# Supplementary Material (ESI) for New Journal of Chemistry # This journal is © The Royal Society of Chemistry and # The Centre National de la Recherche Scientifique, 2003 data_global _publ_contact_author_email gr@soton.ac.uk _publ_contact_author_name 'Dr Gillian Reid' _journal_name_full 'New J.Chem.(Nouv.J.Chim.)' #============================================================================== # SUBMISSION DETAILS # ================== _journal_coden_Cambridge 0440 _publ_contact_author_address ; Department of Chemistry University of Southampton Southampton SO17 1BJ, UK ; _publ_contact_author_fax '023 8059 6805' _publ_contact_author_phone '023 8059 3609' _publ_contact_letter ; 12th July 2003 Dear Sirs, This file contains three cifs to accompany paper ref. number B307863A submitted to the New Journal of Chemistry. Gillian Reid ; _publ_requested_category ? #============================================================================== # PROCESSING SUMMARY (IUCr Office Use Only) # ================== #============================================================================== # TITLE AND AUTHOR LIST # ===================== _publ_section_title ; Unusual Structural Variations Within a Family of Thioether Macrocyclic Complexes. Tin(IV) Halide Adducts of [12]-, [14]- and [16]-aneS4 ; _publ_section_title_footnote ; ? ; _publ_section_references ; Beurskens, P.T., Admiraal, G., Beurskens, G., Bosman, W.P., Garcia-Granda, S., Gould, R.O., Smits, J.M.M. and Smykalla, C. (1992). The DIRDIF program system, Technical Report of the Crystallography Laboratory, University of Nijmegen, The Netherlands. Blessing, R. H. (1997). J. Appl. Cryst. 30, 421-426. Hooft, R. (1998). COLLECT. Nonius BV, Delft, The Netherlands. Johnson, C. K. (1976). ORTEPII. Report ORNL-5138. Oak Ridge National Laboratory, Tennessee, USA. Molecular Structure Corporation. (1997-1999). teXsan for Windows. Single Crystal Structure Analysis Software. Version 1.06. MSC, 9009 New Trails Drive, The Woodlands, TX 77381, USA. Otwinowski, Z. & Minor, W. (1997). Methods in Enzymology, Vol. 276, Macromolecular Crystallography, Part A, edited by C. W. Carter & R. M. Sweet, pp. 307-326. London: Academic Press. Sheldrick, G. M. (1990). Acta Cryst. A46, 467-473. Sheldrick, G. M. (1997). SHELXL97. University of Gottingen, Germany. Sheldrick, G. M. (1997). SHELXS97. University of Gottingen, Germany. ; # The loop structure below should contain the names and addresses of all # authors, in the required order of publication. Repeat as necessary. # Note order: Family_name, first name(s) or initials (or mixture). loop_ _publ_author_name _publ_author_footnote _publ_author_address W.Levason ? ; Department of Chemistry University of Southampton Southampton SO17 1BJ, UK ; M.L.Matthews ? ; Department of Chemistry University of Southampton Southampton SO17 1BJ, UK ; R.Patel ? ; Department of Chemistry University of Southampton Southampton SO17 1BJ, UK ; G.Reid ? ; Department of Chemistry University of Southampton Southampton SO17 1BJ, UK ; M.Webster ? ; Department 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. #============================================================================== data_[SnBr4([12]aneS4)] _database_code_CSD 208975 _chemical_name_common 1,4,7,10-tetrathiacyclododecane-tetrabromotin(IV) # _d010new, 24-06-2003 _audit_creation_method 'SHELXL-97 + hand edit' _chemical_name_systematic ; 1,4,7,10-tetrathiacyclododecane-tetrabromotin(IV) ; _chemical_melting_point ? _chemical_formula_moiety 'C8 H16 Br4 S4 Sn' _chemical_formula_sum 'C8 H16 Br4 S4 Sn' _chemical_formula_weight 678.78 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sn Sn -0.6537 1.4246 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'C m c m' _symmetry_Int_Tables_number 63 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-x, y, -z+1/2' 'x, -y, -z' 'x+1/2, y+1/2, z' '-x+1/2, -y+1/2, z+1/2' '-x+1/2, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x, y, -z-1/2' 'x, -y, z-1/2' '-x, y, z' '-x+1/2, -y+1/2, -z' 'x+1/2, y+1/2, -z-1/2' 'x+1/2, -y+1/2, z-1/2' '-x+1/2, y+1/2, z' _cell_length_a 10.5135(3) _cell_length_b 8.3306(3) _cell_length_c 19.6638(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1722.23(10) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 6593 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description block _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.618 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1272 _exptl_absorpt_coefficient_mu 11.227 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.07609 # shelx 0.1337 _exptl_absorpt_correction_T_max 0.20894 # shelx 0.3998 _exptl_absorpt_process_details 'SORTAV, R H Blessing, J. Appl. Cryst., 1997, 30, 421-426.' _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 'Nonius Kappa CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5824 _diffrn_reflns_av_R_equivalents 0.0983 _diffrn_reflns_av_sigmaI/netI 0.0530 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 3.12 _diffrn_reflns_theta_max 27.45 _reflns_number_total 1069 _reflns_number_gt 991 _reflns_threshold_expression >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^)+(0.0684P)^2^+6.010P] 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 1069 _refine_ls_number_parameters 46 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0447 _refine_ls_R_factor_gt 0.0412 _refine_ls_wR_factor_ref 0.1072 _refine_ls_wR_factor_gt 0.1046 _refine_ls_goodness_of_fit_ref 1.062 _refine_ls_restrained_S_all 1.062 _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 0.17621(7) 0.2500 0.0140(2) Uani 1 4 d S . . Br1 Br 0.24264(6) 0.19916(8) 0.2500 0.0174(2) Uani 1 2 d S . . Br2 Br 0.0000 -0.01554(8) 0.14952(3) 0.0199(2) Uani 1 2 d S . . S1 S 0.28824(16) 0.5000 0.0000 0.0197(4) Uani 1 2 d S . . S2 S 0.0000 0.4363(2) 0.16227(7) 0.0159(3) Uani 1 2 d S . . C1 C 0.1333(5) 0.4001(7) 0.1045(2) 0.0203(10) Uani 1 1 d . . . H1A H 0.2061 0.3579 0.1309 0.024 Uiso 1 1 calc R . . H1B H 0.1083 0.3169 0.0711 0.024 Uiso 1 1 calc R . . C2 C 0.1756(5) 0.5496(6) 0.0663(2) 0.0198(9) Uani 1 1 d . . . H2A H 0.2153 0.6258 0.0986 0.024 Uiso 1 1 calc R . . H2B H 0.1005 0.6027 0.0460 0.024 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 0.0138(3) 0.0175(4) 0.0108(3) 0.000 0.000 0.000 Br1 0.0145(4) 0.0245(4) 0.0133(3) 0.000 0.000 0.0002(2) Br2 0.0200(4) 0.0228(4) 0.0167(3) -0.0057(2) 0.000 0.000 S1 0.0157(8) 0.0305(9) 0.0128(7) 0.0029(6) 0.000 0.000 S2 0.0170(8) 0.0192(8) 0.0115(6) 0.0009(5) 0.000 0.000 C1 0.024(2) 0.023(2) 0.015(2) 0.0044(17) 0.0041(16) 0.002(2) C2 0.023(2) 0.023(2) 0.0136(19) -0.0026(17) 0.0032(17) -0.002(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Sn1 Br2 2.5407(7) . ? Sn1 Br2 2.5407(7) 10_556 ? Sn1 Br1 2.5582(7) . ? Sn1 Br1 2.5582(7) 3 ? Sn1 S2 2.7697(17) 10_556 ? Sn1 S2 2.7697(17) . ? S1 C2 1.810(5) 4_565 ? S1 C2 1.810(5) . ? S2 C1 1.829(5) 12 ? S2 C1 1.829(5) . ? C1 C2 1.520(7) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 H2A 0.9900 . ? C2 H2B 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 Br2 Sn1 Br2 102.09(4) . 10_556 ? Br2 Sn1 Br1 92.693(13) . . ? Br2 Sn1 Br1 92.693(13) 10_556 . ? Br2 Sn1 Br1 92.693(13) . 3 ? Br2 Sn1 Br1 92.693(13) 10_556 3 ? Br1 Sn1 Br1 171.43(4) . 3 ? Br2 Sn1 S2 167.48(4) . 10_556 ? Br2 Sn1 S2 90.43(3) 10_556 10_556 ? Br1 Sn1 S2 86.648(17) . 10_556 ? Br1 Sn1 S2 86.648(17) 3 10_556 ? Br2 Sn1 S2 90.43(3) . . ? Br2 Sn1 S2 167.48(4) 10_556 . ? Br1 Sn1 S2 86.648(17) . . ? Br1 Sn1 S2 86.648(17) 3 . ? S2 Sn1 S2 77.05(7) 10_556 . ? C2 S1 C2 98.2(3) 4_565 . ? C1 S2 C1 100.0(3) 12 . ? C1 S2 Sn1 104.95(17) 12 . ? C1 S2 Sn1 104.95(17) . . ? C2 C1 S2 113.3(4) . . ? C2 C1 H1A 108.9 . . ? S2 C1 H1A 108.9 . . ? C2 C1 H1B 108.9 . . ? S2 C1 H1B 108.9 . . ? H1A C1 H1B 107.7 . . ? C1 C2 S1 111.1(3) . . ? C1 C2 H2A 109.4 . . ? S1 C2 H2A 109.4 . . ? C1 C2 H2B 109.4 . . ? S1 C2 H2B 109.4 . . ? H2A C2 H2B 108.0 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Br2 Sn1 S2 C1 52.46(18) . . . 12 ? Br2 Sn1 S2 C1 -127.54(18) 10_556 . . 12 ? Br1 Sn1 S2 C1 145.13(18) . . . 12 ? Br1 Sn1 S2 C1 -40.22(18) 3 . . 12 ? S2 Sn1 S2 C1 -127.54(18) 10_556 . . 12 ? Br2 Sn1 S2 C1 -52.46(18) . . . . ? Br2 Sn1 S2 C1 127.54(18) 10_556 . . . ? Br1 Sn1 S2 C1 40.22(18) . . . . ? Br1 Sn1 S2 C1 -145.13(18) 3 . . . ? S2 Sn1 S2 C1 127.54(18) 10_556 . . . ? C1 S2 C1 C2 89.0(4) 12 . . . ? Sn1 S2 C1 C2 -162.5(3) . . . . ? S2 C1 C2 S1 -170.2(3) . . . . ? C2 S1 C2 C1 85.4(3) 4_565 . . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 27.45 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.393 _refine_diff_density_min -2.487 _refine_diff_density_rms 0.277 #===END================================================================== data_SnBr4([14]aneS4).2/3CH2Cl2 _database_code_CSD 208976 _chemical_name_common ;1,4,8,11-tetrathiacyclotetradecane-tetrabromotin(IV) dichloromethane solvate ; _audit_creation_method 'SHELXL-97 + hand edit' _chemical_name_systematic ; 1,4,8,11-tetrathiacyclotetradecane-tetrabromotin(IV) dichloromethane solvate ; _chemical_melting_point ? _chemical_formula_moiety 'C10 H20 Br4 S4 Sn, 0.67(C H2 Cl2)' _chemical_formula_sum 'C10.67 H21.33 Br4 Cl1.33 S4 Sn' _chemical_formula_weight 763.45 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sn Sn -0.6537 1.4246 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_Int_Tables_number 2 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.2865(3) _cell_length_b 11.5634(3) _cell_length_c 13.3067(4) _cell_angle_alpha 104.8650(10) _cell_angle_beta 103.4750(10) _cell_angle_gamma 92.8590(10) _cell_volume 1621.19(8) _cell_formula_units_Z 3 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 8678 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description needle _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.346 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1086 _exptl_absorpt_coefficient_mu 9.119 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.53716 # (Shelx 0.2089) _exptl_absorpt_correction_T_max 0.62454 # (Shelx 0.6107) _exptl_absorpt_process_details 'SORTAV, R H Blessing, J. Appl. Cryst., 1997, 30, 421-426.' _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 'Nonius Kappa CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15354 _diffrn_reflns_av_R_equivalents 0.0611 _diffrn_reflns_av_sigmaI/netI 0.0743 _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 -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.94 _diffrn_reflns_theta_max 27.53 _reflns_number_total 7125 _reflns_number_gt 5762 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _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^)+(0.0263P)^2^+10.6581P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7125 _refine_ls_number_parameters 260 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0635 _refine_ls_R_factor_gt 0.0467 _refine_ls_wR_factor_ref 0.1077 _refine_ls_wR_factor_gt 0.0997 _refine_ls_goodness_of_fit_ref 1.034 _refine_ls_restrained_S_all 1.034 _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 0.5000 0.5000 0.01046(13) Uani 1 2 d S . . Sn2 Sn -0.5000 0.0000 0.5000 0.01212(14) Uani 1 2 d S . . Sn3 Sn 0.0000 0.5000 0.0000 0.01340(14) Uani 1 2 d S . . Br1 Br 0.18701(6) 0.42645(6) 0.43482(5) 0.01456(14) Uani 1 1 d . . . Br2 Br -0.13892(6) 0.41750(6) 0.30886(5) 0.01467(14) Uani 1 1 d . . . Br3 Br -0.50169(6) -0.07043(6) 0.30074(5) 0.01731(15) Uani 1 1 d . . . Br4 Br -0.72458(6) 0.04705(6) 0.44997(6) 0.01718(15) Uani 1 1 d . . . Br5 Br 0.10321(6) 0.60132(6) 0.19981(5) 0.01937(16) Uani 1 1 d . . . Br6 Br -0.21183(6) 0.53195(6) 0.03411(6) 0.02117(16) Uani 1 1 d . . . Cl1 Cl 0.5620(2) 0.14196(19) 0.10888(17) 0.0365(5) Uani 1 1 d . . . Cl2 Cl 0.5140(2) 0.3202(2) -0.0113(2) 0.0432(6) Uani 1 1 d . . . S1 S 0.05241(15) 0.71208(14) 0.46789(13) 0.0132(3) Uiso 1 1 d . . . S2 S 0.16801(16) 0.99675(15) 0.77838(14) 0.0172(3) Uiso 1 1 d . . . S3 S -0.40900(15) 0.20742(15) 0.49080(13) 0.0155(3) Uiso 1 1 d . . . S4 S -0.57626(16) 0.40351(16) 0.26528(15) 0.0199(4) Uiso 1 1 d . . . S5 S 0.00091(16) 0.27742(15) 0.01607(14) 0.0174(4) Uiso 1 1 d . . . S6 S 0.17944(18) 0.07056(18) 0.07827(16) 0.0269(4) Uiso 1 1 d . . . C1 C 0.0450(6) 0.8229(6) 0.5922(5) 0.0145(14) Uani 1 1 d . . . H1A H -0.0105 0.8825 0.5745 0.029(4) Uiso 1 1 calc R . . H1B H 0.0113 0.7816 0.6379 0.029(4) Uiso 1 1 calc R . . C2 C 0.1720(6) 0.8874(6) 0.6537(5) 0.0168(14) Uani 1 1 d . . . H2A H 0.2051 0.9292 0.6080 0.029(4) Uiso 1 1 calc R . . H2B H 0.2275 0.8274 0.6702 0.029(4) Uiso 1 1 calc R . . C3 C 0.1749(7) 1.1365(6) 0.7415(6) 0.0191(15) Uani 1 1 d . . . H3A H 0.1832 1.2043 0.8066 0.029(4) Uiso 1 1 calc R . . H3B H 0.2494 1.1443 0.7155 0.029(4) Uiso 1 1 calc R . . C4 C -0.0637(6) 0.8525(6) 0.3449(6) 0.0171(14) Uani 1 1 d . . . H4A H -0.0523 0.9213 0.4098 0.029(4) Uiso 1 1 calc R . . H4B H 0.0110 0.8545 0.3181 0.029(4) Uiso 1 1 calc R . . C5 C -0.0830(6) 0.7340(6) 0.3734(6) 0.0172(14) Uani 1 1 d . . . H5A H -0.1015 0.6661 0.3072 0.029(4) Uiso 1 1 calc R . . H5B H -0.1541 0.7351 0.4054 0.029(4) Uiso 1 1 calc R . . C6 C -0.5183(6) 0.2508(6) 0.3878(6) 0.0177(14) Uani 1 1 d . . . H6A H -0.5386 0.1847 0.3201 0.029(4) Uiso 1 1 calc R . . H6B H -0.5949 0.2662 0.4106 0.029(4) Uiso 1 1 calc R . . C7 C -0.4637(7) 0.3634(6) 0.3693(6) 0.0206(15) Uani 1 1 d . . . H7A H -0.3873 0.3483 0.3461 0.029(4) Uiso 1 1 calc R . . H7B H -0.4438 0.4299 0.4366 0.029(4) Uiso 1 1 calc R . . C8 C -0.4942(6) 0.5401(6) 0.2588(5) 0.0135(13) Uani 1 1 d . . . H8A H -0.4135 0.5220 0.2454 0.029(4) Uiso 1 1 calc R . . H8B H -0.5412 0.5664 0.1975 0.029(4) Uiso 1 1 calc R . . C9 C -0.5258(6) 0.3557(6) 0.6363(6) 0.0183(15) Uani 1 1 d . . . H9A H -0.5731 0.2848 0.6429 0.029(4) Uiso 1 1 calc R . . H9B H -0.5743 0.3811 0.5751 0.029(4) Uiso 1 1 calc R . . C10 C -0.4042(6) 0.3206(6) 0.6140(6) 0.0178(14) Uani 1 1 d . . . H10A H -0.3591 0.2921 0.6746 0.029(4) Uiso 1 1 calc R . . H10B H -0.3555 0.3944 0.6145 0.029(4) Uiso 1 1 calc R . . C11 C 0.1022(6) 0.2937(6) 0.1481(6) 0.0190(15) Uani 1 1 d . . . H11A H 0.1833 0.3337 0.1517 0.029(4) Uiso 1 1 calc R . . H11B H 0.0683 0.3464 0.2031 0.029(4) Uiso 1 1 calc R . . C12 C 0.1193(7) 0.1755(6) 0.1743(5) 0.0187(15) Uani 1 1 d . . . H12A H 0.0393 0.1386 0.1767 0.029(4) Uiso 1 1 calc R . . H12B H 0.1759 0.1908 0.2466 0.029(4) Uiso 1 1 calc R . . C13 C 0.1846(7) -0.0511(6) 0.1427(6) 0.0223(16) Uani 1 1 d . . . H13A H 0.2391 -0.0225 0.2164 0.029(4) Uiso 1 1 calc R . . H13B H 0.1014 -0.0745 0.1484 0.029(4) Uiso 1 1 calc R . . C14 C -0.2317(6) 0.1604(6) -0.0791(6) 0.0220(16) Uani 1 1 d . . . H14A H -0.2446 0.2194 -0.1218 0.029(4) Uiso 1 1 calc R . . H14B H -0.3125 0.1346 -0.0697 0.029(4) Uiso 1 1 calc R . . C15 C -0.1481(6) 0.2229(7) 0.0304(6) 0.0208(15) Uani 1 1 d . . . H15A H -0.1364 0.1659 0.0752 0.029(4) Uiso 1 1 calc R . . H15B H -0.1861 0.2915 0.0668 0.029(4) Uiso 1 1 calc R . . C16 C 0.4525(7) 0.1934(7) 0.0187(6) 0.0283(18) Uani 1 1 d . . . H16A H 0.3826 0.2148 0.0502 0.029(4) Uiso 1 1 calc R . . H16B H 0.4212 0.1279 -0.0487 0.029(4) 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 0.0102(3) 0.0095(3) 0.0123(3) 0.0036(2) 0.0032(2) 0.0035(2) Sn2 0.0101(3) 0.0124(3) 0.0148(3) 0.0056(2) 0.0023(2) 0.0041(2) Sn3 0.0128(3) 0.0144(3) 0.0130(3) 0.0035(2) 0.0033(2) 0.0030(2) Br1 0.0117(3) 0.0153(3) 0.0175(3) 0.0039(3) 0.0052(2) 0.0049(3) Br2 0.0155(3) 0.0139(3) 0.0138(3) 0.0040(3) 0.0019(2) 0.0026(3) Br3 0.0185(3) 0.0193(3) 0.0148(3) 0.0054(3) 0.0038(3) 0.0066(3) Br4 0.0107(3) 0.0219(4) 0.0215(4) 0.0102(3) 0.0033(3) 0.0064(3) Br5 0.0208(3) 0.0204(4) 0.0145(3) 0.0032(3) 0.0021(3) 0.0011(3) Br6 0.0151(3) 0.0238(4) 0.0270(4) 0.0070(3) 0.0094(3) 0.0053(3) Cl1 0.0422(12) 0.0373(12) 0.0316(11) 0.0111(9) 0.0092(9) 0.0124(10) Cl2 0.0432(13) 0.0348(12) 0.0679(17) 0.0263(11) 0.0307(12) 0.0119(10) C1 0.017(3) 0.007(3) 0.018(3) 0.002(3) 0.003(3) 0.005(3) C2 0.017(3) 0.017(3) 0.018(3) 0.004(3) 0.007(3) 0.008(3) C3 0.022(4) 0.013(3) 0.021(4) 0.006(3) 0.002(3) 0.006(3) C4 0.016(3) 0.016(3) 0.018(3) 0.006(3) 0.002(3) 0.003(3) C5 0.014(3) 0.018(3) 0.018(3) 0.004(3) 0.000(3) 0.007(3) C6 0.024(4) 0.012(3) 0.019(4) 0.008(3) 0.004(3) 0.007(3) C7 0.021(4) 0.017(4) 0.025(4) 0.010(3) 0.004(3) 0.000(3) C8 0.010(3) 0.010(3) 0.022(4) 0.008(3) 0.005(3) -0.001(2) C9 0.014(3) 0.015(3) 0.025(4) 0.007(3) 0.001(3) 0.005(3) C10 0.015(3) 0.016(3) 0.018(4) 0.003(3) -0.002(3) 0.001(3) C11 0.020(4) 0.016(3) 0.018(4) 0.003(3) 0.000(3) 0.006(3) C12 0.025(4) 0.020(4) 0.014(3) 0.006(3) 0.008(3) 0.012(3) C13 0.027(4) 0.017(4) 0.022(4) 0.008(3) 0.001(3) 0.004(3) C14 0.013(3) 0.024(4) 0.030(4) 0.011(3) 0.002(3) 0.005(3) C15 0.019(3) 0.028(4) 0.017(4) 0.005(3) 0.008(3) 0.002(3) C16 0.026(4) 0.031(4) 0.028(4) 0.011(4) 0.004(3) 0.007(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Sn1 Br1 2.5660(6) . ? Sn1 Br1 2.5660(6) 2_566 ? Sn1 Br2 2.5661(6) 2_566 ? Sn1 Br2 2.5661(6) . ? Sn1 S1 2.6565(16) . ? Sn1 S1 2.6565(16) 2_566 ? Sn2 Br3 2.5614(7) 2_456 ? Sn2 Br3 2.5614(7) . ? Sn2 Br4 2.5887(6) . ? Sn2 Br4 2.5887(6) 2_456 ? Sn2 S3 2.6050(17) . ? Sn2 S3 2.6050(17) 2_456 ? Sn3 Br6 2.5625(7) 2_565 ? Sn3 Br6 2.5625(7) . ? Sn3 Br5 2.5731(7) . ? Sn3 Br5 2.5731(7) 2_565 ? Sn3 S5 2.6371(17) 2_565 ? Sn3 S5 2.6371(17) . ? Cl1 C16 1.752(8) . ? Cl2 C16 1.766(8) . ? S1 C5 1.813(7) . ? S1 C1 1.837(6) . ? S2 C3 1.808(7) . ? S2 C2 1.822(7) . ? S3 C10 1.804(7) . ? S3 C6 1.811(7) . ? S4 C7 1.820(7) . ? S4 C8 1.822(6) . ? S5 C11 1.817(7) . ? S5 C15 1.836(7) . ? S6 C12 1.805(7) . ? S6 C13 1.822(7) . ? C1 C2 1.521(9) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.527(9) 2_576 ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 C3 1.527(9) 2_576 ? C4 C5 1.532(9) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 C7 1.514(9) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 C9 1.554(9) 2_466 ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C10 1.523(9) . ? C9 C8 1.554(9) 2_466 ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 C12 1.505(9) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 C14 1.525(10) 2 ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 C15 1.512(10) . ? C14 C13 1.525(10) 2 ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 H16A 0.9900 . ? C16 H16B 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 Br1 Sn1 Br1 180.0 . 2_566 ? Br1 Sn1 Br2 89.21(2) . 2_566 ? Br1 Sn1 Br2 90.79(2) 2_566 2_566 ? Br1 Sn1 Br2 90.79(2) . . ? Br1 Sn1 Br2 89.21(2) 2_566 . ? Br2 Sn1 Br2 180.0 2_566 . ? Br1 Sn1 S1 89.31(4) . . ? Br1 Sn1 S1 90.69(4) 2_566 . ? Br2 Sn1 S1 87.73(4) 2_566 . ? Br2 Sn1 S1 92.27(4) . . ? Br1 Sn1 S1 90.69(4) . 2_566 ? Br1 Sn1 S1 89.31(4) 2_566 2_566 ? Br2 Sn1 S1 92.27(4) 2_566 2_566 ? Br2 Sn1 S1 87.73(4) . 2_566 ? S1 Sn1 S1 180.0 . 2_566 ? Br3 Sn2 Br3 180.0 2_456 . ? Br3 Sn2 Br4 89.40(2) 2_456 . ? Br3 Sn2 Br4 90.60(2) . . ? Br3 Sn2 Br4 90.60(2) 2_456 2_456 ? Br3 Sn2 Br4 89.40(2) . 2_456 ? Br4 Sn2 Br4 180.0 . 2_456 ? Br3 Sn2 S3 95.47(4) 2_456 . ? Br3 Sn2 S3 84.53(4) . . ? Br4 Sn2 S3 93.64(4) . . ? Br4 Sn2 S3 86.36(4) 2_456 . ? Br3 Sn2 S3 84.53(4) 2_456 2_456 ? Br3 Sn2 S3 95.47(4) . 2_456 ? Br4 Sn2 S3 86.36(4) . 2_456 ? Br4 Sn2 S3 93.64(4) 2_456 2_456 ? S3 Sn2 S3 180.0 . 2_456 ? Br6 Sn3 Br6 180.0 2_565 . ? Br6 Sn3 Br5 89.50(2) 2_565 . ? Br6 Sn3 Br5 90.50(2) . . ? Br6 Sn3 Br5 90.50(2) 2_565 2_565 ? Br6 Sn3 Br5 89.50(2) . 2_565 ? Br5 Sn3 Br5 180.00(3) . 2_565 ? Br6 Sn3 S5 96.70(4) 2_565 2_565 ? Br6 Sn3 S5 83.30(4) . 2_565 ? Br5 Sn3 S5 84.42(4) . 2_565 ? Br5 Sn3 S5 95.58(4) 2_565 2_565 ? Br6 Sn3 S5 83.30(4) 2_565 . ? Br6 Sn3 S5 96.70(4) . . ? Br5 Sn3 S5 95.58(4) . . ? Br5 Sn3 S5 84.42(4) 2_565 . ? S5 Sn3 S5 180.0 2_565 . ? C5 S1 C1 101.4(3) . . ? C5 S1 Sn1 105.3(2) . . ? C1 S1 Sn1 104.5(2) . . ? C3 S2 C2 101.5(3) . . ? C10 S3 C6 104.9(3) . . ? C10 S3 Sn2 109.4(2) . . ? C6 S3 Sn2 107.0(2) . . ? C7 S4 C8 100.4(3) . . ? C11 S5 C15 102.8(3) . . ? C11 S5 Sn3 103.8(2) . . ? C15 S5 Sn3 110.3(2) . . ? C12 S6 C13 96.8(3) . . ? C2 C1 S1 110.5(4) . . ? C2 C1 H1A 109.6 . . ? S1 C1 H1A 109.6 . . ? C2 C1 H1B 109.6 . . ? S1 C1 H1B 109.6 . . ? H1A C1 H1B 108.1 . . ? C1 C2 S2 111.6(5) . . ? C1 C2 H2A 109.3 . . ? S2 C2 H2A 109.3 . . ? C1 C2 H2B 109.3 . . ? S2 C2 H2B 109.3 . . ? H2A C2 H2B 108.0 . . ? C4 C3 S2 114.4(5) 2_576 . ? C4 C3 H3A 108.7 2_576 . ? S2 C3 H3A 108.7 . . ? C4 C3 H3B 108.7 2_576 . ? S2 C3 H3B 108.7 . . ? H3A C3 H3B 107.6 . . ? C3 C4 C5 109.6(5) 2_576 . ? C3 C4 H4A 109.7 2_576 . ? C5 C4 H4A 109.7 . . ? C3 C4 H4B 109.7 2_576 . ? C5 C4 H4B 109.7 . . ? H4A C4 H4B 108.2 . . ? C4 C5 S1 110.9(5) . . ? C4 C5 H5A 109.5 . . ? S1 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? S1 C5 H5B 109.5 . . ? H5A C5 H5B 108.1 . . ? C7 C6 S3 109.4(5) . . ? C7 C6 H6A 109.8 . . ? S3 C6 H6A 109.8 . . ? C7 C6 H6B 109.8 . . ? S3 C6 H6B 109.8 . . ? H6A C6 H6B 108.2 . . ? C6 C7 S4 107.9(5) . . ? C6 C7 H7A 110.1 . . ? S4 C7 H7A 110.1 . . ? C6 C7 H7B 110.1 . . ? S4 C7 H7B 110.1 . . ? H7A C7 H7B 108.4 . . ? C9 C8 S4 112.5(5) 2_466 . ? C9 C8 H8A 109.1 2_466 . ? S4 C8 H8A 109.1 . . ? C9 C8 H8B 109.1 2_466 . ? S4 C8 H8B 109.1 . . ? H8A C8 H8B 107.8 . . ? C10 C9 C8 111.4(5) . 2_466 ? C10 C9 H9A 109.3 . . ? C8 C9 H9A 109.3 2_466 . ? C10 C9 H9B 109.3 . . ? C8 C9 H9B 109.3 2_466 . ? H9A C9 H9B 108.0 . . ? C9 C10 S3 117.8(5) . . ? C9 C10 H10A 107.8 . . ? S3 C10 H10A 107.8 . . ? C9 C10 H10B 107.8 . . ? S3 C10 H10B 107.8 . . ? H10A C10 H10B 107.2 . . ? C12 C11 S5 113.2(5) . . ? C12 C11 H11A 108.9 . . ? S5 C11 H11A 108.9 . . ? C12 C11 H11B 108.9 . . ? S5 C11 H11B 108.9 . . ? H11A C11 H11B 107.7 . . ? C11 C12 S6 113.1(5) . . ? C11 C12 H12A 109.0 . . ? S6 C12 H12A 109.0 . . ? C11 C12 H12B 109.0 . . ? S6 C12 H12B 109.0 . . ? H12A C12 H12B 107.8 . . ? C14 C13 S6 111.2(5) 2 . ? C14 C13 H13A 109.4 2 . ? S6 C13 H13A 109.4 . . ? C14 C13 H13B 109.4 2 . ? S6 C13 H13B 109.4 . . ? H13A C13 H13B 108.0 . . ? C15 C14 C13 114.9(6) . 2 ? C15 C14 H14A 108.6 . . ? C13 C14 H14A 108.6 2 . ? C15 C14 H14B 108.6 . . ? C13 C14 H14B 108.6 2 . ? H14A C14 H14B 107.5 . . ? C14 C15 S5 109.9(5) . . ? C14 C15 H15A 109.7 . . ? S5 C15 H15A 109.7 . . ? C14 C15 H15B 109.7 . . ? S5 C15 H15B 109.7 . . ? H15A C15 H15B 108.2 . . ? Cl1 C16 Cl2 111.9(4) . . ? Cl1 C16 H16A 109.2 . . ? Cl2 C16 H16A 109.2 . . ? Cl1 C16 H16B 109.2 . . ? Cl2 C16 H16B 109.2 . . ? H16A C16 H16B 107.9 . . ? 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 Br1 Sn1 S1 C5 121.8(2) . . . . ? Br1 Sn1 S1 C5 -58.2(2) 2_566 . . . ? Br2 Sn1 S1 C5 -148.9(2) 2_566 . . . ? Br2 Sn1 S1 C5 31.1(2) . . . . ? Br1 Sn1 S1 C1 -131.8(2) . . . . ? Br1 Sn1 S1 C1 48.2(2) 2_566 . . . ? Br2 Sn1 S1 C1 -42.5(2) 2_566 . . . ? Br2 Sn1 S1 C1 137.5(2) . . . . ? Br3 Sn2 S3 C10 -9.1(2) 2_456 . . . ? Br3 Sn2 S3 C10 170.9(2) . . . . ? Br4 Sn2 S3 C10 80.6(2) . . . . ? Br4 Sn2 S3 C10 -99.4(2) 2_456 . . . ? Br3 Sn2 S3 C6 -122.3(2) 2_456 . . . ? Br3 Sn2 S3 C6 57.7(2) . . . . ? Br4 Sn2 S3 C6 -32.5(2) . . . . ? Br4 Sn2 S3 C6 147.5(2) 2_456 . . . ? Br6 Sn3 S5 C11 76.3(2) 2_565 . . . ? Br6 Sn3 S5 C11 -103.7(2) . . . . ? Br5 Sn3 S5 C11 -12.6(2) . . . . ? Br5 Sn3 S5 C11 167.4(2) 2_565 . . . ? Br6 Sn3 S5 C15 -174.2(2) 2_565 . . . ? Br6 Sn3 S5 C15 5.8(2) . . . . ? Br5 Sn3 S5 C15 96.9(2) . . . . ? Br5 Sn3 S5 C15 -83.1(2) 2_565 . . . ? C5 S1 C1 C2 -138.6(5) . . . . ? Sn1 S1 C1 C2 112.0(4) . . . . ? S1 C1 C2 S2 -179.3(3) . . . . ? C3 S2 C2 C1 -101.5(5) . . . . ? C2 S2 C3 C4 65.0(6) . . . 2_576 ? C3 C4 C5 S1 175.4(5) 2_576 . . . ? C1 S1 C5 C4 73.1(5) . . . . ? Sn1 S1 C5 C4 -178.3(4) . . . . ? C10 S3 C6 C7 70.6(6) . . . . ? Sn2 S3 C6 C7 -173.2(4) . . . . ? S3 C6 C7 S4 179.9(4) . . . . ? C8 S4 C7 C6 178.7(5) . . . . ? C7 S4 C8 C9 -66.2(5) . . . 2_466 ? C8 C9 C10 S3 -176.1(5) 2_466 . . . ? C6 S3 C10 C9 46.2(6) . . . . ? Sn2 S3 C10 C9 -68.2(6) . . . . ? C15 S5 C11 C12 66.4(6) . . . . ? Sn3 S5 C11 C12 -178.7(5) . . . . ? S5 C11 C12 S6 58.0(6) . . . . ? C13 S6 C12 C11 179.5(5) . . . . ? C12 S6 C13 C14 179.2(5) . . . 2 ? C13 C14 C15 S5 60.5(7) 2 . . . ? C11 S5 C15 C14 -158.7(5) . . . . ? Sn3 S5 C15 C14 91.2(5) . . . . ? _diffrn_measured_fraction_theta_max 0.952 _diffrn_reflns_theta_full 27.53 _diffrn_measured_fraction_theta_full 0.952 _refine_diff_density_max 2.099 _refine_diff_density_min -2.172 _refine_diff_density_rms 0.227 #===END================================================================ data_[SnBr4([16]aneS4)] _database_code_CSD 208977 _chemical_name_common 1,5,9,13-tetrathiacyclohexadecane-tetrabromotin(IV) _audit_creation_method 'SHELXL-97 + hand edit' _chemical_name_systematic ; 1,5,9,13-tetrathiacyclohexadecane-tetrabromotin(IV) ; _chemical_melting_point ? _chemical_formula_moiety 'C12 H24 Br4 S4 Sn' _chemical_formula_sum 'C12 H24 Br4 S4 Sn' _chemical_formula_weight 734.88 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sn Sn -0.6537 1.4246 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P c a 21' _symmetry_Int_Tables_number 29 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-x+1/2, y, z+1/2' 'x+1/2, -y, z' _cell_length_a 19.4987(7) _cell_length_b 10.0624(3) _cell_length_c 10.9104(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2140.66(12) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 16449 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description block _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.280 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1400 _exptl_absorpt_coefficient_mu 9.042 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SORTAV, R H Blessing, J. Appl. Cryst., 1997, 30, 421-426.' _exptl_absorpt_correction_T_min 0.6117 # shelxl 0.4650 _exptl_absorpt_correction_T_max 0.8916 # shelxl 0.6130 _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 ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4590 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0537 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.91 _diffrn_reflns_theta_max 27.47 _reflns_number_total 4590 _reflns_number_gt 4105 _reflns_threshold_expression >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^)+(0.0850P)^2^+7.0400P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.520(16) _chemical_absolute_configuration unk _refine_ls_number_reflns 4590 _refine_ls_number_parameters 191 _refine_ls_number_restraints 7 _refine_ls_R_factor_all 0.0626 _refine_ls_R_factor_gt 0.0535 _refine_ls_wR_factor_ref 0.1380 _refine_ls_wR_factor_gt 0.1314 _refine_ls_goodness_of_fit_ref 1.039 _refine_ls_restrained_S_all 1.038 _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 0.38189(3) 0.99963(6) 0.82509(9) 0.01525(15) Uani 1 1 d . . . Br1 Br 0.33300(5) 1.14524(9) 0.99683(9) 0.0242(2) Uani 1 1 d . . . Br2 Br 0.32331(5) 1.14314(10) 0.66300(9) 0.0237(2) Uani 1 1 d . . . Br3 Br 0.42502(5) 0.83996(9) 0.65723(9) 0.0223(2) Uani 1 1 d . . . Br4 Br 0.44468(5) 0.86281(9) 0.98653(8) 0.0227(2) Uani 1 1 d . . . S1 S 0.27062(11) 0.8420(2) 0.8399(3) 0.0241(5) Uani 1 1 d . . . S2 S 0.18744(15) 0.4994(3) 0.9601(4) 0.0418(8) Uani 1 1 d . . . S3 S 0.05172(15) 0.5001(3) 0.6966(3) 0.0301(6) Uani 1 1 d . . . S4 S -0.00936(11) 0.8520(2) 0.7793(2) 0.0153(4) Uani 1 1 d . . . C1 C 0.2638(5) 0.7854(10) 1.0015(12) 0.035(3) Uani 1 1 d . . . H1 H 0.2842 0.8546 1.0547 0.046 Uiso 1 1 calc R . . H2 H 0.2145 0.7791 1.0228 0.046 Uiso 1 1 calc R . . C2 C 0.2969(7) 0.6558(10) 1.0311(13) 0.043(3) Uani 1 1 d . . . H3 H 0.2851 0.6325 1.1166 0.056 Uiso 1 1 calc R . . H4 H 0.3472 0.6682 1.0275 0.056 Uiso 1 1 calc R . . C3 C 0.2786(5) 0.5407(12) 0.9511(13) 0.040(3) Uani 1 1 d . . . H5 H 0.3060 0.4623 0.9761 0.052 Uiso 1 1 calc R . . H6 H 0.2906 0.5621 0.8652 0.052 Uiso 1 1 calc R . . C4 C 0.1868(6) 0.3867(11) 0.8314(14) 0.042(3) Uani 1 1 d . . . H7 H 0.1912 0.4383 0.7546 0.055 Uiso 1 1 calc R . . H8 H 0.2268 0.3265 0.8373 0.055 Uiso 1 1 calc R . . C5 C 0.1213(5) 0.3039(10) 0.8262(17) 0.037(2) Uani 1 1 d . . . H9 H 0.1205 0.2433 0.8977 0.048 Uiso 1 1 calc R . . H10 H 0.1225 0.2483 0.7514 0.048 Uiso 1 1 calc R . . C6 C 0.0547(5) 0.3855(9) 0.8257(12) 0.029(2) Uani 1 1 d . . . H11 H 0.0512 0.4364 0.9031 0.037 Uiso 1 1 calc R . . H12 H 0.0149 0.3245 0.8214 0.037 Uiso 1 1 calc R . . C7 C -0.0376(6) 0.5507(11) 0.7082(10) 0.032(2) Uani 1 1 d . . . H13 H -0.0464 0.6202 0.6460 0.041 Uiso 1 1 calc R . . H14 H -0.0669 0.4734 0.6878 0.041 Uiso 1 1 calc R . . C8 C -0.0592(5) 0.6036(9) 0.8326(10) 0.0253(19) Uani 1 1 d . . . H15 H -0.0602 0.5288 0.8914 0.033 Uiso 1 1 calc R . . H16 H -0.1064 0.6388 0.8259 0.033 Uiso 1 1 calc R . . C9 C -0.0124(5) 0.7139(8) 0.8848(9) 0.0189(18) Uani 1 1 d . . . H17 H 0.0344 0.6785 0.8978 0.025 Uiso 1 1 calc R . . H18 H -0.0305 0.7442 0.9649 0.025 Uiso 1 1 calc R . . C10 C 0.0657(4) 0.9453(10) 0.8261(11) 0.0235(19) Uani 1 1 d . . . H19 H 0.0694 1.0269 0.7759 0.031 Uiso 1 1 calc R . . H20 H 0.0608 0.9721 0.9130 0.031 Uiso 1 1 calc R . . C11 C 0.1307(4) 0.8618(9) 0.8108(11) 0.020(2) Uani 1 1 d U . . H21 H 0.1320 0.8237 0.7272 0.026 Uiso 1 1 calc R . . H22 H 0.1301 0.7874 0.8702 0.026 Uiso 1 1 calc R . . C12 C 0.1952(4) 0.9475(8) 0.8321(11) 0.0197(17) Uani 1 1 d . . . H23 H 0.1903 0.9979 0.9095 0.026 Uiso 1 1 calc R . . H24 H 0.2003 1.0120 0.7642 0.026 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 0.0097(2) 0.0220(3) 0.0141(3) -0.0011(2) -0.0007(3) 0.00029(18) Br1 0.0202(5) 0.0286(5) 0.0238(5) -0.0069(5) 0.0091(4) -0.0021(4) Br2 0.0163(4) 0.0301(6) 0.0247(5) 0.0034(5) -0.0066(4) 0.0032(3) Br3 0.0230(4) 0.0259(5) 0.0179(5) -0.0042(4) 0.0018(4) 0.0044(4) Br4 0.0160(4) 0.0351(6) 0.0168(5) 0.0063(4) -0.0010(4) -0.0002(4) S1 0.0098(10) 0.0258(12) 0.0366(14) -0.0052(11) -0.0008(10) -0.0001(8) S2 0.0221(14) 0.0350(17) 0.068(2) -0.0173(14) 0.0033(14) -0.0020(11) S3 0.0369(15) 0.0288(14) 0.0245(13) 0.0009(10) 0.0092(11) 0.0011(11) S4 0.0111(10) 0.0183(11) 0.0165(10) -0.0010(8) -0.0008(8) -0.0006(8) C1 0.016(4) 0.026(6) 0.065(8) 0.017(6) -0.005(5) -0.008(4) C2 0.042(7) 0.031(6) 0.057(8) 0.025(6) -0.018(6) -0.013(5) C3 0.014(5) 0.041(7) 0.064(9) 0.004(6) 0.011(5) 0.006(4) C4 0.036(6) 0.036(6) 0.055(7) 0.017(7) 0.011(7) 0.016(5) C5 0.041(6) 0.028(5) 0.043(6) 0.005(6) -0.003(7) -0.003(4) C6 0.035(6) 0.017(5) 0.034(5) 0.001(5) 0.002(5) -0.009(4) C7 0.035(6) 0.029(6) 0.031(6) -0.001(4) -0.010(5) -0.013(5) C8 0.024(5) 0.027(5) 0.025(5) -0.004(5) 0.000(5) 0.000(4) C9 0.022(5) 0.011(4) 0.023(5) -0.002(3) 0.000(4) 0.003(3) C10 0.011(4) 0.034(5) 0.025(5) 0.000(5) -0.006(4) 0.000(3) C11 0.004(3) 0.025(4) 0.030(6) -0.001(4) 0.004(3) 0.004(3) C12 0.011(4) 0.023(4) 0.026(5) 0.001(4) 0.004(4) 0.003(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 Sn1 Br4 2.5489(12) . ? Sn1 Br2 2.5528(13) . ? Sn1 Br1 2.5625(13) . ? Sn1 Br3 2.5774(12) . ? Sn1 S4 2.641(2) 4_575 ? Sn1 S1 2.693(2) . ? S1 C12 1.816(8) . ? S1 C1 1.857(13) . ? S2 C4 1.805(15) . ? S2 C3 1.828(11) . ? S3 C7 1.819(12) . ? S3 C6 1.822(11) . ? S4 C9 1.805(9) . ? S4 C10 1.811(9) . ? S4 Sn1 2.641(2) 4_475 ? C1 C2 1.491(14) . ? C1 H1 0.9900 . ? C1 H2 0.9900 . ? C2 C3 1.493(18) . ? C2 H3 0.9900 . ? C2 H4 0.9900 . ? C3 H5 0.9900 . ? C3 H6 0.9900 . ? C4 C5 1.526(15) . ? C4 H7 0.9900 . ? C4 H8 0.9900 . ? C5 C6 1.536(14) . ? C5 H9 0.9900 . ? C5 H10 0.9900 . ? C6 H11 0.9900 . ? C6 H12 0.9900 . ? C7 C8 1.517(15) . ? C7 H13 0.9900 . ? C7 H14 0.9900 . ? C8 C9 1.545(13) . ? C8 H15 0.9900 . ? C8 H16 0.9900 . ? C9 H17 0.9900 . ? C9 H18 0.9900 . ? C10 C11 1.530(11) . ? C10 H19 0.9900 . ? C10 H20 0.9900 . ? C11 C12 1.542(12) . ? C11 H21 0.9900 . ? C11 H22 0.9900 . ? C12 H23 0.9900 . ? C12 H24 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 Br4 Sn1 Br2 177.61(4) . . ? Br4 Sn1 Br1 88.98(5) . . ? Br2 Sn1 Br1 90.96(3) . . ? Br4 Sn1 Br3 89.86(3) . . ? Br2 Sn1 Br3 90.36(5) . . ? Br1 Sn1 Br3 175.87(4) . . ? Br4 Sn1 S4 92.88(5) . 4_575 ? Br2 Sn1 S4 84.75(6) . 4_575 ? Br1 Sn1 S4 96.53(6) . 4_575 ? Br3 Sn1 S4 87.48(6) . 4_575 ? Br4 Sn1 S1 91.56(7) . . ? Br2 Sn1 S1 90.83(7) . . ? Br1 Sn1 S1 89.61(7) . . ? Br3 Sn1 S1 86.47(7) . . ? S4 Sn1 S1 172.48(10) 4_575 . ? C12 S1 C1 99.5(5) . . ? C12 S1 Sn1 107.8(3) . . ? C1 S1 Sn1 107.2(3) . . ? C4 S2 C3 96.2(6) . . ? C7 S3 C6 98.8(5) . . ? C9 S4 C10 104.2(5) . . ? C9 S4 Sn1 106.7(3) . 4_475 ? C10 S4 Sn1 107.6(3) . 4_475 ? C2 C1 S1 116.2(10) . . ? C2 C1 H1 108.2 . . ? S1 C1 H1 108.2 . . ? C2 C1 H2 108.2 . . ? S1 C1 H2 108.2 . . ? H1 C1 H2 107.4 . . ? C1 C2 C3 116.7(11) . . ? C1 C2 H3 108.1 . . ? C3 C2 H3 108.1 . . ? C1 C2 H4 108.1 . . ? C3 C2 H4 108.1 . . ? H3 C2 H4 107.3 . . ? C2 C3 S2 112.2(9) . . ? C2 C3 H5 109.2 . . ? S2 C3 H5 109.2 . . ? C2 C3 H6 109.2 . . ? S2 C3 H6 109.2 . . ? H5 C3 H6 107.9 . . ? C5 C4 S2 112.2(10) . . ? C5 C4 H7 109.2 . . ? S2 C4 H7 109.2 . . ? C5 C4 H8 109.2 . . ? S2 C4 H8 109.2 . . ? H7 C4 H8 107.9 . . ? C4 C5 C6 114.6(8) . . ? C4 C5 H9 108.6 . . ? C6 C5 H9 108.6 . . ? C4 C5 H10 108.6 . . ? C6 C5 H10 108.6 . . ? H9 C5 H10 107.6 . . ? C5 C6 S3 111.6(9) . . ? C5 C6 H11 109.3 . . ? S3 C6 H11 109.3 . . ? C5 C6 H12 109.3 . . ? S3 C6 H12 109.3 . . ? H11 C6 H12 108.0 . . ? C8 C7 S3 115.2(7) . . ? C8 C7 H13 108.5 . . ? S3 C7 H13 108.5 . . ? C8 C7 H14 108.5 . . ? S3 C7 H14 108.5 . . ? H13 C7 H14 107.5 . . ? C7 C8 C9 114.8(8) . . ? C7 C8 H15 108.6 . . ? C9 C8 H15 108.6 . . ? C7 C8 H16 108.6 . . ? C9 C8 H16 108.6 . . ? H15 C8 H16 107.6 . . ? C8 C9 S4 109.7(7) . . ? C8 C9 H17 109.7 . . ? S4 C9 H17 109.7 . . ? C8 C9 H18 109.7 . . ? S4 C9 H18 109.7 . . ? H17 C9 H18 108.2 . . ? C11 C10 S4 110.8(6) . . ? C11 C10 H19 109.5 . . ? S4 C10 H19 109.5 . . ? C11 C10 H20 109.5 . . ? S4 C10 H20 109.5 . . ? H19 C10 H20 108.1 . . ? C10 C11 C12 110.7(7) . . ? C10 C11 H21 109.5 . . ? C12 C11 H21 109.5 . . ? C10 C11 H22 109.5 . . ? C12 C11 H22 109.5 . . ? H21 C11 H22 108.1 . . ? C11 C12 S1 109.9(6) . . ? C11 C12 H23 109.7 . . ? S1 C12 H23 109.7 . . ? C11 C12 H24 109.7 . . ? S1 C12 H24 109.7 . . ? H23 C12 H24 108.2 . . ? 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 Br4 Sn1 S1 C12 140.0(4) . . . . ? Br2 Sn1 S1 C12 -39.9(4) . . . . ? Br1 Sn1 S1 C12 51.0(4) . . . . ? Br3 Sn1 S1 C12 -130.2(4) . . . . ? Br4 Sn1 S1 C1 33.7(4) . . . . ? Br2 Sn1 S1 C1 -146.3(4) . . . . ? Br1 Sn1 S1 C1 -55.3(4) . . . . ? Br3 Sn1 S1 C1 123.4(4) . . . . ? C12 S1 C1 C2 154.7(8) . . . . ? Sn1 S1 C1 C2 -93.2(8) . . . . ? S1 C1 C2 C3 -51.6(13) . . . . ? C1 C2 C3 S2 -62.6(14) . . . . ? C4 S2 C3 C2 168.7(9) . . . . ? C3 S2 C4 C5 166.5(9) . . . . ? S2 C4 C5 C6 54.9(16) . . . . ? C4 C5 C6 S3 58.4(16) . . . . ? C7 S3 C6 C5 169.1(8) . . . . ? C6 S3 C7 C8 53.9(9) . . . . ? S3 C7 C8 C9 51.1(11) . . . . ? C7 C8 C9 S4 58.2(10) . . . . ? C10 S4 C9 C8 -162.3(6) . . . . ? Sn1 S4 C9 C8 84.0(6) 4_475 . . . ? C9 S4 C10 C11 62.9(9) . . . . ? Sn1 S4 C10 C11 176.0(7) 4_475 . . . ? S4 C10 C11 C12 171.5(7) . . . . ? C10 C11 C12 S1 170.2(7) . . . . ? C1 S1 C12 C11 -81.1(9) . . . . ? Sn1 S1 C12 C11 167.3(7) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.47 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.664 _refine_diff_density_min -1.409 _refine_diff_density_rms 0.269 #===END=============================================================== # # 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 ======================================================