Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_name_full 'Dalton Trans.' #============================================================================== _journal_coden_Cambridge 0222 _publ_contact_author_name 'Professor Gillian Reid' _publ_contact_author_address ; School of Chemistry University of Southampton Southampton SO17 1BJ, UK ; _publ_contact_author_email gr@soton.ac.uk _publ_contact_author_fax '023 8059 3781' _publ_contact_author_phone '023 8059 3609' _publ_contact_letter ; August 2007 Dear Sirs, This file contains crystallographic data in CIF format for four crystal structures. The data are being offered as supporting information for a paper. Gillian Reid ; _publ_requested_category ? #============================================================================ # TITLE AND AUTHOR LIST # ===================== _publ_section_title ; The first examples of germanium tetrafluoride and tin tetrafluoride complexes with soft thioether coordination synthesis, properties and crystal structures ; loop_ _publ_author_name _publ_author_address M.F.Davis ; School of Chemistry University of Southampton Southampton SO17 1BJ, UK ; W.Levason ; School of Chemistry University of Southampton Southampton SO17 1BJ, UK ; G.Reid ; School of Chemistry University of Southampton Southampton SO17 1BJ, UK ; M.Webster ; School of Chemistry University of Southampton Southampton SO17 1BJ, UK ; W.Zhang ; School of Chemistry University of Southampton Southampton SO17 1BJ, UK ; #============================================================================ # If more than one structure is reported, the remaining sections should be # completed per structure. For each data set, replace the '?' in the # data_? line below by a unique (to this file) identifier. #============================================================================ # 07wz096 data_07wz096_[C4H10F4GeS2] _database_code_depnum_ccdc_archive 'CCDC 652440' _audit_creation_method 'SHELXL-97 + hand edit' _audit_creation_date 2007-06-23 _chemical_name_systematic ; Tetrafluorido(2,5-dithiahexane)germanium(IV) ; _chemical_name_common Tetrafluorido(2,5-dithiahexane)germanium(IV) _chemical_melting_point ? _chemical_formula_moiety 'C4 H10 F4 Ge S2' _chemical_formula_sum 'C4 H10 F4 Ge S2' _chemical_formula_weight 270.83 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ge Ge 0.1547 1.8001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_Int_Tables_number 14 # Superceded ** _symmetry_space_group_name_Hall '-P 2yn' # Superceded ** 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 7.1148(10) _cell_length_b 11.1822(15) _cell_length_c 10.9875(15) _cell_angle_alpha 90.00 _cell_angle_beta 98.884(10) _cell_angle_gamma 90.00 _cell_volume 863.7(2) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 2023 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.03 # 0.02 +/- 0.01 _exptl_crystal_size_mid 0.02 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.083 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 536 _exptl_absorpt_coefficient_mu 4.030 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8912 # _exptl_absorpt_correction_T_max 1.0000 # _exptl_absorpt_process_details 'G.M. Sheldrick, (2007). SADABS. Version 2007/2. Bruker AXS Inc.' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Bruker-Nonius FR591 rotating anode' _diffrn_radiation_monochromator '10cm confocal mirrors' _diffrn_measurement_device_type 'Bruker-Nonius 95mm CCD camera on \k-goniostat' _diffrn_measurement_method '\f & \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 10496 _diffrn_reflns_av_R_equivalents 0.0274 _diffrn_reflns_av_sigmaI/netI 0.0265 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 3.20 _diffrn_reflns_theta_max 27.53 _reflns_number_total 1981 _reflns_number_gt 1776 _reflns_threshold_expression I>2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0318P)^2^+0.8904P] 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 noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1981 _refine_ls_number_parameters 100 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0312 _refine_ls_R_factor_gt 0.0257 _refine_ls_wR_factor_ref 0.0690 _refine_ls_wR_factor_gt 0.0652 _refine_ls_goodness_of_fit_ref 1.093 _refine_ls_restrained_S_all 1.093 _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 Ge1 Ge 0.07058(3) 0.251655(19) 0.86976(2) 0.01413(10) Uani 1 1 d . . . F1 F 0.0822(2) 0.16347(13) 1.00519(13) 0.0208(3) Uani 1 1 d . . . F2 F 0.3116(2) 0.29342(14) 0.90131(14) 0.0251(3) Uani 1 1 d . . . F3 F -0.0161(2) 0.37525(12) 0.94130(13) 0.0241(3) Uani 1 1 d . . . F4 F 0.0342(2) 0.32119(12) 0.72294(13) 0.0226(3) Uani 1 1 d . . . S1 S 0.17119(9) 0.06949(5) 0.77719(6) 0.01980(15) Uani 1 1 d . . . S2 S -0.26058(8) 0.18346(5) 0.80589(6) 0.01900(14) Uani 1 1 d . . . C1 C 0.2252(4) 0.1136(2) 0.6291(3) 0.0276(6) Uani 1 1 d . . . H1A H 0.3459 0.1575 0.6399 0.041 Uiso 1 1 calc R . . H1B H 0.1233 0.1651 0.5879 0.041 Uiso 1 1 calc R . . H1C H 0.2357 0.0423 0.5787 0.041 Uiso 1 1 calc R . . C2 C -0.0521(4) -0.0079(2) 0.7357(2) 0.0234(5) Uani 1 1 d . . . H2A H -0.0395 -0.0663 0.6697 0.028 Uiso 1 1 calc R . . H2B H -0.0809 -0.0531 0.8081 0.028 Uiso 1 1 calc R . . C3 C -0.2168(4) 0.0756(2) 0.6917(2) 0.0248(5) Uani 1 1 d . . . H3A H -0.3333 0.0274 0.6674 0.030 Uiso 1 1 calc R . . H3B H -0.1898 0.1187 0.6175 0.030 Uiso 1 1 calc R . . C4 C -0.3244(4) 0.0886(2) 0.9263(2) 0.0238(5) Uani 1 1 d . . . H4A H -0.3515 0.1382 0.9951 0.036 Uiso 1 1 calc R . . H4B H -0.2187 0.0343 0.9552 0.036 Uiso 1 1 calc R . . H4C H -0.4376 0.0418 0.8940 0.036 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ge1 0.01605(15) 0.01254(14) 0.01372(16) -0.00041(8) 0.00204(11) -0.00102(9) F1 0.0230(7) 0.0240(7) 0.0143(7) 0.0047(5) -0.0001(6) 0.0003(6) F2 0.0192(7) 0.0298(8) 0.0261(8) -0.0004(7) 0.0032(6) -0.0068(6) F3 0.0312(8) 0.0177(7) 0.0239(8) -0.0050(6) 0.0054(6) 0.0032(6) F4 0.0303(8) 0.0192(7) 0.0185(7) 0.0056(6) 0.0050(6) -0.0001(6) S1 0.0216(3) 0.0190(3) 0.0184(3) -0.0018(2) 0.0018(2) 0.0050(2) S2 0.0161(3) 0.0173(3) 0.0227(3) 0.0032(2) 0.0001(2) 0.0008(2) C1 0.0339(15) 0.0258(13) 0.0265(14) -0.0039(11) 0.0153(12) -0.0005(11) C2 0.0334(14) 0.0161(11) 0.0223(13) -0.0047(10) 0.0093(11) -0.0047(10) C3 0.0249(12) 0.0259(13) 0.0223(13) -0.0057(10) -0.0006(10) -0.0083(11) C4 0.0222(12) 0.0231(12) 0.0273(14) 0.0039(10) 0.0077(10) -0.0028(10) _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 Ge1 F3 1.7487(14) . ? Ge1 F2 1.7592(15) . ? Ge1 F4 1.7734(14) . ? Ge1 F1 1.7764(14) . ? Ge1 S1 2.4334(7) . ? Ge1 S2 2.4728(7) . ? S1 C1 1.798(3) . ? S1 C2 1.805(3) . ? S2 C3 1.802(3) . ? S2 C4 1.808(3) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 C3 1.518(4) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag F3 Ge1 F2 95.87(7) . . ? F3 Ge1 F4 92.89(7) . . ? F2 Ge1 F4 93.65(7) . . ? F3 Ge1 F1 92.07(7) . . ? F2 Ge1 F1 93.70(7) . . ? F4 Ge1 F1 170.67(6) . . ? F3 Ge1 S1 175.15(5) . . ? F2 Ge1 S1 87.93(5) . . ? F4 Ge1 S1 89.87(5) . . ? F1 Ge1 S1 84.66(5) . . ? F3 Ge1 S2 89.12(5) . . ? F2 Ge1 S2 174.15(5) . . ? F4 Ge1 S2 83.01(5) . . ? F1 Ge1 S2 89.17(5) . . ? S1 Ge1 S2 87.26(2) . . ? C1 S1 C2 101.88(13) . . ? C1 S1 Ge1 105.45(9) . . ? C2 S1 Ge1 101.68(8) . . ? C3 S2 C4 101.96(13) . . ? C3 S2 Ge1 98.30(8) . . ? C4 S2 Ge1 108.02(9) . . ? S1 C1 H1A 109.5 . . ? S1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? S1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C3 C2 S1 113.06(17) . . ? C3 C2 H2A 109.0 . . ? S1 C2 H2A 109.0 . . ? C3 C2 H2B 109.0 . . ? S1 C2 H2B 109.0 . . ? H2A C2 H2B 107.8 . . ? C2 C3 S2 113.42(18) . . ? C2 C3 H3A 108.9 . . ? S2 C3 H3A 108.9 . . ? C2 C3 H3B 108.9 . . ? S2 C3 H3B 108.9 . . ? H3A C3 H3B 107.7 . . ? S2 C4 H4A 109.5 . . ? S2 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? S2 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag # F3 Ge1 S1 C1 141.7(6) . . . . ? # F3 Ge1 S1 C2 35.7(6) . . . . ? # F2 Ge1 S2 C3 16.4(5) . . . . ? # F2 Ge1 S2 C4 121.9(5) . . . . ? F2 Ge1 S1 C1 -76.62(11) . . . . ? F4 Ge1 S1 C1 17.03(11) . . . . ? F1 Ge1 S1 C1 -170.54(11) . . . . ? S2 Ge1 S1 C1 100.04(10) . . . . ? F2 Ge1 S1 C2 177.41(10) . . . . ? F4 Ge1 S1 C2 -88.94(10) . . . . ? F1 Ge1 S1 C2 83.49(10) . . . . ? S2 Ge1 S1 C2 -5.93(9) . . . . ? F3 Ge1 S2 C3 164.86(10) . . . . ? F4 Ge1 S2 C3 71.84(10) . . . . ? F1 Ge1 S2 C3 -103.05(10) . . . . ? S1 Ge1 S2 C3 -18.36(9) . . . . ? F3 Ge1 S2 C4 -89.62(11) . . . . ? F4 Ge1 S2 C4 177.36(10) . . . . ? F1 Ge1 S2 C4 2.47(10) . . . . ? S1 Ge1 S2 C4 87.16(9) . . . . ? C1 S1 C2 C3 -72.2(2) . . . . ? Ge1 S1 C2 C3 36.60(19) . . . . ? S1 C2 C3 S2 -60.8(2) . . . . ? C4 S2 C3 C2 -63.0(2) . . . . ? Ge1 S2 C3 C2 47.55(18) . . . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 27.53 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.376 _refine_diff_density_min -0.458 _refine_diff_density_rms 0.083 #===END OF CIF ============================================================== # 07wz094 data_07wz094_[C6H14F4GeS2] _database_code_depnum_ccdc_archive 'CCDC 652441' _audit_creation_method 'SHELXL-97 + hand edit' _audit_creation_date 2007-06-23 _chemical_name_systematic ; Tetrafluorido(3,6-dithiaoctane)germanium(IV) ; _chemical_name_common Tetrafluorido(3,6-dithiaoctane)germanium(IV) _chemical_melting_point ? _chemical_formula_moiety 'C6 H14 F4 Ge S2' _chemical_formula_sum 'C6 H14 F4 Ge S2' _chemical_formula_weight 298.88 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ge Ge 0.1547 1.8001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_Int_Tables_number 14 # Superceded ** _symmetry_space_group_name_Hall '-P 2ybc' # Superceded ** loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 10.9011(15) _cell_length_b 8.5151(15) _cell_length_c 11.935(3) _cell_angle_alpha 90.00 _cell_angle_beta 101.202(10) _cell_angle_gamma 90.00 _cell_volume 1086.7(3) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 2575 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.13 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.827 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 600 _exptl_absorpt_coefficient_mu 3.212 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7496 # 0.6802 _exptl_absorpt_correction_T_max 1.0000 # 0.8064 _exptl_absorpt_process_details 'G.M. Sheldrick, (2003). SADABS. Version 2.10. Bruker AXS Inc.' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Nonius rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'area detector, Nonius Kappa ccd' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 13998 _diffrn_reflns_av_R_equivalents 0.0526 _diffrn_reflns_av_sigmaI/netI 0.0449 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 3.06 _diffrn_reflns_theta_max 27.54 _reflns_number_total 2474 _reflns_number_gt 2103 _reflns_threshold_expression I>2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0442P)^2^+0.3000P] 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 noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2474 _refine_ls_number_parameters 118 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0412 _refine_ls_R_factor_gt 0.0310 _refine_ls_wR_factor_ref 0.0817 _refine_ls_wR_factor_gt 0.0770 _refine_ls_goodness_of_fit_ref 1.026 _refine_ls_restrained_S_all 1.026 _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 Ge1 Ge 0.73106(2) 0.05433(3) 0.38908(2) 0.01539(11) Uani 1 1 d . . . F1 F 0.56958(14) 0.03429(18) 0.39027(14) 0.0218(4) Uani 1 1 d . . . F2 F 0.71717(15) 0.24779(19) 0.33854(15) 0.0261(4) Uani 1 1 d . . . F3 F 0.71852(15) -0.04027(19) 0.25659(14) 0.0252(4) Uani 1 1 d . . . F4 F 0.89688(14) 0.05959(17) 0.41078(14) 0.0215(4) Uani 1 1 d . . . S1 S 0.74011(6) 0.16029(8) 0.58236(6) 0.01689(16) Uani 1 1 d . . . S2 S 0.76619(6) -0.20839(7) 0.48141(6) 0.01753(16) Uani 1 1 d . . . C1 C 0.9181(3) 0.3869(4) 0.5845(3) 0.0346(8) Uani 1 1 d . . . H1A H 1.0036 0.4233 0.6139 0.052 Uiso 1 1 calc R . . H1B H 0.8585 0.4630 0.6046 0.052 Uiso 1 1 calc R . . H1C H 0.9049 0.3767 0.5012 0.052 Uiso 1 1 calc R . . C2 C 0.8985(2) 0.2285(3) 0.6368(2) 0.0213(6) Uani 1 1 d . . . H2A H 0.9125 0.2382 0.7210 0.026 Uiso 1 1 calc R . . H2B H 0.9593 0.1516 0.6176 0.026 Uiso 1 1 calc R . . C3 C 0.7393(3) -0.0180(3) 0.6641(2) 0.0208(6) Uani 1 1 d . . . H3A H 0.7707 0.0059 0.7458 0.025 Uiso 1 1 calc R . . H3B H 0.6521 -0.0554 0.6560 0.025 Uiso 1 1 calc R . . C4 C 0.8188(2) -0.1494(3) 0.6278(2) 0.0189(5) Uani 1 1 d . . . H4A H 0.8166 -0.2414 0.6781 0.023 Uiso 1 1 calc R . . H4B H 0.9067 -0.1134 0.6382 0.023 Uiso 1 1 calc R . . C5 C 0.6131(2) -0.2903(3) 0.4880(2) 0.0206(6) Uani 1 1 d . . . H5A H 0.6215 -0.3682 0.5506 0.025 Uiso 1 1 calc R . . H5B H 0.5567 -0.2056 0.5040 0.025 Uiso 1 1 calc R . . C6 C 0.5580(3) -0.3685(4) 0.3756(3) 0.0298(7) Uani 1 1 d . . . H6A H 0.4759 -0.4125 0.3796 0.045 Uiso 1 1 calc R . . H6B H 0.6137 -0.4529 0.3604 0.045 Uiso 1 1 calc R . . H6C H 0.5488 -0.2908 0.3140 0.045 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ge1 0.01378(17) 0.01968(17) 0.01305(17) 0.00173(10) 0.00346(11) 0.00319(9) F1 0.0126(7) 0.0296(9) 0.0229(9) 0.0006(7) 0.0029(7) 0.0038(6) F2 0.0325(9) 0.0229(8) 0.0241(9) 0.0094(7) 0.0083(7) 0.0065(7) F3 0.0277(9) 0.0327(10) 0.0151(9) -0.0038(7) 0.0038(7) 0.0041(7) F4 0.0149(8) 0.0271(9) 0.0240(9) 0.0029(7) 0.0079(7) 0.0010(6) S1 0.0155(3) 0.0194(3) 0.0162(3) 0.0000(3) 0.0040(2) 0.0020(2) S2 0.0145(3) 0.0183(3) 0.0205(4) 0.0007(3) 0.0050(2) 0.0015(2) C1 0.0374(18) 0.0239(16) 0.044(2) 0.0042(14) 0.0118(15) -0.0060(13) C2 0.0196(13) 0.0237(14) 0.0213(15) -0.0023(11) 0.0053(11) -0.0044(11) C3 0.0200(13) 0.0261(14) 0.0172(14) 0.0036(12) 0.0063(11) -0.0056(11) C4 0.0167(12) 0.0197(13) 0.0190(14) 0.0058(11) 0.0001(10) -0.0019(10) C5 0.0164(12) 0.0243(14) 0.0224(15) -0.0021(11) 0.0068(11) -0.0045(10) C6 0.0241(15) 0.0355(18) 0.0293(18) -0.0102(13) 0.0043(13) -0.0054(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 Ge1 F2 1.7507(16) . ? Ge1 F3 1.7561(16) . ? Ge1 F1 1.7714(15) . ? Ge1 F4 1.7761(15) . ? Ge1 S1 2.4611(8) . ? Ge1 S2 2.4903(8) . ? S1 C3 1.805(3) . ? S1 C2 1.818(3) . ? S2 C4 1.802(3) . ? S2 C5 1.825(3) . ? C1 C2 1.519(4) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.529(4) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C6 1.514(4) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag F2 Ge1 F3 97.76(8) . . ? F2 Ge1 F1 94.23(7) . . ? F3 Ge1 F1 93.40(8) . . ? F2 Ge1 F4 92.52(7) . . ? F3 Ge1 F4 92.40(8) . . ? F1 Ge1 F4 170.42(7) . . ? F2 Ge1 S1 87.88(6) . . ? F3 Ge1 S1 173.77(6) . . ? F1 Ge1 S1 83.49(6) . . ? F4 Ge1 S1 89.98(6) . . ? F2 Ge1 S2 173.37(6) . . ? F3 Ge1 S2 87.98(6) . . ? F1 Ge1 S2 88.71(5) . . ? F4 Ge1 S2 83.88(5) . . ? S1 Ge1 S2 86.55(3) . . ? C3 S1 C2 100.34(13) . . ? C3 S1 Ge1 101.24(10) . . ? C2 S1 Ge1 108.34(9) . . ? C4 S2 C5 100.74(13) . . ? C4 S2 Ge1 99.86(9) . . ? C5 S2 Ge1 107.41(9) . . ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C1 C2 S1 109.7(2) . . ? C1 C2 H2A 109.7 . . ? S1 C2 H2A 109.7 . . ? C1 C2 H2B 109.7 . . ? S1 C2 H2B 109.7 . . ? H2A C2 H2B 108.2 . . ? C4 C3 S1 113.57(18) . . ? C4 C3 H3A 108.9 . . ? S1 C3 H3A 108.9 . . ? C4 C3 H3B 108.9 . . ? S1 C3 H3B 108.9 . . ? H3A C3 H3B 107.7 . . ? C3 C4 S2 112.81(19) . . ? C3 C4 H4A 109.0 . . ? S2 C4 H4A 109.0 . . ? C3 C4 H4B 109.0 . . ? S2 C4 H4B 109.0 . . ? H4A C4 H4B 107.8 . . ? C6 C5 S2 109.78(19) . . ? C6 C5 H5A 109.7 . . ? S2 C5 H5A 109.7 . . ? C6 C5 H5B 109.7 . . ? S2 C5 H5B 109.7 . . ? H5A C5 H5B 108.2 . . ? C5 C6 H6A 109.5 . . ? C5 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C5 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag # F3 Ge1 S1 C3 19.4(5) . . . . ? # F3 Ge1 S1 C2 124.4(5) . . . . ? # F2 Ge1 S2 C4 17.6(5) . . . . ? # F2 Ge1 S2 C5 122.2(5) . . . . ? F2 Ge1 S1 C3 174.32(11) . . . . ? F1 Ge1 S1 C3 79.81(10) . . . . ? F4 Ge1 S1 C3 -93.15(10) . . . . ? S2 Ge1 S1 C3 -9.28(9) . . . . ? F2 Ge1 S1 C2 -80.69(11) . . . . ? F1 Ge1 S1 C2 -175.20(11) . . . . ? F4 Ge1 S1 C2 11.83(11) . . . . ? S2 Ge1 S1 C2 95.71(10) . . . . ? F3 Ge1 S2 C4 167.63(10) . . . . ? F1 Ge1 S2 C4 -98.92(10) . . . . ? F4 Ge1 S2 C4 74.99(10) . . . . ? S1 Ge1 S2 C4 -15.36(9) . . . . ? F3 Ge1 S2 C5 -87.73(11) . . . . ? F1 Ge1 S2 C5 5.73(11) . . . . ? F4 Ge1 S2 C5 179.64(11) . . . . ? S1 Ge1 S2 C5 89.29(10) . . . . ? C3 S1 C2 C1 -176.2(2) . . . . ? Ge1 S1 C2 C1 78.2(2) . . . . ? C2 S1 C3 C4 -71.4(2) . . . . ? Ge1 S1 C3 C4 39.9(2) . . . . ? S1 C3 C4 S2 -60.9(2) . . . . ? C5 S2 C4 C3 -65.3(2) . . . . ? Ge1 S2 C4 C3 44.70(19) . . . . ? C4 S2 C5 C6 -172.3(2) . . . . ? Ge1 S2 C5 C6 83.7(2) . . . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 27.54 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.512 _refine_diff_density_min -0.657 _refine_diff_density_rms 0.100 #===END OF CIF ============================================================== # 07mfd003 data_07mfd003_[C6H14F4S2Sn] _database_code_depnum_ccdc_archive 'CCDC 652442' _audit_creation_method 'SHELXL-97 + hand edit' _audit_creation_date 2007-04-26 _chemical_name_systematic ; Tetrafluoro(3,6-dithiaoctane-S,S')tin(IV) ; # Tetrafluoro(1,2-bis(ethylthio)ethane-S,S')tin(IV) _chemical_name_common Tetrafluoro(3,6-dithiaoctane-S,S')tin(IV) _chemical_melting_point ? _chemical_formula_moiety 'C6 H14 F4 S2 Sn' _chemical_formula_sum 'C6 H14 F4 S2 Sn' _chemical_formula_weight 344.98 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sn Sn -0.6537 1.4246 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_Int_Tables_number 14 # Superceded ** _symmetry_space_group_name_Hall '-P 2ybc' # Superceded ** 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 11.093(2) _cell_length_b 8.4148(15) _cell_length_c 12.276(2) _cell_angle_alpha 90.00 _cell_angle_beta 100.627(7) _cell_angle_gamma 90.00 _cell_volume 1126.2(3) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 2704 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.035 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 672 _exptl_absorpt_coefficient_mu 2.649 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8968 # 0.7417 _exptl_absorpt_correction_T_max 1.0000 # 0.8160 _exptl_absorpt_process_details 'G.M. Sheldrick, (2003). SADABS. Version 2.10. Bruker AXS Inc.' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Bruker-Nonius FR591 rotating anode' _diffrn_radiation_monochromator '10cm confocal mirrors' _diffrn_measurement_device_type 'Bruker-Nonius 95mm CCD camera on \k-goniostat' _diffrn_measurement_method '\f & \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 11875 _diffrn_reflns_av_R_equivalents 0.0238 _diffrn_reflns_av_sigmaI/netI 0.0227 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 3.32 _diffrn_reflns_theta_max 27.54 _reflns_number_total 2579 _reflns_number_gt 2400 _reflns_threshold_expression I>2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+1.4000P] 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 noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2579 _refine_ls_number_parameters 120 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0204 _refine_ls_R_factor_gt 0.0177 _refine_ls_wR_factor_ref 0.0377 _refine_ls_wR_factor_gt 0.0363 _refine_ls_goodness_of_fit_ref 1.066 _refine_ls_restrained_S_all 1.066 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Sn1 Sn 0.231468(11) 0.438283(16) 0.888496(10) 0.01301(5) Uani 1 1 d . . . F1 F 0.40994(10) 0.43079(15) 0.90463(10) 0.0213(3) Uani 1 1 d . . . F2 F 0.05637(10) 0.45629(15) 0.88881(10) 0.0207(3) Uani 1 1 d . . . F3 F 0.21998(12) 0.22030(15) 0.83881(11) 0.0247(3) Uani 1 1 d . . . F4 F 0.21675(11) 0.53719(15) 0.74433(10) 0.0226(3) Uani 1 1 d . . . S1 S 0.24382(4) 0.33789(6) 1.08925(4) 0.01490(10) Uani 1 1 d . . . S2 S 0.26476(4) 0.71808(6) 0.97946(4) 0.01502(10) Uani 1 1 d . . . C1 C 0.4241(2) 0.1158(3) 1.0907(2) 0.0294(5) Uani 1 1 d . . . H1A H 0.3664 0.0380 1.1111 0.044 Uiso 1 1 calc R . . H1B H 0.5083 0.0814 1.1197 0.044 Uiso 1 1 calc R . . H1C H 0.4121 0.1243 1.0098 0.044 Uiso 1 1 calc R . . C2 C 0.40183(18) 0.2768(2) 1.13956(18) 0.0188(4) Uani 1 1 d . . . H2A H 0.4587 0.3564 1.1178 0.023 Uiso 1 1 calc R . . H2B H 0.4175 0.2699 1.2215 0.023 Uiso 1 1 calc R . . C3 C 0.23922(18) 0.5254(2) 1.16015(16) 0.0167(4) Uani 1 1 d . . . H3A H 0.1529 0.5612 1.1498 0.020 Uiso 1 1 calc R . . H3B H 0.2681 0.5078 1.2405 0.020 Uiso 1 1 calc R . . C4 C 0.31541(18) 0.6577(2) 1.12243(16) 0.0166(4) Uani 1 1 d . . . H4A H 0.4018 0.6220 1.1321 0.020 Uiso 1 1 calc R . . H4B H 0.3130 0.7512 1.1709 0.020 Uiso 1 1 calc R . . C5 C 0.11154(18) 0.7948(3) 0.98302(17) 0.0181(4) Uani 1 1 d . . . H5A H 0.0584 0.7078 1.0011 0.022 Uiso 1 1 calc R . . H5B H 0.1163 0.8775 1.0410 0.022 Uiso 1 1 calc R . . C6 C 0.0573(2) 0.8651(3) 0.87047(19) 0.0242(5) Uani 1 1 d . . . H6A H 0.1074 0.9553 0.8550 0.036 Uiso 1 1 calc R . . H6B H -0.0266 0.9015 0.8709 0.036 Uiso 1 1 calc R . . H6C H 0.0560 0.7840 0.8130 0.036 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Sn1 0.01292(7) 0.01538(8) 0.01155(8) -0.00187(5) 0.00435(5) -0.00297(5) F1 0.0137(6) 0.0262(7) 0.0257(7) -0.0016(5) 0.0081(5) -0.0009(5) F2 0.0115(5) 0.0287(7) 0.0221(7) -0.0007(5) 0.0034(5) -0.0046(5) F3 0.0344(7) 0.0193(6) 0.0217(7) -0.0067(5) 0.0088(5) -0.0059(6) F4 0.0259(6) 0.0281(7) 0.0139(6) 0.0030(5) 0.0044(5) -0.0054(5) S1 0.0154(2) 0.0159(2) 0.0140(2) 0.00008(19) 0.00430(18) -0.00266(19) S2 0.0145(2) 0.0145(2) 0.0170(3) -0.00110(19) 0.00540(18) -0.00144(19) C1 0.0309(12) 0.0205(12) 0.0396(14) -0.0014(10) 0.0138(11) 0.0051(10) C2 0.0168(9) 0.0182(11) 0.0211(11) 0.0013(8) 0.0029(8) 0.0032(8) C3 0.0166(9) 0.0210(11) 0.0129(10) -0.0023(8) 0.0036(8) 0.0038(8) C4 0.0146(9) 0.0197(11) 0.0147(10) -0.0049(8) 0.0005(7) 0.0007(8) C5 0.0166(9) 0.0192(10) 0.0197(11) 0.0004(8) 0.0065(8) 0.0028(8) C6 0.0221(10) 0.0267(12) 0.0243(12) 0.0088(9) 0.0053(9) 0.0042(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Sn1 F3 1.9298(13) . ? Sn1 F4 1.9352(12) . ? Sn1 F2 1.9490(12) . ? Sn1 F1 1.9540(12) . ? Sn1 S1 2.5849(6) . ? Sn1 S2 2.6028(6) . ? S1 C3 1.807(2) . ? S1 C2 1.822(2) . ? S2 C4 1.814(2) . ? S2 C5 1.826(2) . ? C1 C2 1.520(3) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.521(3) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C6 1.522(3) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag F3 Sn1 F4 97.48(6) . . ? F3 Sn1 F2 93.83(5) . . ? F4 Sn1 F2 93.00(5) . . ? F3 Sn1 F1 90.46(5) . . ? F4 Sn1 F1 91.12(5) . . ? F2 Sn1 F1 173.62(5) . . ? F3 Sn1 S1 88.82(4) . . ? F4 Sn1 S1 173.31(4) . . ? F2 Sn1 S1 84.33(4) . . ? F1 Sn1 S1 91.04(4) . . ? F3 Sn1 S2 172.42(4) . . ? F4 Sn1 S2 89.12(4) . . ? F2 Sn1 S2 89.51(4) . . ? F1 Sn1 S2 85.69(4) . . ? S1 Sn1 S2 84.732(19) . . ? C3 S1 C2 101.19(10) . . ? C3 S1 Sn1 99.94(7) . . ? C2 S1 Sn1 107.10(7) . . ? C4 S2 C5 101.50(9) . . ? C4 S2 Sn1 98.97(7) . . ? C5 S2 Sn1 105.71(7) . . ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C1 C2 S1 109.54(15) . . ? C1 C2 H2A 109.8 . . ? S1 C2 H2A 109.8 . . ? C1 C2 H2B 109.8 . . ? S1 C2 H2B 109.8 . . ? H2A C2 H2B 108.2 . . ? C4 C3 S1 115.21(14) . . ? C4 C3 H3A 108.5 . . ? S1 C3 H3A 108.5 . . ? C4 C3 H3B 108.5 . . ? S1 C3 H3B 108.5 . . ? H3A C3 H3B 107.5 . . ? C3 C4 S2 114.16(14) . . ? C3 C4 H4A 108.7 . . ? S2 C4 H4A 108.7 . . ? C3 C4 H4B 108.7 . . ? S2 C4 H4B 108.7 . . ? H4A C4 H4B 107.6 . . ? C6 C5 S2 109.27(14) . . ? C6 C5 H5A 109.8 . . ? S2 C5 H5A 109.8 . . ? C6 C5 H5B 109.8 . . ? S2 C5 H5B 109.8 . . ? H5A C5 H5B 108.3 . . ? C5 C6 H6A 109.5 . . ? C5 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C5 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag # F4 Sn1 S1 C3 -13.4(3) . . . . ? # F4 Sn1 S1 C2 -118.5(3) . . . . ? # F3 Sn1 S2 C4 -17.4(3) . . . . ? # F3 Sn1 S2 C5 -122.1(3) . . . . ? F3 Sn1 S1 C3 -174.07(8) . . . . ? F2 Sn1 S1 C3 -80.10(8) . . . . ? F1 Sn1 S1 C3 95.49(8) . . . . ? S2 Sn1 S1 C3 9.92(7) . . . . ? F3 Sn1 S1 C2 80.85(8) . . . . ? F2 Sn1 S1 C2 174.82(8) . . . . ? F1 Sn1 S1 C2 -9.58(8) . . . . ? S2 Sn1 S1 C2 -95.15(7) . . . . ? F4 Sn1 S2 C4 -168.13(7) . . . . ? F2 Sn1 S2 C4 98.86(8) . . . . ? F1 Sn1 S2 C4 -76.93(8) . . . . ? S1 Sn1 S2 C4 14.52(7) . . . . ? F4 Sn1 S2 C5 87.15(8) . . . . ? F2 Sn1 S2 C5 -5.86(8) . . . . ? F1 Sn1 S2 C5 178.34(8) . . . . ? S1 Sn1 S2 C5 -90.21(7) . . . . ? C3 S1 C2 C1 178.61(16) . . . . ? Sn1 S1 C2 C1 -77.21(16) . . . . ? C2 S1 C3 C4 68.41(16) . . . . ? Sn1 S1 C3 C4 -41.40(15) . . . . ? S1 C3 C4 S2 63.78(18) . . . . ? C5 S2 C4 C3 63.28(16) . . . . ? Sn1 S2 C4 C3 -44.90(15) . . . . ? C4 S2 C5 C6 175.24(15) . . . . ? Sn1 S2 C5 C6 -81.90(15) . . . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 27.54 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.433 _refine_diff_density_min -0.397 _refine_diff_density_rms 0.080 #===END OF CIF ============================================================== # 07mfd014 data_07mfd014_[C8H18F4S2Sn] _database_code_depnum_ccdc_archive 'CCDC 658599' _audit_creation_method 'SHELXL-97 + hand edit' _audit_creation_date 2007-08-20 _chemical_name_systematic ; Tetrafluorido(2,7-dimethyl-3,6-dithiaoctane)tin(IV) ; _chemical_name_common Tetrafluorido(2,7-dimethyl-3,6-dithiaoctane)tin(IV) _chemical_melting_point ? _chemical_formula_moiety 'C8 H18 F4 S2 Sn' _chemical_formula_sum 'C8 H18 F4 S2 Sn' _chemical_formula_weight 373.03 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sn Sn -0.6537 1.4246 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' _symmetry_Int_Tables_number 15 # Superceded ** _symmetry_space_group_name_Hall '-C 2yc' # Superceded ** loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, z+1/2' 'x+1/2, y+1/2, z' 'x+1/2, -y+1/2, z+1/2' '-x, -y, -z' '-x, y, -z-1/2' '-x+1/2, -y+1/2, -z' '-x+1/2, y+1/2, -z-1/2' _cell_length_a 10.540(3) _cell_length_b 7.573(2) _cell_length_c 17.642(5) _cell_angle_alpha 90.00 _cell_angle_beta 97.456(10) _cell_angle_gamma 90.00 _cell_volume 1396.2(6) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 11615 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description needle _exptl_crystal_colour colourless _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.775 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 736 _exptl_absorpt_coefficient_mu 2.144 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8037 # 0.6989 _exptl_absorpt_correction_T_max 1.0000 # 0.9004 _exptl_absorpt_process_details 'G.M. Sheldrick, (2007). SADABS. Version 2007/2. Bruker AXS Inc.' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Bruker-Nonius FR591 rotating anode' _diffrn_radiation_monochromator '10cm confocal mirrors' _diffrn_measurement_device_type 'Bruker-Nonius 95mm CCD camera on \k-goniostat' _diffrn_measurement_method '\f & \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 7267 _diffrn_reflns_av_R_equivalents 0.0246 _diffrn_reflns_av_sigmaI/netI 0.0224 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 3.32 _diffrn_reflns_theta_max 27.56 _reflns_number_total 1598 _reflns_number_gt 1508 _reflns_threshold_expression I>2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+2.4120P] 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 noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1598 _refine_ls_number_parameters 69 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0215 _refine_ls_R_factor_gt 0.0190 _refine_ls_wR_factor_ref 0.0391 _refine_ls_wR_factor_gt 0.0381 _refine_ls_goodness_of_fit_ref 1.121 _refine_ls_restrained_S_all 1.121 _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 Sn1 Sn 0.0000 0.16148(2) 0.7500 0.02225(7) Uani 1 2 d S . . S1 S -0.02091(4) -0.08738(7) 0.64890(3) 0.02082(11) Uani 1 1 d . . . F1 F 0.18511(11) 0.13824(17) 0.75737(7) 0.0333(3) Uani 1 1 d . . . F2 F -0.00986(15) 0.33230(17) 0.66795(8) 0.0451(4) Uani 1 1 d . . . C1 C 0.1746(2) 0.0344(3) 0.57708(11) 0.0279(4) Uani 1 1 d . . . H1A H 0.1712 0.1418 0.6077 0.042 Uiso 1 1 calc R . . H1B H 0.1132 0.0440 0.5305 0.042 Uiso 1 1 calc R . . H1C H 0.2610 0.0197 0.5632 0.042 Uiso 1 1 calc R . . C2 C 0.1440(2) -0.2964(3) 0.57978(12) 0.0321(5) Uani 1 1 d . . . H2A H 0.1219 -0.3941 0.6120 0.048 Uiso 1 1 calc R . . H2B H 0.2300 -0.3152 0.5658 0.048 Uiso 1 1 calc R . . H2C H 0.0820 -0.2911 0.5333 0.048 Uiso 1 1 calc R . . C3 C 0.14099(18) -0.1244(3) 0.62327(11) 0.0215(4) Uani 1 1 d . . . H3 H 0.2029 -0.1318 0.6711 0.026 Uiso 1 1 calc R . . C4 C -0.0441(2) -0.2688(3) 0.71240(11) 0.0268(4) Uani 1 1 d . . . H4A H -0.1337 -0.2660 0.7236 0.032 Uiso 1 1 calc R . . H4B H -0.0320 -0.3809 0.6854 0.032 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Sn1 0.02754(11) 0.01372(10) 0.02793(11) 0.000 0.01281(8) 0.000 S1 0.0160(2) 0.0245(2) 0.0222(2) -0.00347(19) 0.00322(18) 0.00161(18) F1 0.0234(6) 0.0432(8) 0.0350(7) -0.0110(6) 0.0107(5) -0.0166(5) F2 0.0740(10) 0.0212(6) 0.0455(8) 0.0114(6) 0.0284(7) 0.0069(7) C1 0.0280(11) 0.0339(12) 0.0231(10) 0.0038(9) 0.0077(8) -0.0016(9) C2 0.0377(12) 0.0295(12) 0.0329(11) -0.0026(9) 0.0182(10) 0.0068(9) C3 0.0182(9) 0.0273(10) 0.0204(9) 0.0015(8) 0.0078(8) 0.0041(8) C4 0.0306(11) 0.0182(9) 0.0355(11) -0.0069(8) 0.0191(9) -0.0078(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Sn1 F2 1.9341(13) 6_557 ? Sn1 F2 1.9341(13) . ? Sn1 F1 1.9464(13) 6_557 ? Sn1 F1 1.9464(13) . ? Sn1 S1 2.5844(7) . ? Sn1 S1 2.5844(7) 6_557 ? S1 C4 1.809(2) . ? S1 C3 1.8425(19) . ? C1 C3 1.520(3) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 C3 1.514(3) . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 H3 1.0000 . ? C4 C4 1.518(4) 6_557 ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? 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 F2 Sn1 F2 96.04(9) 6_557 . ? F2 Sn1 F1 93.82(6) 6_557 6_557 ? F2 Sn1 F1 93.12(6) . 6_557 ? F2 Sn1 F1 93.12(6) 6_557 . ? F2 Sn1 F1 93.82(6) . . ? F1 Sn1 F1 169.63(8) 6_557 . ? F2 Sn1 S1 174.71(4) 6_557 . ? F2 Sn1 S1 88.83(5) . . ? F1 Sn1 S1 83.86(4) 6_557 . ? F1 Sn1 S1 88.58(4) . . ? F2 Sn1 S1 88.83(5) 6_557 6_557 ? F2 Sn1 S1 174.71(4) . 6_557 ? F1 Sn1 S1 88.58(4) 6_557 6_557 ? F1 Sn1 S1 83.86(4) . 6_557 ? S1 Sn1 S1 86.37(3) . 6_557 ? C4 S1 C3 103.92(9) . . ? C4 S1 Sn1 97.61(7) . . ? C3 S1 Sn1 106.35(7) . . ? C3 C1 H1A 109.5 . . ? C3 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C3 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C3 C2 H2A 109.5 . . ? C3 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C3 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C2 C3 C1 112.78(16) . . ? C2 C3 S1 109.64(14) . . ? C1 C3 S1 107.40(13) . . ? C2 C3 H3 109.0 . . ? C1 C3 H3 109.0 . . ? S1 C3 H3 109.0 . . ? C4 C4 S1 115.11(12) 6_557 . ? C4 C4 H4A 108.5 6_557 . ? S1 C4 H4A 108.5 . . ? C4 C4 H4B 108.5 6_557 . ? S1 C4 H4B 108.5 . . ? H4A C4 H4B 107.5 . . ? 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 # F2 Sn1 S1 C4 -12.5(5) 6_557 . . . ? # F2 Sn1 S1 C3 -119.5(5) 6_557 . . . ? F2 Sn1 S1 C4 -169.88(8) . . . . ? F1 Sn1 S1 C4 -76.62(8) 6_557 . . . ? F1 Sn1 S1 C4 96.27(8) . . . . ? S1 Sn1 S1 C4 12.34(7) 6_557 . . . ? F2 Sn1 S1 C3 83.13(8) . . . . ? F1 Sn1 S1 C3 176.39(7) 6_557 . . . ? F1 Sn1 S1 C3 -10.72(7) . . . . ? S1 Sn1 S1 C3 -94.65(7) 6_557 . . . ? C4 S1 C3 C2 63.58(16) . . . . ? Sn1 S1 C3 C2 165.99(12) . . . . ? C4 S1 C3 C1 -173.56(14) . . . . ? Sn1 S1 C3 C1 -71.15(14) . . . . ? C3 S1 C4 C4 65.13(17) . . . 6_557 ? Sn1 S1 C4 C4 -43.88(16) . . . 6_557 ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 27.56 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 0.377 _refine_diff_density_min -0.397 _refine_diff_density_rms 0.067 #===END OF CIF ============================================================== # # The following lines are used to test the character set of files sent by # network email or other means. They are not part of the CIF data set. # abcdefghijklmnopqrstuvwxyzABCDEFGHIJKLMNOPQRSTUVWXYZ0123456789 # !@#$%^&*()_+{}:"~<>?|\-=[];'`,./ # #===END OF FILE =============================================================