#------------------------------------------------------------------------------ #$Date: 2011-09-17 23:27:16 +0300 (Sat, 17 Sep 2011) $ #$Revision: 26029 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/2204855.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_2204855 loop_ _publ_author_name 'Churakov, Andrei V.' 'Karlov, Sergey S.' 'Yakubova, Elmira Kh.' 'Selina, Anastasia A.' 'Zaitseva, Galina S.' _publ_section_title ; Tetrakis(phenylethynyl)germanium(IV) ; _journal_issue 1 _journal_name_full 'Acta Crystallographica, Section E' _journal_page_first m52 _journal_page_last m54 _journal_volume 61 _journal_year 2005 _chemical_formula_iupac '[Ge (C8 H5)4]' _chemical_formula_moiety 'C32 H20 Ge' _chemical_formula_sum 'C32 H20 Ge' _chemical_formula_weight 477.07 _chemical_name_systematic ; Tetrakis(phenylethynyl)germanium(IV) ; _symmetry_cell_setting tetragonal _symmetry_space_group_name_Hall 'I -4' _symmetry_space_group_name_H-M 'I -4' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-97 _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_formula_units_Z 2 _cell_length_a 13.532(2) _cell_length_b 13.532(2) _cell_length_c 6.746(2) _cell_measurement_reflns_used 25 _cell_measurement_temperature 295(2) _cell_measurement_theta_max 13 _cell_measurement_theta_min 12 _cell_volume 1235.3(4) _computing_cell_refinement ; CAD-4 Diffractometer Program ; _computing_data_collection ; CAD-4 Diffractometer Program (Schagen et al., 1988) ; _computing_data_reduction 'XCAD4 (Harms, 1997)' _computing_molecular_graphics 'SHELXTL-Plus (Bruker, 2000)' _computing_publication_material SHELXL97 _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS97 (Sheldrick, 1990)' _diffrn_ambient_temperature 295(2) _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.998 _diffrn_measurement_device_type 'Enraf-Nonius CAD-4' _diffrn_measurement_method \w _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 0.0371 _diffrn_reflns_av_sigmaI/netI 0.0232 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_number 4296 _diffrn_reflns_theta_full 25.00 _diffrn_reflns_theta_max 25.00 _diffrn_reflns_theta_min 2.13 _diffrn_standards_decay_% 0 _diffrn_standards_interval_time 120 _diffrn_standards_number 2 _exptl_absorpt_coefficient_mu 1.256 _exptl_absorpt_correction_T_max 0.87911 _exptl_absorpt_correction_T_min 0.53322 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(SHELXTL-Plus; Bruker, 2000)' _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.283 _exptl_crystal_density_method 'not measured' _exptl_crystal_description Needle _exptl_crystal_F_000 488 _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _refine_diff_density_max 0.322 _refine_diff_density_min -0.534 _refine_ls_abs_structure_details 'Flack (1983), 486 Friedel pairs' _refine_ls_abs_structure_Flack 0.370(16) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.149 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 76 _refine_ls_number_reflns 1076 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.149 _refine_ls_R_factor_all 0.0309 _refine_ls_R_factor_gt 0.0276 _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^)+(0.0443P)^2^] where P = (Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0642 _refine_ls_wR_factor_ref 0.0654 _reflns_number_gt 1043 _reflns_number_total 1076 _reflns_threshold_expression I>2\s(I) _[local]_cod_data_source_file ci6492.cif _cod_depositor_comments ; The following automatic conversions were performed: '_symmetry_cell_setting' value 'Tetragonal' changed to 'tetragonal' 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 2204855 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'y, -x, -z' '-y, x, -z' 'x+1/2, y+1/2, z+1/2' '-x+1/2, -y+1/2, z+1/2' 'y+1/2, -x+1/2, -z+1/2' '-y+1/2, x+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_adp_type _atom_site_calc_flag _atom_site_refinement_flags _atom_site_occupancy _atom_site_type_symbol Ge 0.0000 0.5000 0.2500 0.05317(18) Uani d S 1 Ge C1 0.04492(18) 0.39660(18) 0.0856(5) 0.0612(6) Uani d . 1 C C2 0.06966(17) 0.33506(19) -0.0311(4) 0.0569(6) Uani d . 1 C C3 0.1000(2) 0.2647(2) -0.1779(4) 0.0552(7) Uani d . 1 C C4 0.1091(3) 0.1650(2) -0.1319(5) 0.0884(10) Uani d . 1 C H4 0.0947 0.1422 -0.0051 0.106 Uiso calc R 1 H C5 0.1401(3) 0.1001(2) -0.2785(11) 0.1058(15) Uani d . 1 C H5 0.1474 0.0336 -0.2475 0.127 Uiso calc R 1 H C6 0.1601(3) 0.1311(3) -0.4674(5) 0.0848(9) Uani d . 1 C H6 0.1796 0.0862 -0.5641 0.102 Uiso calc R 1 H C7 0.1511(2) 0.2281(2) -0.5107(5) 0.0779(8) Uani d . 1 C H7 0.1660 0.2502 -0.6378 0.093 Uiso calc R 1 H C8 0.1200(3) 0.2949(3) -0.3694(5) 0.0673(10) Uani d . 1 C H8 0.1125 0.3611 -0.4034 0.081 Uiso calc R 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 Ge 0.0507(2) 0.0507(2) 0.0581(3) 0.000 0.000 0.000 C1 0.0528(14) 0.0591(15) 0.0717(18) 0.0051(11) -0.0040(12) -0.0004(13) C2 0.0474(12) 0.0565(14) 0.0668(16) 0.0054(11) -0.0021(11) 0.0007(13) C3 0.0532(15) 0.0516(15) 0.0609(18) 0.0070(12) 0.0017(11) -0.0004(12) C4 0.135(3) 0.0651(19) 0.0652(19) 0.0150(19) 0.020(2) 0.0109(16) C5 0.166(3) 0.0611(15) 0.091(4) 0.0301(17) 0.022(3) 0.001(2) C6 0.094(2) 0.092(2) 0.069(2) 0.0206(18) 0.0082(18) -0.0150(18) C7 0.0763(19) 0.100(2) 0.0573(18) 0.0099(16) 0.0031(14) 0.0075(16) C8 0.077(2) 0.0574(19) 0.068(2) 0.0050(16) -0.0059(16) 0.0117(15) 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' Ge Ge 0.1547 1.8001 '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 Ge C1 8 . 110.24(9) no C1 Ge C1 8 7_455 107.95(17) no C1 Ge C1 . 7_455 110.24(9) yes C1 Ge C1 8 2_565 110.24(9) no C1 Ge C1 . 2_565 107.95(17) yes C1 Ge C1 7_455 2_565 110.24(9) no C2 C1 Ge . . 174.6(2) yes C1 C2 C3 . . 177.4(3) yes C8 C3 C4 . . 118.6(3) no C8 C3 C2 . . 120.3(3) no C4 C3 C2 . . 121.1(3) no C5 C4 C3 . . 118.8(4) no C5 C4 H4 . . 120.6 no C3 C4 H4 . . 120.6 no C6 C5 C4 . . 122.0(3) no C6 C5 H5 . . 119.0 no C4 C5 H5 . . 119.0 no C7 C6 C5 . . 118.8(3) no C7 C6 H6 . . 120.6 no C5 C6 H6 . . 120.6 no C6 C7 C8 . . 121.0(3) no C6 C7 H7 . . 119.5 no C8 C7 H7 . . 119.5 no C7 C8 C3 . . 120.8(3) no C7 C8 H8 . . 119.6 no C3 C8 H8 . . 119.6 no 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 Ge C1 8 1.886(3) no Ge C1 . 1.886(3) yes Ge C1 7_455 1.886(3) no Ge C1 2_565 1.886(3) no C1 C2 . 1.194(4) yes C2 C3 . 1.434(4) yes C3 C8 . 1.382(4) yes C3 C4 . 1.389(4) yes C4 C5 . 1.388(7) yes C4 H4 . 0.93 no C5 C6 . 1.369(8) yes C5 H5 . 0.93 no C6 C7 . 1.350(5) yes C6 H6 . 0.93 no C7 C8 . 1.379(5) yes C7 H7 . 0.93 no C8 H8 . 0.93 no