#------------------------------------------------------------------------------
#$Date: 2016-02-20 00:18:51 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176760 $
#$URL: svn://www.crystallography.net/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
'Matković-Čalogović, Dubravka'
'Mrvoš-Sermek, Draginja'
'Popović, Zora'
'Soldin, Željka'
_publ_section_title
;A new complex of HgBr₂ and pyrimidine-2-thione:
 (pyrimidine-2-thionato-κS)(pyrimidinium-2-thionato-κS)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       θ/2θ
_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/[σ²(Fo²)+(0.0814P)²+0.022P] where P=(Fo²+2Fc²)/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>2σ(I)
_cod_data_source_file            gd1289.cif
_cod_data_source_block           I
_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_original_sg_symbol_H-M      'F d d d'
_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)
