#------------------------------------------------------------------------------ #$Date: 2010-01-30 15:59:17 +0200 (Sat, 30 Jan 2010) $ #$Revision: 966 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/2003136.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_2003136 _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 ; 3-chloropyridinium trichloromercurate(II) ; _chemical_name_common ; ? ; _chemical_formula_moiety 'C5 H5 Cl N 1+, Hg Cl3 1-' _chemical_formula_sum 'C5 H5 Cl4 Hg N' _chemical_formula_structural '(C5 H5 Cl N 1+)2, (Hg2 Cl6 2-)' _chemical_formula_analytical ? _chemical_formula_iupac ? _chemical_formula_weight 421.49 _chemical_melting_point '367-370' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1' _symmetry_space_group_name_Hall '-P 2ybc' 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' _cell_length_a 7.243(5) _cell_length_b 22.145(8) _cell_length_c 12.320(3) _cell_angle_alpha 90 _cell_angle_beta 99.52(3) _cell_angle_gamma 90 _cell_volume 1948.8(13) _cell_formula_units_Z 8 _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 0.38 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.28 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 2.873 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_method ? _exptl_crystal_F_000 1520 _exptl_absorpt_coefficient_mu 16.83 _exptl_absorpt_correction_type 'empirical via psi-scan' _exptl_absorpt_process_details '(North, Phillips & Mathews, 1968)' _exptl_absorpt_correction_T_min 0.004 _exptl_absorpt_correction_T_max 0.009 _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 6239 _diffrn_reflns_av_R_equivalents 0.073 _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 31 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _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 -2 -3 2 3 0 _reflns_number_total 5681 _reflns_number_gt 4100 _reflns_threshold_expression 'I > 2\s(I)' _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_R_factor_all 0.0879 _refine_ls_R_factor_gt 0.0486 _refine_ls_wR_factor_all 0.0513 _refine_ls_wR_factor_ref 0.0489 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_ref 2.014 _refine_ls_restrained_S_all ? _refine_ls_number_reflns 4100 _refine_ls_number_parameters 200 _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 0.001 _refine_ls_shift/su_mean ? _refine_diff_density_max 4.06 _refine_diff_density_min -2.79 _refine_ls_extinction_method 'Zachariasen (1963)' _refine_ls_extinction_coef 1.9E-7(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 -0.05411(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 _cod_database_code 2003136