#------------------------------------------------------------------------------ #$Date: 2015-04-02 12:22:18 +0100 (Thu, 02 Apr 2015) $ #$Revision: 134621 $ #$URL: svn://www.crystallography.net/cod/cif/2/00/51/2005144.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/. The original data for this entry # were provided by IUCr Journals, http://journals.iucr.org/. # # The file may be used within the scientific community so long as # proper attribution is given to the journal article from which the # data were obtained. # data_2005144 loop_ _publ_author_name 'Carvalho, C. C.' 'Francisco, R. H. P.' 'do Gambardella, M. T.' 'de Sousa, G. F.' 'Filgueiras, C. A. L.' _publ_section_title catena-Poly[cis-dichloro-trans-dimethyltin(IV)-\m-meso-1,2-bis(propylsulfinyl)ethane-O:O'] _journal_issue 7 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first 1627 _journal_page_last 1629 _journal_paper_doi 10.1107/S0108270196002090 _journal_volume 52 _journal_year 1996 _chemical_formula_iupac '[Sn1 Cl2 (C1 H3)2 (C8 H18 O2 S2)]~n~' _chemical_formula_moiety 'C10 H24 Cl2 O2 S2 Sn' _chemical_formula_structural '[Sn(CH~3~)~2~Cl~2~(C~3~H~7~SOCH~2~)~2~]~n~' _chemical_formula_sum 'C10 H24 Cl2 O2 S2 Sn' _chemical_formula_weight 430.03 _chemical_melting_point 361 _chemical_name_systematic '[Cis-dichloro-trans-dimethyl-\m-(meso-1,2-bis(n-propilsulfinyl)ethane)tin(IV)]' _space_group_IT_number 14 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-P 2yn' _symmetry_space_group_name_H-M 'P 1 21/n 1' _cell_angle_alpha 90 _cell_angle_beta 104.151(6) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 10.4375(7) _cell_length_b 15.8350(10) _cell_length_c 11.0997(8) _cell_measurement_reflns_used 25 _cell_measurement_temperature 298 _cell_measurement_theta_max 18.10 _cell_measurement_theta_min 10.00 _cell_volume 1778.9(2) _computing_cell_refinement 'CAD-4 Software' _computing_data_collection 'CAD-4 Software (Enraf-Nonius, 1989)' _computing_data_reduction 'SDP (Frenz, 1978)' _computing_molecular_graphics 'ORTEP (Johnson, 1965)' _computing_publication_material 'DOS 6.0, VAX editor' _computing_structure_refinement 'SHELXL93 (Sheldrick, 1993)' _computing_structure_solution 'SHELXS86 (Sheldrick, 1985)' _diffrn_ambient_temperature 298 _diffrn_measurement_device 'Enraf-Nonius CAD-4' _diffrn_measurement_method \w/2\q _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed CAD-4' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.7107 _diffrn_reflns_av_R_equivalents .0201 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_number 3788 _diffrn_reflns_theta_max 26.3 _diffrn_reflns_theta_min 2.5 _diffrn_standards_decay_% 2.1 _diffrn_standards_interval_time 120 _diffrn_standards_number 3 _exptl_absorpt_coefficient_mu 1.962 _exptl_absorpt_correction_T_max 0.9996 _exptl_absorpt_correction_T_min 0.6131 _exptl_absorpt_correction_type 'empirical via \y scan (North, Phillips & Mathews, 1968)' _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 1.606 _exptl_crystal_description prismatic _exptl_crystal_F_000 864 _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.15 _refine_diff_density_max 1.52 _refine_diff_density_min -0.82 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_obs 1.098 _refine_ls_hydrogen_treatment 'H atoms refined as riding atoms' _refine_ls_matrix_type full _refine_ls_number_constraints 0 _refine_ls_number_parameters 167 _refine_ls_number_reflns 3030 _refine_ls_number_restraints 0 _refine_ls_R_factor_obs 0.0325 _refine_ls_shift/esd_max 0.001 _refine_ls_shift/esd_mean 0.001 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_scheme ; w = 1/[\s^2^(F~o~^2^) + (0.0573P)^2^ + 1.8856P] where P = (F~o~^2^ + 2F~c~^2^)/3 ; _refine_ls_wR_factor_obs 0.0927 _reflns_number_observed 3038 _reflns_number_total 3598 _reflns_observed_criterion >3\s(F) _[local]_cod_data_source_file kh1065.cif _[local]_cod_data_source_block Sn _[local]_cod_cif_authors_sg_H-M 'P 21/n' _[local]_cod_chemical_formula_sum_orig 'C10 H24 Cl2 O2 S2 Sn1' _cod_original_cell_volume 1778.86(2) _cod_database_code 2005144 loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z 1/2-x,1/2+y,1/2-z 1/2+x,1/2-y,1/2+z loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Sn 0.0353(2) 0.0343(2) 0.0411(2) 0.00288(9) 0.01270(10) -0.00172(9) Cl1 0.0414(5) 0.0674(7) 0.0888(9) 0.0125(5) 0.0272(5) 0.0012(6) Cl2 0.0889(9) 0.0585(7) 0.0635(7) 0.0150(6) 0.0259(6) 0.0215(6) O1 0.0430(10) 0.051(2) 0.074(2) 0.0010(10) 0.0316(2) -0.0010(10) S1 0.0445(5) 0.0519(6) 0.0530(6) -0.0021(4) 0.0221(4) 0.0012(4) C1 0.063(3) 0.058(3) 0.055(3) -0.008(2) 0.011(2) -0.016(2) C2 0.061(3) 0.049(3) 0.055(3) -0.008(2) 0.013(2) -0.013(2) C3 0.054(2) 0.045(2) 0.051(2) 0.003(2) 0.026(2) 0.003(2) C4 0.040(2) 0.063(3) 0.052(2) 0.002(2) 0.019(2) 0.005(2) C5 0.047(2) 0.073(3) 0.057(3) 0.003(2) 0.017(2) 0.014(3) C6 0.076(3) 0.097(5) 0.079(4) 0.032(3) 0.033(3) 0.008(3) C7 0.103(5) 0.097(5) 0.123(6) 0.052(4) 0.053(4) 0.036(4) O2 0.055(2) 0.0380(10) 0.049(2) 0.0040(10) 0.0180(10) 0.00470(10) S2 0.0475(5) 0.0404(5) 0.0455(5) -0.0007(4) 0.0185(4) -0.0035(4) C8 0.069(3) 0.038(2) 0.062(3) 0.012(2) 0.032(2) 0.002(2) C9 0.103(4) 0.060(3) 0.075(3) 0.024(3) 0.051(3) 0.005(3) C10 0.102(4) 0.058(3) 0.085(4) 0.012(3) 0.050(3) -0.013(3) loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv Sn .16188(2) .200670(10) .38845(2) .03630(10) Cl1 .38260(10) .17381(8) .34140(10) .0639(3) Cl2 .17640(10) .08925(8) .55270(10) .0691(3) O1 -.0363(3) .2487(2) .4224(3) .0529(7) S1 -0.16480(10) .199130(10) .40400(10) .0480(3) C1 .2429(5) .2952(3) .5187(5) .0590(10) C2 .0602(5) .1177(3) .2486(4) .0550(10) C3 .2083(4) .3828(3) .0603(4) .0476(9) C4 -0.1701(4) .1696(3) .5591(4) .0500(10) C5 -0.2929(5) .2772(3) .3646(5) .0580(10) C6 -0.2850(6) .3486(4) .4530(6) .081(2) C7 -0.3910(8) .4145(5) .4017(8) .103(2) O2 .1234(3) .2970(2) .2266(3) .0463(6) S2 .18190(10) .38357(6) .21418(9) .0432(2) C8 .0457(5) .4549(3) .1895(4) .0540(10) C9 .0073(7) .4680(3) .3130(6) .074(2) C10 -.0968(7) .5346(4) .3039(6) .077(2) H1A .3164 .2572 .5806 ? H1B .1812 .3258 .5708 ? H1C .2914 .3425 .4753 ? H2A -0.0112 .0815 .2828 ? H2B .1286 .0752 .2206 ? H2C .0098 .1550 .1699 ? H3A .1317 .3590 .0025 ? H3B .2204 .4401 .0343 ? H4A -0.0915 .1374 .5969 ? H4B -0.1702 .2202 .6084 ? H5A -0.2922 .3004 .2838 ? H5B -0.3772 .2492 .3564 ? H6A -0.1984 .3746 .4678 ? H6B -0.2965 .3274 .5317 ? H7A -0.3768 .4662 .4671 ? H7B -0.4895 .3893 .3896 ? H7C -0.3782 .4368 .3135 ? H8A .0699 .5085 .1590 ? H8B -0.0286 .4319 .1281 ? H9A -0.0251 .4151 .3384 ? H9B .0852 .4841 .3764 ? H10A -0.1251 .5421 .3905 ? H10B -0.1768 .5055 .2362 ? H10C -0.0751 .5957 .2704 ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C .002 .002 International_Tables_Vol_IV_Table_2.3.1 H H .000 .000 International_Tables_Vol_IV_Table_2.3.1 Cl Cl .132 1.159 International_Tables_Vol_IV_Table_2.3.1 O O .008 .006 International_Tables_Vol_IV_Table_2.3.1 S S .110 .124 International_Tables_Vol_IV_Table_2.3.1 Sn Sn -0.873 1.424 International_Tables_Vol_IV_Table_2.3.1 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 4 -5 -3 2 -3 -4 -6 -10 0 loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag Cl1 Sn Cl2 . 97.80(5) yes Cl1 Sn O1 . 170.37(8) yes Cl1 Sn O2 . 86.82(8) yes Cl1 Sn C1 . 91.6(2) yes Cl1 Sn C2 . 93.60(10) yes Cl2 Sn O1 . 90.58(8) yes Cl2 Sn O2 . 173.13(8) yes Cl2 Sn C1 . 93.3(2) yes Cl2 Sn C2 . 91.50(10) yes O1 Sn O2 . 85.30(10) yes O1 Sn C1 . 83.1(2) yes O1 Sn C2 . 90.9(2) yes O2 Sn C1 . 91.6(2) yes O2 Sn C2 . 83.1(2) yes C1 Sn C2 . 172.3(2) yes Sn O1 S1 . 126.9(2) yes O1 S1 C5 . 104.9(2) yes O1 S1 C4 . 103.8(2) yes C5 S1 C4 . 102.6(2) yes S1 C4 C3 4_455 111.8(3) yes Sn O2 S2 . 131.9(2) yes O2 S2 C8 . 105.2(2) yes O2 S2 C3 . 103.8(2) yes C8 S2 C3 . 99.2(2) yes S2 C3 C4 4_554 109.5(3) yes S1 C5 C6 . 116.2(4) no C5 C6 C7 . 110.8(6) no S2 C8 C9 . 108.7(3) no C8 C9 C10 . 112.2(5) no loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Sn Cl1 . 2.5200(10) yes Sn Cl2 . 2.5150(10) yes Sn O1 . 2.320(3) yes Sn O2 . 2.316(3) yes Sn C1 . 2.110(4) yes Sn C2 . 2.111(4) yes O1 S1 . 1.523(3) yes S1 C5 . 1.795(5) yes S1 C4 . 1.798(4) yes C4 C3 4_455 1.519(6) yes O2 S2 . 1.520(3) yes S2 C8 . 1.783(4) yes S2 C3 . 1.796(4) yes C3 C4 4_554 1.519(6) yes C5 C6 . 1.486(8) no C9 C10 . 1.500(7) no C8 C9 . 1.533(6) no C6 C7 . 1.526(8) no