Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2003 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 loop_ _publ_author_name 'Keith Dillon' 'Andrei S. Batsanov' 'Stephanie M. Cornet' 'Andres E. Goeta' 'Amber L. Thompson' ; B.Y.Xue ; _publ_contact_author_name 'Dr Keith Dillon' _publ_contact_author_address ; Department of Chemistry University of Durham South Road Durham DH1 3LE UNITED KINGDOM ; _publ_contact_author_email K.B.DILLON@DURHAM.AC.UK _publ_section_title ; The Synthesis and Characterisation of some Group 14 Compounds containing the 2,4,6-(CF3)3C6H2, 2,6-(CF3)2C6H3 or 2,4-(CF3)3C6H3 Ligands ; data_(4a) _database_code_CSD 205552 _audit_creation_method SHELXL-97 _chemical_name_systematic ; bis-(2,4-bis-trifluoromethyl-phenyl)-dichloro-silane ; _chemical_name_common bis-(2,4-bis-trifluoromethyl-phenyl)-dichloro-silane _chemical_melting_point 'not measured' _chemical_formula_moiety 'C16 H6 Cl2 F12 Si' _chemical_formula_sum 'C16 H6 Cl2 F12 Si' _chemical_formula_weight 525.20 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 '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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 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 10.429(7) _cell_length_b 11.534(7) _cell_length_c 16.608(10) _cell_angle_alpha 90.00 _cell_angle_beta 107.84(2) _cell_angle_gamma 90.00 _cell_volume 1902(2) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 904 _cell_measurement_theta_min 12.0 _cell_measurement_theta_max 24.0 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.26 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.834 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1032 _exptl_absorpt_coefficient_mu 0.520 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.807 _exptl_absorpt_correction_T_max 0.874 _exptl_absorpt_process_details 'SADABS (G.M.Sheldrick, 1998), R(int)=0.045 before correction' _exptl_special_details ; Four sets of \w scans (each scan 0.3\% in \w, exposure time 15 s), each set at different \f and/or 2\q angles, nominally covered over 2/3 of full sphere of reciprocal space. The first 50 scans (220 reflections) were repeated at the end of data collection, revealing no significant crystal decay. Crystal to detector distance 4.51 cm. ; _diffrn_ambient_temperature 120(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 'SMART 1K CCD area detector' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 8 _diffrn_reflns_number 17420 _diffrn_reflns_av_R_equivalents 0.0321 _diffrn_reflns_av_sigmaI/netI 0.0248 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.06 _diffrn_reflns_theta_max 29.13 _reflns_number_total 5059 _reflns_number_gt 4018 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _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. ; _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^)+(0.0417P)^2^+1.3379P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment refall _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_number_reflns 5059 _refine_ls_number_parameters 304 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0507 _refine_ls_R_factor_gt 0.0356 _refine_ls_wR_factor_ref 0.0938 _refine_ls_wR_factor_gt 0.0861 _refine_ls_goodness_of_fit_ref 1.021 _refine_ls_restrained_S_all 1.021 _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 Si Si 0.65768(5) 0.51964(4) 0.20903(3) 0.02141(11) Uani 1 1 d . . . Cl1 Cl 0.68478(5) 0.44718(4) 0.10273(3) 0.03322(12) Uani 1 1 d . . . Cl2 Cl 0.84785(4) 0.56570(4) 0.28110(3) 0.03209(11) Uani 1 1 d . . . F11 F 0.63963(12) 0.63895(11) 0.35897(7) 0.0363(3) Uani 1 1 d . . . F12 F 0.51594(14) 0.78231(11) 0.37067(7) 0.0400(3) Uani 1 1 d . . . F13 F 0.42577(14) 0.61668(14) 0.32785(8) 0.0491(4) Uani 1 1 d . . . F14 F 0.31684(14) 1.03746(11) 0.14684(8) 0.0410(3) Uani 1 1 d . . . F15 F 0.18836(14) 0.93692(13) 0.04535(10) 0.0574(4) Uani 1 1 d . . . F16 F 0.36177(17) 1.02197(12) 0.02999(9) 0.0546(4) Uani 1 1 d . . . F21 F 0.38437(12) 0.46368(10) 0.11266(7) 0.0342(3) Uani 1 1 d . . . F22 F 0.40973(13) 0.28337(11) 0.08869(7) 0.0380(3) Uani 1 1 d . . . F23 F 0.24974(11) 0.33617(13) 0.13642(8) 0.0417(3) Uani 1 1 d . . . F24 F 0.43326(19) 0.03922(11) 0.36202(8) 0.0566(4) Uani 1 1 d . . . F25 F 0.36119(17) 0.16518(14) 0.43117(12) 0.0628(5) Uani 1 1 d . . . F26 F 0.56284(15) 0.10468(14) 0.47861(8) 0.0562(4) Uani 1 1 d . . . C11 C 0.55451(16) 0.65586(14) 0.17816(10) 0.0202(3) Uani 1 1 d . . . C12 C 0.50306(17) 0.72449(15) 0.23154(10) 0.0213(3) Uani 1 1 d . . . C13 C 0.42706(18) 0.82368(15) 0.20197(11) 0.0237(3) Uani 1 1 d . . . H13 H 0.392(2) 0.867(2) 0.2381(14) 0.027(5) Uiso 1 1 d . . . C14 C 0.40010(17) 0.85683(15) 0.11783(11) 0.0238(3) Uani 1 1 d . . . C15 C 0.44899(19) 0.79143(16) 0.06340(11) 0.0259(4) Uani 1 1 d . . . H15 H 0.433(2) 0.815(2) 0.0082(15) 0.035(6) Uiso 1 1 d . . . C16 C 0.52517(18) 0.69245(15) 0.09360(11) 0.0237(3) Uani 1 1 d . . . H16 H 0.555(2) 0.6462(19) 0.0559(13) 0.024(5) Uiso 1 1 d . . . C17 C 0.52133(19) 0.69136(16) 0.32278(11) 0.0268(4) Uani 1 1 d . . . C18 C 0.3167(2) 0.96296(17) 0.08539(12) 0.0315(4) Uani 1 1 d . . . C21 C 0.59136(17) 0.40370(14) 0.26564(10) 0.0209(3) Uani 1 1 d . . . C22 C 0.47015(16) 0.34111(14) 0.23214(10) 0.0200(3) Uani 1 1 d . . . C23 C 0.43092(17) 0.25555(15) 0.27885(10) 0.0212(3) Uani 1 1 d . . . H23 H 0.351(2) 0.2156(19) 0.2555(14) 0.027(5) Uiso 1 1 d . . . C24 C 0.51215(18) 0.22985(15) 0.36062(10) 0.0226(3) Uani 1 1 d . . . C25 C 0.63116(19) 0.28942(16) 0.39549(11) 0.0262(4) Uani 1 1 d . . . H25 H 0.690(2) 0.270(2) 0.4503(15) 0.036(6) Uiso 1 1 d . . . C26 C 0.66982(18) 0.37519(16) 0.34834(11) 0.0248(3) Uani 1 1 d . . . H26 H 0.755(2) 0.413(2) 0.3713(14) 0.032(6) Uiso 1 1 d . . . C27 C 0.37848(18) 0.35707(16) 0.14309(11) 0.0252(3) Uani 1 1 d . . . C28 C 0.4674(2) 0.13455(16) 0.40828(11) 0.0278(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 Si 0.0220(2) 0.0193(2) 0.0233(2) 0.00277(17) 0.00743(17) 0.00156(17) Cl1 0.0423(3) 0.0302(2) 0.0324(2) 0.00030(18) 0.01916(19) 0.00712(19) Cl2 0.0214(2) 0.0327(2) 0.0401(2) 0.00716(19) 0.00635(17) -0.00210(17) F11 0.0440(7) 0.0416(7) 0.0221(5) 0.0055(5) 0.0082(5) 0.0151(5) F12 0.0587(8) 0.0390(7) 0.0241(5) -0.0030(5) 0.0155(5) 0.0130(6) F13 0.0533(8) 0.0603(9) 0.0377(7) 0.0095(6) 0.0196(6) -0.0199(7) F14 0.0495(7) 0.0286(6) 0.0391(6) -0.0049(5) 0.0050(5) 0.0152(5) F15 0.0358(7) 0.0420(8) 0.0722(10) -0.0068(7) -0.0162(7) 0.0094(6) F16 0.0818(11) 0.0371(7) 0.0508(8) 0.0234(6) 0.0292(7) 0.0246(7) F21 0.0394(6) 0.0266(6) 0.0276(5) 0.0098(4) -0.0031(5) -0.0038(5) F22 0.0549(8) 0.0351(6) 0.0201(5) -0.0048(4) 0.0058(5) -0.0018(6) F23 0.0233(5) 0.0589(8) 0.0358(6) 0.0155(6) -0.0017(5) -0.0061(5) F24 0.1074(13) 0.0298(7) 0.0353(7) -0.0043(5) 0.0255(7) -0.0279(7) F25 0.0683(10) 0.0532(9) 0.0891(12) 0.0272(8) 0.0570(9) 0.0113(8) F26 0.0577(9) 0.0579(9) 0.0387(7) 0.0281(6) -0.0062(6) -0.0195(7) C11 0.0207(7) 0.0183(7) 0.0215(7) 0.0007(6) 0.0063(6) -0.0018(6) C12 0.0224(8) 0.0207(8) 0.0206(7) 0.0002(6) 0.0064(6) -0.0023(6) C13 0.0247(8) 0.0215(8) 0.0252(8) -0.0031(6) 0.0079(6) -0.0003(7) C14 0.0246(8) 0.0198(8) 0.0243(8) 0.0000(6) 0.0034(6) 0.0000(6) C15 0.0326(9) 0.0233(8) 0.0203(8) 0.0026(6) 0.0059(6) 0.0001(7) C16 0.0298(9) 0.0208(8) 0.0210(7) 0.0009(6) 0.0086(6) 0.0008(7) C17 0.0314(9) 0.0271(9) 0.0234(8) 0.0011(7) 0.0108(7) 0.0013(7) C18 0.0352(10) 0.0251(9) 0.0295(9) -0.0005(7) 0.0031(7) 0.0055(8) C21 0.0219(8) 0.0183(7) 0.0213(7) 0.0012(6) 0.0049(6) 0.0011(6) C22 0.0225(8) 0.0187(8) 0.0177(7) 0.0001(6) 0.0046(6) 0.0023(6) C23 0.0230(8) 0.0194(8) 0.0204(7) -0.0013(6) 0.0056(6) -0.0010(6) C24 0.0290(9) 0.0180(8) 0.0208(7) 0.0006(6) 0.0075(6) 0.0004(6) C25 0.0306(9) 0.0238(9) 0.0202(7) 0.0032(6) 0.0019(6) -0.0022(7) C26 0.0246(8) 0.0228(8) 0.0226(8) 0.0017(6) 0.0010(6) -0.0031(7) C27 0.0261(8) 0.0257(9) 0.0210(8) 0.0024(6) 0.0031(6) -0.0021(7) C28 0.0364(10) 0.0252(9) 0.0215(8) 0.0025(7) 0.0085(7) -0.0036(7) _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 Si C21 1.8838(19) . ? Si C11 1.8845(19) . ? Si Cl2 2.0479(13) . ? Si Cl1 2.0497(12) . ? Si F21 2.882(2) . ? Si F11 2.9013(18) . ? F21 C27 1.338(2) . ? F22 C27 1.351(2) . ? F23 C27 1.335(2) . ? F24 C28 1.326(2) . ? F25 C28 1.325(3) . ? F26 C28 1.327(2) . ? F11 C17 1.340(2) . ? F12 C17 1.328(2) . ? F13 C17 1.339(2) . ? F14 C18 1.334(2) . ? F15 C18 1.334(3) . ? F16 C18 1.340(3) . ? C21 C26 1.406(2) . ? C21 C22 1.413(2) . ? C22 C23 1.392(2) . ? C22 C27 1.506(2) . ? C23 C24 1.395(2) . ? C23 H23 0.93(2) . ? C24 C25 1.381(3) . ? C24 C28 1.510(2) . ? C25 C26 1.396(3) . ? C25 H25 0.96(2) . ? C26 H26 0.96(2) . ? C11 C16 1.407(2) . ? C11 C12 1.411(2) . ? C12 C13 1.393(2) . ? C12 C17 1.517(3) . ? C13 C14 1.392(3) . ? C13 H13 0.94(2) . ? C14 C15 1.389(3) . ? C14 C18 1.503(3) . ? C15 C16 1.393(3) . ? C15 H15 0.92(2) . ? C16 H16 0.95(2) . ? 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 C21 Si C11 117.47(8) . . ? C21 Si Cl2 109.29(6) . . ? C11 Si Cl2 108.22(7) . . ? C21 Si Cl1 108.00(7) . . ? C11 Si Cl1 108.88(6) . . ? Cl2 Si Cl1 104.17(5) . . ? C21 Si F21 70.51(6) . . ? C11 Si F21 69.55(7) . . ? Cl2 Si F21 176.92(4) . . ? Cl1 Si F21 78.71(5) . . ? C21 Si F11 77.18(7) . . ? C11 Si F11 69.90(6) . . ? Cl2 Si F11 71.41(5) . . ? Cl1 Si F11 174.30(4) . . ? F21 Si F11 105.64(5) . . ? C27 F21 Si 98.52(9) . . ? C17 F11 Si 97.00(10) . . ? C26 C21 C22 116.61(15) . . ? C26 C21 Si 117.44(13) . . ? C22 C21 Si 125.94(12) . . ? C23 C22 C21 121.53(15) . . ? C23 C22 C27 115.30(15) . . ? C21 C22 C27 123.10(15) . . ? C22 C23 C24 119.92(16) . . ? C22 C23 H23 120.0(13) . . ? C24 C23 H23 120.1(13) . . ? C25 C24 C23 120.16(16) . . ? C25 C24 C28 121.65(16) . . ? C23 C24 C28 118.18(16) . . ? C24 C25 C26 119.63(16) . . ? C24 C25 H25 121.3(15) . . ? C26 C25 H25 119.0(15) . . ? C25 C26 C21 122.16(16) . . ? C25 C26 H26 119.6(14) . . ? C21 C26 H26 118.2(14) . . ? F23 C27 F21 107.21(15) . . ? F23 C27 F22 105.87(15) . . ? F21 C27 F22 106.10(15) . . ? F23 C27 C22 112.28(15) . . ? F21 C27 C22 113.23(14) . . ? F22 C27 C22 111.66(15) . . ? F25 C28 F24 106.71(18) . . ? F25 C28 F26 106.51(17) . . ? F24 C28 F26 106.90(17) . . ? F25 C28 C24 112.10(16) . . ? F24 C28 C24 111.79(15) . . ? F26 C28 C24 112.45(16) . . ? C16 C11 C12 116.77(16) . . ? C16 C11 Si 116.93(13) . . ? C12 C11 Si 126.30(13) . . ? C13 C12 C11 121.60(16) . . ? C13 C12 C17 116.30(15) . . ? C11 C12 C17 122.04(15) . . ? C14 C13 C12 119.86(16) . . ? C14 C13 H13 119.9(14) . . ? C12 C13 H13 120.2(14) . . ? C15 C14 C13 120.18(16) . . ? C15 C14 C18 119.78(16) . . ? C13 C14 C18 120.03(16) . . ? C14 C15 C16 119.55(16) . . ? C14 C15 H15 119.7(15) . . ? C16 C15 H15 120.7(15) . . ? C15 C16 C11 122.04(16) . . ? C15 C16 H16 119.4(13) . . ? C11 C16 H16 118.5(13) . . ? F12 C17 F13 107.55(16) . . ? F12 C17 F11 106.85(15) . . ? F13 C17 F11 106.40(16) . . ? F12 C17 C12 112.56(16) . . ? F13 C17 C12 110.90(15) . . ? F11 C17 C12 112.24(15) . . ? F15 C18 F14 106.99(17) . . ? F15 C18 F16 106.35(17) . . ? F14 C18 F16 106.25(17) . . ? F15 C18 C14 112.19(17) . . ? F14 C18 C14 112.69(16) . . ? F16 C18 C14 111.95(17) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Cl2 Si C21 C26 6.43(15) . . . . ? Cl1 Si C11 C16 -6.23(14) . . . . ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 29.13 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 0.405 _refine_diff_density_min -0.342 _refine_diff_density_rms 0.061 #============================================END data_(5) _database_code_CSD 205553 _audit_creation_method SHELXL-97 _chemical_name_systematic ; Bis-(2,6-bis-trifluoromethyl-phenyl)-difluoro-silane ; _chemical_name_common Bis-(2,6-bis-trifluoromethyl-phenyl)-difluoro-silane _chemical_melting_point 'not measured' _chemical_formula_moiety 'C16 H6 F14 Si' _chemical_formula_sum 'C16 H6 F14 Si' _chemical_formula_weight 492.30 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' F F 0.0171 0.0103 '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' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.221(2) _cell_length_b 9.644(2) _cell_length_c 12.267(3) _cell_angle_alpha 98.48(1) _cell_angle_beta 100.30(1) _cell_angle_gamma 112.50(1) _cell_volume 858.8(4) _cell_formula_units_Z 2 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 5211 _cell_measurement_theta_min 4.707 _cell_measurement_theta_max 54.99 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.904 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 484 _exptl_absorpt_coefficient_mu 0.284 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9147 _exptl_absorpt_correction_T_max 0.9667 _exptl_absorpt_process_details 'SADABS (G.M.Sheldrick, 1998)' _exptl_special_details ; The data collection nominally covered half a sphere of reciprocal Space, by a combination of 3 sets of \w scans each set at different \f and/or 2\q angles and each scan (15s exposure) covering 0.3\% in \w. Crystal to detector distance 4.51 cm. ; _diffrn_ambient_temperature 120(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 CCD 1K area detector' _diffrn_measurement_method \w-scans _diffrn_detector_area_resol_mean 8 _diffrn_reflns_number 6314 _diffrn_reflns_av_R_equivalents 0.0224 _diffrn_reflns_av_sigmaI/netI 0.0347 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 1.74 _diffrn_reflns_theta_max 27.48 _reflns_number_total 3601 _reflns_number_gt 2970 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'SMART-NT V5.0 (Bruker, 1998)' _computing_cell_refinement 'SMART-NT V5.0 (Bruker, 1998)' _computing_data_reduction 'SMART-NT V5.0 (Bruker, 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _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. ; _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^)+(0.0342P)^2^+0.3334P] 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 none _refine_ls_number_reflns 3601 _refine_ls_number_parameters 280 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0448 _refine_ls_R_factor_gt 0.0343 _refine_ls_wR_factor_ref 0.0838 _refine_ls_wR_factor_gt 0.0793 _refine_ls_goodness_of_fit_ref 1.032 _refine_ls_restrained_S_all 1.032 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Si Si 0.30303(7) 0.79845(5) 0.78158(4) 0.02193(12) Uani 1 1 d . . . F1 F 0.34709(16) 0.97514(12) 0.80871(10) 0.0341(3) Uani 1 1 d . . . F2 F 0.10860(14) 0.71878(12) 0.80355(10) 0.0312(3) Uani 1 1 d . . . C11 C 0.2709(2) 0.71238(19) 0.62586(16) 0.0227(4) Uani 1 1 d . . . C12 C 0.2648(2) 0.56368(19) 0.58856(16) 0.0242(4) Uani 1 1 d . . . C13 C 0.2499(3) 0.5018(2) 0.47601(18) 0.0327(4) Uani 1 1 d . . . H13 H 0.2470 0.4019 0.4548 0.039 Uiso 1 1 d R . . C14 C 0.2393(3) 0.5850(2) 0.39419(18) 0.0358(5) Uani 1 1 d . . . H14 H 0.2335 0.5445 0.3175 0.043 Uiso 1 1 d R . . C15 C 0.2372(3) 0.7273(2) 0.42552(18) 0.0325(4) Uani 1 1 d . . . H15 H 0.2267 0.7838 0.3694 0.039 Uiso 1 1 d R . . C16 C 0.2503(2) 0.7896(2) 0.53806(17) 0.0261(4) Uani 1 1 d . . . C17 C 0.2757(2) 0.46038(19) 0.66895(17) 0.0263(4) Uani 1 1 d . . . F11 F 0.20434(15) 0.48222(11) 0.75708(10) 0.0303(3) Uani 1 1 d . . . F12 F 0.44854(15) 0.48377(12) 0.71466(10) 0.0343(3) Uani 1 1 d . . . F13 F 0.18575(17) 0.31076(12) 0.61677(11) 0.0384(3) Uani 1 1 d . . . C18 C 0.2316(3) 0.9410(2) 0.56055(18) 0.0324(5) Uani 1 1 d . . . F14 F 0.38949(16) 1.06196(12) 0.61720(12) 0.0411(3) Uani 1 1 d . . . F15 F 0.10949(16) 0.93385(13) 0.62139(11) 0.0357(3) Uani 1 1 d . . . F16 F 0.17360(18) 0.97592(15) 0.46375(11) 0.0453(3) Uani 1 1 d . . . C21 C 0.4896(2) 0.77996(17) 0.88634(15) 0.0211(4) Uani 1 1 d . . . C22 C 0.6634(2) 0.81344(18) 0.86641(16) 0.0231(4) Uani 1 1 d . . . C23 C 0.7978(3) 0.7882(2) 0.93676(18) 0.0292(4) Uani 1 1 d . . . H23 H 0.9120 0.8103 0.9196 0.035 Uiso 1 1 d R . . C24 C 0.7646(3) 0.7313(2) 1.03103(18) 0.0319(4) Uani 1 1 d . . . H24 H 0.8535 0.7096 1.0771 0.038 Uiso 1 1 d R . . C25 C 0.6010(3) 0.7060(2) 1.05816(17) 0.0310(4) Uani 1 1 d . . . H25 H 0.5801 0.6713 1.1250 0.037 Uiso 1 1 d R . . C26 C 0.4664(3) 0.73103(18) 0.98838(16) 0.0247(4) Uani 1 1 d . . . C27 C 0.7200(2) 0.8808(2) 0.76864(17) 0.0267(4) Uani 1 1 d . . . C28 C 0.2976(3) 0.7080(2) 1.02928(18) 0.0316(4) Uani 1 1 d . . . F21 F 0.62559(15) 0.95927(12) 0.73135(10) 0.0312(3) Uani 1 1 d . . . F22 F 0.89594(15) 0.98026(14) 0.79698(11) 0.0394(3) Uani 1 1 d . . . F23 F 0.69648(18) 0.77255(13) 0.67738(10) 0.0401(3) Uani 1 1 d . . . F24 F 0.15161(16) 0.58013(13) 0.96861(11) 0.0405(3) Uani 1 1 d . . . F25 F 0.25171(16) 0.82788(13) 1.02466(10) 0.0336(3) Uani 1 1 d . . . F26 F 0.31984(19) 0.69759(16) 1.13842(11) 0.0481(3) 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 Si 0.0212(2) 0.0223(2) 0.0245(3) 0.00372(19) 0.0062(2) 0.01186(19) F1 0.0404(7) 0.0267(5) 0.0372(7) 0.0033(5) 0.0059(5) 0.0195(5) F2 0.0249(6) 0.0372(6) 0.0333(6) 0.0051(5) 0.0104(5) 0.0148(5) C11 0.0182(8) 0.0246(8) 0.0259(10) 0.0050(7) 0.0060(7) 0.0097(7) C12 0.0197(8) 0.0270(8) 0.0253(10) 0.0033(7) 0.0044(8) 0.0110(7) C13 0.0306(10) 0.0349(10) 0.0305(11) -0.0011(8) 0.0073(9) 0.0151(8) C14 0.0295(10) 0.0506(12) 0.0241(11) 0.0026(9) 0.0079(9) 0.0154(9) C15 0.0252(10) 0.0453(11) 0.0277(11) 0.0130(9) 0.0068(8) 0.0139(8) C16 0.0201(8) 0.0311(9) 0.0285(11) 0.0100(8) 0.0071(8) 0.0108(7) C17 0.0252(9) 0.0227(8) 0.0293(11) 0.0009(7) 0.0050(8) 0.0111(7) F11 0.0358(6) 0.0270(5) 0.0319(6) 0.0087(5) 0.0128(5) 0.0147(5) F12 0.0282(6) 0.0354(6) 0.0426(7) 0.0105(5) 0.0047(5) 0.0185(5) F13 0.0440(7) 0.0216(5) 0.0438(7) -0.0006(5) 0.0049(6) 0.0135(5) C18 0.0295(10) 0.0359(10) 0.0373(12) 0.0173(9) 0.0080(9) 0.0166(8) F14 0.0351(7) 0.0293(6) 0.0582(9) 0.0164(6) 0.0087(6) 0.0121(5) F15 0.0344(6) 0.0412(6) 0.0441(7) 0.0162(5) 0.0137(6) 0.0253(5) F16 0.0507(8) 0.0547(7) 0.0457(8) 0.0301(6) 0.0123(6) 0.0317(6) C21 0.0214(8) 0.0176(7) 0.0242(9) 0.0025(6) 0.0060(7) 0.0090(6) C22 0.0233(9) 0.0206(8) 0.0245(10) 0.0017(7) 0.0058(8) 0.0098(7) C23 0.0225(9) 0.0277(9) 0.0373(12) 0.0034(8) 0.0056(8) 0.0129(7) C24 0.0320(10) 0.0268(9) 0.0354(11) 0.0061(8) -0.0002(9) 0.0153(8) C25 0.0407(11) 0.0239(8) 0.0289(11) 0.0082(8) 0.0065(9) 0.0146(8) C26 0.0289(9) 0.0186(7) 0.0261(10) 0.0035(7) 0.0079(8) 0.0095(7) C27 0.0209(9) 0.0275(8) 0.0308(11) 0.0031(7) 0.0078(8) 0.0100(7) C28 0.0376(11) 0.0320(9) 0.0295(11) 0.0097(8) 0.0139(9) 0.0159(8) F21 0.0299(6) 0.0345(6) 0.0347(7) 0.0143(5) 0.0122(5) 0.0153(5) F22 0.0226(6) 0.0444(6) 0.0451(8) 0.0139(6) 0.0100(5) 0.0059(5) F23 0.0501(8) 0.0375(6) 0.0352(7) 0.0017(5) 0.0224(6) 0.0186(6) F24 0.0338(7) 0.0330(6) 0.0532(8) 0.0126(6) 0.0208(6) 0.0071(5) F25 0.0365(6) 0.0380(6) 0.0330(7) 0.0054(5) 0.0147(5) 0.0213(5) F26 0.0591(9) 0.0671(9) 0.0344(8) 0.0248(6) 0.0259(7) 0.0331(7) _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 Si F1 1.5694(11) . ? Si F2 1.5790(13) . ? Si C11 1.895(2) . ? Si C21 1.8991(19) . ? Si F21 2.7450(13) . ? Si F11 2.7925(13) . ? C11 C16 1.418(3) . ? C11 C12 1.418(2) . ? C12 C13 1.385(3) . ? C12 C17 1.517(3) . ? C13 C14 1.385(3) . ? C14 C15 1.377(3) . ? C15 C16 1.390(3) . ? C16 C18 1.517(3) . ? C17 F13 1.334(2) . ? C17 F11 1.346(2) . ? C17 F12 1.348(2) . ? C18 F16 1.337(2) . ? C18 F15 1.341(2) . ? C18 F14 1.344(2) . ? C21 C22 1.415(3) . ? C21 C26 1.420(3) . ? C22 C23 1.397(3) . ? C22 C27 1.509(3) . ? C23 C24 1.378(3) . ? C24 C25 1.383(3) . ? C25 C26 1.393(3) . ? C26 C28 1.508(3) . ? C27 F22 1.339(2) . ? C27 F23 1.343(2) . ? C27 F21 1.345(2) . ? C28 F24 1.338(2) . ? C28 F26 1.342(2) . ? C28 F25 1.352(2) . ? 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 F1 Si F2 104.06(6) . . ? F1 Si C11 113.76(7) . . ? F2 Si C11 104.65(7) . . ? F1 Si C21 105.27(7) . . ? F2 Si C21 113.17(8) . . ? C11 Si C21 115.53(8) . . ? F1 Si F21 70.83(5) . . ? F2 Si F21 173.14(5) . . ? C11 Si F21 74.09(6) . . ? C21 Si F21 73.07(6) . . ? F1 Si F11 172.60(6) . . ? F2 Si F11 70.18(5) . . ? C11 Si F11 72.78(6) . . ? C21 Si F11 73.72(6) . . ? F21 Si F11 115.29(4) . . ? C16 C11 C12 114.88(17) . . ? C16 C11 Si 123.28(13) . . ? C12 C11 Si 121.84(14) . . ? C13 C12 C11 122.66(18) . . ? C13 C12 C17 114.69(16) . . ? C11 C12 C17 122.65(17) . . ? C12 C13 C14 120.28(18) . . ? C15 C14 C13 119.14(19) . . ? C14 C15 C16 120.93(19) . . ? C15 C16 C11 121.97(17) . . ? C15 C16 C18 116.10(17) . . ? C11 C16 C18 121.86(17) . . ? F13 C17 F11 106.20(15) . . ? F13 C17 F12 106.45(14) . . ? F11 C17 F12 106.43(15) . . ? F13 C17 C12 112.18(16) . . ? F11 C17 C12 112.68(14) . . ? F12 C17 C12 112.42(15) . . ? C17 F11 Si 97.49(9) . . ? F16 C18 F15 106.62(15) . . ? F16 C18 F14 106.20(15) . . ? F15 C18 F14 107.84(17) . . ? F16 C18 C16 111.88(17) . . ? F15 C18 C16 110.96(15) . . ? F14 C18 C16 112.99(16) . . ? C22 C21 C26 115.14(16) . . ? C22 C21 Si 121.37(14) . . ? C26 C21 Si 123.48(13) . . ? C23 C22 C21 122.57(18) . . ? C23 C22 C27 114.40(17) . . ? C21 C22 C27 123.02(16) . . ? C24 C23 C22 119.97(18) . . ? C23 C24 C25 119.58(18) . . ? C24 C25 C26 120.66(19) . . ? C25 C26 C21 121.80(18) . . ? C25 C26 C28 116.19(18) . . ? C21 C26 C28 121.98(17) . . ? F22 C27 F23 106.41(15) . . ? F22 C27 F21 106.04(14) . . ? F23 C27 F21 106.02(15) . . ? F22 C27 C22 112.31(16) . . ? F23 C27 C22 112.72(14) . . ? F21 C27 C22 112.80(15) . . ? F24 C28 F26 106.43(16) . . ? F24 C28 F25 106.82(17) . . ? F26 C28 F25 105.76(16) . . ? F24 C28 C26 113.33(16) . . ? F26 C28 C26 112.35(17) . . ? F25 C28 C26 111.66(15) . . ? C27 F21 Si 99.44(10) . . ? _diffrn_measured_fraction_theta_max 0.914 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.938 _refine_diff_density_max 0.424 _refine_diff_density_min -0.247 _refine_diff_density_rms 0.048 #============================================END data_(1b) _database_code_CSD 205554 _audit_creation_method SHELXL-97 _chemical_name_systematic ; Bis-(2,4,6-tris-trifluoromethyl-phenyl)-dichloro-germane ; _chemical_name_common Bis-(2,4,6-tris-trifluoromethyl-phenyl)-dichloro-germane _chemical_melting_point 'not measured' _chemical_formula_moiety 'C18 H4 Cl2 F18 Ge' _chemical_formula_sum 'C18 H4 Cl2 F18 Ge' _chemical_formula_weight 705.70 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 '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' _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 8.3893(6) _cell_length_b 30.043(2) _cell_length_c 8.6373(6) _cell_angle_alpha 90.00 _cell_angle_beta 96.433(1) _cell_angle_gamma 90.00 _cell_volume 2163.2(3) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 7656 _cell_measurement_theta_min 4.936 _cell_measurement_theta_max 54.790 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.34 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 2.167 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1360 _exptl_absorpt_coefficient_mu 1.826 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5757 _exptl_absorpt_correction_T_max 0.8677 _exptl_absorpt_process_details 'SADABS (G.M.Sheldrick, 1998)' _exptl_special_details ; The data collection nominally covered full sphere of reciprocal Space, by a combination of 5 sets of \w scans each set at different \f and/or 2\q angles and each scan (20s exposure) covering 0.3\% in \w. Crystal to detector distance 5.51 cm. ; _diffrn_ambient_temperature 120(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 CCD 1K area detector' _diffrn_measurement_method \w-scans _diffrn_detector_area_resol_mean 8 _diffrn_reflns_number 16108 _diffrn_reflns_av_R_equivalents 0.0421 _diffrn_reflns_av_sigmaI/netI 0.0378 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -38 _diffrn_reflns_limit_k_max 38 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 2.47 _diffrn_reflns_theta_max 27.48 _reflns_number_total 4795 _reflns_number_gt 3860 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'SMART-NT V5.0 (Bruker, 1998)' _computing_cell_refinement 'SMART-NT V5.0 (Bruker, 1998)' _computing_data_reduction 'SMART-NT V5.0 (Bruker, 1998)' _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. ; _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^)+(0.0216P)^2^+5.1440P] 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 4795 _refine_ls_number_parameters 365 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0564 _refine_ls_R_factor_gt 0.0405 _refine_ls_wR_factor_ref 0.0851 _refine_ls_wR_factor_gt 0.0793 _refine_ls_goodness_of_fit_ref 1.081 _refine_ls_restrained_S_all 1.085 _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 Ge Ge 0.74612(4) 0.618770(11) 1.04001(4) 0.01535(9) Uani 1 1 d . . . Cl1 Cl 0.97859(11) 0.62655(3) 1.16029(11) 0.0276(2) Uani 1 1 d . . . Cl2 Cl 0.59696(11) 0.60346(3) 1.21993(11) 0.0289(2) Uani 1 1 d . . . C11 C 0.6267(4) 0.67390(10) 0.9602(4) 0.0169(6) Uani 1 1 d . . . C12 C 0.4658(4) 0.67011(10) 0.8916(4) 0.0179(7) Uani 1 1 d . . . C13 C 0.3698(4) 0.70695(11) 0.8538(4) 0.0204(7) Uani 1 1 d . . . H13 H 0.2647 0.7030 0.8087 0.025 Uiso 1 1 d R . . C14 C 0.4290(4) 0.74957(11) 0.8827(4) 0.0191(7) Uani 1 1 d . A . C15 C 0.5858(4) 0.75482(11) 0.9471(4) 0.0204(7) Uani 1 1 d . . . H15 H 0.6269 0.7833 0.9655 0.024 Uiso 1 1 d R . . C16 C 0.6834(4) 0.71801(10) 0.9849(4) 0.0171(6) Uani 1 1 d . . . C17 C 0.3760(4) 0.62710(11) 0.8571(4) 0.0233(7) Uani 1 1 d . . . F11 F 0.4662(2) 0.59068(6) 0.8705(3) 0.0322(5) Uani 1 1 d . . . F12 F 0.2996(3) 0.62688(8) 0.7130(3) 0.0475(7) Uani 1 1 d . . . F13 F 0.2626(3) 0.62189(7) 0.9521(3) 0.0457(7) Uani 1 1 d . . . C18 C 0.8494(4) 0.72955(11) 1.0626(4) 0.0241(7) Uani 1 1 d . . . F14 F 0.9668(2) 0.71080(6) 0.9921(2) 0.0250(4) Uani 1 1 d . . . F15 F 0.8665(3) 0.71664(7) 1.2126(2) 0.0325(5) Uani 1 1 d . . . F16 F 0.8781(3) 0.77346(7) 1.0637(3) 0.0384(6) Uani 1 1 d . . . C19 C 0.3214(4) 0.78885(11) 0.8467(4) 0.0243(7) Uani 1 1 d D . . F17 F 0.2989(7) 0.79850(16) 0.6995(4) 0.091(2) Uani 0.872(7) 1 d PD A 1 F18 F 0.1818(4) 0.78438(11) 0.8985(6) 0.0730(16) Uani 0.872(7) 1 d PD A 1 F19 F 0.3814(4) 0.82629(9) 0.9156(5) 0.0611(14) Uani 0.872(7) 1 d PD A 1 F17A F 0.398(2) 0.8213(5) 0.797(2) 0.032(5) Uiso 0.128(7) 1 d PD A 2 F18A F 0.2155(19) 0.7777(6) 0.726(2) 0.025(5) Uiso 0.128(7) 1 d PD A 2 F19A F 0.249(3) 0.8011(8) 0.959(2) 0.045(6) Uiso 0.128(7) 1 d PD A 2 C21 C 0.7721(4) 0.56786(10) 0.8963(4) 0.0139(6) Uani 1 1 d . . . C22 C 0.7860(4) 0.57524(10) 0.7371(4) 0.0151(6) Uani 1 1 d . . . C23 C 0.7797(4) 0.54073(10) 0.6286(4) 0.0169(6) Uani 1 1 d . . . H23 H 0.7877 0.5468 0.5242 0.020 Uiso 1 1 d R . . C24 C 0.7613(4) 0.49720(10) 0.6778(4) 0.0157(6) Uani 1 1 d . . . C25 C 0.7593(4) 0.48845(10) 0.8342(4) 0.0152(6) Uani 1 1 d . . . H25 H 0.7530 0.4591 0.8677 0.018 Uiso 1 1 d R . . C26 C 0.7667(4) 0.52287(10) 0.9426(4) 0.0147(6) Uani 1 1 d . . . C27 C 0.8097(4) 0.62124(11) 0.6729(4) 0.0206(7) Uani 1 1 d . . . C28 C 0.7679(4) 0.50758(10) 1.1101(4) 0.0182(7) Uani 1 1 d . . . C29 C 0.7476(4) 0.46026(10) 0.5591(4) 0.0196(7) Uani 1 1 d . . . F21 F 0.8910(2) 0.64766(6) 0.7799(2) 0.0234(4) Uani 1 1 d . . . F22 F 0.6693(3) 0.64179(6) 0.6281(2) 0.0278(5) Uani 1 1 d . . . F23 F 0.8915(3) 0.62061(7) 0.5490(2) 0.0298(5) Uani 1 1 d . . . F24 F 0.8376(3) 0.46746(6) 1.1307(2) 0.0258(5) Uani 1 1 d . . . F25 F 0.8508(2) 0.53485(6) 1.2126(2) 0.0217(4) Uani 1 1 d . . . F26 F 0.6198(2) 0.50341(7) 1.1516(2) 0.0252(4) Uani 1 1 d . . . F27 F 0.7386(3) 0.42034(6) 0.6229(2) 0.0341(5) Uani 1 1 d . . . F28 F 0.6164(3) 0.46500(8) 0.4571(3) 0.0436(6) Uani 1 1 d . . . F29 F 0.8712(3) 0.45970(8) 0.4756(3) 0.0423(6) 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 Ge 0.01601(17) 0.01369(15) 0.01658(17) -0.00143(13) 0.00277(12) 0.00123(13) Cl1 0.0242(4) 0.0243(4) 0.0327(5) 0.0012(3) -0.0041(4) -0.0010(3) Cl2 0.0325(5) 0.0273(4) 0.0296(5) 0.0025(4) 0.0153(4) 0.0049(4) C11 0.0165(16) 0.0181(15) 0.0165(15) -0.0036(12) 0.0035(13) -0.0011(12) C12 0.0170(16) 0.0163(15) 0.0208(17) -0.0018(12) 0.0037(13) -0.0003(12) C13 0.0132(16) 0.0238(17) 0.0239(17) 0.0000(13) 0.0003(13) -0.0001(13) C14 0.0206(17) 0.0174(15) 0.0200(17) 0.0040(12) 0.0048(14) 0.0028(13) C15 0.0212(17) 0.0155(15) 0.0242(17) -0.0023(13) 0.0020(14) -0.0002(13) C16 0.0147(16) 0.0182(15) 0.0182(16) -0.0035(12) 0.0016(13) -0.0001(12) C17 0.0177(17) 0.0182(17) 0.033(2) -0.0053(14) 0.0001(15) -0.0001(13) F11 0.0204(11) 0.0165(10) 0.0582(15) -0.0097(9) -0.0026(10) 0.0018(8) F12 0.0540(16) 0.0319(13) 0.0493(15) -0.0078(11) -0.0258(13) -0.0067(11) F13 0.0310(13) 0.0276(12) 0.0839(19) -0.0176(12) 0.0299(13) -0.0118(10) C18 0.0200(18) 0.0176(16) 0.034(2) -0.0059(14) -0.0011(15) -0.0001(13) F14 0.0156(10) 0.0227(10) 0.0367(12) -0.0012(8) 0.0031(9) 0.0001(8) F15 0.0265(12) 0.0434(13) 0.0255(11) -0.0117(9) -0.0062(9) 0.0050(10) F16 0.0267(12) 0.0156(10) 0.0694(17) -0.0120(10) -0.0100(11) -0.0020(8) C19 0.0225(18) 0.0189(17) 0.031(2) 0.0036(14) 0.0019(15) 0.0022(14) F17 0.155(5) 0.086(3) 0.0317(19) 0.0227(19) 0.013(2) 0.089(4) F18 0.0269(18) 0.0314(18) 0.167(4) 0.040(2) 0.037(2) 0.0129(14) F19 0.0456(19) 0.0207(14) 0.109(4) -0.0143(16) -0.0248(19) 0.0139(13) C21 0.0111(15) 0.0150(14) 0.0160(15) 0.0001(12) 0.0028(12) 0.0014(11) C22 0.0133(15) 0.0156(15) 0.0162(15) 0.0021(12) 0.0005(12) 0.0017(12) C23 0.0176(16) 0.0184(15) 0.0151(15) 0.0029(12) 0.0037(13) 0.0028(12) C24 0.0148(16) 0.0162(15) 0.0159(15) 0.0001(12) 0.0009(12) 0.0033(12) C25 0.0155(16) 0.0126(14) 0.0178(16) 0.0022(11) 0.0032(13) 0.0017(12) C26 0.0115(15) 0.0166(14) 0.0163(15) 0.0021(12) 0.0037(12) 0.0011(12) C27 0.0255(18) 0.0175(15) 0.0197(16) 0.0028(13) 0.0067(14) 0.0019(14) C28 0.0229(18) 0.0126(15) 0.0189(16) 0.0005(12) 0.0007(14) 0.0012(12) C29 0.0226(17) 0.0178(15) 0.0183(16) -0.0017(13) 0.0021(14) 0.0028(13) F21 0.0294(11) 0.0163(9) 0.0251(10) -0.0006(8) 0.0058(9) -0.0049(8) F22 0.0346(12) 0.0196(10) 0.0284(11) 0.0066(8) 0.0006(9) 0.0074(9) F23 0.0475(13) 0.0216(10) 0.0237(10) 0.0032(8) 0.0189(10) -0.0023(9) F24 0.0404(13) 0.0162(9) 0.0199(10) 0.0045(8) -0.0011(9) 0.0052(8) F25 0.0263(11) 0.0215(9) 0.0165(9) -0.0007(7) -0.0014(8) -0.0004(8) F26 0.0255(11) 0.0309(11) 0.0205(10) 0.0033(8) 0.0085(9) -0.0046(9) F27 0.0635(16) 0.0152(10) 0.0237(11) -0.0011(8) 0.0051(11) -0.0023(10) F28 0.0487(15) 0.0380(13) 0.0383(13) -0.0183(11) -0.0210(12) 0.0153(11) F29 0.0461(15) 0.0383(13) 0.0485(15) -0.0225(11) 0.0311(12) -0.0098(11) _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 Ge C21 1.997(3) . ? Ge C11 2.017(3) . ? Ge Cl1 2.1174(9) . ? Ge Cl2 2.1513(9) . ? Ge F11 2.757(2) . ? Ge F21 2.809(2) . ? Ge F25 3.0095(19) . ? Ge F14 3.3785(19) . ? Ge F15 3.399(2) . ? C11 C16 1.416(4) . ? C11 C12 1.417(4) . ? C12 C13 1.386(4) . ? C12 C17 1.508(4) . ? C13 C14 1.386(5) . ? C14 C15 1.379(5) . ? C14 C19 1.497(4) . ? C15 C16 1.393(4) . ? C16 C18 1.517(5) . ? C17 F11 1.328(4) . ? C17 F13 1.333(4) . ? C17 F12 1.335(4) . ? C18 F14 1.339(4) . ? C18 F16 1.341(4) . ? C18 F15 1.345(4) . ? C19 F19A 1.255(16) . ? C19 F17A 1.270(14) . ? C19 F17 1.297(5) . ? C19 F18 1.306(5) . ? C19 F18A 1.337(14) . ? C19 F19 1.344(4) . ? C21 C22 1.410(4) . ? C21 C26 1.412(4) . ? C22 C23 1.394(4) . ? C22 C27 1.510(4) . ? C23 C24 1.389(4) . ? C24 C25 1.378(4) . ? C24 C29 1.507(4) . ? C25 C26 1.392(4) . ? C26 C28 1.516(4) . ? C27 F23 1.335(4) . ? C27 F21 1.345(4) . ? C27 F22 1.347(4) . ? C29 F27 1.325(4) . ? C29 F29 1.329(4) . ? C29 F28 1.338(4) . ? C28 F26 1.337(4) . ? C28 F25 1.342(4) . ? C28 F24 1.343(4) . ? 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 C21 Ge C11 120.07(12) . . ? C21 Ge Cl1 103.34(9) . . ? C11 Ge Cl1 118.17(9) . . ? C21 Ge Cl2 113.46(9) . . ? C11 Ge Cl2 96.65(9) . . ? Cl1 Ge Cl2 104.33(4) . . ? Cl1 Ge F11 167.77(5) . . ? Cl2 Ge F21 169.32(5) . . ? C11 Ge F25 164.49(10) . . ? C21 Ge F15 152.55(10) . . ? C16 C11 C12 115.2(3) . . ? C16 C11 Ge 124.8(2) . . ? C12 C11 Ge 119.4(2) . . ? C13 C12 C11 122.4(3) . . ? C13 C12 C17 111.9(3) . . ? C11 C12 C17 125.6(3) . . ? C14 C13 C12 120.5(3) . . ? C15 C14 C13 119.0(3) . . ? C15 C14 C19 121.3(3) . . ? C13 C14 C19 119.7(3) . . ? C14 C15 C16 120.9(3) . . ? C15 C16 C11 121.9(3) . . ? C15 C16 C18 114.1(3) . . ? C11 C16 C18 123.8(3) . . ? F11 C17 F13 106.8(3) . . ? F11 C17 F12 106.6(3) . . ? F13 C17 F12 105.8(3) . . ? F11 C17 C12 114.9(3) . . ? F13 C17 C12 110.8(3) . . ? F12 C17 C12 111.4(3) . . ? C17 F11 Ge 103.71(18) . . ? F14 C18 F16 106.1(3) . . ? F15 C18 F14 108.2(3) . . ? F16 C18 F15 106.1(3) . . ? F14 C18 C16 112.8(3) . . ? F16 C18 C16 112.5(3) . . ? F15 C18 C16 110.7(3) . . ? C18 F15 Ge 80.36(16) . . ? C18 F14 Ge 81.24(17) . . ? F19A C19 F17A 110.1(14) . . ? F19A C19 F17 131.4(11) . . ? F17A C19 F17 61.2(9) . . ? F19A C19 F18 40.2(11) . . ? F17A C19 F18 134.6(9) . . ? F17 C19 F18 108.7(4) . . ? F19A C19 F18A 110.0(14) . . ? F17A C19 F18A 104.1(12) . . ? F17 C19 F18A 43.8(7) . . ? F18 C19 F18A 72.5(8) . . ? F19A C19 F19 66.6(12) . . ? F17A C19 F19 47.8(9) . . ? F17 C19 F19 104.6(4) . . ? F18 C19 F19 103.9(4) . . ? F18A C19 F19 137.7(8) . . ? F19A C19 C14 113.8(11) . . ? F17A C19 C14 111.1(9) . . ? F17 C19 C14 113.5(3) . . ? F18 C19 C14 113.0(3) . . ? F18A C19 C14 107.3(8) . . ? F19 C19 C14 112.4(3) . . ? C22 C21 C26 115.8(3) . . ? C22 C21 Ge 120.8(2) . . ? C26 C21 Ge 123.2(2) . . ? C23 C22 C21 122.5(3) . . ? C23 C22 C27 115.5(3) . . ? C21 C22 C27 122.0(3) . . ? C24 C23 C22 119.4(3) . . ? C25 C24 C23 119.6(3) . . ? C25 C24 C29 121.2(3) . . ? C23 C24 C29 119.2(3) . . ? C24 C25 C26 120.9(3) . . ? C25 C26 C21 121.4(3) . . ? C25 C26 C28 114.3(3) . . ? C21 C26 C28 124.3(3) . . ? F23 C27 F21 107.0(3) . . ? F23 C27 F22 106.7(3) . . ? F21 C27 F22 106.7(3) . . ? F23 C27 C22 112.5(3) . . ? F21 C27 C22 111.4(3) . . ? F22 C27 C22 112.2(3) . . ? F27 C29 F29 107.4(3) . . ? F27 C29 F28 106.8(3) . . ? F29 C29 F28 106.2(3) . . ? F27 C29 C24 112.8(3) . . ? F29 C29 C24 112.0(3) . . ? F28 C29 C24 111.4(3) . . ? F26 C28 F25 108.0(3) . . ? F26 C28 F24 106.5(2) . . ? F25 C28 F24 105.9(3) . . ? F26 C28 C26 112.2(3) . . ? F25 C28 C26 113.1(3) . . ? F24 C28 C26 110.8(3) . . ? C27 F21 Ge 97.78(17) . . ? C28 F25 Ge 94.79(16) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C11 C12 C17 F11 -11.2(5) . . . . ? C21 C22 C27 F21 30.5(4) . . . . ? C11 C16 C18 F15 -65.3(4) . . . . ? C21 C26 C28 F25 -31.4(4) . . . . ? C12 C11 Ge Cl1 -174.4(2) . . . . ? C12 C11 Ge Cl2 -64.2(2) . . . . ? C12 C11 Ge C21 57.8(3) . . . . ? C22 C21 Ge Cl1 -101.8(2) . . . . ? C22 C21 Ge Cl2 145.9(2) . . . . ? C22 C21 Ge C11 32.5(3) . . . . ? _diffrn_measured_fraction_theta_max 0.967 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.967 _refine_diff_density_max 0.660 _refine_diff_density_min -0.535 _refine_diff_density_rms 0.092 #============================================END data_(7b) _database_code_CSD 205555 _audit_creation_method SHELXL-97 _chemical_name_systematic ; (2,4,6-tris-trifluoromethyl-phenyl)-trichloro-germane ; _chemical_name_common (2,4,6-tris-trifluoromethyl-phenyl)-trichloro-germane _chemical_melting_point 'not measured' _chemical_formula_moiety 'C9 H2 Cl3 F9 Ge' _chemical_formula_sum 'C9 H2 Cl3 F9 Ge' _chemical_formula_weight 460.05 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' F F 0.0171 0.0103 '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' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pnma loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z' 'x+1/2, -y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z' '-x-1/2, y-1/2, z-1/2' _cell_length_a 11.284(1) _cell_length_b 12.541(1) _cell_length_c 9.710(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1374.1(5) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 931 _cell_measurement_theta_min 12.0 _cell_measurement_theta_max 29.0 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.28 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 2.224 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 880 _exptl_absorpt_coefficient_mu 2.906 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4371 _exptl_absorpt_correction_T_max 0.4926 _exptl_absorpt_process_details 'SADABS (G.M.Sheldrick, 1998), R(int)=0.038 before correction' _exptl_special_details ; Four sets of \w scans (each scan 0.3\% in \w, exposure time 10 s), each set at different \f and/or 2\q angles, nominally covered ca. 2/3 of full sphere of reciprocal space. The first 50 scans (1187 reflections) were repeated at the end of data collection, revealing no significant crystal decay. Crystal to detector distance 4.51 cm. ; _diffrn_ambient_temperature 120(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 'SMART 1K CCD area detector' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 8 _diffrn_reflns_number 11660 _diffrn_reflns_av_R_equivalents 0.0219 _diffrn_reflns_av_sigmaI/netI 0.0128 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -7 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.65 _diffrn_reflns_theta_max 29.10 _reflns_number_total 1921 _reflns_number_gt 1743 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _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. The C(6)F~3~ group is randomly rotationally disordered, the Fourier map showing a completely uniform toroid of electron density. It was nominally approximated by two orientations related via the mirror plane, with very elongated displacement ellipsoids of fluorine atoms. ; _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^)+(0.0317P)^2^+0.6356P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment refall _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_number_reflns 1921 _refine_ls_number_parameters 125 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0251 _refine_ls_R_factor_gt 0.0217 _refine_ls_wR_factor_ref 0.0555 _refine_ls_wR_factor_gt 0.0543 _refine_ls_goodness_of_fit_ref 1.064 _refine_ls_restrained_S_all 1.068 _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 Ge Ge 0.131680(19) 0.2500 0.70979(2) 0.01626(7) Uani 1 2 d S . . Cl1 Cl 0.01118(3) 0.12020(3) 0.69237(4) 0.02761(10) Uani 1 1 d . . . Cl2 Cl 0.20288(5) 0.2500 0.91091(5) 0.02515(12) Uani 1 2 d S . . F1 F 0.25713(9) 0.04734(7) 0.70696(9) 0.0226(2) Uani 1 1 d . . . F2 F 0.37061(8) -0.02094(8) 0.55244(12) 0.0296(2) Uani 1 1 d . . . F3 F 0.18436(9) -0.00268(8) 0.51027(10) 0.0274(2) Uani 1 1 d . . . C1 C 0.25742(17) 0.2500 0.5674(2) 0.0153(4) Uani 1 2 d S . . C2 C 0.30300(12) 0.15432(11) 0.51208(15) 0.0165(3) Uani 1 1 d . . . C3 C 0.38075(13) 0.15423(13) 0.39993(16) 0.0205(3) Uani 1 1 d . . . H3 H 0.4077(18) 0.0893(18) 0.367(2) 0.028(5) Uiso 1 1 d . . . C4 C 0.4169(2) 0.2500 0.3425(2) 0.0217(4) Uani 1 2 d S . . C5 C 0.27722(13) 0.04446(12) 0.57032(17) 0.0200(3) Uani 1 1 d . . . C6 C 0.5006(2) 0.2500 0.2210(3) 0.0320(6) Uani 1 2 d SD . . F4 F 0.5254(4) 0.3478(3) 0.1769(4) 0.0710(13) Uani 0.50 1 d PD . . F5 F 0.4583(4) 0.2021(4) 0.1177(3) 0.0992(19) Uani 0.50 1 d PD . . F6 F 0.6018(3) 0.2115(4) 0.2509(4) 0.110(3) Uani 0.50 1 d PD . . 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 Ge 0.01392(11) 0.01858(12) 0.01628(11) 0.000 0.00214(8) 0.000 Cl1 0.01839(18) 0.0299(2) 0.0346(2) -0.00253(16) 0.00417(15) -0.00787(14) Cl2 0.0338(3) 0.0248(2) 0.0169(2) 0.000 -0.0018(2) 0.000 F1 0.0243(5) 0.0216(4) 0.0217(4) 0.0032(3) -0.0007(4) -0.0026(4) F2 0.0264(5) 0.0196(5) 0.0427(6) -0.0001(4) 0.0044(4) 0.0064(4) F3 0.0265(5) 0.0249(5) 0.0308(5) -0.0071(4) -0.0024(4) -0.0082(4) C1 0.0122(9) 0.0186(9) 0.0152(9) 0.000 -0.0015(7) 0.000 C2 0.0144(6) 0.0178(6) 0.0175(6) -0.0012(5) -0.0025(5) -0.0007(5) C3 0.0190(7) 0.0242(7) 0.0181(7) -0.0041(6) -0.0006(6) 0.0027(6) C4 0.0177(10) 0.0314(11) 0.0161(9) 0.000 0.0018(8) 0.000 C5 0.0182(7) 0.0175(6) 0.0242(7) -0.0026(6) -0.0003(6) -0.0002(5) C6 0.0350(13) 0.0400(14) 0.0209(11) 0.000 0.0097(10) 0.000 F4 0.107(3) 0.0436(16) 0.063(2) 0.0065(15) 0.065(2) -0.0050(19) F5 0.106(3) 0.160(5) 0.0311(15) -0.052(2) 0.0339(17) -0.083(3) F6 0.0597(18) 0.211(8) 0.0590(18) 0.070(3) 0.0432(16) 0.086(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 Ge C1 1.981(2) . ? Ge Cl2 2.1117(8) . ? Ge Cl1 2.1277(4) . ? Ge Cl1 2.1277(4) 7_565 ? F3 C5 1.3370(18) . ? F2 C5 1.3466(17) . ? F1 C5 1.3464(19) . ? C1 C2 1.4117(17) 7_565 ? C1 C2 1.4117(17) . ? C2 C3 1.398(2) . ? C2 C5 1.517(2) . ? C3 C4 1.3855(19) . ? C3 H3 0.93(2) . ? C4 C3 1.3855(19) 7_565 ? C4 C6 1.512(3) . ? C6 F5 1.263(4) . ? C6 F6 1.274(4) . ? C6 F4 1.329(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 Ge Cl2 111.89(6) . . ? C1 Ge Cl1 113.72(4) . . ? Cl2 Ge Cl1 108.461(17) . . ? C1 Ge Cl1 113.72(4) . 7_565 ? Cl2 Ge Cl1 108.461(17) . 7_565 ? Cl1 Ge Cl1 99.82(3) . 7_565 ? C2 C1 C2 116.41(18) 7_565 . ? C2 C1 Ge 121.77(9) 7_565 . ? C2 C1 Ge 121.77(9) . . ? C3 C2 C1 121.71(14) . . ? C3 C2 C5 114.18(13) . . ? C1 C2 C5 124.06(13) . . ? C4 C3 C2 119.81(15) . . ? C4 C3 H3 121.8(13) . . ? C2 C3 H3 118.4(13) . . ? C3 C4 C3 120.2(2) 7_565 . ? C3 C4 C6 119.87(10) 7_565 . ? C3 C4 C6 119.87(10) . . ? F1 C5 F3 108.04(12) . . ? F3 C5 F2 106.72(12) . . ? F1 C5 F2 105.97(13) . . ? F3 C5 C2 112.90(13) . . ? F1 C5 C2 112.03(12) . . ? F2 C5 C2 110.80(12) . . ? F5 C6 F6 109.9(3) . . ? F5 C6 F4 105.2(4) . . ? F6 C6 F4 103.6(4) . . ? F5 C6 C4 112.6(3) . . ? F6 C6 C4 112.5(2) . . ? F4 C6 C4 112.52(16) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 29.10 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.428 _refine_diff_density_min -0.552 _refine_diff_density_rms 0.071 #=============================================END data_(4b) _database_code_CSD 205556 _audit_creation_method SHELXL-97 _chemical_name_systematic ; Bis-(2,4-bis-trifluoromethyl-phenyl),dichloro-germane ; _chemical_name_common Bis-(2,4-bis-trifluoromethyl-phenyl),dichloro-germane _chemical_melting_point 'not measured' _chemical_formula_moiety 'C16 H6 Cl2 F12 Ge' _chemical_formula_sum 'C16 H6 Cl2 F12 Ge' _chemical_formula_weight 569.70 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 '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' _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 10.547(2) _cell_length_b 11.661(2) _cell_length_c 16.636(3) _cell_angle_alpha 90.00 _cell_angle_beta 108.21(1) _cell_angle_gamma 90.00 _cell_volume 1943.6(6) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 6507 _cell_measurement_theta_min 5.32 _cell_measurement_theta_max 54.37 _exptl_crystal_description 'rectangular prism' _exptl_crystal_colour colourless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.947 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1104 _exptl_absorpt_coefficient_mu 1.964 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.633 _exptl_absorpt_correction_T_max 0.806 _exptl_absorpt_process_details 'XPREP (Bruker, 1998)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART-CCD' _diffrn_measurement_method /w _diffrn_detector_area_resol_mean 8 _diffrn_reflns_number 14919 _diffrn_reflns_av_R_equivalents 0.0328 _diffrn_reflns_av_sigmaI/netI 0.0363 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.04 _diffrn_reflns_theta_max 30.44 _reflns_number_total 5376 _reflns_number_gt 3900 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'SMART-NT V5.0 (Bruker, 1998)' _computing_cell_refinement 'SMART-NT V5.0 (Bruker, 1998)' _computing_data_reduction 'SAINT-NT V5.0 (Bruker, 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL-NT V5.1 (Bruker, 1998)' _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. ; _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^)+(0.0371P)^2^+1.3230P] 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 refall _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5376 _refine_ls_number_parameters 304 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0615 _refine_ls_R_factor_gt 0.0360 _refine_ls_wR_factor_ref 0.0869 _refine_ls_wR_factor_gt 0.0780 _refine_ls_goodness_of_fit_ref 1.017 _refine_ls_restrained_S_all 1.017 _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 Ge Ge 0.65362(3) 0.52246(2) 0.210027(16) 0.02576(8) Uani 1 1 d . . . Cl1 Cl 0.68713(8) 0.45253(6) 0.09891(5) 0.04288(17) Uani 1 1 d . . . Cl2 Cl 0.85163(6) 0.56801(6) 0.28741(5) 0.04093(16) Uani 1 1 d . . . C1 C 0.5889(2) 0.39922(19) 0.26689(15) 0.0248(5) Uani 1 1 d . . . C2 C 0.4691(2) 0.3386(2) 0.23239(14) 0.0245(5) Uani 1 1 d . . . C3 C 0.4309(2) 0.2535(2) 0.27821(15) 0.0266(5) Uani 1 1 d . . . H3 H 0.350(3) 0.213(2) 0.2509(17) 0.024(6) Uiso 1 1 d . . . C4 C 0.5120(2) 0.2269(2) 0.35973(15) 0.0276(5) Uani 1 1 d . . . C5 C 0.6298(3) 0.2846(2) 0.39473(17) 0.0342(6) Uani 1 1 d . . . H5 H 0.683(3) 0.267(3) 0.448(2) 0.046(9) Uiso 1 1 d . . . C6 C 0.6684(3) 0.3702(2) 0.34878(17) 0.0322(6) Uani 1 1 d . . . H6 H 0.742(3) 0.403(2) 0.3701(18) 0.033(8) Uiso 1 1 d . . . C7 C 0.3786(3) 0.3582(2) 0.14354(16) 0.0325(6) Uani 1 1 d . . . C8 C 0.4674(3) 0.1327(2) 0.40692(17) 0.0358(6) Uani 1 1 d . . . F1 F 0.38709(18) 0.46311(13) 0.11460(10) 0.0450(4) Uani 1 1 d . . . F2 F 0.4068(2) 0.28601(15) 0.08812(10) 0.0515(5) Uani 1 1 d . . . F3 F 0.25079(16) 0.33863(19) 0.13613(11) 0.0581(5) Uani 1 1 d . . . F4 F 0.4359(3) 0.03807(15) 0.36171(12) 0.0721(7) Uani 1 1 d . . . F5 F 0.3611(2) 0.1624(2) 0.42803(17) 0.0801(7) Uani 1 1 d . . . F6 F 0.5608(2) 0.10431(18) 0.47843(12) 0.0702(7) Uani 1 1 d . . . C11 C 0.5487(2) 0.66304(19) 0.17680(14) 0.0244(5) Uani 1 1 d . . . C12 C 0.4990(2) 0.7297(2) 0.23020(15) 0.0257(5) Uani 1 1 d . . . C13 C 0.4236(3) 0.8277(2) 0.20032(16) 0.0298(5) Uani 1 1 d . . . H13 H 0.395(3) 0.871(2) 0.2385(19) 0.036(8) Uiso 1 1 d . . . C14 C 0.3960(2) 0.8594(2) 0.11615(16) 0.0300(5) Uani 1 1 d . . . C15 C 0.4441(3) 0.7950(2) 0.06182(16) 0.0329(5) Uani 1 1 d . . . H15 H 0.426(3) 0.818(2) 0.005(2) 0.040(8) Uiso 1 1 d . . . C16 C 0.5199(3) 0.6975(2) 0.09250(16) 0.0294(5) Uani 1 1 d . . . H16 H 0.551(3) 0.655(2) 0.0565(17) 0.028(7) Uiso 1 1 d . . . C17 C 0.5182(3) 0.6961(2) 0.32077(16) 0.0344(6) Uani 1 1 d . . . C18 C 0.3123(3) 0.9645(2) 0.08281(19) 0.0426(7) Uani 1 1 d . . . F11 F 0.63148(19) 0.63980(16) 0.35604(10) 0.0515(5) Uani 1 1 d . . . F12 F 0.5152(2) 0.78381(16) 0.37005(11) 0.0566(5) Uani 1 1 d . . . F13 F 0.4205(2) 0.6240(2) 0.32506(13) 0.0690(6) Uani 1 1 d . . . F14 F 0.3118(2) 1.03786(15) 0.14386(12) 0.0556(5) Uani 1 1 d . . . F15 F 0.1869(2) 0.93757(18) 0.04176(16) 0.0794(8) Uani 1 1 d . . . F16 F 0.3591(3) 1.02391(17) 0.02921(14) 0.0736(7) 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 Ge 0.02612(13) 0.02321(12) 0.02841(13) 0.00284(11) 0.00917(9) 0.00135(10) Cl1 0.0542(4) 0.0400(4) 0.0425(4) -0.0005(3) 0.0268(3) 0.0091(3) Cl2 0.0254(3) 0.0410(4) 0.0520(4) 0.0081(3) 0.0058(3) -0.0037(3) C1 0.0265(11) 0.0215(11) 0.0246(11) 0.0022(9) 0.0057(9) 0.0013(9) C2 0.0267(11) 0.0233(11) 0.0220(11) -0.0002(9) 0.0056(9) 0.0027(9) C3 0.0277(12) 0.0248(12) 0.0265(12) -0.0009(9) 0.0074(10) 0.0008(9) C4 0.0322(13) 0.0234(11) 0.0264(12) 0.0005(9) 0.0081(10) 0.0007(9) C5 0.0414(14) 0.0308(13) 0.0246(12) 0.0044(10) 0.0019(10) -0.0026(11) C6 0.0307(13) 0.0291(13) 0.0302(13) 0.0014(10) 0.0001(10) -0.0046(10) C7 0.0304(13) 0.0333(13) 0.0297(13) 0.0053(10) 0.0036(10) -0.0035(10) C8 0.0451(16) 0.0317(13) 0.0315(13) 0.0034(11) 0.0135(12) -0.0027(11) F1 0.0514(10) 0.0352(9) 0.0351(8) 0.0126(7) -0.0056(7) -0.0062(7) F2 0.0737(13) 0.0458(10) 0.0270(8) -0.0063(7) 0.0044(8) 0.0006(9) F3 0.0289(9) 0.0867(14) 0.0485(10) 0.0248(10) -0.0026(7) -0.0081(9) F4 0.137(2) 0.0370(10) 0.0458(11) -0.0052(8) 0.0335(12) -0.0370(12) F5 0.0861(16) 0.0674(14) 0.1144(19) 0.0377(13) 0.0714(15) 0.0144(12) F6 0.0738(14) 0.0720(14) 0.0477(11) 0.0329(10) -0.0056(10) -0.0244(11) C11 0.0242(11) 0.0227(10) 0.0256(11) 0.0008(9) 0.0069(9) -0.0012(9) C12 0.0256(11) 0.0244(11) 0.0263(11) 0.0001(9) 0.0071(9) -0.0021(9) C13 0.0325(13) 0.0256(12) 0.0305(13) -0.0036(10) 0.0088(10) 0.0010(10) C14 0.0297(12) 0.0223(11) 0.0337(13) -0.0007(10) 0.0035(10) -0.0007(9) C15 0.0404(14) 0.0279(13) 0.0270(13) 0.0028(10) 0.0058(10) -0.0008(11) C16 0.0355(13) 0.0267(12) 0.0268(12) -0.0002(10) 0.0107(10) 0.0011(10) C17 0.0404(14) 0.0362(14) 0.0295(13) 0.0021(11) 0.0152(11) 0.0042(12) C18 0.0454(16) 0.0343(15) 0.0398(15) -0.0016(12) 0.0015(12) 0.0090(12) F11 0.0618(11) 0.0627(12) 0.0296(8) 0.0098(8) 0.0134(8) 0.0270(9) F12 0.0883(15) 0.0503(11) 0.0325(9) -0.0025(8) 0.0210(9) 0.0201(10) F13 0.0712(14) 0.0857(15) 0.0547(12) 0.0181(11) 0.0262(11) -0.0260(12) F14 0.0663(12) 0.0390(10) 0.0525(11) -0.0062(8) 0.0055(9) 0.0223(9) F15 0.0487(12) 0.0523(12) 0.1019(17) -0.0099(12) -0.0274(11) 0.0156(9) F16 0.1088(19) 0.0489(11) 0.0682(13) 0.0323(10) 0.0352(13) 0.0336(12) _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 Ge C1 1.957(2) . ? Ge C11 1.958(2) . ? Ge Cl1 2.1484(8) . ? Ge Cl2 2.1496(8) . ? Ge F1 2.8482(18) . ? Ge F11 2.8604(18) . ? C1 C6 1.400(3) . ? C1 C2 1.404(3) . ? C2 C3 1.386(3) . ? C2 C7 1.505(3) . ? C3 C4 1.394(3) . ? C3 H3 0.95(3) . ? C4 C5 1.372(4) . ? C4 C8 1.509(4) . ? C5 C6 1.394(4) . ? C5 H5 0.91(3) . ? C6 H6 0.84(3) . ? C7 F1 1.327(3) . ? C7 F3 1.335(3) . ? C7 F2 1.349(3) . ? C8 F4 1.318(3) . ? C8 F5 1.321(3) . ? C8 F6 1.327(3) . ? C11 C16 1.398(3) . ? C11 C12 1.399(3) . ? C12 C13 1.392(3) . ? C12 C17 1.508(3) . ? C13 C14 1.388(4) . ? C13 H13 0.93(3) . ? C14 C15 1.387(4) . ? C14 C18 1.511(4) . ? C15 C16 1.392(4) . ? C15 H15 0.94(3) . ? C16 H16 0.92(3) . ? C17 F12 1.318(3) . ? C17 F11 1.328(3) . ? C17 F13 1.349(3) . ? C18 F15 1.323(4) . ? C18 F14 1.329(3) . ? C18 F16 1.339(4) . ? 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 Ge C11 119.95(10) . . ? C1 Ge Cl1 108.26(7) . . ? C11 Ge Cl1 107.77(7) . . ? C1 Ge Cl2 108.21(7) . . ? C11 Ge Cl2 108.65(7) . . ? Cl1 Ge Cl2 102.64(3) . . ? C1 Ge F1 70.02(7) . . ? C11 Ge F1 70.96(8) . . ? Cl1 Ge F1 80.06(5) . . ? Cl2 Ge F1 177.20(4) . . ? C1 Ge F11 78.89(8) . . ? C11 Ge F11 69.54(8) . . ? Cl1 Ge F11 172.45(5) . . ? Cl2 Ge F11 72.24(5) . . ? F1 Ge F11 105.15(6) . . ? C6 C1 C2 117.7(2) . . ? C6 C1 Ge 117.02(18) . . ? C2 C1 Ge 125.25(17) . . ? C3 C2 C1 121.0(2) . . ? C3 C2 C7 116.4(2) . . ? C1 C2 C7 122.6(2) . . ? C2 C3 C4 119.9(2) . . ? C2 C3 H3 117.6(16) . . ? C4 C3 H3 122.5(16) . . ? C5 C4 C3 120.2(2) . . ? C5 C4 C8 121.6(2) . . ? C3 C4 C8 118.2(2) . . ? C4 C5 C6 120.0(2) . . ? C4 C5 H5 120(2) . . ? C6 C5 H5 120(2) . . ? C5 C6 C1 121.2(2) . . ? C5 C6 H6 119(2) . . ? C1 C6 H6 120(2) . . ? F1 C7 F3 107.7(2) . . ? F1 C7 F2 105.9(2) . . ? F3 C7 F2 105.2(2) . . ? F1 C7 C2 113.7(2) . . ? F3 C7 C2 112.1(2) . . ? F2 C7 C2 111.7(2) . . ? F4 C8 F5 106.7(3) . . ? F4 C8 F6 106.7(2) . . ? F5 C8 F6 106.3(2) . . ? F4 C8 C4 112.1(2) . . ? F5 C8 C4 112.0(2) . . ? F6 C8 C4 112.5(2) . . ? C7 F1 Ge 100.85(14) . . ? C16 C11 C12 118.0(2) . . ? C16 C11 Ge 116.75(17) . . ? C12 C11 Ge 125.19(17) . . ? C13 C12 C11 121.0(2) . . ? C13 C12 C17 117.0(2) . . ? C11 C12 C17 122.0(2) . . ? C14 C13 C12 119.7(2) . . ? C14 C13 H13 122.0(18) . . ? C12 C13 H13 118.3(18) . . ? C15 C14 C13 120.6(2) . . ? C15 C14 C18 119.4(2) . . ? C13 C14 C18 120.0(2) . . ? C14 C15 C16 119.2(2) . . ? C14 C15 H15 120.0(18) . . ? C16 C15 H15 120.8(18) . . ? C15 C16 C11 121.5(2) . . ? C15 C16 H16 119.1(17) . . ? C11 C16 H16 119.5(17) . . ? F12 C17 F11 107.6(2) . . ? F12 C17 F13 106.5(2) . . ? F11 C17 F13 105.4(2) . . ? F12 C17 C12 113.4(2) . . ? F11 C17 C12 113.0(2) . . ? F13 C17 C12 110.4(2) . . ? F15 C18 F14 107.8(3) . . ? F15 C18 F16 107.2(3) . . ? F14 C18 F16 105.4(2) . . ? F15 C18 C14 111.8(2) . . ? F14 C18 C14 112.5(2) . . ? F16 C18 C14 111.7(3) . . ? C17 F11 Ge 99.32(14) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C11 Ge C1 C6 -118.1(2) . . . . ? Cl1 Ge C1 C6 117.75(19) . . . . ? Cl2 Ge C1 C6 7.2(2) . . . . ? F1 Ge C1 C6 -170.5(2) . . . . ? F11 Ge C1 C6 -59.75(19) . . . . ? C11 Ge C1 C2 61.3(2) . . . . ? Cl1 Ge C1 C2 -62.8(2) . . . . ? Cl2 Ge C1 C2 -173.36(19) . . . . ? F1 Ge C1 C2 8.93(19) . . . . ? F11 Ge C1 C2 119.7(2) . . . . ? C6 C1 C2 C7 -177.0(2) . . . . ? Ge C1 C2 C7 3.5(3) . . . . ? C7 C2 C3 C4 177.4(2) . . . . ? C2 C3 C4 C8 -179.3(2) . . . . ? C8 C4 C5 C6 179.3(3) . . . . ? C3 C2 C7 F1 155.3(2) . . . . ? C1 C2 C7 F1 -27.3(4) . . . . ? C3 C2 C7 F3 32.7(3) . . . . ? C1 C2 C7 F3 -149.9(2) . . . . ? C3 C2 C7 F2 -85.0(3) . . . . ? C1 C2 C7 F2 92.4(3) . . . . ? C5 C4 C8 F4 -128.2(3) . . . . ? C3 C4 C8 F4 50.8(3) . . . . ? C5 C4 C8 F5 111.8(3) . . . . ? C3 C4 C8 F5 -69.2(3) . . . . ? C5 C4 C8 F6 -8.0(4) . . . . ? C3 C4 C8 F6 171.1(2) . . . . ? F3 C7 F1 Ge 152.31(17) . . . . ? F2 C7 F1 Ge -95.55(17) . . . . ? C2 C7 F1 Ge 27.4(2) . . . . ? C1 Ge F1 C7 -21.19(16) . . . . ? C11 Ge F1 C7 -154.62(18) . . . . ? Cl1 Ge F1 C7 92.53(15) . . . . ? Cl2 Ge F1 C7 -72.1(8) . . . . ? F11 Ge F1 C7 -93.08(16) . . . . ? C1 Ge C11 C16 -127.58(19) . . . . ? Cl1 Ge C11 C16 -3.2(2) . . . . ? Cl2 Ge C11 C16 107.32(18) . . . . ? F1 Ge C11 C16 -75.61(18) . . . . ? F11 Ge C11 C16 169.3(2) . . . . ? C1 Ge C11 C12 51.3(2) . . . . ? Cl1 Ge C11 C12 175.62(18) . . . . ? Cl2 Ge C11 C12 -73.9(2) . . . . ? F1 Ge C11 C12 103.2(2) . . . . ? F11 Ge C11 C12 -11.85(19) . . . . ? C16 C11 C12 C17 176.5(2) . . . . ? Ge C11 C12 C17 -2.3(3) . . . . ? C17 C12 C13 C14 -176.4(2) . . . . ? C13 C12 C17 F12 -28.7(3) . . . . ? C11 C12 C17 F12 154.4(2) . . . . ? C13 C12 C17 F11 -151.5(2) . . . . ? C11 C12 C17 F11 31.6(3) . . . . ? C13 C12 C17 F13 90.8(3) . . . . ? C11 C12 C17 F13 -86.1(3) . . . . ? C15 C14 C18 F15 80.2(3) . . . . ? C13 C14 C18 F15 -99.4(3) . . . . ? C15 C14 C18 F14 -158.3(3) . . . . ? C13 C14 C18 F14 22.0(4) . . . . ? C15 C14 C18 F16 -39.9(4) . . . . ? C13 C14 C18 F16 140.4(3) . . . . ? F12 C17 F11 Ge -158.47(17) . . . . ? F13 C17 F11 Ge 88.21(18) . . . . ? C12 C17 F11 Ge -32.4(2) . . . . ? C1 Ge F11 C17 -102.28(17) . . . . ? C11 Ge F11 C17 25.77(16) . . . . ? Cl1 Ge F11 C17 96.2(3) . . . . ? Cl2 Ge F11 C17 144.32(16) . . . . ? F1 Ge F11 C17 -36.73(16) . . . . ? _diffrn_measured_fraction_theta_max 0.914 _diffrn_reflns_theta_full 29.00 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.585 _refine_diff_density_min -0.322 _refine_diff_density_rms 0.074 #============================================END data_(1c) _database_code_CSD 205557 _audit_creation_method SHELXL-97 _chemical_name_systematic ; Bis-(2,4,6-tris-trifluoromethyl-phenyl)-dichloro-stannane ; _chemical_name_common Bis-(2,4,6-tris-trifluoromethyl-phenyl)-dichloro-stannane _chemical_melting_point 'not measured' _chemical_formula_moiety 'C18 H4 Cl2 F18 Sn' _chemical_formula_sum 'C18 H4 Cl2 F18 Sn' _chemical_formula_weight 751.80 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' F F 0.0171 0.0103 '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' _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 8.465(1) _cell_length_b 30.409(4) _cell_length_c 8.724(1) _cell_angle_alpha 90.00 _cell_angle_beta 96.635(2) _cell_angle_gamma 90.00 _cell_volume 2230.6(5) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 4663 _cell_measurement_theta_min 3.09 _cell_measurement_theta_max 26.56 _exptl_crystal_description 'thin plate' _exptl_crystal_colour colourless _exptl_crystal_size_max 0.46 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 2.239 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1432 _exptl_absorpt_coefficient_mu 1.543 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.630 _exptl_absorpt_correction_T_max 0.862 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996 & Blessing, 1995)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART 1K CCD' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 8 _diffrn_reflns_number 11861 _diffrn_reflns_av_R_equivalents 0.0518 _diffrn_reflns_av_sigmaI/netI 0.0592 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -38 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 3.09 _diffrn_reflns_theta_max 26.56 _reflns_number_total 4298 _reflns_number_gt 3130 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'SMART-NT V5.0 (Bruker, 1998)' _computing_cell_refinement 'SMART-NT V5.0 (Bruker, 1998)' _computing_data_reduction 'SAINT-NT V5.0 (Bruker, 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL V5.1 (Bruker, 1998)' _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. ; _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^)+(0.0541P)^2^+8.9971P] 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 4298 _refine_ls_number_parameters 345 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0833 _refine_ls_R_factor_gt 0.0517 _refine_ls_wR_factor_ref 0.1173 _refine_ls_wR_factor_gt 0.1063 _refine_ls_goodness_of_fit_ref 1.043 _refine_ls_restrained_S_all 1.043 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Sn Sn 0.74176(5) 0.617801(13) 0.54372(5) 0.02066(14) Uani 1 1 d . . . Cl1 Cl 0.9903(2) 0.62575(5) 0.67749(19) 0.0322(4) Uani 1 1 d . . . Cl2 Cl 0.5862(2) 0.59971(6) 0.7375(2) 0.0369(4) Uani 1 1 d . . . C11 C 0.6072(7) 0.67685(19) 0.4644(7) 0.0205(13) Uani 1 1 d . . . C12 C 0.4497(7) 0.67259(19) 0.3940(7) 0.0217(13) Uani 1 1 d . . . C13 C 0.3545(8) 0.70878(19) 0.3550(7) 0.0247(14) Uani 1 1 d . . . H13 H 0.2516 0.7046 0.3072 0.030 Uiso 1 1 d R . . C14 C 0.4090(8) 0.7509(2) 0.3860(7) 0.0269(14) Uani 1 1 d . A . C15 C 0.5648(8) 0.7564(2) 0.4532(7) 0.0265(14) Uani 1 1 d . . . H15 H 0.6049 0.7846 0.4726 0.032 Uiso 1 1 d R . . C16 C 0.6608(7) 0.7202(2) 0.4907(7) 0.0232(14) Uani 1 1 d . . . C17 C 0.3671(8) 0.6293(2) 0.3584(8) 0.0298(16) Uani 1 1 d . . . F11 F 0.4629(4) 0.59472(12) 0.3763(5) 0.0379(10) Uani 1 1 d . . . F12 F 0.2956(7) 0.62779(15) 0.2165(6) 0.0671(16) Uani 1 1 d . . . F13 F 0.2556(6) 0.62253(14) 0.4500(7) 0.0644(15) Uani 1 1 d . . . C18 C 0.8236(9) 0.7301(2) 0.5704(8) 0.0333(16) Uani 1 1 d . . . F14 F 0.9387(4) 0.71128(12) 0.4973(5) 0.0357(9) Uani 1 1 d . . . F15 F 0.8405(5) 0.71518(14) 0.7162(5) 0.0423(10) Uani 1 1 d . . . F16 F 0.8566(5) 0.77324(13) 0.5776(6) 0.0556(13) Uani 1 1 d . . . C19 C 0.3034(4) 0.78927(11) 0.3465(5) 0.0346(17) Uani 1 1 d . . . F17 F 0.3109(4) 0.80359(11) 0.2031(5) 0.072(3) Uani 0.583(8) 1 d PR A 1 F18 F 0.1510(4) 0.78041(11) 0.3583(5) 0.089(4) Uani 0.583(8) 1 d PR A 1 F19 F 0.3438(4) 0.82298(11) 0.4406(5) 0.068(3) Uani 0.583(8) 1 d PR A 1 F18A F 0.3777(4) 0.82799(11) 0.3522(5) 0.089(4) Uani 0.42 1 d PR A 2 F19A F 0.2266(4) 0.78540(11) 0.2049(5) 0.068(3) Uani 0.42 1 d PR A 2 F17A F 0.1929(4) 0.79172(11) 0.4434(5) 0.072(3) Uani 0.42 1 d PR A 2 C21 C 0.7712(7) 0.56409(19) 0.3835(7) 0.0198(13) Uani 1 1 d . . . C22 C 0.7823(7) 0.57305(19) 0.2274(6) 0.0192(13) Uani 1 1 d . . . C23 C 0.7763(7) 0.54052(19) 0.1169(7) 0.0231(14) Uani 1 1 d . . . H23 H 0.7833 0.5477 0.0143 0.028 Uiso 1 1 d R . . C24 C 0.7601(7) 0.49712(19) 0.1598(7) 0.0197(13) Uani 1 1 d . . . C25 C 0.7591(7) 0.4864(2) 0.3150(7) 0.0235(14) Uani 1 1 d . . . H25 H 0.7541 0.4572 0.3454 0.028 Uiso 1 1 d R . . C26 C 0.7660(7) 0.51987(19) 0.4237(6) 0.0196(13) Uani 1 1 d . . . C27 C 0.8034(8) 0.6194(2) 0.1721(7) 0.0281(14) Uani 1 1 d . . . F21 F 0.8808(5) 0.64492(12) 0.2836(4) 0.0336(9) Uani 1 1 d . . . F22 F 0.6620(5) 0.63981(12) 0.1313(4) 0.0370(10) Uani 1 1 d . . . F23 F 0.8834(5) 0.62174(12) 0.0503(4) 0.0397(10) Uani 1 1 d . . . C28 C 0.7666(8) 0.5041(2) 0.5894(7) 0.0243(14) Uani 1 1 d . . . F24 F 0.8405(5) 0.46573(12) 0.6106(4) 0.0349(9) Uani 1 1 d . . . F25 F 0.8456(4) 0.53249(11) 0.6900(4) 0.0281(8) Uani 1 1 d . . . F26 F 0.6218(5) 0.49984(13) 0.6305(4) 0.0338(9) Uani 1 1 d . . . C29 C 0.7490(9) 0.4616(2) 0.0377(7) 0.0277(14) Uani 1 1 d . . . F27 F 0.7364(6) 0.42176(12) 0.0963(4) 0.0433(11) Uani 1 1 d . . . F28 F 0.6191(6) 0.46758(14) -0.0628(5) 0.0533(13) Uani 1 1 d . . . F29 F 0.8707(6) 0.46172(15) -0.0424(6) 0.0587(14) 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 Sn 0.0237(2) 0.0201(2) 0.0179(2) -0.00127(19) 0.00104(15) 0.0012(2) Cl1 0.0288(9) 0.0302(9) 0.0349(9) -0.0006(7) -0.0081(7) -0.0006(7) Cl2 0.0398(10) 0.0409(10) 0.0328(9) 0.0055(7) 0.0162(8) 0.0061(8) C11 0.023(3) 0.019(3) 0.020(3) -0.004(2) 0.004(3) 0.000(3) C12 0.021(3) 0.019(3) 0.024(3) -0.002(2) -0.001(3) -0.003(3) C13 0.026(3) 0.021(3) 0.027(3) 0.004(3) 0.001(3) 0.000(3) C14 0.032(4) 0.022(3) 0.027(3) 0.003(3) 0.004(3) 0.005(3) C15 0.029(4) 0.020(3) 0.030(3) -0.001(3) 0.002(3) -0.006(3) C16 0.017(3) 0.024(3) 0.030(3) -0.003(3) 0.007(3) 0.002(3) C17 0.026(4) 0.028(4) 0.035(4) -0.006(3) 0.001(3) 0.004(3) F11 0.028(2) 0.022(2) 0.060(3) -0.0079(18) -0.0069(19) 0.0029(17) F12 0.086(4) 0.043(3) 0.062(3) -0.006(2) -0.039(3) -0.012(3) F13 0.049(3) 0.039(3) 0.113(4) -0.024(3) 0.039(3) -0.017(2) C18 0.036(4) 0.020(3) 0.043(4) -0.006(3) 0.000(3) -0.001(3) F14 0.027(2) 0.035(2) 0.043(2) -0.0012(18) -0.0006(18) -0.0039(18) F15 0.038(2) 0.055(3) 0.031(2) -0.0130(19) -0.0088(18) 0.003(2) F16 0.041(3) 0.026(2) 0.094(4) -0.015(2) -0.020(2) -0.006(2) C19 0.041(4) 0.033(4) 0.029(4) -0.002(3) -0.001(3) 0.005(3) F17 0.092(6) 0.067(5) 0.060(5) 0.029(4) 0.024(4) 0.043(5) F18 0.020(4) 0.034(4) 0.211(11) 0.056(5) 0.007(5) 0.005(3) F19 0.088(6) 0.043(4) 0.068(5) -0.010(4) -0.016(4) 0.030(4) F18A 0.020(4) 0.034(4) 0.211(11) 0.056(5) 0.007(5) 0.005(3) F19A 0.088(6) 0.043(4) 0.068(5) -0.010(4) -0.016(4) 0.030(4) F17A 0.092(6) 0.067(5) 0.060(5) 0.029(4) 0.024(4) 0.043(5) C21 0.018(3) 0.021(3) 0.019(3) -0.001(2) 0.000(2) 0.001(3) C22 0.021(3) 0.021(3) 0.015(3) 0.001(2) 0.002(2) 0.004(3) C23 0.028(4) 0.022(3) 0.020(3) 0.002(3) 0.004(3) -0.001(3) C24 0.016(3) 0.022(3) 0.021(3) -0.002(2) 0.002(2) 0.001(2) C25 0.029(4) 0.023(3) 0.018(3) 0.000(2) 0.001(3) 0.003(3) C26 0.018(3) 0.023(3) 0.018(3) -0.002(2) 0.004(2) -0.001(3) C27 0.039(4) 0.025(3) 0.021(3) -0.002(3) 0.004(3) -0.004(3) F21 0.051(3) 0.024(2) 0.0259(19) 0.0033(16) 0.0070(18) -0.0055(18) F22 0.050(3) 0.0222(19) 0.038(2) 0.0101(17) 0.0002(19) 0.0091(18) F23 0.065(3) 0.025(2) 0.033(2) 0.0045(17) 0.023(2) -0.005(2) C28 0.029(4) 0.025(3) 0.019(3) 0.004(3) 0.001(3) -0.005(3) F24 0.056(3) 0.0235(19) 0.0234(19) 0.0064(15) -0.0033(18) 0.0087(18) F25 0.042(2) 0.0248(18) 0.0156(17) 0.0024(15) -0.0036(16) -0.0031(17) F26 0.033(2) 0.047(2) 0.0213(19) 0.0059(17) 0.0056(16) -0.0092(19) C29 0.033(4) 0.028(3) 0.022(3) 0.000(3) 0.002(3) 0.000(3) F27 0.080(3) 0.023(2) 0.026(2) -0.0034(16) 0.002(2) -0.005(2) F28 0.071(3) 0.046(3) 0.036(2) -0.017(2) -0.025(2) 0.020(2) F29 0.063(3) 0.058(3) 0.064(3) -0.033(2) 0.040(3) -0.018(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 Sn C21 2.183(6) . ? Sn C11 2.195(6) . ? Sn Cl1 2.2977(16) . ? Sn Cl2 2.3262(17) . ? Sn F11 2.720(4) . ? Sn F21 2.799(4) . ? Sn F25 2.979(3) . ? Sn F14 3.344(4) . ? Sn F15 3.382(4) . ? C11 C16 1.405(8) . ? C11 C12 1.408(8) . ? C12 C13 1.383(8) . ? C12 C17 1.507(9) . ? C13 C14 1.377(9) . ? C14 C15 1.390(9) . ? C14 C19 1.486(7) . ? C15 C16 1.385(9) . ? C16 C18 1.501(9) . ? C17 F12 1.314(8) . ? C17 F13 1.321(8) . ? C17 F11 1.325(7) . ? C18 F16 1.341(8) . ? C18 F15 1.342(8) . ? C18 F14 1.351(8) . ? C19 F19 1.3330 . ? C19 F17 1.3330 . ? C19 F19A 1.3331 . ? C19 F17A 1.3331 . ? C19 F18A 1.3331 . ? C19 F18 1.3332 . ? C21 C26 1.392(8) . ? C21 C22 1.403(8) . ? C22 C23 1.378(8) . ? C22 C27 1.507(8) . ? C23 C24 1.383(8) . ? C24 C25 1.394(8) . ? C24 C29 1.513(8) . ? C25 C26 1.387(8) . ? C26 C28 1.522(8) . ? C27 F23 1.326(7) . ? C27 F21 1.353(7) . ? C27 F22 1.359(8) . ? C28 F26 1.323(7) . ? C28 F24 1.328(7) . ? C28 F25 1.351(7) . ? C29 F29 1.310(8) . ? C29 F27 1.323(7) . ? C29 F28 1.337(8) . ? 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 C21 Sn C11 120.3(2) . . ? C21 Sn Cl1 103.78(16) . . ? C11 Sn Cl1 119.04(16) . . ? C21 Sn Cl2 113.87(16) . . ? C11 Sn Cl2 96.08(16) . . ? Cl1 Sn Cl2 102.58(7) . . ? C21 Sn F11 67.64(17) . . ? C11 Sn F11 69.84(17) . . ? Cl1 Sn F11 170.61(9) . . ? Cl2 Sn F11 78.47(11) . . ? C21 Sn F21 67.14(17) . . ? C11 Sn F21 75.81(18) . . ? Cl1 Sn F21 86.25(9) . . ? Cl2 Sn F21 170.26(10) . . ? F11 Sn F21 93.49(12) . . ? C21 Sn F25 64.70(16) . . ? C11 Sn F25 164.63(18) . . ? Cl1 Sn F25 70.51(8) . . ? Cl2 Sn F25 69.29(8) . . ? F11 Sn F25 101.55(10) . . ? F21 Sn F25 118.24(11) . . ? C21 Sn F14 117.59(17) . . ? C11 Sn F14 60.93(17) . . ? Cl1 Sn F14 62.10(8) . . ? Cl2 Sn F14 128.41(8) . . ? F11 Sn F14 124.62(11) . . ? F21 Sn F14 52.34(10) . . ? F25 Sn F14 131.73(10) . . ? C21 Sn F15 154.07(18) . . ? C11 Sn F15 61.09(16) . . ? Cl1 Sn F15 61.14(8) . . ? Cl2 Sn F15 90.88(9) . . ? F11 Sn F15 128.25(10) . . ? F21 Sn F15 89.84(11) . . ? F25 Sn F15 121.76(9) . . ? F14 Sn F15 37.68(10) . . ? C16 C11 C12 115.4(5) . . ? C16 C11 Sn 124.8(4) . . ? C12 C11 Sn 119.5(4) . . ? C13 C12 C11 122.0(5) . . ? C13 C12 C17 113.7(5) . . ? C11 C12 C17 124.3(5) . . ? C14 C13 C12 121.3(6) . . ? C13 C14 C15 118.3(6) . . ? C13 C14 C19 120.4(6) . . ? C15 C14 C19 121.3(5) . . ? C16 C15 C14 120.4(6) . . ? C15 C16 C11 122.5(6) . . ? C15 C16 C18 115.7(5) . . ? C11 C16 C18 121.7(6) . . ? F12 C17 F13 106.3(6) . . ? F12 C17 F11 107.0(5) . . ? F13 C17 F11 106.0(6) . . ? F12 C17 C12 112.1(6) . . ? F13 C17 C12 111.0(5) . . ? F11 C17 C12 114.0(5) . . ? C17 F11 Sn 109.9(3) . . ? F16 C18 F15 106.7(6) . . ? F16 C18 F14 106.2(6) . . ? F15 C18 F14 107.5(5) . . ? F16 C18 C16 113.1(6) . . ? F15 C18 C16 111.3(6) . . ? F14 C18 C16 111.7(5) . . ? C18 F14 Sn 84.6(3) . . ? C18 F15 Sn 83.1(3) . . ? F19 C19 F17 106.9 . . ? F19 C19 F19A 134.6 . . ? F17 C19 F19A 39.7 . . ? F19 C19 F17A 73.5 . . ? F17 C19 F17A 133.6 . . ? F19A C19 F17A 106.8 . . ? F19 C19 F18A 37.9 . . ? F17 C19 F18A 70.9 . . ? F19A C19 F18A 106.9 . . ? F17A C19 F18A 106.8 . . ? F19 C19 F18 106.8 . . ? F17 C19 F18 106.9 . . ? F19A C19 F18 71.4 . . ? F17A C19 F18 37.5 . . ? F18A C19 F18 129.2 . . ? F19 C19 C14 110.9(3) . . ? F17 C19 C14 112.4(3) . . ? F19A C19 C14 111.2(3) . . ? F17A C19 C14 110.1(3) . . ? F18A C19 C14 114.6(3) . . ? F18 C19 C14 112.6(3) . . ? C26 C21 C22 116.1(5) . . ? C26 C21 Sn 123.5(4) . . ? C22 C21 Sn 120.1(4) . . ? C23 C22 C21 122.6(5) . . ? C23 C22 C27 116.3(5) . . ? C21 C22 C27 121.1(5) . . ? C22 C23 C24 119.5(6) . . ? C23 C24 C25 119.9(5) . . ? C23 C24 C29 119.4(5) . . ? C25 C24 C29 120.7(5) . . ? C26 C25 C24 119.3(6) . . ? C25 C26 C21 122.4(5) . . ? C25 C26 C28 114.5(5) . . ? C21 C26 C28 123.1(5) . . ? F23 C27 F21 107.2(5) . . ? F23 C27 F22 106.3(5) . . ? F21 C27 F22 105.3(5) . . ? F23 C27 C22 113.4(5) . . ? F21 C27 C22 111.8(5) . . ? F22 C27 C22 112.2(5) . . ? C27 F21 Sn 101.5(3) . . ? F26 C28 F24 108.2(5) . . ? F26 C28 F25 107.0(5) . . ? F24 C28 F25 106.3(5) . . ? F26 C28 C26 112.8(5) . . ? F24 C28 C26 111.0(5) . . ? F25 C28 C26 111.3(5) . . ? C28 F25 Sn 100.2(3) . . ? F29 C29 F27 108.2(6) . . ? F29 C29 F28 106.7(6) . . ? F27 C29 F28 106.4(5) . . ? F29 C29 C24 112.6(5) . . ? F27 C29 C24 112.5(5) . . ? F28 C29 C24 110.1(5) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C11 C12 C17 F11 -10.2(9) . . . . ? C21 C22 C27 F21 28.6(8) . . . . ? C11 C16 C18 F15 -63.3(8) . . . . ? C21 C26 C28 F25 -29.5(8) . . . . ? C12 C11 Sn Cl1 -174.6(4) . . . . ? C12 C11 Sn Cl2 -66.6(5) . . . . ? C12 C11 Sn C21 55.7(5) . . . . ? C22 C21 Sn Cl1 -103.3(5) . . . . ? C22 C21 Sn Cl2 146.0(4) . . . . ? C22 C21 Sn C11 32.9(6) . . . . ? _diffrn_measured_fraction_theta_max 0.923 _diffrn_reflns_theta_full 26.56 _diffrn_measured_fraction_theta_full 0.923 _refine_diff_density_max 1.652 _refine_diff_density_min -0.786 _refine_diff_density_rms 0.134 #=============================================END data_(3c) _database_code_CSD 205558 _audit_creation_method SHELXL-97 _chemical_name_systematic ; Bis-(2,6-bis-trifluoromethyl-phenyl)-dichloro-stannane ; _chemical_name_common Bis-(2,6-bis-trifluoromethyl-phenyl)-dichloro-stannane _chemical_melting_point ? _chemical_formula_moiety 'C16 H6 Cl2 F12 Sn' _chemical_formula_sum 'C16 H6 Cl2 F12 Sn' _chemical_formula_weight 615.80 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' F F 0.0171 0.0103 '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 triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.783(2) _cell_length_b 9.095(2) _cell_length_c 12.162(3) _cell_angle_alpha 81.697(4) _cell_angle_beta 83.970(4) _cell_angle_gamma 82.135(4) _cell_volume 948.7(4) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 507 _cell_measurement_theta_min 13.66 _cell_measurement_theta_max 21.77 _exptl_crystal_description 'irregular shape' _exptl_crystal_colour colourless _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.38 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 2.156 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 588 _exptl_absorpt_coefficient_mu 1.744 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.440 _exptl_absorpt_correction_T_max 0.515 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996 & Blessing, 1995)' _exptl_special_details ; The data collection nominally covered full sphere of reciprocal Space, by a combination of 5 sets of \w scans each set at different \f and/or 2\q angles and each scan (15s exposure) covering 0.3\% in \w. Crystal to detector distance 4.51 cm. ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART 1K CCD' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 8 _diffrn_reflns_number 7949 _diffrn_reflns_av_R_equivalents 0.0149 _diffrn_reflns_av_sigmaI/netI 0.0157 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.70 _diffrn_reflns_theta_max 30.30 _reflns_number_total 5003 _reflns_number_gt 4708 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'SMART-NT V5.0 (Bruker, 1998)' _computing_cell_refinement 'SMART-NT V5.0 (Bruker, 1998)' _computing_data_reduction 'SAINT-NT V5.0 (Bruker, 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL V5.1 (Bruker, 1998)' _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. CF~3~ group at C(14) is rotatinally disordered between 2 positions, viz. F(17), F(18), F(19) and F(17A), F(18A), F(19A), with occupancies refined to 88.2(9)% and 11.8(9)%, respectively. The minor position was refined with soft restrains to 3-fold symmetry. ; _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^)+(0.0437P)^2^+0.7695P] 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 refU _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_number_reflns 5003 _refine_ls_number_parameters 299 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0277 _refine_ls_R_factor_gt 0.0252 _refine_ls_wR_factor_ref 0.0685 _refine_ls_wR_factor_gt 0.0668 _refine_ls_goodness_of_fit_ref 1.036 _refine_ls_restrained_S_all 1.038 _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 Sn Sn 0.277981(14) 0.763541(15) 0.266634(11) 0.01963(5) Uani 1 1 d . . . Cl1 Cl 0.38129(6) 0.69577(7) 0.43786(4) 0.02986(11) Uani 1 1 d . A . Cl2 Cl 0.45894(8) 0.91497(7) 0.17424(6) 0.03804(14) Uani 1 1 d . A . C11 C 0.2960(2) 0.6031(2) 0.14716(17) 0.0206(4) Uani 1 1 d . A . C12 C 0.2186(2) 0.6429(2) 0.04950(18) 0.0236(4) Uani 1 1 d . . . C13 C 0.2191(3) 0.5424(3) -0.02737(19) 0.0304(5) Uani 1 1 d . A . H13 H 0.1654 0.5713 -0.0904 0.040(9) Uiso 1 1 d R . . C14 C 0.2986(3) 0.4010(3) -0.0100(2) 0.0330(5) Uani 1 1 d . . . H14 H 0.2970 0.3338 -0.0603 0.041(9) Uiso 1 1 d R A . C15 C 0.3806(3) 0.3596(3) 0.0829(2) 0.0294(5) Uani 1 1 d . A . H15 H 0.4369 0.2651 0.0935 0.035(8) Uiso 1 1 d R . . C16 C 0.3798(2) 0.4590(2) 0.16057(18) 0.0237(4) Uani 1 1 d . . . C17 C 0.1313(3) 0.7949(3) 0.01681(19) 0.0303(5) Uani 1 1 d D A . C18 C 0.4743(3) 0.4068(3) 0.2576(2) 0.0313(5) Uani 1 1 d . A . F11 F 0.1490(5) 0.8982(3) 0.0814(2) 0.0434(8) Uani 0.882(9) 1 d P A 1 F12 F 0.1700(5) 0.8532(3) -0.08555(19) 0.0660(11) Uani 0.882(9) 1 d P A 1 F13 F -0.0226(3) 0.7903(3) 0.0267(5) 0.0779(15) Uani 0.882(9) 1 d P A 1 F11A F 0.0934(16) 0.8723(17) 0.0957(10) 0.025(3) Uiso 0.118(9) 1 d PD A 2 F12A F 0.0174(16) 0.7866(15) -0.0363(11) 0.029(4) Uiso 0.118(9) 1 d PD A 2 F13A F 0.2277(17) 0.8605(17) -0.0513(15) 0.042(5) Uiso 0.118(9) 1 d PD A 2 F14 F 0.5667(2) 0.2791(2) 0.24593(18) 0.0543(5) Uani 1 1 d . . . F15 F 0.56749(16) 0.50766(18) 0.27119(13) 0.0355(3) Uani 1 1 d . A . F16 F 0.3869(2) 0.3828(2) 0.35434(14) 0.0413(4) Uani 1 1 d . . . C21 C 0.0448(2) 0.8575(2) 0.31916(17) 0.0208(4) Uani 1 1 d . A . C22 C -0.0745(2) 0.7657(2) 0.33856(18) 0.0238(4) Uani 1 1 d . . . C23 C -0.2272(3) 0.8228(3) 0.3659(2) 0.0335(5) Uani 1 1 d . A . H23 H -0.3036 0.7595 0.3775 0.051(10) Uiso 1 1 d R . . C24 C -0.2653(3) 0.9727(3) 0.3759(2) 0.0390(6) Uani 1 1 d . . . H24 H -0.3675 1.0114 0.3914 0.051(10) Uiso 1 1 d R A . C25 C -0.1504(3) 1.0653(3) 0.3620(2) 0.0333(5) Uani 1 1 d . A . H25 H -0.1748 1.1656 0.3717 0.035(8) Uiso 1 1 d R . . C26 C 0.0020(3) 1.0082(2) 0.33463(18) 0.0247(4) Uani 1 1 d . . . C27 C -0.0455(3) 0.6004(3) 0.33165(19) 0.0266(4) Uani 1 1 d . A . C28 C 0.1184(3) 1.1175(3) 0.3215(2) 0.0348(5) Uani 1 1 d . A . F21 F 0.09805(16) 0.54172(15) 0.35836(13) 0.0304(3) Uani 1 1 d . A . F22 F -0.14335(19) 0.52327(18) 0.39997(15) 0.0412(4) Uani 1 1 d . . . F23 F -0.0563(2) 0.56823(19) 0.22859(14) 0.0408(4) Uani 1 1 d . . . F24 F 0.0722(2) 1.2329(2) 0.3784(2) 0.0648(6) Uani 1 1 d . . . F25 F 0.25433(18) 1.05514(17) 0.35929(14) 0.0377(3) Uani 1 1 d . A . F26 F 0.1507(3) 1.1710(2) 0.21465(18) 0.0631(6) 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 Sn 0.01912(7) 0.02095(8) 0.01937(8) -0.00238(5) -0.00197(5) -0.00449(5) Cl1 0.0250(2) 0.0429(3) 0.0227(2) -0.0042(2) -0.00658(18) -0.0043(2) Cl2 0.0390(3) 0.0338(3) 0.0417(3) -0.0050(2) 0.0116(3) -0.0171(2) C11 0.0193(8) 0.0217(9) 0.0206(9) -0.0011(7) -0.0019(7) -0.0036(7) C12 0.0215(9) 0.0269(10) 0.0223(9) -0.0029(8) -0.0012(7) -0.0037(7) C13 0.0338(11) 0.0370(12) 0.0232(10) -0.0073(9) -0.0027(9) -0.0105(9) C14 0.0378(12) 0.0327(12) 0.0316(12) -0.0124(10) 0.0043(10) -0.0120(10) C15 0.0309(11) 0.0223(10) 0.0346(12) -0.0063(9) 0.0064(9) -0.0061(8) C16 0.0212(9) 0.0227(9) 0.0263(10) -0.0019(8) 0.0001(7) -0.0021(7) C17 0.0326(11) 0.0350(12) 0.0224(10) 0.0001(9) -0.0093(8) 0.0001(9) C18 0.0288(11) 0.0266(10) 0.0353(12) 0.0025(9) -0.0048(9) 0.0025(8) F11 0.067(2) 0.0287(10) 0.0336(10) -0.0050(8) -0.0204(11) 0.0113(11) F12 0.120(3) 0.0442(12) 0.0195(10) 0.0089(8) 0.0010(13) 0.0200(14) F13 0.0281(11) 0.0562(14) 0.143(4) 0.0181(17) -0.0267(17) 0.0008(10) F14 0.0540(10) 0.0372(9) 0.0675(12) -0.0076(8) -0.0216(9) 0.0228(8) F15 0.0247(6) 0.0446(8) 0.0374(8) -0.0041(6) -0.0080(6) -0.0029(6) F16 0.0420(8) 0.0460(9) 0.0321(8) 0.0117(7) -0.0071(6) -0.0071(7) C21 0.0201(8) 0.0226(9) 0.0194(9) -0.0005(7) -0.0031(7) -0.0035(7) C22 0.0220(9) 0.0285(10) 0.0214(9) -0.0009(8) -0.0032(7) -0.0061(8) C23 0.0208(10) 0.0431(13) 0.0362(12) -0.0013(10) -0.0030(9) -0.0057(9) C24 0.0245(11) 0.0432(14) 0.0443(15) -0.0012(11) 0.0008(10) 0.0057(10) C25 0.0331(12) 0.0307(11) 0.0326(12) -0.0028(9) -0.0012(9) 0.0061(9) C26 0.0267(10) 0.0229(9) 0.0237(10) -0.0004(8) -0.0027(8) -0.0025(8) C27 0.0240(9) 0.0303(11) 0.0280(11) -0.0048(8) -0.0016(8) -0.0113(8) C28 0.0386(13) 0.0232(10) 0.0427(14) -0.0036(10) -0.0020(10) -0.0058(9) F21 0.0289(7) 0.0237(6) 0.0388(8) -0.0005(5) -0.0053(6) -0.0062(5) F22 0.0389(8) 0.0364(8) 0.0478(9) 0.0007(7) 0.0096(7) -0.0191(6) F23 0.0470(9) 0.0481(9) 0.0337(8) -0.0160(7) -0.0077(7) -0.0140(7) F24 0.0551(11) 0.0318(9) 0.1129(19) -0.0350(11) 0.0022(12) -0.0042(8) F25 0.0336(7) 0.0350(8) 0.0488(9) -0.0136(7) -0.0056(6) -0.0096(6) F26 0.0672(13) 0.0631(13) 0.0563(12) 0.0277(10) -0.0099(10) -0.0327(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Sn C21 2.177(2) . ? Sn C11 2.183(2) . ? Sn Cl1 2.3266(7) . ? Sn Cl2 2.3372(7) . ? Sn F11 2.686(2) . ? Sn F11A 2.757(15) . ? Sn F21 2.7684(14) . ? Sn F25 3.0017(16) . ? Sn F15 3.2027(16) . ? C11 C12 1.408(3) . ? C11 C16 1.409(3) . ? C12 C13 1.398(3) . ? C12 C17 1.508(3) . ? C13 C14 1.376(4) . ? C13 H13 0.9288 . ? C14 C15 1.382(4) . ? C14 H14 0.9278 . ? C15 C16 1.398(3) . ? C15 H15 0.9294 . ? C16 C18 1.498(3) . ? C17 F11A 1.261(10) . ? C17 F12A 1.262(10) . ? C17 F13A 1.268(10) . ? C17 F12 1.310(3) . ? C17 F11 1.344(3) . ? C17 F13 1.351(3) . ? C18 F14 1.339(3) . ? C18 F16 1.342(3) . ? C18 F15 1.348(3) . ? C21 C26 1.405(3) . ? C21 C22 1.407(3) . ? C22 C23 1.395(3) . ? C22 C27 1.503(3) . ? C23 C24 1.378(4) . ? C23 H23 0.9296 . ? C24 C25 1.383(4) . ? C24 H24 0.9284 . ? C25 C26 1.392(3) . ? C25 H25 0.9299 . ? C26 C28 1.502(3) . ? C27 F22 1.330(3) . ? C27 F23 1.343(3) . ? C27 F21 1.353(3) . ? C28 F24 1.334(3) . ? C28 F26 1.336(3) . ? C28 F25 1.347(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 C21 Sn C11 115.73(7) . . ? C21 Sn Cl1 100.97(6) . . ? C11 Sn Cl1 120.66(6) . . ? C21 Sn Cl2 121.53(6) . . ? C11 Sn Cl2 98.18(6) . . ? Cl1 Sn Cl2 100.11(3) . . ? Cl1 Sn F11 168.26(5) . . ? Cl1 Sn F11A 165.8(2) . . ? Cl2 Sn F21 169.33(3) . . ? C11 Sn F25 160.69(6) . . ? C21 Sn F15 153.92(6) . . ? C12 C11 C16 116.32(19) . . ? C12 C11 Sn 119.05(15) . . ? C16 C11 Sn 124.63(15) . . ? C13 C12 C11 121.8(2) . . ? C13 C12 C17 114.0(2) . . ? C11 C12 C17 124.21(19) . . ? C14 C13 C12 120.3(2) . . ? C14 C13 H13 119.9 . . ? C12 C13 H13 119.8 . . ? C13 C14 C15 119.7(2) . . ? C13 C14 H14 120.2 . . ? C15 C14 H14 120.2 . . ? C14 C15 C16 120.4(2) . . ? C14 C15 H15 119.7 . . ? C16 C15 H15 119.9 . . ? C15 C16 C11 121.5(2) . . ? C15 C16 C18 117.1(2) . . ? C11 C16 C18 121.4(2) . . ? F11A C17 F12A 111.6(8) . . ? F11A C17 F13A 107.8(8) . . ? F12A C17 F13A 106.9(8) . . ? F12 C17 F11 105.6(2) . . ? F12 C17 F13 107.6(3) . . ? F11 C17 F13 103.7(3) . . ? F11A C17 C12 114.8(7) . . ? F12A C17 C12 111.8(6) . . ? F13A C17 C12 103.1(8) . . ? F12 C17 C12 113.4(2) . . ? F11 C17 C12 114.23(19) . . ? F13 C17 C12 111.7(2) . . ? F14 C18 F16 106.8(2) . . ? F14 C18 F15 106.0(2) . . ? F16 C18 F15 106.6(2) . . ? F14 C18 C16 112.6(2) . . ? F16 C18 C16 112.49(19) . . ? F15 C18 C16 111.82(19) . . ? C17 F11 Sn 109.63(14) . . ? C17 F11A Sn 108.9(8) . . ? C18 F15 Sn 89.81(12) . . ? C26 C21 C22 116.00(19) . . ? C26 C21 Sn 124.14(15) . . ? C22 C21 Sn 119.86(15) . . ? C23 C22 C21 121.9(2) . . ? C23 C22 C27 115.9(2) . . ? C21 C22 C27 122.28(19) . . ? C24 C23 C22 120.3(2) . . ? C24 C23 H23 119.8 . . ? C22 C23 H23 119.9 . . ? C23 C24 C25 119.6(2) . . ? C23 C24 H24 120.2 . . ? C25 C24 H24 120.2 . . ? C24 C25 C26 120.1(2) . . ? C24 C25 H25 120.0 . . ? C26 C25 H25 119.9 . . ? C25 C26 C21 122.1(2) . . ? C25 C26 C28 116.1(2) . . ? C21 C26 C28 121.8(2) . . ? F22 C27 F23 106.75(18) . . ? F22 C27 F21 106.60(19) . . ? F23 C27 F21 106.00(19) . . ? F22 C27 C22 112.84(19) . . ? F23 C27 C22 112.5(2) . . ? F21 C27 C22 111.68(17) . . ? F24 C28 F26 108.4(2) . . ? F24 C28 F25 105.5(2) . . ? F26 C28 F25 105.7(2) . . ? F24 C28 C26 112.5(2) . . ? F26 C28 C26 111.8(2) . . ? F25 C28 C26 112.5(2) . . ? C27 F21 Sn 103.47(12) . . ? C28 F25 Sn 98.12(13) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C11 C12 C17 F11 8.2(4) . . . . ? C21 C22 C27 F21 29.4(3) . . . . ? C11 C16 C18 F15 -49.4(3) . . . . ? C21 C26 C28 F25 -37.0(3) . . . . ? C12 C11 Sn Cl1 173.51(13) . . . . ? C12 C11 Sn Cl2 -79.54(16) . . . . ? C12 C11 Sn C21 51.43(18) . . . . ? C22 C21 Sn Cl1 -92.64(16) . . . . ? C22 C21 Sn Cl2 158.17(14) . . . . ? C22 C21 Sn C11 39.43(18) . . . . ? _diffrn_measured_fraction_theta_max 0.881 _diffrn_reflns_theta_full 29.00 _diffrn_measured_fraction_theta_full 0.962 _refine_diff_density_max 0.787 _refine_diff_density_min -0.875 _refine_diff_density_rms 0.095 #==============================================END