#------------------------------------------------------------------------------ #$Date: 2011-09-17 23:27:16 +0300 (Sat, 17 Sep 2011) $ #$Revision: 26029 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/2203530.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_2203530 loop_ _publ_author_name 'Fraser, Stewart' 'Parsons, Simon' _publ_section_title ; (Chloromethyl)trimethylsilane at 160 K ; _journal_issue 4 _journal_name_full 'Acta Crystallographica, Section E' _journal_page_first o564 _journal_page_last o565 _journal_volume 60 _journal_year 2004 _chemical_formula_iupac 'C4 H11 Cl1 Si1' _chemical_formula_moiety 'C4 H11 Cl1 Si1' _chemical_formula_sum 'C4 H11 Cl Si' _chemical_formula_weight 122.67 _chemical_melting_point 182.8 _chemical_name_systematic ; (Chloromethyl)trimethylsilane ; _symmetry_cell_setting orthorhombic _symmetry_space_group_name_Hall 'P 2c -2n' _symmetry_space_group_name_H-M 'P n a 21' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary Patterson _atom_sites_solution_secondary difmap _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 13.8776(13) _cell_length_b 6.3855(9) _cell_length_c 8.4000(10) _cell_measurement_reflns_used 72 _cell_measurement_temperature 160 _cell_measurement_theta_max 16 _cell_measurement_theta_min 15 _cell_volume 744.37(15) _computing_cell_refinement DIF4 _computing_data_collection 'DIF4 (Stoe & Cie, 1990)' _computing_data_reduction 'REDU4 (Stoe & Cie, 1990)' _computing_molecular_graphics 'CAMERON (Watkin et al., 1996) and XP (Sheldrick, 1997)' _computing_publication_material ; CRYSTALS, EnCIFer (CCDC, 2003) and PLATON (Spek, 2003) used within WinGX (Farrugia, 1999) ; _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_structure_solution 'DIRDIF (Beurskens et al., 1996)' _diffrn_ambient_temperature 160 _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 1.000 _diffrn_measurement_device_type ; Stoe STADI-4 diffractometer equipped with an Oxford Cryosystems low-temperature device (Cosier & Glazer, 1986) ; _diffrn_measurement_method \w-\q _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.030 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_h_min -1 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_number 3768 _diffrn_reflns_theta_full 25.0 _diffrn_reflns_theta_max 25.0 _diffrn_reflns_theta_min 2.5 _diffrn_standards_decay_% 0.00 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 60 _diffrn_standards_number 3 _exptl_absorpt_coefficient_mu 0.56 _exptl_absorpt_correction_T_max 0.804 _exptl_absorpt_correction_T_min 0.741 _exptl_absorpt_correction_type '\y scan' _exptl_absorpt_process_details ; Azimuthal absorption correction (North et al., 1968) applied using XPREP (Sheldrick, 1997) ; _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.095 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_method 'not measured' _exptl_crystal_description cylinder _exptl_crystal_F_000 264 _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.39 _exptl_crystal_size_min 0.39 _exptl_crystal_size_rad 0.39 _refine_diff_density_max 0.43 _refine_diff_density_min -0.32 _refine_ls_abs_structure_details 'Flack (1983), 602 Friedel pairs' _refine_ls_abs_structure_Flack -0.17(17) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.02 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 56 _refine_ls_number_reflns 1305 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.044 _refine_ls_R_factor_gt 0.040 _refine_ls_shift/su_max 0.001 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details ; w = 1/[\s^2^(F*)+(0.0706P)^2^+0.41P] where P=0.333*max(Fo^2^,0) + (1-0.333)Fc^2^ (SHELXL97; Sheldrick, 1997) ; _refine_ls_weighting_scheme calc _refine_ls_wR_factor_all 0.115 _refine_ls_wR_factor_gt 0.112 _refine_ls_wR_factor_ref 0.115 _reflns_number_gt 1186 _reflns_number_total 1306 _reflns_threshold_expression I>2\s(I) _[local]_cod_data_source_file ya6200.cif _[local]_cod_chemical_formula_sum_orig 'C4 H11 Cl1 Si1' _cod_depositor_comments ; The following automatic conversions were performed: '_symmetry_cell_setting' value 'Orthorhombic' changed to 'orthorhombic' according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29. Automatic conversion script Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius ; _cod_database_code 2203530 loop_ _symmetry_equiv_pos_as_xyz x,y,z -x+1/2,y+1/2,z+1/2 x+1/2,-y+1/2,z -x,-y,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_occupancy _atom_site_type_symbol Cl1 0.09384(8) 0.28224(18) -0.33332(15) 0.0602 Uani 1.0000 Cl Si1 0.14648(6) 0.17201(14) 0.00888(17) 0.0327 Uani 1.0000 Si C1 0.0582(3) 0.3037(6) -0.1281(5) 0.0430 Uani 1.0000 C C2 0.2681(3) 0.2813(6) -0.0252(5) 0.0492 Uani 1.0000 C C3 0.1468(3) -0.1149(6) -0.0303(5) 0.0464 Uani 1.0000 C C4 0.1032(3) 0.2305(7) 0.2146(5) 0.0522 Uani 1.0000 C H11 0.0538 0.4553 -0.0993 0.0516 Uiso 1.0000 H H12 -0.0064 0.2366 -0.1147 0.0516 Uiso 1.0000 H H21 0.3151 0.2113 0.0476 0.0591 Uiso 1.0000 H H22 0.2673 0.4351 -0.0034 0.0591 Uiso 1.0000 H H23 0.2874 0.2561 -0.1382 0.0591 Uiso 1.0000 H H31 0.1937 -0.1849 0.0426 0.0557 Uiso 1.0000 H H32 0.1659 -0.1411 -0.1433 0.0557 Uiso 1.0000 H H33 0.0808 -0.1727 -0.0112 0.0557 Uiso 1.0000 H H41 0.1477 0.1644 0.2936 0.0629 Uiso 1.0000 H H42 0.1024 0.3857 0.2311 0.0629 Uiso 1.0000 H H43 0.0368 0.1733 0.2286 0.0629 Uiso 1.0000 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 Cl1 0.0550(6) 0.0864(8) 0.0393(6) 0.0021(6) -0.0026(6) 0.0070(7) Si1 0.0317(4) 0.0313(4) 0.0350(5) 0.0017(4) 0.0013(5) -0.0014(5) C1 0.041(2) 0.044(2) 0.044(2) 0.0084(17) -0.0020(17) 0.0021(19) C2 0.039(2) 0.050(2) 0.059(3) -0.0074(17) 0.001(2) -0.001(2) C3 0.048(2) 0.0382(18) 0.053(3) 0.0006(17) 0.0011(19) -0.0025(17) C4 0.060(3) 0.058(3) 0.039(2) 0.006(2) 0.0051(19) -0.0053(18) loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C ' 0.0033 0.0016 International_Tables_Vol_IV_Table_2.2B 'H ' 0.0000 0.0000 International_Tables_Vol_IV_Table_2.2B 'Si ' 0.0817 0.0704 International_Tables_Vol_IV_Table_2.2B 'Cl ' 0.1484 0.1585 International_Tables_Vol_IV_Table_2.2B loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag C1 Si1 C2 109.4(2) yes C1 Si1 C3 109.47(19) yes C1 Si1 C4 105.5(2) yes C2 Si1 C3 110.01(19) yes C2 Si1 C4 111.2(2) yes C3 Si1 C4 111.18(19) yes H12 C1 H11 109.474 no H12 C1 Cl1 108.829 no H11 C1 Cl1 108.829 no H12 C1 Si1 108.878 no H11 C1 Si1 108.891 no Cl1 C1 Si1 111.9(2) yes H23 C2 H22 109.553 no H23 C2 H21 109.488 no H22 C2 H21 109.551 no H23 C2 Si1 109.391 no H22 C2 Si1 109.438 no H21 C2 Si1 109.407 no H33 C3 H32 109.483 no H33 C3 H31 109.471 no H32 C3 H31 109.508 no H33 C3 Si1 109.441 no H32 C3 Si1 109.458 no H31 C3 Si1 109.467 no H43 C4 H42 109.610 no H43 C4 H41 109.690 no H42 C4 H41 109.489 no H43 C4 Si1 109.412 no H42 C4 Si1 109.281 no H41 C4 Si1 109.344 no loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag Cl1 C1 1.798(5) yes Si1 C1 1.880(4) yes Si1 C2 1.848(4) yes Si1 C3 1.862(4) yes Si1 C4 1.867(4) yes C1 H12 1.000 no C1 H11 1.000 no C2 H23 1.000 no C2 H22 0.999 no C2 H21 1.000 no C3 H33 1.000 no C3 H32 1.000 no C3 H31 1.000 no C4 H43 0.998 no C4 H42 1.000 no C4 H41 0.999 no