#------------------------------------------------------------------------------ #$Date: 2015-01-07 18:25:02 +0200 (Wed, 07 Jan 2015) $ #$Revision: 129439 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/00/31/2003137.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_2003137 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+)2, Hg2 Cl6 2-' _chemical_formula_structural '(C5 H5 Cl N 1+)2, Hg2 Cl6 2-' _chemical_formula_sum 'C10 H10 Cl8 Hg2 N2' _chemical_formula_weight 842.98 _chemical_melting_point 385 _chemical_name_common ' ?' _chemical_name_systematic ; bis(4-chloropyridinium) hexachlorodimercurate(II) ; _space_group_IT_number 12 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-C 2y' _symmetry_space_group_name_H-M 'C 1 2/m 1' _cell_angle_alpha 90 _cell_angle_beta 97.48(2) _cell_angle_gamma 90 _cell_formula_units_Z 2 _cell_length_a 13.447(3) _cell_length_b 7.534(2) _cell_length_c 9.939(2) _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 998.3(4) _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 0.088 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_number 1618 _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 16.46 _exptl_absorpt_correction_T_max 0.200 _exptl_absorpt_correction_T_min 0.034 _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details '(De Meulenaer & Tompa, 1965)' _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 2.804 _exptl_crystal_density_meas ? _exptl_crystal_description prism _exptl_crystal_F_000 760 _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.15 _refine_diff_density_max 2.81 _refine_diff_density_min -3.16 _refine_ls_abs_structure_details ' ?' _refine_ls_extinction_coef 1.6E-6(3) _refine_ls_extinction_method 'Zachariasen (1963)' _refine_ls_goodness_of_fit_all 0.0653 _refine_ls_goodness_of_fit_ref 2.187 _refine_ls_hydrogen_treatment noref _refine_ls_matrix_type full _refine_ls_number_constraints 0 _refine_ls_number_parameters 61 _refine_ls_number_reflns 1328 _refine_ls_number_restraints 0 _refine_ls_R_factor_gt 0.0528 _refine_ls_shift/su_max 0.0007 _refine_ls_structure_factor_coef F _refine_ls_weighting_details w=1/[\s^2^(F~o~)+(0.015F~o~)^2^] _refine_ls_weighting_scheme sigma _refine_ls_wR_factor_all 0.0675 _refine_ls_wR_factor_ref 0.0641 _reflns_number_gt 1329 _reflns_number_total 1557 _reflns_threshold_expression 'I > 2\s(I)' _[local]_cod_data_source_file sh0124.cif _[local]_cod_data_source_block V _[local]_cod_chemical_formula_sum_orig 'C10 H10 Cl8 Hg2 N2 ' _cod_original_cell_volume 998.3(3) _cod_database_code 2003137 loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,y,-z -x,-y,-z x,-y,z 1/2+x,1/2+y,z 1/2-x,1/2+y,-z 1/2-x,1/2-y,-z 1/2+x,1/2-y,z loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 2 2 1 3 -1 1 2 -2 1 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_ _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 0.13306(5) 0.0 0.10021(6) 0.0285(2) Uani d ? S 1 . Hg Cl1 0.0973(4) 0.0 0.3259(4) 0.0346(12) Uani d ? S 1 . Cl Cl2 0.2412(3) 0.0 -0.0668(4) 0.0337(12) Uani d ? S 1 . Cl Cl3 0.0 0.2556(4) 0.0 0.0233(9) Uani d ? S 1 . Cl Cl4 -0.1695(4) 0.5 0.6409(4) 0.0365(13) Uani d ? S 1 . Cl N1 -0.0926(11) 0.5 0.2258(14) 0.034(4) Uani d ? S 2 . N C2 -0.1031(9) 0.3417(14) 0.2835(11) 0.031(3) Uani d ? . 1 . C C3 -0.1292(9) 0.3398(14) 0.4131(12) 0.033(3) Uani d ? . 1 . C C4 -0.1415(11) 0.5 0.4790(14) 0.023(4) Uani d ? S 2 . C H1 -0.076 0.5 0.136 0.041 Uiso calc N1 S 1 . H H2 -0.093 0.234 0.237 0.037 Uiso calc C2 ? 1 . H H3 -0.139 0.230 0.457 0.040 Uiso calc C3 ? 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 0.0281(3) 0.0363(4) 0.0220(3) 0.0 0.0065(2) 0.0 Hg Cl1 0.050(3) 0.037(2) 0.0170(16) 0.0 0.0049(15) 0.0 Cl Cl2 0.031(2) 0.043(2) 0.0292(19) 0.0 0.0116(15) 0.0 Cl Cl3 0.0304(17) 0.0172(13) 0.0236(15) 0.0 0.0084(13) 0.0 Cl Cl4 0.051(3) 0.039(2) 0.0224(18) 0.0 0.0156(17) 0.0 Cl N1 0.038(8) 0.043(8) 0.024(7) 0.0 0.013(6) 0.0 N C2 0.036(6) 0.026(5) 0.031(5) 0.001(5) 0.008(4) -0.002(4) C C3 0.041(6) 0.022(5) 0.037(6) 0.000(5) 0.013(5) 0.002(5) C C4 0.028(8) 0.028(7) 0.015(6) 0.0 0.004(5) 0.0 C loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag Cl1 Hg1 Cl2 . 153.72(16) yes Cl1 Hg1 Cl3 . 98.19(8) yes Cl2 Hg1 Cl3 . 100.33(8) yes Cl3 Hg1 Cl3 3 89.84(10) yes Hg1 Cl3 Hg1 3 90.16(10) yes C2 N1 C2 4_565 126.0(13) no N1 C2 C3 . 117.6(10) no C2 C3 C4 . 119.4(10) no Cl4 C4 C3 . 120.0(7) no C3 C4 C3 4_565 120.1(13) no C2 N1 H1 . 117.0 no N1 C2 H2 . 121.2 no C3 C2 H2 . 121.2 no C2 C3 H3 . 120.3 no C4 C3 H3 . 120.3 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 . 2.354(4) yes Hg1 Cl2 . 2.346(4) yes Hg1 Cl3 . 2.727(2) yes Cl4 C4 . 1.700(14) no N1 C2 . 1.339(12) no C2 C3 . 1.378(15) no C3 C4 . 1.393(13) no N1 H1 . .95 no C2 H2 . .95 no C3 H3 . .95 no Hg1 Hg1 3 3.8623(16) yes 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_publ_flag N1 H1 Cl3 .95 2.57 3.272(11) 131 no _cod_database_fobs_code 2003137 _journal_paper_doi 10.1107/S010876819801550X