#------------------------------------------------------------------------------ #$Date: 2013-08-29 16:37:19 +0100 (Thu, 29 Aug 2013) $ #$Revision: 88064 $ #$URL: svn://www.crystallography.net/cod/cif/2/20/22/2202247.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_2202247 loop_ _publ_author_name 'Holger Fleischer' 'Simon Parsons' 'Colin R. Pulham' _publ_section_title ; Tetramethyllead(IV) at 150K ; _journal_issue 1 _journal_name_full 'Acta Crystallographica Section E' _journal_page_first m11 _journal_page_last m13 _journal_volume 59 _journal_year 2003 _chemical_formula_iupac '[Pb (C1 H3)4]' _chemical_formula_moiety 'C4 H12 Pb1' _chemical_formula_sum 'C4 H12 Pb' _chemical_formula_weight 267.34 _chemical_melting_point 243 _chemical_name_systematic ; Tetramethyl lead ; _space_group_IT_number 205 _symmetry_cell_setting cubic _symmetry_space_group_name_Hall '-P 2ac 2ab 3' _symmetry_space_group_name_H-M 'P a -3' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 8 _cell_length_a 11.1725(6) _cell_length_b 11.1725(6) _cell_length_c 11.1725(6) _cell_measurement_reflns_used 3546 _cell_measurement_temperature 150 _cell_measurement_theta_max 28.5 _cell_measurement_theta_min 3 _cell_volume 1394.60(13) _computing_cell_refinement ; SAINT (Bruker, 2002) ; _computing_data_collection ; SMART (Bruker, 2001) ; _computing_data_reduction ; SAINT ; _computing_molecular_graphics ; CAMERON (Watkin et al., 1996) ; _computing_publication_material ; CRYSTALS ; _computing_structure_refinement ; CRYSTALS (Watkin et al., 2001) ; _computing_structure_solution ; SHELXS97 (Sheldrick, 1997) ; _diffrn_ambient_temperature 150 _diffrn_measured_fraction_theta_full 0.997 _diffrn_measured_fraction_theta_max 0.975 _diffrn_measurement_device_type ; Bruker SMART APEX CCD ; _diffrn_measurement_method \w _diffrn_radiation_monochromator graphite _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.062 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_limit_l_min -7 _diffrn_reflns_number 7703 _diffrn_reflns_theta_full 28.1 _diffrn_reflns_theta_max 28.6 _diffrn_reflns_theta_min 3.2 _diffrn_standards_decay_% 0.0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 24.07 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.111 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [SADABS (Sheldrick, 2002) based on the method of Blessing (1995)] ; _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 2.546 _exptl_crystal_density_method 'not measured' _exptl_crystal_description cylinder _exptl_crystal_F_000 944.00 _exptl_crystal_size_max 3.00 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.40 _exptl_crystal_size_rad 0.20 _refine_diff_density_max 1.55 _refine_diff_density_min -1.84 _refine_ls_extinction_coef 139.(12) _refine_ls_extinction_method 'Larson (1970), equation 22' _refine_ls_goodness_of_fit_ref 1.07 _refine_ls_hydrogen_treatment noref _refine_ls_matrix_type full _refine_ls_number_parameters 17 _refine_ls_number_reflns 577 _refine_ls_R_factor_all 0.048 _refine_ls_R_factor_gt 0.033 _refine_ls_shift/su_max <0.001 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details ; Method= Tukey and Prince (Carruthers & Watkin, 1979) W = [weight][1-(deltaF/6\sF)^2]^ where [weight] is given by a five-term Chebychev polynomial with coefficients: 96.4 162. 107. 51.2 13.7 ; _refine_ls_weighting_scheme calc _refine_ls_wR_factor_all 0.121 _refine_ls_wR_factor_gt 0.094 _refine_ls_wR_factor_ref 0.105 _reflns_number_gt 375 _reflns_number_total 586 _reflns_threshold_expression I>2\s(I) _[local]_cod_data_source_file ya6144.cif _[local]_cod_data_source_block I _[local]_cod_cif_authors_sg_Hall ' -P 2ac 2ab 3' _[local]_cod_chemical_formula_sum_orig 'C4 H12 Pb1' _cod_depositor_comments ; The following automatic conversions were performed: '_symmetry_cell_setting' value 'Cubic' changed to 'cubic' 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 The following automatic conversions were performed: '_symmetry_cell_setting' value 'Cubic' changed to 'cubic' 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_values 1715 2011-07-08 13:25:40Z adriana ; _cod_database_code 2202247 loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z y,z,x -y,-z,-x z,x,y -z,-x,-y x+1/2,y,-z+1/2 -x+1/2,-y,z+1/2 y+1/2,z,-x+1/2 -y+1/2,-z,x+1/2 z+1/2,x,-y+1/2 -z+1/2,-x,y+1/2 y+1/2,-z+1/2,-x -y+1/2,z+1/2,x z+1/2,-x+1/2,-y -z+1/2,x+1/2,y -z,x+1/2,-y+1/2 z,-x+1/2,y+1/2 -x,y+1/2,-z+1/2 x,-y+1/2,z+1/2 -y,z+1/2,-x+1/2 y,-z+1/2,x+1/2 x+1/2,-y+1/2,-z -x+1/2,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_occupancy _atom_site_type_symbol Pb1 0.872030(14) 0.372030(14) 0.127970(14) 0.0145 Uani 1.0000 Pb C1 0.7586(8) 0.2586(8) 0.2414(8) 0.0258 Uani 1.0000 C C2 0.9865(8) 0.2561(6) 0.0148(5) 0.0224 Uani 1.0000 C H11 0.7071 0.3109 0.2921 0.0315 Uiso 1.0000 H H21 1.0390 0.3065 -0.0370 0.0254 Uiso 1.0000 H H22 1.0382 0.2043 0.0675 0.0254 Uiso 1.0000 H H23 0.9353 0.2035 -0.0363 0.0254 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 Pb1 0.0145(3) 0.0145(3) 0.0145(3) -0.00001(6) 0.00001(6) 0.00001(6) C1 0.026(2) 0.026(2) 0.026(2) -0.002(3) 0.002(3) 0.002(3) C2 0.027(3) 0.018(3) 0.021(2) 0.003(2) 0.005(3) -0.007(2) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Pb1 C1 . . 2.194(15) yes Pb1 C2 . . 2.216(7) yes C2 H21 . . 0.998 no C2 H22 . . 1.008 no C2 H23 . . 0.999 no C1 H11 . . 0.997 no 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 'Pb ' -3.3944 10.1111 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_site_symmetry_3 _geom_angle _geom_angle_publ_flag C2 Pb1 C1 . 108.96(16) yes C2 Pb1 C2 13_556 109.98(16) yes Pb1 C2 H21 . 109.906 no Pb1 C2 H22 . 109.458 no H21 C2 H22 . 108.993 no Pb1 C2 H23 . 109.858 no H21 C2 H23 . 109.669 no H22 C2 H23 . 108.937 no Pb1 C1 H11 . 108.908 no H11 C1 H11 13_556 110.029 no _cod_database_fobs_code 2202247