#------------------------------------------------------------------------------ #$Date: 2016-02-19 14:29:56 +0000 (Fri, 19 Feb 2016) $ #$Revision: 176759 $ #$URL: svn://www.crystallography.net/cod/cif/2/00/50/2005096.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_2005096 loop_ _publ_author_name 'Genge, A. R. J.' 'Levason, W.' 'Reid, G.' _publ_section_title ; Redetermination of [(\m-OEt)~2~{SnCl~3~(EtOH)}~2~] ; _journal_issue 7 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first 1666 _journal_page_last 1668 _journal_paper_doi 10.1107/S0108270196002909 _journal_volume 52 _journal_year 1996 _chemical_formula_iupac '[Sn2 Cl6 (C2 H5 O1)2 (C2 H6 O1)2]' _chemical_formula_moiety 'C8 H22 Cl6 O4 Sn2' _chemical_formula_structural (\m~2~-OEt)~2~[SnCl~3~(EtOH)]~2~ _chemical_formula_sum 'C8 H22 Cl6 O4 Sn2' _chemical_formula_weight 632.36 _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' _audit_creation_method 'from TEXRAY.INF file' _cell_angle_alpha 90 _cell_angle_beta 107.08(2) _cell_angle_gamma 90 _cell_formula_units_Z 2 _cell_length_a 9.653(3) _cell_length_b 7.472(3) _cell_length_c 14.627(2) _cell_measurement_reflns_used 25 _cell_measurement_temperature 150.0 _cell_measurement_theta_max 20.85 _cell_measurement_theta_min 15.55 _cell_volume 1008.5(5) _computing_cell_refinement 'MSC/AFC Diffractometer Control Software' _computing_data_collection ; MSC/AFC Diffractometer Control Software (Molecular Structure Corporation, 1988) ; _computing_data_reduction 'TEXSAN (Molecular Structure Corporation, 1995)' _computing_publication_material TEXSAN _computing_structure_refinement TEXSAN _computing_structure_solution 'SHELXS86 (Sheldrick, 1985)' _diffrn_ambient_temperature 150.0 _diffrn_measurement_device 'Rigaku AFC-7S' _diffrn_measurement_method \w/2\q _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'X-ray tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.021 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_number 2043 _diffrn_reflns_theta_max 24.97 _diffrn_standards_decay_% none _diffrn_standards_interval_count 150 _diffrn_standards_number 3 _exptl_absorpt_coefficient_mu 3.276 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.749 _exptl_absorpt_correction_type 'empirical via \y scan (North, Phillips & Mathews, 1968)' _exptl_absorpt_process_details psi-scan _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 2.082 _exptl_crystal_density_meas ? _exptl_crystal_description 'plate-like needle' _exptl_crystal_F_000 608 _exptl_crystal_size_max 0.70 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _refine_diff_density_max 0.66 _refine_diff_density_min -0.78 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_all 1.28 _refine_ls_goodness_of_fit_obs 1.32 _refine_ls_hydrogen_treatment noref _refine_ls_matrix_type full _refine_ls_number_parameters 91 _refine_ls_number_reflns 1428 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0394 _refine_ls_R_factor_obs 0.0247 _refine_ls_shift/esd_max <0.0001 _refine_ls_structure_factor_coef F _refine_ls_weighting_scheme 'sigma; w= 1/\s^2^(F)' _refine_ls_wR_factor_all 0.0315 _refine_ls_wR_factor_obs 0.0291 _reflns_number_observed 1428 _reflns_number_total 1925 _reflns_observed_criterion I>3\s(I) _cod_data_source_file bm1062.cif _cod_data_source_block AGSn3 _cod_depositor_comments ; The following automatic conversions were performed: '_exptl_crystal_density_meas' value 'not measured' was changed to '?' - the value is perceived as not measured. Automatic conversion script Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas ; _cod_original_sg_symbol_H-M 'P 21/n' _cod_database_code 2005096 loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' 1/2-x,1/2+y,1/2-z ' -x, -y, -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(1) 0.0184(2) 0.0214(2) 0.0152(2) 0.00060(10) 0.00370(10) 0.00120(10) Cl(1) 0.0328(6) 0.0321(7) 0.0166(5) -0.0006(5) 0.0029(5) -0.0011(5) Cl(2) 0.0365(7) 0.0214(6) 0.0254(6) 0.0049(5) 0.0100(5) 0.0038(5) Cl(3) 0.0249(6) 0.0421(8) 0.0296(6) -0.0053(6) 0.0122(5) 0.0014(6) O(1) 0.035(2) 0.028(2) 0.027(2) 0.013(2) 0.016(2) 0.0060(10) O(2) 0.018(2) 0.022(2) 0.0150(10) -0.0050(10) 0.0010(10) -0.0010(10) C(1) 0.037(3) 0.027(3) 0.031(3) -0.003(2) 0.019(2) -0.005(2) C(2) 0.033(3) 0.049(4) 0.050(3) 0.011(3) 0.016(3) -0.001(3) C(3) 0.024(2) 0.028(3) 0.019(2) -0.007(2) 0.006(2) -0.003(2) C(4) 0.020(2) 0.039(3) 0.032(3) 0.000(2) -0.002(2) -0.009(2) loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type Sn(1) .54473(3) .05148(4) .89943(2) .01863(9) Uij Cl(1) .43040(10) -.0177(2) .73860(8) .0281(3) Uij Cl(2) .44600(10) .3461(2) .89678(8) .0276(3) Uij Cl(3) .76800(10) .1417(2) .88063(8) .0313(3) Uij O(1) .6238(4) -0.2211(5) .9172(2) .0286(9) Uij O(2) .6164(3) .0576(4) 1.0490(2) .0194(8) Uij C(1) .7100(6) -0.3169(7) .8662(3) .0300(10) Uij C(2) .8524(6) -0.3712(9) .9331(4) .043(2) Uij C(3) .7432(5) .1563(7) 1.1058(3) .0240(10) Uij C(4) .8710(5) .0337(8) 1.1409(4) .0320(10) Uij H(1) .5967 -0.2881 .9706 .0382 Uiso H(2) .7261 -0.2412 .8181 .0357 Uiso H(3) .6588 -0.4207 .8372 .0357 Uiso H(4) .9039 -0.2677 .9623 .0520 Uiso H(5) .8367 -0.4476 .9811 .0520 Uiso H(6) .9072 -0.4330 .8987 .0520 Uiso H(7) .7217 .2092 1.1591 .0287 Uiso H(8) .7663 .2475 1.0673 .0287 Uiso H(9) .9522 .1001 1.1776 .0388 Uiso H(10) .8485 -0.0576 1.1795 .0388 Uiso H(11) .8931 -0.0192 1.0878 .0388 Uiso loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C 0.003 0.002 'International Tables' H 0.000 0.000 'International Tables' Cl 0.148 0.159 'International Tables' O 0.011 0.006 'International Tables' Sn -0.654 1.425 'International Tables' loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 3 -3 -1 2 -3 1 1 -3 3 loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag Cl(1) Sn(1) Cl(2) ? ? 96.80(4) yes Cl(1) Sn(1) Cl(3) ? ? 97.10(4) yes Cl(1) Sn(1) O(1) ? ? 87.63(9) yes Cl(1) Sn(1) O(2) ? ? 165.43(9) yes Cl(1) Sn(1) O(2) ? 3_657 95.49(8) yes Cl(2) Sn(1) Cl(3) ? ? 96.22(5) yes Cl(2) Sn(1) O(1) ? ? 172.73(9) yes Cl(2) Sn(1) O(2) ? ? 90.27(9) yes Cl(2) Sn(1) O(2) ? 3_657 91.71(9) yes Cl(3) Sn(1) O(1) ? ? 88.91(10) yes Cl(3) Sn(1) O(2) ? ? 94.76(9) yes Cl(3) Sn(1) O(2) ? 3_657 164.21(8) yes O(1) Sn(1) O(2) ? ? 84.16(12) yes O(1) Sn(1) O(2) ? 3_657 82.11(12) yes O(2) Sn(1) O(2) ? 3_657 71.50(12) yes Sn(1) O(1) C(1) ? ? 129.4(3) yes Sn(1) O(2) Sn(1) ? 3_657 108.50(12) yes Sn(1) O(2) C(3) ? ? 124.8(2) yes Sn(1) O(2) C(3) 3_657 ? 125.5(2) yes O(1) C(1) C(2) ? ? 110.6(4) yes O(2) C(3) C(4) ? ? 110.7(4) yes 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(1) Cl(1) ? 2.3441(11) yes Sn(1) Cl(2) ? 2.3947(12) yes Sn(1) Cl(3) ? 2.3504(14) yes Sn(1) O(1) ? 2.164(3) yes Sn(1) O(2) ? 2.092(3) yes Sn(1) O(2) 3_657 2.084(3) yes O(1) C(1) ? 1.459(6) yes O(2) C(3) ? 1.461(5) yes C(1) C(2) ? 1.491(7) yes C(3) C(4) ? 1.501(7) yes