data_global _audit_creation_method 'APEX2 v2011.8-0' _publ_requested_journal ? _publ_contact_author_name ? _publ_contact_author_address ; ; _publ_contact_author_email ? _publ_contact_author_fax ? _publ_contact_author_phone ? _publ_section_title ; ; _publ_section_abstract ; ; _publ_section_references ; ; _publ_section_comment ; ; data_I _chemical_name_systematic ? _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C54 H63 P Sn' _chemical_formula_iupac ? _chemical_formula_weight 861.70 _chemical_melting_point ? _space_group_crystal_system monoclinic _space_group_name_H-M_alt 'P 1 21/c 1' _space_group_name_Hall '-P 2ybc' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 23.1940(8) _cell_length_b 9.5344(3) _cell_length_c 23.3775(8) _cell_angle_alpha 90 _cell_angle_beta 116.872(2) _cell_angle_gamma 90 _cell_volume 4611.5(3) _cell_formula_units_Z 4 _cell_measurement_reflns_used 9984 _cell_measurement_theta_min 2.5541 _cell_measurement_theta_max 30.1052 _cell_measurement_temperature 120.(2) _exptl_crystal_description prism _exptl_crystal_colour brown _exptl_crystal_size_max 0.340 _exptl_crystal_size_mid 0.250 _exptl_crystal_size_min 0.130 _exptl_crystal_density_diffrn 1.241 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1808 _exptl_absorpt_coefficient_mu 0.623 _exptl_absorpt_correction_type numerical _exptl_absorpt_process_details 'SADABS V2008/1 (Bruker AXS)' _exptl_absorpt_correction_T_min 0.86 _exptl_absorpt_correction_T_max 0.92 _exptl_special_details ; ; _diffrn_ambient_temperature 120.(2) _diffrn_source ? _diffrn_source_type 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean 8.3333 _diffrn_reflns_number 104383 _diffrn_reflns_av_R_equivalents 0.0295 _diffrn_reflns_av_sigmaI/netI 0.0187 _diffrn_reflns_theta_min 1.95 _diffrn_reflns_theta_max 30.12 _diffrn_reflns_theta_full 30.12 _diffrn_measured_fraction_theta_max 0.998 _diffrn_measured_fraction_theta_full 0.998 _diffrn_reflns_limit_h_min -28 _diffrn_reflns_limit_h_max 32 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 32 _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. ; _reflns_number_total 13570 _reflns_number_gt 11676 _reflns_threshold_expression >2sigma(I) _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_R_factor_all 0.0336 _refine_ls_R_factor_gt 0.0256 _refine_ls_wR_factor_gt 0.0617 _refine_ls_wR_factor_ref 0.0661 _refine_ls_goodness_of_fit_ref 1.019 _refine_ls_restrained_S_all 1.017 _refine_ls_number_reflns 13570 _refine_ls_number_parameters 533 _refine_ls_number_restraints 66 _refine_ls_hydrogen_treatment constr _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0308P)^2^+2.7023P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _refine_ls_shift/su_max 0.005 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 0.523 _refine_diff_density_min -0.431 _refine_ls_extinction_method none _refine_ls_extinction_coef ? 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' _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'APEX2 v2011.8-0 (Bruker AXS)' _computing_data_reduction 'SAINT V7.68A (Bruker AXS, 2009)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _computing_publication_material ? loop_ _atom_site_type_symbol _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_refinement_flags _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group C C1 0.78434(7) 0.87637(15) 1.13722(7) 0.0222(3) Uani d . 1.0 . . C C2 0.76948(8) 0.96824(17) 1.08609(8) 0.0287(3) Uani d . 1.0 . . H H2 0.75 0.9334 1.0434 0.034 Uiso calc R 1.0 . . C C3 0.78294(9) 1.11060(19) 1.09714(9) 0.0380(4) Uani d . 1.0 . . H H3 0.7716 1.1731 1.062 0.046 Uiso calc R 1.0 . . C C4 0.81287(10) 1.16110(19) 1.15941(10) 0.0418(4) Uani d . 1.0 . . H H4 0.8224 1.2582 1.1671 0.05 Uiso calc R 1.0 . . C C5 0.82885(12) 1.0698(2) 1.21040(10) 0.0455(5) Uani d . 1.0 . . H H5 0.8499 1.1044 1.2531 0.055 Uiso calc R 1.0 . . C C6 0.81435(10) 0.92780(18) 1.19957(8) 0.0348(4) Uani d . 1.0 . . H H6 0.825 0.8659 1.2348 0.042 Uiso calc R 1.0 . . C C7 0.67587(6) 0.69053(14) 1.10237(6) 0.0173(2) Uani d . 1.0 . . C C8 0.63819(6) 0.64339(13) 1.03942(6) 0.0163(2) Uani d . 1.0 . . C C9 0.57109(6) 0.63826(14) 1.01711(6) 0.0179(2) Uani d . 1.0 . . H H9 0.5441 0.6067 0.9748 0.021 Uiso calc R 1.0 . . C C10 0.54389(7) 0.67907(14) 1.05664(7) 0.0208(3) Uani d . 1.0 . . H H10 0.4984 0.6737 1.0412 0.025 Uiso calc R 1.0 . . C C11 0.58236(7) 0.72772(15) 1.11869(7) 0.0224(3) Uani d . 1.0 . . H H11 0.5629 0.7559 1.1449 0.027 Uiso calc R 1.0 . . C C12 0.64887(7) 0.73507(15) 1.14223(7) 0.0207(3) Uani d . 1.0 . . H H12 0.6755 0.7693 1.1842 0.025 Uiso calc R 1.0 . . C C13 0.80911(7) 0.59697(15) 1.19097(6) 0.0207(3) Uani d . 1.0 . . C C14 0.78353(7) 0.52469(17) 1.22575(7) 0.0254(3) Uani d . 1.0 . . H H14 0.7383 0.5279 1.2125 0.03 Uiso calc R 1.0 . . C C15 0.82336(8) 0.44753(17) 1.27979(8) 0.0291(3) Uani d . 1.0 . . H H15 0.8052 0.3988 1.3033 0.035 Uiso calc R 1.0 . . C C16 0.88897(8) 0.44139(19) 1.29941(8) 0.0336(4) Uani d . 1.0 . . H H16 0.9163 0.3911 1.3371 0.04 Uiso calc R 1.0 . . C C17 0.91469(9) 0.5094(3) 1.26367(10) 0.0493(5) Uani d . 1.0 . . H H17 0.9597 0.5037 1.2763 0.059 Uiso calc R 1.0 . . C C18 0.87505(8) 0.5856(2) 1.20973(9) 0.0416(5) Uani d . 1.0 . . H H18 0.8931 0.6307 1.1852 0.05 Uiso calc R 1.0 . . C C19 0.71315(6) 0.71367(14) 0.93879(6) 0.0166(2) Uani d . 1.0 . . C C20 0.65975(6) 0.78940(13) 0.89348(6) 0.0163(2) Uani d . 1.0 . . C C21 0.66728(7) 0.87825(15) 0.84951(7) 0.0227(3) Uani d . 1.0 . . H H21 0.6315 0.9317 0.8203 0.027 Uiso calc R 1.0 . . C C22 0.72608(8) 0.88901(17) 0.84810(8) 0.0285(3) Uani d . 1.0 . . H H22 0.7307 0.9503 0.8184 0.034 Uiso calc R 1.0 . . C C23 0.77811(7) 0.81023(16) 0.89012(8) 0.0262(3) Uani d . 1.0 . . H H23 0.818 0.8149 0.8879 0.031 Uiso calc R 1.0 . . C C24 0.77276(7) 0.72380(15) 0.93577(6) 0.0199(3) Uani d . 1.0 . . C C25 0.83046(7) 0.63851(17) 0.97946(7) 0.0243(3) Uani d . 1.0 A . C C26 0.88449(7) 0.7027(2) 1.03025(8) 0.0344(4) Uani d . 1.0 . . C C27 0.93569(8) 0.6167(3) 1.07040(9) 0.0499(6) Uani d . 1.0 A . H H27 0.9717 0.6589 1.1049 0.06 Uiso calc R 1.0 . . C C28 0.93639(10) 0.4738(3) 1.06227(10) 0.0561(7) Uani d . 1.0 . . C C29 0.88443(10) 0.4138(3) 1.01062(9) 0.0467(5) Uani d . 1.0 A . H H29 0.8847 0.3157 1.0037 0.056 Uiso calc R 1.0 . . C C30 0.83182(8) 0.49304(19) 0.96851(8) 0.0301(3) Uani d . 1.0 . . C C31 0.78079(9) 0.42512(17) 0.90783(8) 0.0310(3) Uani d . 1.0 A . H H31 0.7396 0.4786 0.8945 0.037 Uiso calc R 1.0 . . C C32 0.80165(11) 0.4409(2) 0.85447(9) 0.0460(5) Uani d . 1.0 . . H H32A 0.7692 0.3976 0.815 0.069 Uiso calc R 1.0 A . H H32B 0.8434 0.3945 0.8675 0.069 Uiso calc R 1.0 . . H H32C 0.8057 0.5407 0.8469 0.069 Uiso calc R 1.0 . . C C33 0.76680(11) 0.2713(2) 0.91498(10) 0.0446(5) Uani d . 1.0 . . H H33A 0.7335 0.2362 0.8739 0.067 Uiso calc R 1.0 A . H H33B 0.7515 0.2629 0.9477 0.067 Uiso calc R 1.0 . . H H33C 0.8064 0.2162 0.928 0.067 Uiso calc R 1.0 . . C C37 0.88987(9) 0.8600(2) 1.03993(9) 0.0431(5) Uani d . 1.0 . . H H37 0.8453 0.9005 1.0184 0.052 Uiso calc R 1.0 . . C C38 0.92097(9) 0.9041(3) 1.11087(10) 0.0556(6) Uani d . 1.0 . . H H38A 0.9228 1.0067 1.1138 0.083 Uiso calc R 1.0 . . H H38B 0.9648 0.8657 1.1329 0.083 Uiso calc R 1.0 . . H H38C 0.895 0.8681 1.1311 0.083 Uiso calc R 1.0 . . C C39 0.92973(13) 0.9246(3) 1.00856(12) 0.0710(9) Uani d . 1.0 . . H H39A 0.9325 1.0264 1.0151 0.107 Uiso calc R 1.0 . . H H39B 0.9086 0.9041 0.9625 0.107 Uiso calc R 1.0 . . H H39C 0.9733 0.8844 1.0282 0.107 Uiso calc R 1.0 . . C C40 0.59223(6) 0.77727(13) 0.88616(6) 0.0152(2) Uani d . 1.0 . . C C41 0.56699(6) 0.88287(13) 0.91042(6) 0.0165(2) Uani d . 1.0 . . C C42 0.60973(7) 0.99986(14) 0.95210(7) 0.0208(3) Uani d . 1.0 . . H H42 0.6557 0.972 0.966 0.025 Uiso calc R 1.0 . . C C43 0.59759(8) 1.13711(15) 0.91414(8) 0.0294(3) Uani d . 1.0 . . H H43A 0.6257 1.2108 0.9421 0.044 Uiso calc R 1.0 . . H H43B 0.5523 1.165 0.8984 0.044 Uiso calc R 1.0 . . H H43C 0.607 1.1232 0.8777 0.044 Uiso calc R 1.0 . . C C44 0.60112(8) 1.02413(15) 1.01256(7) 0.0257(3) Uani d . 1.0 . . H H44A 0.6297 1.1003 1.0378 0.038 Uiso calc R 1.0 . . H H44B 0.6121 0.9381 1.0383 0.038 Uiso calc R 1.0 . . H H44C 0.5561 1.0496 1.0003 0.038 Uiso calc R 1.0 . . C C45 0.50141(6) 0.88048(13) 0.89523(6) 0.0181(2) Uani d . 1.0 . . H H45 0.4844 0.9532 0.9109 0.022 Uiso calc R 1.0 . . C C46 0.46040(6) 0.77496(14) 0.85787(6) 0.0177(2) Uani d . 1.0 . . C C47 0.38973(7) 0.77400(15) 0.84368(7) 0.0212(3) Uani d . 1.0 . . H H47 0.379 0.8694 0.854 0.025 Uiso calc R 1.0 . . C C48 0.34411(8) 0.7441(2) 0.77341(8) 0.0353(4) Uani d . 1.0 . . H H48A 0.2994 0.7449 0.7671 0.053 Uiso calc R 1.0 . . H H48B 0.3541 0.6519 0.7616 0.053 Uiso calc R 1.0 . . H H48C 0.3496 0.8163 0.7464 0.053 Uiso calc R 1.0 . . C C49 0.37777(7) 0.66848(15) 0.88651(7) 0.0231(3) Uani d . 1.0 . . H H49A 0.3319 0.6699 0.8766 0.035 Uiso calc R 1.0 . . H H49B 0.4041 0.6937 0.9316 0.035 Uiso calc R 1.0 . . H H49C 0.3896 0.5742 0.8788 0.035 Uiso calc R 1.0 . . C C50 0.48660(7) 0.66823(14) 0.83589(6) 0.0183(2) Uani d . 1.0 . . H H50 0.4595 0.5935 0.8116 0.022 Uiso calc R 1.0 . . C C51 0.55149(6) 0.66822(13) 0.84855(6) 0.0163(2) Uani d . 1.0 . . C C52 0.57619(7) 0.55625(13) 0.81853(6) 0.0188(2) Uani d . 1.0 . . H H52 0.6228 0.5395 0.8483 0.023 Uiso calc R 1.0 . . C C53 0.54086(9) 0.41624(16) 0.80817(9) 0.0332(4) Uani d . 1.0 . . H H53A 0.5589 0.3491 0.7889 0.05 Uiso calc R 1.0 . . H H53B 0.4948 0.4299 0.7795 0.05 Uiso calc R 1.0 . . H H53C 0.5462 0.3799 0.8495 0.05 Uiso calc R 1.0 . . C C54 0.57178(10) 0.60664(17) 0.75451(8) 0.0329(4) Uani d . 1.0 . . H H54A 0.588 0.5332 0.7362 0.049 Uiso calc R 1.0 . . H H54B 0.5979 0.6916 0.7615 0.049 Uiso calc R 1.0 . . H H54C 0.5266 0.6275 0.7248 0.049 Uiso calc R 1.0 . . C C34 0.9866(2) 0.3544(7) 1.1041(2) 0.0388(11) Uani d PU 0.530(10) A 1 H H34 0.9718 0.2589 1.0857 0.047 Uiso calc PR 0.530(10) A 1 C C35 1.0509(2) 0.3927(8) 1.1056(3) 0.0512(15) Uani d PU 0.530(10) A 1 H H35A 1.0468 0.3885 1.062 0.077 Uiso calc PR 0.530(10) A 1 H H35B 1.0842 0.3264 1.1331 0.077 Uiso calc PR 0.530(10) A 1 H H35C 1.0632 0.4879 1.1225 0.077 Uiso calc PR 0.530(10) A 1 C C36 0.9942(9) 0.3655(18) 1.1711(9) 0.096(5) Uani d PU 0.530(10) A 1 H H36A 0.9533 0.3409 1.1714 0.144 Uiso calc PR 0.530(10) A 1 H H36B 1.0061 0.4618 1.1867 0.144 Uiso calc PR 0.530(10) A 1 H H36C 1.0281 0.301 1.1991 0.144 Uiso calc PR 0.530(10) A 1 C C340 0.9991(3) 0.4165(8) 1.1131(3) 0.0386(13) Uani d PU 0.470(10) A 2 H H340 1.0284 0.4966 1.1358 0.046 Uiso calc PR 0.470(10) A 2 C C350 1.0311(3) 0.3263(7) 1.0827(3) 0.0440(15) Uani d PU 0.470(10) A 2 H H35D 1.0719 0.2895 1.1161 0.066 Uiso calc PR 0.470(10) A 2 H H35E 1.0397 0.3826 1.0524 0.066 Uiso calc PR 0.470(10) A 2 H H35F 1.0025 0.2481 1.06 0.066 Uiso calc PR 0.470(10) A 2 C C360 0.9828(9) 0.3364(15) 1.1611(9) 0.066(4) Uani d PU 0.470(10) A 2 H H36D 1.0225 0.2969 1.1952 0.1 Uiso calc PR 0.470(10) A 2 H H36E 0.9524 0.2604 1.1388 0.1 Uiso calc PR 0.470(10) A 2 H H36F 0.9631 0.4008 1.1799 0.1 Uiso calc PR 0.470(10) A 2 P P1 0.759751(17) 0.69394(4) 1.118163(16) 0.01806(7) Uani d . 1.0 . . Sn Sn1 0.704457(4) 0.551845(9) 1.003511(4) 0.01737(3) Uani d . 1.0 . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 C1 0.0190(6) 0.0254(7) 0.0236(7) -0.0017(5) 0.0107(6) 0.0006(5) C2 0.0213(7) 0.0334(8) 0.0255(7) -0.0032(6) 0.0055(6) 0.0060(6) C3 0.0329(9) 0.0326(8) 0.0443(10) -0.0018(7) 0.0138(8) 0.0120(8) C4 0.0515(11) 0.0263(8) 0.0578(12) -0.0077(8) 0.0336(10) -0.0038(8) C5 0.0705(14) 0.0359(9) 0.0389(10) -0.0182(9) 0.0325(10) -0.0139(8) C6 0.0503(11) 0.0318(8) 0.0262(8) -0.0098(7) 0.0207(8) -0.0036(6) C7 0.0160(6) 0.0190(6) 0.0158(6) 0.0024(5) 0.0062(5) 0.0015(5) C8 0.0183(6) 0.0155(5) 0.0152(6) 0.0016(5) 0.0077(5) 0.0025(4) C9 0.0177(6) 0.0181(6) 0.0156(6) 0.0000(5) 0.0054(5) 0.0016(5) C10 0.0169(6) 0.0229(6) 0.0228(6) 0.0030(5) 0.0090(5) 0.0021(5) C11 0.0220(7) 0.0258(7) 0.0223(7) 0.0049(5) 0.0126(6) -0.0002(5) C12 0.0203(6) 0.0246(6) 0.0161(6) 0.0023(5) 0.0071(5) -0.0021(5) C13 0.0172(6) 0.0251(6) 0.0163(6) 0.0016(5) 0.0045(5) 0.0007(5) C14 0.0187(7) 0.0339(8) 0.0241(7) 0.0060(6) 0.0103(6) 0.0064(6) C15 0.0278(8) 0.0368(8) 0.0251(7) 0.0080(6) 0.0140(6) 0.0097(6) C16 0.0257(8) 0.0420(9) 0.0262(8) 0.0082(7) 0.0056(6) 0.0113(7) C17 0.0166(8) 0.0750(14) 0.0486(11) 0.0075(8) 0.0079(8) 0.0306(11) C18 0.0188(7) 0.0632(12) 0.0395(10) 0.0033(8) 0.0102(7) 0.0245(9) C19 0.0168(6) 0.0191(6) 0.0144(6) -0.0019(5) 0.0076(5) -0.0029(5) C20 0.0179(6) 0.0156(5) 0.0161(6) -0.0022(5) 0.0084(5) -0.0022(4) C21 0.0250(7) 0.0209(6) 0.0243(7) 0.0004(5) 0.0129(6) 0.0039(5) C22 0.0322(8) 0.0272(7) 0.0338(8) -0.0033(6) 0.0218(7) 0.0061(6) C23 0.0223(7) 0.0308(7) 0.0311(8) -0.0055(6) 0.0171(6) -0.0020(6) C24 0.0170(6) 0.0242(6) 0.0185(6) -0.0036(5) 0.0080(5) -0.0056(5) C25 0.0150(6) 0.0405(8) 0.0192(6) 0.0014(6) 0.0092(5) -0.0024(6) C26 0.0157(7) 0.0672(12) 0.0214(7) -0.0051(7) 0.0094(6) -0.0082(7) C27 0.0176(8) 0.1048(19) 0.0231(8) 0.0053(10) 0.0056(7) -0.0032(10) C28 0.0314(10) 0.107(2) 0.0296(9) 0.0345(12) 0.0133(8) 0.0157(11) C29 0.0436(11) 0.0639(13) 0.0343(9) 0.0315(10) 0.0192(9) 0.0114(9) C30 0.0265(8) 0.0415(9) 0.0236(7) 0.0122(7) 0.0125(6) 0.0020(6) C31 0.0370(9) 0.0314(8) 0.0259(8) 0.0082(7) 0.0153(7) -0.0028(6) C32 0.0612(13) 0.0506(11) 0.0329(9) -0.0055(10) 0.0271(10) -0.0116(8) C33 0.0614(13) 0.0322(9) 0.0463(11) 0.0094(9) 0.0297(10) -0.0006(8) C37 0.0276(8) 0.0706(13) 0.0337(9) -0.0249(9) 0.0161(7) -0.0203(9) C38 0.0250(9) 0.1009(18) 0.0400(11) -0.0251(10) 0.0139(8) -0.0343(12) C39 0.0671(16) 0.103(2) 0.0597(15) -0.0567(15) 0.0430(13) -0.0345(14) C40 0.0165(6) 0.0151(5) 0.0138(5) 0.0005(4) 0.0066(5) 0.0032(4) C41 0.0173(6) 0.0149(5) 0.0158(6) 0.0012(5) 0.0060(5) 0.0016(4) C42 0.0176(6) 0.0180(6) 0.0250(7) 0.0000(5) 0.0080(5) -0.0038(5) C43 0.0333(8) 0.0187(6) 0.0396(9) -0.0058(6) 0.0193(7) -0.0018(6) C44 0.0284(8) 0.0214(6) 0.0246(7) 0.0007(5) 0.0097(6) -0.0057(5) C45 0.0179(6) 0.0165(6) 0.0194(6) 0.0031(5) 0.0079(5) 0.0025(5) C46 0.0170(6) 0.0178(6) 0.0169(6) 0.0013(5) 0.0065(5) 0.0054(5) C47 0.0163(6) 0.0204(6) 0.0252(7) 0.0009(5) 0.0080(5) 0.0048(5) C48 0.0185(7) 0.0542(11) 0.0265(8) -0.0055(7) 0.0043(6) 0.0087(7) C49 0.0226(7) 0.0223(6) 0.0264(7) -0.0005(5) 0.0129(6) 0.0027(5) C50 0.0187(6) 0.0174(6) 0.0163(6) -0.0031(5) 0.0056(5) 0.0008(5) C51 0.0196(6) 0.0154(5) 0.0135(5) 0.0004(5) 0.0072(5) 0.0023(4) C52 0.0216(6) 0.0172(6) 0.0172(6) 0.0000(5) 0.0084(5) -0.0016(5) C53 0.0456(10) 0.0176(6) 0.0450(10) -0.0020(6) 0.0281(9) -0.0027(6) C54 0.0545(11) 0.0249(7) 0.0269(8) -0.0003(7) 0.0251(8) -0.0022(6) C34 0.0212(17) 0.037(3) 0.041(2) 0.0044(17) -0.0012(15) -0.002(2) C35 0.024(2) 0.066(3) 0.055(3) 0.013(2) 0.011(2) -0.004(3) C36 0.059(6) 0.165(13) 0.061(4) 0.053(8) 0.024(4) 0.039(7) C340 0.034(3) 0.039(3) 0.031(2) 0.014(2) 0.0040(19) 0.000(2) C350 0.026(2) 0.053(3) 0.048(3) 0.012(2) 0.012(2) -0.001(2) C360 0.064(8) 0.062(4) 0.085(9) 0.036(4) 0.044(7) 0.050(5) P1 0.01522(15) 0.02376(16) 0.01433(15) 0.00126(13) 0.00593(13) 0.00062(12) Sn1 0.01942(5) 0.01846(4) 0.01541(5) 0.00297(3) 0.00892(4) 0.00088(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag C1 C6 . 1.390(2) ? C1 C2 . 1.394(2) ? C1 P1 . 1.8219(15) ? C2 C3 . 1.391(2) ? C2 H2 . 0.95 ? C3 C4 . 1.385(3) ? C3 H3 . 0.95 ? C4 C5 . 1.384(3) ? C4 H4 . 0.95 ? C5 C6 . 1.390(2) ? C5 H5 . 0.95 ? C6 H6 . 0.95 ? C7 C12 . 1.4029(18) ? C7 C8 . 1.4031(18) ? C7 P1 . 1.8091(14) ? C8 C9 . 1.4009(18) ? C8 Sn1 . 2.2351(13) ? C9 C10 . 1.3894(18) ? C9 H9 . 0.95 ? C10 C11 . 1.395(2) ? C10 H10 . 0.95 ? C11 C12 . 1.386(2) ? C11 H11 . 0.95 ? C12 H12 . 0.95 ? C13 C14 . 1.387(2) ? C13 C18 . 1.392(2) ? C13 P1 . 1.8168(14) ? C14 C15 . 1.391(2) ? C14 H14 . 0.95 ? C15 C16 . 1.378(2) ? C15 H15 . 0.95 ? C16 C17 . 1.388(3) ? C16 H16 . 0.95 ? C17 C18 . 1.384(2) ? C17 H17 . 0.95 ? C18 H18 . 0.95 ? C19 C20 . 1.4112(18) ? C19 C24 . 1.4192(18) ? C19 Sn1 . 2.2330(13) ? C20 C21 . 1.4025(18) ? C20 C40 . 1.5009(18) ? C21 C22 . 1.383(2) ? C21 H21 . 0.95 ? C22 C23 . 1.383(2) ? C22 H22 . 0.95 ? C23 C24 . 1.398(2) ? C23 H23 . 0.95 ? C24 C25 . 1.503(2) ? C25 C30 . 1.413(2) ? C25 C26 . 1.418(2) ? C26 C27 . 1.399(3) ? C26 C37 . 1.514(3) ? C27 C28 . 1.377(4) ? C27 H27 . 0.95 ? C28 C29 . 1.386(3) ? C28 C340 . 1.504(5) ? C28 C34 . 1.605(5) ? C29 C30 . 1.394(2) ? C29 H29 . 0.95 ? C30 C31 . 1.522(2) ? C31 C33 . 1.527(3) ? C31 C32 . 1.536(2) ? C31 H31 . 1.0 ? C32 H32A . 0.98 ? C32 H32B . 0.98 ? C32 H32C . 0.98 ? C33 H33A . 0.98 ? C33 H33B . 0.98 ? C33 H33C . 0.98 ? C37 C38 . 1.538(3) ? C37 C39 . 1.544(3) ? C37 H37 . 1.0 ? C38 H38A . 0.98 ? C38 H38B . 0.98 ? C38 H38C . 0.98 ? C39 H39A . 0.98 ? C39 H39B . 0.98 ? C39 H39C . 0.98 ? C40 C41 . 1.4066(17) ? C40 C51 . 1.4128(18) ? C41 C45 . 1.3970(18) ? C41 C42 . 1.5176(19) ? C42 C44 . 1.532(2) ? C42 C43 . 1.534(2) ? C42 H42 . 1.0 ? C43 H43A . 0.98 ? C43 H43B . 0.98 ? C43 H43C . 0.98 ? C44 H44A . 0.98 ? C44 H44B . 0.98 ? C44 H44C . 0.98 ? C45 C46 . 1.3889(19) ? C45 H45 . 0.95 ? C46 C50 . 1.3968(19) ? C46 C47 . 1.5183(18) ? C47 C48 . 1.526(2) ? C47 C49 . 1.5307(19) ? C47 H47 . 1.0 ? C48 H48A . 0.98 ? C48 H48B . 0.98 ? C48 H48C . 0.98 ? C49 H49A . 0.98 ? C49 H49B . 0.98 ? C49 H49C . 0.98 ? C50 C51 . 1.3965(19) ? C50 H50 . 0.95 ? C51 C52 . 1.5244(18) ? C52 C53 . 1.527(2) ? C52 C54 . 1.531(2) ? C52 H52 . 1.0 ? C53 H53A . 0.98 ? C53 H53B . 0.98 ? C53 H53C . 0.98 ? C54 H54A . 0.98 ? C54 H54B . 0.98 ? C54 H54C . 0.98 ? C34 C36 . 1.50(2) ? C34 C35 . 1.523(8) ? C34 H34 . 1.0 ? C35 H35A . 0.98 ? C35 H35B . 0.98 ? C35 H35C . 0.98 ? C36 H36A . 0.98 ? C36 H36B . 0.98 ? C36 H36C . 0.98 ? C340 C350 . 1.507(8) ? C340 C360 . 1.539(16) ? C340 H340 . 1.0 ? C350 H35D . 0.98 ? C350 H35E . 0.98 ? C350 H35F . 0.98 ? C360 H36D . 0.98 ? C360 H36E . 0.98 ? C360 H36F . 0.98 ? P1 Sn1 . 2.7489(4) ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag C6 C1 C2 . . 119.35(15) ? C6 C1 P1 . . 123.11(12) ? C2 C1 P1 . . 117.48(12) ? C3 C2 C1 . . 120.43(16) ? C3 C2 H2 . . 119.8 ? C1 C2 H2 . . 119.8 ? C4 C3 C2 . . 119.88(16) ? C4 C3 H3 . . 120.1 ? C2 C3 H3 . . 120.1 ? C5 C4 C3 . . 119.88(17) ? C5 C4 H4 . . 120.1 ? C3 C4 H4 . . 120.1 ? C4 C5 C6 . . 120.46(18) ? C4 C5 H5 . . 119.8 ? C6 C5 H5 . . 119.8 ? C1 C6 C5 . . 119.98(16) ? C1 C6 H6 . . 120.0 ? C5 C6 H6 . . 120.0 ? C12 C7 C8 . . 122.69(12) ? C12 C7 P1 . . 128.36(11) ? C8 C7 P1 . . 108.81(9) ? C9 C8 C7 . . 117.53(12) ? C9 C8 Sn1 . . 133.11(10) ? C7 C8 Sn1 . . 108.11(9) ? C10 C9 C8 . . 120.30(12) ? C10 C9 H9 . . 119.8 ? C8 C9 H9 . . 119.9 ? C9 C10 C11 . . 121.04(13) ? C9 C10 H10 . . 119.5 ? C11 C10 H10 . . 119.5 ? C12 C11 C10 . . 120.24(12) ? C12 C11 H11 . . 119.9 ? C10 C11 H11 . . 119.9 ? C11 C12 C7 . . 118.17(13) ? C11 C12 H12 . . 120.9 ? C7 C12 H12 . . 120.9 ? C14 C13 C18 . . 118.49(14) ? C14 C13 P1 . . 123.14(11) ? C18 C13 P1 . . 118.17(11) ? C13 C14 C15 . . 120.71(14) ? C13 C14 H14 . . 119.6 ? C15 C14 H14 . . 119.6 ? C16 C15 C14 . . 120.32(15) ? C16 C15 H15 . . 119.8 ? C14 C15 H15 . . 119.8 ? C15 C16 C17 . . 119.36(15) ? C15 C16 H16 . . 120.3 ? C17 C16 H16 . . 120.3 ? C18 C17 C16 . . 120.32(16) ? C18 C17 H17 . . 119.8 ? C16 C17 H17 . . 119.8 ? C17 C18 C13 . . 120.71(16) ? C17 C18 H18 . . 119.6 ? C13 C18 H18 . . 119.6 ? C20 C19 C24 . . 118.17(12) ? C20 C19 Sn1 . . 123.01(9) ? C24 C19 Sn1 . . 117.97(10) ? C21 C20 C19 . . 120.09(12) ? C21 C20 C40 . . 115.61(12) ? C19 C20 C40 . . 124.24(11) ? C22 C21 C20 . . 120.88(14) ? C22 C21 H21 . . 119.6 ? C20 C21 H21 . . 119.6 ? C21 C22 C23 . . 119.74(13) ? C21 C22 H22 . . 120.1 ? C23 C22 H22 . . 120.1 ? C22 C23 C24 . . 120.82(13) ? C22 C23 H23 . . 119.6 ? C24 C23 H23 . . 119.6 ? C23 C24 C19 . . 120.19(13) ? C23 C24 C25 . . 118.60(12) ? C19 C24 C25 . . 121.17(12) ? C30 C25 C26 . . 119.44(15) ? C30 C25 C24 . . 119.59(13) ? C26 C25 C24 . . 120.94(15) ? C27 C26 C25 . . 118.04(19) ? C27 C26 C37 . . 119.54(18) ? C25 C26 C37 . . 122.34(16) ? C28 C27 C26 . . 123.16(19) ? C28 C27 H27 . . 118.4 ? C26 C27 H27 . . 118.4 ? C27 C28 C29 . . 117.93(18) ? C27 C28 C340 . . 108.5(4) ? C29 C28 C340 . . 133.5(4) ? C27 C28 C34 . . 131.9(3) ? C29 C28 C34 . . 110.1(3) ? C340 C28 C34 . . 23.9(2) ? C28 C29 C30 . . 122.1(2) ? C28 C29 H29 . . 119.0 ? C30 C29 H29 . . 119.0 ? C29 C30 C25 . . 119.21(17) ? C29 C30 C31 . . 119.45(17) ? C25 C30 C31 . . 120.99(14) ? C30 C31 C33 . . 114.88(15) ? C30 C31 C32 . . 108.52(15) ? C33 C31 C32 . . 110.09(14) ? C30 C31 H31 . . 107.7 ? C33 C31 H31 . . 107.7 ? C32 C31 H31 . . 107.7 ? C31 C32 H32A . . 109.5 ? C31 C32 H32B . . 109.5 ? H32A C32 H32B . . 109.5 ? C31 C32 H32C . . 109.5 ? H32A C32 H32C . . 109.5 ? H32B C32 H32C . . 109.5 ? C31 C33 H33A . . 109.5 ? C31 C33 H33B . . 109.5 ? H33A C33 H33B . . 109.5 ? C31 C33 H33C . . 109.5 ? H33A C33 H33C . . 109.5 ? H33B C33 H33C . . 109.5 ? C26 C37 C38 . . 113.52(19) ? C26 C37 C39 . . 110.54(17) ? C38 C37 C39 . . 108.26(16) ? C26 C37 H37 . . 108.1 ? C38 C37 H37 . . 108.1 ? C39 C37 H37 . . 108.1 ? C37 C38 H38A . . 109.5 ? C37 C38 H38B . . 109.5 ? H38A C38 H38B . . 109.5 ? C37 C38 H38C . . 109.5 ? H38A C38 H38C . . 109.5 ? H38B C38 H38C . . 109.5 ? C37 C39 H39A . . 109.5 ? C37 C39 H39B . . 109.5 ? H39A C39 H39B . . 109.5 ? C37 C39 H39C . . 109.5 ? H39A C39 H39C . . 109.5 ? H39B C39 H39C . . 109.5 ? C41 C40 C51 . . 119.63(12) ? C41 C40 C20 . . 120.12(11) ? C51 C40 C20 . . 119.84(11) ? C45 C41 C40 . . 119.31(12) ? C45 C41 C42 . . 119.70(11) ? C40 C41 C42 . . 120.98(12) ? C41 C42 C44 . . 112.56(12) ? C41 C42 C43 . . 111.09(12) ? C44 C42 C43 . . 109.79(12) ? C41 C42 H42 . . 107.7 ? C44 C42 H42 . . 107.7 ? C43 C42 H42 . . 107.7 ? C42 C43 H43A . . 109.5 ? C42 C43 H43B . . 109.5 ? H43A C43 H43B . . 109.5 ? C42 C43 H43C . . 109.5 ? H43A C43 H43C . . 109.5 ? H43B C43 H43C . . 109.5 ? C42 C44 H44A . . 109.5 ? C42 C44 H44B . . 109.5 ? H44A C44 H44B . . 109.5 ? C42 C44 H44C . . 109.5 ? H44A C44 H44C . . 109.5 ? H44B C44 H44C . . 109.5 ? C46 C45 C41 . . 121.96(12) ? C46 C45 H45 . . 119.0 ? C41 C45 H45 . . 119.0 ? C45 C46 C50 . . 118.09(12) ? C45 C46 C47 . . 120.45(12) ? C50 C46 C47 . . 121.43(12) ? C46 C47 C48 . . 113.02(12) ? C46 C47 C49 . . 110.98(11) ? C48 C47 C49 . . 109.81(12) ? C46 C47 H47 . . 107.6 ? C48 C47 H47 . . 107.6 ? C49 C47 H47 . . 107.6 ? C47 C48 H48A . . 109.5 ? C47 C48 H48B . . 109.5 ? H48A C48 H48B . . 109.5 ? C47 C48 H48C . . 109.5 ? H48A C48 H48C . . 109.5 ? H48B C48 H48C . . 109.5 ? C47 C49 H49A . . 109.5 ? C47 C49 H49B . . 109.5 ? H49A C49 H49B . . 109.5 ? C47 C49 H49C . . 109.5 ? H49A C49 H49C . . 109.5 ? H49B C49 H49C . . 109.5 ? C51 C50 C46 . . 121.91(12) ? C51 C50 H50 . . 119.0 ? C46 C50 H50 . . 119.0 ? C50 C51 C40 . . 119.04(12) ? C50 C51 C52 . . 119.72(12) ? C40 C51 C52 . . 121.13(12) ? C51 C52 C53 . . 113.50(12) ? C51 C52 C54 . . 110.94(11) ? C53 C52 C54 . . 108.99(12) ? C51 C52 H52 . . 107.7 ? C53 C52 H52 . . 107.7 ? C54 C52 H52 . . 107.7 ? C52 C53 H53A . . 109.5 ? C52 C53 H53B . . 109.5 ? H53A C53 H53B . . 109.5 ? C52 C53 H53C . . 109.5 ? H53A C53 H53C . . 109.5 ? H53B C53 H53C . . 109.5 ? C52 C54 H54A . . 109.5 ? C52 C54 H54B . . 109.5 ? H54A C54 H54B . . 109.5 ? C52 C54 H54C . . 109.5 ? H54A C54 H54C . . 109.5 ? H54B C54 H54C . . 109.5 ? C36 C34 C35 . . 108.0(10) ? C36 C34 C28 . . 107.3(7) ? C35 C34 C28 . . 106.1(4) ? C36 C34 H34 . . 111.7 ? C35 C34 H34 . . 111.7 ? C28 C34 H34 . . 111.7 ? C34 C35 H35A . . 109.5 ? C34 C35 H35B . . 109.5 ? H35A C35 H35B . . 109.5 ? C34 C35 H35C . . 109.5 ? H35A C35 H35C . . 109.5 ? H35B C35 H35C . . 109.5 ? C34 C36 H36A . . 109.5 ? C34 C36 H36B . . 109.5 ? H36A C36 H36B . . 109.5 ? C34 C36 H36C . . 109.5 ? H36A C36 H36C . . 109.5 ? H36B C36 H36C . . 109.5 ? C28 C340 C350 . . 109.9(5) ? C28 C340 C360 . . 106.7(8) ? C350 C340 C360 . . 113.3(9) ? C28 C340 H340 . . 108.9 ? C350 C340 H340 . . 108.9 ? C360 C340 H340 . . 108.9 ? C340 C350 H35D . . 109.5 ? C340 C350 H35E . . 109.5 ? H35D C350 H35E . . 109.5 ? C340 C350 H35F . . 109.5 ? H35D C350 H35F . . 109.5 ? H35E C350 H35F . . 109.5 ? C340 C360 H36D . . 109.5 ? C340 C360 H36E . . 109.5 ? H36D C360 H36E . . 109.5 ? C340 C360 H36F . . 109.5 ? H36D C360 H36F . . 109.5 ? H36E C360 H36F . . 109.5 ? C7 P1 C13 . . 110.25(6) ? C7 P1 C1 . . 104.83(6) ? C13 P1 C1 . . 105.17(7) ? C7 P1 Sn1 . . 78.89(4) ? C13 P1 Sn1 . . 118.77(5) ? C1 P1 Sn1 . . 131.72(5) ? C19 Sn1 C8 . . 105.83(5) ? C19 Sn1 P1 . . 100.07(3) ? C8 Sn1 P1 . . 62.50(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_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag C6 C1 C2 C3 . . . . -1.7(2) ? P1 C1 C2 C3 . . . . 175.64(13) ? C1 C2 C3 C4 . . . . 1.7(3) ? C2 C3 C4 C5 . . . . -0.5(3) ? C3 C4 C5 C6 . . . . -0.8(3) ? C2 C1 C6 C5 . . . . 0.4(3) ? P1 C1 C6 C5 . . . . -176.75(15) ? C4 C5 C6 C1 . . . . 0.8(3) ? C12 C7 C8 C9 . . . . -1.62(19) ? P1 C7 C8 C9 . . . . -177.72(10) ? C12 C7 C8 Sn1 . . . . -170.51(11) ? P1 C7 C8 Sn1 . . . . 13.39(10) ? C7 C8 C9 C10 . . . . 0.11(19) ? Sn1 C8 C9 C10 . . . . 165.57(10) ? C8 C9 C10 C11 . . . . 1.0(2) ? C9 C10 C11 C12 . . . . -0.5(2) ? C10 C11 C12 C7 . . . . -0.9(2) ? C8 C7 C12 C11 . . . . 2.0(2) ? P1 C7 C12 C11 . . . . 177.32(11) ? C18 C13 C14 C15 . . . . 2.7(2) ? P1 C13 C14 C15 . . . . 177.43(13) ? C13 C14 C15 C16 . . . . -0.3(3) ? C14 C15 C16 C17 . . . . -1.9(3) ? C15 C16 C17 C18 . . . . 1.6(3) ? C16 C17 C18 C13 . . . . 0.9(4) ? C14 C13 C18 C17 . . . . -3.0(3) ? P1 C13 C18 C17 . . . . -178.01(19) ? C24 C19 C20 C21 . . . . -3.73(19) ? Sn1 C19 C20 C21 . . . . -172.97(10) ? C24 C19 C20 C40 . . . . 173.21(12) ? Sn1 C19 C20 C40 . . . . 3.98(17) ? C19 C20 C21 C22 . . . . 2.5(2) ? C40 C20 C21 C22 . . . . -174.67(13) ? C20 C21 C22 C23 . . . . 0.6(2) ? C21 C22 C23 C24 . . . . -2.5(2) ? C22 C23 C24 C19 . . . . 1.2(2) ? C22 C23 C24 C25 . . . . 178.93(14) ? C20 C19 C24 C23 . . . . 1.90(19) ? Sn1 C19 C24 C23 . . . . 171.68(10) ? C20 C19 C24 C25 . . . . -175.75(12) ? Sn1 C19 C24 C25 . . . . -5.96(17) ? C23 C24 C25 C30 . . . . -104.18(17) ? C19 C24 C25 C30 . . . . 73.50(18) ? C23 C24 C25 C26 . . . . 73.73(18) ? C19 C24 C25 C26 . . . . -108.59(16) ? C30 C25 C26 C27 . . . . -4.1(2) ? C24 C25 C26 C27 . . . . 177.96(14) ? C30 C25 C26 C37 . . . . 172.53(14) ? C24 C25 C26 C37 . . . . -5.4(2) ? C25 C26 C27 C28 . . . . 1.0(3) ? C37 C26 C27 C28 . . . . -175.74(18) ? C26 C27 C28 C29 . . . . 1.8(3) ? C26 C27 C28 C340 . . . . 179.0(3) ? C26 C27 C28 C34 . . . . -175.3(3) ? C27 C28 C29 C30 . . . . -1.6(3) ? C340 C28 C29 C30 . . . . -177.8(4) ? C34 C28 C29 C30 . . . . 176.2(2) ? C28 C29 C30 C25 . . . . -1.5(3) ? C28 C29 C30 C31 . . . . 171.74(18) ? C26 C25 C30 C29 . . . . 4.4(2) ? C24 C25 C30 C29 . . . . -177.67(15) ? C26 C25 C30 C31 . . . . -168.76(14) ? C24 C25 C30 C31 . . . . 9.2(2) ? C29 C30 C31 C33 . . . . 35.5(2) ? C25 C30 C31 C33 . . . . -151.36(16) ? C29 C30 C31 C32 . . . . -88.2(2) ? C25 C30 C31 C32 . . . . 84.95(18) ? C27 C26 C37 C38 . . . . -41.0(2) ? C25 C26 C37 C38 . . . . 142.40(16) ? C27 C26 C37 C39 . . . . 80.9(2) ? C25 C26 C37 C39 . . . . -95.7(2) ? C21 C20 C40 C41 . . . . -79.57(15) ? C19 C20 C40 C41 . . . . 103.37(15) ? C21 C20 C40 C51 . . . . 93.17(15) ? C19 C20 C40 C51 . . . . -83.90(16) ? C51 C40 C41 C45 . . . . -1.96(18) ? C20 C40 C41 C45 . . . . 170.78(12) ? C51 C40 C41 C42 . . . . 178.75(12) ? C20 C40 C41 C42 . . . . -8.50(18) ? C45 C41 C42 C44 . . . . 48.27(17) ? C40 C41 C42 C44 . . . . -132.45(13) ? C45 C41 C42 C43 . . . . -75.31(16) ? C40 C41 C42 C43 . . . . 103.97(14) ? C40 C41 C45 C46 . . . . 1.42(19) ? C42 C41 C45 C46 . . . . -179.28(12) ? C41 C45 C46 C50 . . . . 0.69(19) ? C41 C45 C46 C47 . . . . 178.54(12) ? C45 C46 C47 C48 . . . . 134.77(14) ? C50 C46 C47 C48 . . . . -47.47(18) ? C45 C46 C47 C49 . . . . -101.36(14) ? C50 C46 C47 C49 . . . . 76.41(16) ? C45 C46 C50 C51 . . . . -2.31(19) ? C47 C46 C50 C51 . . . . 179.87(12) ? C46 C50 C51 C40 . . . . 1.77(19) ? C46 C50 C51 C52 . . . . -174.64(12) ? C41 C40 C51 C50 . . . . 0.42(18) ? C20 C40 C51 C50 . . . . -172.35(11) ? C41 C40 C51 C52 . . . . 176.77(11) ? C20 C40 C51 C52 . . . . 4.00(18) ? C50 C51 C52 C53 . . . . -31.26(18) ? C40 C51 C52 C53 . . . . 152.42(13) ? C50 C51 C52 C54 . . . . 91.85(15) ? C40 C51 C52 C54 . . . . -84.47(16) ? C27 C28 C34 C36 . . . . 54.8(10) ? C29 C28 C34 C36 . . . . -122.6(9) ? C340 C28 C34 C36 . . . . 68.2(12) ? C27 C28 C34 C35 . . . . -60.5(6) ? C29 C28 C34 C35 . . . . 122.2(5) ? C340 C28 C34 C35 . . . . -47.0(7) ? C27 C28 C340 C350 . . . . -129.0(6) ? C29 C28 C340 C350 . . . . 47.5(9) ? C34 C28 C340 C350 . . . . 61.5(8) ? C27 C28 C340 C360 . . . . 107.8(9) ? C29 C28 C340 C360 . . . . -75.7(9) ? C34 C28 C340 C360 . . . . -61.7(12) ? C12 C7 P1 C13 . . . . 56.91(14) ? C8 C7 P1 C13 . . . . -127.28(10) ? C12 C7 P1 C1 . . . . -55.81(14) ? C8 C7 P1 C1 . . . . 120.00(10) ? C12 C7 P1 Sn1 . . . . 173.68(13) ? C8 C7 P1 Sn1 . . . . -10.51(8) ? C14 C13 P1 C7 . . . . 3.75(15) ? C18 C13 P1 C7 . . . . 178.47(14) ? C14 C13 P1 C1 . . . . 116.25(13) ? C18 C13 P1 C1 . . . . -69.03(15) ? C14 C13 P1 Sn1 . . . . -84.44(13) ? C18 C13 P1 Sn1 . . . . 90.28(15) ? C6 C1 P1 C7 . . . . 94.48(15) ? C2 C1 P1 C7 . . . . -82.77(13) ? C6 C1 P1 C13 . . . . -21.80(16) ? C2 C1 P1 C13 . . . . 160.95(12) ? C6 C1 P1 Sn1 . . . . -177.29(11) ? C2 C1 P1 Sn1 . . . . 5.46(15) ? C20 C19 Sn1 C8 . . . . -43.45(11) ? C24 C19 Sn1 C8 . . . . 147.30(10) ? C20 C19 Sn1 P1 . . . . -107.53(10) ? C24 C19 Sn1 P1 . . . . 83.21(10) ? C9 C8 Sn1 C19 . . . . 90.88(13) ? C7 C8 Sn1 C19 . . . . -102.65(9) ? C9 C8 Sn1 P1 . . . . -175.82(14) ? C7 C8 Sn1 P1 . . . . -9.36(7) ? C7 P1 Sn1 C19 . . . . 109.71(5) ? C13 P1 Sn1 C19 . . . . -143.15(6) ? C1 P1 Sn1 C19 . . . . 9.67(7) ? C7 P1 Sn1 C8 . . . . 7.02(5) ? C13 P1 Sn1 C8 . . . . 114.16(6) ? C1 P1 Sn1 C8 . . . . -93.02(7) ? #===END data_global _audit_update_record ; 2012-03-15 # Formatted by publCIF ; _audit_creation_method SHELXL-97 # 1. Submission Details _publ_contact_author_name 'Lars Wesemann' _publ_contact_author_address ; Institut fuer Anorganische Chemie Universitaet Tuebingen Auf der Morgenstelle 18 72076 Tuebingen Germany ; _publ_contact_author_email 'lars.wesemann@uni-tuebingen.de' _publ_contact_author_fax '0049-7071-292436' _publ_contact_author_phone '0049-7071-2976227' _publ_requested_journal ? _publ_requested_category ? _publ_requested_coeditor_name ? _publ_contact_letter ? # 2. Processing Summary (IUCr Office Use Only) _journal_date_recd_electronic ? _journal_date_to_coeditor ? _journal_date_from_coeditor ? _journal_date_accepted ? _journal_date_printers_first ? _journal_date_printers_final ? _journal_date_proofs_out ? _journal_date_proofs_in ? _journal_coeditor_name ? _journal_coeditor_code ? _journal_coeditor_notes ? _journal_techeditor_code ? _journal_techeditor_notes ? _journal_coden_ASTM ? _journal_name_full ? _journal_year ? _journal_volume ? _journal_issue ? _journal_page_first ? _journal_page_last ? _journal_suppl_publ_number ? _journal_suppl_publ_pages ? # 3. Titl and Author List _publ_section_title ; Title (type here to add) ; # The loop structure below should contain the names and addresses of all # authors, in the required order of publication. Repeat as necessary. loop_ _publ_author_name _publ_author_address 'Freitag, Sarah' #<--'Last name, first name' ; Institut fuer Anorganische Chemie Universitaet Tuebingen Auf der Morgenstelle 18 72076 Tuebingen Germany ; 'Henning, Jens' #<--'Last name, first name' ; Institut fuer Anorganische Chemie Universitaet Tuebingen Auf der Morgenstelle 18 72076 Tuebingen Germany ; 'Wesemann, Lars' #<--'Last name, first name' ; Institut fuer Anorganische Chemie Universitaet Tuebingen Auf der Morgenstelle 18 72076 Tuebingen Germany ; # 4. Text _publ_section_abstract ; (type here to add abstract) ; _publ_section_comment ; (type here to add) ; _publ_section_exptl_prep ; (type here to add preparation details) ; _publ_section_exptl_refinement ; ; _publ_section_references ; (type here to add) ; _publ_section_figure_captions ; ; _publ_section_table_legends ? _publ_section_acknowledgements ; ? ; # start Validation Reply Form _vrf_PLAT094_compound1 ; PROBLEM: Ratio of Maximum / Minimum Residual Density .... 5.03 RESPONSE: The largest residual electron density of 3.10 is located near SN1 and probably due to cut off effects. ; _vrf_PLAT213_compound1 ; PROBLEM: Atom C44 has ADP max/min Ratio ..... 4.3 prola RESPONSE: The packing of large m-terphenyl groups create cavities giving rise to pronounced thermal motion of the iso-propyl groups. ; _vrf_PLAT220_compound1 ; PROBLEM: Large Non-Solvent C Ueq(max)/Ueq(min) ... 6.8 Ratio RESPONSE: The packing of large m-terphenyl groups create cavities giving rise to pronounced thermal motion of the iso-propyl groups. ; _vrf_PLAT222_compound1 ; PROBLEM: Large Non-Solvent H Uiso(max)/Uiso(min) .. 6.9 Ratio RESPONSE: The packing of large m-terphenyl groups create cavities giving rise to pronounced thermal motion of the iso-propyl groups. ; _vrf_PLAT250_compound1 ; PROBLEM: Large Non-Solvent C Ueq(max)/Ueq(min) ... 6.8 Ratio RESPONSE: The packing of large m-terphenyl groups create cavities giving rise to pronounced thermal motion of the iso-propyl groups. ; _vrf_PLAT412_compound1 ; PROBLEM: Short Intra XH3 .. XHn H49 .. H20E .. 1.89 Ang. RESPONSE: The 2,4,6-(tri-iso-propyl)phenylgroup at C100 is disordered over two postions. The minor disorder is marginally occupied with a factor of 0.14. Hence, its geometry is restrained to similarity and the displacement ellipsoids are constrained to equality to the major disorder. The H-H contacts involve the minor disordered moiety and are therefore not indicating any interaction. ; _vrf_PLAT413_compound1 ; PROBLEM: Short Inter XH3 .. XHn H44C .. H20E .. 2.14 Ang. RESPONSE: The 2,4,6-(tri-iso-propyl)phenylgroup at C100 is disordered over two postions. The minor disorder is marginally occupied with a factor of 0.14. Hence, its geometry is restrained to similarity and the displacement ellipsoids are constrained to equality to the major disorder. The H-H contacts involve the minor disordered moiety and are therefore not indicating any interaction. ; _vrf_PLAT002_compound1 ; PROBLEM: Number of Distance or Angle Restraints on AtSite 30. RESPONSE: The 2,4,6-(tri-iso-propyl)phenylgroup at C100 is disordered over two postions. The minor disorder is marginally occupied with a factor of 0.14. Hence, its geometry is restrained to similarity and the displacement ellipsoids are constrained to equality to the major disorder. ; _vrf_PLAT242_compound1 ; PROBLEM: Check Low Ueq as Compared to Neighbors for C109 RESPONSE: The packing of large m-terphenyl groups create cavities giving rise to pronounced thermal motion of the iso-propyl groups. ; # end Validation Reply Form data_compound1 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C54 H71 P Sn, C6 H6' _chemical_formula_sum 'C60 H77 P Sn' _chemical_formula_weight 947.88 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' _symmetry_cell_setting monoclinic _space_group_name_H-M_alt 'P 1 21/n 1' _space_group_name_Hall '-P 2yn' 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 19.074(2) _cell_length_b 14.6578(17) _cell_length_c 19.653(2) _cell_angle_alpha 90.00 _cell_angle_beta 113.058(6) _cell_angle_gamma 90.00 _cell_volume 5055.8(10) _cell_formula_units_Z 4 _cell_measurement_reflns_used 366 _cell_measurement_theta_min 2.5433 _cell_measurement_theta_max 22.7204 _cell_measurement_temperature 100.(2) _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.13 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.245 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2008 _exptl_absorpt_coefficient_mu 0.574 _exptl_absorpt_correction_type numerical _exptl_absorpt_process_details 'SADABS V2008/1 (Bruker AXS)' _exptl_absorpt_correction_T_min 0.9275 _exptl_absorpt_correction_T_max 0.9560 _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX--II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 78406 _diffrn_reflns_av_R_equivalents 0.0358 _diffrn_reflns_av_sigmaI/netI 0.0275 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.79 _diffrn_reflns_theta_max 27.67 _reflns_number_total 11709 _reflns_number_gt 9587 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'APEX2 v2011.8--0 (Bruker AXS)' _computing_data_reduction 'SAINT V7.68A (Bruker AXS, 2009)' _computing_bruker_data_scaling 'SADABS V2008/1 (Bruker AXS)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; The 2,4,6-(tri-iso-propyl)phenylgroup at C100 is disordered over two postions. The minor disorder is marginally occupied with a factor of 0.14. Hence, its geometry is restrained to similarity and the displacement ellipsoids are constrained to equality to the major disorder. 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^)+(0.0464P)^2^+6.4803P] 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 11709 _refine_ls_number_parameters 627 _refine_ls_number_restraints 36 _refine_ls_R_factor_all 0.0517 _refine_ls_R_factor_gt 0.0371 _refine_ls_wR_factor_ref 0.0969 _refine_ls_wR_factor_gt 0.0900 _refine_ls_goodness_of_fit_ref 1.040 _refine_ls_restrained_S_all 1.039 _refine_ls_shift/su_max 0.002 _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 0.874195(9) 0.177829(11) 0.698641(8) 0.01811(6) Uani 1 1 d . . . P1 P 0.88374(3) 0.04742(4) 0.61029(3) 0.01714(12) Uani 1 1 d . . . C1 C 0.86208(13) 0.25510(16) 0.59642(13) 0.0201(5) Uani 1 1 d . . . C2 C 0.84740(15) 0.34805(17) 0.58847(14) 0.0249(5) Uani 1 1 d . . . H2 H 0.8514 0.3818 0.6311 0.030 Uiso 1 1 calc R . . C3 C 0.82681(15) 0.39595(17) 0.52064(14) 0.0284(6) Uani 1 1 d . . . H3 H 0.8185 0.4600 0.5190 0.034 Uiso 1 1 calc R . . C4 C 0.81907(14) 0.34999(18) 0.45800(14) 0.0249(5) Uani 1 1 d . . . C5 C 0.83036(13) 0.25467(16) 0.46328(13) 0.0195(5) Uani 1 1 d . . . C6 C 0.81286(13) 0.21358(17) 0.39403(13) 0.0203(5) Uani 1 1 d . . . C7 C 0.81654(14) 0.12059(18) 0.39021(13) 0.0239(5) Uani 1 1 d . . . H7 H 0.8040 0.0910 0.3439 0.029 Uiso 1 1 calc R . . C8 C 0.83942(14) 0.06921(17) 0.45656(13) 0.0232(5) Uani 1 1 d . . . H8 H 0.8422 0.0047 0.4541 0.028 Uiso 1 1 calc R . . C9 C 0.85775(13) 0.11010(16) 0.52469(13) 0.0184(5) Uani 1 1 d . . . C10 C 0.85193(13) 0.20677(16) 0.53023(13) 0.0180(5) Uani 1 1 d . . . C11 C 0.79683(17) 0.37774(18) 0.37749(14) 0.0306(6) Uani 1 1 d . . . H11A H 0.8373 0.4153 0.3717 0.037 Uiso 1 1 calc R . . H11B H 0.7487 0.4130 0.3594 0.037 Uiso 1 1 calc R . . C12 C 0.78674(16) 0.28631(18) 0.33483(14) 0.0275(6) Uani 1 1 d . . . H12A H 0.7327 0.2769 0.3015 0.033 Uiso 1 1 calc R . . H12B H 0.8182 0.2855 0.3050 0.033 Uiso 1 1 calc R . . C13 C 0.99657(12) 0.18771(15) 0.78174(12) 0.0149(4) Uani 1 1 d . A . C14 C 1.02746(13) 0.12035(15) 0.83827(12) 0.0159(4) Uani 1 1 d . . . C15 C 1.09173(13) 0.14012(16) 0.90178(13) 0.0188(5) Uani 1 1 d . A . H15 H 1.1094 0.0962 0.9404 0.023 Uiso 1 1 calc R . . C16 C 1.13067(13) 0.22226(16) 0.91016(13) 0.0193(5) Uani 1 1 d . . . H16 H 1.1758 0.2332 0.9527 0.023 Uiso 1 1 calc R A . C17 C 1.10247(13) 0.28765(16) 0.85549(13) 0.0183(5) Uani 1 1 d . A . H17 H 1.1292 0.3435 0.8599 0.022 Uiso 1 1 calc R . . C18 C 1.03486(13) 0.27244(15) 0.79354(12) 0.0154(4) Uani 1 1 d . . . C34 C 1.00321(13) 0.35773(15) 0.74876(12) 0.0175(4) Uani 1 1 d . A . C35 C 1.02536(14) 0.38644(16) 0.69190(13) 0.0211(5) Uani 1 1 d . . . C36 C 1.00388(16) 0.47398(18) 0.66200(15) 0.0303(6) Uani 1 1 d . A . H36 H 1.0183 0.4934 0.6232 0.036 Uiso 1 1 calc R . . C37 C 0.96249(16) 0.53319(17) 0.68690(16) 0.0328(6) Uani 1 1 d . . . C38 C 0.93873(15) 0.50250(18) 0.74075(16) 0.0302(6) Uani 1 1 d . A . H38 H 0.9083 0.5412 0.7569 0.036 Uiso 1 1 calc R . . C39 C 0.95837(14) 0.41547(16) 0.77225(14) 0.0215(5) Uani 1 1 d . . . C40 C 1.07494(15) 0.32749(17) 0.66531(13) 0.0233(5) Uani 1 1 d . A . H40 H 1.0776 0.2652 0.6869 0.028 Uiso 1 1 calc R . . C41 C 1.15601(15) 0.36564(18) 0.69282(15) 0.0287(6) Uani 1 1 d . . . H41A H 1.1879 0.3253 0.6771 0.043 Uiso 1 1 calc R A . H41B H 1.1771 0.3694 0.7469 0.043 Uiso 1 1 calc R . . H41C H 1.1550 0.4266 0.6720 0.043 Uiso 1 1 calc R . . C42 C 1.04246(17) 0.3179(2) 0.58083(15) 0.0361(7) Uani 1 1 d . . . H42A H 0.9895 0.2969 0.5633 0.054 Uiso 1 1 calc R A . H42B H 1.0728 0.2735 0.5668 0.054 Uiso 1 1 calc R . . H42C H 1.0443 0.3771 0.5585 0.054 Uiso 1 1 calc R . . C43 C 0.9450(2) 0.6316(2) 0.65901(19) 0.0470(9) Uani 1 1 d . A . H43 H 0.9315 0.6639 0.6971 0.056 Uiso 1 1 calc R . . C44 C 1.0109(2) 0.6800(3) 0.6575(3) 0.101(2) Uani 1 1 d . . . H44A H 1.0231 0.6571 0.6165 0.152 Uiso 1 1 calc R A . H44B H 1.0546 0.6702 0.7043 0.152 Uiso 1 1 calc R . . H44C H 0.9996 0.7454 0.6507 0.152 Uiso 1 1 calc R . . C45 C 0.87508(18) 0.6383(2) 0.58862(18) 0.0415(7) Uani 1 1 d . . . H45A H 0.8853 0.6104 0.5481 0.062 Uiso 1 1 calc R A . H45B H 0.8616 0.7026 0.5772 0.062 Uiso 1 1 calc R . . H45C H 0.8328 0.6063 0.5946 0.062 Uiso 1 1 calc R . . C46 C 0.93272(15) 0.38870(18) 0.83386(15) 0.0278(6) Uani 1 1 d . A . H46 H 0.9483 0.3239 0.8474 0.033 Uiso 1 1 calc R . . C47 C 0.97144(18) 0.4466(2) 0.90286(17) 0.0375(7) Uani 1 1 d . . . H47A H 0.9572 0.5107 0.8913 0.056 Uiso 1 1 calc R A . H47B H 1.0268 0.4403 0.9199 0.056 Uiso 1 1 calc R . . H47C H 0.9552 0.4260 0.9419 0.056 Uiso 1 1 calc R . . C48 C 0.84593(18) 0.3934(2) 0.8080(2) 0.0465(8) Uani 1 1 d . . . H48A H 0.8293 0.4571 0.7981 0.070 Uiso 1 1 calc R A . H48B H 0.8308 0.3688 0.8466 0.070 Uiso 1 1 calc R . . H48C H 0.8221 0.3574 0.7627 0.070 Uiso 1 1 calc R . . C49 C 0.97417(13) -0.01168(16) 0.62773(13) 0.0199(5) Uani 1 1 d . . . H49 H 0.9882 -0.0454 0.6755 0.024 Uiso 1 1 calc R . . C50 C 0.97108(15) -0.08165(16) 0.56886(14) 0.0239(5) Uani 1 1 d . . . H50A H 0.9597 -0.0505 0.5216 0.036 Uiso 1 1 calc R . . H50B H 0.9312 -0.1266 0.5633 0.036 Uiso 1 1 calc R . . H50C H 1.0204 -0.1126 0.5840 0.036 Uiso 1 1 calc R . . C51 C 1.03655(14) 0.05975(17) 0.63895(14) 0.0237(5) Uani 1 1 d . . . H51A H 1.0855 0.0289 0.6506 0.036 Uiso 1 1 calc R . . H51B H 1.0401 0.1003 0.6798 0.036 Uiso 1 1 calc R . . H51C H 1.0238 0.0956 0.5936 0.036 Uiso 1 1 calc R . . C52 C 0.80972(14) -0.04073(17) 0.58889(14) 0.0224(5) Uani 1 1 d . . . H52 H 0.8082 -0.0752 0.5444 0.027 Uiso 1 1 calc R . . C53 C 0.82833(16) -0.10786(18) 0.65287(15) 0.0293(6) Uani 1 1 d . . . H53A H 0.7896 -0.1560 0.6393 0.044 Uiso 1 1 calc R . . H53B H 0.8289 -0.0756 0.6967 0.044 Uiso 1 1 calc R . . H53C H 0.8785 -0.1351 0.6637 0.044 Uiso 1 1 calc R . . C54 C 0.73219(14) 0.00542(19) 0.56971(15) 0.0279(6) Uani 1 1 d . . . H54A H 0.7227 0.0481 0.5286 0.042 Uiso 1 1 calc R . . H54B H 0.7323 0.0388 0.6130 0.042 Uiso 1 1 calc R . . H54C H 0.6921 -0.0411 0.5553 0.042 Uiso 1 1 calc R . . C100 C 0.9964(2) 0.02492(17) 0.8373(3) 0.0154(5) Uani 0.856(4) 1 d PD A 1 C101 C 1.03727(18) -0.05237(18) 0.83010(19) 0.0179(6) Uani 0.856(4) 1 d PD A 1 C102 C 1.00986(19) -0.13973(18) 0.83485(17) 0.0209(6) Uani 0.856(4) 1 d PD A 1 H102 H 1.0373 -0.1912 0.8292 0.025 Uiso 0.856(4) 1 calc PR A 1 C103 C 0.94437(19) -0.15377(19) 0.84743(16) 0.0216(7) Uani 0.856(4) 1 d PD A 1 C104 C 0.90565(18) -0.0775(2) 0.85683(17) 0.0208(6) Uani 0.856(4) 1 d PD A 1 H104 H 0.8607 -0.0861 0.8660 0.025 Uiso 0.856(4) 1 calc PR A 1 C105 C 0.93071(17) 0.01174(19) 0.85326(18) 0.0174(6) Uani 0.856(4) 1 d PD A 1 C106 C 1.11583(18) -0.0465(2) 0.82626(16) 0.0203(6) Uani 0.856(4) 1 d PD A 1 H106 H 1.1224 0.0161 0.8094 0.024 Uiso 0.856(4) 1 calc PR A 1 C107 C 1.17892(19) -0.0631(3) 0.9036(2) 0.0262(7) Uani 0.856(4) 1 d PD A 1 H10A H 1.2287 -0.0641 0.8998 0.039 Uiso 0.856(4) 1 calc PR A 1 H10B H 1.1701 -0.1217 0.9228 0.039 Uiso 0.856(4) 1 calc PR A 1 H10C H 1.1780 -0.0140 0.9371 0.039 Uiso 0.856(4) 1 calc PR A 1 C108 C 1.1288(2) -0.1165(2) 0.77417(17) 0.0267(7) Uani 0.856(4) 1 d PD A 1 H10D H 1.0862 -0.1141 0.7258 0.040 Uiso 0.856(4) 1 calc PR A 1 H10E H 1.1321 -0.1778 0.7951 0.040 Uiso 0.856(4) 1 calc PR A 1 H10F H 1.1764 -0.1024 0.7684 0.040 Uiso 0.856(4) 1 calc PR A 1 C109 C 0.91873(19) -0.2514(2) 0.85402(18) 0.0275(7) Uani 0.856(4) 1 d PD A 1 H109 H 0.9546 -0.2920 0.8423 0.033 Uiso 0.856(4) 1 calc PR A 1 C110 C 0.9293(4) -0.2748(3) 0.9313(2) 0.0701(18) Uani 0.856(4) 1 d PD A 1 H11C H 0.9026 -0.2299 0.9494 0.105 Uiso 0.856(4) 1 calc PR A 1 H11D H 0.9837 -0.2741 0.9631 0.105 Uiso 0.856(4) 1 calc PR A 1 H11E H 0.9085 -0.3357 0.9322 0.105 Uiso 0.856(4) 1 calc PR A 1 C111 C 0.8433(3) -0.2736(3) 0.7996(3) 0.0611(15) Uani 0.856(4) 1 d PD A 1 H11F H 0.8404 -0.2581 0.7501 0.092 Uiso 0.856(4) 1 calc PR A 1 H11G H 0.8049 -0.2387 0.8102 0.092 Uiso 0.856(4) 1 calc PR A 1 H11H H 0.8338 -0.3390 0.8019 0.092 Uiso 0.856(4) 1 calc PR A 1 C112 C 0.89274(17) 0.0905(2) 0.87603(17) 0.0199(6) Uani 0.856(4) 1 d PD A 1 H112 H 0.9053 0.1481 0.8560 0.024 Uiso 0.856(4) 1 calc PR A 1 C113 C 0.9261(2) 0.0973(2) 0.96031(19) 0.0322(9) Uani 0.856(4) 1 d PD A 1 H11I H 0.9815 0.1052 0.9784 0.048 Uiso 0.856(4) 1 calc PR A 1 H11J H 0.9146 0.0414 0.9812 0.048 Uiso 0.856(4) 1 calc PR A 1 H11K H 0.9037 0.1498 0.9754 0.048 Uiso 0.856(4) 1 calc PR A 1 C114 C 0.80533(18) 0.0824(3) 0.8470(2) 0.0330(8) Uani 0.856(4) 1 d PD A 1 H11L H 0.7845 0.0731 0.7933 0.049 Uiso 0.856(4) 1 calc PR A 1 H11M H 0.7842 0.1386 0.8584 0.049 Uiso 0.856(4) 1 calc PR A 1 H11N H 0.7917 0.0305 0.8708 0.049 Uiso 0.856(4) 1 calc PR A 1 C900 C 0.8629(2) 0.3816(3) 0.1020(2) 0.0564(10) Uani 1 1 d . . . H900 H 0.9053 0.3914 0.0889 0.068 Uiso 1 1 calc R . . C901 C 0.8066(2) 0.3177(2) 0.06301(19) 0.0459(8) Uani 1 1 d . . . H901 H 0.8106 0.2841 0.0234 0.055 Uiso 1 1 calc R . . C902 C 0.74603(17) 0.30415(18) 0.08219(16) 0.0330(6) Uani 1 1 d . . . H902 H 0.7080 0.2608 0.0559 0.040 Uiso 1 1 calc R . . C903 C 0.73958(19) 0.3528(2) 0.13935(17) 0.0382(7) Uani 1 1 d . . . H903 H 0.6971 0.3434 0.1523 0.046 Uiso 1 1 calc R . . C904 C 0.7950(2) 0.4153(2) 0.17773(18) 0.0517(10) Uani 1 1 d . . . H904 H 0.7908 0.4486 0.2174 0.062 Uiso 1 1 calc R . . C905 C 0.8563(2) 0.4296(2) 0.1590(2) 0.0585(11) Uani 1 1 d . . . H905 H 0.8942 0.4728 0.1856 0.070 Uiso 1 1 calc R . . C200 C 0.9821(15) 0.0333(6) 0.838(2) 0.0154(5) Uani 0.144(4) 1 d PD A 2 C201 C 1.0167(9) -0.0501(7) 0.8332(13) 0.0179(6) Uani 0.144(4) 1 d PD A 2 C202 C 0.9815(9) -0.1322(7) 0.8382(12) 0.0209(6) Uani 0.144(4) 1 d PD A 2 H202 H 1.0015 -0.1879 0.8286 0.025 Uiso 0.144(4) 1 calc PR A 2 C203 C 0.9186(8) -0.1351(7) 0.8565(10) 0.0216(7) Uani 0.144(4) 1 d PD A 2 C204 C 0.8883(9) -0.0527(7) 0.8674(12) 0.0208(6) Uani 0.144(4) 1 d PD A 2 H204 H 0.8463 -0.0537 0.8819 0.025 Uiso 0.144(4) 1 calc PR A 2 C205 C 0.9176(8) 0.0320(7) 0.8576(11) 0.0174(6) Uani 0.144(4) 1 d PD A 2 C206 C 1.0891(8) -0.0567(9) 0.8178(9) 0.0203(6) Uani 0.144(4) 1 d PD A 2 H206 H 1.0936 0.0000 0.7915 0.024 Uiso 0.144(4) 1 calc PR A 2 C207 C 1.1598(10) -0.064(2) 0.8910(12) 0.0262(7) Uani 0.144(4) 1 d PD A 2 H20A H 1.2023 -0.0900 0.8815 0.039 Uiso 0.144(4) 1 calc PR A 2 H20B H 1.1482 -0.1028 0.9257 0.039 Uiso 0.144(4) 1 calc PR A 2 H20C H 1.1739 -0.0027 0.9125 0.039 Uiso 0.144(4) 1 calc PR A 2 C208 C 1.0920(11) -0.1395(12) 0.7710(9) 0.0267(7) Uani 0.144(4) 1 d PD A 2 H20D H 1.1313 -0.1298 0.7513 0.040 Uiso 0.144(4) 1 calc PR A 2 H20E H 1.0424 -0.1470 0.7299 0.040 Uiso 0.144(4) 1 calc PR A 2 H20F H 1.1040 -0.1945 0.8018 0.040 Uiso 0.144(4) 1 calc PR A 2 C209 C 0.8831(9) -0.2277(7) 0.8607(8) 0.0275(7) Uani 0.144(4) 1 d PD A 2 H209 H 0.9265 -0.2716 0.8734 0.033 Uiso 0.144(4) 1 calc PR A 2 C210 C 0.8585(19) -0.2351(14) 0.9231(12) 0.0701(18) Uani 0.144(4) 1 d PD A 2 H21A H 0.8277 -0.2903 0.9172 0.105 Uiso 0.144(4) 1 calc PR A 2 H21B H 0.8281 -0.1814 0.9237 0.105 Uiso 0.144(4) 1 calc PR A 2 H21C H 0.9034 -0.2384 0.9697 0.105 Uiso 0.144(4) 1 calc PR A 2 C211 C 0.8282(18) -0.260(2) 0.7905(10) 0.0611(15) Uani 0.144(4) 1 d PD A 2 H21D H 0.8130 -0.3227 0.7963 0.092 Uiso 0.144(4) 1 calc PR A 2 H21E H 0.8511 -0.2596 0.7537 0.092 Uiso 0.144(4) 1 calc PR A 2 H21F H 0.7832 -0.2206 0.7739 0.092 Uiso 0.144(4) 1 calc PR A 2 C212 C 0.8898(8) 0.1182(8) 0.8820(9) 0.0199(6) Uani 0.144(4) 1 d PD A 2 H212 H 0.9047 0.1713 0.8587 0.024 Uiso 0.144(4) 1 calc PR A 2 C213 C 0.9303(13) 0.1281(17) 0.9657(10) 0.0322(9) Uani 0.144(4) 1 d PD A 2 H21G H 0.9145 0.1852 0.9814 0.048 Uiso 0.144(4) 1 calc PR A 2 H21H H 0.9855 0.1289 0.9794 0.048 Uiso 0.144(4) 1 calc PR A 2 H21I H 0.9168 0.0765 0.9900 0.048 Uiso 0.144(4) 1 calc PR A 2 C214 C 0.8029(8) 0.1223(14) 0.8594(13) 0.0330(8) Uani 0.144(4) 1 d PD A 2 H21J H 0.7896 0.1786 0.8785 0.049 Uiso 0.144(4) 1 calc PR A 2 H21K H 0.7864 0.0695 0.8799 0.049 Uiso 0.144(4) 1 calc PR A 2 H21L H 0.7775 0.1214 0.8053 0.049 Uiso 0.144(4) 1 calc PR A 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 0.01867(9) 0.02051(9) 0.01374(8) -0.00179(6) 0.00481(6) -0.00119(6) P1 0.0180(3) 0.0164(3) 0.0151(3) -0.0005(2) 0.0044(2) -0.0014(2) C1 0.0170(11) 0.0210(11) 0.0191(11) -0.0007(9) 0.0034(9) -0.0007(9) C2 0.0258(13) 0.0230(12) 0.0184(12) -0.0034(10) 0.0007(10) 0.0008(10) C3 0.0312(14) 0.0162(11) 0.0269(13) 0.0006(10) -0.0003(11) -0.0001(10) C4 0.0226(12) 0.0237(12) 0.0216(12) 0.0046(10) 0.0015(10) -0.0013(10) C5 0.0159(11) 0.0226(12) 0.0183(11) 0.0007(9) 0.0046(9) -0.0021(9) C6 0.0153(11) 0.0283(12) 0.0158(11) 0.0026(9) 0.0043(9) 0.0011(9) C7 0.0234(12) 0.0294(13) 0.0153(11) -0.0036(10) 0.0039(10) 0.0040(10) C8 0.0239(12) 0.0222(12) 0.0206(12) -0.0011(10) 0.0055(10) 0.0029(10) C9 0.0163(11) 0.0207(11) 0.0162(11) 0.0005(9) 0.0041(9) 0.0006(9) C10 0.0127(10) 0.0216(11) 0.0173(11) 0.0009(9) 0.0034(9) -0.0011(9) C11 0.0377(15) 0.0252(13) 0.0225(13) 0.0073(10) 0.0046(11) -0.0007(11) C12 0.0303(14) 0.0298(13) 0.0201(12) 0.0057(10) 0.0074(11) 0.0002(11) C13 0.0157(10) 0.0169(10) 0.0136(10) -0.0017(8) 0.0074(9) 0.0004(8) C14 0.0182(11) 0.0148(10) 0.0165(11) -0.0016(8) 0.0089(9) 0.0007(8) C15 0.0209(11) 0.0166(11) 0.0184(11) 0.0027(9) 0.0071(9) 0.0032(9) C16 0.0152(11) 0.0214(11) 0.0183(11) -0.0011(9) 0.0031(9) 0.0012(9) C17 0.0180(11) 0.0157(10) 0.0224(12) -0.0016(9) 0.0092(9) -0.0018(9) C18 0.0177(11) 0.0160(10) 0.0150(10) -0.0003(8) 0.0092(9) 0.0016(8) C34 0.0177(11) 0.0135(10) 0.0171(11) -0.0008(9) 0.0021(9) -0.0039(9) C35 0.0230(12) 0.0201(11) 0.0153(11) -0.0011(9) 0.0023(9) -0.0065(9) C36 0.0347(15) 0.0250(13) 0.0225(13) 0.0064(10) 0.0018(11) -0.0082(11) C37 0.0324(14) 0.0174(12) 0.0341(15) 0.0064(11) -0.0025(12) -0.0015(11) C38 0.0254(13) 0.0197(12) 0.0364(15) -0.0022(11) 0.0024(12) 0.0045(10) C39 0.0180(11) 0.0173(11) 0.0242(12) -0.0027(9) 0.0029(10) -0.0015(9) C40 0.0290(13) 0.0228(12) 0.0201(12) -0.0009(10) 0.0117(10) -0.0091(10) C41 0.0251(13) 0.0267(13) 0.0300(14) 0.0009(11) 0.0062(11) -0.0029(11) C42 0.0307(15) 0.0571(19) 0.0225(13) -0.0062(13) 0.0124(12) -0.0119(13) C43 0.056(2) 0.0206(14) 0.0462(19) 0.0086(13) 0.0006(16) 0.0023(13) C44 0.056(3) 0.0347(19) 0.146(5) 0.053(3) -0.033(3) -0.0170(18) C45 0.0410(17) 0.0279(15) 0.0435(18) 0.0120(13) 0.0035(14) 0.0051(13) C46 0.0289(14) 0.0231(12) 0.0359(15) -0.0061(11) 0.0176(12) 0.0007(10) C47 0.0450(17) 0.0361(16) 0.0350(16) -0.0081(13) 0.0196(14) -0.0026(13) C48 0.0334(17) 0.0502(19) 0.062(2) -0.0210(17) 0.0260(16) -0.0051(14) C49 0.0193(11) 0.0199(11) 0.0180(11) 0.0029(9) 0.0046(9) 0.0016(9) C50 0.0260(13) 0.0191(12) 0.0258(13) 0.0013(10) 0.0092(11) 0.0021(10) C51 0.0218(12) 0.0244(12) 0.0252(12) -0.0010(10) 0.0096(10) -0.0011(10) C52 0.0217(12) 0.0214(12) 0.0237(12) -0.0037(10) 0.0083(10) -0.0055(10) C53 0.0283(14) 0.0261(13) 0.0329(14) 0.0025(11) 0.0114(12) -0.0057(11) C54 0.0231(13) 0.0292(13) 0.0283(14) -0.0012(11) 0.0068(11) -0.0039(10) C100 0.019(2) 0.0142(11) 0.0119(10) 0.0023(11) 0.0042(15) -0.0005(10) C101 0.0217(18) 0.0170(11) 0.0133(11) 0.0009(9) 0.0050(13) 0.0006(11) C102 0.0253(18) 0.0140(12) 0.0204(13) 0.0005(10) 0.0056(14) 0.0031(12) C103 0.0268(18) 0.0167(13) 0.0179(13) 0.0007(11) 0.0051(12) -0.0027(12) C104 0.0219(16) 0.0252(16) 0.0167(14) 0.0008(12) 0.0092(11) -0.0050(13) C105 0.0191(14) 0.0185(14) 0.0128(11) 0.0022(11) 0.0044(10) 0.0014(11) C106 0.0186(16) 0.0191(13) 0.0210(14) 0.0012(10) 0.0052(14) 0.0033(12) C107 0.0245(19) 0.0253(13) 0.0241(18) 0.0007(14) 0.0046(14) 0.0058(17) C108 0.0283(18) 0.0296(16) 0.0213(14) 0.0036(12) 0.0086(14) 0.0104(14) C109 0.0333(18) 0.0176(14) 0.0336(16) -0.0003(12) 0.0153(14) -0.0024(12) C110 0.157(5) 0.0236(19) 0.037(2) -0.0012(16) 0.046(3) -0.031(2) C111 0.043(3) 0.029(2) 0.088(3) 0.014(2) 0.001(2) -0.013(2) C112 0.0229(13) 0.0209(16) 0.0183(13) 0.0025(13) 0.0106(10) 0.0001(12) C113 0.0466(19) 0.032(2) 0.0205(14) 0.0005(15) 0.0162(13) 0.0090(18) C114 0.0237(15) 0.034(2) 0.043(2) 0.0031(17) 0.0154(14) 0.0052(15) C900 0.0383(19) 0.050(2) 0.073(3) 0.035(2) 0.0126(18) 0.0039(16) C901 0.064(2) 0.0335(16) 0.0406(18) 0.0165(14) 0.0207(17) 0.0136(15) C902 0.0381(16) 0.0224(13) 0.0275(14) 0.0051(11) 0.0009(12) -0.0014(11) C903 0.0447(18) 0.0261(14) 0.0374(16) 0.0105(12) 0.0090(14) 0.0091(13) C904 0.081(3) 0.0243(15) 0.0305(16) 0.0018(12) 0.0003(17) 0.0030(16) C905 0.055(2) 0.0358(18) 0.049(2) 0.0164(16) -0.0173(18) -0.0131(16) C200 0.019(2) 0.0142(11) 0.0119(10) 0.0023(11) 0.0042(15) -0.0005(10) C201 0.0217(18) 0.0170(11) 0.0133(11) 0.0009(9) 0.0050(13) 0.0006(11) C202 0.0253(18) 0.0140(12) 0.0204(13) 0.0005(10) 0.0056(14) 0.0031(12) C203 0.0268(18) 0.0167(13) 0.0179(13) 0.0007(11) 0.0051(12) -0.0027(12) C204 0.0219(16) 0.0252(16) 0.0167(14) 0.0008(12) 0.0092(11) -0.0050(13) C205 0.0191(14) 0.0185(14) 0.0128(11) 0.0022(11) 0.0044(10) 0.0014(11) C206 0.0186(16) 0.0191(13) 0.0210(14) 0.0012(10) 0.0052(14) 0.0033(12) C207 0.0245(19) 0.0253(13) 0.0241(18) 0.0007(14) 0.0046(14) 0.0058(17) C208 0.0283(18) 0.0296(16) 0.0213(14) 0.0036(12) 0.0086(14) 0.0104(14) C209 0.0333(18) 0.0176(14) 0.0336(16) -0.0003(12) 0.0153(14) -0.0024(12) C210 0.157(5) 0.0236(19) 0.037(2) -0.0012(16) 0.046(3) -0.031(2) C211 0.043(3) 0.029(2) 0.088(3) 0.014(2) 0.001(2) -0.013(2) C212 0.0229(13) 0.0209(16) 0.0183(13) 0.0025(13) 0.0106(10) 0.0001(12) C213 0.0466(19) 0.032(2) 0.0205(14) 0.0005(15) 0.0162(13) 0.0090(18) C214 0.0237(15) 0.034(2) 0.043(2) 0.0031(17) 0.0154(14) 0.0052(15) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Sn1 C1 2.238(2) . ? Sn1 C13 2.269(2) . ? Sn1 P1 2.6362(6) . ? P1 C9 1.807(2) . ? P1 C52 1.837(2) . ? P1 C49 1.838(2) . ? C1 C2 1.387(3) . ? C1 C10 1.426(3) . ? C2 C3 1.419(4) . ? C3 C4 1.360(4) . ? C4 C5 1.411(4) . ? C4 C11 1.524(3) . ? C5 C10 1.403(3) . ? C5 C6 1.404(3) . ? C6 C7 1.368(4) . ? C6 C12 1.511(3) . ? C7 C8 1.419(3) . ? C8 C9 1.381(3) . ? C9 C10 1.429(3) . ? C11 C12 1.552(4) . ? C13 C18 1.413(3) . ? C13 C14 1.430(3) . ? C14 C15 1.395(3) . ? C14 C100 1.517(3) . ? C14 C200 1.542(11) . ? C15 C16 1.390(3) . ? C16 C17 1.382(3) . ? C17 C18 1.402(3) . ? C18 C34 1.512(3) . ? C34 C39 1.404(3) . ? C34 C35 1.405(3) . ? C35 C36 1.404(3) . ? C35 C40 1.517(4) . ? C36 C37 1.385(4) . ? C37 C38 1.380(4) . ? C37 C43 1.532(4) . ? C38 C39 1.403(3) . ? C39 C46 1.524(4) . ? C40 C41 1.530(3) . ? C40 C42 1.535(4) . ? C43 C44 1.455(6) . ? C43 C45 1.502(4) . ? C46 C47 1.523(4) . ? C46 C48 1.531(4) . ? C49 C50 1.530(3) . ? C49 C51 1.535(3) . ? C52 C53 1.525(4) . ? C52 C54 1.533(4) . ? C100 C101 1.414(4) . ? C100 C105 1.418(4) . ? C101 C102 1.400(4) . ? C101 C106 1.532(4) . ? C102 C103 1.380(4) . ? C103 C104 1.392(4) . ? C103 C109 1.534(4) . ? C104 C105 1.404(4) . ? C105 C112 1.520(4) . ? C106 C108 1.537(4) . ? C106 C107 1.544(4) . ? C109 C111 1.454(5) . ? C109 C110 1.493(5) . ? C112 C113 1.527(4) . ? C112 C114 1.541(4) . ? C900 C905 1.370(6) . ? C900 C901 1.405(5) . ? C901 C902 1.362(5) . ? C902 C903 1.376(4) . ? C903 C904 1.378(5) . ? C904 C905 1.373(6) . ? C200 C201 1.412(5) . ? C200 C205 1.420(5) . ? C201 C202 1.401(5) . ? C201 C206 1.530(5) . ? C202 C203 1.382(6) . ? C203 C204 1.390(6) . ? C203 C209 1.532(5) . ? C204 C205 1.405(5) . ? C205 C212 1.519(6) . ? C206 C208 1.537(6) . ? C206 C207 1.543(6) . ? C209 C211 1.449(7) . ? C209 C210 1.479(7) . ? C212 C213 1.526(6) . ? C212 C214 1.539(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Sn1 C13 109.22(8) . . ? C1 Sn1 P1 77.59(6) . . ? C13 Sn1 P1 101.74(6) . . ? C9 P1 C52 103.79(11) . . ? C9 P1 C49 107.96(11) . . ? C52 P1 C49 106.98(11) . . ? C9 P1 Sn1 100.37(8) . . ? C52 P1 Sn1 114.56(8) . . ? C49 P1 Sn1 121.38(8) . . ? C2 C1 C10 115.8(2) . . ? C2 C1 Sn1 122.91(18) . . ? C10 C1 Sn1 119.79(17) . . ? C1 C2 C3 124.1(2) . . ? C4 C3 C2 119.8(2) . . ? C3 C4 C5 117.7(2) . . ? C3 C4 C11 134.0(2) . . ? C5 C4 C11 108.2(2) . . ? C10 C5 C6 124.4(2) . . ? C10 C5 C4 123.0(2) . . ? C6 C5 C4 112.5(2) . . ? C7 C6 C5 118.9(2) . . ? C7 C6 C12 132.0(2) . . ? C5 C6 C12 109.0(2) . . ? C6 C7 C8 118.8(2) . . ? C9 C8 C7 122.1(2) . . ? C8 C9 C10 120.4(2) . . ? C8 C9 P1 123.69(19) . . ? C10 C9 P1 115.75(17) . . ? C5 C10 C1 119.5(2) . . ? C5 C10 C9 115.3(2) . . ? C1 C10 C9 125.1(2) . . ? C4 C11 C12 104.8(2) . . ? C6 C12 C11 105.0(2) . . ? C18 C13 C14 116.8(2) . . ? C18 C13 Sn1 119.60(16) . . ? C14 C13 Sn1 120.65(15) . . ? C15 C14 C13 120.1(2) . . ? C15 C14 C100 113.9(3) . . ? C13 C14 C100 126.0(3) . . ? C15 C14 C200 117.8(15) . . ? C13 C14 C200 120.8(14) . . ? C16 C15 C14 121.8(2) . . ? C17 C16 C15 118.8(2) . . ? C16 C17 C18 120.7(2) . . ? C17 C18 C13 121.5(2) . . ? C17 C18 C34 113.32(19) . . ? C13 C18 C34 124.6(2) . . ? C39 C34 C35 119.5(2) . . ? C39 C34 C18 117.6(2) . . ? C35 C34 C18 122.3(2) . . ? C36 C35 C34 118.5(2) . . ? C36 C35 C40 119.7(2) . . ? C34 C35 C40 121.7(2) . . ? C37 C36 C35 122.6(3) . . ? C38 C37 C36 118.1(2) . . ? C38 C37 C43 119.4(3) . . ? C36 C37 C43 122.5(3) . . ? C37 C38 C39 121.6(3) . . ? C38 C39 C34 119.7(2) . . ? C38 C39 C46 118.1(2) . . ? C34 C39 C46 122.2(2) . . ? C35 C40 C41 110.5(2) . . ? C35 C40 C42 112.5(2) . . ? C41 C40 C42 109.9(2) . . ? C44 C43 C45 114.3(3) . . ? C44 C43 C37 113.4(3) . . ? C45 C43 C37 112.4(3) . . ? C47 C46 C39 111.7(2) . . ? C47 C46 C48 110.8(2) . . ? C39 C46 C48 111.5(2) . . ? C50 C49 C51 111.3(2) . . ? C50 C49 P1 114.81(17) . . ? C51 C49 P1 108.86(16) . . ? C53 C52 C54 112.2(2) . . ? C53 C52 P1 110.80(17) . . ? C54 C52 P1 109.07(17) . . ? C101 C100 C105 118.9(2) . . ? C101 C100 C14 120.7(2) . . ? C105 C100 C14 119.9(2) . . ? C102 C101 C100 119.4(3) . . ? C102 C101 C106 116.9(2) . . ? C100 C101 C106 123.3(2) . . ? C103 C102 C101 122.4(3) . . ? C102 C103 C104 117.9(2) . . ? C102 C103 C109 119.7(3) . . ? C104 C103 C109 122.3(3) . . ? C103 C104 C105 122.2(3) . . ? C104 C105 C100 119.0(2) . . ? C104 C105 C112 118.8(2) . . ? C100 C105 C112 121.7(2) . . ? C101 C106 C108 114.3(3) . . ? C101 C106 C107 110.1(2) . . ? C108 C106 C107 106.5(2) . . ? C111 C109 C110 113.4(4) . . ? C111 C109 C103 113.8(3) . . ? C110 C109 C103 112.3(3) . . ? C105 C112 C113 109.0(2) . . ? C105 C112 C114 113.8(3) . . ? C113 C112 C114 109.7(2) . . ? C905 C900 C901 119.5(4) . . ? C902 C901 C900 119.8(3) . . ? C901 C902 C903 120.4(3) . . ? C902 C903 C904 119.7(3) . . ? C905 C904 C903 120.4(3) . . ? C900 C905 C904 120.1(3) . . ? C201 C200 C205 119.0(4) . . ? C201 C200 C14 115.9(7) . . ? C205 C200 C14 123.9(7) . . ? C202 C201 C200 119.3(4) . . ? C202 C201 C206 117.0(4) . . ? C200 C201 C206 123.6(4) . . ? C203 C202 C201 122.2(4) . . ? C202 C203 C204 118.0(4) . . ? C202 C203 C209 119.1(5) . . ? C204 C203 C209 122.8(5) . . ? C203 C204 C205 122.3(4) . . ? C204 C205 C200 118.7(4) . . ? C204 C205 C212 119.0(5) . . ? C200 C205 C212 121.2(5) . . ? C201 C206 C208 114.5(5) . . ? C201 C206 C207 110.3(5) . . ? C208 C206 C207 106.5(5) . . ? C211 C209 C210 114.8(6) . . ? C211 C209 C203 114.3(5) . . ? C210 C209 C203 113.5(5) . . ? C205 C212 C213 109.1(5) . . ? C205 C212 C214 114.3(5) . . ? C213 C212 C214 109.9(5) . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 27.67 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 3.096 _refine_diff_density_min -0.616 _refine_diff_density_rms 0.078 #===END data_global _audit_update_record ; 2012-03-15 # Formatted by publCIF ; _audit_creation_method SHELXL-97 # 1. Submission Details _publ_contact_author_name 'Lars Wesemann' _publ_contact_author_address ; Institut fuer Anorganische Chemie Universitaet Tuebingen Auf der Morgenstelle 18 72076 Tuebingen Germany ; _publ_contact_author_email 'lars.wesemann@uni-tuebingen.de' _publ_contact_author_fax '0049-7071-292436' _publ_contact_author_phone '0049-7071-2976227' _publ_requested_journal ? _publ_requested_category ? _publ_requested_coeditor_name ? _publ_contact_letter ? # 2. Processing Summary (IUCr Office Use Only) _journal_date_recd_electronic ? _journal_date_to_coeditor ? _journal_date_from_coeditor ? _journal_date_accepted ? _journal_date_printers_first ? _journal_date_printers_final ? _journal_date_proofs_out ? _journal_date_proofs_in ? _journal_coeditor_name ? _journal_coeditor_code ? _journal_coeditor_notes ? _journal_techeditor_code ? _journal_techeditor_notes ? _journal_coden_ASTM ? _journal_name_full ? _journal_year ? _journal_volume ? _journal_issue ? _journal_page_first ? _journal_page_last ? _journal_suppl_publ_number ? _journal_suppl_publ_pages ? # 3. Titl and Author List _publ_section_title ; Title (type here to add) ; # The loop structure below should contain the names and addresses of all # authors, in the required order of publication. Repeat as necessary. loop_ _publ_author_name _publ_author_address 'Krebs, Kilian' #<--'Last name, first name' ; Institut fuer Anorganische Chemie Universitaet Tuebingen Auf der Morgenstelle 18 72076 Tuebingen Germany ; 'Henning, Jens' #<--'Last name, first name' ; Institut fuer Anorganische Chemie Universitaet Tuebingen Auf der Morgenstelle 18 72076 Tuebingen Germany ; 'Wesemann, Lars' #<--'Last name, first name' ; Institut fuer Anorganische Chemie Universitaet Tuebingen Auf der Morgenstelle 18 72076 Tuebingen Germany ; # 4. Text _publ_section_abstract ; (type here to add abstract) ; _publ_section_comment ; (type here to add) ; _publ_section_exptl_prep ; (type here to add preparation details) ; _publ_section_exptl_refinement ; ; _publ_section_references ; (type here to add) ; _publ_section_figure_captions ; ; _publ_section_table_legends ? _publ_section_acknowledgements ; ? ; # start Validation Reply Form _vrf_PLAT094_SnPhPHCCPh ; PROBLEM: Ratio of Maximum / Minimum Residual Density .... 2.34 RESPONSE: The largest residual electron density is located 0.95 Angstrom next to the tin atom and probably due to cut off effects. ; _vrf_PLAT220_SnPhPHCCPh ; PROBLEM: Large Non-Solvent C Ueq(max)/Ueq(min) ... 3.4 Ratio RESPONSE: The packing of large m-terphenyl groups create cavities giving rise to pronounced thermal motion of the iso-propyl groups. ; _vrf_FORMU01_SnPhPHCCPh ; PROBLEM: There is a discrepancy between the atom counts in the _chemical_formula_sum and _chemical_formula_moiety. This is usually due to the moiety formula being in the wrong format. Atom count from _chemical_formula_sum: C65 H72 P1 Sn1 Atom count from _chemical_formula_moiety:C73 H87 P1 Sn1 RESPONSE: The structure contains canal like cavities in which one molecule of benzene per unit cell could be located and aditionally one molecule of benzene or pentane is heavily disordered. The latter were handeled with the BYPASS algorithm as implented in PLATON. ; _vrf_PLAT002_SnPhPHCCPh ; PROBLEM: Number of Distance or Angle Restraints on AtSite 2 RESPONSE: The postional parameters of H100 were refinded with a DFIX restraint being applied for the C100-H100 distance. ; _vrf_PLAT042_SnPhPHCCPh ; PROBLEM: Calc. and Reported MoietyFormula Strings Differ ? RESPONSE: The structure contains canal like cavities in which one molecule of benzene per unit cell could be located and aditionally one molecule of benzene or pentane is heavily disordered. The latter were handeled with the BYPASS algorithm as implented in PLATON. ; _vrf_PLAT164_SnPhPHCCPh ; PROBLEM: Nr. of Refined C-H H-Atoms in Heavy-Atom Struct. 1 RESPONSE: The postional parameters of H100 were refinded with a DFIX restraint being applied for the C100-H100 distance. ; _vrf_PLAT244_SnPhPHCCPh ; PROBLEM: Low 'Solvent' Ueq as Compared to Neighbors of C201 RESPONSE: The located benzene molecule is disordered. However, the applied split model does not account entirely for the pronounced disorder. ; _vrf_PLAT605_SnPhPHCCPh ; PROBLEM: Structure Contains Solvent Accessible VOIDS of . 325 A**3 RESPONSE: The structure contains canal like cavities in which one molecule of benzene per unit cell could be located and aditionally one molecule of benzene or pentane is heavily disordered. The latter were handeled with the BYPASS algorithm as implented in PLATON. ; _vrf_PLAT869_SnPhPHCCPh ; PROBLEM: ALERTS Related to the use of SQUEEZE Suppressed RESPONSE: The structure contains canal like cavities in which one molecule of benzene per unit cell could be located and aditionally one molecule of benzene or pentane is heavily disordered. The latter were handeled with the BYPASS algorithm as implented in PLATON. ; _vrf_PLAT961_SnPhPHCCPh ; PROBLEM: Dataset Contains no Negative Intensities ....... ! RESPONSE: The structure contains canal like cavities in which one molecule of benzene per unit cell could be located and aditionally one molecule of benzene or pentane is heavily disordered. The latter were handeled with the BYPASS algorithm as implented in PLATON. ; # end Validation Reply Form data_SnPhPHCCPh _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C62 H69 P Sn, 0.5(C6 H6), 0.5(C5 H12)' _chemical_formula_sum 'C65 H72 P Sn' _chemical_formula_weight 1002.89 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' _symmetry_cell_setting monoclinic _space_group_name_H-M_alt 'P 1 21/c 1' _space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 12.4011(5) _cell_length_b 18.8054(8) _cell_length_c 24.7687(10) _cell_angle_alpha 90.00 _cell_angle_beta 93.0458(19) _cell_angle_gamma 90.00 _cell_volume 5768.1(4) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9949 _cell_measurement_theta_min 2.2647 _cell_measurement_theta_max 27.0797 _exptl_crystal_description plate _exptl_crystal_colour orange _exptl_crystal_size_max 0.46 _exptl_crystal_size_mid 0.34 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.155 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2108 _exptl_absorpt_coefficient_mu 0.507 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.7999 _exptl_absorpt_correction_T_max 0.9389 _exptl_absorpt_process_details 'SADABS V2008/1 (Bruker AXS)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX--II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 182209 _diffrn_reflns_av_R_equivalents 0.0232 _diffrn_reflns_av_sigmaI/netI 0.0121 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 1.64 _diffrn_reflns_theta_max 27.51 _reflns_number_total 13235 _reflns_number_gt 12269 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 v2011.8-0 (Bruker AXS)' _computing_cell_refinement 'APEX2 v2011.8-0 (Bruker AXS)' _computing_data_reduction 'SAINT V7.68A (Bruker AXS, 2009)' _computing_bruker_data_scaling 'SADABS V2008/1 (Bruker AXS)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; The geometry of the benzene molecule was constrained using AFIX 66 and the carbon atoms were refined isotropically. The postional parameters of H100 were refinded with a DFIX restraint being applied for the C100-H100 distance. 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^)+(0.0300P)^2^+5.5784P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 13235 _refine_ls_number_parameters 604 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0310 _refine_ls_R_factor_gt 0.0281 _refine_ls_wR_factor_ref 0.0707 _refine_ls_wR_factor_gt 0.0695 _refine_ls_goodness_of_fit_ref 1.077 _refine_ls_restrained_S_all 1.077 _refine_ls_shift/su_max 0.006 _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 0.282613(8) 0.487499(6) 0.873014(4) 0.01291(4) Uani 1 1 d . . . P1 P 0.05650(3) 0.60349(2) 0.857857(15) 0.01189(8) Uani 1 1 d . . . C1 C 0.11930(12) 0.46403(9) 0.83658(6) 0.0141(3) Uani 1 1 d . . . C2 C 0.03425(12) 0.51364(8) 0.83461(6) 0.0137(3) Uani 1 1 d . . . C3 C -0.07165(13) 0.49509(9) 0.81706(7) 0.0164(3) Uani 1 1 d . . . H3 H -0.1276 0.5296 0.8168 0.020 Uiso 1 1 calc R . . C4 C -0.09391(13) 0.42624(9) 0.80013(7) 0.0191(3) Uani 1 1 d . . . H4 H -0.1656 0.4129 0.7890 0.023 Uiso 1 1 calc R . . C6 C 0.09301(13) 0.39546(9) 0.81804(6) 0.0165(3) Uani 1 1 d . . . H6 H 0.1483 0.3605 0.8181 0.020 Uiso 1 1 calc R . . C5 C -0.01089(14) 0.37675(9) 0.79953(7) 0.0188(3) Uani 1 1 d . . . H5 H -0.0251 0.3300 0.7864 0.023 Uiso 1 1 calc R . . C7 C -0.04521(12) 0.65791(8) 0.82345(6) 0.0141(3) Uani 1 1 d . . . C8 C -0.12337(13) 0.69588(9) 0.84969(7) 0.0171(3) Uani 1 1 d . . . H8 H -0.1271 0.6927 0.8878 0.021 Uiso 1 1 calc R . . C9 C -0.19620(13) 0.73857(9) 0.81955(7) 0.0201(3) Uani 1 1 d . . . H9 H -0.2501 0.7643 0.8372 0.024 Uiso 1 1 calc R . . C10 C -0.19037(13) 0.74369(9) 0.76405(7) 0.0215(3) Uani 1 1 d . . . H10 H -0.2399 0.7732 0.7438 0.026 Uiso 1 1 calc R . . C12 C -0.03974(13) 0.66298(9) 0.76734(7) 0.0176(3) Uani 1 1 d . . . H12 H 0.0136 0.6371 0.7494 0.021 Uiso 1 1 calc R . . C11 C -0.11246(14) 0.70593(10) 0.73785(7) 0.0211(3) Uani 1 1 d . . . H11 H -0.1089 0.7095 0.6997 0.025 Uiso 1 1 calc R . . C13 C 0.03974(13) 0.60482(8) 0.92968(6) 0.0153(3) Uani 1 1 d . . . C14 C 0.12361(14) 0.62892(9) 0.96477(7) 0.0197(3) Uani 1 1 d . . . H14 H 0.1892 0.6453 0.9510 0.024 Uiso 1 1 calc R . . C15 C 0.11024(16) 0.62871(10) 1.02015(7) 0.0260(4) Uani 1 1 d . . . H15 H 0.1671 0.6450 1.0442 0.031 Uiso 1 1 calc R . . C16 C 0.01505(17) 0.60501(10) 1.04044(7) 0.0274(4) Uani 1 1 d . . . H16 H 0.0065 0.6057 1.0783 0.033 Uiso 1 1 calc R . . C17 C -0.06823(16) 0.58022(10) 1.00577(7) 0.0252(4) Uani 1 1 d . . . H17 H -0.1334 0.5637 1.0199 0.030 Uiso 1 1 calc R . . C18 C -0.05610(14) 0.57959(9) 0.95038(7) 0.0201(3) Uani 1 1 d . . . H18 H -0.1126 0.5621 0.9266 0.024 Uiso 1 1 calc R . . C19 C 0.36895(12) 0.42249(8) 0.81281(6) 0.0130(3) Uani 1 1 d . . . C20 C 0.41603(12) 0.36010(8) 0.83514(6) 0.0127(3) Uani 1 1 d . . . C21 C 0.45666(12) 0.30722(8) 0.80183(6) 0.0145(3) Uani 1 1 d . . . H21 H 0.4857 0.2649 0.8176 0.017 Uiso 1 1 calc R . . C22 C 0.45510(12) 0.31574(8) 0.74638(6) 0.0148(3) Uani 1 1 d . . . H22 H 0.4805 0.2790 0.7240 0.018 Uiso 1 1 calc R . . C23 C 0.41582(12) 0.37894(8) 0.72376(6) 0.0148(3) Uani 1 1 d . . . H23 H 0.4176 0.3861 0.6859 0.018 Uiso 1 1 calc R . . C24 C 0.37364(12) 0.43220(8) 0.75612(6) 0.0133(3) Uani 1 1 d . . . C25 C 0.43378(12) 0.34644(8) 0.89507(6) 0.0137(3) Uani 1 1 d . . . C26 C 0.51415(12) 0.38495(8) 0.92575(6) 0.0148(3) Uani 1 1 d . . . C27 C 0.53905(13) 0.36456(9) 0.97903(6) 0.0174(3) Uani 1 1 d . . . H27 H 0.5926 0.3904 0.9996 0.021 Uiso 1 1 calc R . . C28 C 0.48822(14) 0.30765(9) 1.00316(6) 0.0185(3) Uani 1 1 d . . . C29 C 0.40807(14) 0.27172(9) 0.97293(7) 0.0184(3) Uani 1 1 d . . . H29 H 0.3715 0.2334 0.9891 0.022 Uiso 1 1 calc R . . C30 C 0.37971(13) 0.29026(8) 0.91949(6) 0.0153(3) Uani 1 1 d . . . C31 C 0.57388(12) 0.44676(9) 0.90105(6) 0.0157(3) Uani 1 1 d . . . H31 H 0.5194 0.4740 0.8781 0.019 Uiso 1 1 calc R . . C32 C 0.66016(13) 0.42066(10) 0.86348(7) 0.0205(3) Uani 1 1 d . . . H32A H 0.6260 0.3914 0.8347 0.031 Uiso 1 1 calc R . . H32B H 0.7141 0.3923 0.8843 0.031 Uiso 1 1 calc R . . H32C H 0.6954 0.4617 0.8475 0.031 Uiso 1 1 calc R . . C33 C 0.62478(15) 0.49910(9) 0.94219(8) 0.0232(4) Uani 1 1 d . . . H33A H 0.6525 0.5404 0.9232 0.035 Uiso 1 1 calc R . . H33B H 0.6843 0.4758 0.9629 0.035 Uiso 1 1 calc R . . H33C H 0.5702 0.5147 0.9668 0.035 Uiso 1 1 calc R . . C34 C 0.52341(16) 0.28365(10) 1.05996(7) 0.0267(4) Uani 1 1 d . . . H34 H 0.5608 0.3246 1.0786 0.032 Uiso 1 1 calc R . . C35 C 0.42911(19) 0.26233(13) 1.09329(8) 0.0378(5) Uani 1 1 d . . . H35A H 0.3760 0.3009 1.0928 0.057 Uiso 1 1 calc R . . H35B H 0.4553 0.2531 1.1307 0.057 Uiso 1 1 calc R . . H35C H 0.3952 0.2193 1.0779 0.057 Uiso 1 1 calc R . . C36 C 0.6045(2) 0.22314(14) 1.05748(9) 0.0436(6) Uani 1 1 d . . . H36A H 0.5705 0.1825 1.0386 0.065 Uiso 1 1 calc R . . H36B H 0.6284 0.2090 1.0943 0.065 Uiso 1 1 calc R . . H36C H 0.6669 0.2390 1.0380 0.065 Uiso 1 1 calc R . . C37 C 0.28856(13) 0.24901(9) 0.89021(7) 0.0177(3) Uani 1 1 d . . . H37 H 0.2773 0.2694 0.8530 0.021 Uiso 1 1 calc R . . C38 C 0.18322(14) 0.25812(11) 0.91915(8) 0.0276(4) Uani 1 1 d . . . H38A H 0.1662 0.3088 0.9219 0.041 Uiso 1 1 calc R . . H38B H 0.1916 0.2375 0.9555 0.041 Uiso 1 1 calc R . . H38C H 0.1244 0.2339 0.8985 0.041 Uiso 1 1 calc R . . C39 C 0.31668(16) 0.17014(10) 0.88449(8) 0.0270(4) Uani 1 1 d . . . H39A H 0.2576 0.1457 0.8642 0.041 Uiso 1 1 calc R . . H39B H 0.3272 0.1487 0.9205 0.041 Uiso 1 1 calc R . . H39C H 0.3832 0.1655 0.8651 0.041 Uiso 1 1 calc R . . C40 C 0.34583(13) 0.50146(8) 0.72853(6) 0.0140(3) Uani 1 1 d . . . C41 C 0.42188(12) 0.55742(8) 0.73339(6) 0.0148(3) Uani 1 1 d . . . C42 C 0.39878(13) 0.62153(9) 0.70707(7) 0.0167(3) Uani 1 1 d . . . H42 H 0.4497 0.6592 0.7108 0.020 Uiso 1 1 calc R . . C43 C 0.30393(13) 0.63250(9) 0.67551(7) 0.0176(3) Uani 1 1 d . . . C44 C 0.23271(13) 0.57571(9) 0.66938(7) 0.0182(3) Uani 1 1 d . . . H44 H 0.1687 0.5816 0.6470 0.022 Uiso 1 1 calc R . . C45 C 0.25187(13) 0.51033(9) 0.69486(7) 0.0159(3) Uani 1 1 d . . . C46 C 0.53121(13) 0.54664(9) 0.76341(7) 0.0182(3) Uani 1 1 d . . . H46 H 0.5221 0.5092 0.7914 0.022 Uiso 1 1 calc R . . C47 C 0.61311(15) 0.51882(10) 0.72418(8) 0.0273(4) Uani 1 1 d . . . H47A H 0.5867 0.4741 0.7080 0.041 Uiso 1 1 calc R . . H47B H 0.6826 0.5106 0.7439 0.041 Uiso 1 1 calc R . . H47C H 0.6223 0.5540 0.6956 0.041 Uiso 1 1 calc R . . C48 C 0.57597(15) 0.61286(10) 0.79222(9) 0.0297(4) Uani 1 1 d . . . H48A H 0.5941 0.6486 0.7654 0.045 Uiso 1 1 calc R . . H48B H 0.6410 0.6003 0.8144 0.045 Uiso 1 1 calc R . . H48C H 0.5215 0.6322 0.8154 0.045 Uiso 1 1 calc R . . C49 C 0.28263(14) 0.70344(9) 0.64750(7) 0.0206(3) Uani 1 1 d . . . H49 H 0.3243 0.7403 0.6689 0.025 Uiso 1 1 calc R . . C50 C 0.32552(17) 0.70301(11) 0.59094(8) 0.0315(4) Uani 1 1 d . . . H50A H 0.2855 0.6680 0.5685 0.047 Uiso 1 1 calc R . . H50B H 0.4023 0.6905 0.5932 0.047 Uiso 1 1 calc R . . H50C H 0.3163 0.7503 0.5747 0.047 Uiso 1 1 calc R . . C51 C 0.16418(15) 0.72552(10) 0.64601(9) 0.0290(4) Uani 1 1 d . . . H51A H 0.1570 0.7743 0.6324 0.043 Uiso 1 1 calc R . . H51B H 0.1378 0.7230 0.6826 0.043 Uiso 1 1 calc R . . H51C H 0.1217 0.6934 0.6221 0.043 Uiso 1 1 calc R . . C52 C 0.17194(13) 0.45026(9) 0.68328(7) 0.0187(3) Uani 1 1 d . . . H52 H 0.1868 0.4121 0.7108 0.022 Uiso 1 1 calc R . . C53 C 0.18745(16) 0.41861(10) 0.62711(7) 0.0266(4) Uani 1 1 d . . . H53A H 0.1752 0.4556 0.5996 0.040 Uiso 1 1 calc R . . H53B H 0.1359 0.3797 0.6203 0.040 Uiso 1 1 calc R . . H53C H 0.2612 0.4003 0.6256 0.040 Uiso 1 1 calc R . . C54 C 0.05476(14) 0.47435(10) 0.68718(7) 0.0231(4) Uani 1 1 d . . . H54A H 0.0350 0.5063 0.6570 0.035 Uiso 1 1 calc R . . H54B H 0.0471 0.4995 0.7214 0.035 Uiso 1 1 calc R . . H54C H 0.0071 0.4327 0.6856 0.035 Uiso 1 1 calc R . . C100 C 0.27090(12) 0.59563(9) 0.83985(6) 0.0152(3) Uani 1 1 d D . . H100 H 0.3358(9) 0.6195(9) 0.8320(8) 0.018 Uiso 1 1 d D . . C101 C 0.18548(12) 0.63991(8) 0.84267(6) 0.0140(3) Uani 1 1 d . . . C102 C 0.19124(12) 0.71878(8) 0.83577(6) 0.0149(3) Uani 1 1 d . . . C103 C 0.25765(13) 0.74784(9) 0.79753(7) 0.0183(3) Uani 1 1 d . . . H103 H 0.2946 0.7172 0.7743 0.022 Uiso 1 1 calc R . . C104 C 0.27025(14) 0.82081(9) 0.79316(7) 0.0216(3) Uani 1 1 d . . . H104 H 0.3159 0.8396 0.7671 0.026 Uiso 1 1 calc R . . C105 C 0.21671(14) 0.86666(9) 0.82653(7) 0.0216(3) Uani 1 1 d . . . H105 H 0.2258 0.9166 0.8236 0.026 Uiso 1 1 calc R . . C106 C 0.14987(14) 0.83872(9) 0.86421(7) 0.0202(3) Uani 1 1 d . . . H106 H 0.1126 0.8697 0.8871 0.024 Uiso 1 1 calc R . . C107 C 0.13700(13) 0.76565(9) 0.86871(7) 0.0169(3) Uani 1 1 d . . . H107 H 0.0906 0.7472 0.8946 0.020 Uiso 1 1 calc R . . C200 C 0.4202(8) 0.5057(6) 0.4762(3) 0.220(9) Uiso 0.50 1 d PG A -1 H200 H 0.3675 0.5135 0.4476 0.264 Uiso 0.50 1 calc PR A -1 C201 C 0.5250(10) 0.4870(6) 0.4648(2) 0.149(5) Uiso 0.50 1 d PG A -1 H201 H 0.5440 0.4820 0.4283 0.179 Uiso 0.50 1 calc PR A -1 C202 C 0.6021(7) 0.4758(5) 0.5067(3) 0.133(4) Uiso 0.50 1 d PG A -1 H202 H 0.6738 0.4630 0.4989 0.160 Uiso 0.50 1 calc PR A -1 C203 C 0.5744(6) 0.4832(4) 0.5601(3) 0.098(3) Uiso 0.50 1 d PG A -1 H203 H 0.6271 0.4755 0.5887 0.118 Uiso 0.50 1 calc PR A -1 C204 C 0.4696(6) 0.5019(4) 0.5715(2) 0.094(3) Uiso 0.50 1 d PG A -1 H204 H 0.4507 0.5069 0.6080 0.113 Uiso 0.50 1 calc PR A -1 C205 C 0.3925(5) 0.5131(5) 0.5296(4) 0.148(5) Uiso 0.50 1 d PG A -1 H205 H 0.3209 0.5259 0.5374 0.178 Uiso 0.50 1 calc PR A -1 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Sn1 0.01203(6) 0.01222(6) 0.01441(6) -0.00035(4) 0.00005(4) 0.00270(4) P1 0.01075(17) 0.01177(18) 0.01310(18) -0.00020(14) 0.00020(13) 0.00183(14) C1 0.0141(7) 0.0152(7) 0.0131(7) 0.0009(6) 0.0021(5) 0.0005(6) C2 0.0140(7) 0.0138(7) 0.0134(7) -0.0016(6) 0.0016(5) -0.0004(6) C3 0.0138(7) 0.0182(8) 0.0174(8) -0.0012(6) 0.0019(6) 0.0010(6) C4 0.0150(7) 0.0224(9) 0.0202(8) -0.0021(6) 0.0023(6) -0.0052(6) C6 0.0177(8) 0.0140(7) 0.0179(8) 0.0012(6) 0.0035(6) 0.0011(6) C5 0.0219(8) 0.0154(8) 0.0194(8) -0.0025(6) 0.0044(6) -0.0050(6) C7 0.0116(7) 0.0129(7) 0.0175(7) 0.0008(6) -0.0014(6) 0.0005(6) C8 0.0159(7) 0.0164(8) 0.0192(8) 0.0005(6) 0.0010(6) 0.0011(6) C9 0.0136(7) 0.0190(8) 0.0279(9) 0.0016(7) 0.0021(6) 0.0040(6) C10 0.0149(8) 0.0203(8) 0.0287(9) 0.0083(7) -0.0036(6) 0.0010(6) C12 0.0161(7) 0.0185(8) 0.0184(8) 0.0005(6) 0.0014(6) 0.0025(6) C11 0.0196(8) 0.0251(9) 0.0182(8) 0.0049(7) -0.0023(6) -0.0005(7) C13 0.0196(8) 0.0127(7) 0.0137(7) 0.0004(6) 0.0015(6) 0.0049(6) C14 0.0209(8) 0.0193(8) 0.0186(8) -0.0005(6) -0.0012(6) 0.0041(6) C15 0.0346(10) 0.0253(9) 0.0175(8) -0.0029(7) -0.0056(7) 0.0082(8) C16 0.0423(11) 0.0248(9) 0.0156(8) 0.0016(7) 0.0061(7) 0.0123(8) C17 0.0316(10) 0.0216(9) 0.0235(9) 0.0041(7) 0.0115(7) 0.0058(7) C18 0.0217(8) 0.0183(8) 0.0205(8) 0.0012(6) 0.0038(6) 0.0021(6) C19 0.0101(7) 0.0123(7) 0.0166(7) -0.0007(6) 0.0002(5) -0.0004(5) C20 0.0104(7) 0.0131(7) 0.0145(7) -0.0006(6) 0.0000(5) -0.0013(5) C21 0.0132(7) 0.0113(7) 0.0189(8) 0.0004(6) -0.0004(6) 0.0019(5) C22 0.0140(7) 0.0129(7) 0.0177(7) -0.0033(6) 0.0016(6) -0.0003(6) C23 0.0155(7) 0.0150(7) 0.0139(7) 0.0005(6) 0.0016(6) -0.0022(6) C24 0.0105(7) 0.0119(7) 0.0176(7) 0.0009(6) -0.0001(5) -0.0015(5) C25 0.0140(7) 0.0123(7) 0.0147(7) -0.0007(6) 0.0007(5) 0.0044(6) C26 0.0126(7) 0.0141(7) 0.0176(7) -0.0017(6) 0.0013(6) 0.0032(6) C27 0.0171(7) 0.0184(8) 0.0165(8) -0.0035(6) -0.0012(6) 0.0008(6) C28 0.0231(8) 0.0186(8) 0.0137(7) -0.0006(6) -0.0004(6) 0.0021(6) C29 0.0226(8) 0.0161(8) 0.0166(8) 0.0019(6) 0.0022(6) -0.0011(6) C30 0.0161(7) 0.0136(7) 0.0161(7) -0.0012(6) 0.0006(6) 0.0019(6) C31 0.0136(7) 0.0150(8) 0.0183(7) -0.0002(6) -0.0003(6) 0.0002(6) C32 0.0155(8) 0.0243(9) 0.0218(8) 0.0003(7) 0.0020(6) 0.0007(6) C33 0.0252(9) 0.0184(9) 0.0260(9) -0.0037(7) 0.0025(7) -0.0055(7) C34 0.0363(10) 0.0282(10) 0.0149(8) 0.0028(7) -0.0051(7) -0.0082(8) C35 0.0499(13) 0.0485(13) 0.0151(9) 0.0048(8) 0.0032(8) -0.0084(10) C36 0.0434(13) 0.0585(15) 0.0274(11) 0.0121(10) -0.0123(9) 0.0132(11) C37 0.0177(8) 0.0182(8) 0.0170(7) 0.0009(6) -0.0012(6) -0.0019(6) C38 0.0189(8) 0.0373(11) 0.0267(9) -0.0023(8) 0.0024(7) -0.0030(8) C39 0.0302(10) 0.0172(9) 0.0330(10) -0.0032(7) -0.0048(8) -0.0024(7) C40 0.0150(7) 0.0125(7) 0.0148(7) 0.0009(6) 0.0029(6) 0.0007(6) C41 0.0144(7) 0.0137(7) 0.0167(7) 0.0004(6) 0.0027(6) -0.0001(6) C42 0.0163(7) 0.0134(7) 0.0207(8) 0.0013(6) 0.0040(6) -0.0021(6) C43 0.0181(8) 0.0145(8) 0.0204(8) 0.0038(6) 0.0046(6) 0.0024(6) C44 0.0157(7) 0.0189(8) 0.0199(8) 0.0045(6) -0.0009(6) 0.0009(6) C45 0.0155(7) 0.0156(8) 0.0168(7) 0.0007(6) 0.0021(6) -0.0012(6) C46 0.0146(7) 0.0146(8) 0.0253(8) 0.0045(6) -0.0007(6) -0.0014(6) C47 0.0172(8) 0.0274(10) 0.0375(11) 0.0025(8) 0.0020(7) 0.0052(7) C48 0.0193(9) 0.0255(10) 0.0433(11) -0.0060(8) -0.0067(8) -0.0029(7) C49 0.0205(8) 0.0150(8) 0.0264(9) 0.0071(7) 0.0018(7) 0.0008(6) C50 0.0370(11) 0.0268(10) 0.0317(10) 0.0137(8) 0.0106(8) 0.0061(8) C51 0.0266(9) 0.0207(9) 0.0401(11) 0.0113(8) 0.0059(8) 0.0068(7) C52 0.0183(8) 0.0160(8) 0.0214(8) 0.0042(6) -0.0036(6) -0.0038(6) C53 0.0296(9) 0.0229(9) 0.0268(9) -0.0021(7) -0.0036(7) -0.0019(7) C54 0.0174(8) 0.0270(9) 0.0246(9) 0.0049(7) -0.0021(6) -0.0057(7) C100 0.0132(7) 0.0173(8) 0.0150(7) -0.0014(6) 0.0008(6) -0.0008(6) C101 0.0139(7) 0.0140(7) 0.0141(7) -0.0009(6) 0.0005(5) -0.0009(6) C102 0.0133(7) 0.0137(7) 0.0173(7) 0.0008(6) -0.0029(6) 0.0002(6) C103 0.0165(7) 0.0182(8) 0.0201(8) 0.0014(6) 0.0010(6) 0.0032(6) C104 0.0180(8) 0.0205(9) 0.0263(9) 0.0069(7) 0.0020(6) 0.0004(6) C105 0.0206(8) 0.0137(8) 0.0300(9) 0.0041(7) -0.0027(7) 0.0010(6) C106 0.0195(8) 0.0153(8) 0.0255(9) -0.0025(6) -0.0011(6) 0.0036(6) C107 0.0159(7) 0.0150(8) 0.0198(8) 0.0003(6) 0.0013(6) 0.0009(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Sn1 C100 2.1950(16) . ? Sn1 C1 2.2174(16) . ? Sn1 C19 2.2437(15) . ? P1 C101 1.7980(16) . ? P1 C2 1.8015(16) . ? P1 C13 1.8021(16) . ? P1 C7 1.8029(16) . ? C1 C6 1.401(2) . ? C1 C2 1.407(2) . ? C2 C3 1.405(2) . ? C3 C4 1.384(2) . ? C4 C5 1.388(2) . ? C6 C5 1.390(2) . ? C7 C8 1.392(2) . ? C7 C12 1.398(2) . ? C8 C9 1.395(2) . ? C9 C10 1.384(2) . ? C10 C11 1.388(2) . ? C12 C11 1.389(2) . ? C13 C14 1.395(2) . ? C13 C18 1.402(2) . ? C14 C15 1.390(2) . ? C15 C16 1.381(3) . ? C16 C17 1.388(3) . ? C17 C18 1.388(2) . ? C19 C20 1.410(2) . ? C19 C24 1.420(2) . ? C20 C21 1.403(2) . ? C20 C25 1.511(2) . ? C21 C22 1.382(2) . ? C22 C23 1.391(2) . ? C23 C24 1.401(2) . ? C24 C40 1.503(2) . ? C25 C30 1.405(2) . ? C25 C26 1.419(2) . ? C26 C27 1.393(2) . ? C26 C31 1.524(2) . ? C27 C28 1.393(2) . ? C28 C29 1.388(2) . ? C28 C34 1.519(2) . ? C29 C30 1.396(2) . ? C30 C37 1.523(2) . ? C31 C33 1.529(2) . ? C31 C32 1.535(2) . ? C34 C35 1.521(3) . ? C34 C36 1.522(3) . ? C37 C39 1.532(2) . ? C37 C38 1.533(2) . ? C40 C45 1.406(2) . ? C40 C41 1.414(2) . ? C41 C42 1.393(2) . ? C41 C46 1.525(2) . ? C42 C43 1.393(2) . ? C43 C44 1.389(2) . ? C43 C49 1.520(2) . ? C44 C45 1.397(2) . ? C45 C52 1.520(2) . ? C46 C48 1.525(2) . ? C46 C47 1.534(2) . ? C49 C50 1.525(2) . ? C49 C51 1.525(2) . ? C52 C54 1.530(2) . ? C52 C53 1.535(2) . ? C100 C101 1.352(2) . ? C101 C102 1.495(2) . ? C102 C107 1.398(2) . ? C102 C103 1.399(2) . ? C103 C104 1.386(2) . ? C104 C105 1.388(3) . ? C105 C106 1.384(2) . ? C106 C107 1.388(2) . ? C200 C201 1.3900 . ? C200 C205 1.3900 . ? C201 C202 1.3900 . ? C202 C203 1.3900 . ? C203 C204 1.3900 . ? C204 C205 1.3900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C100 Sn1 C1 89.50(6) . . ? C100 Sn1 C19 106.29(6) . . ? C1 Sn1 C19 94.52(5) . . ? C101 P1 C2 114.41(7) . . ? C101 P1 C13 110.59(7) . . ? C2 P1 C13 107.74(7) . . ? C101 P1 C7 107.02(7) . . ? C2 P1 C7 106.85(7) . . ? C13 P1 C7 110.14(7) . . ? C6 C1 C2 115.97(14) . . ? C6 C1 Sn1 120.53(11) . . ? C2 C1 Sn1 123.29(12) . . ? C3 C2 C1 122.18(15) . . ? C3 C2 P1 117.16(12) . . ? C1 C2 P1 120.60(12) . . ? C4 C3 C2 119.60(15) . . ? C3 C4 C5 119.61(15) . . ? C5 C6 C1 122.44(15) . . ? C4 C5 C6 120.13(15) . . ? C8 C7 C12 120.05(14) . . ? C8 C7 P1 123.87(12) . . ? C12 C7 P1 116.03(12) . . ? C7 C8 C9 119.49(15) . . ? C10 C9 C8 120.34(15) . . ? C9 C10 C11 120.22(15) . . ? C11 C12 C7 119.86(15) . . ? C10 C11 C12 120.03(16) . . ? C14 C13 C18 120.03(15) . . ? C14 C13 P1 119.89(12) . . ? C18 C13 P1 120.05(13) . . ? C15 C14 C13 119.32(17) . . ? C16 C15 C14 120.59(17) . . ? C15 C16 C17 120.35(16) . . ? C18 C17 C16 119.88(17) . . ? C17 C18 C13 119.81(17) . . ? C20 C19 C24 117.18(14) . . ? C20 C19 Sn1 113.26(10) . . ? C24 C19 Sn1 129.28(11) . . ? C21 C20 C19 120.88(14) . . ? C21 C20 C25 114.78(13) . . ? C19 C20 C25 124.21(13) . . ? C22 C21 C20 121.06(14) . . ? C21 C22 C23 119.03(14) . . ? C22 C23 C24 120.92(14) . . ? C23 C24 C19 120.64(14) . . ? C23 C24 C40 116.30(14) . . ? C19 C24 C40 122.73(14) . . ? C30 C25 C26 119.37(14) . . ? C30 C25 C20 120.18(14) . . ? C26 C25 C20 120.05(14) . . ? C27 C26 C25 118.74(15) . . ? C27 C26 C31 120.15(14) . . ? C25 C26 C31 121.10(14) . . ? C28 C27 C26 122.37(15) . . ? C29 C28 C27 118.04(15) . . ? C29 C28 C34 121.15(15) . . ? C27 C28 C34 120.75(15) . . ? C28 C29 C30 121.82(15) . . ? C29 C30 C25 119.61(15) . . ? C29 C30 C37 117.90(14) . . ? C25 C30 C37 122.48(14) . . ? C26 C31 C33 114.57(14) . . ? C26 C31 C32 111.64(13) . . ? C33 C31 C32 109.47(14) . . ? C28 C34 C35 112.94(16) . . ? C28 C34 C36 110.04(16) . . ? C35 C34 C36 110.71(18) . . ? C30 C37 C39 111.74(14) . . ? C30 C37 C38 110.48(14) . . ? C39 C37 C38 110.81(15) . . ? C45 C40 C41 119.35(14) . . ? C45 C40 C24 122.37(14) . . ? C41 C40 C24 118.07(14) . . ? C42 C41 C40 118.98(15) . . ? C42 C41 C46 119.91(14) . . ? C40 C41 C46 120.95(14) . . ? C43 C42 C41 122.51(15) . . ? C44 C43 C42 117.43(15) . . ? C44 C43 C49 122.05(15) . . ? C42 C43 C49 120.48(15) . . ? C43 C44 C45 122.38(15) . . ? C44 C45 C40 119.21(15) . . ? C44 C45 C52 118.39(15) . . ? C40 C45 C52 122.36(14) . . ? C41 C46 C48 114.31(14) . . ? C41 C46 C47 109.75(14) . . ? C48 C46 C47 109.76(15) . . ? C43 C49 C50 110.73(14) . . ? C43 C49 C51 113.19(14) . . ? C50 C49 C51 111.22(15) . . ? C45 C52 C54 112.34(14) . . ? C45 C52 C53 110.32(14) . . ? C54 C52 C53 109.71(14) . . ? C101 C100 Sn1 125.99(12) . . ? C100 C101 C102 124.24(14) . . ? C100 C101 P1 118.96(12) . . ? C102 C101 P1 116.76(11) . . ? C107 C102 C103 117.88(15) . . ? C107 C102 C101 122.12(14) . . ? C103 C102 C101 119.89(14) . . ? C104 C103 C102 120.84(16) . . ? C103 C104 C105 120.60(16) . . ? C106 C105 C104 119.23(16) . . ? C105 C106 C107 120.35(16) . . ? C106 C107 C102 121.10(15) . . ? C201 C200 C205 120.0 . . ? C200 C201 C202 120.0 . . ? C203 C202 C201 120.0 . . ? C202 C203 C204 120.0 . . ? C205 C204 C203 120.0 . . ? C204 C205 C200 120.0 . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.51 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.227 _refine_diff_density_min -0.525 _refine_diff_density_rms 0.060 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.000 0.000 0.000 319 43 ' ' 2 0.000 0.500 0.500 319 43 ' ' _platon_squeeze_details ; The structure contains 2 molecules of pentane and/or benzene per unit cell in the squeezed area. ; #===END data_global _audit_creation_method 'APEX2 v2011.8-0' _publ_requested_journal ? _publ_contact_author_name ? _publ_contact_author_address ; ; _publ_contact_author_email ? _publ_contact_author_fax ? _publ_contact_author_phone ? _publ_section_title ; ; _publ_section_abstract ; ; _publ_section_references ; ; _publ_section_comment ; ; data_I _chemical_name_systematic ? _chemical_name_common 'Integration of K102Duo' _chemical_formula_moiety ? _chemical_formula_sum 'C140 H184 N2 P2 Sn2' _chemical_formula_iupac ? _chemical_formula_weight 2194.21 _chemical_absolute_configuration ? _chemical_melting_point ? _space_group_crystal_system orthorhombic _space_group_name_H-M_alt 'P n a 21' _space_group_name_Hall 'P 2c -2n' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, z+1/2' '-x+1/2, y+1/2, z+1/2' 'x+1/2, -y+1/2, z' _cell_length_a 28.7237(14) _cell_length_b 23.8226(11) _cell_length_c 17.6686(9) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 12090.1(10) _cell_formula_units_Z 4 _cell_measurement_reflns_used 6703 _cell_measurement_theta_min 2.3054 _cell_measurement_theta_max 24.8751 _cell_measurement_temperature 100.(2) _exptl_crystal_description prism _exptl_crystal_colour 'clear yellow' _exptl_crystal_size_max 0.360 _exptl_crystal_size_mid 0.130 _exptl_crystal_size_min 0.080 _exptl_crystal_density_diffrn 1.205 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4672 _exptl_absorpt_coefficient_mu 0.490 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS V2008/1 (Bruker AXS)' _exptl_absorpt_correction_T_min 0.86 _exptl_absorpt_correction_T_max 0.96 _exptl_special_details ; ; _diffrn_ambient_temperature 100.(2) _diffrn_source ? _diffrn_source_type 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean 8.3333 _diffrn_reflns_number 49699 _diffrn_reflns_av_R_equivalents 0.0702 _diffrn_reflns_av_sigmaI/netI 0.0990 _diffrn_reflns_theta_min 1.11 _diffrn_reflns_theta_max 25.70 _diffrn_reflns_theta_full 25.70 _diffrn_measured_fraction_theta_max 0.999 _diffrn_measured_fraction_theta_full 0.999 _diffrn_reflns_limit_h_min -35 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -29 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _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. ; _reflns_number_total 22087 _reflns_number_gt 16096 _reflns_threshold_expression >2sigma(I) _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_R_factor_all 0.0833 _refine_ls_R_factor_gt 0.0504 _refine_ls_wR_factor_gt 0.1013 _refine_ls_wR_factor_ref 0.1158 _refine_ls_goodness_of_fit_ref 0.988 _refine_ls_restrained_S_all 0.987 _refine_ls_number_reflns 22087 _refine_ls_number_parameters 1315 _refine_ls_number_restraints 85 _refine_ls_hydrogen_treatment constr _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0517P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 1.131 _refine_diff_density_min -0.460 _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 0.100(17) 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' N N 0.0061 0.0033 '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' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'APEX2 v2011.8-0 (Bruker AXS)' _computing_data_reduction 'SAINT V7.68A (Bruker AXS, 2009)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _computing_publication_material ? loop_ _atom_site_type_symbol _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_refinement_flags _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Sn Sn1 0.073006(14) 0.599483(13) 0.74916(2) 0.01949(10) Uani d . 1 . . C C302 -0.0044(2) 0.58769(18) 0.7421(5) 0.0206(15) Uani d . 1 . . Sn Sn3 0.074728(13) 0.086809(13) 0.99446(2) 0.01710(9) Uani d . 1 . . P P1 0.01732(5) 0.48200(5) 0.78684(10) 0.0168(3) Uani d . 1 . . P P2 0.01204(5) -0.02578(5) 0.95716(9) 0.0155(3) Uani d . 1 . . C C323 -0.00204(18) 0.08196(19) 1.0027(4) 0.0143(12) Uani d U 1 . . C C301 -0.02289(18) 0.53441(18) 0.7538(4) 0.0164(12) Uani d . 1 . . C C320 -0.01264(18) -0.0882(2) 1.0001(5) 0.0178(13) Uani d . 1 . . C C0AJ 0.2032(3) 0.8209(3) 0.3218(7) 0.103(4) Uani d . 1 . . H H0A1 0.1798 0.834 0.2856 0.155 Uiso calc R 1 . . H H0A2 0.1961 0.7822 0.3368 0.155 Uiso calc R 1 . . H H0A3 0.2341 0.8222 0.2982 0.155 Uiso calc R 1 . . C C2 0.0559(2) 0.7614(2) 0.7664(4) 0.0225(14) Uani d . 1 . . H H2 0.081 0.7362 0.7858 0.027 Uiso calc R 1 . . C C3 0.0669(2) 0.8211(2) 0.7934(5) 0.043(2) Uani d . 1 . . H H3A 0.0968 0.8331 0.7724 0.064 Uiso calc R 1 . . H H3B 0.0685 0.8216 0.8488 0.064 Uiso calc R 1 . . H H3C 0.0423 0.8467 0.7763 0.064 Uiso calc R 1 . . C C4 0.00974(19) 0.7408(2) 0.7991(4) 0.0207(13) Uani d . 1 . . C C5 -0.0324(2) 0.7655(2) 0.7757(4) 0.0275(15) Uani d . 1 . . H H5 -0.0312 0.7951 0.7398 0.033 Uiso calc R 1 . . C C6 -0.07500(19) 0.7489(2) 0.8023(4) 0.0236(13) Uani d . 1 . . C C7 -0.1190(2) 0.7792(2) 0.7796(4) 0.0312(16) Uani d . 1 . . H H7 -0.1111 0.8054 0.7372 0.037 Uiso calc R 1 . . C C8 -0.1376(2) 0.8141(2) 0.8449(5) 0.0407(19) Uani d . 1 . . H H8A -0.1662 0.8333 0.8292 0.061 Uiso calc R 1 . . H H8B -0.1142 0.842 0.8597 0.061 Uiso calc R 1 . . H H8C -0.1443 0.7895 0.888 0.061 Uiso calc R 1 . . C C9 -0.1569(2) 0.7401(3) 0.7521(5) 0.0414(16) Uani d . 1 . . H H9A -0.1845 0.762 0.7383 0.062 Uiso calc R 1 . . H H9B -0.1649 0.7136 0.7924 0.062 Uiso calc R 1 . . H H9C -0.1458 0.7193 0.7078 0.062 Uiso calc R 1 . . C C10 -0.0756(2) 0.7066(2) 0.8561(4) 0.0234(13) Uani d . 1 . . H H10 -0.1048 0.6941 0.8749 0.028 Uiso calc R 1 . . C C11 -0.03497(19) 0.6816(2) 0.8837(4) 0.0167(13) Uani d . 1 . . C C12 0.00784(19) 0.6989(2) 0.8540(4) 0.0185(13) Uani d . 1 . . C C13 0.05266(19) 0.6806(2) 0.8940(4) 0.0160(13) Uani d . 1 . . C C14 0.06308(19) 0.7134(2) 0.9584(4) 0.0183(13) Uani d . 1 . . H H14 0.0418 0.7417 0.9741 0.022 Uiso calc R 1 . . C C15 0.10333(18) 0.70532(19) 0.9988(4) 0.0217(13) Uani d . 1 . . H H15 0.1092 0.726 1.0437 0.026 Uiso calc R 1 . . C C16 0.1348(2) 0.6668(2) 0.9729(4) 0.0231(15) Uani d . 1 . . H H16 0.1633 0.6619 0.9994 0.028 Uiso calc R 1 . . C C17 0.12612(19) 0.63408(19) 0.9079(4) 0.0184(13) Uani d . 1 . . C C18 0.1687(2) 0.6022(2) 0.8830(4) 0.0238(15) Uani d . 1 . . C C19 0.1852(2) 0.5552(2) 0.9230(4) 0.0232(15) Uani d . 1 . . C C20 0.22742(19) 0.5310(2) 0.9011(4) 0.0241(14) Uani d . 1 . . H H20 0.2388 0.4996 0.9285 0.029 Uiso calc R 1 . . C C21 0.2534(2) 0.5516(2) 0.8403(4) 0.0283(15) Uani d . 1 . . C C22 0.23712(19) 0.5978(2) 0.8031(4) 0.0263(15) Uani d . 1 . . H H22 0.2545 0.6124 0.7617 0.032 Uiso calc R 1 . . C C23 0.19622(19) 0.6241(2) 0.8235(4) 0.0215(13) Uani d . 1 . . C C24 0.1833(2) 0.6800(2) 0.7850(4) 0.0235(14) Uani d . 1 . . H H24 0.1489 0.6848 0.7903 0.028 Uiso calc R 1 . . C C25 0.1945(2) 0.6820(3) 0.6997(4) 0.0401(17) Uani d . 1 . . H H25A 0.1796 0.6502 0.6743 0.06 Uiso calc R 1 . . H H25B 0.2283 0.6799 0.6924 0.06 Uiso calc R 1 . . H H25C 0.1827 0.7172 0.6782 0.06 Uiso calc R 1 . . C C26 0.2065(2) 0.7297(2) 0.8270(4) 0.0343(16) Uani d . 1 . . H H26A 0.199 0.7276 0.8811 0.051 Uiso calc R 1 . . H H26B 0.1948 0.7652 0.8063 0.051 Uiso calc R 1 . . H H26C 0.2403 0.7279 0.8203 0.051 Uiso calc R 1 . . C C27 0.2984(2) 0.5204(2) 0.8178(4) 0.0313(15) Uani d . 1 . . H H27 0.2898 0.4803 0.8082 0.038 Uiso calc R 1 . . C C28 0.3328(2) 0.5212(3) 0.8832(4) 0.0367(17) Uani d . 1 . . H H28A 0.3612 0.5011 0.8685 0.055 Uiso calc R 1 . . H H28B 0.3189 0.5027 0.9274 0.055 Uiso calc R 1 . . H H28C 0.3406 0.5601 0.896 0.055 Uiso calc R 1 . . C C29 0.1608(2) 0.5323(2) 0.9920(5) 0.0264(13) Uani d . 1 . . H H29 0.1287 0.5484 0.9932 0.032 Uiso calc R 1 . . C C30 0.1854(3) 0.5496(2) 1.0649(4) 0.0389(19) Uani d . 1 . . H H30A 0.1686 0.5342 1.1085 0.058 Uiso calc R 1 . . H H30B 0.1861 0.5906 1.0685 0.058 Uiso calc R 1 . . H H30C 0.2173 0.5351 1.0646 0.058 Uiso calc R 1 . . C C31 0.1564(2) 0.46818(19) 0.9910(5) 0.0292(14) Uani d . 1 . . H H31M 0.1405 0.4556 1.0371 0.044 Uiso calc R 1 . . H H31N 0.1875 0.4513 0.9887 0.044 Uiso calc R 1 . . H H31O 0.1383 0.4566 0.9466 0.044 Uiso calc R 1 . . C C32 0.08312(19) 0.63911(18) 0.8680(4) 0.0185(14) Uani d . 1 . . C C33 -0.0383(2) 0.6385(2) 0.9472(4) 0.0219(15) Uani d . 1 . . H H33 -0.0072 0.6199 0.952 0.026 Uiso calc R 1 . . C C34 -0.0493(2) 0.6668(2) 1.0231(4) 0.0271(15) Uani d . 1 . . H H34A -0.0511 0.6383 1.0629 0.041 Uiso calc R 1 . . H H34B -0.0791 0.6866 1.0194 0.041 Uiso calc R 1 . . H H34C -0.0246 0.6937 1.0354 0.041 Uiso calc R 1 . . C C35 -0.0740(2) 0.5931(2) 0.9314(5) 0.0265(16) Uani d . 1 . . H H35A -0.0747 0.5665 0.9736 0.04 Uiso calc R 1 . . H H35B -0.0657 0.5733 0.8847 0.04 Uiso calc R 1 . . H H35C -0.1048 0.6103 0.9255 0.04 Uiso calc R 1 . . C C37 0.0082(2) 0.4730(2) 0.8889(4) 0.0220(14) Uani d . 1 . . C C38 -0.0338(2) 0.4516(2) 0.9160(4) 0.0209(14) Uani d . 1 . . H H38 -0.0579 0.4416 0.8817 0.025 Uiso calc R 1 . . C C39 -0.0400(2) 0.44515(19) 0.9920(5) 0.0277(14) Uani d . 1 . . H H39 -0.0684 0.4302 1.0109 0.033 Uiso calc R 1 . . C C40 -0.0050(2) 0.4604(2) 1.0416(4) 0.0301(16) Uani d . 1 . . H H40 -0.0091 0.4551 1.0945 0.036 Uiso calc R 1 . . C C41 0.0363(2) 0.4835(3) 1.0146(4) 0.0358(18) Uani d . 1 . . H H41 0.0601 0.4945 1.0488 0.043 Uiso calc R 1 . . C C42 0.0424(2) 0.4905(2) 0.9373(4) 0.0245(15) Uani d . 1 . . H H42 0.0701 0.5072 0.9183 0.029 Uiso calc R 1 . . N N1 0.06887(15) 0.50363(15) 0.7655(3) 0.0190(12) Uani d . 1 . . C C44 0.10730(19) 0.4670(2) 0.7363(4) 0.0216(14) Uani d . 1 . . C C45 0.0990(2) 0.4508(2) 0.6523(3) 0.0196(13) Uani d . 1 . . H H45A 0.0694 0.4299 0.6475 0.024 Uiso calc R 1 . . H H45B 0.0967 0.4852 0.6211 0.024 Uiso calc R 1 . . C C46 0.1392(2) 0.4145(2) 0.6238(4) 0.0262(15) Uani d . 1 . . H H46 0.1328 0.4035 0.5702 0.031 Uiso calc R 1 . . C C47 0.1841(2) 0.4476(3) 0.6266(4) 0.0308(15) Uani d . 1 . . H H47A 0.1813 0.4817 0.5949 0.037 Uiso calc R 1 . . H H47B 0.21 0.4245 0.6067 0.037 Uiso calc R 1 . . C C48 0.1938(2) 0.4640(2) 0.7092(4) 0.0318(16) Uani d . 1 . . H H48 0.2233 0.4862 0.7121 0.038 Uiso calc R 1 . . C C49 0.15312(17) 0.4994(2) 0.7393(4) 0.0264(14) Uani d . 1 . . H H49A 0.1596 0.5105 0.7923 0.032 Uiso calc R 1 . . H H49B 0.1503 0.534 0.7087 0.032 Uiso calc R 1 . . C C50 0.19810(19) 0.4109(2) 0.7576(4) 0.0325(15) Uani d . 1 . . H H50A 0.2244 0.3878 0.7391 0.039 Uiso calc R 1 . . H H50B 0.2044 0.4214 0.8108 0.039 Uiso calc R 1 . . C C51 0.1534(2) 0.3774(2) 0.7531(4) 0.0310(14) Uani d . 1 . . H H51 0.1566 0.3425 0.7841 0.037 Uiso calc R 1 . . C C52 0.1434(2) 0.3617(2) 0.6713(4) 0.0293(15) Uani d . 1 . . H H52A 0.1688 0.3378 0.6515 0.035 Uiso calc R 1 . . H H52B 0.114 0.34 0.6685 0.035 Uiso calc R 1 . . C C53 0.1121(2) 0.4132(2) 0.7839(4) 0.0269(15) Uani d . 1 . . H H53A 0.0829 0.3913 0.7812 0.032 Uiso calc R 1 . . H H53B 0.1178 0.4232 0.8375 0.032 Uiso calc R 1 . . C C55 -0.06929(19) 0.52169(19) 0.7403(4) 0.0219(14) Uani d . 1 . . H H55 -0.0815 0.4859 0.7532 0.026 Uiso calc R 1 . . C C56 -0.0976(2) 0.5621(2) 0.7077(4) 0.0256(15) Uani d . 1 . . H H56 -0.1293 0.5539 0.6975 0.031 Uiso calc R 1 . . C C57 -0.0796(2) 0.6138(2) 0.6902(4) 0.0260(15) Uani d . 1 . . H H57 -0.0985 0.641 0.6655 0.031 Uiso calc R 1 . . C C58 -0.0211(2) 0.4170(2) 0.6715(4) 0.0180(13) Uani d . 1 . . H H58 -0.019 0.4502 0.6418 0.022 Uiso calc R 1 . . C C59 -0.0405(2) 0.3688(2) 0.6415(4) 0.0225(14) Uani d . 1 . . H H59 -0.0519 0.3694 0.5911 0.027 Uiso calc R 1 . . C C60 -0.0438(2) 0.3206(2) 0.6824(4) 0.0267(15) Uani d . 1 . . H H60 -0.0575 0.2881 0.6606 0.032 Uiso calc R 1 . . C C61 -0.02654(19) 0.3189(2) 0.7575(4) 0.0243(14) Uani d . 1 . . H H61 -0.0284 0.2854 0.7865 0.029 Uiso calc R 1 . . C C62 -0.0070(2) 0.3668(2) 0.7880(4) 0.0251(14) Uani d . 1 . . H H62 0.005 0.366 0.8382 0.03 Uiso calc R 1 . . N N2 0.06459(15) -0.00773(16) 0.9769(3) 0.0173(12) Uani d . 1 . . C C64 -0.02466(18) 0.03056(17) 0.9888(4) 0.0145(12) Uani d U 1 . . C C65 -0.07170(18) 0.02198(18) 1.0045(4) 0.0175(13) Uani d U 1 . . H H65 -0.0856 -0.0136 0.9953 0.021 Uiso calc R 1 . . C C66 -0.0978(2) 0.0652(2) 1.0333(4) 0.0213(14) Uani d U 1 . . H H66 -0.1301 0.0602 1.0423 0.026 Uiso calc R 1 . . C C67 -0.0768(2) 0.1158(2) 1.0490(4) 0.0230(14) Uani d U 1 . . H H67 -0.0946 0.1454 1.0705 0.028 Uiso calc R 1 . . C C68 -0.02971(19) 0.1240(2) 1.0334(4) 0.0186(13) Uani d U 1 . . H H68 -0.0161 0.1595 1.0442 0.022 Uiso calc R 1 . . C C69 -0.0274(2) -0.0856(2) 1.0758(4) 0.0190(14) Uani d . 1 . . H H69 -0.022 -0.0522 1.1039 0.023 Uiso calc R 1 . . C C70 -0.0493(2) -0.1297(2) 1.1105(4) 0.0252(14) Uani d . 1 . . H H70 -0.0592 -0.1266 1.1616 0.03 Uiso calc R 1 . . C C71 -0.0569(2) -0.1788(2) 1.0708(4) 0.0272(15) Uani d . 1 . . H H71 -0.0721 -0.2096 1.0943 0.033 Uiso calc R 1 . . C C72 -0.04213(19) -0.18266(19) 0.9967(5) 0.0254(13) Uani d . 1 . . H H72 -0.047 -0.2166 0.9695 0.03 Uiso calc R 1 . . C C73 -0.02028(19) -0.13783(18) 0.9610(4) 0.0190(13) Uani d . 1 . . H H73 -0.0106 -0.1412 0.9099 0.023 Uiso calc R 1 . . C C74 0.00188(19) -0.03299(19) 0.8574(3) 0.0148(12) Uani d . 1 . . C C75 0.0357(2) -0.0155(2) 0.8060(4) 0.0234(15) Uani d . 1 . . H H75 0.0645 -0.0014 0.8245 0.028 Uiso calc R 1 . . C C76 0.0286(2) -0.0181(2) 0.7297(4) 0.0254(16) Uani d . 1 . . H H76 0.0517 -0.0048 0.6958 0.031 Uiso calc R 1 . . C C77 -0.0129(2) -0.0404(2) 0.7018(4) 0.0302(16) Uani d . 1 . . H H77 -0.0175 -0.0433 0.6487 0.036 Uiso calc R 1 . . C C78 -0.04748(19) -0.05833(19) 0.7506(4) 0.0235(13) Uani d . 1 . . H H78 -0.0757 -0.0734 0.7313 0.028 Uiso calc R 1 . . C C79 -0.0403(2) -0.0540(2) 0.8282(4) 0.0230(14) Uani d . 1 . . H H79 -0.0642 -0.0654 0.862 0.028 Uiso calc R 1 . . C C80 0.10133(18) -0.04816(19) 1.0032(4) 0.0193(13) Uani d . 1 . . C C81 0.0998(2) -0.1035(2) 0.9585(4) 0.0217(14) Uani d . 1 . . H H81A 0.0687 -0.1209 0.9643 0.026 Uiso calc R 1 . . H H81B 0.1047 -0.0956 0.9041 0.026 Uiso calc R 1 . . C C82 0.13721(17) -0.1448(2) 0.9861(4) 0.0233(13) Uani d . 1 . . H H82 0.1349 -0.1807 0.9569 0.028 Uiso calc R 1 . . C C83 0.1853(2) -0.1186(2) 0.9737(4) 0.0289(15) Uani d . 1 . . H H83A 0.2099 -0.1447 0.9913 0.035 Uiso calc R 1 . . H H83B 0.1903 -0.1112 0.9192 0.035 Uiso calc R 1 . . C C84 0.1879(2) -0.0640(2) 1.0179(4) 0.0264(15) Uani d . 1 . . H H84 0.219 -0.0463 1.0096 0.032 Uiso calc R 1 . . C C85 0.1818(2) -0.0766(2) 1.1017(4) 0.0301(15) Uani d . 1 . . H H85A 0.1852 -0.0416 1.1314 0.036 Uiso calc R 1 . . H H85B 0.2061 -0.1033 1.1186 0.036 Uiso calc R 1 . . C C86 0.1329(2) -0.1022(2) 1.1156(4) 0.0249(15) Uani d . 1 . . H H86 0.1285 -0.11 1.1708 0.03 Uiso calc R 1 . . C C87 0.0956(2) -0.0613(2) 1.0880(3) 0.0210(14) Uani d . 1 . . H H87A 0.0977 -0.026 1.1174 0.025 Uiso calc R 1 . . H H87B 0.0644 -0.0778 1.0969 0.025 Uiso calc R 1 . . C C88 0.1288(2) -0.1565(2) 1.0705(4) 0.0236(14) Uani d . 1 . . H H88A 0.0974 -0.1728 1.0776 0.028 Uiso calc R 1 . . H H88B 0.152 -0.184 1.0891 0.028 Uiso calc R 1 . . C C89 0.14981(17) -0.02361(18) 0.9913(4) 0.0232(13) Uani d . 1 . . H H89A 0.1525 0.0121 1.0196 0.028 Uiso calc R 1 . . H H89B 0.1543 -0.0153 0.9369 0.028 Uiso calc R 1 . . C C90 0.08842(19) 0.12958(19) 0.8783(3) 0.0155(13) Uani d . 1 . . C C91 0.1317(2) 0.1227(2) 0.8390(4) 0.0206(13) Uani d . 1 . . C C92 0.1703(2) 0.0829(2) 0.8605(4) 0.0190(14) Uani d . 1 . . C C93 0.18242(19) 0.0387(2) 0.8109(4) 0.0193(13) Uani d . 1 . . C C94 0.15364(19) 0.0219(2) 0.7422(4) 0.0212(13) Uani d . 1 . . H H94 0.1225 0.0403 0.7462 0.025 Uiso calc R 1 . . C C95 0.14630(19) -0.04175(19) 0.7390(4) 0.0271(14) Uani d . 1 . . H H95A 0.1275 -0.0512 0.6946 0.041 Uiso calc R 1 . . H H95B 0.1302 -0.0542 0.7849 0.041 Uiso calc R 1 . . H H95C 0.1766 -0.0606 0.7355 0.041 Uiso calc R 1 . . C C96 0.1768(2) 0.0412(3) 0.6680(4) 0.0344(17) Uani d . 1 . . H H96A 0.1573 0.0302 0.625 0.052 Uiso calc R 1 . . H H96B 0.2075 0.0236 0.6633 0.052 Uiso calc R 1 . . H H96C 0.1803 0.0821 0.6686 0.052 Uiso calc R 1 . . C C97 0.2230(2) 0.0078(2) 0.8248(4) 0.0284(14) Uani d . 1 . . H H97 0.2311 -0.0217 0.7913 0.034 Uiso calc R 1 . . C C98 0.2520(2) 0.0193(2) 0.8871(4) 0.0315(15) Uani d . 1 . . C C99 0.2966(2) -0.0137(3) 0.8999(4) 0.0395(17) Uani d . 1 . . H H99 0.2998 -0.0189 0.9558 0.047 Uiso calc R 1 . . C C100 0.3373(2) 0.0191(3) 0.8747(7) 0.078(4) Uani d . 1 . . H H10A 0.3371 0.0559 0.8995 0.118 Uiso calc R 1 . . H H10B 0.3359 0.0241 0.8197 0.118 Uiso calc R 1 . . H H10C 0.3659 -0.001 0.8881 0.118 Uiso calc R 1 . . C C101 0.2401(2) 0.0626(3) 0.9328(4) 0.0294(15) Uani d . 1 . . H H101 0.2599 0.0712 0.9743 0.035 Uiso calc R 1 . . C C102 0.19993(19) 0.0958(2) 0.9222(3) 0.0225(13) Uani d . 1 . . C C103 0.1916(2) 0.1466(2) 0.9701(4) 0.0294(15) Uani d . 1 . . H H103 0.1576 0.1554 0.9668 0.035 Uiso calc R 1 . . C C104 0.1438(2) 0.1587(2) 0.7800(4) 0.0220(14) Uani d . 1 . . H H104 0.1727 0.1532 0.7548 0.026 Uiso calc R 1 . . C C105 0.11578(19) 0.2015(2) 0.7573(4) 0.0242(14) Uani d . 1 . . H H105 0.1243 0.2247 0.7159 0.029 Uiso calc R 1 . . C C106 0.07467(19) 0.21045(19) 0.7957(3) 0.0181(12) Uani d . 1 . . H H106 0.0551 0.2408 0.7813 0.022 Uiso calc R 1 . . C C107 0.0613(2) 0.17548(19) 0.8555(4) 0.0187(14) Uani d . 1 . . C C108 0.01826(18) 0.19728(19) 0.8945(4) 0.0147(12) Uani d . 1 . . C C109 -0.0264(2) 0.18329(19) 0.8695(3) 0.0169(13) Uani d . 1 . . C C110 -0.06503(19) 0.2120(2) 0.8974(4) 0.0192(13) Uani d . 1 . . H H110 -0.0953 0.202 0.8804 0.023 Uiso calc R 1 . . C C111 -0.05971(19) 0.2554(2) 0.9505(4) 0.0199(13) Uani d . 1 . . C C112 -0.0158(2) 0.2671(2) 0.9752(3) 0.0206(14) Uani d . 1 . . H H112 -0.0121 0.2957 1.0122 0.025 Uiso calc R 1 . . C C113 0.02397(19) 0.2398(2) 0.9495(4) 0.0183(13) Uani d . 1 . . C C114 0.07188(19) 0.2570(2) 0.9778(4) 0.0228(14) Uani d . 1 . . H H114 0.0952 0.2312 0.9544 0.027 Uiso calc R 1 . . C C115 0.0840(2) 0.3169(2) 0.9535(4) 0.0377(18) Uani d . 1 . . H H11A 0.1153 0.3264 0.9715 0.056 Uiso calc R 1 . . H H11B 0.0614 0.3431 0.9752 0.056 Uiso calc R 1 . . H H11C 0.0831 0.3195 0.8981 0.056 Uiso calc R 1 . . C C116 0.0756(2) 0.2507(2) 1.0643(4) 0.0297(15) Uani d . 1 . . H H11D 0.107 0.2612 1.0807 0.045 Uiso calc R 1 . . H H11E 0.0695 0.2116 1.0784 0.045 Uiso calc R 1 . . H H11F 0.0528 0.2752 1.0888 0.045 Uiso calc R 1 . . C C117 -0.1018(2) 0.2900(2) 0.9763(3) 0.0256(15) Uani d . 1 . . H H117 -0.0912 0.3164 1.0167 0.031 Uiso calc R 1 . . C C118 -0.1409(2) 0.2549(2) 1.0077(4) 0.0335(16) Uani d . 1 . . H H11G -0.1666 0.2794 1.023 0.05 Uiso calc R 1 . . H H11H -0.1297 0.2339 1.0518 0.05 Uiso calc R 1 . . H H11I -0.1517 0.2286 0.9689 0.05 Uiso calc R 1 . . C C119 -0.0331(2) 0.1395(2) 0.8073(4) 0.0191(13) Uani d . 1 . . H H119 -0.004 0.1166 0.804 0.023 Uiso calc R 1 . . C C120 -0.0404(2) 0.1687(2) 0.7307(4) 0.0252(15) Uani d . 1 . . H H12A -0.0444 0.1403 0.6911 0.038 Uiso calc R 1 . . H H12B -0.0132 0.192 0.719 0.038 Uiso calc R 1 . . H H12C -0.0683 0.1924 0.7331 0.038 Uiso calc R 1 . . C C300 -0.0738(2) 0.0996(2) 0.8224(4) 0.0252(16) Uani d . 1 . . H H30D -0.0761 0.0724 0.781 0.038 Uiso calc R 1 . . H H30E -0.1028 0.1212 0.8258 0.038 Uiso calc R 1 . . H H30F -0.0685 0.0797 0.8702 0.038 Uiso calc R 1 . . C C304 0.32091(19) 0.5430(2) 0.7461(4) 0.0368(15) Uani d . 1 . . H H30G 0.2983 0.5421 0.7046 0.055 Uiso calc R 1 . . H H30H 0.3478 0.5197 0.7329 0.055 Uiso calc R 1 . . H H30I 0.3311 0.5817 0.7545 0.055 Uiso calc R 1 . . C C305 0.1988(2) 0.2935(3) 0.4920(5) 0.061(2) Uani d . 1 . . H H30J 0.1687 0.2922 0.4661 0.091 Uiso calc R 1 . . H H30K 0.2239 0.2924 0.4544 0.091 Uiso calc R 1 . . H H30L 0.2011 0.3283 0.5213 0.091 Uiso calc R 1 . . C C306 0.2031(3) 0.2437(3) 0.5446(5) 0.061(2) Uani d . 1 . . H H30M 0.1775 0.2446 0.5821 0.073 Uiso calc R 1 . . H H30N 0.2003 0.2086 0.5151 0.073 Uiso calc R 1 . . C C309 0.3005(3) 0.1944(3) 0.6813(5) 0.069(3) Uani d . 1 . . H H30O 0.3075 0.2304 0.7069 0.083 Uiso calc R 1 . . H H30P 0.3248 0.1879 0.6425 0.083 Uiso calc R 1 . . C C308 0.2534(3) 0.1981(3) 0.6435(5) 0.055(2) Uani d . 1 . . H H30Q 0.2294 0.2039 0.6829 0.066 Uiso calc R 1 . . H H30R 0.2467 0.1618 0.6185 0.066 Uiso calc R 1 . . C C307 0.2493(2) 0.2446(3) 0.5852(5) 0.052(2) Uani d . 1 . . H H30S 0.2531 0.2813 0.6107 0.062 Uiso calc R 1 . . H H30T 0.2746 0.2407 0.5476 0.062 Uiso calc R 1 . . C C303 -0.0344(2) 0.6263(2) 0.7083(4) 0.0242(15) Uani d . 1 . . H H303 -0.023 0.6628 0.6974 0.029 Uiso calc R 1 . . C C310 0.3016(3) 0.1464(3) 0.7396(5) 0.083(3) Uani d . 1 . . H H31D 0.3324 0.1447 0.7631 0.124 Uiso calc R 1 . . H H31E 0.295 0.1108 0.7142 0.124 Uiso calc R 1 . . H H31F 0.278 0.1533 0.7786 0.124 Uiso calc R 1 . . C C312 0.2182(2) 0.1979(2) 0.9377(4) 0.0463(19) Uani d . 1 . . H H31G 0.2109 0.2021 0.8838 0.069 Uiso calc R 1 . . H H31H 0.2518 0.1921 0.9438 0.069 Uiso calc R 1 . . H H31I 0.2088 0.2319 0.9649 0.069 Uiso calc R 1 . . C C311 0.2032(2) 0.1386(3) 1.0540(4) 0.0469(19) Uani d . 1 . . H H31J 0.1968 0.1735 1.0815 0.07 Uiso calc R 1 . . H H31K 0.2362 0.1289 1.0594 0.07 Uiso calc R 1 . . H H31L 0.184 0.1082 1.0749 0.07 Uiso calc R 1 . . C C313 0.0570(2) 0.7585(3) 0.6802(4) 0.0383(17) Uani d . 1 . . H H900 0.0499 0.7202 0.6638 0.057 Uiso calc R 1 . . H H901 0.088 0.7691 0.662 0.057 Uiso calc R 1 . . H H902 0.0338 0.7844 0.6593 0.057 Uiso calc R 1 . . C C316 0.2326(3) 0.8709(4) 0.5287(7) 0.091(4) Uani d . 1 . . H H31P 0.2011 0.8643 0.5495 0.109 Uiso calc R 1 . . H H31Q 0.2366 0.9118 0.5217 0.109 Uiso calc R 1 . . C C314 0.2654(3) 0.8799(4) 0.6564(7) 0.091(4) Uani d . 1 . . H H31R 0.2891 0.866 0.6914 0.137 Uiso calc R 1 . . H H31S 0.2344 0.874 0.6783 0.137 Uiso calc R 1 . . H H31T 0.2702 0.9201 0.6474 0.137 Uiso calc R 1 . . C C318 0.2027(3) 0.8607(3) 0.3955(7) 0.078(3) Uani d . 1 . . H H31U 0.21 0.8997 0.3803 0.094 Uiso calc R 1 . . H H31V 0.1712 0.8605 0.4181 0.094 Uiso calc R 1 . . C C315 0.2688(4) 0.8498(4) 0.5850(7) 0.096(4) Uani d . 1 . . H H31W 0.264 0.8092 0.5941 0.115 Uiso calc R 1 . . H H930 0.3003 0.8549 0.5635 0.115 Uiso calc R 1 . . C C317 0.2368(3) 0.8419(4) 0.4525(8) 0.095(4) Uani d . 1 . . H H931 0.2685 0.8483 0.4324 0.114 Uiso calc R 1 . . H H932 0.233 0.801 0.4601 0.114 Uiso calc R 1 . . C C321 -0.0045(2) 0.41634(18) 0.7460(5) 0.0166(13) Uani d . 1 . . C C319 0.2968(2) -0.0715(3) 0.8650(6) 0.059(2) Uani d . 1 . . H H933 0.3262 -0.0903 0.877 0.088 Uiso calc R 1 . . H H934 0.2935 -0.0682 0.81 0.088 Uiso calc R 1 . . H H935 0.2708 -0.0934 0.8854 0.088 Uiso calc R 1 . . C C322 -0.1205(2) 0.3254(2) 0.9086(5) 0.045(2) Uani d . 1 . . H H32A -0.1474 0.3476 0.9252 0.067 Uiso calc R 1 . . H H32B -0.1299 0.3003 0.8675 0.067 Uiso calc R 1 . . H H32C -0.0959 0.3507 0.8906 0.067 Uiso calc R 1 . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Sn1 0.0223(2) 0.02045(15) 0.0157(2) -0.00147(16) 0.0006(2) -0.00097(17) C302 0.030(3) 0.019(3) 0.013(4) 0.004(2) 0.007(4) -0.001(3) Sn3 0.01885(19) 0.01995(15) 0.0125(2) -0.00291(15) -0.0006(2) 0.00008(16) P1 0.0201(8) 0.0165(6) 0.0139(9) 0.0017(6) -0.0017(7) -0.0016(6) P2 0.0170(8) 0.0180(6) 0.0115(9) 0.0001(6) 0.0010(7) 0.0001(6) C323 0.024(3) 0.013(2) 0.006(4) 0.001(2) -0.002(3) 0.007(2) C301 0.020(3) 0.017(2) 0.013(3) 0.0067(19) 0.009(3) -0.001(3) C320 0.017(3) 0.019(2) 0.017(4) 0.001(2) -0.001(3) 0.000(3) C0AJ 0.098(8) 0.057(5) 0.154(13) 0.003(5) 0.076(8) 0.019(7) C2 0.026(3) 0.022(2) 0.019(4) 0.003(2) 0.000(3) 0.003(2) C3 0.041(4) 0.031(3) 0.056(5) -0.020(3) 0.002(4) -0.008(3) C4 0.022(3) 0.025(3) 0.015(3) -0.003(2) 0.004(3) 0.000(2) C5 0.031(4) 0.026(3) 0.026(4) 0.005(3) -0.008(3) 0.003(3) C6 0.018(3) 0.026(3) 0.026(4) 0.000(3) -0.007(3) -0.006(2) C7 0.025(3) 0.038(3) 0.031(4) 0.006(3) -0.003(3) 0.008(3) C8 0.030(4) 0.032(3) 0.060(6) 0.006(3) -0.018(4) -0.002(3) C9 0.027(3) 0.066(4) 0.031(4) 0.013(3) -0.005(4) -0.008(4) C10 0.023(3) 0.026(3) 0.022(4) -0.005(3) 0.002(3) -0.001(2) C11 0.013(3) 0.017(2) 0.020(4) -0.001(2) 0.004(3) -0.001(2) C12 0.022(3) 0.015(2) 0.019(4) 0.002(2) -0.005(3) -0.001(2) C13 0.014(3) 0.021(3) 0.013(3) -0.008(2) 0.001(3) 0.003(2) C14 0.020(3) 0.019(2) 0.016(3) 0.003(2) 0.013(3) 0.002(2) C15 0.026(3) 0.025(2) 0.015(3) -0.005(2) 0.001(3) 0.000(3) C16 0.021(3) 0.025(3) 0.023(4) -0.002(2) -0.005(3) 0.001(2) C17 0.021(3) 0.018(3) 0.016(4) -0.002(2) -0.006(3) 0.002(2) C18 0.021(3) 0.023(3) 0.027(4) 0.000(2) -0.007(3) -0.004(3) C19 0.021(3) 0.024(3) 0.025(4) -0.001(2) -0.006(3) -0.002(3) C20 0.018(3) 0.028(3) 0.026(4) 0.003(2) -0.008(3) -0.002(3) C21 0.018(3) 0.034(3) 0.033(4) -0.004(3) -0.001(3) -0.010(3) C22 0.020(3) 0.026(3) 0.033(4) -0.003(2) -0.003(3) -0.001(3) C23 0.018(3) 0.028(3) 0.019(4) -0.009(2) -0.002(3) -0.008(3) C24 0.022(3) 0.022(3) 0.026(4) 0.002(2) 0.011(3) 0.004(3) C25 0.032(4) 0.054(4) 0.033(4) 0.000(3) 0.008(3) 0.012(3) C26 0.036(4) 0.026(3) 0.042(5) -0.008(3) 0.002(3) -0.007(3) C27 0.021(3) 0.032(3) 0.041(5) -0.001(3) -0.001(3) -0.008(3) C28 0.020(4) 0.045(4) 0.045(5) 0.011(3) -0.004(3) 0.003(3) C29 0.027(3) 0.030(3) 0.022(4) 0.004(2) -0.005(4) 0.000(3) C30 0.064(5) 0.025(3) 0.028(5) -0.004(3) -0.012(4) 0.005(3) C31 0.032(3) 0.031(3) 0.024(4) 0.005(2) -0.004(4) 0.005(3) C32 0.018(3) 0.016(2) 0.022(4) -0.003(2) -0.003(3) 0.000(2) C33 0.020(3) 0.017(3) 0.029(4) -0.002(2) -0.001(3) 0.004(3) C34 0.039(4) 0.022(3) 0.020(4) -0.009(3) 0.002(3) 0.001(3) C35 0.033(4) 0.023(3) 0.024(4) -0.001(3) 0.004(3) -0.001(2) C37 0.032(4) 0.018(3) 0.017(4) 0.003(2) -0.003(3) 0.004(2) C38 0.024(3) 0.022(3) 0.017(4) -0.002(2) 0.000(3) -0.002(2) C39 0.034(3) 0.024(3) 0.025(4) -0.003(2) 0.006(4) 0.007(3) C40 0.043(4) 0.036(3) 0.012(4) 0.011(3) 0.002(3) 0.005(3) C41 0.035(4) 0.050(4) 0.022(5) 0.000(3) -0.005(3) -0.007(3) C42 0.024(3) 0.029(3) 0.020(4) 0.004(3) 0.002(3) 0.001(3) N1 0.022(2) 0.0189(19) 0.016(3) 0.0021(19) 0.002(2) -0.0080(19) C44 0.020(3) 0.025(3) 0.020(4) 0.006(2) -0.006(3) -0.009(3) C45 0.022(3) 0.023(3) 0.014(4) -0.001(2) 0.001(3) -0.005(2) C46 0.024(3) 0.034(3) 0.021(4) 0.003(3) 0.001(3) -0.009(3) C47 0.020(3) 0.044(3) 0.029(4) 0.004(3) 0.007(3) -0.002(3) C48 0.016(3) 0.042(3) 0.038(4) 0.003(3) -0.004(3) -0.009(3) C49 0.019(3) 0.027(3) 0.033(4) 0.008(2) -0.005(3) -0.010(3) C50 0.021(3) 0.046(3) 0.030(4) 0.011(2) 0.001(3) -0.007(3) C51 0.039(4) 0.027(3) 0.028(4) 0.012(2) -0.008(4) -0.002(3) C52 0.023(3) 0.030(3) 0.035(4) 0.005(3) 0.002(3) -0.016(3) C53 0.027(4) 0.030(3) 0.024(4) 0.006(3) -0.004(3) -0.001(3) C55 0.024(3) 0.019(2) 0.022(4) 0.002(2) 0.002(3) -0.002(3) C56 0.021(3) 0.033(3) 0.023(4) 0.001(3) -0.010(3) -0.003(3) C57 0.033(4) 0.021(3) 0.024(4) 0.010(3) -0.002(3) -0.001(2) C58 0.023(3) 0.018(2) 0.013(4) -0.001(2) 0.001(3) 0.002(2) C59 0.021(3) 0.026(3) 0.020(4) 0.001(2) -0.009(3) -0.007(3) C60 0.033(4) 0.017(3) 0.030(4) -0.004(2) -0.008(3) -0.004(3) C61 0.040(4) 0.018(2) 0.015(4) -0.002(2) 0.001(3) 0.003(3) C62 0.036(4) 0.025(3) 0.014(3) 0.005(3) -0.004(3) 0.000(3) N2 0.017(2) 0.0168(19) 0.019(3) 0.0006(17) -0.001(2) 0.0034(18) C64 0.023(3) 0.012(2) 0.008(3) 0.0060(19) 0.001(3) 0.004(2) C65 0.018(3) 0.020(2) 0.014(4) -0.004(2) 0.000(3) 0.004(2) C66 0.018(3) 0.030(3) 0.016(4) 0.002(2) -0.001(3) 0.001(3) C67 0.027(3) 0.022(3) 0.020(4) 0.007(3) 0.011(3) -0.001(2) C68 0.025(3) 0.016(2) 0.014(4) -0.004(2) 0.000(3) -0.004(2) C69 0.023(3) 0.015(2) 0.019(4) 0.003(2) 0.002(3) 0.001(2) C70 0.028(3) 0.035(3) 0.013(4) 0.003(3) 0.005(3) 0.005(3) C71 0.030(4) 0.026(3) 0.026(4) -0.008(2) -0.001(3) 0.008(3) C72 0.029(3) 0.016(2) 0.031(4) -0.001(2) 0.004(4) 0.001(3) C73 0.029(3) 0.011(2) 0.017(3) 0.002(2) 0.003(3) -0.001(2) C74 0.016(3) 0.017(2) 0.012(3) 0.008(2) 0.005(3) 0.002(2) C75 0.025(3) 0.024(3) 0.021(4) 0.002(2) -0.001(3) 0.005(3) C76 0.031(4) 0.034(3) 0.011(4) 0.007(3) 0.006(3) 0.009(3) C77 0.045(4) 0.031(3) 0.015(4) 0.015(3) -0.005(3) -0.001(3) C78 0.022(3) 0.027(3) 0.022(4) 0.000(2) -0.005(3) 0.000(3) C79 0.024(3) 0.028(3) 0.016(4) -0.002(2) 0.007(3) -0.001(3) C80 0.014(3) 0.023(2) 0.020(4) 0.000(2) 0.004(3) 0.005(3) C81 0.019(3) 0.024(3) 0.022(4) 0.005(2) 0.001(3) -0.003(3) C82 0.019(3) 0.021(2) 0.029(4) 0.005(2) 0.002(3) 0.004(3) C83 0.024(3) 0.035(3) 0.027(4) 0.009(3) 0.005(3) 0.002(3) C84 0.018(3) 0.034(3) 0.027(4) -0.003(2) 0.001(3) 0.009(3) C85 0.031(4) 0.037(3) 0.022(4) 0.006(3) -0.006(3) 0.003(3) C86 0.020(3) 0.032(3) 0.022(4) 0.002(2) -0.001(3) 0.008(3) C87 0.024(3) 0.025(3) 0.014(4) 0.002(2) -0.002(3) -0.002(2) C88 0.023(3) 0.025(3) 0.023(4) 0.007(2) 0.003(3) 0.009(3) C89 0.024(3) 0.021(2) 0.025(3) -0.003(2) 0.003(3) 0.004(3) C90 0.018(3) 0.014(2) 0.015(3) -0.003(2) -0.007(3) -0.004(2) C91 0.022(3) 0.025(3) 0.014(4) -0.007(2) -0.002(3) -0.007(2) C92 0.014(3) 0.027(3) 0.016(4) -0.005(2) 0.003(3) 0.010(3) C93 0.013(3) 0.029(3) 0.016(3) 0.001(2) 0.008(3) 0.002(2) C94 0.017(3) 0.034(3) 0.012(3) 0.001(2) 0.001(3) -0.001(3) C95 0.031(3) 0.028(3) 0.023(4) 0.006(2) 0.004(3) -0.002(3) C96 0.043(4) 0.045(4) 0.015(4) -0.009(3) 0.004(3) -0.006(3) C97 0.023(3) 0.041(3) 0.021(4) 0.005(3) 0.001(3) 0.003(3) C98 0.026(4) 0.042(3) 0.027(4) 0.000(3) 0.004(3) 0.001(3) C99 0.021(3) 0.065(4) 0.033(4) 0.008(3) -0.004(3) -0.003(4) C100 0.029(4) 0.034(4) 0.172(12) -0.001(3) -0.005(6) -0.004(5) C101 0.024(3) 0.046(4) 0.018(4) -0.006(3) -0.016(3) 0.007(3) C102 0.018(3) 0.034(3) 0.016(3) -0.011(2) 0.004(3) 0.002(3) C103 0.025(3) 0.037(3) 0.027(4) -0.011(3) -0.005(3) -0.003(3) C104 0.020(3) 0.029(3) 0.017(4) -0.003(2) 0.001(3) -0.001(2) C105 0.035(3) 0.022(2) 0.015(4) -0.006(2) 0.002(3) 0.004(3) C106 0.027(3) 0.014(2) 0.014(3) -0.002(2) -0.002(3) 0.000(2) C107 0.027(3) 0.013(2) 0.017(4) -0.008(2) -0.001(3) -0.005(2) C108 0.013(3) 0.018(2) 0.013(3) -0.002(2) -0.002(2) 0.007(2) C109 0.030(3) 0.014(2) 0.007(3) -0.002(2) -0.001(3) 0.003(2) C110 0.019(3) 0.022(3) 0.017(3) 0.001(2) -0.004(3) 0.004(2) C111 0.020(3) 0.021(3) 0.018(4) 0.005(2) 0.008(3) 0.006(2) C112 0.037(4) 0.015(2) 0.010(4) -0.001(2) -0.002(3) -0.002(2) C113 0.023(3) 0.017(2) 0.015(3) 0.000(2) 0.005(3) 0.006(2) C114 0.025(3) 0.020(2) 0.023(4) -0.007(2) -0.010(3) 0.000(2) C115 0.036(4) 0.029(3) 0.048(5) -0.010(3) -0.009(3) 0.000(3) C116 0.032(4) 0.037(3) 0.021(4) -0.006(3) -0.006(3) -0.002(3) C117 0.032(3) 0.028(3) 0.017(4) 0.004(2) -0.001(3) -0.008(2) C118 0.035(4) 0.039(3) 0.026(4) 0.010(3) -0.002(3) 0.001(3) C119 0.019(3) 0.022(3) 0.016(4) 0.002(2) -0.004(3) -0.004(2) C120 0.034(4) 0.030(3) 0.011(4) -0.007(3) -0.002(3) -0.002(3) C300 0.029(4) 0.021(3) 0.026(4) -0.005(3) -0.013(3) -0.002(2) C304 0.024(3) 0.043(3) 0.043(4) 0.001(3) 0.000(4) -0.010(4) C305 0.040(4) 0.082(5) 0.060(6) 0.003(4) 0.005(5) -0.020(6) C306 0.047(5) 0.047(4) 0.088(7) -0.009(4) -0.008(5) -0.012(4) C309 0.102(8) 0.075(6) 0.030(5) -0.009(5) 0.008(5) 0.003(4) C308 0.060(5) 0.047(4) 0.058(7) -0.012(4) 0.020(5) 0.001(4) C307 0.047(5) 0.049(4) 0.060(6) -0.003(3) 0.013(4) -0.007(4) C303 0.034(4) 0.015(3) 0.024(4) -0.002(2) -0.005(3) -0.002(2) C310 0.124(8) 0.080(5) 0.043(6) -0.015(5) -0.003(6) -0.004(5) C312 0.055(5) 0.037(4) 0.047(5) -0.015(3) 0.002(4) -0.011(3) C311 0.033(4) 0.084(5) 0.024(4) 0.004(4) -0.013(3) -0.015(4) C313 0.040(4) 0.046(4) 0.029(4) -0.007(3) 0.009(4) 0.007(3) C316 0.034(5) 0.097(7) 0.143(12) -0.010(5) -0.009(6) 0.067(8) C314 0.076(7) 0.084(7) 0.113(11) 0.015(6) 0.019(7) -0.005(7) C318 0.053(5) 0.044(5) 0.137(11) 0.008(4) 0.017(6) 0.027(6) C315 0.093(8) 0.078(7) 0.117(11) 0.031(6) 0.003(7) -0.001(7) C317 0.059(6) 0.076(7) 0.151(13) -0.006(5) 0.020(8) 0.034(8) C321 0.018(3) 0.017(2) 0.015(4) 0.0026(19) 0.001(3) 0.002(3) C319 0.025(4) 0.048(4) 0.103(8) 0.011(3) -0.010(4) 0.012(4) C322 0.038(4) 0.032(3) 0.064(6) 0.014(3) 0.011(4) 0.014(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Sn1 C302 . 2.245(6) ? Sn1 N1 . 2.305(4) ? Sn1 C32 . 2.321(6) ? C302 C301 . 1.391(7) ? C302 C303 . 1.394(8) ? Sn3 C323 . 2.213(5) ? Sn3 N2 . 2.292(4) ? Sn3 C90 . 2.324(6) ? P1 N1 . 1.613(5) ? P1 C301 . 1.798(5) ? P1 C321 . 1.833(6) ? P1 C37 . 1.834(7) ? P2 N2 . 1.608(4) ? P2 C74 . 1.795(6) ? P2 C64 . 1.796(5) ? P2 C320 . 1.813(6) ? C323 C68 . 1.390(8) ? C323 C64 . 1.408(7) ? C301 C55 . 1.387(8) ? C320 C73 . 1.387(8) ? C320 C69 . 1.405(11) ? C0AJ C318 . 1.612(14) ? C0AJ H0A1 . 0.98 ? C0AJ H0A2 . 0.98 ? C0AJ H0A3 . 0.98 ? C2 C313 . 1.525(9) ? C2 C4 . 1.529(8) ? C2 C3 . 1.531(7) ? C2 H2 . 1.0 ? C3 H3A . 0.98 ? C3 H3B . 0.98 ? C3 H3C . 0.98 ? C4 C12 . 1.392(8) ? C4 C5 . 1.408(8) ? C5 C6 . 1.368(8) ? C5 H5 . 0.95 ? C6 C10 . 1.385(8) ? C6 C7 . 1.511(8) ? C7 C9 . 1.512(8) ? C7 C8 . 1.519(9) ? C7 H7 . 1.0 ? C8 H8A . 0.98 ? C8 H8B . 0.98 ? C8 H8C . 0.98 ? C9 H9A . 0.98 ? C9 H9B . 0.98 ? C9 H9C . 0.98 ? C10 C11 . 1.398(8) ? C10 H10 . 0.95 ? C11 C12 . 1.400(8) ? C11 C33 . 1.524(8) ? C12 C13 . 1.533(8) ? C13 C32 . 1.398(7) ? C13 C14 . 1.413(8) ? C14 C15 . 1.372(8) ? C14 H14 . 0.95 ? C15 C16 . 1.367(8) ? C15 H15 . 0.95 ? C16 C17 . 1.410(8) ? C16 H16 . 0.95 ? C17 C32 . 1.427(8) ? C17 C18 . 1.506(8) ? C18 C19 . 1.407(8) ? C18 C23 . 1.414(9) ? C19 C20 . 1.396(8) ? C19 C29 . 1.509(10) ? C20 C21 . 1.398(9) ? C20 H20 . 0.95 ? C21 C22 . 1.365(8) ? C21 C27 . 1.542(8) ? C22 C23 . 1.379(8) ? C22 H22 . 0.95 ? C23 C24 . 1.542(8) ? C24 C25 . 1.541(9) ? C24 C26 . 1.547(8) ? C24 H24 . 1.0 ? C25 H25A . 0.98 ? C25 H25B . 0.98 ? C25 H25C . 0.98 ? C26 H26A . 0.98 ? C26 H26B . 0.98 ? C26 H26C . 0.98 ? C27 C304 . 1.522(9) ? C27 C28 . 1.522(9) ? C27 H27 . 1.0 ? C28 H28A . 0.98 ? C28 H28B . 0.98 ? C28 H28C . 0.98 ? C29 C30 . 1.526(10) ? C29 C31 . 1.532(7) ? C29 H29 . 1.0 ? C30 H30A . 0.98 ? C30 H30B . 0.98 ? C30 H30C . 0.98 ? C31 H31M . 0.98 ? C31 H31N . 0.98 ? C31 H31O . 0.98 ? C33 C35 . 1.517(7) ? C33 C34 . 1.533(9) ? C33 H33 . 1.0 ? C34 H34A . 0.98 ? C34 H34B . 0.98 ? C34 H34C . 0.98 ? C35 H35A . 0.98 ? C35 H35B . 0.98 ? C35 H35C . 0.98 ? C37 C42 . 1.369(9) ? C37 C38 . 1.393(8) ? C38 C39 . 1.365(10) ? C38 H38 . 0.95 ? C39 C40 . 1.383(9) ? C39 H39 . 0.95 ? C40 C41 . 1.391(9) ? C40 H40 . 0.95 ? C41 C42 . 1.386(10) ? C41 H41 . 0.95 ? C42 H42 . 0.95 ? N1 C44 . 1.499(7) ? C44 C49 . 1.527(7) ? C44 C53 . 1.537(8) ? C44 C45 . 1.553(8) ? C45 C46 . 1.527(8) ? C45 H45A . 0.99 ? C45 H45B . 0.99 ? C46 C47 . 1.512(8) ? C46 C52 . 1.518(9) ? C46 H46 . 1.0 ? C47 C48 . 1.537(9) ? C47 H47A . 0.99 ? C47 H47B . 0.99 ? C48 C50 . 1.532(8) ? C48 C49 . 1.535(7) ? C48 H48 . 1.0 ? C49 H49A . 0.99 ? C49 H49B . 0.99 ? C50 C51 . 1.514(8) ? C50 H50A . 0.99 ? C50 H50B . 0.99 ? C51 C52 . 1.520(10) ? C51 C53 . 1.560(8) ? C51 H51 . 1.0 ? C52 H52A . 0.99 ? C52 H52B . 0.99 ? C53 H53A . 0.99 ? C53 H53B . 0.99 ? C55 C56 . 1.384(8) ? C55 H55 . 0.95 ? C56 C57 . 1.372(8) ? C56 H56 . 0.95 ? C57 C303 . 1.371(8) ? C57 H57 . 0.95 ? C58 C59 . 1.382(7) ? C58 C321 . 1.401(10) ? C58 H58 . 0.95 ? C59 C60 . 1.361(8) ? C59 H59 . 0.95 ? C60 C61 . 1.418(9) ? C60 H60 . 0.95 ? C61 C62 . 1.381(7) ? C61 H61 . 0.95 ? C62 C321 . 1.396(8) ? C62 H62 . 0.95 ? N2 C80 . 1.503(6) ? C64 C65 . 1.395(7) ? C65 C66 . 1.371(8) ? C65 H65 . 0.95 ? C66 C67 . 1.376(8) ? C66 H66 . 0.95 ? C67 C68 . 1.394(8) ? C67 H67 . 0.95 ? C68 H68 . 0.95 ? C69 C70 . 1.369(8) ? C69 H69 . 0.95 ? C70 C71 . 1.380(8) ? C70 H70 . 0.95 ? C71 C72 . 1.380(10) ? C71 H71 . 0.95 ? C72 C73 . 1.390(7) ? C72 H72 . 0.95 ? C73 H73 . 0.95 ? C74 C75 . 1.395(8) ? C74 C79 . 1.409(8) ? C75 C76 . 1.364(10) ? C75 H75 . 0.95 ? C76 C77 . 1.394(9) ? C76 H76 . 0.95 ? C77 C78 . 1.382(9) ? C77 H77 . 0.95 ? C78 C79 . 1.391(10) ? C78 H78 . 0.95 ? C79 H79 . 0.95 ? C80 C89 . 1.525(7) ? C80 C81 . 1.539(7) ? C80 C87 . 1.539(9) ? C81 C82 . 1.537(7) ? C81 H81A . 0.99 ? C81 H81B . 0.99 ? C82 C83 . 1.533(7) ? C82 C88 . 1.537(9) ? C82 H82 . 1.0 ? C83 C84 . 1.519(8) ? C83 H83A . 0.99 ? C83 H83B . 0.99 ? C84 C85 . 1.522(9) ? C84 C89 . 1.530(7) ? C84 H84 . 1.0 ? C85 C86 . 1.549(8) ? C85 H85A . 0.99 ? C85 H85B . 0.99 ? C86 C88 . 1.525(8) ? C86 C87 . 1.530(8) ? C86 H86 . 1.0 ? C87 H87A . 0.99 ? C87 H87B . 0.99 ? C88 H88A . 0.99 ? C88 H88B . 0.99 ? C89 H89A . 0.99 ? C89 H89B . 0.99 ? C90 C107 . 1.403(7) ? C90 C91 . 1.435(8) ? C91 C104 . 1.392(8) ? C91 C92 . 1.508(8) ? C92 C93 . 1.412(8) ? C92 C102 . 1.417(9) ? C93 C97 . 1.399(8) ? C93 C94 . 1.522(9) ? C94 C95 . 1.531(7) ? C94 C96 . 1.540(9) ? C94 H94 . 1.0 ? C95 H95A . 0.98 ? C95 H95B . 0.98 ? C95 H95C . 0.98 ? C96 H96A . 0.98 ? C96 H96B . 0.98 ? C96 H96C . 0.98 ? C97 C98 . 1.407(9) ? C97 H97 . 0.95 ? C98 C101 . 1.353(9) ? C98 C99 . 1.520(8) ? C99 C100 . 1.475(10) ? C99 C319 . 1.509(9) ? C99 H99 . 1.0 ? C100 H10A . 0.98 ? C100 H10B . 0.98 ? C100 H10C . 0.98 ? C101 C102 . 1.411(8) ? C101 H101 . 0.95 ? C102 C103 . 1.495(8) ? C103 C311 . 1.532(9) ? C103 C312 . 1.552(8) ? C103 H103 . 1.0 ? C104 C105 . 1.360(7) ? C104 H104 . 0.95 ? C105 C106 . 1.378(8) ? C105 H105 . 0.95 ? C106 C107 . 1.399(8) ? C106 H106 . 0.95 ? C107 C108 . 1.507(8) ? C108 C109 . 1.397(8) ? C108 C113 . 1.413(8) ? C109 C110 . 1.394(8) ? C109 C119 . 1.527(8) ? C110 C111 . 1.404(8) ? C110 H110 . 0.95 ? C111 C112 . 1.364(8) ? C111 C117 . 1.532(7) ? C112 C113 . 1.390(8) ? C112 H112 . 0.95 ? C113 C114 . 1.520(8) ? C114 C115 . 1.530(7) ? C114 C116 . 1.538(9) ? C114 H114 . 1.0 ? C115 H11A . 0.98 ? C115 H11B . 0.98 ? C115 H11C . 0.98 ? C116 H11D . 0.98 ? C116 H11E . 0.98 ? C116 H11F . 0.98 ? C117 C118 . 1.506(8) ? C117 C322 . 1.559(9) ? C117 H117 . 1.0 ? C118 H11G . 0.98 ? C118 H11H . 0.98 ? C118 H11I . 0.98 ? C119 C300 . 1.529(8) ? C119 C120 . 1.536(8) ? C119 H119 . 1.0 ? C120 H12A . 0.98 ? C120 H12B . 0.98 ? C120 H12C . 0.98 ? C300 H30D . 0.98 ? C300 H30E . 0.98 ? C300 H30F . 0.98 ? C304 H30G . 0.98 ? C304 H30H . 0.98 ? C304 H30I . 0.98 ? C305 C306 . 1.512(11) ? C305 H30J . 0.98 ? C305 H30K . 0.98 ? C305 H30L . 0.98 ? C306 C307 . 1.508(10) ? C306 H30M . 0.99 ? C306 H30N . 0.99 ? C309 C308 . 1.512(11) ? C309 C310 . 1.539(11) ? C309 H30O . 0.99 ? C309 H30P . 0.99 ? C308 C307 . 1.518(10) ? C308 H30Q . 0.99 ? C308 H30R . 0.99 ? C307 H30S . 0.99 ? C307 H30T . 0.99 ? C303 H303 . 0.95 ? C310 H31D . 0.98 ? C310 H31E . 0.98 ? C310 H31F . 0.98 ? C312 H31G . 0.98 ? C312 H31H . 0.98 ? C312 H31I . 0.98 ? C311 H31J . 0.98 ? C311 H31K . 0.98 ? C311 H31L . 0.98 ? C313 H900 . 0.98 ? C313 H901 . 0.98 ? C313 H902 . 0.98 ? C316 C317 . 1.517(15) ? C316 C315 . 1.523(13) ? C316 H31P . 0.99 ? C316 H31Q . 0.99 ? C314 C315 . 1.454(13) ? C314 H31R . 0.98 ? C314 H31S . 0.98 ? C314 H31T . 0.98 ? C318 C317 . 1.473(14) ? C318 H31U . 0.99 ? C318 H31V . 0.99 ? C315 H31W . 0.99 ? C315 H930 . 0.99 ? C317 H931 . 0.99 ? C317 H932 . 0.99 ? C319 H933 . 0.98 ? C319 H934 . 0.98 ? C319 H935 . 0.98 ? C322 H32A . 0.98 ? C322 H32B . 0.98 ? C322 H32C . 0.98 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag C302 Sn1 N1 . . 80.32(16) ? C302 Sn1 C32 . . 103.0(2) ? N1 Sn1 C32 . . 107.24(17) ? C301 C302 C303 . . 115.5(5) ? C301 C302 Sn1 . . 118.9(4) ? C303 C302 Sn1 . . 123.6(4) ? C323 Sn3 N2 . . 80.27(16) ? C323 Sn3 C90 . . 104.5(2) ? N2 Sn3 C90 . . 109.44(17) ? N1 P1 C301 . . 107.0(2) ? N1 P1 C321 . . 119.7(3) ? C301 P1 C321 . . 104.2(3) ? N1 P1 C37 . . 113.5(3) ? C301 P1 C37 . . 107.9(3) ? C321 P1 C37 . . 103.8(3) ? N2 P2 C74 . . 113.0(3) ? N2 P2 C64 . . 106.5(2) ? C74 P2 C64 . . 106.4(3) ? N2 P2 C320 . . 119.7(3) ? C74 P2 C320 . . 105.6(3) ? C64 P2 C320 . . 104.7(3) ? C68 C323 C64 . . 115.6(5) ? C68 C323 Sn3 . . 123.9(4) ? C64 C323 Sn3 . . 119.6(4) ? C55 C301 C302 . . 122.7(5) ? C55 C301 P1 . . 121.4(3) ? C302 C301 P1 . . 115.9(4) ? C73 C320 C69 . . 117.6(5) ? C73 C320 P2 . . 123.6(6) ? C69 C320 P2 . . 118.7(4) ? C318 C0AJ H0A1 . . 109.5 ? C318 C0AJ H0A2 . . 109.5 ? H0A1 C0AJ H0A2 . . 109.5 ? C318 C0AJ H0A3 . . 109.5 ? H0A1 C0AJ H0A3 . . 109.5 ? H0A2 C0AJ H0A3 . . 109.5 ? C313 C2 C4 . . 112.4(5) ? C313 C2 C3 . . 110.5(5) ? C4 C2 C3 . . 111.1(5) ? C313 C2 H2 . . 107.6 ? C4 C2 H2 . . 107.6 ? C3 C2 H2 . . 107.6 ? C2 C3 H3A . . 109.5 ? C2 C3 H3B . . 109.5 ? H3A C3 H3B . . 109.5 ? C2 C3 H3C . . 109.5 ? H3A C3 H3C . . 109.5 ? H3B C3 H3C . . 109.5 ? C12 C4 C5 . . 118.0(5) ? C12 C4 C2 . . 121.9(5) ? C5 C4 C2 . . 120.1(5) ? C6 C5 C4 . . 123.2(6) ? C6 C5 H5 . . 118.4 ? C4 C5 H5 . . 118.4 ? C5 C6 C10 . . 117.2(5) ? C5 C6 C7 . . 121.3(5) ? C10 C6 C7 . . 121.3(5) ? C6 C7 C9 . . 113.1(5) ? C6 C7 C8 . . 110.7(5) ? C9 C7 C8 . . 109.2(5) ? C6 C7 H7 . . 107.9 ? C9 C7 H7 . . 107.9 ? C8 C7 H7 . . 107.9 ? C7 C8 H8A . . 109.5 ? C7 C8 H8B . . 109.5 ? H8A C8 H8B . . 109.5 ? C7 C8 H8C . . 109.5 ? H8A C8 H8C . . 109.5 ? H8B C8 H8C . . 109.5 ? C7 C9 H9A . . 109.5 ? C7 C9 H9B . . 109.5 ? H9A C9 H9B . . 109.5 ? C7 C9 H9C . . 109.5 ? H9A C9 H9C . . 109.5 ? H9B C9 H9C . . 109.5 ? C6 C10 C11 . . 122.6(5) ? C6 C10 H10 . . 118.7 ? C11 C10 H10 . . 118.7 ? C10 C11 C12 . . 118.5(5) ? C10 C11 C33 . . 119.4(5) ? C12 C11 C33 . . 122.0(5) ? C4 C12 C11 . . 120.5(5) ? C4 C12 C13 . . 119.5(5) ? C11 C12 C13 . . 118.7(5) ? C32 C13 C14 . . 121.6(5) ? C32 C13 C12 . . 125.1(5) ? C14 C13 C12 . . 113.1(5) ? C15 C14 C13 . . 121.3(5) ? C15 C14 H14 . . 119.4 ? C13 C14 H14 . . 119.4 ? C16 C15 C14 . . 118.6(6) ? C16 C15 H15 . . 120.7 ? C14 C15 H15 . . 120.7 ? C15 C16 C17 . . 121.8(6) ? C15 C16 H16 . . 119.1 ? C17 C16 H16 . . 119.1 ? C16 C17 C32 . . 120.6(5) ? C16 C17 C18 . . 111.9(5) ? C32 C17 C18 . . 127.0(5) ? C19 C18 C23 . . 118.6(6) ? C19 C18 C17 . . 121.8(6) ? C23 C18 C17 . . 119.0(5) ? C20 C19 C18 . . 118.8(6) ? C20 C19 C29 . . 118.5(5) ? C18 C19 C29 . . 122.6(5) ? C19 C20 C21 . . 122.1(5) ? C19 C20 H20 . . 119.0 ? C21 C20 H20 . . 119.0 ? C22 C21 C20 . . 118.1(5) ? C22 C21 C27 . . 123.5(6) ? C20 C21 C27 . . 118.4(5) ? C21 C22 C23 . . 122.1(6) ? C21 C22 H22 . . 118.9 ? C23 C22 H22 . . 118.9 ? C22 C23 C18 . . 120.2(5) ? C22 C23 C24 . . 118.8(5) ? C18 C23 C24 . . 120.8(5) ? C25 C24 C23 . . 114.0(5) ? C25 C24 C26 . . 110.9(5) ? C23 C24 C26 . . 110.3(5) ? C25 C24 H24 . . 107.1 ? C23 C24 H24 . . 107.1 ? C26 C24 H24 . . 107.1 ? C24 C25 H25A . . 109.5 ? C24 C25 H25B . . 109.5 ? H25A C25 H25B . . 109.5 ? C24 C25 H25C . . 109.5 ? H25A C25 H25C . . 109.5 ? H25B C25 H25C . . 109.5 ? C24 C26 H26A . . 109.5 ? C24 C26 H26B . . 109.5 ? H26A C26 H26B . . 109.5 ? C24 C26 H26C . . 109.5 ? H26A C26 H26C . . 109.5 ? H26B C26 H26C . . 109.5 ? C304 C27 C28 . . 110.6(5) ? C304 C27 C21 . . 113.6(5) ? C28 C27 C21 . . 110.1(5) ? C304 C27 H27 . . 107.4 ? C28 C27 H27 . . 107.4 ? C21 C27 H27 . . 107.4 ? C27 C28 H28A . . 109.5 ? C27 C28 H28B . . 109.5 ? H28A C28 H28B . . 109.5 ? C27 C28 H28C . . 109.5 ? H28A C28 H28C . . 109.5 ? H28B C28 H28C . . 109.5 ? C19 C29 C30 . . 111.7(5) ? C19 C29 C31 . . 113.0(6) ? C30 C29 C31 . . 108.5(5) ? C19 C29 H29 . . 107.8 ? C30 C29 H29 . . 107.8 ? C31 C29 H29 . . 107.8 ? C29 C30 H30A . . 109.5 ? C29 C30 H30B . . 109.5 ? H30A C30 H30B . . 109.5 ? C29 C30 H30C . . 109.5 ? H30A C30 H30C . . 109.5 ? H30B C30 H30C . . 109.5 ? C29 C31 H31M . . 109.5 ? C29 C31 H31N . . 109.5 ? H31M C31 H31N . . 109.5 ? C29 C31 H31O . . 109.5 ? H31M C31 H31O . . 109.5 ? H31N C31 H31O . . 109.5 ? C13 C32 C17 . . 116.0(5) ? C13 C32 Sn1 . . 120.5(4) ? C17 C32 Sn1 . . 121.4(4) ? C35 C33 C11 . . 112.7(5) ? C35 C33 C34 . . 109.7(5) ? C11 C33 C34 . . 111.1(4) ? C35 C33 H33 . . 107.7 ? C11 C33 H33 . . 107.7 ? C34 C33 H33 . . 107.7 ? C33 C34 H34A . . 109.5 ? C33 C34 H34B . . 109.5 ? H34A C34 H34B . . 109.5 ? C33 C34 H34C . . 109.5 ? H34A C34 H34C . . 109.5 ? H34B C34 H34C . . 109.5 ? C33 C35 H35A . . 109.5 ? C33 C35 H35B . . 109.5 ? H35A C35 H35B . . 109.5 ? C33 C35 H35C . . 109.5 ? H35A C35 H35C . . 109.5 ? H35B C35 H35C . . 109.5 ? C42 C37 C38 . . 121.2(6) ? C42 C37 P1 . . 118.4(5) ? C38 C37 P1 . . 120.3(5) ? C39 C38 C37 . . 119.6(6) ? C39 C38 H38 . . 120.2 ? C37 C38 H38 . . 120.2 ? C38 C39 C40 . . 119.9(6) ? C38 C39 H39 . . 120.1 ? C40 C39 H39 . . 120.1 ? C39 C40 C41 . . 120.4(7) ? C39 C40 H40 . . 119.8 ? C41 C40 H40 . . 119.8 ? C42 C41 C40 . . 119.6(7) ? C42 C41 H41 . . 120.2 ? C40 C41 H41 . . 120.2 ? C37 C42 C41 . . 119.2(6) ? C37 C42 H42 . . 120.4 ? C41 C42 H42 . . 120.4 ? C44 N1 P1 . . 124.8(3) ? C44 N1 Sn1 . . 119.8(3) ? P1 N1 Sn1 . . 113.2(2) ? N1 C44 C49 . . 109.1(4) ? N1 C44 C53 . . 111.3(5) ? C49 C44 C53 . . 109.0(5) ? N1 C44 C45 . . 111.1(5) ? C49 C44 C45 . . 106.9(5) ? C53 C44 C45 . . 109.3(4) ? C46 C45 C44 . . 109.8(5) ? C46 C45 H45A . . 109.7 ? C44 C45 H45A . . 109.7 ? C46 C45 H45B . . 109.7 ? C44 C45 H45B . . 109.7 ? H45A C45 H45B . . 108.2 ? C47 C46 C52 . . 110.3(5) ? C47 C46 C45 . . 109.8(5) ? C52 C46 C45 . . 110.4(5) ? C47 C46 H46 . . 108.8 ? C52 C46 H46 . . 108.8 ? C45 C46 H46 . . 108.8 ? C46 C47 C48 . . 108.6(5) ? C46 C47 H47A . . 110.0 ? C48 C47 H47A . . 110.0 ? C46 C47 H47B . . 110.0 ? C48 C47 H47B . . 110.0 ? H47A C47 H47B . . 108.4 ? C50 C48 C49 . . 108.8(5) ? C50 C48 C47 . . 109.5(5) ? C49 C48 C47 . . 109.4(5) ? C50 C48 H48 . . 109.7 ? C49 C48 H48 . . 109.7 ? C47 C48 H48 . . 109.7 ? C44 C49 C48 . . 111.5(4) ? C44 C49 H49A . . 109.3 ? C48 C49 H49A . . 109.3 ? C44 C49 H49B . . 109.3 ? C48 C49 H49B . . 109.3 ? H49A C49 H49B . . 108.0 ? C51 C50 C48 . . 109.7(5) ? C51 C50 H50A . . 109.7 ? C48 C50 H50A . . 109.7 ? C51 C50 H50B . . 109.7 ? C48 C50 H50B . . 109.7 ? H50A C50 H50B . . 108.2 ? C50 C51 C52 . . 109.9(6) ? C50 C51 C53 . . 109.7(4) ? C52 C51 C53 . . 108.8(5) ? C50 C51 H51 . . 109.5 ? C52 C51 H51 . . 109.5 ? C53 C51 H51 . . 109.5 ? C46 C52 C51 . . 109.6(5) ? C46 C52 H52A . . 109.7 ? C51 C52 H52A . . 109.7 ? C46 C52 H52B . . 109.7 ? C51 C52 H52B . . 109.7 ? H52A C52 H52B . . 108.2 ? C44 C53 C51 . . 109.5(5) ? C44 C53 H53A . . 109.8 ? C51 C53 H53A . . 109.8 ? C44 C53 H53B . . 109.8 ? C51 C53 H53B . . 109.8 ? H53A C53 H53B . . 108.2 ? C56 C55 C301 . . 118.9(5) ? C56 C55 H55 . . 120.5 ? C301 C55 H55 . . 120.5 ? C57 C56 C55 . . 119.9(6) ? C57 C56 H56 . . 120.1 ? C55 C56 H56 . . 120.1 ? C303 C57 C56 . . 119.9(6) ? C303 C57 H57 . . 120.1 ? C56 C57 H57 . . 120.1 ? C59 C58 C321 . . 119.1(5) ? C59 C58 H58 . . 120.4 ? C321 C58 H58 . . 120.4 ? C60 C59 C58 . . 121.8(6) ? C60 C59 H59 . . 119.1 ? C58 C59 H59 . . 119.1 ? C59 C60 C61 . . 119.7(5) ? C59 C60 H60 . . 120.1 ? C61 C60 H60 . . 120.1 ? C62 C61 C60 . . 119.0(5) ? C62 C61 H61 . . 120.5 ? C60 C61 H61 . . 120.5 ? C61 C62 C321 . . 120.7(6) ? C61 C62 H62 . . 119.6 ? C321 C62 H62 . . 119.6 ? C80 N2 P2 . . 123.7(3) ? C80 N2 Sn3 . . 119.9(3) ? P2 N2 Sn3 . . 114.3(2) ? C65 C64 C323 . . 122.7(5) ? C65 C64 P2 . . 121.4(3) ? C323 C64 P2 . . 115.7(4) ? C66 C65 C64 . . 119.6(5) ? C66 C65 H65 . . 120.2 ? C64 C65 H65 . . 120.2 ? C65 C66 C67 . . 119.6(5) ? C65 C66 H66 . . 120.2 ? C67 C66 H66 . . 120.2 ? C66 C67 C68 . . 120.5(5) ? C66 C67 H67 . . 119.7 ? C68 C67 H67 . . 119.7 ? C323 C68 C67 . . 122.1(5) ? C323 C68 H68 . . 119.0 ? C67 C68 H68 . . 119.0 ? C70 C69 C320 . . 122.1(6) ? C70 C69 H69 . . 119.0 ? C320 C69 H69 . . 119.0 ? C69 C70 C71 . . 119.7(6) ? C69 C70 H70 . . 120.2 ? C71 C70 H70 . . 120.2 ? C70 C71 C72 . . 119.4(5) ? C70 C71 H71 . . 120.3 ? C72 C71 H71 . . 120.3 ? C71 C72 C73 . . 121.1(5) ? C71 C72 H72 . . 119.4 ? C73 C72 H72 . . 119.4 ? C320 C73 C72 . . 120.1(6) ? C320 C73 H73 . . 119.9 ? C72 C73 H73 . . 119.9 ? C75 C74 C79 . . 117.9(6) ? C75 C74 P2 . . 119.9(5) ? C79 C74 P2 . . 122.2(5) ? C76 C75 C74 . . 121.6(6) ? C76 C75 H75 . . 119.2 ? C74 C75 H75 . . 119.2 ? C75 C76 C77 . . 119.7(6) ? C75 C76 H76 . . 120.1 ? C77 C76 H76 . . 120.1 ? C78 C77 C76 . . 120.7(7) ? C78 C77 H77 . . 119.6 ? C76 C77 H77 . . 119.6 ? C77 C78 C79 . . 119.0(6) ? C77 C78 H78 . . 120.5 ? C79 C78 H78 . . 120.5 ? C78 C79 C74 . . 121.0(6) ? C78 C79 H79 . . 119.5 ? C74 C79 H79 . . 119.5 ? N2 C80 C89 . . 110.7(4) ? N2 C80 C81 . . 111.7(5) ? C89 C80 C81 . . 106.5(5) ? N2 C80 C87 . . 110.8(5) ? C89 C80 C87 . . 108.1(5) ? C81 C80 C87 . . 108.8(4) ? C82 C81 C80 . . 111.5(5) ? C82 C81 H81A . . 109.3 ? C80 C81 H81A . . 109.3 ? C82 C81 H81B . . 109.3 ? C80 C81 H81B . . 109.3 ? H81A C81 H81B . . 108.0 ? C83 C82 C88 . . 110.7(5) ? C83 C82 C81 . . 108.9(4) ? C88 C82 C81 . . 108.3(5) ? C83 C82 H82 . . 109.6 ? C88 C82 H82 . . 109.6 ? C81 C82 H82 . . 109.6 ? C84 C83 C82 . . 108.6(5) ? C84 C83 H83A . . 110.0 ? C82 C83 H83A . . 110.0 ? C84 C83 H83B . . 110.0 ? C82 C83 H83B . . 110.0 ? H83A C83 H83B . . 108.3 ? C83 C84 C85 . . 109.0(5) ? C83 C84 C89 . . 110.3(5) ? C85 C84 C89 . . 109.9(5) ? C83 C84 H84 . . 109.2 ? C85 C84 H84 . . 109.2 ? C89 C84 H84 . . 109.2 ? C84 C85 C86 . . 109.7(5) ? C84 C85 H85A . . 109.7 ? C86 C85 H85A . . 109.7 ? C84 C85 H85B . . 109.7 ? C86 C85 H85B . . 109.7 ? H85A C85 H85B . . 108.2 ? C88 C86 C87 . . 108.7(5) ? C88 C86 C85 . . 108.7(5) ? C87 C86 C85 . . 109.5(5) ? C88 C86 H86 . . 110.0 ? C87 C86 H86 . . 110.0 ? C85 C86 H86 . . 110.0 ? C86 C87 C80 . . 111.4(5) ? C86 C87 H87A . . 109.4 ? C80 C87 H87A . . 109.4 ? C86 C87 H87B . . 109.4 ? C80 C87 H87B . . 109.4 ? H87A C87 H87B . . 108.0 ? C86 C88 C82 . . 110.0(5) ? C86 C88 H88A . . 109.7 ? C82 C88 H88A . . 109.7 ? C86 C88 H88B . . 109.7 ? C82 C88 H88B . . 109.7 ? H88A C88 H88B . . 108.2 ? C80 C89 C84 . . 111.6(4) ? C80 C89 H89A . . 109.3 ? C84 C89 H89A . . 109.3 ? C80 C89 H89B . . 109.3 ? C84 C89 H89B . . 109.3 ? H89A C89 H89B . . 108.0 ? C107 C90 C91 . . 115.6(5) ? C107 C90 Sn3 . . 120.1(4) ? C91 C90 Sn3 . . 121.6(4) ? C104 C91 C90 . . 120.5(5) ? C104 C91 C92 . . 113.1(5) ? C90 C91 C92 . . 126.0(5) ? C93 C92 C102 . . 119.5(5) ? C93 C92 C91 . . 119.6(6) ? C102 C92 C91 . . 119.9(5) ? C97 C93 C92 . . 119.1(6) ? C97 C93 C94 . . 117.0(5) ? C92 C93 C94 . . 123.8(5) ? C93 C94 C95 . . 111.4(5) ? C93 C94 C96 . . 111.4(5) ? C95 C94 C96 . . 108.9(5) ? C93 C94 H94 . . 108.4 ? C95 C94 H94 . . 108.4 ? C96 C94 H94 . . 108.4 ? C94 C95 H95A . . 109.5 ? C94 C95 H95B . . 109.5 ? H95A C95 H95B . . 109.5 ? C94 C95 H95C . . 109.5 ? H95A C95 H95C . . 109.5 ? H95B C95 H95C . . 109.5 ? C94 C96 H96A . . 109.5 ? C94 C96 H96B . . 109.5 ? H96A C96 H96B . . 109.5 ? C94 C96 H96C . . 109.5 ? H96A C96 H96C . . 109.5 ? H96B C96 H96C . . 109.5 ? C93 C97 C98 . . 121.9(6) ? C93 C97 H97 . . 119.0 ? C98 C97 H97 . . 119.0 ? C101 C98 C97 . . 117.7(6) ? C101 C98 C99 . . 121.2(6) ? C97 C98 C99 . . 121.0(6) ? C100 C99 C319 . . 110.8(6) ? C100 C99 C98 . . 110.5(6) ? C319 C99 C98 . . 114.5(6) ? C100 C99 H99 . . 106.9 ? C319 C99 H99 . . 106.9 ? C98 C99 H99 . . 106.9 ? C99 C100 H10A . . 109.5 ? C99 C100 H10B . . 109.5 ? H10A C100 H10B . . 109.5 ? C99 C100 H10C . . 109.5 ? H10A C100 H10C . . 109.5 ? H10B C100 H10C . . 109.5 ? C98 C101 C102 . . 123.6(6) ? C98 C101 H101 . . 118.2 ? C102 C101 H101 . . 118.2 ? C101 C102 C92 . . 118.1(5) ? C101 C102 C103 . . 120.6(5) ? C92 C102 C103 . . 121.0(5) ? C102 C103 C311 . . 114.3(5) ? C102 C103 C312 . . 110.4(5) ? C311 C103 C312 . . 110.4(5) ? C102 C103 H103 . . 107.1 ? C311 C103 H103 . . 107.1 ? C312 C103 H103 . . 107.1 ? C105 C104 C91 . . 122.3(6) ? C105 C104 H104 . . 118.8 ? C91 C104 H104 . . 118.8 ? C104 C105 C106 . . 118.6(6) ? C104 C105 H105 . . 120.7 ? C106 C105 H105 . . 120.7 ? C105 C106 C107 . . 121.0(5) ? C105 C106 H106 . . 119.5 ? C107 C106 H106 . . 119.5 ? C106 C107 C90 . . 121.9(5) ? C106 C107 C108 . . 111.5(5) ? C90 C107 C108 . . 126.3(5) ? C109 C108 C113 . . 119.7(5) ? C109 C108 C107 . . 121.7(5) ? C113 C108 C107 . . 117.8(5) ? C110 C109 C108 . . 120.1(5) ? C110 C109 C119 . . 119.2(5) ? C108 C109 C119 . . 120.5(5) ? C109 C110 C111 . . 120.7(5) ? C109 C110 H110 . . 119.6 ? C111 C110 H110 . . 119.6 ? C112 C111 C110 . . 117.7(5) ? C112 C111 C117 . . 121.6(5) ? C110 C111 C117 . . 120.6(5) ? C111 C112 C113 . . 124.0(5) ? C111 C112 H112 . . 118.0 ? C113 C112 H112 . . 118.0 ? C112 C113 C108 . . 117.7(5) ? C112 C113 C114 . . 120.7(5) ? C108 C113 C114 . . 121.6(5) ? C113 C114 C115 . . 111.3(5) ? C113 C114 C116 . . 111.4(5) ? C115 C114 C116 . . 110.8(5) ? C113 C114 H114 . . 107.7 ? C115 C114 H114 . . 107.7 ? C116 C114 H114 . . 107.7 ? C114 C115 H11A . . 109.5 ? C114 C115 H11B . . 109.5 ? H11A C115 H11B . . 109.5 ? C114 C115 H11C . . 109.5 ? H11A C115 H11C . . 109.5 ? H11B C115 H11C . . 109.5 ? C114 C116 H11D . . 109.5 ? C114 C116 H11E . . 109.5 ? H11D C116 H11E . . 109.5 ? C114 C116 H11F . . 109.5 ? H11D C116 H11F . . 109.5 ? H11E C116 H11F . . 109.5 ? C118 C117 C111 . . 113.6(4) ? C118 C117 C322 . . 109.0(5) ? C111 C117 C322 . . 109.6(5) ? C118 C117 H117 . . 108.2 ? C111 C117 H117 . . 108.2 ? C322 C117 H117 . . 108.2 ? C117 C118 H11G . . 109.5 ? C117 C118 H11H . . 109.5 ? H11G C118 H11H . . 109.5 ? C117 C118 H11I . . 109.5 ? H11G C118 H11I . . 109.5 ? H11H C118 H11I . . 109.5 ? C109 C119 C300 . . 113.3(5) ? C109 C119 C120 . . 110.0(4) ? C300 C119 C120 . . 109.3(5) ? C109 C119 H119 . . 108.0 ? C300 C119 H119 . . 108.0 ? C120 C119 H119 . . 108.0 ? C119 C120 H12A . . 109.5 ? C119 C120 H12B . . 109.5 ? H12A C120 H12B . . 109.5 ? C119 C120 H12C . . 109.5 ? H12A C120 H12C . . 109.5 ? H12B C120 H12C . . 109.5 ? C119 C300 H30D . . 109.5 ? C119 C300 H30E . . 109.5 ? H30D C300 H30E . . 109.5 ? C119 C300 H30F . . 109.5 ? H30D C300 H30F . . 109.5 ? H30E C300 H30F . . 109.5 ? C27 C304 H30G . . 109.5 ? C27 C304 H30H . . 109.5 ? H30G C304 H30H . . 109.5 ? C27 C304 H30I . . 109.5 ? H30G C304 H30I . . 109.5 ? H30H C304 H30I . . 109.5 ? C306 C305 H30J . . 109.5 ? C306 C305 H30K . . 109.5 ? H30J C305 H30K . . 109.5 ? C306 C305 H30L . . 109.5 ? H30J C305 H30L . . 109.5 ? H30K C305 H30L . . 109.5 ? C307 C306 C305 . . 110.7(6) ? C307 C306 H30M . . 109.5 ? C305 C306 H30M . . 109.5 ? C307 C306 H30N . . 109.5 ? C305 C306 H30N . . 109.5 ? H30M C306 H30N . . 108.1 ? C308 C309 C310 . . 110.9(7) ? C308 C309 H30O . . 109.5 ? C310 C309 H30O . . 109.5 ? C308 C309 H30P . . 109.5 ? C310 C309 H30P . . 109.5 ? H30O C309 H30P . . 108.0 ? C309 C308 C307 . . 114.3(6) ? C309 C308 H30Q . . 108.7 ? C307 C308 H30Q . . 108.7 ? C309 C308 H30R . . 108.7 ? C307 C308 H30R . . 108.7 ? H30Q C308 H30R . . 107.6 ? C306 C307 C308 . . 112.4(6) ? C306 C307 H30S . . 109.1 ? C308 C307 H30S . . 109.1 ? C306 C307 H30T . . 109.1 ? C308 C307 H30T . . 109.1 ? H30S C307 H30T . . 107.9 ? C57 C303 C302 . . 122.8(5) ? C57 C303 H303 . . 118.6 ? C302 C303 H303 . . 118.6 ? C309 C310 H31D . . 109.5 ? C309 C310 H31E . . 109.5 ? H31D C310 H31E . . 109.5 ? C309 C310 H31F . . 109.5 ? H31D C310 H31F . . 109.5 ? H31E C310 H31F . . 109.5 ? C103 C312 H31G . . 109.5 ? C103 C312 H31H . . 109.5 ? H31G C312 H31H . . 109.5 ? C103 C312 H31I . . 109.5 ? H31G C312 H31I . . 109.5 ? H31H C312 H31I . . 109.5 ? C103 C311 H31J . . 109.5 ? C103 C311 H31K . . 109.5 ? H31J C311 H31K . . 109.5 ? C103 C311 H31L . . 109.5 ? H31J C311 H31L . . 109.5 ? H31K C311 H31L . . 109.5 ? C2 C313 H900 . . 109.5 ? C2 C313 H901 . . 109.5 ? H900 C313 H901 . . 109.5 ? C2 C313 H902 . . 109.5 ? H900 C313 H902 . . 109.5 ? H901 C313 H902 . . 109.5 ? C317 C316 C315 . . 112.1(10) ? C317 C316 H31P . . 109.2 ? C315 C316 H31P . . 109.2 ? C317 C316 H31Q . . 109.2 ? C315 C316 H31Q . . 109.2 ? H31P C316 H31Q . . 107.9 ? C315 C314 H31R . . 109.5 ? C315 C314 H31S . . 109.5 ? H31R C314 H31S . . 109.5 ? C315 C314 H31T . . 109.5 ? H31R C314 H31T . . 109.5 ? H31S C314 H31T . . 109.5 ? C317 C318 C0AJ . . 111.5(8) ? C317 C318 H31U . . 109.3 ? C0AJ C318 H31U . . 109.3 ? C317 C318 H31V . . 109.3 ? C0AJ C318 H31V . . 109.3 ? H31U C318 H31V . . 108.0 ? C314 C315 C316 . . 110.9(9) ? C314 C315 H31W . . 109.5 ? C316 C315 H31W . . 109.4 ? C314 C315 H930 . . 109.4 ? C316 C315 H930 . . 109.4 ? H31W C315 H930 . . 108.0 ? C318 C317 C316 . . 114.6(9) ? C318 C317 H931 . . 108.6 ? C316 C317 H931 . . 108.6 ? C318 C317 H932 . . 108.6 ? C316 C317 H932 . . 108.6 ? H931 C317 H932 . . 107.6 ? C62 C321 C58 . . 119.5(5) ? C62 C321 P1 . . 122.0(6) ? C58 C321 P1 . . 118.4(4) ? C99 C319 H933 . . 109.5 ? C99 C319 H934 . . 109.5 ? H933 C319 H934 . . 109.5 ? C99 C319 H935 . . 109.5 ? H933 C319 H935 . . 109.5 ? H934 C319 H935 . . 109.5 ? C117 C322 H32A . . 109.5 ? C117 C322 H32B . . 109.5 ? H32A C322 H32B . . 109.5 ? C117 C322 H32C . . 109.5 ? H32A C322 H32C . . 109.5 ? H32B C322 H32C . . 109.5 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag N1 Sn1 C302 C301 . . . . 3.7(6) ? C32 Sn1 C302 C301 . . . . -101.9(6) ? N1 Sn1 C302 C303 . . . . -159.3(6) ? C32 Sn1 C302 C303 . . . . 95.1(6) ? N2 Sn3 C323 C68 . . . . 163.3(6) ? C90 Sn3 C323 C68 . . . . -89.0(6) ? N2 Sn3 C323 C64 . . . . -5.3(5) ? C90 Sn3 C323 C64 . . . . 102.5(5) ? C303 C302 C301 C55 . . . . -6.5(11) ? Sn1 C302 C301 C55 . . . . -170.8(5) ? C303 C302 C301 P1 . . . . 172.9(5) ? Sn1 C302 C301 P1 . . . . 8.6(8) ? N1 P1 C301 C55 . . . . 158.5(6) ? C321 P1 C301 C55 . . . . 30.9(7) ? C37 P1 C301 C55 . . . . -79.0(6) ? N1 P1 C301 C302 . . . . -20.9(6) ? C321 P1 C301 C302 . . . . -148.5(6) ? C37 P1 C301 C302 . . . . 101.6(6) ? N2 P2 C320 C73 . . . . -106.9(5) ? C74 P2 C320 C73 . . . . 21.9(5) ? C64 P2 C320 C73 . . . . 133.9(5) ? N2 P2 C320 C69 . . . . 76.8(5) ? C74 P2 C320 C69 . . . . -154.4(5) ? C64 P2 C320 C69 . . . . -42.3(5) ? C313 C2 C4 C12 . . . . 126.1(6) ? C3 C2 C4 C12 . . . . -109.6(6) ? C313 C2 C4 C5 . . . . -56.0(7) ? C3 C2 C4 C5 . . . . 68.3(7) ? C12 C4 C5 C6 . . . . -2.5(9) ? C2 C4 C5 C6 . . . . 179.6(6) ? C4 C5 C6 C10 . . . . 1.6(9) ? C4 C5 C6 C7 . . . . 175.8(6) ? C5 C6 C7 C9 . . . . 130.2(7) ? C10 C6 C7 C9 . . . . -55.8(8) ? C5 C6 C7 C8 . . . . -106.9(7) ? C10 C6 C7 C8 . . . . 67.1(7) ? C5 C6 C10 C11 . . . . 0.7(9) ? C7 C6 C10 C11 . . . . -173.5(5) ? C6 C10 C11 C12 . . . . -2.1(9) ? C6 C10 C11 C33 . . . . 175.3(5) ? C5 C4 C12 C11 . . . . 1.0(9) ? C2 C4 C12 C11 . . . . 178.9(5) ? C5 C4 C12 C13 . . . . -165.9(5) ? C2 C4 C12 C13 . . . . 11.9(8) ? C10 C11 C12 C4 . . . . 1.1(9) ? C33 C11 C12 C4 . . . . -176.2(5) ? C10 C11 C12 C13 . . . . 168.2(5) ? C33 C11 C12 C13 . . . . -9.1(8) ? C4 C12 C13 C32 . . . . -87.6(7) ? C11 C12 C13 C32 . . . . 105.2(7) ? C4 C12 C13 C14 . . . . 87.3(7) ? C11 C12 C13 C14 . . . . -79.8(6) ? C32 C13 C14 C15 . . . . -0.9(8) ? C12 C13 C14 C15 . . . . -176.1(5) ? C13 C14 C15 C16 . . . . 3.7(8) ? C14 C15 C16 C17 . . . . -2.3(9) ? C15 C16 C17 C32 . . . . -2.0(9) ? C15 C16 C17 C18 . . . . 170.1(5) ? C16 C17 C18 C19 . . . . 73.4(7) ? C32 C17 C18 C19 . . . . -115.2(7) ? C16 C17 C18 C23 . . . . -98.7(7) ? C32 C17 C18 C23 . . . . 72.8(7) ? C23 C18 C19 C20 . . . . -1.7(9) ? C17 C18 C19 C20 . . . . -173.8(5) ? C23 C18 C19 C29 . . . . 173.9(5) ? C17 C18 C19 C29 . . . . 1.8(9) ? C18 C19 C20 C21 . . . . -0.8(9) ? C29 C19 C20 C21 . . . . -176.6(6) ? C19 C20 C21 C22 . . . . 1.8(9) ? C19 C20 C21 C27 . . . . -177.0(5) ? C20 C21 C22 C23 . . . . -0.2(9) ? C27 C21 C22 C23 . . . . 178.5(5) ? C21 C22 C23 C18 . . . . -2.3(9) ? C21 C22 C23 C24 . . . . 172.6(5) ? C19 C18 C23 C22 . . . . 3.2(9) ? C17 C18 C23 C22 . . . . 175.6(5) ? C19 C18 C23 C24 . . . . -171.6(5) ? C17 C18 C23 C24 . . . . 0.7(8) ? C22 C23 C24 C25 . . . . 39.8(8) ? C18 C23 C24 C25 . . . . -145.4(6) ? C22 C23 C24 C26 . . . . -85.8(7) ? C18 C23 C24 C26 . . . . 89.1(6) ? C22 C21 C27 C304 . . . . -4.8(8) ? C20 C21 C27 C304 . . . . 174.0(5) ? C22 C21 C27 C28 . . . . 119.9(7) ? C20 C21 C27 C28 . . . . -61.4(7) ? C20 C19 C29 C30 . . . . 73.4(7) ? C18 C19 C29 C30 . . . . -102.2(7) ? C20 C19 C29 C31 . . . . -49.2(8) ? C18 C19 C29 C31 . . . . 135.1(6) ? C14 C13 C32 C17 . . . . -3.2(8) ? C12 C13 C32 C17 . . . . 171.3(5) ? C14 C13 C32 Sn1 . . . . -166.9(4) ? C12 C13 C32 Sn1 . . . . 7.7(7) ? C16 C17 C32 C13 . . . . 4.6(8) ? C18 C17 C32 C13 . . . . -166.2(5) ? C16 C17 C32 Sn1 . . . . 168.1(4) ? C18 C17 C32 Sn1 . . . . -2.7(7) ? C302 Sn1 C32 C13 . . . . -41.7(4) ? N1 Sn1 C32 C13 . . . . -125.4(4) ? C302 Sn1 C32 C17 . . . . 155.5(4) ? N1 Sn1 C32 C17 . . . . 71.8(4) ? C10 C11 C33 C35 . . . . 50.0(7) ? C12 C11 C33 C35 . . . . -132.7(6) ? C10 C11 C33 C34 . . . . -73.5(7) ? C12 C11 C33 C34 . . . . 103.7(6) ? N1 P1 C37 C42 . . . . 6.8(5) ? C301 P1 C37 C42 . . . . -111.6(4) ? C321 P1 C37 C42 . . . . 138.3(4) ? N1 P1 C37 C38 . . . . -176.4(4) ? C301 P1 C37 C38 . . . . 65.2(5) ? C321 P1 C37 C38 . . . . -44.9(5) ? C42 C37 C38 C39 . . . . -3.4(8) ? P1 C37 C38 C39 . . . . 179.9(4) ? C37 C38 C39 C40 . . . . 0.7(8) ? C38 C39 C40 C41 . . . . 1.4(8) ? C39 C40 C41 C42 . . . . -0.9(9) ? C38 C37 C42 C41 . . . . 3.9(8) ? P1 C37 C42 C41 . . . . -179.3(5) ? C40 C41 C42 C37 . . . . -1.8(9) ? C301 P1 N1 C44 . . . . -139.8(5) ? C321 P1 N1 C44 . . . . -21.8(6) ? C37 P1 N1 C44 . . . . 101.3(5) ? C301 P1 N1 Sn1 . . . . 22.9(4) ? C321 P1 N1 Sn1 . . . . 140.8(3) ? C37 P1 N1 Sn1 . . . . -96.0(3) ? C302 Sn1 N1 C44 . . . . 147.4(5) ? C32 Sn1 N1 C44 . . . . -111.9(4) ? C302 Sn1 N1 P1 . . . . -16.2(3) ? C32 Sn1 N1 P1 . . . . 84.6(3) ? P1 N1 C44 C49 . . . . -167.6(4) ? Sn1 N1 C44 C49 . . . . 30.8(6) ? P1 N1 C44 C53 . . . . -47.3(7) ? Sn1 N1 C44 C53 . . . . 151.1(4) ? P1 N1 C44 C45 . . . . 74.8(6) ? Sn1 N1 C44 C45 . . . . -86.8(5) ? N1 C44 C45 C46 . . . . 178.9(4) ? C49 C44 C45 C46 . . . . 59.9(5) ? C53 C44 C45 C46 . . . . -57.9(6) ? C44 C45 C46 C47 . . . . -62.7(7) ? C44 C45 C46 C52 . . . . 59.0(6) ? C52 C46 C47 C48 . . . . -60.5(6) ? C45 C46 C47 C48 . . . . 61.3(7) ? C46 C47 C48 C50 . . . . 59.8(6) ? C46 C47 C48 C49 . . . . -59.3(6) ? N1 C44 C49 C48 . . . . -179.3(5) ? C53 C44 C49 C48 . . . . 58.9(7) ? C45 C44 C49 C48 . . . . -59.1(6) ? C50 C48 C49 C44 . . . . -59.6(7) ? C47 C48 C49 C44 . . . . 59.9(7) ? C49 C48 C50 C51 . . . . 60.0(7) ? C47 C48 C50 C51 . . . . -59.5(6) ? C48 C50 C51 C52 . . . . 58.9(6) ? C48 C50 C51 C53 . . . . -60.7(7) ? C47 C46 C52 C51 . . . . 60.3(7) ? C45 C46 C52 C51 . . . . -61.2(6) ? C50 C51 C52 C46 . . . . -59.0(6) ? C53 C51 C52 C46 . . . . 61.2(6) ? N1 C44 C53 C51 . . . . -178.2(5) ? C49 C44 C53 C51 . . . . -57.8(7) ? C45 C44 C53 C51 . . . . 58.7(6) ? C50 C51 C53 C44 . . . . 59.7(7) ? C52 C51 C53 C44 . . . . -60.6(6) ? C302 C301 C55 C56 . . . . 5.8(11) ? P1 C301 C55 C56 . . . . -173.5(5) ? C301 C55 C56 C57 . . . . -0.8(10) ? C55 C56 C57 C303 . . . . -3.1(10) ? C321 C58 C59 C60 . . . . -0.3(9) ? C58 C59 C60 C61 . . . . -0.6(9) ? C59 C60 C61 C62 . . . . 0.4(9) ? C60 C61 C62 C321 . . . . 0.7(9) ? C74 P2 N2 C80 . . . . -100.5(5) ? C64 P2 N2 C80 . . . . 143.1(5) ? C320 P2 N2 C80 . . . . 24.9(6) ? C74 P2 N2 Sn3 . . . . 95.9(3) ? C64 P2 N2 Sn3 . . . . -20.5(4) ? C320 P2 N2 Sn3 . . . . -138.7(3) ? C323 Sn3 N2 C80 . . . . -148.7(5) ? C90 Sn3 N2 C80 . . . . 109.2(4) ? C323 Sn3 N2 P2 . . . . 15.5(3) ? C90 Sn3 N2 P2 . . . . -86.5(3) ? C68 C323 C64 C65 . . . . 0.0(10) ? Sn3 C323 C64 C65 . . . . 169.5(5) ? C68 C323 C64 P2 . . . . -174.6(5) ? Sn3 C323 C64 P2 . . . . -5.1(8) ? N2 P2 C64 C65 . . . . -157.8(5) ? C74 P2 C64 C65 . . . . 81.4(6) ? C320 P2 C64 C65 . . . . -30.1(7) ? N2 P2 C64 C323 . . . . 16.9(6) ? C74 P2 C64 C323 . . . . -103.9(5) ? C320 P2 C64 C323 . . . . 144.6(6) ? C323 C64 C65 C66 . . . . 1.4(10) ? P2 C64 C65 C66 . . . . 175.7(5) ? C64 C65 C66 C67 . . . . -2.5(10) ? C65 C66 C67 C68 . . . . 2.2(10) ? C64 C323 C68 C67 . . . . -0.3(10) ? Sn3 C323 C68 C67 . . . . -169.3(5) ? C66 C67 C68 C323 . . . . -0.7(10) ? C73 C320 C69 C70 . . . . -1.1(9) ? P2 C320 C69 C70 . . . . 175.4(5) ? C320 C69 C70 C71 . . . . 0.8(9) ? C69 C70 C71 C72 . . . . 0.2(9) ? C70 C71 C72 C73 . . . . -0.8(9) ? C69 C320 C73 C72 . . . . 0.5(8) ? P2 C320 C73 C72 . . . . -175.8(4) ? C71 C72 C73 C320 . . . . 0.4(9) ? N2 P2 C74 C75 . . . . -9.1(5) ? C64 P2 C74 C75 . . . . 107.4(4) ? C320 P2 C74 C75 . . . . -141.8(4) ? N2 P2 C74 C79 . . . . 173.4(4) ? C64 P2 C74 C79 . . . . -70.1(5) ? C320 P2 C74 C79 . . . . 40.7(5) ? C79 C74 C75 C76 . . . . 0.4(8) ? P2 C74 C75 C76 . . . . -177.2(4) ? C74 C75 C76 C77 . . . . -2.1(9) ? C75 C76 C77 C78 . . . . 2.0(8) ? C76 C77 C78 C79 . . . . -0.2(8) ? C77 C78 C79 C74 . . . . -1.6(8) ? C75 C74 C79 C78 . . . . 1.5(7) ? P2 C74 C79 C78 . . . . 179.0(4) ? P2 N2 C80 C89 . . . . 160.6(4) ? Sn3 N2 C80 C89 . . . . -36.7(7) ? P2 N2 C80 C81 . . . . 42.1(7) ? Sn3 N2 C80 C81 . . . . -155.2(4) ? P2 N2 C80 C87 . . . . -79.5(6) ? Sn3 N2 C80 C87 . . . . 83.2(5) ? N2 C80 C81 C82 . . . . -179.6(5) ? C89 C80 C81 C82 . . . . 59.5(7) ? C87 C80 C81 C82 . . . . -56.9(6) ? C80 C81 C82 C83 . . . . -61.4(7) ? C80 C81 C82 C88 . . . . 59.1(6) ? C88 C82 C83 C84 . . . . -59.5(6) ? C81 C82 C83 C84 . . . . 59.5(7) ? C82 C83 C84 C85 . . . . 61.5(6) ? C82 C83 C84 C89 . . . . -59.2(6) ? C83 C84 C85 C86 . . . . -62.7(6) ? C89 C84 C85 C86 . . . . 58.3(6) ? C84 C85 C86 C88 . . . . 60.4(6) ? C84 C85 C86 C87 . . . . -58.2(7) ? C88 C86 C87 C80 . . . . -59.7(6) ? C85 C86 C87 C80 . . . . 58.9(7) ? N2 C80 C87 C86 . . . . -179.7(4) ? C89 C80 C87 C86 . . . . -58.3(5) ? C81 C80 C87 C86 . . . . 57.0(6) ? C87 C86 C88 C82 . . . . 61.5(6) ? C85 C86 C88 C82 . . . . -57.6(6) ? C83 C82 C88 C86 . . . . 58.3(6) ? C81 C82 C88 C86 . . . . -61.1(6) ? N2 C80 C89 C84 . . . . 179.8(5) ? C81 C80 C89 C84 . . . . -58.5(7) ? C87 C80 C89 C84 . . . . 58.3(6) ? C83 C84 C89 C80 . . . . 60.5(7) ? C85 C84 C89 C80 . . . . -59.7(7) ? C323 Sn3 C90 C107 . . . . 42.3(4) ? N2 Sn3 C90 C107 . . . . 126.9(4) ? C323 Sn3 C90 C91 . . . . -157.0(4) ? N2 Sn3 C90 C91 . . . . -72.4(4) ? C107 C90 C91 C104 . . . . -2.6(8) ? Sn3 C90 C91 C104 . . . . -164.1(4) ? C107 C90 C91 C92 . . . . 169.8(5) ? Sn3 C90 C91 C92 . . . . 8.3(7) ? C104 C91 C92 C93 . . . . -71.1(7) ? C90 C91 C92 C93 . . . . 116.0(6) ? C104 C91 C92 C102 . . . . 97.0(7) ? C90 C91 C92 C102 . . . . -76.0(7) ? C102 C92 C93 C97 . . . . 1.3(8) ? C91 C92 C93 C97 . . . . 169.4(5) ? C102 C92 C93 C94 . . . . -179.0(5) ? C91 C92 C93 C94 . . . . -10.9(8) ? C97 C93 C94 C95 . . . . 47.1(7) ? C92 C93 C94 C95 . . . . -132.6(6) ? C97 C93 C94 C96 . . . . -74.7(6) ? C92 C93 C94 C96 . . . . 105.6(6) ? C92 C93 C97 C98 . . . . 0.4(9) ? C94 C93 C97 C98 . . . . -179.4(5) ? C93 C97 C98 C101 . . . . -1.7(9) ? C93 C97 C98 C99 . . . . -178.3(6) ? C101 C98 C99 C100 . . . . -75.2(9) ? C97 C98 C99 C100 . . . . 101.2(8) ? C101 C98 C99 C319 . . . . 158.8(7) ? C97 C98 C99 C319 . . . . -24.8(9) ? C97 C98 C101 C102 . . . . 1.4(10) ? C99 C98 C101 C102 . . . . 178.0(6) ? C98 C101 C102 C92 . . . . 0.2(9) ? C98 C101 C102 C103 . . . . -173.7(6) ? C93 C92 C102 C101 . . . . -1.6(8) ? C91 C92 C102 C101 . . . . -169.6(5) ? C93 C92 C102 C103 . . . . 172.3(5) ? C91 C92 C102 C103 . . . . 4.3(8) ? C101 C102 C103 C311 . . . . -41.6(8) ? C92 C102 C103 C311 . . . . 144.6(6) ? C101 C102 C103 C312 . . . . 83.5(7) ? C92 C102 C103 C312 . . . . -90.2(7) ? C90 C91 C104 C105 . . . . 0.2(9) ? C92 C91 C104 C105 . . . . -173.2(5) ? C91 C104 C105 C106 . . . . 2.1(9) ? C104 C105 C106 C107 . . . . -1.7(8) ? C105 C106 C107 C90 . . . . -0.9(8) ? C105 C106 C107 C108 . . . . 173.3(5) ? C91 C90 C107 C106 . . . . 3.0(8) ? Sn3 C90 C107 C106 . . . . 164.8(4) ? C91 C90 C107 C108 . . . . -170.3(5) ? Sn3 C90 C107 C108 . . . . -8.5(7) ? C106 C107 C108 C109 . . . . 87.3(6) ? C90 C107 C108 C109 . . . . -98.8(7) ? C106 C107 C108 C113 . . . . -82.2(6) ? C90 C107 C108 C113 . . . . 91.7(6) ? C113 C108 C109 C110 . . . . 1.3(8) ? C107 C108 C109 C110 . . . . -168.1(5) ? C113 C108 C109 C119 . . . . 176.9(5) ? C107 C108 C109 C119 . . . . 7.5(8) ? C108 C109 C110 C111 . . . . 0.5(8) ? C119 C109 C110 C111 . . . . -175.2(5) ? C109 C110 C111 C112 . . . . -2.0(8) ? C109 C110 C111 C117 . . . . 175.0(5) ? C110 C111 C112 C113 . . . . 1.9(9) ? C117 C111 C112 C113 . . . . -175.1(5) ? C111 C112 C113 C108 . . . . -0.2(8) ? C111 C112 C113 C114 . . . . 177.7(5) ? C109 C108 C113 C112 . . . . -1.4(8) ? C107 C108 C113 C112 . . . . 168.3(5) ? C109 C108 C113 C114 . . . . -179.3(5) ? C107 C108 C113 C114 . . . . -9.6(8) ? C112 C113 C114 C115 . . . . -64.7(7) ? C108 C113 C114 C115 . . . . 113.1(6) ? C112 C113 C114 C116 . . . . 59.4(6) ? C108 C113 C114 C116 . . . . -122.7(6) ? C112 C111 C117 C118 . . . . -127.6(6) ? C110 C111 C117 C118 . . . . 55.5(7) ? C112 C111 C117 C322 . . . . 110.2(6) ? C110 C111 C117 C322 . . . . -66.7(7) ? C110 C109 C119 C300 . . . . -45.8(7) ? C108 C109 C119 C300 . . . . 138.6(5) ? C110 C109 C119 C120 . . . . 76.9(6) ? C108 C109 C119 C120 . . . . -98.7(6) ? C310 C309 C308 C307 . . . . 179.8(7) ? C305 C306 C307 C308 . . . . 175.2(7) ? C309 C308 C307 C306 . . . . 175.4(7) ? C56 C57 C303 C302 . . . . 2.3(11) ? C301 C302 C303 C57 . . . . 2.4(11) ? Sn1 C302 C303 C57 . . . . 166.0(5) ? C317 C316 C315 C314 . . . . 177.5(9) ? C0AJ C318 C317 C316 . . . . -169.9(7) ? C315 C316 C317 C318 . . . . -179.9(8) ? C61 C62 C321 C58 . . . . -1.6(9) ? C61 C62 C321 P1 . . . . 175.5(4) ? C59 C58 C321 C62 . . . . 1.4(9) ? C59 C58 C321 P1 . . . . -175.8(4) ? N1 P1 C321 C62 . . . . 104.0(6) ? C301 P1 C321 C62 . . . . -136.6(5) ? C37 P1 C321 C62 . . . . -23.7(6) ? N1 P1 C321 C58 . . . . -78.9(5) ? C301 P1 C321 C58 . . . . 40.5(6) ? C37 P1 C321 C58 . . . . 153.4(5) ? #===END