#------------------------------------------------------------------------------ #$Date: 2011-09-10 05:16:28 +0200 (Sat, 10 Sep 2011) $ #$Revision: 25271 $ #$URL: svn://www.crystallography.net/cod/cif/2/2006514.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_2006514 loop_ _publ_author_name 'Mitzel, N. W.' 'Riede, J.' 'Schmidbaur, H.' _publ_section_title ; 1,1,1,4,4,4-Hexachloro-1,4-disilabutane ; _journal_issue 9 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first 1335 _journal_page_last 1337 _journal_volume 53 _journal_year 1997 _chemical_formula_structural Cl3Si-CH2-CH2-SiCl3 _chemical_formula_sum 'C2 H4 Cl6 Si2' _chemical_formula_weight 296.93 _chemical_melting_point 24 _chemical_name_common Bis(trichlorosilyl)ethane _chemical_name_systematic ; 1,1,1,4,4,4-Hexachloro-1,4-disilabutane ; _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 SHELXL _cell_angle_alpha 90.00 _cell_angle_beta 92.320(10) _cell_angle_gamma 90.00 _cell_formula_units_Z 2 _cell_length_a 6.2310(10) _cell_length_b 9.4470(10) _cell_length_c 9.3940(10) _cell_measurement_reflns_used 96 _cell_measurement_temperature 205(2) _cell_measurement_theta_max 21 _cell_measurement_theta_min 18 _cell_volume 552.52(12) _computing_molecular_graphics SHELXTL/PC _computing_publication_material SHELXL93 _computing_structure_refinement SHELXL93 _computing_structure_solution 'SHELXTL/PC (Sheldrick, 1992)' _diffrn_ambient_temperature 293(2) _diffrn_measurement_device 'Enraf-Nonius CAD4 diffractometer' _diffrn_measurement_method ; \w scans ; _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71069 _diffrn_reflns_av_R_equivalents 0.0128 _diffrn_reflns_av_sigmaI/netI 0.0138 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_number 1259 _diffrn_reflns_theta_max 26.94 _diffrn_reflns_theta_min 3.06 _diffrn_standards_decay_% 0 _diffrn_standards_interval_time 60 _diffrn_standards_number 3 _exptl_absorpt_coefficient_mu 1.706 _exptl_absorpt_correction_T_max 0.599 _exptl_absorpt_correction_T_min 0.533 _exptl_absorpt_correction_type '\y scans (North, Phillips & Mathews, 1968)' _exptl_crystal_colour Colourless _exptl_crystal_density_diffrn 1.785 _exptl_crystal_density_method 'not measured' _exptl_crystal_description Block _exptl_crystal_F_000 292 _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.30 _refine_diff_density_max 0.310 _refine_diff_density_min -0.171 _refine_ls_extinction_coef 0.058(3) _refine_ls_extinction_method 'SHELXL93 (Sheldrick, 1993)' _refine_ls_goodness_of_fit_all 1.120 _refine_ls_goodness_of_fit_obs 1.145 _refine_ls_hydrogen_treatment refall _refine_ls_matrix_type full _refine_ls_number_parameters 55 _refine_ls_number_reflns 1181 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.355 _refine_ls_restrained_S_obs 1.145 _refine_ls_R_factor_all 0.0232 _refine_ls_R_factor_obs 0.0190 _refine_ls_shift/esd_max 0.001 _refine_ls_shift/esd_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^)+(0.0267P)^2^+0.1264P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_all 0.0619 _refine_ls_wR_factor_obs 0.0500 _reflns_number_observed 1085 _reflns_number_total 1190 _reflns_observed_criterion >2sigma(I) _[local]_cod_data_source_file ln1006.cif _[local]_cod_data_source_block micl _cod_database_code 2006514 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' 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 Si1 0.0283(2) 0.0229(2) 0.0226(2) 0.00045(14) 0.00101(14) -0.00108(14) C1 0.0312(8) 0.0327(8) 0.0312(7) 0.0003(6) -0.0015(6) -0.0084(6) Cl1 0.0462(2) 0.0280(2) 0.0511(2) -0.0057(2) 0.0059(2) 0.0076(2) Cl2 0.0303(2) 0.0453(2) 0.0467(2) 0.0030(2) 0.0070(2) -0.0037(2) Cl3 0.0497(2) 0.0478(3) 0.0273(2) 0.0026(2) -0.0065(2) 0.00629(15) 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_occupancy _atom_site_type_symbol Si1 0.13535(6) 0.84311(4) 0.34415(4) 0.02462(12) Uani d 1 Si C1 0.1158(2) 0.9797(2) 0.4837(2) 0.0318(3) Uani d 1 C Cl1 -0.00340(7) 0.65955(4) 0.40238(5) 0.04163(14) Uani d 1 Cl Cl2 0.44841(6) 0.80479(5) 0.30693(5) 0.04061(14) Uani d 1 Cl Cl3 -0.01416(7) 0.90569(5) 0.15966(4) 0.04180(14) Uani d 1 Cl H1 0.202(4) 1.057(3) 0.456(2) 0.057(6) Uiso d 1 H H2 0.193(3) 0.946(2) 0.568(2) 0.043(5) Uiso d 1 H 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' Si Si 0.0817 0.0704 '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' 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 _geom_angle_publ_flag C1 Si1 Cl1 . 111.44(6) y C1 Si1 Cl2 . 109.80(5) y C1 Si1 Cl3 . 111.27(6) y Cl1 Si1 Cl2 . 108.55(3) y Cl1 Si1 Cl3 . 107.17(3) y Cl2 Si1 Cl3 . 108.50(3) y C1 C1 Si1 3_576 113.93(13) y C1 C1 H1 3_576 114.2(14) ? Si1 C1 H1 . 106.5(13) ? C1 C1 H2 3_576 111.4(12) ? Si1 C1 H2 . 107.6(12) ? H1 C1 H2 . 102.5(17) ? 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 Si1 C1 . 1.8469(15) y C1 C1 3_576 1.536(3) y Si1 Cl1 . 2.0229(6) y Si1 Cl2 . 2.0283(6) y Si1 Cl3 . 2.0225(6) y C1 H1 . 0.95(2) n C1 H2 . 0.96(2) n 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 Si1 C1 C1 3_576 -61.7(2) y Cl2 Si1 C1 C1 3_576 177.96(14) y Cl3 Si1 C1 C1 3_576 57.8(2) y