# Electronic Supplementary Material (ESI) for Dalton Transactions # 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_1 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C88 H90 N12 O20 P4 Sn6, 2(C4 H8 O)' _chemical_formula_sum 'C96 H106 N12 O22 P4 Sn6' _chemical_formula_weight 2616.07 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' P P 0.1023 0.0942 '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 ? _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 15.686(5) _cell_length_b 16.555(5) _cell_length_c 25.329(5) _cell_angle_alpha 94.871(5) _cell_angle_beta 104.680(5) _cell_angle_gamma 109.436(5) _cell_volume 5896(3) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 2.20 _cell_measurement_theta_max 22.86 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.474 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2604.0 _exptl_absorpt_coefficient_mu 1.371 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.43234 _exptl_absorpt_correction_T_max 1 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 32223 _diffrn_reflns_av_R_equivalents 0.0444 _diffrn_reflns_av_sigmaI/netI 0.1046 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.86 _diffrn_reflns_theta_max 25.50 _reflns_number_total 21537 _reflns_number_gt 13526 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type fullcycle _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1008P)^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 21537 _refine_ls_number_parameters 1255 _refine_ls_number_restraints 14 _refine_ls_R_factor_all 0.0988 _refine_ls_R_factor_gt 0.0658 _refine_ls_wR_factor_ref 0.1914 _refine_ls_wR_factor_gt 0.1658 _refine_ls_goodness_of_fit_ref 0.956 _refine_ls_restrained_S_all 0.957 _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 Sn1 Sn 0.59489(4) 0.67705(4) 0.52445(2) 0.026 Uani 1 1 d . . . Sn2 Sn 0.64576(4) 0.58140(4) 0.63026(2) 0.027 Uani 1 1 d . . . Sn3 Sn 0.67441(4) 0.48533(4) 0.52077(2) 0.027 Uani 1 1 d . . . Sn4 Sn 0.33768(4) 0.87292(4) 0.92831(2) 0.037 Uani 1 1 d . . . Sn5 Sn 0.44601(4) 0.79952(4) 1.03197(2) 0.037 Uani 1 1 d . . . Sn6 Sn 0.59706(4) 0.90297(4) 0.96937(3) 0.038 Uani 1 1 d . . . P1 P 0.80573(14) 0.68372(14) 0.57692(9) 0.028 Uani 1 1 d . . . P2 P 0.58651(14) 0.55646(14) 0.40783(9) 0.027 Uani 1 1 d . . . P3 P 0.49994(18) 1.00766(17) 0.87980(10) 0.044 Uani 1 1 d . . . P4 P 0.42245(17) 0.72613(16) 0.90592(10) 0.041 Uani 1 1 d . . . O1 O 0.6325(4) 0.5017(4) 0.4409(2) 0.030 Uani 1 1 d . . . O2 O 0.4862(4) 0.5024(4) 0.3707(2) 0.032 Uani 1 1 d . . . O3 O 0.5901(4) 0.6363(4) 0.4436(2) 0.033 Uani 1 1 d . . . O4 O 0.7947(4) 0.6002(4) 0.5409(2) 0.033 Uani 1 1 d . . . O5 O 0.7438(4) 0.7291(4) 0.5453(2) 0.033 Uani 1 1 d . . . O6 O 0.7832(3) 0.6671(3) 0.6325(2) 0.027 Uani 1 1 d . . . O7 O 0.6049(4) 0.5607(3) 0.5428(2) 0.028 Uani 1 1 d . . . O8 O 0.6871(4) 0.4794(4) 0.6065(2) 0.035 Uani 1 1 d . . . O9 O 0.5975(4) 0.6815(4) 0.6102(2) 0.030 Uani 1 1 d . . . O10 O 0.4481(4) 0.6254(4) 0.4988(2) 0.033 Uani 1 1 d . . . O11 O 0.5791(4) 0.9791(4) 0.9118(2) 0.043 Uani 1 1 d . . . O12 O 0.5211(5) 1.1044(4) 0.9006(2) 0.050 Uani 1 1 d . . . O13 O 0.4017(4) 0.9506(4) 0.8799(2) 0.046 Uani 1 1 d . . . O14 O 0.3473(4) 0.7655(4) 0.8838(2) 0.045 Uani 1 1 d . . . O15 O 0.5237(4) 0.7882(4) 0.9097(2) 0.041 Uani 1 1 d . . . O16 O 0.4194(4) 0.7027(4) 0.9627(2) 0.038 Uani 1 1 d . . . O17 O 0.4697(4) 0.8919(4) 0.9815(2) 0.035 Uani 1 1 d . . . O18 O 0.3125(4) 0.8053(4) 0.9940(2) 0.040 Uani 1 1 d . . . O19 O 0.5901(4) 0.8328(4) 1.0357(2) 0.041 Uani 1 1 d . . . O20 O 0.6685(4) 1.0162(4) 1.0298(2) 0.040 Uani 1 1 d . . . O21 O 0.7215(11) 0.7040(9) 0.0063(6) 0.186 Uani 1 1 d . . . O22 O 0.7762(13) 0.6890(12) 0.2213(9) 0.220 Uani 1 1 d . . . N1 N 0.1282(5) 0.8287(5) 0.9428(3) 0.046 Uani 1 1 d . . . N2 N 0.0514(6) 0.7950(6) 0.9543(4) 0.058 Uani 1 1 d . . . N3 N 0.2112(7) 0.5539(6) 1.0165(4) 0.079 Uani 1 1 d . . . N4 N 0.2768(5) 0.6260(5) 1.0292(3) 0.047 Uani 1 1 d . . . N5 N 0.8081(6) 0.9397(6) 1.0544(4) 0.068 Uani 1 1 d . . . N6 N 0.8789(6) 0.9391(6) 1.0911(5) 0.077 Uani 1 1 d . . . N7 N 0.4927(5) 0.8102(5) 0.5623(3) 0.033 Uani 1 1 d . . . N8 N 0.4519(5) 0.8541(5) 0.5782(3) 0.040 Uani 1 1 d . . . N9 N 0.6882(5) 0.2997(5) 0.5478(3) 0.035 Uani 1 1 d . . . N10 N 0.6979(6) 0.2392(5) 0.5715(3) 0.044 Uani 1 1 d . . . N11 N 0.9118(6) 0.5744(6) 0.7413(5) 0.077 Uani 1 1 d . . . N12 N 0.8263(7) 0.5616(7) 0.7164(5) 0.079 Uani 1 1 d . . . C1 C 0.1990(7) 0.8388(6) 0.8701(4) 0.047 Uani 1 1 d . . . C2 C 0.1915(7) 0.8325(6) 0.8142(5) 0.058 Uani 1 1 d . . . H2 H 0.2460 0.8428 0.8034 0.070 Uiso 1 1 calc R . . C3 C 0.1049(8) 0.8113(7) 0.7735(5) 0.074 Uani 1 1 d . . . H3 H 0.1019 0.8080 0.7362 0.089 Uiso 1 1 calc R . . C4 C 0.0239(7) 0.7952(6) 0.7892(4) 0.048 Uani 1 1 d . . . H4 H -0.0339 0.7818 0.7622 0.058 Uiso 1 1 calc R . . C5 C 0.0270(7) 0.7985(7) 0.8460(5) 0.058 Uani 1 1 d . . . H5 H -0.0279 0.7861 0.8567 0.070 Uiso 1 1 calc R . . C6 C 0.1181(7) 0.8216(6) 0.8862(4) 0.048 Uani 1 1 d . . . C7 C 0.0645(7) 0.8072(9) 1.0138(5) 0.071 Uani 1 1 d . . . C8 C -0.0135(9) 0.7645(13) 1.0286(6) 0.134 Uani 1 1 d . . . H8 H -0.0694 0.7296 1.0015 0.161 Uiso 1 1 calc R . . C9 C -0.0100(12) 0.7728(16) 1.0835(8) 0.160 Uani 1 1 d . . . H9 H -0.0633 0.7410 1.0930 0.192 Uiso 1 1 calc R . . C10 C 0.0641(10) 0.8227(11) 1.1222(7) 0.104 Uani 1 1 d . . . H10 H 0.0665 0.8251 1.1594 0.125 Uiso 1 1 calc R . . C11 C 0.1399(10) 0.8726(10) 1.1068(5) 0.093 Uani 1 1 d . . . H11 H 0.1925 0.9124 1.1341 0.112 Uiso 1 1 calc R . . C12 C 0.1410(9) 0.8661(8) 1.0539(5) 0.077 Uani 1 1 d . . . H12 H 0.1931 0.9012 1.0447 0.093 Uiso 1 1 calc R . . C13 C 0.4331(6) 0.7080(6) 1.0873(4) 0.041 Uani 1 1 d . . . C14 C 0.5117(7) 0.7221(8) 1.1333(4) 0.058 Uani 1 1 d . . . H14 H 0.5672 0.7699 1.1390 0.069 Uiso 1 1 calc R . . C15 C 0.5068(8) 0.6646(8) 1.1705(5) 0.062 Uani 1 1 d . . . H15 H 0.5574 0.6758 1.2023 0.075 Uiso 1 1 calc R . . C16 C 0.4285(8) 0.5930(7) 1.1601(5) 0.064 Uani 1 1 d . . . H16 H 0.4265 0.5530 1.1839 0.077 Uiso 1 1 calc R . . C17 C 0.3504(8) 0.5777(7) 1.1146(4) 0.059 Uani 1 1 d . . . H17 H 0.2955 0.5291 1.1088 0.070 Uiso 1 1 calc R . . C18 C 0.3548(7) 0.6353(6) 1.0777(4) 0.048 Uani 1 1 d . . . C19 C 0.1377(10) 0.5464(10) 0.9692(6) 0.100 Uani 1 1 d . . . C20 C 0.1369(10) 0.6001(10) 0.9351(6) 0.100 Uani 1 1 d . . . H20 H 0.1896 0.6515 0.9432 0.120 Uiso 1 1 calc R . . C21 C 0.0630(10) 0.5869(9) 0.8870(7) 0.109 Uani 1 1 d . . . H21 H 0.0672 0.6277 0.8637 0.130 Uiso 1 1 calc R . . C22 C -0.0145(15) 0.5134(14) 0.8751(9) 0.151 Uani 1 1 d U . . H22 H -0.0653 0.5045 0.8439 0.181 Uiso 1 1 calc R . . C23 C -0.0202(15) 0.4508(14) 0.9083(8) 0.151 Uani 1 1 d U . . H23 H -0.0737 0.4001 0.9001 0.181 Uiso 1 1 calc R . . C24 C 0.0630(9) 0.4682(10) 0.9576(6) 0.100 Uani 1 1 d . . . H24 H 0.0644 0.4268 0.9801 0.120 Uiso 1 1 calc R . . C25 C 0.7251(7) 0.9021(7) 0.9558(4) 0.051 Uani 1 1 d . . . C26 C 0.7260(9) 0.8822(8) 0.9010(5) 0.072 Uani 1 1 d . . . H26 H 0.6708 0.8689 0.8719 0.086 Uiso 1 1 calc R . . C27 C 0.8079(10) 0.8821(9) 0.8896(7) 0.094 Uani 1 1 d . . . H27 H 0.8069 0.8690 0.8530 0.113 Uiso 1 1 calc R . . C28 C 0.8914(10) 0.9015(10) 0.9322(8) 0.112 Uani 1 1 d . . . H28 H 0.9460 0.9009 0.9244 0.135 Uiso 1 1 calc R . . C29 C 0.8921(8) 0.9215(8) 0.9860(6) 0.078 Uani 1 1 d . . . H29 H 0.9471 0.9347 1.0153 0.093 Uiso 1 1 calc R . . C30 C 0.8109(8) 0.9215(7) 0.9956(5) 0.064 Uani 1 1 d . . . C31 C 0.8736(10) 0.9482(7) 1.1450(6) 0.091 Uani 1 1 d . . . C32 C 0.7914(9) 0.9364(8) 1.1589(5) 0.077 Uani 1 1 d . . . H32 H 0.7342 0.9247 1.1318 0.092 Uiso 1 1 calc R . . C33 C 0.7967(13) 0.9426(10) 1.2148(6) 0.117 Uani 1 1 d . . . H33 H 0.7400 0.9341 1.2227 0.141 Uiso 1 1 calc R . . C34 C 0.8726(12) 0.9591(10) 1.2587(7) 0.144 Uani 1 1 d D . . H34 H 0.8709 0.9593 1.2951 0.173 Uiso 1 1 calc R . . C35 C 0.9563(11) 0.9762(9) 1.2423(5) 0.111 Uani 1 1 d D . . H35 H 1.0131 0.9939 1.2708 0.133 Uiso 1 1 calc R . . C36 C 0.9633(10) 0.9691(9) 1.1848(6) 0.121 Uani 1 1 d D . . H36 H 1.0193 0.9774 1.1761 0.145 Uiso 1 1 calc R . . C37 C 0.3941(7) 0.6301(6) 0.8558(4) 0.049 Uani 1 1 d . . . C38 C 0.2918(8) 0.5670(7) 0.8501(4) 0.064 Uani 1 1 d . . . H38A H 0.2489 0.5974 0.8423 0.095 Uiso 1 1 calc R . . H38B H 0.2907 0.5459 0.8842 0.095 Uiso 1 1 calc R . . H38C H 0.2727 0.5186 0.8204 0.095 Uiso 1 1 calc R . . C39 C 0.3966(8) 0.6557(6) 0.8003(4) 0.053 Uani 1 1 d . . . H39A H 0.4539 0.7046 0.8051 0.080 Uiso 1 1 calc R . . H39B H 0.3429 0.6712 0.7851 0.080 Uiso 1 1 calc R . . H39C H 0.3947 0.6075 0.7755 0.080 Uiso 1 1 calc R . . C40 C 0.4672(7) 0.5848(7) 0.8758(4) 0.057 Uani 1 1 d . . . H40A H 0.4461 0.5288 0.8525 0.086 Uiso 1 1 calc R . . H40B H 0.4719 0.5775 0.9135 0.086 Uiso 1 1 calc R . . H40C H 0.5282 0.6205 0.8737 0.086 Uiso 1 1 calc R . . C41 C 0.4966(8) 0.9969(6) 0.8089(4) 0.052 Uani 1 1 d . . . C42 C 0.4185(8) 1.0211(7) 0.7753(4) 0.062 Uani 1 1 d . . . H42A H 0.4092 1.0038 0.7365 0.094 Uiso 1 1 calc R . . H42B H 0.4352 1.0831 0.7839 0.094 Uiso 1 1 calc R . . H42C H 0.3611 0.9921 0.7840 0.094 Uiso 1 1 calc R . . C43 C 0.4795(8) 0.9022(7) 0.7864(4) 0.065 Uani 1 1 d . . . H43A H 0.4217 0.8643 0.7912 0.098 Uiso 1 1 calc R . . H43B H 0.5313 0.8873 0.8062 0.098 Uiso 1 1 calc R . . H43C H 0.4747 0.8955 0.7476 0.098 Uiso 1 1 calc R . . C44 C 0.5938(9) 1.0533(8) 0.8061(5) 0.082 Uani 1 1 d . . . H44A H 0.6001 1.0368 0.7704 0.123 Uiso 1 1 calc R . . H44B H 0.6421 1.0452 0.8346 0.123 Uiso 1 1 calc R . . H44C H 0.6005 1.1135 0.8115 0.123 Uiso 1 1 calc R . . C45 C 0.6030(6) 0.8063(6) 0.5141(4) 0.036 Uani 1 1 d . . . C46 C 0.6657(7) 0.8453(6) 0.4826(4) 0.049 Uani 1 1 d . . . H46 H 0.6985 0.8147 0.4693 0.059 Uiso 1 1 calc R . . C47 C 0.6771(8) 0.9284(6) 0.4720(5) 0.059 Uani 1 1 d . . . H47 H 0.7151 0.9534 0.4505 0.071 Uiso 1 1 calc R . . C48 C 0.6277(7) 0.9754(7) 0.4956(5) 0.061 Uani 1 1 d . . . H48 H 0.6394 1.0337 0.4933 0.073 Uiso 1 1 calc R . . C49 C 0.5672(7) 0.9343(6) 0.5200(4) 0.045 Uani 1 1 d . . . H49 H 0.5310 0.9626 0.5316 0.053 Uiso 1 1 calc R . . C50 C 0.5536(6) 0.8499(5) 0.5297(3) 0.030 Uani 1 1 d . . . C51 C 0.3884(6) 0.8164(6) 0.6107(4) 0.038 Uani 1 1 d . . . C52 C 0.3393(6) 0.8644(6) 0.6246(4) 0.041 Uani 1 1 d . . . H52 H 0.3480 0.9185 0.6143 0.049 Uiso 1 1 calc R . . C53 C 0.2766(6) 0.8323(6) 0.6540(4) 0.047 Uani 1 1 d . . . H53 H 0.2414 0.8637 0.6631 0.056 Uiso 1 1 calc R . . C54 C 0.2672(7) 0.7553(7) 0.6692(4) 0.049 Uani 1 1 d . . . H54 H 0.2256 0.7339 0.6895 0.058 Uiso 1 1 calc R . . C55 C 0.3170(7) 0.7070(6) 0.6557(4) 0.042 Uani 1 1 d . . . H55 H 0.3087 0.6534 0.6668 0.050 Uiso 1 1 calc R . . C56 C 0.3776(6) 0.7364(6) 0.6266(4) 0.047 Uani 1 1 d . . . H56 H 0.4117 0.7039 0.6172 0.056 Uiso 1 1 calc R . . C57 C 0.6923(5) 0.6017(5) 0.7186(3) 0.032 Uani 1 1 d . . . C58 C 0.6431(8) 0.6335(7) 0.7493(4) 0.060 Uani 1 1 d . . . H58 H 0.5864 0.6392 0.7314 0.072 Uiso 1 1 calc R . . C59 C 0.6802(10) 0.6559(8) 0.8061(5) 0.085 Uani 1 1 d . . . H59 H 0.6501 0.6808 0.8262 0.102 Uiso 1 1 calc R . . C60 C 0.7581(7) 0.6431(8) 0.8335(4) 0.065 Uani 1 1 d . . . H60 H 0.7791 0.6564 0.8721 0.077 Uiso 1 1 calc R . . C61 C 0.8048(10) 0.6126(8) 0.8072(5) 0.078 Uani 1 1 d . . . H61 H 0.8574 0.6021 0.8271 0.094 Uiso 1 1 calc R . . C62 C 0.7763(8) 0.5948(8) 0.7479(5) 0.062 Uani 1 1 d . . . C63 C 0.9594(8) 0.5454(8) 0.7139(5) 0.071 Uani 1 1 d . . . C64 C 1.0532(8) 0.5734(8) 0.7334(6) 0.082 Uani 1 1 d . . . H64 H 1.0828 0.6125 0.7670 0.098 Uiso 1 1 calc R . . C65 C 1.1105(9) 0.5478(9) 0.7064(6) 0.082 Uani 1 1 d . . . H65 H 1.1760 0.5710 0.7221 0.098 Uiso 1 1 calc R . . C66 C 1.0706(9) 0.4878(10) 0.6563(6) 0.091 Uani 1 1 d . . . H66 H 1.1082 0.4715 0.6379 0.109 Uiso 1 1 calc R . . C67 C 0.9699(10) 0.4529(12) 0.6349(6) 0.119 Uani 1 1 d . . . H67 H 0.9406 0.4119 0.6021 0.143 Uiso 1 1 calc R . . C68 C 0.9150(9) 0.4797(11) 0.6628(5) 0.105 Uani 1 1 d . . . H68 H 0.8493 0.4555 0.6487 0.125 Uiso 1 1 calc R . . C69 C 0.7623(5) 0.4150(5) 0.5051(3) 0.025 Uani 1 1 d . . . C70 C 0.8280(6) 0.4507(6) 0.4798(3) 0.035 Uani 1 1 d . . . H70 H 0.8349 0.5054 0.4708 0.043 Uiso 1 1 calc R . . C71 C 0.8853(6) 0.4099(6) 0.4665(4) 0.045 Uani 1 1 d . . . H71 H 0.9301 0.4368 0.4492 0.054 Uiso 1 1 calc R . . C72 C 0.8756(6) 0.3289(6) 0.4792(4) 0.048 Uani 1 1 d . . . H72 H 0.9123 0.2996 0.4695 0.058 Uiso 1 1 calc R . . C73 C 0.8101(7) 0.2914(7) 0.5067(4) 0.050 Uani 1 1 d . . . H73 H 0.8044 0.2374 0.5164 0.060 Uiso 1 1 calc R . . C74 C 0.7542(6) 0.3334(6) 0.5194(4) 0.036 Uani 1 1 d . . . C75 C 0.6328(7) 0.2064(7) 0.6034(4) 0.058 Uani 1 1 d . . . C76 C 0.5821(9) 0.2501(9) 0.6203(6) 0.083 Uani 1 1 d . . . H76 H 0.5881 0.3052 0.6124 0.100 Uiso 1 1 calc R . . C77 C 0.5219(11) 0.2111(14) 0.6493(7) 0.149 Uani 1 1 d . . . H77 H 0.4870 0.2400 0.6618 0.179 Uiso 1 1 calc R . . C78 C 0.5616(9) 0.0883(9) 0.6463(5) 0.080 Uani 1 1 d . . . H78 H 0.5553 0.0344 0.6565 0.096 Uiso 1 1 calc R . . C79 C 0.6274(9) 0.1256(7) 0.6144(5) 0.082 Uani 1 1 d . . . H79 H 0.6625 0.0963 0.6026 0.098 Uiso 1 1 calc R . . C80 C 0.6559(6) 0.5951(6) 0.3611(3) 0.036 Uani 1 1 d . . . C81 C 0.6138(7) 0.6465(7) 0.3245(4) 0.059 Uani 1 1 d . . . H81A H 0.6566 0.6748 0.3048 0.088 Uiso 1 1 calc R . . H81B H 0.6027 0.6897 0.3467 0.088 Uiso 1 1 calc R . . H81C H 0.5549 0.6083 0.2984 0.088 Uiso 1 1 calc R . . C82 C 0.6588(8) 0.5175(7) 0.3245(4) 0.062 Uani 1 1 d . . . H82A H 0.5970 0.4860 0.2988 0.092 Uiso 1 1 calc R . . H82B H 0.6777 0.4796 0.3476 0.092 Uiso 1 1 calc R . . H82C H 0.7034 0.5386 0.3043 0.092 Uiso 1 1 calc R . . C83 C 0.7564(7) 0.6533(7) 0.3962(4) 0.053 Uani 1 1 d . . . H83A H 0.7950 0.6719 0.3723 0.079 Uiso 1 1 calc R . . H83B H 0.7828 0.6211 0.4210 0.079 Uiso 1 1 calc R . . H83C H 0.7546 0.7033 0.4173 0.079 Uiso 1 1 calc R . . C84 C 0.9278(6) 0.7546(5) 0.5924(4) 0.033 Uani 1 1 d . . . C85 C 0.9465(7) 0.8390(6) 0.6337(4) 0.055 Uani 1 1 d . . . H85A H 0.9478 0.8254 0.6699 0.082 Uiso 1 1 calc R . . H85B H 0.8970 0.8610 0.6209 0.082 Uiso 1 1 calc R . . H85C H 1.0064 0.8824 0.6356 0.082 Uiso 1 1 calc R . . C86 C 0.9468(6) 0.7785(6) 0.5379(3) 0.034 Uani 1 1 d . . . H86A H 0.9043 0.8055 0.5206 0.052 Uiso 1 1 calc R . . H86B H 0.9370 0.7266 0.5133 0.052 Uiso 1 1 calc R . . H86C H 1.0110 0.8181 0.5459 0.052 Uiso 1 1 calc R . . C87 C 0.9915(6) 0.7072(6) 0.6200(4) 0.038 Uani 1 1 d . . . H87A H 1.0562 0.7469 0.6327 0.057 Uiso 1 1 calc R . . H87B H 0.9853 0.6589 0.5936 0.057 Uiso 1 1 calc R . . H87C H 0.9726 0.6862 0.6510 0.057 Uiso 1 1 calc R . . C88 C 0.6621(5) 0.7058(5) 0.0425(4) 0.031 Uani 1 1 d . . . H88A H 0.7022 0.7330 0.0801 0.038 Uiso 1 1 calc R . . H88B H 0.6243 0.7403 0.0298 0.038 Uiso 1 1 calc R . . C89 C 0.6027(9) 0.6215(8) 0.0421(5) 0.076 Uani 1 1 d . . . H89A H 0.5372 0.6120 0.0229 0.091 Uiso 1 1 calc R . . H89B H 0.6075 0.6109 0.0796 0.091 Uiso 1 1 calc R . . C90 C 0.6398(9) 0.5603(8) 0.0097(6) 0.082 Uani 1 1 d . . . H90A H 0.6496 0.5157 0.0303 0.099 Uiso 1 1 calc R . . H90B H 0.5953 0.5324 -0.0268 0.099 Uiso 1 1 calc R . . C91 C 0.7243(15) 0.6168(10) 0.0057(9) 0.159 Uani 1 1 d . . . H91A H 0.7347 0.5971 -0.0284 0.191 Uiso 1 1 calc R . . H91B H 0.7763 0.6180 0.0367 0.191 Uiso 1 1 calc R . . C92 C 0.8293(14) 0.7147(12) 0.1791(6) 0.122 Uani 1 1 d . . . H92A H 0.7862 0.6935 0.1417 0.147 Uiso 1 1 calc R . . H92B H 0.8588 0.7777 0.1846 0.147 Uiso 1 1 calc R . . C93 C 0.897(2) 0.678(2) 0.1872(15) 0.314 Uani 1 1 d . . . H93A H 0.8764 0.6259 0.1594 0.377 Uiso 1 1 calc R . . H93B H 0.9560 0.7188 0.1849 0.377 Uiso 1 1 calc R . . C94 C 0.9066(14) 0.6592(15) 0.2352(8) 0.155 Uani 1 1 d . . . H94A H 0.9646 0.7025 0.2604 0.186 Uiso 1 1 calc R . . H94B H 0.9143 0.6034 0.2340 0.186 Uiso 1 1 calc R . . C102 C 0.8317(12) 0.6546(12) 0.2576(6) 0.114 Uani 1 1 d . . . H10A H 0.7958 0.5948 0.2587 0.137 Uiso 1 1 calc R . . H10B H 0.8556 0.6889 0.2948 0.137 Uiso 1 1 calc R . . C103 C 0.5132(11) 0.1314(13) 0.6597(7) 0.128 Uani 1 1 d . . . H103 H 0.4694 0.1055 0.6779 0.154 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Sn1 0.027 0.033 0.022 0.002 0.006 0.015 Sn2 0.029 0.036 0.019 0.000 0.006 0.016 Sn3 0.026 0.035 0.022 0.002 0.007 0.016 Sn4 0.032 0.042 0.026 -0.005 0.003 0.007 Sn5 0.036 0.042 0.025 -0.002 0.007 0.008 Sn6 0.033 0.043 0.031 -0.005 0.010 0.007 P1 0.027 0.036 0.023 0.000 0.006 0.015 P2 0.029 0.034 0.022 0.002 0.009 0.016 P3 0.051 0.048 0.024 -0.001 0.013 0.007 P4 0.042 0.043 0.027 -0.007 0.007 0.009 O1 0.036 0.039 0.020 0.003 0.013 0.019 O2 0.028 0.044 0.021 0.007 0.008 0.009 O3 0.039 0.044 0.022 0.003 0.007 0.025 O4 0.026 0.037 0.037 0.004 0.009 0.013 O5 0.028 0.040 0.029 0.007 0.007 0.012 O6 0.025 0.044 0.014 -0.001 0.008 0.014 O7 0.031 0.035 0.027 0.006 0.008 0.024 O8 0.042 0.043 0.028 0.000 0.007 0.029 O9 0.031 0.039 0.022 0.004 0.004 0.019 O10 0.027 0.033 0.041 0.004 0.013 0.011 O11 0.046 0.059 0.028 0.001 0.021 0.017 O12 0.058 0.045 0.029 0.004 0.004 0.003 O13 0.042 0.048 0.023 -0.005 -0.003 -0.001 O14 0.047 0.038 0.036 -0.008 -0.004 0.012 O15 0.044 0.046 0.026 -0.011 0.013 0.011 O16 0.044 0.044 0.022 -0.002 0.012 0.012 O17 0.026 0.037 0.034 0.006 0.009 0.002 O18 0.034 0.044 0.039 0.001 0.011 0.011 O19 0.032 0.044 0.034 0.001 0.000 0.007 O20 0.033 0.036 0.037 -0.010 0.004 0.003 O21 0.221 0.123 0.228 0.003 0.145 0.031 O22 0.239 0.217 0.295 0.081 0.171 0.123 N1 0.043 0.056 0.040 0.006 0.019 0.016 N2 0.040 0.065 0.076 0.034 0.018 0.022 N3 0.060 0.074 0.069 0.031 -0.009 -0.001 N4 0.046 0.046 0.043 0.003 0.012 0.012 N5 0.031 0.067 0.084 0.001 -0.008 0.012 N6 0.044 0.062 0.110 0.014 0.001 0.018 N7 0.044 0.051 0.020 0.003 0.020 0.032 N8 0.033 0.038 0.045 0.003 0.010 0.011 N9 0.044 0.040 0.026 0.005 0.006 0.025 N10 0.056 0.047 0.032 0.008 0.012 0.022 N11 0.036 0.074 0.110 0.035 -0.006 0.024 N12 0.063 0.078 0.099 0.030 0.009 0.037 C1 0.046 0.036 0.040 -0.006 -0.008 0.011 C2 0.046 0.037 0.068 -0.005 -0.015 0.013 C3 0.069 0.042 0.077 0.001 -0.024 0.013 C4 0.035 0.045 0.054 -0.003 0.005 0.011 C5 0.038 0.056 0.067 -0.004 0.007 0.011 C6 0.044 0.033 0.051 0.002 -0.007 0.010 C7 0.043 0.103 0.090 0.049 0.025 0.044 C8 0.043 0.254 0.081 0.076 0.020 0.013 C9 0.069 0.291 0.110 0.071 0.047 0.031 C10 0.069 0.163 0.108 0.070 0.059 0.042 C11 0.090 0.130 0.057 0.001 0.038 0.030 C12 0.069 0.089 0.065 0.005 0.037 0.006 C13 0.047 0.044 0.026 -0.007 0.000 0.019 C14 0.047 0.079 0.032 -0.010 0.002 0.017 C15 0.055 0.087 0.049 0.019 0.016 0.031 C16 0.088 0.064 0.053 0.022 0.016 0.046 C17 0.074 0.049 0.049 0.014 0.003 0.028 C18 0.059 0.035 0.047 -0.002 0.009 0.022 C19 0.078 0.099 0.077 0.030 -0.010 -0.003 C20 0.078 0.099 0.077 0.030 -0.010 -0.003 C21 0.090 0.067 0.119 0.022 -0.033 0.014 C22 0.149 0.149 0.149 0.036 0.038 0.051 C23 0.149 0.149 0.149 0.036 0.038 0.051 C24 0.078 0.099 0.077 0.030 -0.010 -0.003 C25 0.050 0.054 0.057 0.020 0.034 0.012 C26 0.080 0.081 0.079 0.016 0.043 0.045 C27 0.101 0.087 0.148 0.044 0.096 0.053 C28 0.072 0.109 0.214 0.079 0.100 0.051 C29 0.046 0.083 0.119 0.031 0.040 0.028 C30 0.060 0.057 0.078 0.021 0.023 0.023 C31 0.102 0.041 0.087 -0.006 -0.033 0.020 C32 0.064 0.069 0.074 0.008 -0.013 0.022 C33 0.165 0.108 0.065 -0.001 -0.036 0.089 C34 0.154 0.086 0.132 0.008 -0.056 0.044 C35 0.127 0.083 0.060 0.006 -0.052 0.020 C36 0.082 0.071 0.143 -0.003 -0.055 0.017 C37 0.050 0.041 0.038 -0.006 0.004 0.004 C38 0.078 0.054 0.051 -0.018 0.020 0.020 C39 0.074 0.045 0.030 -0.016 0.013 0.017 C40 0.069 0.055 0.043 -0.009 0.010 0.027 C41 0.072 0.050 0.020 -0.006 0.017 0.005 C42 0.087 0.065 0.021 -0.008 0.013 0.015 C43 0.068 0.076 0.037 -0.004 0.019 0.007 C44 0.090 0.094 0.040 0.012 0.028 0.000 C45 0.038 0.037 0.031 0.009 0.003 0.015 C46 0.064 0.052 0.056 0.019 0.030 0.041 C47 0.072 0.047 0.085 0.040 0.045 0.034 C48 0.068 0.048 0.088 0.027 0.034 0.037 C49 0.052 0.048 0.047 0.013 0.023 0.027 C50 0.036 0.035 0.027 0.011 0.010 0.020 C51 0.035 0.040 0.038 0.002 0.005 0.018 C52 0.043 0.036 0.049 0.003 0.025 0.015 C53 0.037 0.054 0.049 -0.004 0.018 0.016 C54 0.052 0.061 0.041 0.010 0.020 0.026 C55 0.056 0.038 0.043 0.011 0.025 0.026 C56 0.043 0.050 0.044 -0.010 0.001 0.027 C57 0.028 0.037 0.028 -0.001 0.004 0.012 C58 0.074 0.070 0.033 -0.003 0.017 0.027 C59 0.138 0.087 0.036 -0.007 0.016 0.062 C60 0.044 0.096 0.027 -0.010 0.001 0.006 C61 0.122 0.107 0.040 0.024 0.022 0.084 C62 0.059 0.090 0.051 0.016 0.016 0.045 C63 0.066 0.074 0.069 0.031 0.013 0.023 C64 0.056 0.060 0.126 0.014 0.004 0.034 C65 0.074 0.086 0.087 0.002 0.015 0.041 C66 0.080 0.134 0.079 0.030 0.023 0.061 C67 0.082 0.187 0.078 -0.006 0.003 0.061 C68 0.072 0.186 0.032 -0.020 -0.010 0.046 C69 0.019 0.038 0.014 -0.004 0.002 0.011 C70 0.032 0.044 0.029 -0.001 0.002 0.020 C71 0.041 0.059 0.040 0.002 0.014 0.026 C72 0.041 0.061 0.049 -0.004 0.008 0.034 C73 0.058 0.054 0.052 0.006 0.015 0.039 C74 0.041 0.043 0.030 0.000 0.002 0.030 C75 0.048 0.060 0.052 0.013 -0.006 0.014 C76 0.094 0.110 0.119 0.083 0.078 0.080 C77 0.133 0.262 0.192 0.194 0.138 0.146 C78 0.085 0.076 0.054 0.034 0.006 0.002 C79 0.074 0.049 0.086 0.023 -0.014 0.003 C80 0.027 0.051 0.030 0.003 0.008 0.015 C81 0.066 0.079 0.052 0.036 0.031 0.036 C82 0.075 0.069 0.050 -0.006 0.041 0.026 C83 0.049 0.061 0.047 0.013 0.017 0.016 C84 0.031 0.031 0.035 0.001 0.011 0.011 C85 0.044 0.047 0.053 -0.009 -0.010 0.014 C86 0.031 0.042 0.036 0.012 0.017 0.015 C87 0.033 0.042 0.038 0.003 0.014 0.012 C88 0.027 0.026 0.045 0.009 0.012 0.012 C89 0.077 0.111 0.055 0.007 0.030 0.048 C90 0.097 0.072 0.100 0.031 0.055 0.035 C91 0.203 0.073 0.218 -0.023 0.150 0.018 C92 0.193 0.130 0.065 0.027 0.051 0.074 C93 0.343 0.439 0.435 0.352 0.344 0.254 C94 0.128 0.187 0.160 0.007 0.047 0.074 C102 0.150 0.142 0.056 0.039 0.023 0.060 C103 0.099 0.199 0.148 0.130 0.070 0.082 _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 Sn1 O7 2.066(5) . ? Sn1 O10 2.071(5) . ? Sn1 O3 2.077(5) . ? Sn1 O5 2.106(5) . ? Sn1 C45 2.143(9) . ? Sn1 O9 2.158(5) . ? Sn2 O2 2.066(5) 2_666 ? Sn2 O9 2.088(5) . ? Sn2 O8 2.094(5) . ? Sn2 O7 2.106(5) . ? Sn2 C57 2.129(8) . ? Sn2 O6 2.134(5) . ? Sn3 O1 2.035(5) . ? Sn3 O7 2.039(5) . ? Sn3 O10 2.078(5) 2_666 ? Sn3 O4 2.097(5) . ? Sn3 O8 2.145(6) . ? Sn3 C69 2.164(7) . ? Sn4 O13 2.048(7) . ? Sn4 O17 2.070(5) . ? Sn4 O20 2.084(6) 2_677 ? Sn4 O14 2.093(6) . ? Sn4 O18 2.128(6) . ? Sn4 C1 2.154(9) . ? Sn5 O12 2.063(6) 2_677 ? Sn5 O17 2.075(6) . ? Sn5 O18 2.110(6) . ? Sn5 O19 2.115(6) . ? Sn5 O16 2.129(5) . ? Sn5 C13 2.145(10) . ? Sn5 Sn6 3.2751(11) . ? Sn6 O11 2.033(7) . ? Sn6 O17 2.048(5) . ? Sn6 O20 2.088(5) . ? Sn6 O15 2.096(5) . ? Sn6 C25 2.126(10) . ? Sn6 O19 2.127(6) . ? P1 O4 1.524(6) . ? P1 O5 1.531(6) . ? P1 O6 1.561(5) . ? P1 C84 1.800(8) . ? P2 O3 1.513(5) . ? P2 O1 1.517(6) . ? P2 O2 1.527(5) . ? P2 C80 1.821(9) . ? P3 O13 1.517(7) . ? P3 O12 1.539(7) . ? P3 O11 1.540(7) . ? P3 C41 1.776(9) . ? P4 O16 1.529(6) . ? P4 O14 1.538(6) . ? P4 O15 1.551(6) . ? P4 C37 1.799(9) . ? O2 Sn2 2.066(5) 2_666 ? O10 Sn3 2.078(5) 2_666 ? O12 Sn5 2.063(6) 2_677 ? O20 Sn4 2.084(6) 2_677 ? O21 C91 1.46(2) . ? O21 C88 1.467(14) . ? O22 C102 1.39(2) . ? O22 C92 1.52(2) . ? N1 N2 1.268(10) . ? N1 C6 1.392(12) . ? N2 C7 1.455(14) . ? N3 N4 1.240(11) . ? N3 C19 1.400(15) . ? N4 C18 1.452(12) . ? N5 N6 1.258(12) . ? N5 C30 1.509(14) . ? N6 C31 1.386(17) . ? N7 N8 1.220(9) . ? N7 C50 1.450(10) . ? N8 C51 1.467(11) . ? N9 N10 1.242(10) . ? N9 C74 1.400(11) . ? N10 C75 1.455(13) . ? N11 N12 1.267(11) . ? N11 C63 1.308(15) . ? N12 C62 1.443(14) . ? C1 C6 1.378(14) . ? C1 C2 1.384(14) . ? C2 C3 1.394(13) . ? C3 C4 1.376(15) . ? C4 C5 1.423(14) . ? C5 C6 1.435(13) . ? C7 C8 1.356(16) . ? C7 C12 1.362(16) . ? C8 C9 1.37(2) . ? C9 C10 1.28(2) . ? C10 C11 1.372(17) . ? C11 C12 1.340(15) . ? C13 C18 1.353(13) . ? C13 C14 1.403(12) . ? C14 C15 1.392(15) . ? C15 C16 1.341(15) . ? C16 C17 1.387(14) . ? C17 C18 1.389(14) . ? C19 C20 1.292(18) . ? C19 C24 1.374(17) . ? C20 C21 1.395(16) . ? C21 C22 1.35(2) . ? C22 C23 1.38(2) . ? C23 C24 1.49(2) . ? C25 C30 1.379(14) . ? C25 C26 1.402(14) . ? C26 C27 1.387(15) . ? C27 C28 1.39(2) . ? C28 C29 1.372(19) . ? C29 C30 1.356(15) . ? C31 C32 1.379(19) . ? C31 C36 1.419(16) . ? C32 C33 1.389(18) . ? C33 C34 1.337(18) . ? C34 C35 1.424(16) . ? C35 C36 1.484(15) . ? C37 C39 1.507(14) . ? C37 C38 1.560(14) . ? C37 C40 1.574(14) . ? C41 C42 1.496(15) . ? C41 C44 1.523(15) . ? C41 C43 1.532(14) . ? C45 C50 1.325(11) . ? C45 C46 1.446(13) . ? C46 C47 1.384(13) . ? C47 C48 1.456(13) . ? C48 C49 1.297(13) . ? C49 C50 1.394(12) . ? C51 C52 1.358(11) . ? C51 C56 1.386(13) . ? C52 C53 1.378(12) . ? C53 C54 1.334(13) . ? C54 C55 1.369(12) . ? C55 C56 1.340(13) . ? C57 C62 1.387(12) . ? C57 C58 1.407(12) . ? C58 C59 1.375(14) . ? C59 C60 1.337(16) . ? C60 C61 1.292(14) . ? C61 C62 1.427(14) . ? C63 C64 1.328(15) . ? C63 C68 1.464(16) . ? C64 C65 1.403(17) . ? C65 C66 1.398(17) . ? C66 C67 1.424(18) . ? C67 C68 1.397(18) . ? C69 C70 1.348(11) . ? C69 C74 1.401(12) . ? C70 C71 1.378(11) . ? C71 C72 1.372(13) . ? C72 C73 1.392(14) . ? C73 C74 1.368(11) . ? C75 C76 1.357(15) . ? C75 C79 1.369(15) . ? C76 C77 1.370(15) . ? C77 C103 1.34(2) . ? C78 C103 1.285(19) . ? C78 C79 1.477(17) . ? C80 C81 1.489(13) . ? C80 C83 1.529(12) . ? C80 C82 1.539(12) . ? C84 C87 1.538(11) . ? C84 C86 1.539(11) . ? C84 C85 1.568(11) . ? C88 C89 1.395(14) . ? C89 C90 1.590(15) . ? C90 C91 1.380(19) . ? C92 C93 1.37(3) . ? C93 C94 1.27(3) . ? C94 C102 1.41(2) . ? loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.000 0.000 0.500 1117 321 ' ' _platon_squeeze_details ; ; 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 O7 Sn1 O10 93.0(2) . . ? O7 Sn1 O3 88.6(2) . . ? O10 Sn1 O3 88.0(2) . . ? O7 Sn1 O5 87.9(2) . . ? O10 Sn1 O5 176.4(2) . . ? O3 Sn1 O5 88.6(2) . . ? O7 Sn1 C45 172.1(3) . . ? O10 Sn1 C45 94.0(3) . . ? O3 Sn1 C45 95.4(3) . . ? O5 Sn1 C45 85.4(3) . . ? O7 Sn1 O9 74.9(2) . . ? O10 Sn1 O9 90.9(2) . . ? O3 Sn1 O9 163.4(2) . . ? O5 Sn1 O9 92.7(2) . . ? C45 Sn1 O9 101.2(3) . . ? O2 Sn2 O9 93.4(2) 2_666 . ? O2 Sn2 O8 93.1(2) 2_666 . ? O9 Sn2 O8 150.0(2) . . ? O2 Sn2 O7 91.4(2) 2_666 . ? O9 Sn2 O7 75.56(19) . . ? O8 Sn2 O7 75.1(2) . . ? O2 Sn2 C57 90.2(3) 2_666 . ? O9 Sn2 C57 106.0(3) . . ? O8 Sn2 C57 103.2(3) . . ? O7 Sn2 C57 177.7(2) . . ? O2 Sn2 O6 178.9(2) 2_666 . ? O9 Sn2 O6 87.4(2) . . ? O8 Sn2 O6 86.5(2) . . ? O7 Sn2 O6 89.5(2) . . ? C57 Sn2 O6 88.9(3) . . ? O1 Sn3 O7 89.6(2) . . ? O1 Sn3 O10 87.7(2) . 2_666 ? O7 Sn3 O10 90.8(2) . 2_666 ? O1 Sn3 O4 91.9(2) . . ? O7 Sn3 O4 86.8(2) . . ? O10 Sn3 O4 177.6(2) 2_666 . ? O1 Sn3 O8 164.1(2) . . ? O7 Sn3 O8 75.4(2) . . ? O10 Sn3 O8 87.5(2) 2_666 . ? O4 Sn3 O8 92.3(2) . . ? O1 Sn3 C69 94.5(2) . . ? O7 Sn3 C69 173.4(2) . . ? O10 Sn3 C69 94.6(2) 2_666 . ? O4 Sn3 C69 87.9(2) . . ? O8 Sn3 C69 100.9(2) . . ? O13 Sn4 O17 89.6(2) . . ? O13 Sn4 O20 87.7(2) . 2_677 ? O17 Sn4 O20 92.8(2) . 2_677 ? O13 Sn4 O14 89.4(3) . . ? O17 Sn4 O14 87.1(2) . . ? O20 Sn4 O14 177.1(3) 2_677 . ? O13 Sn4 O18 163.3(2) . . ? O17 Sn4 O18 73.8(2) . . ? O20 Sn4 O18 90.8(2) 2_677 . ? O14 Sn4 O18 92.0(2) . . ? O13 Sn4 C1 92.4(3) . . ? O17 Sn4 C1 173.8(3) . . ? O20 Sn4 C1 93.2(3) 2_677 . ? O14 Sn4 C1 87.0(3) . . ? O18 Sn4 C1 104.3(3) . . ? O12 Sn5 O17 90.8(2) 2_677 . ? O12 Sn5 O18 94.4(2) 2_677 . ? O17 Sn5 O18 74.1(2) . . ? O12 Sn5 O19 92.3(2) 2_677 . ? O17 Sn5 O19 75.3(2) . . ? O18 Sn5 O19 148.7(2) . . ? O12 Sn5 O16 177.1(2) 2_677 . ? O17 Sn5 O16 88.3(2) . . ? O18 Sn5 O16 88.0(2) . . ? O19 Sn5 O16 84.9(2) . . ? O12 Sn5 C13 87.7(3) 2_677 . ? O17 Sn5 C13 175.5(3) . . ? O18 Sn5 C13 110.2(3) . . ? O19 Sn5 C13 100.6(3) . . ? O16 Sn5 C13 93.0(3) . . ? O12 Sn5 Sn6 99.90(18) 2_677 . ? O17 Sn5 Sn6 37.13(15) . . ? O18 Sn5 Sn6 109.14(17) . . ? O19 Sn5 Sn6 39.59(17) . . ? O16 Sn5 Sn6 77.78(16) . . ? C13 Sn5 Sn6 139.2(2) . . ? O11 Sn6 O17 91.0(2) . . ? O11 Sn6 O20 88.5(2) . . ? O17 Sn6 O20 91.8(2) . . ? O11 Sn6 O15 92.3(2) . . ? O17 Sn6 O15 87.3(2) . . ? O20 Sn6 O15 178.8(2) . . ? O11 Sn6 C25 92.3(3) . . ? O17 Sn6 C25 174.9(3) . . ? O20 Sn6 C25 92.3(3) . . ? O15 Sn6 C25 88.6(3) . . ? O11 Sn6 O19 165.7(2) . . ? O17 Sn6 O19 75.6(2) . . ? O20 Sn6 O19 87.1(2) . . ? O15 Sn6 O19 91.9(2) . . ? C25 Sn6 O19 101.5(3) . . ? O11 Sn6 Sn5 128.18(17) . . ? O17 Sn6 Sn5 37.69(17) . . ? O20 Sn6 Sn5 97.40(17) . . ? O15 Sn6 Sn5 81.42(16) . . ? C25 Sn6 Sn5 138.4(3) . . ? O19 Sn6 Sn5 39.33(15) . . ? O4 P1 O5 111.1(3) . . ? O4 P1 O6 112.2(3) . . ? O5 P1 O6 110.2(3) . . ? O4 P1 C84 106.2(3) . . ? O5 P1 C84 108.0(4) . . ? O6 P1 C84 109.0(4) . . ? O3 P2 O1 113.1(3) . . ? O3 P2 O2 112.0(3) . . ? O1 P2 O2 112.2(3) . . ? O3 P2 C80 107.0(4) . . ? O1 P2 C80 106.0(3) . . ? O2 P2 C80 105.9(3) . . ? O13 P3 O12 111.3(4) . . ? O13 P3 O11 113.6(4) . . ? O12 P3 O11 111.1(4) . . ? O13 P3 C41 105.3(4) . . ? O12 P3 C41 106.8(4) . . ? O11 P3 C41 108.2(5) . . ? O16 P4 O14 110.4(4) . . ? O16 P4 O15 110.1(3) . . ? O14 P4 O15 112.2(4) . . ? O16 P4 C37 110.7(4) . . ? O14 P4 C37 106.3(4) . . ? O15 P4 C37 107.2(4) . . ? P2 O1 Sn3 139.4(3) . . ? P2 O2 Sn2 144.3(3) . 2_666 ? P2 O3 Sn1 139.1(4) . . ? P1 O4 Sn3 123.8(3) . . ? P1 O5 Sn1 122.3(3) . . ? P1 O6 Sn2 119.5(3) . . ? Sn3 O7 Sn1 134.1(3) . . ? Sn3 O7 Sn2 104.8(2) . . ? Sn1 O7 Sn2 104.0(2) . . ? Sn2 O8 Sn3 101.5(2) . . ? Sn2 O9 Sn1 101.5(2) . . ? Sn1 O10 Sn3 147.3(3) . 2_666 ? P3 O11 Sn6 137.9(4) . . ? P3 O12 Sn5 146.7(4) . 2_677 ? P3 O13 Sn4 139.7(4) . . ? P4 O14 Sn4 123.4(3) . . ? P4 O15 Sn6 122.5(3) . . ? P4 O16 Sn5 121.3(4) . . ? Sn6 O17 Sn4 133.3(3) . . ? Sn6 O17 Sn5 105.2(3) . . ? Sn4 O17 Sn5 105.7(2) . . ? Sn5 O18 Sn4 102.4(2) . . ? Sn5 O19 Sn6 101.1(2) . . ? Sn4 O20 Sn6 147.3(3) 2_677 . ? C91 O21 C88 102.1(12) . . ? C102 O22 C92 103.8(14) . . ? N2 N1 C6 114.3(8) . . ? N1 N2 C7 112.6(8) . . ? N4 N3 C19 113.3(10) . . ? N3 N4 C18 114.6(8) . . ? N6 N5 C30 114.6(10) . . ? N5 N6 C31 115.2(11) . . ? N8 N7 C50 115.5(7) . . ? N7 N8 C51 117.5(7) . . ? N10 N9 C74 115.1(7) . . ? N9 N10 C75 115.6(8) . . ? N12 N11 C63 118.0(12) . . ? N11 N12 C62 116.4(11) . . ? C6 C1 C2 119.1(9) . . ? C6 C1 Sn4 122.9(7) . . ? C2 C1 Sn4 118.0(8) . . ? C1 C2 C3 122.2(12) . . ? C4 C3 C2 119.1(12) . . ? C3 C4 C5 121.2(10) . . ? C4 C5 C6 117.3(10) . . ? C1 C6 N1 117.6(8) . . ? C1 C6 C5 121.0(10) . . ? N1 C6 C5 121.4(10) . . ? C8 C7 C12 118.0(13) . . ? C8 C7 N2 115.0(11) . . ? C12 C7 N2 126.3(11) . . ? C7 C8 C9 120.0(15) . . ? C10 C9 C8 122.4(16) . . ? C9 C10 C11 117.6(15) . . ? C12 C11 C10 122.5(14) . . ? C11 C12 C7 119.0(13) . . ? C18 C13 C14 119.3(10) . . ? C18 C13 Sn5 122.6(7) . . ? C14 C13 Sn5 118.0(8) . . ? C15 C14 C13 120.2(11) . . ? C16 C15 C14 119.4(11) . . ? C15 C16 C17 121.1(11) . . ? C16 C17 C18 119.6(11) . . ? C13 C18 C17 120.3(10) . . ? C13 C18 N4 115.6(9) . . ? C17 C18 N4 124.0(9) . . ? C20 C19 C24 119.4(13) . . ? C20 C19 N3 127.7(13) . . ? C24 C19 N3 112.7(12) . . ? C19 C20 C21 125.0(14) . . ? C22 C21 C20 118.2(16) . . ? C21 C22 C23 121(2) . . ? C22 C23 C24 117(2) . . ? C19 C24 C23 118.7(15) . . ? C30 C25 C26 114.6(10) . . ? C30 C25 Sn6 126.8(8) . . ? C26 C25 Sn6 118.6(8) . . ? C27 C26 C25 121.1(13) . . ? C26 C27 C28 120.8(14) . . ? C29 C28 C27 119.0(12) . . ? C30 C29 C28 118.6(13) . . ? C29 C30 C25 125.9(12) . . ? C29 C30 N5 120.0(11) . . ? C25 C30 N5 114.0(9) . . ? C32 C31 N6 124.8(11) . . ? C32 C31 C36 123.3(15) . . ? N6 C31 C36 111.9(15) . . ? C31 C32 C33 117.9(13) . . ? C34 C33 C32 128.6(19) . . ? C33 C34 C35 111.1(18) . . ? C34 C35 C36 127.4(13) . . ? C31 C36 C35 111.4(15) . . ? C39 C37 C38 108.7(8) . . ? C39 C37 C40 110.8(9) . . ? C38 C37 C40 110.2(9) . . ? C39 C37 P4 109.1(7) . . ? C38 C37 P4 108.5(7) . . ? C40 C37 P4 109.5(6) . . ? C42 C41 C44 112.7(10) . . ? C42 C41 C43 109.0(8) . . ? C44 C41 C43 107.6(9) . . ? C42 C41 P3 110.5(7) . . ? C44 C41 P3 107.7(7) . . ? C43 C41 P3 109.2(7) . . ? C50 C45 C46 118.3(8) . . ? C50 C45 Sn1 128.0(7) . . ? C46 C45 Sn1 113.6(6) . . ? C47 C46 C45 119.9(8) . . ? C46 C47 C48 118.1(10) . . ? C49 C48 C47 118.6(10) . . ? C48 C49 C50 123.3(9) . . ? C45 C50 C49 121.2(8) . . ? C45 C50 N7 117.3(8) . . ? C49 C50 N7 121.2(7) . . ? C52 C51 C56 121.1(9) . . ? C52 C51 N8 116.1(8) . . ? C56 C51 N8 122.9(8) . . ? C51 C52 C53 119.5(9) . . ? C54 C53 C52 118.9(9) . . ? C53 C54 C55 121.9(10) . . ? C56 C55 C54 120.3(9) . . ? C55 C56 C51 118.4(8) . . ? C62 C57 C58 117.4(9) . . ? C62 C57 Sn2 122.4(7) . . ? C58 C57 Sn2 119.7(7) . . ? C59 C58 C57 119.0(11) . . ? C60 C59 C58 122.1(12) . . ? C61 C60 C59 121.1(11) . . ? C60 C61 C62 120.6(11) . . ? C57 C62 C61 119.3(10) . . ? C57 C62 N12 117.3(9) . . ? C61 C62 N12 123.1(10) . . ? N11 C63 C64 119.9(13) . . ? N11 C63 C68 123.8(11) . . ? C64 C63 C68 116.3(13) . . ? C63 C64 C65 124.1(14) . . ? C66 C65 C64 121.0(13) . . ? C65 C66 C67 117.1(13) . . ? C68 C67 C66 120.4(14) . . ? C67 C68 C63 120.9(13) . . ? C70 C69 C74 117.8(7) . . ? C70 C69 Sn3 118.7(6) . . ? C74 C69 Sn3 123.5(6) . . ? C69 C70 C71 123.0(9) . . ? C72 C71 C70 119.2(9) . . ? C71 C72 C73 119.1(8) . . ? C74 C73 C72 120.5(10) . . ? C73 C74 N9 123.0(9) . . ? C73 C74 C69 120.4(9) . . ? N9 C74 C69 116.6(7) . . ? C76 C75 C79 123.2(13) . . ? C76 C75 N10 124.3(10) . . ? C79 C75 N10 112.5(11) . . ? C75 C76 C77 118.4(13) . . ? C103 C77 C76 120.0(15) . . ? C103 C78 C79 119.0(13) . . ? C75 C79 C78 115.2(13) . . ? C81 C80 C83 109.3(8) . . ? C81 C80 C82 108.8(8) . . ? C83 C80 C82 109.8(8) . . ? C81 C80 P2 110.5(6) . . ? C83 C80 P2 108.3(6) . . ? C82 C80 P2 110.2(7) . . ? C87 C84 C86 111.0(7) . . ? C87 C84 C85 109.1(7) . . ? C86 C84 C85 110.1(8) . . ? C87 C84 P1 108.8(6) . . ? C86 C84 P1 108.8(6) . . ? C85 C84 P1 109.0(6) . . ? C89 C88 O21 110.4(9) . . ? C88 C89 C90 104.3(9) . . ? C91 C90 C89 103.7(11) . . ? C90 C91 O21 109.5(15) . . ? C93 C92 O22 106.9(15) . . ? C94 C93 C92 106(2) . . ? C93 C94 C102 116(2) . . ? O22 C102 C94 104.1(15) . . ? C78 C103 C77 124.2(15) . . ? _diffrn_measured_fraction_theta_max 0.982 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.982 _refine_diff_density_max 2.001 _refine_diff_density_min -1.288 _refine_diff_density_rms 0.174 _database_code_depnum_ccdc_archive 'CCDC 968921' ####################################################################### # # 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_2 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C104 H110 N12 O22 P4 Sn6' _chemical_formula_weight 2716.06 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' P P 0.1023 0.0942 '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 ? _symmetry_space_group_name_H-M 'C 2/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 24.017(5) _cell_length_b 20.738(5) _cell_length_c 21.962(5) _cell_angle_alpha 90.000(5) _cell_angle_beta 96.639(5) _cell_angle_gamma 90.000(5) _cell_volume 10865(4) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.660 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5416 _exptl_absorpt_coefficient_mu 1.492 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.707084 _exptl_absorpt_correction_T_max 1 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 29339 _diffrn_reflns_av_R_equivalents 0.0697 _diffrn_reflns_av_sigmaI/netI 0.0851 _diffrn_reflns_limit_h_min -29 _diffrn_reflns_limit_h_max 29 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.96 _diffrn_reflns_theta_max 25.50 _reflns_number_total 10096 _reflns_number_gt 6945 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0566P)^2^+10.9739P] 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 10096 _refine_ls_number_parameters 667 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0871 _refine_ls_R_factor_gt 0.0531 _refine_ls_wR_factor_ref 0.1348 _refine_ls_wR_factor_gt 0.1131 _refine_ls_goodness_of_fit_ref 1.023 _refine_ls_restrained_S_all 1.023 _refine_ls_shift/su_max 0.007 _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 Sn1 Sn 0.277826(19) 0.13931(2) 0.56687(2) 0.02557(13) Uani 1 1 d . . . Sn2 Sn 0.351848(19) 0.36370(2) 0.50343(2) 0.02703(14) Uani 1 1 d . . . Sn3 Sn 0.329237(19) 0.23072(2) 0.42301(2) 0.02691(14) Uani 1 1 d . . . P1 P 0.30701(7) 0.28604(8) 0.62775(9) 0.0280(4) Uani 1 1 d . . . P2 P 0.17187(8) 0.13066(8) 0.64319(9) 0.0295(4) Uani 1 1 d . . . O1 O 0.34315(18) 0.3254(2) 0.5885(2) 0.0317(11) Uani 1 1 d . . . O2 O 0.31497(18) 0.2135(2) 0.6199(2) 0.0284(11) Uani 1 1 d . . . O3 O 0.24541(18) 0.3062(2) 0.6179(2) 0.0292(11) Uani 1 1 d . . . O4 O 0.23403(18) 0.1117(2) 0.6412(2) 0.0286(11) Uani 1 1 d . . . O5 O 0.13536(18) 0.1043(2) 0.5863(2) 0.0305(11) Uani 1 1 d . . . O6 O 0.16480(19) 0.2039(2) 0.6489(2) 0.0302(11) Uani 1 1 d . . . O7 O 0.32388(18) 0.1690(2) 0.4967(2) 0.0270(11) Uani 1 1 d . . . O8 O 0.28840(17) 0.3027(2) 0.4633(2) 0.0273(11) Uani 1 1 d . . . O9 O 0.39391(18) 0.2803(2) 0.4806(2) 0.0280(11) Uani 1 1 d . . . O10 O 0.27754(18) 0.4169(2) 0.4963(2) 0.0291(11) Uani 1 1 d . . . O11 O 0.4974(2) 0.2903(3) 0.4420(3) 0.0617(17) Uani 1 1 d . . . N1 N 0.3636(2) 0.5163(3) 0.5032(3) 0.0395(16) Uani 1 1 d . . . N2 N 0.3595(3) 0.5770(3) 0.4980(3) 0.0494(19) Uani 1 1 d . . . N3 N 0.4320(2) 0.1310(3) 0.4685(3) 0.0305(14) Uani 1 1 d . . . N4 N 0.4781(2) 0.1087(3) 0.4897(3) 0.0361(15) Uani 1 1 d . . . N5 N 0.3359(2) 0.0188(3) 0.5032(3) 0.0325(14) Uani 1 1 d . . . N6 N 0.3347(3) -0.0362(3) 0.4792(3) 0.0398(16) Uani 1 1 d . . . C1 C 0.4175(3) 0.4256(3) 0.5428(3) 0.0275(16) Uani 1 1 d . . . C2 C 0.4664(3) 0.4000(4) 0.5729(4) 0.0395(19) Uani 1 1 d . . . H2 H 0.4695 0.3557 0.5793 0.047 Uiso 1 1 calc R . . C3 C 0.5106(3) 0.4399(4) 0.5934(4) 0.043(2) Uani 1 1 d . . . H3 H 0.5432 0.4219 0.6132 0.052 Uiso 1 1 calc R . . C4 C 0.5074(3) 0.5059(4) 0.5852(3) 0.0387(19) Uani 1 1 d . . . H4 H 0.5379 0.5318 0.5986 0.046 Uiso 1 1 calc R . . C5 C 0.4603(3) 0.5323(4) 0.5579(4) 0.0403(19) Uani 1 1 d . . . H5 H 0.4577 0.5768 0.5536 0.048 Uiso 1 1 calc R . . C6 C 0.4144(3) 0.4929(3) 0.5357(3) 0.0352(18) Uani 1 1 d . . . C7 C 0.3083(3) 0.5971(4) 0.4631(5) 0.053(2) Uani 1 1 d . . . C8 C 0.2881(4) 0.6552(5) 0.4748(5) 0.070(3) Uani 1 1 d . . . H8 H 0.3076 0.6806 0.5050 0.084 Uiso 1 1 calc R . . C9 C 0.2399(4) 0.6786(5) 0.4439(6) 0.081(4) Uani 1 1 d . . . H9 H 0.2260 0.7189 0.4531 0.097 Uiso 1 1 calc R . . C10 C 0.2124(4) 0.6406(4) 0.3984(5) 0.063(3) Uani 1 1 d . . . H10 H 0.1788 0.6550 0.3774 0.075 Uiso 1 1 calc R . . C11 C 0.2334(4) 0.5822(4) 0.3836(4) 0.055(2) Uani 1 1 d . . . H11 H 0.2154 0.5583 0.3513 0.066 Uiso 1 1 calc R . . C12 C 0.2811(3) 0.5591(4) 0.4165(4) 0.044(2) Uani 1 1 d . . . H12 H 0.2951 0.5188 0.4079 0.053 Uiso 1 1 calc R . . C13 C 0.3788(3) 0.1657(3) 0.3759(3) 0.0322(17) Uani 1 1 d . . . C14 C 0.3688(3) 0.1630(3) 0.3122(3) 0.0361(18) Uani 1 1 d . . . H14 H 0.3413 0.1893 0.2920 0.043 Uiso 1 1 calc R . . C15 C 0.3980(3) 0.1231(4) 0.2788(4) 0.046(2) Uani 1 1 d . . . H15 H 0.3903 0.1225 0.2363 0.055 Uiso 1 1 calc R . . C16 C 0.4390(3) 0.0835(4) 0.3073(4) 0.045(2) Uani 1 1 d . . . H16 H 0.4589 0.0560 0.2844 0.053 Uiso 1 1 calc R . . C17 C 0.4501(3) 0.0850(4) 0.3696(4) 0.042(2) Uani 1 1 d . . . H17 H 0.4776 0.0581 0.3891 0.051 Uiso 1 1 calc R . . C18 C 0.4211(3) 0.1258(3) 0.4035(3) 0.0325(17) Uani 1 1 d . . . C20 C 0.4919(3) 0.1166(3) 0.5544(3) 0.0325(17) Uani 1 1 d . . . C21 C 0.5365(3) 0.0800(4) 0.5800(4) 0.049(2) Uani 1 1 d . . . H21 H 0.5538 0.0513 0.5555 0.059 Uiso 1 1 calc R . . C22 C 0.5559(3) 0.0854(4) 0.6417(4) 0.051(2) Uani 1 1 d . . . H22 H 0.5853 0.0597 0.6592 0.062 Uiso 1 1 calc R . . C23 C 0.5310(3) 0.1292(4) 0.6765(4) 0.049(2) Uani 1 1 d . . . H23 H 0.5440 0.1344 0.7177 0.058 Uiso 1 1 calc R . . C24 C 0.4861(3) 0.1659(4) 0.6502(4) 0.050(2) Uani 1 1 d . . . H24 H 0.4693 0.1949 0.6747 0.059 Uiso 1 1 calc R . . C25 C 0.4658(3) 0.1609(4) 0.5897(4) 0.0406(19) Uani 1 1 d . . . H25 H 0.4359 0.1860 0.5727 0.049 Uiso 1 1 calc R . . C26 C 0.3396(3) 0.0708(3) 0.6012(3) 0.0328(17) Uani 1 1 d . . . C27 C 0.3605(3) 0.0737(4) 0.6628(3) 0.0357(18) Uani 1 1 d . . . H27 H 0.3486 0.1062 0.6874 0.043 Uiso 1 1 calc R . . C28 C 0.3982(3) 0.0294(4) 0.6873(4) 0.043(2) Uani 1 1 d . . . H28 H 0.4111 0.0315 0.7289 0.052 Uiso 1 1 calc R . . C29 C 0.4181(3) -0.0190(4) 0.6518(4) 0.043(2) Uani 1 1 d . . . H29 H 0.4446 -0.0483 0.6694 0.052 Uiso 1 1 calc R . . C30 C 0.3987(3) -0.0235(4) 0.5908(4) 0.042(2) Uani 1 1 d . . . H30 H 0.4120 -0.0555 0.5665 0.050 Uiso 1 1 calc R . . C31 C 0.3584(3) 0.0210(3) 0.5657(3) 0.0307(16) Uani 1 1 d . . . C32 C 0.3142(3) -0.0380(4) 0.4157(4) 0.047(2) Uani 1 1 d . . . C33 C 0.3088(4) -0.0975(5) 0.3902(5) 0.068(3) Uani 1 1 d . . . H33 H 0.3148 -0.1342 0.4144 0.082 Uiso 1 1 calc R . . C34 C 0.2937(4) -0.1029(6) 0.3258(6) 0.093(4) Uani 1 1 d . . . H34 H 0.2910 -0.1432 0.3071 0.112 Uiso 1 1 calc R . . C35 C 0.2834(4) -0.0488(6) 0.2920(5) 0.074(3) Uani 1 1 d . . . H35 H 0.2739 -0.0522 0.2498 0.089 Uiso 1 1 calc R . . C36 C 0.2866(4) 0.0116(6) 0.3189(4) 0.064(3) Uani 1 1 d . . . H36 H 0.2787 0.0482 0.2950 0.077 Uiso 1 1 calc R . . C37 C 0.3011(3) 0.0175(4) 0.3800(4) 0.050(2) Uani 1 1 d . . . H37 H 0.3024 0.0580 0.3984 0.060 Uiso 1 1 calc R . . C38 C 0.1486(3) 0.0953(3) 0.7105(3) 0.0361(18) Uani 1 1 d . . . H38 H 0.1752 0.1093 0.7451 0.043 Uiso 1 1 calc R . . C39 C 0.0922(3) 0.1185(4) 0.7236(4) 0.049(2) Uani 1 1 d . . . H39A H 0.0645 0.1071 0.6896 0.059 Uiso 1 1 calc R . . H39B H 0.0929 0.1652 0.7272 0.059 Uiso 1 1 calc R . . C40 C 0.0755(4) 0.0893(4) 0.7826(4) 0.067(3) Uani 1 1 d . . . H40A H 0.0378 0.1027 0.7883 0.081 Uiso 1 1 calc R . . H40B H 0.1008 0.1045 0.8173 0.081 Uiso 1 1 calc R . . C41 C 0.0782(4) 0.0151(4) 0.7793(5) 0.075(3) Uani 1 1 d . . . H41A H 0.0690 -0.0029 0.8176 0.089 Uiso 1 1 calc R . . H41B H 0.0504 0.0000 0.7468 0.089 Uiso 1 1 calc R . . C42 C 0.1327(4) -0.0076(4) 0.7678(5) 0.062(3) Uani 1 1 d . . . H42A H 0.1319 -0.0542 0.7641 0.074 Uiso 1 1 calc R . . H42B H 0.1599 0.0034 0.8024 0.074 Uiso 1 1 calc R . . C43 C 0.1511(3) 0.0213(3) 0.7100(4) 0.042(2) Uani 1 1 d . . . H43A H 0.1270 0.0052 0.6747 0.050 Uiso 1 1 calc R . . H43B H 0.1891 0.0077 0.7060 0.050 Uiso 1 1 calc R . . C44 C 0.3321(3) 0.3058(3) 0.7056(3) 0.0296(16) Uani 1 1 d . . . H44 H 0.3250 0.3518 0.7113 0.035 Uiso 1 1 calc R . . C45 C 0.3005(4) 0.2689(4) 0.7509(3) 0.053(2) Uani 1 1 d . . . H45A H 0.2607 0.2772 0.7416 0.064 Uiso 1 1 calc R . . H45B H 0.3065 0.2230 0.7459 0.064 Uiso 1 1 calc R . . C46 C 0.3191(4) 0.2876(5) 0.8169(4) 0.072(3) Uani 1 1 d . . . H46A H 0.3102 0.3326 0.8231 0.087 Uiso 1 1 calc R . . H46B H 0.2990 0.2618 0.8441 0.087 Uiso 1 1 calc R . . C47 C 0.3801(5) 0.2772(5) 0.8316(4) 0.076(3) Uani 1 1 d . . . H47A H 0.3882 0.2315 0.8300 0.091 Uiso 1 1 calc R . . H47B H 0.3918 0.2922 0.8729 0.091 Uiso 1 1 calc R . . C48 C 0.4120(4) 0.3123(5) 0.7877(4) 0.074(3) Uani 1 1 d . . . H48A H 0.4516 0.3024 0.7968 0.089 Uiso 1 1 calc R . . H48B H 0.4075 0.3584 0.7931 0.089 Uiso 1 1 calc R . . C49 C 0.3931(3) 0.2949(4) 0.7213(4) 0.052(2) Uani 1 1 d . . . H49A H 0.4135 0.3209 0.6946 0.062 Uiso 1 1 calc R . . H49B H 0.4016 0.2500 0.7145 0.062 Uiso 1 1 calc R . . C50 C 0.5456(4) 0.2722(4) 0.4825(5) 0.064(3) Uani 1 1 d . . . H50A H 0.5350 0.2442 0.5146 0.077 Uiso 1 1 calc R . . H50B H 0.5640 0.3101 0.5013 0.077 Uiso 1 1 calc R . . C51 C 0.5832(5) 0.2381(8) 0.4445(9) 0.151(7) Uani 1 1 d . . . H51 H 0.6194 0.2241 0.4573 0.182 Uiso 1 1 calc R . . C52 C 0.5536(7) 0.2306(9) 0.3843(7) 0.148(7) Uani 1 1 d . . . H52 H 0.5629 0.2033 0.3534 0.178 Uiso 1 1 calc R . . C53 C 0.5066(4) 0.2739(5) 0.3817(5) 0.072(3) Uani 1 1 d . . . H53A H 0.5142 0.3125 0.3591 0.087 Uiso 1 1 calc R . . H53B H 0.4734 0.2534 0.3608 0.087 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Sn1 0.0269(3) 0.0246(3) 0.0242(3) -0.0001(2) -0.0013(2) -0.00283(19) Sn2 0.0261(3) 0.0262(3) 0.0279(3) -0.0008(2) -0.0007(2) -0.0048(2) Sn3 0.0290(3) 0.0258(3) 0.0255(3) -0.0003(2) 0.0010(2) -0.0023(2) P1 0.0297(10) 0.0279(10) 0.0252(10) -0.0038(8) -0.0025(8) -0.0029(8) P2 0.0343(10) 0.0269(10) 0.0275(11) 0.0008(8) 0.0050(8) -0.0032(8) O1 0.031(3) 0.036(3) 0.027(3) 0.002(2) -0.003(2) -0.011(2) O2 0.032(3) 0.030(3) 0.022(3) -0.003(2) -0.003(2) -0.004(2) O3 0.031(3) 0.026(2) 0.029(3) 0.000(2) -0.004(2) -0.003(2) O4 0.031(3) 0.031(3) 0.023(3) 0.009(2) 0.000(2) -0.002(2) O5 0.030(3) 0.029(3) 0.033(3) 0.003(2) 0.005(2) -0.007(2) O6 0.038(3) 0.026(2) 0.027(3) 0.003(2) 0.005(2) -0.007(2) O7 0.030(3) 0.025(2) 0.026(3) 0.000(2) 0.000(2) -0.003(2) O8 0.028(3) 0.027(3) 0.026(3) 0.000(2) 0.000(2) -0.0032(19) O9 0.028(3) 0.024(2) 0.030(3) 0.000(2) -0.005(2) -0.0011(19) O10 0.025(2) 0.030(3) 0.032(3) -0.004(2) -0.002(2) -0.004(2) O11 0.042(4) 0.065(4) 0.076(5) -0.002(4) -0.002(3) -0.004(3) N1 0.037(4) 0.034(4) 0.047(4) -0.004(3) 0.002(3) -0.001(3) N2 0.043(4) 0.031(4) 0.072(5) -0.007(4) 0.000(4) -0.004(3) N3 0.028(3) 0.029(3) 0.034(4) 0.002(3) 0.003(3) 0.003(3) N4 0.034(4) 0.035(3) 0.039(4) -0.001(3) 0.001(3) -0.002(3) N5 0.033(3) 0.033(3) 0.031(4) -0.002(3) 0.002(3) 0.003(3) N6 0.039(4) 0.043(4) 0.036(4) -0.003(3) -0.001(3) 0.007(3) C1 0.031(4) 0.028(4) 0.022(4) -0.003(3) 0.001(3) -0.005(3) C2 0.037(4) 0.039(4) 0.041(5) 0.000(4) 0.000(4) -0.008(3) C3 0.034(4) 0.053(5) 0.042(5) 0.000(4) 0.000(4) -0.001(4) C4 0.032(4) 0.050(5) 0.033(5) -0.004(4) 0.001(4) -0.015(4) C5 0.048(5) 0.031(4) 0.041(5) -0.005(4) 0.003(4) -0.010(4) C6 0.037(4) 0.031(4) 0.036(5) -0.003(3) -0.002(4) -0.005(3) C7 0.042(5) 0.035(5) 0.078(7) 0.000(5) -0.006(5) 0.002(4) C8 0.049(6) 0.058(6) 0.098(9) -0.032(6) -0.017(6) 0.011(5) C9 0.059(7) 0.059(6) 0.122(10) -0.030(7) -0.001(7) 0.020(5) C10 0.045(5) 0.058(6) 0.082(8) 0.001(6) -0.007(5) 0.008(5) C11 0.047(5) 0.054(6) 0.061(6) 0.007(5) -0.001(5) -0.004(4) C12 0.051(5) 0.027(4) 0.057(6) 0.004(4) 0.017(4) -0.002(4) C13 0.034(4) 0.033(4) 0.030(4) -0.004(3) 0.004(3) -0.004(3) C14 0.033(4) 0.042(4) 0.035(5) 0.000(4) 0.007(4) 0.007(3) C15 0.040(5) 0.066(6) 0.031(5) 0.000(4) 0.001(4) 0.006(4) C16 0.040(5) 0.058(5) 0.035(5) -0.008(4) 0.002(4) 0.012(4) C17 0.037(5) 0.044(5) 0.043(5) -0.003(4) -0.005(4) 0.003(4) C18 0.037(4) 0.029(4) 0.033(4) 0.000(3) 0.006(3) -0.007(3) C20 0.022(4) 0.043(4) 0.032(4) 0.007(4) -0.001(3) -0.008(3) C21 0.047(5) 0.055(5) 0.045(5) 0.002(4) 0.003(4) 0.006(4) C22 0.042(5) 0.058(6) 0.052(6) 0.007(5) -0.004(4) 0.008(4) C23 0.046(5) 0.061(6) 0.037(5) 0.000(4) -0.003(4) 0.002(4) C24 0.049(5) 0.055(5) 0.044(5) -0.013(4) 0.000(4) 0.001(4) C25 0.032(4) 0.046(5) 0.042(5) 0.004(4) -0.005(4) -0.001(3) C26 0.035(4) 0.031(4) 0.032(4) -0.001(3) 0.003(3) -0.002(3) C27 0.032(4) 0.045(5) 0.029(4) 0.001(4) 0.000(3) 0.000(3) C28 0.045(5) 0.055(5) 0.030(5) 0.003(4) 0.000(4) 0.005(4) C29 0.037(4) 0.052(5) 0.038(5) 0.012(4) -0.006(4) 0.007(4) C30 0.043(5) 0.044(5) 0.037(5) -0.001(4) -0.002(4) 0.007(4) C31 0.028(4) 0.032(4) 0.030(4) 0.007(3) -0.005(3) 0.005(3) C32 0.041(5) 0.065(6) 0.033(5) -0.018(4) 0.000(4) 0.004(4) C33 0.067(6) 0.064(6) 0.068(7) -0.033(6) -0.018(5) 0.021(5) C34 0.073(8) 0.108(9) 0.088(9) -0.066(8) -0.037(7) 0.040(7) C35 0.044(6) 0.135(11) 0.042(6) -0.021(7) -0.002(5) 0.014(6) C36 0.051(6) 0.108(8) 0.031(5) 0.007(6) -0.005(4) -0.029(6) C37 0.045(5) 0.064(6) 0.040(5) -0.001(5) 0.001(4) -0.017(4) C38 0.051(5) 0.031(4) 0.026(4) 0.003(3) 0.005(4) -0.002(3) C39 0.055(5) 0.046(5) 0.048(6) -0.001(4) 0.010(4) 0.005(4) C40 0.079(7) 0.066(6) 0.063(7) 0.008(5) 0.035(6) 0.003(5) C41 0.096(8) 0.058(6) 0.075(8) 0.009(6) 0.031(7) -0.009(6) C42 0.069(7) 0.050(5) 0.072(7) 0.004(5) 0.028(6) -0.009(5) C43 0.052(5) 0.036(4) 0.039(5) -0.001(4) 0.010(4) -0.001(4) C44 0.037(4) 0.025(4) 0.024(4) -0.003(3) -0.007(3) -0.004(3) C45 0.060(6) 0.075(6) 0.025(5) 0.004(4) 0.003(4) 0.006(5) C46 0.093(8) 0.093(8) 0.030(5) 0.006(5) 0.005(5) 0.031(6) C47 0.108(9) 0.089(8) 0.026(5) -0.005(5) -0.017(6) 0.032(7) C48 0.073(7) 0.087(8) 0.053(7) -0.005(6) -0.034(6) 0.017(6) C49 0.048(5) 0.067(6) 0.037(5) -0.005(4) -0.009(4) 0.002(4) C50 0.047(5) 0.061(6) 0.082(8) 0.008(6) -0.006(5) -0.019(5) C51 0.054(8) 0.179(15) 0.22(2) -0.101(15) 0.008(10) 0.047(9) C52 0.148(15) 0.205(18) 0.091(12) -0.037(12) 0.014(11) 0.080(13) C53 0.054(6) 0.088(8) 0.077(8) 0.022(7) 0.015(6) -0.011(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Sn1 O8 2.042(4) 7_556 ? Sn1 O2 2.069(4) . ? Sn1 O7 2.090(4) . ? Sn1 O4 2.121(4) . ? Sn1 C26 2.127(7) . ? Sn1 O10 2.150(4) 7_556 ? Sn2 O1 2.062(5) . ? Sn2 O10 2.088(4) . ? Sn2 O9 2.092(4) . ? Sn2 O8 2.095(4) . ? Sn2 O5 2.134(5) 7_556 ? Sn2 C1 2.138(6) . ? Sn3 O8 2.043(4) . ? Sn3 O3 2.058(4) 7_556 ? Sn3 O7 2.080(4) . ? Sn3 O6 2.099(4) 7_556 ? Sn3 C13 2.142(7) . ? Sn3 O9 2.149(4) . ? P1 O3 1.528(5) . ? P1 O1 1.529(5) . ? P1 O2 1.529(5) . ? P1 C44 1.794(7) . ? P2 O6 1.535(5) . ? P2 O5 1.541(5) . ? P2 O4 1.549(5) . ? P2 C38 1.797(7) . ? O3 Sn3 2.058(4) 7_556 ? O5 Sn2 2.134(5) 7_556 ? O6 Sn3 2.099(4) 7_556 ? O8 Sn1 2.042(4) 7_556 ? O10 Sn1 2.150(4) 7_556 ? O11 C53 1.410(11) . ? O11 C50 1.425(10) . ? N1 N2 1.266(8) . ? N1 C6 1.425(9) . ? N2 C7 1.434(10) . ? N3 N4 1.240(7) . ? N3 C18 1.425(9) . ? N4 C20 1.430(9) . ? N5 N6 1.254(8) . ? N5 C31 1.417(9) . ? N6 C32 1.425(10) . ? C1 C2 1.385(10) . ? C1 C6 1.405(9) . ? C2 C3 1.378(10) . ? C3 C4 1.381(10) . ? C4 C5 1.333(10) . ? C5 C6 1.414(10) . ? C7 C8 1.335(11) . ? C7 C12 1.393(11) . ? C8 C9 1.362(12) . ? C9 C10 1.380(13) . ? C10 C11 1.366(11) . ? C11 C12 1.369(11) . ? C13 C14 1.394(10) . ? C13 C18 1.394(10) . ? C14 C15 1.353(10) . ? C15 C16 1.376(10) . ? C16 C17 1.362(11) . ? C17 C18 1.369(10) . ? C20 C21 1.380(10) . ? C20 C25 1.396(10) . ? C21 C22 1.387(11) . ? C22 C23 1.369(11) . ? C23 C24 1.389(11) . ? C24 C25 1.365(11) . ? C26 C27 1.390(10) . ? C26 C31 1.400(9) . ? C27 C28 1.357(10) . ? C28 C29 1.390(10) . ? C29 C30 1.369(10) . ? C30 C31 1.404(9) . ? C32 C33 1.355(11) . ? C32 C37 1.409(11) . ? C33 C34 1.424(14) . ? C34 C35 1.353(15) . ? C35 C36 1.384(13) . ? C36 C37 1.352(11) . ? C38 C39 1.495(10) . ? C38 C43 1.535(9) . ? C39 C40 1.527(11) . ? C40 C41 1.541(12) . ? C41 C42 1.442(12) . ? C42 C43 1.515(11) . ? C44 C49 1.482(10) . ? C44 C45 1.523(10) . ? C45 C46 1.517(11) . ? C46 C47 1.479(13) . ? C47 C48 1.491(14) . ? C48 C49 1.519(11) . ? C50 C51 1.479(15) . ? C51 C52 1.435(19) . ? C52 C53 1.440(16) . ? 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 O8 Sn1 O2 90.80(17) 7_556 . ? O8 Sn1 O7 92.66(17) 7_556 . ? O2 Sn1 O7 88.03(17) . . ? O8 Sn1 O4 88.35(17) 7_556 . ? O2 Sn1 O4 89.24(17) . . ? O7 Sn1 O4 177.10(17) . . ? O8 Sn1 C26 173.1(2) 7_556 . ? O2 Sn1 C26 93.4(2) . . ? O7 Sn1 C26 92.9(2) . . ? O4 Sn1 C26 86.3(2) . . ? O8 Sn1 O10 73.12(17) 7_556 7_556 ? O2 Sn1 O10 163.87(17) . 7_556 ? O7 Sn1 O10 91.43(17) . 7_556 ? O4 Sn1 O10 91.46(17) . 7_556 ? C26 Sn1 O10 102.7(2) . 7_556 ? O1 Sn2 O10 95.52(18) . . ? O1 Sn2 O9 90.07(18) . . ? O10 Sn2 O9 148.26(17) . . ? O1 Sn2 O8 90.23(17) . . ? O10 Sn2 O8 73.34(17) . . ? O9 Sn2 O8 75.42(16) . . ? O1 Sn2 O5 174.94(18) . 7_556 ? O10 Sn2 O5 88.82(18) . 7_556 ? O9 Sn2 O5 84.87(17) . 7_556 ? O8 Sn2 O5 88.52(17) . 7_556 ? O1 Sn2 C1 90.7(2) . . ? O10 Sn2 C1 107.3(2) . . ? O9 Sn2 C1 103.8(2) . . ? O8 Sn2 C1 178.8(2) . . ? O5 Sn2 C1 90.5(2) 7_556 . ? O8 Sn3 O3 91.34(17) . 7_556 ? O8 Sn3 O7 92.11(17) . . ? O3 Sn3 O7 88.98(17) 7_556 . ? O8 Sn3 O6 86.09(18) . 7_556 ? O3 Sn3 O6 92.46(17) 7_556 7_556 ? O7 Sn3 O6 177.72(17) . 7_556 ? O8 Sn3 C13 172.0(2) . . ? O3 Sn3 C13 93.4(2) 7_556 . ? O7 Sn3 C13 94.4(2) . . ? O6 Sn3 C13 87.3(2) 7_556 . ? O8 Sn3 O9 75.27(17) . . ? O3 Sn3 O9 165.74(18) 7_556 . ? O7 Sn3 O9 86.66(17) . . ? O6 Sn3 O9 91.52(17) 7_556 . ? C13 Sn3 O9 100.5(2) . . ? O3 P1 O1 112.2(3) . . ? O3 P1 O2 112.6(2) . . ? O1 P1 O2 112.1(3) . . ? O3 P1 C44 106.6(3) . . ? O1 P1 C44 105.4(3) . . ? O2 P1 C44 107.4(3) . . ? O6 P2 O5 111.0(3) . . ? O6 P2 O4 111.7(3) . . ? O5 P2 O4 110.3(3) . . ? O6 P2 C38 106.8(3) . . ? O5 P2 C38 108.7(3) . . ? O4 P2 C38 108.2(3) . . ? P1 O1 Sn2 147.2(3) . . ? P1 O2 Sn1 138.0(3) . . ? P1 O3 Sn3 137.7(3) . 7_556 ? P2 O4 Sn1 121.2(2) . . ? P2 O5 Sn2 120.6(2) . 7_556 ? P2 O6 Sn3 124.0(3) . 7_556 ? Sn3 O7 Sn1 147.2(2) . . ? Sn1 O8 Sn3 133.2(2) 7_556 . ? Sn1 O8 Sn2 106.41(19) 7_556 . ? Sn3 O8 Sn2 105.14(18) . . ? Sn2 O9 Sn3 101.56(18) . . ? Sn2 O10 Sn1 102.81(18) . 7_556 ? C53 O11 C50 108.6(7) . . ? N2 N1 C6 115.8(6) . . ? N1 N2 C7 113.0(6) . . ? N4 N3 C18 113.7(6) . . ? N3 N4 C20 115.2(6) . . ? N6 N5 C31 115.1(6) . . ? N5 N6 C32 115.1(6) . . ? C2 C1 C6 117.9(6) . . ? C2 C1 Sn2 120.5(5) . . ? C6 C1 Sn2 121.5(5) . . ? C3 C2 C1 120.1(7) . . ? C2 C3 C4 121.6(7) . . ? C5 C4 C3 119.8(7) . . ? C4 C5 C6 120.3(7) . . ? C1 C6 C5 120.3(7) . . ? C1 C6 N1 115.2(6) . . ? C5 C6 N1 124.5(7) . . ? C8 C7 C12 120.1(8) . . ? C8 C7 N2 117.9(8) . . ? C12 C7 N2 121.9(7) . . ? C7 C8 C9 122.2(9) . . ? C8 C9 C10 117.7(9) . . ? C11 C10 C9 121.3(9) . . ? C10 C11 C12 119.6(9) . . ? C11 C12 C7 118.9(8) . . ? C14 C13 C18 116.4(7) . . ? C14 C13 Sn3 118.1(5) . . ? C18 C13 Sn3 125.6(5) . . ? C15 C14 C13 122.0(7) . . ? C14 C15 C16 120.3(8) . . ? C17 C16 C15 119.4(8) . . ? C16 C17 C18 120.4(7) . . ? C17 C18 C13 121.4(7) . . ? C17 C18 N3 123.1(7) . . ? C13 C18 N3 115.5(6) . . ? C21 C20 C25 120.9(7) . . ? C21 C20 N4 114.9(7) . . ? C25 C20 N4 124.0(6) . . ? C20 C21 C22 120.8(8) . . ? C23 C22 C21 118.6(8) . . ? C22 C23 C24 120.0(8) . . ? C25 C24 C23 122.4(8) . . ? C24 C25 C20 117.2(7) . . ? C27 C26 C31 118.0(7) . . ? C27 C26 Sn1 118.4(5) . . ? C31 C26 Sn1 123.5(5) . . ? C28 C27 C26 120.5(7) . . ? C27 C28 C29 121.6(7) . . ? C30 C29 C28 119.9(7) . . ? C29 C30 C31 118.7(7) . . ? C26 C31 C30 121.3(7) . . ? C26 C31 N5 116.9(6) . . ? C30 C31 N5 121.8(6) . . ? C33 C32 C37 120.7(8) . . ? C33 C32 N6 115.8(8) . . ? C37 C32 N6 123.5(7) . . ? C32 C33 C34 118.9(10) . . ? C35 C34 C33 119.3(10) . . ? C34 C35 C36 121.2(9) . . ? C37 C36 C35 120.1(10) . . ? C36 C37 C32 119.5(9) . . ? C39 C38 C43 111.2(6) . . ? C39 C38 P2 113.6(5) . . ? C43 C38 P2 112.7(5) . . ? C38 C39 C40 111.5(7) . . ? C39 C40 C41 109.9(8) . . ? C42 C41 C40 112.1(8) . . ? C41 C42 C43 112.1(8) . . ? C42 C43 C38 111.9(7) . . ? C49 C44 C45 108.9(6) . . ? C49 C44 P1 113.6(5) . . ? C45 C44 P1 111.7(5) . . ? C46 C45 C44 112.5(8) . . ? C47 C46 C45 110.2(8) . . ? C46 C47 C48 111.0(8) . . ? C47 C48 C49 112.6(8) . . ? C44 C49 C48 111.5(7) . . ? O11 C50 C51 106.1(10) . . ? C52 C51 C50 107.6(11) . . ? C51 C52 C53 105.7(12) . . ? O11 C53 C52 108.7(10) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.100 _refine_diff_density_min -0.619 _refine_diff_density_rms 0.150 _database_code_depnum_ccdc_archive 'CCDC 968922' ####################################################################### # # 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_3 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C96 H70 N16 O32 P4 Sn6, 2(C4 H8 O)' _chemical_formula_sum 'C104 H86 N16 O34 P4 Sn6 ' _chemical_formula_weight 2940.03 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' P P 0.1023 0.0942 '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 triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.185(5) _cell_length_b 14.386(5) _cell_length_c 16.439(5) _cell_angle_alpha 105.986(5) _cell_angle_beta 100.340(5) _cell_angle_gamma 94.817(5) _cell_volume 2919.4(17) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.672 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1770 _exptl_absorpt_coefficient_mu 1.403 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.777 _exptl_absorpt_correction_T_max 0.799 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15833 _diffrn_reflns_av_R_equivalents 0.0583 _diffrn_reflns_av_sigmaI/netI 0.1388 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.25 _diffrn_reflns_theta_max 25.50 _reflns_number_total 10694 _reflns_number_gt 6259 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1107P)^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 10694 _refine_ls_number_parameters 739 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1369 _refine_ls_R_factor_gt 0.0795 _refine_ls_wR_factor_ref 0.2162 _refine_ls_wR_factor_gt 0.1834 _refine_ls_goodness_of_fit_ref 0.966 _refine_ls_restrained_S_all 0.966 _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 Sn1 Sn 0.95842(7) 0.30860(5) 0.50302(5) 0.0272(2) Uani 1 1 d . . . Sn3 Sn 1.03650(6) 0.42099(5) 0.33579(5) 0.0268(2) Uani 1 1 d . . . Sn2 Sn 0.79492(7) 0.35853(6) 0.35019(5) 0.0280(2) Uani 1 1 d . . . P2 P 0.9435(3) 0.1986(2) 0.3040(2) 0.0295(7) Uani 1 1 d . . . P1 P 1.2003(3) 0.4101(2) 0.5110(2) 0.0286(7) Uani 1 1 d . . . O8 O 1.3033(6) 0.3607(5) 0.5220(5) 0.0329(19) Uani 1 1 d . . . O4 O 0.9459(7) 0.0901(6) 0.2463(5) 0.036(2) Uani 1 1 d . . . O3 O 0.8340(7) 0.2251(5) 0.2822(5) 0.036(2) Uani 1 1 d . . . O6 O 1.1718(6) 0.4126(5) 0.4186(5) 0.0289(19) Uani 1 1 d . . . O1 O 1.0234(6) 0.2680(5) 0.2840(5) 0.0295(19) Uani 1 1 d . . . O2 O 0.9716(6) 0.1927(5) 0.3952(5) 0.0306(19) Uani 1 1 d . . . O9 O 0.9465(5) 0.3930(5) 0.4203(5) 0.0232(17) Uani 1 1 d . . . O7 O 1.2358(6) 0.5084(5) 0.5760(5) 0.0309(19) Uani 1 1 d . . . O12 O 1.0563(6) 0.5726(5) 0.3981(5) 0.0277(18) Uani 1 1 d . . . C1 C 0.9569(9) 0.2102(8) 0.5791(7) 0.029(3) Uani 1 1 d . . . O11 O 0.8807(5) 0.4203(5) 0.2794(5) 0.0242(17) Uani 1 1 d . . . N3 N 0.9735(8) 0.5436(7) 0.1996(6) 0.033(2) Uani 1 1 d . . . O5 O 1.1175(6) 0.3480(5) 0.5351(5) 0.0301(19) Uani 1 1 d . . . N2 N 0.7404(8) 0.2713(7) 0.6716(6) 0.034(2) Uani 1 1 d . . . O13 O 0.6784(8) 0.1203(6) 0.4054(6) 0.052(3) Uani 1 1 d . . . N5 N 0.6711(8) 0.2987(7) 0.1530(6) 0.036(2) Uani 1 1 d . . . C3 C 1.0190(10) 0.0715(8) 0.6183(8) 0.036(3) Uani 1 1 d . . . H3 H 1.0623 0.0233 0.6131 0.043 Uiso 1 1 calc R . . O14 O 1.3476(9) -0.0381(8) 0.2734(8) 0.069(3) Uani 1 1 d . . . C42 C 1.2477(10) 0.2104(9) 0.4042(8) 0.035(3) Uani 1 1 d . . . H42 H 1.1876 0.2331 0.3831 0.042 Uiso 1 1 calc R . . O10 O 0.7974(7) 0.2956(5) 0.4511(5) 0.037(2) Uani 1 1 d . . . N4 N 0.9541(8) 0.6047(7) 0.1612(7) 0.035(2) Uani 1 1 d . . . C12 C 0.6665(10) 0.4001(9) 0.6187(8) 0.036(3) Uani 1 1 d . . . H12 H 0.7103 0.3973 0.5799 0.043 Uiso 1 1 calc R . . C6 C 0.8879(8) 0.2127(8) 0.6362(7) 0.025(3) Uani 1 1 d . . . C25 C 1.1069(9) 0.4396(8) 0.2318(7) 0.030(3) Uani 1 1 d . . . C5 C 0.8819(10) 0.1437(9) 0.6809(8) 0.035(3) Uani 1 1 d . . . H5 H 0.8332 0.1434 0.7155 0.042 Uiso 1 1 calc R . . N6 N 0.6426(10) 0.2600(9) 0.0732(7) 0.055(3) Uani 1 1 d . . . O17 O 0.8191(10) -0.1553(9) -0.1415(7) 0.085(4) Uani 1 1 d . . . C46 C 0.8669(11) -0.0259(11) -0.0174(9) 0.050(4) Uani 1 1 d . . . O15 O 1.4471(9) -0.0448(8) 0.3898(8) 0.070(3) Uani 1 1 d . . . C18 C 0.5967(10) 0.2915(9) 0.2037(9) 0.038(3) Uani 1 1 d . . . C14 C 0.5664(9) 0.3115(9) 0.3458(9) 0.036(3) Uani 1 1 d . . . H14 H 0.5910 0.3268 0.4052 0.044 Uiso 1 1 calc R . . C50 C 0.6960(13) -0.0474(10) 0.3731(10) 0.059(4) Uani 1 1 d . . . H50A H 0.7490 -0.0890 0.3801 0.071 Uiso 1 1 calc R . . H50B H 0.6286 -0.0819 0.3708 0.071 Uiso 1 1 calc R . . C15 C 0.4618(13) 0.2809(10) 0.3103(10) 0.057(4) Uani 1 1 d . . . H15 H 0.4150 0.2786 0.3461 0.068 Uiso 1 1 calc R . . C19 C 0.7216(11) 0.2639(9) 0.0238(9) 0.039(3) Uani 1 1 d . . . C34 C 0.6897(12) 0.7314(10) 0.2057(10) 0.050(4) Uani 1 1 d . . . H34 H 0.6287 0.7577 0.2127 0.060 Uiso 1 1 calc R . . C8 C 0.6078(14) 0.3463(11) 0.7293(9) 0.063(5) Uani 1 1 d . . . H8 H 0.6118 0.3058 0.7648 0.075 Uiso 1 1 calc R . . C31 C 0.8627(10) 0.6486(9) 0.1817(9) 0.040(3) Uani 1 1 d . . . C29 C 1.1129(11) 0.5065(10) 0.1140(8) 0.043(3) Uani 1 1 d . . . H29 H 1.0853 0.5421 0.0780 0.051 Uiso 1 1 calc R . . C26 C 1.1875(9) 0.3958(9) 0.2154(7) 0.035(3) Uani 1 1 d . . . H26 H 1.2127 0.3566 0.2487 0.041 Uiso 1 1 calc R . . C41 C 1.2696(10) 0.1202(9) 0.3606(9) 0.038(3) Uani 1 1 d . . . H41 H 1.2260 0.0815 0.3094 0.045 Uiso 1 1 calc R . . C30 C 1.0658(10) 0.4990(9) 0.1805(7) 0.033(3) Uani 1 1 d . . . C9 C 0.5369(11) 0.4098(11) 0.7342(9) 0.051(4) Uani 1 1 d . . . H9 H 0.4942 0.4136 0.7740 0.061 Uiso 1 1 calc R . . C37 C 1.3142(10) 0.2658(9) 0.4780(8) 0.032(3) Uani 1 1 d . . . C17 C 0.4952(11) 0.2594(10) 0.1672(9) 0.050(4) Uani 1 1 d . . . H17A H 0.4722 0.2419 0.1074 0.060 Uiso 1 1 calc R . . C39 C 1.4286(13) 0.1424(10) 0.4704(9) 0.051(4) Uani 1 1 d . . . H39 H 1.4894 0.1201 0.4909 0.061 Uiso 1 1 calc R . . C36 C 0.8235(10) 0.6496(9) 0.2546(8) 0.040(3) Uani 1 1 d . . . H36 H 0.8575 0.6230 0.2956 0.048 Uiso 1 1 calc R . . C32 C 0.8187(13) 0.6940(11) 0.1229(11) 0.062(4) Uani 1 1 d . . . H32 H 0.8473 0.6968 0.0757 0.074 Uiso 1 1 calc R . . C49 C 0.7204(12) 0.0486(11) 0.4444(11) 0.064(5) Uani 1 1 d . . . H49A H 0.6881 0.0445 0.4921 0.077 Uiso 1 1 calc R . . H49B H 0.7951 0.0661 0.4660 0.077 Uiso 1 1 calc R . . C11 C 0.5910(9) 0.4655(10) 0.6239(9) 0.043(3) Uani 1 1 d . . . H11 H 0.5848 0.5060 0.5884 0.051 Uiso 1 1 calc R . . C43 C 0.9181(12) 0.0546(10) 0.1595(9) 0.047(4) Uani 1 1 d . . . C45 C 0.8675(12) -0.0853(11) 0.0366(10) 0.059(4) Uani 1 1 d . . . H45 H 0.8480 -0.1524 0.0136 0.071 Uiso 1 1 calc R . . O16 O 0.8441(11) -0.0123(10) -0.1561(8) 0.082(4) Uani 1 1 d . . . C27 C 1.2372(11) 0.4065(10) 0.1484(8) 0.048(4) Uani 1 1 d . . . H27 H 1.2948 0.3761 0.1370 0.058 Uiso 1 1 calc R . . C21 C 0.7577(17) 0.2294(12) -0.1164(11) 0.073(5) Uani 1 1 d . . . H21 H 0.7344 0.2039 -0.1760 0.087 Uiso 1 1 calc R . . C35 C 0.7352(12) 0.6897(10) 0.2662(10) 0.051(4) Uani 1 1 d . . . H35 H 0.7065 0.6888 0.3138 0.061 Uiso 1 1 calc R . . C38 C 1.4008(11) 0.2348(10) 0.5142(9) 0.044(4) Uani 1 1 d . . . H38 H 1.4418 0.2730 0.5669 0.052 Uiso 1 1 calc R . . C13 C 0.6341(9) 0.3193(8) 0.2924(7) 0.028(3) Uani 1 1 d . . . C16 C 0.4260(12) 0.2531(10) 0.2201(12) 0.062(4) Uani 1 1 d . . . H16 H 0.3559 0.2305 0.1959 0.074 Uiso 1 1 calc R . . C10 C 0.5281(12) 0.4680(10) 0.6814(9) 0.052(4) Uani 1 1 d . . . H10 H 0.4782 0.5101 0.6846 0.063 Uiso 1 1 calc R . . C40 C 1.3592(15) 0.0899(9) 0.3965(9) 0.058(5) Uani 1 1 d . . . C47 C 0.8878(14) 0.0694(12) 0.0161(10) 0.070(5) Uani 1 1 d . . . H47 H 0.8860 0.1088 -0.0204 0.084 Uiso 1 1 calc R . . C33 C 0.7283(14) 0.7360(11) 0.1380(11) 0.064(5) Uani 1 1 d . . . H33 H 0.6958 0.7671 0.1000 0.077 Uiso 1 1 calc R . . C20 C 0.6892(12) 0.2300(11) -0.0626(9) 0.052(4) Uani 1 1 d . . . H20 H 0.6191 0.2066 -0.0864 0.063 Uiso 1 1 calc R . . C7 C 0.6739(10) 0.3406(9) 0.6726(8) 0.034(3) Uani 1 1 d . . . C28 C 1.1939(12) 0.4660(10) 0.0999(9) 0.049(4) Uani 1 1 d . . . H28 H 1.2251 0.4764 0.0561 0.059 Uiso 1 1 calc R . . C2 C 1.0227(10) 0.1408(8) 0.5714(7) 0.034(3) Uani 1 1 d . . . H2 H 1.0699 0.1391 0.5354 0.041 Uiso 1 1 calc R . . N8 N 0.8395(11) -0.0650(11) -0.1091(9) 0.070(4) Uani 1 1 d . . . C23 C 0.8943(14) 0.3071(11) 0.0055(9) 0.066(5) Uani 1 1 d . . . H23 H 0.9643 0.3308 0.0293 0.079 Uiso 1 1 calc R . . N7 N 1.3857(10) -0.0062(8) 0.3498(9) 0.051(3) Uani 1 1 d . . . C4 C 0.9471(12) 0.0789(9) 0.6729(9) 0.047(4) Uani 1 1 d . . . H4 H 0.9456 0.0352 0.7053 0.057 Uiso 1 1 calc R . . C44 C 0.8964(12) -0.0442(11) 0.1213(11) 0.062(4) Uani 1 1 d . . . H44 H 0.9022 -0.0848 0.1568 0.074 Uiso 1 1 calc R . . C24 C 0.8171(14) 0.3120(12) 0.0598(9) 0.067(5) Uani 1 1 d . . . H24 H 0.8343 0.3479 0.1181 0.081 Uiso 1 1 calc R . . C52 C 0.6425(16) 0.0746(11) 0.3118(10) 0.080(6) Uani 1 1 d . . . H52A H 0.6636 0.1174 0.2795 0.096 Uiso 1 1 calc R . . H52B H 0.5674 0.0574 0.2961 0.096 Uiso 1 1 calc R . . C22 C 0.8587(15) 0.2657(11) -0.0828(10) 0.067(5) Uani 1 1 d . . . H22 H 0.9052 0.2630 -0.1194 0.080 Uiso 1 1 calc R . . C51 C 0.6960(15) -0.0145(11) 0.2961(12) 0.079(6) Uani 1 1 d . . . H51A H 0.6584 -0.0646 0.2443 0.094 Uiso 1 1 calc R . . H51B H 0.7666 0.0012 0.2898 0.094 Uiso 1 1 calc R . . C48 C 0.9128(13) 0.1127(12) 0.1060(9) 0.065(5) Uani 1 1 d . . . H48 H 0.9257 0.1803 0.1290 0.078 Uiso 1 1 calc R . . N1 N 0.8190(8) 0.2856(6) 0.6411(6) 0.030(2) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Sn1 0.0350(5) 0.0255(4) 0.0280(4) 0.0142(3) 0.0167(4) -0.0005(3) Sn3 0.0318(5) 0.0268(4) 0.0282(4) 0.0132(3) 0.0170(4) -0.0008(3) Sn2 0.0327(5) 0.0269(4) 0.0299(4) 0.0136(3) 0.0155(4) -0.0012(3) P2 0.036(2) 0.0275(15) 0.0326(17) 0.0144(13) 0.0194(15) 0.0024(13) P1 0.0296(19) 0.0290(15) 0.0293(17) 0.0102(13) 0.0114(15) -0.0009(13) O8 0.038(5) 0.030(4) 0.033(5) 0.009(4) 0.013(4) 0.002(4) O4 0.053(6) 0.030(4) 0.029(4) 0.011(4) 0.019(4) -0.003(4) O3 0.051(6) 0.030(4) 0.029(4) 0.014(4) 0.017(4) -0.011(4) O6 0.036(5) 0.028(4) 0.032(4) 0.019(3) 0.015(4) 0.000(4) O1 0.038(5) 0.024(4) 0.033(4) 0.011(3) 0.023(4) 0.002(3) O2 0.039(5) 0.029(4) 0.029(4) 0.014(3) 0.013(4) 0.000(4) O9 0.015(4) 0.028(4) 0.035(4) 0.017(3) 0.013(4) 0.005(3) O7 0.024(5) 0.033(4) 0.039(5) 0.012(4) 0.010(4) 0.007(3) O12 0.042(5) 0.023(4) 0.025(4) 0.015(3) 0.017(4) -0.005(3) C1 0.029(7) 0.037(6) 0.030(6) 0.023(5) 0.012(6) 0.003(5) O11 0.015(4) 0.031(4) 0.039(4) 0.017(3) 0.021(4) 0.010(3) N3 0.035(6) 0.033(5) 0.041(6) 0.018(5) 0.021(5) 0.006(5) O5 0.023(5) 0.033(4) 0.048(5) 0.026(4) 0.019(4) 0.005(3) N2 0.041(7) 0.042(6) 0.029(5) 0.023(5) 0.014(5) -0.002(5) O13 0.063(7) 0.036(5) 0.064(7) 0.024(5) 0.018(6) -0.003(5) N5 0.042(7) 0.041(6) 0.026(6) 0.018(5) 0.003(5) 0.000(5) C3 0.036(8) 0.033(7) 0.051(8) 0.024(6) 0.020(7) 0.011(6) O14 0.067(8) 0.064(7) 0.065(8) 0.000(6) 0.015(7) 0.012(6) C42 0.024(7) 0.047(7) 0.041(8) 0.026(6) 0.009(6) 0.003(6) O10 0.056(6) 0.027(4) 0.034(5) 0.018(4) 0.014(4) -0.003(4) N4 0.028(6) 0.043(6) 0.051(7) 0.033(5) 0.021(5) 0.013(5) C12 0.033(8) 0.048(8) 0.034(7) 0.020(6) 0.011(6) 0.004(6) C6 0.014(6) 0.026(6) 0.040(7) 0.012(5) 0.015(5) 0.005(5) C25 0.031(7) 0.031(6) 0.024(6) -0.003(5) 0.013(6) 0.008(5) C5 0.035(8) 0.040(7) 0.043(7) 0.022(6) 0.023(6) 0.009(6) N6 0.066(9) 0.071(8) 0.024(6) 0.016(6) 0.008(6) -0.014(7) O17 0.097(10) 0.069(8) 0.066(8) -0.014(6) 0.027(7) -0.019(7) C46 0.041(9) 0.052(9) 0.051(9) 0.000(7) 0.020(8) 0.012(7) O15 0.072(9) 0.057(7) 0.092(9) 0.037(7) 0.019(7) 0.019(6) C18 0.032(8) 0.035(7) 0.047(8) 0.011(6) 0.012(7) -0.005(6) C14 0.014(7) 0.046(7) 0.058(9) 0.029(7) 0.012(6) 0.000(5) C50 0.060(11) 0.036(8) 0.085(12) 0.015(8) 0.024(9) 0.014(7) C15 0.078(12) 0.044(8) 0.050(9) 0.022(7) 0.015(9) -0.017(8) C19 0.040(9) 0.040(7) 0.043(8) 0.010(6) 0.019(7) 0.018(6) C34 0.051(10) 0.052(9) 0.068(10) 0.035(8) 0.031(8) 0.015(7) C8 0.098(14) 0.054(9) 0.033(8) 0.018(7) 0.015(9) -0.024(9) C31 0.038(8) 0.042(7) 0.055(8) 0.031(7) 0.021(7) 0.012(6) C29 0.051(9) 0.048(8) 0.035(7) 0.017(6) 0.023(7) -0.007(7) C26 0.032(8) 0.040(7) 0.027(6) 0.005(5) 0.006(6) -0.005(6) C41 0.037(8) 0.028(6) 0.051(8) 0.013(6) 0.013(7) 0.011(6) C30 0.037(8) 0.037(7) 0.025(6) 0.011(5) 0.008(6) -0.008(6) C9 0.043(9) 0.063(10) 0.052(9) 0.014(8) 0.027(8) 0.008(7) C37 0.031(7) 0.051(8) 0.031(7) 0.023(6) 0.024(6) 0.017(6) C17 0.045(10) 0.062(9) 0.045(9) 0.022(7) 0.005(8) 0.004(7) C39 0.075(11) 0.037(8) 0.046(9) 0.024(7) 0.014(8) -0.002(7) C36 0.045(9) 0.045(8) 0.044(8) 0.028(6) 0.023(7) 0.004(6) C32 0.065(12) 0.068(10) 0.070(11) 0.038(9) 0.033(9) 0.002(9) C49 0.046(10) 0.055(10) 0.092(13) 0.019(9) 0.018(9) 0.006(8) C11 0.023(7) 0.052(8) 0.065(9) 0.027(7) 0.022(7) 0.016(6) C43 0.062(10) 0.040(8) 0.046(8) 0.019(7) 0.027(8) -0.005(7) C45 0.059(11) 0.048(9) 0.068(11) 0.000(8) 0.034(9) 0.009(8) O16 0.098(11) 0.089(10) 0.067(8) 0.022(7) 0.022(8) 0.043(8) C27 0.055(10) 0.052(8) 0.042(8) 0.010(7) 0.030(7) 0.005(7) C21 0.125(18) 0.053(10) 0.055(10) 0.029(8) 0.039(11) 0.007(11) C35 0.055(10) 0.045(8) 0.055(9) 0.015(7) 0.019(8) -0.005(7) C38 0.035(8) 0.059(9) 0.054(9) 0.024(7) 0.028(7) 0.036(7) C13 0.022(7) 0.027(6) 0.033(7) 0.010(5) 0.003(5) 0.000(5) C16 0.046(10) 0.048(9) 0.097(13) 0.028(9) 0.025(10) -0.015(7) C10 0.062(11) 0.042(8) 0.057(9) 0.017(7) 0.019(8) 0.008(7) C40 0.114(15) 0.024(7) 0.040(8) 0.014(6) 0.030(9) -0.007(8) C47 0.101(15) 0.073(12) 0.041(9) 0.020(8) 0.032(10) 0.001(10) C33 0.070(12) 0.054(10) 0.074(12) 0.039(9) 0.003(10) 0.003(8) C20 0.049(10) 0.069(10) 0.050(9) 0.020(8) 0.023(8) 0.037(8) C7 0.030(7) 0.037(7) 0.045(8) 0.018(6) 0.021(6) 0.014(6) C28 0.055(10) 0.061(9) 0.041(8) 0.025(7) 0.023(8) -0.006(7) C2 0.050(9) 0.029(6) 0.026(6) 0.014(5) 0.009(6) 0.001(6) N8 0.059(10) 0.070(10) 0.060(10) -0.011(8) 0.010(8) 0.011(8) C23 0.076(12) 0.068(11) 0.043(9) -0.001(8) 0.026(9) -0.021(9) N7 0.052(9) 0.042(7) 0.070(9) 0.025(7) 0.033(8) 0.002(6) C4 0.081(11) 0.027(6) 0.051(8) 0.026(6) 0.033(8) 0.008(7) C44 0.057(11) 0.053(9) 0.076(12) 0.010(9) 0.025(9) 0.016(8) C24 0.088(14) 0.074(11) 0.027(8) 0.006(7) 0.010(9) -0.015(10) C52 0.133(17) 0.044(9) 0.051(10) 0.017(8) 0.009(11) -0.038(10) C22 0.102(15) 0.045(9) 0.058(10) 0.003(7) 0.061(11) -0.010(9) C51 0.116(16) 0.035(8) 0.102(14) 0.021(9) 0.064(13) 0.013(9) C48 0.088(13) 0.055(9) 0.037(8) -0.003(7) 0.011(9) -0.015(9) N1 0.035(6) 0.027(5) 0.031(5) 0.014(4) 0.015(5) -0.004(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.500 0.500 1.000 147 48 ' ' 2 0.500 1.000 1.000 169 53 ' ' _platon_squeeze_details ; ; 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 Sn1 O9 2.052(7) . ? Sn1 O5 2.058(8) . ? Sn1 O12 2.059(7) 2_766 ? Sn1 O10 2.113(9) . ? Sn1 O2 2.117(7) . ? Sn1 C1 2.132(10) . ? Sn3 O6 2.075(8) . ? Sn3 O9 2.078(7) . ? Sn3 O11 2.095(7) . ? Sn3 O1 2.109(7) . ? Sn3 O12 2.110(7) . ? Sn3 C25 2.153(11) . ? Sn2 O9 2.064(7) . ? Sn2 O11 2.072(7) . ? Sn2 O7 2.080(7) 2_766 ? Sn2 O10 2.094(7) . ? Sn2 O3 2.095(8) . ? Sn2 C13 2.121(11) . ? P2 O2 1.507(8) . ? P2 O3 1.530(9) . ? P2 O1 1.531(8) . ? P2 O4 1.595(8) . ? P1 O7 1.495(8) . ? P1 O6 1.510(8) . ? P1 O5 1.529(8) . ? P1 O8 1.589(8) . ? O8 C37 1.391(14) . ? O4 C43 1.345(15) . ? O7 Sn2 2.080(7) 2_766 ? O12 Sn1 2.059(7) 2_766 ? C1 C2 1.372(15) . ? C1 C6 1.416(14) . ? N3 N4 1.233(12) . ? N3 C30 1.466(15) . ? N2 N1 1.255(13) . ? N2 C7 1.382(14) . ? O13 C49 1.454(17) . ? O13 C52 1.468(17) . ? N5 N6 1.248(13) . ? N5 C18 1.411(15) . ? C3 C4 1.410(17) . ? C3 C2 1.421(15) . ? O14 N7 1.209(15) . ? C42 C37 1.357(17) . ? C42 C41 1.380(16) . ? N4 C31 1.456(15) . ? C12 C7 1.388(16) . ? C12 C11 1.424(16) . ? C6 C5 1.394(15) . ? C6 N1 1.439(13) . ? C25 C26 1.312(16) . ? C25 C30 1.430(16) . ? C5 C4 1.317(17) . ? N6 C19 1.439(17) . ? O17 N8 1.246(17) . ? C46 C47 1.31(2) . ? C46 C45 1.39(2) . ? C46 N8 1.422(19) . ? O15 N7 1.216(15) . ? C18 C17 1.349(18) . ? C18 C13 1.384(17) . ? C14 C13 1.377(16) . ? C14 C15 1.380(19) . ? C50 C51 1.47(2) . ? C50 C49 1.51(2) . ? C15 C16 1.41(2) . ? C19 C24 1.33(2) . ? C19 C20 1.343(18) . ? C34 C33 1.32(2) . ? C34 C35 1.373(19) . ? C8 C9 1.36(2) . ? C8 C7 1.376(18) . ? C31 C32 1.381(19) . ? C31 C36 1.385(16) . ? C29 C28 1.285(18) . ? C29 C30 1.376(16) . ? C26 C27 1.415(16) . ? C41 C40 1.38(2) . ? C9 C10 1.359(19) . ? C37 C38 1.359(16) . ? C17 C16 1.382(19) . ? C39 C40 1.37(2) . ? C39 C38 1.439(18) . ? C36 C35 1.363(18) . ? C32 C33 1.41(2) . ? C11 C10 1.362(18) . ? C43 C48 1.367(19) . ? C43 C44 1.369(19) . ? C45 C44 1.32(2) . ? O16 N8 1.227(18) . ? C27 C28 1.411(19) . ? C21 C22 1.35(2) . ? C21 C20 1.37(2) . ? C40 N7 1.489(17) . ? C47 C48 1.401(19) . ? C23 C22 1.38(2) . ? C23 C24 1.46(2) . ? C52 C51 1.50(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 O9 Sn1 O5 90.1(3) . . ? O9 Sn1 O12 89.5(3) . 2_766 ? O5 Sn1 O12 89.6(3) . 2_766 ? O9 Sn1 O10 74.6(3) . . ? O5 Sn1 O10 164.6(3) . . ? O12 Sn1 O10 88.9(3) 2_766 . ? O9 Sn1 O2 86.3(3) . . ? O5 Sn1 O2 90.8(3) . . ? O12 Sn1 O2 175.9(3) 2_766 . ? O10 Sn1 O2 89.6(3) . . ? O9 Sn1 C1 173.7(4) . . ? O5 Sn1 C1 95.1(4) . . ? O12 Sn1 C1 94.1(4) 2_766 . ? O10 Sn1 C1 100.3(4) . . ? O2 Sn1 C1 90.0(4) . . ? O6 Sn3 O9 91.2(3) . . ? O6 Sn3 O11 163.8(3) . . ? O9 Sn3 O11 72.6(3) . . ? O6 Sn3 O1 86.9(3) . . ? O9 Sn3 O1 86.2(3) . . ? O11 Sn3 O1 91.6(3) . . ? O6 Sn3 O12 88.7(3) . . ? O9 Sn3 O12 91.4(3) . . ? O11 Sn3 O12 91.9(3) . . ? O1 Sn3 O12 174.9(3) . . ? O6 Sn3 C25 97.3(4) . . ? O9 Sn3 C25 170.5(4) . . ? O11 Sn3 C25 98.8(4) . . ? O1 Sn3 C25 90.0(3) . . ? O12 Sn3 C25 93.1(3) . . ? O9 Sn2 O11 73.4(3) . . ? O9 Sn2 O7 88.5(3) . 2_766 ? O11 Sn2 O7 94.5(3) . 2_766 ? O9 Sn2 O10 74.7(3) . . ? O11 Sn2 O10 147.0(3) . . ? O7 Sn2 O10 93.0(3) 2_766 . ? O9 Sn2 O3 88.0(3) . . ? O11 Sn2 O3 85.8(3) . . ? O7 Sn2 O3 176.3(3) 2_766 . ? O10 Sn2 O3 84.8(3) . . ? O9 Sn2 C13 172.6(4) . . ? O11 Sn2 C13 113.9(4) . . ? O7 Sn2 C13 89.6(4) 2_766 . ? O10 Sn2 C13 98.2(4) . . ? O3 Sn2 C13 93.6(4) . . ? O2 P2 O3 112.5(5) . . ? O2 P2 O1 112.8(5) . . ? O3 P2 O1 110.5(4) . . ? O2 P2 O4 103.3(4) . . ? O3 P2 O4 108.9(5) . . ? O1 P2 O4 108.5(4) . . ? O7 P1 O6 114.1(5) . . ? O7 P1 O5 113.3(5) . . ? O6 P1 O5 112.9(5) . . ? O7 P1 O8 100.9(4) . . ? O6 P1 O8 108.3(4) . . ? O5 P1 O8 106.2(4) . . ? C37 O8 P1 125.9(8) . . ? C43 O4 P2 127.0(8) . . ? P2 O3 Sn2 121.0(5) . . ? P1 O6 Sn3 135.6(5) . . ? P2 O1 Sn3 121.8(4) . . ? P2 O2 Sn1 121.7(4) . . ? Sn1 O9 Sn2 105.8(3) . . ? Sn1 O9 Sn3 133.6(3) . . ? Sn2 O9 Sn3 105.8(3) . . ? P1 O7 Sn2 151.2(5) . 2_766 ? Sn1 O12 Sn3 152.2(4) 2_766 . ? C2 C1 C6 118.6(10) . . ? C2 C1 Sn1 119.4(8) . . ? C6 C1 Sn1 121.9(8) . . ? Sn2 O11 Sn3 104.9(3) . . ? N4 N3 C30 112.6(9) . . ? P1 O5 Sn1 138.5(5) . . ? N1 N2 C7 114.9(9) . . ? C49 O13 C52 109.1(11) . . ? N6 N5 C18 117.0(11) . . ? C4 C3 C2 117.3(11) . . ? C37 C42 C41 119.9(12) . . ? Sn2 O10 Sn1 102.6(3) . . ? N3 N4 C31 111.6(9) . . ? C7 C12 C11 119.0(12) . . ? C5 C6 C1 121.6(10) . . ? C5 C6 N1 121.5(9) . . ? C1 C6 N1 116.7(9) . . ? C26 C25 C30 120.1(11) . . ? C26 C25 Sn3 119.7(9) . . ? C30 C25 Sn3 120.2(8) . . ? C4 C5 C6 118.1(11) . . ? N5 N6 C19 115.8(12) . . ? C47 C46 C45 119.9(14) . . ? C47 C46 N8 118.2(15) . . ? C45 C46 N8 121.8(14) . . ? C17 C18 C13 122.4(13) . . ? C17 C18 N5 121.4(12) . . ? C13 C18 N5 116.2(11) . . ? C13 C14 C15 119.5(13) . . ? C51 C50 C49 101.5(13) . . ? C14 C15 C16 119.9(15) . . ? C24 C19 C20 121.1(14) . . ? C24 C19 N6 122.2(13) . . ? C20 C19 N6 115.9(13) . . ? C33 C34 C35 123.3(14) . . ? C9 C8 C7 121.3(13) . . ? C32 C31 C36 121.4(13) . . ? C32 C31 N4 114.0(12) . . ? C36 C31 N4 124.6(11) . . ? C28 C29 C30 122.1(13) . . ? C25 C26 C27 121.9(12) . . ? C42 C41 C40 117.1(13) . . ? C29 C30 C25 117.5(12) . . ? C29 C30 N3 124.5(11) . . ? C25 C30 N3 118.0(10) . . ? C8 C9 C10 120.4(14) . . ? C42 C37 C38 122.8(12) . . ? C42 C37 O8 123.9(11) . . ? C38 C37 O8 113.2(11) . . ? C18 C17 C16 118.9(14) . . ? C40 C39 C38 115.0(15) . . ? C35 C36 C31 119.9(13) . . ? C31 C32 C33 116.7(14) . . ? O13 C49 C50 105.7(13) . . ? C10 C11 C12 119.1(13) . . ? O4 C43 C48 123.1(12) . . ? O4 C43 C44 119.5(13) . . ? C48 C43 C44 117.3(14) . . ? C44 C45 C46 118.7(15) . . ? C28 C27 C26 115.8(12) . . ? C22 C21 C20 120.0(16) . . ? C36 C35 C34 118.1(14) . . ? C37 C38 C39 119.5(14) . . ? C14 C13 C18 119.3(11) . . ? C14 C13 Sn2 117.5(9) . . ? C18 C13 Sn2 122.8(9) . . ? C17 C16 C15 119.9(15) . . ? C9 C10 C11 121.1(14) . . ? C39 C40 C41 125.5(14) . . ? C39 C40 N7 116.3(16) . . ? C41 C40 N7 118.2(13) . . ? C46 C47 C48 121.0(15) . . ? C34 C33 C32 120.4(14) . . ? C19 C20 C21 121.0(16) . . ? C8 C7 N2 116.0(12) . . ? C8 C7 C12 119.1(12) . . ? N2 C7 C12 124.8(11) . . ? C29 C28 C27 122.5(13) . . ? C1 C2 C3 120.2(11) . . ? O16 N8 O17 120.0(15) . . ? O16 N8 C46 121.2(15) . . ? O17 N8 C46 118.6(16) . . ? C22 C23 C24 117.1(15) . . ? O14 N7 O15 124.7(13) . . ? O14 N7 C40 116.9(13) . . ? O15 N7 C40 118.3(14) . . ? C5 C4 C3 124.1(11) . . ? C45 C44 C43 123.5(16) . . ? C19 C24 C23 118.4(13) . . ? O13 C52 C51 102.5(14) . . ? C21 C22 C23 121.0(15) . . ? C50 C51 C52 104.8(13) . . ? C43 C48 C47 119.4(15) . . ? N2 N1 C6 116.2(9) . . ? _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 2.143 _refine_diff_density_min -1.095 _refine_diff_density_rms 0.206 _database_code_depnum_ccdc_archive 'CCDC 968923' ####################################################################### # # 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_4 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C60 H78 N6 O10 P3 Sn3, C8 H16 O2 P, C2 H3 N,' _chemical_formula_sum 'C70 H97 N7 O13 P4 Sn3' _chemical_formula_weight 1724.56 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' P P 0.1023 0.0942 '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 ? _symmetry_space_group_name_H-M 'C 2/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 25.319(5) _cell_length_b 14.135(5) _cell_length_c 44.872(5) _cell_angle_alpha 90.000(5) _cell_angle_beta 93.512(5) _cell_angle_gamma 90.000(5) _cell_volume 16029(7) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description blcok _exptl_crystal_colour orange _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.429 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 7040.0 _exptl_absorpt_coefficient_mu 1.068 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.172357 _exptl_absorpt_correction_T_max 1 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 42713 _diffrn_reflns_av_R_equivalents 0.0829 _diffrn_reflns_av_sigmaI/netI 0.0973 _diffrn_reflns_limit_h_min -30 _diffrn_reflns_limit_h_max 30 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -54 _diffrn_reflns_limit_l_max 54 _diffrn_reflns_theta_min 1.91 _diffrn_reflns_theta_max 25.50 _reflns_number_total 14881 _reflns_number_gt 9690 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type fullcycle _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0906P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 14881 _refine_ls_number_parameters 901 _refine_ls_number_restraints 18 _refine_ls_R_factor_all 0.1090 _refine_ls_R_factor_gt 0.0685 _refine_ls_wR_factor_ref 0.1879 _refine_ls_wR_factor_gt 0.1620 _refine_ls_goodness_of_fit_ref 1.030 _refine_ls_restrained_S_all 1.034 _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 Sn1 Sn 0.91473(2) 0.19970(4) 0.113638(11) 0.038 Uani 1 1 d . . . Sn2 Sn 0.94761(2) 0.42535(4) 0.111840(11) 0.034 Uani 1 1 d . . . Sn3 Sn 1.03926(2) 0.26336(4) 0.108974(10) 0.034 Uani 1 1 d . . . P1 P 0.84735(8) 0.35524(16) 0.14756(5) 0.043 Uani 1 1 d . . . P2 P 1.06329(8) 0.45686(14) 0.14565(4) 0.033 Uani 1 1 d . . . P3 P 1.00990(8) 0.07805(14) 0.14762(4) 0.035 Uani 1 1 d . . . P4 P 0.93148(10) 0.29644(18) 1.00552(5) 0.053 Uani 1 1 d . . . O1 O 0.86604(19) 0.2532(4) 0.14556(11) 0.040 Uani 1 1 d . . . O2 O 0.89088(18) 0.4282(3) 0.14407(10) 0.035 Uani 1 1 d . . . O3 O 1.00440(18) 0.4811(3) 0.14336(10) 0.032 Uani 1 1 d . . . O4 O 1.07663(17) 0.3522(3) 0.14103(10) 0.033 Uani 1 1 d . . . O5 O 1.04893(19) 0.1548(3) 0.14049(10) 0.035 Uani 1 1 d . . . O6 O 0.95199(19) 0.1086(3) 0.14509(10) 0.036 Uani 1 1 d . . . O7 O 1.0124(2) 0.3874(4) 0.08758(10) 0.038 Uani 1 1 d . . . O8 O 0.9797(2) 0.1748(4) 0.08711(11) 0.046 Uani 1 1 d . . . O9 O 0.97125(18) 0.2968(3) 0.13001(10) 0.031 Uani 1 1 d . . . O12 O 0.9640(2) 0.3779(4) 0.99714(11) 0.047 Uani 1 1 d . . . O13 O 0.9352(2) 0.2681(4) 1.03826(11) 0.058 Uani 1 1 d . . . O14 O 0.0403(2) 0.4523(4) 0.03497(11) 0.047 Uani 1 1 d . . . O15 O 0.8949(2) 0.3253(4) 0.08920(11) 0.043 Uani 1 1 d . . . N1 N 0.8347(3) 0.0434(5) 0.13903(14) 0.049 Uani 1 1 d . . . N2 N 0.8045(3) -0.0104(5) 0.15180(15) 0.049 Uani 1 1 d . . . N3 N 0.9159(2) 0.6352(5) 0.13043(13) 0.039 Uani 1 1 d . . . N4 N 0.9025(2) 0.7104(5) 0.14149(14) 0.042 Uani 1 1 d . . . N5 N 1.1602(3) 0.2094(5) 0.11911(16) 0.049 Uani 1 1 d . . . N6 N 1.2077(3) 0.1977(6) 0.12800(17) 0.060 Uani 1 1 d . . . N7 N 0.9269(5) 0.2613(10) 0.2469(3) 0.140 Uani 1 1 d . . . C1 C 0.8633(4) 0.0969(7) 0.09207(18) 0.059 Uani 1 1 d . . . C2 C 0.8624(6) 0.0893(9) 0.0608(2) 0.108 Uani 1 1 d . . . H2 H 0.8827 0.1296 0.0498 0.130 Uiso 1 1 calc R . . C3 C 0.8310(8) 0.0212(12) 0.0469(2) 0.182 Uani 1 1 d . . . H3 H 0.8286 0.0191 0.0261 0.218 Uiso 1 1 calc R . . C4 C 0.8031(7) -0.0436(11) 0.0623(2) 0.160 Uani 1 1 d . . . H4 H 0.7847 -0.0920 0.0522 0.192 Uiso 1 1 calc R . . C5 C 0.8024(5) -0.0371(8) 0.0929(2) 0.098 Uani 1 1 d . . . H5 H 0.7821 -0.0784 0.1036 0.118 Uiso 1 1 calc R . . C6 C 0.8329(4) 0.0328(7) 0.10742(18) 0.058 Uani 1 1 d . . . C7 C 0.8090(3) -0.0009(5) 0.18387(18) 0.044 Uani 1 1 d . . . C8 C 0.7755(3) -0.0593(6) 0.19894(19) 0.047 Uani 1 1 d . . . H8 H 0.7526 -0.1009 0.1885 0.056 Uiso 1 1 calc R . . C9 C 0.7769(4) -0.0544(6) 0.2298(2) 0.054 Uani 1 1 d . . . H9 H 0.7546 -0.0929 0.2402 0.065 Uiso 1 1 calc R . . C10 C 0.8095(3) 0.0044(6) 0.24472(19) 0.047 Uani 1 1 d . . . H10 H 0.8098 0.0072 0.2654 0.057 Uiso 1 1 calc R . . C11 C 0.8438(3) 0.0625(6) 0.2293(2) 0.055 Uani 1 1 d . . . H11 H 0.8671 0.1028 0.2400 0.066 Uiso 1 1 calc R . . C12 C 0.8430(3) 0.0599(6) 0.19885(19) 0.049 Uani 1 1 d . . . H12 H 0.8652 0.0988 0.1885 0.059 Uiso 1 1 calc R . . C13 C 0.9232(3) 0.5440(5) 0.08563(16) 0.038 Uani 1 1 d . . . C14 C 0.9185(3) 0.5358(6) 0.05460(17) 0.051 Uani 1 1 d . . . H14 H 0.9280 0.4795 0.0456 0.061 Uiso 1 1 calc R . . C15 C 0.9001(4) 0.6097(7) 0.0373(2) 0.068 Uani 1 1 d . . . H15 H 0.8974 0.6033 0.0166 0.082 Uiso 1 1 calc R . . C16 C 0.8854(4) 0.6943(7) 0.0502(2) 0.072 Uani 1 1 d . . . H16 H 0.8731 0.7441 0.0382 0.086 Uiso 1 1 calc R . . C17 C 0.8892(4) 0.7044(6) 0.08104(19) 0.059 Uani 1 1 d . . . H17 H 0.8793 0.7607 0.0898 0.071 Uiso 1 1 calc R . . C18 C 0.9081(3) 0.6288(6) 0.09873(17) 0.042 Uani 1 1 d . . . C19 C 0.9110(3) 0.7146(5) 0.17287(17) 0.037 Uani 1 1 d . . . C20 C 0.9312(3) 0.6394(6) 0.19040(18) 0.047 Uani 1 1 d . . . H20 H 0.9397 0.5823 0.1816 0.056 Uiso 1 1 calc R . . C21O C 0.9384(3) 0.6507(7) 0.22082(18) 0.055 Uani 1 1 d . . . H21 H 0.9518 0.6012 0.2327 0.066 Uiso 1 1 calc R . . C22 C 0.9255(3) 0.7361(7) 0.23379(18) 0.052 Uani 1 1 d . . . H22 H 0.9309 0.7436 0.2543 0.062 Uiso 1 1 calc R . . C23 C 0.9049(3) 0.8105(6) 0.2167(2) 0.051 Uani 1 1 d . . . H23 H 0.8961 0.8674 0.2255 0.061 Uiso 1 1 calc R . . C24 C 0.8977(3) 0.7979(6) 0.18627(18) 0.046 Uani 1 1 d . . . H24 H 0.8836 0.8470 0.1745 0.055 Uiso 1 1 calc R . . C25 C 1.0964(3) 0.2245(6) 0.07853(17) 0.047 Uani 1 1 d . . . C26 C 1.0810(5) 0.2180(7) 0.0481(2) 0.070 Uani 1 1 d . . . H26 H 1.0470 0.2353 0.0412 0.084 Uiso 1 1 calc R . . C27 C 1.1165(5) 0.1861(9) 0.0283(2) 0.105 Uani 1 1 d . . . H27 H 1.1058 0.1810 0.0082 0.126 Uiso 1 1 calc R . . C28 C 1.1676(6) 0.1616(12) 0.0378(2) 0.147 Uani 1 1 d . . . H28 H 1.1912 0.1397 0.0243 0.177 Uiso 1 1 calc R . . C29 C 1.1829(5) 0.1702(10) 0.0675(2) 0.110 Uani 1 1 d . . . H29 H 1.2173 0.1542 0.0741 0.132 Uiso 1 1 calc R . . C30 C 1.1483(4) 0.2020(7) 0.08784(19) 0.058 Uani 1 1 d . . . C31 C 1.2175(3) 0.2019(6) 0.1592(2) 0.048 Uani 1 1 d . . . C32 C 1.2691(4) 0.1922(6) 0.1701(2) 0.062 Uani 1 1 d . . . H32 H 1.2960 0.1870 0.1570 0.075 Uiso 1 1 calc R . . C33 C 1.2809(3) 0.1900(6) 0.2002(2) 0.055 Uani 1 1 d . . . H33 H 1.3158 0.1810 0.2073 0.066 Uiso 1 1 calc R . . C34 C 1.2425(3) 0.2008(6) 0.2203(2) 0.053 Uani 1 1 d . . . H34 H 1.2510 0.1995 0.2408 0.063 Uiso 1 1 calc R . . C35 C 1.1913(3) 0.2135(6) 0.2093(2) 0.052 Uani 1 1 d . . . H35 H 1.1650 0.2224 0.2226 0.062 Uiso 1 1 calc R . . C36 C 1.1775(3) 0.2134(6) 0.17905(18) 0.046 Uani 1 1 d . . . H36 H 1.1424 0.2209 0.1720 0.055 Uiso 1 1 calc R . . C37 C 1.0980(4) 0.5076(8) 0.1789(2) 0.083 Uani 1 1 d . . . C38 C 1.1324(5) 0.5604(9) 0.1570(2) 0.083 Uani 1 1 d U . . H38 H 1.158(4) 0.509(7) 0.156(2) 0.100 Uiso 1 1 calc . . . C39 C 1.1053(3) 0.5362(6) 0.12622(18) 0.052 Uani 1 1 d . . . C40 C 1.1301(5) 0.4379(7) 0.1982(3) 0.097 Uani 1 1 d . . . H40A H 1.1522 0.4717 0.2127 0.146 Uiso 1 1 calc R . . H40B H 1.1518 0.4008 0.1858 0.146 Uiso 1 1 calc R . . H40C H 1.1066 0.3970 0.2082 0.146 Uiso 1 1 calc R . . C41 C 1.0672(4) 0.5699(9) 0.1973(3) 0.116 Uani 1 1 d . . . H41A H 1.0469 0.5325 0.2102 0.174 Uiso 1 1 calc R . . H41B H 1.0438 0.6078 0.1846 0.174 Uiso 1 1 calc R . . H41C H 1.0908 0.6104 0.2090 0.174 Uiso 1 1 calc R . . C42 C 1.1429(4) 0.4894(8) 0.1049(2) 0.084 Uani 1 1 d . . . H42A H 1.1236 0.4737 0.0864 0.126 Uiso 1 1 calc R . . H42B H 1.1575 0.4328 0.1139 0.126 Uiso 1 1 calc R . . H42C H 1.1710 0.5324 0.1010 0.126 Uiso 1 1 calc R . . C43 C 1.0778(4) 0.6178(7) 0.1106(2) 0.075 Uani 1 1 d . . . H43A H 1.1033 0.6651 0.1062 0.112 Uiso 1 1 calc R . . H43B H 1.0524 0.6444 0.1233 0.112 Uiso 1 1 calc R . . H43C H 1.0599 0.5961 0.0924 0.112 Uiso 1 1 calc R . . C44 C 1.1707(4) 0.6289(7) 0.1637(2) 0.069 Uani 1 1 d . . . H44A H 1.1542 0.6900 0.1643 0.103 Uiso 1 1 calc R . . H44B H 1.1960 0.6288 0.1487 0.103 Uiso 1 1 calc R . . H44C H 1.1883 0.6154 0.1828 0.103 Uiso 1 1 calc R . . C45 C 1.0216(4) -0.0358(6) 0.13037(18) 0.054 Uani 1 1 d . . . C46 C 1.0196(5) -0.0755(7) 0.1628(2) 0.067 Uani 1 1 d U . . H46 H 0.982(4) -0.092(7) 0.164(2) 0.081 Uiso 1 1 calc . . . C47 C 1.0273(4) 0.0152(7) 0.1819(2) 0.067 Uani 1 1 d . . . C48 C 0.9759(5) -0.0783(7) 0.1122(3) 0.103 Uani 1 1 d . . . H48A H 0.9740 -0.0513 0.0925 0.155 Uiso 1 1 calc R . . H48B H 0.9436 -0.0654 0.1216 0.155 Uiso 1 1 calc R . . H48C H 0.9808 -0.1455 0.1108 0.155 Uiso 1 1 calc R . . C49 C 1.0695(4) -0.0394(7) 0.1136(2) 0.076 Uani 1 1 d . . . H49A H 1.0779 -0.1041 0.1093 0.114 Uiso 1 1 calc R . . H49B H 1.0985 -0.0113 0.1253 0.114 Uiso 1 1 calc R . . H49C H 1.0636 -0.0053 0.0952 0.114 Uiso 1 1 calc R . . C50 C 1.0489(4) -0.1648(7) 0.1713(2) 0.072 Uani 1 1 d . . . H50A H 1.0863 -0.1534 0.1716 0.108 Uiso 1 1 calc R . . H50B H 1.0394 -0.2134 0.1570 0.108 Uiso 1 1 calc R . . H50C H 1.0396 -0.1847 0.1908 0.108 Uiso 1 1 calc R . . C51 C 1.0802(4) 0.0377(11) 0.1968(3) 0.134 Uani 1 1 d . . . H51A H 1.0796 0.1003 0.2050 0.201 Uiso 1 1 calc R . . H51B H 1.1066 0.0343 0.1824 0.201 Uiso 1 1 calc R . . H51C H 1.0883 -0.0071 0.2125 0.201 Uiso 1 1 calc R . . C52 C 0.9864(4) 0.0117(8) 0.2047(2) 0.079 Uani 1 1 d . . . H52A H 0.9909 -0.0451 0.2163 0.118 Uiso 1 1 calc R . . H52B H 0.9517 0.0121 0.1948 0.118 Uiso 1 1 calc R . . H52C H 0.9903 0.0657 0.2176 0.118 Uiso 1 1 calc R . . C53 C 0.8087(3) 0.3775(6) 0.17967(19) 0.051 Uani 1 1 d . . . C54 C 0.7653(5) 0.4103(12) 0.1562(4) 0.116 Uani 1 1 d U . . H54 H 0.776(5) 0.477(9) 0.156(3) 0.139 Uiso 1 1 calc . . . C56 C 0.8278(4) 0.4579(7) 0.1999(3) 0.086 Uani 1 1 d . . . H56A H 0.7986 0.4822 0.2103 0.129 Uiso 1 1 calc R . . H56B H 0.8420 0.5074 0.1881 0.129 Uiso 1 1 calc R . . H56C H 0.8547 0.4352 0.2141 0.129 Uiso 1 1 calc R . . C57 C 0.7942(5) 0.2941(8) 0.1970(3) 0.103 Uani 1 1 d . . . H57A H 0.8239 0.2747 0.2099 0.154 Uiso 1 1 calc R . . H57B H 0.7840 0.2434 0.1837 0.154 Uiso 1 1 calc R . . H57C H 0.7651 0.3098 0.2089 0.154 Uiso 1 1 calc R . . C58 C 0.7089(4) 0.4250(11) 0.1624(3) 0.116 Uani 1 1 d . . . H58A H 0.6910 0.4565 0.1457 0.173 Uiso 1 1 calc R . . H58B H 0.7068 0.4632 0.1800 0.173 Uiso 1 1 calc R . . H58C H 0.6924 0.3649 0.1655 0.173 Uiso 1 1 calc R . . C61 C 0.8744(6) 0.1942(11) 0.9799(3) 0.119 Uani 1 1 d . . . H61 H 0.864(5) 0.152(9) 0.996(3) 0.142 Uiso 1 1 calc . . . C62 C 0.9352(5) 0.1932(7) 0.9809(2) 0.081 Uani 1 1 d . . . C66 C 0.9574(7) 0.1000(7) 0.9954(2) 0.130 Uani 1 1 d . . . H66A H 0.9393 0.0468 0.9863 0.195 Uiso 1 1 calc R . . H66B H 0.9521 0.1006 1.0164 0.195 Uiso 1 1 calc R . . H66C H 0.9946 0.0952 0.9925 0.195 Uiso 1 1 calc R . . C67 C 0.9625(6) 0.2135(8) 0.9532(2) 0.098 Uani 1 1 d . . . H67A H 0.9550 0.1640 0.9390 0.147 Uiso 1 1 calc R . . H67B H 1.0000 0.2169 0.9578 0.147 Uiso 1 1 calc R . . H67C H 0.9502 0.2728 0.9450 0.147 Uiso 1 1 calc R . . C68 C 0.8429(6) 0.1620(13) 0.9506(2) 0.157 Uani 1 1 d . . . H68A H 0.8619 0.1802 0.9336 0.235 Uiso 1 1 calc R . . H68B H 0.8087 0.1915 0.9494 0.235 Uiso 1 1 calc R . . H68C H 0.8387 0.0945 0.9508 0.235 Uiso 1 1 calc R . . C69 C 0.8620(4) 0.3003(9) 0.9908(2) 0.084 Uani 1 1 d . . . C70 C 0.8519(4) 0.3724(12) 0.9668(2) 0.121 Uani 1 1 d . . . H70A H 0.8171 0.3631 0.9575 0.182 Uiso 1 1 calc R . . H70B H 0.8778 0.3659 0.9522 0.182 Uiso 1 1 calc R . . H70C H 0.8543 0.4346 0.9754 0.182 Uiso 1 1 calc R . . C71 C 0.8193(4) 0.3058(14) 1.0136(3) 0.154 Uani 1 1 d . . . H71A H 0.8230 0.3642 1.0245 0.231 Uiso 1 1 calc R . . H71B H 0.8234 0.2536 1.0272 0.231 Uiso 1 1 calc R . . H71C H 0.7849 0.3031 1.0034 0.231 Uiso 1 1 calc R . . C72 C 0.9495(5) 0.2863(10) 0.2243(3) 0.093 Uani 1 1 d . . . C73 C 0.9771(4) 0.3070(8) 0.19988(19) 0.066 Uani 1 1 d . . . H73A H 1.0138 0.2924 0.2041 0.100 Uiso 1 1 calc R . . H73B H 0.9734 0.3731 0.1953 0.100 Uiso 1 1 calc R . . H73C H 0.9635 0.2702 0.1831 0.100 Uiso 1 1 calc R . . C74 C 0.7855(3) 0.3835(8) 0.1267(2) 0.064 Uani 1 1 d . . . C75 C 0.7866(4) 0.4614(8) 0.1048(3) 0.108 Uani 1 1 d . . . H75A H 0.7511 0.4758 0.0974 0.162 Uiso 1 1 calc R . . H75B H 0.8071 0.4426 0.0886 0.162 Uiso 1 1 calc R . . H75C H 0.8022 0.5164 0.1143 0.162 Uiso 1 1 calc R . . C76 C 0.7599(4) 0.2986(8) 0.1117(3) 0.099 Uani 1 1 d . . . H76A H 0.7236 0.3129 0.1059 0.149 Uiso 1 1 calc R . . H76B H 0.7612 0.2462 0.1254 0.149 Uiso 1 1 calc R . . H76C H 0.7784 0.2825 0.0944 0.149 Uiso 1 1 calc R . . H1OH H 0.973(3) 0.194(5) 0.0714(15) 0.034 Uiso 1 1 d . . . H2OH H 1.018(3) 0.402(6) 0.0767(15) 0.038 Uiso 1 1 d . . . H3OH H 0.901(3) 0.329(6) 0.0776(16) 0.051 Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Sn1 0.051 0.036 0.026 0.004 -0.005 -0.011 Sn2 0.043 0.033 0.025 0.005 -0.001 -0.004 Sn3 0.049 0.032 0.023 0.000 0.009 -0.003 P1 0.036 0.043 0.049 0.014 0.001 -0.001 P2 0.039 0.032 0.028 0.002 0.004 -0.003 P3 0.048 0.031 0.027 0.001 0.006 -0.003 P4 0.075 0.055 0.027 0.009 -0.005 -0.023 O1 0.037 0.041 0.043 0.006 0.005 -0.006 O2 0.032 0.038 0.034 0.003 0.004 0.002 O3 0.039 0.027 0.029 -0.001 0.001 -0.003 O4 0.033 0.033 0.033 -0.001 0.003 -0.002 O5 0.048 0.030 0.027 0.001 0.007 -0.001 O6 0.051 0.033 0.023 0.005 0.001 -0.008 O7 0.052 0.039 0.023 0.007 0.009 -0.006 O8 0.076 0.042 0.021 0.004 0.002 -0.019 O9 0.040 0.026 0.026 0.001 -0.001 -0.002 O12 0.060 0.046 0.033 0.006 -0.002 -0.014 O13 0.089 0.058 0.027 0.007 -0.006 -0.028 O14 0.057 0.056 0.030 0.014 0.003 0.001 O15 0.058 0.043 0.027 0.012 -0.008 -0.012 N1 0.059 0.045 0.042 0.009 -0.005 -0.016 N2 0.050 0.045 0.052 0.017 -0.004 -0.014 N3 0.042 0.037 0.038 0.002 -0.002 0.000 N4 0.047 0.035 0.043 0.004 0.003 -0.001 N5 0.050 0.046 0.053 0.008 0.017 0.009 N6 0.058 0.066 0.057 0.008 0.023 0.016 N7 0.110 0.193 0.121 0.008 0.033 -0.028 C1 0.083 0.056 0.036 0.004 -0.005 -0.033 C2 0.182 0.108 0.031 0.001 -0.021 -0.093 C3 0.325 0.176 0.037 0.027 -0.048 -0.184 C4 0.259 0.167 0.049 0.021 -0.032 -0.174 C5 0.156 0.088 0.047 0.004 -0.019 -0.089 C6 0.083 0.053 0.034 0.008 -0.024 -0.029 C7 0.056 0.028 0.048 0.010 0.005 0.001 C8 0.049 0.031 0.061 0.005 0.001 -0.007 C9 0.065 0.033 0.064 0.013 0.019 0.001 C10 0.059 0.038 0.046 0.002 0.015 0.004 C11 0.059 0.050 0.057 -0.002 0.006 -0.009 C12 0.059 0.039 0.050 0.002 0.006 -0.015 C13 0.043 0.035 0.034 0.009 -0.007 -0.005 C14 0.066 0.049 0.035 0.011 -0.008 -0.002 C15 0.103 0.064 0.036 0.018 -0.007 0.009 C16 0.117 0.052 0.043 0.016 -0.018 0.007 C17 0.096 0.040 0.039 0.013 -0.010 0.012 C18 0.052 0.038 0.038 0.012 0.003 0.002 C19 0.039 0.033 0.039 0.000 0.011 -0.002 C20 0.044 0.050 0.047 0.000 0.010 -0.005 C21O 0.072 0.054 0.039 0.003 0.006 0.020 C22 0.056 0.065 0.035 -0.013 0.012 -0.001 C23 0.058 0.039 0.059 0.000 0.017 -0.004 C24 0.052 0.039 0.048 0.004 0.011 0.002 C25 0.068 0.041 0.034 0.002 0.021 0.004 C26 0.106 0.065 0.042 0.002 0.033 0.028 C27 0.138 0.140 0.038 0.013 0.019 0.066 C28 0.169 0.240 0.037 0.016 0.046 0.136 C29 0.123 0.154 0.055 0.016 0.029 0.088 C30 0.079 0.058 0.040 0.010 0.028 0.023 C31 0.038 0.045 0.062 0.003 0.012 0.004 C32 0.056 0.052 0.082 -0.004 0.029 0.006 C33 0.044 0.040 0.080 0.002 0.002 0.001 C34 0.064 0.029 0.064 0.003 -0.005 0.004 C35 0.051 0.046 0.058 0.005 0.004 0.004 C36 0.041 0.046 0.052 0.002 0.007 0.004 C37 0.095 0.093 0.059 0.001 -0.010 -0.059 C38 0.095 0.093 0.059 0.001 -0.010 -0.059 C39 0.062 0.052 0.041 0.007 0.000 -0.026 C40 0.116 0.057 0.108 -0.007 -0.085 0.010 C41 0.076 0.142 0.124 -0.109 -0.046 0.045 C42 0.061 0.077 0.119 0.050 0.052 0.008 C43 0.095 0.045 0.089 0.030 0.050 0.013 C44 0.056 0.052 0.097 0.012 -0.007 -0.018 C45 0.095 0.031 0.038 -0.004 0.014 0.004 C46 0.103 0.046 0.053 0.007 0.006 0.009 C47 0.103 0.046 0.053 0.007 0.006 0.009 C48 0.114 0.054 0.146 -0.051 0.044 -0.033 C49 0.080 0.057 0.092 -0.041 0.014 0.005 C50 0.092 0.046 0.077 0.013 0.001 0.012 C51 0.073 0.198 0.126 0.115 -0.036 -0.035 C52 0.067 0.122 0.048 0.048 0.017 0.009 C53 0.046 0.052 0.055 0.008 0.012 0.011 C54 0.066 0.155 0.126 0.009 0.007 0.028 C56 0.093 0.064 0.108 -0.011 0.066 -0.010 C57 0.131 0.069 0.120 0.013 0.091 -0.010 C58 0.066 0.155 0.126 0.009 0.007 0.028 C61 0.161 0.136 0.057 -0.004 -0.007 -0.098 C62 0.137 0.069 0.035 0.001 -0.007 -0.040 C66 0.291 0.042 0.056 -0.004 0.000 -0.014 C67 0.171 0.081 0.043 -0.010 0.013 -0.022 C68 0.172 0.251 0.044 -0.008 -0.014 -0.148 C69 0.068 0.130 0.052 0.027 -0.018 -0.052 C70 0.064 0.226 0.071 0.045 -0.015 -0.033 C71 0.060 0.339 0.063 0.051 -0.010 -0.069 C72 0.092 0.122 0.061 -0.026 -0.016 -0.007 C73 0.069 0.095 0.035 0.012 0.009 0.004 C74 0.039 0.079 0.073 0.014 -0.011 0.008 C75 0.048 0.086 0.184 0.062 -0.041 -0.017 C76 0.063 0.064 0.163 0.031 -0.056 -0.014 _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 Sn1 O9 2.083(5) . ? Sn1 O1 2.088(5) . ? Sn1 O6 2.092(5) . ? Sn1 O8 2.118(6) . ? Sn1 O15 2.130(6) . ? Sn1 C1 2.142(8) . ? Sn2 O9 2.066(5) . ? Sn2 O7 2.093(5) . ? Sn2 O2 2.100(5) . ? Sn2 O3 2.107(5) . ? Sn2 C13 2.119(7) . ? Sn2 O15 2.156(6) . ? Sn3 O9 2.068(5) . ? Sn3 O5 2.091(5) . ? Sn3 O4 2.091(5) . ? Sn3 O7 2.092(6) . ? Sn3 C25 2.123(8) . ? Sn3 O8 2.150(5) . ? P1 O1 1.522(6) . ? P1 O2 1.525(5) . ? P1 C53 1.818(8) . ? P1 C74 1.819(8) . ? P2 O3 1.527(5) . ? P2 O4 1.535(5) . ? P2 C39 1.806(8) . ? P2 C37 1.832(10) . ? P3 O5 1.515(5) . ? P3 O6 1.526(5) . ? P3 C47 1.808(9) . ? P3 C45 1.818(8) . ? P4 O12 1.477(6) . ? P4 O13 1.520(5) . ? P4 C62 1.837(11) . ? P4 C69 1.843(10) . ? N1 N2 1.242(8) . ? N1 C6 1.424(10) . ? N2 C7 1.443(10) . ? N3 N4 1.229(8) . ? N3 C18 1.427(9) . ? N4 C19 1.413(9) . ? N5 N6 1.253(9) . ? N5 C30 1.421(11) . ? N6 C31 1.409(11) . ? N7 C72 1.246(15) . ? C1 C6 1.398(11) . ? C1 C2 1.406(12) . ? C2 C3 1.374(14) . ? C3 C4 1.372(15) . ? C4 C5 1.378(14) . ? C5 C6 1.390(12) . ? C7 C12 1.365(11) . ? C7 C8 1.389(10) . ? C8 C9 1.386(11) . ? C9 C10 1.324(11) . ? C10 C11 1.406(11) . ? C11 C12 1.368(11) . ? C13 C14 1.395(10) . ? C13 C18 1.397(11) . ? C14 C15 1.367(11) . ? C15 C16 1.389(13) . ? C16 C17 1.389(12) . ? C17 C18 1.398(10) . ? C19 C24 1.374(11) . ? C19 C20 1.400(11) . ? C20 C21O 1.375(11) . ? C21O C22 1.387(12) . ? C22 C23 1.385(11) . ? C23 C24 1.377(11) . ? C25 C30 1.391(12) . ? C25 C26 1.401(12) . ? C26 C27 1.375(13) . ? C27 C28 1.382(16) . ? C28 C29 1.370(15) . ? C29 C30 1.377(12) . ? C31 C32 1.373(12) . ? C31 C36 1.398(10) . ? C32 C33 1.367(13) . ? C33 C34 1.372(12) . ? C34 C35 1.371(12) . ? C35 C36 1.380(11) . ? C37 C41 1.463(14) . ? C37 C40 1.512(14) . ? C37 C38 1.545(14) . ? C38 C44 1.391(12) . ? C38 C39 1.541(13) . ? C39 C43 1.498(12) . ? C39 C42 1.541(12) . ? C45 C49 1.469(12) . ? C45 C48 1.500(14) . ? C45 C46 1.564(12) . ? C46 C50 1.501(13) . ? C46 C47 1.548(13) . ? C47 C51 1.493(14) . ? C47 C52 1.499(12) . ? C53 C57 1.472(12) . ? C53 C56 1.514(13) . ? C53 C54 1.546(16) . ? C54 C58 1.487(16) . ? C54 C74 1.496(17) . ? C61 C62 1.538(19) . ? C61 C68 1.563(15) . ? C61 C69 1.615(19) . ? C62 C67 1.485(14) . ? C62 C66 1.559(15) . ? C69 C70 1.491(15) . ? C69 C71 1.535(15) . ? C72 C73 1.367(14) . ? C74 C75 1.475(14) . ? C74 C76 1.504(14) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O9 Sn1 O1 86.63(19) . . ? O9 Sn1 O6 84.03(18) . . ? O1 Sn1 O6 91.20(19) . . ? O9 Sn1 O8 76.55(19) . . ? O1 Sn1 O8 163.2(2) . . ? O6 Sn1 O8 86.8(2) . . ? O9 Sn1 O15 76.6(2) . . ? O1 Sn1 O15 85.5(2) . . ? O6 Sn1 O15 160.5(2) . . ? O8 Sn1 O15 90.9(2) . . ? O9 Sn1 C1 172.4(3) . . ? O1 Sn1 C1 100.8(3) . . ? O6 Sn1 C1 97.1(3) . . ? O8 Sn1 C1 96.0(3) . . ? O15 Sn1 C1 102.4(3) . . ? O9 Sn2 O7 76.25(19) . . ? O9 Sn2 O2 86.50(18) . . ? O7 Sn2 O2 162.50(19) . . ? O9 Sn2 O3 83.98(18) . . ? O7 Sn2 O3 85.5(2) . . ? O2 Sn2 O3 89.88(18) . . ? O9 Sn2 C13 169.5(2) . . ? O7 Sn2 C13 97.2(3) . . ? O2 Sn2 C13 100.3(2) . . ? O3 Sn2 C13 103.9(2) . . ? O9 Sn2 O15 76.4(2) . . ? O7 Sn2 O15 93.9(2) . . ? O2 Sn2 O15 84.7(2) . . ? O3 Sn2 O15 159.89(19) . . ? C13 Sn2 O15 96.1(3) . . ? O9 Sn3 O5 85.71(18) . . ? O9 Sn3 O4 84.46(17) . . ? O5 Sn3 O4 86.91(19) . . ? O9 Sn3 O7 76.20(19) . . ? O5 Sn3 O7 161.17(19) . . ? O4 Sn3 O7 86.2(2) . . ? O9 Sn3 C25 166.5(3) . . ? O5 Sn3 C25 100.9(3) . . ? O4 Sn3 C25 107.5(3) . . ? O7 Sn3 C25 97.9(3) . . ? O9 Sn3 O8 76.2(2) . . ? O5 Sn3 O8 86.1(2) . . ? O4 Sn3 O8 159.80(19) . . ? O7 Sn3 O8 94.5(2) . . ? C25 Sn3 O8 92.4(3) . . ? O1 P1 O2 113.9(3) . . ? O1 P1 C53 113.3(4) . . ? O2 P1 C53 113.1(4) . . ? O1 P1 C74 116.0(4) . . ? O2 P1 C74 113.8(4) . . ? C53 P1 C74 83.2(4) . . ? O3 P2 O4 115.4(3) . . ? O3 P2 C39 115.4(4) . . ? O4 P2 C39 113.1(4) . . ? O3 P2 C37 112.6(4) . . ? O4 P2 C37 112.9(5) . . ? C39 P2 C37 83.3(4) . . ? O5 P3 O6 114.7(3) . . ? O5 P3 C47 113.8(4) . . ? O6 P3 C47 112.6(4) . . ? O5 P3 C45 114.8(4) . . ? O6 P3 C45 113.5(4) . . ? C47 P3 C45 83.7(4) . . ? O12 P4 O13 116.7(3) . . ? O12 P4 C62 114.6(4) . . ? O13 P4 C62 111.7(4) . . ? O12 P4 C69 114.8(4) . . ? O13 P4 C69 110.9(4) . . ? C62 P4 C69 83.7(6) . . ? P1 O1 Sn1 125.6(3) . . ? P1 O2 Sn2 125.9(3) . . ? P2 O3 Sn2 125.8(3) . . ? P2 O4 Sn3 125.3(3) . . ? P3 O5 Sn3 128.1(3) . . ? P3 O6 Sn1 128.0(3) . . ? Sn3 O7 Sn2 102.68(19) . . ? Sn1 O8 Sn3 101.2(2) . . ? Sn2 O9 Sn3 104.5(2) . . ? Sn2 O9 Sn1 105.3(2) . . ? Sn3 O9 Sn1 105.2(2) . . ? Sn1 O15 Sn2 100.6(2) . . ? N2 N1 C6 114.3(7) . . ? N1 N2 C7 113.0(7) . . ? N4 N3 C18 115.6(6) . . ? N3 N4 C19 114.2(6) . . ? N6 N5 C30 116.5(7) . . ? N5 N6 C31 114.7(7) . . ? C6 C1 C2 117.8(8) . . ? C6 C1 Sn1 123.7(6) . . ? C2 C1 Sn1 118.4(7) . . ? C3 C2 C1 118.8(10) . . ? C4 C3 C2 122.6(10) . . ? C3 C4 C5 119.9(11) . . ? C4 C5 C6 118.2(9) . . ? C5 C6 C1 122.5(8) . . ? C5 C6 N1 121.6(8) . . ? C1 C6 N1 115.9(7) . . ? C12 C7 C8 121.4(8) . . ? C12 C7 N2 124.0(7) . . ? C8 C7 N2 114.7(7) . . ? C9 C8 C7 118.6(8) . . ? C10 C9 C8 120.9(8) . . ? C9 C10 C11 120.3(8) . . ? C12 C11 C10 120.2(8) . . ? C7 C12 C11 118.7(8) . . ? C14 C13 C18 118.9(7) . . ? C14 C13 Sn2 119.5(6) . . ? C18 C13 Sn2 121.5(5) . . ? C15 C14 C13 120.6(9) . . ? C14 C15 C16 120.8(8) . . ? C15 C16 C17 120.0(8) . . ? C16 C17 C18 119.2(9) . . ? C13 C18 C17 120.6(7) . . ? C13 C18 N3 116.7(7) . . ? C17 C18 N3 122.6(7) . . ? C24 C19 C20 119.7(7) . . ? C24 C19 N4 116.5(7) . . ? C20 C19 N4 123.8(7) . . ? C21O C20 C19 119.4(8) . . ? C20 C21O C22 119.9(8) . . ? C23 C22 C21O 121.2(8) . . ? C24 C23 C22 118.2(8) . . ? C19 C24 C23 121.6(8) . . ? C30 C25 C26 118.6(8) . . ? C30 C25 Sn3 122.3(6) . . ? C26 C25 Sn3 119.0(7) . . ? C27 C26 C25 119.8(10) . . ? C26 C27 C28 121.3(10) . . ? C29 C28 C27 118.8(10) . . ? C28 C29 C30 121.3(11) . . ? C29 C30 C25 120.2(9) . . ? C29 C30 N5 124.9(9) . . ? C25 C30 N5 114.8(7) . . ? C32 C31 C36 119.7(8) . . ? C32 C31 N6 117.0(8) . . ? C36 C31 N6 123.2(7) . . ? C33 C32 C31 119.9(8) . . ? C32 C33 C34 121.7(8) . . ? C35 C34 C33 118.0(9) . . ? C34 C35 C36 122.2(8) . . ? C35 C36 C31 118.4(8) . . ? C41 C37 C40 110.9(10) . . ? C41 C37 C38 114.1(11) . . ? C40 C37 C38 112.0(10) . . ? C41 C37 P2 116.6(8) . . ? C40 C37 P2 115.1(8) . . ? C38 C37 P2 86.0(6) . . ? C44 C38 C39 127.9(9) . . ? C44 C38 C37 127.6(10) . . ? C39 C38 C37 103.1(7) . . ? C43 C39 C42 109.2(7) . . ? C43 C39 C38 114.6(9) . . ? C42 C39 C38 113.2(9) . . ? C43 C39 P2 115.6(6) . . ? C42 C39 P2 116.0(6) . . ? C38 C39 P2 87.0(5) . . ? C49 C45 C48 110.0(8) . . ? C49 C45 C46 122.6(9) . . ? C48 C45 C46 107.2(9) . . ? C49 C45 P3 114.2(7) . . ? C48 C45 P3 116.5(7) . . ? C46 C45 P3 84.6(5) . . ? C50 C46 C47 120.8(9) . . ? C50 C46 C45 119.7(9) . . ? C47 C46 C45 102.0(7) . . ? C51 C47 C52 110.0(9) . . ? C51 C47 C46 120.1(11) . . ? C52 C47 C46 106.4(9) . . ? C51 C47 P3 116.1(7) . . ? C52 C47 P3 117.0(7) . . ? C46 C47 P3 85.4(6) . . ? C57 C53 C56 111.4(9) . . ? C57 C53 C54 114.2(10) . . ? C56 C53 C54 111.7(10) . . ? C57 C53 P1 116.5(7) . . ? C56 C53 P1 115.9(6) . . ? C54 C53 P1 84.6(7) . . ? C58 C54 C74 125.8(13) . . ? C58 C54 C53 124.5(13) . . ? C74 C54 C53 105.1(9) . . ? C62 C61 C68 118.8(12) . . ? C62 C61 C69 102.3(9) . . ? C68 C61 C69 115.2(14) . . ? C67 C62 C61 119.3(10) . . ? C67 C62 C66 109.8(11) . . ? C61 C62 C66 110.8(11) . . ? C67 C62 P4 113.2(7) . . ? C61 C62 P4 85.5(8) . . ? C66 C62 P4 116.8(7) . . ? C70 C69 C71 110.5(11) . . ? C70 C69 C61 116.4(10) . . ? C71 C69 C61 114.0(11) . . ? C70 C69 P4 113.4(7) . . ? C71 C69 P4 117.2(7) . . ? C61 C69 P4 83.2(8) . . ? N7 C72 C73 175.1(15) . . ? C75 C74 C54 114.9(11) . . ? C75 C74 C76 108.9(9) . . ? C54 C74 C76 115.9(11) . . ? C75 C74 P1 117.1(7) . . ? C54 C74 P1 86.0(7) . . ? C76 C74 P1 112.9(7) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.798 _refine_diff_density_min -1.868 _refine_diff_density_rms 0.142 _database_code_depnum_ccdc_archive 'CCDC 968924' ####################################################################### # # 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 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum ' C87 H75 Cl2 N7 O12 P4 Sn3' _chemical_formula_weight 1961.45 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' P P 0.1023 0.0942 '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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.747(5) _cell_length_b 15.940(5) _cell_length_c 26.121(5) _cell_angle_alpha 102.795(5) _cell_angle_beta 94.468(5) _cell_angle_gamma 108.233(5) _cell_volume 4092(2) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.592 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1972.0 _exptl_absorpt_coefficient_mu 1.119 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.868314 _exptl_absorpt_correction_T_max 1 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 23171 _diffrn_reflns_av_R_equivalents 0.0313 _diffrn_reflns_av_sigmaI/netI 0.0675 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 1.84 _diffrn_reflns_theta_max 26.00 _reflns_number_total 15702 _reflns_number_gt 12197 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0958P)^2^+1.0690P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 15702 _refine_ls_number_parameters 1049 _refine_ls_number_restraints 8 _refine_ls_R_factor_all 0.0709 _refine_ls_R_factor_gt 0.0518 _refine_ls_wR_factor_ref 0.1658 _refine_ls_wR_factor_gt 0.1319 _refine_ls_goodness_of_fit_ref 1.053 _refine_ls_restrained_S_all 1.057 _refine_ls_shift/su_max 0.046 _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 Sn1 Sn -0.08289(4) 0.13072(3) 0.273249(15) 0.01560(11) Uani 1 1 d . . . Sn2 Sn 0.19520(4) 0.30561(3) 0.303129(15) 0.01604(11) Uani 1 1 d . . . Sn3 Sn 0.09575(4) 0.17958(3) 0.180573(14) 0.01582(11) Uani 1 1 d . . . P1 P -0.23225(14) 0.11757(10) 0.15466(6) 0.0168(3) Uani 1 1 d . . . P2 P -0.07204(14) 0.32453(10) 0.35262(6) 0.0180(3) Uani 1 1 d . . . P3 P 0.20336(14) 0.40521(10) 0.20538(6) 0.0176(3) Uani 1 1 d . . . P4 P 0.31080(16) 1.04016(11) 0.28075(6) 0.0227(3) Uani 1 1 d . . . O1 O -0.2365(4) 0.1116(3) 0.21192(14) 0.0169(8) Uani 1 1 d . . . O2 O -0.0946(4) 0.1530(3) 0.14047(15) 0.0181(8) Uani 1 1 d . . . O3 O -0.1462(4) 0.2248(3) 0.32264(15) 0.0198(9) Uani 1 1 d . . . O4 O 0.0710(4) 0.3651(3) 0.34366(15) 0.0206(9) Uani 1 1 d . . . O5 O 0.2374(4) 0.4098(3) 0.26377(15) 0.0195(9) Uani 1 1 d . . . O6 O 0.1680(4) 0.3105(3) 0.16695(15) 0.0190(9) Uani 1 1 d . . . O7 O 0.3922(4) 1.1216(3) 0.26366(16) 0.0243(9) Uani 1 1 d . . . O8 O 0.1649(4) 1.0262(3) 0.27940(16) 0.0268(10) Uani 1 1 d . . . O9 O 0.0037(4) 0.0662(2) 0.21320(14) 0.0143(8) Uani 1 1 d D . . O10 O 0.0993(4) 0.1835(3) 0.32555(18) 0.0178(9) Uani 1 1 d . . . O11 O 0.2648(4) 0.2310(3) 0.24123(15) 0.0164(8) Uani 1 1 d . . . O12 O 0.0271(3) 0.2408(2) 0.24565(14) 0.0147(8) Uani 1 1 d . . . N1 N -0.0699(5) 0.0732(3) 0.3883(2) 0.0240(11) Uani 1 1 d . . . N2 N -0.0803(5) 0.0745(4) 0.4359(2) 0.0275(12) Uani 1 1 d . . . N3 N 0.3629(5) 0.5045(3) 0.37828(19) 0.0236(11) Uani 1 1 d . . . N4 N 0.4225(5) 0.5881(3) 0.4007(2) 0.0265(12) Uani 1 1 d . . . N5 N 0.0889(5) 0.1771(3) 0.0579(2) 0.0242(11) Uani 1 1 d . . . N6 N 0.0743(5) 0.1815(4) 0.0106(2) 0.0268(12) Uani 1 1 d . . . Cl1 Cl 0.9160(2) 0.74422(13) 0.27674(8) 0.0454(5) Uani 1 1 d . . . Cl2 Cl 0.9190(2) 0.79223(16) 0.17553(8) 0.0548(5) Uani 1 1 d . . . C1 C -0.1961(5) 0.0151(4) 0.2992(2) 0.0161(11) Uani 1 1 d . . . C2 C -0.1759(6) 0.0040(4) 0.3505(2) 0.0214(13) Uani 1 1 d . . . C3 C -0.2576(6) -0.0734(4) 0.3638(3) 0.0259(14) Uani 1 1 d . . . H3 H -0.2442 -0.0798 0.3981 0.031 Uiso 1 1 calc R . . C4 C -0.3564(6) -0.1391(4) 0.3267(3) 0.0305(15) Uani 1 1 d . . . H4 H -0.4085 -0.1910 0.3355 0.037 Uiso 1 1 calc R . . C5 C -0.3794(6) -0.1288(4) 0.2762(3) 0.0285(14) Uani 1 1 d . . . H5 H -0.4473 -0.1737 0.2511 0.034 Uiso 1 1 calc R . . C6 C -0.3011(6) -0.0514(4) 0.2625(2) 0.0230(13) Uani 1 1 d . . . H6 H -0.3190 -0.0441 0.2286 0.028 Uiso 1 1 calc R . . C7 C 0.0266(6) 0.1387(4) 0.4745(2) 0.0259(14) Uani 1 1 d . . . C8 C 0.0182(7) 0.1383(5) 0.5268(3) 0.0346(16) Uani 1 1 d . . . H8 H -0.0547 0.0965 0.5350 0.042 Uiso 1 1 calc R . . C9 C 0.1160(8) 0.1988(5) 0.5670(3) 0.0387(17) Uani 1 1 d . . . H9 H 0.1083 0.1986 0.6022 0.046 Uiso 1 1 calc R . . C10 C 0.2259(7) 0.2602(5) 0.5554(3) 0.0393(18) Uani 1 1 d . . . H10 H 0.2918 0.3017 0.5826 0.047 Uiso 1 1 calc R . . C11 C 0.2370(7) 0.2593(5) 0.5031(3) 0.0357(17) Uani 1 1 d . . . H11 H 0.3125 0.2992 0.4953 0.043 Uiso 1 1 calc R . . C12 C 0.1380(7) 0.2001(4) 0.4620(3) 0.0298(15) Uani 1 1 d . . . H12 H 0.1452 0.2011 0.4268 0.036 Uiso 1 1 calc R . . C13 C 0.3599(5) 0.3522(4) 0.3657(2) 0.0174(12) Uani 1 1 d . . . C14 C 0.4106(6) 0.2866(4) 0.3789(2) 0.0237(13) Uani 1 1 d . . . H14 H 0.3732 0.2256 0.3599 0.028 Uiso 1 1 calc R . . C15 C 0.5158(6) 0.3125(5) 0.4200(3) 0.0286(14) Uani 1 1 d . . . H15 H 0.5458 0.2685 0.4296 0.034 Uiso 1 1 calc R . . C16 C 0.5762(6) 0.4043(4) 0.4468(2) 0.0271(14) Uani 1 1 d . . . H16 H 0.6481 0.4217 0.4738 0.033 Uiso 1 1 calc R . . C17 C 0.5301(6) 0.4693(4) 0.4336(2) 0.0256(14) Uani 1 1 d . . . H17 H 0.5718 0.5307 0.4513 0.031 Uiso 1 1 calc R . . C18 C 0.4209(6) 0.4432(4) 0.3938(2) 0.0217(13) Uani 1 1 d . . . C19 C 0.3575(6) 0.6460(4) 0.3851(2) 0.0251(13) Uani 1 1 d . . . C20 C 0.4122(7) 0.7382(4) 0.4116(3) 0.0301(15) Uani 1 1 d . . . H20 H 0.4896 0.7598 0.4362 0.036 Uiso 1 1 calc R . . C21 C 0.3495(7) 0.7976(5) 0.4006(3) 0.0335(16) Uani 1 1 d . . . H21 H 0.3862 0.8595 0.4179 0.040 Uiso 1 1 calc R . . C22 C 0.2326(8) 0.7668(5) 0.3642(3) 0.0362(17) Uani 1 1 d . . . H22 H 0.1898 0.8072 0.3586 0.043 Uiso 1 1 calc R . . C23 C 0.1812(7) 0.6757(5) 0.3365(3) 0.0339(16) Uani 1 1 d . . . H23 H 0.1047 0.6549 0.3114 0.041 Uiso 1 1 calc R . . C24 C 0.2440(6) 0.6141(4) 0.3462(2) 0.0263(14) Uani 1 1 d . . . H24 H 0.2107 0.5530 0.3271 0.032 Uiso 1 1 calc R . . C25 C 0.1598(5) 0.1008(4) 0.1181(2) 0.0204(13) Uani 1 1 d . . . C26 C 0.1428(6) 0.1086(4) 0.0660(2) 0.0216(13) Uani 1 1 d . . . C27 C 0.1743(7) 0.0496(5) 0.0247(2) 0.0307(15) Uani 1 1 d . . . H27 H 0.1608 0.0544 -0.0100 0.037 Uiso 1 1 calc R . . C28 C 0.2243(6) -0.0148(4) 0.0349(2) 0.0269(14) Uani 1 1 d . . . H28 H 0.2462 -0.0531 0.0075 0.032 Uiso 1 1 calc R . . C29 C 0.2426(6) -0.0228(4) 0.0876(2) 0.0268(14) Uani 1 1 d . . . H29 H 0.2768 -0.0664 0.0951 0.032 Uiso 1 1 calc R . . C30 C 0.2092(6) 0.0347(4) 0.1278(2) 0.0203(12) Uani 1 1 d . . . H30 H 0.2203 0.0287 0.1623 0.024 Uiso 1 1 calc R . . C31 C 0.0214(6) 0.2495(4) 0.0034(2) 0.0245(13) Uani 1 1 d . . . C32 C -0.0242(7) 0.2447(5) -0.0489(3) 0.0336(16) Uani 1 1 d . . . H32 H -0.0154 0.1999 -0.0766 0.040 Uiso 1 1 calc R . . C33 C -0.0825(7) 0.3058(5) -0.0600(3) 0.0392(18) Uani 1 1 d . . . H33 H -0.1123 0.3024 -0.0951 0.047 Uiso 1 1 calc R . . C34 C -0.0969(7) 0.3735(5) -0.0183(3) 0.0375(17) Uani 1 1 d . . . H34 H -0.1378 0.4139 -0.0257 0.045 Uiso 1 1 calc R . . C35 C -0.0498(7) 0.3796(5) 0.0339(3) 0.0366(17) Uani 1 1 d . . . H35 H -0.0567 0.4256 0.0613 0.044 Uiso 1 1 calc R . . C36 C 0.0072(6) 0.3183(4) 0.0454(3) 0.0285(14) Uani 1 1 d . . . H36 H 0.0364 0.3218 0.0805 0.034 Uiso 1 1 calc R . . C37 C -0.3247(5) 0.1880(4) 0.1403(2) 0.0160(11) Uani 1 1 d . . . C38 C -0.4254(6) 0.1985(4) 0.1677(2) 0.0247(13) Uani 1 1 d . . . H38 H -0.4449 0.1710 0.1954 0.030 Uiso 1 1 calc R . . C39 C -0.4979(6) 0.2511(4) 0.1535(2) 0.0249(14) Uani 1 1 d . . . H39 H -0.5653 0.2591 0.1721 0.030 Uiso 1 1 calc R . . C40 C -0.4709(6) 0.2912(4) 0.1123(3) 0.0291(15) Uani 1 1 d . . . H40 H -0.5215 0.3244 0.1024 0.035 Uiso 1 1 calc R . . C41 C -0.3672(6) 0.2815(4) 0.0856(3) 0.0286(14) Uani 1 1 d . . . H41 H -0.3462 0.3105 0.0586 0.034 Uiso 1 1 calc R . . C42 C -0.2959(6) 0.2297(4) 0.0987(2) 0.0211(13) Uani 1 1 d . . . H42 H -0.2282 0.2222 0.0801 0.025 Uiso 1 1 calc R . . C43 C -0.3138(6) 0.0036(4) 0.1113(2) 0.0193(12) Uani 1 1 d . . . C44 C -0.4248(6) -0.0172(4) 0.0736(2) 0.0225(13) Uani 1 1 d . . . H44 H -0.4619 0.0274 0.0710 0.027 Uiso 1 1 calc R . . C45 C -0.4809(6) -0.1050(4) 0.0396(2) 0.0285(14) Uani 1 1 d . . . H45 H -0.5556 -0.1190 0.0145 0.034 Uiso 1 1 calc R . . C46 C -0.4253(6) -0.1708(4) 0.0433(2) 0.0266(14) Uani 1 1 d . . . H46 H -0.4621 -0.2290 0.0202 0.032 Uiso 1 1 calc R . . C47 C -0.3130(6) -0.1513(4) 0.0817(3) 0.0269(14) Uani 1 1 d . . . H47 H -0.2773 -0.1965 0.0845 0.032 Uiso 1 1 calc R . . C48 C -0.2566(6) -0.0639(4) 0.1151(2) 0.0254(14) Uani 1 1 d . . . H48 H -0.1815 -0.0497 0.1400 0.030 Uiso 1 1 calc R . . C49 C -0.1669(6) 0.3909(4) 0.3350(2) 0.0200(12) Uani 1 1 d . . . C50 C -0.2991(6) 0.3487(4) 0.3112(2) 0.0240(13) Uani 1 1 d . . . H50 H -0.3379 0.2854 0.3027 0.029 Uiso 1 1 calc R . . C51 C -0.3736(7) 0.4034(5) 0.3002(3) 0.0340(16) Uani 1 1 d . . . H51 H -0.4616 0.3756 0.2838 0.041 Uiso 1 1 calc R . . C52 C -0.3178(7) 0.4965(5) 0.3134(3) 0.0350(16) Uani 1 1 d . . . H52 H -0.3678 0.5323 0.3069 0.042 Uiso 1 1 calc R . . C53 C -0.1847(7) 0.5371(5) 0.3369(3) 0.0341(16) Uani 1 1 d . . . H53 H -0.1463 0.6005 0.3454 0.041 Uiso 1 1 calc R . . C54 C -0.1090(6) 0.4860(4) 0.3477(2) 0.0254(14) Uani 1 1 d . . . H54 H -0.0204 0.5143 0.3632 0.030 Uiso 1 1 calc R . . C55 C -0.0665(6) 0.3331(4) 0.4220(2) 0.0227(13) Uani 1 1 d . . . C56 C -0.1737(6) 0.2755(4) 0.4389(3) 0.0286(14) Uani 1 1 d . . . H56 H -0.2457 0.2337 0.4143 0.034 Uiso 1 1 calc R . . C57 C -0.1704(7) 0.2820(5) 0.4931(2) 0.0318(16) Uani 1 1 d . . . H57 H -0.2408 0.2440 0.5048 0.038 Uiso 1 1 calc R . . C58 C -0.0647(7) 0.3437(5) 0.5294(3) 0.0339(16) Uani 1 1 d . . . H58 H -0.0642 0.3473 0.5655 0.041 Uiso 1 1 calc R . . C59 C 0.0402(7) 0.4000(4) 0.5130(2) 0.0312(15) Uani 1 1 d . . . H59 H 0.1121 0.4411 0.5379 0.037 Uiso 1 1 calc R . . C60 C 0.0396(7) 0.3960(4) 0.4590(2) 0.0301(15) Uani 1 1 d . . . H60 H 0.1099 0.4353 0.4479 0.036 Uiso 1 1 calc R . . C61 C 0.0701(5) 0.4493(4) 0.1971(2) 0.0170(12) Uani 1 1 d . . . C62 C -0.0553(5) 0.4011(4) 0.2076(2) 0.0206(12) Uani 1 1 d . . . H62 H -0.0675 0.3480 0.2188 0.025 Uiso 1 1 calc R . . C63 C -0.1604(6) 0.4324(4) 0.2014(2) 0.0255(14) Uani 1 1 d . . . H63 H -0.2431 0.4005 0.2083 0.031 Uiso 1 1 calc R . . C64 C -0.1420(6) 0.5119(4) 0.1847(2) 0.0270(14) Uani 1 1 d . . . H64 H -0.2126 0.5331 0.1808 0.032 Uiso 1 1 calc R . . C65 C -0.0200(6) 0.5596(5) 0.1739(3) 0.0323(15) Uani 1 1 d . . . H65 H -0.0081 0.6128 0.1629 0.039 Uiso 1 1 calc R . . C66 C 0.0850(6) 0.5272(4) 0.1797(3) 0.0278(14) Uani 1 1 d . . . H66 H 0.1668 0.5585 0.1717 0.033 Uiso 1 1 calc R . . C67 C 0.3465(6) 0.4834(4) 0.1887(2) 0.0233(13) Uani 1 1 d . . . C68 C 0.3635(6) 0.4773(4) 0.1357(3) 0.0301(15) Uani 1 1 d . . . H68 H 0.3057 0.4294 0.1086 0.036 Uiso 1 1 calc R . . C69 C 0.4674(8) 0.5434(5) 0.1242(3) 0.044(2) Uani 1 1 d . . . H69 H 0.4783 0.5405 0.0890 0.053 Uiso 1 1 calc R . . C70 C 0.5553(7) 0.6137(5) 0.1640(3) 0.0363(17) Uani 1 1 d . . . H70 H 0.6261 0.6568 0.1556 0.044 Uiso 1 1 calc R . . C71 C 0.5378(6) 0.6201(4) 0.2169(3) 0.0322(16) Uani 1 1 d . . . H71 H 0.5956 0.6683 0.2439 0.039 Uiso 1 1 calc R . . C72 C 0.4348(6) 0.5549(4) 0.2287(2) 0.0263(14) Uani 1 1 d . . . H72 H 0.4238 0.5584 0.2640 0.032 Uiso 1 1 calc R . . C73 C 0.3275(6) 0.9373(4) 0.2406(2) 0.0218(13) Uani 1 1 d . . . C74 C 0.2633(6) 0.8533(4) 0.2507(2) 0.0256(14) Uani 1 1 d . . . H74 H 0.2150 0.8514 0.2787 0.031 Uiso 1 1 calc R . . C75 C 0.2701(6) 0.7721(4) 0.2195(3) 0.0281(14) Uani 1 1 d . . . H75 H 0.2281 0.7167 0.2271 0.034 Uiso 1 1 calc R . . C76 C 0.3400(7) 0.7746(5) 0.1770(3) 0.0339(16) Uani 1 1 d . . . H76 H 0.3437 0.7205 0.1557 0.041 Uiso 1 1 calc R . . C77 C 0.4053(6) 0.8583(4) 0.1659(2) 0.0276(14) Uani 1 1 d . . . H77 H 0.4518 0.8601 0.1374 0.033 Uiso 1 1 calc R . . C78 C 0.3992(6) 0.9380(4) 0.1981(2) 0.0262(14) Uani 1 1 d . . . H78 H 0.4439 0.9936 0.1913 0.031 Uiso 1 1 calc R . . C79 C 0.3742(6) 1.0468(4) 0.3488(2) 0.0231(13) Uani 1 1 d . . . C80 C 0.2916(7) 1.0434(5) 0.3869(3) 0.0322(15) Uani 1 1 d . . . H80 H 0.2020 1.0334 0.3772 0.039 Uiso 1 1 calc R . . C81 C 0.3423(7) 1.0551(5) 0.4397(3) 0.0343(16) Uani 1 1 d . . . H81 H 0.2871 1.0550 0.4654 0.041 Uiso 1 1 calc R . . C82 C 0.4719(8) 1.0665(5) 0.4537(3) 0.0395(18) Uani 1 1 d . . . H82 H 0.5050 1.0747 0.4891 0.047 Uiso 1 1 calc R . . C83 C 0.5560(7) 1.0662(4) 0.4158(3) 0.0346(16) Uani 1 1 d . . . H83 H 0.6440 1.0721 0.4256 0.042 Uiso 1 1 calc R . . C84 C 0.5073(7) 1.0568(4) 0.3630(3) 0.0295(14) Uani 1 1 d . . . H84 H 0.5629 1.0571 0.3374 0.035 Uiso 1 1 calc R . . C87 C 0.9231(8) 0.8316(5) 0.2451(3) 0.0443(19) Uani 1 1 d . . . H87A H 1.0040 0.8831 0.2601 0.053 Uiso 1 1 calc R . . H87B H 0.8484 0.8523 0.2513 0.053 Uiso 1 1 calc R . . N1S N 0.6006(9) 0.6168(5) -0.0002(3) 0.050(2) Uani 1 1 d . . . C1S C 0.7459(12) 0.5509(8) 0.0478(5) 0.087(3) Uani 1 1 d DU . . H1S1 H 0.7837 0.5913 0.0825 0.130 Uiso 1 1 calc R . . H1S2 H 0.8157 0.5446 0.0282 0.130 Uiso 1 1 calc R . . H1S3 H 0.6933 0.4920 0.0513 0.130 Uiso 1 1 calc R . . C2S C 0.6566(10) 0.5909(7) 0.0179(4) 0.064(3) Uani 1 1 d D . . H1H H 0.322(10) 0.190(7) 0.245(4) 0.09(3) Uiso 1 1 d . . . H3H H 0.118(7) 0.153(4) 0.319(3) 0.00(2) Uiso 1 1 d . . . H2H H -0.004(11) 0.104(6) 0.243(3) 0.11(4) Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Sn1 0.0131(2) 0.0162(2) 0.0156(2) 0.00320(15) 0.00327(14) 0.00282(15) Sn2 0.0129(2) 0.0167(2) 0.0164(2) 0.00292(15) 0.00244(15) 0.00301(15) Sn3 0.0138(2) 0.0164(2) 0.0158(2) 0.00260(15) 0.00393(15) 0.00392(15) P1 0.0138(7) 0.0190(7) 0.0162(7) 0.0035(6) 0.0027(6) 0.0043(6) P2 0.0169(7) 0.0198(8) 0.0156(7) 0.0030(6) 0.0042(6) 0.0046(6) P3 0.0144(7) 0.0175(7) 0.0182(7) 0.0040(6) 0.0032(6) 0.0023(6) P4 0.0207(8) 0.0255(8) 0.0250(8) 0.0069(7) 0.0058(6) 0.0113(6) O1 0.0111(18) 0.020(2) 0.0163(19) 0.0012(16) 0.0012(15) 0.0033(15) O2 0.0141(19) 0.022(2) 0.018(2) 0.0057(16) 0.0026(15) 0.0050(16) O3 0.017(2) 0.019(2) 0.022(2) 0.0022(16) 0.0080(16) 0.0048(16) O4 0.021(2) 0.018(2) 0.019(2) 0.0001(16) 0.0047(16) 0.0044(17) O5 0.027(2) 0.0128(19) 0.016(2) 0.0044(16) 0.0048(17) 0.0026(16) O6 0.018(2) 0.018(2) 0.019(2) 0.0043(16) 0.0027(16) 0.0036(16) O7 0.027(2) 0.027(2) 0.022(2) 0.0092(18) 0.0103(18) 0.0104(18) O8 0.024(2) 0.039(3) 0.026(2) 0.015(2) 0.0098(18) 0.016(2) O9 0.0146(19) 0.0104(18) 0.0154(19) -0.0011(15) 0.0086(15) 0.0023(15) O10 0.015(2) 0.017(2) 0.020(2) 0.0073(19) 0.0032(17) 0.003(2) O11 0.0129(19) 0.0131(19) 0.019(2) -0.0018(16) 0.0023(15) 0.0026(15) O12 0.0101(18) 0.0162(19) 0.0156(19) 0.0029(15) 0.0047(15) 0.0018(15) N1 0.023(3) 0.028(3) 0.024(3) 0.009(2) 0.004(2) 0.010(2) N2 0.026(3) 0.029(3) 0.027(3) 0.007(2) 0.005(2) 0.008(2) N3 0.027(3) 0.021(3) 0.020(3) 0.005(2) 0.003(2) 0.003(2) N4 0.028(3) 0.016(3) 0.029(3) 0.000(2) 0.005(2) 0.003(2) N5 0.021(3) 0.024(3) 0.023(3) 0.005(2) 0.003(2) 0.002(2) N6 0.033(3) 0.027(3) 0.019(3) 0.008(2) 0.004(2) 0.007(2) Cl1 0.0451(11) 0.0458(11) 0.0494(11) 0.0189(9) 0.0133(9) 0.0153(9) Cl2 0.0565(13) 0.0633(14) 0.0483(12) 0.0235(10) 0.0009(10) 0.0210(11) C1 0.018(3) 0.008(3) 0.026(3) 0.005(2) 0.008(2) 0.007(2) C2 0.020(3) 0.026(3) 0.023(3) 0.011(3) 0.008(2) 0.010(2) C3 0.027(3) 0.029(3) 0.028(3) 0.015(3) 0.007(3) 0.012(3) C4 0.026(3) 0.022(3) 0.047(4) 0.018(3) 0.015(3) 0.005(3) C5 0.016(3) 0.027(3) 0.040(4) 0.010(3) 0.001(3) 0.004(3) C6 0.019(3) 0.024(3) 0.024(3) 0.005(3) 0.006(2) 0.005(2) C7 0.031(3) 0.033(4) 0.019(3) 0.005(3) 0.003(3) 0.019(3) C8 0.035(4) 0.042(4) 0.031(4) 0.016(3) 0.007(3) 0.013(3) C9 0.046(4) 0.048(5) 0.027(4) 0.010(3) 0.006(3) 0.024(4) C10 0.042(4) 0.040(4) 0.033(4) -0.004(3) -0.009(3) 0.023(3) C11 0.027(4) 0.033(4) 0.044(4) 0.002(3) 0.012(3) 0.010(3) C12 0.035(4) 0.029(4) 0.029(3) 0.006(3) 0.012(3) 0.013(3) C13 0.009(3) 0.024(3) 0.015(3) -0.001(2) 0.003(2) 0.004(2) C14 0.019(3) 0.022(3) 0.025(3) 0.000(3) -0.004(2) 0.006(2) C15 0.025(3) 0.034(4) 0.032(4) 0.014(3) 0.005(3) 0.014(3) C16 0.022(3) 0.033(4) 0.020(3) 0.004(3) -0.004(2) 0.006(3) C17 0.027(3) 0.021(3) 0.021(3) -0.006(2) -0.007(2) 0.007(3) C18 0.017(3) 0.024(3) 0.020(3) 0.002(2) 0.008(2) 0.005(2) C19 0.023(3) 0.028(3) 0.027(3) 0.006(3) 0.011(3) 0.012(3) C20 0.031(4) 0.029(4) 0.029(3) 0.001(3) 0.010(3) 0.013(3) C21 0.050(4) 0.023(3) 0.024(3) 0.001(3) 0.013(3) 0.010(3) C22 0.056(5) 0.027(4) 0.029(4) 0.011(3) 0.008(3) 0.016(3) C23 0.041(4) 0.030(4) 0.033(4) 0.013(3) 0.004(3) 0.011(3) C24 0.035(4) 0.024(3) 0.020(3) 0.005(3) 0.002(3) 0.012(3) C25 0.014(3) 0.020(3) 0.022(3) 0.000(2) 0.001(2) 0.002(2) C26 0.015(3) 0.022(3) 0.023(3) 0.004(2) 0.006(2) 0.001(2) C27 0.036(4) 0.034(4) 0.019(3) 0.001(3) 0.012(3) 0.011(3) C28 0.027(3) 0.028(3) 0.022(3) -0.002(3) 0.007(3) 0.010(3) C29 0.023(3) 0.025(3) 0.032(3) 0.004(3) 0.002(3) 0.011(3) C30 0.017(3) 0.026(3) 0.021(3) 0.003(2) 0.009(2) 0.011(2) C31 0.023(3) 0.026(3) 0.025(3) 0.008(3) 0.009(3) 0.006(3) C32 0.039(4) 0.034(4) 0.028(3) 0.012(3) 0.004(3) 0.009(3) C33 0.041(4) 0.041(4) 0.033(4) 0.019(3) 0.003(3) 0.004(3) C34 0.036(4) 0.026(4) 0.051(5) 0.017(3) 0.000(3) 0.008(3) C35 0.042(4) 0.027(4) 0.044(4) 0.011(3) 0.003(3) 0.014(3) C36 0.025(3) 0.025(3) 0.032(4) 0.004(3) 0.000(3) 0.007(3) C37 0.009(3) 0.021(3) 0.017(3) 0.003(2) -0.001(2) 0.004(2) C38 0.027(3) 0.026(3) 0.019(3) 0.008(3) 0.004(2) 0.004(3) C39 0.023(3) 0.023(3) 0.027(3) 0.003(3) 0.009(3) 0.007(3) C40 0.024(3) 0.030(4) 0.031(4) 0.002(3) -0.005(3) 0.013(3) C41 0.028(3) 0.031(4) 0.025(3) 0.006(3) -0.001(3) 0.010(3) C42 0.023(3) 0.020(3) 0.020(3) 0.006(2) 0.008(2) 0.006(2) C43 0.019(3) 0.018(3) 0.019(3) 0.002(2) 0.007(2) 0.004(2) C44 0.021(3) 0.023(3) 0.019(3) 0.003(2) -0.001(2) 0.005(2) C45 0.026(3) 0.030(4) 0.024(3) 0.005(3) -0.003(3) 0.004(3) C46 0.027(3) 0.021(3) 0.023(3) -0.003(3) -0.001(3) 0.005(3) C47 0.029(3) 0.020(3) 0.036(4) 0.012(3) 0.008(3) 0.011(3) C48 0.017(3) 0.027(3) 0.026(3) 0.000(3) 0.000(2) 0.003(2) C49 0.022(3) 0.019(3) 0.014(3) 0.003(2) 0.003(2) 0.001(2) C50 0.016(3) 0.029(3) 0.026(3) 0.009(3) 0.012(2) 0.003(2) C51 0.024(3) 0.053(5) 0.027(3) 0.016(3) 0.009(3) 0.013(3) C52 0.038(4) 0.052(5) 0.033(4) 0.023(3) 0.014(3) 0.029(4) C53 0.052(5) 0.033(4) 0.029(4) 0.011(3) 0.018(3) 0.026(3) C54 0.022(3) 0.026(3) 0.026(3) 0.004(3) 0.001(3) 0.008(3) C55 0.019(3) 0.023(3) 0.023(3) 0.001(3) 0.000(2) 0.008(2) C56 0.023(3) 0.033(4) 0.029(3) 0.007(3) 0.006(3) 0.007(3) C57 0.036(4) 0.038(4) 0.022(3) 0.008(3) 0.015(3) 0.011(3) C58 0.054(5) 0.035(4) 0.018(3) 0.009(3) 0.011(3) 0.019(3) C59 0.038(4) 0.028(4) 0.020(3) 0.002(3) -0.006(3) 0.007(3) C60 0.040(4) 0.029(4) 0.020(3) 0.003(3) 0.007(3) 0.013(3) C61 0.018(3) 0.018(3) 0.013(3) 0.000(2) 0.003(2) 0.006(2) C62 0.014(3) 0.025(3) 0.024(3) 0.007(2) 0.006(2) 0.008(2) C63 0.024(3) 0.030(3) 0.023(3) 0.003(3) 0.007(3) 0.012(3) C64 0.020(3) 0.031(4) 0.029(3) 0.003(3) 0.001(3) 0.010(3) C65 0.024(3) 0.028(4) 0.050(4) 0.016(3) 0.005(3) 0.013(3) C66 0.025(3) 0.025(3) 0.036(4) 0.015(3) 0.012(3) 0.005(3) C67 0.024(3) 0.018(3) 0.029(3) 0.011(3) 0.008(3) 0.005(2) C68 0.025(3) 0.027(3) 0.035(4) 0.004(3) 0.014(3) 0.004(3) C69 0.048(5) 0.042(4) 0.034(4) 0.010(3) 0.025(4) -0.001(4) C70 0.022(3) 0.036(4) 0.049(4) 0.020(3) 0.014(3) -0.001(3) C71 0.023(3) 0.024(3) 0.041(4) 0.008(3) 0.002(3) -0.004(3) C72 0.027(3) 0.025(3) 0.026(3) 0.011(3) 0.008(3) 0.004(3) C73 0.018(3) 0.024(3) 0.024(3) 0.005(3) 0.000(2) 0.010(2) C74 0.022(3) 0.035(4) 0.029(3) 0.017(3) 0.011(3) 0.015(3) C75 0.021(3) 0.021(3) 0.044(4) 0.016(3) 0.006(3) 0.004(3) C76 0.039(4) 0.028(4) 0.032(4) 0.001(3) -0.009(3) 0.016(3) C77 0.026(3) 0.033(4) 0.026(3) 0.009(3) 0.007(3) 0.011(3) C78 0.029(3) 0.026(3) 0.024(3) 0.011(3) 0.003(3) 0.007(3) C79 0.025(3) 0.022(3) 0.023(3) 0.004(2) 0.005(2) 0.009(3) C80 0.034(4) 0.033(4) 0.033(4) 0.005(3) 0.006(3) 0.017(3) C81 0.048(4) 0.032(4) 0.025(3) 0.014(3) 0.015(3) 0.012(3) C82 0.065(5) 0.028(4) 0.022(3) 0.003(3) -0.003(3) 0.015(4) C83 0.033(4) 0.025(3) 0.039(4) 0.002(3) -0.008(3) 0.008(3) C84 0.029(3) 0.030(4) 0.034(4) 0.009(3) 0.008(3) 0.016(3) C87 0.038(4) 0.034(4) 0.067(5) 0.015(4) 0.014(4) 0.018(3) N1S 0.093(7) 0.019(3) 0.042(5) 0.007(3) 0.029(4) 0.020(4) C1S 0.085(4) 0.087(4) 0.087(4) 0.0209(13) 0.0148(12) 0.0294(15) C2S 0.059(7) 0.057(7) 0.042(6) -0.004(5) 0.027(5) -0.019(5) _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 Sn1 O3 2.073(4) . ? Sn1 O12 2.095(4) . ? Sn1 O1 2.107(4) . ? Sn1 O10 2.110(4) . ? Sn1 O9 2.120(4) . ? Sn1 C1 2.149(5) . ? Sn1 Sn2 3.2820(11) . ? Sn1 Sn3 3.2827(8) . ? Sn2 O12 2.075(4) . ? Sn2 O4 2.090(4) . ? Sn2 O5 2.092(4) . ? Sn2 O11 2.118(4) . ? Sn2 O10 2.129(5) . ? Sn2 C13 2.132(5) . ? Sn2 Sn3 3.2712(8) . ? Sn3 O12 2.072(4) . ? Sn3 O2 2.095(4) . ? Sn3 O6 2.108(4) . ? Sn3 C25 2.127(6) . ? Sn3 O11 2.128(4) . ? Sn3 O9 2.160(4) . ? P1 O2 1.517(4) . ? P1 O1 1.523(4) . ? P1 C37 1.793(6) . ? P1 C43 1.814(6) . ? P2 O3 1.528(4) . ? P2 O4 1.529(4) . ? P2 C55 1.783(6) . ? P2 C49 1.785(6) . ? P3 O5 1.521(4) . ? P3 O6 1.530(4) . ? P3 C61 1.799(6) . ? P3 C67 1.804(6) . ? P4 O7 1.502(4) . ? P4 O8 1.510(4) . ? P4 C73 1.808(6) . ? P4 C79 1.821(6) . ? N1 N2 1.255(7) . ? N1 C2 1.429(8) . ? N2 C7 1.418(8) . ? N3 N4 1.262(7) . ? N3 C18 1.424(8) . ? N4 C19 1.426(8) . ? N5 N6 1.252(7) . ? N5 C26 1.433(8) . ? N6 C31 1.413(8) . ? Cl1 C87 1.756(8) . ? Cl2 C87 1.779(8) . ? C1 C6 1.397(8) . ? C1 C2 1.399(8) . ? C2 C3 1.403(8) . ? C3 C4 1.363(9) . ? C4 C5 1.379(9) . ? C5 C6 1.398(8) . ? C7 C8 1.378(9) . ? C7 C12 1.402(9) . ? C8 C9 1.373(10) . ? C9 C10 1.382(11) . ? C10 C11 1.377(10) . ? C11 C12 1.387(9) . ? C13 C18 1.390(8) . ? C13 C14 1.412(8) . ? C14 C15 1.387(8) . ? C15 C16 1.390(9) . ? C16 C17 1.375(9) . ? C17 C18 1.394(8) . ? C19 C20 1.390(9) . ? C19 C24 1.403(9) . ? C20 C21 1.386(10) . ? C21 C22 1.394(10) . ? C22 C23 1.382(9) . ? C23 C24 1.408(9) . ? C25 C30 1.379(8) . ? C25 C26 1.398(8) . ? C26 C27 1.402(8) . ? C27 C28 1.362(10) . ? C28 C29 1.414(9) . ? C29 C30 1.383(8) . ? C31 C32 1.392(9) . ? C31 C36 1.424(9) . ? C32 C33 1.381(10) . ? C33 C34 1.409(10) . ? C34 C35 1.387(10) . ? C35 C36 1.378(9) . ? C37 C38 1.376(8) . ? C37 C42 1.400(8) . ? C38 C39 1.397(9) . ? C39 C40 1.373(9) . ? C40 C41 1.390(9) . ? C41 C42 1.367(9) . ? C43 C44 1.389(8) . ? C43 C48 1.413(9) . ? C44 C45 1.395(8) . ? C45 C46 1.378(9) . ? C46 C47 1.413(9) . ? C47 C48 1.386(8) . ? C49 C50 1.392(8) . ? C49 C54 1.396(8) . ? C50 C51 1.412(10) . ? C51 C52 1.366(10) . ? C52 C53 1.396(10) . ? C53 C54 1.374(9) . ? C55 C60 1.387(9) . ? C55 C56 1.399(8) . ? C56 C57 1.396(8) . ? C57 C58 1.369(9) . ? C58 C59 1.368(9) . ? C59 C60 1.398(9) . ? C61 C66 1.382(8) . ? C61 C62 1.410(8) . ? C62 C63 1.382(8) . ? C63 C64 1.391(9) . ? C64 C65 1.381(9) . ? C65 C66 1.392(9) . ? C67 C72 1.390(8) . ? C67 C68 1.397(9) . ? C68 C69 1.380(9) . ? C69 C70 1.377(10) . ? C70 C71 1.394(10) . ? C71 C72 1.370(8) . ? C73 C74 1.395(9) . ? C73 C78 1.399(8) . ? C74 C75 1.396(9) . ? C75 C76 1.389(9) . ? C76 C77 1.404(9) . ? C77 C78 1.383(9) . ? C79 C80 1.382(9) . ? C79 C84 1.400(9) . ? C80 C81 1.395(9) . ? C81 C82 1.356(11) . ? C82 C83 1.393(10) . ? C83 C84 1.394(9) . ? N1S C2S 0.976(12) . ? C1S C2S 1.558(13) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O3 Sn1 O12 86.10(15) . . ? O3 Sn1 O1 89.88(15) . . ? O12 Sn1 O1 85.91(14) . . ? O3 Sn1 O10 88.25(18) . . ? O12 Sn1 O10 76.80(16) . . ? O1 Sn1 O10 162.69(16) . . ? O3 Sn1 O9 163.66(15) . . ? O12 Sn1 O9 77.80(14) . . ? O1 Sn1 O9 86.25(15) . . ? O10 Sn1 O9 90.74(18) . . ? O3 Sn1 C1 95.44(18) . . ? O12 Sn1 C1 178.25(17) . . ? O1 Sn1 C1 93.27(19) . . ? O10 Sn1 C1 104.0(2) . . ? O9 Sn1 C1 100.62(17) . . ? O3 Sn1 Sn2 81.29(11) . . ? O12 Sn1 Sn2 37.88(10) . . ? O1 Sn1 Sn2 123.27(11) . . ? O10 Sn1 Sn2 39.48(13) . . ? O9 Sn1 Sn2 87.58(10) . . ? C1 Sn1 Sn2 143.15(15) . . ? O3 Sn1 Sn3 123.31(11) . . ? O12 Sn1 Sn3 37.79(10) . . ? O1 Sn1 Sn3 80.87(10) . . ? O10 Sn1 Sn3 85.81(12) . . ? O9 Sn1 Sn3 40.37(10) . . ? C1 Sn1 Sn3 140.55(14) . . ? Sn2 Sn1 Sn3 59.775(19) . . ? O12 Sn2 O4 83.44(15) . . ? O12 Sn2 O5 85.79(15) . . ? O4 Sn2 O5 88.40(16) . . ? O12 Sn2 O11 77.25(14) . . ? O4 Sn2 O11 160.39(15) . . ? O5 Sn2 O11 86.81(15) . . ? O12 Sn2 O10 76.80(16) . . ? O4 Sn2 O10 88.41(18) . . ? O5 Sn2 O10 162.55(16) . . ? O11 Sn2 O10 90.47(18) . . ? O12 Sn2 C13 170.87(19) . . ? O4 Sn2 C13 98.24(18) . . ? O5 Sn2 C13 103.20(19) . . ? O11 Sn2 C13 101.37(18) . . ? O10 Sn2 C13 94.2(2) . . ? O12 Sn2 Sn3 37.90(10) . . ? O4 Sn2 Sn3 120.70(11) . . ? O5 Sn2 Sn3 81.10(10) . . ? O11 Sn2 Sn3 39.72(11) . . ? O10 Sn2 Sn3 85.80(13) . . ? C13 Sn2 Sn3 141.03(15) . . ? O12 Sn2 Sn1 38.31(10) . . ? O4 Sn2 Sn1 79.71(11) . . ? O5 Sn2 Sn1 123.52(11) . . ? O11 Sn2 Sn1 87.13(10) . . ? O10 Sn2 Sn1 39.05(12) . . ? C13 Sn2 Sn1 133.00(16) . . ? Sn3 Sn2 Sn1 60.123(14) . . ? O12 Sn3 O2 84.22(15) . . ? O12 Sn3 O6 86.45(15) . . ? O2 Sn3 O6 92.62(15) . . ? O12 Sn3 C25 172.12(19) . . ? O2 Sn3 C25 96.80(19) . . ? O6 Sn3 C25 101.28(19) . . ? O12 Sn3 O11 77.08(15) . . ? O2 Sn3 O11 161.18(15) . . ? O6 Sn3 O11 84.15(15) . . ? C25 Sn3 O11 102.02(19) . . ? O12 Sn3 O9 77.40(14) . . ? O2 Sn3 O9 85.90(15) . . ? O6 Sn3 O9 163.85(14) . . ? C25 Sn3 O9 94.86(19) . . ? O11 Sn3 O9 92.06(15) . . ? O12 Sn3 Sn2 37.97(10) . . ? O2 Sn3 Sn2 121.69(10) . . ? O6 Sn3 Sn2 79.88(10) . . ? C25 Sn3 Sn2 141.49(15) . . ? O11 Sn3 Sn2 39.49(10) . . ? O9 Sn3 Sn2 87.21(10) . . ? O12 Sn3 Sn1 38.28(10) . . ? O2 Sn3 Sn1 79.59(11) . . ? O6 Sn3 Sn1 124.45(11) . . ? C25 Sn3 Sn1 134.15(16) . . ? O11 Sn3 Sn1 86.95(11) . . ? O9 Sn3 Sn1 39.48(10) . . ? Sn2 Sn3 Sn1 60.10(2) . . ? O2 P1 O1 115.4(2) . . ? O2 P1 C37 109.0(2) . . ? O1 P1 C37 109.3(2) . . ? O2 P1 C43 107.1(2) . . ? O1 P1 C43 108.1(2) . . ? C37 P1 C43 107.6(3) . . ? O3 P2 O4 116.3(2) . . ? O3 P2 C55 108.0(3) . . ? O4 P2 C55 106.9(3) . . ? O3 P2 C49 107.5(3) . . ? O4 P2 C49 109.7(3) . . ? C55 P2 C49 108.1(3) . . ? O5 P3 O6 115.4(2) . . ? O5 P3 C61 109.4(2) . . ? O6 P3 C61 109.6(2) . . ? O5 P3 C67 106.4(3) . . ? O6 P3 C67 109.4(3) . . ? C61 P3 C67 106.2(3) . . ? O7 P4 O8 116.5(3) . . ? O7 P4 C73 109.6(3) . . ? O8 P4 C73 108.5(3) . . ? O7 P4 C79 110.6(3) . . ? O8 P4 C79 105.8(3) . . ? C73 P4 C79 105.3(3) . . ? P1 O1 Sn1 130.7(2) . . ? P1 O2 Sn3 132.9(2) . . ? P2 O3 Sn1 130.6(2) . . ? P2 O4 Sn2 131.7(2) . . ? P3 O5 Sn2 130.1(2) . . ? P3 O6 Sn3 130.1(2) . . ? Sn1 O9 Sn3 100.15(15) . . ? Sn1 O10 Sn2 101.5(2) . . ? Sn2 O11 Sn3 100.79(17) . . ? Sn3 O12 Sn2 104.13(16) . . ? Sn3 O12 Sn1 103.94(16) . . ? Sn2 O12 Sn1 103.81(16) . . ? N2 N1 C2 114.5(5) . . ? N1 N2 C7 116.2(5) . . ? N4 N3 C18 115.4(5) . . ? N3 N4 C19 113.0(5) . . ? N6 N5 C26 114.2(5) . . ? N5 N6 C31 113.5(5) . . ? C6 C1 C2 118.2(5) . . ? C6 C1 Sn1 116.8(4) . . ? C2 C1 Sn1 124.9(4) . . ? C1 C2 C3 120.4(5) . . ? C1 C2 N1 117.9(5) . . ? C3 C2 N1 121.7(5) . . ? C4 C3 C2 120.5(6) . . ? C3 C4 C5 120.1(6) . . ? C4 C5 C6 120.3(6) . . ? C1 C6 C5 120.4(6) . . ? C8 C7 C12 119.7(6) . . ? C8 C7 N2 116.5(6) . . ? C12 C7 N2 123.7(6) . . ? C9 C8 C7 120.8(7) . . ? C8 C9 C10 120.2(7) . . ? C11 C10 C9 119.4(7) . . ? C10 C11 C12 121.3(7) . . ? C11 C12 C7 118.5(6) . . ? C18 C13 C14 118.2(5) . . ? C18 C13 Sn2 123.9(5) . . ? C14 C13 Sn2 117.9(4) . . ? C15 C14 C13 120.5(6) . . ? C14 C15 C16 119.9(6) . . ? C17 C16 C15 120.3(6) . . ? C16 C17 C18 120.0(6) . . ? C13 C18 C17 121.0(6) . . ? C13 C18 N3 114.5(5) . . ? C17 C18 N3 124.5(5) . . ? C20 C19 C24 120.6(6) . . ? C20 C19 N4 115.8(6) . . ? C24 C19 N4 123.6(6) . . ? C21 C20 C19 118.8(6) . . ? C20 C21 C22 121.6(6) . . ? C23 C22 C21 119.3(7) . . ? C22 C23 C24 120.2(7) . . ? C19 C24 C23 119.2(6) . . ? C30 C25 C26 118.4(5) . . ? C30 C25 Sn3 119.7(4) . . ? C26 C25 Sn3 121.6(5) . . ? C25 C26 C27 120.3(6) . . ? C25 C26 N5 116.2(5) . . ? C27 C26 N5 123.5(6) . . ? C28 C27 C26 120.7(6) . . ? C27 C28 C29 119.5(6) . . ? C30 C29 C28 119.3(6) . . ? C25 C30 C29 121.8(6) . . ? C32 C31 N6 116.1(6) . . ? C32 C31 C36 119.3(6) . . ? N6 C31 C36 124.6(6) . . ? C33 C32 C31 120.5(7) . . ? C32 C33 C34 120.1(7) . . ? C35 C34 C33 119.8(7) . . ? C36 C35 C34 120.6(7) . . ? C35 C36 C31 119.8(6) . . ? C38 C37 C42 120.1(5) . . ? C38 C37 P1 121.4(5) . . ? C42 C37 P1 118.5(4) . . ? C37 C38 C39 119.1(6) . . ? C40 C39 C38 120.9(6) . . ? C39 C40 C41 119.5(6) . . ? C42 C41 C40 120.4(6) . . ? C41 C42 C37 120.0(6) . . ? C44 C43 C48 120.1(5) . . ? C44 C43 P1 122.2(5) . . ? C48 C43 P1 117.6(4) . . ? C43 C44 C45 120.2(6) . . ? C46 C45 C44 119.8(6) . . ? C45 C46 C47 120.9(6) . . ? C48 C47 C46 119.3(6) . . ? C47 C48 C43 119.7(6) . . ? C50 C49 C54 120.3(6) . . ? C50 C49 P2 120.3(5) . . ? C54 C49 P2 119.3(4) . . ? C49 C50 C51 119.1(6) . . ? C52 C51 C50 120.7(6) . . ? C51 C52 C53 119.1(6) . . ? C54 C53 C52 121.7(7) . . ? C53 C54 C49 119.1(6) . . ? C60 C55 C56 120.2(6) . . ? C60 C55 P2 121.5(5) . . ? C56 C55 P2 118.3(5) . . ? C57 C56 C55 118.7(6) . . ? C58 C57 C56 120.8(6) . . ? C59 C58 C57 120.5(6) . . ? C58 C59 C60 120.2(6) . . ? C55 C60 C59 119.5(6) . . ? C66 C61 C62 118.7(6) . . ? C66 C61 P3 122.7(4) . . ? C62 C61 P3 118.5(4) . . ? C63 C62 C61 120.3(6) . . ? C62 C63 C64 119.8(6) . . ? C65 C64 C63 120.7(6) . . ? C64 C65 C66 119.2(6) . . ? C61 C66 C65 121.3(6) . . ? C72 C67 C68 119.7(6) . . ? C72 C67 P3 119.5(5) . . ? C68 C67 P3 120.6(5) . . ? C69 C68 C67 118.9(6) . . ? C70 C69 C68 121.2(7) . . ? C69 C70 C71 119.9(6) . . ? C72 C71 C70 119.3(6) . . ? C71 C72 C67 121.0(6) . . ? C74 C73 C78 118.1(6) . . ? C74 C73 P4 119.5(5) . . ? C78 C73 P4 122.4(5) . . ? C73 C74 C75 121.2(6) . . ? C76 C75 C74 119.5(6) . . ? C75 C76 C77 120.4(6) . . ? C78 C77 C76 119.0(6) . . ? C77 C78 C73 121.9(6) . . ? C80 C79 C84 119.6(6) . . ? C80 C79 P4 120.2(5) . . ? C84 C79 P4 120.2(5) . . ? C79 C80 C81 120.2(6) . . ? C82 C81 C80 120.1(6) . . ? C81 C82 C83 120.9(6) . . ? C82 C83 C84 119.6(7) . . ? C83 C84 C79 119.5(6) . . ? Cl1 C87 Cl2 110.8(4) . . ? N1S C2S C1S 178.8(13) . . ? _diffrn_measured_fraction_theta_max 0.977 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.977 _refine_diff_density_max 2.918 _refine_diff_density_min -1.005 _refine_diff_density_rms 0.180 _database_code_depnum_ccdc_archive 'CCDC 968925'