#------------------------------------------------------------------------------ #$Date: 2025-08-19 07:12:48 +0100 (Tue, 19 Aug 2025) $ #$Revision: 301798 $ #$URL: svn://www.crystallography.net/cod/cif/2/01/15/2011552.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_2011552 loop_ _publ_author_name 'Bolte, Michael' 'Hensen, Karl' 'Faber, Alexander' _publ_section_title ; trans-Tetrachlorobis(4-methylpyridine)germanium(IV) ; _journal_issue 11 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first e497 _journal_page_last e498 _journal_paper_doi 10.1107/S0108270100013482 _journal_volume 56 _journal_year 2000 _chemical_formula_iupac '[Ge Cl4 (C6 H7 N)2]' _chemical_formula_sum 'C12 H14 Cl4 Ge N2' _chemical_formula_weight 400.64 _space_group_IT_number 53 _symmetry_cell_setting orthorhombic _symmetry_space_group_name_Hall '-P 2ac 2' _symmetry_space_group_name_H-M 'P m n 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 2 _cell_length_a 7.154(2) _cell_length_b 7.933(2) _cell_length_c 13.731(3) _cell_measurement_reflns_used 2407 _cell_measurement_temperature 173(2) _cell_measurement_theta_max 25 _cell_measurement_theta_min 1 _cell_volume 779.3(3) _computing_cell_refinement SMART _computing_data_collection 'SMART (Siemens, 1995)' _computing_data_reduction 'SAINT (Siemens, 1995)' _computing_publication_material SHELXL97 _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS97 (Sheldrick, 1990)' _diffrn_ambient_temperature 173(2) _diffrn_measured_fraction_theta_full .991 _diffrn_measured_fraction_theta_max .991 _diffrn_measurement_device_type 'Siemens CCD three-circle' _diffrn_measurement_method \w _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength .71073 _diffrn_reflns_av_R_equivalents .031 _diffrn_reflns_av_sigmaI/netI .0290 _diffrn_reflns_limit_h_max 5 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_number 3722 _diffrn_reflns_theta_full 28.25 _diffrn_reflns_theta_max 28.25 _diffrn_reflns_theta_min 2.57 _diffrn_standards_decay_% 0 _diffrn_standards_interval_time 300 _diffrn_standards_number 10 _exptl_absorpt_coefficient_mu 2.638 _exptl_absorpt_correction_T_max .621 _exptl_absorpt_correction_T_min .301 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details '(SADABS; Sheldrick, 1996)' _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.707 _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 400 _exptl_crystal_size_max .60 _exptl_crystal_size_mid .20 _exptl_crystal_size_min .20 _refine_diff_density_max .412 _refine_diff_density_min -.511 _refine_ls_extinction_coef .0063(14) _refine_ls_extinction_method SHELXL97 _refine_ls_goodness_of_fit_ref 1.064 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 57 _refine_ls_number_reflns 1036 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.064 _refine_ls_R_factor_all .034 _refine_ls_R_factor_gt .026 _refine_ls_shift/su_max <0.001 _refine_ls_shift/su_mean <0.001 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w = 1/[\s^2^(Fo^2^)+(0.0334P)^2^+0.1042P] where P = (Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_ref .062 _reflns_number_gt 895 _reflns_number_total 1036 _reflns_threshold_expression I>2\s(I) _cod_data_source_file qa0414.cif _cod_data_source_block I _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 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_values 1715 2011-07-08 13:25:40Z adriana ; _cod_database_code 2011552 _cod_database_fobs_code 2011552 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x+1/2, y, -z+1/2' 'x, -y, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x-1/2, -y, z-1/2' '-x, y, 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_calc_flag _atom_site_refinement_flags _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_type_symbol Cl1 .72510(7) .16635(6) .43468(3) .02974(16) Uani d . 1 . . Cl Ge1 .5000 .0000 .5000 .01699(14) Uani d S 1 . . Ge N1 .5000 .1450(3) .62414(15) .0186(4) Uani d S 1 . . N C2 .5000 .3149(3) .6175(2) .0230(6) Uani d S 1 . . C H2 .5000 .3659 .5549 .028 Uiso calc SR 1 . . H C3 .5000 .4162(3) .6989(2) .0240(6) Uani d S 1 . . C H3 .5000 .5354 .6919 .029 Uiso calc SR 1 . . H C4 .5000 .3445(3) .79128(19) .0205(5) Uani d S 1 . . C C41 .5000 .4504(4) .8814(2) .0285(6) Uani d S 1 . . C H41A .5000 .5623 .8628 .043 Uiso d SPR .50 A 1 H H41B .3975 .4180 .9215 .043 Uiso d PR .50 A 1 H H41C .5000 .3836 .9399 .043 Uiso d SPR .50 A 2 H H41D .3929 .5179 .8789 .043 Uiso d PR .50 A 2 H C5 .5000 .1696(3) .79704(19) .0230(5) Uani d S 1 . . C H5 .5000 .1156 .8588 .028 Uiso calc SR 1 . . H C6 .5000 .0748(3) .71332(19) .0220(5) Uani d S 1 . . C H6 .5000 -.0446 .7186 .026 Uiso calc SR 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 Cl1 .0322(3) .0279(3) .0291(3) -.01187(19) .0090(2) -.00667(19) Ge1 .0192(2) .01502(19) .0167(2) .000 .000 -.00263(14) N1 .0210(11) .0165(9) .0183(11) .000 .000 -.0028(8) C2 .0272(14) .0195(12) .0224(14) .000 .000 .0010(10) C3 .0272(14) .0158(12) .0288(14) .000 .000 -.0032(10) C4 .0155(12) .0234(12) .0226(13) .000 .000 -.0064(11) C41 .0313(15) .0290(13) .0251(15) .000 .000 -.0112(11) C5 .0252(14) .0258(13) .0181(13) .000 .000 -.0006(11) C6 .0261(13) .0178(12) .0221(13) .000 .000 .0018(10) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C .0033 .0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H .0000 .0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N .0061 .0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ge Ge .1547 1.8001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl .1484 .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_site_symmetry_3 _geom_angle N1 Ge1 N1 . 5_656 180.0 N1 Ge1 Cl1 . . 90.13(4) N1 Ge1 Cl1 5_656 . 89.87(4) N1 Ge1 Cl1 . 8_655 90.13(4) N1 Ge1 Cl1 5_656 8_655 89.87(4) Cl1 Ge1 Cl1 . 8_655 90.53(3) N1 Ge1 Cl1 . 5_656 89.87(4) N1 Ge1 Cl1 5_656 5_656 90.13(4) Cl1 Ge1 Cl1 . 5_656 180.0 Cl1 Ge1 Cl1 8_655 5_656 89.47(3) N1 Ge1 Cl1 . 4_556 89.87(4) N1 Ge1 Cl1 5_656 4_556 90.13(4) Cl1 Ge1 Cl1 . 4_556 89.47(3) Cl1 Ge1 Cl1 8_655 4_556 180.0 Cl1 Ge1 Cl1 5_656 4_556 90.53(3) C6 N1 C2 . . 118.3(2) C6 N1 Ge1 . . 121.53(17) C2 N1 Ge1 . . 120.14(17) N1 C2 C3 . . 121.9(2) N1 C2 H2 . . 119.1 C3 C2 H2 . . 119.1 C2 C3 C4 . . 120.1(2) C2 C3 H3 . . 119.9 C4 C3 H3 . . 119.9 C3 C4 C5 . . 117.4(2) C3 C4 C41 . . 121.7(2) C5 C4 C41 . . 120.9(2) C4 C41 H41A . . 108.2 C4 C41 H41B . . 109.1 H41A C41 H41B . . 114.8 C4 C41 H41C . . 112.4 H41A C41 H41C . . 139.4 H41B C41 H41C . . 50.8 C4 C41 H41D . . 107.0 H41A C41 H41D . . 55.9 H41B C41 H41D . . 62.9 H41C C41 H41D . . 110.2 C6 C5 C4 . . 119.9(2) C6 C5 H5 . . 120.0 C4 C5 H5 . . 120.0 N1 C6 C5 . . 122.4(2) N1 C6 H6 . . 118.8 C5 C6 H6 . . 118.8 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 Cl1 Ge1 . 2.2670(6) ? Ge1 N1 . 2.057(2) ? Ge1 N1 5_656 2.057(2) ? Ge1 Cl1 8_655 2.2670(6) ? Ge1 Cl1 5_656 2.2670(6) ? Ge1 Cl1 4_556 2.2670(6) ? N1 C6 . 1.345(3) ? N1 C2 . 1.350(3) ? C2 C3 . 1.377(4) ? C2 H2 . .9500 ? C3 C4 . 1.390(4) ? C3 H3 . .9500 ? C4 C5 . 1.390(4) ? C4 C41 . 1.495(4) ? C41 H41A . .9240 ? C41 H41B . .9530 ? C41 H41C . .9620 ? C41 H41D . .9355 ? C5 C6 . 1.373(4) ? C5 H5 . .9500 ? C6 H6 . .9500 ? 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_1 _geom_torsion N1 Ge1 N1 C6 5_656 .0(3) Cl1 Ge1 N1 C6 . -134.736(16) Cl1 Ge1 N1 C6 8_655 134.736(16) Cl1 Ge1 N1 C6 5_656 45.264(17) Cl1 Ge1 N1 C6 4_556 -45.264(16) N1 Ge1 N1 C2 5_656 180.0(3) Cl1 Ge1 N1 C2 . 45.264(17) Cl1 Ge1 N1 C2 8_655 -45.264(16) Cl1 Ge1 N1 C2 5_656 -134.736(17) Cl1 Ge1 N1 C2 4_556 134.736(17) C6 N1 C2 C3 . .0 Ge1 N1 C2 C3 . 180.0 N1 C2 C3 C4 . .0 C2 C3 C4 C5 . .0 C2 C3 C4 C41 . 180.0 C3 C4 C5 C6 . .0 C41 C4 C5 C6 . 180.0 C2 N1 C6 C5 . .0 Ge1 N1 C6 C5 . 180.0 C4 C5 C6 N1 . .0 loop_ _cod_related_entry_id _cod_related_entry_database _cod_related_entry_code 1 PubChem 139058013