#------------------------------------------------------------------------------ #$Date: 2012-02-03 17:16:24 +0000 (Fri, 03 Feb 2012) $ #$Revision: 32112 $ #$URL: svn://www.crystallography.net/cod/cif/2/01/03/2010302.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_2010302 loop_ _publ_author_name 'Frank, Walter' 'Reiss, Guido J.' 'Kuhn, Dietmar' _publ_section_title ; Trichloromethyltin(IV) ; _journal_issue 12 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first 1904 _journal_page_last 1906 _journal_volume 50 _journal_year 1994 _chemical_formula_sum 'C H3 Cl3 Sn' _chemical_formula_weight 240.07 _chemical_name_common methyltin(IV)trichlorine _chemical_name_systematic ; Methyltin(IV) Trichloride ; _space_group_IT_number 62 _symmetry_cell_setting orthorhombic _symmetry_space_group_name_Hall '-P 2ac 2n' _symmetry_space_group_name_H-M 'P n m a' _audit_creation_method SHELXL _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 6.4110(10) _cell_length_b 9.564(2) _cell_length_c 10.637(2) _cell_measurement_reflns_used 25 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 17.10 _cell_measurement_theta_min 12.97 _cell_volume 652.2(2) _computing_cell_refinement 'CAD-4 Software' _computing_data_collection 'CAD-4 Software (Enraf-Nonius, 1989)' _computing_data_reduction 'MolEN (Fair, 1990)' _computing_molecular_graphics 'SHELXTL-Plus (Sheldrick, 1991)' _computing_publication_material SHELXL93 _computing_structure_refinement 'SHELXL93 (Sheldrick, 1994)' _computing_structure_solution 'SHELXS86 (Sheldrick, 1990)' _diffrn_ambient_temperature 293(2) _diffrn_measurement_device 'Enraf-Nonius CAD-4' _diffrn_measurement_method \w/2\q _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 0.0394 _diffrn_reflns_av_sigmaI/netI 0.0272 _diffrn_reflns_limit_h_max 1 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_l_max 1 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_number 1985 _diffrn_reflns_theta_max 29.85 _diffrn_reflns_theta_min 2.86 _diffrn_standards_decay_% 0 _diffrn_standards_interval_time 60 _diffrn_standards_number 3 _exptl_absorpt_coefficient_mu 5.003 _exptl_absorpt_correction_T_max 0.999 _exptl_absorpt_correction_T_min 0.598 _exptl_absorpt_correction_type empirical _exptl_crystal_colour Colourless _exptl_crystal_density_diffrn 2.445 _exptl_crystal_description 'transparent needle' _exptl_crystal_F_000 440 _exptl_crystal_size_max 0.7 _exptl_crystal_size_mid 0.4 _exptl_crystal_size_min 0.3 _refine_diff_density_max 2.274 _refine_diff_density_min -1.524 _refine_ls_extinction_coef 0.0038(10) _refine_ls_extinction_method SHELXL93 _refine_ls_goodness_of_fit_all 4.139 _refine_ls_goodness_of_fit_obs 4.308 _refine_ls_matrix_type full _refine_ls_number_parameters 35 _refine_ls_number_reflns 983 _refine_ls_number_restraints 5 _refine_ls_restrained_S_all 4.129 _refine_ls_restrained_S_obs 4.297 _refine_ls_R_factor_all 0.0477 _refine_ls_R_factor_obs 0.0446 _refine_ls_shift/esd_max -0.319 _refine_ls_shift/esd_mean 0.050 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_scheme 'calc w = 1/[\s^2^(F~o~^2^)]' _refine_ls_wR_factor_all 0.0862 _refine_ls_wR_factor_obs 0.0860 _reflns_number_observed 905 _reflns_number_total 983 _reflns_observed_criterion >2sigma(I) _[local]_cod_data_source_file hu1116.cif _[local]_cod_data_source_block kuhn _cod_database_code 2010302 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z' 'x+1/2, -y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z' '-x-1/2, 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_thermal_displace_type _atom_site_calc_flag _atom_site_refinement_flags _atom_site_occupancy _atom_site_disorder_group _atom_site_type_symbol Sn 0.02310(8) 0.2500 0.52960(4) 0.0488(2) Uani d SD 1 . Sn Cl1 0.2001(3) 0.2500 0.3434(2) 0.0746(6) Uani d S 1 . Cl Cl2 0.1692(3) 0.4354(2) 0.63900(14) 0.0781(5) Uani d . 1 . Cl C -0.3004(13) 0.2500 0.5314(9) 0.073(2) Uani d SD 1 . C H1 -0.362(4) 0.2500 0.615(3) 0.18(3) Uiso d SD 1 . H H2 -0.364(4) 0.169(6) 0.487(4) 0.18(3) 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 Sn 0.0450(3) 0.0522(3) 0.0491(3) 0.000 -0.0023(2) 0.000 Cl1 0.0650(12) 0.099(2) 0.0595(9) 0.000 0.0115(10) 0.000 Cl2 0.0923(11) 0.0628(8) 0.0793(9) -0.0047(9) -0.0233(8) -0.0144(7) C 0.045(3) 0.091(6) 0.083(5) 0.000 0.005(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 Sn C . 2.074(8) yes Sn Cl1 . 2.283(2) yes Sn Cl2 7_565 2.3180(10) ? Sn Cl2 . 2.3180(10) yes Sn Cl2 5_565 3.714(2) yes C H1 . 0.980(10) no C H2 . 0.99(2) 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 C Sn Cl1 . . 120.3(3) yes C Sn Cl2 . 7_565 113.50(10) ? Cl1 Sn Cl2 . 7_565 103.57(6) ? C Sn Cl2 . . 113.50(10) yes Cl1 Sn Cl2 . . 103.58(6) yes Cl2 Sn Cl2 7_565 . 99.76(8) ? Sn C H1 . . 115.(2) no Sn C H2 . . 114.0(19) no H1 C H1 . . 105.(2) ?