#------------------------------------------------------------------------------ #$Date: 2013-12-28 15:58:47 +0200 (Sat, 28 Dec 2013) $ #$Revision: 91933 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/01/39/2013998.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_2013998 loop_ _publ_author_name 'Genge, Anthony R. J.' 'Levason, William' 'Patel, Rina' 'Reid, Gillian' 'Webster, Michael' _publ_section_title ; Hydrates of tin tetrachloride ; _journal_issue 4 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first i47 _journal_page_last i49 _journal_volume 60 _journal_year 2004 _chemical_formula_iupac '[Sn Cl4 (H2 O1)2], H2 O' _chemical_formula_moiety 'Cl4 H4 O2 Sn, H2 O' _chemical_formula_sum 'Cl4 H6 O3 Sn' _chemical_formula_weight 314.54 _chemical_name_systematic ; Tetrachlorodiaquatin(IV) monohydrate ; _space_group_IT_number 14 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_space_group_name_H-M 'P 1 21/c 1' _atom_sites_solution_hydrogens difmap _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method 'SHELXL-97 + hand edit' _cell_angle_alpha 90.00 _cell_angle_beta 90.22(2) _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 6.362(3) _cell_length_b 11.071(4) _cell_length_c 11.895(4) _cell_measurement_reflns_used 25 _cell_measurement_temperature 150(2) _cell_measurement_theta_max 24.9 _cell_measurement_theta_min 23.0 _cell_volume 837.8(6) _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS97 (Sheldrick, 1997)' _diffrn_ambient_temperature 150(2) _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.998 _diffrn_measurement_device_type 'Rigaku AFC-7S' _diffrn_measurement_method \w/2\q _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus Mo sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0106 _diffrn_reflns_av_sigmaI/netI 0.0217 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_number 1549 _diffrn_reflns_theta_full 25.00 _diffrn_reflns_theta_max 25.00 _diffrn_reflns_theta_min 2.51 _diffrn_standards_decay_% 0 _diffrn_standards_interval_count 200 _diffrn_standards_number 3 _exptl_absorpt_coefficient_mu 4.260 _exptl_absorpt_correction_T_max 0.427 _exptl_absorpt_correction_T_min 0.268 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_process_details '(North et al., 1968)' _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 2.494 _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 592 _exptl_crystal_size_max 0.48 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.20 _refine_diff_density_max 0.834 _refine_diff_density_min -2.440 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.074 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 92 _refine_ls_number_reflns 1475 _refine_ls_number_restraints 7 _refine_ls_restrained_S_all 1.071 _refine_ls_R_factor_all 0.0318 _refine_ls_R_factor_gt 0.0286 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^)+(0.0569P)^2^+1.1933P] where P = (Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0793 _refine_ls_wR_factor_ref 0.0815 _reflns_number_gt 1356 _reflns_number_total 1475 _reflns_threshold_expression I>2\s(I) _[local]_cod_data_source_file gd1307.cif _[local]_cod_data_source_block I _[local]_cod_cif_authors_sg_H-M 'P 21/c' _cod_database_code 2013998 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' loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_refinement_flags _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_type_symbol Sn1 0.36858(4) 0.23528(3) 0.66346(2) 0.01350(15) Uani d . 1 . . Sn Cl1 0.23914(17) 0.09273(10) 0.53026(9) 0.0210(3) Uani d . 1 . . Cl Cl2 0.69212(16) 0.13053(9) 0.68652(9) 0.0179(2) Uani d . 1 . . Cl Cl3 0.21634(17) 0.13467(10) 0.82238(9) 0.0199(3) Uani d . 1 . . Cl Cl4 0.09960(18) 0.37715(10) 0.64014(10) 0.0238(3) Uani d . 1 . . Cl O1 0.5134(5) 0.3672(3) 0.7697(3) 0.0198(7) Uani d D 1 . . O O2 0.5277(5) 0.3335(3) 0.5309(3) 0.0209(7) Uani d D 1 . . O O3 0.8115(5) 0.2091(3) 0.4126(3) 0.0238(7) Uani d D 1 . . O H1 0.582(9) 0.353(7) 0.827(3) 0.057(9) Uiso d D 1 . . H H2 0.446(10) 0.425(4) 0.797(5) 0.057(9) Uiso d D 1 . . H H3 0.450(10) 0.350(7) 0.475(4) 0.057(9) Uiso d D 1 . . H H4 0.603(10) 0.289(6) 0.492(5) 0.057(9) Uiso d D 1 . . H H5 0.884(9) 0.242(6) 0.362(4) 0.057(9) Uiso d D 1 . . H H6 0.876(10) 0.161(5) 0.454(5) 0.057(9) Uiso d D 1 . . H 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 Sn1 0.0129(2) 0.0107(2) 0.0169(2) 0.00045(10) -0.00213(13) -0.00132(10) Cl1 0.0221(6) 0.0173(5) 0.0235(6) 0.0010(4) -0.0064(4) -0.0064(4) Cl2 0.0145(5) 0.0143(5) 0.0248(5) 0.0022(4) -0.0031(4) -0.0007(4) Cl3 0.0184(5) 0.0205(6) 0.0209(5) -0.0029(4) 0.0003(4) 0.0002(4) Cl4 0.0191(6) 0.0182(5) 0.0339(6) 0.0073(4) -0.0045(4) -0.0025(5) O1 0.0218(17) 0.0121(15) 0.0254(17) 0.0012(12) -0.0075(13) -0.0062(13) O2 0.0195(17) 0.0211(17) 0.0222(17) -0.0014(13) -0.0008(13) 0.0035(13) O3 0.0185(17) 0.0308(18) 0.0221(17) 0.0008(15) -0.0024(13) 0.0070(15) 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 Sn1 Cl1 . 2.3810(12) ? Sn1 Cl2 . 2.3775(13) ? Sn1 Cl3 . 2.4013(13) ? Sn1 Cl4 . 2.3384(12) ? Sn1 O1 . 2.138(3) ? Sn1 O2 . 2.169(3) ? O1 H1 . 0.82(2) ? O1 H2 . 0.84(5) ? O2 H3 . 0.85(5) ? O2 H4 . 0.83(6) ? O3 H5 . 0.84(6) ? O3 H6 . 0.83(6) ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sn Sn -0.6537 1.4246 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle O1 Sn1 O2 83.46(13) O1 Sn1 Cl4 85.69(9) O2 Sn1 Cl4 85.43(10) O1 Sn1 Cl3 91.47(10) O2 Sn1 Cl3 174.56(9) O1 Sn1 Cl2 83.92(9) O2 Sn1 Cl2 85.55(9) O1 Sn1 Cl1 173.42(10) O2 Sn1 Cl1 90.56(9) Cl4 Sn1 Cl2 166.94(4) Cl4 Sn1 Cl1 96.61(5) Cl2 Sn1 Cl1 92.90(4) Cl4 Sn1 Cl3 96.19(5) Cl2 Sn1 Cl3 91.98(4) Cl1 Sn1 Cl3 94.41(5) Sn1 O1 H1 126(6) Sn1 O1 H2 122(5) H1 O1 H2 96(6) Sn1 O2 H3 114(5) Sn1 O2 H4 112(5) H3 O2 H4 91(7) H5 O3 H6 115(7) loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_publ_flag O1 H1 O3 4_566 0.82(2) 1.91(3) 2.678(5) 156(6) y O1 H2 Cl2 2_656 0.84(5) 2.44(3) 3.238(3) 158(6) y O2 H3 Cl3 4_565 0.85(5) 2.35(6) 3.188(4) 172(7) y O2 H4 O3 . 0.83(6) 1.85(3) 2.675(5) 169(8) y O3 H5 Cl3 4_665 0.84(6) 2.56(4) 3.286(4) 144(5) y O3 H5 Cl2 4_565 0.84(6) 2.80(6) 3.309(4) 121(5) y O3 H6 Cl1 1_655 0.83(6) 2.59(5) 3.315(4) 146(7) y O3 H6 Cl1 3_656 0.83(6) 2.91(6) 3.425(4) 122(6) y _cod_database_fobs_code 2013998 _journal_paper_doi 10.1107/S0108270104005633