# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name K.Jurkschat _publ_contact_author_email klaus.jurkschat@uni-dortmund.de _publ_author_name K.Jurkschat # Attachment '- compound1_revised2.cif' data_c2533 #TrackingRef 'C1DT10321K_ccdc_802872_802876_cif.txt' _database_code_depnum_ccdc_archive 'CCDC 802872' #TrackingRef '- compound1_revised2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C27 H39 Cl O11 P2 Sn W, 0.5(C7 H8)' _chemical_formula_sum 'C30.50 H43 Cl O11 P2 Sn W' _chemical_formula_weight 985.58 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sn Sn -0.6537 1.4246 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall -P1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.901(2) _cell_length_b 11.298(2) _cell_length_c 16.406(3) _cell_angle_alpha 85.89(3) _cell_angle_beta 84.23(3) _cell_angle_gamma 78.72(3) _cell_volume 1968.6(7) _cell_formula_units_Z 2 _cell_measurement_temperature 173(1) _cell_measurement_reflns_used 26002 _cell_measurement_theta_min 3.01 _cell_measurement_theta_max 27.50 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.663 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 970 _exptl_absorpt_coefficient_mu 3.753 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.427 _exptl_absorpt_correction_T_max 0.622 _exptl_absorpt_process_details ; SCALEPACK (Otwinowski & Minor, 1997) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method ; 424 frames via \w-rotation (\D\w = 1\%) and two times 10 s per frame (4 sets at different \k-angles) ; _diffrn_detector_area_resol_mean '19 vertical, 18 horizontal' _diffrn_standards_number none _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 26002 _diffrn_reflns_av_R_equivalents 0.054 _diffrn_reflns_av_sigmaI/netI 0.0863 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 3.01 _diffrn_reflns_theta_max 27.50 _reflns_number_total 9008 _reflns_number_gt 6339 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Nonius, 1998)' _computing_cell_refinement ; DENZO and SCALEPACK (Otwinowski & Minor, 1997) ; _computing_data_reduction ; DENZO and SCALEPACK ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL-Plus (Sheldrick, 1991)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 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^)+(0.0000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9008 _refine_ls_number_parameters 439 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0486 _refine_ls_R_factor_gt 0.0272 _refine_ls_wR_factor_ref 0.0475 _refine_ls_wR_factor_gt 0.0456 _refine_ls_goodness_of_fit_ref 0.834 _refine_ls_restrained_S_all 0.834 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group W1 W 0.219820(13) 0.915554(13) 0.329232(8) 0.02485(5) Uani 1 1 d . . . Sn1 Sn 0.40869(2) 0.76859(2) 0.242512(13) 0.02123(6) Uani 1 1 d . . . Cl1 Cl 0.39698(9) 0.73546(8) 0.10082(5) 0.0363(2) Uani 1 1 d . . . P1 P 0.47353(8) 0.47889(8) 0.29470(5) 0.0220(2) Uani 1 1 d . . . P2 P 0.67432(8) 0.86600(8) 0.19649(5) 0.0242(2) Uani 1 1 d . . . O2 O 0.53619(19) 0.91115(19) 0.20216(13) 0.0272(5) Uani 1 1 d . . . O2' O 0.7461(2) 0.9449(2) 0.24216(12) 0.0282(6) Uani 1 1 d . . . O1'' O 0.46752(19) 0.4203(2) 0.38374(12) 0.0256(5) Uani 1 1 d . . . O1 O 0.36524(19) 0.5781(2) 0.27747(12) 0.0255(5) Uani 1 1 d . . . O1' O 0.4878(2) 0.36842(19) 0.23993(12) 0.0261(5) Uani 1 1 d . . . O2'' O 0.7422(2) 0.8629(2) 0.10850(12) 0.0270(5) Uani 1 1 d . . . C1 C 0.5964(3) 0.6620(3) 0.25447(17) 0.0186(7) Uani 1 1 d . . . C2 C 0.6131(3) 0.5402(3) 0.27962(18) 0.0208(8) Uani 1 1 d . . . C3 C 0.7333(3) 0.4717(3) 0.28661(18) 0.0240(8) Uani 1 1 d . . . H3A H 0.7423 0.3904 0.3035 0.029 Uiso 1 1 calc R . . C4 C 0.8407(3) 0.5228(3) 0.26878(19) 0.0240(8) Uani 1 1 d . . . C5 C 0.8229(3) 0.6436(3) 0.24310(18) 0.0244(8) Uani 1 1 d . . . H5A H 0.8925 0.6798 0.2304 0.029 Uiso 1 1 calc R . . C6 C 0.7040(3) 0.7124(3) 0.23570(18) 0.0210(8) Uani 1 1 d . . . C7 C 0.9701(3) 0.4445(3) 0.2789(2) 0.0318(9) Uani 1 1 d . . . C8 C 0.9794(3) 0.4034(4) 0.3694(2) 0.0566(12) Uani 1 1 d . . . H8A H 0.9706 0.4729 0.4015 0.085 Uiso 1 1 calc R . . H8B H 1.0597 0.3523 0.3759 0.085 Uiso 1 1 calc R . . H8C H 0.9139 0.3593 0.3876 0.085 Uiso 1 1 calc R . . C9 C 0.9881(4) 0.3338(4) 0.2266(3) 0.0560(12) Uani 1 1 d . . . H9A H 0.9802 0.3603 0.1701 0.084 Uiso 1 1 calc R . . H9B H 0.9254 0.2865 0.2449 0.084 Uiso 1 1 calc R . . H9C H 1.0701 0.2855 0.2320 0.084 Uiso 1 1 calc R . . C10 C 1.0761(3) 0.5129(4) 0.2514(2) 0.0457(11) Uani 1 1 d . . . H10A H 1.0684 0.5811 0.2846 0.069 Uiso 1 1 calc R . . H10B H 1.0709 0.5405 0.1949 0.069 Uiso 1 1 calc R . . H10C H 1.1555 0.4602 0.2575 0.069 Uiso 1 1 calc R . . O11 O 0.3047(2) 1.1386(2) 0.22433(15) 0.0463(7) Uani 1 1 d . . . C11 C 0.2740(3) 1.0577(3) 0.2617(2) 0.0316(9) Uani 1 1 d . . . O12 O 0.0452(3) 0.8819(3) 0.19157(18) 0.0708(10) Uani 1 1 d . . . C12 C 0.1064(3) 0.8966(4) 0.2408(2) 0.0416(10) Uani 1 1 d . . . O13 O 0.4215(3) 0.9247(3) 0.45389(16) 0.0570(8) Uani 1 1 d . . . C13 C 0.3467(3) 0.9211(3) 0.4101(2) 0.0346(9) Uani 1 1 d . . . O14 O 0.1392(3) 0.6897(3) 0.43285(18) 0.0680(9) Uani 1 1 d . . . C14 C 0.1684(4) 0.7705(4) 0.3954(2) 0.0407(10) Uani 1 1 d . . . O15 O 0.0143(3) 1.0970(2) 0.42891(16) 0.0531(8) Uani 1 1 d . . . C15 C 0.0890(4) 1.0300(3) 0.3923(2) 0.0349(9) Uani 1 1 d . . . C21 C 0.5102(3) 0.3833(3) 0.14957(19) 0.0317(9) Uani 1 1 d . . . H21A H 0.5468 0.4554 0.1349 0.038 Uiso 1 1 calc R . . C22 C 0.3891(4) 0.3959(4) 0.1115(2) 0.0471(11) Uani 1 1 d . . . H22A H 0.3312 0.4649 0.1320 0.071 Uiso 1 1 calc R . . H22B H 0.3543 0.3244 0.1250 0.071 Uiso 1 1 calc R . . H22C H 0.4040 0.4064 0.0530 0.071 Uiso 1 1 calc R . . C23 C 0.6032(4) 0.2729(4) 0.1249(2) 0.0739(16) Uani 1 1 d . . . H23A H 0.6794 0.2699 0.1503 0.111 Uiso 1 1 calc R . . H23B H 0.6208 0.2760 0.0664 0.111 Uiso 1 1 calc R . . H23C H 0.5691 0.2022 0.1423 0.111 Uiso 1 1 calc R . . C24 C 0.3501(3) 0.3889(3) 0.42543(19) 0.0304(9) Uani 1 1 d . . . H24A H 0.2777 0.4421 0.4031 0.037 Uiso 1 1 calc R . . C25 C 0.3469(4) 0.2608(4) 0.4106(2) 0.0505(12) Uani 1 1 d . . . H25A H 0.3495 0.2516 0.3527 0.076 Uiso 1 1 calc R . . H25B H 0.2711 0.2398 0.4374 0.076 Uiso 1 1 calc R . . H25C H 0.4182 0.2086 0.4321 0.076 Uiso 1 1 calc R . . C26 C 0.3515(4) 0.4117(4) 0.5144(2) 0.0561(13) Uani 1 1 d . . . H26A H 0.3556 0.4949 0.5197 0.084 Uiso 1 1 calc R . . H26B H 0.4234 0.3608 0.5360 0.084 Uiso 1 1 calc R . . H26C H 0.2764 0.3940 0.5444 0.084 Uiso 1 1 calc R . . C31 C 0.7046(3) 0.9800(4) 0.3274(2) 0.0384(10) Uani 1 1 d . . . H31A H 0.6171 0.9712 0.3412 0.046 Uiso 1 1 calc R . . C32 C 0.7882(4) 0.8988(4) 0.3844(2) 0.0586(13) Uani 1 1 d . . . H32A H 0.7733 0.8178 0.3844 0.088 Uiso 1 1 calc R . . H32B H 0.7701 0.9270 0.4389 0.088 Uiso 1 1 calc R . . H32C H 0.8745 0.8998 0.3661 0.088 Uiso 1 1 calc R . . C33 C 0.7152(5) 1.1088(4) 0.3303(3) 0.0720(15) Uani 1 1 d . . . H33A H 0.6605 1.1576 0.2934 0.108 Uiso 1 1 calc R . . H33B H 0.8003 1.1174 0.3143 0.108 Uiso 1 1 calc R . . H33C H 0.6916 1.1347 0.3851 0.108 Uiso 1 1 calc R . . C34 C 0.7130(3) 0.9629(3) 0.04585(19) 0.0312(9) Uani 1 1 d . . . H34A H 0.6452 1.0250 0.0689 0.037 Uiso 1 1 calc R . . C35 C 0.8291(4) 1.0155(4) 0.0258(3) 0.0590(13) Uani 1 1 d . . . H35A H 0.8529 1.0435 0.0747 0.089 Uiso 1 1 calc R . . H35B H 0.8129 1.0821 -0.0139 0.089 Uiso 1 1 calc R . . H35C H 0.8961 0.9548 0.0037 0.089 Uiso 1 1 calc R . . C36 C 0.6681(4) 0.9102(4) -0.0249(2) 0.0587(13) Uani 1 1 d . . . H36A H 0.6383 0.9740 -0.0640 0.088 Uiso 1 1 calc R . . H36B H 0.6011 0.8688 -0.0050 0.088 Uiso 1 1 calc R . . H36C H 0.7362 0.8543 -0.0506 0.088 Uiso 1 1 calc R . . C41 C -0.0292(12) 0.4392(8) -0.0088(5) 0.076(4) Uani 0.50 1 d PGD . . C42 C -0.0917(8) 0.5494(10) 0.0205(5) 0.074(6) Uani 0.50 1 d PGD . . H42 H -0.1775 0.5615 0.0357 0.089 Uiso 0.50 1 calc PR . . C43 C -0.0258(10) 0.6414(8) 0.0271(5) 0.096(6) Uani 0.50 1 d PGD . . H43 H -0.0676 0.7151 0.0467 0.115 Uiso 0.50 1 calc PR . . C44 C 0.1025(10) 0.6233(10) 0.0043(5) 0.111(9) Uani 0.50 1 d PGD . . H44 H 0.1466 0.6849 0.0087 0.133 Uiso 0.50 1 calc PR . . C45 C 0.1650(8) 0.5131(12) -0.0250(5) 0.085(4) Uani 0.50 1 d PGD . . H45 H 0.2508 0.5010 -0.0402 0.102 Uiso 0.50 1 calc PR . . C46 C 0.0991(12) 0.4211(9) -0.0316(4) 0.089(8) Uani 0.50 1 d PGD . . H46 H 0.1409 0.3474 -0.0512 0.106 Uiso 0.50 1 calc PR . . C47 C -0.1022(19) 0.3373(12) -0.0161(7) 0.219(18) Uani 0.50 1 d PD . . H47A H -0.0833 0.3066 -0.0699 0.329 Uiso 0.50 1 calc PR . . H47B H -0.1907 0.3683 -0.0071 0.329 Uiso 0.50 1 calc PR . . H47C H -0.0780 0.2733 0.0243 0.329 Uiso 0.50 1 calc PR . . 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 W1 0.02302(9) 0.02492(9) 0.02502(8) -0.00316(6) 0.00004(6) -0.00110(6) Sn1 0.01959(13) 0.02199(15) 0.02142(13) -0.00181(10) -0.00237(10) -0.00172(11) Cl1 0.0483(6) 0.0383(6) 0.0231(5) -0.0016(4) -0.0094(4) -0.0067(5) P1 0.0244(5) 0.0225(5) 0.0198(5) -0.0014(4) -0.0017(4) -0.0060(4) P2 0.0237(5) 0.0225(6) 0.0262(5) 0.0007(4) -0.0008(4) -0.0056(4) O2 0.0241(14) 0.0204(14) 0.0358(14) 0.0024(11) -0.0019(10) -0.0026(10) O2' 0.0288(14) 0.0304(15) 0.0271(13) -0.0031(11) 0.0020(10) -0.0114(11) O1'' 0.0286(14) 0.0302(15) 0.0196(12) 0.0015(10) -0.0018(10) -0.0109(11) O1 0.0202(13) 0.0265(15) 0.0309(13) -0.0027(11) -0.0019(10) -0.0068(11) O1' 0.0349(14) 0.0245(14) 0.0192(12) -0.0019(10) -0.0016(10) -0.0066(11) O2'' 0.0307(14) 0.0249(15) 0.0227(12) 0.0019(10) 0.0010(10) -0.0013(11) C1 0.0170(18) 0.024(2) 0.0144(17) -0.0027(14) -0.0035(13) -0.0003(15) C2 0.0220(19) 0.024(2) 0.0168(17) -0.0044(15) -0.0016(14) -0.0036(16) C3 0.029(2) 0.021(2) 0.0203(18) -0.0015(15) -0.0040(15) 0.0001(16) C4 0.020(2) 0.027(2) 0.0235(19) -0.0020(16) -0.0037(14) -0.0009(16) C5 0.021(2) 0.030(2) 0.0232(19) -0.0007(16) -0.0036(14) -0.0070(16) C6 0.024(2) 0.021(2) 0.0180(17) -0.0030(14) -0.0025(14) -0.0037(16) C7 0.023(2) 0.037(2) 0.033(2) 0.0027(18) -0.0041(16) -0.0007(17) C8 0.031(2) 0.080(4) 0.051(3) 0.027(2) -0.015(2) 0.003(2) C9 0.034(3) 0.041(3) 0.087(3) -0.015(2) -0.006(2) 0.011(2) C10 0.023(2) 0.053(3) 0.056(3) 0.014(2) -0.0064(18) 0.001(2) O11 0.061(2) 0.0333(18) 0.0415(16) 0.0047(13) 0.0015(14) -0.0083(15) C11 0.027(2) 0.031(2) 0.034(2) -0.0068(18) 0.0019(16) 0.0006(18) O12 0.0373(18) 0.125(3) 0.054(2) -0.024(2) -0.0159(15) -0.0122(18) C12 0.028(2) 0.059(3) 0.037(2) -0.014(2) 0.0019(18) -0.002(2) O13 0.055(2) 0.076(2) 0.0433(18) -0.0108(16) -0.0204(15) -0.0101(17) C13 0.034(2) 0.036(3) 0.033(2) -0.0083(18) -0.0027(18) -0.0032(18) O14 0.093(3) 0.041(2) 0.066(2) 0.0022(16) 0.0293(18) -0.0220(18) C14 0.042(3) 0.034(3) 0.043(2) -0.007(2) 0.0135(19) -0.005(2) O15 0.0518(19) 0.043(2) 0.0541(18) -0.0086(15) 0.0162(15) 0.0077(15) C15 0.037(2) 0.036(3) 0.030(2) 0.0049(18) -0.0003(18) -0.0044(19) C21 0.039(2) 0.036(2) 0.0190(19) -0.0033(16) 0.0007(16) -0.0070(18) C22 0.058(3) 0.058(3) 0.030(2) -0.002(2) -0.0113(19) -0.017(2) C23 0.091(4) 0.086(4) 0.027(2) -0.018(2) -0.006(2) 0.032(3) C24 0.027(2) 0.037(2) 0.029(2) 0.0044(17) 0.0000(15) -0.0128(17) C25 0.070(3) 0.051(3) 0.040(2) 0.000(2) -0.005(2) -0.037(2) C26 0.073(3) 0.067(3) 0.035(2) -0.012(2) 0.018(2) -0.038(3) C31 0.041(2) 0.049(3) 0.028(2) -0.0115(19) 0.0039(17) -0.014(2) C32 0.099(4) 0.041(3) 0.036(3) 0.003(2) -0.013(2) -0.012(3) C33 0.127(5) 0.038(3) 0.048(3) -0.007(2) -0.023(3) 0.002(3) C34 0.036(2) 0.029(2) 0.027(2) 0.0034(17) -0.0026(16) -0.0039(18) C35 0.053(3) 0.053(3) 0.068(3) 0.027(2) 0.001(2) -0.018(2) C36 0.096(4) 0.047(3) 0.035(2) 0.004(2) -0.022(2) -0.012(3) C41 0.104(11) 0.102(13) 0.031(6) 0.031(7) -0.034(7) -0.038(10) C42 0.031(9) 0.122(14) 0.046(8) 0.023(9) 0.003(6) 0.029(10) C43 0.123(14) 0.099(13) 0.035(7) 0.001(8) 0.003(8) 0.048(10) C44 0.20(2) 0.108(14) 0.070(11) 0.054(9) -0.092(14) -0.120(19) C45 0.046(7) 0.134(14) 0.063(8) 0.039(9) -0.015(6) -0.001(8) C46 0.17(2) 0.044(9) 0.041(9) 0.008(7) -0.022(11) 0.004(10) C47 0.37(4) 0.26(3) 0.111(16) 0.076(16) -0.11(2) -0.25(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_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag W1 C15 1.988(4) . ? W1 C13 2.024(4) . ? W1 C11 2.034(4) . ? W1 C14 2.040(4) . ? W1 C12 2.046(4) . ? W1 Sn1 2.7263(11) . ? Sn1 C1 2.181(3) . ? Sn1 O1 2.313(2) . ? Sn1 O2 2.346(2) . ? Sn1 Cl1 2.4007(10) . ? P1 O1 1.495(2) . ? P1 O1'' 1.561(2) . ? P1 O1' 1.564(2) . ? P1 C2 1.780(3) . ? P2 O2 1.488(2) . ? P2 O2'' 1.554(2) . ? P2 O2' 1.567(2) . ? P2 C6 1.786(3) . ? O2' C31 1.484(4) . ? O1'' C24 1.483(4) . ? O1' C21 1.481(4) . ? O2'' C34 1.481(4) . ? C1 C2 1.390(4) . ? C1 C6 1.400(4) . ? C2 C3 1.396(4) . ? C3 C4 1.400(4) . ? C4 C5 1.381(4) . ? C4 C7 1.529(5) . ? C5 C6 1.386(4) . ? C7 C10 1.527(5) . ? C7 C8 1.531(5) . ? C7 C9 1.537(5) . ? O11 C11 1.149(4) . ? O12 C12 1.139(4) . ? O13 C13 1.147(4) . ? O14 C14 1.142(4) . ? O15 C15 1.150(4) . ? C21 C22 1.495(5) . ? C21 C23 1.497(5) . ? C24 C25 1.492(5) . ? C24 C26 1.502(4) . ? C31 C33 1.487(5) . ? C31 C32 1.506(5) . ? C34 C35 1.500(5) . ? C34 C36 1.506(4) . ? C41 C42 1.3900 . ? C41 C46 1.3900 . ? C41 C47 1.5395(11) . ? C42 C43 1.3900 . ? C43 C44 1.3900 . ? C44 C45 1.3900 . ? C45 C46 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 C15 W1 C13 91.47(14) . . ? C15 W1 C11 89.64(14) . . ? C13 W1 C11 90.54(15) . . ? C15 W1 C14 91.63(15) . . ? C13 W1 C14 89.49(15) . . ? C11 W1 C14 178.73(14) . . ? C15 W1 C12 94.77(14) . . ? C13 W1 C12 173.75(14) . . ? C11 W1 C12 89.71(15) . . ? C14 W1 C12 90.13(16) . . ? C15 W1 Sn1 176.49(10) . . ? C13 W1 Sn1 86.43(10) . . ? C11 W1 Sn1 87.57(10) . . ? C14 W1 Sn1 91.16(10) . . ? C12 W1 Sn1 87.35(10) . . ? C1 Sn1 O1 78.39(10) . . ? C1 Sn1 O2 78.03(10) . . ? O1 Sn1 O2 156.03(7) . . ? C1 Sn1 Cl1 97.37(8) . . ? O1 Sn1 Cl1 89.30(6) . . ? O2 Sn1 Cl1 89.49(6) . . ? C1 Sn1 W1 141.15(7) . . ? O1 Sn1 W1 102.89(6) . . ? O2 Sn1 W1 98.13(6) . . ? Cl1 Sn1 W1 121.38(3) . . ? O1 P1 O1'' 114.84(12) . . ? O1 P1 O1' 114.00(12) . . ? O1'' P1 O1' 103.26(12) . . ? O1 P1 C2 108.06(15) . . ? O1'' P1 C2 107.08(13) . . ? O1' P1 C2 109.28(13) . . ? O2 P2 O2'' 115.91(13) . . ? O2 P2 O2' 113.01(13) . . ? O2'' P2 O2' 103.34(12) . . ? O2 P2 C6 108.69(14) . . ? O2'' P2 C6 104.65(14) . . ? O2' P2 C6 110.89(14) . . ? P2 O2 Sn1 116.71(12) . . ? C31 O2' P2 121.51(19) . . ? C24 O1'' P1 122.0(2) . . ? P1 O1 Sn1 117.32(11) . . ? C21 O1' P1 120.7(2) . . ? C34 O2'' P2 122.3(2) . . ? C2 C1 C6 117.6(3) . . ? C2 C1 Sn1 120.8(2) . . ? C6 C1 Sn1 121.6(2) . . ? C1 C2 C3 120.7(3) . . ? C1 C2 P1 115.3(2) . . ? C3 C2 P1 123.8(3) . . ? C2 C3 C4 121.5(3) . . ? C5 C4 C3 117.2(3) . . ? C5 C4 C7 123.4(3) . . ? C3 C4 C7 119.4(3) . . ? C4 C5 C6 121.9(3) . . ? C5 C6 C1 121.1(3) . . ? C5 C6 P2 124.3(2) . . ? C1 C6 P2 114.6(2) . . ? C10 C7 C4 112.0(3) . . ? C10 C7 C8 108.3(3) . . ? C4 C7 C8 109.2(3) . . ? C10 C7 C9 107.9(3) . . ? C4 C7 C9 109.5(3) . . ? C8 C7 C9 109.9(3) . . ? O11 C11 W1 179.3(3) . . ? O12 C12 W1 177.6(4) . . ? O13 C13 W1 177.8(3) . . ? O14 C14 W1 179.6(4) . . ? O15 C15 W1 179.3(3) . . ? O1' C21 C22 109.8(3) . . ? O1' C21 C23 105.1(3) . . ? C22 C21 C23 112.9(3) . . ? O1'' C24 C25 109.0(3) . . ? O1'' C24 C26 105.9(3) . . ? C25 C24 C26 113.6(3) . . ? O2' C31 C33 106.6(3) . . ? O2' C31 C32 108.3(3) . . ? C33 C31 C32 112.0(3) . . ? O2'' C34 C35 107.2(3) . . ? O2'' C34 C36 106.8(3) . . ? C35 C34 C36 115.2(3) . . ? C42 C41 C46 120.0 . . ? C42 C41 C47 120.0 . . ? C46 C41 C47 120.0 . . ? C43 C42 C41 120.0 . . ? C42 C43 C44 120.0 . . ? C45 C44 C43 120.0 . . ? C46 C45 C44 120.0 . . ? C45 C46 C41 120.0 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C15 W1 Sn1 C1 66.9(17) . . . . ? C13 W1 Sn1 C1 13.56(17) . . . . ? C11 W1 Sn1 C1 104.25(17) . . . . ? C14 W1 Sn1 C1 -75.85(17) . . . . ? C12 W1 Sn1 C1 -165.93(18) . . . . ? C15 W1 Sn1 O1 154.3(17) . . . . ? C13 W1 Sn1 O1 100.99(12) . . . . ? C11 W1 Sn1 O1 -168.32(11) . . . . ? C14 W1 Sn1 O1 11.57(12) . . . . ? C12 W1 Sn1 O1 -78.51(13) . . . . ? C15 W1 Sn1 O2 -14.1(17) . . . . ? C13 W1 Sn1 O2 -67.43(12) . . . . ? C11 W1 Sn1 O2 23.26(11) . . . . ? C14 W1 Sn1 O2 -156.85(12) . . . . ? C12 W1 Sn1 O2 113.07(13) . . . . ? C15 W1 Sn1 Cl1 -108.5(17) . . . . ? C13 W1 Sn1 Cl1 -161.84(11) . . . . ? C11 W1 Sn1 Cl1 -71.15(10) . . . . ? C14 W1 Sn1 Cl1 108.75(12) . . . . ? C12 W1 Sn1 Cl1 18.67(12) . . . . ? O2'' P2 O2 Sn1 110.37(14) . . . . ? O2' P2 O2 Sn1 -130.63(13) . . . . ? C6 P2 O2 Sn1 -7.09(16) . . . . ? C1 Sn1 O2 P2 4.76(13) . . . . ? O1 Sn1 O2 P2 -5.7(3) . . . . ? Cl1 Sn1 O2 P2 -92.88(12) . . . . ? W1 Sn1 O2 P2 145.47(11) . . . . ? O2 P2 O2' C31 48.8(3) . . . . ? O2'' P2 O2' C31 174.8(2) . . . . ? C6 P2 O2' C31 -73.5(3) . . . . ? O1 P1 O1'' C24 43.7(3) . . . . ? O1' P1 O1'' C24 -81.0(2) . . . . ? C2 P1 O1'' C24 163.7(2) . . . . ? O1'' P1 O1 Sn1 117.86(13) . . . . ? O1' P1 O1 Sn1 -123.26(12) . . . . ? C2 P1 O1 Sn1 -1.57(16) . . . . ? C1 Sn1 O1 P1 2.58(13) . . . . ? O2 Sn1 O1 P1 13.1(3) . . . . ? Cl1 Sn1 O1 P1 100.25(12) . . . . ? W1 Sn1 O1 P1 -137.65(11) . . . . ? O1 P1 O1' C21 61.1(2) . . . . ? O1'' P1 O1' C21 -173.6(2) . . . . ? C2 P1 O1' C21 -59.9(3) . . . . ? O2 P2 O2'' C34 42.6(3) . . . . ? O2' P2 O2'' C34 -81.5(2) . . . . ? C6 P2 O2'' C34 162.3(2) . . . . ? O1 Sn1 C1 C2 -3.4(2) . . . . ? O2 Sn1 C1 C2 -179.1(2) . . . . ? Cl1 Sn1 C1 C2 -91.1(2) . . . . ? W1 Sn1 C1 C2 92.8(2) . . . . ? O1 Sn1 C1 C6 175.3(2) . . . . ? O2 Sn1 C1 C6 -0.4(2) . . . . ? Cl1 Sn1 C1 C6 87.6(2) . . . . ? W1 Sn1 C1 C6 -88.5(2) . . . . ? C6 C1 C2 C3 0.7(4) . . . . ? Sn1 C1 C2 C3 179.5(2) . . . . ? C6 C1 C2 P1 -175.3(2) . . . . ? Sn1 C1 C2 P1 3.5(3) . . . . ? O1 P1 C2 C1 -1.1(3) . . . . ? O1'' P1 C2 C1 -125.3(2) . . . . ? O1' P1 C2 C1 123.5(2) . . . . ? O1 P1 C2 C3 -176.9(2) . . . . ? O1'' P1 C2 C3 58.9(3) . . . . ? O1' P1 C2 C3 -52.4(3) . . . . ? C1 C2 C3 C4 0.1(4) . . . . ? P1 C2 C3 C4 175.7(2) . . . . ? C2 C3 C4 C5 -0.7(4) . . . . ? C2 C3 C4 C7 178.9(3) . . . . ? C3 C4 C5 C6 0.5(4) . . . . ? C7 C4 C5 C6 -179.1(3) . . . . ? C4 C5 C6 C1 0.3(5) . . . . ? C4 C5 C6 P2 -175.7(2) . . . . ? C2 C1 C6 C5 -0.9(4) . . . . ? Sn1 C1 C6 C5 -179.6(2) . . . . ? C2 C1 C6 P2 175.4(2) . . . . ? Sn1 C1 C6 P2 -3.3(3) . . . . ? O2 P2 C6 C5 -177.0(2) . . . . ? O2'' P2 C6 C5 58.6(3) . . . . ? O2' P2 C6 C5 -52.2(3) . . . . ? O2 P2 C6 C1 6.8(3) . . . . ? O2'' P2 C6 C1 -117.6(2) . . . . ? O2' P2 C6 C1 131.6(2) . . . . ? C5 C4 C7 C10 -4.2(4) . . . . ? C3 C4 C7 C10 176.3(3) . . . . ? C5 C4 C7 C8 115.8(4) . . . . ? C3 C4 C7 C8 -63.8(4) . . . . ? C5 C4 C7 C9 -123.8(3) . . . . ? C3 C4 C7 C9 56.6(4) . . . . ? C15 W1 C11 O11 49(26) . . . . ? C13 W1 C11 O11 -42(26) . . . . ? C14 W1 C11 O11 -133(24) . . . . ? C12 W1 C11 O11 144(26) . . . . ? Sn1 W1 C11 O11 -128(26) . . . . ? C15 W1 C12 O12 -143(8) . . . . ? C13 W1 C12 O12 35(9) . . . . ? C11 W1 C12 O12 128(8) . . . . ? C14 W1 C12 O12 -51(8) . . . . ? Sn1 W1 C12 O12 40(8) . . . . ? C15 W1 C13 O13 -134(9) . . . . ? C11 W1 C13 O13 -44(9) . . . . ? C14 W1 C13 O13 134(9) . . . . ? C12 W1 C13 O13 48(9) . . . . ? Sn1 W1 C13 O13 43(9) . . . . ? C15 W1 C14 O14 -24(64) . . . . ? C13 W1 C14 O14 68(64) . . . . ? C11 W1 C14 O14 159(100) . . . . ? C12 W1 C14 O14 -119(64) . . . . ? Sn1 W1 C14 O14 154(100) . . . . ? C13 W1 C15 O15 46(27) . . . . ? C11 W1 C15 O15 -45(27) . . . . ? C14 W1 C15 O15 135(27) . . . . ? C12 W1 C15 O15 -135(27) . . . . ? Sn1 W1 C15 O15 -8(29) . . . . ? P1 O1' C21 C22 -97.9(3) . . . . ? P1 O1' C21 C23 140.4(3) . . . . ? P1 O1'' C24 C25 92.5(3) . . . . ? P1 O1'' C24 C26 -144.9(3) . . . . ? P2 O2' C31 C33 -137.9(3) . . . . ? P2 O2' C31 C32 101.4(3) . . . . ? P2 O2'' C34 C35 116.2(3) . . . . ? P2 O2'' C34 C36 -119.7(3) . . . . ? C46 C41 C42 C43 0.0 . . . . ? C47 C41 C42 C43 180.0 . . . . ? C41 C42 C43 C44 0.0 . . . . ? C42 C43 C44 C45 0.0 . . . . ? C43 C44 C45 C46 0.0 . . . . ? C44 C45 C46 C41 0.0 . . . . ? C42 C41 C46 C45 0.0 . . . . ? C47 C41 C46 C45 180.0 . . . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.049 _refine_diff_density_min -0.956 _refine_diff_density_rms 0.103 # Attachment '- compound3_revised2.cif' data_o0018 #TrackingRef 'C1DT10321K_ccdc_802872_802876_cif.txt' _database_code_depnum_ccdc_archive 'CCDC 802873' #TrackingRef '- compound3_revised2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C39 H49 O11 P3 Sn W, C7 H8' _chemical_formula_sum 'C46 H57 O11 P3 Sn W' _chemical_formula_weight 1181.37 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/n _symmetry_space_group_name_Hall -P2yn 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 11.3682(3) _cell_length_b 23.9843(6) _cell_length_c 18.4609(5) _cell_angle_alpha 90.00 _cell_angle_beta 95.285(2) _cell_angle_gamma 90.00 _cell_volume 5012.1(2) _cell_formula_units_Z 4 _cell_measurement_temperature 173(1) _cell_measurement_reflns_used 14834 _cell_measurement_theta_min 1.9918 _cell_measurement_theta_max 28.1708 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.566 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2360 _exptl_absorpt_coefficient_mu 2.942 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.782 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.37 (release 24-10-2008 CrysAlis171 .NET) (compiled Oct 24 2008,09:44:38) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(1) _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 'Xcalibur2 CCD diffractometer' _diffrn_measurement_method ; 486 frames via \w-rotation (\D\w = 1\%) and two times 30 s per frame (8 sets at different \k-angles) ; _diffrn_detector_area_resol_mean 16.0560 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 26261 _diffrn_reflns_av_R_equivalents 0.0355 _diffrn_reflns_av_sigmaI/netI 0.0510 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.99 _diffrn_reflns_theta_max 25.00 _reflns_number_total 8755 _reflns_number_gt 6718 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlis CCD (Oxford Diffraction, 2008) ; _computing_cell_refinement ; CrysAlis RED (Oxford Diffraction, 2008) ; _computing_data_reduction ; CrysAlis RED (Oxford Diffraction, 2008) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL-Plus (Sheldrick, 1991)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 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^)+(0.0175P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8755 _refine_ls_number_parameters 571 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0333 _refine_ls_R_factor_gt 0.0215 _refine_ls_wR_factor_ref 0.0422 _refine_ls_wR_factor_gt 0.0414 _refine_ls_goodness_of_fit_ref 0.905 _refine_ls_restrained_S_all 0.905 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group W1 W 0.143470(11) 0.173373(6) 0.064012(7) 0.01722(4) Uani 1 1 d . . . Sn1 Sn 0.148454(18) 0.284044(9) 0.106257(11) 0.01560(6) Uani 1 1 d . . . P1 P 0.31645(7) 0.29057(4) 0.26300(4) 0.01716(19) Uani 1 1 d . . . P2 P -0.11363(7) 0.33627(3) 0.13199(4) 0.01565(19) Uani 1 1 d . . . P3 P 0.18923(7) 0.37231(4) 0.03494(4) 0.0207(2) Uani 1 1 d . . . O1 O 0.33256(16) 0.28351(9) 0.18448(11) 0.0193(5) Uani 1 1 d . . . O1' O 0.41748(16) 0.32486(9) 0.30671(10) 0.0195(5) Uani 1 1 d . . . O1" O 0.30991(17) 0.23601(9) 0.30809(11) 0.0218(5) Uani 1 1 d . . . O2 O -0.05365(16) 0.30402(9) 0.07687(10) 0.0190(5) Uani 1 1 d . . . O2' O -0.15151(16) 0.39643(9) 0.10835(10) 0.0182(5) Uani 1 1 d . . . O2" O -0.23170(16) 0.30874(9) 0.15150(11) 0.0180(5) Uani 1 1 d . . . O11 O -0.12045(19) 0.18397(11) -0.00986(13) 0.0363(6) Uani 1 1 d . . . O12 O 0.0451(2) 0.15147(12) 0.21669(13) 0.0534(8) Uani 1 1 d . . . O13 O 0.4069(2) 0.15899(11) 0.13508(12) 0.0402(7) Uani 1 1 d . . . O14 O 0.2368(2) 0.20702(11) -0.08739(13) 0.0388(7) Uani 1 1 d . . . O15 O 0.1406(2) 0.04550(11) 0.02992(15) 0.0531(8) Uani 1 1 d . . . C1 C 0.0969(2) 0.31948(13) 0.20749(15) 0.0143(7) Uani 1 1 d . . . C2 C 0.1769(2) 0.32243(13) 0.26981(15) 0.0159(7) Uani 1 1 d . . . C3 C 0.1471(3) 0.34921(12) 0.33281(15) 0.0169(7) Uani 1 1 d . . . H3A H 0.2022 0.3506 0.3733 0.020 Uiso 1 1 calc R . . C4 C 0.0358(2) 0.37406(13) 0.33644(15) 0.0159(7) Uani 1 1 d . . . C5 C -0.0437(2) 0.36987(13) 0.27490(15) 0.0156(7) Uani 1 1 d . . . H5A H -0.1187 0.3853 0.2758 0.019 Uiso 1 1 calc R . . C6 C -0.0143(2) 0.34323(12) 0.21181(15) 0.0145(7) Uani 1 1 d . . . C7 C 0.0093(3) 0.40446(14) 0.40570(16) 0.0214(8) Uani 1 1 d . . . C8 C 0.0948(3) 0.45312(15) 0.41947(18) 0.0355(9) Uani 1 1 d . . . H8A H 0.1745 0.4396 0.4217 0.053 Uiso 1 1 calc R . . H8B H 0.0816 0.4707 0.4647 0.053 Uiso 1 1 calc R . . H8C H 0.0820 0.4797 0.3806 0.053 Uiso 1 1 calc R . . C9 C -0.1175(3) 0.42648(14) 0.40036(17) 0.0279(9) Uani 1 1 d . . . H9A H -0.1290 0.4524 0.3608 0.042 Uiso 1 1 calc R . . H9B H -0.1316 0.4449 0.4449 0.042 Uiso 1 1 calc R . . H9C H -0.1717 0.3959 0.3920 0.042 Uiso 1 1 calc R . . C10 C 0.0253(3) 0.36293(15) 0.46972(16) 0.0330(9) Uani 1 1 d . . . H10A H 0.1061 0.3508 0.4761 0.049 Uiso 1 1 calc R . . H10B H -0.0253 0.3313 0.4595 0.049 Uiso 1 1 calc R . . H10C H 0.0051 0.3809 0.5134 0.049 Uiso 1 1 calc R . . C11 C -0.0263(3) 0.18127(14) 0.01696(17) 0.0225(8) Uani 1 1 d . . . C12 C 0.0812(3) 0.15938(14) 0.16192(19) 0.0295(9) Uani 1 1 d . . . C13 C 0.3121(3) 0.16501(14) 0.10926(17) 0.0254(8) Uani 1 1 d . . . C14 C 0.2038(3) 0.19481(14) -0.03304(18) 0.0232(8) Uani 1 1 d . . . C15 C 0.1411(3) 0.09253(15) 0.04038(18) 0.0293(9) Uani 1 1 d . . . C21 C 0.4025(3) 0.19293(14) 0.31596(18) 0.0256(8) Uani 1 1 d . . . H21A H 0.4468 0.1930 0.2729 0.031 Uiso 1 1 calc R . . C22 C 0.3384(3) 0.13841(15) 0.32062(19) 0.0381(10) Uani 1 1 d . . . H22A H 0.2917 0.1315 0.2755 0.057 Uiso 1 1 calc R . . H22B H 0.2879 0.1401 0.3594 0.057 Uiso 1 1 calc R . . H22C H 0.3948 0.1089 0.3299 0.057 Uiso 1 1 calc R . . C23 C 0.4851(3) 0.20483(17) 0.38274(19) 0.0439(11) Uani 1 1 d . . . H23A H 0.5215 0.2406 0.3778 0.066 Uiso 1 1 calc R . . H23B H 0.5451 0.1766 0.3881 0.066 Uiso 1 1 calc R . . H23C H 0.4415 0.2049 0.4249 0.066 Uiso 1 1 calc R . . C24 C 0.4506(3) 0.38039(13) 0.28209(17) 0.0222(8) Uani 1 1 d . . . H24A H 0.3873 0.3953 0.2479 0.027 Uiso 1 1 calc R . . C25 C 0.5621(3) 0.37421(15) 0.24443(19) 0.0377(10) Uani 1 1 d . . . H25A H 0.5481 0.3491 0.2040 0.057 Uiso 1 1 calc R . . H25B H 0.6239 0.3596 0.2781 0.057 Uiso 1 1 calc R . . H25C H 0.5853 0.4100 0.2272 0.057 Uiso 1 1 calc R . . C26 C 0.4650(3) 0.41643(15) 0.34932(19) 0.0395(10) Uani 1 1 d . . . H26A H 0.3929 0.4163 0.3726 0.059 Uiso 1 1 calc R . . H26B H 0.4832 0.4539 0.3359 0.059 Uiso 1 1 calc R . . H26C H 0.5280 0.4021 0.3823 0.059 Uiso 1 1 calc R . . C31 C -0.2363(3) 0.24820(14) 0.16614(18) 0.0262(8) Uani 1 1 d . . . H31A H -0.1611 0.2312 0.1562 0.031 Uiso 1 1 calc R . . C32 C -0.3317(4) 0.22563(19) 0.1149(3) 0.0856(18) Uani 1 1 d . . . H32A H -0.3189 0.2367 0.0662 0.128 Uiso 1 1 calc R . . H32B H -0.4064 0.2398 0.1270 0.128 Uiso 1 1 calc R . . H32C H -0.3319 0.1857 0.1180 0.128 Uiso 1 1 calc R . . C33 C -0.2546(5) 0.23990(19) 0.2441(2) 0.0856(18) Uani 1 1 d . . . H33A H -0.1907 0.2567 0.2740 0.128 Uiso 1 1 calc R . . H33B H -0.2573 0.2007 0.2545 0.128 Uiso 1 1 calc R . . H33C H -0.3278 0.2569 0.2543 0.128 Uiso 1 1 calc R . . C34 C -0.2055(3) 0.40724(15) 0.03336(16) 0.0270(8) Uani 1 1 d . . . H34A H -0.1983 0.3737 0.0038 0.032 Uiso 1 1 calc R . . C35 C -0.3330(3) 0.42071(17) 0.03616(19) 0.0435(11) Uani 1 1 d . . . H35A H -0.3706 0.3912 0.0606 0.065 Uiso 1 1 calc R . . H35B H -0.3702 0.4245 -0.0124 0.065 Uiso 1 1 calc R . . H35C H -0.3404 0.4550 0.0621 0.065 Uiso 1 1 calc R . . C36 C -0.1352(3) 0.45327(17) 0.0037(2) 0.0472(12) Uani 1 1 d . . . H36A H -0.0549 0.4413 0.0020 0.071 Uiso 1 1 calc R . . H36B H -0.1372 0.4854 0.0345 0.071 Uiso 1 1 calc R . . H36C H -0.1683 0.4626 -0.0445 0.071 Uiso 1 1 calc R . . C41 C 0.3118(3) 0.35202(14) -0.01757(17) 0.0215(8) Uani 1 1 d . . . C42 C 0.4009(3) 0.31549(15) 0.00571(19) 0.0312(9) Uani 1 1 d . . . H42A H 0.4024 0.3002 0.0521 0.037 Uiso 1 1 calc R . . C43 C 0.4888(3) 0.30090(16) -0.0387(2) 0.0401(10) Uani 1 1 d . . . H43A H 0.5471 0.2754 -0.0226 0.048 Uiso 1 1 calc R . . C44 C 0.4884(3) 0.32473(17) -0.1070(2) 0.0426(10) Uani 1 1 d . . . H44A H 0.5469 0.3155 -0.1369 0.051 Uiso 1 1 calc R . . C45 C 0.4015(3) 0.36212(18) -0.1306(2) 0.0435(11) Uani 1 1 d . . . H45A H 0.4020 0.3787 -0.1761 0.052 Uiso 1 1 calc R . . C46 C 0.3128(3) 0.37503(16) -0.08615(18) 0.0345(9) Uani 1 1 d . . . H46A H 0.2531 0.3996 -0.1029 0.041 Uiso 1 1 calc R . . C51 C 0.2587(3) 0.42300(13) 0.10023(16) 0.0199(7) Uani 1 1 d . . . C52 C 0.3692(3) 0.44611(14) 0.09469(17) 0.0268(8) Uani 1 1 d . . . H52A H 0.4163 0.4321 0.0604 0.032 Uiso 1 1 calc R . . C53 C 0.4108(3) 0.48955(15) 0.13910(19) 0.0321(9) Uani 1 1 d . . . H53A H 0.4847 0.5048 0.1335 0.039 Uiso 1 1 calc R . . C54 C 0.3444(3) 0.51059(14) 0.19149(19) 0.0328(9) Uani 1 1 d . . . H54A H 0.3731 0.5396 0.2215 0.039 Uiso 1 1 calc R . . C55 C 0.2340(3) 0.48776(15) 0.19869(18) 0.0318(9) Uani 1 1 d . . . H55A H 0.1886 0.5011 0.2343 0.038 Uiso 1 1 calc R . . C56 C 0.1916(3) 0.44542(14) 0.15334(17) 0.0248(8) Uani 1 1 d . . . H56A H 0.1165 0.4313 0.1580 0.030 Uiso 1 1 calc R . . C61 C -0.2462(3) 0.05472(15) 0.17121(19) 0.0299(9) Uani 1 1 d . . . C62 C -0.3639(3) 0.07109(15) 0.16961(19) 0.0347(9) Uani 1 1 d . . . H62A H -0.3968 0.0924 0.1309 0.042 Uiso 1 1 calc R . . C63 C -0.4326(3) 0.05625(16) 0.2244(2) 0.0396(10) Uani 1 1 d . . . H63A H -0.5109 0.0677 0.2224 0.047 Uiso 1 1 calc R . . C64 C -0.3855(3) 0.02472(17) 0.2816(2) 0.0407(10) Uani 1 1 d . . . H64A H -0.4318 0.0143 0.3183 0.049 Uiso 1 1 calc R . . C65 C -0.2690(3) 0.00862(16) 0.28447(19) 0.0413(10) Uani 1 1 d . . . H65A H -0.2361 -0.0125 0.3235 0.050 Uiso 1 1 calc R . . C66 C -0.2015(3) 0.02351(15) 0.23006(19) 0.0349(9) Uani 1 1 d . . . H66A H -0.1229 0.0122 0.2328 0.042 Uiso 1 1 calc R . . C67 C -0.1731(3) 0.06845(18) 0.1099(2) 0.0528(12) Uani 1 1 d . . . H67A H -0.0910 0.0685 0.1275 0.079 Uiso 1 1 calc R . . H67B H -0.1949 0.1046 0.0908 0.079 Uiso 1 1 calc R . . H67C H -0.1868 0.0410 0.0722 0.079 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 W1 0.01933(7) 0.01830(7) 0.01418(7) -0.00180(7) 0.00233(5) 0.00159(7) Sn1 0.01488(11) 0.01844(12) 0.01358(12) -0.00295(10) 0.00175(9) 0.00054(10) P1 0.0143(4) 0.0192(5) 0.0173(5) 0.0002(4) -0.0025(3) 0.0014(4) P2 0.0141(4) 0.0190(5) 0.0135(4) -0.0013(4) -0.0007(3) 0.0012(4) P3 0.0197(4) 0.0234(5) 0.0186(5) 0.0023(4) -0.0005(3) 0.0001(4) O1 0.0138(11) 0.0268(13) 0.0171(12) -0.0021(10) 0.0011(9) 0.0032(10) O1' 0.0194(11) 0.0182(12) 0.0198(12) 0.0039(10) -0.0037(9) -0.0003(11) O1" 0.0200(12) 0.0178(12) 0.0270(14) 0.0047(10) -0.0005(10) 0.0042(10) O2 0.0149(11) 0.0264(13) 0.0155(12) -0.0051(10) 0.0004(9) 0.0005(10) O2' 0.0209(12) 0.0201(12) 0.0129(12) 0.0008(10) -0.0020(9) 0.0016(10) O2" 0.0138(11) 0.0194(12) 0.0210(13) -0.0003(10) 0.0028(9) -0.0014(10) O11 0.0233(14) 0.0494(19) 0.0346(15) -0.0006(13) -0.0055(11) -0.0034(13) O12 0.0536(17) 0.084(2) 0.0252(16) 0.0098(15) 0.0175(13) -0.0114(16) O13 0.0260(14) 0.064(2) 0.0295(15) -0.0017(13) -0.0023(11) 0.0175(14) O14 0.0430(15) 0.0555(19) 0.0199(14) 0.0058(13) 0.0130(12) 0.0071(14) O15 0.071(2) 0.0263(17) 0.063(2) -0.0088(14) 0.0088(15) 0.0005(16) C1 0.0153(16) 0.0143(17) 0.0139(17) -0.0012(14) 0.0042(12) -0.0030(14) C2 0.0149(15) 0.0172(17) 0.0152(17) 0.0038(15) -0.0001(12) -0.0007(15) C3 0.0194(17) 0.0184(17) 0.0119(17) -0.0007(14) -0.0038(13) -0.0025(15) C4 0.0216(17) 0.0154(17) 0.0109(17) -0.0015(14) 0.0021(13) -0.0026(15) C5 0.0119(16) 0.0195(17) 0.0162(17) 0.0003(14) 0.0053(12) 0.0036(15) C6 0.0130(16) 0.0142(17) 0.0160(17) -0.0003(13) -0.0011(12) 0.0004(13) C7 0.0253(19) 0.0243(19) 0.0148(18) -0.0069(15) 0.0027(14) -0.0003(16) C8 0.040(2) 0.036(2) 0.031(2) -0.0173(18) 0.0062(17) -0.0020(19) C9 0.033(2) 0.031(2) 0.021(2) -0.0074(16) 0.0073(15) 0.0004(17) C10 0.040(2) 0.044(2) 0.0150(19) 0.0015(17) 0.0061(15) 0.008(2) C11 0.027(2) 0.023(2) 0.0180(18) -0.0006(16) 0.0066(15) -0.0054(17) C12 0.0247(19) 0.034(2) 0.029(2) -0.0022(18) -0.0004(16) -0.0021(17) C13 0.027(2) 0.034(2) 0.0168(18) -0.0069(16) 0.0079(15) 0.0074(18) C14 0.0240(19) 0.0234(19) 0.022(2) -0.0053(16) 0.0007(15) 0.0032(16) C15 0.037(2) 0.020(2) 0.031(2) -0.0097(17) 0.0019(17) -0.0067(18) C21 0.0231(19) 0.0243(19) 0.029(2) 0.0011(16) 0.0016(15) 0.0066(16) C22 0.046(2) 0.025(2) 0.042(2) 0.0075(18) -0.0023(18) 0.004(2) C23 0.046(2) 0.042(3) 0.040(3) 0.005(2) -0.0179(19) 0.008(2) C24 0.0219(18) 0.0185(19) 0.0249(19) 0.0035(16) -0.0058(14) -0.0002(16) C25 0.033(2) 0.034(2) 0.048(3) 0.0050(19) 0.0101(18) -0.0058(19) C26 0.049(2) 0.029(2) 0.041(2) -0.0091(19) 0.0040(19) -0.012(2) C31 0.0229(19) 0.0187(19) 0.038(2) 0.0031(17) 0.0087(16) -0.0009(16) C32 0.112(4) 0.042(3) 0.092(4) 0.010(3) -0.045(3) -0.039(3) C33 0.172(6) 0.044(3) 0.041(3) 0.020(2) 0.013(3) -0.010(4) C34 0.037(2) 0.030(2) 0.0131(18) -0.0017(16) -0.0052(15) 0.0063(18) C35 0.029(2) 0.061(3) 0.038(2) 0.008(2) -0.0118(17) -0.003(2) C36 0.041(2) 0.056(3) 0.045(3) 0.032(2) 0.0085(19) 0.005(2) C41 0.0225(18) 0.0229(19) 0.0192(19) -0.0019(15) 0.0026(14) -0.0073(16) C42 0.027(2) 0.038(2) 0.030(2) 0.0053(18) 0.0109(16) -0.0023(18) C43 0.031(2) 0.037(2) 0.054(3) 0.006(2) 0.0130(19) 0.0068(19) C44 0.047(2) 0.049(3) 0.036(2) -0.005(2) 0.0236(19) -0.004(2) C45 0.055(3) 0.054(3) 0.024(2) 0.004(2) 0.0127(19) -0.005(2) C46 0.037(2) 0.041(2) 0.025(2) 0.0026(19) 0.0010(16) -0.003(2) C51 0.0194(17) 0.0159(18) 0.0238(19) 0.0062(15) -0.0018(14) 0.0029(15) C52 0.0233(19) 0.028(2) 0.029(2) -0.0003(17) 0.0006(15) 0.0016(17) C53 0.027(2) 0.027(2) 0.040(2) 0.0022(19) -0.0071(17) -0.0052(18) C54 0.044(2) 0.019(2) 0.033(2) -0.0040(17) -0.0090(18) 0.0052(19) C55 0.039(2) 0.027(2) 0.029(2) -0.0025(17) 0.0025(17) 0.0080(19) C56 0.0269(19) 0.0193(19) 0.028(2) 0.0046(16) 0.0023(15) 0.0030(16) C61 0.036(2) 0.020(2) 0.033(2) -0.0020(17) 0.0018(17) -0.0068(18) C62 0.039(2) 0.025(2) 0.038(2) 0.0089(18) -0.0059(18) 0.0057(19) C63 0.032(2) 0.036(2) 0.050(3) 0.001(2) 0.0045(19) 0.005(2) C64 0.044(2) 0.046(3) 0.034(2) 0.002(2) 0.0113(19) -0.006(2) C65 0.056(3) 0.038(3) 0.028(2) 0.0124(19) -0.0043(19) 0.001(2) C66 0.027(2) 0.034(2) 0.042(2) 0.000(2) -0.0048(17) 0.0060(18) C67 0.051(3) 0.061(3) 0.048(3) 0.011(2) 0.011(2) -0.012(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag W1 C15 1.987(3) . ? W1 C12 2.029(3) . ? W1 C13 2.030(3) . ? W1 C14 2.042(3) . ? W1 C11 2.051(3) . ? W1 Sn1 2.7657(3) . ? Sn1 C1 2.182(3) . ? Sn1 O2 2.3607(19) . ? Sn1 O1 2.4308(19) . ? Sn1 P3 2.5577(9) . ? P1 O1 1.487(2) . ? P1 O1" 1.556(2) . ? P1 O1' 1.574(2) . ? P1 C2 1.776(3) . ? P2 O2 1.492(2) . ? P2 O2' 1.557(2) . ? P2 O2" 1.567(2) . ? P2 C6 1.780(3) . ? P3 C41 1.835(3) . ? P3 C51 1.838(3) . ? O1' C24 1.467(4) . ? O1" C21 1.472(4) . ? O2' C34 1.485(3) . ? O2" C31 1.479(4) . ? O11 C11 1.139(4) . ? O12 C12 1.142(4) . ? O13 C13 1.147(4) . ? O14 C14 1.142(3) . ? O15 C15 1.144(4) . ? C1 C6 1.396(4) . ? C1 C2 1.401(4) . ? C2 C3 1.397(4) . ? C3 C4 1.406(4) . ? C4 C5 1.389(4) . ? C4 C7 1.526(4) . ? C5 C6 1.396(4) . ? C7 C8 1.525(4) . ? C7 C9 1.531(4) . ? C7 C10 1.544(4) . ? C21 C22 1.503(4) . ? C21 C23 1.507(4) . ? C24 C25 1.508(4) . ? C24 C26 1.509(4) . ? C31 C32 1.475(5) . ? C31 C33 1.487(5) . ? C34 C35 1.491(4) . ? C34 C36 1.496(5) . ? C41 C42 1.377(4) . ? C41 C46 1.382(4) . ? C42 C43 1.395(4) . ? C43 C44 1.383(5) . ? C44 C45 1.375(5) . ? C45 C46 1.392(4) . ? C51 C52 1.385(4) . ? C51 C56 1.404(4) . ? C52 C53 1.382(4) . ? C53 C54 1.376(4) . ? C54 C55 1.387(4) . ? C55 C56 1.375(4) . ? C61 C66 1.377(5) . ? C61 C62 1.392(4) . ? C61 C67 1.501(4) . ? C62 C63 1.380(5) . ? C63 C64 1.368(5) . ? C64 C65 1.376(5) . ? C65 C66 1.367(5) . ? 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 C15 W1 C12 92.04(14) . . ? C15 W1 C13 89.24(14) . . ? C12 W1 C13 90.61(12) . . ? C15 W1 C14 92.97(13) . . ? C12 W1 C14 174.93(14) . . ? C13 W1 C14 90.30(12) . . ? C15 W1 C11 90.24(14) . . ? C12 W1 C11 90.05(12) . . ? C13 W1 C11 179.17(13) . . ? C14 W1 C11 89.08(12) . . ? C15 W1 Sn1 176.32(10) . . ? C12 W1 Sn1 84.68(10) . . ? C13 W1 Sn1 89.13(10) . . ? C14 W1 Sn1 90.34(9) . . ? C11 W1 Sn1 91.42(9) . . ? C1 Sn1 O2 77.60(9) . . ? C1 Sn1 O1 77.15(9) . . ? O2 Sn1 O1 154.70(6) . . ? C1 Sn1 P3 101.20(8) . . ? O2 Sn1 P3 86.13(5) . . ? O1 Sn1 P3 97.07(5) . . ? C1 Sn1 W1 127.97(8) . . ? O2 Sn1 W1 97.80(5) . . ? O1 Sn1 W1 99.01(5) . . ? P3 Sn1 W1 130.48(2) . . ? O1 P1 O1" 116.22(12) . . ? O1 P1 O1' 114.19(11) . . ? O1" P1 O1' 103.52(12) . . ? O1 P1 C2 108.00(12) . . ? O1" P1 C2 103.70(12) . . ? O1' P1 C2 110.70(13) . . ? O2 P2 O2' 114.92(12) . . ? O2 P2 O2" 113.15(12) . . ? O2' P2 O2" 103.55(11) . . ? O2 P2 C6 108.56(13) . . ? O2' P2 C6 106.45(13) . . ? O2" P2 C6 109.92(12) . . ? C41 P3 C51 102.73(14) . . ? C41 P3 Sn1 103.59(11) . . ? C51 P3 Sn1 107.29(10) . . ? P1 O1 Sn1 113.69(10) . . ? C24 O1' P1 120.76(18) . . ? C21 O1" P1 125.02(18) . . ? P2 O2 Sn1 116.40(11) . . ? C34 O2' P2 120.22(19) . . ? C31 O2" P2 120.09(18) . . ? C6 C1 C2 117.1(3) . . ? C6 C1 Sn1 121.6(2) . . ? C2 C1 Sn1 121.2(2) . . ? C3 C2 C1 121.2(3) . . ? C3 C2 P1 122.9(2) . . ? C1 C2 P1 115.9(2) . . ? C2 C3 C4 121.5(3) . . ? C5 C4 C3 116.8(3) . . ? C5 C4 C7 123.8(3) . . ? C3 C4 C7 119.4(3) . . ? C4 C5 C6 121.8(3) . . ? C5 C6 C1 121.5(3) . . ? C5 C6 P2 123.5(2) . . ? C1 C6 P2 115.0(2) . . ? C8 C7 C4 109.5(2) . . ? C8 C7 C9 109.2(3) . . ? C4 C7 C9 111.6(2) . . ? C8 C7 C10 109.8(3) . . ? C4 C7 C10 108.4(3) . . ? C9 C7 C10 108.4(2) . . ? O11 C11 W1 177.9(3) . . ? O12 C12 W1 179.3(3) . . ? O13 C13 W1 178.4(3) . . ? O14 C14 W1 179.5(3) . . ? O15 C15 W1 177.0(3) . . ? O1" C21 C22 105.7(2) . . ? O1" C21 C23 109.5(3) . . ? C22 C21 C23 112.8(3) . . ? O1' C24 C25 107.7(3) . . ? O1' C24 C26 106.1(2) . . ? C25 C24 C26 113.8(3) . . ? C32 C31 O2" 106.2(3) . . ? C32 C31 C33 114.3(4) . . ? O2" C31 C33 108.6(3) . . ? O2' C34 C35 109.0(2) . . ? O2' C34 C36 106.4(3) . . ? C35 C34 C36 114.0(3) . . ? C42 C41 C46 118.2(3) . . ? C42 C41 P3 125.2(2) . . ? C46 C41 P3 116.6(3) . . ? C41 C42 C43 121.5(3) . . ? C44 C43 C42 119.3(4) . . ? C45 C44 C43 120.0(3) . . ? C44 C45 C46 119.8(3) . . ? C41 C46 C45 121.2(4) . . ? C52 C51 C56 116.9(3) . . ? C52 C51 P3 123.6(2) . . ? C56 C51 P3 118.9(2) . . ? C53 C52 C51 121.4(3) . . ? C54 C53 C52 120.9(3) . . ? C53 C54 C55 118.8(3) . . ? C56 C55 C54 120.2(3) . . ? C55 C56 C51 121.7(3) . . ? C66 C61 C62 117.0(3) . . ? C66 C61 C67 121.6(3) . . ? C62 C61 C67 121.3(3) . . ? C63 C62 C61 121.3(3) . . ? C64 C63 C62 120.1(3) . . ? C63 C64 C65 119.4(3) . . ? C66 C65 C64 120.2(4) . . ? C65 C66 C61 122.0(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C15 W1 Sn1 C1 -27.2(15) . . . . ? C12 W1 Sn1 C1 -0.28(13) . . . . ? C13 W1 Sn1 C1 -90.97(13) . . . . ? C14 W1 Sn1 C1 178.73(13) . . . . ? C11 W1 Sn1 C1 89.64(13) . . . . ? C15 W1 Sn1 O2 -107.5(15) . . . . ? C12 W1 Sn1 O2 -80.61(10) . . . . ? C13 W1 Sn1 O2 -171.31(10) . . . . ? C14 W1 Sn1 O2 98.40(10) . . . . ? C11 W1 Sn1 O2 9.31(9) . . . . ? C15 W1 Sn1 O1 53.5(15) . . . . ? C12 W1 Sn1 O1 80.41(10) . . . . ? C13 W1 Sn1 O1 -10.29(9) . . . . ? C14 W1 Sn1 O1 -100.58(10) . . . . ? C11 W1 Sn1 O1 170.33(9) . . . . ? C15 W1 Sn1 P3 160.9(15) . . . . ? C12 W1 Sn1 P3 -172.17(9) . . . . ? C13 W1 Sn1 P3 97.13(9) . . . . ? C14 W1 Sn1 P3 6.84(9) . . . . ? C11 W1 Sn1 P3 -82.25(9) . . . . ? C1 Sn1 P3 C41 145.63(13) . . . . ? O2 Sn1 P3 C41 -137.82(11) . . . . ? O1 Sn1 P3 C41 67.40(11) . . . . ? W1 Sn1 P3 C41 -40.87(11) . . . . ? C1 Sn1 P3 C51 37.41(13) . . . . ? O2 Sn1 P3 C51 113.95(11) . . . . ? O1 Sn1 P3 C51 -40.83(11) . . . . ? W1 Sn1 P3 C51 -149.09(10) . . . . ? O1" P1 O1 Sn1 94.45(13) . . . . ? O1' P1 O1 Sn1 -145.10(11) . . . . ? C2 P1 O1 Sn1 -21.50(16) . . . . ? C1 Sn1 O1 P1 16.35(13) . . . . ? O2 Sn1 O1 P1 20.4(2) . . . . ? P3 Sn1 O1 P1 116.28(11) . . . . ? W1 Sn1 O1 P1 -110.72(11) . . . . ? O1 P1 O1' C24 53.5(2) . . . . ? O1" P1 O1' C24 -179.2(2) . . . . ? C2 P1 O1' C24 -68.6(2) . . . . ? O1 P1 O1" C21 58.1(3) . . . . ? O1' P1 O1" C21 -67.9(2) . . . . ? C2 P1 O1" C21 176.4(2) . . . . ? O2' P2 O2 Sn1 111.93(13) . . . . ? O2" P2 O2 Sn1 -129.41(12) . . . . ? C6 P2 O2 Sn1 -7.11(17) . . . . ? C1 Sn1 O2 P2 8.01(14) . . . . ? O1 Sn1 O2 P2 4.0(3) . . . . ? P3 Sn1 O2 P2 -94.35(12) . . . . ? W1 Sn1 O2 P2 135.29(12) . . . . ? O2 P2 O2' C34 42.1(2) . . . . ? O2" P2 O2' C34 -81.8(2) . . . . ? C6 P2 O2' C34 162.3(2) . . . . ? O2 P2 O2" C31 45.7(2) . . . . ? O2' P2 O2" C31 170.8(2) . . . . ? C6 P2 O2" C31 -75.8(2) . . . . ? O2 Sn1 C1 C6 -7.4(2) . . . . ? O1 Sn1 C1 C6 170.8(3) . . . . ? P3 Sn1 C1 C6 76.0(2) . . . . ? W1 Sn1 C1 C6 -97.7(2) . . . . ? O2 Sn1 C1 C2 176.5(3) . . . . ? O1 Sn1 C1 C2 -5.2(2) . . . . ? P3 Sn1 C1 C2 -100.0(2) . . . . ? W1 Sn1 C1 C2 86.3(2) . . . . ? C6 C1 C2 C3 -1.5(4) . . . . ? Sn1 C1 C2 C3 174.7(2) . . . . ? C6 C1 C2 P1 178.8(2) . . . . ? Sn1 C1 C2 P1 -5.0(3) . . . . ? O1 P1 C2 C3 -161.4(3) . . . . ? O1" P1 C2 C3 74.8(3) . . . . ? O1' P1 C2 C3 -35.7(3) . . . . ? O1 P1 C2 C1 18.3(3) . . . . ? O1" P1 C2 C1 -105.5(2) . . . . ? O1' P1 C2 C1 144.0(2) . . . . ? C1 C2 C3 C4 0.3(5) . . . . ? P1 C2 C3 C4 180.0(2) . . . . ? C2 C3 C4 C5 1.1(4) . . . . ? C2 C3 C4 C7 -178.0(3) . . . . ? C3 C4 C5 C6 -1.2(5) . . . . ? C7 C4 C5 C6 177.8(3) . . . . ? C4 C5 C6 C1 -0.1(5) . . . . ? C4 C5 C6 P2 179.4(2) . . . . ? C2 C1 C6 C5 1.4(4) . . . . ? Sn1 C1 C6 C5 -174.7(2) . . . . ? C2 C1 C6 P2 -178.1(2) . . . . ? Sn1 C1 C6 P2 5.7(3) . . . . ? O2 P2 C6 C5 -178.1(2) . . . . ? O2' P2 C6 C5 57.7(3) . . . . ? O2" P2 C6 C5 -53.8(3) . . . . ? O2 P2 C6 C1 1.4(3) . . . . ? O2' P2 C6 C1 -122.8(2) . . . . ? O2" P2 C6 C1 125.6(2) . . . . ? C5 C4 C7 C8 -117.6(3) . . . . ? C3 C4 C7 C8 61.4(4) . . . . ? C5 C4 C7 C9 3.4(4) . . . . ? C3 C4 C7 C9 -177.6(3) . . . . ? C5 C4 C7 C10 122.7(3) . . . . ? C3 C4 C7 C10 -58.3(4) . . . . ? C15 W1 C11 O11 -6(8) . . . . ? C12 W1 C11 O11 -98(8) . . . . ? C13 W1 C11 O11 46(14) . . . . ? C14 W1 C11 O11 87(8) . . . . ? Sn1 W1 C11 O11 178(100) . . . . ? C15 W1 C12 O12 -81(24) . . . . ? C13 W1 C12 O12 -170(100) . . . . ? C14 W1 C12 O12 89(24) . . . . ? C11 W1 C12 O12 9(24) . . . . ? Sn1 W1 C12 O12 101(24) . . . . ? C15 W1 C13 O13 -24(10) . . . . ? C12 W1 C13 O13 68(10) . . . . ? C14 W1 C13 O13 -117(10) . . . . ? C11 W1 C13 O13 -76(15) . . . . ? Sn1 W1 C13 O13 152(10) . . . . ? C15 W1 C14 O14 123(49) . . . . ? C12 W1 C14 O14 -47(49) . . . . ? C13 W1 C14 O14 -147(100) . . . . ? C11 W1 C14 O14 33(49) . . . . ? Sn1 W1 C14 O14 -58(49) . . . . ? C12 W1 C15 O15 -29(6) . . . . ? C13 W1 C15 O15 62(6) . . . . ? C14 W1 C15 O15 152(6) . . . . ? C11 W1 C15 O15 -119(6) . . . . ? Sn1 W1 C15 O15 -2(8) . . . . ? P1 O1" C21 C22 -146.1(2) . . . . ? P1 O1" C21 C23 92.2(3) . . . . ? P1 O1' C24 C25 -101.4(3) . . . . ? P1 O1' C24 C26 136.4(2) . . . . ? P2 O2" C31 C32 -123.7(3) . . . . ? P2 O2" C31 C33 112.8(3) . . . . ? P2 O2' C34 C35 109.5(3) . . . . ? P2 O2' C34 C36 -127.2(2) . . . . ? C51 P3 C41 C42 77.7(3) . . . . ? Sn1 P3 C41 C42 -33.9(3) . . . . ? C51 P3 C41 C46 -103.2(3) . . . . ? Sn1 P3 C41 C46 145.2(2) . . . . ? C46 C41 C42 C43 -1.3(5) . . . . ? P3 C41 C42 C43 177.9(3) . . . . ? C41 C42 C43 C44 1.7(6) . . . . ? C42 C43 C44 C45 -0.4(6) . . . . ? C43 C44 C45 C46 -1.3(6) . . . . ? C42 C41 C46 C45 -0.4(5) . . . . ? P3 C41 C46 C45 -179.6(3) . . . . ? C44 C45 C46 C41 1.7(6) . . . . ? C41 P3 C51 C52 12.5(3) . . . . ? Sn1 P3 C51 C52 121.3(3) . . . . ? C41 P3 C51 C56 -176.2(3) . . . . ? Sn1 P3 C51 C56 -67.3(3) . . . . ? C56 C51 C52 C53 -0.5(5) . . . . ? P3 C51 C52 C53 171.0(3) . . . . ? C51 C52 C53 C54 1.3(5) . . . . ? C52 C53 C54 C55 -0.6(5) . . . . ? C53 C54 C55 C56 -1.0(5) . . . . ? C54 C55 C56 C51 1.8(5) . . . . ? C52 C51 C56 C55 -1.0(5) . . . . ? P3 C51 C56 C55 -173.0(3) . . . . ? C66 C61 C62 C63 -0.5(5) . . . . ? C67 C61 C62 C63 177.0(4) . . . . ? C61 C62 C63 C64 -0.2(6) . . . . ? C62 C63 C64 C65 0.8(6) . . . . ? C63 C64 C65 C66 -0.7(6) . . . . ? C64 C65 C66 C61 0.1(6) . . . . ? C62 C61 C66 C65 0.5(5) . . . . ? C67 C61 C66 C65 -176.9(4) . . . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.862 _refine_diff_density_min -0.504 _refine_diff_density_rms 0.078 # Attachment '- compound5_revised3.cif' data_nox0085 _database_code_depnum_ccdc_archive 'CCDC 802874' #TrackingRef '- compound5_revised3.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C48 H78 O20 P4 Sn2 W2, C7 H8' _chemical_formula_sum 'C55 H86 O20 P4 Sn2 W2' _chemical_formula_weight 1796.20 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/n _symmetry_space_group_name_Hall -P2yn 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 22.0762(9) _cell_length_b 12.1870(4) _cell_length_c 26.8904(11) _cell_angle_alpha 90.00 _cell_angle_beta 106.306(4) _cell_angle_gamma 90.00 _cell_volume 6943.7(5) _cell_formula_units_Z 4 _cell_measurement_temperature 173(1) _cell_measurement_reflns_used 13299 _cell_measurement_theta_min 1.98 _cell_measurement_theta_max 29.09 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.718 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3536 _exptl_absorpt_coefficient_mu 4.170 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.793 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.37 (release 24-10-2008 CrysAlis171 .NET) (compiled Oct 24 2008,09:44:38) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(1) _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 'Xcalibur2 CCD diffractometer' _diffrn_measurement_method ; 348 frames via \w-rotation (\D\w = 1\%) and two times 45 s per frame (6 sets at different \k-angles) ; _diffrn_detector_area_resol_mean 16.0560 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 38853 _diffrn_reflns_av_R_equivalents 0.0575 _diffrn_reflns_av_sigmaI/netI 0.1108 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 1.98 _diffrn_reflns_theta_max 25.50 _reflns_number_total 12710 _reflns_number_gt 7891 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlis CCD (Oxford Diffraction, 2008) ; _computing_cell_refinement ; CrysAlis RED (Oxford Diffraction, 2008) ; _computing_data_reduction ; CrysAlis RED (Oxford Diffraction, 2008) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL-Plus (Sheldrick, 1991)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 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. C48, C63 and C64 have been refined with ISOR (0.01). Disorder in C48, C63, C64 and O11 cannot be modelled. ; _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^)+(0.0655P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 12710 _refine_ls_number_parameters 741 _refine_ls_number_restraints 30 _refine_ls_R_factor_all 0.0934 _refine_ls_R_factor_gt 0.0535 _refine_ls_wR_factor_ref 0.1292 _refine_ls_wR_factor_gt 0.1218 _refine_ls_goodness_of_fit_ref 0.962 _refine_ls_restrained_S_all 0.963 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group W1 W -0.034720(19) 0.04278(3) 0.165301(16) 0.02042(11) Uani 1 1 d . . . W2 W 0.07267(2) 0.25099(4) 0.324313(17) 0.03350(13) Uani 1 1 d . . . Sn1 Sn -0.02203(3) 0.01551(5) 0.26745(3) 0.02373(18) Uani 1 1 d . . . Sn2 Sn 0.02055(3) 0.24375(5) 0.18524(3) 0.02142(16) Uani 1 1 d . . . P1 P -0.14628(12) 0.0279(2) 0.31422(11) 0.0279(6) Uani 1 1 d . . . P2 P 0.07612(12) -0.1694(2) 0.33461(10) 0.0245(6) Uani 1 1 d . . . P3 P 0.15176(12) 0.2903(2) 0.15261(10) 0.0232(6) Uani 1 1 d . . . P4 P -0.07071(13) 0.4619(2) 0.15580(11) 0.0292(6) Uani 1 1 d . . . O1 O -0.1200(3) 0.0820(5) 0.2751(2) 0.0276(16) Uani 1 1 d . . . O1' O -0.1519(3) 0.1058(6) 0.3590(3) 0.0335(18) Uani 1 1 d . . . O1" O -0.2157(3) -0.0135(5) 0.2947(3) 0.0320(18) Uani 1 1 d . . . O2 O 0.0709(3) -0.0846(5) 0.2938(2) 0.0287(17) Uani 1 1 d . . . O2' O 0.1326(3) -0.1475(6) 0.3841(2) 0.0301(17) Uani 1 1 d . . . O2" O 0.0877(3) -0.2882(5) 0.3205(3) 0.0354(18) Uani 1 1 d . . . O3 O 0.1224(3) 0.2090(5) 0.1800(2) 0.0243(16) Uani 1 1 d . . . O3' O 0.2166(3) 0.3391(5) 0.1838(3) 0.0273(16) Uani 1 1 d . . . O3" O 0.1728(3) 0.2453(5) 0.1058(3) 0.0317(17) Uani 1 1 d . . . O4 O -0.0674(3) 0.3558(5) 0.1831(3) 0.0282(16) Uani 1 1 d . . . O4' O -0.0766(4) 0.5638(6) 0.1890(3) 0.058(3) Uani 1 1 d . . . O4" O -0.1265(3) 0.4727(7) 0.1045(3) 0.052(2) Uani 1 1 d . . . C1 C -0.0407(4) -0.0925(7) 0.3265(4) 0.020(2) Uani 1 1 d . . . C2 C -0.0966(5) -0.0848(8) 0.3407(4) 0.027(2) Uani 1 1 d . . . C3 C -0.1084(5) -0.1567(8) 0.3766(4) 0.034(3) Uani 1 1 d . . . H3A H -0.1458 -0.1494 0.3857 0.041 Uiso 1 1 calc R . . C4 C -0.0669(5) -0.2390(8) 0.3995(4) 0.029(2) Uani 1 1 d . . . C5 C -0.0096(5) -0.2436(8) 0.3876(4) 0.032(3) Uani 1 1 d . . . H5A H 0.0207 -0.2952 0.4035 0.038 Uiso 1 1 calc R . . C6 C 0.0023(4) -0.1685(8) 0.3507(4) 0.023(2) Uani 1 1 d . . . C7 C -0.0846(5) -0.3207(10) 0.4369(4) 0.039(3) Uani 1 1 d . . . C8 C -0.0940(8) -0.2552(13) 0.4838(5) 0.096(6) Uani 1 1 d . . . H8A H -0.1029 -0.3052 0.5085 0.144 Uiso 1 1 calc R . . H8B H -0.1287 -0.2052 0.4720 0.144 Uiso 1 1 calc R . . H8C H -0.0563 -0.2147 0.5000 0.144 Uiso 1 1 calc R . . C9 C -0.1453(7) -0.3773(12) 0.4104(6) 0.084(5) Uani 1 1 d . . . H9A H -0.1384 -0.4275 0.3850 0.126 Uiso 1 1 calc R . . H9B H -0.1762 -0.3237 0.3936 0.126 Uiso 1 1 calc R . . H9C H -0.1602 -0.4168 0.4355 0.126 Uiso 1 1 calc R . . C10 C -0.0361(8) -0.4023(16) 0.4570(8) 0.133(9) Uani 1 1 d . . . H10A H -0.0293 -0.4443 0.4288 0.199 Uiso 1 1 calc R . . H10B H -0.0492 -0.4503 0.4803 0.199 Uiso 1 1 calc R . . H10C H 0.0025 -0.3664 0.4751 0.199 Uiso 1 1 calc R . . O11 O -0.0959(4) -0.1888(6) 0.1357(3) 0.061(3) Uani 1 1 d . . . C11 C -0.0739(5) -0.1022(11) 0.1481(4) 0.039(3) Uani 1 1 d . . . O12 O 0.0998(4) -0.0684(6) 0.1828(3) 0.047(2) Uani 1 1 d . . . C12 C 0.0510(5) -0.0262(8) 0.1771(4) 0.027(2) Uani 1 1 d . . . O13 O -0.0425(4) 0.0701(7) 0.0485(3) 0.055(2) Uani 1 1 d . . . C13 C -0.0404(4) 0.0606(8) 0.0924(4) 0.020(2) Uani 1 1 d . . . O14 O -0.1688(3) 0.1541(6) 0.1514(3) 0.044(2) Uani 1 1 d . . . C14 C -0.1197(5) 0.1149(9) 0.1571(4) 0.029(2) Uani 1 1 d . . . O16 O 0.0208(3) 0.1318(5) 0.3210(2) 0.0318(18) Uani 1 1 d . . . O17 O 0.0616(3) 0.3004(6) 0.2591(3) 0.0343(18) Uani 1 1 d . . . O18 O 0.0554(4) 0.3519(7) 0.3630(3) 0.060(3) Uani 1 1 d . . . O19 O 0.1515(4) 0.2139(7) 0.3514(3) 0.063(3) Uani 1 1 d . . . C21 C -0.0926(5) 0.1605(10) 0.3910(4) 0.041(3) Uani 1 1 d . . . H21A H -0.0569 0.1300 0.3806 0.049 Uiso 1 1 calc R . . C22 C -0.0968(7) 0.2769(11) 0.3786(6) 0.071(4) Uani 1 1 d . . . H22A H -0.0566 0.3110 0.3937 0.106 Uiso 1 1 calc R . . H22B H -0.1281 0.3104 0.3923 0.106 Uiso 1 1 calc R . . H22C H -0.1084 0.2863 0.3417 0.106 Uiso 1 1 calc R . . C23 C -0.0847(7) 0.1313(13) 0.4452(5) 0.073(5) Uani 1 1 d . . . H23A H -0.0440 0.1553 0.4659 0.109 Uiso 1 1 calc R . . H23B H -0.0879 0.0532 0.4482 0.109 Uiso 1 1 calc R . . H23C H -0.1170 0.1663 0.4572 0.109 Uiso 1 1 calc R . . C24 C -0.2299(5) -0.0947(10) 0.2518(5) 0.043(3) Uani 1 1 d . . . H24A H -0.1901 -0.1252 0.2486 0.051 Uiso 1 1 calc R . . C25 C -0.2627(6) -0.0370(10) 0.2027(5) 0.055(4) Uani 1 1 d . . . H25A H -0.2354 0.0183 0.1955 0.083 Uiso 1 1 calc R . . H25B H -0.3006 -0.0032 0.2062 0.083 Uiso 1 1 calc R . . H25C H -0.2732 -0.0889 0.1747 0.083 Uiso 1 1 calc R . . C26 C -0.2673(6) -0.1848(10) 0.2677(5) 0.058(4) Uani 1 1 d . . . H26A H -0.2435 -0.2146 0.3004 0.088 Uiso 1 1 calc R . . H26B H -0.2757 -0.2417 0.2419 0.088 Uiso 1 1 calc R . . H26C H -0.3064 -0.1557 0.2708 0.088 Uiso 1 1 calc R . . C31 C 0.1564(5) -0.0340(9) 0.4001(4) 0.032(3) Uani 1 1 d . . . H31A H 0.1484 0.0132 0.3694 0.039 Uiso 1 1 calc R . . C32 C 0.2235(5) -0.0456(11) 0.4228(5) 0.062(4) Uani 1 1 d . . . H32A H 0.2427 -0.0703 0.3968 0.093 Uiso 1 1 calc R . . H32B H 0.2314 -0.0982 0.4504 0.093 Uiso 1 1 calc R . . H32C H 0.2412 0.0239 0.4361 0.093 Uiso 1 1 calc R . . C33 C 0.1221(6) 0.0097(10) 0.4363(5) 0.061(4) Uani 1 1 d . . . H33A H 0.1317 0.0862 0.4425 0.091 Uiso 1 1 calc R . . H33B H 0.1350 -0.0297 0.4684 0.091 Uiso 1 1 calc R . . H33C H 0.0775 0.0009 0.4212 0.091 Uiso 1 1 calc R . . C34 C 0.1387(5) -0.3189(10) 0.2979(5) 0.043(3) Uani 1 1 d . . . H34A H 0.1646 -0.2536 0.2978 0.051 Uiso 1 1 calc R . . C35 C 0.1107(6) -0.3542(11) 0.2432(5) 0.057(4) Uani 1 1 d . . . H35A H 0.0894 -0.2933 0.2231 0.086 Uiso 1 1 calc R . . H35B H 0.0810 -0.4124 0.2421 0.086 Uiso 1 1 calc R . . H35C H 0.1435 -0.3799 0.2291 0.086 Uiso 1 1 calc R . . C36 C 0.1790(6) -0.4027(11) 0.3329(5) 0.056(4) Uani 1 1 d . . . H36A H 0.1987 -0.3701 0.3660 0.083 Uiso 1 1 calc R . . H36B H 0.2109 -0.4284 0.3177 0.083 Uiso 1 1 calc R . . H36C H 0.1532 -0.4633 0.3373 0.083 Uiso 1 1 calc R . . C41 C 0.0395(4) 0.3912(7) 0.1459(4) 0.020(2) Uani 1 1 d . . . C42 C 0.0958(4) 0.3988(7) 0.1323(4) 0.021(2) Uani 1 1 d . . . C43 C 0.1074(5) 0.4919(7) 0.1053(4) 0.024(2) Uani 1 1 d . . . H43A H 0.1447 0.4961 0.0959 0.029 Uiso 1 1 calc R . . C44 C 0.0645(5) 0.5770(8) 0.0926(4) 0.024(2) Uani 1 1 d . . . C45 C 0.0096(5) 0.5693(8) 0.1079(4) 0.027(2) Uani 1 1 d . . . H45A H -0.0193 0.6267 0.1008 0.032 Uiso 1 1 calc R . . C46 C -0.0027(4) 0.4770(7) 0.1338(4) 0.018(2) Uani 1 1 d . . . C47 C 0.0794(5) 0.6767(9) 0.0627(4) 0.036(3) Uani 1 1 d . . . C48 C 0.0808(8) 0.6389(11) 0.0102(5) 0.078(5) Uani 1 1 d U . . H48A H 0.0406 0.6079 -0.0077 0.117 Uiso 1 1 calc R . . H48B H 0.1131 0.5844 0.0137 0.117 Uiso 1 1 calc R . . H48C H 0.0896 0.7002 -0.0091 0.117 Uiso 1 1 calc R . . C49 C 0.1434(6) 0.7281(11) 0.0920(6) 0.069(4) Uani 1 1 d . . . H49A H 0.1767 0.6768 0.0929 0.103 Uiso 1 1 calc R . . H49B H 0.1432 0.7456 0.1267 0.103 Uiso 1 1 calc R . . H49C H 0.1501 0.7938 0.0745 0.103 Uiso 1 1 calc R . . C50 C 0.0304(6) 0.7688(9) 0.0571(5) 0.058(4) Uani 1 1 d . . . H50A H -0.0086 0.7466 0.0329 0.087 Uiso 1 1 calc R . . H50B H 0.0456 0.8340 0.0446 0.087 Uiso 1 1 calc R . . H50C H 0.0235 0.7832 0.0902 0.087 Uiso 1 1 calc R . . C51 C 0.2231(5) 0.4047(8) 0.2312(4) 0.027(2) Uani 1 1 d . . . H51A H 0.1818 0.4347 0.2310 0.033 Uiso 1 1 calc R . . C52 C 0.2670(6) 0.4977(9) 0.2272(5) 0.046(3) Uani 1 1 d . . . H52A H 0.2502 0.5358 0.1950 0.069 Uiso 1 1 calc R . . H52B H 0.3078 0.4686 0.2285 0.069 Uiso 1 1 calc R . . H52C H 0.2707 0.5478 0.2554 0.069 Uiso 1 1 calc R . . C53 C 0.2471(5) 0.3350(9) 0.2776(4) 0.040(3) Uani 1 1 d . . . H53A H 0.2195 0.2734 0.2757 0.060 Uiso 1 1 calc R . . H53B H 0.2489 0.3771 0.3081 0.060 Uiso 1 1 calc R . . H53C H 0.2887 0.3093 0.2789 0.060 Uiso 1 1 calc R . . C54 C 0.1298(5) 0.1829(9) 0.0638(4) 0.036(3) Uani 1 1 d . . . H54A H 0.0860 0.1993 0.0627 0.043 Uiso 1 1 calc R . . C55 C 0.1422(6) 0.2211(12) 0.0151(4) 0.058(4) Uani 1 1 d . . . H55A H 0.1315 0.2974 0.0098 0.087 Uiso 1 1 calc R . . H55B H 0.1171 0.1793 -0.0136 0.087 Uiso 1 1 calc R . . H55C H 0.1861 0.2113 0.0175 0.087 Uiso 1 1 calc R . . C56 C 0.1424(7) 0.0634(9) 0.0737(5) 0.060(4) Uani 1 1 d . . . H56A H 0.1276 0.0410 0.1025 0.090 Uiso 1 1 calc R . . H56B H 0.1869 0.0500 0.0815 0.090 Uiso 1 1 calc R . . H56C H 0.1206 0.0224 0.0434 0.090 Uiso 1 1 calc R . . C61 C -0.1928(6) 0.4885(13) 0.1054(6) 0.067(4) Uani 1 1 d . . . H61A H -0.1958 0.4816 0.1409 0.080 Uiso 1 1 calc R . . C62 C -0.2126(7) 0.5962(15) 0.0856(7) 0.101(6) Uani 1 1 d . . . H62A H -0.1862 0.6503 0.1072 0.151 Uiso 1 1 calc R . . H62B H -0.2556 0.6078 0.0854 0.151 Uiso 1 1 calc R . . H62C H -0.2091 0.6024 0.0509 0.151 Uiso 1 1 calc R . . C63 C -0.2299(8) 0.4007(14) 0.0726(6) 0.095(5) Uani 1 1 d U . . H63A H -0.2178 0.3308 0.0888 0.143 Uiso 1 1 calc R . . H63B H -0.2219 0.4015 0.0393 0.143 Uiso 1 1 calc R . . H63C H -0.2740 0.4128 0.0683 0.143 Uiso 1 1 calc R . . C64 C -0.0885(8) 0.5665(12) 0.2385(6) 0.075(4) Uani 1 1 d U . . H64A H -0.1217 0.5111 0.2343 0.090 Uiso 1 1 calc R . . C65 C -0.1228(7) 0.6683(10) 0.2428(5) 0.065(4) Uani 1 1 d . . . H65A H -0.1562 0.6793 0.2115 0.097 Uiso 1 1 calc R . . H65B H -0.0942 0.7293 0.2482 0.097 Uiso 1 1 calc R . . H65C H -0.1403 0.6624 0.2716 0.097 Uiso 1 1 calc R . . C66 C -0.0414(7) 0.5257(12) 0.2818(6) 0.076(5) Uani 1 1 d . . . H66A H -0.0288 0.4538 0.2741 0.113 Uiso 1 1 calc R . . H66B H -0.0580 0.5219 0.3112 0.113 Uiso 1 1 calc R . . H66C H -0.0056 0.5739 0.2896 0.113 Uiso 1 1 calc R . . C71 C 0.2867(7) -0.0476(10) 0.0232(5) 0.055(7) Uiso 0.50 1 d PGD A 1 C72 C 0.2377(7) -0.0286(12) -0.0213(6) 0.067(8) Uiso 0.50 1 d PGD A 1 H72 H 0.2047 -0.0787 -0.0316 0.080 Uiso 0.50 1 calc PR A 1 C73 C 0.2378(7) 0.0655(13) -0.0506(6) 0.059(8) Uiso 0.50 1 d PGD A 1 H73 H 0.2050 0.0782 -0.0804 0.071 Uiso 0.50 1 calc PR A 1 C74 C 0.2870(7) 0.1404(10) -0.0352(5) 0.046(6) Uiso 0.50 1 d PGD A 1 H74 H 0.2871 0.2033 -0.0548 0.055 Uiso 0.50 1 calc PR A 1 C75 C 0.3360(7) 0.1213(11) 0.0093(6) 0.036(6) Uiso 0.50 1 d PGD A 1 H75 H 0.3690 0.1715 0.0195 0.043 Uiso 0.50 1 calc PR A 1 C76 C 0.3359(6) 0.0273(11) 0.0385(5) 0.056(8) Uiso 0.50 1 d PGD A 1 H76 H 0.3687 0.0146 0.0683 0.067 Uiso 0.50 1 calc PR A 1 C77 C 0.2865(12) -0.1518(13) 0.0556(8) 0.111(13) Uiso 0.50 1 d PD A 1 H77A H 0.2724 -0.1337 0.0852 0.166 Uiso 0.50 1 calc PR A 1 H77B H 0.3284 -0.1814 0.0669 0.166 Uiso 0.50 1 calc PR A 1 H77C H 0.2586 -0.2052 0.0348 0.166 Uiso 0.50 1 calc PR A 1 C71' C 0.3136(7) 0.0320(12) 0.0216(6) 0.095(12) Uiso 0.50 1 d PGD B 2 C72' C 0.3119(8) -0.0671(13) 0.0468(6) 0.052(7) Uiso 0.50 1 d PGD B 2 H72' H 0.3441 -0.0851 0.0762 0.063 Uiso 0.50 1 calc PR B 2 C73' C 0.2620(10) -0.1393(13) 0.0278(8) 0.079(10) Uiso 0.50 1 d PGD B 2 H73' H 0.2608 -0.2057 0.0446 0.094 Uiso 0.50 1 calc PR B 2 C74' C 0.2139(8) -0.1124(16) -0.0162(8) 0.087(10) Uiso 0.50 1 d PGD B 2 H74' H 0.1805 -0.1608 -0.0289 0.105 Uiso 0.50 1 calc PR B 2 C75' C 0.2156(8) -0.0133(18) -0.0413(7) 0.088(11) Uiso 0.50 1 d PGD B 2 H75' H 0.1834 0.0047 -0.0708 0.106 Uiso 0.50 1 calc PR B 2 C76' C 0.2655(9) 0.0589(14) -0.0224(7) 0.088(11) Uiso 0.50 1 d PGD B 2 H76' H 0.2667 0.1253 -0.0392 0.106 Uiso 0.50 1 calc PR B 2 C77' C 0.3689(10) 0.1121(18) 0.0426(10) 0.110(13) Uiso 0.50 1 d PD B 2 H77D H 0.3980 0.0810 0.0727 0.164 Uiso 0.50 1 calc PR B 2 H77E H 0.3530 0.1803 0.0517 0.164 Uiso 0.50 1 calc PR B 2 H77F H 0.3901 0.1248 0.0164 0.164 Uiso 0.50 1 calc PR B 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 W1 0.0210(2) 0.0174(2) 0.0240(2) 0.00286(19) 0.00813(17) -0.00152(18) W2 0.0368(3) 0.0307(3) 0.0327(3) 0.0011(2) 0.0091(2) -0.0092(2) Sn1 0.0224(4) 0.0237(4) 0.0270(4) 0.0041(3) 0.0101(3) -0.0018(3) Sn2 0.0217(4) 0.0158(3) 0.0292(4) 0.0028(3) 0.0113(3) -0.0020(3) P1 0.0203(14) 0.0300(16) 0.0361(16) 0.0021(13) 0.0126(12) 0.0013(12) P2 0.0191(14) 0.0246(15) 0.0316(16) 0.0048(12) 0.0100(12) 0.0004(12) P3 0.0169(13) 0.0198(13) 0.0354(16) -0.0018(12) 0.0112(12) 0.0003(11) P4 0.0250(15) 0.0279(15) 0.0415(17) 0.0050(14) 0.0202(13) 0.0071(13) O1 0.025(4) 0.026(4) 0.035(4) 0.004(3) 0.014(3) 0.005(3) O1' 0.025(4) 0.038(4) 0.039(4) -0.006(4) 0.011(4) 0.000(3) O1" 0.027(4) 0.027(4) 0.043(5) -0.005(3) 0.012(4) -0.001(3) O2 0.029(4) 0.034(4) 0.027(4) 0.003(3) 0.015(3) -0.003(3) O2' 0.028(4) 0.033(4) 0.028(4) 0.004(3) 0.007(3) 0.002(3) O2" 0.039(5) 0.022(4) 0.052(5) 0.000(3) 0.023(4) -0.007(3) O3 0.024(4) 0.012(3) 0.038(4) 0.008(3) 0.011(3) 0.005(3) O3' 0.015(4) 0.031(4) 0.038(4) -0.001(3) 0.010(3) 0.000(3) O3" 0.021(4) 0.033(4) 0.043(4) -0.009(4) 0.012(3) -0.006(3) O4 0.025(4) 0.023(4) 0.043(4) 0.008(3) 0.020(3) 0.004(3) O4' 0.097(7) 0.025(5) 0.084(6) 0.014(4) 0.076(6) 0.019(4) O4" 0.020(4) 0.081(6) 0.056(5) 0.011(5) 0.013(4) 0.005(4) C1 0.009(5) 0.014(5) 0.040(6) -0.001(5) 0.013(5) 0.002(4) C2 0.031(6) 0.015(5) 0.039(6) -0.004(5) 0.017(5) -0.004(5) C3 0.026(6) 0.034(7) 0.043(7) 0.000(6) 0.012(5) -0.007(5) C4 0.025(6) 0.029(6) 0.037(6) 0.003(5) 0.015(5) -0.004(5) C5 0.029(6) 0.032(6) 0.034(6) 0.013(5) 0.009(5) -0.006(5) C6 0.019(5) 0.027(6) 0.026(6) -0.001(5) 0.011(5) -0.008(5) C7 0.031(7) 0.054(8) 0.037(7) 0.026(6) 0.016(6) 0.003(6) C8 0.123(15) 0.121(15) 0.049(9) 0.015(9) 0.030(10) -0.073(12) C9 0.100(13) 0.073(11) 0.075(11) 0.026(9) 0.017(10) -0.045(10) C10 0.103(15) 0.135(17) 0.19(2) 0.111(16) 0.089(15) 0.015(13) O11 0.079(7) 0.025(5) 0.072(6) 0.000(4) 0.011(5) -0.040(5) C11 0.022(6) 0.064(9) 0.032(7) 0.022(6) 0.008(5) 0.000(6) O12 0.040(5) 0.044(5) 0.059(6) 0.002(4) 0.019(4) 0.020(4) C12 0.039(7) 0.023(6) 0.021(5) 0.003(5) 0.011(5) -0.003(5) O13 0.068(6) 0.060(6) 0.039(5) 0.011(4) 0.016(5) -0.011(5) C13 0.007(5) 0.033(6) 0.020(5) -0.003(5) 0.003(4) 0.000(4) O14 0.024(4) 0.055(5) 0.056(5) 0.006(4) 0.016(4) 0.006(4) C14 0.026(6) 0.037(7) 0.026(6) 0.005(5) 0.012(5) -0.008(5) O16 0.042(5) 0.028(4) 0.029(4) -0.003(3) 0.015(4) -0.006(3) O17 0.028(4) 0.044(5) 0.034(4) 0.007(4) 0.013(4) -0.008(3) O18 0.086(7) 0.052(6) 0.050(5) -0.014(4) 0.032(5) -0.020(5) O19 0.038(5) 0.065(6) 0.080(7) 0.015(5) 0.005(5) -0.006(5) C21 0.034(7) 0.045(8) 0.045(7) -0.013(6) 0.012(6) -0.015(6) C22 0.071(11) 0.058(10) 0.088(11) -0.005(8) 0.032(9) -0.005(8) C23 0.066(10) 0.094(12) 0.046(9) -0.019(8) -0.004(8) -0.025(9) C24 0.021(6) 0.047(7) 0.059(8) 0.003(7) 0.011(6) 0.001(5) C25 0.057(9) 0.063(9) 0.044(8) -0.009(7) 0.014(7) -0.011(7) C26 0.052(9) 0.037(8) 0.077(10) 0.003(7) 0.002(8) -0.013(6) C31 0.029(6) 0.035(7) 0.033(6) -0.005(5) 0.010(5) -0.008(5) C32 0.034(7) 0.062(9) 0.091(11) -0.036(8) 0.022(7) -0.008(7) C33 0.062(9) 0.053(9) 0.076(10) -0.010(7) 0.033(8) 0.004(7) C34 0.025(6) 0.051(8) 0.061(8) -0.004(7) 0.026(6) 0.006(6) C35 0.055(9) 0.067(9) 0.052(9) -0.010(7) 0.020(7) 0.005(7) C36 0.052(9) 0.064(9) 0.053(8) -0.005(7) 0.017(7) 0.017(7) C41 0.023(5) 0.014(5) 0.029(6) -0.002(4) 0.015(5) -0.005(4) C42 0.018(5) 0.018(5) 0.026(6) 0.004(4) 0.005(4) -0.003(4) C43 0.020(5) 0.019(5) 0.038(6) 0.002(5) 0.015(5) 0.003(4) C44 0.028(6) 0.023(6) 0.022(5) 0.000(4) 0.009(5) -0.012(5) C45 0.021(6) 0.032(6) 0.023(5) 0.001(5) 0.000(5) 0.005(5) C46 0.013(5) 0.020(5) 0.025(5) -0.006(4) 0.010(4) -0.003(4) C47 0.045(7) 0.031(6) 0.034(7) 0.016(5) 0.015(6) 0.003(5) C48 0.114(9) 0.060(7) 0.070(8) 0.020(6) 0.043(7) -0.018(7) C49 0.060(10) 0.050(9) 0.096(12) 0.014(8) 0.022(9) -0.022(7) C50 0.073(10) 0.028(7) 0.084(10) 0.029(7) 0.040(8) 0.016(7) C51 0.028(6) 0.021(6) 0.033(6) -0.011(5) 0.008(5) -0.001(5) C52 0.051(8) 0.038(7) 0.050(8) -0.014(6) 0.014(7) -0.011(6) C53 0.036(7) 0.043(7) 0.042(7) 0.006(6) 0.014(6) -0.007(6) C54 0.021(6) 0.045(7) 0.046(7) -0.016(6) 0.015(5) -0.004(5) C55 0.049(8) 0.086(11) 0.039(7) 0.000(7) 0.013(6) 0.010(8) C56 0.085(11) 0.039(8) 0.062(9) -0.016(7) 0.031(8) -0.019(7) C61 0.044(8) 0.094(12) 0.061(9) 0.020(9) 0.013(7) -0.001(8) C62 0.057(11) 0.118(16) 0.125(16) 0.020(13) 0.022(11) 0.029(11) C63 0.083(9) 0.099(9) 0.097(9) 0.023(8) 0.013(7) -0.019(7) C64 0.096(9) 0.059(7) 0.066(8) -0.009(6) 0.018(7) 0.028(7) C65 0.084(11) 0.043(8) 0.076(10) -0.002(7) 0.038(9) 0.020(8) C66 0.060(10) 0.073(11) 0.075(11) -0.001(9) -0.012(8) 0.019(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag W1 C13 1.941(10) . ? W1 C11 1.964(13) . ? W1 C12 2.013(11) . ? W1 C14 2.026(11) . ? W1 Sn1 2.7022(8) . ? W1 Sn2 2.7218(8) . ? W2 O18 1.720(8) . ? W2 O19 1.747(8) . ? W2 O17 1.804(6) . ? W2 O16 1.837(7) . ? Sn1 O16 2.052(6) . ? Sn1 C1 2.188(9) . ? Sn1 O2 2.321(7) . ? Sn1 O1 2.372(6) . ? Sn2 O17 2.058(7) . ? Sn2 C41 2.184(9) . ? Sn2 O3 2.331(6) . ? Sn2 O4 2.361(6) . ? P1 O1 1.491(7) . ? P1 O1" 1.559(7) . ? P1 O1' 1.566(7) . ? P1 C2 1.777(10) . ? P2 O2 1.488(7) . ? P2 O2" 1.536(7) . ? P2 O2' 1.570(7) . ? P2 C6 1.799(9) . ? P3 O3 1.487(7) . ? P3 O3' 1.558(7) . ? P3 O3" 1.561(7) . ? P3 C42 1.787(10) . ? P4 O4 1.479(7) . ? P4 O4' 1.555(8) . ? P4 O4" 1.576(8) . ? P4 C46 1.772(9) . ? O1' C21 1.505(12) . ? O1" C24 1.485(13) . ? O2' C31 1.499(12) . ? O2" C34 1.471(12) . ? O3' C51 1.478(11) . ? O3" C54 1.467(12) . ? O4' C64 1.427(16) . ? O4" C61 1.484(15) . ? C1 C6 1.355(13) . ? C1 C2 1.395(13) . ? C2 C3 1.381(14) . ? C3 C4 1.381(14) . ? C4 C5 1.391(14) . ? C4 C7 1.541(13) . ? C5 C6 1.428(13) . ? C7 C10 1.450(19) . ? C7 C9 1.498(16) . ? C7 C8 1.556(19) . ? O11 C11 1.171(13) . ? O12 C12 1.164(12) . ? O13 C13 1.175(11) . ? O14 C14 1.156(12) . ? C21 C22 1.454(16) . ? C21 C23 1.464(16) . ? C24 C25 1.493(15) . ? C24 C26 1.505(15) . ? C31 C32 1.442(14) . ? C31 C33 1.489(15) . ? C34 C35 1.492(15) . ? C34 C36 1.500(16) . ? C41 C46 1.376(12) . ? C41 C42 1.394(13) . ? C42 C43 1.408(12) . ? C43 C44 1.382(13) . ? C44 C45 1.388(13) . ? C44 C47 1.542(13) . ? C45 C46 1.390(13) . ? C47 C48 1.492(16) . ? C47 C50 1.537(15) . ? C47 C49 1.544(16) . ? C51 C53 1.479(13) . ? C51 C52 1.515(14) . ? C54 C55 1.486(15) . ? C54 C56 1.492(15) . ? C61 C62 1.438(19) . ? C61 C63 1.48(2) . ? C64 C66 1.416(17) . ? C64 C65 1.474(16) . ? C71 C72 1.3900 . ? C71 C76 1.3900 . ? C71 C77 1.5399(10) . ? C72 C73 1.3900 . ? C73 C74 1.3900 . ? C74 C75 1.3900 . ? C75 C76 1.3900 . ? C71' C77' 1.5398(10) . ? C71' C72' 1.3900 . ? C71' C76' 1.3900 . ? C72' C73' 1.3900 . ? C73' C74' 1.3900 . ? C74' C75' 1.3900 . ? C75' C76' 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 C13 W1 C11 87.9(4) . . ? C13 W1 C12 89.8(4) . . ? C11 W1 C12 89.6(4) . . ? C13 W1 C14 92.6(4) . . ? C11 W1 C14 91.9(4) . . ? C12 W1 C14 177.2(4) . . ? C13 W1 Sn1 177.7(3) . . ? C11 W1 Sn1 92.4(3) . . ? C12 W1 Sn1 87.9(3) . . ? C14 W1 Sn1 89.6(3) . . ? C13 W1 Sn2 89.8(3) . . ? C11 W1 Sn2 177.6(3) . . ? C12 W1 Sn2 89.7(3) . . ? C14 W1 Sn2 88.9(3) . . ? Sn1 W1 Sn2 89.86(2) . . ? O18 W2 O19 107.3(4) . . ? O18 W2 O17 110.8(4) . . ? O19 W2 O17 109.8(4) . . ? O18 W2 O16 110.7(3) . . ? O19 W2 O16 110.5(4) . . ? O17 W2 O16 107.7(3) . . ? O16 Sn1 C1 92.9(3) . . ? O16 Sn1 O2 87.4(3) . . ? C1 Sn1 O2 78.1(3) . . ? O16 Sn1 O1 87.4(3) . . ? C1 Sn1 O1 77.3(3) . . ? O2 Sn1 O1 154.6(2) . . ? O16 Sn1 W1 121.63(18) . . ? C1 Sn1 W1 145.5(2) . . ? O2 Sn1 W1 101.85(16) . . ? O1 Sn1 W1 102.05(16) . . ? O17 Sn2 C41 95.7(3) . . ? O17 Sn2 O3 87.0(2) . . ? C41 Sn2 O3 78.5(3) . . ? O17 Sn2 O4 88.0(3) . . ? C41 Sn2 O4 77.3(3) . . ? O3 Sn2 O4 154.7(2) . . ? O17 Sn2 W1 122.93(19) . . ? C41 Sn2 W1 141.4(2) . . ? O3 Sn2 W1 102.20(15) . . ? O4 Sn2 W1 101.26(16) . . ? O1 P1 O1" 116.5(4) . . ? O1 P1 O1' 114.0(4) . . ? O1" P1 O1' 99.9(4) . . ? O1 P1 C2 107.9(4) . . ? O1" P1 C2 108.8(4) . . ? O1' P1 C2 109.5(4) . . ? O2 P2 O2" 117.1(4) . . ? O2 P2 O2' 112.7(4) . . ? O2" P2 O2' 102.8(4) . . ? O2 P2 C6 106.6(4) . . ? O2" P2 C6 106.8(4) . . ? O2' P2 C6 110.7(4) . . ? O3 P3 O3' 116.7(4) . . ? O3 P3 O3" 115.8(4) . . ? O3' P3 O3" 97.5(4) . . ? O3 P3 C42 106.5(4) . . ? O3' P3 C42 109.5(4) . . ? O3" P3 C42 110.5(4) . . ? O4 P4 O4' 114.4(4) . . ? O4 P4 O4" 115.2(4) . . ? O4' P4 O4" 105.4(5) . . ? O4 P4 C46 109.1(4) . . ? O4' P4 C46 108.9(4) . . ? O4" P4 C46 103.1(4) . . ? P1 O1 Sn1 117.1(4) . . ? C21 O1' P1 117.6(6) . . ? C24 O1" P1 116.7(6) . . ? P2 O2 Sn1 117.9(4) . . ? C31 O2' P2 122.1(6) . . ? C34 O2" P2 122.8(7) . . ? P3 O3 Sn2 118.0(3) . . ? C51 O3' P3 121.5(6) . . ? C54 O3" P3 121.9(6) . . ? P4 O4 Sn2 116.3(4) . . ? C64 O4' P4 128.3(8) . . ? C61 O4" P4 121.9(8) . . ? C6 C1 C2 118.0(9) . . ? C6 C1 Sn1 120.7(7) . . ? C2 C1 Sn1 121.3(7) . . ? C3 C2 C1 120.3(9) . . ? C3 C2 P1 123.7(8) . . ? C1 C2 P1 115.8(7) . . ? C4 C3 C2 122.7(10) . . ? C3 C4 C5 117.3(9) . . ? C3 C4 C7 120.1(9) . . ? C5 C4 C7 122.5(9) . . ? C4 C5 C6 119.4(10) . . ? C1 C6 C5 122.1(9) . . ? C1 C6 P2 116.6(7) . . ? C5 C6 P2 121.3(8) . . ? C10 C7 C9 109.3(13) . . ? C10 C7 C4 113.0(10) . . ? C9 C7 C4 110.1(9) . . ? C10 C7 C8 107.6(13) . . ? C9 C7 C8 108.5(11) . . ? C4 C7 C8 108.3(10) . . ? O11 C11 W1 176.5(10) . . ? O12 C12 W1 177.9(9) . . ? O13 C13 W1 178.4(9) . . ? O14 C14 W1 178.2(10) . . ? W2 O16 Sn1 137.6(4) . . ? W2 O17 Sn2 136.8(4) . . ? C22 C21 C23 116.5(11) . . ? C22 C21 O1' 108.2(10) . . ? C23 C21 O1' 107.6(9) . . ? O1" C24 C25 108.6(9) . . ? O1" C24 C26 106.2(9) . . ? C25 C24 C26 115.2(10) . . ? C32 C31 C33 114.2(10) . . ? C32 C31 O2' 105.5(9) . . ? C33 C31 O2' 108.4(9) . . ? O2" C34 C35 109.1(9) . . ? O2" C34 C36 107.6(9) . . ? C35 C34 C36 115.5(10) . . ? C46 C41 C42 118.7(8) . . ? C46 C41 Sn2 122.1(7) . . ? C42 C41 Sn2 119.2(7) . . ? C41 C42 C43 119.6(9) . . ? C41 C42 P3 117.5(7) . . ? C43 C42 P3 122.9(7) . . ? C44 C43 C42 121.4(9) . . ? C43 C44 C45 118.1(9) . . ? C43 C44 C47 119.2(9) . . ? C45 C44 C47 122.7(9) . . ? C46 C45 C44 120.9(9) . . ? C41 C46 C45 121.3(8) . . ? C41 C46 P4 115.0(7) . . ? C45 C46 P4 123.6(7) . . ? C48 C47 C50 109.5(10) . . ? C48 C47 C44 108.3(9) . . ? C50 C47 C44 112.3(9) . . ? C48 C47 C49 110.4(11) . . ? C50 C47 C49 105.8(10) . . ? C44 C47 C49 110.6(9) . . ? O3' C51 C53 110.0(8) . . ? O3' C51 C52 104.6(8) . . ? C53 C51 C52 113.9(9) . . ? O3" C54 C55 106.0(9) . . ? O3" C54 C56 108.7(9) . . ? C55 C54 C56 113.1(10) . . ? C62 C61 O4" 108.1(12) . . ? C62 C61 C63 112.3(13) . . ? O4" C61 C63 106.3(13) . . ? C66 C64 O4' 118.3(13) . . ? C66 C64 C65 120.3(13) . . ? O4' C64 C65 109.1(11) . . ? C72 C71 C76 120.0 . . ? C72 C71 C77 120.0 . . ? C76 C71 C77 120.0 . . ? C71 C72 C73 120.0 . . ? C74 C73 C72 120.0 . . ? C73 C74 C75 120.0 . . ? C76 C75 C74 120.0 . . ? C75 C76 C71 120.0 . . ? C77' C71' C72' 120.0 . . ? C77' C71' C76' 120.0 . . ? C72' C71' C76' 120.0 . . ? C71' C72' C73' 120.0 . . ? C74' C73' C72' 120.0 . . ? C73' C74' C75' 120.0 . . ? C74' C75' C76' 120.0 . . ? C75' C76' C71' 120.0 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C13 W1 Sn1 O16 79(7) . . . . ? C11 W1 Sn1 O16 177.5(4) . . . . ? C12 W1 Sn1 O16 87.9(4) . . . . ? C14 W1 Sn1 O16 -90.7(4) . . . . ? Sn2 W1 Sn1 O16 -1.8(2) . . . . ? C13 W1 Sn1 C1 -101(7) . . . . ? C11 W1 Sn1 C1 -3.0(5) . . . . ? C12 W1 Sn1 C1 -92.5(5) . . . . ? C14 W1 Sn1 C1 88.9(5) . . . . ? Sn2 W1 Sn1 C1 177.8(4) . . . . ? C13 W1 Sn1 O2 -15(7) . . . . ? C11 W1 Sn1 O2 83.1(4) . . . . ? C12 W1 Sn1 O2 -6.4(3) . . . . ? C14 W1 Sn1 O2 175.0(3) . . . . ? Sn2 W1 Sn1 O2 -96.12(17) . . . . ? C13 W1 Sn1 O1 174(7) . . . . ? C11 W1 Sn1 O1 -88.1(4) . . . . ? C12 W1 Sn1 O1 -177.6(3) . . . . ? C14 W1 Sn1 O1 3.7(3) . . . . ? Sn2 W1 Sn1 O1 92.66(16) . . . . ? C13 W1 Sn2 O17 -169.6(4) . . . . ? C11 W1 Sn2 O17 -154(8) . . . . ? C12 W1 Sn2 O17 -79.8(4) . . . . ? C14 W1 Sn2 O17 97.8(4) . . . . ? Sn1 W1 Sn2 O17 8.2(2) . . . . ? C13 W1 Sn2 C41 11.7(5) . . . . ? C11 W1 Sn2 C41 28(8) . . . . ? C12 W1 Sn2 C41 101.5(5) . . . . ? C14 W1 Sn2 C41 -81.0(5) . . . . ? Sn1 W1 Sn2 C41 -170.6(4) . . . . ? C13 W1 Sn2 O3 -75.2(3) . . . . ? C11 W1 Sn2 O3 -59(8) . . . . ? C12 W1 Sn2 O3 14.7(3) . . . . ? C14 W1 Sn2 O3 -167.8(3) . . . . ? Sn1 W1 Sn2 O3 102.59(16) . . . . ? C13 W1 Sn2 O4 95.4(3) . . . . ? C11 W1 Sn2 O4 111(8) . . . . ? C12 W1 Sn2 O4 -174.8(3) . . . . ? C14 W1 Sn2 O4 2.8(3) . . . . ? Sn1 W1 Sn2 O4 -86.84(17) . . . . ? O1" P1 O1 Sn1 -128.1(4) . . . . ? O1' P1 O1 Sn1 116.3(4) . . . . ? C2 P1 O1 Sn1 -5.5(5) . . . . ? O16 Sn1 O1 P1 -91.5(4) . . . . ? C1 Sn1 O1 P1 2.0(4) . . . . ? O2 Sn1 O1 P1 -13.0(8) . . . . ? W1 Sn1 O1 P1 146.7(4) . . . . ? O1 P1 O1' C21 -58.0(8) . . . . ? O1" P1 O1' C21 177.0(7) . . . . ? C2 P1 O1' C21 62.9(8) . . . . ? O1 P1 O1" C24 58.6(8) . . . . ? O1' P1 O1" C24 -178.2(7) . . . . ? C2 P1 O1" C24 -63.5(8) . . . . ? O2" P2 O2 Sn1 120.6(4) . . . . ? O2' P2 O2 Sn1 -120.4(4) . . . . ? C6 P2 O2 Sn1 1.2(5) . . . . ? O16 Sn1 O2 P2 93.7(4) . . . . ? C1 Sn1 O2 P2 0.3(4) . . . . ? O1 Sn1 O2 P2 15.2(8) . . . . ? W1 Sn1 O2 P2 -144.4(4) . . . . ? O2 P2 O2' C31 28.8(8) . . . . ? O2" P2 O2' C31 155.8(7) . . . . ? C6 P2 O2' C31 -90.5(8) . . . . ? O2 P2 O2" C34 51.5(9) . . . . ? O2' P2 O2" C34 -72.6(8) . . . . ? C6 P2 O2" C34 170.8(8) . . . . ? O3' P3 O3 Sn2 124.2(4) . . . . ? O3" P3 O3 Sn2 -121.9(4) . . . . ? C42 P3 O3 Sn2 1.5(5) . . . . ? O17 Sn2 O3 P3 -99.4(4) . . . . ? C41 Sn2 O3 P3 -3.0(4) . . . . ? O4 Sn2 O3 P3 -20.4(8) . . . . ? W1 Sn2 O3 P3 137.5(4) . . . . ? O3 P3 O3' C51 -62.6(8) . . . . ? O3" P3 O3' C51 173.5(7) . . . . ? C42 P3 O3' C51 58.5(8) . . . . ? O3 P3 O3" C54 51.9(8) . . . . ? O3' P3 O3" C54 176.5(7) . . . . ? C42 P3 O3" C54 -69.3(8) . . . . ? O4' P4 O4 Sn2 -124.7(5) . . . . ? O4" P4 O4 Sn2 112.9(4) . . . . ? C46 P4 O4 Sn2 -2.4(5) . . . . ? O17 Sn2 O4 P4 99.5(4) . . . . ? C41 Sn2 O4 P4 3.2(4) . . . . ? O3 Sn2 O4 P4 20.7(8) . . . . ? W1 Sn2 O4 P4 -137.3(4) . . . . ? O4 P4 O4' C64 -10.2(13) . . . . ? O4" P4 O4' C64 117.3(12) . . . . ? C46 P4 O4' C64 -132.7(12) . . . . ? O4 P4 O4" C61 74.3(11) . . . . ? O4' P4 O4" C61 -52.9(10) . . . . ? C46 P4 O4" C61 -167.0(10) . . . . ? O16 Sn1 C1 C6 -89.1(8) . . . . ? O2 Sn1 C1 C6 -2.3(7) . . . . ? O1 Sn1 C1 C6 -175.8(8) . . . . ? W1 Sn1 C1 C6 91.2(8) . . . . ? O16 Sn1 C1 C2 90.2(8) . . . . ? O2 Sn1 C1 C2 176.9(8) . . . . ? O1 Sn1 C1 C2 3.5(7) . . . . ? W1 Sn1 C1 C2 -89.5(8) . . . . ? C6 C1 C2 C3 -3.2(15) . . . . ? Sn1 C1 C2 C3 177.5(7) . . . . ? C6 C1 C2 P1 171.8(7) . . . . ? Sn1 C1 C2 P1 -7.5(11) . . . . ? O1 P1 C2 C3 -176.9(8) . . . . ? O1" P1 C2 C3 -49.6(10) . . . . ? O1' P1 C2 C3 58.6(10) . . . . ? O1 P1 C2 C1 8.3(9) . . . . ? O1" P1 C2 C1 135.5(7) . . . . ? O1' P1 C2 C1 -116.2(8) . . . . ? C1 C2 C3 C4 -0.6(16) . . . . ? P1 C2 C3 C4 -175.2(8) . . . . ? C2 C3 C4 C5 4.0(16) . . . . ? C2 C3 C4 C7 -176.5(10) . . . . ? C3 C4 C5 C6 -3.5(15) . . . . ? C7 C4 C5 C6 177.0(10) . . . . ? C2 C1 C6 C5 3.6(14) . . . . ? Sn1 C1 C6 C5 -177.0(7) . . . . ? C2 C1 C6 P2 -175.6(7) . . . . ? Sn1 C1 C6 P2 3.7(11) . . . . ? C4 C5 C6 C1 -0.3(15) . . . . ? C4 C5 C6 P2 179.0(8) . . . . ? O2 P2 C6 C1 -3.1(9) . . . . ? O2" P2 C6 C1 -129.0(8) . . . . ? O2' P2 C6 C1 119.8(8) . . . . ? O2 P2 C6 C5 177.7(8) . . . . ? O2" P2 C6 C5 51.7(9) . . . . ? O2' P2 C6 C5 -59.5(9) . . . . ? C3 C4 C7 C10 179.4(14) . . . . ? C5 C4 C7 C10 -1.1(18) . . . . ? C3 C4 C7 C9 57.0(15) . . . . ? C5 C4 C7 C9 -123.6(12) . . . . ? C3 C4 C7 C8 -61.5(14) . . . . ? C5 C4 C7 C8 118.0(12) . . . . ? C13 W1 C11 O11 26(17) . . . . ? C12 W1 C11 O11 -63(17) . . . . ? C14 W1 C11 O11 119(17) . . . . ? Sn1 W1 C11 O11 -151(17) . . . . ? Sn2 W1 C11 O11 11(24) . . . . ? C13 W1 C12 O12 -58(26) . . . . ? C11 W1 C12 O12 30(26) . . . . ? C14 W1 C12 O12 152(23) . . . . ? Sn1 W1 C12 O12 123(26) . . . . ? Sn2 W1 C12 O12 -147(26) . . . . ? C11 W1 C13 O13 -85(35) . . . . ? C12 W1 C13 O13 4(35) . . . . ? C14 W1 C13 O13 -177(100) . . . . ? Sn1 W1 C13 O13 13(41) . . . . ? Sn2 W1 C13 O13 94(35) . . . . ? C13 W1 C14 O14 58(32) . . . . ? C11 W1 C14 O14 -30(32) . . . . ? C12 W1 C14 O14 -152(28) . . . . ? Sn1 W1 C14 O14 -122(32) . . . . ? Sn2 W1 C14 O14 148(32) . . . . ? O18 W2 O16 Sn1 145.5(6) . . . . ? O19 W2 O16 Sn1 -95.7(6) . . . . ? O17 W2 O16 Sn1 24.2(6) . . . . ? C1 Sn1 O16 W2 163.4(6) . . . . ? O2 Sn1 O16 W2 85.5(6) . . . . ? O1 Sn1 O16 W2 -119.4(6) . . . . ? W1 Sn1 O16 W2 -16.8(6) . . . . ? O18 W2 O17 Sn2 -134.9(6) . . . . ? O19 W2 O17 Sn2 106.8(6) . . . . ? O16 W2 O17 Sn2 -13.6(6) . . . . ? C41 Sn2 O17 W2 177.8(6) . . . . ? O3 Sn2 O17 W2 -104.0(6) . . . . ? O4 Sn2 O17 W2 100.8(6) . . . . ? W1 Sn2 O17 W2 -1.4(7) . . . . ? P1 O1' C21 C22 109.8(10) . . . . ? P1 O1' C21 C23 -123.5(9) . . . . ? P1 O1" C24 C25 -102.9(9) . . . . ? P1 O1" C24 C26 132.7(8) . . . . ? P2 O2' C31 C32 -146.0(8) . . . . ? P2 O2' C31 C33 91.3(10) . . . . ? P2 O2" C34 C35 -111.2(10) . . . . ? P2 O2" C34 C36 122.8(9) . . . . ? O17 Sn2 C41 C46 -90.4(8) . . . . ? O3 Sn2 C41 C46 -176.2(8) . . . . ? O4 Sn2 C41 C46 -3.7(7) . . . . ? W1 Sn2 C41 C46 88.6(8) . . . . ? O17 Sn2 C41 C42 90.0(7) . . . . ? O3 Sn2 C41 C42 4.2(7) . . . . ? O4 Sn2 C41 C42 176.6(8) . . . . ? W1 Sn2 C41 C42 -91.1(8) . . . . ? C46 C41 C42 C43 -1.9(14) . . . . ? Sn2 C41 C42 C43 177.8(7) . . . . ? C46 C41 C42 P3 175.7(7) . . . . ? Sn2 C41 C42 P3 -4.7(10) . . . . ? O3 P3 C42 C41 1.9(9) . . . . ? O3' P3 C42 C41 -125.2(7) . . . . ? O3" P3 C42 C41 128.5(7) . . . . ? O3 P3 C42 C43 179.3(8) . . . . ? O3' P3 C42 C43 52.3(9) . . . . ? O3" P3 C42 C43 -54.1(9) . . . . ? C41 C42 C43 C44 0.9(15) . . . . ? P3 C42 C43 C44 -176.5(7) . . . . ? C42 C43 C44 C45 1.1(14) . . . . ? C42 C43 C44 C47 -179.6(9) . . . . ? C43 C44 C45 C46 -2.1(14) . . . . ? C47 C44 C45 C46 178.6(9) . . . . ? C42 C41 C46 C45 0.9(14) . . . . ? Sn2 C41 C46 C45 -178.8(7) . . . . ? C42 C41 C46 P4 -176.9(7) . . . . ? Sn2 C41 C46 P4 3.4(10) . . . . ? C44 C45 C46 C41 1.2(14) . . . . ? C44 C45 C46 P4 178.7(7) . . . . ? O4 P4 C46 C41 -0.4(8) . . . . ? O4' P4 C46 C41 125.2(7) . . . . ? O4" P4 C46 C41 -123.3(8) . . . . ? O4 P4 C46 C45 -178.1(8) . . . . ? O4' P4 C46 C45 -52.5(9) . . . . ? O4" P4 C46 C45 59.0(9) . . . . ? C43 C44 C47 C48 65.3(13) . . . . ? C45 C44 C47 C48 -115.3(12) . . . . ? C43 C44 C47 C50 -173.7(10) . . . . ? C45 C44 C47 C50 5.6(14) . . . . ? C43 C44 C47 C49 -55.8(13) . . . . ? C45 C44 C47 C49 123.5(11) . . . . ? P3 O3' C51 C53 98.2(9) . . . . ? P3 O3' C51 C52 -139.2(7) . . . . ? P3 O3" C54 C55 140.1(8) . . . . ? P3 O3" C54 C56 -98.1(9) . . . . ? P4 O4" C61 C62 113.2(12) . . . . ? P4 O4" C61 C63 -126.0(11) . . . . ? P4 O4' C64 C66 67.7(19) . . . . ? P4 O4' C64 C65 -149.9(10) . . . . ? C76 C71 C72 C73 0.0 . . . . ? C77 C71 C72 C73 180.0 . . . . ? C71 C72 C73 C74 0.0 . . . . ? C72 C73 C74 C75 0.0 . . . . ? C73 C74 C75 C76 0.0 . . . . ? C74 C75 C76 C71 0.0 . . . . ? C72 C71 C76 C75 0.0 . . . . ? C77 C71 C76 C75 180.0 . . . . ? C77' C71' C72' C73' 180.0 . . . . ? C76' C71' C72' C73' 0.0 . . . . ? C71' C72' C73' C74' 0.0 . . . . ? C72' C73' C74' C75' 0.0 . . . . ? C73' C74' C75' C76' 0.0 . . . . ? C74' C75' C76' C71' 0.0 . . . . ? C77' C71' C76' C75' 180.0 . . . . ? C72' C71' C76' C75' 0.0 . . . . ? _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 4.026 _refine_diff_density_min -2.117 _refine_diff_density_rms 0.187 # Attachment '- compound2_revised2.cif' data_ox0097 #TrackingRef 'C1DT10321K_ccdc_802872_802876_cif.txt' _database_code_depnum_ccdc_archive 'CCDC 802875' #TrackingRef '- compound2_revised2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C27 H39 F O11 P2 Sn W' _chemical_formula_sum 'C27 H39 F O11 P2 Sn W' _chemical_formula_weight 923.06 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 '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' W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall -P1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.6089(3) _cell_length_b 11.7686(5) _cell_length_c 15.4337(6) _cell_angle_alpha 78.061(3) _cell_angle_beta 72.319(3) _cell_angle_gamma 79.707(3) _cell_volume 1782.26(11) _cell_formula_units_Z 2 _cell_measurement_temperature 173(1) _cell_measurement_reflns_used 10350 _cell_measurement_theta_min 2.03 _cell_measurement_theta_max 29.06 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.720 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 904 _exptl_absorpt_coefficient_mu 4.071 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.812 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.37 (release 24-10-2008 CrysAlis171 .NET) (compiled Oct 24 2008,09:44:38) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(1) _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 'Xcalibur2 CCD diffractometer' _diffrn_measurement_method ; 464 frames via \w-rotation (\D\w = 1\%) and two times 5 s per frame (10 sets at different \k-angles) ; _diffrn_detector_area_resol_mean 16.0560 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 14282 _diffrn_reflns_av_R_equivalents 0.0310 _diffrn_reflns_av_sigmaI/netI 0.0418 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.03 _diffrn_reflns_theta_max 25.50 _reflns_number_total 6606 _reflns_number_gt 5508 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlis CCD (Oxford Diffraction, 2008) ; _computing_cell_refinement ; CrysAlis RED (Oxford Diffraction, 2008) ; _computing_data_reduction ; CrysAlis RED (Oxford Diffraction, 2008) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL-Plus (Sheldrick, 1991)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 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^)+(0.0625P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6606 _refine_ls_number_parameters 399 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0436 _refine_ls_R_factor_gt 0.0363 _refine_ls_wR_factor_ref 0.0919 _refine_ls_wR_factor_gt 0.0903 _refine_ls_goodness_of_fit_ref 0.988 _refine_ls_restrained_S_all 0.988 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group W1 W 0.15501(2) -0.164550(19) 0.348169(15) 0.01995(9) Uani 1 1 d . . . Sn1 Sn 0.38413(3) -0.27101(3) 0.24282(2) 0.01736(10) Uani 1 1 d . . . P1 P 0.46616(13) -0.55665(12) 0.28672(9) 0.0180(3) Uani 1 1 d . . . P2 P 0.65168(13) -0.14128(12) 0.19574(9) 0.0184(3) Uani 1 1 d . . . F1 F 0.4046(3) -0.2837(3) 0.1136(2) 0.0313(8) Uani 1 1 d . . . O1 O 0.3509(3) -0.4678(3) 0.2756(3) 0.0222(8) Uani 1 1 d . . . O1' O 0.4471(3) -0.6325(3) 0.3840(2) 0.0259(9) Uani 1 1 d . . . O1" O 0.5021(3) -0.6528(3) 0.2242(2) 0.0214(8) Uani 1 1 d . . . O2 O 0.5114(4) -0.1164(3) 0.1894(3) 0.0264(9) Uani 1 1 d . . . O2' O 0.6783(4) -0.0909(3) 0.2731(2) 0.0239(8) Uani 1 1 d . . . O2" O 0.7548(3) -0.0886(3) 0.1067(2) 0.0226(8) Uani 1 1 d . . . C1 C 0.5831(5) -0.3593(4) 0.2456(3) 0.0158(10) Uani 1 1 d . . . C2 C 0.6080(5) -0.4810(5) 0.2625(3) 0.0179(11) Uani 1 1 d . . . C3 C 0.7364(5) -0.5365(5) 0.2551(4) 0.0219(12) Uani 1 1 d . . . H3A H 0.7505 -0.6177 0.2678 0.026 Uiso 1 1 calc R . . C4 C 0.8456(5) -0.4734(5) 0.2292(4) 0.0192(11) Uani 1 1 d . . . C5 C 0.8206(5) -0.3532(5) 0.2127(4) 0.0219(12) Uani 1 1 d . . . H5A H 0.8914 -0.3091 0.1956 0.026 Uiso 1 1 calc R . . C6 C 0.6913(5) -0.2960(4) 0.2210(3) 0.0172(11) Uani 1 1 d . . . C7 C 0.9876(6) -0.5395(6) 0.2148(5) 0.0328(15) Uani 1 1 d . . . C8 C 0.9992(7) -0.6199(7) 0.3043(6) 0.063(2) Uani 1 1 d . . . H8A H 0.9867 -0.5735 0.3513 0.094 Uiso 1 1 calc R . . H8B H 1.0859 -0.6646 0.2942 0.094 Uiso 1 1 calc R . . H8C H 0.9322 -0.6721 0.3235 0.094 Uiso 1 1 calc R . . C9 C 1.0138(7) -0.6107(8) 0.1373(7) 0.076(3) Uani 1 1 d . . . H9A H 1.0080 -0.5588 0.0814 0.115 Uiso 1 1 calc R . . H9B H 0.9484 -0.6641 0.1536 0.115 Uiso 1 1 calc R . . H9C H 1.1012 -0.6540 0.1282 0.115 Uiso 1 1 calc R . . C10 C 1.0928(6) -0.4561(6) 0.1865(6) 0.0478(19) Uani 1 1 d . . . H10A H 1.0885 -0.4068 0.1293 0.072 Uiso 1 1 calc R . . H10B H 1.1796 -0.5004 0.1790 0.072 Uiso 1 1 calc R . . H10C H 1.0767 -0.4087 0.2333 0.072 Uiso 1 1 calc R . . O11 O 0.2558(5) 0.0857(5) 0.2724(4) 0.0631(16) Uani 1 1 d . . . C11 C 0.2221(6) -0.0060(6) 0.2989(5) 0.0333(14) Uani 1 1 d . . . O12 O 0.2903(6) -0.2048(5) 0.5118(4) 0.0636(16) Uani 1 1 d . . . C12 C 0.2436(6) -0.1891(6) 0.4526(5) 0.0374(15) Uani 1 1 d . . . O13 O 0.0423(5) -0.4083(4) 0.4287(3) 0.0533(14) Uani 1 1 d . . . C13 C 0.0862(6) -0.3206(5) 0.3991(4) 0.0283(13) Uani 1 1 d . . . O14 O 0.0319(4) -0.1413(4) 0.1806(3) 0.0396(11) Uani 1 1 d . . . C14 C 0.0760(5) -0.1488(5) 0.2404(4) 0.0256(13) Uani 1 1 d . . . O15 O -0.1124(4) -0.0443(5) 0.4656(4) 0.0526(14) Uani 1 1 d . . . C15 C -0.0123(6) -0.0852(6) 0.4236(5) 0.0359(15) Uani 1 1 d . . . C21 C 0.3222(6) -0.6259(6) 0.4578(4) 0.0415(17) Uani 1 1 d . . . H21A H 0.2439 -0.6055 0.4339 0.050 Uiso 1 1 calc R . . C22 C 0.3350(13) -0.5317(11) 0.5117(7) 0.120(5) Uani 1 1 d . . . H22A H 0.2580 -0.5256 0.5638 0.181 Uiso 1 1 calc R . . H22B H 0.3411 -0.4573 0.4718 0.181 Uiso 1 1 calc R . . H22C H 0.4137 -0.5542 0.5327 0.181 Uiso 1 1 calc R . . C23 C 0.3164(9) -0.7318(10) 0.5211(7) 0.111(5) Uani 1 1 d . . . H23A H 0.2876 -0.7890 0.4976 0.167 Uiso 1 1 calc R . . H23B H 0.2546 -0.7183 0.5791 0.167 Uiso 1 1 calc R . . H23C H 0.4033 -0.7598 0.5296 0.167 Uiso 1 1 calc R . . C24 C 0.5113(6) -0.6223(5) 0.1241(4) 0.0298(13) Uani 1 1 d . . . H24A H 0.4742 -0.5404 0.1099 0.036 Uiso 1 1 calc R . . C25 C 0.4302(6) -0.7006(7) 0.1049(4) 0.0405(17) Uani 1 1 d . . . H25A H 0.3394 -0.6874 0.1412 0.061 Uiso 1 1 calc R . . H25B H 0.4654 -0.7808 0.1205 0.061 Uiso 1 1 calc R . . H25C H 0.4338 -0.6841 0.0407 0.061 Uiso 1 1 calc R . . C26 C 0.6561(7) -0.6393(9) 0.0705(5) 0.062(3) Uani 1 1 d . . . H26A H 0.7032 -0.5851 0.0832 0.093 Uiso 1 1 calc R . . H26B H 0.6633 -0.6259 0.0057 0.093 Uiso 1 1 calc R . . H26C H 0.6941 -0.7179 0.0883 0.093 Uiso 1 1 calc R . . C31 C 0.6444(6) 0.0362(5) 0.2781(4) 0.0288(13) Uani 1 1 d . . . H31A H 0.5908 0.0733 0.2357 0.035 Uiso 1 1 calc R . . C32 C 0.5645(8) 0.0460(6) 0.3747(5) 0.052(2) Uani 1 1 d . . . H32A H 0.4809 0.0166 0.3870 0.077 Uiso 1 1 calc R . . H32B H 0.5484 0.1265 0.3827 0.077 Uiso 1 1 calc R . . H32C H 0.6127 0.0010 0.4165 0.077 Uiso 1 1 calc R . . C33 C 0.7723(7) 0.0880(6) 0.2500(5) 0.0491(19) Uani 1 1 d . . . H33A H 0.8212 0.0751 0.1886 0.074 Uiso 1 1 calc R . . H33B H 0.8244 0.0517 0.2917 0.074 Uiso 1 1 calc R . . H33C H 0.7536 0.1706 0.2514 0.074 Uiso 1 1 calc R . . C34 C 0.7473(7) -0.0948(6) 0.0146(4) 0.0359(15) Uani 1 1 d . . . H34A H 0.6938 -0.1565 0.0185 0.043 Uiso 1 1 calc R . . C35 C 0.6845(8) 0.0198(7) -0.0240(5) 0.054(2) Uani 1 1 d . . . H35A H 0.6003 0.0409 0.0185 0.082 Uiso 1 1 calc R . . H35B H 0.6706 0.0141 -0.0816 0.082 Uiso 1 1 calc R . . H35C H 0.7419 0.0785 -0.0340 0.082 Uiso 1 1 calc R . . C36 C 0.8879(8) -0.1255(7) -0.0406(5) 0.056(2) Uani 1 1 d . . . H36A H 0.9268 -0.1959 -0.0094 0.084 Uiso 1 1 calc R . . H36B H 0.9387 -0.0628 -0.0474 0.084 Uiso 1 1 calc R . . H36C H 0.8883 -0.1375 -0.1003 0.084 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 W1 0.01663(13) 0.01895(13) 0.02468(14) -0.00727(9) -0.00483(9) -0.00053(8) Sn1 0.01526(19) 0.0181(2) 0.01743(19) -0.00205(15) -0.00449(14) 0.00021(14) P1 0.0177(7) 0.0170(7) 0.0185(7) -0.0019(5) -0.0040(5) -0.0032(5) P2 0.0198(7) 0.0146(7) 0.0199(7) 0.0006(5) -0.0059(5) -0.0028(5) F1 0.0345(19) 0.042(2) 0.0198(17) -0.0099(15) -0.0097(14) -0.0012(15) O1 0.0175(18) 0.022(2) 0.028(2) -0.0004(16) -0.0085(16) -0.0055(15) O1' 0.0216(19) 0.030(2) 0.021(2) 0.0023(17) -0.0031(15) -0.0004(17) O1" 0.025(2) 0.021(2) 0.0195(19) -0.0043(16) -0.0069(16) -0.0043(16) O2 0.024(2) 0.016(2) 0.035(2) 0.0048(17) -0.0070(17) -0.0035(16) O2' 0.035(2) 0.013(2) 0.024(2) -0.0016(15) -0.0110(17) -0.0014(16) O2" 0.023(2) 0.026(2) 0.0192(19) 0.0001(16) -0.0059(16) -0.0086(16) C1 0.016(2) 0.019(3) 0.014(2) -0.003(2) -0.006(2) 0.000(2) C2 0.022(3) 0.019(3) 0.016(3) -0.005(2) -0.008(2) -0.003(2) C3 0.024(3) 0.016(3) 0.028(3) -0.008(2) -0.010(2) 0.000(2) C4 0.012(2) 0.023(3) 0.025(3) -0.013(2) -0.005(2) 0.003(2) C5 0.018(3) 0.028(3) 0.023(3) -0.007(2) -0.008(2) -0.003(2) C6 0.019(3) 0.012(3) 0.020(3) -0.003(2) -0.004(2) -0.002(2) C7 0.019(3) 0.035(4) 0.050(4) -0.017(3) -0.017(3) 0.005(3) C8 0.040(4) 0.044(5) 0.101(7) 0.010(4) -0.035(4) 0.006(4) C9 0.026(4) 0.095(7) 0.127(8) -0.087(7) -0.011(4) 0.008(4) C10 0.018(3) 0.045(4) 0.086(6) -0.023(4) -0.018(3) 0.001(3) O11 0.068(4) 0.032(3) 0.085(4) -0.006(3) -0.008(3) -0.022(3) C11 0.026(3) 0.028(4) 0.048(4) -0.013(3) -0.010(3) -0.002(3) O12 0.069(4) 0.075(4) 0.067(4) -0.028(3) -0.048(3) 0.008(3) C12 0.035(4) 0.037(4) 0.043(4) -0.018(3) -0.014(3) 0.007(3) O13 0.059(3) 0.037(3) 0.049(3) 0.006(2) 0.005(2) -0.019(3) C13 0.031(3) 0.027(3) 0.023(3) -0.003(3) -0.002(2) -0.004(3) O14 0.041(3) 0.045(3) 0.043(3) 0.005(2) -0.031(2) -0.013(2) C14 0.017(3) 0.018(3) 0.038(3) 0.002(2) -0.006(3) -0.005(2) O15 0.028(2) 0.066(4) 0.066(3) -0.045(3) 0.000(2) 0.006(2) C15 0.039(4) 0.037(4) 0.042(4) -0.018(3) -0.015(3) -0.008(3) C21 0.022(3) 0.055(5) 0.028(3) 0.005(3) 0.009(3) 0.001(3) C22 0.184(13) 0.106(10) 0.066(7) -0.046(7) -0.032(8) 0.031(9) C23 0.057(6) 0.111(9) 0.090(8) 0.053(7) 0.031(5) 0.013(6) C24 0.036(3) 0.031(4) 0.023(3) -0.001(3) -0.010(3) -0.007(3) C25 0.028(3) 0.065(5) 0.036(4) -0.019(3) -0.012(3) -0.008(3) C26 0.045(4) 0.124(8) 0.022(4) -0.017(4) 0.002(3) -0.038(5) C31 0.034(3) 0.020(3) 0.034(3) -0.006(3) -0.012(3) -0.001(2) C32 0.070(5) 0.035(4) 0.042(4) -0.015(3) 0.001(4) -0.002(4) C33 0.050(4) 0.024(4) 0.070(5) -0.002(3) -0.011(4) -0.012(3) C34 0.055(4) 0.031(4) 0.023(3) -0.003(3) -0.008(3) -0.016(3) C35 0.058(5) 0.068(6) 0.029(4) 0.009(4) -0.015(3) 0.001(4) C36 0.074(5) 0.045(5) 0.031(4) -0.009(3) 0.007(4) 0.008(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag W1 C15 1.995(6) . ? W1 C13 2.015(6) . ? W1 C11 2.031(6) . ? W1 C14 2.041(6) . ? W1 C12 2.048(7) . ? W1 Sn1 2.7342(4) . ? Sn1 F1 1.974(3) . ? Sn1 C1 2.188(5) . ? Sn1 O2 2.323(4) . ? Sn1 O1 2.333(4) . ? P1 O1 1.488(4) . ? P1 O1' 1.554(4) . ? P1 O1" 1.559(4) . ? P1 C2 1.788(5) . ? P2 O2 1.493(4) . ? P2 O2' 1.554(4) . ? P2 O2" 1.564(4) . ? P2 C6 1.782(5) . ? O1' C21 1.464(6) . ? O1" C24 1.490(6) . ? O2' C31 1.487(6) . ? O2" C34 1.466(7) . ? C1 C6 1.393(7) . ? C1 C2 1.393(7) . ? C2 C3 1.383(7) . ? C3 C4 1.398(7) . ? C4 C5 1.377(8) . ? C4 C7 1.540(7) . ? C5 C6 1.397(7) . ? C7 C10 1.523(9) . ? C7 C9 1.530(9) . ? C7 C8 1.530(10) . ? O11 C11 1.152(8) . ? O12 C12 1.135(8) . ? O13 C13 1.157(7) . ? O14 C14 1.136(7) . ? O15 C15 1.144(7) . ? C21 C23 1.413(11) . ? C21 C22 1.564(12) . ? C24 C25 1.492(8) . ? C24 C26 1.507(9) . ? C31 C32 1.490(8) . ? C31 C33 1.494(8) . ? C34 C35 1.486(9) . ? C34 C36 1.498(9) . ? 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 C15 W1 C13 90.2(2) . . ? C15 W1 C11 88.8(3) . . ? C13 W1 C11 179.0(2) . . ? C15 W1 C14 92.1(2) . . ? C13 W1 C14 89.4(2) . . ? C11 W1 C14 91.1(2) . . ? C15 W1 C12 91.5(2) . . ? C13 W1 C12 89.3(3) . . ? C11 W1 C12 90.3(3) . . ? C14 W1 C12 176.1(2) . . ? C15 W1 Sn1 179.2(2) . . ? C13 W1 Sn1 90.32(16) . . ? C11 W1 Sn1 90.64(16) . . ? C14 W1 Sn1 87.35(15) . . ? C12 W1 Sn1 89.02(17) . . ? F1 Sn1 C1 95.53(15) . . ? F1 Sn1 O2 88.69(14) . . ? C1 Sn1 O2 78.15(16) . . ? F1 Sn1 O1 85.47(14) . . ? C1 Sn1 O1 77.93(16) . . ? O2 Sn1 O1 154.69(13) . . ? F1 Sn1 W1 121.66(9) . . ? C1 Sn1 W1 142.81(12) . . ? O2 Sn1 W1 100.51(9) . . ? O1 Sn1 W1 103.51(9) . . ? O1 P1 O1' 115.0(2) . . ? O1 P1 O1" 115.4(2) . . ? O1' P1 O1" 101.3(2) . . ? O1 P1 C2 107.7(2) . . ? O1' P1 C2 108.4(2) . . ? O1" P1 C2 108.6(2) . . ? O2 P2 O2' 115.4(2) . . ? O2 P2 O2" 113.4(2) . . ? O2' P2 O2" 103.1(2) . . ? O2 P2 C6 107.9(2) . . ? O2' P2 C6 105.9(2) . . ? O2" P2 C6 110.8(2) . . ? P1 O1 Sn1 117.76(19) . . ? C21 O1' P1 123.5(4) . . ? C24 O1" P1 121.4(3) . . ? P2 O2 Sn1 116.8(2) . . ? C31 O2' P2 120.4(3) . . ? C34 O2" P2 121.5(3) . . ? C6 C1 C2 117.9(4) . . ? C6 C1 Sn1 120.8(4) . . ? C2 C1 Sn1 121.0(4) . . ? C3 C2 C1 120.7(5) . . ? C3 C2 P1 123.8(4) . . ? C1 C2 P1 115.4(4) . . ? C2 C3 C4 121.7(5) . . ? C5 C4 C3 117.5(5) . . ? C5 C4 C7 122.8(5) . . ? C3 C4 C7 119.6(5) . . ? C4 C5 C6 121.4(5) . . ? C1 C6 C5 120.8(5) . . ? C1 C6 P2 115.0(4) . . ? C5 C6 P2 124.1(4) . . ? C10 C7 C9 108.0(6) . . ? C10 C7 C8 108.6(6) . . ? C9 C7 C8 110.6(7) . . ? C10 C7 C4 111.9(5) . . ? C9 C7 C4 108.2(5) . . ? C8 C7 C4 109.5(5) . . ? O11 C11 W1 177.6(6) . . ? O12 C12 W1 178.2(7) . . ? O13 C13 W1 177.7(5) . . ? O14 C14 W1 179.2(5) . . ? O15 C15 W1 175.8(5) . . ? C23 C21 O1' 109.8(6) . . ? C23 C21 C22 105.3(9) . . ? O1' C21 C22 104.6(7) . . ? O1" C24 C25 106.7(5) . . ? O1" C24 C26 108.4(5) . . ? C25 C24 C26 112.6(5) . . ? O2' C31 C32 106.7(5) . . ? O2' C31 C33 107.5(5) . . ? C32 C31 C33 113.5(6) . . ? O2" C34 C35 108.9(5) . . ? O2" C34 C36 105.8(5) . . ? C35 C34 C36 112.8(6) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C15 W1 Sn1 F1 -40(13) . . . . ? C13 W1 Sn1 F1 94.5(2) . . . . ? C11 W1 Sn1 F1 -85.9(2) . . . . ? C14 W1 Sn1 F1 5.15(19) . . . . ? C12 W1 Sn1 F1 -176.2(2) . . . . ? C15 W1 Sn1 C1 139(13) . . . . ? C13 W1 Sn1 C1 -86.3(3) . . . . ? C11 W1 Sn1 C1 93.3(3) . . . . ? C14 W1 Sn1 C1 -175.6(3) . . . . ? C12 W1 Sn1 C1 3.0(3) . . . . ? C15 W1 Sn1 O2 55(13) . . . . ? C13 W1 Sn1 O2 -170.5(2) . . . . ? C11 W1 Sn1 O2 9.1(2) . . . . ? C14 W1 Sn1 O2 100.15(18) . . . . ? C12 W1 Sn1 O2 -81.2(2) . . . . ? C15 W1 Sn1 O1 -133(13) . . . . ? C13 W1 Sn1 O1 1.47(19) . . . . ? C11 W1 Sn1 O1 -178.9(2) . . . . ? C14 W1 Sn1 O1 -87.87(18) . . . . ? C12 W1 Sn1 O1 90.8(2) . . . . ? O1' P1 O1 Sn1 117.0(2) . . . . ? O1" P1 O1 Sn1 -125.5(2) . . . . ? C2 P1 O1 Sn1 -4.0(3) . . . . ? F1 Sn1 O1 P1 99.0(2) . . . . ? C1 Sn1 O1 P1 2.3(2) . . . . ? O2 Sn1 O1 P1 21.7(5) . . . . ? W1 Sn1 O1 P1 -139.5(2) . . . . ? O1 P1 O1' C21 5.2(5) . . . . ? O1" P1 O1' C21 -120.0(5) . . . . ? C2 P1 O1' C21 125.8(5) . . . . ? O1 P1 O1" C24 46.4(4) . . . . ? O1' P1 O1" C24 171.3(4) . . . . ? C2 P1 O1" C24 -74.6(4) . . . . ? O2' P2 O2 Sn1 -105.6(2) . . . . ? O2" P2 O2 Sn1 135.8(2) . . . . ? C6 P2 O2 Sn1 12.6(3) . . . . ? F1 Sn1 O2 P2 -105.1(2) . . . . ? C1 Sn1 O2 P2 -9.2(2) . . . . ? O1 Sn1 O2 P2 -28.6(5) . . . . ? W1 Sn1 O2 P2 132.9(2) . . . . ? O2 P2 O2' C31 -55.4(4) . . . . ? O2" P2 O2' C31 68.8(4) . . . . ? C6 P2 O2' C31 -174.7(4) . . . . ? O2 P2 O2" C34 -42.3(5) . . . . ? O2' P2 O2" C34 -167.8(4) . . . . ? C6 P2 O2" C34 79.2(5) . . . . ? F1 Sn1 C1 C6 89.6(4) . . . . ? O2 Sn1 C1 C6 2.1(4) . . . . ? O1 Sn1 C1 C6 173.8(4) . . . . ? W1 Sn1 C1 C6 -89.7(4) . . . . ? F1 Sn1 C1 C2 -83.5(4) . . . . ? O2 Sn1 C1 C2 -171.0(4) . . . . ? O1 Sn1 C1 C2 0.6(4) . . . . ? W1 Sn1 C1 C2 97.2(4) . . . . ? C6 C1 C2 C3 0.2(7) . . . . ? Sn1 C1 C2 C3 173.6(4) . . . . ? C6 C1 C2 P1 -176.3(4) . . . . ? Sn1 C1 C2 P1 -2.9(5) . . . . ? O1 P1 C2 C3 -171.9(4) . . . . ? O1' P1 C2 C3 63.1(5) . . . . ? O1" P1 C2 C3 -46.2(5) . . . . ? O1 P1 C2 C1 4.4(4) . . . . ? O1' P1 C2 C1 -120.5(4) . . . . ? O1" P1 C2 C1 130.1(4) . . . . ? C1 C2 C3 C4 -1.1(8) . . . . ? P1 C2 C3 C4 175.1(4) . . . . ? C2 C3 C4 C5 1.2(8) . . . . ? C2 C3 C4 C7 -175.3(5) . . . . ? C3 C4 C5 C6 -0.3(8) . . . . ? C7 C4 C5 C6 176.0(5) . . . . ? C2 C1 C6 C5 0.6(7) . . . . ? Sn1 C1 C6 C5 -172.7(4) . . . . ? C2 C1 C6 P2 177.4(4) . . . . ? Sn1 C1 C6 P2 4.0(5) . . . . ? C4 C5 C6 C1 -0.6(8) . . . . ? C4 C5 C6 P2 -177.0(4) . . . . ? O2 P2 C6 C1 -11.0(4) . . . . ? O2' P2 C6 C1 113.1(4) . . . . ? O2" P2 C6 C1 -135.7(4) . . . . ? O2 P2 C6 C5 165.7(4) . . . . ? O2' P2 C6 C5 -70.2(5) . . . . ? O2" P2 C6 C5 41.0(5) . . . . ? C5 C4 C7 C10 3.6(8) . . . . ? C3 C4 C7 C10 179.8(5) . . . . ? C5 C4 C7 C9 -115.3(7) . . . . ? C3 C4 C7 C9 60.9(8) . . . . ? C5 C4 C7 C8 124.0(6) . . . . ? C3 C4 C7 C8 -59.7(7) . . . . ? C15 W1 C11 O11 -9(15) . . . . ? C13 W1 C11 O11 -31(24) . . . . ? C14 W1 C11 O11 84(15) . . . . ? C12 W1 C11 O11 -100(15) . . . . ? Sn1 W1 C11 O11 171(15) . . . . ? C15 W1 C12 O12 66(19) . . . . ? C13 W1 C12 O12 -24(19) . . . . ? C11 W1 C12 O12 155(19) . . . . ? C14 W1 C12 O12 -94(19) . . . . ? Sn1 W1 C12 O12 -114(19) . . . . ? C15 W1 C13 O13 29(13) . . . . ? C11 W1 C13 O13 52(22) . . . . ? C14 W1 C13 O13 -63(13) . . . . ? C12 W1 C13 O13 121(13) . . . . ? Sn1 W1 C13 O13 -150(13) . . . . ? C15 W1 C14 O14 -107(37) . . . . ? C13 W1 C14 O14 -17(37) . . . . ? C11 W1 C14 O14 164(37) . . . . ? C12 W1 C14 O14 53(38) . . . . ? Sn1 W1 C14 O14 73(37) . . . . ? C13 W1 C15 O15 -39(9) . . . . ? C11 W1 C15 O15 141(9) . . . . ? C14 W1 C15 O15 50(9) . . . . ? C12 W1 C15 O15 -128(9) . . . . ? Sn1 W1 C15 O15 95(15) . . . . ? P1 O1' C21 C23 156.5(7) . . . . ? P1 O1' C21 C22 -91.0(7) . . . . ? P1 O1" C24 C25 -130.5(4) . . . . ? P1 O1" C24 C26 108.0(5) . . . . ? P2 O2' C31 C32 129.6(5) . . . . ? P2 O2' C31 C33 -108.3(5) . . . . ? P2 O2" C34 C35 100.5(5) . . . . ? P2 O2" C34 C36 -137.9(5) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 2.810 _refine_diff_density_min -1.789 _refine_diff_density_rms 0.166 data_nox0164 _database_code_depnum_ccdc_archive 'CCDC 802876' #TrackingRef '- compound4_revised3.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C44 H49 O16 P3 Sn W2, C7 H8' _chemical_formula_sum 'C51 H57 O16 P3 Sn W2' _chemical_formula_weight 1505.27 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/c _symmetry_space_group_name_Hall -P2ybc 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 20.8155(6) _cell_length_b 12.6552(3) _cell_length_c 21.8652(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.595(2) _cell_angle_gamma 90.00 _cell_volume 5759.5(3) _cell_formula_units_Z 4 _cell_measurement_temperature 173(1) _cell_measurement_reflns_used 27819 _cell_measurement_theta_min 2.09 _cell_measurement_theta_max 29.11 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.736 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2936 _exptl_absorpt_coefficient_mu 4.562 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.523 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.37 (release 24-10-2008 CrysAlis171 .NET) (compiled Oct 24 2008,09:44:38) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(1) _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 'Xcalibur2 CCD diffractometer' _diffrn_measurement_method ; 486 frames via \w-rotation (\D\w = 1\%) and two times 30 s per frame (8 sets at different \k-angles) ; _diffrn_detector_area_resol_mean 16.0560 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 48744 _diffrn_reflns_av_R_equivalents 0.0361 _diffrn_reflns_av_sigmaI/netI 0.0385 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 2.10 _diffrn_reflns_theta_max 25.50 _reflns_number_total 10716 _reflns_number_gt 8588 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlis CCD (Oxford Diffraction, 2008) ; _computing_cell_refinement ; CrysAlis RED (Oxford Diffraction, 2008) ; _computing_data_reduction ; CrysAlis RED (Oxford Diffraction, 2008) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL-Plus (Sheldrick, 1991)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 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^)+(0.0304P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10716 _refine_ls_number_parameters 627 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.0326 _refine_ls_R_factor_gt 0.0227 _refine_ls_wR_factor_ref 0.0530 _refine_ls_wR_factor_gt 0.0520 _refine_ls_goodness_of_fit_ref 0.947 _refine_ls_restrained_S_all 0.947 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group W1 W 0.156980(8) 0.141299(12) 0.063633(7) 0.01970(5) Uani 1 1 d . . . W2 W 0.405937(8) 0.330295(12) 0.110276(7) 0.01733(5) Uani 1 1 d . . . Sn1 Sn 0.245704(12) 0.113473(19) 0.157302(10) 0.01474(6) Uani 1 1 d . . . P1 P 0.22518(5) 0.24827(8) 0.28424(4) 0.0183(2) Uani 1 1 d . . . P2 P 0.24426(5) -0.14107(7) 0.19198(4) 0.0196(2) Uani 1 1 d . . . P3 P 0.36832(5) 0.15457(7) 0.15577(4) 0.0154(2) Uani 1 1 d . . . O1 O 0.23566(12) 0.26331(18) 0.21716(10) 0.0193(6) Uani 1 1 d . . . O1' O 0.26999(12) 0.31274(19) 0.32760(10) 0.0208(6) Uani 1 1 d . . . O1" O 0.15693(13) 0.2852(2) 0.30493(11) 0.0252(6) Uani 1 1 d . . . O2 O 0.26162(13) -0.07121(19) 0.14014(10) 0.0204(6) Uani 1 1 d . . . O2" O 0.17695(13) -0.1951(2) 0.18658(11) 0.0268(6) Uani 1 1 d . . . O2' O 0.29190(14) -0.2356(2) 0.20126(12) 0.0281(7) Uani 1 1 d . . . C1 C 0.23813(18) 0.0459(3) 0.24912(15) 0.0168(8) Uani 1 1 d . . . C2 C 0.23634(18) 0.1112(3) 0.30069(16) 0.0184(8) Uani 1 1 d . . . C3 C 0.23895(19) 0.0690(3) 0.35928(16) 0.0214(9) Uani 1 1 d . . . H3A H 0.2380 0.1144 0.3927 0.026 Uiso 1 1 calc R . . C4 C 0.2430(2) -0.0396(3) 0.36938(17) 0.0240(9) Uani 1 1 d . . . C5 C 0.24249(19) -0.1041(3) 0.31821(16) 0.0224(9) Uani 1 1 d . . . H5A H 0.2437 -0.1770 0.3233 0.027 Uiso 1 1 calc R . . C6 C 0.24029(18) -0.0624(3) 0.25935(15) 0.0170(8) Uani 1 1 d . . . C7 C 0.2495(2) -0.0825(3) 0.43497(17) 0.0312(10) Uani 1 1 d . . . C8 C 0.1933(2) -0.0427(4) 0.47308(18) 0.0446(13) Uani 1 1 d . . . H8A H 0.1934 0.0332 0.4736 0.067 Uiso 1 1 calc R . . H8B H 0.1975 -0.0688 0.5141 0.067 Uiso 1 1 calc R . . H8C H 0.1536 -0.0675 0.4555 0.067 Uiso 1 1 calc R . . C9 C 0.2498(3) -0.2036(3) 0.4357(2) 0.0514(15) Uani 1 1 d . . . H9A H 0.2876 -0.2290 0.4157 0.077 Uiso 1 1 calc R . . H9B H 0.2123 -0.2295 0.4146 0.077 Uiso 1 1 calc R . . H9C H 0.2496 -0.2282 0.4772 0.077 Uiso 1 1 calc R . . C10 C 0.3124(2) -0.0426(3) 0.46282(18) 0.0345(11) Uani 1 1 d . . . H10A H 0.3126 0.0333 0.4626 0.052 Uiso 1 1 calc R . . H10B H 0.3477 -0.0685 0.4393 0.052 Uiso 1 1 calc R . . H10C H 0.3164 -0.0675 0.5042 0.052 Uiso 1 1 calc R . . O11 O 0.20702(18) -0.0728(3) 0.00465(15) 0.0559(10) Uani 1 1 d . . . C11 C 0.1884(2) 0.0028(3) 0.02732(19) 0.0316(10) Uani 1 1 d . . . O12 O 0.25561(15) 0.2644(3) -0.01910(13) 0.0419(8) Uani 1 1 d . . . C12 C 0.2206(2) 0.2190(3) 0.01103(17) 0.0271(10) Uani 1 1 d . . . O13 O 0.11605(16) 0.3655(2) 0.11581(15) 0.0456(8) Uani 1 1 d . . . C13 C 0.13054(19) 0.2841(3) 0.09833(18) 0.0260(9) Uani 1 1 d . . . O14 O 0.05946(17) 0.0293(3) 0.15343(17) 0.0593(10) Uani 1 1 d . . . C14 C 0.0940(2) 0.0681(3) 0.1213(2) 0.0334(11) Uani 1 1 d . . . O15 O 0.05575(17) 0.1568(3) -0.04281(15) 0.0603(11) Uani 1 1 d . . . C15 C 0.0920(2) 0.1508(4) -0.0033(2) 0.0354(11) Uani 1 1 d . . . O16 O 0.54812(15) 0.2418(2) 0.11340(14) 0.0425(8) Uani 1 1 d . . . C16 C 0.4972(2) 0.2733(3) 0.11322(17) 0.0245(9) Uani 1 1 d . . . O17 O 0.39503(15) 0.2286(2) -0.02198(12) 0.0362(7) Uani 1 1 d . . . C17 C 0.39690(18) 0.2633(3) 0.02624(17) 0.0224(9) Uani 1 1 d . . . O18 O 0.26381(14) 0.4236(2) 0.10828(13) 0.0333(7) Uani 1 1 d . . . C18 C 0.3135(2) 0.3876(3) 0.10893(17) 0.0214(9) Uani 1 1 d . . . O19 O 0.43477(17) 0.4596(2) 0.23182(13) 0.0440(9) Uani 1 1 d . . . C19 C 0.4234(2) 0.4102(3) 0.18938(18) 0.0264(9) Uani 1 1 d . . . O20 O 0.45179(14) 0.5357(2) 0.04231(13) 0.0342(7) Uani 1 1 d . . . C20 C 0.43560(19) 0.4599(3) 0.06711(17) 0.0226(9) Uani 1 1 d . . . C41 C 0.40297(18) 0.0465(3) 0.11134(16) 0.0180(8) Uani 1 1 d . . . C42 C 0.4645(2) 0.0085(3) 0.12422(18) 0.0258(9) Uani 1 1 d . . . H42A H 0.4877 0.0355 0.1573 0.031 Uiso 1 1 calc R . . C43 C 0.4915(2) -0.0693(3) 0.08794(19) 0.0342(11) Uani 1 1 d . . . H43A H 0.5325 -0.0942 0.0969 0.041 Uiso 1 1 calc R . . C44 C 0.4577(2) -0.1100(3) 0.03874(19) 0.0359(11) Uani 1 1 d . . . H44A H 0.4755 -0.1636 0.0153 0.043 Uiso 1 1 calc R . . C45 C 0.3979(2) -0.0712(3) 0.02443(17) 0.0287(10) Uani 1 1 d . . . H45A H 0.3759 -0.0968 -0.0097 0.034 Uiso 1 1 calc R . . C46 C 0.3701(2) 0.0055(3) 0.06020(16) 0.0222(9) Uani 1 1 d . . . H46A H 0.3293 0.0304 0.0504 0.027 Uiso 1 1 calc R . . C51 C 0.39238(18) 0.1244(3) 0.23487(15) 0.0177(8) Uani 1 1 d . . . C52 C 0.3987(2) 0.2064(3) 0.27603(17) 0.0340(11) Uani 1 1 d . . . H52A H 0.3935 0.2757 0.2626 0.041 Uiso 1 1 calc R . . C53 C 0.4125(3) 0.1873(4) 0.33677(19) 0.0447(13) Uani 1 1 d . . . H53A H 0.4161 0.2436 0.3639 0.054 Uiso 1 1 calc R . . C54 C 0.4209(2) 0.0862(4) 0.35766(18) 0.0342(11) Uani 1 1 d . . . H54A H 0.4309 0.0734 0.3985 0.041 Uiso 1 1 calc R . . C55 C 0.4143(2) 0.0046(4) 0.31730(19) 0.0379(12) Uani 1 1 d . . . H55A H 0.4197 -0.0645 0.3309 0.045 Uiso 1 1 calc R . . C56 C 0.3996(2) 0.0232(3) 0.25630(17) 0.0301(10) Uani 1 1 d . . . H56A H 0.3945 -0.0335 0.2296 0.036 Uiso 1 1 calc R . . C21 C 0.2596(2) 0.4258(3) 0.34192(18) 0.0311(10) Uani 1 1 d . . . H21A H 0.2186 0.4334 0.3631 0.037 Uiso 1 1 calc R . . C22 C 0.3136(3) 0.4556(4) 0.3853(2) 0.0616(17) Uani 1 1 d . . . H22A H 0.3050 0.5237 0.4027 0.092 Uiso 1 1 calc R . . H22B H 0.3533 0.4580 0.3634 0.092 Uiso 1 1 calc R . . H22C H 0.3167 0.4039 0.4174 0.092 Uiso 1 1 calc R . . C23 C 0.2579(3) 0.4901(4) 0.2856(2) 0.0596(16) Uani 1 1 d . . . H23A H 0.2257 0.4627 0.2582 0.089 Uiso 1 1 calc R . . H23B H 0.2991 0.4873 0.2663 0.089 Uiso 1 1 calc R . . H23C H 0.2479 0.5619 0.2958 0.089 Uiso 1 1 calc R . . C24 C 0.0975(2) 0.2677(4) 0.2695(2) 0.0398(12) Uani 1 1 d . . . H24A H 0.1079 0.2553 0.2265 0.048 Uiso 1 1 calc R . . C25 C 0.0640(3) 0.1737(5) 0.2947(3) 0.083(2) Uani 1 1 d . . . H25A H 0.0903 0.1121 0.2891 0.125 Uiso 1 1 calc R . . H25B H 0.0237 0.1642 0.2736 0.125 Uiso 1 1 calc R . . H25C H 0.0565 0.1841 0.3375 0.125 Uiso 1 1 calc R . . C26 C 0.0589(3) 0.3657(4) 0.2750(3) 0.0706(18) Uani 1 1 d . . . H26A H 0.0829 0.4243 0.2593 0.106 Uiso 1 1 calc R . . H26B H 0.0492 0.3781 0.3172 0.106 Uiso 1 1 calc R . . H26C H 0.0196 0.3581 0.2520 0.106 Uiso 1 1 calc R . . C31 C 0.1617(2) -0.2672(3) 0.13506(18) 0.0313(10) Uani 1 1 d . . . H31A H 0.1966 -0.2645 0.1054 0.038 Uiso 1 1 calc R . . C32 C 0.1019(3) -0.2280(4) 0.1055(2) 0.0611(16) Uani 1 1 d . . . H32A H 0.1084 -0.1570 0.0914 0.092 Uiso 1 1 calc R . . H32B H 0.0677 -0.2290 0.1346 0.092 Uiso 1 1 calc R . . H32C H 0.0910 -0.2726 0.0715 0.092 Uiso 1 1 calc R . . C33 C 0.1564(3) -0.3748(3) 0.1588(2) 0.0540(15) Uani 1 1 d . . . H33A H 0.1965 -0.3951 0.1776 0.081 Uiso 1 1 calc R . . H33B H 0.1464 -0.4224 0.1259 0.081 Uiso 1 1 calc R . . H33C H 0.1230 -0.3777 0.1887 0.081 Uiso 1 1 calc R . . C34 C 0.3573(2) -0.2378(3) 0.1774(2) 0.0327(10) Uani 1 1 d . . . H34A H 0.3690 -0.1669 0.1634 0.039 Uiso 1 1 calc R . . C35 C 0.3588(3) -0.3117(4) 0.1248(3) 0.0683(19) Uani 1 1 d . . . H35A H 0.3298 -0.2873 0.0934 0.102 Uiso 1 1 calc R . . H35B H 0.3460 -0.3808 0.1380 0.102 Uiso 1 1 calc R . . H35C H 0.4016 -0.3147 0.1089 0.102 Uiso 1 1 calc R . . C36 C 0.4007(3) -0.2688(4) 0.2300(3) 0.0700(18) Uani 1 1 d . . . H36A H 0.3970 -0.2177 0.2622 0.105 Uiso 1 1 calc R . . H36B H 0.4444 -0.2713 0.2164 0.105 Uiso 1 1 calc R . . H36C H 0.3884 -0.3371 0.2449 0.105 Uiso 1 1 calc R . . C61 C 0.0635(3) -0.1922(4) 0.3703(3) 0.0658(9) Uiso 0.50 1 d PGD A 1 C62 C 0.0482(5) -0.2432(5) 0.4245(3) 0.0658(9) Uiso 0.50 1 d PGD A 1 H62 H 0.0276 -0.2065 0.4555 0.079 Uiso 0.50 1 calc PR A 1 C63 C 0.0637(6) -0.3492(5) 0.4325(3) 0.0658(9) Uiso 0.50 1 d PGD A 1 H63 H 0.0534 -0.3834 0.4688 0.079 Uiso 0.50 1 calc PR A 1 C64 C 0.0945(4) -0.4042(4) 0.3862(4) 0.0658(9) Uiso 0.50 1 d PGD A 1 H64 H 0.1048 -0.4751 0.3915 0.079 Uiso 0.50 1 calc PR A 1 C65 C 0.1098(4) -0.3532(5) 0.3320(3) 0.0658(9) Uiso 0.50 1 d PGD A 1 H65 H 0.1304 -0.3899 0.3010 0.079 Uiso 0.50 1 calc PR A 1 C66 C 0.0943(4) -0.2472(5) 0.3240(3) 0.0658(9) Uiso 0.50 1 d PGD A 1 H66 H 0.1046 -0.2130 0.2878 0.079 Uiso 0.50 1 calc PR A 1 C67 C 0.0464(5) -0.0749(5) 0.3615(4) 0.0658(9) Uiso 0.50 1 d PD A 1 H67A H 0.0006 -0.0674 0.3580 0.099 Uiso 0.50 1 calc PR A 1 H67B H 0.0662 -0.0490 0.3250 0.099 Uiso 0.50 1 calc PR A 1 H67C H 0.0617 -0.0351 0.3961 0.099 Uiso 0.50 1 calc PR A 1 C61' C 0.0504(3) -0.1513(4) 0.3854(3) 0.0658(9) Uiso 0.50 1 d PGD B 2 C62' C 0.0399(5) -0.2203(5) 0.4337(3) 0.0658(9) Uiso 0.50 1 d PGD B 2 H62' H 0.0188 -0.1969 0.4684 0.079 Uiso 0.50 1 calc PR B 2 C63' C 0.0610(6) -0.3243(5) 0.4301(4) 0.0658(9) Uiso 0.50 1 d PGD B 2 H63' H 0.0540 -0.3705 0.4624 0.079 Uiso 0.50 1 calc PR B 2 C64' C 0.0927(5) -0.3593(4) 0.3782(4) 0.0658(9) Uiso 0.50 1 d PGD B 2 H64' H 0.1068 -0.4288 0.3758 0.079 Uiso 0.50 1 calc PR B 2 C65' C 0.1032(4) -0.2902(5) 0.3299(3) 0.0658(9) Uiso 0.50 1 d PGD B 2 H65' H 0.1243 -0.3136 0.2952 0.079 Uiso 0.50 1 calc PR B 2 C66' C 0.0820(4) -0.1862(5) 0.3335(3) 0.0658(9) Uiso 0.50 1 d PGD B 2 H66' H 0.0890 -0.1400 0.3011 0.079 Uiso 0.50 1 calc PR B 2 C67' C 0.0270(5) -0.0362(5) 0.3894(4) 0.0658(9) Uiso 0.50 1 d PD B 2 H67D H -0.0074 -0.0252 0.3605 0.099 Uiso 0.50 1 calc PR B 2 H67E H 0.0618 0.0108 0.3802 0.099 Uiso 0.50 1 calc PR B 2 H67F H 0.0120 -0.0222 0.4299 0.099 Uiso 0.50 1 calc PR B 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 W1 0.02003(9) 0.02091(9) 0.01806(8) 0.00005(6) -0.00539(7) 0.00223(7) W2 0.01888(9) 0.01675(8) 0.01639(8) -0.00130(6) 0.00078(6) 0.00147(7) Sn1 0.01695(14) 0.01543(13) 0.01179(12) 0.00018(9) -0.00130(10) 0.00228(11) P1 0.0226(6) 0.0168(5) 0.0154(5) -0.0020(4) 0.0005(4) 0.0021(4) P2 0.0266(6) 0.0142(5) 0.0180(5) -0.0011(4) -0.0005(4) 0.0004(4) P3 0.0179(5) 0.0149(5) 0.0135(4) -0.0010(4) -0.0015(4) 0.0031(4) O1 0.0263(16) 0.0136(13) 0.0181(13) -0.0011(10) 0.0002(11) 0.0049(11) O1' 0.0272(16) 0.0165(13) 0.0185(13) -0.0048(11) -0.0040(12) 0.0029(12) O1" 0.0240(16) 0.0307(15) 0.0209(14) -0.0049(12) 0.0012(12) 0.0034(13) O2 0.0316(16) 0.0148(13) 0.0147(13) -0.0005(10) 0.0009(11) 0.0023(12) O2" 0.0304(17) 0.0267(15) 0.0234(14) -0.0080(12) 0.0019(13) -0.0055(13) O2' 0.0357(18) 0.0184(15) 0.0304(15) 0.0053(12) 0.0035(13) 0.0076(13) C1 0.019(2) 0.019(2) 0.0128(18) -0.0011(15) -0.0022(16) 0.0011(16) C2 0.019(2) 0.021(2) 0.0160(18) -0.0007(15) 0.0003(16) -0.0025(17) C3 0.026(2) 0.022(2) 0.0155(19) -0.0023(16) -0.0005(17) -0.0052(18) C4 0.026(2) 0.027(2) 0.018(2) 0.0032(17) -0.0032(17) -0.0091(18) C5 0.026(2) 0.020(2) 0.021(2) 0.0036(16) -0.0046(17) -0.0022(18) C6 0.017(2) 0.018(2) 0.0155(18) -0.0008(15) -0.0027(16) -0.0022(16) C7 0.048(3) 0.028(2) 0.018(2) 0.0071(18) -0.006(2) -0.013(2) C8 0.053(3) 0.061(3) 0.020(2) 0.012(2) -0.003(2) -0.020(3) C9 0.094(4) 0.031(3) 0.029(2) 0.017(2) -0.019(3) -0.024(3) C10 0.045(3) 0.038(3) 0.020(2) 0.0081(19) -0.006(2) -0.004(2) O11 0.074(3) 0.038(2) 0.056(2) -0.0242(18) -0.022(2) 0.0178(19) C11 0.035(3) 0.029(2) 0.031(2) -0.005(2) -0.014(2) 0.003(2) O12 0.041(2) 0.051(2) 0.0334(18) 0.0149(16) 0.0039(16) -0.0017(17) C12 0.031(3) 0.031(2) 0.019(2) 0.0009(18) -0.0038(19) 0.007(2) O13 0.043(2) 0.0322(18) 0.061(2) -0.0099(16) 0.0004(17) 0.0072(16) C13 0.021(2) 0.028(2) 0.029(2) 0.0016(19) -0.0050(18) 0.0068(19) O14 0.045(2) 0.065(3) 0.068(2) 0.023(2) 0.017(2) -0.0124(19) C14 0.030(3) 0.032(3) 0.038(3) 0.005(2) -0.007(2) 0.002(2) O15 0.047(2) 0.098(3) 0.0356(19) -0.0120(19) -0.0228(18) 0.016(2) C15 0.024(3) 0.048(3) 0.034(2) -0.003(2) -0.004(2) 0.008(2) O16 0.0281(19) 0.044(2) 0.056(2) -0.0140(16) -0.0056(16) 0.0060(16) C16 0.020(2) 0.026(2) 0.028(2) -0.0074(18) -0.0027(18) -0.0017(19) O17 0.042(2) 0.0462(19) 0.0206(15) -0.0061(14) 0.0016(14) 0.0076(16) C17 0.019(2) 0.024(2) 0.024(2) 0.0028(17) 0.0063(18) 0.0065(18) O18 0.0245(18) 0.0311(17) 0.0444(18) 0.0041(14) 0.0029(14) 0.0106(14) C18 0.028(3) 0.015(2) 0.022(2) 0.0034(16) 0.0022(18) 0.0006(18) O19 0.070(3) 0.0367(18) 0.0254(16) -0.0132(14) 0.0020(16) -0.0130(17) C19 0.032(3) 0.023(2) 0.024(2) 0.0004(18) 0.0008(19) 0.0008(19) O20 0.0339(19) 0.0288(17) 0.0402(18) 0.0095(14) 0.0131(15) -0.0006(14) C20 0.019(2) 0.026(2) 0.023(2) -0.0068(18) 0.0018(18) 0.0019(18) C41 0.019(2) 0.0162(19) 0.0188(19) 0.0021(15) 0.0045(16) 0.0010(17) C42 0.027(2) 0.024(2) 0.026(2) -0.0013(17) -0.0009(19) 0.0041(19) C43 0.030(3) 0.035(3) 0.038(3) -0.004(2) 0.001(2) 0.017(2) C44 0.046(3) 0.030(2) 0.032(2) -0.010(2) 0.008(2) 0.017(2) C45 0.039(3) 0.027(2) 0.020(2) -0.0100(17) 0.0028(19) 0.001(2) C46 0.024(2) 0.024(2) 0.019(2) -0.0015(16) 0.0018(17) 0.0044(18) C51 0.017(2) 0.024(2) 0.0125(18) -0.0003(15) -0.0037(15) 0.0009(17) C52 0.056(3) 0.024(2) 0.021(2) -0.0018(18) 0.005(2) -0.012(2) C53 0.074(4) 0.039(3) 0.021(2) -0.005(2) -0.005(2) -0.025(3) C54 0.028(3) 0.056(3) 0.019(2) 0.007(2) -0.0033(19) -0.004(2) C55 0.053(3) 0.032(3) 0.028(2) 0.009(2) -0.001(2) 0.018(2) C56 0.045(3) 0.025(2) 0.021(2) -0.0029(17) -0.003(2) 0.013(2) C21 0.038(3) 0.019(2) 0.036(2) -0.0065(18) -0.003(2) 0.002(2) C22 0.090(5) 0.035(3) 0.059(3) -0.011(2) -0.041(3) -0.005(3) C23 0.097(5) 0.023(3) 0.059(3) 0.001(2) -0.028(3) 0.002(3) C24 0.022(3) 0.058(3) 0.039(3) -0.011(2) -0.002(2) 0.000(2) C25 0.038(4) 0.070(4) 0.143(6) -0.019(4) 0.017(4) -0.021(3) C26 0.032(3) 0.080(4) 0.100(5) 0.002(4) -0.019(3) 0.020(3) C31 0.038(3) 0.032(2) 0.024(2) -0.0119(18) 0.004(2) -0.010(2) C32 0.076(4) 0.042(3) 0.064(4) -0.001(3) -0.037(3) -0.014(3) C33 0.087(5) 0.023(3) 0.052(3) -0.007(2) -0.016(3) -0.007(3) C34 0.031(3) 0.021(2) 0.046(3) -0.002(2) 0.000(2) 0.003(2) C35 0.092(5) 0.038(3) 0.076(4) -0.025(3) 0.043(4) -0.004(3) C36 0.055(4) 0.043(3) 0.111(5) 0.026(3) -0.033(4) 0.007(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_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag W1 C15 1.986(4) . ? W1 C12 2.018(4) . ? W1 C11 2.035(4) . ? W1 C13 2.037(4) . ? W1 C14 2.049(5) . ? W1 Sn1 2.7660(3) . ? W2 C20 1.993(4) . ? W2 C17 2.030(4) . ? W2 C16 2.032(4) . ? W2 C19 2.033(4) . ? W2 C18 2.057(4) . ? W2 P3 2.5621(9) . ? Sn1 C1 2.189(3) . ? Sn1 O1 2.315(2) . ? Sn1 O2 2.391(2) . ? Sn1 P3 2.6053(10) . ? P1 O1 1.497(2) . ? P1 O1' 1.554(3) . ? P1 O1" 1.567(3) . ? P1 C2 1.786(4) . ? P2 O2 1.485(2) . ? P2 O2" 1.562(3) . ? P2 O2' 1.566(3) . ? P2 C6 1.781(4) . ? P3 C41 1.830(4) . ? P3 C51 1.836(4) . ? O1' C21 1.481(4) . ? O1" C24 1.469(5) . ? O2" C31 1.481(4) . ? O2' C34 1.464(5) . ? C1 C6 1.389(5) . ? C1 C2 1.398(5) . ? C2 C3 1.389(5) . ? C3 C4 1.394(5) . ? C4 C5 1.385(5) . ? C4 C7 1.538(5) . ? C5 C6 1.391(5) . ? C7 C10 1.524(6) . ? C7 C8 1.528(6) . ? C7 C9 1.533(6) . ? O11 C11 1.147(5) . ? O12 C12 1.143(5) . ? O13 C13 1.141(5) . ? O14 C14 1.124(5) . ? O15 C15 1.144(5) . ? O16 C16 1.133(5) . ? O17 C17 1.143(4) . ? O18 C18 1.130(4) . ? O19 C19 1.142(4) . ? O20 C20 1.154(4) . ? C41 C42 1.395(5) . ? C41 C46 1.404(5) . ? C42 C43 1.386(5) . ? C43 C44 1.378(6) . ? C44 C45 1.371(6) . ? C45 C46 1.378(5) . ? C51 C56 1.371(5) . ? C51 C52 1.380(5) . ? C52 C53 1.377(5) . ? C53 C54 1.368(6) . ? C54 C55 1.365(6) . ? C55 C56 1.385(5) . ? C21 C23 1.476(6) . ? C21 C22 1.510(6) . ? C24 C26 1.484(6) . ? C24 C25 1.487(7) . ? C31 C33 1.462(6) . ? C31 C32 1.481(6) . ? C34 C35 1.482(6) . ? C34 C36 1.508(6) . ? C61 C62 1.3900 . ? C61 C66 1.3900 . ? C61 C67 1.5382(10) . ? C62 C63 1.3900 . ? C63 C64 1.3900 . ? C64 C65 1.3900 . ? C65 C66 1.3900 . ? C61' C62' 1.3900 . ? C61' C66' 1.3900 . ? C61' C67' 1.5391(10) . ? C62' C63' 1.3900 . ? C63' C64' 1.3900 . ? C64' C65' 1.3900 . ? C65' C66' 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 C15 W1 C12 89.81(17) . . ? C15 W1 C11 89.07(17) . . ? C12 W1 C11 88.97(17) . . ? C15 W1 C13 92.08(17) . . ? C12 W1 C13 87.79(16) . . ? C11 W1 C13 176.56(17) . . ? C15 W1 C14 92.59(18) . . ? C12 W1 C14 176.58(17) . . ? C11 W1 C14 93.50(17) . . ? C13 W1 C14 89.69(17) . . ? C15 W1 Sn1 176.08(13) . . ? C12 W1 Sn1 92.70(11) . . ? C11 W1 Sn1 87.97(11) . . ? C13 W1 Sn1 91.03(11) . . ? C14 W1 Sn1 85.03(12) . . ? C20 W2 C17 86.62(15) . . ? C20 W2 C16 90.76(16) . . ? C17 W2 C16 87.61(15) . . ? C20 W2 C19 86.56(15) . . ? C17 W2 C19 172.55(16) . . ? C16 W2 C19 89.48(16) . . ? C20 W2 C18 89.87(15) . . ? C17 W2 C18 93.22(15) . . ? C16 W2 C18 178.99(15) . . ? C19 W2 C18 89.76(16) . . ? C20 W2 P3 174.46(10) . . ? C17 W2 P3 87.90(11) . . ? C16 W2 P3 88.21(11) . . ? C19 W2 P3 98.87(11) . . ? C18 W2 P3 91.24(10) . . ? C1 Sn1 O1 78.08(11) . . ? C1 Sn1 O2 76.92(11) . . ? O1 Sn1 O2 154.56(8) . . ? C1 Sn1 P3 99.76(10) . . ? O1 Sn1 P3 86.45(7) . . ? O2 Sn1 P3 93.20(7) . . ? C1 Sn1 W1 132.45(10) . . ? O1 Sn1 W1 104.53(6) . . ? O2 Sn1 W1 95.78(6) . . ? P3 Sn1 W1 127.71(2) . . ? O1 P1 O1' 115.99(15) . . ? O1 P1 O1" 112.75(15) . . ? O1' P1 O1" 101.99(14) . . ? O1 P1 C2 107.50(15) . . ? O1' P1 C2 108.12(16) . . ? O1" P1 C2 110.35(16) . . ? O2 P2 O2" 115.34(15) . . ? O2 P2 O2' 113.27(15) . . ? O2" P2 O2' 103.98(15) . . ? O2 P2 C6 108.18(15) . . ? O2" P2 C6 104.95(16) . . ? O2' P2 C6 110.79(16) . . ? C41 P3 C51 103.85(17) . . ? C41 P3 W2 108.60(12) . . ? C51 P3 W2 117.70(12) . . ? C41 P3 Sn1 104.43(12) . . ? C51 P3 Sn1 101.77(12) . . ? W2 P3 Sn1 118.79(4) . . ? P1 O1 Sn1 117.69(13) . . ? C21 O1' P1 123.3(2) . . ? C24 O1" P1 124.3(2) . . ? P2 O2 Sn1 115.28(13) . . ? C31 O2" P2 120.8(2) . . ? C34 O2' P2 124.0(2) . . ? C6 C1 C2 117.0(3) . . ? C6 C1 Sn1 122.0(2) . . ? C2 C1 Sn1 120.8(3) . . ? C3 C2 C1 121.0(3) . . ? C3 C2 P1 124.3(3) . . ? C1 C2 P1 114.6(3) . . ? C2 C3 C4 121.8(3) . . ? C5 C4 C3 116.9(3) . . ? C5 C4 C7 123.1(3) . . ? C3 C4 C7 120.0(3) . . ? C4 C5 C6 121.6(3) . . ? C1 C6 C5 121.6(3) . . ? C1 C6 P2 114.9(3) . . ? C5 C6 P2 123.5(3) . . ? C10 C7 C8 109.4(3) . . ? C10 C7 C9 108.8(4) . . ? C8 C7 C9 109.1(4) . . ? C10 C7 C4 108.8(3) . . ? C8 C7 C4 109.4(4) . . ? C9 C7 C4 111.3(3) . . ? O11 C11 W1 177.0(4) . . ? O12 C12 W1 178.6(4) . . ? O13 C13 W1 177.6(4) . . ? O14 C14 W1 179.0(4) . . ? O15 C15 W1 178.3(4) . . ? O16 C16 W2 178.4(4) . . ? O17 C17 W2 176.0(3) . . ? O18 C18 W2 176.8(3) . . ? O19 C19 W2 176.0(4) . . ? O20 C20 W2 178.9(3) . . ? C42 C41 C46 118.2(3) . . ? C42 C41 P3 121.1(3) . . ? C46 C41 P3 120.5(3) . . ? C43 C42 C41 120.3(4) . . ? C44 C43 C42 120.4(4) . . ? C45 C44 C43 119.9(4) . . ? C44 C45 C46 120.6(4) . . ? C45 C46 C41 120.6(4) . . ? C56 C51 C52 118.1(3) . . ? C56 C51 P3 123.0(3) . . ? C52 C51 P3 118.8(3) . . ? C53 C52 C51 120.9(4) . . ? C54 C53 C52 120.7(4) . . ? C55 C54 C53 118.7(4) . . ? C54 C55 C56 120.9(4) . . ? C51 C56 C55 120.6(4) . . ? C23 C21 O1' 111.0(3) . . ? C23 C21 C22 113.5(4) . . ? O1' C21 C22 105.4(3) . . ? O1" C24 C26 106.6(4) . . ? O1" C24 C25 108.7(4) . . ? C26 C24 C25 112.5(4) . . ? C33 C31 C32 113.7(4) . . ? C33 C31 O2" 108.6(3) . . ? C32 C31 O2" 107.4(4) . . ? O2' C34 C35 108.4(4) . . ? O2' C34 C36 106.6(4) . . ? C35 C34 C36 114.3(4) . . ? C62 C61 C66 120.0 . . ? C62 C61 C67 120.0 . . ? C66 C61 C67 120.0 . . ? C61 C62 C63 120.0 . . ? C62 C63 C64 120.0 . . ? C65 C64 C63 120.0 . . ? C64 C65 C66 120.0 . . ? C65 C66 C61 120.0 . . ? C62' C61' C66' 120.0 . . ? C62' C61' C67' 120.0 . . ? C66' C61' C67' 120.0 . . ? C63' C62' C61' 120.0 . . ? C62' C63' C64' 120.0 . . ? C65' C64' C63' 120.0 . . ? C66' C65' C64' 120.0 . . ? C65' C66' C61' 120.0 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C15 W1 Sn1 C1 -54.7(18) . . . . ? C12 W1 Sn1 C1 175.52(17) . . . . ? C11 W1 Sn1 C1 -95.61(18) . . . . ? C13 W1 Sn1 C1 87.69(17) . . . . ? C14 W1 Sn1 C1 -1.91(17) . . . . ? C15 W1 Sn1 O1 -141.7(18) . . . . ? C12 W1 Sn1 O1 88.51(13) . . . . ? C11 W1 Sn1 O1 177.38(14) . . . . ? C13 W1 Sn1 O1 0.67(13) . . . . ? C14 W1 Sn1 O1 -88.92(14) . . . . ? C15 W1 Sn1 O2 22.9(18) . . . . ? C12 W1 Sn1 O2 -106.93(13) . . . . ? C11 W1 Sn1 O2 -18.06(14) . . . . ? C13 W1 Sn1 O2 165.24(13) . . . . ? C14 W1 Sn1 O2 75.64(14) . . . . ? C15 W1 Sn1 P3 121.5(18) . . . . ? C12 W1 Sn1 P3 -8.35(12) . . . . ? C11 W1 Sn1 P3 80.52(13) . . . . ? C13 W1 Sn1 P3 -96.18(12) . . . . ? C14 W1 Sn1 P3 174.22(13) . . . . ? C20 W2 P3 C41 29.6(12) . . . . ? C17 W2 P3 C41 37.91(17) . . . . ? C16 W2 P3 C41 -49.76(17) . . . . ? C19 W2 P3 C41 -138.95(18) . . . . ? C18 W2 P3 C41 131.09(17) . . . . ? C20 W2 P3 C51 147.1(12) . . . . ? C17 W2 P3 C51 155.43(17) . . . . ? C16 W2 P3 C51 67.76(17) . . . . ? C19 W2 P3 C51 -21.44(18) . . . . ? C18 W2 P3 C51 -111.39(17) . . . . ? C20 W2 P3 Sn1 -89.5(12) . . . . ? C17 W2 P3 Sn1 -81.10(11) . . . . ? C16 W2 P3 Sn1 -168.77(11) . . . . ? C19 W2 P3 Sn1 102.03(12) . . . . ? C18 W2 P3 Sn1 12.08(11) . . . . ? C1 Sn1 P3 C41 101.20(15) . . . . ? O1 Sn1 P3 C41 178.45(13) . . . . ? O2 Sn1 P3 C41 23.93(13) . . . . ? W1 Sn1 P3 C41 -75.91(12) . . . . ? C1 Sn1 P3 C51 -6.63(15) . . . . ? O1 Sn1 P3 C51 70.62(13) . . . . ? O2 Sn1 P3 C51 -83.90(13) . . . . ? W1 Sn1 P3 C51 176.27(12) . . . . ? C1 Sn1 P3 W2 -137.66(10) . . . . ? O1 Sn1 P3 W2 -60.41(7) . . . . ? O2 Sn1 P3 W2 145.07(6) . . . . ? W1 Sn1 P3 W2 45.24(5) . . . . ? O1' P1 O1 Sn1 130.23(15) . . . . ? O1" P1 O1 Sn1 -112.71(16) . . . . ? C2 P1 O1 Sn1 9.1(2) . . . . ? C1 Sn1 O1 P1 -3.62(17) . . . . ? O2 Sn1 O1 P1 -14.4(3) . . . . ? P3 Sn1 O1 P1 -104.38(15) . . . . ? W1 Sn1 O1 P1 127.52(14) . . . . ? O1 P1 O1' C21 79.8(3) . . . . ? O1" P1 O1' C21 -43.1(3) . . . . ? C2 P1 O1' C21 -159.4(3) . . . . ? O1 P1 O1" C24 39.9(4) . . . . ? O1' P1 O1" C24 164.9(3) . . . . ? C2 P1 O1" C24 -80.4(3) . . . . ? O2" P2 O2 Sn1 99.25(16) . . . . ? O2' P2 O2 Sn1 -141.10(15) . . . . ? C6 P2 O2 Sn1 -17.9(2) . . . . ? C1 Sn1 O2 P2 13.59(17) . . . . ? O1 Sn1 O2 P2 24.4(3) . . . . ? P3 Sn1 O2 P2 112.88(15) . . . . ? W1 Sn1 O2 P2 -118.70(14) . . . . ? O2 P2 O2" C31 60.6(3) . . . . ? O2' P2 O2" C31 -64.0(3) . . . . ? C6 P2 O2" C31 179.5(3) . . . . ? O2 P2 O2' C34 19.9(3) . . . . ? O2" P2 O2' C34 145.9(3) . . . . ? C6 P2 O2' C34 -101.8(3) . . . . ? O1 Sn1 C1 C6 -179.6(3) . . . . ? O2 Sn1 C1 C6 -4.4(3) . . . . ? P3 Sn1 C1 C6 -95.4(3) . . . . ? W1 Sn1 C1 C6 81.5(3) . . . . ? O1 Sn1 C1 C2 -5.1(3) . . . . ? O2 Sn1 C1 C2 170.2(3) . . . . ? P3 Sn1 C1 C2 79.1(3) . . . . ? W1 Sn1 C1 C2 -104.0(3) . . . . ? C6 C1 C2 C3 2.2(6) . . . . ? Sn1 C1 C2 C3 -172.6(3) . . . . ? C6 C1 C2 P1 -173.8(3) . . . . ? Sn1 C1 C2 P1 11.4(4) . . . . ? O1 P1 C2 C3 171.1(3) . . . . ? O1' P1 C2 C3 45.2(4) . . . . ? O1" P1 C2 C3 -65.6(4) . . . . ? O1 P1 C2 C1 -13.0(3) . . . . ? O1' P1 C2 C1 -138.9(3) . . . . ? O1" P1 C2 C1 110.3(3) . . . . ? C1 C2 C3 C4 -0.5(6) . . . . ? P1 C2 C3 C4 175.1(3) . . . . ? C2 C3 C4 C5 -1.7(6) . . . . ? C2 C3 C4 C7 176.7(4) . . . . ? C3 C4 C5 C6 2.1(6) . . . . ? C7 C4 C5 C6 -176.2(4) . . . . ? C2 C1 C6 C5 -1.8(6) . . . . ? Sn1 C1 C6 C5 172.9(3) . . . . ? C2 C1 C6 P2 -178.7(3) . . . . ? Sn1 C1 C6 P2 -4.0(4) . . . . ? C4 C5 C6 C1 -0.3(6) . . . . ? C4 C5 C6 P2 176.3(3) . . . . ? O2 P2 C6 C1 14.8(3) . . . . ? O2" P2 C6 C1 -108.9(3) . . . . ? O2' P2 C6 C1 139.5(3) . . . . ? O2 P2 C6 C5 -162.0(3) . . . . ? O2" P2 C6 C5 74.3(4) . . . . ? O2' P2 C6 C5 -37.3(4) . . . . ? C5 C4 C7 C10 115.4(4) . . . . ? C3 C4 C7 C10 -62.8(5) . . . . ? C5 C4 C7 C8 -125.1(4) . . . . ? C3 C4 C7 C8 56.7(5) . . . . ? C5 C4 C7 C9 -4.5(6) . . . . ? C3 C4 C7 C9 177.3(4) . . . . ? C15 W1 C11 O11 67(7) . . . . ? C12 W1 C11 O11 -23(7) . . . . ? C13 W1 C11 O11 -43(9) . . . . ? C14 W1 C11 O11 159(7) . . . . ? Sn1 W1 C11 O11 -116(7) . . . . ? C15 W1 C12 O12 43(16) . . . . ? C11 W1 C12 O12 132(16) . . . . ? C13 W1 C12 O12 -49(16) . . . . ? C14 W1 C12 O12 -91(16) . . . . ? Sn1 W1 C12 O12 -140(16) . . . . ? C15 W1 C13 O13 -54(9) . . . . ? C12 W1 C13 O13 36(9) . . . . ? C11 W1 C13 O13 56(10) . . . . ? C14 W1 C13 O13 -146(9) . . . . ? Sn1 W1 C13 O13 129(9) . . . . ? C15 W1 C14 O14 -112(25) . . . . ? C12 W1 C14 O14 23(27) . . . . ? C11 W1 C14 O14 159(25) . . . . ? C13 W1 C14 O14 -20(25) . . . . ? Sn1 W1 C14 O14 71(25) . . . . ? C12 W1 C15 O15 16(14) . . . . ? C11 W1 C15 O15 -73(14) . . . . ? C13 W1 C15 O15 104(14) . . . . ? C14 W1 C15 O15 -166(14) . . . . ? Sn1 W1 C15 O15 -114(14) . . . . ? C20 W2 C16 O16 -55(13) . . . . ? C17 W2 C16 O16 32(13) . . . . ? C19 W2 C16 O16 -141(13) . . . . ? C18 W2 C16 O16 177(100) . . . . ? P3 W2 C16 O16 120(13) . . . . ? C20 W2 C17 O17 40(5) . . . . ? C16 W2 C17 O17 -51(5) . . . . ? C19 W2 C17 O17 16(6) . . . . ? C18 W2 C17 O17 129(5) . . . . ? P3 W2 C17 O17 -140(5) . . . . ? C20 W2 C18 O18 -30(6) . . . . ? C17 W2 C18 O18 -117(6) . . . . ? C16 W2 C18 O18 98(10) . . . . ? C19 W2 C18 O18 57(6) . . . . ? P3 W2 C18 O18 155(6) . . . . ? C20 W2 C19 O19 -8(6) . . . . ? C17 W2 C19 O19 16(7) . . . . ? C16 W2 C19 O19 83(6) . . . . ? C18 W2 C19 O19 -97(6) . . . . ? P3 W2 C19 O19 171(6) . . . . ? C17 W2 C20 O20 106(18) . . . . ? C16 W2 C20 O20 -167(100) . . . . ? C19 W2 C20 O20 -77(18) . . . . ? C18 W2 C20 O20 13(18) . . . . ? P3 W2 C20 O20 114(18) . . . . ? C51 P3 C41 C42 -41.0(3) . . . . ? W2 P3 C41 C42 85.0(3) . . . . ? Sn1 P3 C41 C42 -147.3(3) . . . . ? C51 P3 C41 C46 144.1(3) . . . . ? W2 P3 C41 C46 -89.8(3) . . . . ? Sn1 P3 C41 C46 37.8(3) . . . . ? C46 C41 C42 C43 -1.4(6) . . . . ? P3 C41 C42 C43 -176.3(3) . . . . ? C41 C42 C43 C44 0.0(6) . . . . ? C42 C43 C44 C45 1.9(7) . . . . ? C43 C44 C45 C46 -2.4(7) . . . . ? C44 C45 C46 C41 1.0(6) . . . . ? C42 C41 C46 C45 0.9(6) . . . . ? P3 C41 C46 C45 175.9(3) . . . . ? C41 P3 C51 C56 -32.3(4) . . . . ? W2 P3 C51 C56 -152.3(3) . . . . ? Sn1 P3 C51 C56 76.0(4) . . . . ? C41 P3 C51 C52 153.0(3) . . . . ? W2 P3 C51 C52 33.0(4) . . . . ? Sn1 P3 C51 C52 -98.7(3) . . . . ? C56 C51 C52 C53 0.7(7) . . . . ? P3 C51 C52 C53 175.7(4) . . . . ? C51 C52 C53 C54 0.6(7) . . . . ? C52 C53 C54 C55 -1.1(7) . . . . ? C53 C54 C55 C56 0.2(7) . . . . ? C52 C51 C56 C55 -1.6(7) . . . . ? P3 C51 C56 C55 -176.3(3) . . . . ? C54 C55 C56 C51 1.1(7) . . . . ? P1 O1' C21 C23 -57.0(5) . . . . ? P1 O1' C21 C22 179.8(3) . . . . ? P1 O1" C24 C26 -139.9(4) . . . . ? P1 O1" C24 C25 98.6(4) . . . . ? P2 O2" C31 C33 110.7(4) . . . . ? P2 O2" C31 C32 -126.0(3) . . . . ? P2 O2' C34 C35 -106.5(4) . . . . ? P2 O2' C34 C36 130.1(3) . . . . ? C66 C61 C62 C63 0.0 . . . . ? C67 C61 C62 C63 180.0 . . . . ? C61 C62 C63 C64 0.0 . . . . ? C62 C63 C64 C65 0.0 . . . . ? C63 C64 C65 C66 0.0 . . . . ? C64 C65 C66 C61 0.0 . . . . ? C62 C61 C66 C65 0.0 . . . . ? C67 C61 C66 C65 180.0 . . . . ? C66' C61' C62' C63' 0.0 . . . . ? C67' C61' C62' C63' 180.0 . . . . ? C61' C62' C63' C64' 0.0 . . . . ? C62' C63' C64' C65' 0.0 . . . . ? C63' C64' C65' C66' 0.0 . . . . ? C64' C65' C66' C61' 0.0 . . . . ? C62' C61' C66' C65' 0.0 . . . . ? C67' C61' C66' C65' 180.0 . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.637 _refine_diff_density_min -1.412 _refine_diff_density_rms 0.097