Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'G. Nikonov' _publ_contact_author_address ; Department of Chemistry Brock University St. Catharines Ontario L2S 3A1 CANADA ; _publ_contact_author_email GNIKONOV@BROCKU.CA _publ_section_title ; Synthesis and structural studies of germyl and germyl/stannyl substituted tungstenocenes ; loop_ _publ_author_name 'G. Nikonov' 'Andrei V. Churakov' 'Konstantin Yu. Dorogov' 'J. Howard' 'Andrey Yu. Khalimon' ; L.G.Kuzmin ; 'Dmitry A. Lemenovskii' data_1 _database_code_depnum_ccdc_archive 'CCDC 632228' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C12 H17 Cl Ge W' _chemical_formula_sum 'C12 H17 Cl Ge W' _chemical_formula_weight 453.15 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ge Ge 0.1547 1.8001 '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 'P 21/n' _symmetry_space_group_name_Hall '-P 2yn' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 11.7637(7) _cell_length_b 8.6051(5) _cell_length_c 13.7051(8) _cell_angle_alpha 90.00 _cell_angle_beta 112.080(1) _cell_angle_gamma 90.00 _cell_volume 1285.59(13) _cell_formula_units_Z 4 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 6791 _cell_measurement_theta_min 2.859 _cell_measurement_theta_max 29.881 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.32 _exptl_crystal_size_min 0.28 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.341 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 848 _exptl_absorpt_coefficient_mu 11.452 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.0976 _exptl_absorpt_correction_T_max 0.1418 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(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 SMART 1K' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 8382 _diffrn_reflns_av_R_equivalents 0.0289 _diffrn_reflns_av_sigmaI/netI 0.0357 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.95 _diffrn_reflns_theta_max 29.00 _reflns_number_total 3327 _reflns_number_gt 3106 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0395P)^2^+1.5409P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00070(13) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 3327 _refine_ls_number_parameters 205 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0305 _refine_ls_R_factor_gt 0.0277 _refine_ls_wR_factor_ref 0.0707 _refine_ls_wR_factor_gt 0.0695 _refine_ls_goodness_of_fit_ref 1.100 _refine_ls_restrained_S_all 1.100 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group W1 W 0.736913(14) 0.563690(16) -0.005245(11) 0.01243(7) Uani 1 1 d . . . Ge1 Ge 0.70432(4) 0.27037(5) -0.00820(3) 0.01568(10) Uani 1 1 d . . . Cl1 Cl 0.88442(10) 0.13213(12) 0.05916(12) 0.0376(3) Uani 1 1 d . . . C1 C 0.7998(4) 0.4880(5) 0.1719(3) 0.0225(9) Uani 1 1 d . . . C2 C 0.8900(4) 0.5837(5) 0.1595(4) 0.0246(9) Uani 1 1 d . . . C3 C 0.8350(5) 0.7332(6) 0.1259(3) 0.0326(12) Uani 1 1 d . . . C4 C 0.7100(5) 0.7239(6) 0.1152(4) 0.0350(12) Uani 1 1 d . . . C5 C 0.6897(5) 0.5722(6) 0.1439(4) 0.0305(11) Uani 1 1 d . . . C6 C 0.7895(5) 0.4859(5) -0.1465(3) 0.0234(9) Uani 1 1 d . . . C7 C 0.8664(4) 0.6125(5) -0.0958(3) 0.0224(8) Uani 1 1 d . . . C8 C 0.7901(4) 0.7437(5) -0.1038(4) 0.0236(9) Uani 1 1 d . . . C9 C 0.6652(4) 0.6998(5) -0.1583(3) 0.0241(9) Uani 1 1 d . . . C10 C 0.6656(5) 0.5391(6) -0.1841(3) 0.0266(10) Uani 1 1 d . . . C11 C 0.6272(5) 0.1612(6) -0.1433(4) 0.0321(11) Uani 1 1 d . . . C12 C 0.6198(5) 0.1811(5) 0.0782(4) 0.0246(9) Uani 1 1 d . . . H1 H 0.592(5) 0.541(6) -0.037(4) 0.026(14) Uiso 1 1 d . . . H1A H 0.806(5) 0.388(6) 0.207(4) 0.032(15) Uiso 1 1 d . . . H2A H 0.975(8) 0.550(7) 0.177(6) 0.06(2) Uiso 1 1 d . . . H3A H 0.881(6) 0.815(7) 0.116(4) 0.042(16) Uiso 1 1 d . . . H4A H 0.658(7) 0.797(8) 0.100(5) 0.06(2) Uiso 1 1 d . . . H5A H 0.612(8) 0.510(10) 0.130(6) 0.07(2) Uiso 1 1 d . . . H6A H 0.813(5) 0.389(6) -0.154(4) 0.023(13) Uiso 1 1 d . . . H7A H 0.957(5) 0.622(6) -0.062(4) 0.020(12) Uiso 1 1 d . . . H8A H 0.812(5) 0.847(7) -0.080(4) 0.034(15) Uiso 1 1 d . . . H9A H 0.592(5) 0.766(6) -0.172(4) 0.027(14) Uiso 1 1 d . . . H10A H 0.594(5) 0.472(6) -0.230(4) 0.018(12) Uiso 1 1 d . . . H11A H 0.620(6) 0.049(6) -0.123(5) 0.034(16) Uiso 1 1 d . . . H11B H 0.666(6) 0.161(7) -0.189(4) 0.035(16) Uiso 1 1 d . . . H11C H 0.549(8) 0.224(10) -0.184(7) 0.09(3) Uiso 1 1 d . . . H12A H 0.599(8) 0.079(8) 0.071(6) 0.06(2) Uiso 1 1 d . . . H12B H 0.543(6) 0.245(7) 0.060(5) 0.045(17) Uiso 1 1 d . . . H12C H 0.659(6) 0.187(7) 0.147(5) 0.050(19) Uiso 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 W1 0.01417(10) 0.01158(10) 0.01021(10) -0.00017(4) 0.00307(6) 0.00006(4) Ge1 0.0172(2) 0.01211(18) 0.0160(2) -0.00197(14) 0.00429(15) -0.00168(14) Cl1 0.0203(5) 0.0153(5) 0.0695(9) 0.0004(5) 0.0081(5) 0.0023(4) C1 0.032(2) 0.021(2) 0.0113(18) -0.0020(15) 0.0043(16) -0.0003(17) C2 0.019(2) 0.038(2) 0.014(2) -0.0046(16) 0.0027(16) 0.0004(17) C3 0.054(3) 0.025(2) 0.0125(19) -0.0055(16) 0.005(2) -0.018(2) C4 0.048(3) 0.030(2) 0.020(2) -0.0047(19) 0.005(2) 0.021(2) C5 0.022(2) 0.053(3) 0.016(2) -0.0080(18) 0.0069(18) -0.0020(19) C6 0.034(2) 0.021(2) 0.021(2) -0.0019(16) 0.0171(18) -0.0031(18) C7 0.026(2) 0.026(2) 0.018(2) 0.0041(17) 0.0121(17) -0.0026(17) C8 0.029(2) 0.020(2) 0.021(2) 0.0056(16) 0.0087(17) -0.0024(16) C9 0.025(2) 0.028(2) 0.0161(19) 0.0113(17) 0.0037(16) 0.0024(17) C10 0.034(3) 0.034(2) 0.013(2) 0.0004(17) 0.0099(18) -0.0094(19) C11 0.044(3) 0.028(2) 0.023(2) -0.0089(19) 0.010(2) -0.012(2) C12 0.032(2) 0.022(2) 0.020(2) 0.0036(17) 0.0096(18) -0.0053(17) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag W1 C4 2.262(5) . ? W1 C3 2.265(4) . ? W1 C9 2.270(4) . ? W1 C10 2.283(4) . ? W1 C8 2.292(4) . ? W1 C2 2.305(4) . ? W1 C5 2.312(5) . ? W1 C7 2.336(4) . ? W1 C6 2.340(4) . ? W1 C1 2.349(4) . ? W1 Ge1 2.5510(4) . ? W1 H1 1.60(6) . ? Ge1 C12 1.966(5) . ? Ge1 C11 1.968(5) . ? Ge1 Cl1 2.2991(11) . ? C1 C2 1.403(7) . ? C1 C5 1.406(7) . ? C1 H1A 0.97(5) . ? C2 C3 1.436(7) . ? C2 H2A 0.98(8) . ? C3 C4 1.424(8) . ? C3 H3A 0.93(6) . ? C4 C5 1.410(8) . ? C4 H4A 0.85(7) . ? C5 H5A 1.01(8) . ? C6 C7 1.419(6) . ? C6 C10 1.426(7) . ? C6 H6A 0.90(5) . ? C7 C8 1.421(6) . ? C7 H7A 0.99(5) . ? C8 C9 1.426(6) . ? C8 H8A 0.95(6) . ? C9 C10 1.428(7) . ? C9 H9A 0.99(5) . ? C10 H10A 1.02(5) . ? C11 H11A 1.02(5) . ? C11 H11B 0.90(6) . ? C11 H11C 1.03(9) . ? C12 H12A 0.91(7) . ? C12 H12B 1.00(6) . ? C12 H12C 0.88(7) . ? 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 C4 W1 C3 36.7(2) . . ? C4 W1 C9 104.73(18) . . ? C3 W1 C9 107.60(17) . . ? C4 W1 C10 138.08(19) . . ? C3 W1 C10 141.60(17) . . ? C9 W1 C10 36.55(17) . . ? C4 W1 C8 99.3(2) . . ? C3 W1 C8 82.06(17) . . ? C9 W1 C8 36.44(16) . . ? C10 W1 C8 60.08(17) . . ? C4 W1 C2 60.78(18) . . ? C3 W1 C2 36.61(17) . . ? C9 W1 C2 138.49(17) . . ? C10 W1 C2 153.54(19) . . ? C8 W1 C2 103.96(17) . . ? C4 W1 C5 35.9(2) . . ? C3 W1 C5 59.89(19) . . ? C9 W1 C5 132.16(18) . . ? C10 W1 C5 147.01(19) . . ? C8 W1 C5 135.19(18) . . ? C2 W1 C5 59.37(18) . . ? C4 W1 C7 125.2(2) . . ? C3 W1 C7 93.80(18) . . ? C9 W1 C7 60.43(16) . . ? C10 W1 C7 59.74(17) . . ? C8 W1 C7 35.75(16) . . ? C2 W1 C7 94.69(17) . . ? C5 W1 C7 152.29(17) . . ? C4 W1 C6 158.53(19) . . ? C3 W1 C6 128.77(18) . . ? C9 W1 C6 60.34(17) . . ? C10 W1 C6 35.91(18) . . ? C8 W1 C6 59.35(16) . . ? C2 W1 C6 118.67(17) . . ? C5 W1 C6 165.07(16) . . ? C7 W1 C6 35.33(15) . . ? C4 W1 C1 59.40(17) . . ? C3 W1 C1 59.33(16) . . ? C9 W1 C1 164.06(16) . . ? C10 W1 C1 158.46(16) . . ? C8 W1 C1 138.35(16) . . ? C2 W1 C1 35.07(16) . . ? C5 W1 C1 35.10(17) . . ? C7 W1 C1 125.74(16) . . ? C6 W1 C1 134.21(17) . . ? C4 W1 Ge1 123.59(15) . . ? C3 W1 Ge1 132.73(12) . . ? C9 W1 Ge1 119.63(12) . . ? C10 W1 Ge1 84.20(12) . . ? C8 W1 Ge1 137.07(12) . . ? C2 W1 Ge1 98.44(12) . . ? C5 W1 Ge1 87.74(13) . . ? C7 W1 Ge1 107.06(11) . . ? C6 W1 Ge1 77.81(11) . . ? C1 W1 Ge1 74.28(10) . . ? C4 W1 H1 81.2(18) . . ? C3 W1 H1 117.8(18) . . ? C9 W1 H1 80.0(19) . . ? C10 W1 H1 77.0(19) . . ? C8 W1 H1 115.0(18) . . ? C2 W1 H1 129.2(19) . . ? C5 W1 H1 70.0(19) . . ? C7 W1 H1 135.8(19) . . ? C6 W1 H1 109.0(19) . . ? C1 W1 H1 97.7(19) . . ? Ge1 W1 H1 74.7(17) . . ? C12 Ge1 C11 102.8(2) . . ? C12 Ge1 Cl1 98.86(15) . . ? C11 Ge1 Cl1 99.21(18) . . ? C12 Ge1 W1 118.97(14) . . ? C11 Ge1 W1 120.06(16) . . ? Cl1 Ge1 W1 113.28(3) . . ? C2 C1 C5 109.0(4) . . ? C2 C1 W1 70.8(2) . . ? C5 C1 W1 71.0(3) . . ? C2 C1 H1A 131(4) . . ? C5 C1 H1A 119(4) . . ? W1 C1 H1A 133(3) . . ? C1 C2 C3 107.2(4) . . ? C1 C2 W1 74.2(2) . . ? C3 C2 W1 70.2(2) . . ? C1 C2 H2A 123(4) . . ? C3 C2 H2A 130(4) . . ? W1 C2 H2A 125(4) . . ? C4 C3 C2 107.8(4) . . ? C4 C3 W1 71.6(3) . . ? C2 C3 W1 73.2(3) . . ? C4 C3 H3A 132(4) . . ? C2 C3 H3A 120(4) . . ? W1 C3 H3A 121(4) . . ? C5 C4 C3 107.5(4) . . ? C5 C4 W1 74.0(3) . . ? C3 C4 W1 71.8(3) . . ? C5 C4 H4A 125(5) . . ? C3 C4 H4A 127(5) . . ? W1 C4 H4A 124(5) . . ? C1 C5 C4 108.6(5) . . ? C1 C5 W1 73.9(3) . . ? C4 C5 W1 70.1(3) . . ? C1 C5 H5A 117(5) . . ? C4 C5 H5A 132(5) . . ? W1 C5 H5A 109(5) . . ? C7 C6 C10 107.9(4) . . ? C7 C6 W1 72.2(2) . . ? C10 C6 W1 69.8(3) . . ? C7 C6 H6A 127(4) . . ? C10 C6 H6A 125(4) . . ? W1 C6 H6A 124(3) . . ? C6 C7 C8 107.7(4) . . ? C6 C7 W1 72.5(2) . . ? C8 C7 W1 70.4(3) . . ? C6 C7 H7A 132(3) . . ? C8 C7 H7A 120(3) . . ? W1 C7 H7A 125(3) . . ? C7 C8 C9 109.0(4) . . ? C7 C8 W1 73.8(2) . . ? C9 C8 W1 71.0(2) . . ? C7 C8 H8A 129(4) . . ? C9 C8 H8A 121(3) . . ? W1 C8 H8A 122(3) . . ? C8 C9 C10 106.7(4) . . ? C8 C9 W1 72.6(2) . . ? C10 C9 W1 72.2(2) . . ? C8 C9 H9A 127(3) . . ? C10 C9 H9A 127(3) . . ? W1 C9 H9A 118(3) . . ? C6 C10 C9 108.6(4) . . ? C6 C10 W1 74.2(3) . . ? C9 C10 W1 71.2(2) . . ? C6 C10 H10A 123(3) . . ? C9 C10 H10A 128(3) . . ? W1 C10 H10A 127(3) . . ? Ge1 C11 H11A 105(3) . . ? Ge1 C11 H11B 118(4) . . ? H11A C11 H11B 108(5) . . ? Ge1 C11 H11C 105(5) . . ? H11A C11 H11C 119(6) . . ? H11B C11 H11C 102(6) . . ? Ge1 C12 H12A 120(5) . . ? Ge1 C12 H12B 105(3) . . ? H12A C12 H12B 109(7) . . ? Ge1 C12 H12C 116(4) . . ? H12A C12 H12C 100(6) . . ? H12B C12 H12C 107(5) . . ? _diffrn_measured_fraction_theta_max 0.973 _diffrn_reflns_theta_full 29.00 _diffrn_measured_fraction_theta_full 0.973 _refine_diff_density_max 3.385 _refine_diff_density_min -2.077 _refine_diff_density_rms 0.268 data_3 _database_code_depnum_ccdc_archive 'CCDC 632229' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C14 H22 Cl2 Ge Sn W' _chemical_formula_sum 'C14 H22 Cl2 Ge Sn W' _chemical_formula_weight 636.35 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' 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' Ge Ge 0.1547 1.8001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 13.7812(3) _cell_length_b 8.9668(2) _cell_length_c 29.2034(6) _cell_angle_alpha 90.00 _cell_angle_beta 100.515(1) _cell_angle_gamma 90.00 _cell_volume 3548.16(13) _cell_formula_units_Z 8 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 7841 _cell_measurement_theta_min 2.677 _cell_measurement_theta_max 30.490 _exptl_crystal_description block _exptl_crystal_colour yellow-orange _exptl_crystal_size_max 0.34 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.26 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.382 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2368 _exptl_absorpt_coefficient_mu 9.835 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.1348 _exptl_absorpt_correction_T_max 0.1842 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(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 SMART 6K' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 28307 _diffrn_reflns_av_R_equivalents 0.0269 _diffrn_reflns_av_sigmaI/netI 0.0278 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -39 _diffrn_reflns_limit_l_max 39 _diffrn_reflns_theta_min 1.50 _diffrn_reflns_theta_max 28.50 _reflns_number_total 8965 _reflns_number_gt 7887 _reflns_threshold_expression I>2\s(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0191P)^2^+9.7235P] 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 8965 _refine_ls_number_parameters 394 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0322 _refine_ls_R_factor_gt 0.0265 _refine_ls_wR_factor_ref 0.0595 _refine_ls_wR_factor_gt 0.0578 _refine_ls_goodness_of_fit_ref 1.055 _refine_ls_restrained_S_all 1.055 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group W1 W 0.392794(11) 0.902441(17) 0.124176(5) 0.01800(4) Uani 1 1 d . . . W2 W 0.109777(11) 0.409231(17) 0.877276(5) 0.01883(4) Uani 1 1 d . . . Sn1' Sn 0.49380(2) 1.08091(4) 0.189280(11) 0.02329(7) Uani 0.60 1 d P A . Sn1 Sn 0.33574(3) 1.15296(4) 0.080245(12) 0.02464(8) Uani 0.40 1 d P A . Ge1' Ge 0.33574(3) 1.15296(4) 0.080245(12) 0.02464(8) Uani 0.60 1 d P A 5 Cl1' Cl 0.5266(2) 1.3242(4) 0.16036(13) 0.0515(7) Uani 0.60 1 d P A 1 Cl2' Cl 0.2185(6) 1.0838(9) 0.0150(3) 0.057(2) Uani 0.60 1 d P A 1 C11' C 0.6483(9) 1.0488(14) 0.2105(5) 0.034(2) Uani 0.60 1 d P A 1 H11A H 0.6746 1.1237 0.2340 0.051 Uiso 0.60 1 calc PR A 1 H11B H 0.6808 1.0591 0.1835 0.051 Uiso 0.60 1 calc PR A 1 H11C H 0.6608 0.9489 0.2238 0.051 Uiso 0.60 1 calc PR A 1 C12' C 0.4322(14) 1.137(2) 0.2500(5) 0.046(4) Uani 0.60 1 d P A 1 H12A H 0.4779 1.2030 0.2703 0.070 Uiso 0.60 1 calc PR A 1 H12B H 0.4218 1.0460 0.2669 0.070 Uiso 0.60 1 calc PR A 1 H12C H 0.3690 1.1885 0.2402 0.070 Uiso 0.60 1 calc PR A 1 C13' C 0.2474(9) 1.2882(14) 0.1083(5) 0.024(2) Uani 0.60 1 d P A 1 H13A H 0.2322 1.3769 0.0887 0.036 Uiso 0.60 1 calc PR A 1 H13B H 0.2805 1.3184 0.1395 0.036 Uiso 0.60 1 calc PR A 1 H13C H 0.1860 1.2358 0.1105 0.036 Uiso 0.60 1 calc PR A 1 C14' C 0.4226(11) 1.2708(15) 0.0499(5) 0.036(3) Uani 0.60 1 d P A 1 H14A H 0.3875 1.3595 0.0360 0.054 Uiso 0.60 1 calc PR A 1 H14B H 0.4444 1.2113 0.0255 0.054 Uiso 0.60 1 calc PR A 1 H14C H 0.4802 1.3016 0.0729 0.054 Uiso 0.60 1 calc PR A 1 Ge1 Ge 0.49380(2) 1.08091(4) 0.189280(11) 0.02329(7) Uani 0.40 1 d P A 5 Cl1 Cl 0.5123(4) 1.3467(6) 0.17265(16) 0.0423(12) Uiso 0.40 1 d P A 2 Cl2 Cl 0.2134(6) 1.0819(8) 0.0156(3) 0.0230(17) Uani 0.40 1 d P A 2 C11 C 0.6372(16) 1.026(3) 0.2205(7) 0.036(5) Uiso 0.40 1 d P A 2 H11D H 0.6625 1.1009 0.2441 0.054 Uiso 0.40 1 calc PR A 2 H11E H 0.6793 1.0232 0.1968 0.054 Uiso 0.40 1 calc PR A 2 H11F H 0.6375 0.9278 0.2353 0.054 Uiso 0.40 1 calc PR A 2 C12 C 0.438(2) 1.155(3) 0.2410(8) 0.045(7) Uiso 0.40 1 d P A 2 H12D H 0.4859 1.2201 0.2603 0.068 Uiso 0.40 1 calc PR A 2 H12E H 0.4221 1.0707 0.2597 0.068 Uiso 0.40 1 calc PR A 2 H12F H 0.3778 1.2113 0.2291 0.068 Uiso 0.40 1 calc PR A 2 C13 C 0.2634(16) 1.312(3) 0.1138(8) 0.029(5) Uiso 0.40 1 d P A 2 H13D H 0.2464 1.3981 0.0933 0.043 Uiso 0.40 1 calc PR A 2 H13E H 0.3068 1.3439 0.1425 0.043 Uiso 0.40 1 calc PR A 2 H13F H 0.2030 1.2685 0.1214 0.043 Uiso 0.40 1 calc PR A 2 C14 C 0.4187(18) 1.282(3) 0.0386(7) 0.035(5) Uiso 0.40 1 d P A 2 H14D H 0.3803 1.3694 0.0262 0.053 Uiso 0.40 1 calc PR A 2 H14E H 0.4326 1.2204 0.0128 0.053 Uiso 0.40 1 calc PR A 2 H14F H 0.4810 1.3138 0.0579 0.053 Uiso 0.40 1 calc PR A 2 Sn2 Sn 0.14596(2) 0.65581(4) 0.930111(11) 0.02245(7) Uani 0.60 1 d P B . Sn2' Sn 0.06220(3) 0.59951(4) 0.809442(13) 0.02865(9) Uani 0.40 1 d P B . Ge2 Ge 0.06220(3) 0.59951(4) 0.809442(13) 0.02865(9) Uani 0.60 1 d P B 5 Cl3 Cl 0.2000(3) 0.5536(9) 1.0088(2) 0.0283(16) Uani 0.60 1 d P B 3 C11A C 0.1346(14) 0.608(4) 0.7556(9) 0.048(5) Uani 0.60 1 d P B 3 H11G H 0.1051 0.6855 0.7337 0.071 Uiso 0.60 1 calc PR B 3 H11H H 0.1298 0.5115 0.7398 0.071 Uiso 0.60 1 calc PR B 3 H11I H 0.2041 0.6323 0.7672 0.071 Uiso 0.60 1 calc PR B 3 C12A C -0.0671(9) 0.6259(16) 0.7720(4) 0.048(3) Uani 0.60 1 d P B 3 H12G H -0.0648 0.7057 0.7493 0.072 Uiso 0.60 1 calc PR B 3 H12H H -0.1141 0.6526 0.7921 0.072 Uiso 0.60 1 calc PR B 3 H12I H -0.0881 0.5328 0.7555 0.072 Uiso 0.60 1 calc PR B 3 Ge2' Ge 0.14596(2) 0.65581(4) 0.930111(11) 0.02245(7) Uani 0.40 1 d P B 5 Cl3' Cl 0.2032(8) 0.5597(15) 1.0070(4) 0.044(3) Uani 0.40 1 d P B 4 C11B C 0.1606(19) 0.621(5) 0.7625(11) 0.033(5) Uani 0.40 1 d P B 4 H11J H 0.1352 0.6953 0.7388 0.050 Uiso 0.40 1 calc PR B 4 H11K H 0.1670 0.5245 0.7475 0.050 Uiso 0.40 1 calc PR B 4 H11L H 0.2253 0.6526 0.7794 0.050 Uiso 0.40 1 calc PR B 4 C12B C -0.0953(14) 0.616(3) 0.7772(8) 0.044(5) Uiso 0.40 1 d P B 4 H12J H -0.1033 0.6904 0.7521 0.066 Uiso 0.40 1 calc PR B 4 H12K H -0.1336 0.6470 0.8008 0.066 Uiso 0.40 1 calc PR B 4 H12L H -0.1189 0.5192 0.7644 0.066 Uiso 0.40 1 calc PR B 4 Cl4 Cl 0.07773(15) 0.85529(16) 0.83122(6) 0.0651(5) Uani 1 1 d . . . C1 C 0.5474(3) 0.8104(5) 0.12639(17) 0.0342(10) Uani 1 1 d . A . H1A H 0.5998 0.7981 0.1547 0.041 Uiso 1 1 calc R . . C2 C 0.5345(3) 0.9353(5) 0.09577(18) 0.0340(10) Uani 1 1 d . A . H2A H 0.5760 1.0276 0.0993 0.041 Uiso 1 1 calc R . . C3 C 0.4606(4) 0.8992(5) 0.05656(16) 0.0319(10) Uani 1 1 d . A . H3A H 0.4395 0.9632 0.0285 0.038 Uiso 1 1 calc R . . C4 C 0.4262(3) 0.7565(5) 0.06312(15) 0.0297(9) Uani 1 1 d . A . H4A H 0.3764 0.7000 0.0405 0.036 Uiso 1 1 calc R . . C5 C 0.4802(3) 0.7002(5) 0.10568(17) 0.0315(10) Uani 1 1 d . A . H5A H 0.4754 0.5965 0.1177 0.038 Uiso 1 1 calc R . . C6 C 0.2509(3) 0.7598(5) 0.11651(16) 0.0326(10) Uani 1 1 d . A . H6A H 0.2250 0.6922 0.0899 0.039 Uiso 1 1 calc R . . C7 C 0.2229(3) 0.9096(5) 0.12114(15) 0.0300(9) Uani 1 1 d . A . H7A H 0.1742 0.9670 0.0982 0.036 Uiso 1 1 calc R . . C8 C 0.2720(3) 0.9622(5) 0.16538(14) 0.0250(8) Uani 1 1 d . A . H8A H 0.2622 1.0618 0.1792 0.030 Uiso 1 1 calc R . . C9 C 0.3276(3) 0.8405(5) 0.18882(14) 0.0266(8) Uani 1 1 d . A . H9A H 0.3637 0.8403 0.2218 0.032 Uiso 1 1 calc R . . C10 C 0.3147(3) 0.7177(5) 0.15842(16) 0.0311(9) Uani 1 1 d . A . H10A H 0.3411 0.6151 0.1661 0.037 Uiso 1 1 calc R . . C1A C 0.2789(3) 0.4035(5) 0.90718(15) 0.0299(9) Uani 1 1 d . B . H1AA H 0.3135 0.4592 0.9351 0.036 Uiso 1 1 calc R . . C2A C 0.2624(3) 0.4560(5) 0.86036(15) 0.0270(9) Uani 1 1 d . B . H2AA H 0.2853 0.5537 0.8497 0.032 Uiso 1 1 calc R . . C3A C 0.2183(3) 0.3382(5) 0.83070(15) 0.0270(9) Uani 1 1 d . B . H3AA H 0.2057 0.3380 0.7959 0.032 Uiso 1 1 calc R . . C4A C 0.2064(3) 0.2160(5) 0.85989(17) 0.0313(10) Uani 1 1 d . B . H4AA H 0.1823 0.1146 0.8491 0.038 Uiso 1 1 calc R . . C5A C 0.2429(3) 0.2576(5) 0.90682(16) 0.0327(10) Uani 1 1 d . B . H5AA H 0.2477 0.1908 0.9346 0.039 Uiso 1 1 calc R . . C6A C -0.0498(3) 0.3419(6) 0.84905(17) 0.0348(10) Uani 1 1 d . B . H6AA H -0.0837 0.3438 0.8157 0.042 Uiso 1 1 calc R . . C7A C -0.0500(3) 0.4581(5) 0.88254(17) 0.0310(10) Uani 1 1 d . B . H7AA H -0.0836 0.5568 0.8762 0.037 Uiso 1 1 calc R . . C8A C -0.0048(3) 0.4043(5) 0.92728(17) 0.0340(10) Uani 1 1 d . B . H8AA H 0.0005 0.4589 0.9575 0.041 Uiso 1 1 calc R . . C9A C 0.0259(3) 0.2561(6) 0.92130(18) 0.0377(11) Uani 1 1 d . B . H9AA H 0.0569 0.1872 0.9467 0.045 Uiso 1 1 calc R . . C10A C -0.0023(3) 0.2184(5) 0.87338(19) 0.0371(11) Uani 1 1 d . B . H10B H 0.0049 0.1176 0.8597 0.045 Uiso 1 1 calc R . . C13A C 0.0348(4) 0.7895(6) 0.94697(19) 0.0446(12) Uani 1 1 d . B 6 H13G H 0.0642 0.8737 0.9660 0.067 Uiso 1 1 calc R B 6 H13H H -0.0059 0.7309 0.9645 0.067 Uiso 1 1 calc R B 6 H13I H -0.0063 0.8270 0.9183 0.067 Uiso 1 1 calc R B 6 C14A C 0.2693(4) 0.7852(6) 0.92771(19) 0.0437(12) Uani 1 1 d . B 6 H14G H 0.2702 0.8706 0.9487 0.065 Uiso 1 1 calc R B 6 H14H H 0.2671 0.8211 0.8958 0.065 Uiso 1 1 calc R B 6 H14I H 0.3289 0.7252 0.9374 0.065 Uiso 1 1 calc R B 6 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 0.01686(7) 0.01609(7) 0.02213(8) -0.00046(6) 0.00645(5) -0.00065(6) W2 0.01591(7) 0.01689(8) 0.02475(8) -0.00298(6) 0.00652(6) -0.00118(6) Sn1' 0.02086(15) 0.02026(15) 0.02776(16) -0.00291(13) 0.00183(12) -0.00247(12) Sn1 0.02589(17) 0.02462(18) 0.02464(17) 0.00318(14) 0.00785(13) 0.00688(14) Ge1' 0.02589(17) 0.02462(18) 0.02464(17) 0.00318(14) 0.00785(13) 0.00688(14) Cl1' 0.0504(16) 0.0404(15) 0.067(2) 0.0134(15) 0.0207(15) -0.0085(12) Cl2' 0.070(4) 0.065(4) 0.029(4) 0.002(3) -0.012(3) 0.007(3) C11' 0.029(5) 0.031(5) 0.041(6) -0.002(5) 0.007(4) -0.004(4) C12' 0.059(7) 0.055(8) 0.027(6) -0.028(6) 0.013(6) -0.029(6) C13' 0.018(5) 0.020(5) 0.032(5) -0.001(4) -0.001(4) 0.001(4) C14' 0.049(6) 0.033(5) 0.028(6) 0.015(5) 0.011(5) 0.006(4) Ge1 0.02086(15) 0.02026(15) 0.02776(16) -0.00291(13) 0.00183(12) -0.00247(12) Cl2 0.028(3) 0.020(3) 0.021(4) 0.005(2) 0.005(3) 0.002(2) Sn2 0.01939(14) 0.02607(16) 0.02231(14) -0.00738(13) 0.00488(11) -0.00274(12) Sn2' 0.0388(2) 0.02458(18) 0.02176(16) 0.00282(14) 0.00341(15) 0.00379(16) Ge2 0.0388(2) 0.02458(18) 0.02176(16) 0.00282(14) 0.00341(15) 0.00379(16) Cl3 0.0214(16) 0.039(3) 0.024(3) -0.0012(19) 0.0041(16) 0.0016(16) C11A 0.039(12) 0.063(9) 0.039(9) 0.023(7) 0.002(8) 0.006(10) C12A 0.036(6) 0.060(7) 0.045(6) 0.025(5) -0.002(5) 0.008(5) Ge2' 0.01939(14) 0.02607(16) 0.02231(14) -0.00738(13) 0.00488(11) -0.00274(12) Cl3' 0.076(6) 0.034(5) 0.016(4) -0.007(3) -0.008(3) -0.004(4) C11B 0.017(11) 0.061(12) 0.022(9) 0.022(9) 0.004(8) 0.002(9) Cl4 0.1060(14) 0.0310(7) 0.0546(9) -0.0041(6) 0.0051(9) -0.0064(8) C1 0.0186(19) 0.039(3) 0.045(3) -0.011(2) 0.0048(18) 0.0079(18) C2 0.029(2) 0.026(2) 0.054(3) -0.009(2) 0.026(2) -0.0022(18) C3 0.042(3) 0.028(2) 0.033(2) 0.0028(18) 0.023(2) 0.0097(19) C4 0.029(2) 0.030(2) 0.031(2) -0.0105(18) 0.0103(17) 0.0037(18) C5 0.034(2) 0.019(2) 0.044(3) -0.0039(18) 0.014(2) 0.0051(17) C6 0.028(2) 0.037(2) 0.036(2) -0.010(2) 0.0128(18) -0.0166(19) C7 0.0137(17) 0.047(3) 0.032(2) 0.004(2) 0.0097(16) -0.0050(18) C8 0.0190(18) 0.030(2) 0.029(2) 0.0014(17) 0.0126(16) 0.0007(16) C9 0.029(2) 0.027(2) 0.0258(19) 0.0036(17) 0.0117(16) -0.0023(17) C10 0.038(2) 0.024(2) 0.036(2) 0.0066(18) 0.0188(19) -0.0051(18) C1A 0.0172(18) 0.039(2) 0.032(2) -0.0110(19) 0.0022(16) 0.0051(17) C2A 0.0201(18) 0.028(2) 0.035(2) -0.0029(18) 0.0131(17) -0.0040(16) C3A 0.0205(18) 0.033(2) 0.030(2) -0.0074(18) 0.0101(16) 0.0018(17) C4A 0.0200(19) 0.025(2) 0.052(3) -0.008(2) 0.0138(19) 0.0022(16) C5A 0.026(2) 0.035(2) 0.039(2) 0.010(2) 0.0084(18) 0.0128(18) C6A 0.0181(19) 0.043(3) 0.044(3) -0.012(2) 0.0066(18) -0.0074(19) C7A 0.0163(18) 0.031(2) 0.048(3) -0.008(2) 0.0120(18) -0.0031(17) C8A 0.027(2) 0.041(3) 0.038(2) -0.009(2) 0.0190(19) -0.0118(19) C9A 0.029(2) 0.038(3) 0.051(3) 0.011(2) 0.017(2) -0.008(2) C10A 0.027(2) 0.027(2) 0.063(3) -0.011(2) 0.022(2) -0.0114(18) C13A 0.038(3) 0.050(3) 0.045(3) -0.005(2) 0.004(2) -0.005(2) C14A 0.046(3) 0.039(3) 0.048(3) -0.008(2) 0.015(2) -0.004(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 C1 2.275(4) . ? W1 C2 2.276(4) . ? W1 C8 2.289(4) . ? W1 C5 2.296(4) . ? W1 C10 2.301(4) . ? W1 C9 2.302(4) . ? W1 C6 2.313(4) . ? W1 C4 2.324(4) . ? W1 C7 2.328(4) . ? W1 C3 2.334(4) . ? W1 Sn1 2.6347(4) . ? W1 Sn1' 2.6735(3) . ? W1 Ge1' 2.6347(4) . ? W1 Ge1 2.6735(3) . ? W2 C7A 2.278(4) . ? W2 C6A 2.285(4) . ? W2 C2A 2.286(4) . ? W2 C3A 2.289(4) . ? W2 C10A 2.294(4) . ? W2 C4A 2.298(4) . ? W2 C5A 2.320(4) . ? W2 C9A 2.328(4) . ? W2 C1A 2.336(4) . ? W2 C8A 2.338(4) . ? W2 Sn2' 2.6060(4) . ? W2 Sn2 2.6902(3) . ? W2 Ge2 2.6060(4) . ? W2 Ge2' 2.6902(3) . ? Ge1 C12 1.93(3) . ? Ge1 C11 2.08(2) . ? Sn1' C11' 2.126(12) . ? Sn1' C12' 2.160(15) . ? Sn1' Cl1' 2.411(3) . ? Ge1 Cl1 2.454(6) . ? Ge1' C14' 1.929(13) . ? Ge1' C13' 1.998(12) . ? Sn1 C13 2.08(2) . ? Sn1 C14 2.15(2) . ? Ge1' Cl2' 2.345(9) . ? Sn1 Cl2 2.378(10) . ? C11' H11A 0.9800 . ? C11' H11B 0.9800 . ? C11' H11C 0.9800 . ? C12' H12A 0.9800 . ? C12' H12B 0.9800 . ? C12' H12C 0.9800 . ? C13' H13A 0.9800 . ? C13' H13B 0.9800 . ? C13' H13C 0.9800 . ? C14' H14A 0.9800 . ? C14' H14B 0.9800 . ? C14' H14C 0.9800 . ? C11 H11D 0.9800 . ? C11 H11E 0.9800 . ? C11 H11F 0.9800 . ? C12 H12D 0.9800 . ? C12 H12E 0.9800 . ? C12 H12F 0.9800 . ? C13 H13D 0.9800 . ? C13 H13E 0.9800 . ? C13 H13F 0.9800 . ? C14 H14D 0.9800 . ? C14 H14E 0.9800 . ? C14 H14F 0.9800 . ? Sn2 C14A 2.069(5) . ? Sn2 C13A 2.074(5) . ? Ge2' C14A 2.069(5) . ? Ge2' C13A 2.074(5) . ? Ge2' Cl3' 2.401(12) . ? Sn2 Cl3 2.460(7) . ? Ge2 C12A 1.927(11) . ? Ge2 C11A 2.01(3) . ? Sn2' C11B 2.11(3) . ? Sn2' C12B 2.21(2) . ? Sn2' Cl4 2.3792(15) . ? Ge2 Cl4 2.3792(15) . ? C11A H11G 0.9800 . ? C11A H11H 0.9800 . ? C11A H11I 0.9800 . ? C12A H12G 0.9800 . ? C12A H12H 0.9800 . ? C12A H12I 0.9800 . ? C11B H11J 0.9800 . ? C11B H11K 0.9800 . ? C11B H11L 0.9800 . ? C12B H12J 0.9800 . ? C12B H12K 0.9800 . ? C12B H12L 0.9800 . ? C1 C5 1.413(6) . ? C1 C2 1.424(7) . ? C1 H1A 1.0000 . ? C2 C3 1.424(7) . ? C2 H2A 1.0000 . ? C3 C4 1.389(6) . ? C3 H3A 1.0000 . ? C4 C5 1.420(6) . ? C4 H4A 1.0000 . ? C5 H5A 1.0000 . ? C6 C7 1.411(7) . ? C6 C10 1.421(7) . ? C6 H6A 1.0000 . ? C7 C8 1.424(6) . ? C7 H7A 1.0000 . ? C8 C9 1.433(6) . ? C8 H8A 1.0000 . ? C9 C10 1.405(6) . ? C9 H9A 1.0000 . ? C10 H10A 1.0000 . ? C1A C5A 1.399(7) . ? C1A C2A 1.424(6) . ? C1A H1AA 1.0000 . ? C2A C3A 1.429(6) . ? C2A H2AA 1.0000 . ? C3A C4A 1.416(6) . ? C3A H3AA 1.0000 . ? C4A C5A 1.421(7) . ? C4A H4AA 1.0000 . ? C5A H5AA 1.0000 . ? C6A C10A 1.411(7) . ? C6A C7A 1.429(6) . ? C6A H6AA 1.0000 . ? C7A C8A 1.425(7) . ? C7A H7AA 1.0000 . ? C8A C9A 1.415(7) . ? C8A H8AA 1.0000 . ? C9A C10A 1.423(7) . ? C9A H9AA 1.0000 . ? C10A H10B 1.0000 . ? C13A H13G 0.9800 . ? C13A H13H 0.9800 . ? C13A H13I 0.9800 . ? C14A H14G 0.9800 . ? C14A H14H 0.9800 . ? C14A H14I 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 C1 W1 C2 36.48(18) . . ? C1 W1 C8 146.87(16) . . ? C2 W1 C8 156.39(16) . . ? C1 W1 C5 36.01(16) . . ? C2 W1 C5 59.65(16) . . ? C8 W1 C5 140.52(16) . . ? C1 W1 C10 103.68(18) . . ? C2 W1 C10 138.79(17) . . ? C8 W1 C10 59.80(16) . . ? C5 W1 C10 80.83(17) . . ? C1 W1 C9 113.13(17) . . ? C2 W1 C9 145.04(17) . . ? C8 W1 C9 36.39(15) . . ? C5 W1 C9 107.60(16) . . ? C10 W1 C9 35.55(15) . . ? C1 W1 C6 124.97(18) . . ? C2 W1 C6 143.41(16) . . ? C8 W1 C6 59.79(16) . . ? C5 W1 C6 90.63(17) . . ? C10 W1 C6 35.88(17) . . ? C9 W1 C6 59.75(15) . . ? C1 W1 C4 60.14(16) . . ? C2 W1 C4 59.35(16) . . ? C8 W1 C4 143.11(16) . . ? C5 W1 C4 35.80(16) . . ? C10 W1 C4 95.85(16) . . ? C9 W1 C4 130.91(16) . . ? C6 W1 C4 84.07(16) . . ? C1 W1 C7 160.31(17) . . ? C2 W1 C7 155.03(17) . . ? C8 W1 C7 35.93(15) . . ? C5 W1 C7 125.46(17) . . ? C10 W1 C7 59.29(17) . . ? C9 W1 C7 59.83(15) . . ? C6 W1 C7 35.39(17) . . ? C4 W1 C7 108.96(16) . . ? C1 W1 C3 60.14(17) . . ? C2 W1 C3 35.97(17) . . ? C8 W1 C3 152.83(16) . . ? C5 W1 C3 58.85(16) . . ? C10 W1 C3 130.54(16) . . ? C9 W1 C3 165.32(16) . . ? C6 W1 C3 111.90(17) . . ? C4 W1 C3 34.71(16) . . ? C7 W1 C3 121.55(16) . . ? C1 W1 Sn1 121.19(13) . . ? C2 W1 Sn1 84.93(12) . . ? C8 W1 Sn1 82.84(11) . . ? C5 W1 Sn1 132.98(12) . . ? C10 W1 Sn1 134.71(12) . . ? C9 W1 Sn1 118.59(11) . . ? C6 W1 Sn1 104.62(13) . . ? C4 W1 Sn1 100.93(11) . . ? C7 W1 Sn1 75.47(12) . . ? C3 W1 Sn1 74.25(11) . . ? C1 W1 Sn1' 80.42(12) . . ? C2 W1 Sn1' 79.14(12) . . ? C8 W1 Sn1' 79.66(11) . . ? C5 W1 Sn1' 114.39(12) . . ? C10 W1 Sn1' 110.24(12) . . ? C9 W1 Sn1' 77.98(11) . . ? C6 W1 Sn1' 136.14(11) . . ? C4 W1 Sn1' 137.08(11) . . ? C7 W1 Sn1' 113.58(12) . . ? C3 W1 Sn1' 111.87(12) . . ? Sn1 W1 Sn1' 84.624(12) . . ? C7A W2 C6A 36.50(16) . . ? C7A W2 C2A 156.73(17) . . ? C6A W2 C2A 146.50(17) . . ? C7A W2 C3A 146.99(16) . . ? C6A W2 C3A 113.75(16) . . ? C2A W2 C3A 36.41(15) . . ? C7A W2 C10A 59.76(17) . . ? C6A W2 C10A 35.90(18) . . ? C2A W2 C10A 139.80(16) . . ? C3A W2 C10A 105.67(16) . . ? C7A W2 C4A 140.03(16) . . ? C6A W2 C4A 106.25(17) . . ? C2A W2 C4A 59.79(16) . . ? C3A W2 C4A 35.96(16) . . ? C10A W2 C4A 80.72(16) . . ? C7A W2 C5A 142.78(17) . . ? C6A W2 C5A 128.56(18) . . ? C2A W2 C5A 59.41(16) . . ? C3A W2 C5A 59.96(16) . . ? C10A W2 C5A 93.48(18) . . ? C4A W2 C5A 35.83(16) . . ? C7A W2 C9A 59.48(18) . . ? C6A W2 C9A 60.05(18) . . ? C2A W2 C9A 142.86(17) . . ? C3A W2 C9A 127.50(17) . . ? C10A W2 C9A 35.86(18) . . ? C4A W2 C9A 92.52(18) . . ? C5A W2 C9A 83.56(17) . . ? C7A W2 C1A 152.89(16) . . ? C6A W2 C1A 163.42(18) . . ? C2A W2 C1A 35.88(16) . . ? C3A W2 C1A 60.00(15) . . ? C10A W2 C1A 128.25(18) . . ? C4A W2 C1A 59.12(15) . . ? C5A W2 C1A 34.97(16) . . ? C9A W2 C1A 110.07(17) . . ? C7A W2 C8A 35.93(17) . . ? C6A W2 C8A 60.33(17) . . ? C2A W2 C8A 153.04(16) . . ? C3A W2 C8A 162.76(17) . . ? C10A W2 C8A 59.46(17) . . ? C4A W2 C8A 127.48(17) . . ? C5A W2 C8A 109.57(17) . . ? C9A W2 C8A 35.30(17) . . ? C1A W2 C8A 120.50(16) . . ? C7A W2 Sn2' 79.24(13) . . ? C6A W2 Sn2' 78.86(14) . . ? C2A W2 Sn2' 80.19(11) . . ? C3A W2 Sn2' 80.30(11) . . ? C10A W2 Sn2' 112.15(14) . . ? C4A W2 Sn2' 113.66(12) . . ? C5A W2 Sn2' 137.61(12) . . ? C9A W2 Sn2' 136.43(13) . . ? C1A W2 Sn2' 113.20(12) . . ? C8A W2 Sn2' 112.47(13) . . ? C7A W2 Sn2 83.32(11) . . ? C6A W2 Sn2 119.31(12) . . ? C2A W2 Sn2 83.78(11) . . ? C3A W2 Sn2 119.79(11) . . ? C10A W2 Sn2 133.97(12) . . ? C4A W2 Sn2 133.79(11) . . ? C5A W2 Sn2 102.54(12) . . ? C9A W2 Sn2 103.10(13) . . ? C1A W2 Sn2 74.67(11) . . ? C8A W2 Sn2 74.51(12) . . ? Sn2' W2 Sn2 83.827(12) . . ? C12 Sn1' C11 102.7(10) . . ? C12 Sn1' C11' 109.8(10) . . ? C11 Sn1' C11' 11.1(6) . . ? C12 Sn1' C12' 6.6(13) . . ? C11 Sn1' C12' 100.4(7) . . ? C11' Sn1' C12' 108.4(6) . . ? C12 Sn1' Cl1' 95.2(9) . . ? C11 Sn1' Cl1' 98.3(6) . . ? C11' Sn1' Cl1' 89.0(4) . . ? C12' Sn1' Cl1' 101.7(5) . . ? C12 Sn1' Cl1 83.8(9) . . ? C11 Sn1' Cl1 101.1(6) . . ? C11' Sn1' Cl1 93.1(4) . . ? C12' Sn1' Cl1 90.3(5) . . ? Cl1' Sn1' Cl1 11.37(12) . . ? C12 Sn1' W1 122.1(9) . . ? C11 Sn1' W1 120.0(6) . . ? C11' Sn1' W1 119.4(3) . . ? C12' Sn1' W1 119.5(4) . . ? Cl1' Sn1' W1 113.51(9) . . ? Cl1 Sn1' W1 119.99(12) . . ? C14' Sn1 C13' 109.4(6) . . ? C14' Sn1 C13 103.4(7) . . ? C13' Sn1 C13 8.9(7) . . ? C14' Sn1 C14 7.2(9) . . ? C13' Sn1 C14 109.4(8) . . ? C13 Sn1 C14 104.4(9) . . ? C14' Sn1 Cl2' 99.5(5) . . ? C13' Sn1 Cl2' 96.5(4) . . ? C13 Sn1 Cl2' 104.2(6) . . ? C14 Sn1 Cl2' 92.3(6) . . ? C14' Sn1 Cl2 101.1(5) . . ? C13' Sn1 Cl2 95.2(4) . . ? C13 Sn1 Cl2 103.1(6) . . ? C14 Sn1 Cl2 93.9(6) . . ? Cl2' Sn1 Cl2 1.7(4) . . ? C14' Sn1 W1 122.4(4) . . ? C13' Sn1 W1 117.9(4) . . ? C13 Sn1 W1 118.7(7) . . ? C14 Sn1 W1 126.2(7) . . ? Cl2' Sn1 W1 105.69(19) . . ? Cl2 Sn1 W1 105.29(17) . . ? Sn1' C11' H11A 109.5 . . ? Sn1' C11' H11B 109.5 . . ? H11A C11' H11B 109.5 . . ? Sn1' C11' H11C 109.5 . . ? H11A C11' H11C 109.5 . . ? H11B C11' H11C 109.5 . . ? Sn1' C12' H12A 109.5 . . ? Sn1' C12' H12B 109.5 . . ? H12A C12' H12B 109.5 . . ? Sn1' C12' H12C 109.5 . . ? H12A C12' H12C 109.5 . . ? H12B C12' H12C 109.5 . . ? Sn1 C13' H13A 109.5 . . ? Sn1 C13' H13B 109.5 . . ? H13A C13' H13B 109.5 . . ? Sn1 C13' H13C 109.5 . . ? H13A C13' H13C 109.5 . . ? H13B C13' H13C 109.5 . . ? Sn1 C14' H14A 109.5 . . ? Sn1 C14' H14B 109.5 . . ? H14A C14' H14B 109.5 . . ? Sn1 C14' H14C 109.5 . . ? H14A C14' H14C 109.5 . . ? H14B C14' H14C 109.5 . . ? Sn1' C11 H11D 109.5 . . ? Sn1' C11 H11E 109.5 . . ? H11D C11 H11E 109.5 . . ? Sn1' C11 H11F 109.5 . . ? H11D C11 H11F 109.5 . . ? H11E C11 H11F 109.5 . . ? Sn1' C12 H12D 109.5 . . ? Sn1' C12 H12E 109.5 . . ? H12D C12 H12E 109.5 . . ? Sn1' C12 H12F 109.5 . . ? H12D C12 H12F 109.5 . . ? H12E C12 H12F 109.5 . . ? Sn1 C13 H13D 109.5 . . ? Sn1 C13 H13E 109.5 . . ? H13D C13 H13E 109.5 . . ? Sn1 C13 H13F 109.5 . . ? H13D C13 H13F 109.5 . . ? H13E C13 H13F 109.5 . . ? Sn1 C14 H14D 109.5 . . ? Sn1 C14 H14E 109.5 . . ? H14D C14 H14E 109.5 . . ? Sn1 C14 H14F 109.5 . . ? H14D C14 H14F 109.5 . . ? H14E C14 H14F 109.5 . . ? C14A Sn2 C13A 109.3(2) . . ? C14A Sn2 Cl3' 95.8(3) . . ? C13A Sn2 Cl3' 96.7(3) . . ? C14A Sn2 Cl3 97.5(2) . . ? C13A Sn2 Cl3 96.0(2) . . ? Cl3' Sn2 Cl3 1.6(4) . . ? C14A Sn2 W2 120.58(15) . . ? C13A Sn2 W2 122.93(15) . . ? Cl3' Sn2 W2 103.7(3) . . ? Cl3 Sn2 W2 102.86(18) . . ? C12A Sn2' C11A 95.2(7) . . ? C12A Sn2' C11B 104.9(8) . . ? C11A Sn2' C11B 10.7(11) . . ? C12A Sn2' C12B 9.8(8) . . ? C11A Sn2' C12B 104.7(8) . . ? C11B Sn2' C12B 114.6(9) . . ? C12A Sn2' Cl4 93.6(4) . . ? C11A Sn2' Cl4 97.9(9) . . ? C11B Sn2' Cl4 92.8(13) . . ? C12B Sn2' Cl4 94.7(6) . . ? C12A Sn2' W2 126.2(4) . . ? C11A Sn2' W2 121.9(8) . . ? C11B Sn2' W2 116.9(11) . . ? C12B Sn2' W2 117.4(6) . . ? Cl4 Sn2' W2 115.47(4) . . ? Sn2' C11A H11G 109.5 . . ? Sn2' C11A H11H 109.5 . . ? H11G C11A H11H 109.5 . . ? Sn2' C11A H11I 109.5 . . ? H11G C11A H11I 109.5 . . ? H11H C11A H11I 109.5 . . ? Sn2' C12A H12G 109.5 . . ? Sn2' C12A H12H 109.5 . . ? H12G C12A H12H 109.5 . . ? Sn2' C12A H12I 109.5 . . ? H12G C12A H12I 109.5 . . ? H12H C12A H12I 109.5 . . ? Sn2' C11B H11J 109.5 . . ? Sn2' C11B H11K 109.5 . . ? H11J C11B H11K 109.5 . . ? Sn2' C11B H11L 109.5 . . ? H11J C11B H11L 109.5 . . ? H11K C11B H11L 109.5 . . ? Sn2' C12B H12J 109.5 . . ? Sn2' C12B H12K 109.5 . . ? H12J C12B H12K 109.5 . . ? Sn2' C12B H12L 109.5 . . ? H12J C12B H12L 109.5 . . ? H12K C12B H12L 109.5 . . ? C5 C1 C2 106.5(4) . . ? C5 C1 W1 72.8(2) . . ? C2 C1 W1 71.8(2) . . ? C5 C1 H1A 126.5 . . ? C2 C1 H1A 126.5 . . ? W1 C1 H1A 126.5 . . ? C1 C2 C3 108.3(4) . . ? C1 C2 W1 71.7(2) . . ? C3 C2 W1 74.2(2) . . ? C1 C2 H2A 125.6 . . ? C3 C2 H2A 125.6 . . ? W1 C2 H2A 125.6 . . ? C4 C3 C2 108.1(4) . . ? C4 C3 W1 72.3(2) . . ? C2 C3 W1 69.8(2) . . ? C4 C3 H3A 125.9 . . ? C2 C3 H3A 125.9 . . ? W1 C3 H3A 125.9 . . ? C3 C4 C5 108.1(4) . . ? C3 C4 W1 73.0(2) . . ? C5 C4 W1 71.0(2) . . ? C3 C4 H4A 125.8 . . ? C5 C4 H4A 125.8 . . ? W1 C4 H4A 125.8 . . ? C1 C5 C4 108.9(4) . . ? C1 C5 W1 71.2(2) . . ? C4 C5 W1 73.2(2) . . ? C1 C5 H5A 125.5 . . ? C4 C5 H5A 125.5 . . ? W1 C5 H5A 125.5 . . ? C7 C6 C10 107.9(4) . . ? C7 C6 W1 72.9(2) . . ? C10 C6 W1 71.6(2) . . ? C7 C6 H6A 125.9 . . ? C10 C6 H6A 125.9 . . ? W1 C6 H6A 125.9 . . ? C6 C7 C8 108.0(4) . . ? C6 C7 W1 71.7(2) . . ? C8 C7 W1 70.5(2) . . ? C6 C7 H7A 126.0 . . ? C8 C7 H7A 126.0 . . ? W1 C7 H7A 126.0 . . ? C7 C8 C9 107.8(4) . . ? C7 C8 W1 73.5(2) . . ? C9 C8 W1 72.3(2) . . ? C7 C8 H8A 125.9 . . ? C9 C8 H8A 125.9 . . ? W1 C8 H8A 125.9 . . ? C10 C9 C8 107.4(4) . . ? C10 C9 W1 72.2(2) . . ? C8 C9 W1 71.3(2) . . ? C10 C9 H9A 126.2 . . ? C8 C9 H9A 126.2 . . ? W1 C9 H9A 126.2 . . ? C9 C10 C6 108.8(4) . . ? C9 C10 W1 72.3(2) . . ? C6 C10 W1 72.5(2) . . ? C9 C10 H10A 125.5 . . ? C6 C10 H10A 125.5 . . ? W1 C10 H10A 125.5 . . ? C5A C1A C2A 107.9(4) . . ? C5A C1A W2 71.9(2) . . ? C2A C1A W2 70.1(2) . . ? C5A C1A H1AA 126.0 . . ? C2A C1A H1AA 126.0 . . ? W2 C1A H1AA 126.0 . . ? C1A C2A C3A 108.3(4) . . ? C1A C2A W2 74.0(2) . . ? C3A C2A W2 71.9(2) . . ? C1A C2A H2AA 125.7 . . ? C3A C2A H2AA 125.7 . . ? W2 C2A H2AA 125.7 . . ? C4A C3A C2A 106.8(4) . . ? C4A C3A W2 72.4(2) . . ? C2A C3A W2 71.7(2) . . ? C4A C3A H3AA 126.4 . . ? C2A C3A H3AA 126.4 . . ? W2 C3A H3AA 126.4 . . ? C3A C4A C5A 108.6(4) . . ? C3A C4A W2 71.7(2) . . ? C5A C4A W2 72.9(2) . . ? C3A C4A H4AA 125.6 . . ? C5A C4A H4AA 125.6 . . ? W2 C4A H4AA 125.6 . . ? C1A C5A C4A 108.4(4) . . ? C1A C5A W2 73.2(2) . . ? C4A C5A W2 71.2(2) . . ? C1A C5A H5AA 125.7 . . ? C4A C5A H5AA 125.7 . . ? W2 C5A H5AA 125.7 . . ? C10A C6A C7A 106.6(4) . . ? C10A C6A W2 72.4(2) . . ? C7A C6A W2 71.5(2) . . ? C10A C6A H6AA 126.5 . . ? C7A C6A H6AA 126.5 . . ? W2 C6A H6AA 126.5 . . ? C8A C7A C6A 109.0(4) . . ? C8A C7A W2 74.3(2) . . ? C6A C7A W2 72.0(2) . . ? C8A C7A H7AA 125.3 . . ? C6A C7A H7AA 125.3 . . ? W2 C7A H7AA 125.3 . . ? C9A C8A C7A 107.2(4) . . ? C9A C8A W2 71.9(3) . . ? C7A C8A W2 69.7(2) . . ? C9A C8A H8AA 126.4 . . ? C7A C8A H8AA 126.4 . . ? W2 C8A H8AA 126.4 . . ? C8A C9A C10A 108.1(4) . . ? C8A C9A W2 72.8(3) . . ? C10A C9A W2 70.8(3) . . ? C8A C9A H9AA 125.9 . . ? C10A C9A H9AA 125.9 . . ? W2 C9A H9AA 125.9 . . ? C6A C10A C9A 109.1(4) . . ? C6A C10A W2 71.7(3) . . ? C9A C10A W2 73.4(3) . . ? C6A C10A H10B 125.4 . . ? C9A C10A H10B 125.4 . . ? W2 C10A H10B 125.4 . . ? Sn2 C13A H13G 109.5 . . ? Sn2 C13A H13H 109.5 . . ? H13G C13A H13H 109.5 . . ? Sn2 C13A H13I 109.5 . . ? H13G C13A H13I 109.5 . . ? H13H C13A H13I 109.5 . . ? Sn2 C14A H14G 109.5 . . ? Sn2 C14A H14H 109.5 . . ? H14G C14A H14H 109.5 . . ? Sn2 C14A H14I 109.5 . . ? H14G C14A H14I 109.5 . . ? H14H C14A H14I 109.5 . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 28.50 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 2.240 _refine_diff_density_min -1.355 _refine_diff_density_rms 0.140 data_4 _database_code_depnum_ccdc_archive 'CCDC 632230' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C16 H26 Br1.71 Cl0.29 Ge Sn W' _chemical_formula_sum 'C16 H26 Br1.71 Cl0.29 Ge Sn W' _chemical_formula_weight 740.42 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ge Ge 0.1547 1.8001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 '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 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 15.5322(3) _cell_length_b 8.7717(2) _cell_length_c 14.2873(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.741(1) _cell_angle_gamma 90.00 _cell_volume 1946.39(6) _cell_formula_units_Z 4 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 7509 _cell_measurement_theta_min 2.623 _cell_measurement_theta_max 30.000 _exptl_crystal_description block _exptl_crystal_colour yellow-orange _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.527 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1371 _exptl_absorpt_coefficient_mu 12.246 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.1308 _exptl_absorpt_correction_T_max 0.2166 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(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 SMART 6K' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 10353 _diffrn_reflns_av_R_equivalents 0.0205 _diffrn_reflns_av_sigmaI/netI 0.0280 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.31 _diffrn_reflns_theta_max 28.50 _reflns_number_total 4906 _reflns_number_gt 4540 _reflns_threshold_expression I>2\s(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0620P)^2^+24.9074P] 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 4906 _refine_ls_number_parameters 193 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0401 _refine_ls_R_factor_gt 0.0375 _refine_ls_wR_factor_ref 0.1171 _refine_ls_wR_factor_gt 0.1155 _refine_ls_goodness_of_fit_ref 1.093 _refine_ls_restrained_S_all 1.093 _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 0.174094(15) 0.59040(3) 0.111521(16) 0.01269(9) Uani 1 1 d . A . Ge1 Ge 0.19921(5) 0.30378(8) 0.12271(5) 0.01780(16) Uani 1 1 d . . . Sn1 Sn 0.33247(3) 0.60637(5) 0.19782(3) 0.01732(12) Uani 1 1 d . . . Br1 Br 0.3585(4) 0.8904(6) 0.2295(5) 0.0342(6) Uani 0.71 1 d P A 1 Cl1 Cl 0.365(3) 0.874(4) 0.238(3) 0.0342(6) Uani 0.29 1 d P A 2 Br2 Br 0.08349(8) 0.16257(13) 0.04599(9) 0.0539(3) Uani 1 1 d . . . C1 C 0.1223(5) 0.6342(10) -0.0377(5) 0.0258(15) Uani 1 1 d . . . H1A H 0.0602 0.6307 -0.0571 0.031 Uiso 1 1 calc R A . C2 C 0.1799(5) 0.5133(9) -0.0441(5) 0.0229(14) Uani 1 1 d . A . H2A H 0.1666 0.4090 -0.0685 0.028 Uiso 1 1 calc R . . C3 C 0.2625(5) 0.5675(9) -0.0151(5) 0.0234(14) Uani 1 1 d . . . H3A H 0.3176 0.5087 -0.0170 0.028 Uiso 1 1 calc R A . C4 C 0.2540(5) 0.7276(10) 0.0061(5) 0.0284(16) Uani 1 1 d . A . H4A H 0.3021 0.7994 0.0218 0.034 Uiso 1 1 calc R . . C5 C 0.1672(6) 0.7671(9) -0.0075(5) 0.0289(16) Uani 1 1 d . A . H5A H 0.1425 0.8721 -0.0030 0.035 Uiso 1 1 calc R . . C6 C 0.0600(5) 0.5145(9) 0.2027(5) 0.0229(14) Uani 1 1 d . . . H6A H 0.0307 0.4130 0.2006 0.028 Uiso 1 1 calc R A . C7 C 0.1309(5) 0.5568(9) 0.2632(5) 0.0216(14) Uani 1 1 d . A . H7A H 0.1594 0.4895 0.3108 0.026 Uiso 1 1 calc R . . C8 C 0.1468(5) 0.7161(9) 0.2509(5) 0.0216(13) Uani 1 1 d . . . H8A H 0.1886 0.7797 0.2877 0.026 Uiso 1 1 calc R A . C9 C 0.0868(5) 0.7697(9) 0.1826(5) 0.0244(14) Uani 1 1 d . A . H9A H 0.0795 0.8781 0.1625 0.029 Uiso 1 1 calc R . . C10 C 0.0345(4) 0.6457(10) 0.1538(5) 0.0249(15) Uani 1 1 d . A . H10A H -0.0159 0.6526 0.1097 0.030 Uiso 1 1 calc R . . C11 C 0.2947(5) 0.2045(9) 0.0570(6) 0.0281(16) Uani 1 1 d . . . H11A H 0.2937 0.0947 0.0697 0.042 Uiso 1 1 calc R . . H11B H 0.3495 0.2475 0.0792 0.042 Uiso 1 1 calc R . . H11C H 0.2883 0.2219 -0.0105 0.042 Uiso 1 1 calc R . . C12 C 0.1909(4) 0.1951(8) 0.2458(4) 0.0183(12) Uani 1 1 d . . . H12A H 0.2024 0.0863 0.2368 0.027 Uiso 1 1 calc R . . H12B H 0.1329 0.2083 0.2708 0.027 Uiso 1 1 calc R . . H12C H 0.2332 0.2377 0.2900 0.027 Uiso 1 1 calc R . . C13 C 0.3493(5) 0.5241(9) 0.3405(5) 0.0227(14) Uani 1 1 d . A . H13A H 0.2976 0.5510 0.3767 0.027 Uiso 1 1 calc R . . H13B H 0.3537 0.4115 0.3392 0.027 Uiso 1 1 calc R . . C14 C 0.4287(6) 0.5882(11) 0.3910(7) 0.036(2) Uani 1 1 d . . . H14B H 0.4323 0.5459 0.4544 0.054 Uiso 1 1 calc R A . H14C H 0.4242 0.6995 0.3944 0.054 Uiso 1 1 calc R . . H14D H 0.4805 0.5604 0.3564 0.054 Uiso 1 1 calc R . . C15 C 0.4518(5) 0.5477(11) 0.1269(6) 0.0313(18) Uani 1 1 d . A . H15B H 0.4745 0.4519 0.1543 0.038 Uiso 1 1 calc R . . H15C H 0.4382 0.5278 0.0602 0.038 Uiso 1 1 calc R . . C16 C 0.5213(5) 0.6668(11) 0.1325(7) 0.038(2) Uani 1 1 d . . . H16D H 0.5722 0.6309 0.0991 0.058 Uiso 1 1 calc R A . H16A H 0.5367 0.6857 0.1982 0.058 Uiso 1 1 calc R . . H16B H 0.5005 0.7615 0.1037 0.058 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 0.01210(14) 0.01527(14) 0.01073(13) 0.00010(8) 0.00133(9) 0.00017(8) Ge1 0.0177(3) 0.0161(3) 0.0197(3) 0.0015(3) 0.0012(2) 0.0011(2) Sn1 0.0127(2) 0.0210(2) 0.0182(2) -0.00204(16) -0.00047(16) 0.00149(15) Br1 0.0262(12) 0.0264(16) 0.0499(17) -0.0015(10) -0.0072(9) 0.0003(9) Cl1 0.0262(12) 0.0264(16) 0.0499(17) -0.0015(10) -0.0072(9) 0.0003(9) Br2 0.0513(6) 0.0373(5) 0.0727(8) 0.0003(5) -0.0175(5) -0.0005(4) C1 0.024(3) 0.041(4) 0.012(3) 0.003(3) -0.003(3) 0.004(3) C2 0.033(4) 0.025(3) 0.011(3) -0.002(3) 0.000(3) -0.003(3) C3 0.026(3) 0.032(4) 0.013(3) 0.000(3) 0.007(3) 0.004(3) C4 0.035(4) 0.033(4) 0.018(3) 0.005(3) 0.007(3) -0.015(3) C5 0.048(5) 0.022(3) 0.017(3) 0.007(3) 0.007(3) 0.010(3) C6 0.019(3) 0.028(4) 0.022(3) 0.001(3) 0.010(3) -0.004(3) C7 0.020(3) 0.031(4) 0.014(3) 0.002(3) 0.007(2) 0.001(3) C8 0.021(3) 0.027(3) 0.016(3) -0.007(3) 0.009(2) 0.001(3) C9 0.026(3) 0.022(3) 0.025(3) 0.002(3) 0.013(3) 0.008(3) C10 0.011(3) 0.041(4) 0.022(3) 0.003(3) 0.003(2) 0.006(3) C11 0.029(4) 0.022(4) 0.034(4) 0.000(3) 0.009(3) 0.004(3) C12 0.020(3) 0.020(3) 0.014(3) 0.004(2) 0.003(2) 0.003(2) C13 0.020(3) 0.032(4) 0.016(3) -0.002(3) -0.002(2) 0.005(3) C14 0.025(4) 0.051(6) 0.032(4) -0.004(4) -0.008(3) 0.006(3) C15 0.016(3) 0.048(5) 0.030(4) -0.015(4) 0.001(3) 0.001(3) C16 0.021(4) 0.041(5) 0.054(6) 0.004(4) 0.012(4) -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 W1 C3 2.294(7) . ? W1 C7 2.296(7) . ? W1 C1 2.301(7) . ? W1 C5 2.302(7) . ? W1 C4 2.304(7) . ? W1 C10 2.309(7) . ? W1 C6 2.312(7) . ? W1 C9 2.319(7) . ? W1 C8 2.320(6) . ? W1 C2 2.327(7) . ? W1 Ge1 2.5489(8) . ? W1 Sn1 2.7409(5) . ? Ge1 C11 1.968(8) . ? Ge1 C12 2.006(6) . ? Ge1 Br2 2.4321(13) . ? Sn1 C13 2.175(7) . ? Sn1 C15 2.185(7) . ? Sn1 Cl1 2.46(4) . ? Sn1 Br1 2.564(6) . ? C1 C2 1.392(11) . ? C1 C5 1.423(12) . ? C1 H1A 1.0000 . ? C2 C3 1.424(11) . ? C2 H2A 1.0000 . ? C3 C4 1.443(11) . ? C3 H3A 1.0000 . ? C4 C5 1.403(12) . ? C4 H4A 1.0000 . ? C5 H5A 1.0000 . ? C6 C10 1.400(11) . ? C6 C7 1.440(10) . ? C6 H6A 1.0000 . ? C7 C8 1.430(11) . ? C7 H7A 1.0000 . ? C8 C9 1.420(11) . ? C8 H8A 1.0000 . ? C9 C10 1.416(11) . ? C9 H9A 1.0000 . ? C10 H10A 1.0000 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 C14 1.527(11) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C14 H14D 0.9800 . ? C15 C16 1.504(12) . ? C15 H15B 0.9900 . ? C15 H15C 0.9900 . ? C16 H16D 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 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 C3 W1 C7 156.7(3) . . ? C3 W1 C1 59.3(3) . . ? C7 W1 C1 142.4(3) . . ? C3 W1 C5 59.9(3) . . ? C7 W1 C5 140.6(3) . . ? C1 W1 C5 36.0(3) . . ? C3 W1 C4 36.6(3) . . ? C7 W1 C4 148.3(3) . . ? C1 W1 C4 59.5(3) . . ? C5 W1 C4 35.5(3) . . ? C3 W1 C10 142.9(3) . . ? C7 W1 C10 59.5(3) . . ? C1 W1 C10 83.6(3) . . ? C5 W1 C10 91.0(3) . . ? C4 W1 C10 125.2(3) . . ? C3 W1 C6 152.9(3) . . ? C7 W1 C6 36.4(3) . . ? C1 W1 C6 108.0(3) . . ? C5 W1 C6 125.6(3) . . ? C4 W1 C6 160.5(3) . . ? C10 W1 C6 35.3(3) . . ? C3 W1 C9 139.8(3) . . ? C7 W1 C9 59.6(3) . . ? C1 W1 C9 95.3(3) . . ? C5 W1 C9 81.1(3) . . ? C4 W1 C9 104.8(3) . . ? C10 W1 C9 35.6(3) . . ? C6 W1 C9 59.4(3) . . ? C3 W1 C8 146.8(3) . . ? C7 W1 C8 36.1(3) . . ? C1 W1 C8 130.5(3) . . ? C5 W1 C8 107.9(3) . . ? C4 W1 C8 114.8(3) . . ? C10 W1 C8 59.5(3) . . ? C6 W1 C8 60.2(3) . . ? C9 W1 C8 35.6(3) . . ? C3 W1 C2 35.9(3) . . ? C7 W1 C2 151.7(3) . . ? C1 W1 C2 35.0(3) . . ? C5 W1 C2 59.5(3) . . ? C4 W1 C2 59.9(3) . . ? C10 W1 C2 111.1(3) . . ? C6 W1 C2 119.6(3) . . ? C9 W1 C2 130.2(3) . . ? C8 W1 C2 165.5(3) . . ? C3 W1 Ge1 82.6(2) . . ? C7 W1 Ge1 82.0(2) . . ? C1 W1 Ge1 105.9(2) . . ? C5 W1 Ge1 135.7(2) . . ? C4 W1 Ge1 118.2(2) . . ? C10 W1 Ge1 109.5(2) . . ? C6 W1 Ge1 78.4(2) . . ? C9 W1 Ge1 136.98(18) . . ? C8 W1 Ge1 116.40(19) . . ? C2 W1 Ge1 76.43(19) . . ? C3 W1 Sn1 79.42(19) . . ? C7 W1 Sn1 81.59(18) . . ? C1 W1 Sn1 135.2(2) . . ? C5 W1 Sn1 109.3(2) . . ? C4 W1 Sn1 77.2(2) . . ? C10 W1 Sn1 135.37(19) . . ? C6 W1 Sn1 116.85(19) . . ? C9 W1 Sn1 107.1(2) . . ? C8 W1 Sn1 76.27(18) . . ? C2 W1 Sn1 113.51(19) . . ? Ge1 W1 Sn1 83.48(2) . . ? C11 Ge1 C12 105.4(3) . . ? C11 Ge1 Br2 96.7(3) . . ? C12 Ge1 Br2 95.6(2) . . ? C11 Ge1 W1 121.5(2) . . ? C12 Ge1 W1 120.8(2) . . ? Br2 Ge1 W1 111.25(4) . . ? C13 Sn1 C15 105.3(3) . . ? C13 Sn1 Cl1 94.2(10) . . ? C15 Sn1 Cl1 99.2(11) . . ? C13 Sn1 Br1 98.1(2) . . ? C15 Sn1 Br1 100.2(3) . . ? Cl1 Sn1 Br1 4.4(9) . . ? C13 Sn1 W1 120.07(19) . . ? C15 Sn1 W1 122.8(2) . . ? Cl1 Sn1 W1 109.5(8) . . ? Br1 Sn1 W1 105.53(11) . . ? C2 C1 C5 109.3(7) . . ? C2 C1 W1 73.5(4) . . ? C5 C1 W1 72.0(4) . . ? C2 C1 H1A 125.2 . . ? C5 C1 H1A 125.2 . . ? W1 C1 H1A 125.2 . . ? C1 C2 C3 107.7(7) . . ? C1 C2 W1 71.5(4) . . ? C3 C2 W1 70.8(4) . . ? C1 C2 H2A 126.1 . . ? C3 C2 H2A 126.1 . . ? W1 C2 H2A 126.1 . . ? C2 C3 C4 107.6(7) . . ? C2 C3 W1 73.3(4) . . ? C4 C3 W1 72.1(4) . . ? C2 C3 H3A 126.0 . . ? C4 C3 H3A 126.0 . . ? W1 C3 H3A 126.0 . . ? C5 C4 C3 107.5(7) . . ? C5 C4 W1 72.2(4) . . ? C3 C4 W1 71.3(4) . . ? C5 C4 H4A 126.1 . . ? C3 C4 H4A 126.1 . . ? W1 C4 H4A 126.1 . . ? C4 C5 C1 107.9(7) . . ? C4 C5 W1 72.3(4) . . ? C1 C5 W1 72.0(4) . . ? C4 C5 H5A 125.9 . . ? C1 C5 H5A 125.9 . . ? W1 C5 H5A 125.9 . . ? C10 C6 C7 107.2(7) . . ? C10 C6 W1 72.3(4) . . ? C7 C6 W1 71.2(4) . . ? C10 C6 H6A 126.3 . . ? C7 C6 H6A 126.3 . . ? W1 C6 H6A 126.3 . . ? C8 C7 C6 108.1(7) . . ? C8 C7 W1 72.8(4) . . ? C6 C7 W1 72.4(4) . . ? C8 C7 H7A 125.8 . . ? C6 C7 H7A 125.8 . . ? W1 C7 H7A 125.8 . . ? C9 C8 C7 107.2(7) . . ? C9 C8 W1 72.2(4) . . ? C7 C8 W1 71.1(4) . . ? C9 C8 H8A 126.3 . . ? C7 C8 H8A 126.3 . . ? W1 C8 H8A 126.3 . . ? C10 C9 C8 108.3(7) . . ? C10 C9 W1 71.8(4) . . ? C8 C9 W1 72.2(4) . . ? C10 C9 H9A 125.7 . . ? C8 C9 H9A 125.7 . . ? W1 C9 H9A 125.7 . . ? C6 C10 C9 109.2(7) . . ? C6 C10 W1 72.5(4) . . ? C9 C10 W1 72.6(4) . . ? C6 C10 H10A 125.3 . . ? C9 C10 H10A 125.3 . . ? W1 C10 H10A 125.3 . . ? Ge1 C11 H11A 109.5 . . ? Ge1 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? Ge1 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? Ge1 C12 H12A 109.5 . . ? Ge1 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? Ge1 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C14 C13 Sn1 114.0(6) . . ? C14 C13 H13A 108.7 . . ? Sn1 C13 H13A 108.7 . . ? C14 C13 H13B 108.7 . . ? Sn1 C13 H13B 108.7 . . ? H13A C13 H13B 107.6 . . ? C13 C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C13 C14 H14D 109.5 . . ? H14B C14 H14D 109.5 . . ? H14C C14 H14D 109.5 . . ? C16 C15 Sn1 115.2(6) . . ? C16 C15 H15B 108.5 . . ? Sn1 C15 H15B 108.5 . . ? C16 C15 H15C 108.5 . . ? Sn1 C15 H15C 108.5 . . ? H15B C15 H15C 107.5 . . ? C15 C16 H16D 109.5 . . ? C15 C16 H16A 109.5 . . ? H16D C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16D C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 28.50 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 2.224 _refine_diff_density_min -4.672 _refine_diff_density_rms 0.281 data_14 _database_code_depnum_ccdc_archive 'CCDC 632231' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C16 H27 Br Ge Sn W' _chemical_formula_sum 'C16 H27 Br Ge Sn W' _chemical_formula_weight 674.42 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' Ge Ge 0.1547 1.8001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 '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 'P 21/n' _symmetry_space_group_name_Hall '-P 2yn' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 10.5494(3) _cell_length_b 13.8654(4) _cell_length_c 13.0943(4) _cell_angle_alpha 90.00 _cell_angle_beta 97.093(1) _cell_angle_gamma 90.00 _cell_volume 1900.67(10) _cell_formula_units_Z 4 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 5636 _cell_measurement_theta_min 2.343 _cell_measurement_theta_max 30.018 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.357 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1256 _exptl_absorpt_coefficient_mu 11.005 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3080 _exptl_absorpt_correction_T_max 0.3518 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(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 SMART 1K' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 11690 _diffrn_reflns_av_R_equivalents 0.0366 _diffrn_reflns_av_sigmaI/netI 0.0499 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.15 _diffrn_reflns_theta_max 28.99 _reflns_number_total 4919 _reflns_number_gt 3893 _reflns_threshold_expression I>2\s(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0360P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4919 _refine_ls_number_parameters 184 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0512 _refine_ls_R_factor_gt 0.0350 _refine_ls_wR_factor_ref 0.0790 _refine_ls_wR_factor_gt 0.0749 _refine_ls_goodness_of_fit_ref 1.022 _refine_ls_restrained_S_all 1.022 _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 0.10785(2) 0.147163(15) 0.284166(17) 0.02119(7) Uani 1 1 d . . . Sn1 Sn -0.14940(4) 0.12879(3) 0.23203(3) 0.02323(10) Uani 1 1 d . . . Ge1 Ge 0.09333(6) 0.21969(4) 0.09835(5) 0.02633(14) Uani 1 1 d . . . Br1 Br -0.23741(7) 0.01313(4) 0.36554(5) 0.03705(16) Uani 1 1 d . . . C1 C 0.0421(6) 0.2988(4) 0.3233(5) 0.0299(13) Uani 1 1 d . . . H1A H -0.0298 0.3360 0.2848 0.036 Uiso 1 1 calc R . . C2 C 0.0344(6) 0.2378(4) 0.4116(5) 0.0300(13) Uani 1 1 d . . . H2A H -0.0444 0.2246 0.4446 0.036 Uiso 1 1 calc R . . C3 C 0.1592(6) 0.2070(4) 0.4484(5) 0.0332(14) Uani 1 1 d . . . H3A H 0.1840 0.1678 0.5118 0.040 Uiso 1 1 calc R . . C4 C 0.2442(6) 0.2497(4) 0.3862(5) 0.0309(13) Uani 1 1 d . . . H4A H 0.3394 0.2438 0.3977 0.037 Uiso 1 1 calc R . . C5 C 0.1756(6) 0.3055(4) 0.3091(5) 0.0326(14) Uani 1 1 d . . . H5A H 0.2127 0.3471 0.2579 0.039 Uiso 1 1 calc R . . C6 C 0.0736(8) -0.0141(5) 0.2387(7) 0.053(2) Uani 1 1 d . . . H6A H -0.0108 -0.0429 0.2117 0.063 Uiso 1 1 calc R . . C7 C 0.1229(8) -0.0090(5) 0.3414(6) 0.0484(19) Uani 1 1 d . . . H7A H 0.0820 -0.0358 0.4002 0.058 Uiso 1 1 calc R . . C8 C 0.2424(7) 0.0294(5) 0.3473(6) 0.0463(19) Uani 1 1 d . . . H8A H 0.3041 0.0342 0.4116 0.056 Uiso 1 1 calc R . . C9 C 0.2705(8) 0.0530(4) 0.2462(7) 0.051(2) Uani 1 1 d . . . H9A H 0.3545 0.0753 0.2268 0.062 Uiso 1 1 calc R . . C10 C 0.1622(9) 0.0243(5) 0.1779(5) 0.055(2) Uani 1 1 d . . . H10A H 0.1538 0.0255 0.1010 0.066 Uiso 1 1 calc R . . C11 C 0.0060(6) 0.3447(4) 0.0715(5) 0.0309(13) Uani 1 1 d . . . H11A H 0.0077 0.3628 -0.0006 0.046 Uiso 1 1 calc R . . H11B H 0.0497 0.3941 0.1163 0.046 Uiso 1 1 calc R . . H11C H -0.0828 0.3391 0.0856 0.046 Uiso 1 1 calc R . . C12 C 0.2619(7) 0.2408(5) 0.0553(6) 0.0485(19) Uani 1 1 d . . . H12A H 0.2523 0.2678 -0.0144 0.073 Uiso 1 1 calc R . . H12B H 0.3077 0.1793 0.0558 0.073 Uiso 1 1 calc R . . H12C H 0.3103 0.2858 0.1029 0.073 Uiso 1 1 calc R . . C13 C -0.2791(6) 0.2489(4) 0.2504(5) 0.0321(14) Uani 1 1 d . . . H13A H -0.2502 0.2816 0.3165 0.039 Uiso 1 1 calc R . . H13B H -0.2719 0.2960 0.1946 0.039 Uiso 1 1 calc R . . C14 C -0.4174(7) 0.2224(5) 0.2491(8) 0.059(2) Uani 1 1 d . . . H14B H -0.4675 0.2807 0.2581 0.088 Uiso 1 1 calc R . . H14C H -0.4266 0.1772 0.3052 0.088 Uiso 1 1 calc R . . H14D H -0.4485 0.1921 0.1831 0.088 Uiso 1 1 calc R . . C15 C -0.2315(7) 0.0510(5) 0.0919(5) 0.0381(16) Uani 1 1 d . . . H15A H -0.2224 0.0940 0.0329 0.046 Uiso 1 1 calc R . . H15B H -0.1758 -0.0055 0.0848 0.046 Uiso 1 1 calc R . . C16 C -0.3490(11) 0.0193(8) 0.0796(8) 0.102(4) Uani 1 1 d . . . H16C H -0.3659 -0.0137 0.0132 0.153 Uiso 1 1 calc R . . H16D H -0.4079 0.0738 0.0813 0.153 Uiso 1 1 calc R . . H16A H -0.3612 -0.0258 0.1351 0.153 Uiso 1 1 calc R . . H1 H 0.028(6) 0.149(4) -0.012(5) 0.030 Uiso 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 W1 0.02736(13) 0.01493(11) 0.02076(11) 0.00002(8) 0.00093(9) 0.00060(9) Sn1 0.0288(2) 0.01903(19) 0.02145(19) 0.00282(14) 0.00136(16) -0.00324(15) Ge1 0.0319(3) 0.0234(3) 0.0240(3) 0.0042(2) 0.0045(3) 0.0029(2) Br1 0.0495(4) 0.0272(3) 0.0360(3) 0.0099(3) 0.0118(3) -0.0057(3) C1 0.035(3) 0.014(3) 0.040(3) -0.007(2) 0.001(3) 0.001(2) C2 0.034(3) 0.029(3) 0.027(3) -0.013(2) 0.004(3) -0.003(3) C3 0.044(4) 0.032(3) 0.022(3) -0.008(2) -0.003(3) -0.003(3) C4 0.030(3) 0.024(3) 0.037(3) -0.009(3) -0.003(3) -0.004(2) C5 0.037(4) 0.022(3) 0.038(4) -0.001(3) 0.002(3) -0.009(3) C6 0.048(5) 0.014(3) 0.090(7) -0.017(4) -0.015(4) 0.009(3) C7 0.069(6) 0.024(3) 0.054(5) 0.012(3) 0.016(4) 0.009(3) C8 0.056(5) 0.035(4) 0.043(4) -0.001(3) -0.014(4) 0.025(3) C9 0.053(5) 0.019(3) 0.090(6) 0.000(4) 0.036(5) 0.008(3) C10 0.109(7) 0.026(4) 0.029(3) -0.001(3) 0.005(4) 0.037(4) C11 0.031(3) 0.028(3) 0.032(3) 0.006(3) -0.006(3) 0.001(3) C12 0.046(4) 0.054(5) 0.049(4) 0.018(4) 0.019(4) 0.007(4) C13 0.037(4) 0.023(3) 0.037(3) 0.007(3) 0.007(3) 0.003(3) C14 0.041(4) 0.038(4) 0.099(7) 0.010(4) 0.014(5) 0.007(3) C15 0.055(5) 0.039(4) 0.022(3) -0.004(3) 0.011(3) -0.004(3) C16 0.108(9) 0.124(10) 0.074(7) -0.058(7) 0.014(7) -0.038(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 C8 2.253(6) . ? W1 C9 2.260(6) . ? W1 C7 2.290(6) . ? W1 C1 2.293(5) . ? W1 C2 2.299(5) . ? W1 C3 2.306(6) . ? W1 C10 2.316(6) . ? W1 C5 2.320(6) . ? W1 C4 2.324(6) . ? W1 C6 2.331(6) . ? W1 Ge1 2.6196(6) . ? W1 Sn1 2.7274(5) . ? Sn1 C13 2.188(6) . ? Sn1 C15 2.211(6) . ? Sn1 Br1 2.6251(7) . ? Ge1 C12 1.953(7) . ? Ge1 C11 1.974(6) . ? Ge1 H1 1.81(6) . ? C1 C2 1.442(8) . ? C1 C5 1.446(9) . ? C1 H1A 1.0000 . ? C2 C3 1.411(9) . ? C2 H2A 1.0000 . ? C3 C4 1.415(9) . ? C3 H3A 1.0000 . ? C4 C5 1.401(9) . ? C4 H4A 1.0000 . ? C5 H5A 1.0000 . ? C6 C7 1.382(11) . ? C6 C10 1.405(11) . ? C6 H6A 1.0000 . ? C7 C8 1.362(11) . ? C7 H7A 1.0000 . ? C8 C9 1.430(11) . ? C8 H8A 1.0000 . ? C9 C10 1.418(12) . ? C9 H9A 1.0000 . ? C10 H10A 1.0000 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 C14 1.503(10) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C14 H14D 0.9800 . ? C15 C16 1.306(12) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 H16C 0.9800 . ? C16 H16D 0.9800 . ? C16 H16A 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 C8 W1 C9 37.0(3) . . ? C8 W1 C7 34.9(3) . . ? C9 W1 C7 60.1(3) . . ? C8 W1 C1 141.0(3) . . ? C9 W1 C1 147.0(2) . . ? C7 W1 C1 143.6(3) . . ? C8 W1 C2 112.6(2) . . ? C9 W1 C2 144.0(3) . . ? C7 W1 C2 107.2(2) . . ? C1 W1 C2 36.6(2) . . ? C8 W1 C3 81.6(2) . . ? C9 W1 C3 108.4(3) . . ? C7 W1 C3 92.1(3) . . ? C1 W1 C3 60.3(2) . . ? C2 W1 C3 35.7(2) . . ? C8 W1 C10 59.7(3) . . ? C9 W1 C10 36.1(3) . . ? C7 W1 C10 59.3(3) . . ? C1 W1 C10 156.0(2) . . ? C2 W1 C10 165.7(3) . . ? C3 W1 C10 141.1(2) . . ? C8 W1 C5 117.7(3) . . ? C9 W1 C5 110.4(2) . . ? C7 W1 C5 147.3(3) . . ? C1 W1 C5 36.5(2) . . ? C2 W1 C5 60.4(2) . . ? C3 W1 C5 59.7(2) . . ? C10 W1 C5 133.3(3) . . ? C8 W1 C4 85.1(3) . . ? C9 W1 C4 92.7(3) . . ? C7 W1 C4 112.2(3) . . ? C1 W1 C4 59.6(2) . . ? C2 W1 C4 59.2(2) . . ? C3 W1 C4 35.6(2) . . ? C10 W1 C4 127.9(3) . . ? C5 W1 C4 35.1(2) . . ? C8 W1 C6 57.9(3) . . ? C9 W1 C6 59.2(3) . . ? C7 W1 C6 34.8(3) . . ? C1 W1 C6 153.6(2) . . ? C2 W1 C6 130.9(3) . . ? C3 W1 C6 126.5(3) . . ? C10 W1 C6 35.2(3) . . ? C5 W1 C6 168.4(3) . . ? C4 W1 C6 143.1(3) . . ? C8 W1 Ge1 125.5(2) . . ? C9 W1 Ge1 88.6(2) . . ? C7 W1 Ge1 131.3(2) . . ? C1 W1 Ge1 82.58(16) . . ? C2 W1 Ge1 118.54(16) . . ? C3 W1 Ge1 135.07(16) . . ? C10 W1 Ge1 73.43(17) . . ? C5 W1 Ge1 75.46(16) . . ? C4 W1 Ge1 105.06(16) . . ? C6 W1 Ge1 98.1(2) . . ? C8 W1 Sn1 125.9(2) . . ? C9 W1 Sn1 130.5(2) . . ? C7 W1 Sn1 91.1(2) . . ? C1 W1 Sn1 79.76(16) . . ? C2 W1 Sn1 79.54(16) . . ? C3 W1 Sn1 112.26(16) . . ? C10 W1 Sn1 95.4(2) . . ? C5 W1 Sn1 113.78(16) . . ? C4 W1 Sn1 136.66(15) . . ? C6 W1 Sn1 74.24(19) . . ? Ge1 W1 Sn1 82.017(17) . . ? C13 Sn1 C15 106.1(3) . . ? C13 Sn1 Br1 96.57(16) . . ? C15 Sn1 Br1 96.89(17) . . ? C13 Sn1 W1 121.19(17) . . ? C15 Sn1 W1 121.94(18) . . ? Br1 Sn1 W1 108.25(2) . . ? C12 Ge1 C11 103.8(3) . . ? C12 Ge1 W1 112.0(2) . . ? C11 Ge1 W1 118.35(18) . . ? C12 Ge1 H1 96.9(19) . . ? C11 Ge1 H1 102.4(18) . . ? W1 Ge1 H1 120.2(18) . . ? C2 C1 C5 107.0(6) . . ? C2 C1 W1 71.9(3) . . ? C5 C1 W1 72.7(3) . . ? C2 C1 H1A 126.3 . . ? C5 C1 H1A 126.3 . . ? W1 C1 H1A 126.3 . . ? C3 C2 C1 108.0(5) . . ? C3 C2 W1 72.4(3) . . ? C1 C2 W1 71.5(3) . . ? C3 C2 H2A 125.9 . . ? C1 C2 H2A 125.9 . . ? W1 C2 H2A 125.9 . . ? C2 C3 C4 107.9(6) . . ? C2 C3 W1 71.9(3) . . ? C4 C3 W1 72.9(3) . . ? C2 C3 H3A 125.9 . . ? C4 C3 H3A 125.9 . . ? W1 C3 H3A 125.9 . . ? C5 C4 C3 109.7(6) . . ? C5 C4 W1 72.3(3) . . ? C3 C4 W1 71.5(3) . . ? C5 C4 H4A 125.1 . . ? C3 C4 H4A 125.1 . . ? W1 C4 H4A 125.1 . . ? C4 C5 C1 107.3(5) . . ? C4 C5 W1 72.6(3) . . ? C1 C5 W1 70.7(3) . . ? C4 C5 H5A 126.2 . . ? C1 C5 H5A 126.2 . . ? W1 C5 H5A 126.2 . . ? C7 C6 C10 109.6(7) . . ? C7 C6 W1 71.0(4) . . ? C10 C6 W1 71.8(4) . . ? C7 C6 H6A 125.2 . . ? C10 C6 H6A 125.2 . . ? W1 C6 H6A 125.2 . . ? C8 C7 C6 108.1(7) . . ? C8 C7 W1 71.1(4) . . ? C6 C7 W1 74.2(4) . . ? C8 C7 H7A 125.8 . . ? C6 C7 H7A 125.8 . . ? W1 C7 H7A 125.8 . . ? C7 C8 C9 109.4(7) . . ? C7 C8 W1 74.0(4) . . ? C9 C8 W1 71.8(4) . . ? C7 C8 H8A 125.2 . . ? C9 C8 H8A 125.2 . . ? W1 C8 H8A 125.2 . . ? C10 C9 C8 106.1(7) . . ? C10 C9 W1 74.1(4) . . ? C8 C9 W1 71.2(4) . . ? C10 C9 H9A 126.6 . . ? C8 C9 H9A 126.6 . . ? W1 C9 H9A 126.6 . . ? C6 C10 C9 106.8(7) . . ? C6 C10 W1 73.0(4) . . ? C9 C10 W1 69.8(4) . . ? C6 C10 H10A 126.5 . . ? C9 C10 H10A 126.5 . . ? W1 C10 H10A 126.5 . . ? Ge1 C11 H11A 109.5 . . ? Ge1 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? Ge1 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? Ge1 C12 H12A 109.5 . . ? Ge1 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? Ge1 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C14 C13 Sn1 115.6(4) . . ? C14 C13 H13A 108.4 . . ? Sn1 C13 H13A 108.4 . . ? C14 C13 H13B 108.4 . . ? Sn1 C13 H13B 108.4 . . ? H13A C13 H13B 107.4 . . ? C13 C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C13 C14 H14D 109.5 . . ? H14B C14 H14D 109.5 . . ? H14C C14 H14D 109.5 . . ? C16 C15 Sn1 122.3(6) . . ? C16 C15 H15A 106.7 . . ? Sn1 C15 H15A 106.7 . . ? C16 C15 H15B 106.7 . . ? Sn1 C15 H15B 106.7 . . ? H15A C15 H15B 106.6 . . ? C15 C16 H16C 109.5 . . ? C15 C16 H16D 109.5 . . ? H16C C16 H16D 109.5 . . ? C15 C16 H16A 109.5 . . ? H16C C16 H16A 109.5 . . ? H16D C16 H16A 109.5 . . ? _diffrn_measured_fraction_theta_max 0.974 _diffrn_reflns_theta_full 28.99 _diffrn_measured_fraction_theta_full 0.974 _refine_diff_density_max 2.217 _refine_diff_density_min -0.966 _refine_diff_density_rms 0.199