#------------------------------------------------------------------------------ #$Date: 2009-11-18 16:56:34 +0200 (Wed, 18 Nov 2009) $ #$Revision: 858 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/2003137.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_2003137 _journal_name_full 'Acta Crystallographica, Section B' _journal_volume 55 _journal_year 1999 _journal_page_first 396 _journal_page_last 409 _publ_section_title ; Polynuclear Chloromercurate(II) Systems in their Chloropyridinium Salts ; loop_ _publ_author_name 'Linden, Anthony' 'James, Bruce D.' 'Liesegang, John' 'Gonis, Nick' _publ_section_synopsis ; The chloromercurate(II) salts of monochloropyridines display a variety of anion stoichiometries and structures. The 2-chloropridinium salt has the [HgCl~3~]^-^ stoichiometry, but the anions are infinite chains composed of [HgCl~3~]^-^, HgCl~2~ and Cl^-^ moieties linked by longer Hg...Cl contacts. Chains of interconnected [HgCl~4~]^2-^ and HgCl~2~ entities in the 3- and 4-chloropridinium salts yield the rare [Hg~3~Cl~10~]^4-^ stoichiometry. Second forms of the 3- and 4-chloropridinium salts contain distorted [Hg~2~Cl~6~]^2-^ moieties linked into chains and symmetrical discrete [Hg~2~Cl~6~]^2-^ anions, respectively. ; _chemical_name_systematic ; bis(4-chloropyridinium) hexachlorodimercurate(II) ; _chemical_name_common ; ? ; _chemical_formula_moiety '(C5 H5 Cl N 1+)2, Hg2 Cl6 2-' _chemical_formula_sum 'C10 H10 Cl8 Hg2 N2' _[local]_cod_chemical_formula_sum_orig 'C10 H10 Cl8 Hg2 N2 ' _chemical_formula_structural '(C5 H5 Cl N 1+)2, Hg2 Cl6 2-' _chemical_formula_analytical ? _chemical_formula_iupac ? _chemical_formula_weight 842.98 _chemical_melting_point 385 _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 1 2/m 1' _symmetry_space_group_name_Hall '-C 2y' 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' _cell_length_a 13.447(3) _cell_length_b 7.534(2) _cell_length_c 9.939(2) _cell_angle_alpha 90 _cell_angle_beta 97.48(2) _cell_angle_gamma 90 _cell_volume 998.3(3) _cell_formula_units_Z 2 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 19.0 _cell_measurement_theta_max 20.0 _cell_measurement_temperature 173.0(10) _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.15 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 2.804 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_method ? _exptl_crystal_F_000 760 _exptl_absorpt_coefficient_mu 16.46 _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details '(De Meulenaer & Tompa, 1965)' _exptl_absorpt_correction_T_min 0.034 _exptl_absorpt_correction_T_max 0.200 _diffrn_ambient_temperature 173.0(10) _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_source 'Rigaku rotating anode generator' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku AFC-5R diffractometer' _diffrn_measurement_method '\w--2\q' _diffrn_reflns_number 1618 _diffrn_reflns_av_R_equivalents 0.088 _diffrn_reflns_av_sigmaI/netI ? _diffrn_reflns_theta_min 2.5 _diffrn_reflns_theta_max 30 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_reduction_process ? _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 'no decay' 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 _reflns_number_total 1557 _reflns_number_gt 1329 _reflns_threshold_expression 'I > 2\s(I)' _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_R_factor_all ? _refine_ls_R_factor_gt 0.0528 _refine_ls_wR_factor_all 0.0675 _refine_ls_wR_factor_ref 0.0641 _refine_ls_goodness_of_fit_all 0.0653 _refine_ls_goodness_of_fit_ref 2.187 _refine_ls_restrained_S_all ? _refine_ls_number_reflns 1328 _refine_ls_number_parameters 61 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_hydrogen_treatment noref _refine_ls_weighting_scheme sigma _refine_ls_weighting_details 'w=1/[\s^2^(F~o~)+(0.015F~o~)^2^]' _refine_ls_shift/su_max 0.0007 _refine_ls_shift/su_mean ? _refine_diff_density_max 2.81 _refine_diff_density_min -3.16 _refine_ls_extinction_method 'Zachariasen (1963)' _refine_ls_extinction_coef 1.6E-6(3) _refine_ls_abs_structure_details ; ? ; _refine_ls_abs_structure_Flack ? 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