#------------------------------------------------------------------------------ #$Date: 2011-09-10 06:16:28 +0300 (Sat, 10 Sep 2011) $ #$Revision: 25271 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/2003133.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_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_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+, 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) ; _space_group_IT_number 14 _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) _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 'SHELXS86 Patterson (Sheldrick, 1990)' _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 .273 _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_theta_max 27.5 _diffrn_reflns_theta_min 2.5 _diffrn_standards_decay_% 'no decay' _diffrn_standards_interval_count 150 _diffrn_standards_number 3 _exptl_absorpt_coefficient_mu 16.04 _exptl_absorpt_correction_T_max .090 _exptl_absorpt_correction_T_min .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_description prism _exptl_crystal_F_000 1520 _exptl_crystal_size_max .40 _exptl_crystal_size_mid .25 _exptl_crystal_size_min .15 _refine_diff_density_max 1.66 _refine_diff_density_min -2.33 _refine_ls_abs_structure_details ' ?' _refine_ls_extinction_coef 9.3E-8(8) _refine_ls_extinction_method 'Zachariasen (1963)' _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_R_factor_all .1002 _refine_ls_R_factor_gt .0437 _refine_ls_shift/su_max .0002 _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 .0392 _refine_ls_wR_factor_ref .0358 _reflns_number_gt 3153 _reflns_number_total 4679 _reflns_threshold_expression 'I > 2\s(I)' _[local]_cod_data_source_file sh0124.cif _[local]_cod_data_source_block 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 1715 2011-07-08 13:25:40Z 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_occupancy _atom_site_type_symbol Hg1 .13401(6) .04692(3) .13608(4) .03324(18) Uani d ? 1 Hg Hg2 .26398(6) .00416(3) .46822(3) .03023(17) Uani d ? 1 Hg Cl1 .1802(3) -.05881(15) .0335(2) .0248(10) Uani d ? 1 Cl Cl2 .0080(3) .03031(16) .2800(2) .0276(10) Uani d ? 1 Cl Cl3 .2063(4) .17045(16) .1019(2) .0279(10) Uani d ? 1 Cl Cl4 .2795(4) .12691(17) .5241(2) .0347(11) Uani d ? 1 Cl Cl5 .4371(3) .01605(15) .3200(2) .0264(10) Uani d ? 1 Cl Cl6 .2392(4) -.12373(17) .4683(2) .0369(12) Uani d ? 1 Cl Cl7 .6412(4) -.05774(17) .1025(3) .0425(13) Uani d ? 1 Cl N1 .4981(11) -.1340(5) .2147(7) .026(4) Uani d ? 1 N C2 .5716(12) -.1372(6) .1377(8) .022(4) Uani d ? 1 C C3 .5874(13) -.2044(7) .0922(8) .024(4) Uani d ? 1 C C4 .5298(14) -.2665(6) .1280(8) .025(4) Uani d ? 1 C C5 .4548(15) -.2609(7) .2069(9) .030(5) Uani d ? 1 C C6 .4387(15) -.1935(7) .2499(8) .030(5) Uani d ? 1 C Cl8 .6674(4) .1408(2) .1466(3) .0599(16) Uani d ? 1 Cl N21 .5387(11) .1780(5) .2937(7) .025(4) Uani d ? 1 N C22 .5934(13) .2036(7) .2158(8) .024(4) Uani d ? 1 C C23 .5908(16) .2777(7) .1946(9) .035(5) Uani d ? 1 C C24 .5280(18) .3256(8) .2562(12) .057(7) Uani d ? 1 C C25 .4776(16) .2969(10) .3378(11) .052(6) Uani d ? 1 C C26 .4813(16) .2231(9) .3554(9) .046(6) Uani d ? 1 C H1 .488 -.087 .246 .031 Uiso calc N1 1 H H3 .638 -.208 .037 .029 Uiso calc C3 1 H H4 .542 -.313 .098 .030 Uiso calc C4 1 H H5 .414 -.304 .231 .036 Uiso calc C5 1 H H6 .386 -.189 .304 .036 Uiso calc C6 1 H H21 .540 .126 .306 .031 Uiso calc N21 1 H H31 .631 .296 .139 .042 Uiso calc C23 1 H H41 .521 .377 .241 .068 Uiso calc C24 1 H H51 .440 .329 .383 .063 Uiso calc C25 1 H H61 .444 .203 .411 .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 .0408(3) .0252(3) .0342(3) -.0022(3) .0113(2) -.0032(2) Hg Hg2 .0278(3) .0277(3) .0342(2) .0019(3) .0070(2) -.0017(2) Hg Cl1 .0237(16) .0235(16) .0275(14) -.0015(13) .0077(12) -.0032(12) Cl Cl2 .0245(17) .0304(18) .0249(13) .0048(14) .0019(12) .0017(12) Cl Cl3 .0299(18) .0302(17) .0245(14) -.0038(15) .0093(13) -.0006(12) Cl Cl4 .040(2) .0308(18) .0312(15) .0092(16) .0053(15) -.0083(13) Cl Cl5 .0296(17) .0226(16) .0265(13) .0021(13) .0072(12) -.0020(11) Cl Cl6 .040(2) .0279(18) .0353(16) -.0072(16) -.0016(15) .0056(14) Cl Cl7 .048(2) .0248(18) .059(2) -.0079(17) .0218(18) .0058(15) Cl N1 .022(6) .027(6) .028(5) .000(5) .005(4) -.003(4) N C2 .007(6) .029(7) .026(6) -.008(5) .000(5) .000(5) C C3 .011(6) .034(8) .026(6) -.004(6) .004(5) -.003(5) C C4 .024(7) .026(7) .026(6) .003(6) .009(5) -.002(5) C C5 .039(8) .025(7) .031(6) -.008(6) .016(6) .004(5) C C6 .038(8) .038(8) .019(6) -.007(7) .014(6) .006(5) C Cl8 .043(3) .080(3) .053(2) .024(2) .0065(19) -.026(2) Cl N21 .031(6) .024(6) .020(5) -.003(5) .005(4) .006(4) N C22 .011(6) .031(7) .025(6) .002(6) -.002(5) -.001(5) C C23 .036(9) .033(8) .033(7) .001(7) .004(6) .016(6) C C24 .052(11) .024(8) .069(11) -.002(8) -.025(9) .001(7) C C25 .023(8) .077(13) .047(9) .015(9) -.007(7) -.038(9) C C26 .032(9) .075(12) .025(7) .007(9) .001(6) .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 .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 1 2 3 1 0 3 2 0 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 . 3 86.28(9) yes Cl1 Hg1 Cl2 . . 120.13(9) yes Cl1 Hg1 Cl3 . . 122.45(10) yes Cl1 Hg1 Cl5 . . 91.29(9) yes Cl2 Hg1 Cl1 . 3 90.57(10) yes Cl2 Hg1 Cl3 . . 117.42(10) yes Cl2 Hg1 Cl5 . . 84.44(10) yes Cl3 Hg1 Cl1 . 3 92.92(9) yes Cl3 Hg1 Cl5 . . 94.43(9) yes Cl1 Hg1 Cl5 3 . 172.43(8) yes Cl2 Hg2 Cl4 . . 93.91(9) yes Cl2 Hg2 Cl5 . . 83.59(10) yes Cl2 Hg2 Cl5 . 3_656 176.65(8) yes Cl2 Hg2 Cl6 . . 96.21(9) yes Cl4 Hg2 Cl5 . . 98.04(10) yes Cl4 Hg2 Cl5 . 3_656 83.39(9) yes Cl4 Hg2 Cl6 . . 161.35(11) yes Cl5 Hg2 Cl5 . 3_656 94.81(8) yes Cl5 Hg2 Cl6 . . 98.62(10) yes Cl6 Hg2 Cl5 . 3_656 86.93(9) yes Hg1 Cl1 Hg1 . 3 93.72(9) yes Hg1 Cl2 Hg2 . . 102.63(12) yes Hg2 Cl5 Hg1 . . 89.30(10) yes Hg1 Cl5 Hg2 . 3_656 173.03(10) yes Hg2 Cl5 Hg2 . 3_656 85.19(8) yes C2 N1 C6 . . 123.2(10) no Cl7 C2 N1 . . 117.6(9) no Cl7 C2 C3 . . 123.4(9) no N1 C2 C3 . . 119.0(10) no C2 C3 C4 . . 119.1(10) no C3 C4 C5 . . 120.1(11) no C4 C5 C6 . . 119.8(11) no N1 C6 C5 . . 118.8(11) no C22 N21 C26 . . 121.8(11) no Cl8 C22 N21 . . 116.8(9) no Cl8 C22 C23 . . 122.7(10) no N21 C22 C23 . . 120.4(11) no C22 C23 C24 . . 118.8(12) no C23 C24 C25 . . 118.6(13) no C24 C25 C26 . . 120.5(13) no N21 C26 C25 . . 119.8(13) no C2 N1 H1 . . 118.4 no C6 N1 H1 . . 118.4 no C2 C3 H3 . . 120.4 no C4 C3 H3 . . 120.4 no C3 C4 H4 . . 120.0 no C5 C4 H4 . . 120.0 no C4 C5 H5 . . 120.1 no C6 C5 H5 . . 120.1 no N1 C6 H6 . . 120.6 no C5 C6 H6 . . 120.6 no C22 N21 H21 . . 119.1 no C26 N21 H21 . . 119.1 no C22 C23 H31 . . 120.6 no C24 C23 H31 . . 120.6 no C23 C24 H41 . . 120.7 no C25 C24 H41 . . 120.7 no C24 C25 H51 . . 119.8 no C26 C25 H51 . . 119.7 no N21 C26 H61 . . 120.1 no C25 C26 H61 . . 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 . 2.432(3) yes Hg1 Cl1 3 3.086(4) yes Hg1 Cl2 . 2.456(3) yes Hg1 Cl3 . 2.411(3) yes Hg1 Cl5 . 3.148(4) yes Hg2 Cl2 . 2.898(3) yes Hg2 Cl4 . 2.333(3) yes Hg2 Cl5 . 2.803(3) yes Hg2 Cl5 3_656 3.296(3) yes Hg2 Cl6 . 2.331(3) yes Cl7 C2 . 1.686(11) no N1 C2 . 1.344(13) no N1 C6 . 1.341(14) no C2 C3 . 1.378(15) no C3 C4 . 1.376(15) no C4 C5 . 1.377(15) no C5 C6 . 1.368(16) no Cl8 C22 . 1.699(12) no N21 C22 . 1.323(13) no N21 C26 . 1.343(16) no C22 C23 . 1.370(15) no C23 C24 . 1.402(19) no C24 C25 . 1.36(2) no C25 C26 . 1.36(2) no N1 H1 . .95 no C3 H3 . .95 no C4 H4 . .95 no C5 H5 . .95 no C6 H6 . .95 no N21 H21 . .95 no C23 H31 . .95 no C24 H41 . .95 no C25 H51 . .95 no C26 H61 . .95 no loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_publ_flag N1 H1 Cl5 .95 2.22 3.161(10) 173 no N21 H21 Cl5 .95 2.24 3.127(10) 155 no