#------------------------------------------------------------------------------ #$Date: 2016-02-19 14:29:56 +0000 (Fri, 19 Feb 2016) $ #$Revision: 176759 $ #$URL: svn://www.crystallography.net/cod/cif/2/00/82/2008267.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_2008267 loop_ _publ_author_name 'Gabriele Kociok-K\"ohn' 'Johannes G. Winter' 'Alexander C. Filippou' _publ_section_title ; Trimethylphosphonium trichlorogermanate(II) ; _journal_issue 3 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first 351 _journal_page_last 353 _journal_paper_doi 10.1107/S010827019801169X _journal_volume 55 _journal_year 1999 _chemical_formula_iupac '(C3 H10 P)GeCl3' _chemical_formula_moiety 'C3 H10 P 1+ Ge Cl3 -1' _chemical_formula_sum 'C3 H10 Cl3 Ge P' _chemical_formula_weight 256.04 _chemical_melting_point 414.15 _chemical_name_common 'Trimethylphosphonium trichlorogermanate(II)' _chemical_name_systematic ; Trimethylphosphonium trichlorogermanate(II) ; _space_group_IT_number 61 _symmetry_cell_setting orthorhombic _symmetry_space_group_name_Hall '-P 2ac 2ab' _symmetry_space_group_name_H-M 'P b c a' _audit_creation_method SHELXL-97 _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_formula_units_Z 8 _cell_length_a 12.225(2) _cell_length_b 13.290(3) _cell_length_c 12.387(3) _cell_measurement_reflns_used 5000 _cell_measurement_temperature 180(2) _cell_measurement_theta_max 26.24 _cell_measurement_theta_min 2.80 _cell_volume 2012.5(7) _diffrn_ambient_temperature 180(2) _diffrn_detector_area_resol_mean 6.667 _diffrn_measured_fraction_theta_full 0.856 _diffrn_measured_fraction_theta_max 0.856 _diffrn_measurement_device_type STOE-IPDS _diffrn_measurement_method \f-rotation _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 0.0802 _diffrn_reflns_av_sigmaI/netI 0.0349 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_number 16964 _diffrn_reflns_theta_full 26.24 _diffrn_reflns_theta_max 26.24 _diffrn_reflns_theta_min 2.80 _diffrn_standards_decay_% none _diffrn_standards_number 200 _exptl_absorpt_coefficient_mu 3.806 _exptl_absorpt_correction_T_max 0.358 _exptl_absorpt_correction_T_min 0.130 _exptl_absorpt_correction_type integration _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.690 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_description column _exptl_crystal_F_000 1008 _exptl_crystal_size_max 0.84 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.27 _refine_diff_density_max 0.385 _refine_diff_density_min -0.594 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.044 _refine_ls_hydrogen_treatment refall _refine_ls_matrix_type full _refine_ls_number_parameters 113 _refine_ls_number_reflns 1984 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.044 _refine_ls_R_factor_all 0.0365 _refine_ls_R_factor_gt 0.0307 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^)+(0.0498P)^2^+0.4045P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_ref 0.0845 _reflns_number_gt 1689 _reflns_number_total 1984 _reflns_threshold_expression I>2sigma(I) _cod_data_source_file jz1290.cif _cod_data_source_block hansi33a _cod_depositor_comments ; The following automatic conversions were performed: '_chemical_melting_point' value '141\%' was changed to '414.15' - it was converted from degrees Celsius(C) to Kelvins(K). Automatic conversion script Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana The following automatic conversions were performed: '_chemical_melting_point' value '141\%' was changed to '414.15' - it was converted from degrees Celsius(C) to Kelvins(K). Automatic conversion script Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana The following automatic conversions were performed: '_exptl_crystal_density_meas' value 'not measured' was changed to '?' - the value is perceived as not measured. Automatic conversion script Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas The following automatic conversions were performed: '_refine_ls_weighting_scheme' value 'calc w = 1/[\s^2^(Fo^2^)+(0.0498P)^2^+0.4045P] where P=(Fo^2^+2Fc^2^)/3' was changed to 'calc'. New tag '_refine_ls_weighting_details' was created. The value of the new tag was set to 'w = 1/[\s^2^(Fo^2^)+(0.0498P)^2^+0.4045P] where P=(Fo^2^+2Fc^2^)/3'. Automatic conversion script Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas ; _cod_database_code 2008267 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x+1/2, -y, z+1/2' '-x, -y, -z' '-x-1/2, y-1/2, z' 'x, -y-1/2, z-1/2' 'x-1/2, 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_calc_flag _atom_site_refinement_flags _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_type_symbol Ge 0.24077(3) 0.25649(2) 0.97223(3) 0.04661(14) Uani d . 1 . . Ge Cl1 0.22883(6) 0.28650(6) 1.15454(6) 0.04872(19) Uani d . 1 . . Cl Cl2 0.24625(7) 0.42440(7) 0.92307(7) 0.0649(2) Uani d . 1 . . Cl Cl3 0.05503(6) 0.23630(5) 0.94598(6) 0.04864(19) Uani d . 1 . . Cl P 0.53625(5) 0.02725(5) 0.74875(6) 0.03528(17) Uani d . 1 . . P H 0.608(2) 0.073(2) 0.692(2) 0.043(7) Uiso d . 1 . . H C1 0.6031(3) -0.0520(3) 0.8418(3) 0.0576(8) Uani d . 1 . . C H1A 0.644(3) -0.011(3) 0.889(3) 0.057(10) Uiso d . 1 . . H H1B 0.647(4) -0.101(4) 0.802(3) 0.096(15) Uiso d . 1 . . H H1C 0.550(4) -0.084(3) 0.882(4) 0.088(14) Uiso d . 1 . . H C2 0.4529(3) -0.0429(4) 0.6592(4) 0.0667(10) Uani d . 1 . . C H2A 0.409(4) -0.004(3) 0.620(4) 0.090(16) Uiso d . 1 . . H H2B 0.407(4) -0.080(3) 0.705(3) 0.077(13) Uiso d . 1 . . H H2C 0.493(3) -0.092(3) 0.625(3) 0.075(11) Uiso d . 1 . . H C3 0.4555(3) 0.1183(3) 0.8164(3) 0.0520(7) Uani d . 1 . . C H3A 0.500(4) 0.155(4) 0.867(4) 0.097(14) Uiso d . 1 . . H H3B 0.409(3) 0.083(3) 0.851(3) 0.068(11) Uiso d . 1 . . H H3C 0.424(4) 0.161(4) 0.766(4) 0.097(15) Uiso 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 Ge 0.0467(2) 0.0461(2) 0.0471(2) 0.01337(12) 0.00904(12) -0.00503(13) Cl1 0.0482(4) 0.0542(4) 0.0438(4) 0.0099(3) -0.0071(3) -0.0011(3) Cl2 0.0738(5) 0.0575(5) 0.0635(5) -0.0072(4) 0.0183(4) 0.0123(4) Cl3 0.0540(4) 0.0485(4) 0.0434(3) 0.0021(3) -0.0047(3) -0.0072(3) P 0.0364(3) 0.0348(3) 0.0346(3) 0.0006(3) 0.0015(2) -0.0035(3) C1 0.067(2) 0.0460(17) 0.0597(19) 0.0021(15) -0.0043(17) 0.0138(16) C2 0.062(2) 0.075(3) 0.063(2) -0.0066(19) -0.0052(18) -0.030(2) C3 0.0437(15) 0.0573(19) 0.0549(18) 0.0043(13) 0.0018(14) -0.0148(16) 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' P P 0.1023 0.0942 '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' Ge Ge 0.0810 1.8010 '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 Cl1 Ge Cl3 . . 95.51(3) yes Cl1 Ge Cl2 . . 95.34(3) yes Cl3 Ge Cl2 . . 95.94(3) yes Cl1 Ge Cl3 . 2_557 78.86(2) yes Cl3 Ge Cl3 . 2_557 171.536(16) yes Cl2 Ge Cl3 . 2_557 90.91(3) yes Cl1 Ge Cl1 . 7_565 173.99(3) yes Cl3 Ge Cl1 . 7_565 78.93(2) yes Cl2 Ge Cl1 . 7_565 83.07(3) yes Cl3 Ge Cl1 2_557 7_565 106.920(16) yes Cl1 Ge Cl2 . 6_655 107.96(3) yes Cl3 Ge Cl2 . 6_655 84.30(2) yes Cl2 Ge Cl2 . 6_655 156.59(4) yes Cl3 Ge Cl2 2_557 6_655 91.391(16) yes Cl1 Ge Cl2 7_565 6_655 73.983(17) yes C1 P C2 . . 111.2(2) yes C1 P C3 . . 110.91(19) yes C2 P C3 . . 109.55(19) yes C1 P H . . 108.9(12) no C2 P H . . 107.5(12) no C3 P H . . 108.7(12) no P C1 H1A . . 108(2) no P C1 H1B . . 109(3) no H1A C1 H1B . . 114(3) no P C1 H1C . . 108(3) no H1A C1 H1C . . 107(3) no H1B C1 H1C . . 111(4) no P C2 H2A . . 113(3) no P C2 H2B . . 104(2) no H2A C2 H2B . . 107(4) no P C2 H2C . . 111(2) no H2A C2 H2C . . 118(4) no H2B C2 H2C . . 103(3) no P C3 Cl1 . 7_565 113.59(14) no P C3 Cl2 . 6_655 93.60(14) no Cl1 C3 Cl2 7_565 6_655 86.18(7) no P C3 H3A . . 110(3) ? Cl1 C3 H3A 7_565 . 128(3) no Cl2 C3 H3A 6_655 . 119(3) no P C3 H3B . . 104(2) no Cl1 C3 H3B 7_565 . 88(2) no Cl2 C3 H3B 6_655 . 12(3) no H3A C3 H3B . . 109(4) no P C3 H3C . . 109(3) no Cl1 C3 H3C 7_565 . 26(3) no Cl2 C3 H3C 6_655 . 112(3) no H3A C3 H3C . . 112(4) no H3B C3 H3C . . 113(4) 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 Cl1 . 2.2978(9) yes Ge Cl3 . 2.3095(9) yes Ge Cl2 . 2.3141(10) yes Ge Cl3 2_557 3.9742(11) yes Ge Cl1 7_565 3.9791(12) yes Ge Cl2 6_655 4.4583(13) yes Cl3 P 8_557 3.6865(11) no P C1 . 1.763(3) yes P C2 . 1.771(3) yes P C3 . 1.772(3) yes P H . 1.28(3) yes C1 Cl3 6_655 3.649(4) no C1 Cl2 2_557 3.798(4) no C1 H1A . 0.94(4) no C1 H1B . 0.98(5) no C1 H1C . 0.92(5) no C2 Cl3 4_554 3.687(4) no C2 H2A . 0.89(5) no C2 H2B . 0.94(4) no C2 H2C . 0.92(4) no C3 Cl1 7_565 3.647(4) no C3 Cl2 6_655 3.804(4) no C3 Cl3 2_557 3.725(3) no C3 H3A . 0.96(5) no C3 H3B . 0.86(4) no C3 H3C . 0.93(5) no