 1 calc R . . C20 C 0.5820(10) 0.4612(13) 0.1185(6) 0.026(10) Uiso 1 1 d R . . C21 C 0.600(2) 0.4439(17) 0.0202(15) 0.024(10) Uiso 1 1 d D . . C22 C 0.5536(11) 0.2424(17) -0.0207(8) 0.024(9) Uiso 1 1 d . . . C23 C 0.5392(11) 0.1783(17) -0.0792(8) 0.036(11) Uiso 1 1 d R . . C24 C 0.5493(11) 0.2379(17) -0.1292(8) 0.045(12) Uiso 1 1 d R . . H24 H 0.5667 0.3207 -0.1285 0.054 Uiso 1 1 calc R . . C25 C 0.5339(11) 0.1765(17) -0.1803(8) 0.060(14) Uiso 1 1 d R . . H25 H 0.5408 0.2173 -0.2145 0.072 Uiso 1 1 calc R . . C26 C 0.5084(11) 0.0555(17) -0.1813(8) 0.076(16) Uiso 1 1 d R . . H26 H 0.4979 0.0135 -0.2163 0.092 Uiso 1 1 calc R . . C27 C 0.4983(11) -0.0042(17) -0.1313(8) 0.077(16) Uiso 1 1 d R . . H27 H 0.4809 -0.0869 -0.1320 0.093 Uiso 1 1 calc R . . C28 C 0.5137(11) 0.0572(17) -0.0802(8) 0.10(2) Uiso 1 1 d R . . H28 H 0.5068 0.0164 -0.0460 0.124 Uiso 1 1 calc R . . C29 C 0.720(2) 0.838(3) 0.1422(14) 0.024(10) Uiso 1 1 d . . . H29A H 0.6556 0.8158 0.1402 0.029 Uiso 1 1 calc R . . H29B H 0.7326 0.9038 0.1705 0.029 Uiso 1 1 calc R . . N6 N 0.5779(17) 0.407(3) 0.0696(11) 0.020(7) Uiso 1 1 d . . . H6 H 0.5570 0.3320 0.0694 0.024 Uiso 1 1 calc R . . N7 N 0.5907(9) 0.3529(14) -0.0199(7) 0.025(8) Uiso 1 1 d . . . H7 H 0.6141 0.3712 -0.0509 0.030 Uiso 1 1 calc R . . N8 N 0.7555(9) 0.7922(14) 0.0492(7) 0.029(8) Uiso 1 1 d R . . C30 C 0.7389(9) 0.8826(14) 0.0870(7) 0.043(11) Uiso 1 1 d R . . C31 C 0.7307(9) 1.0022(14) 0.0692(7) 0.089(18) Uiso 1 1 d R . . H31 H 0.7193 1.0639 0.0951 0.107 Uiso 1 1 calc R . . C32 C 0.7392(9) 1.0315(14) 0.0136(7) 0.069(15) Uiso 1 1 d R . . H32 H 0.7336 1.1133 0.0014 0.083 Uiso 1 1 calc R . . C33 C 0.7558(9) 0.9412(14) -0.0242(7) 0.058(14) Uiso 1 1 d R . . H33 H 0.7617 0.9612 -0.0623 0.070 Uiso 1 1 calc R . . C34 C 0.7640(9) 0.8215(14) -0.0064(7) 0.057(13) Uiso 1 1 d R . . H34 H 0.7754 0.7598 -0.0323 0.069 Uiso 1 1 calc R . . O1 O 1.003(2) 0.222(3) 0.0238(14) 0.069(10) Uani 1 1 d U . . O2 O 0.5277(19) 0.199(3) 0.0194(12) 0.059(9) Uani 1 1 d U . . O3 O 0.7782(12) 0.3751(15) 0.0957(5) 0.024(6) Uani 1 1 d DU . . O4 O 0.8187(15) 0.3884(17) 0.1939(6) 0.067(9) Uani 1 1 d DU . . O5 O 0.7101(10) 0.2463(19) 0.1562(9) 0.073(10) Uani 1 1 d DU . . O6 O 0.8633(12) 0.2201(15) 0.1442(9) 0.047(8) Uani 1 1 d DU . . O7 O 1.174(3) 0.669(3) 0.3137(17) 0.28(4) Uani 1 1 d DU . . O8 O 1.164(3) 0.878(3) 0.2987(16) 0.25(3) Uani 1 1 d DU . . O9 O 1.271(2) 0.800(4) 0.3706(7) 0.122(15) Uani 1 1 d DU . . O10 O 1.2909(18) 0.771(4) 0.2757(11) 0.121(15) Uani 1 1 d DU . . O11 O 0.7214(19) 0.431(3) -0.0975(12) 0.058(9) Uani 1 1 d U . . O12 O 1.319(3) 0.594(4) 0.2059(19) 0.119(15) Uani 1 1 d U . . S1 S 0.8542(11) 0.5640(15) 0.0006(7) 0.089(5) Uani 1 1 d D . . S2 S 0.6324(8) 0.5763(10) 0.0047(5) 0.052(3) Uani 1 1 d D . . Mn1 Mn 0.7661(4) 0.6000(5) 0.0829(2) 0.0202(17) Uani 1 1 d . . . Cl1 Cl 0.7925(7) 0.3076(9) 0.1477(4) 0.043(3) Uani 1 1 d D . . Cl2 Cl 1.2249(7) 0.7794(9) 0.3148(4) 0.047(3) Uani 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 O1 0.066(12) 0.069(12) 0.072(12) -0.004(9) 0.005(9) 0.005(9) O2 0.063(12) 0.053(12) 0.059(12) 0.001(9) 0.003(9) 0.001(9) O3 0.025(9) 0.025(9) 0.022(9) 0.001(8) 0.005(7) 0.002(8) O4 0.071(12) 0.062(12) 0.066(12) 0.007(9) 0.005(9) 0.004(9) O5 0.074(13) 0.071(13) 0.075(13) 0.009(9) 0.011(9) -0.003(9) O6 0.040(11) 0.049(11) 0.053(11) 0.008(9) 0.010(8) 0.004(9) O7 0.28(4) 0.28(4) 0.28(4) 0.000(10) 0.034(11) -0.004(10) O8 0.25(4) 0.25(4) 0.24(4) 0.001(10) 0.034(11) 0.006(10) O9 0.125(17) 0.121(18) 0.120(17) 0.002(10) 0.012(10) -0.002(10) O10 0.120(17) 0.121(17) 0.120(17) 0.000(10) 0.014(10) 0.006(10) O11 0.056(11) 0.055(12) 0.062(12) -0.006(9) 0.006(9) -0.002(9) O12 0.121(17) 0.118(17) 0.118(17) 0.000(10) 0.017(10) 0.000(10) S1 0.086(11) 0.101(13) 0.082(11) -0.023(10) 0.017(8) 0.023(10) S2 0.048(8) 0.044(8) 0.062(8) -0.004(6) 0.000(6) -0.011(6) Mn1 0.026(4) 0.014(3) 0.019(3) -0.007(3) -0.005(2) 0.000(3) Cl1 0.054(8) 0.040(7) 0.036(7) 0.005(6) 0.012(5) -0.011(6) Cl2 0.071(8) 0.029(6) 0.039(7) -0.006(5) -0.007(6) -0.003(6) _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 C1 N1 1.45(4) . ? C1 C2 1.51(4) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? N1 C29 1.50(4) . ? N1 C15 1.50(2) . ? N1 Mn1 2.335(15) . ? N2 C6 1.3888 . ? N2 C2 1.3889 . ? N2 Mn1 2.262(15) . ? C2 C3 1.3883 . ? C3 C4 1.3888 . ? C3 H3 0.9500 . ? C4 C5 1.3889 . ? C4 H4 0.9500 . ? C5 C6 1.3883 . ? C5 H5 0.9500 . ? C6 N3 1.28(3) . ? C7 N4 1.27(4) . ? C7 N3 1.40(4) . ? C7 S1 1.598(10) . ? C8 O1 1.23(4) . ? C8 N4 1.36(4) . ? C8 C9 1.57(4) . ? N3 H3A 0.8800 . ? N4 H4A 0.8800 . ? C9 C10 1.3884 . ? C9 C14 1.3889 . ? C10 C11 1.3889 . ? C10 H10 0.9500 . ? C11 C12 1.3889 . ? C11 H11 0.9500 . ? C12 C13 1.3884 . ? C12 H12 0.9500 . ? C13 C14 1.3889 . ? C13 H13 0.9500 . ? C14 H14 0.9500 . ? C15 C16 1.4598 . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? N5 C20 1.3887 . ? N5 C16 1.3888 . ? N5 Mn1 2.298(16) . ? C16 C17 1.3887 . ? C17 C18 1.3886 . ? C17 H17 0.9500 . ? C18 C19 1.3888 . ? C18 H18 0.9500 . ? C19 C20 1.3886 . ? C19 H19 0.9500 . ? C20 N6 1.31(3) . ? C21 N6 1.33(4) . ? C21 N7 1.38(3) . ? C21 S2 1.600(10) . ? C22 O2 1.18(3) . ? C22 N7 1.34(2) . ? C22 C23 1.5576 . ? C23 C24 1.3889 . ? C23 C28 1.3892 . ? C24 C25 1.3889 . ? C24 H24 0.9500 . ? C25 C26 1.3892 . ? C25 H25 0.9500 . ? C26 C27 1.3889 . ? C26 H26 0.9500 . ? C27 C28 1.3889 . ? C27 H27 0.9500 . ? C28 H28 0.9500 . ? C29 C30 1.46(4) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? N6 H6 0.8800 . ? N7 H7 0.8800 . ? N8 C34 1.3888 . ? N8 C30 1.3890 . ? N8 Mn1 2.269(16) . ? C30 C31 1.3892 . ? C31 C32 1.3888 . ? C31 H31 0.9500 . ? C32 C33 1.3890 . ? C32 H32 0.9500 . ? C33 C34 1.3892 . ? C33 H33 0.9500 . ? C34 H34 0.9500 . ? O3 Cl1 1.442(8) . ? O3 Mn1 2.508(17) . ? O4 Cl1 1.433(8) . ? O5 Cl1 1.436(8) . ? O6 Cl1 1.438(8) . ? O7 Cl2 1.436(9) . ? O8 Cl2 1.437(9) . ? O9 Cl2 1.435(9) . ? O10 Cl2 1.439(9) . ? S1 Mn1 2.527(16) . ? S2 Mn1 2.560(12) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 C2 108(3) . . ? N1 C1 H1A 110.2 . . ? C2 C1 H1A 110.2 . . ? N1 C1 H1B 110.2 . . ? C2 C1 H1B 110.2 . . ? H1A C1 H1B 108.5 . . ? C1 N1 C29 109(2) . . ? C1 N1 C15 113.5(19) . . ? C29 N1 C15 111.0(17) . . ? C1 N1 Mn1 109.5(17) . . ? C29 N1 Mn1 106.2(15) . . ? C15 N1 Mn1 107.6(9) . . ? C6 N2 C2 120.0 . . ? C6 N2 Mn1 127.0(4) . . ? C2 N2 Mn1 112.2(4) . . ? C3 C2 N2 120.0 . . ? C3 C2 C1 120.0(15) . . ? N2 C2 C1 119.0(15) . . ? C2 C3 C4 120.0 . . ? C2 C3 H3 120.0 . . ? C4 C3 H3 120.0 . . ? C3 C4 C5 120.0 . . ? C3 C4 H4 120.0 . . ? C5 C4 H4 120.0 . . ? C6 C5 C4 120.0 . . ? C6 C5 H5 120.0 . . ? C4 C5 H5 120.0 . . ? N3 C6 C5 118.2(14) . . ? N3 C6 N2 121.7(14) . . ? C5 C6 N2 120.0 . . ? N4 C7 N3 122(2) . . ? N4 C7 S1 116(2) . . ? N3 C7 S1 121(3) . . ? O1 C8 N4 127(4) . . ? O1 C8 C9 115(3) . . ? N4 C8 C9 119(3) . . ? C6 N3 C7 131(3) . . ? C6 N3 H3A 114.4 . . ? C7 N3 H3A 114.4 . . ? C7 N4 C8 124(2) . . ? C7 N4 H4A 117.8 . . ? C8 N4 H4A 117.8 . . ? C10 C9 C14 120.0 . . ? C10 C9 C8 118.5(16) . . ? C14 C9 C8 121.5(16) . . ? C9 C10 C11 120.0 . . ? C9 C10 H10 120.0 . . ? C11 C10 H10 120.0 . . ? C12 C11 C10 120.0 . . ? C12 C11 H11 120.0 . . ? C10 C11 H11 120.0 . . ? C13 C12 C11 120.0 . . ? C13 C12 H12 120.0 . . ? C11 C12 H12 120.0 . . ? C12 C13 C14 120.0 . . ? C12 C13 H13 120.0 . . ? C14 C13 H13 120.0 . . ? C9 C14 C13 120.0 . . ? C9 C14 H14 120.0 . . ? C13 C14 H14 120.0 . . ? C16 C15 N1 111.8(8) . . ? C16 C15 H15A 109.3 . . ? N1 C15 H15A 109.3 . . ? C16 C15 H15B 109.3 . . ? N1 C15 H15B 109.3 . . ? H15A C15 H15B 107.9 . . ? C20 N5 C16 120.0 . . ? C20 N5 Mn1 128.1(4) . . ? C16 N5 Mn1 111.9(4) . . ? C17 C16 N5 120.0 . . ? C17 C16 C15 118.5 . . ? N5 C16 C15 121.4 . . ? C18 C17 C16 120.0 . . ? C18 C17 H17 120.0 . . ? C16 C17 H17 120.0 . . ? C17 C18 C19 120.0 . . ? C17 C18 H18 120.0 . . ? C19 C18 H18 120.0 . . ? C20 C19 C18 120.0 . . ? C20 C19 H19 120.0 . . ? C18 C19 H19 120.0 . . ? N6 C20 C19 121.1(14) . . ? N6 C20 N5 118.7(13) . . ? C19 C20 N5 120.0 . . ? N6 C21 N7 112.1(17) . . ? N6 C21 S2 127(3) . . ? N7 C21 S2 121(2) . . ? O2 C22 N7 122(2) . . ? O2 C22 C23 121.5(17) . . ? N7 C22 C23 115.9(11) . . ? C24 C23 C28 120.0 . . ? C24 C23 C22 122.6 . . ? C28 C23 C22 117.4 . . ? C25 C24 C23 120.0 . . ? C25 C24 H24 120.0 . . ? C23 C24 H24 120.0 . . ? C24 C25 C26 120.0 . . ? C24 C25 H25 120.0 . . ? C26 C25 H25 120.0 . . ? C27 C26 C25 120.0 . . ? C27 C26 H26 120.0 . . ? C25 C26 H26 120.0 . . ? C28 C27 C26 120.0 . . ? C28 C27 H27 120.0 . . ? C26 C27 H27 120.0 . . ? C27 C28 C23 120.0 . . ? C27 C28 H28 120.0 . . ? C23 C28 H28 120.0 . . ? C30 C29 N1 111(2) . . ? C30 C29 H29A 109.5 . . ? N1 C29 H29A 109.5 . . ? C30 C29 H29B 109.5 . . ? N1 C29 H29B 109.5 . . ? H29A C29 H29B 108.0 . . ? C20 N6 C21 131(3) . . ? C20 N6 H6 114.4 . . ? C21 N6 H6 114.4 . . ? C22 N7 C21 132.5(17) . . ? C22 N7 H7 113.8 . . ? C21 N7 H7 113.8 . . ? C34 N8 C30 120.0 . . ? C34 N8 Mn1 123.1(4) . . ? C30 N8 Mn1 116.9(4) . . ? N8 C30 C31 120.0 . . ? N8 C30 C29 114.5(16) . . ? C31 C30 C29 125.0(15) . . ? C32 C31 C30 120.0 . . ? C32 C31 H31 120.0 . . ? C30 C31 H31 120.0 . . ? C31 C32 C33 120.0 . . ? C31 C32 H32 120.0 . . ? C33 C32 H32 120.0 . . ? C32 C33 C34 120.0 . . ? C32 C33 H33 120.0 . . ? C34 C33 H33 120.0 . . ? N8 C34 C33 120.0 . . ? N8 C34 H34 120.0 . . ? C33 C34 H34 120.0 . . ? Cl1 O3 Mn1 128.2(10) . . ? C7 S1 Mn1 100.7(16) . . ? C21 S2 Mn1 98.9(13) . . ? N2 Mn1 N8 104.2(5) . . ? N2 Mn1 N5 117.7(6) . . ? N8 Mn1 N5 116.5(6) . . ? N2 Mn1 N1 74.9(5) . . ? N8 Mn1 N1 72.3(6) . . ? N5 Mn1 N1 75.2(5) . . ? N2 Mn1 O3 79.6(6) . . ? N8 Mn1 O3 166.3(6) . . ? N5 Mn1 O3 71.7(5) . . ? N1 Mn1 O3 121.3(5) . . ? N2 Mn1 S1 75.8(5) . . ? N8 Mn1 S1 83.8(6) . . ? N5 Mn1 S1 148.7(6) . . ? N1 Mn1 S1 135.8(6) . . ? O3 Mn1 S1 84.4(5) . . ? N2 Mn1 S2 155.9(5) . . ? N8 Mn1 S2 79.9(5) . . ? N5 Mn1 S2 79.5(5) . . ? N1 Mn1 S2 128.0(5) . . ? O3 Mn1 S2 91.4(5) . . ? S1 Mn1 S2 81.2(5) . . ? O4 Cl1 O5 109.8(8) . . ? O4 Cl1 O6 109.6(8) . . ? O5 Cl1 O6 109.5(8) . . ? O4 Cl1 O3 109.7(8) . . ? O5 Cl1 O3 109.2(8) . . ? O6 Cl1 O3 109.1(7) . . ? O9 Cl2 O7 109.7(8) . . ? O9 Cl2 O8 109.6(8) . . ? O7 Cl2 O8 109.5(8) . . ? O9 Cl2 O10 109.4(8) . . ? O7 Cl2 O10 109.4(8) . . ? O8 Cl2 O10 109.3(8) . . ? _diffrn_measured_fraction_theta_max 0.858 _diffrn_reflns_theta_full 19.30 _diffrn_measured_fraction_theta_full 0.858 _refine_diff_density_max 1.081 _refine_diff_density_min -0.961 _refine_diff_density_rms 0.208