# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Cheuk-Wai So' _publ_contact_author_email CWSO@NTU.EDU.SG _publ_section_title ; Synthesis and characterization of a tin(II) bis(phosphinoyl)methanediide complex: a stannavinylidene derivative ; loop_ _publ_author_name 'Cheuk-Wai So.' 'Jiayi Guo.' 'Kai-Chung Lau.' 'Kok Hwa Lim.' 'Hong-Wei Xi.' # Attachment 'scw27.cif' data_scw27 _database_code_depnum_ccdc_archive 'CCDC 744565' #TrackingRef 'scw27.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C56 H58 N2 P4 S2 Si2 Sn2, C5 H12' _chemical_formula_sum 'C61 H70 N2 P4 S2 Si2 Sn2' _chemical_formula_weight 1312.75 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 '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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sn Sn -0.6537 1.4246 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c 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 10.8134(3) _cell_length_b 21.6674(5) _cell_length_c 15.5769(4) _cell_angle_alpha 90.00 _cell_angle_beta 108.8510(10) _cell_angle_gamma 90.00 _cell_volume 3453.88(15) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 9736 _cell_measurement_theta_min 2.76 _cell_measurement_theta_max 30.49 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.32 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.262 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1340 _exptl_absorpt_coefficient_mu 0.946 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7518 _exptl_absorpt_correction_T_max 0.7646 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 44780 _diffrn_reflns_av_R_equivalents 0.0570 _diffrn_reflns_av_sigmaI/netI 0.0473 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -31 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.20 _diffrn_reflns_theta_max 30.74 _reflns_number_total 10468 _reflns_number_gt 8676 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.1132P)^2^+2.7364P] 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 10468 _refine_ls_number_parameters 412 _refine_ls_number_restraints 401 _refine_ls_R_factor_all 0.0710 _refine_ls_R_factor_gt 0.0578 _refine_ls_wR_factor_ref 0.2027 _refine_ls_wR_factor_gt 0.1867 _refine_ls_goodness_of_fit_ref 1.208 _refine_ls_restrained_S_all 1.201 _refine_ls_shift/su_max 0.003 _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 C2 C 0.4009(9) 0.3027(3) 0.5193(7) 0.0279(19) Uani 0.649(16) 1 d PDU A 1 C3 C 0.5287(8) 0.2800(3) 0.5402(7) 0.042(2) Uani 0.649(16) 1 d PDU A 1 H3 H 0.5995 0.3078 0.5486 0.051 Uiso 0.649(16) 1 calc PR A 1 C4 C 0.5515(10) 0.2172(4) 0.5486(9) 0.060(3) Uani 0.649(16) 1 d PDU A 1 H4 H 0.6381 0.2020 0.5615 0.072 Uiso 0.649(16) 1 calc PR A 1 C5 C 0.4509(11) 0.1765(4) 0.5385(11) 0.054(3) Uani 0.649(16) 1 d PDU A 1 H5 H 0.4674 0.1334 0.5448 0.065 Uiso 0.649(16) 1 calc PR A 1 C6 C 0.3248(10) 0.1988(3) 0.5191(9) 0.068(3) Uani 0.649(16) 1 d PDU A 1 H6 H 0.2545 0.1709 0.5126 0.081 Uiso 0.649(16) 1 calc PR A 1 C7 C 0.3008(9) 0.2613(3) 0.5092(9) 0.053(2) Uani 0.649(16) 1 d PDU A 1 H7 H 0.2137 0.2760 0.4951 0.063 Uiso 0.649(16) 1 calc PR A 1 C2A C 0.4159(18) 0.3043(5) 0.5241(17) 0.041(4) Uani 0.351(16) 1 d PDU A 2 C3A C 0.5280(15) 0.2835(6) 0.5074(12) 0.046(4) Uani 0.351(16) 1 d PDU A 2 H3A H 0.5813 0.3117 0.4885 0.056 Uiso 0.351(16) 1 calc PR A 2 C4A C 0.5612(19) 0.2223(7) 0.5184(15) 0.063(4) Uani 0.351(16) 1 d PDU A 2 H4A H 0.6376 0.2083 0.5068 0.076 Uiso 0.351(16) 1 calc PR A 2 C5A C 0.485(2) 0.1808(7) 0.546(2) 0.065(5) Uani 0.351(16) 1 d PDU A 2 H5A H 0.5075 0.1382 0.5517 0.078 Uiso 0.351(16) 1 calc PR A 2 C6A C 0.376(2) 0.2018(6) 0.5653(16) 0.070(4) Uani 0.351(16) 1 d PDU A 2 H6A H 0.3263 0.1739 0.5881 0.084 Uiso 0.351(16) 1 calc PR A 2 C7A C 0.3393(19) 0.2629(5) 0.5517(14) 0.052(3) Uani 0.351(16) 1 d PDU A 2 H7A H 0.2613 0.2765 0.5614 0.062 Uiso 0.351(16) 1 calc PR A 2 Sn1 Sn 0.34112(2) 0.531271(10) 0.412568(15) 0.02322(10) Uani 1 1 d . . . C1 C 0.4770(4) 0.42831(16) 0.5966(2) 0.0240(6) Uani 1 1 d . . . C8 C 0.2038(4) 0.39467(17) 0.4970(3) 0.0295(7) Uani 1 1 d . A . C9 C 0.1635(5) 0.4190(2) 0.5655(4) 0.0454(11) Uani 1 1 d . . . H9 H 0.2260 0.4307 0.6215 0.055 Uiso 1 1 calc R . . C10 C 0.0312(6) 0.4262(3) 0.5517(5) 0.0639(16) Uani 1 1 d . . . H10 H 0.0035 0.4426 0.5991 0.077 Uiso 1 1 calc R . . C11 C -0.0596(5) 0.4103(4) 0.4716(5) 0.0708(19) Uani 1 1 d . . . H11 H -0.1500 0.4154 0.4633 0.085 Uiso 1 1 calc R . . C12 C -0.0206(6) 0.3871(4) 0.4031(5) 0.075(2) Uani 1 1 d . . . H12 H -0.0837 0.3766 0.3467 0.090 Uiso 1 1 calc R . . C13 C 0.1115(5) 0.3789(3) 0.4159(4) 0.0568(15) Uani 1 1 d . . . H13 H 0.1384 0.3623 0.3684 0.068 Uiso 1 1 calc R . . C14 C 0.5573(4) 0.53689(19) 0.2285(3) 0.0304(8) Uani 1 1 d . . . C15 C 0.5678(6) 0.5562(3) 0.1461(3) 0.0483(12) Uani 1 1 d . . . H15 H 0.5307 0.5943 0.1202 0.058 Uiso 1 1 calc R . . C16 C 0.6328(6) 0.5194(3) 0.1022(4) 0.0594(15) Uani 1 1 d . . . H16 H 0.6409 0.5330 0.0463 0.071 Uiso 1 1 calc R . . C17 C 0.6859(6) 0.4636(3) 0.1372(4) 0.0559(15) Uani 1 1 d . . . H17 H 0.7312 0.4392 0.1064 0.067 Uiso 1 1 calc R . . C18 C 0.6726(5) 0.4432(3) 0.2189(4) 0.0493(12) Uani 1 1 d . . . H18 H 0.7061 0.4041 0.2431 0.059 Uiso 1 1 calc R . . C19 C 0.6101(5) 0.4804(2) 0.2644(3) 0.0369(9) Uani 1 1 d . . . H19 H 0.6034 0.4672 0.3208 0.044 Uiso 1 1 calc R . . C20 C 0.4542(4) 0.65730(19) 0.2464(3) 0.0334(8) Uani 1 1 d . . . C21 C 0.3354(6) 0.6882(2) 0.2233(4) 0.0549(14) Uani 1 1 d . . . H21 H 0.2591 0.6668 0.2241 0.066 Uiso 1 1 calc R . . C22 C 0.3274(7) 0.7504(2) 0.1990(5) 0.0680(18) Uani 1 1 d . . . H22 H 0.2466 0.7716 0.1859 0.082 Uiso 1 1 calc R . . C23 C 0.4357(8) 0.7807(3) 0.1941(5) 0.074(2) Uani 1 1 d . . . H23 H 0.4295 0.8225 0.1744 0.089 Uiso 1 1 calc R . . C24 C 0.5533(8) 0.7505(3) 0.2176(6) 0.079(2) Uani 1 1 d . . . H24 H 0.6292 0.7720 0.2161 0.095 Uiso 1 1 calc R . . C25 C 0.5627(6) 0.6899(3) 0.2434(4) 0.0567(14) Uani 1 1 d . . . H25 H 0.6451 0.6698 0.2595 0.068 Uiso 1 1 calc R . . C26 C 0.2708(6) 0.4431(3) 0.1359(4) 0.0548(14) Uani 1 1 d . . . H26A H 0.3469 0.4523 0.1170 0.082 Uiso 1 1 calc R . . H26B H 0.2018 0.4248 0.0849 0.082 Uiso 1 1 calc R . . H26C H 0.2960 0.4139 0.1867 0.082 Uiso 1 1 calc R . . C27 C 0.0625(5) 0.4961(4) 0.2034(4) 0.0644(17) Uani 1 1 d . . . H27A H 0.0837 0.4992 0.2693 0.097 Uiso 1 1 calc R . . H27B H 0.0340 0.4540 0.1838 0.097 Uiso 1 1 calc R . . H27C H -0.0078 0.5252 0.1738 0.097 Uiso 1 1 calc R . . C28 C 0.1659(7) 0.5689(3) 0.0724(4) 0.0690(19) Uani 1 1 d . . . H28A H 0.1249 0.6061 0.0870 0.103 Uiso 1 1 calc R . . H28B H 0.1046 0.5484 0.0196 0.103 Uiso 1 1 calc R . . H28C H 0.2450 0.5805 0.0586 0.103 Uiso 1 1 calc R . . C29 C 0.145(3) 0.3539(15) 0.850(2) 0.189(12) Uani 0.50 1 d PDU . . H29A H 0.2056 0.3251 0.8917 0.284 Uiso 0.50 1 calc PR . . H29B H 0.1092 0.3822 0.8852 0.284 Uiso 0.50 1 calc PRD . . H29C H 0.1918 0.3775 0.8167 0.284 Uiso 0.50 1 calc PR . . C30 C 0.036(2) 0.3185(14) 0.785(2) 0.157(9) Uani 0.50 1 d PDU . . H30A H -0.0105 0.2980 0.8221 0.188 Uiso 0.50 1 calc PRD . . H30B H -0.0245 0.3499 0.7481 0.188 Uiso 0.50 1 calc PRD . . C31 C 0.0491(19) 0.2726(13) 0.7216(16) 0.156(8) Uani 0.50 1 d PDU . . H31A H 0.0967 0.2373 0.7576 0.188 Uiso 0.50 1 calc PR . . H31B H 0.1064 0.2903 0.6895 0.188 Uiso 0.50 1 calc PR . . C32 C -0.072(2) 0.2463(15) 0.6488(19) 0.195(10) Uani 0.50 1 d PDU . . H32A H -0.1200 0.2200 0.6794 0.234 Uiso 0.50 1 calc PRD . . H32B H -0.1302 0.2812 0.6204 0.234 Uiso 0.50 1 calc PRD . . C33 C -0.046(3) 0.2093(13) 0.5752(19) 0.180(11) Uani 0.50 1 d PDU . . H33A H -0.1294 0.1944 0.5330 0.270 Uiso 0.50 1 calc PRD . . H33B H 0.0093 0.1740 0.6020 0.270 Uiso 0.50 1 calc PR . . H33C H -0.0023 0.2352 0.5425 0.270 Uiso 0.50 1 calc PR . . N1 N 0.3203(3) 0.54815(14) 0.2664(2) 0.0252(6) Uani 1 1 d . . . P1 P 0.37716(9) 0.38630(4) 0.51113(6) 0.02209(18) Uani 1 1 d D . . P2 P 0.46316(10) 0.57885(4) 0.28789(6) 0.02432(19) Uani 1 1 d . . . S1 S 0.40282(10) 0.41294(4) 0.39293(6) 0.0271(2) Uani 1 1 d . A . Si1 Si 0.20976(12) 0.51514(6) 0.17167(8) 0.0339(2) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C2 0.047(4) 0.017(3) 0.017(3) 0.000(3) 0.006(3) 0.003(3) C3 0.052(4) 0.025(3) 0.053(5) 0.002(3) 0.020(4) 0.006(3) C4 0.074(5) 0.036(4) 0.069(6) 0.000(4) 0.022(5) 0.017(4) C5 0.073(6) 0.021(3) 0.061(5) 0.002(3) 0.012(5) 0.003(4) C6 0.081(6) 0.024(3) 0.084(6) 0.003(4) 0.008(5) -0.016(4) C7 0.066(5) 0.028(3) 0.057(5) 0.008(3) 0.010(4) -0.012(3) C2A 0.057(7) 0.021(7) 0.041(8) 0.002(6) 0.011(7) -0.014(6) C3A 0.063(7) 0.035(6) 0.040(7) 0.003(5) 0.014(6) 0.017(5) C4A 0.083(8) 0.041(6) 0.060(8) -0.002(6) 0.015(7) 0.020(6) C5A 0.084(9) 0.028(7) 0.068(8) 0.000(6) 0.003(8) 0.005(7) C6A 0.093(9) 0.034(6) 0.070(8) 0.012(6) 0.009(7) -0.021(6) C7A 0.074(8) 0.022(5) 0.053(7) 0.007(5) 0.012(6) -0.011(5) Sn1 0.02686(16) 0.02126(14) 0.02415(15) 0.00068(8) 0.01185(11) 0.00048(8) C1 0.0283(17) 0.0216(14) 0.0235(15) 0.0011(12) 0.0104(13) -0.0047(12) C8 0.0258(18) 0.0277(17) 0.0348(19) 0.0023(14) 0.0096(15) -0.0051(14) C9 0.040(3) 0.052(3) 0.050(3) -0.012(2) 0.022(2) -0.004(2) C10 0.045(3) 0.075(4) 0.084(4) -0.019(3) 0.037(3) -0.006(3) C11 0.028(3) 0.103(5) 0.083(5) 0.000(4) 0.020(3) 0.004(3) C12 0.031(3) 0.120(6) 0.064(4) -0.009(4) 0.000(3) -0.008(3) C13 0.033(2) 0.097(5) 0.038(2) -0.015(3) 0.008(2) -0.013(3) C14 0.0281(19) 0.039(2) 0.0265(18) -0.0024(14) 0.0127(15) -0.0050(15) C15 0.059(3) 0.062(3) 0.028(2) 0.004(2) 0.019(2) 0.006(2) C16 0.065(4) 0.092(4) 0.033(2) -0.002(3) 0.032(3) 0.001(3) C17 0.050(3) 0.081(4) 0.045(3) -0.021(3) 0.027(2) 0.000(3) C18 0.043(3) 0.057(3) 0.048(3) -0.009(2) 0.015(2) 0.010(2) C19 0.040(2) 0.041(2) 0.036(2) -0.0021(17) 0.0196(19) 0.0039(17) C20 0.047(2) 0.0284(17) 0.0247(17) 0.0058(14) 0.0107(16) -0.0062(16) C21 0.074(4) 0.031(2) 0.073(4) 0.009(2) 0.041(3) 0.006(2) C22 0.088(5) 0.034(2) 0.096(5) 0.020(3) 0.048(4) 0.013(3) C23 0.106(6) 0.039(3) 0.082(4) 0.024(3) 0.037(4) -0.009(3) C24 0.080(5) 0.052(3) 0.107(6) 0.030(4) 0.033(4) -0.015(3) C25 0.052(3) 0.049(3) 0.066(3) 0.022(3) 0.013(3) -0.012(2) C26 0.072(4) 0.048(3) 0.040(3) -0.018(2) 0.012(2) -0.003(3) C27 0.036(3) 0.107(5) 0.049(3) -0.014(3) 0.011(2) -0.026(3) C28 0.090(5) 0.070(4) 0.031(2) 0.010(2) -0.004(3) 0.002(3) C29 0.134(18) 0.24(3) 0.23(2) 0.02(2) 0.111(18) 0.033(19) C30 0.085(12) 0.195(19) 0.176(18) 0.005(15) 0.023(12) -0.011(13) C31 0.087(11) 0.179(18) 0.212(18) 0.028(14) 0.062(12) -0.019(12) C32 0.124(15) 0.220(19) 0.24(2) -0.023(17) 0.063(15) -0.059(14) C33 0.175(19) 0.185(19) 0.20(2) -0.154(16) 0.087(16) -0.106(16) N1 0.0288(16) 0.0262(13) 0.0195(13) 0.0021(11) 0.0062(12) -0.0007(12) P1 0.0287(5) 0.0167(4) 0.0213(4) 0.0009(3) 0.0087(3) -0.0025(3) P2 0.0305(5) 0.0231(4) 0.0205(4) 0.0016(3) 0.0098(3) -0.0028(3) S1 0.0414(5) 0.0213(4) 0.0220(4) 0.0009(3) 0.0148(4) -0.0002(3) Si1 0.0344(6) 0.0388(6) 0.0241(5) -0.0032(4) 0.0032(4) -0.0030(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C2 C7 1.375(9) . ? C2 C3 1.403(9) . ? C2 P1 1.828(6) . ? C3 C4 1.383(9) . ? C3 H3 0.9500 . ? C4 C5 1.370(10) . ? C4 H4 0.9500 . ? C5 C6 1.385(10) . ? C5 H5 0.9500 . ? C6 C7 1.377(9) . ? C6 H6 0.9500 . ? C7 H7 0.9500 . ? C2A C7A 1.381(12) . ? C2A C3A 1.394(12) . ? C2A P1 1.822(11) . ? C3A C4A 1.371(12) . ? C3A H3A 0.9500 . ? C4A C5A 1.377(13) . ? C4A H4A 0.9500 . ? C5A C6A 1.386(13) . ? C5A H5A 0.9500 . ? C6A C7A 1.380(12) . ? C6A H6A 0.9500 . ? C7A H7A 0.9500 . ? Sn1 C1 2.199(4) 3_666 ? Sn1 N1 2.244(3) . ? Sn1 S1 2.6915(9) . ? C1 P1 1.685(4) . ? C1 P2 1.711(4) 3_666 ? C1 Sn1 2.199(3) 3_666 ? C8 C13 1.376(6) . ? C8 C9 1.380(6) . ? C8 P1 1.824(4) . ? C9 C10 1.385(7) . ? C9 H9 0.9500 . ? C10 C11 1.360(9) . ? C10 H10 0.9500 . ? C11 C12 1.363(10) . ? C11 H11 0.9500 . ? C12 C13 1.389(8) . ? C12 H12 0.9500 . ? C13 H13 0.9500 . ? C14 C19 1.389(6) . ? C14 C15 1.389(6) . ? C14 P2 1.824(4) . ? C15 C16 1.381(8) . ? C15 H15 0.9500 . ? C16 C17 1.373(9) . ? C16 H16 0.9500 . ? C17 C18 1.398(8) . ? C17 H17 0.9500 . ? C18 C19 1.384(6) . ? C18 H18 0.9500 . ? C19 H19 0.9500 . ? C20 C25 1.382(7) . ? C20 C21 1.389(7) . ? C20 P2 1.810(4) . ? C21 C22 1.394(7) . ? C21 H21 0.9500 . ? C22 C23 1.368(10) . ? C22 H22 0.9500 . ? C23 C24 1.370(11) . ? C23 H23 0.9500 . ? C24 C25 1.369(8) . ? C24 H24 0.9500 . ? C25 H25 0.9500 . ? C26 Si1 1.850(6) . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 Si1 1.859(6) . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 Si1 1.871(6) . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 C30 1.494(13) . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 C31 1.438(16) . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? C31 C32 1.538(16) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 C33 1.498(14) . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? N1 P2 1.615(3) . ? N1 Si1 1.726(3) . ? P1 S1 2.0323(12) . ? P2 C1 1.711(4) 3_666 ? 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 C7 C2 C3 118.5(6) . . ? C7 C2 P1 123.5(6) . . ? C3 C2 P1 118.0(6) . . ? C4 C3 C2 120.0(7) . . ? C4 C3 H3 120.0 . . ? C2 C3 H3 120.0 . . ? C5 C4 C3 120.8(8) . . ? C5 C4 H4 119.6 . . ? C3 C4 H4 119.6 . . ? C4 C5 C6 119.3(7) . . ? C4 C5 H5 120.3 . . ? C6 C5 H5 120.3 . . ? C7 C6 C5 120.3(7) . . ? C7 C6 H6 119.9 . . ? C5 C6 H6 119.9 . . ? C2 C7 C6 121.1(7) . . ? C2 C7 H7 119.5 . . ? C6 C7 H7 119.5 . . ? C7A C2A C3A 119.6(10) . . ? C7A C2A P1 121.9(9) . . ? C3A C2A P1 118.5(9) . . ? C4A C3A C2A 119.9(11) . . ? C4A C3A H3A 120.1 . . ? C2A C3A H3A 120.1 . . ? C3A C4A C5A 120.8(11) . . ? C3A C4A H4A 119.6 . . ? C5A C4A H4A 119.6 . . ? C4A C5A C6A 119.3(11) . . ? C4A C5A H5A 120.3 . . ? C6A C5A H5A 120.3 . . ? C7A C6A C5A 120.3(11) . . ? C7A C6A H6A 119.8 . . ? C5A C6A H6A 119.8 . . ? C6A C7A C2A 120.0(11) . . ? C6A C7A H7A 120.0 . . ? C2A C7A H7A 120.0 . . ? C1 Sn1 N1 70.60(12) 3_666 . ? C1 Sn1 S1 96.45(10) 3_666 . ? N1 Sn1 S1 89.27(8) . . ? P1 C1 P2 135.2(2) . 3_666 ? P1 C1 Sn1 121.46(18) . 3_666 ? P2 C1 Sn1 93.58(16) 3_666 3_666 ? C13 C8 C9 119.2(4) . . ? C13 C8 P1 119.9(4) . . ? C9 C8 P1 120.9(3) . . ? C8 C9 C10 119.5(5) . . ? C8 C9 H9 120.3 . . ? C10 C9 H9 120.3 . . ? C11 C10 C9 121.1(6) . . ? C11 C10 H10 119.4 . . ? C9 C10 H10 119.4 . . ? C10 C11 C12 119.8(5) . . ? C10 C11 H11 120.1 . . ? C12 C11 H11 120.1 . . ? C11 C12 C13 119.9(6) . . ? C11 C12 H12 120.0 . . ? C13 C12 H12 120.0 . . ? C8 C13 C12 120.5(5) . . ? C8 C13 H13 119.8 . . ? C12 C13 H13 119.8 . . ? C19 C14 C15 119.4(4) . . ? C19 C14 P2 117.4(3) . . ? C15 C14 P2 123.0(4) . . ? C16 C15 C14 119.4(5) . . ? C16 C15 H15 120.3 . . ? C14 C15 H15 120.3 . . ? C17 C16 C15 121.7(5) . . ? C17 C16 H16 119.1 . . ? C15 C16 H16 119.1 . . ? C16 C17 C18 119.1(5) . . ? C16 C17 H17 120.4 . . ? C18 C17 H17 120.4 . . ? C19 C18 C17 119.5(5) . . ? C19 C18 H18 120.2 . . ? C17 C18 H18 120.2 . . ? C18 C19 C14 120.8(4) . . ? C18 C19 H19 119.6 . . ? C14 C19 H19 119.6 . . ? C25 C20 C21 118.0(4) . . ? C25 C20 P2 122.9(4) . . ? C21 C20 P2 118.9(3) . . ? C20 C21 C22 120.5(6) . . ? C20 C21 H21 119.8 . . ? C22 C21 H21 119.8 . . ? C23 C22 C21 120.1(6) . . ? C23 C22 H22 120.0 . . ? C21 C22 H22 120.0 . . ? C22 C23 C24 119.5(5) . . ? C22 C23 H23 120.2 . . ? C24 C23 H23 120.2 . . ? C25 C24 C23 120.8(6) . . ? C25 C24 H24 119.6 . . ? C23 C24 H24 119.6 . . ? C24 C25 C20 121.1(6) . . ? C24 C25 H25 119.4 . . ? C20 C25 H25 119.4 . . ? Si1 C26 H26A 109.5 . . ? Si1 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? Si1 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? Si1 C27 H27A 109.5 . . ? Si1 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? Si1 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? Si1 C28 H28A 109.5 . . ? Si1 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? Si1 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C30 C29 H29A 109.5 . . ? C30 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C30 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C31 C30 C29 126.3(19) . . ? C31 C30 H30A 105.7 . . ? C29 C30 H30A 105.7 . . ? C31 C30 H30B 105.7 . . ? C29 C30 H30B 105.7 . . ? H30A C30 H30B 106.2 . . ? C30 C31 C32 120.9(19) . . ? C30 C31 H31A 107.1 . . ? C32 C31 H31A 107.1 . . ? C30 C31 H31B 107.1 . . ? C32 C31 H31B 107.1 . . ? H31A C31 H31B 106.8 . . ? C33 C32 C31 116.0(18) . . ? C33 C32 H32A 108.3 . . ? C31 C32 H32A 108.3 . . ? C33 C32 H32B 108.3 . . ? C31 C32 H32B 108.3 . . ? H32A C32 H32B 107.4 . . ? C32 C33 H33A 109.5 . . ? C32 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C32 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? P2 N1 Si1 134.4(2) . . ? P2 N1 Sn1 94.66(14) . . ? Si1 N1 Sn1 127.93(17) . . ? C1 P1 C2A 111.9(8) . . ? C1 P1 C8 114.37(18) . . ? C2A P1 C8 107.5(5) . . ? C1 P1 C2 116.1(3) . . ? C2A P1 C2 5.0(9) . . ? C8 P1 C2 102.8(3) . . ? C1 P1 S1 108.81(12) . . ? C2A P1 S1 106.5(7) . . ? C8 P1 S1 107.36(13) . . ? C2 P1 S1 106.7(3) . . ? N1 P2 C1 101.06(17) . 3_666 ? N1 P2 C20 112.07(19) . . ? C1 P2 C20 114.78(18) 3_666 . ? N1 P2 C14 110.06(18) . . ? C1 P2 C14 113.87(19) 3_666 . ? C20 P2 C14 105.14(19) . . ? P1 S1 Sn1 93.22(4) . . ? N1 Si1 C26 113.1(2) . . ? N1 Si1 C27 106.3(2) . . ? C26 Si1 C27 108.2(3) . . ? N1 Si1 C28 111.7(2) . . ? C26 Si1 C28 107.3(3) . . ? C27 Si1 C28 110.3(3) . . ? _diffrn_measured_fraction_theta_max 0.972 _diffrn_reflns_theta_full 30.74 _diffrn_measured_fraction_theta_full 0.972 _refine_diff_density_max 1.858 _refine_diff_density_min -1.147 _refine_diff_density_rms 0.202 # Attachment 'compound_2.cif' data_scw63s _database_code_depnum_ccdc_archive 'CCDC 751809' #TrackingRef 'compound_2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_absolute_configuration unk _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C34 H48 N2 P2 S Si3 Sn, 0.5(C4 H10 O)' _chemical_formula_sum 'C36 H53 N2 O0.50 P2 S Si3 Sn' _chemical_formula_weight 818.76 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 '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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sn Sn -0.6537 1.4246 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 9.2762(3) _cell_length_b 40.3235(12) _cell_length_c 11.5632(3) _cell_angle_alpha 90.00 _cell_angle_beta 110.8640(10) _cell_angle_gamma 90.00 _cell_volume 4041.6(2) _cell_formula_units_Z 4 _cell_measurement_temperature 103(2) _cell_measurement_reflns_used 9851 _cell_measurement_theta_min 2.42 _cell_measurement_theta_max 27.18 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.346 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1700 _exptl_absorpt_coefficient_mu 0.880 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7197 _exptl_absorpt_correction_T_max 0.9171 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 103(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 46207 _diffrn_reflns_av_R_equivalents 0.0429 _diffrn_reflns_av_sigmaI/netI 0.0614 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -51 _diffrn_reflns_limit_k_max 50 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.40 _diffrn_reflns_theta_max 27.32 _reflns_number_total 17778 _reflns_number_gt 15592 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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. restrains used: omit 0 -1 1 omit 0 0 1 omit 0 -2 1 omit 0 4 0 omit 0 -4 0 omit 0 1 1 omit 0 2 1 omit 1 0 0 omit 1 -1 0 sadi c69 o1 c72 o1 DFIX 1.54 0.02 C69 C70 C71 C72 DFIX 1.4 0.02 C70 O1 O1 C71 ; _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^)+(0.0202P)^2^+3.4809P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.463(12) _refine_ls_number_reflns 17778 _refine_ls_number_parameters 841 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0495 _refine_ls_R_factor_gt 0.0367 _refine_ls_wR_factor_ref 0.0750 _refine_ls_wR_factor_gt 0.0683 _refine_ls_goodness_of_fit_ref 1.043 _refine_ls_restrained_S_all 1.044 _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 C1 C -0.1997(5) 0.28621(9) -0.2264(4) 0.0128(9) Uani 1 1 d . . . C2 C -0.1994(5) 0.27805(10) -0.3436(4) 0.0146(9) Uani 1 1 d . . . H2 H -0.1297 0.2888 -0.3748 0.018 Uiso 1 1 calc R . . C3 C -0.2998(5) 0.25438(10) -0.4144(4) 0.0181(9) Uani 1 1 d . . . H3 H -0.2983 0.2487 -0.4938 0.022 Uiso 1 1 calc R . . C4 C -0.4030(5) 0.23883(11) -0.3699(4) 0.0182(10) Uani 1 1 d . . . H4 H -0.4722 0.2226 -0.4187 0.022 Uiso 1 1 calc R . . C5 C -0.4047(6) 0.24712(11) -0.2538(4) 0.0187(10) Uani 1 1 d . . . H5 H -0.4755 0.2365 -0.2234 0.022 Uiso 1 1 calc R . . C6 C -0.3051(5) 0.27062(10) -0.1825(4) 0.0142(9) Uani 1 1 d . . . H6 H -0.3076 0.2763 -0.1035 0.017 Uiso 1 1 calc R . . C7 C -0.0305(5) 0.34512(10) -0.2339(4) 0.0120(8) Uani 1 1 d . . . C8 C -0.1597(5) 0.36033(11) -0.3222(4) 0.0179(10) Uani 1 1 d . . . H8 H -0.2605 0.3537 -0.3283 0.022 Uiso 1 1 calc R . . C9 C -0.1419(6) 0.38446(11) -0.3991(4) 0.0215(10) Uani 1 1 d . . . H9 H -0.2302 0.3943 -0.4587 0.026 Uiso 1 1 calc R . . C10 C 0.0051(6) 0.39462(12) -0.3905(4) 0.0216(11) Uani 1 1 d . . . H10 H 0.0174 0.4119 -0.4420 0.026 Uiso 1 1 calc R . . C11 C 0.1326(6) 0.37931(11) -0.3065(4) 0.0210(10) Uani 1 1 d . . . H11 H 0.2330 0.3856 -0.3023 0.025 Uiso 1 1 calc R . . C12 C 0.1156(5) 0.35462(10) -0.2276(4) 0.0148(9) Uani 1 1 d . . . H12 H 0.2041 0.3444 -0.1697 0.018 Uiso 1 1 calc R . . C13 C 0.1087(4) 0.29474(11) -0.0346(3) 0.0118(8) Uani 1 1 d . . . H13 H 0.1925 0.3118 -0.0105 0.014 Uiso 1 1 calc R . . C14 C 0.0858(5) 0.22323(9) -0.0440(4) 0.0145(9) Uani 1 1 d . . . C15 C -0.0345(5) 0.20833(10) -0.1397(4) 0.0209(10) Uani 1 1 d . . . H15 H -0.0594 0.2157 -0.2227 0.025 Uiso 1 1 calc R . . C16 C -0.1179(5) 0.18257(10) -0.1125(5) 0.0265(11) Uani 1 1 d . . . H16 H -0.1996 0.1724 -0.1775 0.032 Uiso 1 1 calc R . . C17 C -0.0836(6) 0.17184(12) 0.0063(5) 0.0260(11) Uani 1 1 d . . . H17 H -0.1420 0.1545 0.0237 0.031 Uiso 1 1 calc R . . C18 C 0.0360(6) 0.18628(12) 0.1012(5) 0.0269(11) Uani 1 1 d . . . H18 H 0.0606 0.1785 0.1836 0.032 Uiso 1 1 calc R . . C19 C 0.1214(6) 0.21223(10) 0.0770(4) 0.0214(10) Uani 1 1 d . . . H19 H 0.2029 0.2222 0.1427 0.026 Uiso 1 1 calc R . . C20 C 0.3824(5) 0.25547(10) 0.0377(4) 0.0124(9) Uani 1 1 d . . . C21 C 0.4331(5) 0.27416(10) 0.1471(4) 0.0168(9) Uani 1 1 d . . . H21 H 0.3645 0.2892 0.1642 0.020 Uiso 1 1 calc R . . C22 C 0.5832(6) 0.27079(11) 0.2305(4) 0.0211(10) Uani 1 1 d . . . H22 H 0.6168 0.2835 0.3046 0.025 Uiso 1 1 calc R . . C23 C 0.6836(6) 0.24901(12) 0.2061(5) 0.0233(11) Uani 1 1 d . . . H23 H 0.7861 0.2467 0.2634 0.028 Uiso 1 1 calc R . . C24 C 0.6352(5) 0.23054(12) 0.0982(4) 0.0229(11) Uani 1 1 d . . . H24 H 0.7049 0.2159 0.0807 0.028 Uiso 1 1 calc R . . C25 C 0.4843(5) 0.23344(11) 0.0154(4) 0.0186(10) Uani 1 1 d . . . H25 H 0.4508 0.2202 -0.0573 0.022 Uiso 1 1 calc R . . C26 C 0.2214(6) 0.25622(10) 0.4045(4) 0.0233(11) Uani 1 1 d . . . H26A H 0.1302 0.2461 0.3429 0.035 Uiso 1 1 calc R . . H26B H 0.2371 0.2468 0.4863 0.035 Uiso 1 1 calc R . . H26C H 0.3122 0.2517 0.3825 0.035 Uiso 1 1 calc R . . C27 C 0.3531(5) 0.31807(11) 0.5469(4) 0.0217(10) Uani 1 1 d . . . H27A H 0.4519 0.3139 0.5366 0.032 Uiso 1 1 calc R . . H27B H 0.3514 0.3066 0.6211 0.032 Uiso 1 1 calc R . . H27C H 0.3405 0.3420 0.5557 0.032 Uiso 1 1 calc R . . C28 C 0.0110(6) 0.30914(12) 0.4411(4) 0.0255(12) Uani 1 1 d . . . H28A H -0.0047 0.3330 0.4487 0.038 Uiso 1 1 calc R . . H28B H 0.0194 0.2980 0.5185 0.038 Uiso 1 1 calc R . . H28C H -0.0768 0.3000 0.3731 0.038 Uiso 1 1 calc R . . C29 C 0.2553(5) 0.37004(11) 0.1050(4) 0.0197(10) Uani 1 1 d . . . H29A H 0.3190 0.3547 0.0780 0.030 Uiso 1 1 calc R . . H29B H 0.2936 0.3927 0.1057 0.030 Uiso 1 1 calc R . . H29C H 0.1481 0.3687 0.0477 0.030 Uiso 1 1 calc R . . C30 C 0.4769(6) 0.36107(15) 0.3578(5) 0.0304(14) Uani 1 1 d . . . H30A H 0.4913 0.3650 0.4448 0.046 Uiso 1 1 calc R . . H30B H 0.5230 0.3793 0.3270 0.046 Uiso 1 1 calc R . . H30C H 0.5270 0.3402 0.3504 0.046 Uiso 1 1 calc R . . C31 C 0.1692(6) 0.39215(11) 0.3221(4) 0.0248(11) Uani 1 1 d . . . H31A H 0.0620 0.3946 0.2658 0.037 Uiso 1 1 calc R . . H31B H 0.2243 0.4131 0.3259 0.037 Uiso 1 1 calc R . . H31C H 0.1710 0.3864 0.4049 0.037 Uiso 1 1 calc R . . C32 C -0.2704(6) 0.35402(12) 0.1363(5) 0.0253(12) Uani 1 1 d . . . H32A H -0.3084 0.3316 0.1419 0.038 Uiso 1 1 calc R . . H32B H -0.3433 0.3704 0.1462 0.038 Uiso 1 1 calc R . . H32C H -0.1694 0.3571 0.2018 0.038 Uiso 1 1 calc R . . C33 C -0.1842(6) 0.40230(11) -0.0342(5) 0.0245(11) Uani 1 1 d . . . H33A H -0.0839 0.4063 0.0310 0.037 Uiso 1 1 calc R . . H33B H -0.2593 0.4185 -0.0272 0.037 Uiso 1 1 calc R . . H33C H -0.1740 0.4045 -0.1153 0.037 Uiso 1 1 calc R . . C34 C -0.4460(6) 0.35344(13) -0.1373(5) 0.0307(13) Uani 1 1 d . . . H34A H -0.4396 0.3560 -0.2196 0.046 Uiso 1 1 calc R . . H34B H -0.5176 0.3699 -0.1262 0.046 Uiso 1 1 calc R . . H34C H -0.4832 0.3311 -0.1294 0.046 Uiso 1 1 calc R . . C35 C 0.4274(5) -0.00328(10) 0.5080(4) 0.0127(9) Uani 1 1 d . . . C36 C 0.5726(5) -0.01372(10) 0.5146(4) 0.0163(9) Uani 1 1 d . . . H36 H 0.6618 -0.0039 0.5734 0.020 Uiso 1 1 calc R . . C37 C 0.5888(5) -0.03832(11) 0.4363(4) 0.0178(10) Uani 1 1 d . . . H37 H 0.6888 -0.0453 0.4418 0.021 Uiso 1 1 calc R . . C38 C 0.4601(6) -0.05252(12) 0.3508(4) 0.0203(11) Uani 1 1 d . . . H38 H 0.4717 -0.0695 0.2979 0.024 Uiso 1 1 calc R . . C39 C 0.3137(6) -0.04227(11) 0.3411(4) 0.0224(11) Uani 1 1 d . . . H39 H 0.2253 -0.0522 0.2817 0.027 Uiso 1 1 calc R . . C40 C 0.2967(5) -0.01739(11) 0.4188(4) 0.0176(10) Uani 1 1 d . . . H40 H 0.1966 -0.0100 0.4114 0.021 Uiso 1 1 calc R . . C41 C 0.2664(5) 0.05669(9) 0.5194(4) 0.0130(9) Uani 1 1 d . . . C42 C 0.2716(5) 0.06553(10) 0.4034(4) 0.0163(9) Uani 1 1 d . . . H42 H 0.3422 0.0549 0.3729 0.020 Uiso 1 1 calc R . . C43 C 0.1733(5) 0.08988(11) 0.3337(4) 0.0205(10) Uani 1 1 d . . . H43 H 0.1769 0.0960 0.2554 0.025 Uiso 1 1 calc R . . C44 C 0.0702(5) 0.10524(11) 0.3776(4) 0.0215(10) Uani 1 1 d . . . H44 H 0.0041 0.1221 0.3299 0.026 Uiso 1 1 calc R . . C45 C 0.0625(5) 0.09626(11) 0.4902(4) 0.0205(10) Uani 1 1 d . . . H45 H -0.0103 0.1066 0.5190 0.025 Uiso 1 1 calc R . . C46 C 0.1611(5) 0.07201(10) 0.5620(4) 0.0161(9) Uani 1 1 d . . . H46 H 0.1561 0.0660 0.6400 0.019 Uiso 1 1 calc R . . C47 C 0.5728(5) 0.04610(11) 0.7130(3) 0.0121(8) Uani 1 1 d . . . H47 H 0.6540 0.0285 0.7368 0.015 Uiso 1 1 calc R . . C48 C 0.5485(5) 0.11713(9) 0.6874(4) 0.0136(9) Uani 1 1 d . . . C49 C 0.4524(5) 0.13456(10) 0.5856(4) 0.0188(10) Uani 1 1 d . . . H49 H 0.4475 0.1287 0.5047 0.023 Uiso 1 1 calc R . . C50 C 0.3633(5) 0.16067(11) 0.6024(5) 0.0248(11) Uani 1 1 d . . . H50 H 0.2964 0.1724 0.5326 0.030 Uiso 1 1 calc R . . C51 C 0.3720(6) 0.16947(11) 0.7196(5) 0.0238(11) Uani 1 1 d . . . H51 H 0.3107 0.1872 0.7306 0.029 Uiso 1 1 calc R . . C52 C 0.4699(5) 0.15255(11) 0.8219(5) 0.0226(11) Uani 1 1 d . . . H52 H 0.4766 0.1589 0.9028 0.027 Uiso 1 1 calc R . . C53 C 0.5575(5) 0.12644(10) 0.8059(4) 0.0164(9) Uani 1 1 d . . . H53 H 0.6242 0.1148 0.8760 0.020 Uiso 1 1 calc R . . C54 C 0.8450(5) 0.08541(11) 0.7885(4) 0.0148(9) Uani 1 1 d . . . C55 C 0.9481(5) 0.10819(11) 0.7680(4) 0.0211(10) Uani 1 1 d . . . H55 H 0.9170 0.1206 0.6933 0.025 Uiso 1 1 calc R . . C56 C 1.0940(6) 0.11276(12) 0.8550(5) 0.0245(11) Uani 1 1 d . . . H56 H 1.1628 0.1282 0.8401 0.029 Uiso 1 1 calc R . . C57 C 1.1392(6) 0.09476(12) 0.9633(5) 0.0219(11) Uani 1 1 d . . . H57 H 1.2401 0.0976 1.0227 0.026 Uiso 1 1 calc R . . C58 C 1.0397(5) 0.07277(11) 0.9861(4) 0.0226(10) Uani 1 1 d . . . H58 H 1.0715 0.0609 1.0620 0.027 Uiso 1 1 calc R . . C59 C 0.8924(5) 0.06771(10) 0.8992(4) 0.0180(9) Uani 1 1 d . . . H59 H 0.8247 0.0522 0.9154 0.022 Uiso 1 1 calc R . . C60 C 0.6932(6) 0.08381(11) 1.1469(5) 0.0266(12) Uani 1 1 d . . . H60A H 0.7844 0.0875 1.1245 0.040 Uiso 1 1 calc R . . H60B H 0.7107 0.0934 1.2286 0.040 Uiso 1 1 calc R . . H60C H 0.6034 0.0944 1.0854 0.040 Uiso 1 1 calc R . . C61 C 0.4768(6) 0.03249(13) 1.1858(4) 0.0305(12) Uani 1 1 d . . . H61A H 0.3897 0.0423 1.1190 0.046 Uiso 1 1 calc R . . H61B H 0.4883 0.0435 1.2641 0.046 Uiso 1 1 calc R . . H61C H 0.4576 0.0088 1.1925 0.046 Uiso 1 1 calc R . . C62 C 0.8196(6) 0.02169(12) 1.2885(4) 0.0292(12) Uani 1 1 d . . . H62A H 0.8102 -0.0024 1.2931 0.044 Uiso 1 1 calc R . . H62B H 0.8154 0.0319 1.3642 0.044 Uiso 1 1 calc R . . H62C H 0.9183 0.0271 1.2798 0.044 Uiso 1 1 calc R . . C63 C 0.9316(6) -0.02155(13) 1.0960(5) 0.0306(13) Uani 1 1 d . . . H63A H 0.9842 -0.0025 1.0764 0.046 Uiso 1 1 calc R . . H63B H 0.9732 -0.0421 1.0750 0.046 Uiso 1 1 calc R . . H63C H 0.9482 -0.0214 1.1846 0.046 Uiso 1 1 calc R . . C64 C 0.6247(6) -0.05250(11) 1.0644(4) 0.0273(12) Uani 1 1 d . . . H64A H 0.6321 -0.0471 1.1490 0.041 Uiso 1 1 calc R . . H64B H 0.6765 -0.0737 1.0645 0.041 Uiso 1 1 calc R . . H64C H 0.5159 -0.0542 1.0112 0.041 Uiso 1 1 calc R . . C65 C 0.7071(6) -0.03095(10) 0.8444(4) 0.0201(10) Uani 1 1 d . . . H65A H 0.6010 -0.0279 0.7868 0.030 Uiso 1 1 calc R . . H65B H 0.7370 -0.0542 0.8440 0.030 Uiso 1 1 calc R . . H65C H 0.7767 -0.0169 0.8187 0.030 Uiso 1 1 calc R . . C66 C 0.1856(6) -0.01192(11) 0.8775(4) 0.0229(11) Uani 1 1 d . . . H66A H 0.2870 -0.0143 0.9430 0.034 Uiso 1 1 calc R . . H66B H 0.1149 -0.0286 0.8887 0.034 Uiso 1 1 calc R . . H66C H 0.1450 0.0103 0.8817 0.034 Uiso 1 1 calc R . . C67 C 0.2722(6) -0.06077(11) 0.7084(4) 0.0243(11) Uani 1 1 d . . . H67A H 0.2964 -0.0622 0.6327 0.036 Uiso 1 1 calc R . . H67B H 0.1909 -0.0767 0.7041 0.036 Uiso 1 1 calc R . . H67C H 0.3649 -0.0658 0.7801 0.036 Uiso 1 1 calc R . . C68 C 0.0107(6) -0.01137(14) 0.6026(5) 0.0282(13) Uani 1 1 d . . . H68A H -0.0258 0.0110 0.6102 0.042 Uiso 1 1 calc R . . H68B H -0.0619 -0.0277 0.6132 0.042 Uiso 1 1 calc R . . H68C H 0.0180 -0.0141 0.5207 0.042 Uiso 1 1 calc R . . O1 O 0.6881(4) 0.19247(8) 0.3754(3) 0.0318(8) Uani 1 1 d D . . C69 C 0.9418(6) 0.18425(13) 0.5164(5) 0.0387(13) Uani 1 1 d D . . H69A H 0.9764 0.1813 0.4463 0.058 Uiso 1 1 calc R . . H69B H 1.0066 0.1709 0.5865 0.058 Uiso 1 1 calc R . . H69C H 0.9500 0.2077 0.5403 0.058 Uiso 1 1 calc R . . C71 C 0.5281(6) 0.18515(11) 0.3277(5) 0.0310(11) Uani 1 1 d D . . H71A H 0.4724 0.2041 0.2771 0.037 Uiso 1 1 calc R . . H71B H 0.4912 0.1826 0.3977 0.037 Uiso 1 1 calc R . . C70 C 0.7780(6) 0.17330(12) 0.4802(5) 0.0329(12) Uani 1 1 d D . . H70A H 0.7690 0.1494 0.4589 0.039 Uiso 1 1 calc R . . H70B H 0.7408 0.1768 0.5496 0.039 Uiso 1 1 calc R . . N1 N 0.1820(4) 0.32011(8) 0.2685(3) 0.0119(8) Uani 1 1 d . . . N2 N -0.1153(4) 0.33080(8) -0.0236(3) 0.0136(8) Uani 1 1 d . . . N3 N 0.6407(4) 0.01937(8) 1.0110(3) 0.0133(8) Uani 1 1 d . . . N4 N 0.3414(4) 0.01046(8) 0.7181(3) 0.0115(8) Uani 1 1 d . . . P1 P -0.06012(13) 0.31519(3) -0.12828(10) 0.0103(2) Uani 1 1 d . . . P2 P 0.18891(13) 0.25834(3) -0.07771(10) 0.0121(2) Uani 1 1 d . . . P3 P 0.40059(13) 0.02665(3) 0.61548(10) 0.0110(2) Uani 1 1 d . . . P4 P 0.65649(13) 0.08111(3) 0.66716(10) 0.0113(2) Uani 1 1 d . . . S1 S 0.19219(13) 0.25678(3) -0.24598(10) 0.0180(2) Uani 1 1 d . . . S2 S 0.67292(13) 0.07918(3) 0.50291(10) 0.0178(2) Uani 1 1 d . . . Si1 Si 0.19216(14) 0.30238(3) 0.40837(11) 0.0152(3) Uani 1 1 d . . . Si2 Si 0.26495(15) 0.35853(3) 0.26391(12) 0.0152(3) Uani 1 1 d . . . Si3 Si -0.25141(14) 0.35964(3) -0.01706(12) 0.0144(3) Uani 1 1 d . . . Si4 Si 0.65715(14) 0.03796(3) 1.15123(11) 0.0157(3) Uani 1 1 d . . . Si5 Si 0.71975(15) -0.01896(3) 1.00440(12) 0.0154(3) Uani 1 1 d . . . Si6 Si 0.20453(14) -0.01785(3) 0.72410(12) 0.0148(3) Uani 1 1 d . . . Sn1 Sn 0.00619(3) 0.293646(6) 0.12688(2) 0.01203(7) Uani 1 1 d . . . Sn2 Sn 0.46452(3) 0.046951(5) 0.87155(2) 0.01194(7) Uani 1 1 d . . . C72 C 0.4890(7) 0.15447(13) 0.2504(5) 0.0423(14) Uani 1 1 d D . . H72A H 0.5257 0.1567 0.1811 0.063 Uiso 1 1 calc R . . H72B H 0.3769 0.1513 0.2183 0.063 Uiso 1 1 calc R . . H72C H 0.5387 0.1353 0.3010 0.063 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 C1 0.011(2) 0.009(2) 0.016(2) 0.0006(15) 0.0016(17) 0.0020(16) C2 0.013(2) 0.015(2) 0.015(2) -0.0003(17) 0.0032(18) 0.0013(17) C3 0.019(2) 0.018(2) 0.016(2) -0.0045(17) 0.0041(19) 0.0024(18) C4 0.014(2) 0.013(2) 0.022(2) -0.0044(19) 0.000(2) 0.0002(18) C5 0.023(3) 0.016(2) 0.020(2) 0.0019(18) 0.010(2) -0.0001(19) C6 0.016(2) 0.010(2) 0.018(2) -0.0014(17) 0.0073(19) -0.0023(17) C7 0.014(2) 0.009(2) 0.0114(19) -0.0017(16) 0.0024(18) 0.0016(17) C8 0.015(2) 0.021(2) 0.016(2) 0.0037(18) 0.0035(19) 0.0013(18) C9 0.023(3) 0.016(2) 0.021(2) 0.0053(19) 0.003(2) 0.005(2) C10 0.029(3) 0.012(2) 0.025(3) 0.005(2) 0.011(2) -0.0007(19) C11 0.021(3) 0.022(2) 0.021(2) 0.0026(19) 0.008(2) -0.006(2) C12 0.011(2) 0.021(2) 0.012(2) 0.0019(17) 0.0039(19) -0.0014(18) C13 0.014(2) 0.0097(18) 0.0131(19) -0.0020(19) 0.0068(17) -0.0005(19) C14 0.018(2) 0.0046(19) 0.025(2) -0.0013(17) 0.011(2) 0.0019(16) C15 0.020(3) 0.018(2) 0.021(2) -0.0005(18) 0.003(2) 0.0024(18) C16 0.017(3) 0.011(2) 0.045(3) -0.007(2) 0.003(2) -0.0051(18) C17 0.022(3) 0.020(2) 0.041(3) 0.001(2) 0.017(2) -0.001(2) C18 0.027(3) 0.025(3) 0.029(3) 0.008(2) 0.011(2) -0.001(2) C19 0.026(3) 0.016(2) 0.024(2) -0.0001(18) 0.011(2) -0.0026(19) C20 0.013(2) 0.010(2) 0.014(2) 0.0022(17) 0.0047(19) 0.0013(17) C21 0.018(3) 0.016(2) 0.017(2) 0.0015(17) 0.007(2) -0.0003(18) C22 0.021(3) 0.018(2) 0.020(2) 0.0002(19) 0.002(2) -0.0045(19) C23 0.014(3) 0.025(3) 0.030(3) 0.009(2) 0.008(2) 0.000(2) C24 0.012(2) 0.029(3) 0.028(3) 0.007(2) 0.008(2) 0.010(2) C25 0.019(3) 0.019(2) 0.018(2) 0.0052(18) 0.008(2) 0.0078(19) C26 0.033(3) 0.015(2) 0.019(2) 0.0009(19) 0.006(2) 0.000(2) C27 0.024(3) 0.021(2) 0.017(2) 0.0029(19) 0.005(2) -0.002(2) C28 0.022(3) 0.037(3) 0.021(3) 0.005(2) 0.012(2) 0.004(2) C29 0.022(3) 0.014(2) 0.024(2) -0.0046(18) 0.009(2) -0.0058(19) C30 0.028(3) 0.033(3) 0.029(3) 0.001(2) 0.008(3) -0.013(2) C31 0.036(3) 0.016(2) 0.027(3) -0.007(2) 0.018(2) -0.006(2) C32 0.029(3) 0.022(3) 0.030(3) -0.007(2) 0.016(3) 0.004(2) C33 0.025(3) 0.014(2) 0.034(3) 0.005(2) 0.010(2) 0.008(2) C34 0.018(3) 0.034(3) 0.036(3) -0.006(2) 0.006(2) 0.003(2) C35 0.013(2) 0.012(2) 0.013(2) -0.0008(16) 0.0041(18) 0.0000(17) C36 0.016(2) 0.017(2) 0.011(2) -0.0009(17) 0.0002(19) -0.0004(18) C37 0.015(3) 0.020(2) 0.017(2) -0.0021(18) 0.005(2) 0.0049(19) C38 0.026(3) 0.017(3) 0.017(2) -0.0072(19) 0.008(2) 0.001(2) C39 0.024(3) 0.021(2) 0.019(2) -0.0073(19) 0.003(2) -0.006(2) C40 0.015(2) 0.019(2) 0.019(2) -0.0052(19) 0.006(2) 0.0010(19) C41 0.013(2) 0.011(2) 0.013(2) -0.0018(16) 0.0022(18) -0.0029(16) C42 0.014(2) 0.018(2) 0.015(2) -0.0045(17) 0.0043(19) -0.0014(18) C43 0.023(3) 0.021(2) 0.016(2) 0.0017(18) 0.004(2) -0.006(2) C44 0.016(3) 0.016(2) 0.025(2) 0.0012(19) -0.003(2) 0.0029(19) C45 0.011(2) 0.018(2) 0.031(3) 0.003(2) 0.006(2) 0.0035(18) C46 0.018(3) 0.015(2) 0.016(2) -0.0007(17) 0.006(2) -0.0025(18) C47 0.015(2) 0.0101(19) 0.0112(18) -0.0020(18) 0.0041(16) 0.000(2) C48 0.017(2) 0.009(2) 0.017(2) -0.0045(16) 0.0079(19) -0.0037(17) C49 0.019(2) 0.013(2) 0.023(2) 0.0000(17) 0.005(2) -0.0045(18) C50 0.014(2) 0.018(2) 0.036(3) 0.003(2) 0.002(2) -0.0006(18) C51 0.018(3) 0.010(2) 0.045(3) -0.007(2) 0.013(2) -0.0027(19) C52 0.023(3) 0.014(2) 0.031(3) -0.006(2) 0.010(2) -0.0080(19) C53 0.018(2) 0.010(2) 0.023(2) -0.0015(17) 0.010(2) -0.0031(17) C54 0.013(2) 0.017(2) 0.015(2) -0.0052(18) 0.0057(19) -0.0005(18) C55 0.018(3) 0.022(2) 0.025(2) 0.0016(19) 0.010(2) -0.0029(19) C56 0.019(3) 0.021(3) 0.036(3) -0.007(2) 0.013(2) -0.007(2) C57 0.007(2) 0.026(3) 0.027(3) -0.007(2) -0.001(2) 0.0016(19) C58 0.019(3) 0.024(3) 0.022(2) -0.0016(19) 0.004(2) 0.001(2) C59 0.015(2) 0.015(2) 0.021(2) -0.0032(17) 0.002(2) -0.0035(18) C60 0.026(3) 0.020(3) 0.024(3) -0.010(2) -0.003(2) 0.005(2) C61 0.033(3) 0.044(3) 0.019(3) 0.002(2) 0.015(2) 0.011(2) C62 0.035(3) 0.035(3) 0.015(2) -0.004(2) 0.006(2) 0.006(2) C63 0.030(3) 0.034(3) 0.025(3) 0.000(2) 0.006(2) 0.016(2) C64 0.042(3) 0.020(3) 0.023(3) 0.003(2) 0.015(3) 0.004(2) C65 0.033(3) 0.009(2) 0.020(2) -0.0020(18) 0.011(2) 0.0074(19) C66 0.023(3) 0.022(3) 0.027(3) -0.001(2) 0.013(2) -0.006(2) C67 0.027(3) 0.014(2) 0.032(3) 0.004(2) 0.009(2) -0.005(2) C68 0.016(3) 0.032(3) 0.032(3) 0.011(2) 0.003(2) -0.009(2) O1 0.026(2) 0.0264(18) 0.038(2) 0.0059(15) 0.0055(16) 0.0014(15) C69 0.026(3) 0.033(3) 0.047(3) -0.005(2) 0.001(3) -0.001(2) C71 0.028(3) 0.027(3) 0.036(3) 0.006(2) 0.008(2) 0.001(2) C70 0.033(3) 0.020(2) 0.041(3) 0.010(2) 0.007(3) 0.006(2) N1 0.016(2) 0.0075(18) 0.0106(18) -0.0048(14) 0.0025(16) -0.0017(14) N2 0.015(2) 0.0103(18) 0.0155(19) -0.0021(14) 0.0057(16) -0.0016(15) N3 0.015(2) 0.0125(19) 0.0115(18) -0.0002(14) 0.0042(16) 0.0012(15) N4 0.014(2) 0.0090(18) 0.0118(17) -0.0034(14) 0.0053(15) -0.0006(14) P1 0.0103(6) 0.0095(5) 0.0111(5) -0.0005(4) 0.0037(5) -0.0004(4) P2 0.0114(6) 0.0120(5) 0.0128(5) -0.0010(4) 0.0043(5) 0.0008(4) P3 0.0095(6) 0.0106(5) 0.0122(5) -0.0016(4) 0.0033(5) -0.0006(4) P4 0.0122(6) 0.0090(5) 0.0128(5) -0.0013(4) 0.0045(5) -0.0017(4) S1 0.0197(6) 0.0212(6) 0.0138(5) -0.0003(4) 0.0071(5) 0.0040(5) S2 0.0205(6) 0.0190(5) 0.0164(5) -0.0019(4) 0.0096(5) -0.0046(5) Si1 0.0162(7) 0.0168(6) 0.0119(6) 0.0010(5) 0.0041(5) -0.0015(5) Si2 0.0161(7) 0.0146(7) 0.0148(6) -0.0032(5) 0.0054(5) -0.0043(5) Si3 0.0111(6) 0.0146(7) 0.0163(6) -0.0031(5) 0.0036(5) 0.0020(5) Si4 0.0165(7) 0.0184(7) 0.0115(6) -0.0016(5) 0.0041(5) 0.0019(5) Si5 0.0180(7) 0.0150(7) 0.0135(6) 0.0018(5) 0.0057(6) 0.0040(5) Si6 0.0125(7) 0.0149(6) 0.0161(6) 0.0029(5) 0.0038(5) -0.0038(5) Sn1 0.01211(14) 0.01211(15) 0.01185(15) -0.00019(12) 0.00425(12) -0.00098(12) Sn2 0.01232(14) 0.01145(15) 0.01189(14) -0.00071(11) 0.00412(11) 0.00084(12) C72 0.038(4) 0.039(3) 0.044(3) -0.003(3) 0.008(3) 0.001(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 C1 C2 1.395(6) . ? C1 C6 1.401(6) . ? C1 P1 1.812(4) . ? C2 C3 1.381(6) . ? C2 H2 0.9500 . ? C3 C4 1.388(6) . ? C3 H3 0.9500 . ? C4 C5 1.389(6) . ? C4 H4 0.9500 . ? C5 C6 1.374(6) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C7 C12 1.385(6) . ? C7 C8 1.408(6) . ? C7 P1 1.807(4) . ? C8 C9 1.367(6) . ? C8 H8 0.9500 . ? C9 C10 1.394(6) . ? C9 H9 0.9500 . ? C10 C11 1.381(6) . ? C10 H10 0.9500 . ? C11 C12 1.397(6) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? C13 P1 1.760(4) . ? C13 P2 1.794(4) . ? C13 Sn1 2.379(4) . ? C13 H13 1.0000 . ? C14 C19 1.391(6) . ? C14 C15 1.397(6) . ? C14 P2 1.827(4) . ? C15 C16 1.397(6) . ? C15 H15 0.9500 . ? C16 C17 1.365(7) . ? C16 H16 0.9500 . ? C17 C18 1.381(7) . ? C17 H17 0.9500 . ? C18 C19 1.399(6) . ? C18 H18 0.9500 . ? C19 H19 0.9500 . ? C20 C25 1.387(6) . ? C20 C21 1.402(6) . ? C20 P2 1.819(5) . ? C21 C22 1.389(6) . ? C21 H21 0.9500 . ? C22 C23 1.381(6) . ? C22 H22 0.9500 . ? C23 C24 1.383(7) . ? C23 H23 0.9500 . ? C24 C25 1.391(6) . ? C24 H24 0.9500 . ? C25 H25 0.9500 . ? C26 Si1 1.884(4) . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 Si1 1.869(4) . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 Si1 1.870(5) . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 Si2 1.866(4) . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 Si2 1.880(5) . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 Si2 1.872(4) . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 Si3 1.858(5) . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 Si3 1.864(5) . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C34 Si3 1.862(5) . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 C36 1.386(6) . ? C35 C40 1.402(6) . ? C35 P3 1.812(4) . ? C36 C37 1.387(6) . ? C36 H36 0.9500 . ? C37 C38 1.375(6) . ? C37 H37 0.9500 . ? C38 C39 1.385(6) . ? C38 H38 0.9500 . ? C39 C40 1.392(6) . ? C39 H39 0.9500 . ? C40 H40 0.9500 . ? C41 C46 1.386(6) . ? C41 C42 1.405(5) . ? C41 P3 1.807(4) . ? C42 C43 1.386(6) . ? C42 H42 0.9500 . ? C43 C44 1.379(6) . ? C43 H43 0.9500 . ? C44 C45 1.378(6) . ? C44 H44 0.9500 . ? C45 C46 1.393(6) . ? C45 H45 0.9500 . ? C46 H46 0.9500 . ? C47 P3 1.776(4) . ? C47 P4 1.780(4) . ? C47 Sn2 2.384(4) . ? C47 H47 1.0000 . ? C48 C49 1.388(6) . ? C48 C53 1.394(5) . ? C48 P4 1.826(4) . ? C49 C50 1.394(6) . ? C49 H49 0.9500 . ? C50 C51 1.376(6) . ? C50 H50 0.9500 . ? C51 C52 1.387(7) . ? C51 H51 0.9500 . ? C52 C53 1.382(6) . ? C52 H52 0.9500 . ? C53 H53 0.9500 . ? C54 C59 1.393(6) . ? C54 C55 1.406(6) . ? C54 P4 1.819(5) . ? C55 C56 1.381(7) . ? C55 H55 0.9500 . ? C56 C57 1.378(7) . ? C56 H56 0.9500 . ? C57 C58 1.371(7) . ? C57 H57 0.9500 . ? C58 C59 1.393(6) . ? C58 H58 0.9500 . ? C59 H59 0.9500 . ? C60 Si4 1.883(5) . ? C60 H60A 0.9800 . ? C60 H60B 0.9800 . ? C60 H60C 0.9800 . ? C61 Si4 1.867(5) . ? C61 H61A 0.9800 . ? C61 H61B 0.9800 . ? C61 H61C 0.9800 . ? C62 Si4 1.875(5) . ? C62 H62A 0.9800 . ? C62 H62B 0.9800 . ? C62 H62C 0.9800 . ? C63 Si5 1.874(5) . ? C63 H63A 0.9800 . ? C63 H63B 0.9800 . ? C63 H63C 0.9800 . ? C64 Si5 1.877(5) . ? C64 H64A 0.9800 . ? C64 H64B 0.9800 . ? C64 H64C 0.9800 . ? C65 Si5 1.875(4) . ? C65 H65A 0.9800 . ? C65 H65B 0.9800 . ? C65 H65C 0.9800 . ? C66 Si6 1.859(4) . ? C66 H66A 0.9800 . ? C66 H66B 0.9800 . ? C66 H66C 0.9800 . ? C67 Si6 1.872(5) . ? C67 H67A 0.9800 . ? C67 H67B 0.9800 . ? C67 H67C 0.9800 . ? C68 Si6 1.864(5) . ? C68 H68A 0.9800 . ? C68 H68B 0.9800 . ? C68 H68C 0.9800 . ? O1 C71 1.418(5) . ? O1 C70 1.428(5) . ? C69 C70 1.492(7) . ? C69 H69A 0.9800 . ? C69 H69B 0.9800 . ? C69 H69C 0.9800 . ? C71 C72 1.494(6) . ? C71 H71A 0.9900 . ? C71 H71B 0.9900 . ? C70 H70A 0.9900 . ? C70 H70B 0.9900 . ? N1 Si2 1.739(4) . ? N1 Si1 1.740(4) . ? N1 Sn1 2.139(3) . ? N2 P1 1.601(3) . ? N2 Si3 1.738(4) . ? N2 Sn1 2.269(4) . ? N3 Si5 1.724(4) . ? N3 Si4 1.743(4) . ? N3 Sn2 2.152(4) . ? N4 P3 1.612(3) . ? N4 Si6 1.727(4) . ? N4 Sn2 2.275(3) . ? P1 Sn1 2.9233(11) . ? P2 S1 1.9578(15) . ? P3 Sn2 2.9221(11) . ? P4 S2 1.9603(15) . ? C72 H72A 0.9800 . ? C72 H72B 0.9800 . ? C72 H72C 0.9800 . ? 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 C2 C1 C6 119.3(4) . . ? C2 C1 P1 120.8(3) . . ? C6 C1 P1 119.8(3) . . ? C3 C2 C1 120.3(4) . . ? C3 C2 H2 119.9 . . ? C1 C2 H2 119.9 . . ? C2 C3 C4 120.1(4) . . ? C2 C3 H3 120.0 . . ? C4 C3 H3 120.0 . . ? C3 C4 C5 119.8(4) . . ? C3 C4 H4 120.1 . . ? C5 C4 H4 120.1 . . ? C6 C5 C4 120.6(4) . . ? C6 C5 H5 119.7 . . ? C4 C5 H5 119.7 . . ? C5 C6 C1 119.9(4) . . ? C5 C6 H6 120.0 . . ? C1 C6 H6 120.0 . . ? C12 C7 C8 118.8(4) . . ? C12 C7 P1 122.1(3) . . ? C8 C7 P1 119.0(3) . . ? C9 C8 C7 120.8(4) . . ? C9 C8 H8 119.6 . . ? C7 C8 H8 119.6 . . ? C8 C9 C10 120.3(4) . . ? C8 C9 H9 119.8 . . ? C10 C9 H9 119.8 . . ? C11 C10 C9 119.3(4) . . ? C11 C10 H10 120.3 . . ? C9 C10 H10 120.3 . . ? C10 C11 C12 120.7(4) . . ? C10 C11 H11 119.7 . . ? C12 C11 H11 119.7 . . ? C7 C12 C11 119.9(4) . . ? C7 C12 H12 120.0 . . ? C11 C12 H12 120.0 . . ? P1 C13 P2 125.3(2) . . ? P1 C13 Sn1 88.55(15) . . ? P2 C13 Sn1 121.6(2) . . ? P1 C13 H13 106.4 . . ? P2 C13 H13 106.4 . . ? Sn1 C13 H13 106.4 . . ? C19 C14 C15 119.8(4) . . ? C19 C14 P2 120.5(3) . . ? C15 C14 P2 119.7(3) . . ? C16 C15 C14 119.4(4) . . ? C16 C15 H15 120.3 . . ? C14 C15 H15 120.3 . . ? C17 C16 C15 120.9(5) . . ? C17 C16 H16 119.6 . . ? C15 C16 H16 119.6 . . ? C16 C17 C18 119.9(4) . . ? C16 C17 H17 120.0 . . ? C18 C17 H17 120.0 . . ? C17 C18 C19 120.6(5) . . ? C17 C18 H18 119.7 . . ? C19 C18 H18 119.7 . . ? C14 C19 C18 119.4(4) . . ? C14 C19 H19 120.3 . . ? C18 C19 H19 120.3 . . ? C25 C20 C21 118.7(4) . . ? C25 C20 P2 117.7(3) . . ? C21 C20 P2 123.6(3) . . ? C22 C21 C20 120.4(4) . . ? C22 C21 H21 119.8 . . ? C20 C21 H21 119.8 . . ? C23 C22 C21 120.1(4) . . ? C23 C22 H22 119.9 . . ? C21 C22 H22 119.9 . . ? C22 C23 C24 120.1(5) . . ? C22 C23 H23 120.0 . . ? C24 C23 H23 120.0 . . ? C23 C24 C25 120.0(4) . . ? C23 C24 H24 120.0 . . ? C25 C24 H24 120.0 . . ? C20 C25 C24 120.7(4) . . ? C20 C25 H25 119.6 . . ? C24 C25 H25 119.6 . . ? Si1 C26 H26A 109.5 . . ? Si1 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? Si1 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? Si1 C27 H27A 109.5 . . ? Si1 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? Si1 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? Si1 C28 H28A 109.5 . . ? Si1 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? Si1 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? Si2 C29 H29A 109.5 . . ? Si2 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? Si2 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? Si2 C30 H30A 109.5 . . ? Si2 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? Si2 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? Si2 C31 H31A 109.5 . . ? Si2 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? Si2 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? Si3 C32 H32A 109.5 . . ? Si3 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? Si3 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? Si3 C33 H33A 109.5 . . ? Si3 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? Si3 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? Si3 C34 H34A 109.5 . . ? Si3 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? Si3 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C36 C35 C40 119.1(4) . . ? C36 C35 P3 122.1(3) . . ? C40 C35 P3 118.7(3) . . ? C35 C36 C37 120.7(4) . . ? C35 C36 H36 119.7 . . ? C37 C36 H36 119.7 . . ? C38 C37 C36 119.9(4) . . ? C38 C37 H37 120.0 . . ? C36 C37 H37 120.0 . . ? C37 C38 C39 120.6(4) . . ? C37 C38 H38 119.7 . . ? C39 C38 H38 119.7 . . ? C38 C39 C40 119.7(4) . . ? C38 C39 H39 120.2 . . ? C40 C39 H39 120.2 . . ? C39 C40 C35 120.0(4) . . ? C39 C40 H40 120.0 . . ? C35 C40 H40 120.0 . . ? C46 C41 C42 119.6(4) . . ? C46 C41 P3 119.9(3) . . ? C42 C41 P3 120.4(3) . . ? C43 C42 C41 119.7(4) . . ? C43 C42 H42 120.1 . . ? C41 C42 H42 120.1 . . ? C44 C43 C42 120.2(4) . . ? C44 C43 H43 119.9 . . ? C42 C43 H43 119.9 . . ? C45 C44 C43 120.4(4) . . ? C45 C44 H44 119.8 . . ? C43 C44 H44 119.8 . . ? C44 C45 C46 120.2(4) . . ? C44 C45 H45 119.9 . . ? C46 C45 H45 119.9 . . ? C41 C46 C45 119.8(4) . . ? C41 C46 H46 120.1 . . ? C45 C46 H46 120.1 . . ? P3 C47 P4 123.4(2) . . ? P3 C47 Sn2 87.96(15) . . ? P4 C47 Sn2 124.4(2) . . ? P3 C47 H47 106.3 . . ? P4 C47 H47 106.3 . . ? Sn2 C47 H47 106.3 . . ? C49 C48 C53 119.5(4) . . ? C49 C48 P4 120.6(3) . . ? C53 C48 P4 119.8(3) . . ? C48 C49 C50 119.9(4) . . ? C48 C49 H49 120.1 . . ? C50 C49 H49 120.1 . . ? C51 C50 C49 120.1(4) . . ? C51 C50 H50 119.9 . . ? C49 C50 H50 119.9 . . ? C50 C51 C52 120.3(4) . . ? C50 C51 H51 119.9 . . ? C52 C51 H51 119.9 . . ? C53 C52 C51 119.9(4) . . ? C53 C52 H52 120.1 . . ? C51 C52 H52 120.1 . . ? C52 C53 C48 120.3(4) . . ? C52 C53 H53 119.9 . . ? C48 C53 H53 119.9 . . ? C59 C54 C55 118.5(4) . . ? C59 C54 P4 124.2(3) . . ? C55 C54 P4 117.2(3) . . ? C56 C55 C54 120.9(4) . . ? C56 C55 H55 119.5 . . ? C54 C55 H55 119.5 . . ? C57 C56 C55 119.6(4) . . ? C57 C56 H56 120.2 . . ? C55 C56 H56 120.2 . . ? C58 C57 C56 120.5(5) . . ? C58 C57 H57 119.7 . . ? C56 C57 H57 119.7 . . ? C57 C58 C59 120.7(5) . . ? C57 C58 H58 119.7 . . ? C59 C58 H58 119.7 . . ? C58 C59 C54 119.7(4) . . ? C58 C59 H59 120.1 . . ? C54 C59 H59 120.1 . . ? Si4 C60 H60A 109.5 . . ? Si4 C60 H60B 109.5 . . ? H60A C60 H60B 109.5 . . ? Si4 C60 H60C 109.5 . . ? H60A C60 H60C 109.5 . . ? H60B C60 H60C 109.5 . . ? Si4 C61 H61A 109.5 . . ? Si4 C61 H61B 109.5 . . ? H61A C61 H61B 109.5 . . ? Si4 C61 H61C 109.5 . . ? H61A C61 H61C 109.5 . . ? H61B C61 H61C 109.5 . . ? Si4 C62 H62A 109.5 . . ? Si4 C62 H62B 109.5 . . ? H62A C62 H62B 109.5 . . ? Si4 C62 H62C 109.5 . . ? H62A C62 H62C 109.5 . . ? H62B C62 H62C 109.5 . . ? Si5 C63 H63A 109.5 . . ? Si5 C63 H63B 109.5 . . ? H63A C63 H63B 109.5 . . ? Si5 C63 H63C 109.5 . . ? H63A C63 H63C 109.5 . . ? H63B C63 H63C 109.5 . . ? Si5 C64 H64A 109.5 . . ? Si5 C64 H64B 109.5 . . ? H64A C64 H64B 109.5 . . ? Si5 C64 H64C 109.5 . . ? H64A C64 H64C 109.5 . . ? H64B C64 H64C 109.5 . . ? Si5 C65 H65A 109.5 . . ? Si5 C65 H65B 109.5 . . ? H65A C65 H65B 109.5 . . ? Si5 C65 H65C 109.5 . . ? H65A C65 H65C 109.5 . . ? H65B C65 H65C 109.5 . . ? Si6 C66 H66A 109.5 . . ? Si6 C66 H66B 109.5 . . ? H66A C66 H66B 109.5 . . ? Si6 C66 H66C 109.5 . . ? H66A C66 H66C 109.5 . . ? H66B C66 H66C 109.5 . . ? Si6 C67 H67A 109.5 . . ? Si6 C67 H67B 109.5 . . ? H67A C67 H67B 109.5 . . ? Si6 C67 H67C 109.5 . . ? H67A C67 H67C 109.5 . . ? H67B C67 H67C 109.5 . . ? Si6 C68 H68A 109.5 . . ? Si6 C68 H68B 109.5 . . ? H68A C68 H68B 109.5 . . ? Si6 C68 H68C 109.5 . . ? H68A C68 H68C 109.5 . . ? H68B C68 H68C 109.5 . . ? C71 O1 C70 115.5(3) . . ? C70 C69 H69A 109.5 . . ? C70 C69 H69B 109.5 . . ? H69A C69 H69B 109.5 . . ? C70 C69 H69C 109.5 . . ? H69A C69 H69C 109.5 . . ? H69B C69 H69C 109.5 . . ? O1 C71 C72 113.7(4) . . ? O1 C71 H71A 108.8 . . ? C72 C71 H71A 108.8 . . ? O1 C71 H71B 108.8 . . ? C72 C71 H71B 108.8 . . ? H71A C71 H71B 107.7 . . ? O1 C70 C69 107.9(4) . . ? O1 C70 H70A 110.1 . . ? C69 C70 H70A 110.1 . . ? O1 C70 H70B 110.1 . . ? C69 C70 H70B 110.1 . . ? H70A C70 H70B 108.4 . . ? Si2 N1 Si1 121.1(2) . . ? Si2 N1 Sn1 130.25(19) . . ? Si1 N1 Sn1 106.30(17) . . ? P1 N2 Si3 136.8(2) . . ? P1 N2 Sn1 96.59(16) . . ? Si3 N2 Sn1 125.35(18) . . ? Si5 N3 Si4 121.9(2) . . ? Si5 N3 Sn2 130.7(2) . . ? Si4 N3 Sn2 105.44(17) . . ? P3 N4 Si6 138.2(2) . . ? P3 N4 Sn2 95.99(16) . . ? Si6 N4 Sn2 124.62(18) . . ? N2 P1 C13 99.98(18) . . ? N2 P1 C7 114.53(18) . . ? C13 P1 C7 114.4(2) . . ? N2 P1 C1 112.16(19) . . ? C13 P1 C1 111.34(19) . . ? C7 P1 C1 104.73(18) . . ? N2 P1 Sn1 50.44(13) . . ? C13 P1 Sn1 54.44(12) . . ? C7 P1 Sn1 148.55(14) . . ? C1 P1 Sn1 106.68(13) . . ? C13 P2 C20 104.28(19) . . ? C13 P2 C14 105.93(18) . . ? C20 P2 C14 104.4(2) . . ? C13 P2 S1 117.20(14) . . ? C20 P2 S1 111.50(14) . . ? C14 P2 S1 112.44(14) . . ? N4 P3 C47 100.18(18) . . ? N4 P3 C41 112.54(19) . . ? C47 P3 C41 111.16(19) . . ? N4 P3 C35 113.64(18) . . ? C47 P3 C35 114.65(19) . . ? C41 P3 C35 104.94(19) . . ? N4 P3 Sn2 50.74(12) . . ? C47 P3 Sn2 54.63(12) . . ? C41 P3 Sn2 106.36(13) . . ? C35 P3 Sn2 148.62(14) . . ? C47 P4 C54 104.32(19) . . ? C47 P4 C48 105.98(19) . . ? C54 P4 C48 104.24(19) . . ? C47 P4 S2 116.70(14) . . ? C54 P4 S2 111.46(15) . . ? C48 P4 S2 113.05(14) . . ? N1 Si1 C27 114.85(19) . . ? N1 Si1 C28 111.9(2) . . ? C27 Si1 C28 106.2(2) . . ? N1 Si1 C26 110.15(18) . . ? C27 Si1 C26 106.1(2) . . ? C28 Si1 C26 107.2(2) . . ? N1 Si2 C29 112.62(18) . . ? N1 Si2 C31 111.27(19) . . ? C29 Si2 C31 108.1(2) . . ? N1 Si2 C30 114.5(2) . . ? C29 Si2 C30 103.2(2) . . ? C31 Si2 C30 106.6(2) . . ? N2 Si3 C32 106.1(2) . . ? N2 Si3 C34 113.8(2) . . ? C32 Si3 C34 107.5(2) . . ? N2 Si3 C33 109.7(2) . . ? C32 Si3 C33 111.3(2) . . ? C34 Si3 C33 108.5(2) . . ? N3 Si4 C61 111.1(2) . . ? N3 Si4 C62 114.49(19) . . ? C61 Si4 C62 106.8(2) . . ? N3 Si4 C60 110.8(2) . . ? C61 Si4 C60 107.6(2) . . ? C62 Si4 C60 105.6(2) . . ? N3 Si5 C63 113.7(2) . . ? N3 Si5 C65 113.34(18) . . ? C63 Si5 C65 103.2(2) . . ? N3 Si5 C64 111.5(2) . . ? C63 Si5 C64 106.7(2) . . ? C65 Si5 C64 107.9(2) . . ? N4 Si6 C66 105.90(19) . . ? N4 Si6 C68 113.7(2) . . ? C66 Si6 C68 107.9(2) . . ? N4 Si6 C67 109.3(2) . . ? C66 Si6 C67 111.1(2) . . ? C68 Si6 C67 108.9(2) . . ? N1 Sn1 N2 107.02(13) . . ? N1 Sn1 C13 100.51(13) . . ? N2 Sn1 C13 67.29(13) . . ? N1 Sn1 P1 116.94(9) . . ? N2 Sn1 P1 32.97(9) . . ? C13 Sn1 P1 37.01(10) . . ? N3 Sn2 N4 106.64(13) . . ? N3 Sn2 C47 98.80(13) . . ? N4 Sn2 C47 67.83(13) . . ? N3 Sn2 P3 116.12(9) . . ? N4 Sn2 P3 33.28(9) . . ? C47 Sn2 P3 37.41(10) . . ? C71 C72 H72A 109.5 . . ? C71 C72 H72B 109.5 . . ? H72A C72 H72B 109.5 . . ? C71 C72 H72C 109.5 . . ? H72A C72 H72C 109.5 . . ? H72B C72 H72C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 27.32 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 0.863 _refine_diff_density_min -1.403 _refine_diff_density_rms 0.112 # Attachment 'compound_3.cif' data_scw40 _database_code_depnum_ccdc_archive 'CCDC 761168' #TrackingRef 'compound_3.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C56 H58 N2 P4 S2 Si2 Sn2' _chemical_formula_sum 'C56 H58 N2 P4 S2 Si2 Sn2' _chemical_formula_weight 1240.60 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 '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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sn Sn -0.6537 1.4246 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 10.6210(2) _cell_length_b 12.6848(3) _cell_length_c 20.9770(5) _cell_angle_alpha 90.00 _cell_angle_beta 101.3440(10) _cell_angle_gamma 90.00 _cell_volume 2770.92(11) _cell_formula_units_Z 2 _cell_measurement_temperature 143(2) _cell_measurement_reflns_used 9403 _cell_measurement_theta_min 2.57 _cell_measurement_theta_max 44.85 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.36 _exptl_crystal_size_min 0.28 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.487 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1256 _exptl_absorpt_coefficient_mu 1.174 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6640 _exptl_absorpt_correction_T_max 0.7346 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 143(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 116621 _diffrn_reflns_av_R_equivalents 0.0343 _diffrn_reflns_av_sigmaI/netI 0.0291 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -39 _diffrn_reflns_limit_l_max 41 _diffrn_reflns_theta_min 1.89 _diffrn_reflns_theta_max 45.46 _reflns_number_total 23274 _reflns_number_gt 18471 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0357P)^2^+0.3864P] 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 23274 _refine_ls_number_parameters 310 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0431 _refine_ls_R_factor_gt 0.0268 _refine_ls_wR_factor_ref 0.0793 _refine_ls_wR_factor_gt 0.0667 _refine_ls_goodness_of_fit_ref 1.121 _refine_ls_restrained_S_all 1.121 _refine_ls_shift/su_max 0.006 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Sn1 Sn 0.894993(5) 0.547999(4) 0.055978(3) 0.01198(1) Uani 1 1 d . . . C1 C 0.87349(8) 0.37745(7) 0.03528(4) 0.01288(12) Uani 1 1 d . . . C2 C 0.68570(9) 0.29256(8) 0.10851(5) 0.01670(14) Uani 1 1 d . . . C3 C 0.58616(10) 0.35643(10) 0.12090(6) 0.02384(19) Uani 1 1 d . . . H3 H 0.6037 0.4269 0.1353 0.029 Uiso 1 1 calc R . . C4 C 0.46119(12) 0.31751(13) 0.11237(7) 0.0332(3) Uani 1 1 d . . . H4 H 0.3940 0.3613 0.1211 0.040 Uiso 1 1 calc R . . C5 C 0.43522(12) 0.21510(14) 0.09119(7) 0.0345(3) Uani 1 1 d . . . H5 H 0.3499 0.1888 0.0849 0.041 Uiso 1 1 calc R . . C6 C 0.53291(13) 0.15095(12) 0.07913(7) 0.0316(3) Uani 1 1 d . . . H6 H 0.5148 0.0805 0.0649 0.038 Uiso 1 1 calc R . . C7 C 0.65830(11) 0.18950(9) 0.08778(6) 0.02325(18) Uani 1 1 d . . . H7 H 0.7252 0.1451 0.0795 0.028 Uiso 1 1 calc R . . C8 C 0.95543(9) 0.25872(7) 0.15891(4) 0.01511(13) Uani 1 1 d . . . C9 C 0.92149(10) 0.20142(8) 0.20986(5) 0.01937(16) Uani 1 1 d . . . H9 H 0.8346 0.2000 0.2150 0.023 Uiso 1 1 calc R . . C10 C 1.01469(12) 0.14644(9) 0.25310(5) 0.0246(2) Uani 1 1 d . . . H10 H 0.9915 0.1083 0.2880 0.029 Uiso 1 1 calc R . . C11 C 1.14139(12) 0.14728(10) 0.24530(6) 0.0268(2) Uani 1 1 d . . . H11 H 1.2048 0.1093 0.2747 0.032 Uiso 1 1 calc R . . C12 C 1.17558(11) 0.20358(10) 0.19450(6) 0.0256(2) Uani 1 1 d . . . H12 H 1.2623 0.2037 0.1891 0.031 Uiso 1 1 calc R . . C13 C 1.08326(10) 0.25976(9) 0.15155(5) 0.01977(16) Uani 1 1 d . . . H13 H 1.1072 0.2989 0.1172 0.024 Uiso 1 1 calc R . . C14 C 0.77383(12) 0.45840(9) 0.27193(5) 0.02267(18) Uani 1 1 d . . . H14A H 0.6875 0.4791 0.2495 0.034 Uiso 1 1 calc R . . H14B H 0.7920 0.4896 0.3155 0.034 Uiso 1 1 calc R . . H14C H 0.7787 0.3814 0.2755 0.034 Uiso 1 1 calc R . . C15 C 1.05830(11) 0.46422(10) 0.26752(5) 0.02322(19) Uani 1 1 d . . . H15A H 1.0601 0.3874 0.2728 0.035 Uiso 1 1 calc R . . H15B H 1.0787 0.4979 0.3104 0.035 Uiso 1 1 calc R . . H15C H 1.1219 0.4853 0.2419 0.035 Uiso 1 1 calc R . . C16 C 0.89115(14) 0.65333(9) 0.22122(6) 0.0267(2) Uani 1 1 d . . . H16A H 0.9545 0.6784 0.1965 0.040 Uiso 1 1 calc R . . H16B H 0.9118 0.6819 0.2655 0.040 Uiso 1 1 calc R . . H16C H 0.8053 0.6770 0.1999 0.040 Uiso 1 1 calc R . . C17 C 1.09428(9) 0.77804(7) 0.06576(5) 0.01625(14) Uani 1 1 d . . . C18 C 1.11987(13) 0.81216(10) 0.13045(6) 0.0270(2) Uani 1 1 d . . . H18 H 1.1837 0.7775 0.1615 0.032 Uiso 1 1 calc R . . C19 C 1.05247(17) 0.89641(11) 0.14952(7) 0.0363(3) Uani 1 1 d . . . H19 H 1.0712 0.9201 0.1933 0.044 Uiso 1 1 calc R . . C20 C 0.95833(18) 0.94565(11) 0.10487(9) 0.0399(4) Uani 1 1 d . . . H20 H 0.9114 1.0026 0.1181 0.048 Uiso 1 1 calc R . . C21 C 0.93184(16) 0.91238(12) 0.04077(9) 0.0388(3) Uani 1 1 d . . . H21 H 0.8669 0.9466 0.0102 0.047 Uiso 1 1 calc R . . C22 C 1.00038(12) 0.82856(9) 0.02103(6) 0.0256(2) Uani 1 1 d . . . H22 H 0.9826 0.8062 -0.0231 0.031 Uiso 1 1 calc R . . C23 C 1.34679(8) 0.69823(7) 0.06244(4) 0.01477(13) Uani 1 1 d . . . C24 C 1.43487(10) 0.61900(10) 0.05666(6) 0.02429(19) Uani 1 1 d . . . H24 H 1.4054 0.5497 0.0448 0.029 Uiso 1 1 calc R . . C25 C 1.56506(11) 0.64104(12) 0.06814(8) 0.0320(3) Uani 1 1 d . . . H25 H 1.6245 0.5865 0.0645 0.038 Uiso 1 1 calc R . . C26 C 1.60942(11) 0.74217(12) 0.08498(6) 0.0292(2) Uani 1 1 d . . . H26 H 1.6987 0.7573 0.0919 0.035 Uiso 1 1 calc R . . C27 C 1.52283(12) 0.82026(11) 0.09150(7) 0.0286(2) Uani 1 1 d . . . H27 H 1.5529 0.8892 0.1040 0.034 Uiso 1 1 calc R . . C28 C 1.39145(10) 0.79926(9) 0.08002(6) 0.02321(18) Uani 1 1 d . . . H28 H 1.3325 0.8539 0.0842 0.028 Uiso 1 1 calc R . . N1 N 0.85767(8) 0.46333(6) 0.14497(4) 0.01401(11) Uani 1 1 d . . . P1 P 0.84332(2) 0.348955(18) 0.110387(11) 0.01189(3) Uani 1 1 d . . . P2 P 1.17767(2) 0.663890(18) 0.041910(11) 0.01146(3) Uani 1 1 d . . . S1 S 1.15001(2) 0.544012(18) 0.102439(11) 0.01414(3) Uani 1 1 d . . . Si1 Si 0.89475(3) 0.50632(2) 0.224647(13) 0.01550(4) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Sn1 0.01115(2) 0.01213(2) 0.01285(2) 0.00082(2) 0.00280(2) 0.00044(2) C1 0.0132(3) 0.0138(3) 0.0115(3) -0.0009(2) 0.0020(2) -0.0013(2) C2 0.0152(3) 0.0197(4) 0.0152(3) 0.0029(3) 0.0029(3) -0.0032(3) C3 0.0162(4) 0.0288(5) 0.0277(5) 0.0012(4) 0.0074(3) -0.0011(3) C4 0.0167(4) 0.0497(8) 0.0348(6) 0.0026(6) 0.0087(4) -0.0028(5) C5 0.0216(5) 0.0529(8) 0.0285(6) 0.0052(5) 0.0034(4) -0.0171(5) C6 0.0310(6) 0.0333(6) 0.0293(6) 0.0006(5) 0.0027(4) -0.0177(5) C7 0.0233(4) 0.0219(4) 0.0237(4) 0.0010(3) 0.0025(3) -0.0067(3) C8 0.0162(3) 0.0150(3) 0.0134(3) 0.0009(2) 0.0012(2) 0.0013(3) C9 0.0231(4) 0.0188(4) 0.0157(3) 0.0042(3) 0.0025(3) -0.0005(3) C10 0.0335(5) 0.0209(4) 0.0170(4) 0.0057(3) -0.0008(4) 0.0014(4) C11 0.0300(5) 0.0257(5) 0.0204(4) 0.0024(4) -0.0056(4) 0.0092(4) C12 0.0205(4) 0.0314(5) 0.0227(4) 0.0011(4) -0.0012(3) 0.0086(4) C13 0.0168(4) 0.0250(4) 0.0167(4) 0.0019(3) 0.0015(3) 0.0035(3) C14 0.0250(5) 0.0277(5) 0.0177(4) 0.0016(3) 0.0101(3) 0.0023(4) C15 0.0211(4) 0.0303(5) 0.0170(4) -0.0009(3) 0.0008(3) -0.0018(4) C16 0.0427(7) 0.0173(4) 0.0212(4) -0.0027(3) 0.0087(4) -0.0008(4) C17 0.0176(3) 0.0137(3) 0.0186(4) -0.0016(3) 0.0064(3) 0.0002(3) C18 0.0383(6) 0.0230(5) 0.0212(4) -0.0064(4) 0.0096(4) 0.0041(4) C19 0.0549(9) 0.0253(5) 0.0340(6) -0.0098(5) 0.0215(6) 0.0040(6) C20 0.0510(9) 0.0227(5) 0.0532(9) -0.0040(5) 0.0279(8) 0.0119(5) C21 0.0380(7) 0.0283(6) 0.0509(9) 0.0012(6) 0.0109(6) 0.0173(5) C22 0.0264(5) 0.0212(4) 0.0286(5) -0.0008(4) 0.0040(4) 0.0084(4) C23 0.0122(3) 0.0178(3) 0.0138(3) -0.0014(3) 0.0015(2) -0.0025(3) C24 0.0137(4) 0.0247(5) 0.0346(6) -0.0051(4) 0.0050(3) -0.0008(3) C25 0.0131(4) 0.0376(7) 0.0452(7) -0.0011(6) 0.0057(4) 0.0007(4) C26 0.0145(4) 0.0450(7) 0.0266(5) 0.0037(5) 0.0003(3) -0.0092(4) C27 0.0222(5) 0.0304(6) 0.0312(5) -0.0030(4) 0.0002(4) -0.0131(4) C28 0.0185(4) 0.0215(4) 0.0281(5) -0.0045(4) 0.0009(3) -0.0062(3) N1 0.0166(3) 0.0141(3) 0.0120(3) -0.0003(2) 0.0045(2) -0.0004(2) P1 0.01188(8) 0.01252(8) 0.01129(8) 0.00106(6) 0.00230(6) -0.00022(6) P2 0.01080(8) 0.01228(8) 0.01118(8) -0.00105(6) 0.00190(6) -0.00076(6) S1 0.01356(8) 0.01590(9) 0.01219(8) 0.00182(6) 0.00070(6) -0.00182(6) Si1 0.01896(11) 0.01657(11) 0.01162(9) -0.00097(8) 0.00459(8) -0.00004(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Sn1 C1 2.2094(9) . ? Sn1 N1 2.2554(8) . ? Sn1 S1 2.6926(2) . ? Sn1 P1 2.8679(2) . ? C1 P2 1.6870(9) 3_765 ? C1 P1 1.7071(9) . ? C2 C7 1.3903(15) . ? C2 C3 1.3964(15) . ? C2 P1 1.8138(9) . ? C3 C4 1.3942(16) . ? C3 H3 0.9500 . ? C4 C5 1.383(2) . ? C4 H4 0.9500 . ? C5 C6 1.381(2) . ? C5 H5 0.9500 . ? C6 C7 1.3966(16) . ? C6 H6 0.9500 . ? C7 H7 0.9500 . ? C8 C13 1.3963(14) . ? C8 C9 1.3973(13) . ? C8 P1 1.8131(9) . ? C9 C10 1.3914(15) . ? C9 H9 0.9500 . ? C10 C11 1.3873(19) . ? C10 H10 0.9500 . ? C11 C12 1.3893(18) . ? C11 H11 0.9500 . ? C12 C13 1.3905(15) . ? C12 H12 0.9500 . ? C13 H13 0.9500 . ? C14 Si1 1.8719(11) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 Si1 1.8700(12) . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 Si1 1.8662(12) . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 C22 1.3847(16) . ? C17 C18 1.3991(15) . ? C17 P2 1.8182(9) . ? C18 C19 1.3882(17) . ? C18 H18 0.9500 . ? C19 C20 1.378(3) . ? C19 H19 0.9500 . ? C20 C21 1.384(3) . ? C20 H20 0.9500 . ? C21 C22 1.3966(17) . ? C21 H21 0.9500 . ? C22 H22 0.9500 . ? C23 C28 1.3910(14) . ? C23 C24 1.3944(15) . ? C23 P2 1.8159(9) . ? C24 C25 1.3847(16) . ? C24 H24 0.9500 . ? C25 C26 1.388(2) . ? C25 H25 0.9500 . ? C26 C27 1.377(2) . ? C26 H26 0.9500 . ? C27 C28 1.3942(16) . ? C27 H27 0.9500 . ? C28 H28 0.9500 . ? N1 P1 1.6158(8) . ? N1 Si1 1.7283(8) . ? P2 C1 1.6870(9) 3_765 ? P2 S1 2.0390(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Sn1 N1 70.62(3) . . ? C1 Sn1 S1 96.34(2) . . ? N1 Sn1 S1 91.12(2) . . ? C1 Sn1 P1 36.46(2) . . ? N1 Sn1 P1 34.19(2) . . ? S1 Sn1 P1 95.568(7) . . ? P2 C1 P1 137.44(5) 3_765 . ? P2 C1 Sn1 119.62(5) 3_765 . ? P1 C1 Sn1 93.26(4) . . ? C7 C2 C3 118.96(10) . . ? C7 C2 P1 120.88(8) . . ? C3 C2 P1 119.77(8) . . ? C4 C3 C2 120.48(12) . . ? C4 C3 H3 119.8 . . ? C2 C3 H3 119.8 . . ? C5 C4 C3 119.90(13) . . ? C5 C4 H4 120.1 . . ? C3 C4 H4 120.1 . . ? C6 C5 C4 120.19(11) . . ? C6 C5 H5 119.9 . . ? C4 C5 H5 119.9 . . ? C5 C6 C7 120.11(13) . . ? C5 C6 H6 119.9 . . ? C7 C6 H6 119.9 . . ? C2 C7 C6 120.36(12) . . ? C2 C7 H7 119.8 . . ? C6 C7 H7 119.8 . . ? C13 C8 C9 119.49(9) . . ? C13 C8 P1 118.52(7) . . ? C9 C8 P1 121.20(7) . . ? C10 C9 C8 120.13(10) . . ? C10 C9 H9 119.9 . . ? C8 C9 H9 119.9 . . ? C11 C10 C9 120.10(10) . . ? C11 C10 H10 119.9 . . ? C9 C10 H10 119.9 . . ? C10 C11 C12 120.03(10) . . ? C10 C11 H11 120.0 . . ? C12 C11 H11 120.0 . . ? C11 C12 C13 120.20(11) . . ? C11 C12 H12 119.9 . . ? C13 C12 H12 119.9 . . ? C12 C13 C8 120.04(10) . . ? C12 C13 H13 120.0 . . ? C8 C13 H13 120.0 . . ? Si1 C14 H14A 109.5 . . ? Si1 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? Si1 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? Si1 C15 H15A 109.5 . . ? Si1 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? Si1 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? Si1 C16 H16A 109.5 . . ? Si1 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? Si1 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C22 C17 C18 119.38(10) . . ? C22 C17 P2 120.46(8) . . ? C18 C17 P2 120.07(8) . . ? C19 C18 C17 120.32(13) . . ? C19 C18 H18 119.8 . . ? C17 C18 H18 119.8 . . ? C20 C19 C18 119.96(13) . . ? C20 C19 H19 120.0 . . ? C18 C19 H19 120.0 . . ? C19 C20 C21 120.25(12) . . ? C19 C20 H20 119.9 . . ? C21 C20 H20 119.9 . . ? C20 C21 C22 120.12(14) . . ? C20 C21 H21 119.9 . . ? C22 C21 H21 119.9 . . ? C17 C22 C21 119.96(12) . . ? C17 C22 H22 120.0 . . ? C21 C22 H22 120.0 . . ? C28 C23 C24 119.18(9) . . ? C28 C23 P2 123.62(8) . . ? C24 C23 P2 117.11(7) . . ? C25 C24 C23 120.23(11) . . ? C25 C24 H24 119.9 . . ? C23 C24 H24 119.9 . . ? C24 C25 C26 120.55(12) . . ? C24 C25 H25 119.7 . . ? C26 C25 H25 119.7 . . ? C27 C26 C25 119.36(10) . . ? C27 C26 H26 120.3 . . ? C25 C26 H26 120.3 . . ? C26 C27 C28 120.72(11) . . ? C26 C27 H27 119.6 . . ? C28 C27 H27 119.6 . . ? C23 C28 C27 119.96(11) . . ? C23 C28 H28 120.0 . . ? C27 C28 H28 120.0 . . ? P1 N1 Si1 134.51(5) . . ? P1 N1 Sn1 94.15(3) . . ? Si1 N1 Sn1 127.33(4) . . ? N1 P1 C1 101.89(4) . . ? N1 P1 C8 108.74(4) . . ? C1 P1 C8 115.47(4) . . ? N1 P1 C2 111.66(4) . . ? C1 P1 C2 113.79(4) . . ? C8 P1 C2 105.35(4) . . ? N1 P1 Sn1 51.66(3) . . ? C1 P1 Sn1 50.28(3) . . ? C8 P1 Sn1 128.55(3) . . ? C2 P1 Sn1 125.92(3) . . ? C1 P2 C23 114.77(4) 3_765 . ? C1 P2 C17 115.43(5) 3_765 . ? C23 P2 C17 104.86(4) . . ? C1 P2 S1 107.89(3) 3_765 . ? C23 P2 S1 106.75(3) . . ? C17 P2 S1 106.55(3) . . ? P2 S1 Sn1 91.058(10) . . ? N1 Si1 C16 106.20(5) . . ? N1 Si1 C15 112.86(5) . . ? C16 Si1 C15 108.30(6) . . ? N1 Si1 C14 111.12(5) . . ? C16 Si1 C14 109.51(5) . . ? C15 Si1 C14 108.77(5) . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 45.46 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.922 _refine_diff_density_min -1.548 _refine_diff_density_rms 0.277