#------------------------------------------------------------------------------ #$Date: 2010-01-30 15:59:17 +0200 (Sat, 30 Jan 2010) $ #$Revision: 966 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/2003134.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_2003134 _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 ; tetrakis(3-chloropyridinium) decachlorotrimercurate(II) ; _chemical_name_common ; ? ; _chemical_formula_moiety '(C5 H5 Cl N 1+)4, Hg3 Cl10 4-' _chemical_formula_sum 'C20 H20 Cl14 Hg3 N4' _chemical_formula_structural '(C5 H5 Cl N 1+)4, Hg Cl2, (Hg Cl4 2-)2' _chemical_formula_analytical ? _chemical_formula_iupac ? _chemical_formula_weight 1414.52 _chemical_melting_point ? _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/n 1' _symmetry_space_group_name_Hall '-P 2yn' loop_ _symmetry_equiv_pos_as_xyz 'x,y,z' '1/2-x,1/2+y,1/2-z' '-x,-y,-z' '1/2+x,1/2-y,1/2+z' _cell_length_a 7.522(2) _cell_length_b 28.046(3) _cell_length_c 9.165(2) _cell_angle_alpha 90 _cell_angle_beta 105.78(2) _cell_angle_gamma 90 _cell_volume 1860.5(7) _cell_formula_units_Z 2 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 19.5 _cell_measurement_theta_max 20.0 _cell_measurement_temperature 173.0(10) _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.37 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.28 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 2.524 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_method ? _exptl_crystal_F_000 1292 _exptl_absorpt_coefficient_mu 13.37 _exptl_absorpt_correction_type 'empirical via psi-scan' _exptl_absorpt_process_details '(North, Phillips & Mathews, 1968)' _exptl_absorpt_correction_T_min 0.010 _exptl_absorpt_correction_T_max 0.024 _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' _diffrn_reflns_number 5915 _diffrn_reflns_av_R_equivalents 0.046 _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 10 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 39 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _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 -1 5 -1 -1 1 -2 -1 -1 -2 _reflns_number_total 5426 _reflns_number_gt 4337 _reflns_threshold_expression 'I > 2\s(I)' _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_R_factor_all 0.0562 _refine_ls_R_factor_gt 0.0357 _refine_ls_wR_factor_all 0.0388 _refine_ls_wR_factor_ref 0.0375 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_ref 1.950 _refine_ls_restrained_S_all ? _refine_ls_number_reflns 4337 _refine_ls_number_parameters 188 _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~)+(0.005F~o~)^2^]' _refine_ls_shift/su_max 0.0005 _refine_ls_shift/su_mean ? _refine_diff_density_max 2.15 _refine_diff_density_min -2.32 _refine_ls_extinction_method 'Zachariasen (1963)' _refine_ls_extinction_coef 1.3E-7(2) _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 0.0 0.0 0.0 0.02077(13) Uani d ? S 1 ? Hg Hg2 0.44770(4) 0.126030(10) -0.21367(3) 0.02059(9) Uani d ? . 1 . Hg Cl1 -0.0673(3) -0.04381(6) -0.2260(2) 0.0243(6) Uani d ? . 1 . Cl Cl2 0.2445(3) 0.06871(6) -0.0959(2) 0.0238(6) Uani d ? . 1 . Cl Cl3 0.3173(3) 0.12483(8) -0.4810(2) 0.0368(7) Uani d ? . 1 . Cl Cl4 0.4927(3) 0.18989(7) -0.0298(2) 0.0326(7) Uani d ? . 1 . Cl Cl5 0.7291(3) 0.07370(7) -0.1353(3) 0.0315(7) Uani d ? . 1 . Cl Cl6 -0.0203(3) 0.25279(8) -0.2269(3) 0.0408(8) Uani d ? . 1 . Cl N1 0.0286(10) 0.1501(2) 0.0704(8) 0.031(2) Uani d ? . 1 . N C2 0.0188(11) 0.1736(3) -0.0608(9) 0.026(3) Uani d ? . 1 . C C3 -0.0109(10) 0.2217(3) -0.0638(9) 0.023(2) Uani d ? . 1 . C C4 -0.0348(12) 0.2441(3) 0.0637(11) 0.033(3) Uani d ? . 1 . C C5 -0.0191(13) 0.2187(3) 0.1975(10) 0.036(3) Uani d ? . 1 . C C6 0.0113(11) 0.1704(3) 0.1980(9) 0.028(3) Uani d ? . 1 . C Cl7 0.8257(3) 0.15591(8) 0.5247(3) 0.0384(8) Uani d ? . 1 . Cl N21 0.5482(9) 0.0657(3) 0.2230(7) 0.031(2) Uani d ? . 1 . N C22 0.6193(12) 0.1067(3) 0.2914(9) 0.028(3) Uani d ? . 1 . C C23 0.7391(11) 0.1037(3) 0.4323(9) 0.025(3) Uani d ? . 1 . C C24 0.7860(12) 0.0592(3) 0.5012(10) 0.033(3) Uani d ? . 1 . C C25 0.7089(12) 0.0196(3) 0.4243(10) 0.034(3) Uani d ? . 1 . C C26 0.5876(12) 0.0236(3) 0.2864(10) 0.032(3) Uani d ? . 1 . C H1 0.049 0.117 0.072 0.037 Uiso calc N1 ? 1 . H H2 0.032 0.157 -0.148 0.031 Uiso calc C2 ? 1 . H H4 -0.062 0.277 0.060 0.040 Uiso calc C4 ? 1 . H H5 -0.029 0.234 0.287 0.043 Uiso calc C5 ? 1 . H H6 0.020 0.152 0.287 0.034 Uiso calc C6 ? 1 . H H21 0.466 0.067 0.124 0.037 Uiso calc N21 ? 1 . H H22 0.587 0.137 0.243 0.034 Uiso calc C22 ? 1 . H H24 0.870 0.057 0.599 0.039 Uiso calc C24 ? 1 . H H25 0.741 -0.011 0.468 0.040 Uiso calc C25 ? 1 . H H26 0.530 -0.004 0.235 0.039 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 0.0241(2) 0.02007(19) 0.0191(2) -0.00327(16) 0.00748(15) -0.00288(16) Hg Hg2 0.02245(15) 0.02047(14) 0.01912(15) -0.00038(12) 0.00612(11) 0.00143(11) Hg Cl1 0.0352(11) 0.0209(8) 0.0169(9) -0.0024(8) 0.0073(8) -0.0008(7) Cl Cl2 0.0244(9) 0.0218(9) 0.0289(10) -0.0049(7) 0.0137(8) 0.0010(7) Cl Cl3 0.0376(12) 0.0498(13) 0.0191(10) -0.0004(11) 0.0008(8) 0.0015(9) Cl Cl4 0.0497(13) 0.0231(9) 0.0255(10) -0.0043(9) 0.0113(9) -0.0053(8) Cl Cl5 0.0211(9) 0.0277(10) 0.0413(12) 0.0057(8) 0.0010(9) -0.0011(9) Cl Cl6 0.0559(15) 0.0328(11) 0.0322(11) -0.0076(11) 0.0096(10) 0.0087(10) Cl N1 0.039(4) 0.018(3) 0.038(4) 0.001(3) 0.013(3) 0.000(3) N C2 0.028(4) 0.022(4) 0.027(4) 0.003(3) 0.006(3) -0.005(3) C C3 0.025(4) 0.021(4) 0.022(4) -0.006(3) 0.005(3) 0.004(3) C C4 0.043(5) 0.019(4) 0.041(5) -0.001(4) 0.017(4) -0.003(4) C C5 0.047(6) 0.034(5) 0.029(5) -0.001(4) 0.015(4) -0.009(4) C C6 0.033(5) 0.028(4) 0.022(4) 0.000(3) 0.003(3) 0.003(3) C Cl7 0.0456(13) 0.0344(11) 0.0344(12) -0.0078(10) 0.0093(10) -0.0105(10) Cl N21 0.034(4) 0.035(4) 0.019(3) 0.002(3) -0.001(3) -0.002(3) N C22 0.036(5) 0.023(4) 0.023(4) 0.001(3) 0.005(4) 0.003(3) C C23 0.026(4) 0.030(4) 0.022(4) 0.000(3) 0.010(3) -0.005(3) C C24 0.030(5) 0.038(5) 0.030(5) 0.005(4) 0.008(4) 0.004(4) C C25 0.046(5) 0.021(4) 0.037(5) 0.006(4) 0.017(4) 0.003(4) C C26 0.039(5) 0.025(4) 0.035(5) -0.002(4) 0.015(4) -0.003(4) C _cod_database_code 2003134