#------------------------------------------------------------------------------ #$Date: 2015-01-23 14:30:19 +0200 (Fri, 23 Jan 2015) $ #$Revision: 130086 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/01/37/2013790.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_2013790 loop_ _publ_author_name 'Matkovi\'c-\S)(pyrimidinium-2-thionato-\kS)mercury(II) tetrabromomercury(II) ; _journal_issue 2 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first m44 _journal_page_last m46 _journal_paper_doi 10.1107/S0108270103028014 _journal_volume 60 _journal_year 2004 _chemical_formula_iupac '[Hg (C4 H4 N2 S) (C4 H3 N2 S)]2 [Hg Br4]' _chemical_formula_moiety '2C8 H7 Hg N4 S2 + , Br4 Hg 2-' _chemical_formula_sum 'C16 H14 Br4 Hg3 N8 S4' _chemical_formula_weight 1368.00 _chemical_name_systematic ; (pyrimidine-2-thionato-\kS)(pyrimidinium-2-thionato-\kS)mercury(II) tetrabromomercury(II) ; _space_group_IT_number 70 _symmetry_cell_setting orthorhombic _symmetry_space_group_name_Hall '-F 2uv 2vw' _symmetry_space_group_name_H-M 'F d d d :2' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL97 _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 8 _cell_length_a 9.0573(7) _cell_length_b 17.1999(13) _cell_length_c 37.754(9) _cell_measurement_reflns_used 65 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 17.6 _cell_measurement_theta_min 10.2 _cell_volume 5881.5(15) _computing_cell_refinement 'X-RED (Stoe & Cie, 1995)' _computing_data_collection 'STADI4 (Stoe & Cie, 1995)' _computing_data_reduction X-RED _computing_molecular_graphics 'PLATON98 (Spek, 1990)' _computing_publication_material SHELXL97 _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS97 (Sheldrick, 1990)' _diffrn_ambient_temperature 293(2) _diffrn_measured_fraction_theta_full 0.988 _diffrn_measured_fraction_theta_max 0.988 _diffrn_measurement_device_type 'Philips PW1100 updated by Stoe' _diffrn_measurement_method \q/2\q _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.078 _diffrn_reflns_av_sigmaI/netI 0.066 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_h_min -3 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_k_min -2 _diffrn_reflns_limit_l_max 52 _diffrn_reflns_limit_l_min -1 _diffrn_reflns_number 3401 _diffrn_reflns_theta_full 29.91 _diffrn_reflns_theta_max 29.91 _diffrn_reflns_theta_min 3.71 _diffrn_standards_decay_% 6.1 _diffrn_standards_interval_time 90 _diffrn_standards_number 5 _exptl_absorpt_coefficient_mu 21.366 _exptl_absorpt_correction_T_max 0.328 _exptl_absorpt_correction_T_min 0.022 _exptl_absorpt_correction_type integration _exptl_absorpt_process_details '(X-RED; Stoe & Cie, 1995)' _exptl_crystal_colour yellow _exptl_crystal_density_diffrn 3.090 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_description Plate _exptl_crystal_F_000 4880 _exptl_crystal_size_max 0.488 _exptl_crystal_size_mid 0.400 _exptl_crystal_size_min 0.052 _refine_diff_density_max 2.39 _refine_diff_density_min -3.63 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.033 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 81 _refine_ls_number_reflns 2115 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.033 _refine_ls_R_factor_all 0.101 _refine_ls_R_factor_gt 0.054 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w = 1/[\s^2^(Fo^2^)+(0.0814P)^2^+0.022P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.126 _refine_ls_wR_factor_ref 0.145 _reflns_number_gt 1288 _reflns_number_total 2115 _reflns_threshold_expression I>2\s(I) _[local]_cod_data_source_file gd1289.cif _[local]_cod_data_source_block I _[local]_cod_cif_authors_sg_H-M 'F d d d' _cod_depositor_comments ; The following automatic conversions were performed: '_symmetry_cell_setting' value 'Orthorhombic' changed to 'orthorhombic' according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29. Automatic conversion script Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius The following automatic conversions were performed: '_symmetry_cell_setting' value 'Orthorhombic' changed to 'orthorhombic' according to /home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29. Automatic conversion script Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana The following automatic conversions were performed: '_exptl_crystal_density_meas' value 'none' was changed to '?' - the value is perceived as not measured. Automatic conversion script Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas ; _cod_database_code 2013790 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y+1/4, -z+1/4' '-x+1/4, y, -z+1/4' '-x+1/4, -y+1/4, z' 'x, y+1/2, z+1/2' 'x, -y+3/4, -z+3/4' '-x+1/4, y+1/2, -z+3/4' '-x+1/4, -y+3/4, z+1/2' 'x+1/2, y, z+1/2' 'x+1/2, -y+1/4, -z+3/4' '-x+3/4, y, -z+3/4' '-x+3/4, -y+1/4, z+1/2' 'x+1/2, y+1/2, z' 'x+1/2, -y+3/4, -z+1/4' '-x+3/4, y+1/2, -z+1/4' '-x+3/4, -y+3/4, z' '-x, -y, -z' '-x, y-1/4, z-1/4' 'x-1/4, -y, z-1/4' 'x-1/4, y-1/4, -z' '-x, -y+1/2, -z+1/2' '-x, y+1/4, z+1/4' 'x-1/4, -y+1/2, z+1/4' 'x-1/4, y+1/4, -z+1/2' '-x+1/2, -y, -z+1/2' '-x+1/2, y-1/4, z+1/4' 'x+1/4, -y, z+1/4' 'x+1/4, y-1/4, -z+1/2' '-x+1/2, -y+1/2, -z' '-x+1/2, y+1/4, z-1/4' 'x+1/4, -y+1/2, z-1/4' 'x+1/4, y+1/4, -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_refinement_flags _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_type_symbol Hg2 0.1250 0.1250 0.1250 0.0451(2) Uani d S 1 . . Hg Hg1 0.1250 0.1250 0.011593(15) 0.0579(2) Uani d S 1 . . Hg Br -0.03274(11) 0.03698(6) 0.08365(3) 0.0518(3) Uani d . 1 . . Br S 0.2248(3) -0.00143(18) 0.00846(7) 0.0574(7) Uani d . 1 . . S C1 0.3261(10) 0.0145(5) -0.0290(3) 0.044(2) Uani d . 1 . . C N1 0.3286(10) 0.0854(4) -0.0433(3) 0.053(2) Uani d . 1 . . N C2 0.4080(13) 0.0962(7) -0.0729(3) 0.058(3) Uani d . 1 . . C H2 0.4080 0.1448 -0.0837 0.070 Uiso calc R 1 . . H C3 0.4887(13) 0.0373(7) -0.0876(3) 0.060(3) Uani d . 1 . . C H3 0.5481 0.0460 -0.1073 0.072 Uiso calc R 1 . . H C4 0.4800(11) -0.0346(7) -0.0725(3) 0.060(3) Uani d . 1 . . C H4 0.5313 -0.0760 -0.0826 0.072 Uiso calc R 1 . . H N2 0.3973(10) -0.0465(5) -0.0431(3) 0.057(2) Uani d . 1 . . N H 0.3907 -0.0918 -0.0337 0.069 Uiso calc PR 0.50 . . 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 Hg2 0.0524(4) 0.0478(4) 0.0352(4) 0.000 0.000 0.000 Hg1 0.0678(4) 0.0663(4) 0.0395(3) 0.0121(3) 0.000 0.000 Br 0.0573(5) 0.0529(5) 0.0453(5) -0.0035(4) -0.0063(5) -0.0130(5) S 0.0671(16) 0.0573(15) 0.0479(14) 0.0008(13) -0.0031(13) 0.0152(12) C1 0.045(5) 0.040(4) 0.047(5) -0.006(4) -0.005(4) -0.004(4) N1 0.069(5) 0.032(4) 0.058(5) -0.003(3) 0.006(4) -0.004(4) C2 0.077(7) 0.044(5) 0.053(6) -0.013(5) 0.012(6) -0.007(5) C3 0.062(6) 0.068(7) 0.050(6) 0.003(5) 0.011(5) -0.014(6) C4 0.046(5) 0.059(6) 0.075(8) 0.010(5) -0.002(5) -0.027(6) N2 0.065(5) 0.038(4) 0.068(6) 0.008(4) -0.012(5) -0.008(4) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Hg Hg -2.3894 9.2266 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 0 2 18 2 10 0 0 0 24 4 8 0 6 2 0 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 S Hg1 S . 4 174.25(13) y Br Hg2 Br . 2 113.39(5) y Br Hg2 Br . 3 108.84(5) y Br Hg2 Br 2 3 106.26(5) y Br Hg2 Br . 4 106.26(5) ? Br Hg2 Br 2 4 108.84(5) ? Br Hg2 Br 3 4 113.39(5) ? C1 S Hg1 . . 95.7(3) ? N1 C1 N2 . . 123.3(10) ? N1 C1 S . . 119.3(8) ? N2 C1 S . . 117.4(8) ? C1 N1 C2 . . 118.1(9) ? N1 C2 C3 . . 121.4(11) ? N1 C2 H2 . . 119.3 ? C3 C2 H2 . . 119.3 ? C4 C3 C2 . . 118.3(10) ? C4 C3 H3 . . 120.9 ? C2 C3 H3 . . 120.9 ? N2 C4 C3 . . 120.6(10) ? N2 C4 H4 . . 119.7 ? C3 C4 H4 . . 119.7 ? C1 N2 C4 . . 118.2(9) ? C1 N2 H . . 120.9 ? C4 N2 H . . 120.9 ? 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 S . 2.358(3) y Hg1 S 4 2.358(3) ? Hg2 Br . 2.6020(10) y Hg2 Br 2 2.6020(10) ? Hg2 Br 3 2.6020(10) ? Hg2 Br 4 2.6020(10) ? S C1 . 1.710(10) y C1 N1 . 1.333(12) ? C1 N2 . 1.340(13) ? N1 C2 . 1.343(14) ? C2 C3 . 1.366(16) ? C2 H2 . 0.9300 ? C3 C4 . 1.363(17) ? C3 H3 . 0.9300 ? C4 N2 . 1.356(16) ? C4 H4 . 0.9300 ? N2 H . 0.8600 ? 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 N2 H N2 16_545 0.86 1.98 2.730(12) 145 loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion Hg1 S C1 N1 3.6(8) Hg1 S C1 N2 -175.1(7) N2 C1 N1 C2 -0.8(16) S C1 N1 C2 -179.4(8) C1 N1 C2 C3 -2.4(17) N1 C2 C3 C4 3.9(18) C2 C3 C4 N2 -2.3(17) N1 C1 N2 C4 2.3(15) S C1 N2 C4 -179.0(8) C3 C4 N2 C1 -0.7(15)