#------------------------------------------------------------------------------ #$Date: 2011-09-10 06:16:28 +0300 (Sat, 10 Sep 2011) $ #$Revision: 25271 $ #$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/. The original data for this entry # were provided by IUCr Journals, http://journals.iucr.org/. # # The file may be used within the scientific community so long as # proper attribution is given to the journal article from which the # data were obtained. # data_2003135 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_issue 3 _journal_name_full 'Acta Crystallographica Section B' _journal_page_first 396 _journal_page_last 409 _journal_volume 55 _journal_year 1999 _chemical_formula_moiety '(C5 H5 Cl N 1+)4, Hg3 Cl10 4-' _chemical_formula_structural '(C5 H5 Cl N 1+)4, Hg Cl2, (Hg Cl4 2-)2' _chemical_formula_sum 'C20 H20 Cl14 Hg3 N4' _chemical_formula_weight 1414.52 _chemical_melting_point 374.0(10) _chemical_name_common ' ?' _chemical_name_systematic ; tetrakis(4-chloropyridinium) decachlorotrimercurate(II) ; _space_group_IT_number 2 _symmetry_cell_setting triclinic _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' _cell_angle_alpha 84.41(2) _cell_angle_beta 74.81(2) _cell_angle_gamma 87.34(2) _cell_formula_units_Z 1 _cell_length_a 9.907(3) _cell_length_b 13.226(2) _cell_length_c 7.282(2) _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 916.2(4) _computing_cell_refinement ; MSC/AFC Diffractometer Control Software (Molecular Structure Corporation, 1991) ; _computing_data_collection ; MSC/AFC Diffractometer Control Software (Molecular Structure Corporation, 1991) ; _computing_data_reduction ; TEXSAN PROCESS (Molecular Structure Corporation, 1989) ; _computing_molecular_graphics 'ORTEPIII (Burnett & Johnson, 1996)' _computing_publication_material ; TEXSAN FINISH (Molecular Structure Corporation, 1989) and local programs ; _computing_structure_refinement ; TEXSAN LS (Molecular Structure Corporation, 1989) ; _computing_structure_solution 'DIRDIF92 Patterson (Beurskens et al., 1992)' _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 .71069 _diffrn_reflns_av_R_equivalents .019 _diffrn_reflns_limit_h_max 0 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_number 5621 _diffrn_reflns_theta_max 30 _diffrn_reflns_theta_min 2.5 _diffrn_standards_decay_% 'no decay' _diffrn_standards_interval_count 150 _diffrn_standards_number 3 _exptl_absorpt_coefficient_mu 13.58 _exptl_absorpt_correction_T_max .270 _exptl_absorpt_correction_T_min .055 _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details '(De Meulenaer & Tompa, 1965)' _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 2.564 _exptl_crystal_density_meas 'not measured' _exptl_crystal_description prism _exptl_crystal_F_000 646 _exptl_crystal_size_max .43 _exptl_crystal_size_mid .27 _exptl_crystal_size_min .11 _refine_diff_density_max 2.31 _refine_diff_density_min -2.12 _refine_ls_abs_structure_details ' ?' _refine_ls_extinction_coef 1.8E-6(1) _refine_ls_extinction_method 'Zachariasen (1963)' _refine_ls_goodness_of_fit_ref 2.200 _refine_ls_hydrogen_treatment refU _refine_ls_matrix_type full _refine_ls_number_constraints 0 _refine_ls_number_parameters 198 _refine_ls_number_reflns 4398 _refine_ls_number_restraints 0 _refine_ls_R_factor_all .0550 _refine_ls_R_factor_gt .0383 _refine_ls_shift/su_max .003 _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 .0396 _refine_ls_wR_factor_ref .0386 _reflns_number_gt 4398 _reflns_number_total 5337 _reflns_threshold_expression 'I > 2\s(I)' _[local]_cod_data_source_file sh0124.cif _[local]_cod_data_source_block III _cod_depositor_comments ; The following automatic conversions were performed: '_chemical_melting_point' value '373-375' was changed to '374.0(10)' - the average value was taken and precision was estimated. Automatic conversion script Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana ; _cod_database_code 2003135 loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-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_type_symbol Hg1 .00000 .00000 .00000 .03401(15) Uani d ? S 1 Hg Hg2 .21586(3) -.21696(2) .36228(4) .02723(10) Uani d ? . 1 Hg Cl1 -.22481(19) -.05156(16) .0342(3) .0339(6) Uani d ? . 1 Cl Cl2 .0786(2) -.23234(16) .1300(3) .0418(8) Uani d ? . 1 Cl Cl3 .45688(19) -.15944(14) .2166(3) .0308(6) Uani d ? . 1 Cl Cl4 .2307(2) -.39314(15) .5343(3) .0330(6) Uani d ? . 1 Cl Cl5 .0895(2) -.11267(15) .6232(3) .0354(6) Uani d ? . 1 Cl Cl6 .2874(2) .36338(16) .4862(3) .0389(7) Uani d ? . 1 Cl N1 .4770(8) .0724(5) .2840(9) .039(3) Uani d ? . 1 N C2 .3415(10) .0747(6) .3784(12) .042(3) Uani d ? . 1 C C3 .2802(9) .1644(7) .4447(11) .036(3) Uani d ? . 1 C C4 .3625(8) .2487(6) .4119(9) .025(2) Uani d ? . 1 C C5 .5014(9) .2444(6) .3187(10) .031(3) Uani d ? . 1 C C6 .5590(10) .1536(7) .2530(11) .041(3) Uani d ? . 1 C Cl7 -.4724(2) -.45326(18) 1.2083(3) .0378(7) Uani d ? . 1 Cl N21 -.0582(6) -.3942(6) .8109(8) .031(2) Uani d ? . 1 N C22 -.1042(8) -.4889(7) .8448(10) .033(3) Uani d ? . 1 C C23 -.2321(8) -.5115(6) .9670(10) .030(3) Uani d ? . 1 C C24 -.3116(7) -.4303(6) 1.0525(9) .026(2) Uani d ? . 1 C C25 -.2618(8) -.3331(6) 1.0169(10) .028(2) Uani d ? . 1 C C26 -.1333(8) -.3164(7) .8931(10) .032(3) Uani d ? . 1 C H1 .517 .010 .237 .07(2) Uiso calc N1 ? 1 H H2 .288 .015 .399 .04(2) Uiso calc C2 ? 1 H H3 .184 .168 .511 .06(2) Uiso calc C3 ? 1 H H5 .557 .303 .300 .04(2) Uiso calc C5 ? 1 H H6 .655 .149 .187 .10(2) Uiso calc C6 ? 1 H H21 .031 -.382 .725 .06(2) Uiso calc N21 ? 1 H H22 -.047 -.542 .783 .06(2) Uiso calc C22 ? 1 H H23 -.265 -.579 .992 .024(18) Uiso calc C23 ? 1 H H25 -.316 -.279 1.077 .05(2) Uiso calc C25 ? 1 H H26 -.097 -.250 .866 .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 .0243(2) .0378(3) .0390(2) -.00639(2) -.00424(2) -.0071(2) Hg Hg2 .02805(2) .02555(2) .026930(10) -.001940(10) -.004310(10) -.003740(10) Hg Cl1 .0208(9) .0337(11) .0465(11) -.0025(8) -.0028(8) -.0160(9) Cl Cl2 .0611(14) .0276(11) .0506(12) -.0019(10) -.0393(11) -.0024(9) Cl Cl3 .0254(9) .0247(9) .0375(9) -.0013(8) .0000(7) -.0019(8) Cl Cl4 .0300(10) .0238(9) .0366(9) .0038(8) .0039(8) .0022(8) Cl Cl5 .0394(11) .0316(11) .0291(9) -.0038(9) .0057(8) -.0123(8) Cl Cl6 .0526(13) .0301(11) .0356(10) .0060(10) -.0128(9) -.0110(8) Cl N1 .057(5) .026(4) .034(4) .009(4) -.012(3) -.005(3) N C2 .061(6) .022(4) .048(5) -.010(4) -.022(5) .001(4) C C3 .035(5) .031(5) .042(4) -.004(4) -.011(4) .000(4) C C4 .037(4) .021(4) .019(3) .002(3) -.010(3) -.001(3) C C5 .039(5) .025(4) .031(4) -.005(4) -.010(3) -.001(3) C C6 .052(6) .042(5) .028(4) .006(5) -.012(4) -.002(4) C Cl7 .0257(10) .0492(13) .0342(10) -.0084(9) .0023(8) -.0062(9) Cl N21 .020(3) .044(4) .026(3) -.002(3) -.002(2) -.001(3) N C22 .027(4) .037(5) .033(4) .004(4) -.004(3) -.008(4) C C23 .033(4) .029(4) .028(4) .000(4) -.006(3) -.005(3) C C24 .026(4) .034(4) .020(3) -.006(3) -.006(3) -.004(3) C C25 .030(4) .026(4) .027(3) -.001(3) -.007(3) -.006(3) C C26 .033(4) .037(5) .030(4) -.003(4) -.013(3) -.002(3) C loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C .0033 .0016 ; International Tables for Crystallography (1992). Vol.C, Tables 4.2.6.8 and 6.1.1.1 ; H H .0000 .0000 ; International Tables for Crystallography (1992). Vol.C, Tables 4.2.6.8 and 6.1.1.1 ; Cl Cl .1484 .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 .0061 .0033 ; International Tables for Crystallography (1992). Vol.C, Tables 4.2.6.8 and 6.1.1.1 ; 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 loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag Cl1 Hg1 Cl1 . 2 180.0 no Cl1 Hg1 Cl2 . . 88.07(7) no Cl1 Hg1 Cl2 . 2 91.93(7) no Cl1 Hg1 Cl5 . 1_554 87.71(6) no Cl1 Hg1 Cl5 . 2_556 92.29(6) no Cl2 Hg1 Cl2 . 2 180.0 no Cl2 Hg1 Cl5 . 1_554 73.91(6) no Cl2 Hg1 Cl5 . 2_556 106.09(6) no Cl5 Hg1 Cl5 1_554 2_556 180.0 no Cl2 Hg2 Cl3 . . 113.94(7) no Cl2 Hg2 Cl4 . . 107.15(7) no Cl2 Hg2 Cl5 . . 111.63(8) no Cl3 Hg2 Cl4 . . 107.82(7) no Cl3 Hg2 Cl5 . . 112.14(7) no Cl4 Hg2 Cl5 . . 103.41(7) no Hg1 Cl2 Hg2 . . 104.82(7) no Hg1 Cl5 Hg2 2_556 . 164.11(9) no C2 N1 C6 . . 123.1(8) no N1 C2 C3 . . 119.5(8) no C2 C3 C4 . . 118.1(8) no Cl6 C4 C3 . . 119.1(6) no Cl6 C4 C5 . . 119.2(6) no C3 C4 C5 . . 121.6(7) no C4 C5 C6 . . 118.8(8) no N1 C6 C5 . . 118.9(8) no C22 N21 C26 . . 122.2(7) no N21 C22 C23 . . 121.3(7) no C22 C23 C24 . . 116.8(7) no Cl7 C24 C23 . . 119.3(6) no Cl7 C24 C25 . . 119.7(6) no C23 C24 C25 . . 121.1(7) no C24 C25 C26 . . 118.8(7) no N21 C26 C25 . . 119.8(8) no C2 N1 H1 . . 118.4 no C6 N1 H1 . . 118.4 no N1 C2 H2 . . 120.2 no C3 C2 H2 . . 120.2 no C2 C3 H3 . . 121.0 no C4 C3 H3 . . 121.0 no C4 C5 H5 . . 120.6 no C6 C5 H5 . . 120.6 no N1 C6 H6 . . 120.6 no C5 C6 H6 . . 120.6 no C22 N21 H21 . . 118.9 no C26 N21 H21 . . 118.9 no N21 C22 H22 . . 119.3 no C23 C22 H22 . . 119.3 no C22 C23 H23 . . 121.6 no C24 C23 H23 . . 121.6 no C24 C25 H25 . . 120.6 no C26 C25 H25 . . 120.6 no N21 C26 H26 . . 120.1 no C25 C26 H26 . . 120.1 no loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Hg1 Cl1 . 2.3032(19) no Hg1 Cl2 . 3.247(2) no Hg1 Cl5 1_554 3.1518(19) no Hg2 Cl2 . 2.4598(18) no Hg2 Cl3 . 2.4677(19) no Hg2 Cl4 . 2.553(2) no Hg2 Cl5 . 2.4869(19) no Cl6 C4 . 1.729(7) no N1 C2 . 1.339(12) no N1 C6 . 1.343(11) no C2 C3 . 1.378(12) no C3 C4 . 1.376(10) no C4 C5 . 1.367(10) no C5 C6 . 1.379(11) no Cl7 C24 . 1.717(7) no N21 C22 . 1.330(10) no N21 C26 . 1.337(10) no C22 C23 . 1.371(10) no C23 C24 . 1.398(10) no C24 C25 . 1.375(10) no C25 C26 . 1.367(10) no N1 H1 . .95 no C2 H2 . .95 no C3 H3 . .95 no C5 H5 . .95 no C6 H6 . .95 no N21 H21 . .95 no C22 H22 . .95 no C23 H23 . .95 no C25 H25 . .95 no C26 H26 . .95 no loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_publ_flag N1 H1 Cl3 . .95 2.38 3.175(7) 141 no N1 H1 Cl1 1_655 .95 2.73 3.469(8) 135 no N21 H21 Cl4 . .95 2.11 3.037(6) 166 no