#------------------------------------------------------------------------------ #$Date: 2014-07-12 07:06:18 +0300 (Sat, 12 Jul 2014) $ #$Revision: 120112 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/20/17/7201763.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_7201763 loop_ _publ_author_name 'Dobrzycki, Lukasz' 'Wo\'zniak, Krzysztof' _publ_section_title ; Structures of hybrid inorganic--organic salts with benzidine dication derivatives ; _journal_issue 5 _journal_name_full CrystEngComm _journal_page_first 525 _journal_volume 10 _journal_year 2008 _chemical_formula_sum 'C6 H6 Cl4 N Pb' _chemical_formula_weight 441.11 _chemical_name_systematic ; ? ; _space_group_IT_number 15 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-C 2yc' _symmetry_space_group_name_H-M 'C 1 2/c 1' _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 97.438(15) _cell_angle_gamma 90.00 _cell_formula_units_Z 8 _cell_length_a 34.087(7) _cell_length_b 7.9663(12) _cell_length_c 7.6109(12) _cell_measurement_temperature 100(2) _cell_volume 2049.3(6) _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.28cycle2 beta (release 25-10-2005 CrysAlis171 .NET) (compiled Oct 25 2005,08:50:05) ; _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.28cycle2 beta (release 25-10-2005 CrysAlis171 .NET) (compiled Oct 25 2005,08:50:05) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.28cycle2 beta (release 25-10-2005 CrysAlis171 .NET) (compiled Oct 25 2005,08:50:05) ; _computing_molecular_graphics Diamond _computing_publication_material SHELXTL-97 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _diffrn_ambient_temperature 100(2) _diffrn_detector_area_resol_mean 8.6479 _diffrn_measured_fraction_theta_full 0.990 _diffrn_measured_fraction_theta_max 0.990 _diffrn_measurement_device_type KM4CCD _diffrn_measurement_method 'omega scan' _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 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0691 _diffrn_reflns_limit_h_max 45 _diffrn_reflns_limit_h_min -44 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_number 19343 _diffrn_reflns_theta_full 28.00 _diffrn_reflns_theta_max 28.00 _diffrn_reflns_theta_min 3.13 _diffrn_standards_decay_% 2 _diffrn_standards_number '1 frame' _exptl_absorpt_coefficient_mu 17.451 _exptl_absorpt_correction_T_max 0.87 _exptl_absorpt_correction_T_min 0.01 _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.28cycle2 beta (release 25-10-2005 CrysAlis171 .NET) (compiled Oct 25 2005,08:50:05) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. ; _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 2.859 _exptl_crystal_density_method 'not measured' _exptl_crystal_description planar _exptl_crystal_F_000 1592 _exptl_crystal_size_max 0.56 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.01 _refine_diff_density_max 6.620 _refine_diff_density_min -4.393 _refine_diff_density_rms 0.671 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.227 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 121 _refine_ls_number_reflns 19343 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.227 _refine_ls_R_factor_all 0.1172 _refine_ls_R_factor_gt 0.0998 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.3079 _refine_ls_wR_factor_ref 0.3237 _reflns_number_gt 13977 _reflns_number_total 19343 _reflns_threshold_expression >2sigma(I) _[local]_cod_data_source_file b714587j.txt _[local]_cod_data_source_block 2_PbCl3 _[local]_cod_cif_authors_sg_H-M C2/c _cod_depositor_comments ; The following automatic conversions were performed: '_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic' 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 7201763 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' loop_ _atom_site_label _atom_site_type_symbol _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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pb1 Pb 0.220641(14) 0.79045(4) 0.20565(6) 0.02746(16) Uani 1 1 d . . . Cl1 Cl 0.22003(8) 0.5563(3) 0.4910(3) 0.0301(5) Uani 1 1 d . . . Cl2 Cl 0.14061(8) 0.7001(3) 0.1716(5) 0.0341(7) Uani 1 1 d . . . Cl3 Cl 0.19199(9) 1.1019(3) 0.3194(4) 0.0370(7) Uani 1 1 d . . . Cl4 Cl 0.05574(8) 0.5100(3) -0.0991(4) 0.0394(7) Uani 1 1 d . . . N1 N 0.1292(3) 0.3208(10) 0.0750(14) 0.026(2) Uani 1 1 d . . . H1B H 0.1367 0.3459 -0.0325 0.039 Uiso 1 1 calc R . . H1A H 0.1478 0.2540 0.1366 0.039 Uiso 1 1 calc R . . H1C H 0.1267 0.4173 0.1366 0.039 Uiso 1 1 calc R . . C1 C 0.0906(3) 0.2312(12) 0.0494(16) 0.026(2) Uani 1 1 d . . . C2 C 0.0557(3) 0.3043(11) -0.0206(15) 0.020(2) Uani 1 1 d . . . C3 C 0.0203(3) 0.2137(11) -0.0401(14) 0.021(2) Uani 1 1 d . . . H3 H -0.0034 0.2679 -0.0890 0.025 Uiso 1 1 calc R . . C4 C 0.0190(3) 0.0465(12) 0.0101(17) 0.027(2) Uani 1 1 d . . . C5 C 0.0548(3) -0.0250(13) 0.0854(18) 0.039(3) Uani 1 1 d . . . H5 H 0.0552 -0.1381 0.1253 0.047 Uiso 1 1 calc R . . C6 C 0.0898(3) 0.0681(13) 0.1026(16) 0.031(3) Uani 1 1 d . . . H6 H 0.1138 0.0161 0.1528 0.037 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pb1 0.0275(3) 0.0274(2) 0.0279(3) 0.00092(16) 0.0054(2) 0.00182(17) Cl1 0.0277(13) 0.0323(11) 0.0287(13) 0.0063(11) -0.0028(12) -0.0017(11) Cl2 0.0224(13) 0.0245(12) 0.056(2) 0.0013(12) 0.0060(14) -0.0019(9) Cl3 0.0351(16) 0.0354(14) 0.0370(15) -0.0113(13) -0.0084(13) 0.0130(12) Cl4 0.0308(14) 0.0268(12) 0.0586(19) 0.0110(14) -0.0016(15) 0.0024(11) N1 0.018(5) 0.021(4) 0.040(6) 0.002(4) 0.006(4) 0.009(3) C1 0.022(6) 0.025(5) 0.029(6) 0.015(5) -0.006(5) -0.002(4) C2 0.016(5) 0.020(4) 0.020(5) 0.001(4) -0.008(4) 0.006(4) C3 0.012(5) 0.028(5) 0.020(5) 0.005(4) -0.009(4) 0.005(4) C4 0.018(5) 0.021(5) 0.042(6) 0.010(5) 0.001(5) -0.004(4) C5 0.013(5) 0.030(5) 0.069(8) 0.025(6) -0.015(6) -0.002(4) C6 0.022(6) 0.028(5) 0.042(7) 0.010(5) 0.003(5) -0.004(4) 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' N N 0.0061 0.0033 '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' Pb Pb -3.3944 10.1111 '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 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Cl2 Pb1 Cl3 83.31(8) . . ? Cl2 Pb1 Cl1 78.48(9) . . ? Cl3 Pb1 Cl1 107.52(9) . . ? C1 N1 H1B 109.5 . . ? C1 N1 H1A 109.5 . . ? H1B N1 H1A 109.5 . . ? C1 N1 H1C 109.5 . . ? H1B N1 H1C 109.5 . . ? H1A N1 H1C 109.5 . . ? C6 C1 C2 118.2(10) . . ? C6 C1 N1 118.0(9) . . ? C2 C1 N1 123.8(9) . . ? C1 C2 C3 121.1(9) . . ? C1 C2 Cl4 119.7(8) . . ? C3 C2 Cl4 119.2(7) . . ? C4 C3 C2 121.6(9) . . ? C4 C3 H3 119.2 . . ? C2 C3 H3 119.2 . . ? C3 C4 C5 116.6(9) . . ? C3 C4 C4 120.6(12) . 5 ? C5 C4 C4 122.8(11) . 5 ? C4 C5 C6 120.7(9) . . ? C4 C5 H5 119.6 . . ? C6 C5 H5 119.6 . . ? C1 C6 C5 121.8(10) . . ? C1 C6 H6 119.1 . . ? C5 C6 H6 119.1 . . ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pb1 Cl2 2.801(3) . ? Pb1 Cl3 2.842(3) . ? Pb1 Cl1 2.865(3) . ? Cl4 C2 1.744(9) . ? N1 C1 1.488(14) . ? N1 H1B 0.9100 . ? N1 H1A 0.9100 . ? N1 H1C 0.9100 . ? C1 C6 1.362(13) . ? C1 C2 1.368(14) . ? C2 C3 1.397(14) . ? C3 C4 1.388(13) . ? C3 H3 0.9500 . ? C4 C5 1.398(13) . ? C4 C4 1.486(19) 5 ? C5 C6 1.398(14) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N1 H1B Cl2 0.91 2.30 3.149(11) 154.5 6_565 N1 H1B Cl1 0.91 2.93 3.386(9) 112.7 6_565 N1 H1A Cl3 0.91 2.26 3.170(9) 173.1 1_545 N1 H1C Cl2 0.91 2.31 3.122(9) 148.4 . _journal_paper_doi 10.1039/b714587j