# Electronic Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_3a #TrackingRef '19484_web_deposit_cif_file_0_KlausHarms_1366045723.3a-etj088rkf.cif' #data_etj088rkf _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C73 H84 Cl10 N16 S10 Sn6' _chemical_formula_weight 2572.80 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' Cl Cl 0.1484 0.1585 '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' Sn Sn -0.6537 1.4246 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclini _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.9249(7) _cell_length_b 15.2293(12) _cell_length_c 17.0702(14) _cell_angle_alpha 78.062(6) _cell_angle_beta 71.424(6) _cell_angle_gamma 69.028(6) _cell_volume 2499.9(3) _cell_formula_units_Z 1 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9895 _cell_measurement_theta_min 1.5 _cell_measurement_theta_max 25 _exptl_crystal_description plate _exptl_crystal_colour clourless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.709 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1264 _exptl_absorpt_coefficient_mu 1.999 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6906 _exptl_absorpt_correction_T_max 0.9067 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 'STOE IPDS 2T' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17491 _diffrn_reflns_av_R_equivalents 0.0476 _diffrn_reflns_av_sigmaI/netI 0.0648 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.44 _diffrn_reflns_theta_max 25.50 _reflns_number_total 9159 _reflns_number_gt 6879 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'STOE X-AREA' _computing_cell_refinement 'STOE X-AREA' _computing_data_reduction 'STOE X-AREA' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'DIAMOND (Crystal Impact)' _computing_publication_material ? _refine_special_details ; Pseudo merohedral twin TWIN 1 0 0 1 -1 0 1 0 -1 BASF 0.36(4) 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^)+(0.0793P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0036(4) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 9159 _refine_ls_number_parameters 579 _refine_ls_number_restraints 102 _refine_ls_R_factor_all 0.0699 _refine_ls_R_factor_gt 0.0512 _refine_ls_wR_factor_ref 0.1293 _refine_ls_wR_factor_gt 0.1209 _refine_ls_goodness_of_fit_ref 0.950 _refine_ls_restrained_S_all 0.954 _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 -0.0533(11) 0.0946(8) 0.3580(7) 0.069(3) Uani 1 1 d . . . C2 C -0.0810(11) 0.1103(9) 0.2729(7) 0.073(3) Uani 1 1 d . . . H2A H -0.1665 0.0969 0.2805 0.087 Uiso 1 1 calc R . . H2B H -0.0959 0.1779 0.2518 0.087 Uiso 1 1 calc R . . C3 C 0.0282(12) 0.0521(7) 0.2079(7) 0.067(3) Uani 1 1 d . . . C6 C 0.2986(10) -0.1166(7) 0.1726(6) 0.053(2) Uani 1 1 d . . . C7 C 0.2233(11) -0.1727(8) 0.2397(6) 0.061(3) Uani 1 1 d . . . C9 C 0.0274(12) -0.2146(8) 0.2917(8) 0.073(3) Uani 1 1 d . . . H9 H -0.0576 -0.2133 0.2871 0.088 Uiso 1 1 calc R . . C10 C 0.0703(15) -0.2642(8) 0.3597(7) 0.079(4) Uani 1 1 d . . . H10 H 0.0152 -0.2965 0.4013 0.094 Uiso 1 1 calc R . . C11 C 0.1898(14) -0.2675(8) 0.3680(8) 0.077(3) Uani 1 1 d . . . H11 H 0.2180 -0.3020 0.4158 0.092 Uiso 1 1 calc R . . C12 C 0.2731(13) -0.2215(8) 0.3086(7) 0.073(3) Uani 1 1 d . . . H12 H 0.3577 -0.2229 0.3138 0.087 Uiso 1 1 calc R . . C13 C 0.4257(11) -0.1667(7) 0.1117(6) 0.063(3) Uani 1 1 d . . . C15 C 0.5594(13) -0.3070(8) 0.0601(8) 0.079(3) Uani 1 1 d . . . H15 H 0.5780 -0.3731 0.0609 0.095 Uiso 1 1 calc R . . C16 C 0.6447(13) -0.2642(8) 0.0023(7) 0.074(3) Uani 1 1 d . . . H16 H 0.7202 -0.2989 -0.0376 0.089 Uiso 1 1 calc R . . C17 C 0.6180(13) -0.1691(9) 0.0035(8) 0.085(4) Uani 1 1 d . . . H17 H 0.6783 -0.1382 -0.0348 0.102 Uiso 1 1 calc R . . C18 C 0.5101(13) -0.1197(8) 0.0567(7) 0.080(4) Uani 1 1 d . . . H18 H 0.4915 -0.0539 0.0570 0.096 Uiso 1 1 calc R . . C19 C -0.1551(13) 0.1704(10) 0.4122(8) 0.088(4) Uani 1 1 d . . . H19A H -0.1362 0.1584 0.4665 0.132 Uiso 1 1 calc R . . H19B H -0.2473 0.1694 0.4196 0.132 Uiso 1 1 calc R . . H19C H -0.1476 0.2324 0.3856 0.132 Uiso 1 1 calc R . . C20 C -0.0535(12) -0.0052(9) 0.4019(7) 0.075(3) Uani 1 1 d . . . H20A H 0.0120 -0.0531 0.3654 0.113 Uiso 1 1 calc R . . H20B H -0.1447 -0.0105 0.4141 0.113 Uiso 1 1 calc R . . H20C H -0.0278 -0.0152 0.4538 0.113 Uiso 1 1 calc R . . C21 C -0.0031(14) 0.0381(10) 0.1349(8) 0.087(4) Uani 1 1 d . . . H21A H 0.0789 -0.0022 0.0995 0.130 Uiso 1 1 calc R . . H21B H -0.0349 0.0995 0.1035 0.130 Uiso 1 1 calc R . . H21C H -0.0744 0.0078 0.1529 0.130 Uiso 1 1 calc R . . C22 C 0.1717(14) 0.4298(8) 0.3407(9) 0.086(4) Uani 1 1 d . . . C23 C 0.1720(18) 0.4863(8) 0.2532(8) 0.119(6) Uani 1 1 d . . . H23A H 0.0972 0.4817 0.2350 0.143 Uiso 1 1 calc R . . H23B H 0.1539 0.5539 0.2576 0.143 Uiso 1 1 calc R . . C24 C 0.3040(19) 0.4515(9) 0.1884(9) 0.112(6) Uani 1 1 d . . . C27 C 0.6156(17) 0.3453(8) 0.1414(8) 0.083(3) Uani 1 1 d . . . C28 C 0.7378(14) 0.3007(7) 0.0816(7) 0.077(4) Uani 1 1 d . . . C30 C 0.867(2) 0.2190(12) -0.0361(9) 0.116(7) Uani 1 1 d . . . H30 H 0.8734 0.1865 -0.0798 0.139 Uiso 1 1 calc R . . C31 C 0.976(3) 0.2310(13) -0.0279(15) 0.153(11) Uani 1 1 d . . . H31 H 1.0617 0.2080 -0.0663 0.183 Uiso 1 1 calc R . . C32 C 0.964(2) 0.2776(15) 0.0374(19) 0.181(12) Uani 1 1 d . . . H32 H 1.0439 0.2837 0.0429 0.217 Uiso 1 1 calc R . . N29 N 0.8490(15) 0.3136(10) 0.0917(11) 0.133(6) Uani 1 1 d . . . C34 C 0.6084(14) 0.4026(8) 0.2033(9) 0.092(4) Uani 1 1 d D . . N35 N 0.6539(12) 0.3662(10) 0.2751(11) 0.125(5) Uani 1 1 d D A . C36 C 0.6501(19) 0.4186(13) 0.3351(13) 0.136(7) Uani 1 1 d D . . C37 C 0.579(3) 0.5144(14) 0.3203(16) 0.132(9) Uani 0.73 1 d PDU A 1 H37 H 0.5578 0.5560 0.3606 0.158 Uiso 0.73 1 calc PR A 1 C38 C 0.541(3) 0.5480(13) 0.2510(15) 0.116(7) Uani 0.73 1 d PDU A 1 H38 H 0.5091 0.6148 0.2396 0.139 Uiso 0.73 1 calc PR A 1 C39 C 0.5420(17) 0.4973(9) 0.1956(10) 0.076(5) Uani 0.73 1 d PDU A 1 H39 H 0.4983 0.5261 0.1525 0.091 Uiso 0.73 1 calc PR A 1 C40 C 0.2497(15) 0.4550(9) 0.3858(11) 0.105(5) Uani 1 1 d . . . H40A H 0.3431 0.4466 0.3512 0.158 Uiso 1 1 calc R . . H40B H 0.2512 0.4138 0.4381 0.158 Uiso 1 1 calc R . . H40C H 0.2058 0.5210 0.3977 0.158 Uiso 1 1 calc R . . C41 C 0.0230(13) 0.4401(9) 0.3915(9) 0.096(4) Uani 1 1 d . . . H41A H -0.0236 0.4239 0.3588 0.144 Uiso 1 1 calc R . . H41B H -0.0239 0.5055 0.4048 0.144 Uiso 1 1 calc R . . H41C H 0.0223 0.3975 0.4431 0.144 Uiso 1 1 calc R . . C42 C 0.330(2) 0.5197(11) 0.1066(11) 0.150(9) Uani 1 1 d . . . H42A H 0.4186 0.4903 0.0695 0.226 Uiso 1 1 calc R . . H42B H 0.3279 0.5795 0.1204 0.226 Uiso 1 1 calc R . . H42C H 0.2583 0.5318 0.0789 0.226 Uiso 1 1 calc R . . C200 C 0.4296(13) 0.2697(8) 0.5594(10) 0.127(7) Uani 1 1 d D . . H20D H 0.4712 0.2150 0.5958 0.153 Uiso 1 1 calc R . . H20E H 0.4312 0.2456 0.5094 0.153 Uiso 1 1 calc R . . S5 S 0.6356(2) -0.05646(18) 0.42141(15) 0.0546(6) Uani 1 1 d . . . Cl20 Cl 0.2578(7) 0.3252(4) 0.6131(6) 0.185(3) Uani 1 1 d D . . Cl21 Cl 0.5216(7) 0.3433(7) 0.5309(5) 0.194(3) Uani 1 1 d D . . N4 N 0.1465(9) 0.0215(6) 0.2219(5) 0.060(2) Uani 1 1 d . . . N5 N 0.2584(9) -0.0258(6) 0.1615(5) 0.062(2) Uani 1 1 d . . . N8 N 0.1014(10) -0.1672(7) 0.2309(6) 0.072(2) Uani 1 1 d . . . N14 N 0.4507(10) -0.2601(6) 0.1158(6) 0.071(2) Uani 1 1 d . . . N25 N 0.3867(11) 0.3709(6) 0.2003(6) 0.080(3) Uani 1 1 d . A . N26 N 0.5058(13) 0.3351(7) 0.1390(6) 0.084(3) Uani 1 1 d . . . C33 C 0.7441(15) 0.2551(8) 0.0209(8) 0.091(4) Uani 1 1 d . . . H33 H 0.6639 0.2473 0.0167 0.109 Uiso 1 1 calc R . . S1 S 0.2153(3) 0.2171(2) 0.21933(16) 0.0672(7) Uani 1 1 d . A . S2 S 0.1543(3) 0.19045(17) 0.44003(15) 0.0548(6) Uani 1 1 d . A . S4 S 0.4915(3) 0.18648(18) 0.34053(17) 0.0596(6) Uani 1 1 d . A . S3 S 0.3363(2) -0.02961(16) 0.36212(15) 0.0527(6) Uani 1 1 d . A . Sn1 Sn 0.14993(7) 0.10200(5) 0.33117(4) 0.05363(19) Uani 1 1 d . . . Sn2 Sn 0.27446(7) 0.28032(5) 0.31655(5) 0.0595(2) Uani 1 1 d . . . Sn3 Sn 0.40688(6) 0.06239(4) 0.43076(4) 0.04901(18) Uani 1 1 d . . . C37A C 0.687(6) 0.499(3) 0.291(2) 0.111(13) Uani 0.27 1 d PDU A 2 H37A H 0.7072 0.5377 0.3191 0.133 Uiso 0.27 1 calc PR A 2 C38A C 0.695(6) 0.522(3) 0.210(2) 0.122(14) Uani 0.27 1 d PDU A 2 H38A H 0.7260 0.5746 0.1831 0.146 Uiso 0.27 1 calc PR A 2 C39A C 0.663(5) 0.477(2) 0.1635(18) 0.072(9) Uani 0.27 1 d PDU A 2 H39A H 0.6765 0.4944 0.1054 0.087 Uiso 0.27 1 calc PR A 2 Cl31 Cl 0.3027(7) -0.0196(6) 0.9116(4) 0.173(3) Uani 1 1 d D . . Cl30 Cl 0.3159(7) 0.1420(7) 0.7907(4) 0.211(4) Uani 1 1 d D . . C300 C 0.388(2) 0.0165(12) 0.8142(9) 0.189(12) Uani 1 1 d D . . H30A H 0.3812 -0.0173 0.7727 0.226 Uiso 1 1 calc R . . H30B H 0.4850 0.0008 0.8113 0.226 Uiso 1 1 calc R . . C100 C 0.102(4) 0.4823(18) 0.8857(16) 0.149(16) Uani 0.50 1 d PD . . H10A H 0.1862 0.4936 0.8854 0.179 Uiso 0.40 1 calc PR B 1 H10B H 0.0576 0.4632 0.9438 0.179 Uiso 0.40 1 calc PR B 1 H10C H 0.1258 0.4905 0.8248 0.223 Uiso 0.20 1 calc PR B 2 H10D H 0.1342 0.4149 0.9050 0.223 Uiso 0.20 1 calc PR B 2 H10E H 0.1459 0.5167 0.9050 0.223 Uiso 0.20 1 calc PR B 2 H10F H 0.0572 0.5047 0.8407 0.223 Uiso 0.20 1 calc PR B 3 H10G H 0.1574 0.4157 0.8818 0.223 Uiso 0.20 1 calc PR B 3 H10H H 0.1611 0.5200 0.8808 0.223 Uiso 0.20 1 calc PR B 3 Cl10 Cl 0.1434(12) 0.3954(8) 0.8283(8) 0.117(3) Uani 0.40 1 d PD C 1 Cl12 Cl -0.066(2) 0.5242(16) 0.9234(19) 0.127(9) Uani 0.20 1 d PD C 2 Cl13 Cl -0.015(4) 0.493(3) 0.9774(15) 0.151(16) Uani 0.20 1 d PD . 3 Cl15 Cl -0.002(3) 0.582(2) 0.851(3) 0.21(2) Uani 0.20 1 d PD C 1 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.059(6) 0.083(7) 0.069(6) -0.005(6) -0.025(5) -0.021(5) C2 0.050(6) 0.081(8) 0.079(7) -0.014(6) -0.017(5) -0.009(5) C3 0.072(7) 0.060(6) 0.067(6) 0.006(5) -0.024(6) -0.020(6) C6 0.059(6) 0.057(5) 0.049(5) 0.004(4) -0.020(4) -0.024(5) C7 0.063(6) 0.063(6) 0.062(6) -0.004(5) -0.019(5) -0.023(5) C9 0.065(7) 0.064(6) 0.084(8) -0.014(6) -0.002(6) -0.026(6) C10 0.104(10) 0.055(6) 0.065(7) -0.010(5) 0.007(7) -0.034(6) C11 0.097(10) 0.065(7) 0.069(7) -0.009(6) -0.018(7) -0.029(7) C12 0.083(8) 0.059(6) 0.075(7) 0.010(5) -0.017(6) -0.034(6) C13 0.063(6) 0.057(6) 0.063(6) 0.002(5) -0.017(5) -0.015(5) C15 0.079(8) 0.056(6) 0.088(8) -0.008(6) -0.010(7) -0.013(6) C16 0.074(7) 0.070(7) 0.070(7) -0.004(6) -0.006(6) -0.026(6) C17 0.077(8) 0.082(8) 0.088(8) -0.003(7) 0.001(7) -0.040(7) C18 0.096(9) 0.053(6) 0.067(7) 0.000(5) 0.013(6) -0.029(6) C19 0.063(7) 0.114(10) 0.082(7) -0.032(7) -0.013(6) -0.016(7) C20 0.056(6) 0.091(8) 0.083(7) 0.002(6) -0.016(6) -0.036(6) C21 0.074(8) 0.094(9) 0.081(8) 0.004(7) -0.034(7) -0.008(7) C22 0.074(8) 0.055(6) 0.100(9) -0.008(6) -0.001(7) -0.008(6) C23 0.145(13) 0.045(6) 0.095(9) 0.038(6) -0.004(9) 0.006(7) C24 0.133(13) 0.057(7) 0.097(9) 0.017(7) 0.005(10) -0.020(8) C27 0.107(11) 0.051(6) 0.089(8) 0.012(6) -0.023(8) -0.035(7) C28 0.087(8) 0.041(5) 0.074(7) 0.003(5) 0.009(6) -0.017(6) C30 0.119(13) 0.102(11) 0.059(8) 0.003(7) -0.013(9) 0.028(11) C31 0.130(18) 0.084(11) 0.149(17) 0.008(11) 0.060(15) -0.020(12) C32 0.090(13) 0.119(15) 0.30(3) -0.070(19) 0.056(17) -0.056(11) N29 0.099(10) 0.104(10) 0.191(15) -0.044(10) 0.023(10) -0.064(8) C34 0.106(10) 0.049(6) 0.086(8) 0.002(6) 0.001(8) -0.014(6) N35 0.085(8) 0.103(10) 0.177(14) -0.011(10) -0.024(9) -0.029(7) C36 0.18(2) 0.093(12) 0.155(16) -0.047(12) -0.044(14) -0.049(12) C37 0.159(19) 0.072(12) 0.148(18) -0.032(13) 0.021(17) -0.060(13) C38 0.145(15) 0.049(9) 0.129(15) -0.023(10) 0.014(14) -0.038(10) C39 0.083(10) 0.034(7) 0.093(10) -0.002(7) -0.003(9) -0.018(7) C40 0.086(9) 0.056(7) 0.163(14) -0.039(8) -0.002(9) -0.022(7) C41 0.075(8) 0.062(7) 0.107(10) -0.011(7) 0.010(7) 0.000(6) C42 0.135(14) 0.088(10) 0.141(14) 0.066(10) 0.022(12) -0.028(10) C200 0.190(19) 0.047(7) 0.121(11) -0.033(7) -0.057(13) 0.017(10) S5 0.0449(12) 0.0569(13) 0.0587(13) -0.0122(11) -0.0090(10) -0.0130(10) Cl20 0.138(5) 0.107(4) 0.300(9) 0.001(5) -0.049(5) -0.048(3) Cl21 0.139(5) 0.241(8) 0.199(6) -0.045(6) -0.033(5) -0.053(5) N4 0.055(5) 0.051(5) 0.064(5) -0.004(4) -0.014(4) -0.009(4) N5 0.061(5) 0.062(5) 0.058(5) 0.000(4) -0.018(4) -0.017(4) N8 0.071(6) 0.069(6) 0.078(6) 0.002(4) -0.021(5) -0.028(5) N14 0.074(6) 0.051(5) 0.082(6) 0.000(4) -0.014(5) -0.022(4) N25 0.084(7) 0.052(5) 0.076(6) 0.006(4) 0.010(5) -0.022(5) N26 0.110(9) 0.053(5) 0.069(6) -0.009(4) 0.008(6) -0.031(5) C33 0.094(9) 0.062(7) 0.073(7) 0.009(6) -0.018(7) 0.014(7) S1 0.0720(17) 0.0620(15) 0.0597(14) 0.0085(12) -0.0137(13) -0.0237(14) S2 0.0530(13) 0.0461(12) 0.0563(13) -0.0030(10) -0.0075(11) -0.0126(10) S4 0.0545(14) 0.0481(13) 0.0718(16) -0.0030(11) -0.0076(12) -0.0210(11) S3 0.0489(13) 0.0483(12) 0.0638(14) -0.0075(11) -0.0145(11) -0.0181(10) Sn1 0.0469(4) 0.0532(4) 0.0569(4) -0.0005(3) -0.0118(3) -0.0160(3) Sn2 0.0590(4) 0.0420(3) 0.0654(4) -0.0004(3) -0.0069(3) -0.0132(3) Sn3 0.0467(4) 0.0432(3) 0.0571(4) -0.0054(3) -0.0112(3) -0.0164(3) C37A 0.14(3) 0.11(2) 0.11(2) -0.07(2) -0.07(2) 0.00(2) C38A 0.14(2) 0.08(2) 0.13(2) -0.02(2) -0.02(2) -0.02(2) C39A 0.11(2) 0.038(16) 0.09(2) -0.011(15) -0.055(19) -0.020(17) Cl31 0.151(5) 0.252(8) 0.154(5) -0.031(5) -0.020(4) -0.120(5) Cl30 0.140(5) 0.295(10) 0.122(4) -0.050(5) -0.038(4) 0.039(6) C300 0.16(2) 0.29(4) 0.095(13) -0.067(18) 0.023(14) -0.08(2) C100 0.17(4) 0.09(2) 0.19(4) -0.03(3) -0.07(3) -0.01(2) Cl10 0.118(8) 0.087(6) 0.147(9) -0.018(6) -0.029(7) -0.036(6) Cl12 0.17(3) 0.073(12) 0.16(2) -0.004(14) -0.08(2) -0.031(15) Cl13 0.22(3) 0.12(2) 0.10(3) -0.03(2) 0.03(3) -0.09(2) Cl15 0.12(2) 0.16(3) 0.39(7) -0.10(4) -0.13(3) -0.01(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C19 1.514(16) . ? C1 C2 1.530(16) . ? C1 C20 1.550(16) . ? C1 Sn1 2.159(11) . ? C2 C3 1.499(15) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 N4 1.290(15) . ? C3 C21 1.465(17) . ? C6 N5 1.285(13) . ? C6 C7 1.490(14) . ? C6 C13 1.497(14) . ? C7 N8 1.359(15) . ? C7 C12 1.409(16) . ? C9 N8 1.351(14) . ? C9 C10 1.367(18) . ? C9 H9 0.9500 . ? C10 C11 1.340(19) . ? C10 H10 0.9500 . ? C11 C12 1.386(16) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? C13 N14 1.340(13) . ? C13 C18 1.372(15) . ? C15 N14 1.334(14) . ? C15 C16 1.361(16) . ? C15 H15 0.9500 . ? C16 C17 1.375(17) . ? C16 H16 0.9500 . ? C17 C18 1.322(16) . ? C17 H17 0.9500 . ? C18 H18 0.9500 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 C40 1.50(2) . ? C22 C41 1.547(18) . ? C22 C23 1.562(18) . ? C22 Sn2 2.208(11) . ? C23 C24 1.50(2) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 N25 1.259(17) . ? C24 C42 1.569(17) . ? C27 N26 1.278(19) . ? C27 C28 1.434(18) . ? C27 C34 1.47(2) . ? C28 C33 1.334(19) . ? C28 N29 1.37(2) . ? C30 C31 1.31(3) . ? C30 C33 1.39(2) . ? C30 H30 0.9500 . ? C31 C32 1.39(3) . ? C31 H31 0.9500 . ? C32 N29 1.31(2) . ? C32 H32 0.9500 . ? C34 C39 1.363(17) . ? C34 N35 1.40(2) . ? C34 C39A 1.42(2) . ? N35 C36 1.41(2) . ? C36 C37 1.40(3) . ? C36 C37A 1.42(3) . ? C37 C38 1.32(3) . ? C37 H37 0.9500 . ? C38 C39 1.33(3) . ? C38 H38 0.9500 . ? C39 H39 0.9500 . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C200 Cl21 1.664(12) . ? C200 Cl20 1.779(12) . ? C200 H20D 0.9900 . ? C200 H20E 0.9900 . ? S5 Sn3 2.404(3) 2_656 ? S5 Sn3 2.485(2) . ? N4 N5 1.397(12) . ? N4 Sn1 2.450(9) . ? N25 N26 1.394(14) . ? N25 Sn2 2.424(8) . ? C33 H33 0.9500 . ? S1 Sn1 2.423(3) . ? S1 Sn2 2.427(3) . ? S2 Sn2 2.523(2) . ? S2 Sn1 2.532(3) . ? S2 Sn3 2.727(3) . ? S4 Sn2 2.405(3) . ? S4 Sn3 2.437(3) . ? S3 Sn1 2.402(3) . ? S3 Sn3 2.441(2) . ? Sn3 S5 2.404(3) 2_656 ? C37A C38A 1.33(4) . ? C37A H37A 0.9500 . ? C38A C39A 1.34(3) . ? C38A H38A 0.9500 . ? C39A H39A 0.9500 . ? Cl31 C300 1.711(13) . ? Cl30 C300 1.801(15) . ? C300 H30A 0.9900 . ? C300 H30B 0.9900 . ? C100 Cl10 1.66(2) . ? C100 Cl15 1.66(3) . ? C100 Cl12 1.66(3) . ? C100 Cl13 1.67(2) . ? C100 H10A 0.9900 . ? C100 H10B 0.9900 . ? C100 H10C 0.9800 . ? C100 H10D 0.9800 . ? C100 H10E 0.9800 . ? C100 H10F 0.9800 . ? C100 H10G 0.9800 . ? C100 H10H 0.9800 . ? Cl13 Cl13 1.01(7) 2_567 ? 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 C19 C1 C2 111.0(10) . . ? C19 C1 C20 110.8(10) . . ? C2 C1 C20 111.3(10) . . ? C19 C1 Sn1 110.8(8) . . ? C2 C1 Sn1 104.8(7) . . ? C20 C1 Sn1 108.0(7) . . ? C3 C2 C1 116.0(9) . . ? C3 C2 H2A 108.3 . . ? C1 C2 H2A 108.3 . . ? C3 C2 H2B 108.3 . . ? C1 C2 H2B 108.3 . . ? H2A C2 H2B 107.4 . . ? N4 C3 C21 126.1(11) . . ? N4 C3 C2 113.6(10) . . ? C21 C3 C2 120.2(11) . . ? N5 C6 C7 123.6(9) . . ? N5 C6 C13 116.8(8) . . ? C7 C6 C13 119.6(9) . . ? N8 C7 C12 124.1(10) . . ? N8 C7 C6 114.3(9) . . ? C12 C7 C6 121.4(10) . . ? N8 C9 C10 122.4(12) . . ? N8 C9 H9 118.8 . . ? C10 C9 H9 118.8 . . ? C11 C10 C9 120.2(11) . . ? C11 C10 H10 119.9 . . ? C9 C10 H10 119.9 . . ? C10 C11 C12 121.5(13) . . ? C10 C11 H11 119.3 . . ? C12 C11 H11 119.3 . . ? C11 C12 C7 115.2(12) . . ? C11 C12 H12 122.4 . . ? C7 C12 H12 122.4 . . ? N14 C13 C18 123.2(10) . . ? N14 C13 C6 114.9(9) . . ? C18 C13 C6 121.9(9) . . ? N14 C15 C16 122.6(11) . . ? N14 C15 H15 118.7 . . ? C16 C15 H15 118.7 . . ? C15 C16 C17 117.8(11) . . ? C15 C16 H16 121.1 . . ? C17 C16 H16 121.1 . . ? C18 C17 C16 121.3(11) . . ? C18 C17 H17 119.3 . . ? C16 C17 H17 119.3 . . ? C17 C18 C13 117.9(11) . . ? C17 C18 H18 121.1 . . ? C13 C18 H18 121.1 . . ? C1 C19 H19A 109.5 . . ? C1 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C1 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C1 C20 H20A 109.5 . . ? C1 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C1 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C3 C21 H21A 109.5 . . ? C3 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C3 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C40 C22 C41 112.9(11) . . ? C40 C22 C23 113.7(13) . . ? C41 C22 C23 109.0(13) . . ? C40 C22 Sn2 107.7(9) . . ? C41 C22 Sn2 107.9(8) . . ? C23 C22 Sn2 105.2(8) . . ? C24 C23 C22 113.1(12) . . ? C24 C23 H23A 109.0 . . ? C22 C23 H23A 109.0 . . ? C24 C23 H23B 109.0 . . ? C22 C23 H23B 109.0 . . ? H23A C23 H23B 107.8 . . ? N25 C24 C23 120.4(11) . . ? N25 C24 C42 123.1(13) . . ? C23 C24 C42 116.5(12) . . ? N26 C27 C28 116.7(13) . . ? N26 C27 C34 118.6(13) . . ? C28 C27 C34 124.7(15) . . ? C33 C28 N29 123.1(13) . . ? C33 C28 C27 125.3(15) . . ? N29 C28 C27 111.6(13) . . ? C31 C30 C33 117.9(19) . . ? C31 C30 H30 121.0 . . ? C33 C30 H30 121.0 . . ? C30 C31 C32 119.5(18) . . ? C30 C31 H31 120.2 . . ? C32 C31 H31 120.2 . . ? N29 C32 C31 124(2) . . ? N29 C32 H32 117.8 . . ? C31 C32 H32 117.8 . . ? C32 N29 C28 115.0(18) . . ? C39 C34 N35 116.2(15) . . ? C39 C34 C39A 51.5(19) . . ? N35 C34 C39A 107.3(17) . . ? C39 C34 C27 118.7(15) . . ? N35 C34 C27 124.8(12) . . ? C39A C34 C27 110.2(16) . . ? C34 N35 C36 126.5(15) . . ? C37 C36 N35 111(2) . . ? C37 C36 C37A 45(2) . . ? N35 C36 C37A 106.3(19) . . ? C38 C37 C36 121(2) . . ? C38 C37 H37 119.5 . . ? C36 C37 H37 119.5 . . ? C37 C38 C39 126.4(18) . . ? C37 C38 H38 116.8 . . ? C39 C38 H38 116.8 . . ? C38 C39 C34 117.4(18) . . ? C38 C39 H39 121.3 . . ? C34 C39 H39 121.3 . . ? C22 C40 H40A 109.5 . . ? C22 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C22 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? C22 C41 H41A 109.5 . . ? C22 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C22 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C24 C42 H42A 109.5 . . ? C24 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C24 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? Cl21 C200 Cl20 112.3(7) . . ? Cl21 C200 H20D 109.1 . . ? Cl20 C200 H20D 109.1 . . ? Cl21 C200 H20E 109.1 . . ? Cl20 C200 H20E 109.1 . . ? H20D C200 H20E 107.9 . . ? Sn3 S5 Sn3 89.15(8) 2_656 . ? C3 N4 N5 118.6(9) . . ? C3 N4 Sn1 111.1(7) . . ? N5 N4 Sn1 127.0(7) . . ? C6 N5 N4 117.0(8) . . ? C9 N8 C7 116.4(10) . . ? C15 N14 C13 117.1(9) . . ? C24 N25 N26 121.3(10) . . ? C24 N25 Sn2 109.4(9) . . ? N26 N25 Sn2 126.6(7) . . ? C27 N26 N25 118.6(12) . . ? C28 C33 C30 120.1(18) . . ? C28 C33 H33 120.0 . . ? C30 C33 H33 120.0 . . ? Sn1 S1 Sn2 88.42(9) . . ? Sn2 S2 Sn1 83.98(8) . . ? Sn2 S2 Sn3 84.94(7) . . ? Sn1 S2 Sn3 84.56(7) . . ? Sn2 S4 Sn3 94.27(9) . . ? Sn1 S3 Sn3 93.97(8) . . ? C1 Sn1 S3 123.0(3) . . ? C1 Sn1 S1 117.5(3) . . ? S3 Sn1 S1 114.77(10) . . ? C1 Sn1 N4 72.6(4) . . ? S3 Sn1 N4 90.5(2) . . ? S1 Sn1 N4 85.6(2) . . ? C1 Sn1 S2 108.2(3) . . ? S3 Sn1 S2 90.78(8) . . ? S1 Sn1 S2 92.27(9) . . ? N4 Sn1 S2 177.8(2) . . ? C22 Sn2 S4 124.5(4) . . ? C22 Sn2 N25 74.3(4) . . ? S4 Sn2 N25 89.7(3) . . ? C22 Sn2 S1 119.6(4) . . ? S4 Sn2 S1 112.69(10) . . ? N25 Sn2 S1 88.9(3) . . ? C22 Sn2 S2 104.0(3) . . ? S4 Sn2 S2 90.95(9) . . ? N25 Sn2 S2 178.2(2) . . ? S1 Sn2 S2 92.37(9) . . ? S5 Sn3 S4 119.05(9) 2_656 . ? S5 Sn3 S3 125.05(8) 2_656 . ? S4 Sn3 S3 115.05(9) . . ? S5 Sn3 S5 90.85(8) 2_656 . ? S4 Sn3 S5 95.05(9) . . ? S3 Sn3 S5 93.46(8) . . ? S5 Sn3 S2 89.63(8) 2_656 . ? S4 Sn3 S2 85.58(8) . . ? S3 Sn3 S2 85.46(8) . . ? S5 Sn3 S2 178.90(9) . . ? C38A C37A C36 122(3) . . ? C38A C37A H37A 119.2 . . ? C36 C37A H37A 119.2 . . ? C37A C38A C39A 125(3) . . ? C37A C38A H38A 117.4 . . ? C39A C38A H38A 117.4 . . ? C38A C39A C34 118(2) . . ? C38A C39A H39A 120.8 . . ? C34 C39A H39A 120.8 . . ? Cl31 C300 Cl30 110.2(11) . . ? Cl31 C300 H30A 109.6 . . ? Cl30 C300 H30A 109.6 . . ? Cl31 C300 H30B 109.6 . . ? Cl30 C300 H30B 109.6 . . ? H30A C300 H30B 108.1 . . ? Cl10 C100 Cl15 112(2) . . ? Cl10 C100 Cl12 111(3) . . ? Cl15 C100 Cl12 53(2) . . ? Cl10 C100 Cl13 124(3) . . ? Cl15 C100 Cl13 87(3) . . ? Cl12 C100 Cl13 40.5(18) . . ? Cl10 C100 H10A 109.2 . . ? Cl15 C100 H10A 109.2 . . ? Cl12 C100 H10A 140.2 . . ? Cl13 C100 H10A 113.6 . . ? Cl10 C100 H10B 109.2 . . ? Cl15 C100 H10B 109.2 . . ? Cl12 C100 H10B 59.3 . . ? Cl13 C100 H10B 22.9 . . ? H10A C100 H10B 107.9 . . ? Cl10 C100 H10C 56.5 . . ? Cl15 C100 H10C 68.8 . . ? Cl12 C100 H10C 109.5 . . ? Cl13 C100 H10C 150.0 . . ? H10A C100 H10C 91.4 . . ? H10B C100 H10C 159.7 . . ? Cl10 C100 H10D 55.6 . . ? Cl15 C100 H10D 156.8 . . ? Cl12 C100 H10D 109.5 . . ? Cl13 C100 H10D 86.2 . . ? H10A C100 H10D 93.9 . . ? H10B C100 H10D 63.9 . . ? H10C C100 H10D 109.5 . . ? Cl10 C100 H10E 139.9 . . ? Cl15 C100 H10E 92.3 . . ? Cl12 C100 H10E 109.5 . . ? Cl13 C100 H10E 87.8 . . ? H10A C100 H10E 30.7 . . ? H10B C100 H10E 90.7 . . ? H10C C100 H10E 109.5 . . ? H10D C100 H10E 109.5 . . ? Cl10 C100 H10F 70.2 . . ? Cl15 C100 H10F 41.8 . . ? Cl12 C100 H10F 69.1 . . ? Cl13 C100 H10F 109.5 . . ? H10A C100 H10F 125.2 . . ? H10B C100 H10F 124.4 . . ? H10C C100 H10F 40.5 . . ? H10D C100 H10F 121.6 . . ? H10E C100 H10F 126.4 . . ? Cl10 C100 H10G 39.3 . . ? Cl15 C100 H10G 151.3 . . ? Cl12 C100 H10G 126.6 . . ? Cl13 C100 H10G 109.5 . . ? H10A C100 H10G 86.5 . . ? H10B C100 H10G 87.3 . . ? H10C C100 H10G 87.5 . . ? H10D C100 H10G 23.4 . . ? H10E C100 H10G 111.4 . . ? H10F C100 H10G 109.5 . . ? Cl10 C100 H10H 124.0 . . ? Cl15 C100 H10H 85.8 . . ? Cl12 C100 H10H 121.4 . . ? Cl13 C100 H10H 109.5 . . ? H10A C100 H10H 23.7 . . ? H10B C100 H10H 113.8 . . ? H10C C100 H10H 86.5 . . ? H10D C100 H10H 117.4 . . ? H10E C100 H10H 23.1 . . ? H10F C100 H10H 109.5 . . ? H10G C100 H10H 109.5 . . ? Cl13 Cl13 C100 114(5) 2_567 . ? 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 C19 C1 C2 C3 168.2(11) . . . . ? C20 C1 C2 C3 -67.9(13) . . . . ? Sn1 C1 C2 C3 48.6(12) . . . . ? C1 C2 C3 N4 -22.2(15) . . . . ? C1 C2 C3 C21 160.5(11) . . . . ? N5 C6 C7 N8 67.4(13) . . . . ? C13 C6 C7 N8 -110.2(11) . . . . ? N5 C6 C7 C12 -108.7(13) . . . . ? C13 C6 C7 C12 73.8(14) . . . . ? N8 C9 C10 C11 -0.1(17) . . . . ? C9 C10 C11 C12 -0.3(18) . . . . ? C10 C11 C12 C7 -0.4(17) . . . . ? N8 C7 C12 C11 1.6(17) . . . . ? C6 C7 C12 C11 177.3(10) . . . . ? N5 C6 C13 N14 -168.4(10) . . . . ? C7 C6 C13 N14 9.4(14) . . . . ? N5 C6 C13 C18 12.4(15) . . . . ? C7 C6 C13 C18 -169.9(11) . . . . ? N14 C15 C16 C17 2(2) . . . . ? C15 C16 C17 C18 -3(2) . . . . ? C16 C17 C18 C13 1(2) . . . . ? N14 C13 C18 C17 3(2) . . . . ? C6 C13 C18 C17 -178.0(12) . . . . ? C40 C22 C23 C24 76.4(17) . . . . ? C41 C22 C23 C24 -156.8(14) . . . . ? Sn2 C22 C23 C24 -41.3(18) . . . . ? C22 C23 C24 N25 18(3) . . . . ? C22 C23 C24 C42 -163.4(17) . . . . ? N26 C27 C28 C33 4.6(16) . . . . ? C34 C27 C28 C33 -174.2(11) . . . . ? N26 C27 C28 N29 -177.9(12) . . . . ? C34 C27 C28 N29 3.2(16) . . . . ? C33 C30 C31 C32 1(3) . . . . ? C30 C31 C32 N29 -2(4) . . . . ? C31 C32 N29 C28 1(3) . . . . ? C33 C28 N29 C32 0(2) . . . . ? C27 C28 N29 C32 -177.7(16) . . . . ? N26 C27 C34 C39 -67.0(16) . . . . ? C28 C27 C34 C39 111.8(14) . . . . ? N26 C27 C34 N35 106.6(15) . . . . ? C28 C27 C34 N35 -74.6(15) . . . . ? N26 C27 C34 C39A -123(2) . . . . ? C28 C27 C34 C39A 55(2) . . . . ? C39 C34 N35 C36 -6.9(15) . . . . ? C39A C34 N35 C36 48(2) . . . . ? C27 C34 N35 C36 179.3(14) . . . . ? C34 N35 C36 C37 7.1(17) . . . . ? C34 N35 C36 C37A -41(3) . . . . ? N35 C36 C37 C38 -9(3) . . . . ? C37A C36 C37 C38 83(3) . . . . ? C36 C37 C38 C39 12(4) . . . . ? C37 C38 C39 C34 -11(3) . . . . ? N35 C34 C39 C38 8(2) . . . . ? C39A C34 C39 C38 -84(2) . . . . ? C27 C34 C39 C38 -177.9(16) . . . . ? C21 C3 N4 N5 3.2(16) . . . . ? C2 C3 N4 N5 -173.9(9) . . . . ? C21 C3 N4 Sn1 164.1(10) . . . . ? C2 C3 N4 Sn1 -13.0(11) . . . . ? C7 C6 N5 N4 7.5(14) . . . . ? C13 C6 N5 N4 -174.9(9) . . . . ? C3 N4 N5 C6 -99.2(11) . . . . ? Sn1 N4 N5 C6 103.3(9) . . . . ? C10 C9 N8 C7 1.1(16) . . . . ? C12 C7 N8 C9 -2.0(16) . . . . ? C6 C7 N8 C9 -177.9(9) . . . . ? C16 C15 N14 C13 1.6(19) . . . . ? C18 C13 N14 C15 -3.8(18) . . . . ? C6 C13 N14 C15 176.9(10) . . . . ? C23 C24 N25 N26 176.1(16) . . . . ? C42 C24 N25 N26 -3(3) . . . . ? C23 C24 N25 Sn2 14(2) . . . . ? C42 C24 N25 Sn2 -164.9(17) . . . . ? C28 C27 N26 N25 174.9(9) . . . . ? C34 C27 N26 N25 -6.2(16) . . . . ? C24 N25 N26 C27 95.2(18) . . . . ? Sn2 N25 N26 C27 -105.6(11) . . . . ? N29 C28 C33 C30 -0.6(19) . . . . ? C27 C28 C33 C30 176.5(11) . . . . ? C31 C30 C33 C28 0(2) . . . . ? C19 C1 Sn1 S3 123.9(8) . . . . ? C2 C1 Sn1 S3 -116.4(7) . . . . ? C20 C1 Sn1 S3 2.4(9) . . . . ? C19 C1 Sn1 S1 -81.9(8) . . . . ? C2 C1 Sn1 S1 37.8(9) . . . . ? C20 C1 Sn1 S1 156.5(6) . . . . ? C19 C1 Sn1 N4 -157.3(9) . . . . ? C2 C1 Sn1 N4 -37.5(7) . . . . ? C20 C1 Sn1 N4 81.2(7) . . . . ? C19 C1 Sn1 S2 20.6(9) . . . . ? C2 C1 Sn1 S2 140.3(7) . . . . ? C20 C1 Sn1 S2 -100.9(7) . . . . ? Sn3 S3 Sn1 C1 -130.9(4) . . . . ? Sn3 S3 Sn1 S1 74.28(11) . . . . ? Sn3 S3 Sn1 N4 159.7(2) . . . . ? Sn3 S3 Sn1 S2 -18.58(8) . . . . ? Sn2 S1 Sn1 C1 125.0(4) . . . . ? Sn2 S1 Sn1 S3 -78.71(10) . . . . ? Sn2 S1 Sn1 N4 -167.2(2) . . . . ? Sn2 S1 Sn1 S2 13.21(9) . . . . ? C3 N4 Sn1 C1 31.3(7) . . . . ? N5 N4 Sn1 C1 -169.8(8) . . . . ? C3 N4 Sn1 S3 155.9(7) . . . . ? N5 N4 Sn1 S3 -45.2(7) . . . . ? C3 N4 Sn1 S1 -89.3(7) . . . . ? N5 N4 Sn1 S1 69.6(7) . . . . ? C3 N4 Sn1 S2 -79(6) . . . . ? N5 N4 Sn1 S2 80(6) . . . . ? Sn2 S2 Sn1 C1 -132.7(3) . . . . ? Sn3 S2 Sn1 C1 141.9(3) . . . . ? Sn2 S2 Sn1 S3 102.07(8) . . . . ? Sn3 S2 Sn1 S3 16.61(7) . . . . ? Sn2 S2 Sn1 S1 -12.76(9) . . . . ? Sn3 S2 Sn1 S1 -98.23(9) . . . . ? Sn2 S2 Sn1 N4 -23(6) . . . . ? Sn3 S2 Sn1 N4 -109(6) . . . . ? C40 C22 Sn2 S4 -8.7(11) . . . . ? C41 C22 Sn2 S4 -130.9(9) . . . . ? C23 C22 Sn2 S4 112.9(11) . . . . ? C40 C22 Sn2 N25 -87.2(9) . . . . ? C41 C22 Sn2 N25 150.6(11) . . . . ? C23 C22 Sn2 N25 34.4(11) . . . . ? C40 C22 Sn2 S1 -166.8(8) . . . . ? C41 C22 Sn2 S1 71.1(10) . . . . ? C23 C22 Sn2 S1 -45.1(12) . . . . ? C40 C22 Sn2 S2 92.3(9) . . . . ? C41 C22 Sn2 S2 -29.9(11) . . . . ? C23 C22 Sn2 S2 -146.1(10) . . . . ? Sn3 S4 Sn2 C22 124.5(4) . . . . ? Sn3 S4 Sn2 N25 -164.8(3) . . . . ? Sn3 S4 Sn2 S1 -76.17(11) . . . . ? Sn3 S4 Sn2 S2 16.79(9) . . . . ? C24 N25 Sn2 C22 -28.9(12) . . . . ? N26 N25 Sn2 C22 170.0(13) . . . . ? C24 N25 Sn2 S4 -155.0(12) . . . . ? N26 N25 Sn2 S4 43.9(11) . . . . ? C24 N25 Sn2 S1 92.3(12) . . . . ? N26 N25 Sn2 S1 -68.8(11) . . . . ? C24 N25 Sn2 S2 -44(10) . . . . ? N26 N25 Sn2 S2 155(9) . . . . ? Sn1 S1 Sn2 C22 -120.8(4) . . . . ? Sn1 S1 Sn2 S4 78.77(11) . . . . ? Sn1 S1 Sn2 N25 168.0(2) . . . . ? Sn1 S1 Sn2 S2 -13.25(9) . . . . ? Sn1 S2 Sn2 C22 134.0(4) . . . . ? Sn3 S2 Sn2 C22 -140.9(4) . . . . ? Sn1 S2 Sn2 S4 -100.02(9) . . . . ? Sn3 S2 Sn2 S4 -14.98(8) . . . . ? Sn1 S2 Sn2 N25 149(10) . . . . ? Sn3 S2 Sn2 N25 -126(10) . . . . ? Sn1 S2 Sn2 S1 12.74(9) . . . . ? Sn3 S2 Sn2 S1 97.78(9) . . . . ? Sn2 S4 Sn3 S5 -102.67(10) . . . 2_656 ? Sn2 S4 Sn3 S3 67.34(11) . . . . ? Sn2 S4 Sn3 S5 163.55(9) . . . . ? Sn2 S4 Sn3 S2 -15.55(9) . . . . ? Sn1 S3 Sn3 S5 103.61(10) . . . 2_656 ? Sn1 S3 Sn3 S4 -65.71(10) . . . . ? Sn1 S3 Sn3 S5 -162.92(8) . . . . ? Sn1 S3 Sn3 S2 17.26(8) . . . . ? Sn3 S5 Sn3 S5 0.0 2_656 . . 2_656 ? Sn3 S5 Sn3 S4 119.26(9) 2_656 . . . ? Sn3 S5 Sn3 S3 -125.19(8) 2_656 . . . ? Sn3 S5 Sn3 S2 -116(5) 2_656 . . . ? Sn2 S2 Sn3 S5 133.99(8) . . . 2_656 ? Sn1 S2 Sn3 S5 -141.60(8) . . . 2_656 ? Sn2 S2 Sn3 S4 14.82(9) . . . . ? Sn1 S2 Sn3 S4 99.23(9) . . . . ? Sn2 S2 Sn3 S3 -100.79(8) . . . . ? Sn1 S2 Sn3 S3 -16.38(8) . . . . ? Sn2 S2 Sn3 S5 -110(5) . . . . ? Sn1 S2 Sn3 S5 -26(5) . . . . ? C37 C36 C37A C38A -92(6) . . . . ? N35 C36 C37A C38A 12(7) . . . . ? C36 C37A C38A C39A 4(10) . . . . ? C37A C38A C39A C34 4(9) . . . . ? C39 C34 C39A C38A 85(5) . . . . ? N35 C34 C39A C38A -25(5) . . . . ? C27 C34 C39A C38A -164(4) . . . . ? Cl10 C100 Cl13 Cl13 133(5) . . . 2_567 ? Cl15 C100 Cl13 Cl13 -112(6) . . . 2_567 ? Cl12 C100 Cl13 Cl13 -144(7) . . . 2_567 ? _diffrn_measured_fraction_theta_max 0.982 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.982 _refine_diff_density_max 0.716 _refine_diff_density_min -0.957 _refine_diff_density_rms 0.126 _database_code_depnum_ccdc_archive 'CCDC 934166' ####################################################################### # # 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_3b #TrackingRef 'web_deposit_cif_file_1_KlausHarms_1366045723.3b-bb100.cif' #data_bb100 _audit_creation_method SHELXL-2013 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C77 H104 N16 O7 S10 Sn6' _chemical_formula_weight 2398.50 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' Sn Sn -0.6537 1.4246 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system monoclinic _space_group_IT_number 12 _space_group_name_H-M_alt 'C 2/m' _space_group_name_Hall '-C 2y' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' '-x, -y, -z' 'x, -y, z' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z' _cell_length_a 13.0812(11) _cell_length_b 22.5874(14) _cell_length_c 16.9755(13) _cell_angle_alpha 90 _cell_angle_beta 96.153(6) _cell_angle_gamma 90 _cell_volume 4986.9(6) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 7089 _cell_measurement_theta_min 1.8 _cell_measurement_theta_max 24.7 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 1.597 _exptl_crystal_F_000 2388 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.140 _exptl_crystal_size_mid 0.130 _exptl_crystal_size_min 0.100 _exptl_absorpt_coefficient_mu 1.743 _shelx_estimated_absorpt_T_min 0.792 _shelx_estimated_absorpt_T_max 0.845 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.80 _exptl_absorpt_correction_T_max 0.90 _exptl_absorpt_process_details 'STOE X-RED' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_source ? _diffrn_measurement_device_type 'STOE IPDS 2T' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 13664 _diffrn_reflns_av_unetI/netI 0.1273 _diffrn_reflns_av_R_equivalents 0.0949 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.803 _diffrn_reflns_theta_max 25.249 _diffrn_reflns_theta_full 25.242 _diffrn_measured_fraction_theta_max 1.000 _diffrn_measured_fraction_theta_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 1.000 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 1.000 _diffrn_reflns_point_group_measured_fraction_full 1.000 _reflns_number_total 4651 _reflns_number_gt 2484 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_max . _reflns_Friedel_fraction_full . _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _computing_data_collection 'STOE X-AREA' _computing_cell_refinement 'STOE X-AREA' _computing_data_reduction 'STOE X-AREA' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-2013 (Sheldrick, 2013)' _computing_molecular_graphics 'DIAMOND (Crystal Impact)' _computing_publication_material ? _refine_special_details ; ? ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; w=1/[\s^2^(Fo^2^)+(0.0241P)^2^] 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 4651 _refine_ls_number_parameters 310 _refine_ls_number_restraints 208 _refine_ls_R_factor_all 0.1115 _refine_ls_R_factor_gt 0.0463 _refine_ls_wR_factor_ref 0.0855 _refine_ls_wR_factor_gt 0.0718 _refine_ls_goodness_of_fit_ref 0.821 _refine_ls_restrained_S_all 0.819 _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_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.4495(5) 0.6470(4) 0.1786(6) 0.073(3) Uani 1 1 d . . . . . H1A H 0.4243 0.6107 0.1515 0.109 Uiso 1 1 calc R U . . . H1B H 0.4184 0.6815 0.1504 0.109 Uiso 1 1 calc R U . . . H1C H 0.4310 0.6468 0.2330 0.109 Uiso 1 1 calc R U . . . C2 C 0.5675(5) 0.6503(3) 0.1801(5) 0.052(2) Uani 1 1 d . . . . . C3 C 0.6123(5) 0.7039(3) 0.2245(6) 0.061(2) Uani 1 1 d . . . . . H3A H 0.5761 0.7099 0.2722 0.073 Uiso 1 1 calc R U . . . H3B H 0.5997 0.7393 0.1903 0.073 Uiso 1 1 calc R U . . . C4 C 0.7273(6) 0.6989(4) 0.2498(5) 0.053(2) Uani 1 1 d . . . . . C7 C 0.9344(6) 0.6334(3) 0.2237(6) 0.053(2) Uani 1 1 d . . . . . C8 C 1.0413(6) 0.6177(4) 0.2514(6) 0.056(2) Uani 1 1 d . . . . . C10 C 1.1994(6) 0.5894(4) 0.2174(6) 0.075(3) Uani 1 1 d . . . . . H10 H 1.2427 0.5806 0.1774 0.090 Uiso 1 1 calc R U . . . C11 C 1.2382(6) 0.5842(4) 0.2941(6) 0.074(3) Uani 1 1 d . . . . . H11 H 1.3075 0.5720 0.3071 0.089 Uiso 1 1 calc R U . . . C12 C 1.1773(7) 0.5964(5) 0.3536(6) 0.084(3) Uani 1 1 d . . . . . H12 H 1.2030 0.5932 0.4079 0.100 Uiso 1 1 calc R U . . . C13 C 1.0765(7) 0.6136(5) 0.3302(6) 0.080(3) Uani 1 1 d . . . . . H13 H 1.0318 0.6225 0.3692 0.096 Uiso 1 1 calc R U . . . C14 C 0.5972(6) 0.6468(4) 0.0956(5) 0.063(2) Uani 1 1 d . . . . . H14A H 0.6721 0.6497 0.0966 0.094 Uiso 1 1 calc R U . . . H14B H 0.5649 0.6796 0.0642 0.094 Uiso 1 1 calc R U . . . H14C H 0.5737 0.6091 0.0716 0.094 Uiso 1 1 calc R U . . . C15 C 0.7832(7) 0.7543(4) 0.2775(7) 0.084(3) Uani 1 1 d . . . . . H15A H 0.8366 0.7447 0.3206 0.126 Uiso 1 1 calc R U . . . H15B H 0.7345 0.7825 0.2967 0.126 Uiso 1 1 calc R U . . . H15C H 0.8150 0.7720 0.2334 0.126 Uiso 1 1 calc R U . . . C16 C 0.9053(5) 0.6420(4) 0.1368(6) 0.053(2) Uani 1 1 d . . . . . C18 C 0.8658(6) 0.7100(4) 0.0383(6) 0.062(2) Uani 1 1 d . . . . . H18 H 0.8551 0.7499 0.0217 0.075 Uiso 1 1 calc R U . . . C19 C 0.8542(6) 0.6671(5) -0.0175(6) 0.066(3) Uani 1 1 d . . . . . H19 H 0.8369 0.6769 -0.0717 0.079 Uiso 1 1 calc R U . . . C20 C 0.8681(6) 0.6088(4) 0.0054(6) 0.065(2) Uani 1 1 d . . . . . H20 H 0.8586 0.5779 -0.0327 0.078 Uiso 1 1 calc R U . . . C21 C 0.8952(6) 0.5961(4) 0.0826(6) 0.059(2) Uani 1 1 d . . . . . H21 H 0.9070 0.5564 0.0994 0.070 Uiso 1 1 calc R U . . . N5 N 0.7679(4) 0.6483(3) 0.2473(4) 0.0468(16) Uani 1 1 d . . . . . N6 N 0.8713(4) 0.6398(3) 0.2766(4) 0.0517(18) Uani 1 1 d . . . . . N9 N 1.1017(5) 0.6066(3) 0.1949(5) 0.067(2) Uani 1 1 d . . . . . N17 N 0.8911(5) 0.7000(3) 0.1147(5) 0.0583(19) Uani 1 1 d . . . . . S1 S 0.65208(14) 0.58883(9) 0.38804(13) 0.0500(5) Uani 1 1 d . . . . . S2 S 0.49191(19) 0.5000 0.24761(18) 0.0476(7) Uani 1 2 d S T P . . S3 S 0.74955(19) 0.5000 0.20443(19) 0.0471(7) Uani 1 2 d S T P . . S4 S 0.3871(2) 0.5000 0.43564(18) 0.0542(8) Uani 1 2 d S T P . . Sn1 Sn 0.63379(4) 0.57400(2) 0.24649(3) 0.04361(16) Uani 1 1 d . . . . . Sn2 Sn 0.56579(5) 0.5000 0.42063(5) 0.0453(2) Uani 1 2 d S T P . . C901 C 0.0518(15) 0.5241(10) 0.5631(17) 0.073(7) Uani 0.5 1 d . U P A 1 H90A H 0.1051 0.5463 0.5932 0.088 Uiso 0.5 1 d R U P A 1 H90B H 0.0029 0.5121 0.5983 0.088 Uiso 0.5 1 d R U P A 1 C902 C 0.0929(15) 0.4716(10) 0.5302(17) 0.073(7) Uani 0.5 1 d . U P A 1 H90C H 0.1336 0.4822 0.4885 0.087 Uiso 0.5 1 d R U P A 1 H90D H 0.1344 0.4493 0.5698 0.087 Uiso 0.5 1 d R U P A 1 O901 O 0.0000 0.5615(4) 0.5000 0.082(3) Uani 1 2 d S TU P . . C905 C 0.362(2) 0.492(4) 0.0286(17) 0.066(11) Uani 0.25 1 d . U P B -1 H90K H 0.4336 0.5030 0.0450 0.099 Uiso 0.25 1 calc R U P B -1 H90L H 0.3304 0.5216 -0.0085 0.099 Uiso 0.25 1 calc R U P B -1 H90M H 0.3600 0.4531 0.0028 0.099 Uiso 0.25 1 calc R U P B -1 O904 O 0.3118(14) 0.490(2) 0.0904(13) 0.066(11) Uani 0.25 1 d . U P B -1 H904 H 0.3536 0.4887 0.1316 0.099 Uiso 0.25 1 calc R U P B -1 C904 C 0.574(2) 0.2139(12) 0.5273(18) 0.139(9) Uani 0.5 1 d . U P C -1 H90H H 0.5223 0.1844 0.5075 0.208 Uiso 0.5 1 calc R U P C -1 H90I H 0.5491 0.2355 0.5717 0.208 Uiso 0.5 1 calc R U P C -1 H90J H 0.6385 0.1939 0.5454 0.208 Uiso 0.5 1 calc R U P C -1 O903 O 0.5900(17) 0.2547(8) 0.4651(14) 0.150(7) Uani 0.5 1 d . U P C -1 H903 H 0.6466 0.2473 0.4480 0.226 Uiso 0.5 1 calc R U P C -1 C903 C 0.5432(16) 0.3022(9) 0.5364(12) 0.081(6) Uani 0.5 1 d . U P D -2 H90E H 0.4889 0.3183 0.4981 0.121 Uiso 0.5 1 calc R U P D -2 H90F H 0.5969 0.2844 0.5080 0.121 Uiso 0.5 1 calc R U P D -2 H90G H 0.5730 0.3341 0.5706 0.121 Uiso 0.5 1 calc R U P D -2 O902 O 0.5014(13) 0.2589(8) 0.5829(8) 0.111(6) Uani 0.5 1 d . U P D -2 H902 H 0.4879 0.2283 0.5555 0.167 Uiso 0.5 1 calc R U P D -2 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 0.037(4) 0.074(6) 0.108(9) 0.032(6) 0.015(5) 0.006(4) C2 0.034(4) 0.050(5) 0.073(7) 0.010(5) 0.008(4) 0.014(4) C3 0.049(5) 0.047(5) 0.087(8) 0.004(5) 0.008(5) 0.010(4) C4 0.048(5) 0.049(5) 0.064(6) 0.000(4) 0.019(4) -0.012(4) C7 0.042(4) 0.051(5) 0.065(7) 0.009(5) 0.001(4) -0.008(4) C8 0.042(5) 0.062(5) 0.065(7) 0.011(5) 0.006(5) 0.000(4) C10 0.046(5) 0.101(8) 0.080(8) 0.012(6) 0.008(5) 0.005(5) C11 0.053(5) 0.089(7) 0.079(8) 0.027(6) 0.001(5) 0.007(5) C12 0.064(6) 0.119(9) 0.069(7) 0.025(6) 0.010(5) 0.021(6) C13 0.065(6) 0.109(8) 0.064(8) 0.015(6) 0.002(5) 0.012(5) C14 0.053(5) 0.076(6) 0.057(6) 0.012(5) -0.007(4) 0.001(4) C15 0.079(6) 0.068(6) 0.104(9) -0.005(6) 0.007(6) -0.008(5) C16 0.032(4) 0.059(6) 0.068(7) 0.006(5) 0.005(4) -0.002(4) C18 0.066(6) 0.070(6) 0.050(7) 0.009(5) 0.004(5) 0.000(5) C19 0.061(5) 0.094(7) 0.041(6) 0.020(6) 0.004(4) 0.002(5) C20 0.070(6) 0.083(7) 0.040(6) -0.002(5) 0.003(5) 0.000(5) C21 0.058(5) 0.052(5) 0.067(7) 0.000(5) 0.008(5) 0.004(4) N5 0.043(4) 0.050(4) 0.048(5) 0.005(3) 0.008(3) 0.000(3) N6 0.033(3) 0.055(4) 0.066(5) 0.009(4) 0.000(3) -0.005(3) N9 0.044(4) 0.091(5) 0.066(5) 0.008(4) 0.012(4) 0.004(4) N17 0.047(4) 0.069(5) 0.058(5) 0.002(4) 0.005(4) -0.003(3) S1 0.0506(11) 0.0522(13) 0.0481(14) -0.0029(10) 0.0091(9) -0.0051(9) S2 0.0379(14) 0.0527(17) 0.052(2) 0.000 0.0055(13) 0.000 S3 0.0389(14) 0.0485(17) 0.055(2) 0.000 0.0119(13) 0.000 S4 0.0392(14) 0.080(2) 0.043(2) 0.000 0.0053(13) 0.000 Sn1 0.0376(3) 0.0480(3) 0.0458(3) 0.0043(3) 0.0070(2) 0.0030(3) Sn2 0.0393(4) 0.0525(5) 0.0454(6) 0.000 0.0103(4) 0.000 C901 0.044(12) 0.064(13) 0.11(2) -0.010(12) -0.019(11) 0.002(10) C902 0.039(12) 0.077(13) 0.10(2) 0.001(12) -0.005(10) 0.020(10) O901 0.069(5) 0.075(6) 0.098(8) 0.000 -0.016(5) 0.000 C905 0.076(10) 0.05(3) 0.064(12) -0.003(15) -0.010(8) -0.020(15) O904 0.076(10) 0.05(3) 0.064(12) -0.003(15) -0.010(8) -0.020(15) C904 0.149(17) 0.144(18) 0.115(18) 0.060(16) -0.021(16) 0.024(16) O903 0.174(15) 0.114(12) 0.174(17) 0.034(13) 0.070(14) -0.011(12) C903 0.090(13) 0.090(13) 0.062(13) -0.014(11) 0.011(10) 0.006(11) O902 0.121(12) 0.169(14) 0.037(8) 0.040(9) -0.016(8) -0.065(11) _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 C2 1.543(9) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 C3 1.513(11) . ? C2 C14 1.528(11) . ? C2 Sn1 2.186(7) . ? C3 C4 1.523(10) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 N5 1.263(9) . ? C4 C15 1.499(11) . ? C7 N6 1.292(10) . ? C7 C8 1.470(10) . ? C7 C16 1.495(12) . ? C8 N9 1.330(10) . ? C8 C13 1.371(11) . ? C10 N9 1.351(10) . ? C10 C11 1.351(12) . ? C10 H10 0.9500 . ? C11 C12 1.379(12) . ? C11 H11 0.9500 . ? C12 C13 1.391(11) . ? C12 H12 0.9500 . ? C13 H13 0.9500 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 N17 1.369(10) . ? C16 C21 1.383(11) . ? C18 N17 1.322(11) . ? C18 C19 1.354(12) . ? C18 H18 0.9500 . ? C19 C20 1.380(12) . ? C19 H19 0.9500 . ? C20 C21 1.351(11) . ? C20 H20 0.9500 . ? C21 H21 0.9500 . ? N5 N6 1.403(8) . ? N5 Sn1 2.427(6) . ? S1 Sn2 2.396(2) . ? S1 Sn1 2.413(2) . ? S2 Sn1 2.4992(19) 6_565 ? S2 Sn1 2.4992(19) . ? S3 Sn1 2.4142(19) 6_565 ? S3 Sn1 2.4142(19) . ? S4 Sn2 2.379(3) . ? S4 Sn2 2.452(3) 5_666 ? Sn2 S1 2.396(2) 6_565 ? Sn2 S4 2.452(3) 5_666 ? C901 C902 0.82(3) 6_565 ? C901 C901 1.09(4) 6_565 ? C901 C902 1.44(2) . ? C901 O901 1.47(3) . ? C901 H90A 0.9600 . ? C901 H90B 0.9599 . ? C902 C901 0.82(3) 6_565 ? C902 C902 1.28(5) 6_565 ? C902 O901 1.47(2) 5_566 ? C902 H90C 0.9604 . ? C902 H90D 0.9599 . ? O901 C901 1.47(3) 2_556 ? O901 C902 1.47(2) 5_566 ? O901 C902 1.47(2) 6_565 ? C905 O904 1.30(3) . ? C905 H90K 0.9800 . ? C905 H90L 0.9800 . ? C905 H90M 0.9800 . ? O904 H904 0.8400 . ? C904 O903 1.43(3) . ? C904 H90H 0.9800 . ? C904 H90I 0.9800 . ? C904 H90J 0.9800 . ? O903 H903 0.8400 . ? C903 O902 1.40(2) . ? C903 H90E 0.9800 . ? C903 H90F 0.9800 . ? C903 H90G 0.9800 . ? O902 H902 0.8400 . ? 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 C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C3 C2 C14 112.6(7) . . ? C3 C2 C1 112.3(7) . . ? C14 C2 C1 109.7(7) . . ? C3 C2 Sn1 105.3(5) . . ? C14 C2 Sn1 108.5(5) . . ? C1 C2 Sn1 108.2(5) . . ? C2 C3 C4 113.5(6) . . ? C2 C3 H3A 108.9 . . ? C4 C3 H3A 108.9 . . ? C2 C3 H3B 108.9 . . ? C4 C3 H3B 108.9 . . ? H3A C3 H3B 107.7 . . ? N5 C4 C15 125.0(7) . . ? N5 C4 C3 117.6(7) . . ? C15 C4 C3 117.4(7) . . ? N6 C7 C8 117.5(8) . . ? N6 C7 C16 123.9(7) . . ? C8 C7 C16 118.7(8) . . ? N9 C8 C13 121.8(8) . . ? N9 C8 C7 115.7(8) . . ? C13 C8 C7 122.5(8) . . ? N9 C10 C11 122.9(9) . . ? N9 C10 H10 118.5 . . ? C11 C10 H10 118.5 . . ? C10 C11 C12 120.1(8) . . ? C10 C11 H11 120.0 . . ? C12 C11 H11 120.0 . . ? C11 C12 C13 116.8(10) . . ? C11 C12 H12 121.6 . . ? C13 C12 H12 121.6 . . ? C8 C13 C12 120.4(9) . . ? C8 C13 H13 119.8 . . ? C12 C13 H13 119.8 . . ? C2 C14 H14A 109.5 . . ? C2 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C2 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C4 C15 H15A 109.5 . . ? C4 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C4 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? N17 C16 C21 122.2(8) . . ? N17 C16 C7 114.1(8) . . ? C21 C16 C7 123.7(8) . . ? N17 C18 C19 124.1(9) . . ? N17 C18 H18 117.9 . . ? C19 C18 H18 117.9 . . ? C18 C19 C20 119.0(9) . . ? C18 C19 H19 120.5 . . ? C20 C19 H19 120.5 . . ? C21 C20 C19 119.2(9) . . ? C21 C20 H20 120.4 . . ? C19 C20 H20 120.4 . . ? C20 C21 C16 118.9(8) . . ? C20 C21 H21 120.5 . . ? C16 C21 H21 120.5 . . ? C4 N5 N6 120.3(6) . . ? C4 N5 Sn1 108.6(5) . . ? N6 N5 Sn1 125.2(4) . . ? C7 N6 N5 115.6(7) . . ? C8 N9 C10 117.9(8) . . ? C18 N17 C16 116.5(8) . . ? Sn2 S1 Sn1 96.59(7) . . ? Sn1 S2 Sn1 83.95(8) 6_565 . ? Sn1 S3 Sn1 87.63(9) 6_565 . ? Sn2 S4 Sn2 87.79(9) . 5_666 ? C2 Sn1 S1 113.3(2) . . ? C2 Sn1 S3 128.3(2) . . ? S1 Sn1 S3 113.10(9) . . ? C2 Sn1 N5 72.8(2) . . ? S1 Sn1 N5 84.47(16) . . ? S3 Sn1 N5 90.27(15) . . ? C2 Sn1 S2 106.1(2) . . ? S1 Sn1 S2 94.58(9) . . ? S3 Sn1 S2 91.67(6) . . ? N5 Sn1 S2 178.05(16) . . ? S4 Sn2 S1 121.17(5) . . ? S4 Sn2 S1 121.17(5) . 6_565 ? S1 Sn2 S1 113.75(10) . 6_565 ? S4 Sn2 S4 92.22(9) . 5_666 ? S1 Sn2 S4 98.93(6) . 5_666 ? S1 Sn2 S4 98.93(6) 6_565 5_666 ? C902 C901 C901 97(3) 6_565 6_565 ? C902 C901 C902 62(3) 6_565 . ? C901 C901 C902 34.5(10) 6_565 . ? C902 C901 O901 74(3) 6_565 . ? C901 C901 O901 125.1(10) 6_565 . ? C902 C901 O901 111(3) . . ? C902 C901 H90A 79.0 6_565 . ? C901 C901 H90A 121.5 6_565 . ? C902 C901 H90A 110.9 . . ? O901 C901 H90A 109.8 . . ? C902 C901 H90B 170.0 6_565 . ? C901 C901 H90B 73.6 6_565 . ? C902 C901 H90B 108.1 . . ? O901 C901 H90B 109.2 . . ? H90A C901 H90B 108.2 . . ? C901 C902 C902 83(3) 6_565 6_565 ? C901 C902 C901 49(3) 6_565 . ? C902 C902 C901 34.5(10) 6_565 . ? C901 C902 O901 74(3) 6_565 5_566 ? C902 C902 O901 120.6(9) 6_565 5_566 ? C901 C902 O901 103.0(15) . 5_566 ? C901 C902 H90C 157.9 6_565 . ? C902 C902 H90C 75.6 6_565 . ? C901 C902 H90C 109.9 . . ? O901 C902 H90C 111.8 5_566 . ? C901 C902 H90D 87.0 6_565 . ? C902 C902 H90D 121.6 6_565 . ? C901 C902 H90D 111.5 . . ? O901 C902 H90D 111.2 5_566 . ? H90C C902 H90D 109.2 . . ? C901 O901 C901 109.9(19) . 2_556 ? C901 O901 C902 105.1(10) . 5_566 ? C901 O901 C902 32.4(11) 2_556 5_566 ? C901 O901 C902 32.4(11) . 6_565 ? C901 O901 C902 105.1(10) 2_556 6_565 ? C902 O901 C902 118.8(18) 5_566 6_565 ? O904 C905 H90K 109.5 . . ? O904 C905 H90L 109.5 . . ? H90K C905 H90L 109.5 . . ? O904 C905 H90M 109.5 . . ? H90K C905 H90M 109.5 . . ? H90L C905 H90M 109.5 . . ? C905 O904 H904 109.5 . . ? O903 C904 H90H 109.5 . . ? O903 C904 H90I 109.5 . . ? H90H C904 H90I 109.5 . . ? O903 C904 H90J 109.5 . . ? H90H C904 H90J 109.5 . . ? H90I C904 H90J 109.5 . . ? C904 O903 H903 109.5 . . ? O902 C903 H90E 109.5 . . ? O902 C903 H90F 109.5 . . ? H90E C903 H90F 109.5 . . ? O902 C903 H90G 109.5 . . ? H90E C903 H90G 109.5 . . ? H90F C903 H90G 109.5 . . ? C903 O902 H902 109.5 . . ? 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 C14 C2 C3 C4 -73.9(9) . . . . ? C1 C2 C3 C4 161.6(7) . . . . ? Sn1 C2 C3 C4 44.2(8) . . . . ? C2 C3 C4 N5 -14.7(12) . . . . ? C2 C3 C4 C15 166.5(8) . . . . ? N6 C7 C8 N9 174.6(7) . . . . ? C16 C7 C8 N9 -6.6(11) . . . . ? N6 C7 C8 C13 -4.1(13) . . . . ? C16 C7 C8 C13 174.7(8) . . . . ? N9 C10 C11 C12 0.2(16) . . . . ? C10 C11 C12 C13 0.4(15) . . . . ? N9 C8 C13 C12 -1.1(15) . . . . ? C7 C8 C13 C12 177.5(9) . . . . ? C11 C12 C13 C8 0.1(15) . . . . ? N6 C7 C16 N17 73.0(10) . . . . ? C8 C7 C16 N17 -105.8(8) . . . . ? N6 C7 C16 C21 -108.2(9) . . . . ? C8 C7 C16 C21 73.1(10) . . . . ? N17 C18 C19 C20 0.9(14) . . . . ? C18 C19 C20 C21 -1.6(13) . . . . ? C19 C20 C21 C16 1.9(12) . . . . ? N17 C16 C21 C20 -1.5(12) . . . . ? C7 C16 C21 C20 179.7(7) . . . . ? C15 C4 N5 N6 4.4(13) . . . . ? C3 C4 N5 N6 -174.2(7) . . . . ? C15 C4 N5 Sn1 158.8(7) . . . . ? C3 C4 N5 Sn1 -19.8(9) . . . . ? C8 C7 N6 N5 -173.3(6) . . . . ? C16 C7 N6 N5 7.9(11) . . . . ? C4 N5 N6 C7 -105.6(9) . . . . ? Sn1 N5 N6 C7 104.5(7) . . . . ? C13 C8 N9 C10 1.7(13) . . . . ? C7 C8 N9 C10 -177.1(7) . . . . ? C11 C10 N9 C8 -1.2(14) . . . . ? C19 C18 N17 C16 -0.5(12) . . . . ? C21 C16 N17 C18 0.8(11) . . . . ? C7 C16 N17 C18 179.7(7) . . . . ? C902 C901 C902 C901 179.996(10) 6_565 . . 6_565 ? O901 C901 C902 C901 -122(2) . . . 6_565 ? C901 C901 C902 C902 180.004(15) 6_565 . . 6_565 ? O901 C901 C902 C902 58(2) . . . 6_565 ? C902 C901 C902 O901 -125.8(18) 6_565 . . 5_566 ? C901 C901 C902 O901 54.2(18) 6_565 . . 5_566 ? O901 C901 C902 O901 -68.1(15) . . . 5_566 ? C902 C901 O901 C901 87(3) 6_565 . . 2_556 ? C901 C901 O901 C901 0.002(12) 6_565 . . 2_556 ? C902 C901 O901 C901 35.8(10) . . . 2_556 ? C902 C901 O901 C902 121(3) 6_565 . . 5_566 ? C901 C901 O901 C902 33.7(10) 6_565 . . 5_566 ? C902 C901 O901 C902 69.5(14) . . . 5_566 ? C901 C901 O901 C902 -87(3) 6_565 . . 6_565 ? C902 C901 O901 C902 -51(3) . . . 6_565 ? _refine_diff_density_max 0.826 _refine_diff_density_min -0.517 _refine_diff_density_rms 0.100 _database_code_depnum_ccdc_archive 'CCDC 934167' ####################################################################### # # 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_bb126 #TrackingRef 'web_deposit_cif_file_2_KlausHarms_1366045723.4-bb126.cif' _audit_creation_method SHELXL-2013 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C72 H82 Cl18 N16 S10 Sn4 Zn8' _chemical_formula_weight 3127.95 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' Cl Cl 0.1484 0.1585 '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' Sn Sn -0.6537 1.4246 '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' _space_group_crystal_system tetragonal _space_group_IT_number 88 _space_group_name_H-M_alt 'I 41/a' _space_group_name_Hall '-I 4ad' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; loop_ _space_group_symop_operation_xyz 'x, y, z' '-y+3/4, x+1/4, z+1/4' '-x, -y+1/2, z' 'y+1/4, -x+1/4, z+1/4' 'x+1/2, y+1/2, z+1/2' '-y+5/4, x+3/4, z+3/4' '-x+1/2, -y+1, z+1/2' 'y+3/4, -x+3/4, z+3/4' '-x, -y, -z' 'y-3/4, -x-1/4, -z-1/4' 'x, y-1/2, -z' '-y-1/4, x-1/4, -z-1/4' '-x+1/2, -y+1/2, -z+1/2' 'y-1/4, -x+1/4, -z+1/4' 'x+1/2, y, -z+1/2' '-y+1/4, x+1/4, -z+1/4' _cell_length_a 26.7544(15) _cell_length_b 26.7544(15) _cell_length_c 15.6480(11) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 11200.8(15) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 1.855 _exptl_crystal_F_000 6128 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.120 _exptl_crystal_size_mid 0.050 _exptl_crystal_size_min 0.050 _exptl_absorpt_coefficient_mu 3.215 _shelx_estimated_absorpt_T_min 0.699 _shelx_estimated_absorpt_T_max 0.856 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_source ? _diffrn_measurement_device_type 'STOE IPDS 2T' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 18558 _diffrn_reflns_av_unetI/netI 0.2218 _diffrn_reflns_av_R_equivalents 0.1472 _diffrn_reflns_limit_h_min -29 _diffrn_reflns_limit_h_max 31 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 31 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.508 _diffrn_reflns_theta_max 25.000 _diffrn_reflns_theta_full 25.242 _diffrn_measured_fraction_theta_max 1.000 _diffrn_measured_fraction_theta_full 0.974 _diffrn_reflns_Laue_measured_fraction_max 1.000 _diffrn_reflns_Laue_measured_fraction_full 0.974 _diffrn_reflns_point_group_measured_fraction_max 1.000 _diffrn_reflns_point_group_measured_fraction_full 0.974 _reflns_number_total 4939 _reflns_number_gt 1758 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_max . _reflns_Friedel_fraction_full . _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _computing_data_collection 'STOE X-AREA' _computing_cell_refinement 'STOE X-AREA' _computing_data_reduction 'STOE X-AREA' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-2013 (Sheldrick, 2013)' _computing_molecular_graphics 'DIAMOND (Crystal Impact)' _computing_publication_material ? _refine_special_details ; ? ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; w=1/[\s^2^(Fo^2^)+(0.0485P)^2^] 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 4939 _refine_ls_number_parameters 314 _refine_ls_number_restraints 86 _refine_ls_R_factor_all 0.1996 _refine_ls_R_factor_gt 0.0667 _refine_ls_wR_factor_ref 0.1590 _refine_ls_wR_factor_gt 0.1217 _refine_ls_goodness_of_fit_ref 0.806 _refine_ls_restrained_S_all 0.800 _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_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.6341(7) 0.1549(6) 0.6797(12) 0.081(5) Uani 1 1 d . U . . . H1A H 0.6301 0.1330 0.6299 0.121 Uiso 1 1 calc R U . . . H1B H 0.6064 0.1493 0.7196 0.121 Uiso 1 1 calc R U . . . H1C H 0.6658 0.1473 0.7083 0.121 Uiso 1 1 calc R U . . . C2 C 0.6341(7) 0.2093(6) 0.6507(9) 0.068(4) Uani 1 1 d . U . . . C3 C 0.6351(7) 0.2427(6) 0.7319(10) 0.075(5) Uani 1 1 d . U . . . H3A H 0.6111 0.2285 0.7735 0.090 Uiso 1 1 calc R U . . . H3B H 0.6688 0.2399 0.7576 0.090 Uiso 1 1 calc R U . . . C4 C 0.6235(7) 0.2968(6) 0.7221(9) 0.070(5) Uani 1 1 d . U . . . C7 C 0.6195(6) 0.3946(6) 0.6164(9) 0.055(3) Uani 1 1 d . U . . . C8 C 0.5986(7) 0.4449(6) 0.6016(8) 0.059(3) Uani 1 1 d . U . . . C10 C 0.5255(7) 0.4904(7) 0.6017(9) 0.067(4) Uani 1 1 d . U . . . H10 H 0.4901 0.4915 0.6067 0.081 Uiso 1 1 calc R U . . . C11 C 0.5504(7) 0.5334(7) 0.5862(10) 0.070(4) Uani 1 1 d . U . . . H11 H 0.5331 0.5643 0.5821 0.084 Uiso 1 1 calc R U . . . C12 C 0.6013(7) 0.5313(6) 0.5766(10) 0.069(4) Uani 1 1 d . U . . . H12 H 0.6199 0.5608 0.5655 0.083 Uiso 1 1 calc R U . . . C13 C 0.6251(7) 0.4856(6) 0.5834(9) 0.064(4) Uani 1 1 d . U . . . H13 H 0.6602 0.4833 0.5752 0.077 Uiso 1 1 calc R U . . . C14 C 0.6780(6) 0.2210(8) 0.5972(12) 0.095(6) Uani 1 1 d . U . . . H14A H 0.6749 0.2550 0.5745 0.143 Uiso 1 1 calc R U . . . H14B H 0.6799 0.1972 0.5498 0.143 Uiso 1 1 calc R U . . . H14C H 0.7084 0.2186 0.6319 0.143 Uiso 1 1 calc R U . . . C15 C 0.6276(9) 0.3324(6) 0.7929(10) 0.094(7) Uani 1 1 d . U . . . H15A H 0.5943 0.3447 0.8082 0.141 Uiso 1 1 calc R U . . . H15B H 0.6487 0.3606 0.7754 0.141 Uiso 1 1 calc R U . . . H15C H 0.6427 0.3158 0.8424 0.141 Uiso 1 1 calc R U . . . C16 C 0.6751(6) 0.3867(6) 0.6129(10) 0.063(4) Uani 1 1 d . U . . . C18 C 0.7499(8) 0.4055(8) 0.6696(14) 0.098(6) Uani 1 1 d . U . . . H18 H 0.7681 0.4228 0.7126 0.117 Uiso 1 1 calc R U . . . C19 C 0.7764(7) 0.3765(9) 0.6190(12) 0.090(6) Uani 1 1 d . U . . . H19 H 0.8118 0.3752 0.6225 0.108 Uiso 1 1 calc R U . . . C20 C 0.7499(8) 0.3479(9) 0.5599(10) 0.101(6) Uani 1 1 d . U . . . H20 H 0.7664 0.3244 0.5242 0.121 Uiso 1 1 calc R U . . . C21 C 0.6988(7) 0.3549(8) 0.5551(10) 0.086(6) Uani 1 1 d . U . . . H21 H 0.6799 0.3380 0.5126 0.103 Uiso 1 1 calc R U . . . N5 N 0.6073(5) 0.3105(5) 0.6464(7) 0.053(3) Uani 1 1 d . U . . . N6 N 0.5895(5) 0.3595(5) 0.6325(7) 0.054(3) Uani 1 1 d . U . . . N9 N 0.5492(5) 0.4455(5) 0.6105(7) 0.062(3) Uani 1 1 d . U . . . N17 N 0.7013(6) 0.4136(6) 0.6684(10) 0.085(4) Uani 1 1 d . U . . . S1 S 0.46494(16) 0.35506(15) 0.5268(2) 0.0555(10) Uani 1 1 d . U . . . Cl2 Cl 0.57556(16) 0.40581(16) 0.4033(2) 0.0635(11) Uani 1 1 d . U . . . S3 S 0.41783(16) 0.22693(16) 0.4496(2) 0.0587(11) Uani 1 1 d . U . . . S2 S 0.5000 0.2500 0.6715(4) 0.0630(16) Uani 1 2 d S TU P . . Cl1 Cl 0.4945(2) 0.3859(2) 0.7746(3) 0.0975(17) Uani 1 1 d . U . . . Zn1 Zn 0.51490(8) 0.37801(8) 0.63938(11) 0.0637(6) Uani 1 1 d . U . . . Zn2 Zn 0.52641(7) 0.33765(6) 0.42361(10) 0.0555(5) Uani 1 1 d . U . . . Sn1 Sn 0.43261(4) 0.27388(4) 0.57761(7) 0.0564(3) Uani 1 1 d . U . . . C901 C 0.3516(13) 0.5083(17) 0.7040(18) 0.13(2) Uiso 0.5 1 d D . P A 1 H901 H 0.3695 0.5373 0.6775 0.161 Uiso 0.5 1 calc R U P A 1 C902 C 0.3695(16) 0.501(3) 0.720(2) 0.14(2) Uiso 0.5 1 d D . P B 2 H90A H 0.3872 0.5338 0.7201 0.170 Uiso 0.5 1 calc R U P B 2 H90B H 0.3890 0.4783 0.6829 0.170 Uiso 0.5 1 calc R U P B 2 Cl11 Cl 0.3134(8) 0.4830(8) 0.6273(11) 0.157(8) Uani 0.5 1 d D . P A 1 Cl12 Cl 0.3957(5) 0.4644(4) 0.7309(10) 0.111(4) Uani 0.5 1 d D . P A 1 Cl13 Cl 0.3190(6) 0.5305(5) 0.7903(11) 0.146(5) Uani 0.5 1 d D . P A 1 Cl21 Cl 0.3125(14) 0.5103(10) 0.673(2) 0.251(14) Uani 0.5 1 d D . P B 2 Cl22 Cl 0.3698(7) 0.4779(9) 0.821(2) 0.242(12) Uani 0.5 1 d D . P B 2 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 0.090(13) 0.067(8) 0.086(13) -0.018(8) -0.036(10) 0.009(9) C2 0.086(11) 0.075(9) 0.043(9) 0.000(7) -0.014(8) 0.016(10) C3 0.100(14) 0.058(7) 0.066(9) 0.003(7) -0.022(9) -0.009(10) C4 0.110(15) 0.061(8) 0.039(8) 0.005(6) -0.006(9) -0.005(10) C7 0.078(6) 0.054(7) 0.033(8) 0.009(7) -0.017(7) -0.012(6) C8 0.085(8) 0.060(7) 0.031(8) 0.006(7) -0.001(8) -0.004(6) C10 0.093(10) 0.071(7) 0.038(9) -0.007(9) 0.004(9) -0.001(7) C11 0.099(10) 0.065(8) 0.047(9) -0.004(9) -0.005(11) 0.001(8) C12 0.105(10) 0.064(8) 0.038(8) 0.008(9) 0.008(10) -0.001(8) C13 0.088(10) 0.064(8) 0.040(8) 0.017(9) 0.002(9) -0.005(7) C14 0.052(11) 0.144(17) 0.089(13) 0.000(11) -0.021(8) 0.003(11) C15 0.18(2) 0.063(10) 0.043(8) 0.009(7) -0.034(11) -0.006(13) C16 0.076(7) 0.071(11) 0.042(8) 0.005(7) -0.012(7) -0.010(7) C18 0.078(10) 0.130(18) 0.086(14) -0.002(11) -0.020(11) -0.017(12) C19 0.063(11) 0.15(2) 0.061(11) 0.026(10) -0.007(8) -0.001(10) C20 0.084(10) 0.18(2) 0.039(10) 0.002(10) 0.014(9) -0.005(12) C21 0.080(9) 0.141(18) 0.037(9) -0.019(9) 0.004(8) -0.022(11) N5 0.072(8) 0.053(6) 0.034(6) -0.010(5) -0.011(6) -0.014(5) N6 0.079(6) 0.055(6) 0.029(6) -0.009(6) -0.005(5) -0.013(5) N9 0.079(7) 0.074(6) 0.032(6) -0.009(6) -0.008(6) -0.001(5) N17 0.073(8) 0.100(12) 0.083(10) -0.024(8) -0.014(8) -0.006(8) S1 0.068(3) 0.058(3) 0.041(2) 0.0009(18) 0.0074(19) 0.000(2) Cl2 0.077(3) 0.073(3) 0.040(2) 0.003(2) 0.001(2) -0.016(2) S3 0.072(3) 0.066(3) 0.038(2) 0.0014(19) -0.0070(19) -0.004(2) S2 0.069(4) 0.080(4) 0.040(3) 0.000 0.000 0.002(3) Cl1 0.118(4) 0.131(5) 0.044(2) -0.010(3) 0.022(3) -0.009(4) Zn1 0.0761(14) 0.0739(14) 0.0412(10) -0.0035(9) 0.0065(9) -0.0037(11) Zn2 0.0663(12) 0.0615(12) 0.0388(9) -0.0001(9) 0.0016(10) -0.0023(10) Sn1 0.0623(8) 0.0627(8) 0.0440(5) 0.0017(6) 0.0042(6) -0.0017(6) Cl11 0.219(19) 0.144(17) 0.108(12) 0.033(11) 0.070(13) 0.011(15) Cl12 0.118(10) 0.064(7) 0.150(11) 0.000(7) 0.029(9) 0.004(7) Cl13 0.170(14) 0.090(9) 0.177(14) -0.009(9) 0.003(11) 0.017(9) Cl21 0.35(4) 0.18(3) 0.22(3) 0.01(2) -0.04(3) 0.05(2) Cl22 0.160(16) 0.22(2) 0.35(3) 0.13(2) -0.04(2) -0.060(15) _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 C2 1.53(2) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 C14 1.48(2) . ? C2 C3 1.55(2) . ? C2 Sn1 2.167(16) 3_655 ? C3 C4 1.49(2) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 N5 1.315(18) . ? C4 C15 1.47(2) . ? C7 N6 1.260(17) . ? C7 C8 1.48(2) . ? C7 C16 1.50(2) . ? C8 N9 1.330(19) . ? C8 C13 1.33(2) . ? C10 C11 1.35(2) . ? C10 N9 1.366(19) . ? C10 H10 0.9500 . ? C11 C12 1.37(2) . ? C11 H11 0.9500 . ? C12 C13 1.38(2) . ? C12 H12 0.9500 . ? C13 H13 0.9500 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 N17 1.327(19) . ? C16 C21 1.39(2) . ? C18 C19 1.32(3) . ? C18 N17 1.32(2) . ? C18 H18 0.9500 . ? C19 C20 1.39(3) . ? C19 H19 0.9500 . ? C20 C21 1.38(2) . ? C20 H20 0.9500 . ? C21 H21 0.9500 . ? N5 N6 1.411(16) . ? N6 Zn1 2.058(13) . ? N9 Zn1 2.075(14) . ? S1 Zn1 2.295(4) . ? S1 Zn2 2.352(4) . ? S1 Sn1 2.469(4) . ? Cl2 Zn2 2.271(4) . ? S3 Zn2 2.318(5) 3_655 ? S3 Zn2 2.343(4) 12_656 ? S3 Sn1 2.398(4) . ? S2 Sn1 2.412(4) . ? S2 Sn1 2.412(4) 3_655 ? Cl1 Zn1 2.195(4) . ? Zn2 S3 2.319(5) 3_655 ? Zn2 S3 2.343(4) 10_666 ? Sn1 C2 2.167(16) 3_655 ? C901 Cl13 1.71(2) . ? C901 Cl11 1.72(2) . ? C901 Cl12 1.72(2) . ? C901 H901 1.0000 . ? C902 Cl21 1.71(2) . ? C902 Cl22 1.71(2) . ? C902 H90A 0.9900 . ? C902 H90B 0.9900 . ? Cl11 Cl13 2.14(3) 8_454 ? Cl13 Cl11 2.14(3) 2 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C14 C2 C1 111.8(16) . . ? C14 C2 C3 109.2(15) . . ? C1 C2 C3 107.8(13) . . ? C14 C2 Sn1 108.2(10) . 3_655 ? C1 C2 Sn1 110.7(11) . 3_655 ? C3 C2 Sn1 109.1(11) . 3_655 ? C4 C3 C2 118.1(13) . . ? C4 C3 H3A 107.8 . . ? C2 C3 H3A 107.8 . . ? C4 C3 H3B 107.8 . . ? C2 C3 H3B 107.8 . . ? H3A C3 H3B 107.1 . . ? N5 C4 C15 121.6(15) . . ? N5 C4 C3 115.7(14) . . ? C15 C4 C3 122.7(14) . . ? N6 C7 C8 118.0(16) . . ? N6 C7 C16 122.2(15) . . ? C8 C7 C16 119.7(15) . . ? N9 C8 C13 122.8(17) . . ? N9 C8 C7 111.7(15) . . ? C13 C8 C7 125.4(17) . . ? C11 C10 N9 122.6(18) . . ? C11 C10 H10 118.7 . . ? N9 C10 H10 118.7 . . ? C10 C11 C12 118.3(18) . . ? C10 C11 H11 120.9 . . ? C12 C11 H11 120.9 . . ? C11 C12 C13 119.1(17) . . ? C11 C12 H12 120.5 . . ? C13 C12 H12 120.5 . . ? C8 C13 C12 119.7(18) . . ? C8 C13 H13 120.2 . . ? C12 C13 H13 120.2 . . ? C2 C14 H14A 109.5 . . ? C2 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C2 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C4 C15 H15A 109.5 . . ? C4 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C4 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? N17 C16 C21 121.0(17) . . ? N17 C16 C7 115.0(15) . . ? C21 C16 C7 124.0(15) . . ? C19 C18 N17 128(2) . . ? C19 C18 H18 115.9 . . ? N17 C18 H18 115.9 . . ? C18 C19 C20 117(2) . . ? C18 C19 H19 121.7 . . ? C20 C19 H19 121.7 . . ? C21 C20 C19 118(2) . . ? C21 C20 H20 121.2 . . ? C19 C20 H20 121.2 . . ? C20 C21 C16 119.8(17) . . ? C20 C21 H21 120.1 . . ? C16 C21 H21 120.1 . . ? C4 N5 N6 120.6(12) . . ? C7 N6 N5 120.4(14) . . ? C7 N6 Zn1 116.6(12) . . ? N5 N6 Zn1 123.0(9) . . ? C8 N9 C10 117.5(15) . . ? C8 N9 Zn1 116.9(11) . . ? C10 N9 Zn1 125.6(12) . . ? C18 N17 C16 116.1(17) . . ? Zn1 S1 Zn2 99.95(18) . . ? Zn1 S1 Sn1 101.09(15) . . ? Zn2 S1 Sn1 106.96(17) . . ? Zn2 S3 Zn2 108.49(17) 3_655 12_656 ? Zn2 S3 Sn1 115.51(17) 3_655 . ? Zn2 S3 Sn1 113.69(18) 12_656 . ? Sn1 S2 Sn1 105.0(2) . 3_655 ? N6 Zn1 N9 76.7(5) . . ? N6 Zn1 Cl1 108.3(3) . . ? N9 Zn1 Cl1 103.7(4) . . ? N6 Zn1 S1 117.4(3) . . ? N9 Zn1 S1 108.8(3) . . ? Cl1 Zn1 S1 128.4(2) . . ? Cl2 Zn2 S3 104.49(17) . 3_655 ? Cl2 Zn2 S3 105.21(16) . 10_666 ? S3 Zn2 S3 117.46(18) 3_655 10_666 ? Cl2 Zn2 S1 110.00(16) . . ? S3 Zn2 S1 118.51(15) 3_655 . ? S3 Zn2 S1 100.50(15) 10_666 . ? C2 Sn1 S3 114.4(5) 3_655 . ? C2 Sn1 S2 110.4(4) 3_655 . ? S3 Sn1 S2 119.56(14) . . ? C2 Sn1 S1 106.0(5) 3_655 . ? S3 Sn1 S1 104.46(14) . . ? S2 Sn1 S1 99.63(11) . . ? Cl13 C901 Cl11 113(2) . . ? Cl13 C901 Cl12 113(2) . . ? Cl11 C901 Cl12 108(2) . . ? Cl13 C901 H901 107.6 . . ? Cl11 C901 H901 107.6 . . ? Cl12 C901 H901 107.6 . . ? Cl21 C902 Cl22 117(3) . . ? Cl21 C902 H90A 108.0 . . ? Cl22 C902 H90A 108.0 . . ? Cl21 C902 H90B 108.0 . . ? Cl22 C902 H90B 108.0 . . ? H90A C902 H90B 107.3 . . ? C901 Cl11 Cl13 161.6(18) . 8_454 ? C901 Cl13 Cl11 167.5(13) . 2 ? 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 C14 C2 C3 C4 72(2) . . . . ? C1 C2 C3 C4 -166.0(16) . . . . ? Sn1 C2 C3 C4 -45.7(19) 3_655 . . . ? C2 C3 C4 N5 8(2) . . . . ? C2 C3 C4 C15 -174.6(18) . . . . ? N6 C7 C8 N9 1.9(19) . . . . ? C16 C7 C8 N9 -177.5(12) . . . . ? N6 C7 C8 C13 -179.5(14) . . . . ? C16 C7 C8 C13 1(2) . . . . ? N9 C10 C11 C12 2(2) . . . . ? C10 C11 C12 C13 0(2) . . . . ? N9 C8 C13 C12 3(2) . . . . ? C7 C8 C13 C12 -175.7(14) . . . . ? C11 C12 C13 C8 -2(2) . . . . ? N6 C7 C16 N17 -120.1(17) . . . . ? C8 C7 C16 N17 59.3(19) . . . . ? N6 C7 C16 C21 62(2) . . . . ? C8 C7 C16 C21 -119.1(18) . . . . ? N17 C18 C19 C20 -5(4) . . . . ? C18 C19 C20 C21 5(3) . . . . ? C19 C20 C21 C16 -5(3) . . . . ? N17 C16 C21 C20 5(3) . . . . ? C7 C16 C21 C20 -176.3(17) . . . . ? C15 C4 N5 N6 -5(3) . . . . ? C3 C4 N5 N6 172.3(14) . . . . ? C8 C7 N6 N5 179.4(11) . . . . ? C16 C7 N6 N5 -1(2) . . . . ? C8 C7 N6 Zn1 -1.8(16) . . . . ? C16 C7 N6 Zn1 177.6(10) . . . . ? C4 N5 N6 C7 83.9(18) . . . . ? C4 N5 N6 Zn1 -94.9(15) . . . . ? C13 C8 N9 C10 -1(2) . . . . ? C7 C8 N9 C10 177.4(12) . . . . ? C13 C8 N9 Zn1 -179.7(11) . . . . ? C7 C8 N9 Zn1 -1.1(15) . . . . ? C11 C10 N9 C8 -1(2) . . . . ? C11 C10 N9 Zn1 177.2(11) . . . . ? C19 C18 N17 C16 5(3) . . . . ? C21 C16 N17 C18 -5(3) . . . . ? C7 C16 N17 C18 176.6(16) . . . . ? Cl13 C901 Cl11 Cl13 -122(4) . . . 8_454 ? Cl12 C901 Cl11 Cl13 4(8) . . . 8_454 ? Cl11 C901 Cl13 Cl11 -39(13) . . . 2 ? Cl12 C901 Cl13 Cl11 -162(8) . . . 2 ? _refine_diff_density_max 0.810 _refine_diff_density_min -0.468 _refine_diff_density_rms 0.126 _database_code_depnum_ccdc_archive 'CCDC 934168' ####################################################################### # # 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_5 #TrackingRef '19485_web_deposit_cif_file_3_KlausHarms_1366045723.5-bb135.cif' #data_bb135 _vrf_PLAT029_5 ; PROBLEM: _diffrn_measured_fraction_theta_full Low ....... 0.715 RESPONSE: Only data of one twin domain were used ; _vrf_PLAT241_5 ; PROBLEM: Check High Ueq as Compared to Neighbors for C320 RESPONSE: Due to non resolved disorder. ; _vrf_PLAT411_5 ; PROBLEM: Short Inter H...H Contact H20 .. H321 .. 1.79 Ang. RESPONSE: Probably C20 or C321 is the N-atom in the ring. ; # # _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C68 H76 Br8 N16 S10 Sn4 Zn8, C H2 Cl2, C H Cl3' _chemical_formula_sum 'C70 H79 Br8 Cl5 N16 S10 Sn4 Zn8' _chemical_formula_weight 3279.34 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' Br Br -0.2901 2.4595 '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' 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' Sn Sn -0.6537 1.4246 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 16.0625(11) _cell_length_b 18.7495(10) _cell_length_c 20.2991(12) _cell_angle_alpha 85.537(5) _cell_angle_beta 70.132(5) _cell_angle_gamma 70.846(5) _cell_volume 5427.3(6) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9864 _cell_measurement_theta_min 1.42 _cell_measurement_theta_max 25.66 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.11 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.007 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3152 _exptl_absorpt_coefficient_mu 5.940 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.3599 _exptl_absorpt_correction_T_max 0.5370 _exptl_absorpt_process_details XPREP _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 'STOE IPDS-2T' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 6.67 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 31482 _diffrn_reflns_av_R_equivalents 0.1008 _diffrn_reflns_av_sigmaI/netI 0.1715 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.42 _diffrn_reflns_theta_max 25.50 _reflns_number_total 14453 _reflns_number_gt 6506 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'STOE X-AREA' _computing_cell_refinement 'STOE X-AREA' _computing_data_reduction 'STOE X-RED' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'DIAMOND 3.2h' _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0301P)^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 14453 _refine_ls_number_parameters 1129 _refine_ls_number_restraints 419 _refine_ls_R_factor_all 0.1551 _refine_ls_R_factor_gt 0.0589 _refine_ls_wR_factor_ref 0.1188 _refine_ls_wR_factor_gt 0.0938 _refine_ls_goodness_of_fit_ref 0.863 _refine_ls_restrained_S_all 0.855 _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 0.7484(11) 0.2292(9) 0.0256(7) 0.054(4) Uani 1 1 d U . . H1A H 0.7014 0.2328 0.0037 0.081 Uiso 1 1 calc R . . H1B H 0.8111 0.2074 -0.0085 0.081 Uiso 1 1 calc R . . H1C H 0.7411 0.2796 0.0413 0.081 Uiso 1 1 calc R . . C2 C 0.7349(11) 0.1777(9) 0.0895(8) 0.052(3) Uani 1 1 d U . . C3 C 0.8073(10) 0.1734(9) 0.1223(7) 0.047(3) Uani 1 1 d U . . H3A H 0.8066 0.2254 0.1287 0.057 Uiso 1 1 calc R . . H3B H 0.8695 0.1457 0.0890 0.057 Uiso 1 1 calc R . . C4 C 0.7965(12) 0.1360(8) 0.1918(8) 0.049(4) Uani 1 1 d U . . C7 C 0.7319(11) 0.0043(9) 0.2800(8) 0.048(3) Uani 1 1 d U . . C8 C 0.6963(10) -0.0277(9) 0.3516(8) 0.045(3) Uani 1 1 d U . . C10 C 0.6141(11) 0.0017(9) 0.4701(8) 0.048(3) Uani 1 1 d U . . H10 H 0.5778 0.0377 0.5080 0.058 Uiso 1 1 calc R . . C11 C 0.6363(13) -0.0740(11) 0.4823(10) 0.068(5) Uani 1 1 d U . . H11 H 0.6152 -0.0905 0.5287 0.082 Uiso 1 1 calc R . . C12 C 0.6881(11) -0.1256(10) 0.4286(9) 0.053(4) Uani 1 1 d U . . H12 H 0.7032 -0.1778 0.4387 0.064 Uiso 1 1 calc R . . C13 C 0.7196(12) -0.1059(9) 0.3605(9) 0.057(4) Uani 1 1 d U . . H13 H 0.7543 -0.1419 0.3225 0.069 Uiso 1 1 calc R . . C14 C 0.7415(11) 0.1017(9) 0.0634(7) 0.050(4) Uani 1 1 d U . . H14A H 0.7264 0.0699 0.1034 0.076 Uiso 1 1 calc R . . H14B H 0.8052 0.0771 0.0318 0.076 Uiso 1 1 calc R . . H14C H 0.6972 0.1092 0.0381 0.076 Uiso 1 1 calc R . . C15 C 0.8606(11) 0.1362(10) 0.2313(8) 0.066(5) Uani 1 1 d U . . H15A H 0.8714 0.1852 0.2268 0.099 Uiso 1 1 calc R . . H15B H 0.9204 0.0960 0.2119 0.099 Uiso 1 1 calc R . . H15C H 0.8318 0.1278 0.2809 0.099 Uiso 1 1 calc R . . C16 C 0.7985(11) -0.0430(9) 0.2192(8) 0.047(3) Uani 1 1 d U . . C18 C 0.9446(14) -0.0801(10) 0.1386(9) 0.069(5) Uani 1 1 d U . . H18 H 1.0061 -0.0769 0.1206 0.082 Uiso 1 1 calc R . . C19 C 0.9239(13) -0.1292(10) 0.1067(10) 0.069(5) Uani 1 1 d U . . H19 H 0.9697 -0.1576 0.0662 0.083 Uiso 1 1 calc R . . C20 C 0.8372(13) -0.1385(12) 0.1324(9) 0.076(5) Uani 1 1 d U . . H20 H 0.8224 -0.1742 0.1114 0.091 Uiso 1 1 calc R . . C21 C 0.7718(12) -0.0930(9) 0.1909(9) 0.055(4) Uani 1 1 d U . . H21 H 0.7106 -0.0965 0.2106 0.066 Uiso 1 1 calc R . . C121 C 0.4286(14) 0.6213(11) 0.3558(9) 0.074(6) Uani 1 1 d U . . H121 H 0.4912 0.5969 0.3543 0.089 Uiso 1 1 calc R . . C201 C 0.4551(10) 0.3332(8) 0.5100(7) 0.047(4) Uani 1 1 d U . . H20A H 0.4006 0.3157 0.5248 0.070 Uiso 1 1 calc R . . H20B H 0.4533 0.3627 0.5485 0.070 Uiso 1 1 calc R . . H20C H 0.5124 0.2895 0.4973 0.070 Uiso 1 1 calc R . . C202 C 0.4536(10) 0.3831(9) 0.4459(7) 0.043(3) Uani 1 1 d U . . C203 C 0.5385(10) 0.4115(8) 0.4238(6) 0.040(3) Uani 1 1 d U . . H20D H 0.5306 0.4460 0.4616 0.048 Uiso 1 1 calc R . . H20E H 0.5951 0.3676 0.4199 0.048 Uiso 1 1 calc R . . C204 C 0.5551(11) 0.4526(8) 0.3552(8) 0.045(3) Uani 1 1 d U . . C207 C 0.4657(11) 0.5552(9) 0.2499(8) 0.041(3) Uani 1 1 d U . . C208 C 0.4858(11) 0.5772(9) 0.1734(8) 0.050(4) Uani 1 1 d U . . C210 C 0.5517(13) 0.5354(12) 0.0564(8) 0.072(5) Uani 1 1 d U . . H210 H 0.5842 0.4952 0.0220 0.086 Uiso 1 1 calc R . . C211 C 0.5202(16) 0.6096(14) 0.0372(11) 0.088(6) Uani 1 1 d U . . H211 H 0.5340 0.6200 -0.0112 0.106 Uiso 1 1 calc R . . C212 C 0.4702(17) 0.6683(14) 0.0856(12) 0.091(6) Uani 1 1 d U . . H212 H 0.4485 0.7186 0.0716 0.109 Uiso 1 1 calc R . . C213 C 0.4521(13) 0.6513(10) 0.1566(9) 0.065(5) Uani 1 1 d U . . H213 H 0.4174 0.6900 0.1922 0.079 Uiso 1 1 calc R . . C214 C 0.3615(10) 0.4513(8) 0.4671(7) 0.049(4) Uani 1 1 d U . . H21A H 0.3571 0.4814 0.4260 0.074 Uiso 1 1 calc R . . H21B H 0.3615 0.4828 0.5034 0.074 Uiso 1 1 calc R . . H21C H 0.3079 0.4328 0.4852 0.074 Uiso 1 1 calc R . . C215 C 0.6347(10) 0.4811(9) 0.3297(7) 0.046(4) Uani 1 1 d U . . H21D H 0.6739 0.4597 0.2824 0.070 Uiso 1 1 calc R . . H21E H 0.6717 0.4663 0.3612 0.070 Uiso 1 1 calc R . . H21F H 0.6119 0.5363 0.3284 0.070 Uiso 1 1 calc R . . C216 C 0.4008(12) 0.6069(10) 0.3069(9) 0.060(4) Uani 1 1 d U . . C218 C 0.2472(12) 0.6984(10) 0.3614(10) 0.069(5) Uani 1 1 d U . . H218 H 0.1853 0.7262 0.3631 0.082 Uiso 1 1 calc R . . C219 C 0.2817(14) 0.7041(13) 0.4153(11) 0.096(7) Uani 1 1 d U . . H219 H 0.2405 0.7328 0.4571 0.115 Uiso 1 1 calc R . . C220 C 0.3688(15) 0.6708(14) 0.4085(12) 0.107(9) Uani 1 1 d U . . H220 H 0.3916 0.6820 0.4426 0.128 Uiso 1 1 calc R . . C301 C -0.0520(10) 0.4681(9) 0.2466(8) 0.051(4) Uani 1 1 d U . . H30A H -0.0861 0.4390 0.2810 0.077 Uiso 1 1 calc R . . H30B H -0.0957 0.5067 0.2281 0.077 Uiso 1 1 calc R . . H30C H -0.0228 0.4925 0.2692 0.077 Uiso 1 1 calc R . . C302 C 0.0228(12) 0.4156(9) 0.1871(8) 0.051(3) Uani 1 1 d U . . C303 C -0.0218(12) 0.3716(10) 0.1539(9) 0.062(4) Uani 1 1 d U . . H30D H -0.0670 0.3540 0.1925 0.074 Uiso 1 1 calc R . . H30E H -0.0576 0.4075 0.1272 0.074 Uiso 1 1 calc R . . C304 C 0.0439(11) 0.3049(9) 0.1063(8) 0.052(4) Uani 1 1 d U . . C307 C 0.2419(10) 0.2245(9) 0.0019(8) 0.044(3) Uani 1 1 d U . . C308 C 0.3121(10) 0.1543(9) -0.0338(8) 0.046(4) Uani 1 1 d U . . C310 C 0.3814(11) 0.0247(9) -0.0261(8) 0.050(4) Uani 1 1 d U . . H310 H 0.3863 -0.0194 0.0007 0.059 Uiso 1 1 calc R . . C311 C 0.4382(12) 0.0187(10) -0.0950(8) 0.054(4) Uani 1 1 d U . . H311 H 0.4802 -0.0292 -0.1154 0.065 Uiso 1 1 calc R . . C312 C 0.4340(13) 0.0819(10) -0.1341(9) 0.061(4) Uani 1 1 d U . . H312 H 0.4740 0.0788 -0.1814 0.073 Uiso 1 1 calc R . . C313 C 0.3705(12) 0.1500(9) -0.1034(8) 0.052(4) Uani 1 1 d U . . H313 H 0.3663 0.1944 -0.1298 0.063 Uiso 1 1 calc R . . C314 C 0.0813(10) 0.4579(9) 0.1316(7) 0.052(4) Uani 1 1 d U . . H31A H 0.1064 0.4858 0.1547 0.078 Uiso 1 1 calc R . . H31B H 0.0415 0.4934 0.1080 0.078 Uiso 1 1 calc R . . H31C H 0.1331 0.4213 0.0969 0.078 Uiso 1 1 calc R . . C315 C 0.0043(12) 0.2672(10) 0.0673(9) 0.067(5) Uani 1 1 d U . . H31D H 0.0315 0.2727 0.0169 0.100 Uiso 1 1 calc R . . H31E H -0.0638 0.2908 0.0821 0.100 Uiso 1 1 calc R . . H31F H 0.0193 0.2134 0.0776 0.100 Uiso 1 1 calc R . . C316 C 0.2289(11) 0.2970(9) -0.0338(8) 0.050(4) Uani 1 1 d U . . C318 C 0.2538(12) 0.4143(9) -0.0635(10) 0.067(5) Uani 1 1 d U . . H318 H 0.2802 0.4518 -0.0603 0.081 Uiso 1 1 calc R . . C319 C 0.2005(16) 0.4244(12) -0.1033(14) 0.111(9) Uani 1 1 d U . . H319 H 0.1864 0.4711 -0.1257 0.133 Uiso 1 1 calc R . . C320 C 0.165(2) 0.3715(14) -0.1137(17) 0.158(14) Uani 1 1 d U . . H320 H 0.1329 0.3791 -0.1463 0.189 Uiso 1 1 calc R . . C321 C 0.1771(14) 0.3057(9) -0.0760(10) 0.080(6) Uani 1 1 d U . . H321 H 0.1501 0.2687 -0.0798 0.096 Uiso 1 1 calc R . . C401 C 0.2086(13) -0.0336(9) 0.2730(8) 0.058(4) Uani 1 1 d U . . H40A H 0.1801 -0.0111 0.2374 0.088 Uiso 1 1 calc R . . H40B H 0.1888 -0.0774 0.2917 0.088 Uiso 1 1 calc R . . H40C H 0.2768 -0.0498 0.2518 0.088 Uiso 1 1 calc R . . C402 C 0.1776(12) 0.0243(9) 0.3320(8) 0.048(3) Uani 1 1 d U . . C403 C 0.0697(11) 0.0447(9) 0.3710(8) 0.048(3) Uani 1 1 d U . . H40D H 0.0391 0.0513 0.3349 0.057 Uiso 1 1 calc R . . H40E H 0.0585 0.0006 0.3982 0.057 Uiso 1 1 calc R . . C404 C 0.0220(10) 0.1113(8) 0.4184(7) 0.039(3) Uani 1 1 d U . . C407 C 0.0106(10) 0.2356(9) 0.5204(8) 0.046(3) Uani 1 1 d U . . C408 C -0.0323(11) 0.3152(10) 0.5454(9) 0.051(4) Uani 1 1 d U . . C410 C -0.1033(12) 0.4396(10) 0.5244(9) 0.062(5) Uani 1 1 d U . . H410 H -0.1254 0.4759 0.4937 0.075 Uiso 1 1 calc R . . C411 C -0.1168(12) 0.4632(10) 0.5909(8) 0.057(4) Uani 1 1 d U . . H411 H -0.1465 0.5152 0.6047 0.069 Uiso 1 1 calc R . . C412 C -0.0886(12) 0.4137(10) 0.6364(9) 0.061(4) Uani 1 1 d U . . H412 H -0.0993 0.4292 0.6828 0.074 Uiso 1 1 calc R . . C413 C -0.0431(11) 0.3386(10) 0.6129(9) 0.054(4) Uani 1 1 d U . . H413 H -0.0188 0.3026 0.6429 0.065 Uiso 1 1 calc R . . C414 C 0.2307(11) -0.0081(9) 0.3831(7) 0.049(4) Uani 1 1 d U . . H41A H 0.2980 -0.0211 0.3581 0.074 Uiso 1 1 calc R . . H41B H 0.2161 -0.0536 0.4032 0.074 Uiso 1 1 calc R . . H41C H 0.2119 0.0296 0.4207 0.074 Uiso 1 1 calc R . . C415 C -0.0786(11) 0.1270(9) 0.4602(8) 0.060(4) Uani 1 1 d U . . H41D H -0.0998 0.0868 0.4506 0.090 Uiso 1 1 calc R . . H41E H -0.1152 0.1756 0.4472 0.090 Uiso 1 1 calc R . . H41F H -0.0870 0.1291 0.5102 0.090 Uiso 1 1 calc R . . C416 C 0.0354(11) 0.1727(9) 0.5662(8) 0.050(3) Uani 1 1 d U . . C418 C -0.0094(12) 0.1163(10) 0.6693(9) 0.061(4) Uani 1 1 d U . . H418 H -0.0531 0.1180 0.7151 0.073 Uiso 1 1 calc R . . C419 C 0.0696(13) 0.0556(10) 0.6503(9) 0.062(4) Uani 1 1 d U . . H419 H 0.0796 0.0153 0.6810 0.074 Uiso 1 1 calc R . . C420 C 0.1331(13) 0.0544(9) 0.5870(9) 0.063(5) Uani 1 1 d U . . H420 H 0.1883 0.0120 0.5721 0.076 Uiso 1 1 calc R . . C421 C 0.1195(13) 0.1140(9) 0.5427(9) 0.058(4) Uani 1 1 d U . . H421 H 0.1654 0.1148 0.4985 0.069 Uiso 1 1 calc R . . N5 N 0.7288(9) 0.1118(7) 0.2146(6) 0.050(3) Uani 1 1 d U . . N6 N 0.7078(9) 0.0796(7) 0.2822(6) 0.046(3) Uani 1 1 d U . . N9 N 0.6446(8) 0.0255(7) 0.4029(7) 0.049(3) Uani 1 1 d U . . N17 N 0.8830(9) -0.0353(8) 0.1945(7) 0.055(3) Uani 1 1 d U . . N205 N 0.4976(8) 0.4542(7) 0.3233(6) 0.040(3) Uani 1 1 d U . . N206 N 0.5129(9) 0.4840(7) 0.2558(6) 0.048(3) Uani 1 1 d U . . N209 N 0.5346(10) 0.5219(8) 0.1258(6) 0.053(3) Uani 1 1 d U . . N217 N 0.3135(12) 0.6466(11) 0.3030(10) 0.102(6) Uani 1 1 d U . . N305 N 0.1285(10) 0.2850(7) 0.1048(7) 0.052(3) Uani 1 1 d U . . N306 N 0.1913(10) 0.2184(7) 0.0668(7) 0.049(3) Uani 1 1 d U . . N309 N 0.3182(9) 0.0917(7) 0.0050(6) 0.050(3) Uani 1 1 d U . . N317 N 0.2709(11) 0.3481(9) -0.0264(8) 0.076(4) Uani 1 1 d U . . N405 N 0.0671(10) 0.1557(7) 0.4184(7) 0.049(3) Uani 1 1 d U . . N406 N 0.0225(9) 0.2264(7) 0.4534(7) 0.045(3) Uani 1 1 d U . . N409 N -0.0588(9) 0.3651(8) 0.5005(7) 0.055(3) Uani 1 1 d U . . N417 N -0.0301(9) 0.1743(8) 0.6277(7) 0.057(3) Uani 1 1 d U . . S1 S 0.6139(3) 0.2851(2) 0.2677(2) 0.0479(10) Uani 1 1 d U . . S2 S 0.5171(3) 0.3442(2) 0.12676(19) 0.0462(9) Uani 1 1 d U . . S3 S 0.5029(3) 0.1485(2) 0.19917(19) 0.0457(9) Uani 1 1 d U . . S4 S 0.4649(3) 0.1929(2) 0.39984(19) 0.0441(9) Uani 1 1 d U . . S5 S 0.3295(3) 0.3720(2) 0.32046(19) 0.0431(9) Uani 1 1 d U . . S6 S 0.2880(3) 0.3118(2) 0.15889(19) 0.0439(9) Uani 1 1 d U . . S7 S 0.0938(3) 0.3767(2) 0.3430(2) 0.0478(10) Uani 1 1 d U . . S8 S 0.0806(3) 0.2162(2) 0.2589(2) 0.0502(10) Uani 1 1 d U . . S9 S 0.3226(3) 0.0905(2) 0.17457(19) 0.0453(9) Uani 1 1 d U . . S10 S 0.2730(3) 0.1753(2) 0.36000(19) 0.0433(9) Uani 1 1 d U . . Zn1 Zn 0.62219(13) 0.13708(11) 0.37585(9) 0.0472(5) Uani 1 1 d U . . Zn2 Zn 0.58486(13) 0.41631(12) 0.16528(9) 0.0499(5) Uani 1 1 d U . . Zn3 Zn 0.22818(12) 0.10985(10) 0.10699(9) 0.0464(4) Uani 1 1 d U . . Zn4 Zn -0.02212(13) 0.32477(10) 0.40061(9) 0.0506(5) Uani 1 1 d U . . Zn5 Zn 0.43695(12) 0.13186(10) 0.31738(8) 0.0421(4) Uani 1 1 d U . . Zn6 Zn 0.38925(12) 0.18811(10) 0.14350(9) 0.0447(4) Uani 1 1 d U . . Zn7 Zn 0.35969(13) 0.38173(10) 0.20023(9) 0.0445(4) Uani 1 1 d U . . Zn8 Zn 0.22208(12) 0.30677(10) 0.37704(9) 0.0440(4) Uani 1 1 d U . . Br1 Br 0.70023(13) 0.18342(11) 0.43231(10) 0.0671(5) Uani 1 1 d U . . Br2 Br 0.74783(11) 0.39345(10) 0.12845(8) 0.0536(4) Uani 1 1 d U . . Br3 Br 0.11705(12) 0.04982(11) 0.11818(9) 0.0644(5) Uani 1 1 d U . . Br4 Br -0.15900(12) 0.33536(10) 0.37823(9) 0.0610(5) Uani 1 1 d U . . Br5 Br 0.48802(11) -0.00346(9) 0.32827(8) 0.0473(4) Uani 1 1 d U . . Br6 Br 0.48260(11) 0.17690(9) 0.02152(8) 0.0492(4) Uani 1 1 d U . . Br7 Br 0.29510(12) 0.51212(9) 0.17658(9) 0.0579(5) Uani 1 1 d U . . Br8 Br 0.19211(11) 0.32582(9) 0.49957(8) 0.0504(4) Uani 1 1 d U . . Sn1 Sn 0.59977(7) 0.22687(6) 0.17002(5) 0.0435(3) Uani 1 1 d U . . Sn2 Sn 0.46172(7) 0.31979(6) 0.35832(5) 0.0413(3) Uani 1 1 d U . . Sn3 Sn 0.12670(7) 0.32834(6) 0.22525(6) 0.0453(3) Uani 1 1 d U . . Sn4 Sn 0.20654(7) 0.12720(6) 0.29154(5) 0.0437(3) Uani 1 1 d U . . C903 C 0.0972(15) 0.6627(12) 0.1592(10) 0.085(5) Uani 1 1 d U . . H903 H 0.1373 0.6137 0.1711 0.102 Uiso 1 1 calc R . . Cl5 Cl 0.1055(5) 0.6547(3) 0.0743(3) 0.107(2) Uani 1 1 d U . . Cl6 Cl -0.0201(5) 0.6770(4) 0.2161(3) 0.116(2) Uani 1 1 d U . . Cl7 Cl 0.1353(5) 0.7340(3) 0.1765(3) 0.1088(19) Uani 1 1 d U . . C902 C 0.4645(15) 0.2609(17) 0.716(2) 0.23(3) Uani 0.50 1 d PDU A 2 H90C H 0.4866 0.2924 0.6772 0.275 Uiso 0.50 1 calc PR A 2 H90D H 0.4312 0.2340 0.6997 0.275 Uiso 0.50 1 calc PR A 2 Cl3 Cl 0.5606(10) 0.1943(7) 0.7178(6) 0.109(4) Uani 0.50 1 d PDU A 2 Cl4 Cl 0.3806(13) 0.3223(9) 0.7761(8) 0.146(5) Uani 0.50 1 d PDU A 2 C901 C 0.364(2) 0.3000(15) 0.7061(17) 0.125(13) Uani 0.50 1 d PDU B 1 H90A H 0.4083 0.3274 0.6807 0.150 Uiso 0.50 1 calc PR B 1 H90B H 0.3460 0.3108 0.7569 0.150 Uiso 0.50 1 calc PR B 1 Cl1 Cl 0.4145(14) 0.2122(8) 0.6899(7) 0.143(6) Uani 0.50 1 d PDU B 1 Cl2 Cl 0.2712(11) 0.3304(10) 0.6824(8) 0.148(5) Uani 0.50 1 d PDU B 1 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.055(10) 0.063(10) 0.044(8) 0.012(7) -0.017(6) -0.020(8) C2 0.061(7) 0.052(8) 0.043(7) 0.010(5) -0.019(5) -0.017(6) C3 0.043(7) 0.053(10) 0.044(8) 0.011(6) -0.014(6) -0.016(7) C4 0.059(10) 0.036(9) 0.062(9) 0.017(7) -0.035(8) -0.017(7) C7 0.045(8) 0.046(6) 0.055(7) 0.010(4) -0.019(6) -0.014(7) C8 0.042(9) 0.053(6) 0.052(6) 0.016(5) -0.026(6) -0.025(7) C10 0.043(9) 0.067(8) 0.048(7) 0.009(6) -0.019(7) -0.031(8) C11 0.074(13) 0.078(10) 0.063(9) 0.028(7) -0.038(9) -0.030(10) C12 0.049(10) 0.050(8) 0.076(10) 0.030(6) -0.037(8) -0.026(8) C13 0.060(11) 0.054(7) 0.068(8) 0.019(7) -0.036(8) -0.021(8) C14 0.056(10) 0.059(8) 0.037(9) 0.005(6) -0.017(7) -0.019(7) C15 0.042(10) 0.092(14) 0.063(10) -0.002(9) -0.029(8) -0.008(9) C16 0.049(8) 0.046(9) 0.050(8) 0.013(6) -0.023(6) -0.018(7) C18 0.062(10) 0.058(12) 0.076(12) -0.007(8) -0.016(8) -0.010(8) C19 0.065(9) 0.057(12) 0.079(12) -0.003(8) -0.028(8) -0.005(9) C20 0.062(10) 0.103(15) 0.072(12) -0.019(9) -0.044(9) -0.013(9) C21 0.045(8) 0.055(11) 0.073(11) 0.001(7) -0.036(7) -0.009(7) C121 0.057(10) 0.092(15) 0.058(11) -0.014(8) -0.016(8) -0.005(9) C201 0.041(9) 0.059(10) 0.035(7) 0.010(6) -0.013(7) -0.011(7) C202 0.038(7) 0.052(7) 0.038(6) 0.007(5) -0.018(5) -0.010(5) C203 0.055(8) 0.041(9) 0.028(7) 0.001(5) -0.019(6) -0.013(6) C204 0.065(10) 0.031(9) 0.052(8) 0.006(6) -0.031(7) -0.021(7) C207 0.059(9) 0.040(7) 0.049(6) 0.013(4) -0.036(6) -0.031(6) C208 0.055(10) 0.059(7) 0.049(6) 0.017(5) -0.036(7) -0.020(7) C210 0.083(14) 0.113(12) 0.038(7) 0.026(7) -0.020(9) -0.062(11) C211 0.111(19) 0.136(14) 0.060(10) 0.057(8) -0.062(12) -0.069(14) C212 0.108(19) 0.111(13) 0.092(12) 0.057(9) -0.071(14) -0.057(13) C213 0.096(14) 0.060(8) 0.077(9) 0.032(7) -0.057(10) -0.048(9) C214 0.048(8) 0.053(9) 0.041(9) 0.007(6) -0.013(7) -0.013(6) C215 0.053(9) 0.057(11) 0.045(9) 0.016(7) -0.032(7) -0.024(7) C216 0.038(8) 0.072(11) 0.059(8) 0.006(7) -0.015(7) -0.007(7) C218 0.035(9) 0.065(12) 0.100(13) 0.009(9) -0.020(8) -0.012(7) C219 0.050(10) 0.124(19) 0.091(14) -0.018(12) -0.021(10) 0.004(11) C220 0.062(11) 0.14(2) 0.104(16) -0.049(13) -0.040(12) 0.011(12) C301 0.040(8) 0.055(10) 0.063(9) -0.004(7) -0.029(6) -0.007(6) C302 0.053(8) 0.042(7) 0.056(9) -0.002(5) -0.029(6) 0.001(6) C303 0.049(9) 0.062(11) 0.070(12) -0.019(7) -0.027(8) 0.000(6) C304 0.051(8) 0.054(10) 0.052(10) -0.007(6) -0.032(8) -0.001(7) C307 0.037(8) 0.047(6) 0.057(7) 0.004(5) -0.028(6) -0.014(6) C308 0.027(8) 0.046(7) 0.060(7) 0.012(6) -0.019(5) -0.004(6) C310 0.042(9) 0.049(8) 0.066(8) 0.012(6) -0.028(6) -0.017(6) C311 0.051(10) 0.058(9) 0.058(8) -0.002(7) -0.027(7) -0.014(8) C312 0.062(11) 0.075(10) 0.048(9) 0.003(6) -0.020(7) -0.023(8) C313 0.069(11) 0.055(8) 0.043(7) 0.010(6) -0.027(6) -0.024(7) C314 0.047(9) 0.058(10) 0.050(8) 0.002(6) -0.031(6) 0.001(7) C315 0.052(10) 0.059(12) 0.097(14) -0.023(9) -0.035(10) -0.011(9) C316 0.046(10) 0.040(7) 0.069(10) 0.002(6) -0.031(7) -0.007(6) C318 0.061(11) 0.044(9) 0.113(15) 0.023(9) -0.053(10) -0.018(8) C319 0.112(18) 0.076(14) 0.21(3) 0.081(15) -0.122(17) -0.058(13) C320 0.22(3) 0.12(2) 0.28(3) 0.14(2) -0.22(3) -0.12(2) C321 0.115(16) 0.034(10) 0.137(17) 0.028(9) -0.101(14) -0.027(10) C401 0.081(12) 0.048(8) 0.051(9) 0.004(6) -0.014(7) -0.036(9) C402 0.057(8) 0.045(7) 0.041(8) 0.001(5) -0.011(5) -0.019(6) C403 0.060(7) 0.048(9) 0.045(9) 0.010(5) -0.021(6) -0.027(6) C404 0.039(7) 0.047(8) 0.036(8) 0.010(6) -0.013(6) -0.021(6) C407 0.032(8) 0.059(7) 0.047(6) -0.001(5) -0.013(7) -0.016(7) C408 0.041(10) 0.059(7) 0.058(7) -0.003(6) -0.018(8) -0.022(8) C410 0.060(12) 0.065(8) 0.070(9) -0.007(7) -0.037(10) -0.014(9) C411 0.065(12) 0.062(9) 0.062(9) 0.001(7) -0.033(9) -0.030(9) C412 0.056(11) 0.075(10) 0.055(9) -0.004(7) -0.018(9) -0.022(9) C413 0.046(10) 0.062(9) 0.060(8) -0.003(7) -0.018(8) -0.025(8) C414 0.050(9) 0.054(10) 0.045(8) 0.014(7) -0.009(7) -0.027(8) C415 0.057(8) 0.060(11) 0.060(10) 0.005(8) -0.009(7) -0.026(8) C416 0.051(9) 0.062(8) 0.055(8) 0.007(7) -0.032(6) -0.028(6) C418 0.063(10) 0.077(12) 0.051(9) 0.008(7) -0.023(7) -0.029(8) C419 0.073(11) 0.064(10) 0.069(10) 0.012(8) -0.046(8) -0.028(7) C420 0.068(11) 0.043(9) 0.076(10) -0.012(7) -0.030(7) -0.004(8) C421 0.068(9) 0.055(10) 0.064(10) -0.003(7) -0.032(7) -0.025(7) N5 0.067(9) 0.053(8) 0.046(6) 0.016(5) -0.034(6) -0.025(7) N6 0.044(7) 0.047(6) 0.050(6) 0.011(4) -0.016(5) -0.019(5) N9 0.033(7) 0.062(6) 0.055(6) 0.015(5) -0.017(6) -0.018(5) N17 0.040(7) 0.058(9) 0.061(8) 0.006(6) -0.013(6) -0.012(6) N205 0.043(7) 0.048(8) 0.031(5) 0.007(5) -0.016(5) -0.015(6) N206 0.061(8) 0.043(6) 0.039(5) 0.012(4) -0.017(5) -0.018(5) N209 0.067(8) 0.070(6) 0.039(5) 0.017(5) -0.028(6) -0.035(6) N217 0.060(9) 0.117(16) 0.120(13) -0.023(10) -0.035(9) -0.008(8) N305 0.051(7) 0.047(7) 0.061(8) -0.008(6) -0.033(6) -0.004(6) N306 0.053(8) 0.047(6) 0.054(7) -0.010(4) -0.031(5) -0.006(5) N309 0.050(7) 0.050(6) 0.049(5) 0.011(5) -0.023(5) -0.012(5) N317 0.084(11) 0.076(10) 0.097(12) 0.033(8) -0.050(9) -0.049(9) N405 0.054(8) 0.045(6) 0.056(8) 0.003(5) -0.029(7) -0.016(6) N406 0.031(7) 0.050(6) 0.048(6) -0.001(4) -0.010(6) -0.009(5) N409 0.046(8) 0.056(6) 0.070(6) -0.007(5) -0.027(5) -0.015(7) N417 0.054(8) 0.071(9) 0.060(7) 0.014(6) -0.033(5) -0.028(7) S1 0.043(2) 0.058(3) 0.044(2) 0.0066(18) -0.0178(18) -0.017(2) S2 0.053(2) 0.052(2) 0.043(2) 0.0147(18) -0.0271(18) -0.0209(19) S3 0.046(2) 0.052(3) 0.043(2) 0.0105(18) -0.0212(18) -0.0168(19) S4 0.046(2) 0.047(2) 0.044(2) 0.0111(17) -0.0219(18) -0.0160(18) S5 0.044(2) 0.047(2) 0.044(2) 0.0044(17) -0.0233(17) -0.0129(18) S6 0.050(2) 0.043(2) 0.047(2) 0.0053(17) -0.0289(18) -0.0129(18) S7 0.044(2) 0.045(2) 0.059(2) 0.0031(18) -0.0270(19) -0.0105(18) S8 0.046(2) 0.045(2) 0.067(3) 0.0009(19) -0.029(2) -0.0136(18) S9 0.044(2) 0.046(2) 0.046(2) 0.0001(17) -0.0167(17) -0.0121(18) S10 0.039(2) 0.044(2) 0.049(2) 0.0049(17) -0.0190(18) -0.0129(17) Zn1 0.0454(11) 0.0537(12) 0.0471(11) 0.0083(9) -0.0227(9) -0.0157(9) Zn2 0.0520(12) 0.0630(13) 0.0430(11) 0.0052(9) -0.0215(9) -0.0240(10) Zn3 0.0422(11) 0.0487(11) 0.0519(11) 0.0001(8) -0.0194(9) -0.0152(9) Zn4 0.0460(11) 0.0493(12) 0.0596(12) 0.0027(9) -0.0235(9) -0.0134(9) Zn5 0.0430(10) 0.0452(11) 0.0427(10) 0.0071(8) -0.0204(8) -0.0149(8) Zn6 0.0474(11) 0.0443(11) 0.0478(10) 0.0097(8) -0.0233(9) -0.0159(9) Zn7 0.0510(11) 0.0446(11) 0.0478(10) 0.0108(8) -0.0282(9) -0.0178(9) Zn8 0.0440(10) 0.0435(11) 0.0501(11) 0.0063(8) -0.0231(9) -0.0144(8) Br1 0.0651(12) 0.0714(13) 0.0847(13) 0.0075(10) -0.0476(10) -0.0247(10) Br2 0.0523(10) 0.0570(11) 0.0589(10) 0.0137(8) -0.0248(8) -0.0230(8) Br3 0.0517(11) 0.0728(13) 0.0742(12) -0.0121(9) -0.0161(9) -0.0287(9) Br4 0.0476(10) 0.0625(12) 0.0776(12) 0.0057(9) -0.0292(9) -0.0158(9) Br5 0.0492(9) 0.0447(10) 0.0504(9) 0.0078(7) -0.0223(8) -0.0135(7) Br6 0.0564(10) 0.0521(10) 0.0457(9) 0.0145(7) -0.0246(8) -0.0208(8) Br7 0.0629(11) 0.0472(10) 0.0780(12) 0.0197(8) -0.0424(9) -0.0202(8) Br8 0.0509(10) 0.0562(11) 0.0491(9) 0.0056(7) -0.0232(8) -0.0178(8) Sn1 0.0442(6) 0.0497(7) 0.0409(6) 0.0098(5) -0.0194(5) -0.0169(5) Sn2 0.0463(6) 0.0432(7) 0.0407(6) 0.0078(5) -0.0226(5) -0.0157(5) Sn3 0.0448(6) 0.0420(7) 0.0540(7) 0.0024(5) -0.0252(5) -0.0112(5) Sn4 0.0443(6) 0.0421(7) 0.0474(6) 0.0022(5) -0.0176(5) -0.0149(5) C903 0.092(10) 0.097(15) 0.088(9) 0.024(11) -0.052(9) -0.039(12) Cl5 0.155(6) 0.105(5) 0.091(4) 0.027(3) -0.066(4) -0.062(4) Cl6 0.100(4) 0.135(6) 0.108(4) 0.020(4) -0.039(3) -0.030(4) Cl7 0.143(6) 0.096(5) 0.107(4) -0.002(3) -0.061(4) -0.042(4) C902 0.20(4) 0.19(4) 0.17(3) 0.06(3) 0.00(3) 0.02(3) Cl3 0.153(11) 0.090(9) 0.124(10) 0.030(7) -0.070(8) -0.073(7) Cl4 0.193(15) 0.138(13) 0.122(11) 0.019(9) -0.056(10) -0.075(9) C901 0.13(3) 0.185(18) 0.04(2) -0.02(2) 0.01(2) -0.05(3) Cl1 0.290(18) 0.128(10) 0.120(11) 0.067(8) -0.144(12) -0.140(10) Cl2 0.124(11) 0.182(14) 0.143(12) -0.011(11) -0.010(9) -0.085(9) _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 C2 1.55(2) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 C3 1.50(2) . ? C2 C14 1.52(2) . ? C2 Sn1 2.177(16) . ? C3 C4 1.506(19) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 N5 1.247(19) . ? C4 C15 1.51(2) . ? C7 N6 1.336(18) . ? C7 C16 1.45(2) . ? C7 C8 1.52(2) . ? C8 N9 1.342(19) . ? C8 C13 1.40(2) . ? C10 C11 1.37(2) . ? C10 N9 1.377(17) . ? C10 H10 0.9500 . ? C11 C12 1.36(2) . ? C11 H11 0.9500 . ? C12 C13 1.37(2) . ? C12 H12 0.9500 . ? C13 H13 0.9500 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 N17 1.33(2) . ? C16 C21 1.38(2) . ? C18 N17 1.35(2) . ? C18 C19 1.35(3) . ? C18 H18 0.9500 . ? C19 C20 1.38(3) . ? C19 H19 0.9500 . ? C20 C21 1.40(2) . ? C20 H20 0.9500 . ? C21 H21 0.9500 . ? C121 C216 1.29(2) . ? C121 C220 1.34(2) . ? C121 H121 0.9500 . ? C201 C202 1.544(18) . ? C201 H20A 0.9800 . ? C201 H20B 0.9800 . ? C201 H20C 0.9800 . ? C202 C203 1.54(2) . ? C202 C214 1.557(18) . ? C202 Sn2 2.158(15) . ? C203 C204 1.524(18) . ? C203 H20D 0.9900 . ? C203 H20E 0.9900 . ? C204 N205 1.288(18) . ? C204 C215 1.46(2) . ? C207 N206 1.320(17) . ? C207 C216 1.43(2) . ? C207 C208 1.528(19) . ? C208 N209 1.316(19) . ? C208 C213 1.38(2) . ? C210 N209 1.360(18) . ? C210 C211 1.39(3) . ? C210 H210 0.9500 . ? C211 C212 1.37(3) . ? C211 H211 0.9500 . ? C212 C213 1.40(2) . ? C212 H212 0.9500 . ? C213 H213 0.9500 . ? C214 H21A 0.9800 . ? C214 H21B 0.9800 . ? C214 H21C 0.9800 . ? C215 H21D 0.9800 . ? C215 H21E 0.9800 . ? C215 H21F 0.9800 . ? C216 N217 1.38(2) . ? C218 C219 1.41(3) . ? C218 N217 1.46(2) . ? C218 H218 0.9500 . ? C219 C220 1.29(3) . ? C219 H219 0.9500 . ? C220 H220 0.9500 . ? C301 C302 1.514(19) . ? C301 H30A 0.9800 . ? C301 H30B 0.9800 . ? C301 H30C 0.9800 . ? C302 C314 1.55(2) . ? C302 C303 1.56(2) . ? C302 Sn3 2.225(15) . ? C303 C304 1.50(2) . ? C303 H30D 0.9900 . ? C303 H30E 0.9900 . ? C304 N305 1.276(19) . ? C304 C315 1.50(2) . ? C307 N306 1.310(19) . ? C307 C308 1.47(2) . ? C307 C316 1.48(2) . ? C308 N309 1.356(18) . ? C308 C313 1.40(2) . ? C310 N309 1.363(19) . ? C310 C311 1.38(2) . ? C310 H310 0.9500 . ? C311 C312 1.37(2) . ? C311 H311 0.9500 . ? C312 C313 1.38(2) . ? C312 H312 0.9500 . ? C313 H313 0.9500 . ? C314 H31A 0.9800 . ? C314 H31B 0.9800 . ? C314 H31C 0.9800 . ? C315 H31D 0.9800 . ? C315 H31E 0.9800 . ? C315 H31F 0.9800 . ? C316 C321 1.35(2) . ? C316 N317 1.38(2) . ? C318 C319 1.33(2) . ? C318 N317 1.40(2) . ? C318 H318 0.9500 . ? C319 C320 1.35(3) . ? C319 H319 0.9500 . ? C320 C321 1.39(2) . ? C320 H320 0.9500 . ? C321 H321 0.9500 . ? C401 C402 1.52(2) . ? C401 H40A 0.9800 . ? C401 H40B 0.9800 . ? C401 H40C 0.9800 . ? C402 C414 1.53(2) . ? C402 C403 1.57(2) . ? C402 Sn4 2.166(16) . ? C403 C404 1.460(19) . ? C403 H40D 0.9900 . ? C403 H40E 0.9900 . ? C404 N405 1.271(19) . ? C404 C415 1.49(2) . ? C407 N406 1.323(18) . ? C407 C408 1.47(2) . ? C407 C416 1.48(2) . ? C408 N409 1.33(2) . ? C408 C413 1.41(2) . ? C410 C411 1.38(2) . ? C410 N409 1.38(2) . ? C410 H410 0.9500 . ? C411 C412 1.34(2) . ? C411 H411 0.9500 . ? C412 C413 1.39(2) . ? C412 H412 0.9500 . ? C413 H413 0.9500 . ? C414 H41A 0.9800 . ? C414 H41B 0.9800 . ? C414 H41C 0.9800 . ? C415 H41D 0.9800 . ? C415 H41E 0.9800 . ? C415 H41F 0.9800 . ? C416 N417 1.326(19) . ? C416 C421 1.39(2) . ? C418 N417 1.349(19) . ? C418 C419 1.36(2) . ? C418 H418 0.9500 . ? C419 C420 1.34(2) . ? C419 H419 0.9500 . ? C420 C421 1.39(2) . ? C420 H420 0.9500 . ? C421 H421 0.9500 . ? N5 N6 1.432(15) . ? N6 Zn1 2.057(13) . ? N9 Zn1 2.066(13) . ? N205 N206 1.413(15) . ? N206 Zn2 2.069(13) . ? N209 Zn2 2.088(13) . ? N305 N306 1.403(17) . ? N306 Zn3 2.106(14) . ? N309 Zn3 2.060(13) . ? N405 N406 1.397(18) . ? N406 Zn4 2.101(13) . ? N409 Zn4 2.041(14) . ? S1 Sn2 2.423(4) . ? S1 Sn1 2.445(4) . ? S2 Zn2 2.310(5) . ? S2 Zn7 2.354(4) . ? S2 Sn1 2.439(4) . ? S3 Zn5 2.313(4) . ? S3 Zn6 2.354(4) . ? S3 Sn1 2.381(4) . ? S4 Zn1 2.286(4) . ? S4 Zn5 2.336(4) . ? S4 Sn2 2.452(4) . ? S5 Zn7 2.326(4) . ? S5 Zn8 2.370(5) . ? S5 Sn2 2.385(4) . ? S6 Zn6 2.327(4) . ? S6 Zn7 2.359(4) . ? S6 Sn3 2.406(4) . ? S7 Zn4 2.305(5) . ? S7 Zn8 2.344(4) . ? S7 Sn3 2.445(4) . ? S8 Sn4 2.417(4) . ? S8 Sn3 2.427(4) . ? S9 Zn3 2.300(4) . ? S9 Zn6 2.354(5) . ? S9 Sn4 2.447(4) . ? S10 Zn8 2.341(4) . ? S10 Zn5 2.345(4) . ? S10 Sn4 2.392(4) . ? Zn1 Br1 2.342(3) . ? Zn2 Br2 2.362(3) . ? Zn3 Br3 2.347(3) . ? Zn4 Br4 2.336(2) . ? Zn5 Br5 2.414(2) . ? Zn6 Br6 2.403(2) . ? Zn7 Br7 2.403(2) . ? Zn8 Br8 2.399(2) . ? C903 Cl5 1.697(19) . ? C903 Cl7 1.74(2) . ? C903 Cl6 1.79(2) . ? C903 H903 1.0000 . ? C902 Cl4 1.643(17) . ? C902 Cl3 1.644(17) . ? C902 H90C 0.9900 . ? C902 H90D 0.9900 . ? C901 Cl1 1.580(17) . ? C901 Cl2 1.634(16) . ? C901 H90A 0.9900 . ? C901 H90B 0.9900 . ? 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 C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C3 C2 C14 113.7(13) . . ? C3 C2 C1 108.4(14) . . ? C14 C2 C1 107.6(12) . . ? C3 C2 Sn1 106.1(10) . . ? C14 C2 Sn1 110.0(11) . . ? C1 C2 Sn1 111.1(10) . . ? C2 C3 C4 116.4(13) . . ? C2 C3 H3A 108.2 . . ? C4 C3 H3A 108.2 . . ? C2 C3 H3B 108.2 . . ? C4 C3 H3B 108.2 . . ? H3A C3 H3B 107.3 . . ? N5 C4 C15 124.7(14) . . ? N5 C4 C3 115.6(14) . . ? C15 C4 C3 119.4(15) . . ? N6 C7 C16 123.6(15) . . ? N6 C7 C8 112.9(14) . . ? C16 C7 C8 122.6(15) . . ? N9 C8 C13 125.3(15) . . ? N9 C8 C7 113.5(14) . . ? C13 C8 C7 121.2(15) . . ? C11 C10 N9 119.8(16) . . ? C11 C10 H10 120.1 . . ? N9 C10 H10 120.1 . . ? C12 C11 C10 120.4(17) . . ? C12 C11 H11 119.8 . . ? C10 C11 H11 119.8 . . ? C11 C12 C13 122.8(17) . . ? C11 C12 H12 118.6 . . ? C13 C12 H12 118.6 . . ? C12 C13 C8 114.1(16) . . ? C12 C13 H13 123.0 . . ? C8 C13 H13 123.0 . . ? C2 C14 H14A 109.5 . . ? C2 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C2 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C4 C15 H15A 109.5 . . ? C4 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C4 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? N17 C16 C21 124.0(16) . . ? N17 C16 C7 116.8(16) . . ? C21 C16 C7 119.2(16) . . ? N17 C18 C19 123.6(19) . . ? N17 C18 H18 118.2 . . ? C19 C18 H18 118.2 . . ? C18 C19 C20 120.7(19) . . ? C18 C19 H19 119.7 . . ? C20 C19 H19 119.7 . . ? C19 C20 C21 116.9(19) . . ? C19 C20 H20 121.5 . . ? C21 C20 H20 121.5 . . ? C16 C21 C20 118.4(17) . . ? C16 C21 H21 120.8 . . ? C20 C21 H21 120.8 . . ? C216 C121 C220 119.9(19) . . ? C216 C121 H121 120.0 . . ? C220 C121 H121 120.0 . . ? C202 C201 H20A 109.5 . . ? C202 C201 H20B 109.5 . . ? H20A C201 H20B 109.5 . . ? C202 C201 H20C 109.5 . . ? H20A C201 H20C 109.5 . . ? H20B C201 H20C 109.5 . . ? C203 C202 C201 109.1(11) . . ? C203 C202 C214 109.9(13) . . ? C201 C202 C214 108.4(11) . . ? C203 C202 Sn2 108.3(9) . . ? C201 C202 Sn2 111.1(10) . . ? C214 C202 Sn2 110.0(10) . . ? C204 C203 C202 115.8(12) . . ? C204 C203 H20D 108.3 . . ? C202 C203 H20D 108.3 . . ? C204 C203 H20E 108.3 . . ? C202 C203 H20E 108.3 . . ? H20D C203 H20E 107.4 . . ? N205 C204 C215 126.7(13) . . ? N205 C204 C203 113.6(13) . . ? C215 C204 C203 119.6(13) . . ? N206 C207 C216 125.6(14) . . ? N206 C207 C208 111.9(14) . . ? C216 C207 C208 122.5(15) . . ? N209 C208 C213 122.9(14) . . ? N209 C208 C207 116.5(14) . . ? C213 C208 C207 120.6(15) . . ? N209 C210 C211 118.0(18) . . ? N209 C210 H210 121.0 . . ? C211 C210 H210 121.0 . . ? C212 C211 C210 122.3(17) . . ? C212 C211 H211 118.8 . . ? C210 C211 H211 118.8 . . ? C211 C212 C213 117(2) . . ? C211 C212 H212 121.3 . . ? C213 C212 H212 121.3 . . ? C208 C213 C212 118.4(19) . . ? C208 C213 H213 120.8 . . ? C212 C213 H213 120.8 . . ? C202 C214 H21A 109.5 . . ? C202 C214 H21B 109.5 . . ? H21A C214 H21B 109.5 . . ? C202 C214 H21C 109.5 . . ? H21A C214 H21C 109.5 . . ? H21B C214 H21C 109.5 . . ? C204 C215 H21D 109.5 . . ? C204 C215 H21E 109.5 . . ? H21D C215 H21E 109.5 . . ? C204 C215 H21F 109.5 . . ? H21D C215 H21F 109.5 . . ? H21E C215 H21F 109.5 . . ? C121 C216 N217 122.0(18) . . ? C121 C216 C207 119.7(16) . . ? N217 C216 C207 117.8(16) . . ? C219 C218 N217 115.2(16) . . ? C219 C218 H218 122.4 . . ? N217 C218 H218 122.4 . . ? C220 C219 C218 121(2) . . ? C220 C219 H219 119.6 . . ? C218 C219 H219 119.6 . . ? C219 C220 C121 123(2) . . ? C219 C220 H220 118.3 . . ? C121 C220 H220 118.3 . . ? C302 C301 H30A 109.5 . . ? C302 C301 H30B 109.5 . . ? H30A C301 H30B 109.5 . . ? C302 C301 H30C 109.5 . . ? H30A C301 H30C 109.5 . . ? H30B C301 H30C 109.5 . . ? C301 C302 C314 112.1(15) . . ? C301 C302 C303 110.2(14) . . ? C314 C302 C303 112.2(14) . . ? C301 C302 Sn3 111.3(9) . . ? C314 C302 Sn3 104.6(10) . . ? C303 C302 Sn3 106.1(11) . . ? C304 C303 C302 116.9(13) . . ? C304 C303 H30D 108.1 . . ? C302 C303 H30D 108.1 . . ? C304 C303 H30E 108.1 . . ? C302 C303 H30E 108.1 . . ? H30D C303 H30E 107.3 . . ? N305 C304 C303 115.2(14) . . ? N305 C304 C315 126.9(14) . . ? C303 C304 C315 117.9(13) . . ? N306 C307 C308 115.7(13) . . ? N306 C307 C316 122.6(14) . . ? C308 C307 C316 121.6(13) . . ? N309 C308 C313 120.6(14) . . ? N309 C308 C307 116.0(13) . . ? C313 C308 C307 123.4(13) . . ? N309 C310 C311 122.3(14) . . ? N309 C310 H310 118.8 . . ? C311 C310 H310 118.8 . . ? C312 C311 C310 119.8(16) . . ? C312 C311 H311 120.1 . . ? C310 C311 H311 120.1 . . ? C311 C312 C313 118.6(16) . . ? C311 C312 H312 120.7 . . ? C313 C312 H312 120.7 . . ? C312 C313 C308 120.4(14) . . ? C312 C313 H313 119.8 . . ? C308 C313 H313 119.8 . . ? C302 C314 H31A 109.5 . . ? C302 C314 H31B 109.5 . . ? H31A C314 H31B 109.5 . . ? C302 C314 H31C 109.5 . . ? H31A C314 H31C 109.5 . . ? H31B C314 H31C 109.5 . . ? C304 C315 H31D 109.5 . . ? C304 C315 H31E 109.5 . . ? H31D C315 H31E 109.5 . . ? C304 C315 H31F 109.5 . . ? H31D C315 H31F 109.5 . . ? H31E C315 H31F 109.5 . . ? C321 C316 N317 124.5(15) . . ? C321 C316 C307 113.7(15) . . ? N317 C316 C307 121.7(13) . . ? C319 C318 N317 119.7(18) . . ? C319 C318 H318 120.1 . . ? N317 C318 H318 120.1 . . ? C318 C319 C320 123.3(18) . . ? C318 C319 H319 118.4 . . ? C320 C319 H319 118.4 . . ? C319 C320 C321 119(2) . . ? C319 C320 H320 120.3 . . ? C321 C320 H320 120.3 . . ? C316 C321 C320 116.7(18) . . ? C316 C321 H321 121.7 . . ? C320 C321 H321 121.7 . . ? C402 C401 H40A 109.5 . . ? C402 C401 H40B 109.5 . . ? H40A C401 H40B 109.5 . . ? C402 C401 H40C 109.5 . . ? H40A C401 H40C 109.5 . . ? H40B C401 H40C 109.5 . . ? C401 C402 C414 109.2(14) . . ? C401 C402 C403 109.9(14) . . ? C414 C402 C403 110.1(12) . . ? C401 C402 Sn4 110.9(10) . . ? C414 C402 Sn4 108.7(11) . . ? C403 C402 Sn4 108.1(10) . . ? C404 C403 C402 118.6(13) . . ? C404 C403 H40D 107.7 . . ? C402 C403 H40D 107.7 . . ? C404 C403 H40E 107.7 . . ? C402 C403 H40E 107.7 . . ? H40D C403 H40E 107.1 . . ? N405 C404 C403 118.0(13) . . ? N405 C404 C415 123.2(14) . . ? C403 C404 C415 118.6(14) . . ? N406 C407 C408 112.9(13) . . ? N406 C407 C416 123.9(14) . . ? C408 C407 C416 123.1(14) . . ? N409 C408 C413 120.7(16) . . ? N409 C408 C407 116.8(15) . . ? C413 C408 C407 122.4(15) . . ? C411 C410 N409 122.5(15) . . ? C411 C410 H410 118.7 . . ? N409 C410 H410 118.7 . . ? C412 C411 C410 120.7(18) . . ? C412 C411 H411 119.6 . . ? C410 C411 H411 119.6 . . ? C411 C412 C413 117.3(17) . . ? C411 C412 H412 121.3 . . ? C413 C412 H412 121.3 . . ? C412 C413 C408 121.1(15) . . ? C412 C413 H413 119.5 . . ? C408 C413 H413 119.5 . . ? C402 C414 H41A 109.5 . . ? C402 C414 H41B 109.5 . . ? H41A C414 H41B 109.5 . . ? C402 C414 H41C 109.5 . . ? H41A C414 H41C 109.5 . . ? H41B C414 H41C 109.5 . . ? C404 C415 H41D 109.5 . . ? C404 C415 H41E 109.5 . . ? H41D C415 H41E 109.5 . . ? C404 C415 H41F 109.5 . . ? H41D C415 H41F 109.5 . . ? H41E C415 H41F 109.5 . . ? N417 C416 C421 123.7(15) . . ? N417 C416 C407 115.3(14) . . ? C421 C416 C407 120.8(15) . . ? N417 C418 C419 124.4(16) . . ? N417 C418 H418 117.8 . . ? C419 C418 H418 117.8 . . ? C420 C419 C418 118.0(16) . . ? C420 C419 H419 121.0 . . ? C418 C419 H419 121.0 . . ? C419 C420 C421 121.1(16) . . ? C419 C420 H420 119.5 . . ? C421 C420 H420 119.5 . . ? C420 C421 C416 116.5(16) . . ? C420 C421 H421 121.7 . . ? C416 C421 H421 121.7 . . ? C4 N5 N6 120.6(13) . . ? C7 N6 N5 113.9(13) . . ? C7 N6 Zn1 118.4(10) . . ? N5 N6 Zn1 126.3(9) . . ? C8 N9 C10 117.6(14) . . ? C8 N9 Zn1 117.5(10) . . ? C10 N9 Zn1 124.8(11) . . ? C16 N17 C18 116.3(17) . . ? C204 N205 N206 118.1(13) . . ? C207 N206 N205 118.4(12) . . ? C207 N206 Zn2 118.0(10) . . ? N205 N206 Zn2 122.4(9) . . ? C208 N209 C210 120.8(15) . . ? C208 N209 Zn2 115.0(10) . . ? C210 N209 Zn2 124.2(12) . . ? C216 N217 C218 117.7(16) . . ? C304 N305 N306 117.9(13) . . ? C307 N306 N305 117.7(13) . . ? C307 N306 Zn3 115.1(10) . . ? N305 N306 Zn3 126.5(9) . . ? C308 N309 C310 118.3(13) . . ? C308 N309 Zn3 114.8(10) . . ? C310 N309 Zn3 126.9(10) . . ? C316 N317 C318 116.1(15) . . ? C404 N405 N406 121.3(13) . . ? C407 N406 N405 122.1(12) . . ? C407 N406 Zn4 116.5(10) . . ? N405 N406 Zn4 121.4(9) . . ? C408 N409 C410 117.4(15) . . ? C408 N409 Zn4 116.1(11) . . ? C410 N409 Zn4 126.3(11) . . ? C416 N417 C418 116.1(14) . . ? Sn2 S1 Sn1 106.95(16) . . ? Zn2 S2 Zn7 105.20(17) . . ? Zn2 S2 Sn1 94.08(14) . . ? Zn7 S2 Sn1 107.77(15) . . ? Zn5 S3 Zn6 111.50(17) . . ? Zn5 S3 Sn1 116.15(18) . . ? Zn6 S3 Sn1 110.64(15) . . ? Zn1 S4 Zn5 101.89(16) . . ? Zn1 S4 Sn2 99.79(16) . . ? Zn5 S4 Sn2 107.23(14) . . ? Zn7 S5 Zn8 114.56(17) . . ? Zn7 S5 Sn2 116.69(17) . . ? Zn8 S5 Sn2 107.12(15) . . ? Zn6 S6 Zn7 105.28(15) . . ? Zn6 S6 Sn3 115.91(17) . . ? Zn7 S6 Sn3 116.12(16) . . ? Zn4 S7 Zn8 105.01(16) . . ? Zn4 S7 Sn3 97.04(16) . . ? Zn8 S7 Sn3 105.90(16) . . ? Sn4 S8 Sn3 105.60(16) . . ? Zn3 S9 Zn6 103.51(15) . . ? Zn3 S9 Sn4 101.34(15) . . ? Zn6 S9 Sn4 105.54(16) . . ? Zn8 S10 Zn5 108.59(17) . . ? Zn8 S10 Sn4 116.31(15) . . ? Zn5 S10 Sn4 112.54(16) . . ? N6 Zn1 N9 77.5(5) . . ? N6 Zn1 S4 122.1(4) . . ? N9 Zn1 S4 107.5(4) . . ? N6 Zn1 Br1 113.7(4) . . ? N9 Zn1 Br1 105.2(4) . . ? S4 Zn1 Br1 119.56(14) . . ? N206 Zn2 N209 77.9(5) . . ? N206 Zn2 S2 121.3(4) . . ? N209 Zn2 S2 102.5(4) . . ? N206 Zn2 Br2 112.8(4) . . ? N209 Zn2 Br2 103.4(4) . . ? S2 Zn2 Br2 123.47(14) . . ? N309 Zn3 N306 78.3(5) . . ? N309 Zn3 S9 105.1(4) . . ? N306 Zn3 S9 116.1(4) . . ? N309 Zn3 Br3 107.6(4) . . ? N306 Zn3 Br3 111.8(4) . . ? S9 Zn3 Br3 126.04(13) . . ? N409 Zn4 N406 77.3(6) . . ? N409 Zn4 S7 100.5(4) . . ? N406 Zn4 S7 114.0(4) . . ? N409 Zn4 Br4 108.1(4) . . ? N406 Zn4 Br4 112.6(4) . . ? S7 Zn4 Br4 129.37(12) . . ? S3 Zn5 S4 119.69(16) . . ? S3 Zn5 S10 114.74(14) . . ? S4 Zn5 S10 98.96(15) . . ? S3 Zn5 Br5 104.12(12) . . ? S4 Zn5 Br5 111.20(11) . . ? S10 Zn5 Br5 107.87(12) . . ? S6 Zn6 S9 117.60(15) . . ? S6 Zn6 S3 120.71(16) . . ? S9 Zn6 S3 99.73(15) . . ? S6 Zn6 Br6 104.19(12) . . ? S9 Zn6 Br6 111.18(12) . . ? S3 Zn6 Br6 102.57(12) . . ? S5 Zn7 S2 117.71(14) . . ? S5 Zn7 S6 111.70(16) . . ? S2 Zn7 S6 105.65(15) . . ? S5 Zn7 Br7 108.25(12) . . ? S2 Zn7 Br7 105.41(12) . . ? S6 Zn7 Br7 107.56(11) . . ? S10 Zn8 S7 117.23(15) . . ? S10 Zn8 S5 118.06(15) . . ? S7 Zn8 S5 100.65(15) . . ? S10 Zn8 Br8 104.31(12) . . ? S7 Zn8 Br8 111.95(12) . . ? S5 Zn8 Br8 104.15(12) . . ? C2 Sn1 S3 114.2(5) . . ? C2 Sn1 S2 107.9(4) . . ? S3 Sn1 S2 107.73(14) . . ? C2 Sn1 S1 111.9(5) . . ? S3 Sn1 S1 116.86(14) . . ? S2 Sn1 S1 96.26(14) . . ? C202 Sn2 S5 112.6(4) . . ? C202 Sn2 S1 113.5(4) . . ? S5 Sn2 S1 116.59(13) . . ? C202 Sn2 S4 106.1(4) . . ? S5 Sn2 S4 108.21(14) . . ? S1 Sn2 S4 98.05(14) . . ? C302 Sn3 S6 115.4(5) . . ? C302 Sn3 S8 111.2(5) . . ? S6 Sn3 S8 118.17(14) . . ? C302 Sn3 S7 103.1(4) . . ? S6 Sn3 S7 108.34(13) . . ? S8 Sn3 S7 97.78(14) . . ? C402 Sn4 S10 112.5(4) . . ? C402 Sn4 S8 113.0(5) . . ? S10 Sn4 S8 117.30(14) . . ? C402 Sn4 S9 104.8(4) . . ? S10 Sn4 S9 108.34(14) . . ? S8 Sn4 S9 99.05(13) . . ? Cl5 C903 Cl7 114.3(11) . . ? Cl5 C903 Cl6 110.7(11) . . ? Cl7 C903 Cl6 109.1(12) . . ? Cl5 C903 H903 107.5 . . ? Cl7 C903 H903 107.5 . . ? Cl6 C903 H903 107.5 . . ? Cl4 C902 Cl3 133(3) . . ? Cl4 C902 H90C 104.0 . . ? Cl3 C902 H90C 104.0 . . ? Cl4 C902 H90D 104.0 . . ? Cl3 C902 H90D 104.0 . . ? H90C C902 H90D 105.5 . . ? Cl1 C901 Cl2 111.6(17) . . ? Cl1 C901 H90A 109.3 . . ? Cl2 C901 H90A 109.3 . . ? Cl1 C901 H90B 109.3 . . ? Cl2 C901 H90B 109.3 . . ? H90A C901 H90B 108.0 . . ? 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 C14 C2 C3 C4 -69.6(18) . . . . ? C1 C2 C3 C4 170.8(13) . . . . ? Sn1 C2 C3 C4 51.4(15) . . . . ? C2 C3 C4 N5 1(2) . . . . ? C2 C3 C4 C15 -174.0(14) . . . . ? N6 C7 C8 N9 2.3(18) . . . . ? C16 C7 C8 N9 172.0(14) . . . . ? N6 C7 C8 C13 -175.9(14) . . . . ? C16 C7 C8 C13 -6(2) . . . . ? N9 C10 C11 C12 0(3) . . . . ? C10 C11 C12 C13 -1(3) . . . . ? C11 C12 C13 C8 2(2) . . . . ? N9 C8 C13 C12 -3(2) . . . . ? C7 C8 C13 C12 175.4(14) . . . . ? N6 C7 C16 N17 56(2) . . . . ? C8 C7 C16 N17 -112.7(18) . . . . ? N6 C7 C16 C21 -124.6(18) . . . . ? C8 C7 C16 C21 67(2) . . . . ? N17 C18 C19 C20 -3(3) . . . . ? C18 C19 C20 C21 2(3) . . . . ? N17 C16 C21 C20 0(3) . . . . ? C7 C16 C21 C20 -179.7(15) . . . . ? C19 C20 C21 C16 -1(3) . . . . ? C201 C202 C203 C204 171.9(12) . . . . ? C214 C202 C203 C204 -69.3(16) . . . . ? Sn2 C202 C203 C204 50.9(14) . . . . ? C202 C203 C204 N205 -3.4(19) . . . . ? C202 C203 C204 C215 -179.5(14) . . . . ? N206 C207 C208 N209 9(2) . . . . ? C216 C207 C208 N209 -169.3(15) . . . . ? N206 C207 C208 C213 -172.2(15) . . . . ? C216 C207 C208 C213 9(2) . . . . ? N209 C210 C211 C212 -3(3) . . . . ? C210 C211 C212 C213 1(3) . . . . ? N209 C208 C213 C212 0(3) . . . . ? C207 C208 C213 C212 -178.2(16) . . . . ? C211 C212 C213 C208 0(3) . . . . ? C220 C121 C216 N217 7(3) . . . . ? C220 C121 C216 C207 179(2) . . . . ? N206 C207 C216 C121 58(3) . . . . ? C208 C207 C216 C121 -123.3(19) . . . . ? N206 C207 C216 N217 -129.4(18) . . . . ? C208 C207 C216 N217 49(2) . . . . ? N217 C218 C219 C220 6(3) . . . . ? C218 C219 C220 C121 -9(4) . . . . ? C216 C121 C220 C219 3(4) . . . . ? C301 C302 C303 C304 -166.1(14) . . . . ? C314 C302 C303 C304 68.2(18) . . . . ? Sn3 C302 C303 C304 -45.4(17) . . . . ? C302 C303 C304 N305 9(2) . . . . ? C302 C303 C304 C315 -173.0(16) . . . . ? N306 C307 C308 N309 -2(2) . . . . ? C316 C307 C308 N309 179.1(14) . . . . ? N306 C307 C308 C313 178.4(16) . . . . ? C316 C307 C308 C313 -1(2) . . . . ? N309 C310 C311 C312 2(2) . . . . ? C310 C311 C312 C313 -2(3) . . . . ? C311 C312 C313 C308 0(3) . . . . ? N309 C308 C313 C312 1(2) . . . . ? C307 C308 C313 C312 -179.0(15) . . . . ? N306 C307 C316 C321 -99(2) . . . . ? C308 C307 C316 C321 80(2) . . . . ? N306 C307 C316 N317 84(2) . . . . ? C308 C307 C316 N317 -97(2) . . . . ? N317 C318 C319 C320 -4(4) . . . . ? C318 C319 C320 C321 6(5) . . . . ? N317 C316 C321 C320 -1(3) . . . . ? C307 C316 C321 C320 -177(2) . . . . ? C319 C320 C321 C316 -4(4) . . . . ? C401 C402 C403 C404 -166.1(13) . . . . ? C414 C402 C403 C404 73.6(17) . . . . ? Sn4 C402 C403 C404 -45.0(15) . . . . ? C402 C403 C404 N405 10.0(19) . . . . ? C402 C403 C404 C415 -174.8(13) . . . . ? N406 C407 C408 N409 5(2) . . . . ? C416 C407 C408 N409 -174.0(15) . . . . ? N406 C407 C408 C413 -173.7(15) . . . . ? C416 C407 C408 C413 8(2) . . . . ? N409 C410 C411 C412 -1(3) . . . . ? C410 C411 C412 C413 2(3) . . . . ? C411 C412 C413 C408 -4(2) . . . . ? N409 C408 C413 C412 5(2) . . . . ? C407 C408 C413 C412 -176.4(14) . . . . ? N406 C407 C416 N417 -131.7(16) . . . . ? C408 C407 C416 N417 47(2) . . . . ? N406 C407 C416 C421 44(2) . . . . ? C408 C407 C416 C421 -137.6(17) . . . . ? N417 C418 C419 C420 3(3) . . . . ? C418 C419 C420 C421 1(3) . . . . ? C419 C420 C421 C416 -3(3) . . . . ? N417 C416 C421 C420 1(3) . . . . ? C407 C416 C421 C420 -174.6(15) . . . . ? C15 C4 N5 N6 -1(3) . . . . ? C3 C4 N5 N6 -175.8(12) . . . . ? C16 C7 N6 N5 19(2) . . . . ? C8 C7 N6 N5 -171.6(12) . . . . ? C16 C7 N6 Zn1 -174.1(11) . . . . ? C8 C7 N6 Zn1 -4.5(17) . . . . ? C4 N5 N6 C7 -104.6(18) . . . . ? C4 N5 N6 Zn1 89.6(17) . . . . ? C13 C8 N9 C10 2(2) . . . . ? C7 C8 N9 C10 -176.2(12) . . . . ? C13 C8 N9 Zn1 179.1(12) . . . . ? C7 C8 N9 Zn1 0.9(16) . . . . ? C11 C10 N9 C8 -1(2) . . . . ? C11 C10 N9 Zn1 -177.4(12) . . . . ? C21 C16 N17 C18 0(2) . . . . ? C7 C16 N17 C18 179.2(14) . . . . ? C19 C18 N17 C16 2(3) . . . . ? C215 C204 N205 N206 2(2) . . . . ? C203 C204 N205 N206 -173.5(11) . . . . ? C216 C207 N206 N205 2(2) . . . . ? C208 C207 N206 N205 -176.5(12) . . . . ? C216 C207 N206 Zn2 169.9(13) . . . . ? C208 C207 N206 Zn2 -8.6(17) . . . . ? C204 N205 N206 C207 -97.1(17) . . . . ? C204 N205 N206 Zn2 95.5(15) . . . . ? C213 C208 N209 C210 -2(3) . . . . ? C207 C208 N209 C210 176.4(14) . . . . ? C213 C208 N209 Zn2 176.0(13) . . . . ? C207 C208 N209 Zn2 -5.3(17) . . . . ? C211 C210 N209 C208 3(3) . . . . ? C211 C210 N209 Zn2 -174.8(14) . . . . ? C121 C216 N217 C218 -9(3) . . . . ? C207 C216 N217 C218 179.3(17) . . . . ? C219 C218 N217 C216 2(3) . . . . ? C303 C304 N305 N306 173.7(13) . . . . ? C315 C304 N305 N306 -4(3) . . . . ? C308 C307 N306 N305 175.0(12) . . . . ? C316 C307 N306 N305 -6(2) . . . . ? C308 C307 N306 Zn3 3.6(17) . . . . ? C316 C307 N306 Zn3 -177.2(11) . . . . ? C304 N305 N306 C307 94.8(18) . . . . ? C304 N305 N306 Zn3 -94.8(15) . . . . ? C313 C308 N309 C310 -1(2) . . . . ? C307 C308 N309 C310 179.0(13) . . . . ? C313 C308 N309 Zn3 178.8(12) . . . . ? C307 C308 N309 Zn3 -1.1(17) . . . . ? C311 C310 N309 C308 0(2) . . . . ? C311 C310 N309 Zn3 179.8(12) . . . . ? C321 C316 N317 C318 3(3) . . . . ? C307 C316 N317 C318 179.3(15) . . . . ? C319 C318 N317 C316 -1(3) . . . . ? C403 C404 N405 N406 169.5(11) . . . . ? C415 C404 N405 N406 -6(2) . . . . ? C408 C407 N406 N405 176.2(12) . . . . ? C416 C407 N406 N405 -5(2) . . . . ? C408 C407 N406 Zn4 -0.3(17) . . . . ? C416 C407 N406 Zn4 178.3(12) . . . . ? C404 N405 N406 C407 87.6(18) . . . . ? C404 N405 N406 Zn4 -96.0(15) . . . . ? C413 C408 N409 C410 -5(2) . . . . ? C407 C408 N409 C410 177.0(14) . . . . ? C413 C408 N409 Zn4 171.6(12) . . . . ? C407 C408 N409 Zn4 -6.7(19) . . . . ? C411 C410 N409 C408 3(2) . . . . ? C411 C410 N409 Zn4 -173.0(14) . . . . ? C421 C416 N417 C418 3(2) . . . . ? C407 C416 N417 C418 178.4(14) . . . . ? C419 C418 N417 C416 -5(3) . . . . ? C7 N6 Zn1 N9 3.9(11) . . . . ? N5 N6 Zn1 N9 169.2(12) . . . . ? C7 N6 Zn1 S4 -99.0(11) . . . . ? N5 N6 Zn1 S4 66.2(12) . . . . ? C7 N6 Zn1 Br1 105.2(11) . . . . ? N5 N6 Zn1 Br1 -89.5(11) . . . . ? C8 N9 Zn1 N6 -2.4(10) . . . . ? C10 N9 Zn1 N6 174.4(12) . . . . ? C8 N9 Zn1 S4 117.6(10) . . . . ? C10 N9 Zn1 S4 -65.6(12) . . . . ? C8 N9 Zn1 Br1 -114.0(10) . . . . ? C10 N9 Zn1 Br1 62.9(11) . . . . ? Zn5 S4 Zn1 N6 18.4(5) . . . . ? Sn2 S4 Zn1 N6 -91.7(5) . . . . ? Zn5 S4 Zn1 N9 -67.6(4) . . . . ? Sn2 S4 Zn1 N9 -177.7(4) . . . . ? Zn5 S4 Zn1 Br1 172.76(11) . . . . ? Sn2 S4 Zn1 Br1 62.66(16) . . . . ? C207 N206 Zn2 N209 4.8(12) . . . . ? N205 N206 Zn2 N209 172.3(12) . . . . ? C207 N206 Zn2 S2 -92.6(12) . . . . ? N205 N206 Zn2 S2 74.9(11) . . . . ? C207 N206 Zn2 Br2 104.5(11) . . . . ? N205 N206 Zn2 Br2 -88.0(11) . . . . ? C208 N209 Zn2 N206 0.7(11) . . . . ? C210 N209 Zn2 N206 178.9(14) . . . . ? C208 N209 Zn2 S2 120.4(11) . . . . ? C210 N209 Zn2 S2 -61.4(14) . . . . ? C208 N209 Zn2 Br2 -110.2(11) . . . . ? C210 N209 Zn2 Br2 67.9(14) . . . . ? Zn7 S2 Zn2 N206 7.8(4) . . . . ? Sn1 S2 Zn2 N206 -101.9(4) . . . . ? Zn7 S2 Zn2 N209 -75.6(4) . . . . ? Sn1 S2 Zn2 N209 174.8(4) . . . . ? Zn7 S2 Zn2 Br2 168.84(11) . . . . ? Sn1 S2 Zn2 Br2 59.17(17) . . . . ? C308 N309 Zn3 N306 2.2(11) . . . . ? C310 N309 Zn3 N306 -177.9(14) . . . . ? C308 N309 Zn3 S9 -111.9(11) . . . . ? C310 N309 Zn3 S9 68.0(13) . . . . ? C308 N309 Zn3 Br3 111.6(11) . . . . ? C310 N309 Zn3 Br3 -68.5(13) . . . . ? C307 N306 Zn3 N309 -3.2(11) . . . . ? N305 N306 Zn3 N309 -173.8(12) . . . . ? C307 N306 Zn3 S9 98.0(11) . . . . ? N305 N306 Zn3 S9 -72.5(12) . . . . ? C307 N306 Zn3 Br3 -107.6(11) . . . . ? N305 N306 Zn3 Br3 81.8(11) . . . . ? Zn6 S9 Zn3 N309 64.9(4) . . . . ? Sn4 S9 Zn3 N309 174.1(4) . . . . ? Zn6 S9 Zn3 N306 -19.3(5) . . . . ? Sn4 S9 Zn3 N306 89.9(4) . . . . ? Zn6 S9 Zn3 Br3 -169.44(11) . . . . ? Sn4 S9 Zn3 Br3 -60.23(19) . . . . ? C408 N409 Zn4 N406 4.9(13) . . . . ? C410 N409 Zn4 N406 -179.2(14) . . . . ? C408 N409 Zn4 S7 -107.6(12) . . . . ? C410 N409 Zn4 S7 68.4(13) . . . . ? C408 N409 Zn4 Br4 114.8(12) . . . . ? C410 N409 Zn4 Br4 -69.3(13) . . . . ? C407 N406 Zn4 N409 -2.3(12) . . . . ? N405 N406 Zn4 N409 -178.9(11) . . . . ? C407 N406 Zn4 S7 93.6(11) . . . . ? N405 N406 Zn4 S7 -82.9(10) . . . . ? C407 N406 Zn4 Br4 -106.9(11) . . . . ? N405 N406 Zn4 Br4 76.6(10) . . . . ? Zn8 S7 Zn4 N409 73.4(4) . . . . ? Sn3 S7 Zn4 N409 -178.0(4) . . . . ? Zn8 S7 Zn4 N406 -7.3(4) . . . . ? Sn3 S7 Zn4 N406 101.3(4) . . . . ? Zn8 S7 Zn4 Br4 -162.59(12) . . . . ? Sn3 S7 Zn4 Br4 -54.0(2) . . . . ? Zn6 S3 Zn5 S4 -126.65(18) . . . . ? Sn1 S3 Zn5 S4 1.3(2) . . . . ? Zn6 S3 Zn5 S10 -9.3(2) . . . . ? Sn1 S3 Zn5 S10 118.73(18) . . . . ? Zn6 S3 Zn5 Br5 108.41(16) . . . . ? Sn1 S3 Zn5 Br5 -123.61(15) . . . . ? Zn1 S4 Zn5 S3 -64.97(19) . . . . ? Sn2 S4 Zn5 S3 39.3(2) . . . . ? Zn1 S4 Zn5 S10 169.74(15) . . . . ? Sn2 S4 Zn5 S10 -85.94(17) . . . . ? Zn1 S4 Zn5 Br5 56.52(16) . . . . ? Sn2 S4 Zn5 Br5 160.84(11) . . . . ? Zn8 S10 Zn5 S3 -78.8(2) . . . . ? Sn4 S10 Zn5 S3 51.5(2) . . . . ? Zn8 S10 Zn5 S4 49.90(17) . . . . ? Sn4 S10 Zn5 S4 -179.87(16) . . . . ? Zn8 S10 Zn5 Br5 165.72(12) . . . . ? Sn4 S10 Zn5 Br5 -64.05(17) . . . . ? Zn7 S6 Zn6 S9 141.01(16) . . . . ? Sn3 S6 Zn6 S9 11.2(2) . . . . ? Zn7 S6 Zn6 S3 18.9(2) . . . . ? Sn3 S6 Zn6 S3 -110.95(19) . . . . ? Zn7 S6 Zn6 Br6 -95.44(15) . . . . ? Sn3 S6 Zn6 Br6 134.76(14) . . . . ? Zn3 S9 Zn6 S6 57.6(2) . . . . ? Sn4 S9 Zn6 S6 -48.4(2) . . . . ? Zn3 S9 Zn6 S3 -169.99(15) . . . . ? Sn4 S9 Zn6 S3 83.95(16) . . . . ? Zn3 S9 Zn6 Br6 -62.34(16) . . . . ? Sn4 S9 Zn6 Br6 -168.40(10) . . . . ? Zn5 S3 Zn6 S6 75.2(2) . . . . ? Sn1 S3 Zn6 S6 -55.7(2) . . . . ? Zn5 S3 Zn6 S9 -55.3(2) . . . . ? Sn1 S3 Zn6 S9 173.85(16) . . . . ? Zn5 S3 Zn6 Br6 -169.71(15) . . . . ? Sn1 S3 Zn6 Br6 59.40(17) . . . . ? Zn8 S5 Zn7 S2 -128.76(18) . . . . ? Sn2 S5 Zn7 S2 -2.5(3) . . . . ? Zn8 S5 Zn7 S6 -6.3(2) . . . . ? Sn2 S5 Zn7 S6 120.01(18) . . . . ? Zn8 S5 Zn7 Br7 111.95(16) . . . . ? Sn2 S5 Zn7 Br7 -121.75(16) . . . . ? Zn2 S2 Zn7 S5 -56.5(2) . . . . ? Sn1 S2 Zn7 S5 42.9(2) . . . . ? Zn2 S2 Zn7 S6 177.95(14) . . . . ? Sn1 S2 Zn7 S6 -82.58(17) . . . . ? Zn2 S2 Zn7 Br7 64.23(15) . . . . ? Sn1 S2 Zn7 Br7 163.70(13) . . . . ? Zn6 S6 Zn7 S5 -82.49(18) . . . . ? Sn3 S6 Zn7 S5 47.2(2) . . . . ? Zn6 S6 Zn7 S2 46.65(18) . . . . ? Sn3 S6 Zn7 S2 176.34(15) . . . . ? Zn6 S6 Zn7 Br7 158.87(12) . . . . ? Sn3 S6 Zn7 Br7 -71.45(17) . . . . ? Zn5 S10 Zn8 S7 138.44(16) . . . . ? Sn4 S10 Zn8 S7 10.3(2) . . . . ? Zn5 S10 Zn8 S5 17.8(2) . . . . ? Sn4 S10 Zn8 S5 -110.33(18) . . . . ? Zn5 S10 Zn8 Br8 -97.16(15) . . . . ? Sn4 S10 Zn8 Br8 134.72(15) . . . . ? Zn4 S7 Zn8 S10 54.4(2) . . . . ? Sn3 S7 Zn8 S10 -47.7(2) . . . . ? Zn4 S7 Zn8 S5 -176.22(16) . . . . ? Sn3 S7 Zn8 S5 81.75(18) . . . . ? Zn4 S7 Zn8 Br8 -66.11(18) . . . . ? Sn3 S7 Zn8 Br8 -168.13(12) . . . . ? Zn7 S5 Zn8 S10 73.5(2) . . . . ? Sn2 S5 Zn8 S10 -57.6(2) . . . . ? Zn7 S5 Zn8 S7 -55.4(2) . . . . ? Sn2 S5 Zn8 S7 173.49(15) . . . . ? Zn7 S5 Zn8 Br8 -171.48(14) . . . . ? Sn2 S5 Zn8 Br8 57.41(16) . . . . ? C3 C2 Sn1 S3 -120.8(10) . . . . ? C14 C2 Sn1 S3 2.6(11) . . . . ? C1 C2 Sn1 S3 121.6(11) . . . . ? C3 C2 Sn1 S2 119.5(9) . . . . ? C14 C2 Sn1 S2 -117.1(9) . . . . ? C1 C2 Sn1 S2 1.9(12) . . . . ? C3 C2 Sn1 S1 14.8(11) . . . . ? C14 C2 Sn1 S1 138.2(8) . . . . ? C1 C2 Sn1 S1 -102.8(11) . . . . ? Zn5 S3 Sn1 C2 130.9(4) . . . . ? Zn6 S3 Sn1 C2 -100.7(4) . . . . ? Zn5 S3 Sn1 S2 -109.28(18) . . . . ? Zn6 S3 Sn1 S2 19.1(2) . . . . ? Zn5 S3 Sn1 S1 -2.4(2) . . . . ? Zn6 S3 Sn1 S1 125.99(16) . . . . ? Zn2 S2 Sn1 C2 -86.1(5) . . . . ? Zn7 S2 Sn1 C2 166.6(5) . . . . ? Zn2 S2 Sn1 S3 150.24(14) . . . . ? Zn7 S2 Sn1 S3 42.85(19) . . . . ? Zn2 S2 Sn1 S1 29.43(16) . . . . ? Zn7 S2 Sn1 S1 -77.96(17) . . . . ? Sn2 S1 Sn1 C2 -171.9(4) . . . . ? Sn2 S1 Sn1 S3 -37.6(2) . . . . ? Sn2 S1 Sn1 S2 75.88(17) . . . . ? C203 C202 Sn2 S5 -120.2(8) . . . . ? C201 C202 Sn2 S5 120.0(9) . . . . ? C214 C202 Sn2 S5 0.0(11) . . . . ? C203 C202 Sn2 S1 15.1(10) . . . . ? C201 C202 Sn2 S1 -104.7(9) . . . . ? C214 C202 Sn2 S1 135.2(9) . . . . ? C203 C202 Sn2 S4 121.6(8) . . . . ? C201 C202 Sn2 S4 1.8(10) . . . . ? C214 C202 Sn2 S4 -118.3(9) . . . . ? Zn7 S5 Sn2 C202 135.2(5) . . . . ? Zn8 S5 Sn2 C202 -94.9(5) . . . . ? Zn7 S5 Sn2 S1 1.5(3) . . . . ? Zn8 S5 Sn2 S1 131.37(17) . . . . ? Zn7 S5 Sn2 S4 -107.79(19) . . . . ? Zn8 S5 Sn2 S4 22.13(19) . . . . ? Sn1 S1 Sn2 C202 -174.0(4) . . . . ? Sn1 S1 Sn2 S5 -40.6(2) . . . . ? Sn1 S1 Sn2 S4 74.51(16) . . . . ? Zn1 S4 Sn2 C202 -87.7(4) . . . . ? Zn5 S4 Sn2 C202 166.5(4) . . . . ? Zn1 S4 Sn2 S5 151.14(14) . . . . ? Zn5 S4 Sn2 S5 45.33(18) . . . . ? Zn1 S4 Sn2 S1 29.64(16) . . . . ? Zn5 S4 Sn2 S1 -76.17(17) . . . . ? C301 C302 Sn3 S6 -131.6(11) . . . . ? C314 C302 Sn3 S6 -10.4(12) . . . . ? C303 C302 Sn3 S6 108.4(11) . . . . ? C301 C302 Sn3 S8 90.2(12) . . . . ? C314 C302 Sn3 S8 -148.6(9) . . . . ? C303 C302 Sn3 S8 -29.8(12) . . . . ? C301 C302 Sn3 S7 -13.7(13) . . . . ? C314 C302 Sn3 S7 107.5(10) . . . . ? C303 C302 Sn3 S7 -133.6(10) . . . . ? Zn6 S6 Sn3 C302 -141.8(5) . . . . ? Zn7 S6 Sn3 C302 93.9(5) . . . . ? Zn6 S6 Sn3 S8 -6.6(2) . . . . ? Zn7 S6 Sn3 S8 -130.93(17) . . . . ? Zn6 S6 Sn3 S7 103.28(18) . . . . ? Zn7 S6 Sn3 S7 -21.1(2) . . . . ? Sn4 S8 Sn3 C302 176.7(5) . . . . ? Sn4 S8 Sn3 S6 39.7(2) . . . . ? Sn4 S8 Sn3 S7 -75.96(16) . . . . ? Zn4 S7 Sn3 C302 86.3(5) . . . . ? Zn8 S7 Sn3 C302 -165.9(5) . . . . ? Zn4 S7 Sn3 S6 -150.93(13) . . . . ? Zn8 S7 Sn3 S6 -43.08(19) . . . . ? Zn4 S7 Sn3 S8 -27.75(15) . . . . ? Zn8 S7 Sn3 S8 80.10(17) . . . . ? C401 C402 Sn4 S10 -135.9(11) . . . . ? C414 C402 Sn4 S10 -15.9(11) . . . . ? C403 C402 Sn4 S10 103.6(10) . . . . ? C401 C402 Sn4 S8 88.4(12) . . . . ? C414 C402 Sn4 S8 -151.6(9) . . . . ? C403 C402 Sn4 S8 -32.1(11) . . . . ? C401 C402 Sn4 S9 -18.4(13) . . . . ? C414 C402 Sn4 S9 101.6(10) . . . . ? C403 C402 Sn4 S9 -138.9(9) . . . . ? Zn8 S10 Sn4 C402 -141.0(5) . . . . ? Zn5 S10 Sn4 C402 92.8(5) . . . . ? Zn8 S10 Sn4 S8 -7.4(2) . . . . ? Zn5 S10 Sn4 S8 -133.53(17) . . . . ? Zn8 S10 Sn4 S9 103.59(18) . . . . ? Zn5 S10 Sn4 S9 -22.6(2) . . . . ? Sn3 S8 Sn4 C402 175.4(5) . . . . ? Sn3 S8 Sn4 S10 42.0(2) . . . . ? Sn3 S8 Sn4 S9 -74.14(17) . . . . ? Zn3 S9 Sn4 C402 89.3(5) . . . . ? Zn6 S9 Sn4 C402 -163.1(5) . . . . ? Zn3 S9 Sn4 S10 -150.39(15) . . . . ? Zn6 S9 Sn4 S10 -42.75(17) . . . . ? Zn3 S9 Sn4 S8 -27.56(18) . . . . ? Zn6 S9 Sn4 S8 80.08(17) . . . . ? _diffrn_measured_fraction_theta_max 0.715 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.715 _refine_diff_density_max 1.131 _refine_diff_density_min -0.920 _refine_diff_density_rms 0.123 _database_code_depnum_ccdc_archive 'CCDC 934169' ####################################################################### # # 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_6 #TrackingRef '19486_web_deposit_cif_file_4_KlausHarms_1366045723.6-bb137_2.cif' _vrf_PLAT029_6 ; PROBLEM: _diffrn_measured_fraction_theta_full Low ....... 0.682 RESPONSE: Only data of one twin domain were used. ; _vrf_PLAT413_6 ; PROBLEM: Short Inter XH3 .. XHn H418 .. H20F .. 1.62 Ang. RESPONSE: These atoms with short contacts are not fully occupied. ; #data_bb137_2 _audit_creation_method SHELXL-2013 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C68 H76 I8 N16 S10 Sn4 Zn8, 1.25(C H Cl3), 0.75(C H3 O H), 0.5(H2 O)' _chemical_formula_sum 'C70 H81.25 Cl3.75 I8 N16 O1.25 S10 Sn4 Zn8' _chemical_formula_weight 3633.21 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 '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' Sn Sn -0.6537 1.4246 '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' _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_H-M_alt 'P -1' _space_group_name_Hall '-P 1' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 16.5734(5) _cell_length_b 19.2405(5) _cell_length_c 20.2479(6) _cell_angle_alpha 85.019(2) _cell_angle_beta 69.865(2) _cell_angle_gamma 70.661(2) _cell_volume 5717.3(3) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 36456 _cell_measurement_theta_min 1.4 _cell_measurement_theta_max 25.5 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 2.110 _exptl_crystal_F_000 3422 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.110 _exptl_crystal_size_mid 0.100 _exptl_crystal_size_min 0.040 _exptl_absorpt_coefficient_mu 4.975 _shelx_estimated_absorpt_T_min 0.611 _shelx_estimated_absorpt_T_max 0.826 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.59 _exptl_absorpt_correction_T_max 0.77 _exptl_absorpt_process_details 'Bruker XPREP' _exptl_special_details ; Non merohedral twin. Integration using two matrices. ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_source ? _diffrn_measurement_device_type 'STOE IPDS-2T' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 28709 _diffrn_reflns_av_unetI/netI 0.0731 _diffrn_reflns_av_R_equivalents 0.0506 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.382 _diffrn_reflns_theta_max 25.499 _diffrn_reflns_theta_full 25.242 _diffrn_measured_fraction_theta_max 0.682 _diffrn_measured_fraction_theta_full 0.682 _diffrn_reflns_Laue_measured_fraction_max 0.682 _diffrn_reflns_Laue_measured_fraction_full 0.682 _diffrn_reflns_point_group_measured_fraction_max 0.682 _diffrn_reflns_point_group_measured_fraction_full 0.682 _reflns_number_total 14527 _reflns_number_gt 9223 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_max . _reflns_Friedel_fraction_full . _reflns_special_details ; Only reflections of one twin domain were used during refinement. Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _computing_data_collection 'STOE X-AREA' _computing_cell_refinement 'STOE X-AREA' _computing_data_reduction 'STOE X-AREA' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-2013 (Sheldrick, 2013)' _computing_molecular_graphics 'DIAMOND (Crystal Impact)' _computing_publication_material ? _refine_special_details ; Only the reflections of one twin domain were used during refinement ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; w=1/[\s^2^(Fo^2^)+(0.0677P)^2^] 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 14527 _refine_ls_number_parameters 1126 _refine_ls_number_restraints 29 _refine_ls_R_factor_all 0.0903 _refine_ls_R_factor_gt 0.0496 _refine_ls_wR_factor_ref 0.1281 _refine_ls_wR_factor_gt 0.1089 _refine_ls_goodness_of_fit_ref 0.952 _refine_ls_restrained_S_all 0.953 _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_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.7367(10) 0.2320(8) 0.0242(7) 0.059(4) Uani 1 1 d . . . . . H1A H 0.7433 0.2771 0.0374 0.088 Uiso 1 1 calc R U . . . H1B H 0.6818 0.2446 0.0113 0.088 Uiso 1 1 calc R U . . . H1C H 0.7898 0.2073 -0.0160 0.088 Uiso 1 1 calc R U . . . C2 C 0.7292(9) 0.1807(7) 0.0862(7) 0.050(3) Uani 1 1 d . . . . . C3 C 0.8028(9) 0.1728(8) 0.1189(8) 0.063(4) Uani 1 1 d . . . . . H3A H 0.8058 0.2225 0.1239 0.076 Uiso 1 1 calc R U . . . H3B H 0.8620 0.1438 0.0854 0.076 Uiso 1 1 calc R U . . . C4 C 0.7910(9) 0.1362(7) 0.1914(7) 0.052(3) Uani 1 1 d . . . . . C7 C 0.7293(9) 0.0106(7) 0.2793(7) 0.050(3) Uani 1 1 d . . . . . C8 C 0.6978(9) -0.0236(7) 0.3484(7) 0.050(3) Uani 1 1 d . . . . . C10 C 0.6158(10) -0.0012(8) 0.4644(8) 0.057(4) Uani 1 1 d . . . . . H10 H 0.5782 0.0322 0.5031 0.068 Uiso 1 1 calc R U . . . C11 C 0.6383(11) -0.0772(8) 0.4772(9) 0.066(4) Uani 1 1 d . . . . . H11 H 0.6183 -0.0953 0.5231 0.079 Uiso 1 1 calc R U . . . C12 C 0.6880(12) -0.1214(9) 0.4224(10) 0.070(4) Uani 1 1 d . . . . . H12 H 0.7004 -0.1728 0.4295 0.084 Uiso 1 1 calc R U . . . C13 C 0.7231(10) -0.0998(7) 0.3568(8) 0.054(3) Uani 1 1 d . . . . . H13 H 0.7623 -0.1339 0.3189 0.065 Uiso 1 1 calc R U . . . C14 C 0.7334(10) 0.1039(8) 0.0609(8) 0.066(4) Uani 1 1 d . . . . . H14A H 0.6869 0.1114 0.0390 0.099 Uiso 1 1 calc R U . . . H14B H 0.7224 0.0722 0.1013 0.099 Uiso 1 1 calc R U . . . H14C H 0.7934 0.0803 0.0265 0.099 Uiso 1 1 calc R U . . . C15 C 0.8541(9) 0.1365(9) 0.2251(8) 0.065(4) Uani 1 1 d . . . . . H15A H 0.9160 0.1107 0.1946 0.098 Uiso 1 1 calc R U . . . H15B H 0.8409 0.1115 0.2699 0.098 Uiso 1 1 calc R U . . . H15C H 0.8485 0.1875 0.2337 0.098 Uiso 1 1 calc R U . . . C16 C 0.7931(11) -0.0381(9) 0.2161(9) 0.064(4) Uani 1 1 d . . . . . C18 C 0.9381(11) -0.0771(10) 0.1356(10) 0.085(5) Uani 1 1 d . . . . . H18 H 0.9988 -0.0764 0.1195 0.101 Uiso 1 1 calc R U . . . C19 C 0.9179(12) -0.1236(11) 0.1017(10) 0.088(6) Uani 1 1 d . . . . . H19 H 0.9627 -0.1533 0.0624 0.106 Uiso 1 1 calc R U . . . C20 C 0.8340(15) -0.1267(14) 0.1249(11) 0.115(8) Uani 1 1 d . . . . . H20 H 0.8177 -0.1582 0.1018 0.138 Uiso 1 1 calc R U . . . C21 C 0.7689(11) -0.0827(12) 0.1844(10) 0.091(6) Uani 1 1 d . . . . . H21 H 0.7088 -0.0848 0.2018 0.110 Uiso 1 1 calc R U . . . C201 C 0.4536(12) 0.3273(9) 0.5131(7) 0.067(4) Uani 1 1 d . . . . . H20A H 0.5077 0.2837 0.4980 0.100 Uiso 1 1 calc R U . . . H20B H 0.3991 0.3123 0.5287 0.100 Uiso 1 1 calc R U . . . H20C H 0.4555 0.3529 0.5521 0.100 Uiso 1 1 calc R U . . . C202 C 0.4512(11) 0.3797(8) 0.4510(7) 0.058(4) Uani 1 1 d . . . . . C203 C 0.5348(10) 0.4054(8) 0.4257(7) 0.057(4) Uani 1 1 d . . . . . H20D H 0.5308 0.4372 0.4633 0.068 Uiso 1 1 calc R U . . . H20E H 0.5893 0.3615 0.4195 0.068 Uiso 1 1 calc R U . . . C204 C 0.5485(8) 0.4466(7) 0.3589(7) 0.044(3) Uani 1 1 d . . . . . C207 C 0.4683(8) 0.5460(6) 0.2493(7) 0.040(3) Uani 1 1 d . . . . . C208 C 0.4875(9) 0.5661(7) 0.1743(7) 0.051(3) Uani 1 1 d . . . . . C210 C 0.5544(12) 0.5296(11) 0.0574(8) 0.068(4) Uani 1 1 d . . . . . H210 H 0.5891 0.4912 0.0226 0.082 Uiso 1 1 calc R U . . . C211 C 0.5235(14) 0.5992(12) 0.0367(9) 0.083(6) Uani 1 1 d . . . . . H211 H 0.5374 0.6102 -0.0118 0.100 Uiso 1 1 calc R U . . . C212 C 0.4725(12) 0.6525(10) 0.0868(10) 0.075(5) Uani 1 1 d . . . . . H212 H 0.4499 0.7013 0.0725 0.089 Uiso 1 1 calc R U . . . C213 C 0.4516(12) 0.6400(8) 0.1572(9) 0.069(4) Uani 1 1 d . . . . . H213 H 0.4156 0.6782 0.1920 0.083 Uiso 1 1 calc R U . . . C214 C 0.3615(9) 0.4427(8) 0.4705(6) 0.052(3) Uani 1 1 d . . . . . H21A H 0.3111 0.4226 0.4840 0.078 Uiso 1 1 calc R U . . . H21B H 0.3595 0.4742 0.4300 0.078 Uiso 1 1 calc R U . . . H21C H 0.3562 0.4719 0.5100 0.078 Uiso 1 1 calc R U . . . C215 C 0.6209(10) 0.4811(8) 0.3370(7) 0.056(3) Uani 1 1 d . . . . . H21D H 0.6061 0.5205 0.3710 0.083 Uiso 1 1 calc R U . . . H21E H 0.6258 0.5018 0.2903 0.083 Uiso 1 1 calc R U . . . H21F H 0.6789 0.4439 0.3351 0.083 Uiso 1 1 calc R U . . . C216 C 0.4059(10) 0.5966(9) 0.3089(9) 0.061(4) Uani 1 1 d . . . . . C218 C 0.388(3) 0.696(2) 0.382(2) 0.084(10) Uiso 0.5 1 d . . P A 1 H218 H 0.4102 0.7303 0.3953 0.100 Uiso 0.5 1 calc R U P A 1 C219 C 0.2971(17) 0.6944(13) 0.4171(13) 0.109(7) Uiso 1 1 d . . . . . H21G H 0.2609 0.7261 0.4572 0.131 Uiso 0.5 1 calc R U P A 2 H219 H 0.2505 0.7370 0.4416 0.131 Uiso 0.5 1 calc R U P A 1 C220 C 0.279(2) 0.6317(19) 0.4144(19) 0.077(9) Uiso 0.5 1 d . . P A 1 H220 H 0.2340 0.6193 0.4527 0.092 Uiso 0.5 1 calc R U P A 1 C221 C 0.327(2) 0.5853(18) 0.3550(17) 0.072(8) Uiso 0.5 1 d . . P A 1 H221 H 0.3068 0.5473 0.3463 0.086 Uiso 0.5 1 calc R U P A 1 C223 C 0.369(2) 0.6556(17) 0.4135(17) 0.063(8) Uiso 0.5 1 d . . P A 2 H223 H 0.3883 0.6566 0.4524 0.076 Uiso 0.5 1 calc R U P A 2 C224 C 0.258(2) 0.6945(16) 0.3538(15) 0.060(7) Uiso 0.5 1 d . . P A 2 H224 H 0.2009 0.7272 0.3531 0.072 Uiso 0.5 1 calc R U P A 2 C225 C 0.3150(17) 0.6431(13) 0.3019(14) 0.048(6) Uiso 0.5 1 d . . P A 2 H225 H 0.2987 0.6364 0.2628 0.057 Uiso 0.5 1 calc R U P A 2 C301 C -0.0255(12) 0.4691(8) 0.2371(10) 0.073(5) Uani 1 1 d . . . . . H30A H -0.0656 0.5079 0.2174 0.109 Uiso 1 1 calc R U . . . H30B H 0.0082 0.4908 0.2560 0.109 Uiso 1 1 calc R U . . . H30C H -0.0619 0.4455 0.2750 0.109 Uiso 1 1 calc R U . . . C302 C 0.0403(11) 0.4124(8) 0.1803(9) 0.058(4) Uani 1 1 d . . . . . C303 C -0.0066(9) 0.3696(7) 0.1537(8) 0.055(4) Uani 1 1 d . . . . . H30D H -0.0509 0.3555 0.1950 0.066 Uiso 1 1 calc R U . . . H30E H -0.0412 0.4030 0.1257 0.066 Uiso 1 1 calc R U . . . C304 C 0.0549(10) 0.3016(8) 0.1099(8) 0.059(4) Uani 1 1 d . . . . . C307 C 0.2446(10) 0.2214(8) 0.0017(8) 0.054(4) Uani 1 1 d . . . . . C308 C 0.3131(9) 0.1526(8) -0.0341(7) 0.051(3) Uani 1 1 d . . . . . C310 C 0.3790(9) 0.0296(8) -0.0239(8) 0.061(4) Uani 1 1 d . . . . . H310 H 0.3828 -0.0133 0.0035 0.073 Uiso 1 1 calc R U . . . C311 C 0.4342(10) 0.0225(9) -0.0912(8) 0.065(4) Uani 1 1 d . . . . . H311 H 0.4774 -0.0241 -0.1094 0.078 Uiso 1 1 calc R U . . . C312 C 0.4284(10) 0.0811(10) -0.1327(8) 0.066(4) Uani 1 1 d . . . . . H312 H 0.4656 0.0764 -0.1809 0.080 Uiso 1 1 calc R U . . . C313 C 0.3652(11) 0.1503(10) -0.1026(8) 0.068(4) Uani 1 1 d . . . . . H313 H 0.3596 0.1934 -0.1296 0.082 Uiso 1 1 calc R U . . . C314 C 0.0967(11) 0.4497(8) 0.1216(8) 0.066(4) Uani 1 1 d . . . . . H31A H 0.0570 0.4859 0.0996 0.098 Uiso 1 1 calc R U . . . H31B H 0.1428 0.4124 0.0861 0.098 Uiso 1 1 calc R U . . . H31C H 0.1266 0.4745 0.1413 0.098 Uiso 1 1 calc R U . . . C315 C 0.0139(10) 0.2641(8) 0.0739(8) 0.069(4) Uani 1 1 d . . . . . H31D H -0.0522 0.2802 0.0968 0.103 Uiso 1 1 calc R U . . . H31E H 0.0386 0.2106 0.0772 0.103 Uiso 1 1 calc R U . . . H31F H 0.0285 0.2772 0.0243 0.103 Uiso 1 1 calc R U . . . C316 C 0.2319(10) 0.2929(8) -0.0361(8) 0.059(4) Uani 1 1 d . . . . . C317 C 0.2815(12) 0.3395(9) -0.0388(10) 0.081(5) Uani 1 1 d . . . . . H317 H 0.3278 0.3268 -0.0182 0.098 Uiso 1 1 calc R U . . . C318 C 0.2604(13) 0.4060(10) -0.0733(11) 0.095(6) Uani 1 1 d . . . . . H318 H 0.2911 0.4404 -0.0754 0.115 Uiso 1 1 calc R U . . . C319 C 0.1976(15) 0.4202(12) -0.1027(13) 0.110(7) Uani 1 1 d . . . . . H319 H 0.1844 0.4647 -0.1271 0.132 Uiso 1 1 calc R U . . . C320 C 0.1517(18) 0.3735(12) -0.0991(15) 0.133(10) Uani 1 1 d . . . . . H320 H 0.1059 0.3866 -0.1203 0.159 Uiso 1 1 calc R U . . . C401 C 0.2174(12) -0.0282(7) 0.2832(10) 0.077(5) Uani 1 1 d . . . . . H40A H 0.2152 -0.0758 0.3037 0.115 Uiso 1 1 calc R U . . . H40B H 0.2804 -0.0320 0.2556 0.115 Uiso 1 1 calc R U . . . H40C H 0.1803 -0.0141 0.2525 0.115 Uiso 1 1 calc R U . . . C402 C 0.1810(12) 0.0296(8) 0.3414(9) 0.062(4) Uani 1 1 d . . . . . C403 C 0.0768(10) 0.0513(8) 0.3718(7) 0.054(3) Uani 1 1 d . . . . . H40D H 0.0538 0.0585 0.3318 0.065 Uiso 1 1 calc R U . . . H40E H 0.0614 0.0090 0.3980 0.065 Uiso 1 1 calc R U . . . C404 C 0.0261(8) 0.1179(6) 0.4191(7) 0.043(3) Uani 1 1 d . . . . . C407 C 0.0072(10) 0.2403(8) 0.5191(9) 0.056(4) Uani 1 1 d . . . . . C408 C -0.0366(10) 0.3168(8) 0.5486(8) 0.054(4) Uani 1 1 d . . . . . C410 C -0.0947(10) 0.4384(8) 0.5199(10) 0.073(5) Uani 1 1 d . . . . . H410 H -0.1087 0.4737 0.4863 0.087 Uiso 1 1 calc R U . . . C411 C -0.1182(11) 0.4624(10) 0.5899(10) 0.073(5) Uani 1 1 d . . . . . H411 H -0.1471 0.5130 0.6038 0.088 Uiso 1 1 calc R U . . . C412 C -0.0974(11) 0.4095(9) 0.6373(9) 0.068(5) Uani 1 1 d . . . . . H412 H -0.1100 0.4240 0.6844 0.082 Uiso 1 1 calc R U . . . C413 C -0.0589(10) 0.3361(10) 0.6173(9) 0.074(5) Uani 1 1 d . . . . . H413 H -0.0480 0.2996 0.6508 0.089 Uiso 1 1 calc R U . . . C414 C 0.2243(10) 0.0055(9) 0.3985(8) 0.064(4) Uani 1 1 d . . . . . H41A H 0.2135 -0.0401 0.4187 0.097 Uiso 1 1 calc R U . . . H41B H 0.1973 0.0442 0.4355 0.097 Uiso 1 1 calc R U . . . H41C H 0.2897 -0.0031 0.3780 0.097 Uiso 1 1 calc R U . . . C415 C -0.0720(9) 0.1330(8) 0.4580(9) 0.067(4) Uani 1 1 d . . . . . H41D H -0.1054 0.1840 0.4511 0.100 Uiso 1 1 calc R U . . . H41E H -0.0815 0.1254 0.5083 0.100 Uiso 1 1 calc R U . . . H41F H -0.0939 0.0994 0.4405 0.100 Uiso 1 1 calc R U . . . C416 C 0.0270(9) 0.1769(8) 0.5672(7) 0.056(4) Uani 1 1 d . . . . . C418 C -0.0304(13) 0.1178(11) 0.6675(9) 0.080(5) Uani 1 1 d . . . . . H418 H -0.0789 0.1154 0.7087 0.096 Uiso 1 1 calc R U . . . C419 C 0.0545(14) 0.0615(10) 0.6524(10) 0.080(5) Uani 1 1 d . . . . . H419 H 0.0618 0.0215 0.6833 0.096 Uiso 1 1 calc R U . . . C420 C 0.1255(12) 0.0638(9) 0.5946(9) 0.071(4) Uani 1 1 d . . . . . H420 H 0.1821 0.0253 0.5836 0.085 Uiso 1 1 calc R U . . . C421 C 0.1133(11) 0.1243(8) 0.5515(9) 0.066(4) Uani 1 1 d . . . . . H421 H 0.1626 0.1297 0.5124 0.079 Uiso 1 1 calc R U . . . N5 N 0.7228(7) 0.1127(6) 0.2128(6) 0.056(3) Uani 1 1 d . . . . . N6 N 0.7023(8) 0.0809(6) 0.2783(6) 0.049(3) Uani 1 1 d . . . . . N9 N 0.6440(7) 0.0263(6) 0.4017(6) 0.052(3) Uani 1 1 d . . . . . N17 N 0.8760(9) -0.0309(8) 0.1918(7) 0.073(4) Uani 1 1 d . . . . . N205 N 0.4978(7) 0.4468(6) 0.3246(5) 0.049(3) Uani 1 1 d . . . . . N206 N 0.5102(8) 0.4774(6) 0.2584(6) 0.048(3) Uani 1 1 d . . . . . N209 N 0.5376(7) 0.5129(6) 0.1261(5) 0.045(2) Uani 1 1 d . . . . . N217 N 0.444(2) 0.6425(16) 0.3265(16) 0.079(8) Uiso 0.5 1 d . . P A 1 N222 N 0.4288(15) 0.6088(12) 0.3584(12) 0.048(5) Uiso 0.5 1 d . . P A 2 N305 N 0.1375(8) 0.2821(7) 0.1028(6) 0.049(3) Uani 1 1 d . . . . . N306 N 0.1966(8) 0.2176(6) 0.0668(7) 0.053(3) Uani 1 1 d . . . . . N309 N 0.3198(7) 0.0930(6) 0.0061(6) 0.048(3) Uani 1 1 d . . . . . N321 N 0.1684(11) 0.3072(9) -0.0658(9) 0.097(5) Uani 1 1 d . . . . . N405 N 0.0704(8) 0.1622(6) 0.4205(6) 0.047(3) Uani 1 1 d . . . . . N406 N 0.0253(8) 0.2301(7) 0.4532(7) 0.053(3) Uani 1 1 d . . . . . N409 N -0.0544(8) 0.3692(7) 0.4997(7) 0.061(3) Uani 1 1 d . . . . . N417 N -0.0442(9) 0.1754(7) 0.6243(7) 0.067(3) Uani 1 1 d . . . . . S1 S 0.6095(2) 0.28196(19) 0.26806(17) 0.0506(8) Uani 1 1 d . . . . . S2 S 0.5176(2) 0.34205(17) 0.12695(16) 0.0440(7) Uani 1 1 d . . . . . S3 S 0.5030(2) 0.14937(17) 0.19987(17) 0.0455(7) Uani 1 1 d . . . . . S4 S 0.4662(2) 0.19084(16) 0.40084(16) 0.0429(7) Uani 1 1 d . . . . . S5 S 0.3340(2) 0.36821(17) 0.32090(16) 0.0438(7) Uani 1 1 d . . . . . S6 S 0.2957(2) 0.30836(16) 0.15745(17) 0.0459(7) Uani 1 1 d . . . . . S7 S 0.1041(2) 0.37621(17) 0.34062(19) 0.0503(8) Uani 1 1 d . . . . . S8 S 0.0932(2) 0.21828(17) 0.2585(2) 0.0538(8) Uani 1 1 d . . . . . S9 S 0.3267(2) 0.09267(16) 0.17664(17) 0.0453(7) Uani 1 1 d . . . . . S10 S 0.2771(2) 0.17895(16) 0.36128(17) 0.0434(7) Uani 1 1 d . . . . . Zn1 Zn 0.61943(11) 0.13527(9) 0.37485(9) 0.0503(4) Uani 1 1 d . . . . . Zn2 Zn 0.58410(11) 0.41033(9) 0.16661(8) 0.0483(4) Uani 1 1 d . . . . . Zn3 Zn 0.23334(10) 0.11238(8) 0.11015(8) 0.0488(4) Uani 1 1 d . . . . . Zn4 Zn -0.01062(11) 0.32745(9) 0.39832(9) 0.0552(4) Uani 1 1 d . . . . . Zn5 Zn 0.43587(10) 0.13433(8) 0.31851(7) 0.0437(3) Uani 1 1 d . . . . . Zn6 Zn 0.39225(10) 0.18677(8) 0.14457(8) 0.0454(3) Uani 1 1 d . . . . . Zn7 Zn 0.36407(10) 0.37662(7) 0.19968(7) 0.0418(3) Uani 1 1 d . . . . . Zn8 Zn 0.22643(10) 0.30741(7) 0.37685(8) 0.0438(3) Uani 1 1 d . . . . . Sn1 Sn 0.59694(6) 0.22626(5) 0.16946(4) 0.0436(2) Uani 1 1 d . . . . . Sn2 Sn 0.46168(6) 0.31593(5) 0.35991(4) 0.0432(2) Uani 1 1 d . . . . . Sn3 Sn 0.13832(6) 0.32786(4) 0.22261(5) 0.0478(2) Uani 1 1 d . . . . . Sn4 Sn 0.21273(6) 0.13067(4) 0.29409(5) 0.0458(2) Uani 1 1 d . . . . . I1 I 0.70381(8) 0.18045(6) 0.43526(7) 0.0779(3) Uani 1 1 d . . . . . I2 I 0.75363(6) 0.39205(5) 0.13157(5) 0.0589(2) Uani 1 1 d . . . . . I3 I 0.11944(7) 0.04566(6) 0.12425(7) 0.0768(3) Uani 1 1 d . . . . . I4 I -0.15348(6) 0.34107(6) 0.37151(6) 0.0695(3) Uani 1 1 d . . . . . I5 I 0.48607(6) -0.00855(4) 0.32819(5) 0.0495(2) Uani 1 1 d . . . . . I6 I 0.49228(6) 0.17607(5) 0.01184(4) 0.0514(2) Uani 1 1 d . . . . . I7 I 0.29308(6) 0.51335(4) 0.17052(5) 0.0499(2) Uani 1 1 d . . . . . I8 I 0.18672(6) 0.32781(5) 0.51139(4) 0.0479(2) Uani 1 1 d . . . . . C5 C -0.0762(11) 0.3326(10) 0.8348(7) 0.105(10) Uani 0.75 1 d D U P B 1 H5 H -0.1163 0.3800 0.8230 0.126 Uiso 0.75 1 calc R U P B 1 O401 O 0.057(3) 0.212(2) 0.745(2) 0.071(11) Uiso 0.25 1 d . . P C 2 H40H H 0.0085 0.2344 0.7808 0.106 Uiso 0.25 1 d R U P C 2 H40I H 0.0553 0.2376 0.7079 0.106 Uiso 0.25 1 d R U P C 2 Cl4 Cl 0.0345(7) 0.3212(5) 0.7817(5) 0.138(3) Uani 0.75 1 d D . P B 1 Cl5 Cl -0.1106(6) 0.2605(5) 0.8186(4) 0.121(3) Uani 0.75 1 d D . P B 1 Cl6 Cl -0.0899(7) 0.3364(4) 0.9233(4) 0.120(3) Uani 0.75 1 d D . P B 1 C200 C 0.816(3) 0.144(3) 0.839(3) 0.054(13) Uiso 0.25 1 d D . P D 1 H20F H 0.8543 0.1356 0.7892 0.081 Uiso 0.25 1 calc R U P D 1 H20G H 0.8200 0.0970 0.8620 0.081 Uiso 0.25 1 calc R U P D 1 H20H H 0.8363 0.1744 0.8620 0.081 Uiso 0.25 1 calc R U P D 1 O201 O 0.723(3) 0.182(2) 0.844(2) 0.082(12) Uiso 0.25 1 d D . P D 1 H201 H 0.6902 0.1575 0.8672 0.123 Uiso 0.25 1 calc R U P D 1 C100 C 0.401(5) 0.816(4) 0.229(4) 0.23(4) Uiso 0.5 1 d D . P . . H10A H 0.4447 0.8056 0.1814 0.350 Uiso 0.5 1 calc R U P . . H10B H 0.3665 0.8690 0.2350 0.350 Uiso 0.5 1 calc R U P . . H10C H 0.3584 0.7883 0.2367 0.350 Uiso 0.5 1 calc R U P . . O101 O 0.4475(18) 0.7952(14) 0.2797(14) 0.094(7) Uiso 0.5 1 d D . P . . H101 H 0.4274 0.7650 0.3074 0.141 Uiso 0.5 1 calc R U P . . C300 C 0.369(2) 0.3116(12) 0.6993(16) 0.19(3) Uani 0.5 1 d D U P E 2 H300 H 0.4130 0.3308 0.6618 0.232 Uiso 0.5 1 calc R U P E 2 Cl1 Cl 0.4039(11) 0.2191(7) 0.6824(8) 0.138(5) Uani 0.5 1 d D . P E 2 Cl2 Cl 0.2640(14) 0.3592(15) 0.6926(10) 0.231(12) Uani 0.5 1 d D . P E 2 Cl3 Cl 0.3828(13) 0.3245(8) 0.7760(11) 0.174(7) Uani 0.5 1 d D . P E 2 O400 O 0.146(3) 0.297(2) 0.721(2) 0.080(12) Uiso 0.25 1 d . . P F 2 H40F H 0.1226 0.2721 0.7014 0.120 Uiso 0.25 1 d R U P F 2 H40G H 0.1993 0.2678 0.7232 0.120 Uiso 0.25 1 d R U P F 2 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 0.051(8) 0.062(9) 0.048(8) 0.008(7) -0.011(7) -0.007(7) C2 0.047(7) 0.037(7) 0.050(8) 0.012(6) -0.009(6) -0.004(6) C3 0.035(7) 0.059(8) 0.067(9) 0.017(7) -0.007(7) 0.007(6) C4 0.040(7) 0.038(7) 0.066(9) 0.005(6) -0.017(7) 0.001(6) C7 0.047(8) 0.048(8) 0.060(9) 0.015(7) -0.026(7) -0.017(6) C8 0.044(7) 0.049(8) 0.061(9) 0.014(7) -0.028(7) -0.011(6) C10 0.046(8) 0.051(8) 0.064(10) 0.018(7) -0.016(7) -0.012(7) C11 0.063(10) 0.060(9) 0.080(11) 0.032(9) -0.039(9) -0.017(8) C12 0.072(11) 0.053(10) 0.084(13) 0.014(10) -0.029(10) -0.018(9) C13 0.058(9) 0.038(7) 0.069(10) 0.016(7) -0.034(8) -0.010(6) C14 0.056(9) 0.069(10) 0.055(9) -0.019(7) 0.005(7) -0.017(8) C15 0.046(8) 0.074(10) 0.066(10) 0.013(8) -0.009(7) -0.019(7) C16 0.059(10) 0.075(11) 0.062(10) 0.009(9) -0.027(9) -0.024(9) C18 0.052(10) 0.096(13) 0.097(14) -0.025(11) -0.011(9) -0.020(9) C19 0.051(10) 0.115(15) 0.086(13) -0.031(11) -0.005(9) -0.021(10) C20 0.104(16) 0.17(2) 0.099(15) -0.057(15) -0.032(13) -0.063(16) C21 0.048(9) 0.133(16) 0.087(13) -0.042(12) -0.013(9) -0.020(10) C201 0.091(11) 0.097(12) 0.033(7) 0.007(7) -0.024(7) -0.055(10) C202 0.087(11) 0.073(9) 0.037(7) 0.002(6) -0.028(7) -0.047(9) C203 0.081(10) 0.060(8) 0.046(8) 0.003(6) -0.034(7) -0.029(8) C204 0.034(6) 0.050(7) 0.055(8) 0.005(6) -0.027(6) -0.009(6) C207 0.044(7) 0.031(6) 0.051(7) 0.005(6) -0.020(6) -0.015(6) C208 0.050(8) 0.049(8) 0.064(9) 0.021(7) -0.027(7) -0.026(7) C210 0.079(11) 0.104(13) 0.035(8) 0.008(8) -0.020(8) -0.046(10) C211 0.105(15) 0.125(16) 0.054(11) 0.032(12) -0.039(11) -0.074(14) C212 0.080(12) 0.073(11) 0.092(14) 0.050(11) -0.057(11) -0.033(10) C213 0.083(11) 0.055(9) 0.074(11) 0.005(8) -0.027(9) -0.031(9) C214 0.049(8) 0.066(9) 0.032(7) -0.016(6) 0.000(6) -0.015(7) C215 0.069(9) 0.059(8) 0.048(8) 0.016(6) -0.033(7) -0.023(7) C216 0.042(8) 0.064(10) 0.074(11) -0.019(8) -0.015(8) -0.015(7) C301 0.080(11) 0.043(9) 0.107(13) -0.026(9) -0.060(11) 0.002(8) C302 0.060(10) 0.040(9) 0.068(10) -0.006(8) -0.029(8) -0.001(8) C303 0.052(8) 0.031(7) 0.083(10) -0.016(6) -0.046(8) 0.013(6) C304 0.050(9) 0.058(9) 0.068(10) 0.002(7) -0.025(8) -0.013(7) C307 0.054(8) 0.052(9) 0.064(10) -0.004(7) -0.019(8) -0.026(7) C308 0.045(8) 0.050(8) 0.049(8) -0.007(7) -0.007(7) -0.010(7) C310 0.053(9) 0.065(10) 0.060(9) -0.018(8) -0.006(7) -0.019(8) C311 0.048(9) 0.069(10) 0.058(10) -0.021(8) 0.005(7) -0.011(8) C312 0.058(9) 0.088(12) 0.045(9) -0.018(9) -0.001(7) -0.026(9) C313 0.069(10) 0.090(12) 0.057(9) -0.003(9) -0.016(8) -0.043(10) C314 0.079(10) 0.047(8) 0.080(11) 0.000(7) -0.050(9) -0.006(7) C315 0.055(9) 0.073(10) 0.081(11) -0.036(8) -0.021(8) -0.016(8) C316 0.059(9) 0.053(8) 0.070(10) 0.001(7) -0.026(8) -0.021(7) C317 0.074(11) 0.061(10) 0.123(15) 0.012(10) -0.055(11) -0.018(8) C318 0.096(13) 0.079(12) 0.147(18) 0.052(12) -0.078(14) -0.046(11) C319 0.110(16) 0.094(14) 0.17(2) 0.050(14) -0.100(17) -0.050(13) C320 0.18(2) 0.099(16) 0.21(3) 0.074(17) -0.16(2) -0.084(17) C401 0.069(11) 0.025(7) 0.105(14) -0.010(8) 0.007(10) -0.011(7) C402 0.067(10) 0.041(9) 0.073(11) -0.015(8) -0.003(9) -0.029(8) C403 0.056(9) 0.063(9) 0.045(8) -0.003(7) -0.011(7) -0.025(7) C404 0.041(7) 0.029(6) 0.054(8) 0.005(6) -0.015(6) -0.007(5) C407 0.043(8) 0.062(10) 0.062(10) -0.004(8) -0.013(8) -0.019(7) C408 0.046(8) 0.050(9) 0.054(9) -0.020(8) 0.001(7) -0.013(7) C410 0.064(10) 0.044(8) 0.098(13) -0.041(9) -0.017(9) -0.004(7) C411 0.052(9) 0.070(11) 0.096(13) -0.028(11) -0.019(9) -0.016(8) C412 0.057(10) 0.067(11) 0.072(11) -0.028(9) 0.001(9) -0.025(8) C413 0.050(9) 0.085(12) 0.076(11) -0.036(10) 0.001(8) -0.021(8) C414 0.044(8) 0.079(10) 0.070(10) 0.005(8) -0.014(7) -0.026(8) C415 0.043(8) 0.065(9) 0.088(11) -0.012(8) -0.011(8) -0.020(7) C416 0.046(8) 0.063(9) 0.057(9) -0.023(7) -0.007(7) -0.020(7) C418 0.088(13) 0.097(14) 0.072(11) -0.017(10) -0.021(10) -0.052(12) C419 0.098(14) 0.074(11) 0.093(13) -0.009(10) -0.048(12) -0.040(11) C420 0.068(10) 0.068(10) 0.087(12) -0.009(9) -0.035(10) -0.023(8) C421 0.070(10) 0.064(10) 0.073(10) -0.001(8) -0.027(9) -0.029(8) N5 0.050(7) 0.059(7) 0.066(8) 0.016(6) -0.023(6) -0.026(6) N6 0.052(7) 0.040(6) 0.053(7) 0.015(5) -0.020(6) -0.014(5) N9 0.043(6) 0.058(7) 0.057(7) 0.013(6) -0.020(6) -0.020(6) N17 0.052(8) 0.088(10) 0.075(9) -0.014(8) -0.014(7) -0.023(7) N205 0.054(7) 0.052(6) 0.044(6) 0.005(5) -0.020(5) -0.017(5) N206 0.055(7) 0.054(7) 0.050(7) 0.011(5) -0.026(6) -0.030(6) N209 0.045(6) 0.053(7) 0.040(6) 0.008(5) -0.016(5) -0.020(5) N305 0.052(7) 0.050(8) 0.043(7) -0.009(6) -0.015(6) -0.012(6) N306 0.052(7) 0.037(7) 0.065(8) -0.017(6) -0.020(7) -0.004(6) N309 0.042(6) 0.042(7) 0.053(7) -0.016(6) -0.007(6) -0.012(5) N321 0.112(12) 0.087(11) 0.138(14) 0.030(10) -0.085(12) -0.052(10) N405 0.041(6) 0.040(7) 0.051(7) -0.013(6) -0.011(6) -0.001(5) N406 0.044(7) 0.046(8) 0.064(9) -0.013(6) -0.007(6) -0.016(6) N409 0.041(7) 0.059(8) 0.065(8) -0.019(7) -0.004(6) -0.004(6) N417 0.069(8) 0.071(8) 0.069(8) 0.000(7) -0.025(7) -0.032(7) S1 0.0480(18) 0.061(2) 0.0479(19) 0.0025(15) -0.0165(15) -0.0235(16) S2 0.0444(17) 0.0441(17) 0.0411(17) 0.0037(13) -0.0168(14) -0.0093(14) S3 0.0442(17) 0.0435(17) 0.0473(18) 0.0019(14) -0.0154(15) -0.0121(14) S4 0.0428(16) 0.0399(16) 0.0469(17) 0.0074(13) -0.0194(14) -0.0115(13) S5 0.0442(17) 0.0462(17) 0.0406(17) -0.0006(13) -0.0142(14) -0.0136(14) S6 0.0487(18) 0.0384(16) 0.0516(19) -0.0036(14) -0.0220(16) -0.0088(14) S7 0.0517(19) 0.0386(16) 0.062(2) -0.0096(15) -0.0255(17) -0.0077(14) S8 0.0488(19) 0.0401(17) 0.073(2) -0.0080(16) -0.0232(18) -0.0097(15) S9 0.0420(17) 0.0386(16) 0.0503(18) -0.0050(14) -0.0123(15) -0.0085(13) S10 0.0417(16) 0.0338(15) 0.0518(18) -0.0020(13) -0.0151(14) -0.0082(13) Zn1 0.0476(9) 0.0506(9) 0.0573(10) 0.0100(8) -0.0236(8) -0.0175(7) Zn2 0.0430(9) 0.0523(9) 0.0493(9) 0.0000(7) -0.0164(7) -0.0137(7) Zn3 0.0428(8) 0.0451(8) 0.0526(9) -0.0096(7) -0.0101(7) -0.0100(7) Zn4 0.0485(9) 0.0498(9) 0.0671(11) -0.0089(8) -0.0213(8) -0.0110(7) Zn5 0.0425(8) 0.0412(8) 0.0449(8) 0.0028(6) -0.0151(7) -0.0103(6) Zn6 0.0459(8) 0.0405(8) 0.0481(8) -0.0018(6) -0.0160(7) -0.0108(6) Zn7 0.0451(8) 0.0394(7) 0.0415(8) 0.0009(6) -0.0169(7) -0.0115(6) Zn8 0.0434(8) 0.0393(7) 0.0473(8) -0.0024(6) -0.0155(7) -0.0103(6) Sn1 0.0411(5) 0.0421(5) 0.0415(5) 0.0048(4) -0.0119(4) -0.0088(4) Sn2 0.0492(5) 0.0449(5) 0.0397(5) 0.0039(4) -0.0180(4) -0.0179(4) Sn3 0.0483(5) 0.0359(4) 0.0599(6) -0.0082(4) -0.0255(4) -0.0044(4) Sn4 0.0452(5) 0.0378(4) 0.0498(5) -0.0070(4) -0.0100(4) -0.0118(4) I1 0.0755(7) 0.0824(7) 0.1022(9) 0.0111(6) -0.0558(7) -0.0339(6) I2 0.0445(5) 0.0570(5) 0.0728(6) 0.0123(5) -0.0183(5) -0.0174(4) I3 0.0531(6) 0.0733(7) 0.0996(8) -0.0324(6) -0.0059(6) -0.0266(5) I4 0.0469(5) 0.0697(6) 0.0905(8) -0.0126(5) -0.0276(5) -0.0085(5) I5 0.0484(5) 0.0411(4) 0.0542(5) 0.0015(4) -0.0163(4) -0.0096(4) I6 0.0551(5) 0.0495(5) 0.0479(5) 0.0065(4) -0.0158(4) -0.0173(4) I7 0.0482(5) 0.0407(4) 0.0576(5) 0.0035(4) -0.0194(4) -0.0091(4) I8 0.0475(5) 0.0491(5) 0.0459(5) -0.0008(4) -0.0152(4) -0.0137(4) C5 0.12(2) 0.065(14) 0.092(18) -0.034(13) -0.052(17) 0.052(14) Cl4 0.130(7) 0.146(8) 0.134(7) 0.012(6) -0.032(6) -0.055(6) Cl5 0.146(7) 0.116(6) 0.114(6) -0.002(5) -0.044(5) -0.055(5) Cl6 0.172(8) 0.112(6) 0.091(5) 0.012(4) -0.060(5) -0.049(6) C300 0.17(5) 0.27(7) 0.09(3) -0.04(4) 0.08(3) -0.12(5) Cl1 0.176(13) 0.088(7) 0.170(13) 0.026(8) -0.058(11) -0.073(8) Cl2 0.159(16) 0.39(3) 0.139(14) -0.063(17) 0.037(12) -0.16(2) Cl3 0.208(17) 0.119(11) 0.23(2) 0.008(11) -0.090(16) -0.088(12) _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 C2 1.525(18) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 C3 1.54(2) . ? C2 C14 1.579(18) . ? C2 Sn1 2.203(13) . ? C3 C4 1.551(19) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 N5 1.279(16) . ? C4 C15 1.43(2) . ? C7 N6 1.277(16) . ? C7 C8 1.492(18) . ? C7 C16 1.50(2) . ? C8 N9 1.354(18) . ? C8 C13 1.397(17) . ? C10 N9 1.323(17) . ? C10 C11 1.408(19) . ? C10 H10 0.9500 . ? C11 C12 1.30(2) . ? C11 H11 0.9500 . ? C12 C13 1.34(2) . ? C12 H12 0.9500 . ? C13 H13 0.9500 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 N17 1.34(2) . ? C16 C21 1.34(2) . ? C18 C19 1.36(2) . ? C18 N17 1.38(2) . ? C18 H18 0.9500 . ? C19 C20 1.32(2) . ? C19 H19 0.9500 . ? C20 C21 1.42(3) . ? C20 H20 0.9500 . ? C21 H21 0.9500 . ? C201 C202 1.544(19) . ? C201 H20A 0.9800 . ? C201 H20B 0.9800 . ? C201 H20C 0.9800 . ? C202 C214 1.52(2) . ? C202 C203 1.533(19) . ? C202 Sn2 2.229(12) . ? C203 C204 1.493(18) . ? C203 H20D 0.9900 . ? C203 H20E 0.9900 . ? C204 N205 1.259(15) . ? C204 C215 1.480(17) . ? C207 N206 1.303(16) . ? C207 C216 1.47(2) . ? C207 C208 1.484(18) . ? C208 N209 1.320(18) . ? C208 C213 1.411(19) . ? C210 C211 1.35(2) . ? C210 N209 1.353(17) . ? C210 H210 0.9500 . ? C211 C212 1.35(3) . ? C211 H211 0.9500 . ? C212 C213 1.37(2) . ? C212 H212 0.9500 . ? C213 H213 0.9500 . ? C214 H21A 0.9800 . ? C214 H21B 0.9800 . ? C214 H21C 0.9800 . ? C215 H21D 0.9800 . ? C215 H21E 0.9800 . ? C215 H21F 0.9800 . ? C216 N222 1.25(3) . ? C216 N217 1.38(3) . ? C216 C221 1.39(3) . ? C216 C225 1.52(3) . ? C218 N217 1.42(5) . ? C218 C219 1.44(4) . ? C218 H218 0.9500 . ? C219 C223 1.16(4) . ? C219 C220 1.34(4) . ? C219 C224 1.62(4) . ? C219 H21G 0.9500 . ? C219 H219 0.9500 . ? C220 C221 1.39(4) . ? C220 H220 0.9500 . ? C221 H221 0.9500 . ? C223 N222 1.36(4) . ? C223 H223 0.9500 . ? C224 C225 1.36(4) . ? C224 H224 0.9500 . ? C225 H225 0.9500 . ? C301 C302 1.51(2) . ? C301 H30A 0.9800 . ? C301 H30B 0.9800 . ? C301 H30C 0.9800 . ? C302 C314 1.53(2) . ? C302 C303 1.537(19) . ? C302 Sn3 2.234(16) . ? C303 C304 1.49(2) . ? C303 H30D 0.9900 . ? C303 H30E 0.9900 . ? C304 N305 1.252(18) . ? C304 C315 1.507(18) . ? C307 N306 1.294(18) . ? C307 C308 1.48(2) . ? C307 C316 1.50(2) . ? C308 N309 1.344(18) . ? C308 C313 1.35(2) . ? C310 N309 1.322(18) . ? C310 C311 1.341(19) . ? C310 H310 0.9500 . ? C311 C312 1.34(2) . ? C311 H311 0.9500 . ? C312 C313 1.42(2) . ? C312 H312 0.9500 . ? C313 H313 0.9500 . ? C314 H31A 0.9800 . ? C314 H31B 0.9800 . ? C314 H31C 0.9800 . ? C315 H31D 0.9800 . ? C315 H31E 0.9800 . ? C315 H31F 0.9800 . ? C316 N321 1.33(2) . ? C316 C317 1.39(2) . ? C317 C318 1.40(2) . ? C317 H317 0.9500 . ? C318 C319 1.31(2) . ? C318 H318 0.9500 . ? C319 C320 1.34(2) . ? C319 H319 0.9500 . ? C320 N321 1.38(2) . ? C320 H320 0.9500 . ? C401 C402 1.51(2) . ? C401 H40A 0.9800 . ? C401 H40B 0.9800 . ? C401 H40C 0.9800 . ? C402 C414 1.52(2) . ? C402 C403 1.54(2) . ? C402 Sn4 2.232(14) . ? C403 C404 1.487(19) . ? C403 H40D 0.9900 . ? C403 H40E 0.9900 . ? C404 N405 1.304(15) . ? C404 C415 1.481(18) . ? C407 N406 1.281(19) . ? C407 C408 1.48(2) . ? C407 C416 1.51(2) . ? C408 C413 1.36(2) . ? C408 N409 1.38(2) . ? C410 N409 1.305(18) . ? C410 C411 1.41(2) . ? C410 H410 0.9500 . ? C411 C412 1.38(2) . ? C411 H411 0.9500 . ? C412 C413 1.37(2) . ? C412 H412 0.9500 . ? C413 H413 0.9500 . ? C414 H41A 0.9800 . ? C414 H41B 0.9800 . ? C414 H41C 0.9800 . ? C415 H41D 0.9800 . ? C415 H41E 0.9800 . ? C415 H41F 0.9800 . ? C416 N417 1.345(18) . ? C416 C421 1.40(2) . ? C418 N417 1.36(2) . ? C418 C419 1.41(3) . ? C418 H418 0.9500 . ? C419 C420 1.36(2) . ? C419 H419 0.9500 . ? C420 C421 1.40(2) . ? C420 H420 0.9500 . ? C421 H421 0.9500 . ? N5 N6 1.391(15) . ? N6 Zn1 2.087(12) . ? N9 Zn1 2.060(11) . ? N205 N206 1.393(15) . ? N206 Zn2 2.102(12) . ? N209 Zn2 2.076(11) . ? N305 N306 1.376(18) . ? N306 Zn3 2.118(12) . ? N309 Zn3 2.081(11) . ? N405 N406 1.365(18) . ? N406 Zn4 2.110(13) . ? N409 Zn4 2.065(13) . ? S1 Sn2 2.429(3) . ? S1 Sn1 2.446(3) . ? S2 Zn2 2.310(3) . ? S2 Zn7 2.357(3) . ? S2 Sn1 2.437(3) . ? S3 Zn5 2.312(3) . ? S3 Zn6 2.355(4) . ? S3 Sn1 2.387(3) . ? S4 Zn1 2.291(3) . ? S4 Zn5 2.339(3) . ? S4 Sn2 2.462(3) . ? S5 Zn7 2.333(3) . ? S5 Zn8 2.365(3) . ? S5 Sn2 2.390(3) . ? S6 Zn6 2.333(3) . ? S6 Zn7 2.364(3) . ? S6 Sn3 2.399(3) . ? S7 Zn4 2.307(4) . ? S7 Zn8 2.340(4) . ? S7 Sn3 2.450(3) . ? S8 Sn4 2.418(4) . ? S8 Sn3 2.437(3) . ? S9 Zn3 2.304(4) . ? S9 Zn6 2.343(3) . ? S9 Sn4 2.460(3) . ? S10 Zn5 2.340(3) . ? S10 Zn8 2.343(3) . ? S10 Sn4 2.393(3) . ? Zn1 I1 2.5249(18) . ? Zn2 I2 2.5568(18) . ? Zn3 I3 2.5424(17) . ? Zn4 I4 2.5335(18) . ? Zn5 I5 2.6061(16) . ? Zn6 I6 2.6108(17) . ? Zn7 I7 2.6100(16) . ? Zn8 I8 2.6054(16) . ? C5 Cl4 1.728(13) . ? C5 Cl6 1.732(14) . ? C5 Cl5 1.758(13) . ? C5 H5 1.0000 . ? O401 H40H 0.8822 . ? O401 H40I 0.8710 . ? C200 O201 1.44(2) . ? C200 H20F 0.9800 . ? C200 H20G 0.9800 . ? C200 H20H 0.9800 . ? O201 H201 0.8400 . ? C100 O101 1.45(2) . ? C100 H10A 0.9800 . ? C100 H10B 0.9800 . ? C100 H10C 0.9800 . ? O101 H101 0.8400 . ? C300 Cl3 1.698(16) . ? C300 Cl1 1.705(16) . ? C300 Cl2 1.718(16) . ? C300 H300 1.0000 . ? O400 H40F 0.8902 . ? O400 H40G 0.8942 . ? 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 C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C1 C2 C3 111.6(11) . . ? C1 C2 C14 108.9(12) . . ? C3 C2 C14 112.0(11) . . ? C1 C2 Sn1 109.8(8) . . ? C3 C2 Sn1 107.0(9) . . ? C14 C2 Sn1 107.5(8) . . ? C2 C3 C4 116.9(11) . . ? C2 C3 H3A 108.1 . . ? C4 C3 H3A 108.1 . . ? C2 C3 H3B 108.1 . . ? C4 C3 H3B 108.1 . . ? H3A C3 H3B 107.3 . . ? N5 C4 C15 130.2(13) . . ? N5 C4 C3 113.2(12) . . ? C15 C4 C3 116.5(12) . . ? N6 C7 C8 117.2(13) . . ? N6 C7 C16 123.6(13) . . ? C8 C7 C16 119.2(13) . . ? N9 C8 C13 123.8(12) . . ? N9 C8 C7 113.4(12) . . ? C13 C8 C7 122.9(13) . . ? N9 C10 C11 123.9(15) . . ? N9 C10 H10 118.1 . . ? C11 C10 H10 118.1 . . ? C12 C11 C10 116.2(14) . . ? C12 C11 H11 121.9 . . ? C10 C11 H11 121.9 . . ? C11 C12 C13 125.1(16) . . ? C11 C12 H12 117.5 . . ? C13 C12 H12 117.5 . . ? C12 C13 C8 115.2(15) . . ? C12 C13 H13 122.4 . . ? C8 C13 H13 122.4 . . ? C2 C14 H14A 109.5 . . ? C2 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C2 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C4 C15 H15A 109.5 . . ? C4 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C4 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? N17 C16 C21 122.5(16) . . ? N17 C16 C7 113.8(14) . . ? C21 C16 C7 123.6(15) . . ? C19 C18 N17 124.2(15) . . ? C19 C18 H18 117.9 . . ? N17 C18 H18 117.9 . . ? C20 C19 C18 118.4(17) . . ? C20 C19 H19 120.8 . . ? C18 C19 H19 120.8 . . ? C19 C20 C21 119.5(17) . . ? C19 C20 H20 120.3 . . ? C21 C20 H20 120.3 . . ? C16 C21 C20 119.5(16) . . ? C16 C21 H21 120.3 . . ? C20 C21 H21 120.3 . . ? C202 C201 H20A 109.5 . . ? C202 C201 H20B 109.5 . . ? H20A C201 H20B 109.5 . . ? C202 C201 H20C 109.5 . . ? H20A C201 H20C 109.5 . . ? H20B C201 H20C 109.5 . . ? C214 C202 C203 113.6(11) . . ? C214 C202 C201 110.2(12) . . ? C203 C202 C201 111.1(12) . . ? C214 C202 Sn2 108.4(8) . . ? C203 C202 Sn2 105.1(8) . . ? C201 C202 Sn2 108.2(9) . . ? C204 C203 C202 116.6(11) . . ? C204 C203 H20D 108.1 . . ? C202 C203 H20D 108.1 . . ? C204 C203 H20E 108.1 . . ? C202 C203 H20E 108.1 . . ? H20D C203 H20E 107.3 . . ? N205 C204 C215 125.4(12) . . ? N205 C204 C203 115.9(11) . . ? C215 C204 C203 118.7(10) . . ? N206 C207 C216 121.7(12) . . ? N206 C207 C208 113.9(12) . . ? C216 C207 C208 124.4(13) . . ? N209 C208 C213 122.8(12) . . ? N209 C208 C207 117.6(11) . . ? C213 C208 C207 119.6(13) . . ? C211 C210 N209 122.0(16) . . ? C211 C210 H210 119.0 . . ? N209 C210 H210 119.0 . . ? C212 C211 C210 118.1(14) . . ? C212 C211 H211 121.0 . . ? C210 C211 H211 121.0 . . ? C211 C212 C213 123.5(16) . . ? C211 C212 H212 118.3 . . ? C213 C212 H212 118.3 . . ? C212 C213 C208 114.9(15) . . ? C212 C213 H213 122.6 . . ? C208 C213 H213 122.6 . . ? C202 C214 H21A 109.5 . . ? C202 C214 H21B 109.5 . . ? H21A C214 H21B 109.5 . . ? C202 C214 H21C 109.5 . . ? H21A C214 H21C 109.5 . . ? H21B C214 H21C 109.5 . . ? C204 C215 H21D 109.5 . . ? C204 C215 H21E 109.5 . . ? H21D C215 H21E 109.5 . . ? C204 C215 H21F 109.5 . . ? H21D C215 H21F 109.5 . . ? H21E C215 H21F 109.5 . . ? N217 C216 C221 122(2) . . ? N222 C216 C207 123.0(16) . . ? N217 C216 C207 113.3(16) . . ? C221 C216 C207 122.6(18) . . ? N222 C216 C225 120.6(18) . . ? C207 C216 C225 115.8(15) . . ? N217 C218 C219 117(3) . . ? N217 C218 H218 121.7 . . ? C219 C218 H218 121.7 . . ? C220 C219 C218 119(3) . . ? C223 C219 C224 120(3) . . ? C223 C219 H21G 119.9 . . ? C224 C219 H21G 119.9 . . ? C220 C219 H219 120.6 . . ? C218 C219 H219 120.6 . . ? C219 C220 C221 119(3) . . ? C219 C220 H220 120.4 . . ? C221 C220 H220 120.4 . . ? C220 C221 C216 117(3) . . ? C220 C221 H221 121.3 . . ? C216 C221 H221 121.3 . . ? C219 C223 N222 126(3) . . ? C219 C223 H223 117.0 . . ? N222 C223 H223 117.0 . . ? C225 C224 C219 113(2) . . ? C225 C224 H224 123.4 . . ? C219 C224 H224 123.4 . . ? C224 C225 C216 118(2) . . ? C224 C225 H225 121.2 . . ? C216 C225 H225 121.2 . . ? C302 C301 H30A 109.5 . . ? C302 C301 H30B 109.5 . . ? H30A C301 H30B 109.5 . . ? C302 C301 H30C 109.5 . . ? H30A C301 H30C 109.5 . . ? H30B C301 H30C 109.5 . . ? C301 C302 C314 109.1(14) . . ? C301 C302 C303 112.7(12) . . ? C314 C302 C303 113.1(13) . . ? C301 C302 Sn3 109.9(10) . . ? C314 C302 Sn3 106.2(10) . . ? C303 C302 Sn3 105.6(9) . . ? C304 C303 C302 115.7(11) . . ? C304 C303 H30D 108.4 . . ? C302 C303 H30D 108.4 . . ? C304 C303 H30E 108.4 . . ? C302 C303 H30E 108.4 . . ? H30D C303 H30E 107.4 . . ? N305 C304 C303 117.7(12) . . ? N305 C304 C315 124.7(14) . . ? C303 C304 C315 117.5(12) . . ? N306 C307 C308 117.2(13) . . ? N306 C307 C316 121.8(13) . . ? C308 C307 C316 121.0(13) . . ? N309 C308 C313 122.9(14) . . ? N309 C308 C307 115.2(12) . . ? C313 C308 C307 121.9(14) . . ? N309 C310 C311 123.5(15) . . ? N309 C310 H310 118.3 . . ? C311 C310 H310 118.3 . . ? C310 C311 C312 120.2(15) . . ? C310 C311 H311 119.9 . . ? C312 C311 H311 119.9 . . ? C311 C312 C313 118.1(14) . . ? C311 C312 H312 121.0 . . ? C313 C312 H312 121.0 . . ? C308 C313 C312 117.7(15) . . ? C308 C313 H313 121.1 . . ? C312 C313 H313 121.1 . . ? C302 C314 H31A 109.5 . . ? C302 C314 H31B 109.5 . . ? H31A C314 H31B 109.5 . . ? C302 C314 H31C 109.5 . . ? H31A C314 H31C 109.5 . . ? H31B C314 H31C 109.5 . . ? C304 C315 H31D 109.5 . . ? C304 C315 H31E 109.5 . . ? H31D C315 H31E 109.5 . . ? C304 C315 H31F 109.5 . . ? H31D C315 H31F 109.5 . . ? H31E C315 H31F 109.5 . . ? N321 C316 C317 123.7(15) . . ? N321 C316 C307 113.4(12) . . ? C317 C316 C307 123.0(14) . . ? C316 C317 C318 117.2(15) . . ? C316 C317 H317 121.4 . . ? C318 C317 H317 121.4 . . ? C319 C318 C317 119.2(17) . . ? C319 C318 H318 120.4 . . ? C317 C318 H318 120.4 . . ? C318 C319 C320 121.7(19) . . ? C318 C319 H319 119.1 . . ? C320 C319 H319 119.1 . . ? C319 C320 N321 122.4(18) . . ? C319 C320 H320 118.8 . . ? N321 C320 H320 118.8 . . ? C402 C401 H40A 109.5 . . ? C402 C401 H40B 109.5 . . ? H40A C401 H40B 109.5 . . ? C402 C401 H40C 109.5 . . ? H40A C401 H40C 109.5 . . ? H40B C401 H40C 109.5 . . ? C401 C402 C414 112.6(15) . . ? C401 C402 C403 109.8(12) . . ? C414 C402 C403 111.9(13) . . ? C401 C402 Sn4 108.0(10) . . ? C414 C402 Sn4 107.9(9) . . ? C403 C402 Sn4 106.4(10) . . ? C404 C403 C402 118.2(11) . . ? C404 C403 H40D 107.8 . . ? C402 C403 H40D 107.8 . . ? C404 C403 H40E 107.8 . . ? C402 C403 H40E 107.8 . . ? H40D C403 H40E 107.1 . . ? N405 C404 C415 123.7(12) . . ? N405 C404 C403 117.2(11) . . ? C415 C404 C403 119.0(10) . . ? N406 C407 C408 118.2(14) . . ? N406 C407 C416 122.1(13) . . ? C408 C407 C416 119.7(14) . . ? C413 C408 N409 121.2(14) . . ? C413 C408 C407 124.8(16) . . ? N409 C408 C407 114.0(14) . . ? N409 C410 C411 122.2(18) . . ? N409 C410 H410 118.9 . . ? C411 C410 H410 118.9 . . ? C412 C411 C410 117.3(15) . . ? C412 C411 H411 121.4 . . ? C410 C411 H411 121.4 . . ? C413 C412 C411 120.9(17) . . ? C413 C412 H412 119.5 . . ? C411 C412 H412 119.5 . . ? C408 C413 C412 118.7(19) . . ? C408 C413 H413 120.7 . . ? C412 C413 H413 120.7 . . ? C402 C414 H41A 109.5 . . ? C402 C414 H41B 109.5 . . ? H41A C414 H41B 109.5 . . ? C402 C414 H41C 109.5 . . ? H41A C414 H41C 109.5 . . ? H41B C414 H41C 109.5 . . ? C404 C415 H41D 109.5 . . ? C404 C415 H41E 109.5 . . ? H41D C415 H41E 109.5 . . ? C404 C415 H41F 109.5 . . ? H41D C415 H41F 109.5 . . ? H41E C415 H41F 109.5 . . ? N417 C416 C421 123.8(15) . . ? N417 C416 C407 115.0(13) . . ? C421 C416 C407 121.2(13) . . ? N417 C418 C419 121.6(17) . . ? N417 C418 H418 119.2 . . ? C419 C418 H418 119.2 . . ? C420 C419 C418 120.8(18) . . ? C420 C419 H419 119.6 . . ? C418 C419 H419 119.6 . . ? C419 C420 C421 118.2(17) . . ? C419 C420 H420 120.9 . . ? C421 C420 H420 120.9 . . ? C420 C421 C416 118.6(15) . . ? C420 C421 H421 120.7 . . ? C416 C421 H421 120.7 . . ? C4 N5 N6 119.4(11) . . ? C7 N6 N5 117.2(12) . . ? C7 N6 Zn1 115.7(10) . . ? N5 N6 Zn1 126.8(8) . . ? C10 N9 C8 115.7(12) . . ? C10 N9 Zn1 128.5(10) . . ? C8 N9 Zn1 115.7(9) . . ? C16 N17 C18 115.7(14) . . ? C204 N205 N206 121.0(11) . . ? C207 N206 N205 122.6(11) . . ? C207 N206 Zn2 116.1(9) . . ? N205 N206 Zn2 120.7(8) . . ? C208 N209 C210 118.8(13) . . ? C208 N209 Zn2 114.3(8) . . ? C210 N209 Zn2 126.9(11) . . ? C216 N217 C218 118(3) . . ? C216 N222 C223 122(2) . . ? C304 N305 N306 120.5(12) . . ? C307 N306 N305 118.1(12) . . ? C307 N306 Zn3 114.6(10) . . ? N305 N306 Zn3 126.6(9) . . ? C310 N309 C308 117.5(12) . . ? C310 N309 Zn3 127.5(10) . . ? C308 N309 Zn3 115.0(9) . . ? C316 N321 C320 115.8(14) . . ? C404 N405 N406 120.4(11) . . ? C407 N406 N405 122.4(13) . . ? C407 N406 Zn4 114.5(10) . . ? N405 N406 Zn4 123.0(10) . . ? C410 N409 C408 119.6(15) . . ? C410 N409 Zn4 126.1(13) . . ? C408 N409 Zn4 114.3(9) . . ? C416 N417 C418 116.9(15) . . ? Sn2 S1 Sn1 107.79(12) . . ? Zn2 S2 Zn7 106.46(13) . . ? Zn2 S2 Sn1 94.02(12) . . ? Zn7 S2 Sn1 107.38(12) . . ? Zn5 S3 Zn6 109.91(14) . . ? Zn5 S3 Sn1 116.80(14) . . ? Zn6 S3 Sn1 111.13(13) . . ? Zn1 S4 Zn5 102.24(13) . . ? Zn1 S4 Sn2 100.44(12) . . ? Zn5 S4 Sn2 106.70(12) . . ? Zn7 S5 Zn8 113.28(13) . . ? Zn7 S5 Sn2 116.95(14) . . ? Zn8 S5 Sn2 108.20(13) . . ? Zn6 S6 Zn7 105.78(13) . . ? Zn6 S6 Sn3 116.43(13) . . ? Zn7 S6 Sn3 115.08(13) . . ? Zn4 S7 Zn8 105.14(15) . . ? Zn4 S7 Sn3 97.05(12) . . ? Zn8 S7 Sn3 105.74(13) . . ? Sn4 S8 Sn3 106.78(12) . . ? Zn3 S9 Zn6 103.95(14) . . ? Zn3 S9 Sn4 100.27(12) . . ? Zn6 S9 Sn4 105.06(12) . . ? Zn5 S10 Zn8 110.10(12) . . ? Zn5 S10 Sn4 111.81(13) . . ? Zn8 S10 Sn4 116.31(14) . . ? N9 Zn1 N6 78.1(4) . . ? N9 Zn1 S4 108.9(3) . . ? N6 Zn1 S4 122.1(3) . . ? N9 Zn1 I1 103.2(3) . . ? N6 Zn1 I1 113.4(3) . . ? S4 Zn1 I1 119.82(11) . . ? N209 Zn2 N206 77.9(4) . . ? N209 Zn2 S2 101.9(3) . . ? N206 Zn2 S2 120.2(3) . . ? N209 Zn2 I2 101.4(3) . . ? N206 Zn2 I2 110.8(3) . . ? S2 Zn2 I2 127.07(11) . . ? N309 Zn3 N306 77.9(5) . . ? N309 Zn3 S9 105.5(3) . . ? N306 Zn3 S9 117.6(3) . . ? N309 Zn3 I3 106.1(3) . . ? N306 Zn3 I3 112.4(3) . . ? S9 Zn3 I3 124.93(10) . . ? N409 Zn4 N406 78.9(5) . . ? N409 Zn4 S7 102.4(4) . . ? N406 Zn4 S7 116.2(3) . . ? N409 Zn4 I4 105.6(3) . . ? N406 Zn4 I4 110.6(3) . . ? S7 Zn4 I4 128.86(12) . . ? S3 Zn5 S4 119.25(12) . . ? S3 Zn5 S10 115.71(13) . . ? S4 Zn5 S10 99.53(12) . . ? S3 Zn5 I5 102.55(9) . . ? S4 Zn5 I5 111.87(9) . . ? S10 Zn5 I5 107.85(9) . . ? S6 Zn6 S9 118.11(12) . . ? S6 Zn6 S3 120.24(12) . . ? S9 Zn6 S3 100.78(12) . . ? S6 Zn6 I6 102.93(10) . . ? S9 Zn6 I6 112.15(10) . . ? S3 Zn6 I6 101.72(10) . . ? S5 Zn7 S2 117.27(12) . . ? S5 Zn7 S6 112.65(12) . . ? S2 Zn7 S6 106.30(12) . . ? S5 Zn7 I7 109.02(9) . . ? S2 Zn7 I7 105.28(9) . . ? S6 Zn7 I7 105.45(9) . . ? S7 Zn8 S10 118.13(12) . . ? S7 Zn8 S5 101.49(13) . . ? S10 Zn8 S5 116.61(12) . . ? S7 Zn8 I8 110.58(10) . . ? S10 Zn8 I8 103.94(10) . . ? S5 Zn8 I8 105.60(9) . . ? C2 Sn1 S3 115.2(3) . . ? C2 Sn1 S2 106.6(3) . . ? S3 Sn1 S2 108.77(11) . . ? C2 Sn1 S1 112.4(4) . . ? S3 Sn1 S1 115.99(11) . . ? S2 Sn1 S1 95.55(11) . . ? C202 Sn2 S5 111.9(4) . . ? C202 Sn2 S1 114.7(4) . . ? S5 Sn2 S1 115.79(11) . . ? C202 Sn2 S4 106.6(4) . . ? S5 Sn2 S4 108.94(10) . . ? S1 Sn2 S4 97.30(11) . . ? C302 Sn3 S6 115.4(4) . . ? C302 Sn3 S8 111.9(4) . . ? S6 Sn3 S8 116.82(11) . . ? C302 Sn3 S7 104.0(4) . . ? S6 Sn3 S7 108.73(11) . . ? S8 Sn3 S7 97.43(12) . . ? C402 Sn4 S10 111.5(5) . . ? C402 Sn4 S8 114.1(5) . . ? S10 Sn4 S8 116.63(11) . . ? C402 Sn4 S9 106.3(4) . . ? S10 Sn4 S9 108.25(11) . . ? S8 Sn4 S9 98.47(12) . . ? Cl4 C5 Cl6 112.1(10) . . ? Cl4 C5 Cl5 110.2(9) . . ? Cl6 C5 Cl5 109.5(10) . . ? Cl4 C5 H5 108.3 . . ? Cl6 C5 H5 108.3 . . ? Cl5 C5 H5 108.3 . . ? H40H O401 H40I 108.0 . . ? O201 C200 H20F 109.5 . . ? O201 C200 H20G 109.5 . . ? H20F C200 H20G 109.5 . . ? O201 C200 H20H 109.5 . . ? H20F C200 H20H 109.5 . . ? H20G C200 H20H 109.5 . . ? C200 O201 H201 109.5 . . ? O101 C100 H10A 109.5 . . ? O101 C100 H10B 109.5 . . ? H10A C100 H10B 109.5 . . ? O101 C100 H10C 109.5 . . ? H10A C100 H10C 109.5 . . ? H10B C100 H10C 109.5 . . ? C100 O101 H101 109.5 . . ? Cl3 C300 Cl1 107.9(15) . . ? Cl3 C300 Cl2 116.0(18) . . ? Cl1 C300 Cl2 115(2) . . ? Cl3 C300 H300 105.8 . . ? Cl1 C300 H300 105.8 . . ? Cl2 C300 H300 105.8 . . ? H40F O400 H40G 109.6 . . ? 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 C1 C2 C3 C4 167.3(12) . . . . ? C14 C2 C3 C4 -70.3(15) . . . . ? Sn1 C2 C3 C4 47.2(13) . . . . ? C2 C3 C4 N5 4.2(17) . . . . ? C2 C3 C4 C15 -173.2(13) . . . . ? N6 C7 C8 N9 -0.4(17) . . . . ? C16 C7 C8 N9 177.2(11) . . . . ? N6 C7 C8 C13 -179.3(13) . . . . ? C16 C7 C8 C13 -1.7(19) . . . . ? N9 C10 C11 C12 -2(2) . . . . ? C10 C11 C12 C13 4(3) . . . . ? C11 C12 C13 C8 -4(2) . . . . ? N9 C8 C13 C12 2(2) . . . . ? C7 C8 C13 C12 -179.4(13) . . . . ? N6 C7 C16 N17 64(2) . . . . ? C8 C7 C16 N17 -113.3(16) . . . . ? N6 C7 C16 C21 -113(2) . . . . ? C8 C7 C16 C21 69(2) . . . . ? N17 C18 C19 C20 -2(3) . . . . ? C18 C19 C20 C21 -1(4) . . . . ? N17 C16 C21 C20 3(3) . . . . ? C7 C16 C21 C20 180.0(19) . . . . ? C19 C20 C21 C16 1(4) . . . . ? C214 C202 C203 C204 -64.4(15) . . . . ? C201 C202 C203 C204 170.6(12) . . . . ? Sn2 C202 C203 C204 53.8(14) . . . . ? C202 C203 C204 N205 -10.0(18) . . . . ? C202 C203 C204 C215 172.1(12) . . . . ? N206 C207 C208 N209 5.1(15) . . . . ? C216 C207 C208 N209 -173.0(11) . . . . ? N206 C207 C208 C213 -175.5(12) . . . . ? C216 C207 C208 C213 6.4(18) . . . . ? N209 C210 C211 C212 -2(2) . . . . ? C210 C211 C212 C213 1(3) . . . . ? C211 C212 C213 C208 0(2) . . . . ? N209 C208 C213 C212 0(2) . . . . ? C207 C208 C213 C212 -179.3(13) . . . . ? N206 C207 C216 N222 56(2) . . . . ? C208 C207 C216 N222 -126(2) . . . . ? N206 C207 C216 N217 101(2) . . . . ? C208 C207 C216 N217 -81(2) . . . . ? N206 C207 C216 C221 -62(2) . . . . ? C208 C207 C216 C221 116(2) . . . . ? N206 C207 C216 C225 -132.8(15) . . . . ? C208 C207 C216 C225 45.1(19) . . . . ? N217 C218 C219 C223 68(4) . . . . ? N217 C218 C219 C220 23(5) . . . . ? N217 C218 C219 C224 -50(4) . . . . ? C223 C219 C220 C221 -62(4) . . . . ? C218 C219 C220 C221 -32(5) . . . . ? C224 C219 C220 C221 63(3) . . . . ? C219 C220 C221 C216 15(5) . . . . ? N222 C216 C221 C220 40(3) . . . . ? N217 C216 C221 C220 11(4) . . . . ? C207 C216 C221 C220 172(2) . . . . ? C225 C216 C221 C220 -84(3) . . . . ? C220 C219 C223 N222 63(4) . . . . ? C218 C219 C223 N222 -78(4) . . . . ? C224 C219 C223 N222 2(5) . . . . ? C223 C219 C224 C225 4(4) . . . . ? C220 C219 C224 C225 -66(3) . . . . ? C218 C219 C224 C225 49(3) . . . . ? C219 C224 C225 C216 -2(3) . . . . ? N222 C216 C225 C224 -4(3) . . . . ? N217 C216 C225 C224 -47(3) . . . . ? C221 C216 C225 C224 70(3) . . . . ? C207 C216 C225 C224 -175.3(19) . . . . ? C301 C302 C303 C304 -166.5(14) . . . . ? C314 C302 C303 C304 69.1(16) . . . . ? Sn3 C302 C303 C304 -46.6(15) . . . . ? C302 C303 C304 N305 5(2) . . . . ? C302 C303 C304 C315 -171.1(15) . . . . ? N306 C307 C308 N309 -1.8(18) . . . . ? C316 C307 C308 N309 177.8(12) . . . . ? N306 C307 C308 C313 178.3(13) . . . . ? C316 C307 C308 C313 -2(2) . . . . ? N309 C310 C311 C312 -3(2) . . . . ? C310 C311 C312 C313 2(2) . . . . ? N309 C308 C313 C312 1(2) . . . . ? C307 C308 C313 C312 -179.1(13) . . . . ? C311 C312 C313 C308 -1(2) . . . . ? N306 C307 C316 N321 -87.5(18) . . . . ? C308 C307 C316 N321 92.9(18) . . . . ? N306 C307 C316 C317 92(2) . . . . ? C308 C307 C316 C317 -87.7(19) . . . . ? N321 C316 C317 C318 2(3) . . . . ? C307 C316 C317 C318 -177.4(17) . . . . ? C316 C317 C318 C319 -2(3) . . . . ? C317 C318 C319 C320 2(4) . . . . ? C318 C319 C320 N321 -1(4) . . . . ? C401 C402 C403 C404 -167.6(12) . . . . ? C414 C402 C403 C404 66.6(16) . . . . ? Sn4 C402 C403 C404 -51.0(15) . . . . ? C402 C403 C404 N405 13.8(18) . . . . ? C402 C403 C404 C415 -170.1(14) . . . . ? N406 C407 C408 C413 -179.3(14) . . . . ? C416 C407 C408 C413 2(2) . . . . ? N406 C407 C408 N409 1.1(19) . . . . ? C416 C407 C408 N409 -177.4(12) . . . . ? N409 C410 C411 C412 0(2) . . . . ? C410 C411 C412 C413 -3(2) . . . . ? N409 C408 C413 C412 -2(2) . . . . ? C407 C408 C413 C412 178.5(13) . . . . ? C411 C412 C413 C408 4(2) . . . . ? N406 C407 C416 N417 -126.5(14) . . . . ? C408 C407 C416 N417 52.0(17) . . . . ? N406 C407 C416 C421 52.9(19) . . . . ? C408 C407 C416 C421 -128.7(14) . . . . ? N417 C418 C419 C420 1(2) . . . . ? C418 C419 C420 C421 2(2) . . . . ? C419 C420 C421 C416 -4(2) . . . . ? N417 C416 C421 C420 5(2) . . . . ? C407 C416 C421 C420 -174.6(13) . . . . ? C15 C4 N5 N6 -1(2) . . . . ? C3 C4 N5 N6 -177.8(11) . . . . ? C8 C7 N6 N5 -172.8(11) . . . . ? C16 C7 N6 N5 10(2) . . . . ? C8 C7 N6 Zn1 0.7(16) . . . . ? C16 C7 N6 Zn1 -176.8(10) . . . . ? C4 N5 N6 C7 -98.8(15) . . . . ? C4 N5 N6 Zn1 88.6(14) . . . . ? C11 C10 N9 C8 0(2) . . . . ? C11 C10 N9 Zn1 -178.6(10) . . . . ? C13 C8 N9 C10 0.3(19) . . . . ? C7 C8 N9 C10 -178.6(12) . . . . ? C13 C8 N9 Zn1 178.8(10) . . . . ? C7 C8 N9 Zn1 -0.1(13) . . . . ? C21 C16 N17 C18 -5(3) . . . . ? C7 C16 N17 C18 177.2(15) . . . . ? C19 C18 N17 C16 5(3) . . . . ? C215 C204 N205 N206 4(2) . . . . ? C203 C204 N205 N206 -173.8(11) . . . . ? C216 C207 N206 N205 1.2(18) . . . . ? C208 C207 N206 N205 -177.0(10) . . . . ? C216 C207 N206 Zn2 172.8(9) . . . . ? C208 C207 N206 Zn2 -5.4(13) . . . . ? C204 N205 N206 C207 -91.7(16) . . . . ? C204 N205 N206 Zn2 97.1(12) . . . . ? C213 C208 N209 C210 -0.8(19) . . . . ? C207 C208 N209 C210 178.6(11) . . . . ? C213 C208 N209 Zn2 178.4(10) . . . . ? C207 C208 N209 Zn2 -2.3(13) . . . . ? C211 C210 N209 C208 2(2) . . . . ? C211 C210 N209 Zn2 -177.3(12) . . . . ? N222 C216 N217 C218 -68(3) . . . . ? C221 C216 N217 C218 -20(4) . . . . ? C207 C216 N217 C218 178(3) . . . . ? C225 C216 N217 C218 48(3) . . . . ? C219 C218 N217 C216 3(5) . . . . ? N217 C216 N222 C223 93(4) . . . . ? C221 C216 N222 C223 -47(3) . . . . ? C207 C216 N222 C223 -179(2) . . . . ? C225 C216 N222 C223 10(4) . . . . ? C219 C223 N222 C216 -9(5) . . . . ? C303 C304 N305 N306 175.9(12) . . . . ? C315 C304 N305 N306 -8(2) . . . . ? C308 C307 N306 N305 174.9(11) . . . . ? C316 C307 N306 N305 -4.7(19) . . . . ? C308 C307 N306 Zn3 3.6(16) . . . . ? C316 C307 N306 Zn3 -176.0(10) . . . . ? C304 N305 N306 C307 98.4(16) . . . . ? C304 N305 N306 Zn3 -91.5(16) . . . . ? C311 C310 N309 C308 2(2) . . . . ? C311 C310 N309 Zn3 -178.0(11) . . . . ? C313 C308 N309 C310 -1(2) . . . . ? C307 C308 N309 C310 178.7(12) . . . . ? C313 C308 N309 Zn3 178.9(11) . . . . ? C307 C308 N309 Zn3 -1.1(15) . . . . ? C317 C316 N321 C320 -2(3) . . . . ? C307 C316 N321 C320 177.8(19) . . . . ? C319 C320 N321 C316 1(4) . . . . ? C415 C404 N405 N406 -7(2) . . . . ? C403 C404 N405 N406 169.0(12) . . . . ? C408 C407 N406 N405 175.9(11) . . . . ? C416 C407 N406 N405 -6(2) . . . . ? C408 C407 N406 Zn4 0.7(16) . . . . ? C416 C407 N406 Zn4 179.2(10) . . . . ? C404 N405 N406 C407 86.7(16) . . . . ? C404 N405 N406 Zn4 -98.5(13) . . . . ? C411 C410 N409 C408 2(2) . . . . ? C411 C410 N409 Zn4 -176.7(11) . . . . ? C413 C408 N409 C410 -1(2) . . . . ? C407 C408 N409 C410 178.5(12) . . . . ? C413 C408 N409 Zn4 178.0(11) . . . . ? C407 C408 N409 Zn4 -2.4(15) . . . . ? C421 C416 N417 C418 -1.8(19) . . . . ? C407 C416 N417 C418 177.5(12) . . . . ? C419 C418 N417 C416 -1(2) . . . . ? _refine_diff_density_max 0.854 _refine_diff_density_min -0.896 _refine_diff_density_rms 0.152 _database_code_depnum_ccdc_archive 'CCDC 934170'