# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'K Molloy' _publ_contact_author_email CHSKCM@BATH.AC.UK _publ_section_title ; The reaction of tin(IV) iodide with phosphines: formation of new halotin anions ; loop_ _publ_author_name 'K Molloy' 'Leonardo Apostolico' 'Christopher Blackman' 'Claire Carmalt' 'Gabriele Kociok-Kohn' ; I.Parkin ; #===end data_k02kcm2 _database_code_depnum_ccdc_archive 'CCDC 741171' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C18 H33 I P, I5 Sn' _chemical_formula_sum 'C18 H33 I6 P Sn' _chemical_formula_weight 1160.50 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 12.1215(1) _cell_length_b 17.3964(1) _cell_length_c 21.9965(2) _cell_angle_alpha 90.00 _cell_angle_beta 103.533(1) _cell_angle_gamma 90.00 _cell_volume 4509.63(6) _cell_formula_units_Z 6 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 74653 _cell_measurement_theta_min 2.910 _cell_measurement_theta_max 30.034 _exptl_crystal_description 'irregular shape' _exptl_crystal_colour colourless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.564 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3144 _exptl_absorpt_coefficient_mu 7.069 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.2547 _exptl_absorpt_correction_T_max 0.5655 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements Sortav (Blessing 1995) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_measurement_method '384 1.5 degree images with \f and\w scans' _diffrn_standards_number 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 92742 _diffrn_reflns_av_R_equivalents 0.0919 _diffrn_reflns_av_sigmaI/netI 0.0879 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 3.54 _diffrn_reflns_theta_max 30.03 _reflns_number_total 26218 _reflns_number_gt 18523 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinski & Minor, 1997)' _computing_data_reduction ; DENZO-SCALEPACK Z. Otwinowski and W. Minor, " Processing of X-ray Diffraction Data Collected in Oscillation Mode ", Methods in Enzymology, Volume 276: Macromolecular Crystallography, part A, p.307-326, 1997,C.W. Carter, Jr. & R. M. Sweet, Eds., Academic Press. ; _computing_structure_solution ; SIR97- Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C. , Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R. (1999) J. Appl. Cryst. 32, 115-119 ; _computing_structure_refinement ; SHELXL97 -Program for Crystal Structure Analysis (Release 97-2). Sheldrick, G.M., Instit\"ut f\"ur Anorganische Chemie der Universit\"at, Tammanstrasse 4, D-3400 G\"ottingen, Germany, 1998 ; _computing_molecular_graphics 'ORTEP3 for Windows - Farrugia, L. J. J. Appl. Crystallogr. 1997, 30, 565' _computing_publication_material ; 'WinGX publication routines, Farrugia, L. J., J. Appl. Crystallogr., 1999, 32, 837-838 ; _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^)+(0.0498P)^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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.01(2) _refine_ls_number_reflns 26218 _refine_ls_number_parameters 724 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0845 _refine_ls_R_factor_gt 0.0470 _refine_ls_wR_factor_ref 0.1047 _refine_ls_wR_factor_gt 0.0935 _refine_ls_goodness_of_fit_ref 0.967 _refine_ls_restrained_S_all 0.967 _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 0.56730(4) 0.00738(3) 0.86473(3) 0.02861(12) Uani 1 1 d . . . I1 I 0.62684(5) -0.14163(3) 0.84912(3) 0.03620(13) Uani 1 1 d . . . I2 I 0.44272(5) 0.04449(4) 0.94981(3) 0.03997(14) Uani 1 1 d . . . I3 I 0.35684(5) -0.02193(3) 0.77576(3) 0.04089(15) Uani 1 1 d . . . I4 I 0.62332(7) 0.11624(5) 0.78796(4) 0.0784(3) Uani 1 1 d . . . I5 I 0.76987(4) 0.03359(3) 0.95650(3) 0.03970(14) Uani 1 1 d . . . Sn2 Sn 0.74845(4) 0.50807(3) 0.81069(2) 0.02578(12) Uani 1 1 d . . . I6 I 0.69332(5) 0.35648(3) 0.81890(3) 0.03413(13) Uani 1 1 d . . . I7 I 0.68746(6) 0.61275(5) 0.88928(4) 0.0724(3) Uani 1 1 d . . . I8 I 0.54533(5) 0.53516(3) 0.72005(3) 0.04022(14) Uani 1 1 d . . . I9 I 0.87196(5) 0.55190(4) 0.72593(3) 0.03711(13) Uani 1 1 d . . . I10 I 0.95549(5) 0.48115(4) 0.90064(3) 0.04392(16) Uani 1 1 d . . . Sn3 Sn 0.09035(4) 0.52889(3) 0.47315(2) 0.02646(12) Uani 1 1 d . . . I11 I 0.03244(5) 0.37842(3) 0.48411(3) 0.04076(15) Uani 1 1 d . . . I12 I -0.00327(6) 0.64707(4) 0.52681(3) 0.05281(19) Uani 1 1 d . . . I13 I -0.08210(5) 0.54417(4) 0.36274(3) 0.03989(14) Uani 1 1 d . . . I14 I 0.25168(5) 0.55776(4) 0.40547(3) 0.03860(14) Uani 1 1 d . . . I15 I 0.26577(5) 0.51418(3) 0.58379(3) 0.04483(16) Uani 1 1 d . . . P1 P 0.20349(16) 0.29905(11) 0.73911(9) 0.0209(4) Uani 1 1 d . . . I16 I 0.27175(5) 0.18269(3) 0.79278(3) 0.03644(13) Uani 1 1 d . . . C1 C 0.2198(6) 0.3810(4) 0.7928(3) 0.0215(15) Uani 1 1 d . . . H1 H 0.1516 0.3815 0.8111 0.026 Uiso 1 1 calc R . . C2 C 0.3257(7) 0.3764(5) 0.8485(4) 0.0324(19) Uani 1 1 d . . . H2A H 0.3238 0.3279 0.8718 0.039 Uiso 1 1 calc R . . H2B H 0.3955 0.3765 0.8324 0.039 Uiso 1 1 calc R . . C3 C 0.3273(8) 0.4442(5) 0.8917(4) 0.038(2) Uani 1 1 d . . . H3A H 0.2615 0.4407 0.9111 0.045 Uiso 1 1 calc R . . H3B H 0.3973 0.4424 0.9256 0.045 Uiso 1 1 calc R . . C4 C 0.3226(8) 0.5196(6) 0.8571(4) 0.045(2) Uani 1 1 d . . . H4A H 0.3923 0.5255 0.8414 0.054 Uiso 1 1 calc R . . H4B H 0.3198 0.5625 0.8862 0.054 Uiso 1 1 calc R . . C5 C 0.2196(7) 0.5238(5) 0.8025(4) 0.039(2) Uani 1 1 d . . . H5A H 0.2204 0.5731 0.7801 0.046 Uiso 1 1 calc R . . H5B H 0.1496 0.5220 0.8183 0.046 Uiso 1 1 calc R . . C6 C 0.2195(7) 0.4572(5) 0.7574(4) 0.0312(19) Uani 1 1 d . . . H6A H 0.2874 0.4601 0.7398 0.037 Uiso 1 1 calc R . . H6B H 0.1512 0.4601 0.7225 0.037 Uiso 1 1 calc R . . C7 C 0.0539(6) 0.2798(5) 0.7032(4) 0.0251(17) Uani 1 1 d . . . H7 H 0.0514 0.2309 0.6789 0.030 Uiso 1 1 calc R . . C8 C -0.0014(6) 0.3422(5) 0.6564(4) 0.0303(18) Uani 1 1 d . . . H8A H -0.0095 0.3903 0.6790 0.036 Uiso 1 1 calc R . . H8B H 0.0468 0.3529 0.6268 0.036 Uiso 1 1 calc R . . C9 C -0.1184(7) 0.3138(7) 0.6207(4) 0.047(3) Uani 1 1 d . . . H9A H -0.1568 0.3544 0.5919 0.056 Uiso 1 1 calc R . . H9B H -0.1097 0.2680 0.5956 0.056 Uiso 1 1 calc R . . C10 C -0.1903(7) 0.2934(7) 0.6673(5) 0.049(3) Uani 1 1 d . . . H10A H -0.2066 0.3411 0.6881 0.059 Uiso 1 1 calc R . . H10B H -0.2637 0.2721 0.6438 0.059 Uiso 1 1 calc R . . C11 C -0.1356(7) 0.2363(6) 0.7167(5) 0.045(3) Uani 1 1 d . . . H11A H -0.1271 0.1862 0.6970 0.053 Uiso 1 1 calc R . . H11B H -0.1843 0.2287 0.7466 0.053 Uiso 1 1 calc R . . C12 C -0.0181(6) 0.2662(5) 0.7517(4) 0.0326(19) Uani 1 1 d . . . H12A H 0.0194 0.2281 0.7832 0.039 Uiso 1 1 calc R . . H12B H -0.0265 0.3149 0.7736 0.039 Uiso 1 1 calc R . . C13 C 0.2791(6) 0.3098(4) 0.6777(3) 0.0207(15) Uani 1 1 d . . . H13 H 0.2530 0.3594 0.6561 0.025 Uiso 1 1 calc R . . C14 C 0.2478(6) 0.2465(4) 0.6284(4) 0.0256(17) Uani 1 1 d . . . H14A H 0.2653 0.1956 0.6484 0.031 Uiso 1 1 calc R . . H14B H 0.1654 0.2485 0.6091 0.031 Uiso 1 1 calc R . . C15 C 0.3144(7) 0.2571(5) 0.5779(4) 0.0326(19) Uani 1 1 d . . . H15A H 0.2957 0.2147 0.5473 0.039 Uiso 1 1 calc R . . H15B H 0.2911 0.3060 0.5555 0.039 Uiso 1 1 calc R . . C16 C 0.4408(7) 0.2584(5) 0.6050(4) 0.034(2) Uani 1 1 d . . . H16A H 0.4810 0.2653 0.5711 0.041 Uiso 1 1 calc R . . H16B H 0.4653 0.2089 0.6261 0.041 Uiso 1 1 calc R . . C17 C 0.4704(6) 0.3237(5) 0.6516(4) 0.035(2) Uani 1 1 d . . . H17A H 0.5532 0.3235 0.6699 0.041 Uiso 1 1 calc R . . H17B H 0.4506 0.3732 0.6296 0.041 Uiso 1 1 calc R . . C18 C 0.4086(6) 0.3171(5) 0.7034(4) 0.0296(18) Uani 1 1 d . . . H18A H 0.4250 0.3630 0.7305 0.036 Uiso 1 1 calc R . . H18B H 0.4368 0.2714 0.7292 0.036 Uiso 1 1 calc R . . P2 P 0.10440(15) 0.79500(11) 0.92152(9) 0.0200(4) Uani 1 1 d . . . I17 I 0.02299(5) 0.69266(3) 0.85313(3) 0.03390(13) Uani 1 1 d . . . C19 C 0.2528(6) 0.7680(5) 0.9535(3) 0.0255(17) Uani 1 1 d . . . H19 H 0.2517 0.7158 0.9725 0.031 Uiso 1 1 calc R . . C20 C 0.3119(7) 0.8221(5) 1.0068(4) 0.0341(19) Uani 1 1 d . . . H20A H 0.3229 0.8736 0.9900 0.041 Uiso 1 1 calc R . . H20B H 0.2653 0.8277 1.0380 0.041 Uiso 1 1 calc R . . C21 C 0.4258(7) 0.7862(7) 1.0369(4) 0.047(3) Uani 1 1 d . . . H21A H 0.4663 0.8198 1.0713 0.056 Uiso 1 1 calc R . . H21B H 0.4131 0.7360 1.0552 0.056 Uiso 1 1 calc R . . C22 C 0.4979(8) 0.7749(6) 0.9912(5) 0.046(2) Uani 1 1 d . . . H22A H 0.5697 0.7496 1.0125 0.055 Uiso 1 1 calc R . . H22B H 0.5170 0.8257 0.9761 0.055 Uiso 1 1 calc R . . C23 C 0.4385(7) 0.7259(5) 0.9351(4) 0.0335(19) Uani 1 1 d . . . H23A H 0.4867 0.7229 0.9045 0.040 Uiso 1 1 calc R . . H23B H 0.4274 0.6731 0.9493 0.040 Uiso 1 1 calc R . . C24 C 0.3237(6) 0.7610(5) 0.9039(4) 0.0284(18) Uani 1 1 d . . . H24A H 0.2839 0.7278 0.8690 0.034 Uiso 1 1 calc R . . H24B H 0.3345 0.8123 0.8868 0.034 Uiso 1 1 calc R . . C25 C 0.0947(7) 0.8856(5) 0.8783(4) 0.0291(18) Uani 1 1 d . . . H25 H 0.1644 0.8890 0.8614 0.035 Uiso 1 1 calc R . . C26 C -0.0071(7) 0.8917(5) 0.8220(4) 0.036(2) Uani 1 1 d . . . H26A H -0.0063 0.8480 0.7933 0.043 Uiso 1 1 calc R . . H26B H -0.0784 0.8892 0.8366 0.043 Uiso 1 1 calc R . . C27 C -0.0029(8) 0.9664(5) 0.7876(4) 0.041(2) Uani 1 1 d . . . H27A H 0.0648 0.9666 0.7697 0.050 Uiso 1 1 calc R . . H27B H -0.0710 0.9704 0.7526 0.050 Uiso 1 1 calc R . . C28 C 0.0017(7) 1.0350(5) 0.8302(4) 0.042(2) Uani 1 1 d . . . H28A H -0.0703 1.0384 0.8439 0.051 Uiso 1 1 calc R . . H28B H 0.0094 1.0824 0.8066 0.051 Uiso 1 1 calc R . . C29 C 0.1004(8) 1.0301(5) 0.8875(5) 0.046(2) Uani 1 1 d . . . H29A H 0.0960 1.0735 0.9160 0.055 Uiso 1 1 calc R . . H29B H 0.1729 1.0345 0.8744 0.055 Uiso 1 1 calc R . . C30 C 0.0981(7) 0.9544(5) 0.9221(4) 0.0298(18) Uani 1 1 d . . . H30A H 0.0305 0.9531 0.9400 0.036 Uiso 1 1 calc R . . H30B H 0.1663 0.9508 0.9569 0.036 Uiso 1 1 calc R . . C31 C 0.0314(6) 0.7972(4) 0.9841(3) 0.0214(15) Uani 1 1 d . . . H31 H 0.0609 0.8427 1.0107 0.026 Uiso 1 1 calc R . . C32 C -0.0977(6) 0.8085(5) 0.9607(4) 0.0261(17) Uani 1 1 d . . . H32A H -0.1125 0.8571 0.9367 0.031 Uiso 1 1 calc R . . H32B H -0.1295 0.7659 0.9321 0.031 Uiso 1 1 calc R . . C33 C -0.1569(6) 0.8110(5) 1.0145(4) 0.0309(19) Uani 1 1 d . . . H33A H -0.2400 0.8142 0.9975 0.037 Uiso 1 1 calc R . . H33B H -0.1326 0.8575 1.0400 0.037 Uiso 1 1 calc R . . C34 C -0.1297(8) 0.7400(6) 1.0559(4) 0.043(2) Uani 1 1 d . . . H34A H -0.1673 0.7442 1.0912 0.052 Uiso 1 1 calc R . . H34B H -0.1595 0.6936 1.0315 0.052 Uiso 1 1 calc R . . C35 C -0.0036(7) 0.7322(5) 1.0809(4) 0.0322(19) Uani 1 1 d . . . H35A H 0.0125 0.6861 1.1080 0.039 Uiso 1 1 calc R . . H35B H 0.0255 0.7777 1.1067 0.039 Uiso 1 1 calc R . . C36 C 0.0579(7) 0.7250(5) 1.0268(4) 0.0307(18) Uani 1 1 d . . . H36A H 0.0319 0.6781 1.0021 0.037 Uiso 1 1 calc R . . H36B H 0.1408 0.7207 1.0440 0.037 Uiso 1 1 calc R . . P3 P 0.42457(16) 0.81563(11) 0.58720(9) 0.0236(4) Uani 1 1 d . . . I18 I 0.35436(4) 0.71398(3) 0.51548(2) 0.02912(12) Uani 1 1 d . . . C37 C 0.3769(7) 0.9050(4) 0.5452(4) 0.0297(18) Uani 1 1 d . . . H37 H 0.2923 0.9018 0.5331 0.036 Uiso 1 1 calc R . . C38 C 0.4043(10) 0.9759(5) 0.5882(5) 0.053(3) Uani 1 1 d . . . H38A H 0.3756 0.9681 0.6263 0.064 Uiso 1 1 calc R . . H38B H 0.4874 0.9837 0.6009 0.064 Uiso 1 1 calc R . . C39 C 0.3475(12) 1.0464(6) 0.5524(5) 0.067(3) Uani 1 1 d . . . H39A H 0.2641 1.0400 0.5434 0.080 Uiso 1 1 calc R . . H39B H 0.3675 1.0926 0.5790 0.080 Uiso 1 1 calc R . . C40 C 0.3826(11) 1.0578(6) 0.4933(6) 0.070(4) Uani 1 1 d . . . H40A H 0.4647 1.0698 0.5027 0.083 Uiso 1 1 calc R . . H40B H 0.3412 1.1024 0.4709 0.083 Uiso 1 1 calc R . . C41 C 0.3596(11) 0.9875(6) 0.4514(5) 0.064(3) Uani 1 1 d . . . H41A H 0.3907 0.9960 0.4141 0.077 Uiso 1 1 calc R . . H41B H 0.2767 0.9798 0.4369 0.077 Uiso 1 1 calc R . . C42 C 0.4134(9) 0.9157(6) 0.4857(5) 0.050(3) Uani 1 1 d . . . H42A H 0.3910 0.8701 0.4587 0.060 Uiso 1 1 calc R . . H42B H 0.4971 0.9203 0.4949 0.060 Uiso 1 1 calc R . . C43 C 0.3588(6) 0.8039(4) 0.6525(4) 0.0252(17) Uani 1 1 d . . . H43 H 0.3885 0.8461 0.6829 0.030 Uiso 1 1 calc R . . C44 C 0.2294(6) 0.8139(5) 0.6327(4) 0.0320(19) Uani 1 1 d . . . H44A H 0.2119 0.8668 0.6168 0.038 Uiso 1 1 calc R . . H44B H 0.1984 0.7778 0.5981 0.038 Uiso 1 1 calc R . . C45 C 0.1722(8) 0.7995(6) 0.6851(4) 0.039(2) Uani 1 1 d . . . H45A H 0.0890 0.8013 0.6685 0.047 Uiso 1 1 calc R . . H45B H 0.1931 0.8409 0.7165 0.047 Uiso 1 1 calc R . . C46 C 0.2041(8) 0.7226(6) 0.7168(4) 0.043(2) Uani 1 1 d . . . H46A H 0.1782 0.6805 0.6865 0.052 Uiso 1 1 calc R . . H46B H 0.1665 0.7164 0.7518 0.052 Uiso 1 1 calc R . . C47 C 0.3320(8) 0.7182(6) 0.7411(4) 0.044(2) Uani 1 1 d . . . H47A H 0.3528 0.6681 0.7619 0.053 Uiso 1 1 calc R . . H47B H 0.3574 0.7593 0.7724 0.053 Uiso 1 1 calc R . . C48 C 0.3914(7) 0.7276(5) 0.6873(4) 0.0326(19) Uani 1 1 d . . . H48A H 0.3701 0.6843 0.6576 0.039 Uiso 1 1 calc R . . H48B H 0.4747 0.7259 0.7040 0.039 Uiso 1 1 calc R . . C49 C 0.5780(7) 0.8065(8) 0.6126(5) 0.063(4) Uani 1 1 d . . . H49 H 0.6018 0.8390 0.5804 0.075 Uiso 0.50 1 calc PR A 1 H49A H 0.5813 0.7544 0.6323 0.075 Uiso 0.50 1 calc PR A 2 C50 C 0.6277(7) 0.8526(6) 0.6709(4) 0.039(2) Uani 1 1 d . D . H50A H 0.6034 0.8288 0.7065 0.047 Uiso 0.50 1 calc PR B 1 H50B H 0.5950 0.9050 0.6653 0.047 Uiso 0.50 1 calc PR B 1 H50C H 0.5743 0.8525 0.6987 0.047 Uiso 0.50 1 calc PR B 2 H50D H 0.6388 0.9066 0.6592 0.047 Uiso 0.50 1 calc PR B 2 C53 C 0.7645(8) 0.7507(7) 0.6115(5) 0.052(3) Uani 1 1 d . . . H53A H 0.8022 0.7023 0.6041 0.063 Uiso 0.50 1 calc PR C 1 H53B H 0.7803 0.7908 0.5827 0.063 Uiso 0.50 1 calc PR C 1 H53C H 0.7453 0.7039 0.6324 0.063 Uiso 0.50 1 calc PR C 2 H53D H 0.8148 0.7360 0.5839 0.063 Uiso 0.50 1 calc PR C 2 C51 C 0.7577(16) 0.8596(12) 0.6881(11) 0.040(5) Uani 0.50 1 d P D 1 H51A H 0.7848 0.8780 0.7317 0.048 Uiso 0.50 1 calc PR D 1 H51B H 0.7836 0.8959 0.6597 0.048 Uiso 0.50 1 calc PR D 1 C52 C 0.8030(18) 0.7766(12) 0.6808(13) 0.045(7) Uani 0.50 1 d P D 1 H52A H 0.8869 0.7762 0.6940 0.054 Uiso 0.50 1 calc PR D 1 H52B H 0.7733 0.7405 0.7078 0.054 Uiso 0.50 1 calc PR D 1 C54 C 0.6273(12) 0.7383(11) 0.6033(9) 0.038(3) Uani 0.50 1 d P D 1 H54A H 0.5930 0.7188 0.5608 0.046 Uiso 0.50 1 calc PR D 1 H54B H 0.6138 0.6999 0.6340 0.046 Uiso 0.50 1 calc PR D 1 C51A C 0.7442(17) 0.8176(17) 0.7062(11) 0.051(6) Uani 0.50 1 d P D 2 H51C H 0.7801 0.8513 0.7415 0.061 Uiso 0.50 1 calc PR D 2 H51D H 0.7318 0.7665 0.7232 0.061 Uiso 0.50 1 calc PR D 2 C52A C 0.8234(19) 0.8097(18) 0.6601(13) 0.054(7) Uani 0.50 1 d P D 2 H52C H 0.8316 0.8596 0.6401 0.065 Uiso 0.50 1 calc PR D 2 H52D H 0.8995 0.7913 0.6822 0.065 Uiso 0.50 1 calc PR D 2 C54A C 0.6488(12) 0.7917(11) 0.5707(9) 0.038(3) Uani 0.50 1 d P D 2 H54C H 0.6677 0.8403 0.5520 0.046 Uiso 0.50 1 calc PR D 2 H54D H 0.6098 0.7572 0.5366 0.046 Uiso 0.50 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 Sn1 0.0228(3) 0.0269(3) 0.0336(3) 0.0031(2) 0.0015(2) 0.0007(2) I1 0.0341(3) 0.0334(3) 0.0360(3) -0.0036(2) -0.0021(2) 0.0097(2) I2 0.0300(3) 0.0482(3) 0.0399(3) -0.0110(3) 0.0044(2) -0.0010(3) I3 0.0338(3) 0.0375(3) 0.0416(3) -0.0104(3) -0.0110(2) 0.0094(2) I4 0.0505(4) 0.0868(6) 0.0943(6) 0.0612(5) 0.0098(4) -0.0037(4) I5 0.0259(3) 0.0365(3) 0.0506(4) -0.0017(3) -0.0034(2) -0.0058(2) Sn2 0.0209(2) 0.0268(3) 0.0279(3) -0.0022(2) 0.0022(2) 0.0005(2) I6 0.0359(3) 0.0311(3) 0.0315(3) 0.0024(2) 0.0001(2) -0.0063(2) I7 0.0453(4) 0.0869(6) 0.0833(6) -0.0574(5) 0.0118(4) 0.0009(4) I8 0.0277(3) 0.0379(3) 0.0471(3) 0.0028(3) -0.0073(2) 0.0049(2) I9 0.0364(3) 0.0435(3) 0.0314(3) 0.0016(3) 0.0080(2) -0.0045(3) I10 0.0309(3) 0.0465(3) 0.0448(3) 0.0198(3) -0.0103(2) -0.0088(3) Sn3 0.0270(3) 0.0238(3) 0.0246(3) -0.0007(2) -0.0019(2) 0.0022(2) I11 0.0447(3) 0.0300(3) 0.0389(3) 0.0027(2) -0.0078(3) -0.0089(2) I12 0.0454(4) 0.0537(4) 0.0530(4) -0.0267(3) -0.0012(3) 0.0120(3) I13 0.0380(3) 0.0427(3) 0.0303(3) -0.0027(3) -0.0094(2) 0.0108(3) I14 0.0372(3) 0.0404(3) 0.0390(3) -0.0036(3) 0.0105(2) 0.0015(3) I15 0.0485(3) 0.0348(3) 0.0372(3) 0.0109(2) -0.0182(3) -0.0099(3) P1 0.0184(9) 0.0188(9) 0.0250(10) -0.0002(8) 0.0041(8) 0.0004(7) I16 0.0378(3) 0.0268(3) 0.0453(3) 0.0102(3) 0.0110(3) 0.0073(2) C1 0.020(3) 0.024(4) 0.021(4) 0.000(3) 0.007(3) 0.001(3) C2 0.029(4) 0.038(5) 0.024(4) -0.004(4) -0.007(3) 0.000(4) C3 0.041(5) 0.046(5) 0.020(4) -0.008(4) -0.004(4) -0.008(4) C4 0.040(5) 0.049(6) 0.044(5) -0.017(5) 0.008(4) -0.021(4) C5 0.040(5) 0.023(4) 0.052(6) -0.012(4) 0.010(4) 0.000(4) C6 0.024(4) 0.028(4) 0.040(5) -0.003(4) 0.004(4) -0.001(3) C7 0.015(3) 0.032(4) 0.028(4) -0.006(3) 0.003(3) -0.008(3) C8 0.017(4) 0.036(5) 0.035(5) -0.003(4) 0.000(3) 0.001(3) C9 0.024(4) 0.077(7) 0.034(5) -0.009(5) -0.004(4) -0.001(5) C10 0.022(4) 0.079(8) 0.048(6) -0.020(6) 0.010(4) -0.005(5) C11 0.018(4) 0.069(7) 0.053(6) -0.022(5) 0.020(4) -0.012(4) C12 0.022(4) 0.040(5) 0.037(5) -0.004(4) 0.009(4) -0.002(4) C13 0.021(4) 0.019(3) 0.022(4) 0.002(3) 0.005(3) 0.001(3) C14 0.020(4) 0.025(4) 0.031(4) -0.008(3) 0.005(3) -0.004(3) C15 0.036(5) 0.034(5) 0.025(4) -0.003(4) 0.001(4) -0.003(4) C16 0.031(5) 0.030(4) 0.049(6) -0.011(4) 0.027(4) -0.003(4) C17 0.021(4) 0.044(5) 0.041(5) -0.006(4) 0.011(4) -0.012(4) C18 0.015(4) 0.033(4) 0.039(5) -0.004(4) 0.003(3) -0.002(3) P2 0.0184(9) 0.0204(9) 0.0205(10) -0.0023(7) 0.0030(7) -0.0004(7) I17 0.0334(3) 0.0299(3) 0.0389(3) -0.0127(2) 0.0096(2) -0.0078(2) C19 0.023(4) 0.028(4) 0.024(4) 0.003(3) 0.004(3) -0.002(3) C20 0.025(4) 0.041(5) 0.032(5) -0.003(4) -0.001(3) -0.001(4) C21 0.026(5) 0.076(8) 0.034(5) 0.002(5) -0.002(4) 0.005(5) C22 0.025(4) 0.044(6) 0.067(7) 0.002(5) 0.007(4) -0.003(4) C23 0.026(4) 0.031(4) 0.046(5) 0.002(4) 0.012(4) 0.004(3) C24 0.022(4) 0.035(4) 0.028(4) -0.001(3) 0.007(3) -0.002(3) C25 0.027(4) 0.031(4) 0.026(4) 0.002(3) 0.000(3) 0.000(3) C26 0.034(5) 0.034(5) 0.033(5) 0.011(4) -0.005(4) -0.007(4) C27 0.039(5) 0.041(5) 0.039(5) 0.021(4) -0.003(4) 0.001(4) C28 0.039(5) 0.030(4) 0.055(6) 0.020(4) 0.004(4) 0.002(4) C29 0.041(5) 0.025(4) 0.060(6) 0.006(4) -0.008(4) -0.008(4) C30 0.034(4) 0.024(4) 0.025(4) -0.003(3) -0.006(3) -0.001(3) C31 0.019(4) 0.023(4) 0.021(4) 0.003(3) 0.001(3) -0.001(3) C32 0.011(3) 0.034(4) 0.032(4) 0.000(3) 0.004(3) 0.002(3) C33 0.020(4) 0.042(5) 0.030(4) 0.004(4) 0.006(3) 0.000(3) C34 0.049(6) 0.053(6) 0.030(5) 0.006(4) 0.017(4) -0.009(5) C35 0.033(4) 0.037(5) 0.028(4) 0.005(4) 0.009(4) 0.002(4) C36 0.027(4) 0.029(4) 0.034(5) 0.006(4) 0.002(3) -0.002(3) P3 0.0211(9) 0.0233(10) 0.0252(10) -0.0040(8) 0.0033(8) -0.0006(8) I18 0.0289(3) 0.0290(3) 0.0286(3) -0.0054(2) 0.0051(2) -0.0045(2) C37 0.027(4) 0.024(4) 0.040(5) 0.007(3) 0.011(4) -0.002(3) C38 0.078(7) 0.017(4) 0.057(6) -0.004(4) -0.003(5) 0.000(5) C39 0.110(10) 0.028(5) 0.063(7) 0.003(5) 0.021(7) 0.012(6) C40 0.080(8) 0.028(5) 0.096(10) 0.015(6) 0.009(7) -0.005(5) C41 0.086(8) 0.039(6) 0.064(7) 0.030(5) 0.007(6) 0.004(6) C42 0.068(7) 0.037(5) 0.050(6) 0.015(5) 0.021(5) 0.008(5) C43 0.026(4) 0.024(4) 0.023(4) 0.005(3) 0.001(3) -0.001(3) C44 0.027(4) 0.036(5) 0.031(5) 0.010(4) 0.001(3) -0.001(4) C45 0.034(5) 0.047(5) 0.040(5) 0.005(4) 0.015(4) 0.000(4) C46 0.040(5) 0.054(6) 0.040(5) 0.004(5) 0.019(4) 0.001(4) C47 0.054(6) 0.039(5) 0.034(5) 0.010(4) -0.001(4) -0.011(4) C48 0.037(5) 0.027(4) 0.031(4) 0.001(4) 0.001(4) 0.006(4) C49 0.023(5) 0.100(9) 0.061(7) -0.051(7) 0.002(5) 0.001(5) C50 0.022(4) 0.056(6) 0.037(5) -0.012(4) 0.002(4) -0.004(4) C53 0.026(5) 0.069(7) 0.059(7) -0.020(6) 0.005(5) 0.009(5) C51 0.023(9) 0.032(11) 0.059(14) 0.005(10) -0.004(9) -0.011(9) C52 0.016(10) 0.031(12) 0.08(2) 0.006(11) -0.003(10) -0.008(9) C54 0.012(5) 0.051(8) 0.047(8) -0.015(6) -0.003(5) 0.002(5) C51A 0.030(11) 0.067(17) 0.050(14) -0.018(13) -0.001(10) -0.004(12) C52A 0.023(11) 0.08(2) 0.058(16) -0.022(15) 0.006(10) -0.008(13) C54A 0.012(5) 0.051(8) 0.047(8) -0.015(6) -0.003(5) 0.002(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 I4 2.7269(9) . ? Sn1 I1 2.7339(8) . ? Sn1 I2 2.7426(8) . ? Sn1 I5 2.8271(7) . ? Sn1 I3 2.8743(7) . ? Sn2 I7 2.7293(9) . ? Sn2 I6 2.7368(8) . ? Sn2 I9 2.7577(8) . ? Sn2 I8 2.8217(7) . ? Sn2 I10 2.8475(7) . ? Sn3 I11 2.7353(8) . ? Sn3 I12 2.7450(8) . ? Sn3 I14 2.7669(8) . ? Sn3 I13 2.8219(7) . ? Sn3 I15 2.8438(7) . ? P1 C13 1.810(8) . ? P1 C7 1.832(7) . ? P1 C1 1.833(7) . ? P1 I16 2.3915(19) . ? C1 C6 1.536(11) . ? C1 C2 1.555(10) . ? C1 H1 1.0000 . ? C2 C3 1.513(12) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.512(13) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 C5 1.518(12) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C6 1.524(11) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 C8 1.537(11) . ? C7 C12 1.547(11) . ? C7 H7 1.0000 . ? C8 C9 1.533(10) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C10 1.533(14) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 C11 1.507(15) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 C12 1.542(11) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 C14 1.530(10) . ? C13 C18 1.544(10) . ? C13 H13 1.0000 . ? C14 C15 1.529(12) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 C16 1.508(11) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 C17 1.516(12) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 C18 1.506(12) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? P2 C31 1.803(8) . ? P2 C25 1.831(8) . ? P2 C19 1.832(7) . ? P2 I17 2.3899(19) . ? C19 C20 1.543(11) . ? C19 C24 1.544(11) . ? C19 H19 1.0000 . ? C20 C21 1.518(12) . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C21 C22 1.492(14) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 C23 1.533(13) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 C24 1.528(11) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 C30 1.531(11) . ? C25 C26 1.534(10) . ? C25 H25 1.0000 . ? C26 C27 1.511(12) . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C27 C28 1.509(14) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C28 C29 1.524(12) . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C29 C30 1.524(12) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? C31 C32 1.542(9) . ? C31 C36 1.556(10) . ? C31 H31 1.0000 . ? C32 C33 1.523(11) . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C33 C34 1.524(12) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C34 C35 1.505(12) . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? C35 C36 1.552(12) . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? C36 H36A 0.9900 . ? C36 H36B 0.9900 . ? P3 C43 1.810(8) . ? P3 C49 1.819(9) . ? P3 C37 1.832(8) . ? P3 I18 2.390(2) . ? C37 C42 1.487(13) . ? C37 C38 1.542(12) . ? C37 H37 1.0000 . ? C38 C39 1.529(13) . ? C38 H38A 0.9900 . ? C38 H38B 0.9900 . ? C39 C40 1.473(17) . ? C39 H39A 0.9900 . ? C39 H39B 0.9900 . ? C40 C41 1.519(16) . ? C40 H40A 0.9900 . ? C40 H40B 0.9900 . ? C41 C42 1.525(13) . ? C41 H41A 0.9900 . ? C41 H41B 0.9900 . ? C42 H42A 0.9900 . ? C42 H42B 0.9900 . ? C43 C44 1.536(10) . ? C43 C48 1.537(10) . ? C43 H43 1.0000 . ? C44 C45 1.499(12) . ? C44 H44A 0.9900 . ? C44 H44B 0.9900 . ? C45 C46 1.516(13) . ? C45 H45A 0.9900 . ? C45 H45B 0.9900 . ? C46 C47 1.519(12) . ? C46 H46A 0.9900 . ? C46 H46B 0.9900 . ? C47 C48 1.533(13) . ? C47 H47A 0.9900 . ? C47 H47B 0.9900 . ? C48 H48A 0.9900 . ? C48 H48B 0.9900 . ? C49 C54 1.36(2) . ? C49 C54A 1.42(2) . ? C49 C50 1.512(12) . ? C49 H49 1.0000 . ? C49 H49A 1.0000 . ? C50 C51 1.54(2) . ? C50 C51A 1.57(2) . ? C50 H50A 0.9900 . ? C50 H50B 0.9900 . ? C50 H50C 0.9900 . ? C50 H50D 0.9900 . ? C53 C52A 1.53(3) . ? C53 C52 1.55(3) . ? C53 C54A 1.640(18) . ? C53 C54 1.645(18) . ? C53 H53A 0.9900 . ? C53 H53B 0.9900 . ? C53 H53C 0.9900 . ? C53 H53D 0.9900 . ? C51 C52 1.57(3) . ? C51 H51A 0.9900 . ? C51 H51B 0.9900 . ? C52 H52A 0.9900 . ? C52 H52B 0.9900 . ? C54 H54A 0.9900 . ? C54 H54B 0.9900 . ? C51A C52A 1.56(3) . ? C51A H51C 0.9900 . ? C51A H51D 0.9900 . ? C52A H52C 0.9900 . ? C52A H52D 0.9900 . ? C54A H54C 0.9900 . ? C54A H54D 0.9900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag I4 Sn1 I1 118.00(3) . . ? I4 Sn1 I2 121.05(3) . . ? I1 Sn1 I2 120.84(3) . . ? I4 Sn1 I5 91.70(3) . . ? I1 Sn1 I5 91.83(2) . . ? I2 Sn1 I5 89.99(2) . . ? I4 Sn1 I3 90.66(3) . . ? I1 Sn1 I3 87.97(2) . . ? I2 Sn1 I3 87.92(2) . . ? I5 Sn1 I3 177.43(3) . . ? I7 Sn2 I6 119.64(3) . . ? I7 Sn2 I9 120.94(3) . . ? I6 Sn2 I9 119.38(3) . . ? I7 Sn2 I8 90.87(3) . . ? I6 Sn2 I8 91.23(2) . . ? I9 Sn2 I8 89.89(2) . . ? I7 Sn2 I10 89.71(3) . . ? I6 Sn2 I10 89.13(2) . . ? I9 Sn2 I10 89.18(2) . . ? I8 Sn2 I10 179.06(3) . . ? I11 Sn3 I12 122.58(3) . . ? I11 Sn3 I14 116.70(3) . . ? I12 Sn3 I14 120.72(3) . . ? I11 Sn3 I13 90.71(2) . . ? I12 Sn3 I13 90.12(2) . . ? I14 Sn3 I13 89.67(2) . . ? I11 Sn3 I15 89.68(2) . . ? I12 Sn3 I15 90.06(2) . . ? I14 Sn3 I15 89.75(2) . . ? I13 Sn3 I15 179.41(3) . . ? C13 P1 C7 108.6(3) . . ? C13 P1 C1 113.8(3) . . ? C7 P1 C1 111.5(4) . . ? C13 P1 I16 106.2(2) . . ? C7 P1 I16 104.5(3) . . ? C1 P1 I16 111.6(2) . . ? C6 C1 C2 110.3(6) . . ? C6 C1 P1 110.9(5) . . ? C2 C1 P1 114.3(5) . . ? C6 C1 H1 107.0 . . ? C2 C1 H1 107.0 . . ? P1 C1 H1 107.0 . . ? C3 C2 C1 110.0(7) . . ? C3 C2 H2A 109.7 . . ? C1 C2 H2A 109.7 . . ? C3 C2 H2B 109.7 . . ? C1 C2 H2B 109.7 . . ? H2A C2 H2B 108.2 . . ? C4 C3 C2 111.4(7) . . ? C4 C3 H3A 109.3 . . ? C2 C3 H3A 109.3 . . ? C4 C3 H3B 109.3 . . ? C2 C3 H3B 109.3 . . ? H3A C3 H3B 108.0 . . ? C3 C4 C5 111.6(7) . . ? C3 C4 H4A 109.3 . . ? C5 C4 H4A 109.3 . . ? C3 C4 H4B 109.3 . . ? C5 C4 H4B 109.3 . . ? H4A C4 H4B 108.0 . . ? C4 C5 C6 110.7(7) . . ? C4 C5 H5A 109.5 . . ? C6 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? C6 C5 H5B 109.5 . . ? H5A C5 H5B 108.1 . . ? C5 C6 C1 109.1(7) . . ? C5 C6 H6A 109.9 . . ? C1 C6 H6A 109.9 . . ? C5 C6 H6B 109.9 . . ? C1 C6 H6B 109.9 . . ? H6A C6 H6B 108.3 . . ? C8 C7 C12 109.9(7) . . ? C8 C7 P1 113.1(5) . . ? C12 C7 P1 113.0(5) . . ? C8 C7 H7 106.8 . . ? C12 C7 H7 106.8 . . ? P1 C7 H7 106.8 . . ? C9 C8 C7 108.7(7) . . ? C9 C8 H8A 109.9 . . ? C7 C8 H8A 109.9 . . ? C9 C8 H8B 109.9 . . ? C7 C8 H8B 109.9 . . ? H8A C8 H8B 108.3 . . ? C10 C9 C8 109.5(7) . . ? C10 C9 H9A 109.8 . . ? C8 C9 H9A 109.8 . . ? C10 C9 H9B 109.8 . . ? C8 C9 H9B 109.8 . . ? H9A C9 H9B 108.2 . . ? C11 C10 C9 114.3(8) . . ? C11 C10 H10A 108.7 . . ? C9 C10 H10A 108.7 . . ? C11 C10 H10B 108.7 . . ? C9 C10 H10B 108.7 . . ? H10A C10 H10B 107.6 . . ? C10 C11 C12 109.7(8) . . ? C10 C11 H11A 109.7 . . ? C12 C11 H11A 109.7 . . ? C10 C11 H11B 109.7 . . ? C12 C11 H11B 109.7 . . ? H11A C11 H11B 108.2 . . ? C11 C12 C7 108.1(7) . . ? C11 C12 H12A 110.1 . . ? C7 C12 H12A 110.1 . . ? C11 C12 H12B 110.1 . . ? C7 C12 H12B 110.1 . . ? H12A C12 H12B 108.4 . . ? C14 C13 C18 112.3(6) . . ? C14 C13 P1 111.7(5) . . ? C18 C13 P1 112.6(5) . . ? C14 C13 H13 106.6 . . ? C18 C13 H13 106.6 . . ? P1 C13 H13 106.6 . . ? C15 C14 C13 110.0(6) . . ? C15 C14 H14A 109.7 . . ? C13 C14 H14A 109.7 . . ? C15 C14 H14B 109.7 . . ? C13 C14 H14B 109.7 . . ? H14A C14 H14B 108.2 . . ? C16 C15 C14 112.1(7) . . ? C16 C15 H15A 109.2 . . ? C14 C15 H15A 109.2 . . ? C16 C15 H15B 109.2 . . ? C14 C15 H15B 109.2 . . ? H15A C15 H15B 107.9 . . ? C15 C16 C17 109.6(7) . . ? C15 C16 H16A 109.7 . . ? C17 C16 H16A 109.7 . . ? C15 C16 H16B 109.7 . . ? C17 C16 H16B 109.7 . . ? H16A C16 H16B 108.2 . . ? C18 C17 C16 111.9(7) . . ? C18 C17 H17A 109.2 . . ? C16 C17 H17A 109.2 . . ? C18 C17 H17B 109.2 . . ? C16 C17 H17B 109.2 . . ? H17A C17 H17B 107.9 . . ? C17 C18 C13 111.9(7) . . ? C17 C18 H18A 109.2 . . ? C13 C18 H18A 109.2 . . ? C17 C18 H18B 109.2 . . ? C13 C18 H18B 109.2 . . ? H18A C18 H18B 107.9 . . ? C31 P2 C25 113.3(4) . . ? C31 P2 C19 109.0(3) . . ? C25 P2 C19 111.0(4) . . ? C31 P2 I17 107.0(2) . . ? C25 P2 I17 110.3(3) . . ? C19 P2 I17 105.9(3) . . ? C20 C19 C24 110.4(6) . . ? C20 C19 P2 112.0(6) . . ? C24 C19 P2 114.0(5) . . ? C20 C19 H19 106.6 . . ? C24 C19 H19 106.6 . . ? P2 C19 H19 106.6 . . ? C21 C20 C19 107.1(8) . . ? C21 C20 H20A 110.3 . . ? C19 C20 H20A 110.3 . . ? C21 C20 H20B 110.3 . . ? C19 C20 H20B 110.3 . . ? H20A C20 H20B 108.5 . . ? C22 C21 C20 112.1(8) . . ? C22 C21 H21A 109.2 . . ? C20 C21 H21A 109.2 . . ? C22 C21 H21B 109.2 . . ? C20 C21 H21B 109.2 . . ? H21A C21 H21B 107.9 . . ? C21 C22 C23 112.2(8) . . ? C21 C22 H22A 109.2 . . ? C23 C22 H22A 109.2 . . ? C21 C22 H22B 109.2 . . ? C23 C22 H22B 109.2 . . ? H22A C22 H22B 107.9 . . ? C24 C23 C22 110.3(7) . . ? C24 C23 H23A 109.6 . . ? C22 C23 H23A 109.6 . . ? C24 C23 H23B 109.6 . . ? C22 C23 H23B 109.6 . . ? H23A C23 H23B 108.1 . . ? C23 C24 C19 108.2(7) . . ? C23 C24 H24A 110.1 . . ? C19 C24 H24A 110.1 . . ? C23 C24 H24B 110.1 . . ? C19 C24 H24B 110.1 . . ? H24A C24 H24B 108.4 . . ? C30 C25 C26 110.6(7) . . ? C30 C25 P2 110.9(5) . . ? C26 C25 P2 114.8(6) . . ? C30 C25 H25 106.7 . . ? C26 C25 H25 106.7 . . ? P2 C25 H25 106.7 . . ? C27 C26 C25 110.4(7) . . ? C27 C26 H26A 109.6 . . ? C25 C26 H26A 109.6 . . ? C27 C26 H26B 109.6 . . ? C25 C26 H26B 109.6 . . ? H26A C26 H26B 108.1 . . ? C28 C27 C26 111.7(8) . . ? C28 C27 H27A 109.3 . . ? C26 C27 H27A 109.3 . . ? C28 C27 H27B 109.3 . . ? C26 C27 H27B 109.3 . . ? H27A C27 H27B 107.9 . . ? C27 C28 C29 112.2(7) . . ? C27 C28 H28A 109.2 . . ? C29 C28 H28A 109.2 . . ? C27 C28 H28B 109.2 . . ? C29 C28 H28B 109.2 . . ? H28A C28 H28B 107.9 . . ? C28 C29 C30 111.0(7) . . ? C28 C29 H29A 109.4 . . ? C30 C29 H29A 109.4 . . ? C28 C29 H29B 109.4 . . ? C30 C29 H29B 109.4 . . ? H29A C29 H29B 108.0 . . ? C29 C30 C25 111.2(7) . . ? C29 C30 H30A 109.4 . . ? C25 C30 H30A 109.4 . . ? C29 C30 H30B 109.4 . . ? C25 C30 H30B 109.4 . . ? H30A C30 H30B 108.0 . . ? C32 C31 C36 110.8(6) . . ? C32 C31 P2 112.8(5) . . ? C36 C31 P2 112.0(5) . . ? C32 C31 H31 106.9 . . ? C36 C31 H31 106.9 . . ? P2 C31 H31 106.9 . . ? C33 C32 C31 111.7(6) . . ? C33 C32 H32A 109.3 . . ? C31 C32 H32A 109.3 . . ? C33 C32 H32B 109.3 . . ? C31 C32 H32B 109.3 . . ? H32A C32 H32B 107.9 . . ? C32 C33 C34 111.5(7) . . ? C32 C33 H33A 109.3 . . ? C34 C33 H33A 109.3 . . ? C32 C33 H33B 109.3 . . ? C34 C33 H33B 109.3 . . ? H33A C33 H33B 108.0 . . ? C35 C34 C33 110.5(7) . . ? C35 C34 H34A 109.5 . . ? C33 C34 H34A 109.5 . . ? C35 C34 H34B 109.5 . . ? C33 C34 H34B 109.5 . . ? H34A C34 H34B 108.1 . . ? C34 C35 C36 110.9(7) . . ? C34 C35 H35A 109.5 . . ? C36 C35 H35A 109.5 . . ? C34 C35 H35B 109.5 . . ? C36 C35 H35B 109.5 . . ? H35A C35 H35B 108.0 . . ? C35 C36 C31 109.2(7) . . ? C35 C36 H36A 109.8 . . ? C31 C36 H36A 109.8 . . ? C35 C36 H36B 109.8 . . ? C31 C36 H36B 109.8 . . ? H36A C36 H36B 108.3 . . ? C43 P3 C49 110.8(5) . . ? C43 P3 C37 110.5(4) . . ? C49 P3 C37 114.1(5) . . ? C43 P3 I18 106.6(3) . . ? C49 P3 I18 108.6(3) . . ? C37 P3 I18 105.9(3) . . ? C42 C37 C38 112.0(8) . . ? C42 C37 P3 115.2(6) . . ? C38 C37 P3 111.9(6) . . ? C42 C37 H37 105.6 . . ? C38 C37 H37 105.6 . . ? P3 C37 H37 105.6 . . ? C39 C38 C37 108.7(8) . . ? C39 C38 H38A 110.0 . . ? C37 C38 H38A 110.0 . . ? C39 C38 H38B 110.0 . . ? C37 C38 H38B 110.0 . . ? H38A C38 H38B 108.3 . . ? C40 C39 C38 111.9(10) . . ? C40 C39 H39A 109.2 . . ? C38 C39 H39A 109.2 . . ? C40 C39 H39B 109.2 . . ? C38 C39 H39B 109.2 . . ? H39A C39 H39B 107.9 . . ? C39 C40 C41 112.2(9) . . ? C39 C40 H40A 109.2 . . ? C41 C40 H40A 109.2 . . ? C39 C40 H40B 109.2 . . ? C41 C40 H40B 109.2 . . ? H40A C40 H40B 107.9 . . ? C40 C41 C42 111.2(9) . . ? C40 C41 H41A 109.4 . . ? C42 C41 H41A 109.4 . . ? C40 C41 H41B 109.4 . . ? C42 C41 H41B 109.4 . . ? H41A C41 H41B 108.0 . . ? C37 C42 C41 111.0(9) . . ? C37 C42 H42A 109.4 . . ? C41 C42 H42A 109.4 . . ? C37 C42 H42B 109.4 . . ? C41 C42 H42B 109.4 . . ? H42A C42 H42B 108.0 . . ? C44 C43 C48 111.4(7) . . ? C44 C43 P3 111.9(5) . . ? C48 C43 P3 112.5(6) . . ? C44 C43 H43 106.9 . . ? C48 C43 H43 106.9 . . ? P3 C43 H43 106.9 . . ? C45 C44 C43 112.9(7) . . ? C45 C44 H44A 109.0 . . ? C43 C44 H44A 109.0 . . ? C45 C44 H44B 109.0 . . ? C43 C44 H44B 109.0 . . ? H44A C44 H44B 107.8 . . ? C44 C45 C46 112.7(8) . . ? C44 C45 H45A 109.1 . . ? C46 C45 H45A 109.1 . . ? C44 C45 H45B 109.1 . . ? C46 C45 H45B 109.1 . . ? H45A C45 H45B 107.8 . . ? C45 C46 C47 109.6(8) . . ? C45 C46 H46A 109.8 . . ? C47 C46 H46A 109.8 . . ? C45 C46 H46B 109.8 . . ? C47 C46 H46B 109.8 . . ? H46A C46 H46B 108.2 . . ? C46 C47 C48 110.3(7) . . ? C46 C47 H47A 109.6 . . ? C48 C47 H47A 109.6 . . ? C46 C47 H47B 109.6 . . ? C48 C47 H47B 109.6 . . ? H47A C47 H47B 108.1 . . ? C47 C48 C43 111.3(7) . . ? C47 C48 H48A 109.4 . . ? C43 C48 H48A 109.4 . . ? C47 C48 H48B 109.4 . . ? C43 C48 H48B 109.4 . . ? H48A C48 H48B 108.0 . . ? C54 C49 C54A 52.7(11) . . ? C54 C49 C50 119.1(11) . . ? C54A C49 C50 117.6(10) . . ? C54 C49 P3 118.8(9) . . ? C54A C49 P3 123.1(9) . . ? C50 C49 P3 112.9(7) . . ? C54 C49 H49 100.2 . . ? C54A C49 H49 47.6 . . ? C50 C49 H49 100.2 . . ? P3 C49 H49 100.2 . . ? C54 C49 H49A 45.8 . . ? C54A C49 H49A 98.4 . . ? C50 C49 H49A 98.4 . . ? P3 C49 H49A 98.4 . . ? H49 C49 H49A 146.0 . . ? C49 C50 C51 115.7(11) . . ? C49 C50 C51A 110.3(11) . . ? C49 C50 H50A 108.4 . . ? C51 C50 H50A 108.4 . . ? C51A C50 H50A 81.1 . . ? C49 C50 H50B 108.4 . . ? C51 C50 H50B 108.4 . . ? C51A C50 H50B 135.0 . . ? H50A C50 H50B 107.4 . . ? C49 C50 H50C 109.6 . . ? C51 C50 H50C 128.9 . . ? C51A C50 H50C 109.6 . . ? H50B C50 H50C 77.3 . . ? C49 C50 H50D 109.6 . . ? C51 C50 H50D 78.2 . . ? C51A C50 H50D 109.6 . . ? H50A C50 H50D 133.2 . . ? H50C C50 H50D 108.1 . . ? C52A C53 C54A 106.8(14) . . ? C52 C53 C54A 115.7(12) . . ? C52A C53 C54 117.2(12) . . ? C52 C53 C54 102.1(13) . . ? C52A C53 H53A 121.8 . . ? C52 C53 H53A 111.4 . . ? C54A C53 H53A 130.4 . . ? C54 C53 H53A 111.4 . . ? C52A C53 H53B 81.2 . . ? C52 C53 H53B 111.4 . . ? C54A C53 H53B 67.2 . . ? C54 C53 H53B 111.4 . . ? H53A C53 H53B 109.2 . . ? C52A C53 H53C 110.4 . . ? C52 C53 H53C 80.3 . . ? C54A C53 H53C 110.4 . . ? C54 C53 H53C 66.5 . . ? H53A C53 H53C 62.9 . . ? H53B C53 H53C 168.2 . . ? C52A C53 H53D 110.4 . . ? C52 C53 H53D 126.2 . . ? C54A C53 H53D 110.4 . . ? C54 C53 H53D 130.7 . . ? H53A C53 H53D 46.0 . . ? H53B C53 H53D 63.3 . . ? H53C C53 H53D 108.6 . . ? C50 C51 C52 105.4(15) . . ? C50 C51 H51A 110.7 . . ? C52 C51 H51A 110.7 . . ? C50 C51 H51B 110.7 . . ? C52 C51 H51B 110.7 . . ? H51A C51 H51B 108.8 . . ? C53 C52 C51 109.6(17) . . ? C53 C52 H52A 109.7 . . ? C51 C52 H52A 109.7 . . ? C53 C52 H52B 109.7 . . ? C51 C52 H52B 109.7 . . ? H52A C52 H52B 108.2 . . ? C49 C54 C53 109.7(13) . . ? C49 C54 H54A 109.7 . . ? C53 C54 H54A 109.7 . . ? C49 C54 H54B 109.7 . . ? C53 C54 H54B 109.7 . . ? H54A C54 H54B 108.2 . . ? C52A C51A C50 109.5(19) . . ? C52A C51A H51C 109.8 . . ? C50 C51A H51C 109.8 . . ? C52A C51A H51D 109.8 . . ? C50 C51A H51D 109.8 . . ? H51C C51A H51D 108.2 . . ? C53 C52A C51A 104.8(18) . . ? C53 C52A H52C 110.8 . . ? C51A C52A H52C 110.8 . . ? C53 C52A H52D 110.8 . . ? C51A C52A H52D 110.8 . . ? H52C C52A H52D 108.9 . . ? C49 C54A C53 107.0(14) . . ? C49 C54A H54C 110.3 . . ? C53 C54A H54C 110.3 . . ? C49 C54A H54D 110.3 . . ? C53 C54A H54D 110.3 . . ? H54C C54A H54D 108.6 . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 30.03 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.567 _refine_diff_density_min -1.924 _refine_diff_density_rms 0.282 #===end data_k02kcm20 _database_code_depnum_ccdc_archive 'CCDC 741172' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C72 H72 I12 P6 Sn3' _chemical_formula_weight 3001.99 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sn Sn -0.6537 1.4246 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _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 65.6481(5) _cell_length_b 12.1063(1) _cell_length_c 23.3971(2) _cell_angle_alpha 90.00 _cell_angle_beta 104.324(4) _cell_angle_gamma 90.00 _cell_volume 18016.9(3) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 91242 _cell_measurement_theta_min 2.910 _cell_measurement_theta_max 27.485 _exptl_crystal_description block _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.213 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 11040 _exptl_absorpt_coefficient_mu 5.081 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4083 _exptl_absorpt_correction_T_max 0.6667 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements Sortav (Blessing 1995) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator 'horizonally mounted graphite crystal' _diffrn_measurement_device_type '95mm CCD camera on \k-goniostat' _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 100805 _diffrn_reflns_av_R_equivalents 0.1165 _diffrn_reflns_av_sigmaI/netI 0.1037 _diffrn_reflns_limit_h_min -85 _diffrn_reflns_limit_h_max 83 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 3.58 _diffrn_reflns_theta_max 27.52 _reflns_number_total 20252 _reflns_number_gt 12410 _reflns_threshold_expression >2\s(I) _computing_data_collection 'Collect (Bruker AXS BV 1997-2004)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'Denzo & Scalepack (Otwinowski, Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick 1990)' _computing_structure_refinement 'SHELXL-97/2 (Sheldrick 1997)' _computing_molecular_graphics 'ORTEX (P.McArdle 1995)' _computing_publication_material 'SHELXL-97/2 (Sheldrick 1997)' _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^ > 2\s(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^)+(0.0404P)^2^+18.4368P] 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 20252 _refine_ls_number_parameters 834 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1129 _refine_ls_R_factor_gt 0.0528 _refine_ls_wR_factor_ref 0.1071 _refine_ls_wR_factor_gt 0.0907 _refine_ls_goodness_of_fit_ref 0.984 _refine_ls_restrained_S_all 0.984 _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 I1 I 0.150576(8) 0.83677(4) 0.61699(2) 0.02536(12) Uani 1 1 d . . . I2 I 0.152879(9) 1.07320(4) 0.47383(2) 0.03091(14) Uani 1 1 d . . . I3 I 0.153763(9) 0.69879(4) 0.44241(2) 0.03171(14) Uani 1 1 d . . . I4 I 0.094888(8) 1.03711(4) 0.54162(2) 0.02772(13) Uani 1 1 d . . . I5 I 0.089345(10) 0.69655(4) 0.50186(2) 0.03998(16) Uani 1 1 d . . . I6 I 0.092769(8) 0.92217(4) 0.36284(2) 0.02948(13) Uani 1 1 d . . . I7 I 0.028330(8) 0.85451(4) 0.52289(2) 0.02855(13) Uani 1 1 d . . . I8 I 0.027515(10) 1.07847(4) 0.36582(2) 0.03660(15) Uani 1 1 d . . . I9 I 0.033017(9) 0.71932(4) 0.35502(2) 0.03642(15) Uani 1 1 d . . . I10 I 0.210727(9) 1.01550(4) 0.64321(2) 0.03518(14) Uani 1 1 d . . . I11 I 0.210480(8) 0.67182(4) 0.60631(2) 0.03174(14) Uani 1 1 d . . . I12 I 0.220091(9) 0.90398(4) 0.47143(2) 0.03410(14) Uani 1 1 d . . . Sn1 Sn 0.122723(8) 0.87826(4) 0.48708(2) 0.02409(13) Uani 1 1 d . . . Sn2 Sn 0.056471(9) 0.88604(4) 0.43536(2) 0.02565(13) Uani 1 1 d . . . Sn3 Sn 0.187820(9) 0.86987(4) 0.54311(2) 0.02544(13) Uani 1 1 d . . . P1 P -0.03415(3) 0.84688(16) 0.47069(9) 0.0250(5) Uani 1 1 d . . . H1A H -0.0497 0.9003 0.4889 0.030 Uiso 1 1 calc R . . H1B H -0.0153 0.8882 0.5013 0.030 Uiso 1 1 calc R . . P2 P 0.15314(3) 0.86378(17) 0.12893(9) 0.0283(5) Uani 1 1 d . . . H2A H 0.1354 0.9162 0.0991 0.034 Uiso 1 1 calc R . . H2B H 0.1697 0.9107 0.1130 0.034 Uiso 1 1 calc R . . P3 P 0.28407(3) 0.90180(17) 0.54805(9) 0.0282(5) Uani 1 1 d . . . H3A H 0.2665 0.8634 0.5095 0.034 Uiso 1 1 calc R . . H3B H 0.3007 0.8404 0.5414 0.034 Uiso 1 1 calc R . . P4 P 0.04047(4) 0.82171(18) 0.70043(9) 0.0326(5) Uani 1 1 d . A . H4A H 0.0311 0.8753 0.6496 0.039 Uiso 1 1 calc R . . H4B H 0.0353 0.8750 0.7460 0.039 Uiso 1 1 calc R . . P5 P 0.09337(4) 0.60894(18) 0.35725(11) 0.0400(6) Uani 1 1 d . . . H5A H 0.1107 0.6581 0.3919 0.048 Uiso 1 1 calc R . . H5B H 0.0764 0.6723 0.3583 0.048 Uiso 1 1 calc R . . P6 P 0.19270(4) 0.82494(18) 0.74781(9) 0.0311(5) Uani 1 1 d . . . H6A H 0.1830 0.9248 0.7384 0.037 Uiso 1 1 calc R . . H6B H 0.1953 0.7879 0.6952 0.037 Uiso 1 1 calc R . . C1 C -0.03723(12) 0.8693(6) 0.3935(3) 0.0214(17) Uani 1 1 d . . . C2 C -0.02020(13) 0.8632(7) 0.3691(4) 0.039(2) Uani 1 1 d . . . H2 H -0.0065 0.8510 0.3936 0.046 Uiso 1 1 calc R . . C3 C -0.02297(16) 0.8749(7) 0.3088(4) 0.041(2) Uani 1 1 d . . . H3 H -0.0111 0.8716 0.2923 0.049 Uiso 1 1 calc R . . C4 C -0.04252(16) 0.8910(7) 0.2730(4) 0.039(2) Uani 1 1 d . . . H4 H -0.0444 0.8984 0.2316 0.047 Uiso 1 1 calc R . . C5 C -0.05963(16) 0.8966(8) 0.2975(4) 0.049(3) Uani 1 1 d . . . H5 H -0.0733 0.9076 0.2726 0.058 Uiso 1 1 calc R . . C6 C -0.05703(14) 0.8862(7) 0.3586(4) 0.040(2) Uani 1 1 d . . . H6 H -0.0688 0.8909 0.3754 0.048 Uiso 1 1 calc R . . C7 C -0.03533(14) 0.7015(6) 0.4850(3) 0.032(2) Uani 1 1 d . . . C8 C -0.02061(16) 0.6480(8) 0.5255(6) 0.070(3) Uani 1 1 d . . . H8 H -0.0089 0.6874 0.5485 0.084 Uiso 1 1 calc R . . C9 C -0.02237(18) 0.5371(8) 0.5336(6) 0.088(5) Uani 1 1 d . . . H9 H -0.0115 0.4996 0.5610 0.105 Uiso 1 1 calc R . . C10 C -0.0390(2) 0.4802(8) 0.5040(5) 0.064(3) Uani 1 1 d . . . H10 H -0.0402 0.4033 0.5108 0.077 Uiso 1 1 calc R . . C11 C -0.0537(3) 0.5320(11) 0.4656(6) 0.186(11) Uani 1 1 d . . . H11 H -0.0656 0.4922 0.4436 0.223 Uiso 1 1 calc R . . C12 C -0.0522(3) 0.6452(10) 0.4565(6) 0.173(10) Uani 1 1 d . . . H12 H -0.0634 0.6825 0.4298 0.208 Uiso 1 1 calc R . . C13 C 0.15157(16) 0.7211(7) 0.1090(3) 0.038(2) Uani 1 1 d . . . C14 C 0.13300(17) 0.6782(7) 0.0757(4) 0.045(3) Uani 1 1 d . . . H14 H 0.1210 0.7240 0.0630 0.054 Uiso 1 1 calc R . . C15 C 0.1321(2) 0.5682(9) 0.0611(5) 0.080(4) Uani 1 1 d . . . H15 H 0.1192 0.5397 0.0383 0.096 Uiso 1 1 calc R . . C16 C 0.1483(4) 0.4990(10) 0.0769(6) 0.134(10) Uani 1 1 d . . . H16 H 0.1471 0.4233 0.0659 0.161 Uiso 1 1 calc R . . C17 C 0.1668(3) 0.5428(11) 0.1099(6) 0.106(7) Uani 1 1 d . . . H17 H 0.1786 0.4953 0.1223 0.127 Uiso 1 1 calc R . . C18 C 0.1690(2) 0.6531(9) 0.1261(4) 0.074(4) Uani 1 1 d . . . H18 H 0.1821 0.6814 0.1482 0.089 Uiso 1 1 calc R . . C19 C 0.15624(13) 0.8816(6) 0.2071(3) 0.0272(19) Uani 1 1 d . . . C20 C 0.14062(14) 0.9354(7) 0.2267(4) 0.039(2) Uani 1 1 d . . . H20 H 0.1283 0.9609 0.1996 0.047 Uiso 1 1 calc R . . C21 C 0.14345(19) 0.9513(8) 0.2873(5) 0.061(3) Uani 1 1 d . . . H21 H 0.1329 0.9882 0.3016 0.073 Uiso 1 1 calc R . . C22 C 0.16126(19) 0.9144(8) 0.3263(4) 0.054(3) Uani 1 1 d . . . H22 H 0.1630 0.9251 0.3675 0.065 Uiso 1 1 calc R . . C23 C 0.17689(17) 0.8610(7) 0.3057(4) 0.052(3) Uani 1 1 d . . . H23 H 0.1893 0.8359 0.3328 0.063 Uiso 1 1 calc R . . C24 C 0.17426(14) 0.8446(7) 0.2454(3) 0.034(2) Uani 1 1 d . . . H24 H 0.1848 0.8083 0.2309 0.041 Uiso 1 1 calc R . . C25 C 0.28814(12) 1.0447(6) 0.5322(3) 0.0249(18) Uani 1 1 d . . . C26 C 0.30497(12) 1.0725(6) 0.5103(3) 0.0293(19) Uani 1 1 d . . . H26 H 0.3143 1.0173 0.5030 0.035 Uiso 1 1 calc R . . C27 C 0.30820(14) 1.1840(6) 0.4988(4) 0.036(2) Uani 1 1 d . . . H27 H 0.3197 1.2043 0.4833 0.043 Uiso 1 1 calc R . . C28 C 0.29478(14) 1.2647(7) 0.5099(3) 0.036(2) Uani 1 1 d . . . H28 H 0.2970 1.3401 0.5020 0.043 Uiso 1 1 calc R . . C29 C 0.27756(15) 1.2338(7) 0.5333(4) 0.039(2) Uani 1 1 d . . . H29 H 0.2683 1.2885 0.5414 0.047 Uiso 1 1 calc R . . C30 C 0.27438(13) 1.1239(7) 0.5440(4) 0.036(2) Uani 1 1 d . . . H30 H 0.2629 1.1024 0.5594 0.043 Uiso 1 1 calc R . . C31 C 0.28132(12) 0.8885(6) 0.6211(3) 0.0278(19) Uani 1 1 d . . . C32 C 0.29612(16) 0.9347(7) 0.6670(4) 0.054(3) Uani 1 1 d . . . H32 H 0.3078 0.9732 0.6594 0.065 Uiso 1 1 calc R . . C33 C 0.29395(19) 0.9249(8) 0.7240(4) 0.070(4) Uani 1 1 d . . . H33 H 0.3042 0.9579 0.7553 0.084 Uiso 1 1 calc R . . C34 C 0.27778(16) 0.8698(8) 0.7362(4) 0.050(3) Uani 1 1 d . . . H34 H 0.2766 0.8643 0.7757 0.060 Uiso 1 1 calc R . . C35 C 0.26271(14) 0.8206(9) 0.6903(4) 0.056(3) Uani 1 1 d . . . H35 H 0.2514 0.7805 0.6986 0.067 Uiso 1 1 calc R . . C36 C 0.26440(14) 0.8306(8) 0.6326(4) 0.048(3) Uani 1 1 d . . . H36 H 0.2541 0.7983 0.6012 0.058 Uiso 1 1 calc R . . C37 C 0.03138(13) 0.6828(6) 0.6970(3) 0.031(2) Uani 1 1 d . . . C38 C 0.0285(2) 0.6373(11) 0.7493(6) 0.052(4) Uiso 0.703(9) 1 d P A 1 H38 H 0.0288 0.6838 0.7822 0.062 Uiso 0.703(9) 1 calc PR A 1 C39 C 0.0252(2) 0.5264(11) 0.7534(6) 0.054(4) Uiso 0.703(9) 1 d P A 1 H39 H 0.0233 0.4956 0.7891 0.065 Uiso 0.703(9) 1 calc PR A 1 C40 C 0.0247(3) 0.4614(15) 0.7065(8) 0.059(5) Uiso 0.703(9) 1 d P A 1 H40 H 0.0215 0.3852 0.7092 0.071 Uiso 0.703(9) 1 calc PR A 1 C41 C 0.0285(2) 0.5003(11) 0.6548(6) 0.053(4) Uiso 0.703(9) 1 d P A 1 H41 H 0.0287 0.4519 0.6229 0.064 Uiso 0.703(9) 1 calc PR A 1 C42 C 0.0322(2) 0.6141(11) 0.6510(6) 0.056(4) Uiso 0.703(9) 1 d P A 1 H42 H 0.0352 0.6437 0.6164 0.067 Uiso 0.703(9) 1 calc PR A 1 C38A C 0.0439(5) 0.596(2) 0.7104(12) 0.033(7) Uiso 0.297(9) 1 d P A 2 H38A H 0.0586 0.6077 0.7221 0.039 Uiso 0.297(9) 1 calc PR A 2 C39A C 0.0353(5) 0.478(3) 0.7079(14) 0.036(8) Uiso 0.297(9) 1 d P A 2 H39A H 0.0442 0.4172 0.7227 0.043 Uiso 0.297(9) 1 calc PR A 2 C40A C 0.0145(6) 0.465(3) 0.6834(15) 0.041(9) Uiso 0.297(9) 1 d P A 2 H40A H 0.0091 0.3923 0.6782 0.049 Uiso 0.297(9) 1 calc PR A 2 C41A C 0.0012(6) 0.548(3) 0.6660(16) 0.069(12) Uiso 0.297(9) 1 d P A 2 H41A H -0.0133 0.5329 0.6498 0.082 Uiso 0.297(9) 1 calc PR A 2 C42A C 0.0083(6) 0.663(3) 0.6714(14) 0.057(10) Uiso 0.297(9) 1 d P A 2 H42A H -0.0012 0.7223 0.6593 0.068 Uiso 0.297(9) 1 calc PR A 2 C43 C 0.06812(14) 0.8233(6) 0.7106(3) 0.032(2) Uani 1 1 d . . . C44 C 0.08095(15) 0.8195(7) 0.7673(4) 0.039(2) Uani 1 1 d . A . H44 H 0.0749 0.8229 0.8003 0.047 Uiso 1 1 calc R . . C45 C 0.10262(15) 0.8109(7) 0.7761(4) 0.044(2) Uani 1 1 d . . . H45 H 0.1114 0.8090 0.8150 0.053 Uiso 1 1 calc R A . C46 C 0.11129(14) 0.8052(7) 0.7287(4) 0.040(2) Uani 1 1 d . A . H46 H 0.1261 0.7986 0.7349 0.048 Uiso 1 1 calc R . . C47 C 0.09858(14) 0.8089(7) 0.6718(4) 0.040(2) Uani 1 1 d . . . H47 H 0.1047 0.8052 0.6391 0.048 Uiso 1 1 calc R A . C48 C 0.07724(14) 0.8178(7) 0.6629(4) 0.038(2) Uani 1 1 d . A . H48 H 0.0686 0.8203 0.6238 0.046 Uiso 1 1 calc R . . C49 C 0.09019(15) 0.4739(6) 0.3854(4) 0.036(2) Uani 1 1 d . . . C50 C 0.07017(16) 0.4357(8) 0.3825(5) 0.067(3) Uani 1 1 d . . . H50 H 0.0585 0.4833 0.3687 0.080 Uiso 1 1 calc R . . C51 C 0.0669(2) 0.3305(8) 0.3991(5) 0.069(3) Uani 1 1 d . . . H51 H 0.0531 0.3048 0.3972 0.082 Uiso 1 1 calc R . . C52 C 0.0839(2) 0.2622(8) 0.4185(4) 0.062(3) Uani 1 1 d . . . H52 H 0.0818 0.1882 0.4293 0.075 Uiso 1 1 calc R . . C53 C 0.1044(2) 0.3000(9) 0.4225(4) 0.065(3) Uani 1 1 d . . . H53 H 0.1160 0.2525 0.4366 0.078 Uiso 1 1 calc R . . C54 C 0.10745(16) 0.4063(8) 0.4060(4) 0.047(3) Uani 1 1 d . . . H54 H 0.1213 0.4331 0.4087 0.057 Uiso 1 1 calc R . . C55 C 0.09614(13) 0.5985(7) 0.2827(4) 0.040(2) Uani 1 1 d . . . C56 C 0.1064(3) 0.6748(10) 0.2618(6) 0.117(6) Uani 1 1 d . . . H56 H 0.1122 0.7365 0.2854 0.140 Uiso 1 1 calc R . . C57 C 0.1087(3) 0.6644(11) 0.2052(7) 0.151(9) Uani 1 1 d . . . H57 H 0.1167 0.7187 0.1909 0.181 Uiso 1 1 calc R . . C58 C 0.10037(17) 0.5819(10) 0.1697(5) 0.071(4) Uani 1 1 d . . . H58 H 0.1012 0.5804 0.1297 0.086 Uiso 1 1 calc R . . C59 C 0.0910(2) 0.5023(10) 0.1917(5) 0.092(5) Uani 1 1 d . . . H59 H 0.0853 0.4407 0.1679 0.110 Uiso 1 1 calc R . . C60 C 0.0894(3) 0.5085(9) 0.2492(5) 0.118(6) Uani 1 1 d . . . H60 H 0.0835 0.4483 0.2656 0.141 Uiso 1 1 calc R . . C61 C 0.21792(12) 0.8415(7) 0.7982(3) 0.0281(19) Uani 1 1 d . . . C62 C 0.23099(14) 0.7492(7) 0.8146(4) 0.038(2) Uani 1 1 d . . . H62 H 0.2266 0.6777 0.7999 0.045 Uiso 1 1 calc R . . C63 C 0.25057(15) 0.7662(9) 0.8533(4) 0.050(3) Uani 1 1 d . . . H63 H 0.2598 0.7054 0.8655 0.060 Uiso 1 1 calc R . . C64 C 0.25661(14) 0.8698(9) 0.8737(4) 0.044(2) Uani 1 1 d . . . H64 H 0.2700 0.8799 0.9000 0.053 Uiso 1 1 calc R . . C65 C 0.24407(15) 0.9578(8) 0.8576(4) 0.046(2) Uani 1 1 d . . . H65 H 0.2487 1.0293 0.8720 0.055 Uiso 1 1 calc R . . C66 C 0.22458(14) 0.9441(7) 0.8204(4) 0.035(2) Uani 1 1 d . . . H66 H 0.2156 1.0061 0.8098 0.042 Uiso 1 1 calc R . . C67 C 0.17630(12) 0.7301(7) 0.7746(3) 0.0287(19) Uani 1 1 d . . . C68 C 0.17233(13) 0.7469(7) 0.8296(4) 0.038(2) Uani 1 1 d . . . H68 H 0.1783 0.8083 0.8530 0.045 Uiso 1 1 calc R . . C69 C 0.15967(14) 0.6740(9) 0.8498(4) 0.050(3) Uani 1 1 d . . . H69 H 0.1570 0.6850 0.8875 0.060 Uiso 1 1 calc R . . C70 C 0.15070(15) 0.5845(8) 0.8157(5) 0.052(3) Uani 1 1 d . . . H70 H 0.1419 0.5348 0.8298 0.062 Uiso 1 1 calc R . . C71 C 0.15473(14) 0.5678(7) 0.7605(4) 0.043(2) Uani 1 1 d . . . H71 H 0.1489 0.5061 0.7370 0.052 Uiso 1 1 calc R . . C72 C 0.16723(12) 0.6416(6) 0.7406(3) 0.0285(19) Uani 1 1 d . . . H72 H 0.1697 0.6316 0.7027 0.034 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 I1 0.0229(3) 0.0282(3) 0.0239(3) 0.0003(2) 0.0037(2) 0.0011(2) I2 0.0325(3) 0.0296(3) 0.0321(3) -0.0002(2) 0.0107(3) -0.0001(2) I3 0.0296(3) 0.0325(3) 0.0333(3) -0.0014(2) 0.0084(3) 0.0041(2) I4 0.0218(3) 0.0281(3) 0.0331(3) -0.0034(2) 0.0065(2) 0.0026(2) I5 0.0498(4) 0.0258(3) 0.0390(3) -0.0010(2) 0.0009(3) -0.0049(3) I6 0.0277(3) 0.0370(3) 0.0226(3) 0.0010(2) 0.0041(2) -0.0022(2) I7 0.0233(3) 0.0327(3) 0.0296(3) 0.0044(2) 0.0065(2) -0.0026(2) I8 0.0516(4) 0.0287(3) 0.0323(3) -0.0007(2) 0.0159(3) -0.0042(3) I9 0.0438(4) 0.0270(3) 0.0327(3) -0.0017(2) -0.0014(3) -0.0095(3) I10 0.0318(3) 0.0339(3) 0.0396(3) -0.0054(3) 0.0085(3) -0.0071(3) I11 0.0258(3) 0.0297(3) 0.0388(3) 0.0007(2) 0.0062(3) 0.0036(2) I12 0.0342(4) 0.0357(3) 0.0375(3) 0.0033(3) 0.0184(3) 0.0014(3) Sn1 0.0209(3) 0.0247(3) 0.0244(3) -0.0012(2) 0.0015(2) 0.0014(2) Sn2 0.0260(3) 0.0239(3) 0.0268(3) -0.0017(2) 0.0061(3) -0.0046(2) Sn3 0.0232(3) 0.0268(3) 0.0276(3) -0.0006(2) 0.0086(3) 0.0027(2) P1 0.0273(13) 0.0252(11) 0.0232(11) 0.0000(9) 0.0074(10) -0.0010(9) P2 0.0290(13) 0.0282(12) 0.0281(11) 0.0051(9) 0.0079(10) 0.0027(10) P3 0.0273(13) 0.0255(12) 0.0319(12) 0.0001(9) 0.0076(10) 0.0001(10) P4 0.0391(15) 0.0321(12) 0.0295(12) 0.0035(10) 0.0140(11) 0.0018(11) P5 0.0366(15) 0.0267(13) 0.0492(15) -0.0015(11) -0.0036(12) -0.0014(11) P6 0.0289(14) 0.0340(12) 0.0269(12) 0.0030(10) 0.0000(10) -0.0036(10) C1 0.018(5) 0.023(4) 0.021(4) 0.001(3) 0.001(4) -0.001(3) C2 0.022(5) 0.051(6) 0.038(5) 0.014(4) -0.004(4) -0.009(4) C3 0.056(7) 0.047(6) 0.025(5) 0.002(4) 0.018(5) -0.014(5) C4 0.056(7) 0.042(5) 0.023(5) 0.003(4) 0.015(5) 0.005(5) C5 0.050(7) 0.069(7) 0.025(5) 0.008(5) 0.004(5) 0.023(5) C6 0.034(6) 0.056(6) 0.037(5) 0.011(4) 0.021(5) 0.019(5) C7 0.041(6) 0.031(5) 0.020(4) 0.000(4) 0.001(4) -0.010(4) C8 0.031(7) 0.037(6) 0.134(11) 0.013(7) 0.004(7) -0.009(5) C9 0.048(8) 0.031(6) 0.188(14) 0.048(8) 0.037(9) 0.006(5) C10 0.116(11) 0.023(5) 0.056(7) 0.006(5) 0.028(7) -0.025(6) C11 0.29(2) 0.072(10) 0.109(12) 0.050(9) -0.108(14) -0.108(13) C12 0.24(2) 0.071(9) 0.130(12) 0.075(9) -0.111(13) -0.097(11) C13 0.070(7) 0.036(5) 0.017(4) 0.011(4) 0.025(5) 0.013(5) C14 0.076(8) 0.025(5) 0.039(5) -0.005(4) 0.021(6) -0.004(5) C15 0.175(14) 0.030(6) 0.056(7) -0.025(6) 0.066(9) -0.043(8) C16 0.37(3) 0.017(7) 0.053(9) 0.008(6) 0.131(14) 0.026(12) C17 0.23(2) 0.053(9) 0.057(9) 0.028(7) 0.083(11) 0.096(11) C18 0.114(11) 0.077(8) 0.042(6) 0.023(6) 0.036(7) 0.067(8) C19 0.027(5) 0.030(5) 0.024(4) -0.002(4) 0.005(4) 0.001(4) C20 0.044(6) 0.032(5) 0.046(6) 0.009(4) 0.019(5) -0.003(4) C21 0.094(10) 0.049(6) 0.055(7) 0.013(5) 0.047(7) 0.008(6) C22 0.093(9) 0.041(6) 0.033(5) 0.007(5) 0.026(6) -0.005(6) C23 0.072(8) 0.049(6) 0.036(6) 0.007(5) 0.013(6) -0.001(6) C24 0.037(6) 0.041(5) 0.026(5) 0.003(4) 0.008(4) 0.002(4) C25 0.015(4) 0.031(5) 0.027(4) 0.004(4) 0.001(4) -0.001(4) C26 0.020(5) 0.034(5) 0.031(5) -0.005(4) 0.001(4) 0.004(4) C27 0.035(6) 0.032(5) 0.039(5) -0.001(4) 0.007(4) -0.006(4) C28 0.047(6) 0.023(5) 0.033(5) 0.003(4) 0.000(4) 0.007(4) C29 0.054(7) 0.025(5) 0.040(5) -0.004(4) 0.015(5) 0.005(4) C30 0.028(5) 0.042(6) 0.040(5) -0.001(4) 0.013(4) 0.000(4) C31 0.015(5) 0.027(4) 0.038(5) 0.005(4) 0.002(4) 0.005(4) C32 0.062(7) 0.055(6) 0.042(6) 0.015(5) 0.007(5) -0.034(5) C33 0.100(10) 0.068(7) 0.032(6) 0.010(5) -0.003(6) -0.037(7) C34 0.044(7) 0.071(7) 0.038(6) 0.014(5) 0.016(5) 0.006(6) C35 0.020(6) 0.106(9) 0.043(6) 0.005(6) 0.012(5) -0.008(5) C36 0.023(5) 0.079(7) 0.042(6) -0.002(5) 0.008(4) -0.010(5) C37 0.028(5) 0.034(5) 0.034(5) 0.013(4) 0.014(4) -0.001(4) C43 0.044(6) 0.027(5) 0.024(4) 0.003(4) 0.008(4) -0.005(4) C44 0.056(7) 0.039(5) 0.026(5) 0.001(4) 0.015(5) 0.000(5) C45 0.042(7) 0.054(6) 0.028(5) 0.003(4) -0.005(5) -0.002(5) C46 0.028(5) 0.046(6) 0.043(6) 0.007(4) 0.003(5) 0.003(4) C47 0.028(6) 0.054(6) 0.039(5) 0.007(4) 0.009(5) 0.001(4) C48 0.035(6) 0.052(6) 0.028(5) 0.009(4) 0.008(4) -0.003(5) C49 0.044(6) 0.021(5) 0.042(5) -0.004(4) 0.006(5) -0.001(4) C50 0.035(7) 0.038(6) 0.119(10) 0.000(6) 0.004(7) -0.006(5) C51 0.079(9) 0.031(6) 0.103(9) -0.010(6) 0.034(8) -0.017(6) C52 0.128(12) 0.034(6) 0.031(6) -0.005(4) 0.029(7) 0.002(7) C53 0.093(10) 0.056(8) 0.047(7) 0.008(5) 0.017(7) 0.044(7) C54 0.050(7) 0.051(6) 0.043(6) 0.002(5) 0.015(5) 0.022(5) C55 0.022(5) 0.025(5) 0.066(6) -0.002(5) -0.002(5) 0.000(4) C56 0.208(17) 0.066(8) 0.118(12) -0.048(8) 0.117(12) -0.059(10) C57 0.27(2) 0.101(11) 0.140(14) -0.075(10) 0.168(16) -0.108(13) C58 0.067(8) 0.083(9) 0.079(8) -0.033(7) 0.048(7) -0.021(7) C59 0.147(14) 0.061(8) 0.047(7) -0.019(6) -0.011(8) -0.035(9) C60 0.225(18) 0.063(8) 0.043(7) -0.004(6) -0.010(9) -0.068(10) C61 0.025(5) 0.035(5) 0.026(4) 0.001(4) 0.009(4) 0.003(4) C62 0.040(6) 0.036(5) 0.041(5) 0.002(4) 0.017(5) 0.004(4) C63 0.023(6) 0.075(8) 0.053(6) 0.025(6) 0.007(5) 0.017(5) C64 0.022(5) 0.079(8) 0.029(5) -0.001(5) 0.001(4) -0.016(5) C65 0.026(6) 0.060(7) 0.052(6) -0.019(5) 0.010(5) -0.010(5) C66 0.032(6) 0.034(5) 0.038(5) -0.007(4) 0.007(4) 0.001(4) C67 0.021(5) 0.040(5) 0.022(4) 0.000(4) 0.001(4) 0.002(4) C68 0.031(6) 0.048(6) 0.030(5) 0.000(4) 0.000(4) -0.002(4) C69 0.033(6) 0.083(8) 0.033(5) 0.017(5) 0.006(5) -0.002(6) C70 0.033(6) 0.056(7) 0.061(7) 0.019(6) 0.004(5) -0.013(5) C71 0.039(6) 0.029(5) 0.056(6) 0.009(5) -0.001(5) -0.010(4) C72 0.029(5) 0.029(5) 0.024(4) -0.005(4) -0.001(4) 0.001(4) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 I1 Sn1 3.1755(7) . ? I1 Sn3 3.3492(7) . ? I2 Sn1 3.1446(7) . ? I2 Sn3 3.4797(8) . ? I3 Sn1 3.3195(7) . ? I3 Sn3 3.4976(8) . ? I4 Sn1 3.1336(7) . ? I4 Sn2 3.5755(7) . ? I5 Sn1 3.1836(8) . ? I5 Sn2 3.2680(8) . ? I6 Sn1 3.1258(7) . ? I6 Sn2 3.2785(7) . ? I7 Sn2 3.1024(7) . ? I8 Sn2 3.1870(8) . ? I9 Sn2 2.9234(7) . ? I10 Sn3 3.0186(8) . ? I11 Sn3 3.0100(7) . ? I12 Sn3 3.0380(7) . ? P1 C1 1.787(7) . ? P1 C7 1.797(8) . ? P1 H1A 1.3600 . ? P1 H1B 1.3600 . ? P2 C13 1.786(9) . ? P2 C19 1.803(8) . ? P2 H2A 1.3600 . ? P2 H2B 1.3600 . ? P3 C31 1.770(8) . ? P3 C25 1.803(8) . ? P3 H3A 1.3600 . ? P3 H3B 1.3600 . ? P4 C43 1.772(9) . ? P4 C37 1.780(8) . ? P4 H4A 1.3600 . ? P4 H4B 1.3600 . ? P5 C49 1.794(8) . ? P5 C55 1.803(10) . ? P5 H5A 1.3600 . ? P5 H5B 1.3600 . ? P6 C67 1.790(8) . ? P6 C61 1.790(8) . ? P6 H6A 1.3600 . ? P6 H6B 1.3600 . ? C1 C6 1.369(11) . ? C1 C2 1.378(10) . ? C2 C3 1.383(11) . ? C2 H2 0.9500 . ? C3 C4 1.362(12) . ? C3 H3 0.9500 . ? C4 C5 1.382(12) . ? C4 H4 0.9500 . ? C5 C6 1.404(11) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C7 C12 1.332(14) . ? C7 C8 1.340(12) . ? C8 C9 1.366(12) . ? C8 H8 0.9500 . ? C9 C10 1.332(15) . ? C9 H9 0.9500 . ? C10 C11 1.307(17) . ? C10 H10 0.9500 . ? C11 C12 1.394(16) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? C13 C14 1.376(12) . ? C13 C18 1.387(12) . ? C14 C15 1.372(12) . ? C14 H14 0.9500 . ? C15 C16 1.33(2) . ? C15 H15 0.9500 . ? C16 C17 1.37(2) . ? C16 H16 0.9500 . ? C17 C18 1.386(17) . ? C17 H17 0.9500 . ? C18 H18 0.9500 . ? C19 C24 1.370(11) . ? C19 C20 1.385(11) . ? C20 C21 1.397(12) . ? C20 H20 0.9500 . ? C21 C22 1.368(14) . ? C21 H21 0.9500 . ? C22 C23 1.396(13) . ? C22 H22 0.9500 . ? C23 C24 1.394(11) . ? C23 H23 0.9500 . ? C24 H24 0.9500 . ? C25 C26 1.370(10) . ? C25 C30 1.391(10) . ? C26 C27 1.402(10) . ? C26 H26 0.9500 . ? C27 C28 1.382(11) . ? C27 H27 0.9500 . ? C28 C29 1.422(12) . ? C28 H28 0.9500 . ? C29 C30 1.380(11) . ? C29 H29 0.9500 . ? C30 H30 0.9500 . ? C31 C32 1.376(11) . ? C31 C36 1.394(11) . ? C32 C33 1.381(12) . ? C32 H32 0.9500 . ? C33 C34 1.343(13) . ? C33 H33 0.9500 . ? C34 C35 1.401(13) . ? C34 H34 0.9500 . ? C35 C36 1.386(12) . ? C35 H35 0.9500 . ? C36 H36 0.9500 . ? C37 C38A 1.32(3) . ? C37 C42 1.370(15) . ? C37 C38 1.397(14) . ? C37 C42A 1.50(4) . ? C38 C39 1.367(17) . ? C38 H38 0.9500 . ? C39 C40 1.34(2) . ? C39 H39 0.9500 . ? C40 C41 1.38(2) . ? C40 H40 0.9500 . ? C41 C42 1.405(18) . ? C41 H41 0.9500 . ? C42 H42 0.9500 . ? C38A C39A 1.53(4) . ? C38A H38A 0.9500 . ? C39A C40A 1.35(5) . ? C39A H39A 0.9500 . ? C40A C41A 1.33(4) . ? C40A H40A 0.9500 . ? C41A C42A 1.46(4) . ? C41A H41A 0.9500 . ? C42A H42A 0.9500 . ? C43 C44 1.385(11) . ? C43 C48 1.394(10) . ? C44 C45 1.390(12) . ? C44 H44 0.9500 . ? C45 C46 1.366(11) . ? C45 H45 0.9500 . ? C46 C47 1.386(11) . ? C46 H46 0.9500 . ? C47 C48 1.368(11) . ? C47 H47 0.9500 . ? C48 H48 0.9500 . ? C49 C50 1.379(12) . ? C49 C54 1.384(11) . ? C50 C51 1.364(13) . ? C50 H50 0.9500 . ? C51 C52 1.373(15) . ? C51 H51 0.9500 . ? C52 C53 1.399(15) . ? C52 H52 0.9500 . ? C53 C54 1.373(13) . ? C53 H53 0.9500 . ? C54 H54 0.9500 . ? C55 C56 1.306(13) . ? C55 C60 1.350(13) . ? C56 C57 1.377(16) . ? C56 H56 0.9500 . ? C57 C58 1.327(15) . ? C57 H57 0.9500 . ? C58 C59 1.316(14) . ? C58 H58 0.9500 . ? C59 C60 1.376(15) . ? C59 H59 0.9500 . ? C60 H60 0.9500 . ? C61 C66 1.375(10) . ? C61 C62 1.404(11) . ? C62 C63 1.392(12) . ? C62 H62 0.9500 . ? C63 C64 1.366(13) . ? C63 H63 0.9500 . ? C64 C65 1.342(12) . ? C64 H64 0.9500 . ? C65 C66 1.368(12) . ? C65 H65 0.9500 . ? C66 H66 0.9500 . ? C67 C72 1.378(10) . ? C67 C68 1.388(10) . ? C68 C69 1.374(12) . ? C68 H68 0.9500 . ? C69 C70 1.388(13) . ? C69 H69 0.9500 . ? C70 C71 1.394(12) . ? C70 H70 0.9500 . ? C71 C72 1.370(11) . ? C71 H71 0.9500 . ? C72 H72 0.9500 . ? 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 I1 Sn3 78.936(17) . . ? Sn1 I2 Sn3 77.390(17) . . ? Sn1 I3 Sn3 74.941(16) . . ? Sn1 I4 Sn2 77.585(17) . . ? Sn1 I5 Sn2 81.628(18) . . ? Sn1 I6 Sn2 82.335(18) . . ? I6 Sn1 I4 88.753(19) . . ? I6 Sn1 I2 92.708(19) . . ? I4 Sn1 I2 91.395(19) . . ? I6 Sn1 I1 176.18(2) . . ? I4 Sn1 I1 87.880(18) . . ? I2 Sn1 I1 89.175(19) . . ? I6 Sn1 I5 85.812(19) . . ? I4 Sn1 I5 83.884(19) . . ? I2 Sn1 I5 175.08(2) . . ? I1 Sn1 I5 92.037(19) . . ? I6 Sn1 I3 96.458(19) . . ? I4 Sn1 I3 174.34(2) . . ? I2 Sn1 I3 90.557(19) . . ? I1 Sn1 I3 86.840(18) . . ? I5 Sn1 I3 94.273(19) . . ? I9 Sn2 I7 91.98(2) . . ? I9 Sn2 I8 91.36(2) . . ? I7 Sn2 I8 92.84(2) . . ? I9 Sn2 I5 90.12(2) . . ? I7 Sn2 I5 91.733(19) . . ? I8 Sn2 I5 175.14(2) . . ? I9 Sn2 I6 95.39(2) . . ? I7 Sn2 I6 170.33(2) . . ? I8 Sn2 I6 93.232(19) . . ? I5 Sn2 I6 82.018(19) . . ? I9 Sn2 I4 165.69(2) . . ? I7 Sn2 I4 92.103(18) . . ? I8 Sn2 I4 102.129(18) . . ? I5 Sn2 I4 76.049(17) . . ? I6 Sn2 I4 79.261(17) . . ? I11 Sn3 I10 89.62(2) . . ? I11 Sn3 I12 92.98(2) . . ? I10 Sn3 I12 93.86(2) . . ? I11 Sn3 I1 89.217(18) . . ? I10 Sn3 I1 87.514(18) . . ? I12 Sn3 I1 177.41(2) . . ? I11 Sn3 I2 168.83(2) . . ? I10 Sn3 I2 95.319(19) . . ? I12 Sn3 I2 96.663(19) . . ? I1 Sn3 I2 81.014(16) . . ? I11 Sn3 I3 90.864(19) . . ? I10 Sn3 I3 168.88(2) . . ? I12 Sn3 I3 97.207(19) . . ? I1 Sn3 I3 81.385(17) . . ? I2 Sn3 I3 82.372(17) . . ? C1 P1 C7 109.8(3) . . ? C1 P1 H1A 109.7 . . ? C7 P1 H1A 109.7 . . ? C1 P1 H1B 109.7 . . ? C7 P1 H1B 109.7 . . ? H1A P1 H1B 108.2 . . ? C13 P2 C19 111.4(3) . . ? C13 P2 H2A 109.3 . . ? C19 P2 H2A 109.3 . . ? C13 P2 H2B 109.3 . . ? C19 P2 H2B 109.3 . . ? H2A P2 H2B 108.0 . . ? C31 P3 C25 110.0(4) . . ? C31 P3 H3A 109.7 . . ? C25 P3 H3A 109.7 . . ? C31 P3 H3B 109.7 . . ? C25 P3 H3B 109.7 . . ? H3A P3 H3B 108.2 . . ? C43 P4 C37 109.7(4) . . ? C43 P4 H4A 109.7 . . ? C37 P4 H4A 109.7 . . ? C43 P4 H4B 109.7 . . ? C37 P4 H4B 109.7 . . ? H4A P4 H4B 108.2 . . ? C49 P5 C55 109.9(4) . . ? C49 P5 H5A 109.7 . . ? C55 P5 H5A 109.7 . . ? C49 P5 H5B 109.7 . . ? C55 P5 H5B 109.7 . . ? H5A P5 H5B 108.2 . . ? C67 P6 C61 112.3(4) . . ? C67 P6 H6A 109.1 . . ? C61 P6 H6A 109.1 . . ? C67 P6 H6B 109.1 . . ? C61 P6 H6B 109.1 . . ? H6A P6 H6B 107.9 . . ? C6 C1 C2 120.5(7) . . ? C6 C1 P1 118.7(6) . . ? C2 C1 P1 120.7(6) . . ? C3 C2 C1 120.1(8) . . ? C3 C2 H2 119.9 . . ? C1 C2 H2 119.9 . . ? C4 C3 C2 120.5(8) . . ? C4 C3 H3 119.7 . . ? C2 C3 H3 119.7 . . ? C3 C4 C5 119.4(8) . . ? C3 C4 H4 120.3 . . ? C5 C4 H4 120.3 . . ? C4 C5 C6 120.7(9) . . ? C4 C5 H5 119.7 . . ? C6 C5 H5 119.7 . . ? C1 C6 C5 118.7(8) . . ? C1 C6 H6 120.7 . . ? C5 C6 H6 120.7 . . ? C12 C7 C8 118.2(9) . . ? C12 C7 P1 118.5(8) . . ? C8 C7 P1 123.2(7) . . ? C7 C8 C9 120.1(10) . . ? C7 C8 H8 119.9 . . ? C9 C8 H8 119.9 . . ? C10 C9 C8 121.5(11) . . ? C10 C9 H9 119.2 . . ? C8 C9 H9 119.2 . . ? C11 C10 C9 118.8(10) . . ? C11 C10 H10 120.6 . . ? C9 C10 H10 120.6 . . ? C10 C11 C12 120.5(13) . . ? C10 C11 H11 119.7 . . ? C12 C11 H11 119.7 . . ? C7 C12 C11 120.6(13) . . ? C7 C12 H12 119.7 . . ? C11 C12 H12 119.7 . . ? C14 C13 C18 119.6(9) . . ? C14 C13 P2 119.9(7) . . ? C18 C13 P2 120.5(9) . . ? C15 C14 C13 118.9(11) . . ? C15 C14 H14 120.6 . . ? C13 C14 H14 120.6 . . ? C16 C15 C14 124.1(14) . . ? C16 C15 H15 117.9 . . ? C14 C15 H15 117.9 . . ? C15 C16 C17 116.5(12) . . ? C15 C16 H16 121.8 . . ? C17 C16 H16 121.8 . . ? C16 C17 C18 123.0(14) . . ? C16 C17 H17 118.5 . . ? C18 C17 H17 118.5 . . ? C13 C18 C17 117.9(13) . . ? C13 C18 H18 121.0 . . ? C17 C18 H18 121.0 . . ? C24 C19 C20 121.9(8) . . ? C24 C19 P2 119.1(6) . . ? C20 C19 P2 119.0(6) . . ? C19 C20 C21 118.5(9) . . ? C19 C20 H20 120.7 . . ? C21 C20 H20 120.7 . . ? C22 C21 C20 120.6(10) . . ? C22 C21 H21 119.7 . . ? C20 C21 H21 119.7 . . ? C21 C22 C23 120.1(9) . . ? C21 C22 H22 120.0 . . ? C23 C22 H22 120.0 . . ? C24 C23 C22 119.9(9) . . ? C24 C23 H23 120.0 . . ? C22 C23 H23 120.0 . . ? C19 C24 C23 119.0(8) . . ? C19 C24 H24 120.5 . . ? C23 C24 H24 120.5 . . ? C26 C25 C30 121.9(7) . . ? C26 C25 P3 119.1(6) . . ? C30 C25 P3 118.9(6) . . ? C25 C26 C27 118.8(7) . . ? C25 C26 H26 120.6 . . ? C27 C26 H26 120.6 . . ? C28 C27 C26 120.7(8) . . ? C28 C27 H27 119.6 . . ? C26 C27 H27 119.6 . . ? C27 C28 C29 119.4(8) . . ? C27 C28 H28 120.3 . . ? C29 C28 H28 120.3 . . ? C30 C29 C28 119.6(8) . . ? C30 C29 H29 120.2 . . ? C28 C29 H29 120.2 . . ? C29 C30 C25 119.6(8) . . ? C29 C30 H30 120.2 . . ? C25 C30 H30 120.2 . . ? C32 C31 C36 119.8(8) . . ? C32 C31 P3 119.7(6) . . ? C36 C31 P3 120.6(7) . . ? C31 C32 C33 119.8(9) . . ? C31 C32 H32 120.1 . . ? C33 C32 H32 120.1 . . ? C34 C33 C32 121.6(10) . . ? C34 C33 H33 119.2 . . ? C32 C33 H33 119.2 . . ? C33 C34 C35 119.5(9) . . ? C33 C34 H34 120.2 . . ? C35 C34 H34 120.2 . . ? C36 C35 C34 119.9(9) . . ? C36 C35 H35 120.1 . . ? C34 C35 H35 120.1 . . ? C31 C36 C35 119.4(9) . . ? C31 C36 H36 120.3 . . ? C35 C36 H36 120.3 . . ? C38A C37 C42 64.2(13) . . ? C38A C37 C38 71.9(13) . . ? C42 C37 C38 119.2(10) . . ? C38A C37 C42A 118.2(19) . . ? C42 C37 C42A 79.6(14) . . ? C38 C37 C42A 86.8(14) . . ? C38A C37 P4 123.9(14) . . ? C42 C37 P4 122.1(8) . . ? C38 C37 P4 116.7(8) . . ? C42A C37 P4 117.6(14) . . ? C39 C38 C37 120.5(12) . . ? C39 C38 H38 119.8 . . ? C37 C38 H38 119.8 . . ? C40 C39 C38 119.4(15) . . ? C40 C39 H39 120.3 . . ? C38 C39 H39 120.3 . . ? C39 C40 C41 122.9(16) . . ? C39 C40 H40 118.6 . . ? C41 C40 H40 118.6 . . ? C40 C41 C42 117.4(14) . . ? C40 C41 H41 121.3 . . ? C42 C41 H41 121.3 . . ? C37 C42 C41 120.4(13) . . ? C37 C42 H42 119.8 . . ? C41 C42 H42 119.8 . . ? C37 C38A C39A 122(3) . . ? C37 C38A H38A 118.9 . . ? C39A C38A H38A 118.9 . . ? C40A C39A C38A 116(3) . . ? C40A C39A H39A 121.8 . . ? C38A C39A H39A 121.8 . . ? C39A C40A C41A 124(3) . . ? C39A C40A H40A 117.9 . . ? C41A C40A H40A 117.9 . . ? C40A C41A C42A 121(4) . . ? C40A C41A H41A 119.3 . . ? C42A C41A H41A 119.3 . . ? C41A C42A C37 117(3) . . ? C41A C42A H42A 121.4 . . ? C37 C42A H42A 121.4 . . ? C44 C43 C48 119.1(8) . . ? C44 C43 P4 119.2(6) . . ? C48 C43 P4 121.4(6) . . ? C43 C44 C45 120.0(8) . . ? C43 C44 H44 120.0 . . ? C45 C44 H44 120.0 . . ? C46 C45 C44 120.1(8) . . ? C46 C45 H45 120.0 . . ? C44 C45 H45 120.0 . . ? C45 C46 C47 120.3(9) . . ? C45 C46 H46 119.9 . . ? C47 C46 H46 119.9 . . ? C48 C47 C46 120.0(8) . . ? C48 C47 H47 120.0 . . ? C46 C47 H47 120.0 . . ? C47 C48 C43 120.5(8) . . ? C47 C48 H48 119.7 . . ? C43 C48 H48 119.7 . . ? C50 C49 C54 120.5(8) . . ? C50 C49 P5 118.9(7) . . ? C54 C49 P5 120.5(7) . . ? C51 C50 C49 121.0(10) . . ? C51 C50 H50 119.5 . . ? C49 C50 H50 119.5 . . ? C52 C51 C50 118.9(11) . . ? C52 C51 H51 120.5 . . ? C50 C51 H51 120.5 . . ? C51 C52 C53 120.9(10) . . ? C51 C52 H52 119.6 . . ? C53 C52 H52 119.6 . . ? C54 C53 C52 119.6(10) . . ? C54 C53 H53 120.2 . . ? C52 C53 H53 120.2 . . ? C53 C54 C49 119.1(10) . . ? C53 C54 H54 120.4 . . ? C49 C54 H54 120.4 . . ? C56 C55 C60 118.5(11) . . ? C56 C55 P5 119.8(8) . . ? C60 C55 P5 121.5(8) . . ? C55 C56 C57 119.0(11) . . ? C55 C56 H56 120.5 . . ? C57 C56 H56 120.5 . . ? C58 C57 C56 122.9(12) . . ? C58 C57 H57 118.5 . . ? C56 C57 H57 118.5 . . ? C59 C58 C57 117.9(11) . . ? C59 C58 H58 121.1 . . ? C57 C58 H58 121.1 . . ? C58 C59 C60 119.8(11) . . ? C58 C59 H59 120.1 . . ? C60 C59 H59 120.1 . . ? C55 C60 C59 121.3(11) . . ? C55 C60 H60 119.4 . . ? C59 C60 H60 119.4 . . ? C66 C61 C62 120.0(8) . . ? C66 C61 P6 120.4(6) . . ? C62 C61 P6 119.6(6) . . ? C63 C62 C61 117.7(8) . . ? C63 C62 H62 121.2 . . ? C61 C62 H62 121.2 . . ? C64 C63 C62 120.2(9) . . ? C64 C63 H63 119.9 . . ? C62 C63 H63 119.9 . . ? C65 C64 C63 121.8(9) . . ? C65 C64 H64 119.1 . . ? C63 C64 H64 119.1 . . ? C64 C65 C66 119.6(9) . . ? C64 C65 H65 120.2 . . ? C66 C65 H65 120.2 . . ? C61 C66 C65 120.7(8) . . ? C61 C66 H66 119.7 . . ? C65 C66 H66 119.7 . . ? C72 C67 C68 119.7(8) . . ? C72 C67 P6 120.5(6) . . ? C68 C67 P6 119.8(6) . . ? C69 C68 C67 119.5(8) . . ? C69 C68 H68 120.2 . . ? C67 C68 H68 120.2 . . ? C68 C69 C70 120.7(9) . . ? C68 C69 H69 119.7 . . ? C70 C69 H69 119.7 . . ? C69 C70 C71 119.7(9) . . ? C69 C70 H70 120.2 . . ? C71 C70 H70 120.2 . . ? C72 C71 C70 119.1(8) . . ? C72 C71 H71 120.5 . . ? C70 C71 H71 120.5 . . ? C67 C72 C71 121.4(8) . . ? C67 C72 H72 119.3 . . ? C71 C72 H72 119.3 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Sn2 I6 Sn1 I4 -44.765(17) . . . . ? Sn2 I6 Sn1 I2 -136.103(18) . . . . ? Sn2 I6 Sn1 I1 -16.6(3) . . . . ? Sn2 I6 Sn1 I5 39.193(17) . . . . ? Sn2 I6 Sn1 I3 133.029(18) . . . . ? Sn2 I4 Sn1 I6 40.940(16) . . . . ? Sn2 I4 Sn1 I2 133.619(18) . . . . ? Sn2 I4 Sn1 I1 -137.259(18) . . . . ? Sn2 I4 Sn1 I5 -44.981(16) . . . . ? Sn2 I4 Sn1 I3 -116.2(2) . . . . ? Sn3 I2 Sn1 I6 -140.701(18) . . . . ? Sn3 I2 Sn1 I4 130.481(18) . . . . ? Sn3 I2 Sn1 I1 42.622(16) . . . . ? Sn3 I2 Sn1 I5 146.9(3) . . . . ? Sn3 I2 Sn1 I3 -44.209(16) . . . . ? Sn3 I1 Sn1 I6 -164.0(3) . . . . ? Sn3 I1 Sn1 I4 -135.820(18) . . . . ? Sn3 I1 Sn1 I2 -44.393(17) . . . . ? Sn3 I1 Sn1 I5 140.380(19) . . . . ? Sn3 I1 Sn1 I3 46.210(16) . . . . ? Sn2 I5 Sn1 I6 -39.425(17) . . . . ? Sn2 I5 Sn1 I4 49.767(17) . . . . ? Sn2 I5 Sn1 I2 33.2(3) . . . . ? Sn2 I5 Sn1 I1 137.416(18) . . . . ? Sn2 I5 Sn1 I3 -135.603(19) . . . . ? Sn3 I3 Sn1 I6 137.301(19) . . . . ? Sn3 I3 Sn1 I4 -65.7(2) . . . . ? Sn3 I3 Sn1 I2 44.512(17) . . . . ? Sn3 I3 Sn1 I1 -44.631(16) . . . . ? Sn3 I3 Sn1 I5 -136.441(19) . . . . ? Sn1 I5 Sn2 I9 133.00(2) . . . . ? Sn1 I5 Sn2 I7 -135.012(19) . . . . ? Sn1 I5 Sn2 I8 25.2(3) . . . . ? Sn1 I5 Sn2 I6 37.574(17) . . . . ? Sn1 I5 Sn2 I4 -43.275(15) . . . . ? Sn1 I6 Sn2 I9 -127.68(2) . . . . ? Sn1 I6 Sn2 I7 11.83(14) . . . . ? Sn1 I6 Sn2 I8 140.646(19) . . . . ? Sn1 I6 Sn2 I5 -38.315(17) . . . . ? Sn1 I6 Sn2 I4 38.905(15) . . . . ? Sn1 I4 Sn2 I9 29.64(9) . . . . ? Sn1 I4 Sn2 I7 136.136(19) . . . . ? Sn1 I4 Sn2 I8 -130.50(2) . . . . ? Sn1 I4 Sn2 I5 44.872(17) . . . . ? Sn1 I4 Sn2 I6 -39.475(16) . . . . ? Sn1 I1 Sn3 I11 -134.773(19) . . . . ? Sn1 I1 Sn3 I10 135.577(19) . . . . ? Sn1 I1 Sn3 I12 13.4(5) . . . . ? Sn1 I1 Sn3 I2 39.791(16) . . . . ? Sn1 I1 Sn3 I3 -43.780(16) . . . . ? Sn1 I2 Sn3 I11 -11.26(12) . . . . ? Sn1 I2 Sn3 I10 -127.17(2) . . . . ? Sn1 I2 Sn3 I12 138.30(2) . . . . ? Sn1 I2 Sn3 I1 -40.538(16) . . . . ? Sn1 I2 Sn3 I3 41.886(16) . . . . ? Sn1 I3 Sn3 I11 131.352(19) . . . . ? Sn1 I3 Sn3 I10 38.94(12) . . . . ? Sn1 I3 Sn3 I12 -135.53(2) . . . . ? Sn1 I3 Sn3 I1 42.275(15) . . . . ? Sn1 I3 Sn3 I2 -39.730(15) . . . . ? C7 P1 C1 C6 91.2(7) . . . . ? C7 P1 C1 C2 -85.0(7) . . . . ? C6 C1 C2 C3 0.4(12) . . . . ? P1 C1 C2 C3 176.5(6) . . . . ? C1 C2 C3 C4 -0.8(13) . . . . ? C2 C3 C4 C5 0.5(13) . . . . ? C3 C4 C5 C6 0.2(14) . . . . ? C2 C1 C6 C5 0.4(12) . . . . ? P1 C1 C6 C5 -175.9(6) . . . . ? C4 C5 C6 C1 -0.7(13) . . . . ? C1 P1 C7 C12 -56.1(13) . . . . ? C1 P1 C7 C8 127.9(9) . . . . ? C12 C7 C8 C9 4.7(19) . . . . ? P1 C7 C8 C9 -179.2(9) . . . . ? C7 C8 C9 C10 -3.1(19) . . . . ? C8 C9 C10 C11 1(2) . . . . ? C9 C10 C11 C12 -1(3) . . . . ? C8 C7 C12 C11 -5(3) . . . . ? P1 C7 C12 C11 179.1(15) . . . . ? C10 C11 C12 C7 3(3) . . . . ? C19 P2 C13 C14 111.8(7) . . . . ? C19 P2 C13 C18 -69.2(8) . . . . ? C18 C13 C14 C15 1.3(12) . . . . ? P2 C13 C14 C15 -179.8(6) . . . . ? C13 C14 C15 C16 -0.4(15) . . . . ? C14 C15 C16 C17 0.1(18) . . . . ? C15 C16 C17 C18 -1(2) . . . . ? C14 C13 C18 C17 -1.8(13) . . . . ? P2 C13 C18 C17 179.3(7) . . . . ? C16 C17 C18 C13 1.6(17) . . . . ? C13 P2 C19 C24 65.4(8) . . . . ? C13 P2 C19 C20 -116.6(7) . . . . ? C24 C19 C20 C21 -0.4(12) . . . . ? P2 C19 C20 C21 -178.3(7) . . . . ? C19 C20 C21 C22 -0.1(14) . . . . ? C20 C21 C22 C23 0.5(15) . . . . ? C21 C22 C23 C24 -0.5(14) . . . . ? C20 C19 C24 C23 0.4(12) . . . . ? P2 C19 C24 C23 178.3(6) . . . . ? C22 C23 C24 C19 0.0(13) . . . . ? C31 P3 C25 C26 127.7(6) . . . . ? C31 P3 C25 C30 -50.7(7) . . . . ? C30 C25 C26 C27 -0.7(12) . . . . ? P3 C25 C26 C27 -179.1(6) . . . . ? C25 C26 C27 C28 0.5(12) . . . . ? C26 C27 C28 C29 0.1(12) . . . . ? C27 C28 C29 C30 -0.6(12) . . . . ? C28 C29 C30 C25 0.4(13) . . . . ? C26 C25 C30 C29 0.3(12) . . . . ? P3 C25 C30 C29 178.7(6) . . . . ? C25 P3 C31 C32 -51.2(8) . . . . ? C25 P3 C31 C36 129.4(7) . . . . ? C36 C31 C32 C33 -1.0(14) . . . . ? P3 C31 C32 C33 179.7(8) . . . . ? C31 C32 C33 C34 0.8(17) . . . . ? C32 C33 C34 C35 0.2(17) . . . . ? C33 C34 C35 C36 -1.0(16) . . . . ? C32 C31 C36 C35 0.1(13) . . . . ? P3 C31 C36 C35 179.5(7) . . . . ? C34 C35 C36 C31 0.9(15) . . . . ? C43 P4 C37 C38A 10.9(15) . . . . ? C43 P4 C37 C42 -67.6(10) . . . . ? C43 P4 C37 C38 96.2(8) . . . . ? C43 P4 C37 C42A -162.7(14) . . . . ? C38A C37 C38 C39 -48.8(18) . . . . ? C42 C37 C38 C39 -4.0(18) . . . . ? C42A C37 C38 C39 72.3(18) . . . . ? P4 C37 C38 C39 -168.3(10) . . . . ? C37 C38 C39 C40 0(2) . . . . ? C38 C39 C40 C41 4(3) . . . . ? C39 C40 C41 C42 -3(3) . . . . ? C38A C37 C42 C41 52.9(18) . . . . ? C38 C37 C42 C41 4.7(18) . . . . ? C42A C37 C42 C41 -75.6(18) . . . . ? P4 C37 C42 C41 168.2(10) . . . . ? C40 C41 C42 C37 -1(2) . . . . ? C42 C37 C38A C39A -68(2) . . . . ? C38 C37 C38A C39A 68(2) . . . . ? C42A C37 C38A C39A -8(3) . . . . ? P4 C37 C38A C39A 178.9(18) . . . . ? C37 C38A C39A C40A 9(4) . . . . ? C38A C39A C40A C41A -5(5) . . . . ? C39A C40A C41A C42A 1(5) . . . . ? C40A C41A C42A C37 0(5) . . . . ? C38A C37 C42A C41A 3(3) . . . . ? C42 C37 C42A C41A 56(3) . . . . ? C38 C37 C42A C41A -64(3) . . . . ? P4 C37 C42A C41A 177(2) . . . . ? C37 P4 C43 C44 -87.6(7) . . . . ? C37 P4 C43 C48 86.4(7) . . . . ? C48 C43 C44 C45 0.2(12) . . . . ? P4 C43 C44 C45 174.4(6) . . . . ? C43 C44 C45 C46 -0.5(13) . . . . ? C44 C45 C46 C47 0.6(13) . . . . ? C45 C46 C47 C48 -0.3(13) . . . . ? C46 C47 C48 C43 0.0(13) . . . . ? C44 C43 C48 C47 0.0(12) . . . . ? P4 C43 C48 C47 -174.0(7) . . . . ? C55 P5 C49 C50 -96.1(8) . . . . ? C55 P5 C49 C54 79.6(8) . . . . ? C54 C49 C50 C51 -0.9(16) . . . . ? P5 C49 C50 C51 174.8(8) . . . . ? C49 C50 C51 C52 -0.4(17) . . . . ? C50 C51 C52 C53 1.4(16) . . . . ? C51 C52 C53 C54 -1.0(15) . . . . ? C52 C53 C54 C49 -0.2(14) . . . . ? C50 C49 C54 C53 1.2(14) . . . . ? P5 C49 C54 C53 -174.5(7) . . . . ? C49 P5 C55 C56 -153.4(11) . . . . ? C49 P5 C55 C60 20.7(11) . . . . ? C60 C55 C56 C57 4(2) . . . . ? P5 C55 C56 C57 178.7(13) . . . . ? C55 C56 C57 C58 2(3) . . . . ? C56 C57 C58 C59 -6(3) . . . . ? C57 C58 C59 C60 2(2) . . . . ? C56 C55 C60 C59 -8(2) . . . . ? P5 C55 C60 C59 177.9(11) . . . . ? C58 C59 C60 C55 4(2) . . . . ? C67 P6 C61 C66 -121.5(7) . . . . ? C67 P6 C61 C62 58.9(7) . . . . ? C66 C61 C62 C63 -0.4(12) . . . . ? P6 C61 C62 C63 179.2(6) . . . . ? C61 C62 C63 C64 -0.4(12) . . . . ? C62 C63 C64 C65 0.2(14) . . . . ? C63 C64 C65 C66 0.9(14) . . . . ? C62 C61 C66 C65 1.4(12) . . . . ? P6 C61 C66 C65 -178.2(6) . . . . ? C64 C65 C66 C61 -1.7(13) . . . . ? C61 P6 C67 C72 -126.2(6) . . . . ? C61 P6 C67 C68 55.1(8) . . . . ? C72 C67 C68 C69 1.0(12) . . . . ? P6 C67 C68 C69 179.7(7) . . . . ? C67 C68 C69 C70 -0.5(13) . . . . ? C68 C69 C70 C71 0.5(14) . . . . ? C69 C70 C71 C72 -1.1(13) . . . . ? C68 C67 C72 C71 -1.7(12) . . . . ? P6 C67 C72 C71 179.7(6) . . . . ? C70 C71 C72 C67 1.7(13) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A P1 H1A I4 1.36 2.98 4.170(2) 145.7 5_576 P1 H1B I7 1.36 2.82 3.981(2) 142.4 . P2 H2A I4 1.36 2.72 4.046(2) 163.5 6_575 P2 H2B I10 1.36 2.76 3.989(2) 149.6 6_575 P3 H3A I12 1.36 2.99 4.139(2) 140.9 . P4 H4B I8 1.36 3.02 4.334(2) 161.4 6_576 P3 H3B I3 1.36 2.96 4.212(2) 152.5 7_566 P4 H4A I7 1.36 2.94 4.051(2) 138.1 . P5 H5A I3 1.36 2.82 4.119(2) 158.3 . P5 H5B I9 1.36 2.88 4.169(3) 156.9 . P6 H6B I1 1.36 3.11 3.584(2) 99.0 . P6 H6B I11 1.36 2.88 4.204(2) 163.1 . P6 H6B I10 1.36 3.27 3.761(2) 100.3 . P6 H6B I1 1.36 3.11 3.584(2) 99.0 . _diffrn_measured_fraction_theta_max 0.976 _diffrn_reflns_theta_full 27.52 _diffrn_measured_fraction_theta_full 0.976 _refine_diff_density_max 1.047 _refine_diff_density_min -1.437 _refine_diff_density_rms 0.237 #===end data_h02kcm4 _database_code_depnum_ccdc_archive 'CCDC 741173' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C26 H28 Cl4 I6 P2 Sn' _chemical_formula_weight 1424.31 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' 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' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 8.1060(2) _cell_length_b 14.9990(4) _cell_length_c 16.3210(5) _cell_angle_alpha 90.00 _cell_angle_beta 92.224(1) _cell_angle_gamma 90.00 _cell_volume 1982.84(9) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 20159 _cell_measurement_theta_min 2.910 _cell_measurement_theta_max 27.485 _exptl_crystal_description needle _exptl_crystal_colour 'dark red' _exptl_crystal_size_max 0.08 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.386 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1300 _exptl_absorpt_coefficient_mu 5.683 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6684 _exptl_absorpt_correction_T_max 0.7566 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements Sortav (Blessing 1995) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator 'horizonally mounted graphite crystal' _diffrn_measurement_device_type '95mm CCD camera on \k-goniostat' _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 37579 _diffrn_reflns_av_R_equivalents 0.1419 _diffrn_reflns_av_sigmaI/netI 0.0931 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 3.69 _diffrn_reflns_theta_max 27.46 _reflns_number_total 4528 _reflns_number_gt 2741 _reflns_threshold_expression >2\s(I) _computing_data_collection 'Collect (Bruker AXS BV 1997-2004)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'Denzo & Scalepack (Otwinowski, Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick 1990)' _computing_structure_refinement 'SHELXL-97/2 (Sheldrick 1997)' _computing_molecular_graphics 'ORTEX (P.McArdle 1995)' _computing_publication_material 'SHELXL-97/2 (Sheldrick 1997)' _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^ > 2\s(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^)+(0.0360P)^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 4528 _refine_ls_number_parameters 178 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1017 _refine_ls_R_factor_gt 0.0425 _refine_ls_wR_factor_ref 0.0869 _refine_ls_wR_factor_gt 0.0740 _refine_ls_goodness_of_fit_ref 0.953 _refine_ls_restrained_S_all 0.953 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Sn1 Sn 0.5000 0.5000 0.5000 0.02413(17) Uani 1 2 d S . . I1 I 0.47241(6) 0.31112(3) 0.51913(3) 0.03221(14) Uani 1 1 d . . . I2 I 0.70607(5) 0.47579(3) 0.36464(3) 0.02996(14) Uani 1 1 d . . . I3 I 0.21114(5) 0.49999(3) 0.39254(3) 0.02895(13) Uani 1 1 d . . . P1 P -0.0166(2) 0.30021(13) 0.50992(13) 0.0327(5) Uani 1 1 d . . . H1A H 0.1042 0.3632 0.5122 0.039 Uiso 1 1 calc R . . H1B H -0.1607 0.3409 0.4865 0.039 Uiso 1 1 calc R . . C1 C 0.0310(9) 0.2178(5) 0.4354(5) 0.0352(18) Uani 1 1 d . . . C2 C -0.0070(9) 0.2350(5) 0.3532(5) 0.042(2) Uani 1 1 d . . . H2 H -0.0567 0.2900 0.3375 0.050 Uiso 1 1 calc R . . C3 C 0.0270(11) 0.1727(6) 0.2946(5) 0.053(2) Uani 1 1 d . . . H3 H 0.0036 0.1859 0.2384 0.063 Uiso 1 1 calc R . . C4 C 0.0933(11) 0.0931(6) 0.3156(6) 0.056(3) Uani 1 1 d . . . H4 H 0.1146 0.0499 0.2748 0.067 Uiso 1 1 calc R . . C5 C 0.1305(11) 0.0748(6) 0.3985(6) 0.059(3) Uani 1 1 d . . . H5 H 0.1772 0.0188 0.4137 0.071 Uiso 1 1 calc R . . C6 C 0.1001(10) 0.1371(5) 0.4582(6) 0.050(2) Uani 1 1 d . . . H6 H 0.1265 0.1245 0.5143 0.060 Uiso 1 1 calc R . . C7 C -0.0352(8) 0.2557(4) 0.6093(5) 0.0279(16) Uani 1 1 d . . . C8 C -0.1592(9) 0.1942(5) 0.6257(5) 0.0369(19) Uani 1 1 d . . . H8 H -0.2304 0.1728 0.5824 0.044 Uiso 1 1 calc R . . C9 C -0.1778(9) 0.1651(5) 0.7039(5) 0.039(2) Uani 1 1 d . . . H9 H -0.2610 0.1225 0.7146 0.047 Uiso 1 1 calc R . . C10 C -0.0779(9) 0.1963(5) 0.7672(5) 0.039(2) Uani 1 1 d . . . H10 H -0.0951 0.1769 0.8216 0.047 Uiso 1 1 calc R . . C11 C 0.0499(10) 0.2568(5) 0.7522(5) 0.041(2) Uani 1 1 d . . . H11 H 0.1216 0.2770 0.7958 0.049 Uiso 1 1 calc R . . C12 C 0.0687(9) 0.2861(5) 0.6737(5) 0.0380(19) Uani 1 1 d . . . H12 H 0.1536 0.3276 0.6629 0.046 Uiso 1 1 calc R . . C13 C 0.3765(17) -0.0185(6) 0.6586(7) 0.082(4) Uani 1 1 d . . . H13A H 0.4667 -0.0388 0.6968 0.098 Uiso 1 1 calc R . . H13B H 0.2707 -0.0315 0.6845 0.098 Uiso 1 1 calc R . . Cl1 Cl 0.3932(3) 0.09566(15) 0.64633(17) 0.0660(7) Uani 1 1 d . . . Cl2 Cl 0.3846(4) -0.07924(19) 0.56949(18) 0.0842(9) 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 0.0238(3) 0.0257(4) 0.0229(4) 0.0010(3) 0.0010(3) 0.0003(3) I1 0.0365(3) 0.0254(2) 0.0346(3) 0.0028(2) 0.0014(2) -0.0002(2) I2 0.0295(2) 0.0353(3) 0.0253(3) 0.0012(2) 0.0045(2) 0.0006(2) I3 0.0276(2) 0.0334(3) 0.0255(3) 0.0003(2) -0.00241(19) 0.0012(2) P1 0.0380(10) 0.0318(10) 0.0284(12) 0.0019(9) 0.0049(9) 0.0055(9) C1 0.034(4) 0.037(4) 0.035(5) -0.001(4) 0.003(4) 0.000(3) C2 0.046(5) 0.044(5) 0.036(5) 0.001(4) 0.002(4) 0.001(4) C3 0.066(6) 0.068(6) 0.024(5) -0.001(5) 0.001(4) -0.007(5) C4 0.059(6) 0.072(7) 0.037(6) -0.022(5) 0.009(5) 0.008(5) C5 0.073(6) 0.047(5) 0.056(7) -0.012(5) -0.001(5) 0.026(5) C6 0.073(6) 0.040(5) 0.036(6) -0.010(4) -0.014(5) 0.022(4) C7 0.038(4) 0.024(4) 0.022(4) 0.000(3) 0.001(3) 0.003(3) C8 0.039(4) 0.036(4) 0.035(5) 0.004(4) 0.000(4) -0.010(3) C9 0.035(4) 0.041(5) 0.041(6) 0.012(4) -0.002(4) -0.005(4) C10 0.042(4) 0.045(5) 0.031(5) 0.016(4) -0.003(4) 0.001(4) C11 0.052(5) 0.038(5) 0.032(5) -0.007(4) -0.010(4) 0.001(4) C12 0.045(4) 0.039(5) 0.029(5) 0.003(4) -0.001(4) -0.014(4) C13 0.152(11) 0.053(6) 0.042(7) -0.012(5) 0.015(7) 0.006(6) Cl1 0.0800(16) 0.0483(14) 0.0685(19) 0.0018(12) -0.0115(14) -0.0077(12) Cl2 0.130(2) 0.0719(18) 0.0509(18) -0.0115(14) 0.0068(17) -0.0147(16) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 I2 2.8442(5) . ? Sn1 I2 2.8442(5) 3_666 ? Sn1 I1 2.8599(5) . ? Sn1 I1 2.8599(5) 3_666 ? Sn1 I3 2.8706(4) . ? Sn1 I3 2.8706(5) 3_666 ? P1 C7 1.766(7) . ? P1 C1 1.787(8) . ? P1 H1A 1.3600 . ? P1 H1B 1.3600 . ? C1 C6 1.379(10) . ? C1 C2 1.389(11) . ? C2 C3 1.373(11) . ? C2 H2 0.9500 . ? C3 C4 1.349(12) . ? C3 H3 0.9500 . ? C4 C5 1.401(13) . ? C4 H4 0.9500 . ? C5 C6 1.380(12) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C7 C12 1.398(10) . ? C7 C8 1.398(9) . ? C8 C9 1.363(11) . ? C8 H8 0.9500 . ? C9 C10 1.370(11) . ? C9 H9 0.9500 . ? C10 C11 1.405(10) . ? C10 H10 0.9500 . ? C11 C12 1.368(11) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? C13 Cl2 1.720(10) . ? C13 Cl1 1.730(9) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag I2 Sn1 I2 180.0 . 3_666 ? I2 Sn1 I1 90.524(13) . . ? I2 Sn1 I1 89.476(14) 3_666 . ? I2 Sn1 I1 89.476(14) . 3_666 ? I2 Sn1 I1 90.524(13) 3_666 3_666 ? I1 Sn1 I1 180.0 . 3_666 ? I2 Sn1 I3 90.868(13) . . ? I2 Sn1 I3 89.132(13) 3_666 . ? I1 Sn1 I3 90.072(13) . . ? I1 Sn1 I3 89.928(13) 3_666 . ? I2 Sn1 I3 89.132(13) . 3_666 ? I2 Sn1 I3 90.868(13) 3_666 3_666 ? I1 Sn1 I3 89.928(13) . 3_666 ? I1 Sn1 I3 90.072(13) 3_666 3_666 ? I3 Sn1 I3 180.0 . 3_666 ? C7 P1 C1 113.1(4) . . ? C7 P1 H1A 109.0 . . ? C1 P1 H1A 109.0 . . ? C7 P1 H1B 109.0 . . ? C1 P1 H1B 109.0 . . ? H1A P1 H1B 107.8 . . ? C6 C1 C2 119.8(8) . . ? C6 C1 P1 121.3(6) . . ? C2 C1 P1 118.9(6) . . ? C3 C2 C1 120.3(8) . . ? C3 C2 H2 119.9 . . ? C1 C2 H2 119.9 . . ? C4 C3 C2 120.9(9) . . ? C4 C3 H3 119.5 . . ? C2 C3 H3 119.5 . . ? C3 C4 C5 119.2(8) . . ? C3 C4 H4 120.4 . . ? C5 C4 H4 120.4 . . ? C6 C5 C4 120.8(8) . . ? C6 C5 H5 119.6 . . ? C4 C5 H5 119.6 . . ? C5 C6 C1 119.0(8) . . ? C5 C6 H6 120.5 . . ? C1 C6 H6 120.5 . . ? C12 C7 C8 119.3(7) . . ? C12 C7 P1 119.8(5) . . ? C8 C7 P1 120.8(6) . . ? C9 C8 C7 119.7(7) . . ? C9 C8 H8 120.1 . . ? C7 C8 H8 120.1 . . ? C8 C9 C10 120.9(7) . . ? C8 C9 H9 119.6 . . ? C10 C9 H9 119.6 . . ? C9 C10 C11 120.5(8) . . ? C9 C10 H10 119.7 . . ? C11 C10 H10 119.7 . . ? C12 C11 C10 118.6(7) . . ? C12 C11 H11 120.7 . . ? C10 C11 H11 120.7 . . ? C11 C12 C7 120.9(7) . . ? C11 C12 H12 119.6 . . ? C7 C12 H12 119.6 . . ? Cl2 C13 Cl1 114.9(6) . . ? Cl2 C13 H13A 108.5 . . ? Cl1 C13 H13A 108.5 . . ? Cl2 C13 H13B 108.5 . . ? Cl1 C13 H13B 108.5 . . ? H13A C13 H13B 107.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C7 P1 C1 C6 -20.7(8) . . . . ? C7 P1 C1 C2 157.6(6) . . . . ? C6 C1 C2 C3 -1.3(12) . . . . ? P1 C1 C2 C3 -179.6(6) . . . . ? C1 C2 C3 C4 1.9(13) . . . . ? C2 C3 C4 C5 -1.2(14) . . . . ? C3 C4 C5 C6 0.0(15) . . . . ? C4 C5 C6 C1 0.6(14) . . . . ? C2 C1 C6 C5 0.1(12) . . . . ? P1 C1 C6 C5 178.3(7) . . . . ? C1 P1 C7 C12 120.3(6) . . . . ? C1 P1 C7 C8 -63.6(7) . . . . ? C12 C7 C8 C9 0.3(11) . . . . ? P1 C7 C8 C9 -175.8(6) . . . . ? C7 C8 C9 C10 1.0(12) . . . . ? C8 C9 C10 C11 -2.3(12) . . . . ? C9 C10 C11 C12 2.2(11) . . . . ? C10 C11 C12 C7 -0.8(11) . . . . ? C8 C7 C12 C11 -0.4(11) . . . . ? P1 C7 C12 C11 175.8(6) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.46 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.131 _refine_diff_density_min -1.514 _refine_diff_density_rms 0.222 #===end data_k02kcm28 _database_code_depnum_ccdc_archive 'CCDC 741174' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C12 H28 I4 P2 Sn' _chemical_formula_weight 860.57 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' I I -0.4742 1.8119 '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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' '-x-1/2, y-1/2, z' 'x, -y-1/2, z-1/2' _cell_length_a 9.0343(2) _cell_length_b 8.7669(2) _cell_length_c 28.6850(8) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2271.93(10) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 61519 _cell_measurement_theta_min 2.910 _cell_measurement_theta_max 27.485 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.516 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1568 _exptl_absorpt_coefficient_mu 6.691 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.2027 _exptl_absorpt_correction_T_max 0.5853 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements Sortav (Blessing 1995) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator 'horizonally mounted graphite crystal' _diffrn_measurement_device_type '95mm CCD camera on \k-goniostat' _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 27736 _diffrn_reflns_av_R_equivalents 0.0991 _diffrn_reflns_av_sigmaI/netI 0.0413 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -37 _diffrn_reflns_limit_l_max 37 _diffrn_reflns_theta_min 3.54 _diffrn_reflns_theta_max 27.51 _reflns_number_total 2572 _reflns_number_gt 2138 _reflns_threshold_expression >2\s(I) _computing_data_collection 'Collect (Bruker AXS BV 1997-2004)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'Denzo & Scalepack (Otwinowski, Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick 1990)' _computing_structure_refinement 'SHELXL-97/2 (Sheldrick 1997)' _computing_molecular_graphics 'ORTEX (P.McArdle 1995)' _computing_publication_material 'SHELXL-97/2 (Sheldrick 1997)' _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^ > 2\s(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^)+(0.0512P)^2^+2.3586P] 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 2572 _refine_ls_number_parameters 89 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0498 _refine_ls_R_factor_gt 0.0361 _refine_ls_wR_factor_ref 0.0926 _refine_ls_wR_factor_gt 0.0858 _refine_ls_goodness_of_fit_ref 1.076 _refine_ls_restrained_S_all 1.076 _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 Sn Sn 0.5000 0.5000 0.5000 0.01997(14) Uani 1 2 d S . . I1 I 0.47000(5) 0.47613(4) 0.391939(12) 0.02754(13) Uani 1 1 d . . . I2 I 0.78352(4) 0.28393(4) 0.489036(13) 0.02421(13) Uani 1 1 d . . . P1 P 0.95463(18) 0.47155(17) 0.58651(5) 0.0249(3) Uani 1 1 d . . . H1A H 0.8603 0.3586 0.5997 0.037 Uiso 1 1 calc R . . H1B H 1.0656 0.4114 0.5603 0.037 Uiso 1 1 calc R . . H1C H 0.8798 0.5772 0.5610 0.037 Uiso 1 1 calc R . . C1 C 1.0319(6) 0.5609(7) 0.63760(19) 0.0237(12) Uani 1 1 d . . . H1 H 1.0969 0.6466 0.6271 0.028 Uiso 1 1 calc R . . C2 C 1.1285(6) 0.4470(7) 0.6658(2) 0.0276(12) Uani 1 1 d . . . H2A H 1.0670 0.3603 0.6765 0.033 Uiso 1 1 calc R . . H2B H 1.2085 0.4064 0.6458 0.033 Uiso 1 1 calc R . . C6 C 0.9098(6) 0.6278(6) 0.66882(19) 0.0247(12) Uani 1 1 d . . . H6A H 0.8492 0.7006 0.6506 0.030 Uiso 1 1 calc R . . H6B H 0.8443 0.5449 0.6799 0.030 Uiso 1 1 calc R . . C5 C 0.9783(7) 0.7101(7) 0.71076(19) 0.0268(13) Uani 1 1 d . . . H5A H 1.0365 0.7987 0.6997 0.032 Uiso 1 1 calc R . . H5B H 0.8984 0.7486 0.7313 0.032 Uiso 1 1 calc R . . C3 C 1.1955(6) 0.5289(7) 0.7079(2) 0.0289(13) Uani 1 1 d . . . H3A H 1.2517 0.4544 0.7269 0.035 Uiso 1 1 calc R . . H3B H 1.2658 0.6076 0.6969 0.035 Uiso 1 1 calc R . . C4 C 1.0778(7) 0.6040(7) 0.73827(19) 0.0305(13) Uani 1 1 d . . . H4A H 1.0166 0.5238 0.7530 0.037 Uiso 1 1 calc R . . H4B H 1.1269 0.6625 0.7634 0.037 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 Sn 0.0156(3) 0.0190(3) 0.0253(3) 0.00017(19) -0.0003(2) -0.0002(2) I1 0.0262(3) 0.0314(2) 0.0250(2) 0.00280(14) 0.00026(14) -0.00175(16) I2 0.0202(2) 0.0219(2) 0.0306(2) -0.00084(13) -0.00268(14) 0.00297(14) P1 0.0232(9) 0.0245(8) 0.0270(8) -0.0016(5) 0.0004(6) -0.0008(6) C1 0.018(3) 0.026(3) 0.027(3) 0.001(2) -0.001(2) -0.007(2) C2 0.017(3) 0.034(3) 0.032(3) -0.001(2) 0.000(2) 0.001(2) C6 0.024(3) 0.019(3) 0.031(3) -0.004(2) -0.002(2) 0.003(2) C5 0.024(3) 0.030(3) 0.027(3) -0.004(2) 0.001(2) 0.001(2) C3 0.017(3) 0.038(3) 0.032(3) 0.002(2) -0.001(2) 0.001(2) C4 0.027(3) 0.041(3) 0.023(3) 0.002(2) -0.001(2) -0.006(3) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 Sn I1 3.1186(4) . ? Sn I1 3.1186(4) 5_666 ? Sn I2 3.1812(4) 3_456 ? Sn I2 3.1812(4) 7_765 ? Sn I2 3.2012(4) 5_666 ? Sn I2 3.2012(4) . ? I2 Sn 3.1812(4) 3_556 ? P1 C1 1.802(6) . ? P1 H1A 1.3600 . ? P1 H1B 1.3600 . ? P1 H1C 1.3600 . ? C1 C6 1.537(8) . ? C1 C2 1.553(8) . ? C1 H1 1.0000 . ? C2 C3 1.530(8) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C6 C5 1.533(7) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C5 C4 1.515(8) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C3 C4 1.524(8) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag I1 Sn I1 180.0 . 5_666 ? I1 Sn I2 89.561(10) . 3_456 ? I1 Sn I2 90.439(10) 5_666 3_456 ? I1 Sn I2 90.439(10) . 7_765 ? I1 Sn I2 89.561(10) 5_666 7_765 ? I2 Sn I2 180.0 3_456 7_765 ? I1 Sn I2 93.889(10) . 5_666 ? I1 Sn I2 86.111(10) 5_666 5_666 ? I2 Sn I2 87.787(3) 3_456 5_666 ? I2 Sn I2 92.213(3) 7_765 5_666 ? I1 Sn I2 86.111(10) . . ? I1 Sn I2 93.889(10) 5_666 . ? I2 Sn I2 92.213(3) 3_456 . ? I2 Sn I2 87.787(3) 7_765 . ? I2 Sn I2 180.0 5_666 . ? Sn I2 Sn 160.946(13) 3_556 . ? C1 P1 H1A 109.5 . . ? C1 P1 H1B 109.5 . . ? H1A P1 H1B 109.5 . . ? C1 P1 H1C 109.5 . . ? H1A P1 H1C 109.5 . . ? H1B P1 H1C 109.5 . . ? C6 C1 C2 110.2(5) . . ? C6 C1 P1 111.2(4) . . ? C2 C1 P1 111.2(4) . . ? C6 C1 H1 108.0 . . ? C2 C1 H1 108.0 . . ? P1 C1 H1 108.0 . . ? C3 C2 C1 109.4(5) . . ? C3 C2 H2A 109.8 . . ? C1 C2 H2A 109.8 . . ? C3 C2 H2B 109.8 . . ? C1 C2 H2B 109.8 . . ? H2A C2 H2B 108.2 . . ? C5 C6 C1 110.4(5) . . ? C5 C6 H6A 109.6 . . ? C1 C6 H6A 109.6 . . ? C5 C6 H6B 109.6 . . ? C1 C6 H6B 109.6 . . ? H6A C6 H6B 108.1 . . ? C4 C5 C6 111.1(5) . . ? C4 C5 H5A 109.4 . . ? C6 C5 H5A 109.4 . . ? C4 C5 H5B 109.4 . . ? C6 C5 H5B 109.4 . . ? H5A C5 H5B 108.0 . . ? C4 C3 C2 112.2(5) . . ? C4 C3 H3A 109.2 . . ? C2 C3 H3A 109.2 . . ? C4 C3 H3B 109.2 . . ? C2 C3 H3B 109.2 . . ? H3A C3 H3B 107.9 . . ? C5 C4 C3 112.5(5) . . ? C5 C4 H4A 109.1 . . ? C3 C4 H4A 109.1 . . ? C5 C4 H4B 109.1 . . ? C3 C4 H4B 109.1 . . ? H4A C4 H4B 107.8 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag I1 Sn I2 Sn -120.09(4) . . . 3_556 ? I1 Sn I2 Sn 59.91(4) 5_666 . . 3_556 ? I2 Sn I2 Sn -30.68(3) 3_456 . . 3_556 ? I2 Sn I2 Sn 149.32(3) 7_765 . . 3_556 ? I2 Sn I2 Sn 71(55) 5_666 . . 3_556 ? C6 C1 C2 C3 -57.9(6) . . . . ? P1 C1 C2 C3 178.3(4) . . . . ? C2 C1 C6 C5 59.0(6) . . . . ? P1 C1 C6 C5 -177.2(4) . . . . ? C1 C6 C5 C4 -56.6(6) . . . . ? C1 C2 C3 C4 55.2(6) . . . . ? C6 C5 C4 C3 53.9(7) . . . . ? C2 C3 C4 C5 -54.0(7) . . . . ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 27.51 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 0.914 _refine_diff_density_min -1.269 _refine_diff_density_rms 0.232 #===end # Attachment 'Allcifs.cif' data_k03kcm13 _database_code_depnum_ccdc_archive 'CCDC 741175' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C18 H33 I P, I3 Sn' _chemical_formula_sum 'C18 H33 I4 P Sn' _chemical_formula_weight 906.70 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' 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' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/n 1' 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 10.928(5) _cell_length_b 13.013(5) _cell_length_c 18.512(5) _cell_angle_alpha 90.000 _cell_angle_beta 101.258(5) _cell_angle_gamma 90.000 _cell_volume 2581.9(17) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 18899 _cell_measurement_theta_min 2.910 _cell_measurement_theta_max 30.034 _exptl_crystal_description 'irregular shape' _exptl_crystal_colour colourless _exptl_crystal_size_max 0.55 _exptl_crystal_size_mid 0.50 _exptl_crystal_size_min 0.40 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.333 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1672 _exptl_absorpt_coefficient_mu 5.836 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.0612 _exptl_absorpt_correction_T_max 0.0977 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements Sortav (Blessing 1995) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 'Nonius Kappa CCD' _diffrn_measurement_method '211 1.8 degree images with \f and\w scans' _diffrn_standards_number 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 22566 _diffrn_reflns_av_R_equivalents 0.0719 _diffrn_reflns_av_sigmaI/netI 0.0448 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 3.07 _diffrn_reflns_theta_max 30.08 _reflns_number_total 7359 _reflns_number_gt 6835 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinski & Minor, 1997)' _computing_data_reduction ; DENZO-SCALEPACK Z. Otwinowski and W. Minor, " Processing of X-ray Diffraction Data Collected in Oscillation Mode ", Methods in Enzymology, Volume 276: Macromolecular Crystallography, part A, p.307-326, 1997,C.W. Carter, Jr. & R. M. Sweet, Eds., Academic Press. ; _computing_structure_solution ; SIR97- Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C. , Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R. (1999) J. Appl. Cryst. 32, 115-119 ; _computing_structure_refinement ; SHELXL97 -Program for Crystal Structure Analysis (Release 97-2). Sheldrick, G.M., Instit\"ut f\"ur Anorganische Chemie der Universit\"at, Tammanstrasse 4, D-3400 G\"ottingen, Germany, 1998 ; _computing_molecular_graphics 'ORTEP3 for Windows - Farrugia, L. J. J. Appl. Crystallogr. 1997, 30, 565' _computing_publication_material ; 'WinGX publication routines, Farrugia, L. J., J. Appl. Crystallogr., 1999, 32, 837-838 ; _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^)+(0.0626P)^2^+9.5444P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0052(2) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 7359 _refine_ls_number_parameters 218 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0494 _refine_ls_R_factor_gt 0.0459 _refine_ls_wR_factor_ref 0.1229 _refine_ls_wR_factor_gt 0.1202 _refine_ls_goodness_of_fit_ref 1.129 _refine_ls_restrained_S_all 1.129 _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 Sn Sn 0.30974(3) 0.27464(3) 0.675984(17) 0.02426(10) Uani 1 1 d . . . I1 I 0.91168(3) 0.24853(2) 0.383553(15) 0.01983(9) Uani 1 1 d . . . I2 I 0.57116(3) 0.25205(3) 0.733371(17) 0.02469(10) Uani 1 1 d . . . I3 I 0.24776(4) 0.06201(3) 0.66945(2) 0.03511(11) Uani 1 1 d . . . I4 I 0.32532(3) 0.30004(3) 0.524708(17) 0.03228(11) Uani 1 1 d . . . P P 0.77549(10) 0.26274(8) 0.47035(6) 0.0146(2) Uani 1 1 d . . . C1 C 0.8388(4) 0.3642(3) 0.5364(2) 0.0172(7) Uani 1 1 d . . . H1 H 0.8231 0.4306 0.5088 0.021 Uiso 1 1 calc R . . C2 C 0.9808(4) 0.3583(4) 0.5644(3) 0.0205(8) Uani 1 1 d . . . H2A H 1.0021 0.2961 0.5949 0.025 Uiso 1 1 calc R . . H2B H 1.0241 0.3547 0.5222 0.025 Uiso 1 1 calc R . . C3 C 1.0217(5) 0.4543(4) 0.6100(3) 0.0236(9) Uani 1 1 d . . . H3A H 1.1129 0.4516 0.6286 0.028 Uiso 1 1 calc R . . H3B H 1.0034 0.5159 0.5783 0.028 Uiso 1 1 calc R . . C4 C 0.9556(5) 0.4635(4) 0.6745(3) 0.0276(10) Uani 1 1 d . . . H4A H 0.9818 0.5278 0.7017 0.033 Uiso 1 1 calc R . . H4B H 0.9798 0.4051 0.7086 0.033 Uiso 1 1 calc R . . C5 C 0.8149(5) 0.4639(4) 0.6483(3) 0.0284(10) Uani 1 1 d . . . H5A H 0.7900 0.5277 0.6201 0.034 Uiso 1 1 calc R . . H5B H 0.7742 0.4638 0.6916 0.034 Uiso 1 1 calc R . . C6 C 0.7690(5) 0.3717(4) 0.6000(2) 0.0231(9) Uani 1 1 d . . . H6A H 0.6785 0.3787 0.5802 0.028 Uiso 1 1 calc R . . H6B H 0.7824 0.3081 0.6298 0.028 Uiso 1 1 calc R . . C7 C 0.7631(4) 0.1353(3) 0.5092(2) 0.0166(7) Uani 1 1 d . . . H7 H 0.7482 0.0865 0.4667 0.020 Uiso 1 1 calc R . . C8 C 0.6507(4) 0.1239(4) 0.5476(2) 0.0211(8) Uani 1 1 d . . . H8A H 0.6623 0.1682 0.5919 0.025 Uiso 1 1 calc R . . H8B H 0.5733 0.1455 0.5138 0.025 Uiso 1 1 calc R . . C9 C 0.6400(5) 0.0117(4) 0.5696(3) 0.0279(10) Uani 1 1 d . . . H9A H 0.5701 0.0045 0.5962 0.033 Uiso 1 1 calc R . . H9B H 0.6208 -0.0312 0.5246 0.033 Uiso 1 1 calc R . . C10 C 0.7594(5) -0.0272(4) 0.6185(3) 0.0323(12) Uani 1 1 d . . . H10A H 0.7736 0.0101 0.6660 0.039 Uiso 1 1 calc R . . H10B H 0.7504 -0.1012 0.6288 0.039 Uiso 1 1 calc R . . C11 C 0.8707(5) -0.0120(4) 0.5820(3) 0.0303(10) Uani 1 1 d . . . H11A H 0.8610 -0.0560 0.5376 0.036 Uiso 1 1 calc R . . H11B H 0.9474 -0.0337 0.6164 0.036 Uiso 1 1 calc R . . C12 C 0.8845(4) 0.1002(4) 0.5598(3) 0.0246(9) Uani 1 1 d . . . H12A H 0.9551 0.1068 0.5338 0.030 Uiso 1 1 calc R . . H12B H 0.9020 0.1441 0.6043 0.030 Uiso 1 1 calc R . . C13 C 0.6240(4) 0.3028(3) 0.4188(2) 0.0166(7) Uani 1 1 d . . . H13 H 0.5682 0.3120 0.4552 0.020 Uiso 1 1 calc R . . C14 C 0.5639(5) 0.2188(4) 0.3636(2) 0.0224(8) Uani 1 1 d . . . H14A H 0.6163 0.2069 0.3265 0.027 Uiso 1 1 calc R . . H14B H 0.5581 0.1534 0.3902 0.027 Uiso 1 1 calc R . . C15 C 0.4337(5) 0.2534(4) 0.3256(3) 0.0243(9) Uani 1 1 d . . . H15A H 0.3966 0.2009 0.2891 0.029 Uiso 1 1 calc R . . H15B H 0.3798 0.2596 0.3626 0.029 Uiso 1 1 calc R . . C16 C 0.4379(5) 0.3562(5) 0.2868(3) 0.0333(12) Uani 1 1 d . . . H16A H 0.4861 0.3488 0.2470 0.040 Uiso 1 1 calc R . . H16B H 0.3521 0.3777 0.2641 0.040 Uiso 1 1 calc R . . C17 C 0.4978(6) 0.4377(4) 0.3406(4) 0.0358(12) Uani 1 1 d . . . H17A H 0.4450 0.4496 0.3776 0.043 Uiso 1 1 calc R . . H17B H 0.5026 0.5030 0.3138 0.043 Uiso 1 1 calc R . . C18 C 0.6294(5) 0.4065(4) 0.3801(3) 0.0269(10) Uani 1 1 d . . . H18A H 0.6850 0.4010 0.3440 0.032 Uiso 1 1 calc R . . H18B H 0.6638 0.4595 0.4168 0.032 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 Sn 0.02260(17) 0.03401(19) 0.01655(15) -0.00052(11) 0.00475(11) 0.00641(13) I1 0.02031(16) 0.02583(17) 0.01517(14) -0.00127(9) 0.00790(10) 0.00117(10) I2 0.02034(17) 0.03729(19) 0.01747(15) 0.00177(10) 0.00622(11) -0.00255(11) I3 0.0336(2) 0.0409(2) 0.02947(18) -0.00396(13) 0.00285(14) -0.00893(14) I4 0.03174(19) 0.0486(2) 0.01773(15) 0.00424(13) 0.00795(12) 0.00854(15) P 0.0145(5) 0.0188(5) 0.0107(4) 0.0006(3) 0.0027(3) 0.0002(4) C1 0.0182(18) 0.0183(18) 0.0149(16) -0.0015(14) 0.0025(14) -0.0025(14) C2 0.0131(17) 0.025(2) 0.0234(19) -0.0033(16) 0.0023(14) -0.0016(15) C3 0.022(2) 0.029(2) 0.0194(19) -0.0030(16) 0.0009(16) -0.0052(17) C4 0.028(2) 0.032(2) 0.021(2) -0.0072(18) -0.0002(17) -0.005(2) C5 0.030(2) 0.032(2) 0.022(2) -0.0108(18) 0.0042(18) 0.001(2) C6 0.023(2) 0.032(2) 0.0166(18) -0.0056(16) 0.0085(15) -0.0052(18) C7 0.0168(17) 0.0173(17) 0.0152(16) 0.0005(13) 0.0016(13) -0.0003(14) C8 0.0205(19) 0.023(2) 0.0204(19) 0.0045(16) 0.0069(15) -0.0033(16) C9 0.030(2) 0.025(2) 0.026(2) 0.0073(18) 0.0001(18) -0.0104(19) C10 0.033(3) 0.028(2) 0.031(2) 0.013(2) -0.007(2) -0.008(2) C11 0.028(2) 0.022(2) 0.038(3) 0.0080(19) 0.000(2) 0.0037(18) C12 0.018(2) 0.027(2) 0.026(2) 0.0071(17) -0.0024(16) -0.0004(17) C13 0.0136(17) 0.0230(19) 0.0125(16) 0.0019(14) 0.0011(13) 0.0022(14) C14 0.022(2) 0.025(2) 0.0179(19) -0.0041(16) -0.0022(16) -0.0019(17) C15 0.018(2) 0.035(3) 0.018(2) -0.0023(16) -0.0010(16) -0.0015(17) C16 0.026(2) 0.046(3) 0.023(2) 0.011(2) -0.0074(18) 0.001(2) C17 0.028(3) 0.028(3) 0.046(3) 0.012(2) -0.005(2) 0.004(2) C18 0.024(2) 0.021(2) 0.032(2) 0.0084(18) -0.0027(18) -0.0010(17) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Sn I3 2.8457(12) . ? Sn I4 2.8577(9) . ? Sn I2 2.8620(13) . ? I1 P 2.4010(13) . ? P C13 1.819(4) . ? P C7 1.823(4) . ? P C1 1.840(4) . ? C1 C6 1.526(6) . ? C1 C2 1.539(6) . ? C1 H1 1.0000 . ? C2 C3 1.525(7) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.516(7) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 C5 1.520(7) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C6 1.521(7) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 C12 1.536(6) . ? C7 C8 1.541(6) . ? C7 H7 1.0000 . ? C8 C9 1.526(7) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C10 1.522(7) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 C11 1.514(9) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 C12 1.532(7) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 C18 1.534(6) . ? C13 C14 1.551(6) . ? C13 H13 1.0000 . ? C14 C15 1.527(7) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 C16 1.524(8) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 C17 1.513(9) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 C18 1.536(7) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag I3 Sn I4 97.472(17) . . ? I3 Sn I2 97.352(19) . . ? I4 Sn I2 97.44(2) . . ? C13 P C7 109.7(2) . . ? C13 P C1 109.2(2) . . ? C7 P C1 115.97(19) . . ? C13 P I1 106.89(14) . . ? C7 P I1 107.32(15) . . ? C1 P I1 107.32(15) . . ? C6 C1 C2 111.5(4) . . ? C6 C1 P 112.2(3) . . ? C2 C1 P 114.3(3) . . ? C6 C1 H1 106.0 . . ? C2 C1 H1 106.0 . . ? P C1 H1 106.0 . . ? C3 C2 C1 108.2(4) . . ? C3 C2 H2A 110.0 . . ? C1 C2 H2A 110.0 . . ? C3 C2 H2B 110.0 . . ? C1 C2 H2B 110.0 . . ? H2A C2 H2B 108.4 . . ? C4 C3 C2 111.6(4) . . ? C4 C3 H3A 109.3 . . ? C2 C3 H3A 109.3 . . ? C4 C3 H3B 109.3 . . ? C2 C3 H3B 109.3 . . ? H3A C3 H3B 108.0 . . ? C3 C4 C5 110.9(4) . . ? C3 C4 H4A 109.5 . . ? C5 C4 H4A 109.5 . . ? C3 C4 H4B 109.5 . . ? C5 C4 H4B 109.5 . . ? H4A C4 H4B 108.1 . . ? C4 C5 C6 112.5(4) . . ? C4 C5 H5A 109.1 . . ? C6 C5 H5A 109.1 . . ? C4 C5 H5B 109.1 . . ? C6 C5 H5B 109.1 . . ? H5A C5 H5B 107.8 . . ? C5 C6 C1 110.3(4) . . ? C5 C6 H6A 109.6 . . ? C1 C6 H6A 109.6 . . ? C5 C6 H6B 109.6 . . ? C1 C6 H6B 109.6 . . ? H6A C6 H6B 108.1 . . ? C12 C7 C8 111.2(4) . . ? C12 C7 P 112.9(3) . . ? C8 C7 P 113.4(3) . . ? C12 C7 H7 106.2 . . ? C8 C7 H7 106.2 . . ? P C7 H7 106.2 . . ? C9 C8 C7 109.0(4) . . ? C9 C8 H8A 109.9 . . ? C7 C8 H8A 109.9 . . ? C9 C8 H8B 109.9 . . ? C7 C8 H8B 109.9 . . ? H8A C8 H8B 108.3 . . ? C10 C9 C8 112.0(4) . . ? C10 C9 H9A 109.2 . . ? C8 C9 H9A 109.2 . . ? C10 C9 H9B 109.2 . . ? C8 C9 H9B 109.2 . . ? H9A C9 H9B 107.9 . . ? C11 C10 C9 111.2(4) . . ? C11 C10 H10A 109.4 . . ? C9 C10 H10A 109.4 . . ? C11 C10 H10B 109.4 . . ? C9 C10 H10B 109.4 . . ? H10A C10 H10B 108.0 . . ? C10 C11 C12 112.0(5) . . ? C10 C11 H11A 109.2 . . ? C12 C11 H11A 109.2 . . ? C10 C11 H11B 109.2 . . ? C12 C11 H11B 109.2 . . ? H11A C11 H11B 107.9 . . ? C11 C12 C7 109.2(4) . . ? C11 C12 H12A 109.8 . . ? C7 C12 H12A 109.8 . . ? C11 C12 H12B 109.8 . . ? C7 C12 H12B 109.8 . . ? H12A C12 H12B 108.3 . . ? C18 C13 C14 111.3(4) . . ? C18 C13 P 112.5(3) . . ? C14 C13 P 111.6(3) . . ? C18 C13 H13 107.0 . . ? C14 C13 H13 107.0 . . ? P C13 H13 107.0 . . ? C15 C14 C13 109.4(4) . . ? C15 C14 H14A 109.8 . . ? C13 C14 H14A 109.8 . . ? C15 C14 H14B 109.8 . . ? C13 C14 H14B 109.8 . . ? H14A C14 H14B 108.2 . . ? C16 C15 C14 111.4(4) . . ? C16 C15 H15A 109.3 . . ? C14 C15 H15A 109.3 . . ? C16 C15 H15B 109.3 . . ? C14 C15 H15B 109.3 . . ? H15A C15 H15B 108.0 . . ? C17 C16 C15 110.7(4) . . ? C17 C16 H16A 109.5 . . ? C15 C16 H16A 109.5 . . ? C17 C16 H16B 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 108.1 . . ? C16 C17 C18 111.9(5) . . ? C16 C17 H17A 109.2 . . ? C18 C17 H17A 109.2 . . ? C16 C17 H17B 109.2 . . ? C18 C17 H17B 109.2 . . ? H17A C17 H17B 107.9 . . ? C13 C18 C17 109.7(4) . . ? C13 C18 H18A 109.7 . . ? C17 C18 H18A 109.7 . . ? C13 C18 H18B 109.7 . . ? C17 C18 H18B 109.7 . . ? H18A C18 H18B 108.2 . . ? _diffrn_measured_fraction_theta_max 0.970 _diffrn_reflns_theta_full 30.08 _diffrn_measured_fraction_theta_full 0.970 _refine_diff_density_max 2.012 _refine_diff_density_min -2.562 _refine_diff_density_rms 0.265