# Electronic Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full Chem.Commun. _journal_coden_cambridge 0182 #TrackingRef 'ccdc_sub.cif' loop_ _publ_author_name _publ_author_address C.Drost ; Institut f\"ur Anorganische Chemie Universit\"at Leipzig Johannisallee 29 04103 Leipzig Bundesrepublik Deutschland ; P.Lonnecke ; Institut f\"ur Anorganische Chemie Universit\"at Leipzig Johannisallee 29 04103 Leipzig Bundesrepublik Deutschland ; J.Sieler ; Institut f\"ur Anorganische Chemie Universit\"at Leipzig Johannisallee 29 04103 Leipzig Bundesrepublik Deutschland ; _publ_contact_author ; Christian Drost Structure Determination: Peter L\"onnecke Institut f\"ur Anorganische Chemie Universit\"at Leipzig Johannisallee 29 04103 Leipzig Bundesrepublik Deutschland and Joachim Sieler Institut f\"ur Anorganische Chemie Universit\"at Leipzig Johannisallee 29 04103 Leipzig Bundesrepublik Deutschland ; _publ_contact_author_phone '49 / 341 / 9736130' _publ_contact_author_fax '49 / 341 / 9736199' _publ_contact_author_email cdrost@uni-leipzig.de _publ_section_title ; Stannylplumbylenes: bonding between tetravalent tin and divalent lead ; _publ_contact_author_name 'Christian Drost' #------------------------------------------------------------------------------# # DATA BLOCK # #------------------------------------------------------------------------------# #\#CIF_1.1 data_s047_fin _database_code_depnum_ccdc_archive 'CCDC 864028' #TrackingRef 'ccdc_sub.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C51 H75 O8 Pb Sn' _chemical_formula_weight 1141.99 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Pb Pb -3.3944 10.1111 '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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 26.9800(17) _cell_length_b 12.5178(6) _cell_length_c 31.719(2) _cell_angle_alpha 90.00 _cell_angle_beta 97.596(8) _cell_angle_gamma 90.00 _cell_volume 10618.3(11) _cell_formula_units_Z 8 _cell_measurement_temperature 213(2) _cell_measurement_reflns_used 8000 _cell_measurement_theta_min 1.95 _cell_measurement_theta_max 24.95 _exptl_crystal_description prism _exptl_crystal_colour 'dark violet' _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.429 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4616 _exptl_absorpt_coefficient_mu 3.684 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.3565 _exptl_absorpt_correction_T_max 0.4791 _exptl_absorpt_process_details 'STOE X-RED Software' _exptl_special_details ; ? ; _diffrn_ambient_temperature 213(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Stoe IPDS area detector' _diffrn_measurement_method '\f scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 61579 _diffrn_reflns_av_R_equivalents 0.0580 _diffrn_reflns_av_sigmaI/netI 0.0769 _diffrn_reflns_limit_h_min -31 _diffrn_reflns_limit_h_max 32 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -37 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 1.94 _diffrn_reflns_theta_max 24.98 _reflns_number_total 18514 _reflns_number_gt 11308 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'STOE IPDS software' _computing_cell_refinement 'STOE IPDS software' _computing_data_reduction 'STOE IPDS software, STOE X-RED' _computing_structure_solution SHELXS-97 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP3 for Windows (L. J. Farrugia, 1997)' _computing_publication_material 'WINGX (L.J. Farrugia,1999)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0269P)^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 18514 _refine_ls_number_parameters 1168 _refine_ls_number_restraints 96 _refine_ls_R_factor_all 0.0575 _refine_ls_R_factor_gt 0.0296 _refine_ls_wR_factor_ref 0.0608 _refine_ls_wR_factor_gt 0.0574 _refine_ls_goodness_of_fit_ref 0.733 _refine_ls_restrained_S_all 0.735 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pb1 Pb 0.114554(6) 0.176877(17) 0.611308(6) 0.04416(5) Uani 1 1 d . . . Sn1 Sn 0.045479(10) 0.05809(3) 0.654977(9) 0.03869(8) Uani 1 1 d . . . O1 O 0.02894(11) 0.3023(3) 0.62534(10) 0.0536(9) Uani 1 1 d . . . O2 O -0.02000(12) 0.0790(3) 0.73258(10) 0.0622(10) Uani 1 1 d . . . O3 O 0.10239(12) 0.0881(3) 0.74257(10) 0.0600(10) Uani 1 1 d . . . O4 O 0.02935(14) -0.2014(3) 0.66502(11) 0.0688(11) Uani 1 1 d . . . O5 O -0.07457(10) 0.0242(3) 0.63332(10) 0.0540(9) Uani 1 1 d . . . O6 O 0.07065(10) -0.0553(3) 0.57369(10) 0.0537(9) Uani 1 1 d . . . O7 O 0.19889(12) 0.0365(3) 0.66006(11) 0.0655(10) Uani 1 1 d . . . O8 O 0.15234(12) 0.3924(3) 0.66351(12) 0.0673(11) Uani 1 1 d . . . C1 C 0.00519(15) 0.1901(4) 0.68034(13) 0.0383(11) Uani 1 1 d . . . C2 C 0.00583(17) 0.2892(4) 0.66212(15) 0.0499(13) Uani 1 1 d . . . C3 C -0.0141(2) 0.3794(5) 0.67945(19) 0.0698(16) Uani 1 1 d . . . H3 H -0.0123 0.4470 0.6669 0.084 Uiso 1 1 calc R . . C4 C -0.0369(2) 0.3661(6) 0.7158(2) 0.0812(19) Uani 1 1 d . . . H4 H -0.0510 0.4255 0.7279 0.097 Uiso 1 1 calc R . . C5 C -0.0390(2) 0.2680(6) 0.73436(18) 0.0683(17) Uani 1 1 d . . . H5 H -0.0545 0.2603 0.7590 0.082 Uiso 1 1 calc R . . C6 C -0.01839(17) 0.1804(5) 0.71691(15) 0.0537(13) Uani 1 1 d . . . C7 C -0.00357(19) 0.3450(5) 0.58867(16) 0.0602(15) Uani 1 1 d D . . H7 H -0.0222 0.4068 0.5981 0.072 Uiso 1 1 calc R . . C8 C 0.0283(2) 0.3822(6) 0.5572(2) 0.097(2) Uani 1 1 d D . . H8A H 0.0549 0.4271 0.5712 0.145 Uiso 1 1 calc R . . H8B H 0.0083 0.4229 0.5352 0.145 Uiso 1 1 calc R . . H8C H 0.0428 0.3210 0.5446 0.145 Uiso 1 1 calc R . . C9 C -0.0403(2) 0.2608(6) 0.57112(19) 0.096(2) Uani 1 1 d D . . H9A H -0.0225 0.2020 0.5600 0.144 Uiso 1 1 calc R . . H9B H -0.0638 0.2911 0.5484 0.144 Uiso 1 1 calc R . . H9C H -0.0584 0.2349 0.5936 0.144 Uiso 1 1 calc R . . C10 C -0.04325(19) 0.0582(6) 0.77011(16) 0.0720(18) Uani 1 1 d . . . H10 H -0.0753 0.0976 0.7684 0.086 Uiso 1 1 calc R . . C11 C -0.0086(2) 0.0929(7) 0.80980(19) 0.099(3) Uani 1 1 d . . . H11A H 0.0203 0.0463 0.8139 0.149 Uiso 1 1 calc R . . H11B H -0.0264 0.0885 0.8344 0.149 Uiso 1 1 calc R . . H11C H 0.0022 0.1659 0.8063 0.149 Uiso 1 1 calc R . . C12 C -0.0530(2) -0.0590(6) 0.7697(2) 0.096(2) Uani 1 1 d . . . H12A H -0.0768 -0.0770 0.7451 0.145 Uiso 1 1 calc R . . H12B H -0.0665 -0.0791 0.7954 0.145 Uiso 1 1 calc R . . H12C H -0.0219 -0.0972 0.7683 0.145 Uiso 1 1 calc R . . C13 C 0.06584(15) -0.0577(4) 0.70561(14) 0.0436(12) Uani 1 1 d . . . C14 C 0.09224(17) -0.0183(5) 0.74290(15) 0.0497(13) Uani 1 1 d . . . C15 C 0.10579(18) -0.0845(5) 0.77746(16) 0.0617(15) Uani 1 1 d . . . H15 H 0.1237 -0.0574 0.8026 0.074 Uiso 1 1 calc R . . C16 C 0.09265(19) -0.1901(6) 0.77423(18) 0.0703(17) Uani 1 1 d . . . H16 H 0.1012 -0.2348 0.7979 0.084 Uiso 1 1 calc R . . C17 C 0.06745(19) -0.2328(5) 0.73772(18) 0.0647(15) Uani 1 1 d . . . H17 H 0.0594 -0.3059 0.7359 0.078 Uiso 1 1 calc R . . C18 C 0.05417(16) -0.1651(5) 0.70352(16) 0.0532(13) Uani 1 1 d . . . C19 C 0.12413(19) 0.1421(5) 0.78047(16) 0.0603(15) Uani 1 1 d . . . H19 H 0.1086 0.1158 0.8051 0.072 Uiso 1 1 calc R . . C20 C 0.17998(19) 0.1251(6) 0.78873(18) 0.082(2) Uani 1 1 d . . . H20A H 0.1871 0.0493 0.7911 0.123 Uiso 1 1 calc R . . H20B H 0.1933 0.1605 0.8150 0.123 Uiso 1 1 calc R . . H20C H 0.1954 0.1548 0.7654 0.123 Uiso 1 1 calc R . . C21 C 0.1114(2) 0.2572(5) 0.7730(2) 0.0810(19) Uani 1 1 d . . . H21A H 0.1243 0.2813 0.7475 0.122 Uiso 1 1 calc R . . H21B H 0.1262 0.2991 0.7971 0.122 Uiso 1 1 calc R . . H21C H 0.0753 0.2659 0.7694 0.122 Uiso 1 1 calc R . . C22 C 0.0009(2) -0.2971(5) 0.66340(19) 0.0716(17) Uani 1 1 d . . . H22 H 0.0222 -0.3553 0.6769 0.086 Uiso 1 1 calc R . . C23 C -0.0126(3) -0.3218(5) 0.6169(2) 0.096(2) Uani 1 1 d . . . H23A H -0.0309 -0.2621 0.6029 0.143 Uiso 1 1 calc R . . H23B H -0.0334 -0.3853 0.6138 0.143 Uiso 1 1 calc R . . H23C H 0.0176 -0.3339 0.6042 0.143 Uiso 1 1 calc R . . C24 C -0.0443(2) -0.2852(7) 0.6861(3) 0.114(3) Uani 1 1 d . . . H24A H -0.0337 -0.2721 0.7161 0.172 Uiso 1 1 calc R . . H24B H -0.0640 -0.3502 0.6828 0.172 Uiso 1 1 calc R . . H24C H -0.0643 -0.2256 0.6740 0.172 Uiso 1 1 calc R . . C25 C -0.00280(15) -0.0169(4) 0.60283(13) 0.0389(11) Uani 1 1 d . . . C26 C -0.05479(16) -0.0186(4) 0.59966(15) 0.0443(12) Uani 1 1 d . . . C27 C -0.08427(17) -0.0625(4) 0.56424(16) 0.0544(13) Uani 1 1 d . . . H27 H -0.1193 -0.0625 0.5623 0.065 Uiso 1 1 calc R . . C28 C -0.06062(19) -0.1057(4) 0.53225(16) 0.0588(15) Uani 1 1 d . . . H28 H -0.0801 -0.1364 0.5086 0.071 Uiso 1 1 calc R . . C29 C -0.00937(19) -0.1052(4) 0.53386(15) 0.0547(14) Uani 1 1 d . . . H29 H 0.0060 -0.1346 0.5116 0.066 Uiso 1 1 calc R . . C30 C 0.01921(16) -0.0601(4) 0.56927(14) 0.0463(12) Uani 1 1 d . . . C31 C -0.12767(16) 0.0375(5) 0.63123(18) 0.0627(16) Uani 1 1 d . . . H31 H -0.1418 0.0587 0.6020 0.075 Uiso 1 1 calc R . . C32 C -0.1519(2) -0.0655(6) 0.6431(2) 0.087(2) Uani 1 1 d . . . H32A H -0.1454 -0.1214 0.6234 0.130 Uiso 1 1 calc R . . H32B H -0.1877 -0.0550 0.6416 0.130 Uiso 1 1 calc R . . H32C H -0.1382 -0.0860 0.6717 0.130 Uiso 1 1 calc R . . C33 C -0.13520(19) 0.1273(5) 0.66196(19) 0.0743(18) Uani 1 1 d . . . H33A H -0.1238 0.1044 0.6908 0.111 Uiso 1 1 calc R . . H33B H -0.1704 0.1456 0.6594 0.111 Uiso 1 1 calc R . . H33C H -0.1162 0.1894 0.6552 0.111 Uiso 1 1 calc R . . C34 C 0.09760(19) -0.1067(5) 0.54307(16) 0.0579(15) Uani 1 1 d . . . H34 H 0.0799 -0.0930 0.5142 0.069 Uiso 1 1 calc R . . C35 C 0.1010(2) -0.2251(5) 0.5501(2) 0.0840(19) Uani 1 1 d . . . H35A H 0.1164 -0.2394 0.5789 0.126 Uiso 1 1 calc R . . H35B H 0.1210 -0.2567 0.5301 0.126 Uiso 1 1 calc R . . H35C H 0.0677 -0.2557 0.5459 0.126 Uiso 1 1 calc R . . C36 C 0.14816(18) -0.0534(5) 0.54717(17) 0.0706(17) Uani 1 1 d . . . H36A H 0.1440 0.0218 0.5402 0.106 Uiso 1 1 calc R . . H36B H 0.1684 -0.0869 0.5278 0.106 Uiso 1 1 calc R . . H36C H 0.1646 -0.0608 0.5761 0.106 Uiso 1 1 calc R . . C37 C 0.17789(16) 0.2155(5) 0.66433(14) 0.0466(13) Uani 1 1 d . . . C38 C 0.21246(18) 0.1357(5) 0.67636(15) 0.0540(14) Uani 1 1 d . . . C39 C 0.25735(18) 0.1570(6) 0.70275(17) 0.0682(18) Uani 1 1 d . . . H39 H 0.2810 0.1030 0.7107 0.082 Uiso 1 1 calc R . . C40 C 0.26505(19) 0.2610(7) 0.71647(18) 0.076(2) Uani 1 1 d . . . H40 H 0.2950 0.2770 0.7340 0.091 Uiso 1 1 calc R . . C41 C 0.23145(18) 0.3432(5) 0.70593(16) 0.0650(16) Uani 1 1 d . . . H41 H 0.2373 0.4126 0.7167 0.078 Uiso 1 1 calc R . . C42 C 0.18849(17) 0.3174(5) 0.67855(15) 0.0545(13) Uani 1 1 d . . . C43 C 0.2282(2) -0.0558(6) 0.67474(18) 0.0744(17) Uani 1 1 d . . . H43 H 0.2417 -0.0462 0.7051 0.089 Uiso 1 1 calc R . . C44 C 0.1930(2) -0.1493(6) 0.6703(2) 0.089(2) Uani 1 1 d . . . H44A H 0.1646 -0.1342 0.6852 0.134 Uiso 1 1 calc R . . H44B H 0.2102 -0.2124 0.6825 0.134 Uiso 1 1 calc R . . H44C H 0.1814 -0.1617 0.6404 0.134 Uiso 1 1 calc R . . C45 C 0.2709(2) -0.0678(6) 0.6489(2) 0.101(2) Uani 1 1 d . . . H45A H 0.2577 -0.0827 0.6195 0.151 Uiso 1 1 calc R . . H45B H 0.2923 -0.1262 0.6602 0.151 Uiso 1 1 calc R . . H45C H 0.2902 -0.0022 0.6503 0.151 Uiso 1 1 calc R . . C46 C 0.1566(2) 0.5020(5) 0.67718(19) 0.0678(16) Uani 1 1 d . . . H46 H 0.1915 0.5269 0.6783 0.081 Uiso 1 1 calc R . . C47 C 0.1391(3) 0.5133(6) 0.7205(2) 0.100(2) Uani 1 1 d . . . H47A H 0.1055 0.4849 0.7194 0.150 Uiso 1 1 calc R . . H47B H 0.1392 0.5882 0.7284 0.150 Uiso 1 1 calc R . . H47C H 0.1615 0.4740 0.7414 0.150 Uiso 1 1 calc R . . C48 C 0.1227(3) 0.5634(6) 0.6434(2) 0.114(3) Uani 1 1 d . . . H48A H 0.1367 0.5616 0.6168 0.171 Uiso 1 1 calc R . . H48B H 0.1199 0.6369 0.6525 0.171 Uiso 1 1 calc R . . H48C H 0.0898 0.5307 0.6394 0.171 Uiso 1 1 calc R . . Pb2 Pb 0.618106(7) 0.57000(2) 0.604739(6) 0.05928(7) Uani 1 1 d . . . Sn2 Sn 0.684924(11) 0.54258(3) 0.542155(10) 0.04757(9) Uani 1 1 d . A . O9 O 0.64792(13) 0.7756(3) 0.54959(15) 0.0838(13) Uani 1 1 d D . . O10 O 0.79199(13) 0.6080(3) 0.51388(12) 0.0683(11) Uani 1 1 d . . . O11 O 0.67285(17) 0.6149(5) 0.44502(12) 0.115(2) Uani 1 1 d D . . O12 O 0.58531(15) 0.4165(4) 0.53424(15) 0.1015(16) Uani 1 1 d . . . O13 O 0.77597(12) 0.5096(3) 0.60406(12) 0.0673(11) Uani 1 1 d . . . O14 O 0.69775(16) 0.3213(4) 0.48737(15) 0.1007(16) Uani 1 1 d D . . O15 O 0.6639(2) 0.3360(6) 0.6585(3) 0.141(2) Uani 1 1 d . . . O16 O 0.6663(2) 0.6997(6) 0.67095(16) 0.1209(19) Uani 1 1 d . . . C49 C 0.72126(17) 0.6935(5) 0.53285(15) 0.0531(13) Uani 1 1 d . . . C50 C 0.69651(19) 0.7871(6) 0.53900(19) 0.0706(17) Uani 1 1 d . A . C51 C 0.7179(2) 0.8866(6) 0.5359(2) 0.094(2) Uani 1 1 d . . . H51 H 0.7003 0.9493 0.5407 0.113 Uiso 1 1 calc R A . C52 C 0.7660(2) 0.8907(6) 0.5255(2) 0.095(2) Uani 1 1 d . A . H52 H 0.7811 0.9577 0.5230 0.114 Uiso 1 1 calc R . . C53 C 0.7922(2) 0.8008(6) 0.5187(2) 0.0759(18) Uani 1 1 d . . . H53 H 0.8250 0.8060 0.5120 0.091 Uiso 1 1 calc R A . C54 C 0.77020(18) 0.7018(5) 0.52184(16) 0.0559(14) Uani 1 1 d . A . C55 C 0.6096(4) 0.8528(10) 0.5378(4) 0.086(3) Uiso 0.648(13) 1 d PD A 1 H55 H 0.6225 0.9240 0.5474 0.103 Uiso 0.648(13) 1 calc PR A 1 C56 C 0.5999(5) 0.8531(18) 0.4919(4) 0.164(9) Uani 0.648(13) 1 d PD A 1 H56A H 0.6303 0.8707 0.4803 0.246 Uiso 0.648(13) 1 calc PR A 1 H56B H 0.5744 0.9058 0.4827 0.246 Uiso 0.648(13) 1 calc PR A 1 H56C H 0.5883 0.7830 0.4820 0.246 Uiso 0.648(13) 1 calc PR A 1 C57 C 0.5647(4) 0.8277(13) 0.5598(4) 0.119(6) Uani 0.648(13) 1 d PD A 1 H57A H 0.5736 0.8344 0.5903 0.179 Uiso 0.648(13) 1 calc PR A 1 H57B H 0.5536 0.7552 0.5529 0.179 Uiso 0.648(13) 1 calc PR A 1 H57C H 0.5379 0.8772 0.5502 0.179 Uiso 0.648(13) 1 calc PR A 1 C55F C 0.6125(6) 0.8504(14) 0.5242(7) 0.086(3) Uiso 0.352(13) 1 d PD A 2 H55F H 0.6294 0.8874 0.5024 0.103 Uiso 0.352(13) 1 calc PR A 2 C57F C 0.5977(10) 0.927(2) 0.5552(9) 0.146(13) Uani 0.352(13) 1 d PD A 2 H57D H 0.6267 0.9686 0.5671 0.219 Uiso 0.352(13) 1 calc PR A 2 H57E H 0.5842 0.8894 0.5777 0.219 Uiso 0.352(13) 1 calc PR A 2 H57F H 0.5724 0.9752 0.5411 0.219 Uiso 0.352(13) 1 calc PR A 2 C56F C 0.5686(7) 0.7853(16) 0.5032(8) 0.100(9) Uani 0.352(13) 1 d PD A 2 H56D H 0.5802 0.7345 0.4836 0.150 Uiso 0.352(13) 1 calc PR A 2 H56E H 0.5441 0.8326 0.4878 0.150 Uiso 0.352(13) 1 calc PR A 2 H56F H 0.5534 0.7471 0.5248 0.150 Uiso 0.352(13) 1 calc PR A 2 C58 C 0.84085(19) 0.6064(5) 0.50040(18) 0.0701(17) Uani 1 1 d . . . H58 H 0.8439 0.6645 0.4797 0.084 Uiso 1 1 calc R . . C59 C 0.8807(2) 0.6175(6) 0.5383(2) 0.084(2) Uani 1 1 d . . . H59A H 0.8745 0.6816 0.5540 0.126 Uiso 1 1 calc R . . H59B H 0.9132 0.6224 0.5286 0.126 Uiso 1 1 calc R . . H59C H 0.8798 0.5557 0.5566 0.126 Uiso 1 1 calc R . . C60 C 0.8438(2) 0.4987(6) 0.4792(2) 0.100(2) Uani 1 1 d . . . H60A H 0.8389 0.4426 0.4994 0.150 Uiso 1 1 calc R . . H60B H 0.8763 0.4905 0.4698 0.150 Uiso 1 1 calc R . . H60C H 0.8180 0.4939 0.4549 0.150 Uiso 1 1 calc R . . C61 C 0.62785(17) 0.5167(5) 0.48806(16) 0.0627(16) Uani 1 1 d . . . C62 C 0.63010(19) 0.5608(7) 0.44869(17) 0.082(2) Uani 1 1 d . A . C63 C 0.5913(3) 0.5460(8) 0.4154(2) 0.118(3) Uani 1 1 d . . . H63 H 0.5927 0.5761 0.3885 0.141 Uiso 1 1 calc R A . C64 C 0.5511(3) 0.4862(9) 0.4235(3) 0.134(4) Uani 1 1 d . A . H64 H 0.5250 0.4748 0.4012 0.160 Uiso 1 1 calc R . . C65 C 0.5471(2) 0.4430(9) 0.4614(3) 0.124(3) Uani 1 1 d . . . H65 H 0.5184 0.4043 0.4658 0.149 Uiso 1 1 calc R A . C66 C 0.5860(2) 0.4565(6) 0.4941(2) 0.085(2) Uani 1 1 d . A . C67 C 0.6840(5) 0.6453(13) 0.4034(4) 0.086(3) Uiso 0.586(14) 1 d PD B 1 H67 H 0.6697 0.5967 0.3804 0.104 Uiso 0.586(14) 1 calc PR B 1 C68 C 0.7383(4) 0.658(2) 0.4062(4) 0.161(11) Uani 0.586(14) 1 d PD B 1 H68A H 0.7489 0.7171 0.4252 0.241 Uiso 0.586(14) 1 calc PR B 1 H68B H 0.7472 0.6735 0.3782 0.241 Uiso 0.586(14) 1 calc PR B 1 H68C H 0.7547 0.5931 0.4171 0.241 Uiso 0.586(14) 1 calc PR B 1 C69 C 0.6608(8) 0.7578(15) 0.4007(6) 0.178(10) Uani 0.586(14) 1 d PD B 1 H69A H 0.6251 0.7524 0.4019 0.267 Uiso 0.586(14) 1 calc PR B 1 H69B H 0.6664 0.7911 0.3741 0.267 Uiso 0.586(14) 1 calc PR B 1 H69C H 0.6762 0.8007 0.4243 0.267 Uiso 0.586(14) 1 calc PR B 1 C67F C 0.6790(8) 0.6829(15) 0.4075(5) 0.086(3) Uiso 0.414(14) 1 d PD B 2 H67F H 0.6466 0.7085 0.3927 0.104 Uiso 0.414(14) 1 calc PR B 2 C68F C 0.7142(9) 0.7692(18) 0.4178(6) 0.133(10) Uani 0.414(14) 1 d PD B 2 H68D H 0.6981 0.8262 0.4317 0.199 Uiso 0.414(14) 1 calc PR B 2 H68E H 0.7253 0.7962 0.3920 0.199 Uiso 0.414(14) 1 calc PR B 2 H68F H 0.7428 0.7431 0.4368 0.199 Uiso 0.414(14) 1 calc PR B 2 C69F C 0.7007(10) 0.5914(18) 0.3834(7) 0.156(12) Uani 0.414(14) 1 d PD B 2 H69D H 0.7094 0.6178 0.3566 0.234 Uiso 0.414(14) 1 calc PR B 2 H69E H 0.6760 0.5351 0.3780 0.234 Uiso 0.414(14) 1 calc PR B 2 H69F H 0.7303 0.5633 0.4004 0.234 Uiso 0.414(14) 1 calc PR B 2 C70 C 0.5514(3) 0.3301(8) 0.5422(3) 0.132(3) Uani 1 1 d . . . H70 H 0.5171 0.3491 0.5293 0.159 Uiso 1 1 calc R . . C71 C 0.5669(4) 0.2276(9) 0.5220(4) 0.187(5) Uani 1 1 d . . . H71A H 0.5644 0.2369 0.4915 0.281 Uiso 1 1 calc R . . H71B H 0.5451 0.1699 0.5284 0.281 Uiso 1 1 calc R . . H71C H 0.6012 0.2105 0.5333 0.281 Uiso 1 1 calc R . . C72 C 0.5525(3) 0.3232(8) 0.5894(3) 0.149(4) Uani 1 1 d . . . H72A H 0.5866 0.3121 0.6026 0.224 Uiso 1 1 calc R . . H72B H 0.5319 0.2638 0.5963 0.224 Uiso 1 1 calc R . . H72C H 0.5397 0.3891 0.5999 0.224 Uiso 1 1 calc R . . C73 C 0.73888(18) 0.4126(5) 0.54654(17) 0.0590(15) Uani 1 1 d . . . C74 C 0.7784(2) 0.4218(5) 0.57870(18) 0.0642(15) Uani 1 1 d . A . C75 C 0.8174(2) 0.3456(6) 0.5832(2) 0.084(2) Uani 1 1 d . . . H75 H 0.8445 0.3523 0.6049 0.101 Uiso 1 1 calc R A . C76 C 0.8146(3) 0.2621(7) 0.5553(3) 0.102(3) Uani 1 1 d . A . H76 H 0.8404 0.2110 0.5580 0.122 Uiso 1 1 calc R . . C77 C 0.7757(3) 0.2508(6) 0.5238(3) 0.092(2) Uani 1 1 d . . . H77 H 0.7746 0.1919 0.5053 0.111 Uiso 1 1 calc R A . C78 C 0.7375(2) 0.3257(6) 0.5189(2) 0.0765(18) Uani 1 1 d . A . C79 C 0.8159(2) 0.5361(7) 0.63748(18) 0.078(2) Uani 1 1 d . . . H79 H 0.8484 0.5263 0.6266 0.094 Uiso 1 1 calc R . . C80 C 0.8149(2) 0.4670(7) 0.67614(19) 0.107(3) Uani 1 1 d . . . H80A H 0.7853 0.4832 0.6892 0.160 Uiso 1 1 calc R . . H80B H 0.8445 0.4807 0.6963 0.160 Uiso 1 1 calc R . . H80C H 0.8143 0.3924 0.6678 0.160 Uiso 1 1 calc R . . C81 C 0.8088(2) 0.6515(7) 0.6459(2) 0.101(2) Uani 1 1 d . . . H81A H 0.8106 0.6919 0.6200 0.151 Uiso 1 1 calc R . . H81B H 0.8348 0.6756 0.6679 0.151 Uiso 1 1 calc R . . H81C H 0.7764 0.6623 0.6553 0.151 Uiso 1 1 calc R . . C82 C 0.6997(6) 0.2390(11) 0.4562(4) 0.096(3) Uiso 0.576(12) 1 d PD C 1 H82 H 0.7342 0.2295 0.4494 0.115 Uiso 0.576(12) 1 calc PR C 1 C83 C 0.6781(6) 0.1377(11) 0.4661(5) 0.137(7) Uani 0.576(12) 1 d PD C 1 H83A H 0.6940 0.1129 0.4936 0.205 Uiso 0.576(12) 1 calc PR C 1 H83B H 0.6833 0.0857 0.4445 0.205 Uiso 0.576(12) 1 calc PR C 1 H83C H 0.6425 0.1466 0.4670 0.205 Uiso 0.576(12) 1 calc PR C 1 C84 C 0.6657(12) 0.289(6) 0.418(2) 0.164(8) Uani 0.576(12) 1 d PD C 1 H84A H 0.6346 0.3119 0.4275 0.246 Uiso 0.576(12) 1 calc PR C 1 H84B H 0.6587 0.2360 0.3959 0.246 Uiso 0.576(12) 1 calc PR C 1 H84C H 0.6824 0.3497 0.4076 0.246 Uiso 0.576(12) 1 calc PR C 1 C82F C 0.7019(9) 0.2747(18) 0.4459(5) 0.096(3) Uiso 0.424(12) 1 d PD C 2 H82F H 0.7128 0.1994 0.4496 0.115 Uiso 0.424(12) 1 calc PR C 2 C83F C 0.7374(7) 0.3329(17) 0.4245(6) 0.137(10) Uani 0.424(12) 1 d PD C 2 H83D H 0.7244 0.4037 0.4172 0.205 Uiso 0.424(12) 1 calc PR C 2 H83E H 0.7428 0.2952 0.3988 0.205 Uiso 0.424(12) 1 calc PR C 2 H83F H 0.7688 0.3389 0.4432 0.205 Uiso 0.424(12) 1 calc PR C 2 C84F C 0.6499(15) 0.279(8) 0.420(3) 0.164(8) Uani 0.424(12) 1 d PD C 2 H84D H 0.6394 0.3525 0.4158 0.246 Uiso 0.424(12) 1 calc PR C 2 H84E H 0.6262 0.2407 0.4349 0.246 Uiso 0.424(12) 1 calc PR C 2 H84F H 0.6511 0.2454 0.3924 0.246 Uiso 0.424(12) 1 calc PR C 2 C85 C 0.6647(2) 0.5196(8) 0.6677(2) 0.078(2) Uani 1 1 d . . . C86 C 0.6757(3) 0.4214(10) 0.6851(3) 0.109(3) Uani 1 1 d . . . C87 C 0.6983(3) 0.4110(11) 0.7282(3) 0.143(5) Uani 1 1 d . . . H87 H 0.7052 0.3435 0.7405 0.171 Uiso 1 1 calc R . . C88 C 0.7094(4) 0.5009(15) 0.7505(3) 0.162(7) Uani 1 1 d . . . H88 H 0.7242 0.4945 0.7790 0.194 Uiso 1 1 calc R . . C89 C 0.7004(3) 0.5985(11) 0.7347(2) 0.142(5) Uani 1 1 d . . . H89 H 0.7090 0.6600 0.7510 0.170 Uiso 1 1 calc R . . C90 C 0.6778(2) 0.6051(9) 0.6926(2) 0.097(3) Uani 1 1 d . . . C91 C 0.6906(5) 0.2344(11) 0.6671(5) 0.185(6) Uani 1 1 d . . . H91 H 0.7230 0.2486 0.6847 0.222 Uiso 1 1 calc R . . C92 C 0.6569(5) 0.1737(12) 0.6937(5) 0.268(9) Uani 1 1 d . . . H92A H 0.6304 0.1388 0.6751 0.401 Uiso 1 1 calc R . . H92B H 0.6425 0.2232 0.7122 0.401 Uiso 1 1 calc R . . H92C H 0.6765 0.1205 0.7108 0.401 Uiso 1 1 calc R . . C93 C 0.6997(6) 0.1910(12) 0.6279(5) 0.275(11) Uani 1 1 d . . . H93A H 0.6681 0.1719 0.6112 0.412 Uiso 1 1 calc R . . H93B H 0.7203 0.1277 0.6329 0.412 Uiso 1 1 calc R . . H93C H 0.7168 0.2434 0.6125 0.412 Uiso 1 1 calc R . . C94 C 0.6879(3) 0.7969(9) 0.6889(3) 0.128(3) Uani 1 1 d . . . H94 H 0.7205 0.7817 0.7060 0.154 Uiso 1 1 calc R . . C95 C 0.6953(3) 0.8663(8) 0.6515(3) 0.148(4) Uani 1 1 d . . . H95A H 0.6631 0.8858 0.6363 0.222 Uiso 1 1 calc R . . H95B H 0.7144 0.8275 0.6327 0.222 Uiso 1 1 calc R . . H95C H 0.7134 0.9305 0.6616 0.222 Uiso 1 1 calc R . . C96 C 0.6534(3) 0.8452(9) 0.7160(3) 0.171(5) Uani 1 1 d . . . H96A H 0.6236 0.8699 0.6984 0.256 Uiso 1 1 calc R . . H96B H 0.6698 0.9051 0.7315 0.256 Uiso 1 1 calc R . . H96C H 0.6444 0.7922 0.7360 0.256 Uiso 1 1 calc R . . C97 C -0.0297(12) 0.625(3) 0.8161(13) 0.33(2) Uiso 0.507(16) 1 d PD D 1 H97A H -0.0465 0.6890 0.8238 0.488 Uiso 0.507(16) 1 calc PR D 1 H97B H -0.0493 0.5627 0.8217 0.488 Uiso 0.507(16) 1 calc PR D 1 H97C H -0.0261 0.6271 0.7860 0.488 Uiso 0.507(16) 1 calc PR D 1 C98 C 0.0215(13) 0.618(2) 0.8421(11) 0.30(2) Uiso 0.507(16) 1 d PD D 1 H98A H 0.0185 0.6119 0.8724 0.358 Uiso 0.507(16) 1 calc PR D 1 H98B H 0.0413 0.6816 0.8377 0.358 Uiso 0.507(16) 1 calc PR D 1 C99 C 0.0468(12) 0.516(2) 0.8264(11) 0.263(17) Uiso 0.507(16) 1 d PD D 1 H99A H 0.0799 0.5044 0.8426 0.315 Uiso 0.507(16) 1 calc PR D 1 H99B H 0.0500 0.5210 0.7961 0.315 Uiso 0.507(16) 1 calc PR D 1 C100 C 0.0081(13) 0.426(2) 0.8357(10) 0.30(2) Uiso 0.507(16) 1 d PD D 1 H10A H -0.0258 0.4547 0.8342 0.360 Uiso 0.507(16) 1 calc PR D 1 H10B H 0.0082 0.3667 0.8155 0.360 Uiso 0.507(16) 1 calc PR D 1 C101 C 0.0281(14) 0.389(3) 0.8816(10) 0.28(2) Uiso 0.507(16) 1 d PD D 1 H10C H 0.0006 0.3805 0.8987 0.334 Uiso 0.507(16) 1 calc PR D 1 H10D H 0.0465 0.3219 0.8813 0.334 Uiso 0.507(16) 1 calc PR D 1 C102 C 0.0632(12) 0.482(3) 0.8990(9) 0.259(17) Uiso 0.507(16) 1 d PD D 1 H10E H 0.0792 0.4638 0.9273 0.389 Uiso 0.507(16) 1 calc PR D 1 H10F H 0.0439 0.5467 0.9002 0.389 Uiso 0.507(16) 1 calc PR D 1 H10G H 0.0885 0.4925 0.8803 0.389 Uiso 0.507(16) 1 calc PR D 1 C103 C 0.0524(16) 0.407(2) 0.8697(14) 0.29(2) Uiso 0.493(16) 1 d PD D 2 H10H H 0.0624 0.3408 0.8577 0.436 Uiso 0.493(16) 1 calc PR D 2 H10I H 0.0178 0.4223 0.8590 0.436 Uiso 0.493(16) 1 calc PR D 2 H10J H 0.0563 0.4018 0.9004 0.436 Uiso 0.493(16) 1 calc PR D 2 C104 C 0.0858(10) 0.499(3) 0.8567(11) 0.228(14) Uiso 0.493(16) 1 d PD D 2 H10K H 0.1204 0.4908 0.8702 0.273 Uiso 0.493(16) 1 calc PR D 2 H10L H 0.0853 0.5017 0.8258 0.273 Uiso 0.493(16) 1 calc PR D 2 C105 C 0.0618(11) 0.600(2) 0.8730(13) 0.32(2) Uiso 0.493(16) 1 d PD D 2 H10M H 0.0521 0.6513 0.8500 0.382 Uiso 0.493(16) 1 calc PR D 2 H10N H 0.0842 0.6352 0.8957 0.382 Uiso 0.493(16) 1 calc PR D 2 C106 C 0.0151(11) 0.550(3) 0.8902(7) 0.29(2) Uiso 0.493(16) 1 d PD D 2 H10O H 0.0250 0.4917 0.9103 0.343 Uiso 0.493(16) 1 calc PR D 2 H10P H -0.0033 0.6037 0.9043 0.343 Uiso 0.493(16) 1 calc PR D 2 C107 C -0.0171(10) 0.507(3) 0.8489(9) 0.234(15) Uiso 0.493(16) 1 d PD D 2 H10Q H -0.0126 0.4293 0.8463 0.281 Uiso 0.493(16) 1 calc PR D 2 H10R H -0.0526 0.5212 0.8497 0.281 Uiso 0.493(16) 1 calc PR D 2 C108 C 0.0011(12) 0.564(3) 0.8124(7) 0.212(13) Uiso 0.493(16) 1 d PD D 2 H10S H -0.0181 0.5409 0.7860 0.318 Uiso 0.493(16) 1 calc PR D 2 H10T H 0.0362 0.5480 0.8119 0.318 Uiso 0.493(16) 1 calc PR D 2 H10U H -0.0031 0.6404 0.8158 0.318 Uiso 0.493(16) 1 calc PR D 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pb1 0.04169(9) 0.05542(13) 0.03537(9) 0.00071(10) 0.00515(7) -0.00418(10) Sn1 0.03721(15) 0.0458(2) 0.03283(16) 0.00116(15) 0.00371(12) -0.00070(15) O1 0.0583(19) 0.056(2) 0.048(2) 0.0051(18) 0.0104(15) -0.0009(17) O2 0.064(2) 0.078(3) 0.049(2) 0.017(2) 0.0268(16) 0.014(2) O3 0.070(2) 0.064(3) 0.044(2) -0.0027(19) -0.0038(16) -0.012(2) O4 0.092(3) 0.047(3) 0.060(2) 0.0087(19) -0.016(2) -0.016(2) O5 0.0380(17) 0.076(3) 0.049(2) -0.0039(18) 0.0092(14) -0.0009(17) O6 0.0448(17) 0.070(3) 0.0464(19) -0.0130(19) 0.0078(14) 0.0034(18) O7 0.062(2) 0.071(3) 0.060(2) 0.000(2) -0.0067(17) 0.012(2) O8 0.051(2) 0.074(3) 0.073(3) -0.010(2) -0.0049(18) -0.006(2) C1 0.041(2) 0.042(3) 0.031(2) -0.003(2) 0.0038(18) 0.001(2) C2 0.053(3) 0.057(4) 0.041(3) -0.008(3) 0.010(2) -0.001(3) C3 0.091(4) 0.053(4) 0.067(4) 0.001(3) 0.013(3) 0.013(3) C4 0.105(5) 0.074(5) 0.069(4) -0.020(4) 0.024(4) 0.031(4) C5 0.079(4) 0.081(5) 0.049(3) 0.001(3) 0.023(3) 0.025(4) C6 0.054(3) 0.066(4) 0.042(3) 0.006(3) 0.011(2) 0.012(3) C7 0.068(3) 0.060(4) 0.053(3) 0.009(3) 0.008(3) 0.013(3) C8 0.099(5) 0.113(6) 0.077(5) 0.046(4) 0.008(4) -0.013(4) C9 0.090(4) 0.139(7) 0.056(4) 0.016(4) -0.007(3) -0.032(5) C10 0.060(3) 0.115(6) 0.046(3) 0.024(4) 0.025(3) 0.020(4) C11 0.085(4) 0.154(8) 0.063(4) 0.026(4) 0.029(3) 0.028(4) C12 0.085(4) 0.121(7) 0.091(5) 0.046(5) 0.041(4) 0.014(5) C13 0.037(2) 0.050(4) 0.043(3) 0.006(3) 0.0042(19) 0.003(2) C14 0.043(3) 0.061(4) 0.045(3) 0.002(3) 0.004(2) -0.006(3) C15 0.055(3) 0.077(5) 0.049(3) 0.010(3) -0.008(2) 0.006(3) C16 0.061(3) 0.083(5) 0.064(4) 0.036(4) -0.001(3) 0.010(3) C17 0.071(4) 0.058(4) 0.065(4) 0.018(3) 0.010(3) 0.008(3) C18 0.047(3) 0.053(4) 0.058(3) 0.007(3) 0.000(2) 0.005(3) C19 0.062(3) 0.073(5) 0.046(3) -0.013(3) 0.006(2) -0.012(3) C20 0.065(4) 0.119(6) 0.061(4) -0.013(4) 0.009(3) -0.016(4) C21 0.093(4) 0.076(5) 0.072(4) -0.023(4) 0.005(3) -0.013(4) C22 0.071(4) 0.054(4) 0.084(4) 0.011(3) -0.013(3) -0.004(3) C23 0.125(5) 0.055(4) 0.093(5) 0.004(4) -0.039(4) -0.026(4) C24 0.073(4) 0.110(7) 0.156(8) -0.004(6) 0.000(5) -0.003(4) C25 0.041(2) 0.040(3) 0.035(2) 0.002(2) -0.0004(19) -0.004(2) C26 0.042(3) 0.048(3) 0.042(3) 0.007(2) 0.003(2) -0.001(2) C27 0.043(3) 0.063(4) 0.054(3) 0.006(3) -0.006(2) -0.002(3) C28 0.062(3) 0.064(4) 0.043(3) -0.008(3) -0.016(2) -0.006(3) C29 0.067(3) 0.055(4) 0.041(3) -0.005(3) 0.001(2) 0.002(3) C30 0.047(3) 0.050(3) 0.040(3) 0.007(3) 0.002(2) 0.003(2) C31 0.040(3) 0.080(5) 0.067(4) 0.006(3) 0.004(2) 0.010(3) C32 0.059(3) 0.091(5) 0.112(5) 0.013(4) 0.020(3) -0.018(4) C33 0.056(3) 0.097(5) 0.072(4) 0.005(4) 0.015(3) 0.013(3) C34 0.069(3) 0.067(4) 0.039(3) -0.002(3) 0.012(2) 0.016(3) C35 0.100(5) 0.081(5) 0.072(4) 0.004(4) 0.012(3) 0.015(4) C36 0.064(3) 0.094(5) 0.058(3) -0.008(3) 0.024(3) 0.022(3) C37 0.036(2) 0.065(4) 0.038(3) -0.001(3) 0.000(2) -0.005(3) C38 0.047(3) 0.075(4) 0.040(3) -0.001(3) 0.007(2) -0.001(3) C39 0.042(3) 0.109(6) 0.052(3) 0.001(4) 0.001(2) 0.006(3) C40 0.042(3) 0.133(7) 0.050(3) -0.005(4) -0.003(2) -0.013(4) C41 0.051(3) 0.090(5) 0.052(3) -0.013(3) 0.001(2) -0.023(3) C42 0.048(3) 0.073(4) 0.044(3) 0.000(3) 0.013(2) -0.007(3) C43 0.071(4) 0.090(5) 0.060(4) 0.008(4) 0.001(3) 0.022(4) C44 0.098(5) 0.082(6) 0.084(5) 0.017(4) -0.002(4) 0.016(4) C45 0.092(5) 0.120(7) 0.094(5) -0.004(5) 0.021(4) 0.039(5) C46 0.077(4) 0.053(4) 0.073(4) -0.007(3) 0.008(3) -0.017(3) C47 0.113(5) 0.077(5) 0.106(6) -0.016(4) 0.003(4) 0.008(4) C48 0.150(7) 0.084(6) 0.101(6) 0.015(5) -0.010(5) 0.002(5) Pb2 0.04511(10) 0.08532(18) 0.05010(12) -0.00193(12) 0.01633(8) -0.00161(11) Sn2 0.03781(16) 0.0653(3) 0.04064(18) -0.00306(18) 0.00913(13) -0.00522(17) O9 0.052(2) 0.075(3) 0.125(4) 0.001(3) 0.013(2) 0.008(2) O10 0.055(2) 0.076(3) 0.080(3) 0.002(2) 0.0312(19) -0.008(2) O11 0.097(3) 0.210(6) 0.036(2) 0.020(3) 0.001(2) -0.047(3) O12 0.079(3) 0.132(5) 0.095(4) -0.008(3) 0.017(2) -0.053(3) O13 0.055(2) 0.088(3) 0.057(2) 0.008(2) -0.0009(17) 0.005(2) O14 0.084(3) 0.116(4) 0.104(4) -0.061(3) 0.018(3) 0.004(3) O15 0.130(5) 0.116(6) 0.178(7) 0.069(5) 0.018(4) 0.042(4) O16 0.147(5) 0.133(5) 0.072(3) -0.012(4) -0.029(3) -0.030(4) C49 0.044(3) 0.065(4) 0.050(3) 0.000(3) 0.007(2) -0.002(3) C50 0.048(3) 0.085(5) 0.079(4) 0.005(4) 0.008(3) -0.010(3) C51 0.072(4) 0.067(5) 0.147(7) 0.005(5) 0.023(4) -0.007(4) C52 0.079(5) 0.062(5) 0.143(7) 0.011(5) 0.014(4) -0.025(4) C53 0.063(3) 0.070(5) 0.096(5) 0.016(4) 0.014(3) -0.009(4) C54 0.051(3) 0.064(4) 0.054(3) 0.011(3) 0.008(2) -0.008(3) C56 0.084(10) 0.27(3) 0.134(14) 0.001(14) -0.002(9) 0.044(13) C57 0.063(7) 0.150(14) 0.146(12) -0.002(10) 0.019(7) 0.039(8) C57F 0.12(2) 0.12(2) 0.18(3) -0.06(2) -0.038(19) 0.004(19) C56F 0.062(12) 0.094(17) 0.13(2) 0.010(14) -0.034(12) -0.021(11) C58 0.056(3) 0.093(5) 0.067(4) 0.007(4) 0.030(3) -0.011(3) C59 0.062(4) 0.111(6) 0.082(4) 0.006(4) 0.020(3) -0.008(4) C60 0.081(4) 0.124(7) 0.105(5) -0.033(5) 0.049(4) -0.014(4) C61 0.042(3) 0.097(5) 0.049(3) -0.017(3) 0.006(2) -0.012(3) C62 0.054(3) 0.148(7) 0.043(3) -0.015(4) 0.003(2) -0.013(4) C63 0.077(4) 0.220(10) 0.053(4) -0.023(5) -0.006(3) -0.009(6) C64 0.064(4) 0.246(12) 0.083(6) -0.052(7) -0.020(4) -0.015(6) C65 0.073(4) 0.219(10) 0.078(5) -0.040(6) 0.000(4) -0.044(6) C66 0.059(4) 0.122(6) 0.072(4) -0.029(4) 0.006(3) -0.025(4) C68 0.101(10) 0.34(3) 0.055(8) 0.045(13) 0.048(8) -0.025(15) C69 0.20(2) 0.21(2) 0.138(16) 0.071(16) 0.079(15) 0.019(18) C68F 0.129(19) 0.20(3) 0.083(14) 0.060(16) 0.053(13) -0.011(19) C69F 0.12(2) 0.19(3) 0.14(2) 0.03(2) -0.012(17) 0.030(19) C70 0.116(6) 0.128(8) 0.157(9) -0.018(7) 0.031(6) -0.074(6) C71 0.202(11) 0.150(11) 0.219(13) -0.059(10) 0.064(9) -0.056(9) C72 0.144(7) 0.145(9) 0.170(10) 0.022(8) 0.065(7) -0.071(7) C73 0.053(3) 0.071(4) 0.056(3) 0.008(3) 0.019(3) -0.003(3) C74 0.065(3) 0.069(4) 0.063(4) 0.012(3) 0.025(3) 0.004(3) C75 0.064(4) 0.106(6) 0.086(5) 0.030(5) 0.021(3) 0.027(4) C76 0.101(6) 0.081(6) 0.136(7) 0.026(5) 0.059(5) 0.040(5) C77 0.086(5) 0.079(5) 0.119(6) -0.009(5) 0.043(5) 0.009(4) C78 0.071(4) 0.077(5) 0.088(5) -0.009(4) 0.036(3) 0.005(4) C79 0.049(3) 0.125(7) 0.059(4) 0.009(4) 0.005(3) -0.007(4) C80 0.079(4) 0.179(8) 0.063(4) 0.039(5) 0.010(3) 0.015(5) C81 0.083(4) 0.136(8) 0.081(5) -0.012(5) 0.000(4) -0.030(5) C83 0.182(16) 0.091(12) 0.144(14) -0.030(10) 0.048(11) -0.032(11) C84 0.14(2) 0.20(2) 0.143(10) -0.114(10) 0.01(2) 0.02(2) C83F 0.126(16) 0.14(2) 0.140(19) -0.086(17) 0.001(13) -0.002(15) C84F 0.14(2) 0.20(2) 0.143(10) -0.114(10) 0.01(2) 0.02(2) C85 0.051(3) 0.125(7) 0.060(4) 0.039(5) 0.017(3) 0.007(4) C86 0.075(5) 0.154(10) 0.104(7) 0.043(7) 0.034(4) 0.013(6) C87 0.087(6) 0.243(16) 0.104(8) 0.095(9) 0.033(6) 0.045(8) C88 0.092(6) 0.34(2) 0.059(6) 0.050(9) 0.015(5) 0.041(10) C89 0.094(6) 0.284(16) 0.044(5) 0.002(6) 0.000(4) 0.024(7) C90 0.075(4) 0.161(9) 0.056(4) 0.008(5) 0.011(3) -0.011(5) C91 0.157(10) 0.147(12) 0.256(17) 0.095(12) 0.048(10) 0.017(9) C92 0.249(15) 0.206(15) 0.37(2) 0.136(16) 0.118(15) 0.061(13) C93 0.41(2) 0.167(13) 0.29(2) 0.071(14) 0.231(19) 0.105(15) C94 0.112(6) 0.200(11) 0.075(5) -0.035(7) 0.020(4) -0.044(7) C95 0.144(8) 0.168(10) 0.142(8) -0.039(7) 0.060(6) -0.045(7) C96 0.152(8) 0.224(13) 0.152(9) -0.057(9) 0.078(7) -0.047(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pb1 C37 2.285(4) . ? Pb1 Sn1 2.8784(4) . ? Sn1 C25 2.178(4) . ? Sn1 C13 2.179(5) . ? Sn1 C1 2.188(4) . ? O1 C2 1.403(5) . ? O1 C7 1.462(6) . ? O2 C6 1.365(6) . ? O2 C10 1.441(6) . ? O3 C14 1.360(6) . ? O3 C19 1.436(6) . ? O4 C18 1.389(6) . ? O4 C22 1.419(6) . ? O5 C26 1.365(5) . ? O5 C31 1.435(5) . ? O6 C30 1.378(5) . ? O6 C34 1.440(6) . ? O7 C38 1.375(6) . ? O7 C43 1.443(7) . ? O8 C42 1.392(6) . ? O8 C46 1.439(7) . ? C1 C2 1.370(7) . ? C1 C6 1.400(6) . ? C2 C3 1.395(7) . ? C3 C4 1.387(8) . ? C4 C5 1.365(8) . ? C5 C6 1.379(8) . ? C7 C8 1.477(7) . ? C7 C9 1.503(7) . ? C10 C12 1.491(10) . ? C10 C11 1.528(8) . ? C13 C18 1.381(7) . ? C13 C14 1.388(6) . ? C14 C15 1.383(7) . ? C15 C16 1.369(8) . ? C16 C17 1.372(8) . ? C17 C18 1.386(7) . ? C19 C21 1.492(8) . ? C19 C20 1.510(7) . ? C22 C23 1.502(8) . ? C22 C24 1.503(9) . ? C25 C26 1.393(6) . ? C25 C30 1.394(6) . ? C26 C27 1.400(6) . ? C27 C28 1.378(7) . ? C28 C29 1.377(7) . ? C29 C30 1.395(6) . ? C31 C32 1.515(8) . ? C31 C33 1.520(8) . ? C34 C35 1.499(8) . ? C34 C36 1.509(7) . ? C37 C42 1.371(7) . ? C37 C38 1.386(7) . ? C38 C39 1.404(7) . ? C39 C40 1.380(9) . ? C40 C41 1.382(8) . ? C41 C42 1.391(7) . ? C43 C44 1.504(9) . ? C43 C45 1.507(8) . ? C46 C47 1.517(9) . ? C46 C48 1.521(8) . ? Pb2 C85 2.304(6) . ? Pb2 Sn2 2.8730(4) . ? Sn2 C49 2.166(6) . ? Sn2 C61 2.173(5) . ? Sn2 C73 2.176(6) . ? O9 C50 1.403(6) . ? O9 C55 1.428(10) . ? O9 C55F 1.495(14) . ? O10 C54 1.351(6) . ? O10 C58 1.439(6) . ? O11 C62 1.355(7) . ? O11 C67 1.444(11) . ? O11 C67F 1.491(13) . ? O12 C66 1.370(8) . ? O12 C70 1.461(8) . ? O13 C74 1.368(7) . ? O13 C79 1.448(6) . ? O14 C78 1.367(7) . ? O14 C82 1.434(11) . ? O14 C82F 1.456(13) . ? O15 C86 1.372(11) . ? O15 C91 1.469(12) . ? O16 C90 1.384(10) . ? O16 C94 1.433(10) . ? C49 C50 1.375(8) . ? C49 C54 1.413(6) . ? C50 C51 1.382(9) . ? C51 C52 1.382(9) . ? C52 C53 1.361(9) . ? C53 C54 1.384(8) . ? C55 C56 1.445(13) . ? C55 C57 1.508(12) . ? C55F C57F 1.470(16) . ? C55F C56F 1.518(15) . ? C58 C59 1.509(8) . ? C58 C60 1.513(9) . ? C61 C62 1.374(8) . ? C61 C66 1.391(8) . ? C62 C63 1.397(8) . ? C63 C64 1.369(11) . ? C64 C65 1.336(11) . ? C65 C66 1.385(8) . ? C67 C68 1.465(13) . ? C67 C69 1.539(15) . ? C67F C68F 1.447(14) . ? C67F C69F 1.534(16) . ? C70 C72 1.494(12) . ? C70 C71 1.517(13) . ? C73 C74 1.379(7) . ? C73 C78 1.395(8) . ? C74 C75 1.413(8) . ? C75 C76 1.365(10) . ? C76 C77 1.358(10) . ? C77 C78 1.386(9) . ? C79 C81 1.486(10) . ? C79 C80 1.504(8) . ? C82 C83 1.448(13) . ? C82 C84 1.544(14) . ? C82F C83F 1.442(15) . ? C82F C84F 1.533(15) . ? C85 C90 1.349(10) . ? C85 C86 1.363(11) . ? C86 C87 1.428(12) . ? C87 C88 1.341(16) . ? C88 C89 1.332(16) . ? C89 C90 1.394(10) . ? C91 C93 1.408(17) . ? C91 C92 1.522(15) . ? C94 C96 1.477(11) . ? C94 C95 1.505(12) . ? C97 C98 1.516(19) . ? C98 C99 1.552(19) . ? C99 C100 1.594(18) . ? C100 C101 1.553(18) . ? C101 C102 1.549(18) . ? C103 C104 1.546(18) . ? C104 C105 1.540(18) . ? C105 C106 1.571(18) . ? C106 C107 1.567(18) . ? C107 C108 1.500(18) . ? 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 C37 Pb1 Sn1 102.94(12) . . ? C25 Sn1 C13 109.88(18) . . ? C25 Sn1 C1 109.17(16) . . ? C13 Sn1 C1 108.68(17) . . ? C25 Sn1 Pb1 102.56(12) . . ? C13 Sn1 Pb1 125.60(11) . . ? C1 Sn1 Pb1 99.88(12) . . ? C2 O1 C7 114.7(3) . . ? C6 O2 C10 120.4(4) . . ? C14 O3 C19 121.0(4) . . ? C18 O4 C22 120.2(4) . . ? C26 O5 C31 120.0(4) . . ? C30 O6 C34 120.2(4) . . ? C38 O7 C43 119.6(4) . . ? C42 O8 C46 121.1(4) . . ? C2 C1 C6 117.4(5) . . ? C2 C1 Sn1 119.6(3) . . ? C6 C1 Sn1 122.8(4) . . ? C1 C2 C3 122.7(5) . . ? C1 C2 O1 119.2(4) . . ? C3 C2 O1 118.1(5) . . ? C4 C3 C2 117.9(6) . . ? C5 C4 C3 121.0(5) . . ? C4 C5 C6 120.1(5) . . ? O2 C6 C5 124.0(5) . . ? O2 C6 C1 115.0(5) . . ? C5 C6 C1 121.0(5) . . ? O1 C7 C8 108.1(4) . . ? O1 C7 C9 109.5(4) . . ? C8 C7 C9 112.7(5) . . ? O2 C10 C12 105.4(5) . . ? O2 C10 C11 110.1(5) . . ? C12 C10 C11 112.0(6) . . ? C18 C13 C14 118.4(5) . . ? C18 C13 Sn1 125.4(3) . . ? C14 C13 Sn1 116.3(4) . . ? O3 C14 C15 124.0(5) . . ? O3 C14 C13 115.0(4) . . ? C15 C14 C13 121.0(5) . . ? C16 C15 C14 118.7(5) . . ? C15 C16 C17 122.3(5) . . ? C16 C17 C18 118.0(6) . . ? C13 C18 C17 121.6(5) . . ? C13 C18 O4 116.2(4) . . ? C17 C18 O4 122.2(5) . . ? O3 C19 C21 105.1(4) . . ? O3 C19 C20 111.5(4) . . ? C21 C19 C20 111.6(5) . . ? O4 C22 C23 105.6(5) . . ? O4 C22 C24 111.6(6) . . ? C23 C22 C24 112.5(5) . . ? C26 C25 C30 117.7(4) . . ? C26 C25 Sn1 123.8(3) . . ? C30 C25 Sn1 118.3(3) . . ? O5 C26 C25 115.6(4) . . ? O5 C26 C27 122.9(4) . . ? C25 C26 C27 121.6(4) . . ? C28 C27 C26 118.4(4) . . ? C29 C28 C27 122.1(4) . . ? C28 C29 C30 118.5(5) . . ? O6 C30 C25 115.5(4) . . ? O6 C30 C29 122.8(4) . . ? C25 C30 C29 121.7(4) . . ? O5 C31 C32 110.6(5) . . ? O5 C31 C33 105.8(4) . . ? C32 C31 C33 111.9(5) . . ? O6 C34 C35 111.5(5) . . ? O6 C34 C36 106.0(4) . . ? C35 C34 C36 112.8(5) . . ? C42 C37 C38 118.5(4) . . ? C42 C37 Pb1 122.8(4) . . ? C38 C37 Pb1 117.4(4) . . ? O7 C38 C37 114.3(4) . . ? O7 C38 C39 124.2(5) . . ? C37 C38 C39 121.6(6) . . ? C40 C39 C38 116.7(6) . . ? C39 C40 C41 124.0(5) . . ? C40 C41 C42 116.4(6) . . ? C37 C42 C41 122.8(5) . . ? C37 C42 O8 114.1(4) . . ? C41 C42 O8 123.1(6) . . ? O7 C43 C44 106.3(4) . . ? O7 C43 C45 109.3(5) . . ? C44 C43 C45 113.0(6) . . ? O8 C46 C47 109.9(5) . . ? O8 C46 C48 104.6(5) . . ? C47 C46 C48 111.2(6) . . ? C85 Pb2 Sn2 104.28(15) . . ? C49 Sn2 C61 108.0(2) . . ? C49 Sn2 C73 110.48(19) . . ? C61 Sn2 C73 109.7(2) . . ? C49 Sn2 Pb2 109.06(14) . . ? C61 Sn2 Pb2 96.86(13) . . ? C73 Sn2 Pb2 121.39(13) . . ? C50 O9 C55 122.3(6) . . ? C50 O9 C55F 110.9(10) . . ? C55 O9 C55F 17.6(11) . . ? C54 O10 C58 120.4(4) . . ? C62 O11 C67 119.6(7) . . ? C62 O11 C67F 122.7(9) . . ? C67 O11 C67F 19.9(9) . . ? C66 O12 C70 121.2(6) . . ? C74 O13 C79 121.8(5) . . ? C78 O14 C82 115.9(8) . . ? C78 O14 C82F 122.0(10) . . ? C82 O14 C82F 22.3(11) . . ? C86 O15 C91 119.5(10) . . ? C90 O16 C94 118.5(7) . . ? C50 C49 C54 117.4(5) . . ? C50 C49 Sn2 119.1(4) . . ? C54 C49 Sn2 123.5(4) . . ? C49 C50 C51 122.9(5) . . ? C49 C50 O9 115.7(5) . . ? C51 C50 O9 121.4(6) . . ? C50 C51 C52 117.7(7) . . ? C53 C52 C51 122.0(6) . . ? C52 C53 C54 119.5(6) . . ? O10 C54 C53 124.3(5) . . ? O10 C54 C49 115.2(5) . . ? C53 C54 C49 120.4(6) . . ? O9 C55 C56 107.1(10) . . ? O9 C55 C57 109.7(8) . . ? C56 C55 C57 114.5(10) . . ? C57F C55F O9 105.2(17) . . ? C57F C55F C56F 112.4(16) . . ? O9 C55F C56F 107.8(13) . . ? O10 C58 C59 110.2(5) . . ? O10 C58 C60 104.3(5) . . ? C59 C58 C60 111.2(6) . . ? C62 C61 C66 118.5(5) . . ? C62 C61 Sn2 123.1(4) . . ? C66 C61 Sn2 118.4(4) . . ? O11 C62 C61 114.8(4) . . ? O11 C62 C63 124.3(6) . . ? C61 C62 C63 120.9(6) . . ? C64 C63 C62 117.7(7) . . ? C65 C64 C63 123.3(6) . . ? C64 C65 C66 118.8(7) . . ? O12 C66 C65 123.3(6) . . ? O12 C66 C61 115.9(5) . . ? C65 C66 C61 120.7(7) . . ? O11 C67 C68 107.6(9) . . ? O11 C67 C69 99.2(11) . . ? C68 C67 C69 107.4(13) . . ? C68F C67F O11 112.6(14) . . ? C68F C67F C69F 112.9(16) . . ? O11 C67F C69F 93.5(15) . . ? O12 C70 C72 106.6(7) . . ? O12 C70 C71 109.8(8) . . ? C72 C70 C71 113.8(10) . . ? C74 C73 C78 119.0(6) . . ? C74 C73 Sn2 115.5(5) . . ? C78 C73 Sn2 125.5(4) . . ? O13 C74 C73 114.2(5) . . ? O13 C74 C75 125.2(6) . . ? C73 C74 C75 120.7(6) . . ? C76 C75 C74 118.5(7) . . ? C77 C76 C75 121.7(7) . . ? C76 C77 C78 120.2(7) . . ? O14 C78 C77 123.7(7) . . ? O14 C78 C73 116.4(6) . . ? C77 C78 C73 119.9(6) . . ? O13 C79 C81 104.7(5) . . ? O13 C79 C80 111.9(5) . . ? C81 C79 C80 113.4(6) . . ? O14 C82 C83 115.2(12) . . ? O14 C82 C84 100(4) . . ? C83 C82 C84 108.0(17) . . ? C83F C82F O14 110.9(16) . . ? C83F C82F C84F 110.3(19) . . ? O14 C82F C84F 107(5) . . ? C90 C85 C86 117.0(8) . . ? C90 C85 Pb2 111.1(6) . . ? C86 C85 Pb2 131.4(7) . . ? C85 C86 O15 115.7(8) . . ? C85 C86 C87 120.7(11) . . ? O15 C86 C87 123.6(11) . . ? C88 C87 C86 117.8(12) . . ? C89 C88 C87 123.6(11) . . ? C88 C89 C90 116.8(12) . . ? C85 C90 O16 111.4(6) . . ? C85 C90 C89 124.1(10) . . ? O16 C90 C89 124.5(10) . . ? C93 C91 O15 108.0(12) . . ? C93 C91 C92 118.9(15) . . ? O15 C91 C92 102.8(10) . . ? O16 C94 C96 109.0(7) . . ? O16 C94 C95 105.5(7) . . ? C96 C94 C95 112.5(10) . . ? C97 C98 C99 106.3(17) . . ? C98 C99 C100 101.3(15) . . ? C101 C100 C99 103.2(14) . . ? C102 C101 C100 103.5(14) . . ? C105 C104 C103 103.7(14) . . ? C104 C105 C106 100.2(14) . . ? C107 C106 C105 103.4(14) . . ? C108 C107 C106 106.1(15) . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 24.98 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 1.052 _refine_diff_density_min -0.595 _refine_diff_density_rms 0.075 #\#CIF_1.1 data_c927 _database_code_depnum_ccdc_archive 'CCDC 864029' #TrackingRef 'ccdc_sub.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H34 O4 Pb' _chemical_formula_weight 593.70 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M Cc 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' _cell_length_a 14.645(3) _cell_length_b 14.514(3) _cell_length_c 11.599(2) _cell_angle_alpha 90.00 _cell_angle_beta 93.68(3) _cell_angle_gamma 90.00 _cell_volume 2460.4(8) _cell_formula_units_Z 4 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 1204 _cell_measurement_theta_min 2 _cell_measurement_theta_max 25 _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.603 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1168 _exptl_absorpt_coefficient_mu 6.881 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.2320 _exptl_absorpt_correction_T_max 0.3399 _exptl_absorpt_process_details ; G.M.Sheldrick (1996)SADABS. Program for Absorption Correction ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'SMART CCD diffractometer (BRUKER AXS)' _diffrn_measurement_method Omega-scans _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6913 _diffrn_reflns_av_R_equivalents 0.0530 _diffrn_reflns_av_sigmaI/netI 0.0429 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 1.98 _diffrn_reflns_theta_max 26.04 _reflns_number_total 3395 _reflns_number_gt 3027 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (BRUKER AXS)' _computing_cell_refinement 'SAINT (BRUKER AXS)' _computing_data_reduction 'SAINT (BRUKER AXS)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP for Windows (L.J. Farugia)' _computing_publication_material 'WINGX (L.J.Farugia)' _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^)+(0.0664P)^2^+0.3852P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.019(14) _refine_ls_number_reflns 3395 _refine_ls_number_parameters 263 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0457 _refine_ls_R_factor_gt 0.0383 _refine_ls_wR_factor_ref 0.0996 _refine_ls_wR_factor_gt 0.0945 _refine_ls_goodness_of_fit_ref 1.062 _refine_ls_restrained_S_all 1.061 _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 Pb1 Pb 0.55557(5) 0.215665(19) 0.02532(5) 0.04661(13) Uani 1 1 d . . . O1 O 0.5214(5) 0.0517(5) -0.1289(7) 0.0509(17) Uani 1 1 d . . . O2 O 0.3637(5) 0.1803(5) 0.1640(6) 0.0496(16) Uani 1 1 d . . . O3 O 0.5093(6) 0.3787(5) 0.1898(6) 0.0557(19) Uani 1 1 d . . . O4 O 0.4245(6) 0.2865(5) -0.1817(7) 0.0544(19) Uani 1 1 d . . . C1 C 0.4402(7) 0.1127(6) 0.0148(7) 0.039(2) Uani 1 1 d . . . C2 C 0.4435(7) 0.0455(6) -0.0684(8) 0.041(2) Uani 1 1 d . . . C3 C 0.3745(7) -0.0195(7) -0.0921(9) 0.048(2) Uani 1 1 d . . . H3 H 0.3786 -0.0638 -0.1506 0.057 Uiso 1 1 calc R . . C4 C 0.2998(8) -0.0153(7) -0.0251(10) 0.051(3) Uani 1 1 d . . . H4 H 0.2522 -0.0581 -0.0380 0.062 Uiso 1 1 calc R . . C5 C 0.2937(8) 0.0489(8) 0.0583(9) 0.052(3) Uani 1 1 d . . . H5 H 0.2426 0.0493 0.1034 0.063 Uiso 1 1 calc R . . C6 C 0.3620(7) 0.1139(6) 0.0780(8) 0.040(2) Uani 1 1 d . . . C7 C 0.5437(9) -0.0230(8) -0.2056(10) 0.050(3) Uani 1 1 d . . . H7 H 0.4885 -0.0384 -0.2556 0.060 Uiso 1 1 calc R . . C8 C 0.5735(11) -0.1069(10) -0.1390(14) 0.079(4) Uani 1 1 d . . . H8A H 0.5243 -0.1276 -0.0932 0.118 Uiso 1 1 calc R . . H8B H 0.6269 -0.0924 -0.0884 0.118 Uiso 1 1 calc R . . H8C H 0.5887 -0.1553 -0.1922 0.118 Uiso 1 1 calc R . . C9 C 0.6153(10) 0.0134(11) -0.2797(12) 0.068(4) Uani 1 1 d . . . H9A H 0.5920 0.0674 -0.3210 0.102 Uiso 1 1 calc R . . H9B H 0.6309 -0.0335 -0.3346 0.102 Uiso 1 1 calc R . . H9C H 0.6694 0.0299 -0.2315 0.102 Uiso 1 1 calc R . . C10 C 0.2786(9) 0.2084(8) 0.2129(13) 0.046(3) Uani 1 1 d . . . H10 H 0.2478 0.1529 0.2414 0.055 Uiso 1 1 calc R . . C11 C 0.3026(12) 0.2703(10) 0.3127(14) 0.060(4) Uani 1 1 d . . . H11A H 0.3436 0.2384 0.3682 0.090 Uiso 1 1 calc R . . H11B H 0.2474 0.2877 0.3491 0.090 Uiso 1 1 calc R . . H11C H 0.3325 0.3252 0.2857 0.090 Uiso 1 1 calc R . . C12 C 0.2162(10) 0.2531(11) 0.1196(13) 0.071(3) Uani 1 1 d . . . H12A H 0.2036 0.2098 0.0569 0.106 Uiso 1 1 calc R . . H12B H 0.2458 0.3074 0.0906 0.106 Uiso 1 1 calc R . . H12C H 0.1592 0.2708 0.1517 0.106 Uiso 1 1 calc R . . C13 C 0.4589(7) 0.3380(7) 0.0024(9) 0.044(2) Uani 1 1 d . . . C14 C 0.4530(8) 0.3989(7) 0.0946(9) 0.051(2) Uani 1 1 d . . . C15 C 0.3890(10) 0.4690(7) 0.0858(10) 0.059(3) Uani 1 1 d . . . H15 H 0.3841 0.5110 0.1468 0.071 Uiso 1 1 calc R . . C16 C 0.3327(8) 0.4767(9) -0.0135(11) 0.055(3) Uani 1 1 d . . . H16 H 0.2893 0.5245 -0.0193 0.066 Uiso 1 1 calc R . . C17 C 0.3380(7) 0.4167(8) -0.1042(9) 0.052(3) Uani 1 1 d . . . H17 H 0.2979 0.4216 -0.1704 0.062 Uiso 1 1 calc R . . C18 C 0.4053(8) 0.3476(8) -0.0949(8) 0.051(2) Uani 1 1 d . . . C19 C 0.5164(9) 0.4418(9) 0.2849(11) 0.055(3) Uani 1 1 d . . . H19 H 0.4544 0.4642 0.2996 0.066 Uiso 1 1 calc R . . C20 C 0.5529(9) 0.3878(10) 0.3875(10) 0.065(3) Uani 1 1 d . . . H20A H 0.5125 0.3363 0.4000 0.098 Uiso 1 1 calc R . . H20B H 0.5564 0.4272 0.4552 0.098 Uiso 1 1 calc R . . H20C H 0.6135 0.3649 0.3738 0.098 Uiso 1 1 calc R . . C21 C 0.5742(12) 0.5220(10) 0.2585(15) 0.071(5) Uani 1 1 d . . . H21A H 0.5471 0.5540 0.1913 0.106 Uiso 1 1 calc R . . H21B H 0.6349 0.5008 0.2428 0.106 Uiso 1 1 calc R . . H21C H 0.5782 0.5635 0.3241 0.106 Uiso 1 1 calc R . . C22 C 0.3583(13) 0.2684(9) -0.2758(13) 0.062(4) Uani 1 1 d . . . H22 H 0.3356 0.3269 -0.3111 0.074 Uiso 1 1 calc R . . C23 C 0.4096(18) 0.2128(11) -0.3624(12) 0.097(7) Uani 1 1 d . . . H23A H 0.4594 0.2496 -0.3893 0.146 Uiso 1 1 calc R . . H23B H 0.3681 0.1962 -0.4275 0.146 Uiso 1 1 calc R . . H23C H 0.4342 0.1574 -0.3255 0.146 Uiso 1 1 calc R . . C24 C 0.2794(13) 0.2132(10) -0.2310(17) 0.069(4) Uani 1 1 d . . . H24A H 0.2481 0.2502 -0.1761 0.104 Uiso 1 1 calc R . . H24B H 0.3030 0.1577 -0.1933 0.104 Uiso 1 1 calc R . . H24C H 0.2367 0.1967 -0.2951 0.104 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 Pb1 0.03576(19) 0.04742(17) 0.05654(19) -0.0064(3) 0.00207(12) -0.0024(3) O1 0.044(4) 0.041(4) 0.070(4) -0.011(3) 0.014(3) -0.004(3) O2 0.043(4) 0.051(4) 0.055(4) -0.006(3) 0.004(3) 0.001(3) O3 0.063(5) 0.051(4) 0.053(4) -0.003(3) -0.002(4) 0.012(3) O4 0.051(5) 0.070(5) 0.043(4) -0.006(3) 0.007(3) -0.013(3) C1 0.036(5) 0.047(5) 0.034(4) 0.002(4) -0.002(4) 0.006(4) C2 0.040(5) 0.039(5) 0.043(5) 0.001(4) 0.001(4) -0.004(4) C3 0.044(6) 0.044(5) 0.055(5) -0.005(4) 0.002(4) -0.010(4) C4 0.043(7) 0.045(5) 0.066(7) 0.000(5) 0.000(5) -0.013(5) C5 0.046(6) 0.054(7) 0.058(6) 0.012(5) 0.017(5) 0.000(5) C6 0.041(6) 0.034(4) 0.043(5) 0.000(4) -0.008(4) 0.009(4) C7 0.046(8) 0.051(7) 0.054(8) -0.013(5) -0.002(6) 0.001(6) C8 0.080(10) 0.058(7) 0.099(10) -0.010(7) 0.011(8) 0.017(7) C9 0.062(10) 0.071(8) 0.074(8) -0.003(7) 0.017(7) 0.009(7) C10 0.028(7) 0.055(7) 0.055(7) 0.005(5) 0.009(5) -0.002(4) C11 0.045(9) 0.077(10) 0.058(8) 0.007(7) 0.009(8) 0.003(7) C12 0.062(9) 0.071(7) 0.078(8) 0.000(7) -0.006(7) 0.018(7) C13 0.035(5) 0.045(5) 0.053(5) -0.001(4) 0.007(4) -0.004(4) C14 0.067(7) 0.038(5) 0.048(5) 0.003(4) 0.005(5) -0.001(5) C15 0.079(10) 0.038(5) 0.062(7) -0.003(5) 0.015(6) 0.007(5) C16 0.041(7) 0.058(7) 0.067(7) 0.011(6) 0.012(5) 0.000(5) C17 0.043(6) 0.062(6) 0.050(5) 0.018(5) 0.002(5) -0.004(5) C18 0.053(7) 0.059(6) 0.043(5) 0.004(5) 0.011(4) -0.015(5) C19 0.036(7) 0.075(9) 0.053(6) -0.032(7) 0.001(5) 0.003(6) C20 0.058(8) 0.083(8) 0.056(6) -0.008(6) 0.008(5) 0.007(6) C21 0.072(13) 0.062(11) 0.078(10) -0.021(9) 0.000(8) -0.009(7) C22 0.079(11) 0.054(7) 0.049(7) 0.022(6) -0.015(7) -0.018(6) C23 0.15(2) 0.099(12) 0.042(6) -0.010(7) 0.000(9) -0.018(10) C24 0.061(10) 0.072(9) 0.073(10) 0.022(7) -0.012(9) -0.016(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 Pb1 C1 2.253(10) . ? Pb1 C13 2.276(10) . ? O1 C2 1.380(12) . ? O1 C7 1.453(14) . ? O2 C6 1.386(11) . ? O2 C10 1.461(17) . ? O3 C14 1.367(12) . ? O3 C19 1.433(14) . ? O4 C18 1.383(14) . ? O4 C22 1.436(16) . ? C1 C2 1.375(13) . ? C1 C6 1.398(15) . ? C2 C3 1.397(14) . ? C3 C4 1.383(17) . ? C3 H3 0.9400 . ? C4 C5 1.350(16) . ? C4 H4 0.9400 . ? C5 C6 1.384(15) . ? C5 H5 0.9400 . ? C7 C8 1.492(18) . ? C7 C9 1.49(2) . ? C7 H7 0.9900 . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C8 H8C 0.9700 . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C9 H9C 0.9700 . ? C10 C11 1.49(2) . ? C10 C12 1.517(18) . ? C10 H10 0.9900 . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C11 H11C 0.9700 . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C12 H12C 0.9700 . ? C13 C18 1.340(14) . ? C13 C14 1.395(14) . ? C14 C15 1.383(16) . ? C15 C16 1.377(17) . ? C15 H15 0.9400 . ? C16 C17 1.372(18) . ? C16 H16 0.9400 . ? C17 C18 1.405(17) . ? C17 H17 0.9400 . ? C19 C21 1.48(2) . ? C19 C20 1.495(18) . ? C19 H19 0.9900 . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C20 H20C 0.9700 . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C21 H21C 0.9700 . ? C22 C23 1.52(3) . ? C22 C24 1.53(2) . ? C22 H22 0.9900 . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C23 H23C 0.9700 . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C24 H24C 0.9700 . ? 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 C1 Pb1 C13 93.0(3) . . ? C2 O1 C7 119.3(8) . . ? C6 O2 C10 119.8(9) . . ? C14 O3 C19 119.6(8) . . ? C18 O4 C22 120.8(11) . . ? C2 C1 C6 116.3(9) . . ? C2 C1 Pb1 116.7(7) . . ? C6 C1 Pb1 126.8(7) . . ? C1 C2 O1 112.2(8) . . ? C1 C2 C3 124.1(10) . . ? O1 C2 C3 123.6(9) . . ? C4 C3 C2 116.6(10) . . ? C4 C3 H3 121.7 . . ? C2 C3 H3 121.7 . . ? C5 C4 C3 121.7(10) . . ? C5 C4 H4 119.2 . . ? C3 C4 H4 119.2 . . ? C4 C5 C6 120.5(11) . . ? C4 C5 H5 119.7 . . ? C6 C5 H5 119.7 . . ? C5 C6 O2 124.9(10) . . ? C5 C6 C1 120.9(9) . . ? O2 C6 C1 114.1(8) . . ? O1 C7 C8 111.3(10) . . ? O1 C7 C9 106.4(9) . . ? C8 C7 C9 113.2(13) . . ? O1 C7 H7 108.6 . . ? C8 C7 H7 108.6 . . ? C9 C7 H7 108.6 . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? O2 C10 C11 107.7(13) . . ? O2 C10 C12 109.5(12) . . ? C11 C10 C12 113.4(10) . . ? O2 C10 H10 108.7 . . ? C11 C10 H10 108.7 . . ? C12 C10 H10 108.7 . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C18 C13 C14 121.2(10) . . ? C18 C13 Pb1 120.4(8) . . ? C14 C13 Pb1 118.3(7) . . ? O3 C14 C15 126.1(10) . . ? O3 C14 C13 114.8(9) . . ? C15 C14 C13 119.0(10) . . ? C16 C15 C14 119.2(11) . . ? C16 C15 H15 120.4 . . ? C14 C15 H15 120.4 . . ? C17 C16 C15 122.0(11) . . ? C17 C16 H16 119.0 . . ? C15 C16 H16 119.0 . . ? C16 C17 C18 118.0(10) . . ? C16 C17 H17 121.0 . . ? C18 C17 H17 121.0 . . ? C13 C18 O4 114.3(10) . . ? C13 C18 C17 120.5(10) . . ? O4 C18 C17 125.1(9) . . ? O3 C19 C21 111.0(10) . . ? O3 C19 C20 106.4(10) . . ? C21 C19 C20 113.4(11) . . ? O3 C19 H19 108.7 . . ? C21 C19 H19 108.7 . . ? C20 C19 H19 108.7 . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C19 C21 H21A 109.5 . . ? C19 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C19 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? O4 C22 C23 105.1(15) . . ? O4 C22 C24 109.0(13) . . ? C23 C22 C24 111.3(14) . . ? O4 C22 H22 110.4 . . ? C23 C22 H22 110.4 . . ? C24 C22 H22 110.4 . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C22 C24 H24A 109.5 . . ? C22 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C22 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 26.04 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 2.658 _refine_diff_density_min -1.061 _refine_diff_density_rms 0.147 #\#CIF_1.1 data_c1388 _database_code_depnum_ccdc_archive 'CCDC 864030' #TrackingRef 'ccdc_sub.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C72 H102 O12 Pb Sn2 , 3(C6 H6) ' _chemical_formula_sum 'C90 H120 O12 Pb Sn2' _chemical_formula_weight 1838.43 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sn Sn -0.6537 1.4246 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.272(2) _cell_length_b 15.377(3) _cell_length_c 25.439(4) _cell_angle_alpha 96.850(3) _cell_angle_beta 102.309(3) _cell_angle_gamma 109.506(3) _cell_volume 4325.5(12) _cell_formula_units_Z 2 _cell_measurement_temperature 208(2) _cell_measurement_reflns_used 1235 _cell_measurement_theta_min 2 _cell_measurement_theta_max 27 _exptl_crystal_description prism _exptl_crystal_colour green _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.412 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1876 _exptl_absorpt_coefficient_mu 2.572 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.6273 _exptl_absorpt_correction_T_max 0.7830 _exptl_absorpt_process_details ; G.M.Sheldrick (1996) Program for Absorption Correction ' ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 208(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'SMART CCD-Diffractometer (BRUKER AXS)' _diffrn_measurement_method Omega-scans _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 53958 _diffrn_reflns_av_R_equivalents 0.0284 _diffrn_reflns_av_sigmaI/netI 0.0424 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_theta_min 0.84 _diffrn_reflns_theta_max 29.03 _reflns_number_total 22639 _reflns_number_gt 17703 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker AXS)' _computing_cell_refinement 'SAINT (BRUKER AXS)' _computing_data_reduction 'SAINT (BRUKER AXS)' _computing_structure_solution 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP for Windows (L.J.Farrugia' _computing_publication_material 'WINGX (L.J.Farrugia' _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^)+(0.0349P)^2^+0.5189P] 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 22639 _refine_ls_number_parameters 910 _refine_ls_number_restraints 72 _refine_ls_R_factor_all 0.0481 _refine_ls_R_factor_gt 0.0292 _refine_ls_wR_factor_ref 0.0722 _refine_ls_wR_factor_gt 0.0627 _refine_ls_goodness_of_fit_ref 1.036 _refine_ls_restrained_S_all 1.035 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pb1 Pb 0.276758(10) 0.192275(7) 0.203030(5) 0.02678(3) Uani 1 1 d . . . Sn1 Sn 0.135699(16) 0.104762(12) 0.275266(8) 0.02296(4) Uani 1 1 d . . . Sn2 Sn 0.283143(17) 0.383349(13) 0.194459(8) 0.02507(5) Uani 1 1 d . . . O1 O -0.15313(19) -0.00165(15) 0.26941(10) 0.0406(6) Uani 1 1 d . . . O2 O 0.14182(18) -0.05461(14) 0.19420(9) 0.0344(5) Uani 1 1 d . . . O3 O -0.03547(19) 0.20652(15) 0.25250(9) 0.0366(5) Uani 1 1 d . . . O4 O 0.1916(2) 0.15720(16) 0.40964(9) 0.0386(5) Uani 1 1 d . . . O5 O 0.11037(18) -0.06142(14) 0.34041(9) 0.0343(5) Uani 1 1 d . . . O6 O 0.42704(17) 0.18255(13) 0.30864(9) 0.0309(5) Uani 1 1 d . . . O7 O 0.1308(2) 0.20084(15) 0.09611(9) 0.0420(6) Uani 1 1 d . . . O8 O 0.3292(2) 0.52666(15) 0.11281(9) 0.0420(6) Uani 1 1 d . . . O9 O 0.50196(19) 0.36665(15) 0.16442(9) 0.0367(5) Uani 1 1 d . . . O10 O 0.4309(2) 0.60324(14) 0.26995(11) 0.0470(6) Uani 1 1 d . . . O11 O 0.0676(2) 0.45438(18) 0.14138(10) 0.0464(6) Uani 1 1 d . . . O12 O 0.2746(2) 0.42951(15) 0.31132(9) 0.0380(5) Uani 1 1 d . . . C1 C -0.0077(2) -0.02850(19) 0.22989(12) 0.0271(6) Uani 1 1 d . . . C2 C -0.1252(3) -0.0615(2) 0.23483(13) 0.0308(6) Uani 1 1 d . . . C3 C -0.2072(3) -0.1509(2) 0.20709(15) 0.0415(8) Uani 1 1 d . . . H3 H -0.2857 -0.1722 0.2111 0.050 Uiso 1 1 calc R . . C4 C -0.1720(3) -0.2074(2) 0.17388(15) 0.0431(8) Uani 1 1 d . . . H4 H -0.2277 -0.2674 0.1549 0.052 Uiso 1 1 calc R . . C5 C -0.0574(3) -0.1785(2) 0.16774(14) 0.0387(7) Uani 1 1 d . . . H5 H -0.0344 -0.2178 0.1449 0.046 Uiso 1 1 calc R . . C6 C 0.0239(3) -0.0889(2) 0.19653(12) 0.0291(6) Uani 1 1 d . . . C7 C -0.2514(3) -0.0402(2) 0.29338(15) 0.0397(8) Uani 1 1 d . . . H7 H -0.2599 -0.1054 0.2970 0.048 Uiso 1 1 calc R . . C8 C -0.3684(3) -0.0415(3) 0.25903(17) 0.0515(10) Uani 1 1 d . . . H8A H -0.3894 -0.0816 0.2231 0.077 Uiso 1 1 calc R . . H8B H -0.3601 0.0221 0.2548 0.077 Uiso 1 1 calc R . . H8C H -0.4311 -0.0657 0.2771 0.077 Uiso 1 1 calc R . . C9 C -0.2144(3) 0.0210(3) 0.35005(17) 0.0539(10) Uani 1 1 d . . . H9A H -0.1391 0.0199 0.3709 0.081 Uiso 1 1 calc R . . H9B H -0.2759 -0.0027 0.3688 0.081 Uiso 1 1 calc R . . H9C H -0.2046 0.0853 0.3468 0.081 Uiso 1 1 calc R . . C10 C 0.1944(3) -0.1189(2) 0.17454(14) 0.0392(8) Uani 1 1 d . . . H10 H 0.1580 -0.1803 0.1845 0.047 Uiso 1 1 calc R . . C11 C 0.1719(4) -0.1333(3) 0.11364(17) 0.0620(11) Uani 1 1 d . . . H11A H 0.0861 -0.1610 0.0964 0.093 Uiso 1 1 calc R . . H11B H 0.2096 -0.1753 0.1014 0.093 Uiso 1 1 calc R . . H11C H 0.2054 -0.0731 0.1035 0.093 Uiso 1 1 calc R . . C12 C 0.3261(3) -0.0764(3) 0.20447(18) 0.0570(10) Uani 1 1 d . . . H12A H 0.3357 -0.0682 0.2438 0.085 Uiso 1 1 calc R . . H12B H 0.3620 -0.0156 0.1954 0.085 Uiso 1 1 calc R . . H12C H 0.3654 -0.1180 0.1935 0.085 Uiso 1 1 calc R . . C13 C 0.0738(2) 0.18152(19) 0.33198(12) 0.0269(6) Uani 1 1 d . . . C14 C 0.1108(3) 0.1971(2) 0.38898(13) 0.0310(7) Uani 1 1 d . . . C15 C 0.0698(3) 0.2509(2) 0.42205(14) 0.0365(7) Uani 1 1 d . . . H15 H 0.0938 0.2593 0.4605 0.044 Uiso 1 1 calc R . . C16 C -0.0066(3) 0.2917(2) 0.39730(15) 0.0408(8) Uani 1 1 d . . . H16 H -0.0343 0.3282 0.4195 0.049 Uiso 1 1 calc R . . C17 C -0.0432(3) 0.2807(2) 0.34162(14) 0.0368(7) Uani 1 1 d . . . H17 H -0.0938 0.3103 0.3256 0.044 Uiso 1 1 calc R . . C18 C -0.0038(3) 0.2243(2) 0.30862(13) 0.0309(6) Uani 1 1 d . . . C19 C -0.1110(3) 0.2498(2) 0.22384(14) 0.0390(8) Uani 1 1 d . . . H19 H -0.0817 0.3177 0.2408 0.047 Uiso 1 1 calc R . . C20 C -0.2402(3) 0.2012(3) 0.22525(18) 0.0581(10) Uani 1 1 d . . . H20A H -0.2450 0.2101 0.2630 0.087 Uiso 1 1 calc R . . H20B H -0.2671 0.1343 0.2099 0.087 Uiso 1 1 calc R . . H20C H -0.2910 0.2282 0.2037 0.087 Uiso 1 1 calc R . . C21 C -0.1003(3) 0.2380(3) 0.16583(15) 0.0504(9) Uani 1 1 d . . . H21A H -0.0174 0.2696 0.1660 0.076 Uiso 1 1 calc R . . H21B H -0.1503 0.2654 0.1441 0.076 Uiso 1 1 calc R . . H21C H -0.1265 0.1714 0.1500 0.076 Uiso 1 1 calc R . . C22 C 0.2330(3) 0.1656(3) 0.46749(14) 0.0422(8) Uani 1 1 d . . . H22 H 0.2443 0.2291 0.4869 0.051 Uiso 1 1 calc R . . C23 C 0.3533(3) 0.1544(3) 0.47630(17) 0.0590(11) Uani 1 1 d . . . H23A H 0.4074 0.2034 0.4631 0.088 Uiso 1 1 calc R . . H23B H 0.3424 0.0931 0.4562 0.088 Uiso 1 1 calc R . . H23C H 0.3870 0.1597 0.5152 0.088 Uiso 1 1 calc R . . C24 C 0.1453(4) 0.0918(4) 0.4873(2) 0.0770(15) Uani 1 1 d . . . H24A H 0.0700 0.1017 0.4814 0.116 Uiso 1 1 calc R . . H24B H 0.1776 0.0961 0.5262 0.116 Uiso 1 1 calc R . . H24C H 0.1316 0.0298 0.4671 0.116 Uiso 1 1 calc R . . C25 C 0.2672(3) 0.05654(19) 0.32209(12) 0.0260(6) Uani 1 1 d . . . C26 C 0.2303(3) -0.0253(2) 0.34321(12) 0.0286(6) Uani 1 1 d . . . C27 C 0.3106(3) -0.0654(2) 0.36653(14) 0.0350(7) Uani 1 1 d . . . H27 H 0.2835 -0.1213 0.3796 0.042 Uiso 1 1 calc R . . C28 C 0.4305(3) -0.0213(2) 0.36998(14) 0.0382(7) Uani 1 1 d . . . H28 H 0.4851 -0.0481 0.3853 0.046 Uiso 1 1 calc R . . C29 C 0.4727(3) 0.0611(2) 0.35163(13) 0.0344(7) Uani 1 1 d . . . H29 H 0.5550 0.0910 0.3549 0.041 Uiso 1 1 calc R . . C30 C 0.3903(3) 0.09925(19) 0.32803(12) 0.0283(6) Uani 1 1 d . . . C31 C 0.0617(3) -0.1513(2) 0.35572(15) 0.0387(8) Uani 1 1 d . . . H31 H 0.1153 -0.1524 0.3905 0.046 Uiso 1 1 calc R . . C32 C -0.0582(3) -0.1577(3) 0.36440(19) 0.0621(12) Uani 1 1 d . . . H32A H -0.0468 -0.1056 0.3932 0.093 Uiso 1 1 calc R . . H32B H -0.0951 -0.2169 0.3750 0.093 Uiso 1 1 calc R . . H32C H -0.1098 -0.1548 0.3305 0.093 Uiso 1 1 calc R . . C33 C 0.0491(4) -0.2309(2) 0.31135(19) 0.0602(11) Uani 1 1 d . . . H33A H 0.1279 -0.2253 0.3073 0.090 Uiso 1 1 calc R . . H33B H -0.0004 -0.2281 0.2769 0.090 Uiso 1 1 calc R . . H33C H 0.0118 -0.2907 0.3213 0.090 Uiso 1 1 calc R . . C34 C 0.5554(3) 0.2362(2) 0.32141(14) 0.0355(7) Uani 1 1 d . . . H34 H 0.5951 0.1937 0.3097 0.043 Uiso 1 1 calc R . . C35 C 0.5697(3) 0.3112(2) 0.28692(15) 0.0457(9) Uani 1 1 d . . . H35A H 0.5336 0.2813 0.2484 0.069 Uiso 1 1 calc R . . H35B H 0.6544 0.3474 0.2927 0.069 Uiso 1 1 calc R . . H35C H 0.5303 0.3528 0.2977 0.069 Uiso 1 1 calc R . . C36 C 0.6106(3) 0.2780(2) 0.38226(15) 0.0468(9) Uani 1 1 d . . . H36A H 0.5996 0.2277 0.4026 0.070 Uiso 1 1 calc R . . H36B H 0.5718 0.3193 0.3942 0.070 Uiso 1 1 calc R . . H36C H 0.6957 0.3138 0.3889 0.070 Uiso 1 1 calc R . . C37 C 0.2387(3) 0.3640(2) 0.10453(12) 0.0298(6) Uani 1 1 d . . . C38 C 0.1803(3) 0.2746(2) 0.07069(13) 0.0362(7) Uani 1 1 d . . . C39 C 0.1719(3) 0.2592(3) 0.01419(14) 0.0482(9) Uani 1 1 d . . . H39 H 0.1346 0.1980 -0.0077 0.058 Uiso 1 1 calc R . . C40 C 0.2190(3) 0.3352(3) -0.00846(15) 0.0502(9) Uani 1 1 d . . . H40 H 0.2142 0.3252 -0.0462 0.060 Uiso 1 1 calc R . . C41 C 0.2731(3) 0.4253(3) 0.02257(14) 0.0438(8) Uani 1 1 d . . . H41 H 0.3039 0.4767 0.0063 0.053 Uiso 1 1 calc R . . C42 C 0.2814(3) 0.4391(2) 0.07880(14) 0.0356(7) Uani 1 1 d . . . C43 C 0.3885(3) 0.6083(2) 0.09240(15) 0.0447(9) Uani 1 1 d . . . H43 H 0.3383 0.6070 0.0561 0.054 Uiso 1 1 calc R . . C44 C 0.5105(3) 0.6103(3) 0.08744(19) 0.0617(12) Uani 1 1 d . . . H44A H 0.4999 0.5563 0.0601 0.093 Uiso 1 1 calc R . . H44B H 0.5577 0.6080 0.1227 0.093 Uiso 1 1 calc R . . H44C H 0.5518 0.6679 0.0764 0.093 Uiso 1 1 calc R . . C45 C 0.3986(4) 0.6919(3) 0.13414(19) 0.0657(12) Uani 1 1 d . . . H45A H 0.3189 0.6882 0.1356 0.099 Uiso 1 1 calc R . . H45B H 0.4391 0.7500 0.1233 0.099 Uiso 1 1 calc R . . H45C H 0.4441 0.6908 0.1701 0.099 Uiso 1 1 calc R . . C46 C 0.0426(4) 0.1125(2) 0.06176(15) 0.0507(10) Uani 1 1 d . . . H46 H 0.0760 0.0880 0.0338 0.061 Uiso 1 1 calc R . . C47 C 0.0154(4) 0.0454(2) 0.09959(16) 0.0558(10) Uani 1 1 d . . . H47A H 0.0880 0.0362 0.1170 0.084 Uiso 1 1 calc R . . H47B H -0.0449 -0.0146 0.0787 0.084 Uiso 1 1 calc R . . H47C H -0.0145 0.0712 0.1276 0.084 Uiso 1 1 calc R . . C48 C -0.0734(4) 0.1263(3) 0.03363(18) 0.0666(12) Uani 1 1 d . . . H48A H -0.0560 0.1692 0.0089 0.100 Uiso 1 1 calc R . . H48B H -0.1037 0.1523 0.0614 0.100 Uiso 1 1 calc R . . H48C H -0.1333 0.0659 0.0130 0.100 Uiso 1 1 calc R . . C49 C 0.4684(3) 0.4847(2) 0.21775(12) 0.0285(6) Uani 1 1 d . . . C50 C 0.5498(3) 0.4569(2) 0.19659(13) 0.0319(7) Uani 1 1 d . . . C51 C 0.6702(3) 0.5147(2) 0.20689(15) 0.0420(8) Uani 1 1 d . . . H51 H 0.7238 0.4931 0.1930 0.050 Uiso 1 1 calc R . . C52 C 0.7082(3) 0.6044(2) 0.23798(15) 0.0465(9) Uani 1 1 d . . . H52 H 0.7886 0.6449 0.2448 0.056 Uiso 1 1 calc R . . C53 C 0.6309(3) 0.6358(2) 0.25917(15) 0.0439(8) Uani 1 1 d . . . H53 H 0.6585 0.6974 0.2801 0.053 Uiso 1 1 calc R . . C54 C 0.5121(3) 0.5768(2) 0.24966(13) 0.0342(7) Uani 1 1 d . . . C55 C 0.5706(3) 0.3355(2) 0.13282(15) 0.0428(8) Uani 1 1 d . . . H55 H 0.6519 0.3489 0.1567 0.051 Uiso 1 1 calc R . . C56 C 0.5046(4) 0.2303(3) 0.11453(17) 0.0541(10) Uani 1 1 d . . . H56A H 0.5003 0.2021 0.1465 0.081 Uiso 1 1 calc R . . H56B H 0.5471 0.2040 0.0931 0.081 Uiso 1 1 calc R . . H56C H 0.4241 0.2171 0.0922 0.081 Uiso 1 1 calc R . . C58 C 0.4539(4) 0.7024(2) 0.28698(16) 0.0481(9) Uani 1 1 d . . . H58 H 0.4984 0.7380 0.2633 0.058 Uiso 1 1 calc R . . C57 C 0.5810(4) 0.3845(3) 0.08459(17) 0.0634(12) Uani 1 1 d . . . H57A H 0.6246 0.4517 0.0983 0.095 Uiso 1 1 calc R . . H57B H 0.5014 0.3736 0.0621 0.095 Uiso 1 1 calc R . . H57C H 0.6237 0.3595 0.0627 0.095 Uiso 1 1 calc R . . C59 C 0.5269(4) 0.7412(3) 0.34667(17) 0.0659(12) Uani 1 1 d . . . H59A H 0.6045 0.7353 0.3513 0.099 Uiso 1 1 calc R . . H59B H 0.4845 0.7059 0.3701 0.099 Uiso 1 1 calc R . . H59C H 0.5383 0.8071 0.3567 0.099 Uiso 1 1 calc R . . C60 C 0.3326(4) 0.7096(3) 0.2769(2) 0.0647(12) Uani 1 1 d . . . H60A H 0.2895 0.6845 0.2384 0.097 Uiso 1 1 calc R . . H60B H 0.3420 0.7752 0.2864 0.097 Uiso 1 1 calc R . . H60C H 0.2877 0.6738 0.2994 0.097 Uiso 1 1 calc R . . C61 C 0.1712(3) 0.4462(2) 0.22758(13) 0.0313(7) Uani 1 1 d . . . C62 C 0.0823(3) 0.4713(2) 0.19712(15) 0.0366(7) Uani 1 1 d . . . C63 C 0.0125(3) 0.5089(2) 0.22235(17) 0.0463(9) Uani 1 1 d . . . H63 H -0.0450 0.5281 0.2015 0.056 Uiso 1 1 calc R . . C64 C 0.0297(3) 0.5173(2) 0.27832(17) 0.0474(9) Uani 1 1 d . . . H64 H -0.0181 0.5413 0.2954 0.057 Uiso 1 1 calc R . . C65 C 0.1152(3) 0.4912(2) 0.31008(16) 0.0426(8) Uani 1 1 d . . . H65 H 0.1253 0.4967 0.3482 0.051 Uiso 1 1 calc R . . C66 C 0.1859(3) 0.4567(2) 0.28422(14) 0.0347(7) Uani 1 1 d . . . C67 C 0.2971(3) 0.4330(2) 0.36953(13) 0.0384(7) Uani 1 1 d . . . H67 H 0.2202 0.4064 0.3790 0.046 Uiso 1 1 calc R . . C68 C 0.3705(3) 0.3727(3) 0.38168(16) 0.0485(9) Uani 1 1 d . . . H68A H 0.3251 0.3087 0.3610 0.073 Uiso 1 1 calc R . . H68B H 0.3891 0.3727 0.4207 0.073 Uiso 1 1 calc R . . H68C H 0.4445 0.3979 0.3711 0.073 Uiso 1 1 calc R . . C69 C 0.3653(4) 0.5341(3) 0.40138(17) 0.0565(10) Uani 1 1 d . . . H69A H 0.3160 0.5712 0.3932 0.085 Uiso 1 1 calc R . . H69B H 0.4389 0.5607 0.3907 0.085 Uiso 1 1 calc R . . H69C H 0.3846 0.5349 0.4405 0.085 Uiso 1 1 calc R . . C70 C -0.0229(4) 0.4753(3) 0.10530(17) 0.0542(10) Uani 1 1 d . . . H70 H -0.0959 0.4590 0.1186 0.065 Uiso 1 1 calc R . . C71 C -0.0504(4) 0.4122(3) 0.05016(19) 0.0735(13) Uani 1 1 d . . . H71A H -0.0798 0.3468 0.0535 0.110 Uiso 1 1 calc R . . H71B H 0.0221 0.4258 0.0379 0.110 Uiso 1 1 calc R . . H71C H -0.1111 0.4235 0.0236 0.110 Uiso 1 1 calc R . . C72 C 0.0212(5) 0.5784(3) 0.1031(2) 0.0843(16) Uani 1 1 d . . . H72A H 0.0359 0.6159 0.1392 0.126 Uiso 1 1 calc R . . H72B H -0.0391 0.5905 0.0768 0.126 Uiso 1 1 calc R . . H72C H 0.0950 0.5952 0.0919 0.126 Uiso 1 1 calc R . . C73 C 0.7222(2) 0.11505(14) 0.48374(10) 0.0535(10) Uani 1 1 d G . . H73 H 0.6916 0.0536 0.4623 0.064 Uiso 1 1 calc R . . C74 C 0.8420(2) 0.17181(18) 0.49234(11) 0.0587(11) Uani 1 1 d G . . H74 H 0.8924 0.1488 0.4767 0.070 Uiso 1 1 calc R . . C75 C 0.88738(19) 0.26261(17) 0.52408(12) 0.0593(11) Uani 1 1 d G . . H75 H 0.9684 0.3010 0.5299 0.071 Uiso 1 1 calc R . . C76 C 0.8129(3) 0.29667(14) 0.54723(11) 0.0669(12) Uani 1 1 d G . . H76 H 0.8436 0.3581 0.5687 0.080 Uiso 1 1 calc R . . C77 C 0.6931(2) 0.2399(2) 0.53864(11) 0.0664(12) Uani 1 1 d G . . H77 H 0.6427 0.2629 0.5543 0.080 Uiso 1 1 calc R . . C78 C 0.64774(18) 0.14910(18) 0.50689(11) 0.0578(10) Uani 1 1 d G . . H78 H 0.5667 0.1107 0.5011 0.069 Uiso 1 1 calc R . . C79 C 0.8681(2) 0.5002(2) 0.39886(13) 0.0643(12) Uani 1 1 d GU . . H79 H 0.9172 0.4792 0.3811 0.077 Uiso 1 1 calc R . . C80 C 0.8661(2) 0.48665(19) 0.45176(13) 0.0662(12) Uani 1 1 d GU . . H80 H 0.9139 0.4566 0.4697 0.079 Uiso 1 1 calc R . . C81 C 0.7934(3) 0.5176(2) 0.47809(10) 0.0731(13) Uani 1 1 d GU . . H81 H 0.7921 0.5084 0.5139 0.088 Uiso 1 1 calc R . . C82 C 0.7227(3) 0.5620(2) 0.45152(15) 0.0817(15) Uani 1 1 d GU . . H82 H 0.6736 0.5829 0.4693 0.098 Uiso 1 1 calc R . . C83 C 0.7247(3) 0.5755(2) 0.39862(15) 0.0810(15) Uani 1 1 d GU . . H83 H 0.6769 0.6056 0.3806 0.097 Uiso 1 1 calc R . . C84 C 0.7974(3) 0.5446(2) 0.37229(10) 0.0717(13) Uani 1 1 d GU . . H84 H 0.7987 0.5537 0.3365 0.086 Uiso 1 1 calc R . . C85 C 0.4513(4) 0.8659(4) 0.02310(16) 0.137(3) Uani 1 1 d GU . . H85 H 0.3828 0.8326 -0.0064 0.164 Uiso 1 1 calc R . . C86 C 0.4549(4) 0.9433(4) 0.0587(2) 0.121(2) Uani 1 1 d GU . . H86 H 0.3888 0.9624 0.0533 0.145 Uiso 1 1 calc R . . C87 C 0.5561(5) 0.9925(3) 0.10235(19) 0.112(2) Uani 1 1 d GU . . H87 H 0.5585 1.0449 0.1264 0.134 Uiso 1 1 calc R . . C88 C 0.6538(3) 0.9643(3) 0.11033(17) 0.1015(19) Uani 1 1 d GU . . H88 H 0.7223 0.9976 0.1398 0.122 Uiso 1 1 calc R . . C89 C 0.6502(4) 0.8868(3) 0.0747(2) 0.107(2) Uani 1 1 d GU . . H89 H 0.7163 0.8677 0.0801 0.128 Uiso 1 1 calc R . . C90 C 0.5490(6) 0.8376(3) 0.03109(17) 0.136(3) Uani 1 1 d GU . . H90 H 0.5466 0.7853 0.0070 0.164 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 Pb1 0.02749(6) 0.02362(6) 0.02930(6) 0.00466(4) 0.01020(5) 0.00826(4) Sn1 0.02035(9) 0.01949(9) 0.02821(11) 0.00423(8) 0.00711(8) 0.00625(7) Sn2 0.02581(10) 0.02171(9) 0.02713(11) 0.00499(8) 0.00929(8) 0.00682(7) O1 0.0272(11) 0.0298(11) 0.0615(16) 0.0013(11) 0.0219(11) 0.0031(9) O2 0.0281(11) 0.0298(11) 0.0436(13) -0.0007(9) 0.0128(10) 0.0097(9) O3 0.0381(12) 0.0432(13) 0.0373(13) 0.0102(10) 0.0102(10) 0.0254(10) O4 0.0425(13) 0.0475(13) 0.0325(12) 0.0050(10) 0.0101(10) 0.0262(11) O5 0.0302(11) 0.0285(11) 0.0465(14) 0.0175(10) 0.0127(10) 0.0090(9) O6 0.0223(10) 0.0265(10) 0.0409(13) 0.0098(9) 0.0068(9) 0.0054(8) O7 0.0525(14) 0.0295(11) 0.0303(12) 0.0008(9) 0.0013(11) 0.0059(10) O8 0.0479(14) 0.0340(12) 0.0382(13) 0.0138(10) 0.0123(11) 0.0051(10) O9 0.0321(12) 0.0367(12) 0.0447(14) 0.0057(10) 0.0165(10) 0.0140(10) O10 0.0522(15) 0.0224(11) 0.0634(17) -0.0018(11) 0.0294(13) 0.0051(10) O11 0.0453(14) 0.0614(16) 0.0475(15) 0.0232(13) 0.0154(12) 0.0327(12) O12 0.0429(13) 0.0423(13) 0.0331(13) 0.0057(10) 0.0146(11) 0.0192(11) C1 0.0241(14) 0.0227(13) 0.0314(16) 0.0052(12) 0.0045(12) 0.0066(11) C2 0.0267(15) 0.0265(14) 0.0375(18) 0.0050(13) 0.0096(13) 0.0075(12) C3 0.0260(16) 0.0348(17) 0.053(2) 0.0016(15) 0.0087(15) 0.0016(13) C4 0.0362(18) 0.0282(16) 0.048(2) -0.0026(15) 0.0056(16) -0.0025(14) C5 0.0395(18) 0.0301(16) 0.0396(19) -0.0029(14) 0.0102(15) 0.0078(14) C6 0.0262(15) 0.0270(14) 0.0319(16) 0.0059(12) 0.0067(13) 0.0079(12) C7 0.0290(17) 0.0383(18) 0.054(2) 0.0119(16) 0.0200(16) 0.0084(14) C8 0.0354(19) 0.051(2) 0.072(3) 0.018(2) 0.0197(19) 0.0159(16) C9 0.051(2) 0.052(2) 0.062(3) 0.0068(19) 0.031(2) 0.0146(18) C10 0.0375(18) 0.0387(18) 0.041(2) -0.0019(15) 0.0105(15) 0.0174(15) C11 0.063(3) 0.080(3) 0.050(3) 0.004(2) 0.021(2) 0.035(2) C12 0.043(2) 0.064(3) 0.066(3) -0.002(2) 0.011(2) 0.0300(19) C13 0.0253(14) 0.0206(13) 0.0351(17) 0.0053(12) 0.0118(13) 0.0068(11) C14 0.0296(16) 0.0246(14) 0.0392(18) 0.0064(13) 0.0134(14) 0.0082(12) C15 0.0437(19) 0.0354(17) 0.0341(18) 0.0050(14) 0.0173(15) 0.0159(14) C16 0.052(2) 0.0346(17) 0.049(2) 0.0085(15) 0.0271(18) 0.0236(16) C17 0.0395(18) 0.0324(16) 0.047(2) 0.0109(15) 0.0169(16) 0.0202(14) C18 0.0298(16) 0.0263(14) 0.0377(18) 0.0076(13) 0.0114(14) 0.0101(12) C19 0.0379(18) 0.0342(17) 0.047(2) 0.0142(15) 0.0079(16) 0.0164(14) C20 0.039(2) 0.070(3) 0.067(3) 0.014(2) 0.013(2) 0.0229(19) C21 0.051(2) 0.047(2) 0.050(2) 0.0163(18) 0.0083(18) 0.0161(18) C22 0.049(2) 0.050(2) 0.0312(18) 0.0052(15) 0.0092(16) 0.0250(17) C23 0.051(2) 0.083(3) 0.044(2) 0.009(2) 0.0033(19) 0.035(2) C24 0.075(3) 0.105(4) 0.088(4) 0.060(3) 0.044(3) 0.052(3) C25 0.0268(14) 0.0247(14) 0.0258(15) 0.0016(11) 0.0070(12) 0.0099(11) C26 0.0282(15) 0.0253(14) 0.0289(16) 0.0014(12) 0.0052(13) 0.0088(12) C27 0.0351(17) 0.0254(15) 0.0412(19) 0.0091(13) 0.0027(14) 0.0110(13) C28 0.0362(18) 0.0326(16) 0.046(2) 0.0062(15) 0.0022(15) 0.0194(14) C29 0.0248(15) 0.0330(16) 0.0431(19) 0.0036(14) 0.0050(14) 0.0117(13) C30 0.0280(15) 0.0236(14) 0.0299(16) 0.0016(12) 0.0066(13) 0.0075(12) C31 0.0356(17) 0.0327(16) 0.049(2) 0.0202(15) 0.0127(16) 0.0099(14) C32 0.049(2) 0.061(3) 0.090(3) 0.042(2) 0.036(2) 0.018(2) C33 0.049(2) 0.0301(18) 0.084(3) 0.0015(19) 0.008(2) 0.0023(16) C34 0.0200(14) 0.0334(16) 0.047(2) 0.0068(14) 0.0083(14) 0.0026(12) C35 0.0323(18) 0.0439(19) 0.051(2) 0.0169(17) 0.0068(16) 0.0021(15) C36 0.0374(19) 0.0384(18) 0.050(2) 0.0057(16) -0.0026(16) 0.0052(15) C37 0.0292(15) 0.0324(15) 0.0291(16) 0.0083(13) 0.0081(13) 0.0124(12) C38 0.0402(18) 0.0379(17) 0.0292(17) 0.0049(14) 0.0066(14) 0.0152(14) C39 0.054(2) 0.047(2) 0.0330(19) 0.0004(16) 0.0076(17) 0.0101(17) C40 0.052(2) 0.065(3) 0.0276(18) 0.0082(17) 0.0105(16) 0.0154(19) C41 0.044(2) 0.051(2) 0.0336(19) 0.0154(16) 0.0123(16) 0.0117(16) C42 0.0294(16) 0.0376(17) 0.0365(18) 0.0090(14) 0.0077(14) 0.0084(13) C43 0.048(2) 0.0376(18) 0.047(2) 0.0226(16) 0.0124(17) 0.0087(16) C44 0.043(2) 0.054(2) 0.081(3) 0.028(2) 0.017(2) 0.0039(18) C45 0.083(3) 0.041(2) 0.071(3) 0.020(2) 0.026(3) 0.015(2) C46 0.064(2) 0.0322(18) 0.038(2) -0.0008(15) -0.0001(18) 0.0055(17) C47 0.063(3) 0.0347(19) 0.051(2) 0.0060(17) -0.003(2) 0.0063(18) C48 0.061(3) 0.076(3) 0.049(3) 0.012(2) 0.002(2) 0.016(2) C49 0.0277(15) 0.0264(14) 0.0299(16) 0.0089(12) 0.0088(13) 0.0063(12) C50 0.0301(16) 0.0311(15) 0.0337(17) 0.0107(13) 0.0096(13) 0.0084(13) C51 0.0273(17) 0.048(2) 0.052(2) 0.0179(17) 0.0136(15) 0.0116(15) C52 0.0322(18) 0.042(2) 0.054(2) 0.0150(17) 0.0065(17) 0.0003(15) C53 0.042(2) 0.0272(16) 0.048(2) 0.0051(15) 0.0064(17) -0.0005(14) C54 0.0370(17) 0.0263(15) 0.0360(18) 0.0079(13) 0.0125(14) 0.0054(13) C55 0.044(2) 0.049(2) 0.048(2) 0.0121(17) 0.0235(17) 0.0256(16) C56 0.068(3) 0.050(2) 0.058(3) 0.0088(19) 0.033(2) 0.030(2) C58 0.065(2) 0.0215(15) 0.057(2) 0.0049(15) 0.028(2) 0.0093(16) C57 0.094(3) 0.065(3) 0.052(3) 0.021(2) 0.043(2) 0.038(3) C59 0.099(4) 0.0329(19) 0.056(3) 0.0017(18) 0.028(3) 0.010(2) C60 0.076(3) 0.036(2) 0.090(3) 0.009(2) 0.038(3) 0.022(2) C61 0.0317(16) 0.0251(14) 0.0417(18) 0.0100(13) 0.0169(14) 0.0109(12) C62 0.0372(18) 0.0301(16) 0.049(2) 0.0153(15) 0.0181(16) 0.0136(14) C63 0.044(2) 0.0408(19) 0.069(3) 0.0233(18) 0.0241(19) 0.0251(16) C64 0.049(2) 0.0350(18) 0.072(3) 0.0129(18) 0.034(2) 0.0214(16) C65 0.050(2) 0.0358(18) 0.050(2) 0.0085(16) 0.0275(18) 0.0173(16) C66 0.0347(17) 0.0271(15) 0.0433(19) 0.0066(14) 0.0162(15) 0.0096(13) C67 0.0422(19) 0.0371(17) 0.0336(18) 0.0067(14) 0.0155(15) 0.0090(14) C68 0.048(2) 0.048(2) 0.046(2) 0.0117(17) 0.0106(18) 0.0134(17) C69 0.062(3) 0.044(2) 0.051(2) -0.0045(18) 0.013(2) 0.0095(19) C70 0.047(2) 0.062(2) 0.061(3) 0.024(2) 0.0099(19) 0.0281(19) C71 0.064(3) 0.084(3) 0.068(3) 0.024(3) 0.001(2) 0.030(3) C72 0.106(4) 0.072(3) 0.084(4) 0.039(3) 0.015(3) 0.043(3) C73 0.058(3) 0.058(2) 0.043(2) 0.0093(18) 0.0110(19) 0.022(2) C74 0.062(3) 0.067(3) 0.057(3) 0.018(2) 0.027(2) 0.029(2) C75 0.063(3) 0.053(2) 0.062(3) 0.020(2) 0.021(2) 0.015(2) C76 0.094(4) 0.046(2) 0.066(3) 0.010(2) 0.026(3) 0.030(2) C77 0.075(3) 0.071(3) 0.073(3) 0.016(2) 0.031(3) 0.044(3) C78 0.050(2) 0.069(3) 0.061(3) 0.021(2) 0.013(2) 0.029(2) C79 0.054(3) 0.050(2) 0.079(3) 0.003(2) 0.019(2) 0.009(2) C80 0.054(3) 0.052(2) 0.070(3) 0.001(2) -0.007(2) 0.009(2) C81 0.091(4) 0.065(3) 0.044(3) -0.001(2) 0.008(2) 0.015(3) C82 0.070(3) 0.064(3) 0.106(4) -0.007(3) 0.036(3) 0.020(3) C83 0.072(3) 0.063(3) 0.105(4) 0.027(3) 0.005(3) 0.029(3) C84 0.076(3) 0.061(3) 0.067(3) 0.021(2) 0.019(3) 0.009(2) C85 0.141(7) 0.164(8) 0.074(5) 0.020(5) 0.012(5) 0.029(6) C86 0.115(6) 0.178(7) 0.093(5) 0.038(5) 0.043(4) 0.070(5) C87 0.126(6) 0.092(4) 0.112(5) -0.004(4) 0.016(4) 0.052(4) C88 0.103(5) 0.067(3) 0.130(6) 0.026(4) 0.026(4) 0.029(3) C89 0.163(6) 0.102(5) 0.104(5) 0.051(4) 0.081(5) 0.072(5) C90 0.239(10) 0.110(5) 0.053(4) 0.013(4) 0.022(5) 0.069(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 Pb1 Sn1 2.9283(4) . ? Pb1 Sn2 2.9483(5) . ? Sn1 C13 2.171(3) . ? Sn1 C25 2.183(3) . ? Sn1 C1 2.188(3) . ? Sn2 C61 2.172(3) . ? Sn2 C49 2.188(3) . ? Sn2 C37 2.195(3) . ? O1 C2 1.373(4) . ? O1 C7 1.449(3) . ? O2 C6 1.382(3) . ? O2 C10 1.445(4) . ? O3 C18 1.365(4) . ? O3 C19 1.440(4) . ? O4 C14 1.377(4) . ? O4 C22 1.426(4) . ? O5 C26 1.371(3) . ? O5 C31 1.448(3) . ? O6 C30 1.395(3) . ? O6 C34 1.455(3) . ? O7 C38 1.399(4) . ? O7 C46 1.453(4) . ? O8 C42 1.372(4) . ? O8 C43 1.442(4) . ? O9 C50 1.386(4) . ? O9 C55 1.433(4) . ? O10 C54 1.366(4) . ? O10 C58 1.448(4) . ? O11 C62 1.372(4) . ? O11 C70 1.433(4) . ? O12 C66 1.374(4) . ? O12 C67 1.438(4) . ? C1 C6 1.388(4) . ? C1 C2 1.399(4) . ? C2 C3 1.394(4) . ? C3 C4 1.373(5) . ? C4 C5 1.376(5) . ? C5 C6 1.400(4) . ? C7 C8 1.507(5) . ? C7 C9 1.511(5) . ? C10 C11 1.490(5) . ? C10 C12 1.507(5) . ? C13 C14 1.389(4) . ? C13 C18 1.402(4) . ? C14 C15 1.392(4) . ? C15 C16 1.380(5) . ? C16 C17 1.363(5) . ? C17 C18 1.403(4) . ? C19 C21 1.504(5) . ? C19 C20 1.522(5) . ? C22 C24 1.501(5) . ? C22 C23 1.515(5) . ? C25 C30 1.398(4) . ? C25 C26 1.401(4) . ? C26 C27 1.395(4) . ? C27 C28 1.378(4) . ? C28 C29 1.377(4) . ? C29 C30 1.395(4) . ? C31 C33 1.505(5) . ? C31 C32 1.507(5) . ? C34 C36 1.514(5) . ? C34 C35 1.517(4) . ? C37 C38 1.393(4) . ? C37 C42 1.400(4) . ? C38 C39 1.404(5) . ? C39 C40 1.372(5) . ? C40 C41 1.374(5) . ? C41 C42 1.397(5) . ? C43 C44 1.519(5) . ? C43 C45 1.520(5) . ? C46 C47 1.499(5) . ? C46 C48 1.545(6) . ? C49 C50 1.390(4) . ? C49 C54 1.408(4) . ? C50 C51 1.394(4) . ? C51 C52 1.378(5) . ? C52 C53 1.373(5) . ? C53 C54 1.386(4) . ? C55 C56 1.508(5) . ? C55 C57 1.520(5) . ? C58 C60 1.500(6) . ? C58 C59 1.520(6) . ? C61 C62 1.390(4) . ? C61 C66 1.396(4) . ? C62 C63 1.399(5) . ? C63 C64 1.378(5) . ? C64 C65 1.382(5) . ? C65 C66 1.390(4) . ? C67 C68 1.507(5) . ? C67 C69 1.521(5) . ? C70 C72 1.508(6) . ? C70 C71 1.509(6) . ? C73 C74 1.3900 . ? C73 C78 1.3900 . ? C74 C75 1.3900 . ? C75 C76 1.3900 . ? C76 C77 1.3900 . ? C77 C78 1.3900 . ? C79 C80 1.3900 . ? C79 C84 1.3900 . ? C80 C81 1.3900 . ? C81 C82 1.3900 . ? C82 C83 1.3900 . ? C83 C84 1.3900 . ? C85 C86 1.3900 . ? C85 C90 1.3900 . ? C86 C87 1.3900 . ? C87 C88 1.3900 . ? C88 C89 1.3900 . ? C89 C90 1.3900 . ? 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 Sn1 Pb1 Sn2 114.254(8) . . ? C13 Sn1 C25 109.10(11) . . ? C13 Sn1 C1 111.02(11) . . ? C25 Sn1 C1 102.01(10) . . ? C13 Sn1 Pb1 123.65(7) . . ? C25 Sn1 Pb1 97.65(7) . . ? C1 Sn1 Pb1 110.40(8) . . ? C61 Sn2 C49 109.62(11) . . ? C61 Sn2 C37 110.95(11) . . ? C49 Sn2 C37 101.12(11) . . ? C61 Sn2 Pb1 123.38(7) . . ? C49 Sn2 Pb1 110.75(8) . . ? C37 Sn2 Pb1 98.27(8) . . ? C2 O1 C7 119.3(2) . . ? C6 O2 C10 119.8(2) . . ? C18 O3 C19 119.5(2) . . ? C14 O4 C22 120.3(2) . . ? C26 O5 C31 118.8(2) . . ? C30 O6 C34 117.6(2) . . ? C38 O7 C46 118.5(3) . . ? C42 O8 C43 119.6(3) . . ? C50 O9 C55 119.9(2) . . ? C54 O10 C58 119.7(2) . . ? C62 O11 C70 120.4(3) . . ? C66 O12 C67 120.5(2) . . ? C6 C1 C2 117.1(3) . . ? C6 C1 Sn1 116.7(2) . . ? C2 C1 Sn1 126.0(2) . . ? O1 C2 C3 122.5(3) . . ? O1 C2 C1 116.0(3) . . ? C3 C2 C1 121.4(3) . . ? C4 C3 C2 119.2(3) . . ? C3 C4 C5 121.7(3) . . ? C4 C5 C6 118.1(3) . . ? O2 C6 C1 115.1(2) . . ? O2 C6 C5 122.4(3) . . ? C1 C6 C5 122.4(3) . . ? O1 C7 C8 112.1(3) . . ? O1 C7 C9 105.6(3) . . ? C8 C7 C9 111.8(3) . . ? O2 C10 C11 110.7(3) . . ? O2 C10 C12 106.1(3) . . ? C11 C10 C12 112.8(3) . . ? C14 C13 C18 117.7(3) . . ? C14 C13 Sn1 125.7(2) . . ? C18 C13 Sn1 116.4(2) . . ? O4 C14 C13 115.2(3) . . ? O4 C14 C15 123.3(3) . . ? C13 C14 C15 121.5(3) . . ? C16 C15 C14 118.8(3) . . ? C17 C16 C15 122.1(3) . . ? C16 C17 C18 118.7(3) . . ? O3 C18 C13 114.4(3) . . ? O3 C18 C17 124.4(3) . . ? C13 C18 C17 121.2(3) . . ? O3 C19 C21 105.5(3) . . ? O3 C19 C20 110.3(3) . . ? C21 C19 C20 111.0(3) . . ? O4 C22 C24 110.8(3) . . ? O4 C22 C23 105.1(3) . . ? C24 C22 C23 111.9(3) . . ? C30 C25 C26 116.5(3) . . ? C30 C25 Sn1 122.4(2) . . ? C26 C25 Sn1 120.8(2) . . ? O5 C26 C27 122.8(3) . . ? O5 C26 C25 115.0(2) . . ? C27 C26 C25 122.3(3) . . ? C28 C27 C26 118.5(3) . . ? C29 C28 C27 121.9(3) . . ? C28 C29 C30 118.4(3) . . ? O6 C30 C29 121.4(3) . . ? O6 C30 C25 116.2(2) . . ? C29 C30 C25 122.4(3) . . ? O5 C31 C33 110.7(3) . . ? O5 C31 C32 105.8(3) . . ? C33 C31 C32 111.6(3) . . ? O6 C34 C36 112.1(3) . . ? O6 C34 C35 106.1(3) . . ? C36 C34 C35 112.3(3) . . ? C38 C37 C42 116.7(3) . . ? C38 C37 Sn2 121.4(2) . . ? C42 C37 Sn2 121.4(2) . . ? C37 C38 O7 116.3(3) . . ? C37 C38 C39 121.9(3) . . ? O7 C38 C39 121.7(3) . . ? C40 C39 C38 118.7(3) . . ? C39 C40 C41 121.7(3) . . ? C40 C41 C42 118.7(3) . . ? O8 C42 C41 123.1(3) . . ? O8 C42 C37 114.8(3) . . ? C41 C42 C37 122.1(3) . . ? O8 C43 C44 110.5(3) . . ? O8 C43 C45 104.7(3) . . ? C44 C43 C45 112.2(3) . . ? O7 C46 C47 106.2(3) . . ? O7 C46 C48 110.5(3) . . ? C47 C46 C48 109.4(3) . . ? C50 C49 C54 116.7(3) . . ? C50 C49 Sn2 116.5(2) . . ? C54 C49 Sn2 126.7(2) . . ? O9 C50 C49 114.6(3) . . ? O9 C50 C51 122.4(3) . . ? C49 C50 C51 122.9(3) . . ? C52 C51 C50 118.0(3) . . ? C53 C52 C51 121.3(3) . . ? C52 C53 C54 120.0(3) . . ? O10 C54 C53 123.0(3) . . ? O10 C54 C49 116.1(3) . . ? C53 C54 C49 121.0(3) . . ? O9 C55 C56 104.9(3) . . ? O9 C55 C57 111.2(3) . . ? C56 C55 C57 112.4(3) . . ? O10 C58 C60 105.5(3) . . ? O10 C58 C59 112.0(3) . . ? C60 C58 C59 112.3(3) . . ? C62 C61 C66 117.7(3) . . ? C62 C61 Sn2 125.8(2) . . ? C66 C61 Sn2 116.4(2) . . ? O11 C62 C61 115.0(3) . . ? O11 C62 C63 123.6(3) . . ? C61 C62 C63 121.4(3) . . ? C64 C63 C62 118.8(3) . . ? C63 C64 C65 121.8(3) . . ? C64 C65 C66 118.3(3) . . ? O12 C66 C65 123.8(3) . . ? O12 C66 C61 114.2(3) . . ? C65 C66 C61 122.0(3) . . ? O12 C67 C68 105.7(3) . . ? O12 C67 C69 110.4(3) . . ? C68 C67 C69 111.1(3) . . ? O11 C70 C72 110.6(3) . . ? O11 C70 C71 105.4(3) . . ? C72 C70 C71 112.5(4) . . ? C74 C73 C78 120.0 . . ? C75 C74 C73 120.0 . . ? C76 C75 C74 120.0 . . ? C77 C76 C75 120.0 . . ? C76 C77 C78 120.0 . . ? C77 C78 C73 120.0 . . ? C80 C79 C84 120.0 . . ? C79 C80 C81 120.0 . . ? C82 C81 C80 120.0 . . ? C81 C82 C83 120.0 . . ? C84 C83 C82 120.0 . . ? C83 C84 C79 120.0 . . ? C86 C85 C90 120.0 . . ? C85 C86 C87 120.0 . . ? C88 C87 C86 120.0 . . ? C87 C88 C89 120.0 . . ? C90 C89 C88 120.0 . . ? C89 C90 C85 120.0 . . ? _diffrn_measured_fraction_theta_max 0.982 _diffrn_reflns_theta_full 29.03 _diffrn_measured_fraction_theta_full 0.982 _refine_diff_density_max 0.736 _refine_diff_density_min -0.631 _refine_diff_density_rms 0.113 #------------------------------------------------------------------------------# # END OF DATA BLOCK # #------------------------------------------------------------------------------#