#------------------------------------------------------------------------------
#$Date: 2016-02-21 02:03:34 +0200 (Sun, 21 Feb 2016) $
#$Revision: 176798 $
#$URL: svn://www.crystallography.net/cod/cif/2/23/79/2237916.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_2237916
loop_
_publ_author_name
'Shihabuddeen Syed, A.'
'Rajarajan, K.'
'NizamMohideen, M.'
_publ_section_title
;
 (Thiocyanato-κS)tris(thiourea-κS)mercury(II) chloride
;
_journal_coeditor_code           JJ2165
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              i33
_journal_paper_doi               10.1107/S1600536813011847
_journal_volume                  69
_journal_year                    2013
_chemical_formula_iupac          '[Hg (N C S) (C H4 N2 S)3] Cl'
_chemical_formula_moiety         'C4 H12 Cl Hg N7 S4 +, Cl -'
_chemical_formula_sum            'C4 H12 Cl Hg N7 S4'
_chemical_formula_weight         522.49
_chemical_name_systematic
;
(Thiocyanato-κS)tris(thiourea-κS)mercury(II) chloride
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   8.2175(3)
_cell_length_b                   16.3257(8)
_cell_length_c                   22.6793(10)
_cell_measurement_reflns_used    5125
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      31.2
_cell_measurement_theta_min      2.4
_cell_volume                     3042.6(2)
_computing_cell_refinement       'APEX2 and SAINT (Bruker, 2004)'
_computing_data_collection       'APEX2 (Bruker, 2004)'
_computing_data_reduction        'SAINT and XPREP (Bruker, 2004)'
_computing_molecular_graphics
;
ORTEP-3  for Windows (Farrugia, 2012)
and Mercury (Macrae et al., 2008)
;
_computing_publication_material
'WinGX (Farrugia, 2012) and PLATON (Spek, 2009)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type
;
Bruker Kappa APEXII CCD
;
_diffrn_measurement_method       'ω and φ scans'
_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  0.0568
_diffrn_reflns_av_sigmaI/netI    0.0386
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            38987
_diffrn_reflns_theta_full        31.76
_diffrn_reflns_theta_max         31.76
_diffrn_reflns_theta_min         2.50
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    10.832
_exptl_absorpt_correction_T_max  0.2206
_exptl_absorpt_correction_T_min  0.1395
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2004)'
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    2.281
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             1968
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.20
_refine_diff_density_max         2.165
_refine_diff_density_min         -1.209
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     155
_refine_ls_number_reflns         5125
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0663
_refine_ls_R_factor_gt           0.0355
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0291P)²+7.0058P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0705
_refine_ls_wR_factor_ref         0.0816
_reflns_number_gt                3579
_reflns_number_total             5125
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            jj2165.cif
_cod_data_source_block           I
_cod_database_code               2237916
_cod_database_fobs_code          2237916
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'x+1/2, -y+1/2, -z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'-x-1/2, y-1/2, z'
'x, -y-1/2, z-1/2'
loop_
_atom_site_type_symbol
_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_symmetry_multiplicity
C C1 1.2410(5) 0.1993(3) 0.42350(17) 0.0280(8) Uani d . 1 1
C C2 1.0389(5) 0.3016(3) 0.2771(2) 0.0321(9) Uani d . 1 1
C C3 0.7067(6) 0.0234(3) 0.43089(19) 0.0333(9) Uani d . 1 1
C C4 1.2429(7) -0.0184(3) 0.3691(2) 0.0498(13) Uani d . 1 1
N N1 1.3113(5) 0.1934(3) 0.37245(16) 0.0488(12) Uani d . 1 1
H H1A 1.4063 0.2142 0.3671 0.059 Uiso calc R 1 1
H H1B 1.2628 0.1687 0.3439 0.059 Uiso calc R 1 1
N N2 1.3169(5) 0.2370(3) 0.46633(17) 0.0445(10) Uani d . 1 1
H H2A 1.4119 0.2575 0.4604 0.053 Uiso calc R 1 1
H H2B 1.2718 0.2414 0.5004 0.053 Uiso calc R 1 1
N N3 1.0072(6) 0.3302(3) 0.32922(19) 0.0511(11) Uani d . 1 1
H H3A 1.0352 0.3794 0.3383 0.061 Uiso calc R 1 1
H H3B 0.9582 0.2999 0.3547 0.061 Uiso calc R 1 1
N N4 1.1131(6) 0.3476(3) 0.2386(2) 0.0541(12) Uani d . 1 1
H H4A 1.1409 0.3967 0.2477 0.065 Uiso calc R 1 1
H H4B 1.1342 0.3287 0.2040 0.065 Uiso calc R 1 1
N N5 0.6681(6) 0.0872(3) 0.46201(18) 0.0496(11) Uani d . 1 1
H H5A 0.6676 0.0844 0.4999 0.060 Uiso calc R 1 1
H H5B 0.6430 0.1324 0.4448 0.060 Uiso calc R 1 1
N N6 0.7440(8) -0.0438(3) 0.4576(2) 0.0667(15) Uani d . 1 1
H H6A 0.7430 -0.0458 0.4955 0.080 Uiso calc R 1 1
H H6B 0.7698 -0.0865 0.4375 0.080 Uiso calc R 1 1
N N7 1.2853(8) -0.0407(4) 0.4142(2) 0.0779(18) Uani d . 1 1
Hg Hg1 0.92567(2) 0.123362(12) 0.340864(7) 0.03933(7) Uani d . 1 1
S S1 1.05319(12) 0.15817(7) 0.43857(4) 0.0313(2) Uani d . 1 1
S S2 1.18864(19) 0.01386(9) 0.30317(6) 0.0529(4) Uani d . 1 1
S S3 0.70350(17) 0.02592(8) 0.35487(5) 0.0430(3) Uani d . 1 1
S S4 0.98486(18) 0.20568(7) 0.25448(5) 0.0411(3) Uani d . 1 1
Cl Cl1 0.66976(13) 0.27345(7) 0.39858(4) 0.0323(2) Uani d . 1 1
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 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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Hg Hg -2.3894 9.2266 '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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_3
_geom_angle
N1 C1 N2 . 119.0(4)
N1 C1 S1 . 123.3(3)
N2 C1 S1 . 117.7(3)
N3 C2 N4 . 119.9(4)
N3 C2 S4 . 123.4(4)
N4 C2 S4 . 116.7(4)
N6 C3 N5 . 119.1(4)
N6 C3 S3 . 119.6(4)
N5 C3 S3 . 121.4(4)
N7 C4 S2 1 177.9(6)
N7 C4 S2 . 177.9(6)
C1 N1 H1A . 120.0
C1 N1 H1B . 120.0
H1A N1 H1B . 120.0
C1 N2 H2A . 120.0
C1 N2 H2B . 120.0
H2A N2 H2B . 120.0
C2 N3 H3A . 120.0
C2 N3 H3B . 120.0
H3A N3 H3B . 120.0
C2 N4 H4A . 120.0
C2 N4 H4B . 120.0
H4A N4 H4B . 120.0
C3 N5 H5A . 120.0
C3 N5 H5B . 120.0
H5A N5 H5B . 120.0
C3 N6 H6A . 120.0
C3 N6 H6B . 120.0
H6A N6 H6B . 120.0
S4 Hg1 S3 . 128.02(4)
S4 Hg1 S1 . 120.18(4)
S3 Hg1 S1 . 110.11(4)
S4 Hg1 S2 1 87.39(5)
S3 Hg1 S2 1 101.05(5)
S1 Hg1 S2 1 95.02(4)
S4 Hg1 S2 . 87.39(5)
S3 Hg1 S2 . 101.05(5)
S1 Hg1 S2 . 95.02(4)
C1 S1 Hg1 . 106.69(14)
C4 S2 Hg1 . 97.45(18)
C3 S3 Hg1 . 97.71(15)
C2 S4 Hg1 . 108.55(16)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
C1 N1 . 1.297(5)
C1 N2 . 1.309(5)
C1 S1 . 1.717(4)
C2 N3 . 1.297(6)
C2 N4 . 1.302(6)
C2 S4 . 1.707(4)
C3 N6 . 1.290(6)
C3 N5 . 1.298(6)
C3 S3 . 1.725(4)
C4 N7 . 1.141(7)
C4 S2 1 1.647(6)
C4 S2 . 1.647(6)
N1 H1A . 0.8600
N1 H1B . 0.8600
N2 H2A . 0.8600
N2 H2B . 0.8600
N3 H3A . 0.8600
N3 H3B . 0.8600
N4 H4A . 0.8600
N4 H4B . 0.8600
N5 H5A . 0.8600
N5 H5B . 0.8600
N6 H6A . 0.8600
N6 H6B . 0.8600
Hg1 S4 . 2.4250(11)
Hg1 S3 . 2.4422(12)
Hg1 S1 . 2.5162(10)
Hg1 S2 1 2.9320(14)
Hg1 S2 . 2.9320(14)
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
N1 H1A Cl1 1_655 0.86 2.48 3.277(4) 155.2
N1 H1B S2 1 0.86 2.76 3.475(5) 141.5
N2 H2A Cl1 1_655 0.86 2.55 3.335(4) 151.5
N3 H3B Cl1 1 0.86 2.61 3.320(5) 141.0
N4 H4B Cl1 6_656 0.86 2.51 3.370(5) 175.0
N5 H5B Cl1 1 0.86 2.54 3.363(4) 160.8
N5 H5A N7 5_756 0.86 2.11 2.933(7) 160.0
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_site_symmetry_1
_geom_torsion_site_symmetry_4
_geom_torsion
N1 C1 S1 Hg1 . . -14.6(4)
N2 C1 S1 Hg1 . . 166.6(3)
S4 Hg1 S1 C1 . . -32.03(16)
S3 Hg1 S1 C1 . . 161.59(16)
S2 Hg1 S1 C1 1 . 57.87(16)
S2 Hg1 S1 C1 . . 57.87(16)
S2 C4 S2 Hg1 1 . 0E1(10)
S4 Hg1 S2 S2 . 1 0.00(8)
S3 Hg1 S2 S2 . 1 0.00(8)
S1 Hg1 S2 S2 . 1 0.00(8)
S4 Hg1 S2 C4 . . 150.5(2)
S3 Hg1 S2 C4 . . -81.2(2)
S1 Hg1 S2 C4 . . 30.5(2)
S2 Hg1 S2 C4 1 . 0(9)
N6 C3 S3 Hg1 . . -115.5(4)
N5 C3 S3 Hg1 . . 66.4(4)
S4 Hg1 S3 C3 . . -160.34(16)
S1 Hg1 S3 C3 . . 4.69(17)
S2 Hg1 S3 C3 1 . 104.27(17)
S2 Hg1 S3 C3 . . 104.27(17)
N3 C2 S4 Hg1 . . -17.9(5)
N4 C2 S4 Hg1 . . 163.4(4)
S3 Hg1 S4 C2 . . 138.25(16)
S1 Hg1 S4 C2 . . -25.45(17)
S2 Hg1 S4 C2 1 . -119.74(17)
S2 Hg1 S4 C2 . . -119.74(17)
