#------------------------------------------------------------------------------ #$Date: 2012-02-03 19:16:24 +0200 (Fri, 03 Feb 2012) $ #$Revision: 32112 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/01/26/2012642.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_2012642 loop_ _publ_author_name 'Reuter, Hans' 'Eickmeier, Henning' 'Puff, Heinrich' 'Beckermann, Norbert' 'H\"anssgen, Dieter' _publ_section_title ; Tin--halide compounds. IV. tert-Butyltrichlorotin(IV) ; _journal_issue 4 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first m217 _journal_page_last m218 _journal_volume 58 _journal_year 2002 _chemical_formula_iupac '[Sn (C4 H9) Cl3]' _chemical_formula_moiety 'C4 H9 Cl3 Sn' _chemical_formula_sum 'C4 H9 Cl3 Sn' _chemical_formula_weight 282.15 _chemical_name_common tert-Butyltrichlorotin(IV) _chemical_name_systematic ; tert-Butyltrichlorotin(IV) ; _space_group_IT_number 11 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-P 2yb' _symmetry_space_group_name_H-M 'P 1 21/m 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL97 _cell_angle_alpha 90 _cell_angle_beta 112.77(4) _cell_angle_gamma 90 _cell_formula_units_Z 2 _cell_length_a 7.632(4) _cell_length_b 10.341(5) _cell_length_c 6.289(5) _cell_measurement_reflns_used 25 _cell_measurement_temperature 203(2) _cell_measurement_theta_max 20.33 _cell_measurement_theta_min 9.14 _cell_volume 457.7(5) _computing_cell_refinement 'CAD-4 Operations Manual' _computing_data_collection 'CAD-4 Operations Manual (Enraf-Nonius, 1977)' _computing_data_reduction 'CADSHEL (Kopf & Ruebcke, 1987)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 1997)' _computing_publication_material SHELXL97 _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS97 (Sheldrick, 1997)' _diffrn_ambient_temperature 203(2) _diffrn_measured_fraction_theta_full 0.972 _diffrn_measured_fraction_theta_max 0.972 _diffrn_measurement_device 'Enraf-Nonius CAD-4' _diffrn_measurement_method '\w/2\q scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.026 _diffrn_reflns_av_sigmaI/netI 0.029 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_l_max 7 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_number 1715 _diffrn_reflns_theta_full 24.99 _diffrn_reflns_theta_max 24.99 _diffrn_reflns_theta_min 2.89 _diffrn_standards_decay_% 13.45 _diffrn_standards_interval_count 100 _diffrn_standards_interval_time 60 _diffrn_standards_number 3 _exptl_absorpt_coefficient_mu 3.582 _exptl_absorpt_correction_type none _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 2.047 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_method 'not measured' _exptl_crystal_description 'irregular prism' _exptl_crystal_F_000 268 _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.14 _refine_diff_density_max 1.82 _refine_diff_density_min -1.06 _refine_ls_extinction_coef 0.011(3) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method 'SHELXL97 (Sheldrick, 1997)' _refine_ls_goodness_of_fit_ref 1.149 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 45 _refine_ls_number_reflns 836 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.149 _refine_ls_R_factor_all 0.036 _refine_ls_R_factor_gt 0.036 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w = 1/[\s^2^(Fo^2^)+(0.0633P)^2^+1.6121P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.101 _refine_ls_wR_factor_ref 0.101 _reflns_number_gt 835 _reflns_number_total 836 _reflns_threshold_expression I>2\s(I) _[local]_cod_data_source_file ln1131.cif _[local]_cod_data_source_block I _[local]_cod_cif_authors_sg_H-M 'P 21/m' _cod_database_code 2012642 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' '-x, -y, -z' 'x, -y-1/2, z' 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 0.51352(7) 0.2500 0.09210(8) 0.0313(3) Uani d S 1 . . Sn Cl1 0.5759(3) 0.2500 -0.2397(4) 0.0479(6) Uani d S 1 . . Cl Cl2 0.6932(2) 0.07537(16) 0.2936(3) 0.0499(4) Uani d . 1 . . Cl C1 0.2183(11) 0.2500 0.0534(13) 0.0350(17) Uani d S 1 . . C C2 0.1873(9) 0.1294(7) 0.1722(12) 0.0480(15) Uani d . 1 . . C H21 0.2075 0.0532 0.0946 0.055(10) Uiso calc R 1 . . H H22 0.0583 0.1290 0.1661 0.055(10) Uiso calc R 1 . . H H23 0.2761 0.1290 0.3319 0.055(10) Uiso calc R 1 . . H C3 0.0961(12) 0.2500 -0.2039(15) 0.051(2) Uani d S 1 . . C H31 0.1196 0.3275 -0.2726 0.055(10) Uiso d R 1 . . H H32 -0.0356 0.2500 -0.2265 0.055(10) Uiso d SR 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 0.0208(4) 0.0446(4) 0.0289(4) 0.000 0.0100(2) 0.000 Cl1 0.0405(12) 0.0757(15) 0.0334(10) 0.000 0.0208(9) 0.000 Cl2 0.0448(8) 0.0546(9) 0.0458(9) 0.0122(7) 0.0125(7) 0.0091(7) C1 0.026(4) 0.046(4) 0.032(4) 0.000 0.009(3) 0.000 C2 0.039(3) 0.054(4) 0.054(4) -0.005(3) 0.022(3) 0.002(3) C3 0.026(4) 0.078(7) 0.038(5) 0.000 0.002(4) 0.000 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 C1 . 2.170(8) yes Sn1 Cl1 . 2.313(3) yes Sn1 Cl2 . 2.324(2) yes C1 C2 . 1.519(8) yes C1 C3 . 1.523(11) yes C2 H21 . 0.9700 no C2 H22 . 0.9700 no C2 H23 . 0.9700 no C3 H31 . 0.9600 no C3 H32 . 0.9593 no 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' 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' 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 C1 Sn1 Cl1 . . 117.8(2) yes C1 Sn1 Cl2 . . 115.40(11) yes Cl1 Sn1 Cl2 . . 102.01(6) yes Cl2 Sn1 Cl2 4_565 . 101.97(10) yes C2 C1 C2 . 4_565 110.4(7) yes C2 C1 C3 . . 112.0(4) yes C2 C1 Sn1 . . 107.3(4) yes C3 C1 Sn1 . . 107.6(5) yes C1 C2 H21 . . 109.5 no C1 C2 H22 . . 109.5 no H21 C2 H22 . . 109.5 no C1 C2 H23 . . 109.5 no H21 C2 H23 . . 109.5 no H22 C2 H23 . . 109.5 no C1 C3 H31 . . 109.5 no C1 C3 H32 . . 109.5 no H31 C3 H32 . . 107.5 no 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_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag Cl1 Sn1 C1 C2 . 120.7(4) no Cl1 Sn1 C1 C3 . 0.00(4) yes Cl2 Sn1 C1 C2 . 0.0(5) no Cl2 Sn1 C1 C3 . -120.67(10) no Cl2 Sn1 C1 C2 4_565 118.7(4) no