#------------------------------------------------------------------------------ #$Date: 2015-01-07 18:25:02 +0200 (Wed, 07 Jan 2015) $ #$Revision: 129439 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/00/31/2003136.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_2003136 loop_ _publ_author_name 'Linden, Anthony' 'James, Bruce D.' 'Liesegang, John' 'Gonis, Nick' _publ_section_title ; Polynuclear chloromercurate(II) systems in their chloropyridinium salts ; _journal_issue 3 _journal_name_full 'Acta Crystallographica Section B' _journal_page_first 396 _journal_page_last 409 _journal_volume 55 _journal_year 1999 _chemical_formula_moiety 'C5 H5 Cl N 1+, Hg Cl3 1-' _chemical_formula_structural '(C5 H5 Cl N 1+)2, (Hg2 Cl6 2-)' _chemical_formula_sum 'C5 H5 Cl4 Hg N' _chemical_formula_weight 421.49 _chemical_melting_point 368.5(15) _chemical_name_common ' ?' _chemical_name_systematic ; 3-chloropyridinium trichloromercurate(II) ; _space_group_IT_number 14 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_space_group_name_H-M 'P 1 21/c 1' _cell_angle_alpha 90 _cell_angle_beta 99.52(3) _cell_angle_gamma 90 _cell_formula_units_Z 8 _cell_length_a 7.243(5) _cell_length_b 22.145(8) _cell_length_c 12.320(3) _cell_measurement_reflns_used 25 _cell_measurement_temperature 173.0(10) _cell_measurement_theta_max 20.0 _cell_measurement_theta_min 19.0 _cell_volume 1948.9(16) _computing_cell_refinement ; MSC/AFC Diffractometer Control Software (Molecular Structure Corporation, 1991) ; _computing_data_collection ; MSC/AFC Diffractometer Control Software (Molecular Structure Corporation, 1991) ; _computing_data_reduction ; TEXSAN PROCESS (Molecular Structure Corporation, 1989) ; _computing_molecular_graphics 'ORTEPIII (Burnett & Johnson, 1996)' _computing_publication_material ; TEXSAN FINISH (Molecular Structure Corporation, 1989) and local programs ; _computing_structure_refinement ; TEXSAN LS (Molecular Structure Corporation, 1989) ; _computing_structure_solution 'DIRDIF92 Patterson (Beurskens et al., 1992)' _diffrn_ambient_temperature 173.0(10) _diffrn_measurement_device_type 'Rigaku AFC-5R diffractometer' _diffrn_measurement_method \w--2\q _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'Rigaku rotating anode generator' _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71069 _diffrn_reflns_av_R_equivalents 0.073 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_k_max 31 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_number 6239 _diffrn_reflns_theta_max 30 _diffrn_reflns_theta_min 2.5 _diffrn_standards_decay_% 'no decay' _diffrn_standards_interval_count 150 _diffrn_standards_number 3 _exptl_absorpt_coefficient_mu 16.83 _exptl_absorpt_correction_T_max 0.009 _exptl_absorpt_correction_T_min 0.004 _exptl_absorpt_correction_type 'empirical via psi-scan' _exptl_absorpt_process_details '(North, Phillips & Mathews, 1968)' _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 2.873 _exptl_crystal_density_meas ? _exptl_crystal_description prism _exptl_crystal_F_000 1520 _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.28 _refine_diff_density_max 4.06 _refine_diff_density_min -2.79 _refine_ls_abs_structure_details ' ?' _refine_ls_extinction_coef 1.9E-7(1) _refine_ls_extinction_method 'Zachariasen (1963)' _refine_ls_goodness_of_fit_ref 2.014 _refine_ls_hydrogen_treatment noref _refine_ls_matrix_type full _refine_ls_number_constraints 0 _refine_ls_number_parameters 200 _refine_ls_number_reflns 4100 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0879 _refine_ls_R_factor_gt 0.0486 _refine_ls_shift/su_max 0.001 _refine_ls_structure_factor_coef F _refine_ls_weighting_details w=1/[\s^2^(F~o~)+(0.005F~o~)^2^] _refine_ls_weighting_scheme sigma _refine_ls_wR_factor_all 0.0513 _refine_ls_wR_factor_ref 0.0489 _reflns_number_gt 4100 _reflns_number_total 5681 _reflns_threshold_expression 'I > 2\s(I)' _[local]_cod_data_source_file sh0124.cif _[local]_cod_data_source_block IV _cod_depositor_comments ; The following automatic conversions were performed: '_chemical_melting_point' value '367-370' was changed to '368.5(15)' - the average value was taken and precision was estimated. 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 '367-370' was changed to '368.5(15)' - the average value was taken and precision was estimated. Automatic conversion script Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana ; _cod_original_cell_volume 1948.8(13) _cod_database_code 2003136 loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,1/2+y,1/2-z -x,-y,-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_calc_flag _atom_site_calc_attached_atom _atom_site_refinement_flags _atom_site_occupancy _atom_site_disorder_group _atom_site_type_symbol Hg1 -0.05411(7) 0.57150(3) 0.36436(4) 0.02636(17) Uani d ? . 1 . Hg Hg2 0.38188(7) 0.60230(2) 0.21518(3) 0.01930(14) Uani d ? . 1 . Hg Cl1 -0.1703(4) 0.51782(13) 0.2032(2) 0.0214(9) Uani d ? . 1 . Cl Cl2 -0.0229(5) 0.58621(14) 0.5531(2) 0.0247(10) Uani d ? . 1 . Cl Cl3 0.1175(4) 0.66586(12) 0.2803(2) 0.0180(8) Uani d ? . 1 . Cl Cl4 0.6411(4) 0.66852(13) 0.2927(2) 0.0178(8) Uani d ? . 1 . Cl Cl5 0.3091(5) 0.56245(14) 0.0324(2) 0.0268(10) Uani d ? . 1 . Cl Cl6 0.3566(4) 0.52641(13) 0.3688(2) 0.0207(9) Uani d ? . 1 . Cl Cl7 0.1227(5) 0.23839(14) -0.0429(3) 0.0291(10) Uani d ? . 1 . Cl N1 0.1987(14) 0.4106(5) 0.0256(8) 0.022(3) Uani d ? . 1 . N C2 0.1859(18) 0.3567(6) -0.0270(9) 0.022(4) Uani d ? . 1 . C C3 0.1413(15) 0.3066(5) 0.0255(8) 0.016(3) Uani d ? . 1 . C C4 0.1031(16) 0.3099(6) 0.1328(9) 0.021(4) Uani d ? . 1 . C C5 0.1121(19) 0.3651(7) 0.1814(10) 0.029(4) Uani d ? . 1 . C C6 0.1569(18) 0.4175(6) 0.1280(10) 0.026(4) Uani d ? . 1 . C Cl8 0.6317(5) 0.22561(14) 0.4759(3) 0.0258(10) Uani d ? . 1 . Cl N21 0.5419(15) 0.3964(4) 0.4002(8) 0.024(3) Uani d ? . 1 . N C22 0.5583(18) 0.3430(6) 0.4581(9) 0.022(4) Uani d ? . 1 . C C23 0.6106(15) 0.2930(5) 0.4051(9) 0.015(3) Uani d ? . 1 . C C24 0.6498(15) 0.2970(5) 0.3008(9) 0.017(4) Uani d ? . 1 . C C25 0.6319(18) 0.3536(6) 0.2450(10) 0.024(4) Uani d ? . 1 . C C26 0.5820(16) 0.4024(6) 0.2989(10) 0.022(4) Uani d ? . 1 . C H1 0.238 0.445 -0.011 0.027 Uiso calc N1 ? 1 . H H2 0.208 0.354 -0.101 0.026 Uiso calc C2 ? 1 . H H4 0.072 0.275 0.170 0.026 Uiso calc C4 ? 1 . H H5 0.087 0.368 0.254 0.035 Uiso calc C5 ? 1 . H H6 0.158 0.456 0.162 0.031 Uiso calc C6 ? 1 . H H21 0.499 0.431 0.434 0.028 Uiso calc N21 ? 1 . H H22 0.534 0.341 0.532 0.027 Uiso calc C22 ? 1 . H H24 0.689 0.262 0.265 0.021 Uiso calc C24 ? 1 . H H25 0.655 0.357 0.171 0.028 Uiso calc C25 ? 1 . H H26 0.575 0.441 0.265 0.027 Uiso calc C26 ? 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 _atom_site_aniso_type_symbol Hg1 0.0309(3) 0.0359(3) 0.0121(2) -0.0066(2) 0.00277(18) -0.00733(19) Hg Hg2 0.0236(3) 0.0194(2) 0.0139(2) -0.0034(2) 0.00022(17) -0.00361(18) Hg Cl1 0.0343(18) 0.0170(14) 0.0117(12) -0.0061(12) 0.0000(12) -0.0016(10) Cl Cl2 0.0387(19) 0.0254(17) 0.0106(12) -0.0016(14) 0.0060(12) -0.0024(11) Cl Cl3 0.0137(13) 0.0147(13) 0.0267(14) 0.0011(12) 0.0068(11) 0.0023(11) Cl Cl4 0.0097(13) 0.0204(14) 0.0230(14) -0.0017(11) 0.0022(11) -0.0037(11) Cl Cl5 0.0393(19) 0.0243(17) 0.0151(13) -0.0049(14) -0.0005(12) -0.0080(11) Cl Cl6 0.0311(17) 0.0142(14) 0.0171(13) 0.0065(12) 0.0045(12) 0.0028(10) Cl Cl7 0.0308(18) 0.0218(17) 0.0314(17) 0.0047(14) -0.0045(14) -0.0081(13) Cl N1 0.021(6) 0.022(6) 0.024(5) -0.001(5) 0.003(4) 0.004(4) N C2 0.033(7) 0.022(7) 0.010(5) 0.006(6) 0.004(5) 0.001(4) C C3 0.013(6) 0.018(6) 0.014(5) -0.005(5) -0.002(4) 0.001(4) C C4 0.018(6) 0.030(7) 0.017(6) 0.002(5) 0.003(5) 0.000(5) C C5 0.032(8) 0.043(9) 0.013(6) 0.007(7) 0.005(5) 0.000(5) C C6 0.024(7) 0.024(7) 0.028(7) 0.003(6) -0.004(5) -0.004(5) C Cl8 0.0290(17) 0.0191(15) 0.0275(15) 0.0006(13) -0.0006(13) 0.0075(12) Cl N21 0.038(7) 0.009(5) 0.024(5) 0.006(5) 0.007(5) -0.004(4) N C22 0.028(7) 0.022(7) 0.020(6) -0.004(6) 0.009(5) -0.006(5) C C23 0.008(5) 0.014(6) 0.022(6) -0.002(4) 0.002(4) -0.003(4) C C24 0.009(6) 0.014(6) 0.030(6) 0.002(5) 0.006(5) -0.003(5) C C25 0.026(7) 0.024(7) 0.021(6) -0.001(6) 0.005(5) 0.000(5) C C26 0.016(6) 0.018(6) 0.033(7) -0.003(5) 0.005(5) 0.000(5) C 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 for Crystallography (1992). Vol.C, Tables 4.2.6.8 and 6.1.1.1 ; H H 0.0000 0.0000 ; International Tables for Crystallography (1992). Vol.C, Tables 4.2.6.8 and 6.1.1.1 ; Cl Cl 0.1484 0.1585 ; International Tables for Crystallography (1992). Vol.C, Tables 4.2.6.8 and 6.1.1.1 ; Hg Hg -2.3894 9.2266 ; International Tables for Crystallography (1992). Vol.C, Tables 4.2.6.8 and 6.1.1.1 ; N N 0.0061 0.0033 ; International Tables for Crystallography (1992). Vol.C, Tables 4.2.6.8 and 6.1.1.1 ; ; MSC/AFC Diffractometer Control Software (Molecular Structure Corporation, 1991) ; ; MSC/AFC Diffractometer Control Software (Molecular Structure Corporation, 1991) ; ; TEXSAN PROCESS (Molecular Structure Corporation, 1989) ; ; TEXSAN LS (Molecular Structure Corporation, 1989) ; ; TEXSAN FINISH (Molecular Structure Corporation, 1989) and local programs ; loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 1 -5 1 1 -2 -3 2 3 0 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 Hg1 Cl2 . . 151.65(11) yes Cl1 Hg1 Cl3 . . 100.90(10) yes Cl1 Hg1 Cl4 . 1_455 88.36(10) yes Cl1 Hg1 Cl6 . . 93.42(10) yes Cl2 Hg1 Cl3 . . 107.37(10) yes Cl2 Hg1 Cl4 . 1_455 97.75(10) yes Cl2 Hg1 Cl6 . . 95.31(10) yes Cl3 Hg1 Cl4 . 1_455 73.05(9) yes Cl3 Hg1 Cl6 . . 76.05(8) yes Cl4 Hg1 Cl6 1_455 . 148.81(8) yes Cl3 Hg2 Cl4 . . 96.40(10) yes Cl3 Hg2 Cl5 . . 115.44(11) yes Cl3 Hg2 Cl6 . . 88.92(9) yes Cl4 Hg2 Cl5 . . 128.51(11) yes Cl4 Hg2 Cl6 . . 104.42(10) yes Cl5 Hg2 Cl6 . . 114.94(10) yes Hg1 Cl3 Hg2 . . 96.17(9) yes Hg1 Cl4 Hg2 1_655 . 99.20(10) yes Hg1 Cl6 Hg2 . . 87.81(8) yes C2 N1 C6 . . 122.5(10) no N1 C2 C3 . . 119.9(10) no Cl7 C3 C2 . . 119.4(9) no Cl7 C3 C4 . . 119.8(9) no C2 C3 C4 . . 120.7(11) no C3 C4 C5 . . 117.5(12) no C4 C5 C6 . . 122.5(11) no N1 C6 C5 . . 116.7(11) no C22 N21 C26 . . 123.9(10) no N21 C22 C23 . . 117.0(10) no Cl8 C23 C22 . . 117.9(9) no Cl8 C23 C24 . . 121.2(9) no C22 C23 C24 . . 120.9(11) no C23 C24 C25 . . 119.6(10) no C24 C25 C26 . . 118.5(11) no N21 C26 C25 . . 119.9(11) no C2 N1 H1 . . 118.8 no C6 N1 H1 . . 118.7 no N1 C2 H2 . . 120.0 no C3 C2 H2 . . 120.0 no C3 C4 H4 . . 121.2 no C5 C4 H4 . . 121.2 no C4 C5 H5 . . 118.8 no C6 C5 H5 . . 118.8 no N1 C6 H6 . . 121.6 no C5 C6 H6 . . 121.6 no C22 N21 H21 . . 118.0 no C26 N21 H21 . . 118.0 no N21 C22 H22 . . 121.5 no C23 C22 H22 . . 121.5 no C23 C24 H24 . . 120.2 no C25 C24 H24 . . 120.2 no C24 C25 H25 . . 120.7 no C26 C25 H25 . . 120.7 no N21 C26 H26 . . 120.1 no C25 C26 H26 . . 120.1 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 Hg1 Cl1 . 2.348(3) yes Hg1 Cl2 . 2.322(3) yes Hg1 Cl3 . 2.723(3) yes Hg1 Cl4 1_455 3.103(3) yes Hg1 Cl6 . 3.130(4) yes Hg2 Cl3 . 2.607(3) yes Hg2 Cl4 . 2.448(3) yes Hg2 Cl5 . 2.395(3) yes Hg2 Cl6 . 2.560(3) yes Cl7 C3 . 1.724(12) no N1 C2 . 1.353(15) no N1 C6 . 1.354(15) no C2 C3 . 1.351(16) no C3 C4 . 1.397(15) no C4 C5 . 1.358(18) no C5 C6 . 1.399(18) no Cl8 C23 . 1.722(12) no N21 C22 . 1.376(15) no N21 C26 . 1.333(15) no C22 C23 . 1.371(15) no C23 C24 . 1.365(15) no C24 C25 . 1.426(16) no C25 C26 . 1.349(16) no N1 H1 . .95 no C2 H2 . .95 no C4 H4 . .95 no C5 H5 . .95 no C6 H6 . .95 no N21 H21 . .95 no C22 H22 . .95 no C24 H24 . .95 no C25 H25 . .95 no C26 H26 . .95 no loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_publ_flag N1 H1 Cl1 3_565 .95 2.48 3.210(10) 134 no N1 H1 Cl5 . .95 2.69 3.455(10) 138 no N21 H21 Cl6 . .95 2.43 3.173(10) 135 no N21 H21 Cl6 3_666 .95 2.65 3.298(10) 126 no _cod_database_fobs_code 2003136 _journal_paper_doi 10.1107/S010876819801550X