#------------------------------------------------------------------------------ #$Date: 2008-01-14 00:15:36 +0200 (Mon, 14 Jan 2008) $ #$Revision: 14 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/2003135.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_2003135 _journal_name_full 'Acta Crystallographica, Section B' _journal_year 1999 _journal_volume B55 _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(4-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 '373-375' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x,y,z' '-x,-y,-z' _cell_length_a 9.907(3) _cell_length_b 13.226(2) _cell_length_c 7.282(2) _cell_angle_alpha 84.41(2) _cell_angle_beta 74.81(2) _cell_angle_gamma 87.34(2) _cell_volume 916.2(4) _cell_formula_units_Z 1 _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 0.43 _exptl_crystal_size_mid 0.27 _exptl_crystal_size_min 0.11 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 2.564 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_method ? _exptl_crystal_F_000 646 _exptl_absorpt_coefficient_mu 13.58 _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details '(De Meulenaer & Tompa, 1965)' _exptl_absorpt_correction_T_min 0.055 _exptl_absorpt_correction_T_max 0.270 _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 5621 _diffrn_reflns_av_R_equivalents 0.019 _diffrn_reflns_av_sigmaI/netI ? _diffrn_reflns_theta_min 2.5 _diffrn_reflns_theta_max 30 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 0 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 9 _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 0 3 -1 0 4 -1 -1 1 -2 _reflns_number_total 5337 _reflns_number_gt 4398 _reflns_threshold_expression 'I > 2\s(I)' _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_R_factor_all 0.0550 _refine_ls_R_factor_gt 0.0383 _refine_ls_wR_factor_all 0.0396 _refine_ls_wR_factor_ref 0.0386 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_ref 2.200 _refine_ls_restrained_S_all ? _refine_ls_number_reflns 4398 _refine_ls_number_parameters 198 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_hydrogen_treatment refU _refine_ls_weighting_scheme sigma _refine_ls_weighting_details 'w=1/[\s^2^(F~o~)+(0.005F~o~)^2^]' _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean ? _refine_diff_density_max 2.31 _refine_diff_density_min -2.12 _refine_ls_extinction_method 'Zachariasen (1963)' _refine_ls_extinction_coef 1.8E-6(1) _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 0.00000 0.00000 0.00000 0.03401(15) Uani d ? S 1 ? Hg Hg2 0.21586(3) -0.21696(2) 0.36228(4) 0.02723(10) Uani d ? . 1 . Hg Cl1 -0.22481(19) -0.05156(16) 0.0342(3) 0.0339(6) Uani d ? . 1 . Cl Cl2 0.0786(2) -0.23234(16) 0.1300(3) 0.0418(8) Uani d ? . 1 . Cl Cl3 0.45688(19) -0.15944(14) 0.2166(3) 0.0308(6) Uani d ? . 1 . Cl Cl4 0.2307(2) -0.39314(15) 0.5343(3) 0.0330(6) Uani d ? . 1 . Cl Cl5 0.0895(2) -0.11267(15) 0.6232(3) 0.0354(6) Uani d ? . 1 . Cl Cl6 0.2874(2) 0.36338(16) 0.4862(3) 0.0389(7) Uani d ? . 1 . Cl N1 0.4770(8) 0.0724(5) 0.2840(9) 0.039(3) Uani d ? . 1 . N C2 0.3415(10) 0.0747(6) 0.3784(12) 0.042(3) Uani d ? . 1 . C C3 0.2802(9) 0.1644(7) 0.4447(11) 0.036(3) Uani d ? . 1 . C C4 0.3625(8) 0.2487(6) 0.4119(9) 0.025(2) Uani d ? . 1 . C C5 0.5014(9) 0.2444(6) 0.3187(10) 0.031(3) Uani d ? . 1 . C C6 0.5590(10) 0.1536(7) 0.2530(11) 0.041(3) Uani d ? . 1 . C Cl7 -0.4724(2) -0.45326(18) 1.2083(3) 0.0378(7) Uani d ? . 1 . Cl N21 -0.0582(6) -0.3942(6) 0.8109(8) 0.031(2) Uani d ? . 1 . N C22 -0.1042(8) -0.4889(7) 0.8448(10) 0.033(3) Uani d ? . 1 . C C23 -0.2321(8) -0.5115(6) 0.9670(10) 0.030(3) Uani d ? . 1 . C C24 -0.3116(7) -0.4303(6) 1.0525(9) 0.026(2) Uani d ? . 1 . C C25 -0.2618(8) -0.3331(6) 1.0169(10) 0.028(2) Uani d ? . 1 . C C26 -0.1333(8) -0.3164(7) 0.8931(10) 0.032(3) Uani d ? . 1 . C H1 0.517 0.010 0.237 0.07(2) Uiso calc N1 ? 1 . H H2 0.288 0.015 0.399 0.04(2) Uiso calc C2 ? 1 . H H3 0.184 0.168 0.511 0.06(2) Uiso calc C3 ? 1 . H H5 0.557 0.303 0.300 0.04(2) Uiso calc C5 ? 1 . H H6 0.655 0.149 0.187 0.10(2) Uiso calc C6 ? 1 . H H21 0.031 -0.382 0.725 0.06(2) Uiso calc N21 ? 1 . H H22 -0.047 -0.542 0.783 0.06(2) Uiso calc C22 ? 1 . H H23 -0.265 -0.579 0.992 0.024(18) Uiso calc C23 ? 1 . H H25 -0.316 -0.279 1.077 0.05(2) Uiso calc C25 ? 1 . H H26 -0.097 -0.250 0.866 0.05(2) 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 0.0243(2) 0.0378(3) 0.0390(2) -0.00639(2) -0.00424(2) -0.0071(2) Hg Hg2 0.02805(2) 0.02555(2) 0.026930(10) -0.001940(10) -0.004310(10) -0.003740(10) Hg Cl1 0.0208(9) 0.0337(11) 0.0465(11) -0.0025(8) -0.0028(8) -0.0160(9) Cl Cl2 0.0611(14) 0.0276(11) 0.0506(12) -0.0019(10) -0.0393(11) -0.0024(9) Cl Cl3 0.0254(9) 0.0247(9) 0.0375(9) -0.0013(8) 0.0000(7) -0.0019(8) Cl Cl4 0.0300(10) 0.0238(9) 0.0366(9) 0.0038(8) 0.0039(8) 0.0022(8) Cl Cl5 0.0394(11) 0.0316(11) 0.0291(9) -0.0038(9) 0.0057(8) -0.0123(8) Cl Cl6 0.0526(13) 0.0301(11) 0.0356(10) 0.0060(10) -0.0128(9) -0.0110(8) Cl N1 0.057(5) 0.026(4) 0.034(4) 0.009(4) -0.012(3) -0.005(3) N C2 0.061(6) 0.022(4) 0.048(5) -0.010(4) -0.022(5) 0.001(4) C C3 0.035(5) 0.031(5) 0.042(4) -0.004(4) -0.011(4) 0.000(4) C C4 0.037(4) 0.021(4) 0.019(3) 0.002(3) -0.010(3) -0.001(3) C C5 0.039(5) 0.025(4) 0.031(4) -0.005(4) -0.010(3) -0.001(3) C C6 0.052(6) 0.042(5) 0.028(4) 0.006(5) -0.012(4) -0.002(4) C Cl7 0.0257(10) 0.0492(13) 0.0342(10) -0.0084(9) 0.0023(8) -0.0062(9) Cl N21 0.020(3) 0.044(4) 0.026(3) -0.002(3) -0.002(2) -0.001(3) N C22 0.027(4) 0.037(5) 0.033(4) 0.004(4) -0.004(3) -0.008(4) C C23 0.033(4) 0.029(4) 0.028(4) 0.000(4) -0.006(3) -0.005(3) C C24 0.026(4) 0.034(4) 0.020(3) -0.006(3) -0.006(3) -0.004(3) C C25 0.030(4) 0.026(4) 0.027(3) -0.001(3) -0.007(3) -0.006(3) C C26 0.033(4) 0.037(5) 0.030(4) -0.003(4) -0.013(3) -0.002(3) C