#------------------------------------------------------------------------------ #$Date: 2011-09-28 17:24:46 +0300 (Wed, 28 Sep 2011) $ #$Revision: 26848 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/00/31/2003133.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_2003133 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_name_full 'Acta Crystallographica, Section B' _journal_page_first 396 _journal_page_last 409 _journal_volume 55 _journal_year 1999 _chemical_formula_analytical ? _chemical_formula_iupac ? _chemical_formula_moiety 'C5 H5 Cl N 1+, Hg Cl3 1-' _chemical_formula_structural '(C5 H5 Cl N 1+)2, (Hg Cl3 1-), Hg Cl2, Cl 1-' _chemical_formula_sum 'C5 H5 Cl4 Hg N' _chemical_formula_weight 421.49 _chemical_melting_point 378.0(10) _chemical_name_common ' ?' _chemical_name_systematic ; 2-chloropyridinium trichloromercurate(II) ; _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-P 2yn' _symmetry_space_group_name_H-M 'P 1 21/n 1' _cell_angle_alpha 90 _cell_angle_beta 106.13(4) _cell_angle_gamma 90 _cell_formula_units_Z 8 _cell_length_a 9.094(8) _cell_length_b 18.143(4) _cell_length_c 12.902(3) _cell_measurement_reflns_used 25 _cell_measurement_temperature 173.0(10) _cell_measurement_theta_max 20.0 _cell_measurement_theta_min 19.5 _cell_volume 2045(2) _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 0.273 _diffrn_reflns_av_sigmaI/netI ? _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_number 5129 _diffrn_reflns_reduction_process ? _diffrn_reflns_theta_max 27.5 _diffrn_reflns_theta_min 2.5 _diffrn_standards_decay_% 'no decay' _diffrn_standards_interval_count 150 _diffrn_standards_interval_time ? _diffrn_standards_number 3 _exptl_absorpt_coefficient_mu 16.04 _exptl_absorpt_correction_T_max 0.090 _exptl_absorpt_correction_T_min 0.026 _exptl_absorpt_correction_type 'empirical via psi-scan' _exptl_absorpt_process_details '(North, Phillips & Mathews, 1968)' _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 2.738 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_method ? _exptl_crystal_description prism _exptl_crystal_F_000 1520 _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.15 _exptl_crystal_size_rad ? _refine_diff_density_max 1.66 _refine_diff_density_min -2.33 _refine_ls_abs_structure_details ' ?' _refine_ls_abs_structure_Flack ? _refine_ls_extinction_coef 9.3E-8(8) _refine_ls_extinction_method 'Zachariasen (1963)' _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_ref 1.684 _refine_ls_hydrogen_treatment noref _refine_ls_matrix_type full _refine_ls_number_constraints 0 _refine_ls_number_parameters 200 _refine_ls_number_reflns 3153 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all ? _refine_ls_R_factor_all 0.1002 _refine_ls_R_factor_gt 0.0437 _refine_ls_shift/su_max 0.0002 _refine_ls_shift/su_mean ? _refine_ls_structure_factor_coef F _refine_ls_weighting_details w=1/[\s^2^(F~o~)+(0.005F~o~)^2^] _refine_ls_weighting_scheme sigma _refine_ls_wR_factor_all 0.0392 _refine_ls_wR_factor_ref 0.0358 _reflns_number_gt 3153 _reflns_number_total 4679 _reflns_threshold_expression 'I > 2\s(I)' _cod_depositor_comments ; The following automatic conversions were performed: '_chemical_melting_point' value '377-379' was changed to '378.0(10)' - the average value was taken and precision was estimated. Automatic conversion script Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana ; _cod_database_code 2003133 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 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 0.13401(6) 0.04692(3) 0.13608(4) 0.03324(18) Uani d ? . 1 . Hg Hg2 0.26398(6) 0.00416(3) 0.46822(3) 0.03023(17) Uani d ? . 1 . Hg Cl1 0.1802(3) -0.05881(15) 0.0335(2) 0.0248(10) Uani d ? . 1 . Cl Cl2 0.0080(3) 0.03031(16) 0.2800(2) 0.0276(10) Uani d ? . 1 . Cl Cl3 0.2063(4) 0.17045(16) 0.1019(2) 0.0279(10) Uani d ? . 1 . Cl Cl4 0.2795(4) 0.12691(17) 0.5241(2) 0.0347(11) Uani d ? . 1 . Cl Cl5 0.4371(3) 0.01605(15) 0.3200(2) 0.0264(10) Uani d ? . 1 . Cl Cl6 0.2392(4) -0.12373(17) 0.4683(2) 0.0369(12) Uani d ? . 1 . Cl Cl7 0.6412(4) -0.05774(17) 0.1025(3) 0.0425(13) Uani d ? . 1 . Cl N1 0.4981(11) -0.1340(5) 0.2147(7) 0.026(4) Uani d ? . 1 . N C2 0.5716(12) -0.1372(6) 0.1377(8) 0.022(4) Uani d ? . 1 . C C3 0.5874(13) -0.2044(7) 0.0922(8) 0.024(4) Uani d ? . 1 . C C4 0.5298(14) -0.2665(6) 0.1280(8) 0.025(4) Uani d ? . 1 . C C5 0.4548(15) -0.2609(7) 0.2069(9) 0.030(5) Uani d ? . 1 . C C6 0.4387(15) -0.1935(7) 0.2499(8) 0.030(5) Uani d ? . 1 . C Cl8 0.6674(4) 0.1408(2) 0.1466(3) 0.0599(16) Uani d ? . 1 . Cl N21 0.5387(11) 0.1780(5) 0.2937(7) 0.025(4) Uani d ? . 1 . N C22 0.5934(13) 0.2036(7) 0.2158(8) 0.024(4) Uani d ? . 1 . C C23 0.5908(16) 0.2777(7) 0.1946(9) 0.035(5) Uani d ? . 1 . C C24 0.5280(18) 0.3256(8) 0.2562(12) 0.057(7) Uani d ? . 1 . C C25 0.4776(16) 0.2969(10) 0.3378(11) 0.052(6) Uani d ? . 1 . C C26 0.4813(16) 0.2231(9) 0.3554(9) 0.046(6) Uani d ? . 1 . C H1 0.488 -0.087 0.246 0.031 Uiso calc N1 ? 1 . H H3 0.638 -0.208 0.037 0.029 Uiso calc C3 ? 1 . H H4 0.542 -0.313 0.098 0.030 Uiso calc C4 ? 1 . H H5 0.414 -0.304 0.231 0.036 Uiso calc C5 ? 1 . H H6 0.386 -0.189 0.304 0.036 Uiso calc C6 ? 1 . H H21 0.540 0.126 0.306 0.031 Uiso calc N21 ? 1 . H H31 0.631 0.296 0.139 0.042 Uiso calc C23 ? 1 . H H41 0.521 0.377 0.241 0.068 Uiso calc C24 ? 1 . H H51 0.440 0.329 0.383 0.063 Uiso calc C25 ? 1 . H H61 0.444 0.203 0.411 0.055 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 0.0408(3) 0.0252(3) 0.0342(3) -0.0022(3) 0.0113(2) -0.0032(2) Hg Hg2 0.0278(3) 0.0277(3) 0.0342(2) 0.0019(3) 0.0070(2) -0.0017(2) Hg Cl1 0.0237(16) 0.0235(16) 0.0275(14) -0.0015(13) 0.0077(12) -0.0032(12) Cl Cl2 0.0245(17) 0.0304(18) 0.0249(13) 0.0048(14) 0.0019(12) 0.0017(12) Cl Cl3 0.0299(18) 0.0302(17) 0.0245(14) -0.0038(15) 0.0093(13) -0.0006(12) Cl Cl4 0.040(2) 0.0308(18) 0.0312(15) 0.0092(16) 0.0053(15) -0.0083(13) Cl Cl5 0.0296(17) 0.0226(16) 0.0265(13) 0.0021(13) 0.0072(12) -0.0020(11) Cl Cl6 0.040(2) 0.0279(18) 0.0353(16) -0.0072(16) -0.0016(15) 0.0056(14) Cl Cl7 0.048(2) 0.0248(18) 0.059(2) -0.0079(17) 0.0218(18) 0.0058(15) Cl N1 0.022(6) 0.027(6) 0.028(5) 0.000(5) 0.005(4) -0.003(4) N C2 0.007(6) 0.029(7) 0.026(6) -0.008(5) 0.000(5) 0.000(5) C C3 0.011(6) 0.034(8) 0.026(6) -0.004(6) 0.004(5) -0.003(5) C C4 0.024(7) 0.026(7) 0.026(6) 0.003(6) 0.009(5) -0.002(5) C C5 0.039(8) 0.025(7) 0.031(6) -0.008(6) 0.016(6) 0.004(5) C C6 0.038(8) 0.038(8) 0.019(6) -0.007(7) 0.014(6) 0.006(5) C Cl8 0.043(3) 0.080(3) 0.053(2) 0.024(2) 0.0065(19) -0.026(2) Cl N21 0.031(6) 0.024(6) 0.020(5) -0.003(5) 0.005(4) 0.006(4) N C22 0.011(6) 0.031(7) 0.025(6) 0.002(6) -0.002(5) -0.001(5) C C23 0.036(9) 0.033(8) 0.033(7) 0.001(7) 0.004(6) 0.016(6) C C24 0.052(11) 0.024(8) 0.069(11) -0.002(8) -0.025(9) 0.001(7) C C25 0.023(8) 0.077(13) 0.047(9) 0.015(9) -0.007(7) -0.038(9) C C26 0.032(9) 0.075(12) 0.025(7) 0.007(9) 0.001(6) 0.006(7) C 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_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 1 2 3 1 0 3 2 0 2