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#$Date: 2022-11-23 10:46:17 +0200 (Wed, 23 Nov 2022) $
#$Revision: 279493 $
#$URL: file:///home/coder/svn-repositories/cod/cif/8/10/62/8106212.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_8106212
loop_
_publ_author_name
'Liu, Lian-Wei'
'Zhao, Bang-Tun'
_publ_section_title
;
 The crystal structure of
 catena-poly[chlorido-(μ2-5-methyl-1,3,4-thiadiazole-2-thiolato-κ2
 S:N)mercury(II)], C3H3ClHgN2S2
;
_journal_issue                   4
_journal_name_full
'Zeitschrift für Kristallographie - New Crystal Structures'
_journal_page_first              547
_journal_page_last               548
_journal_paper_doi               10.1515/ncrs-2017-0277
_journal_volume                  233
_journal_year                    2018
_chemical_formula_moiety         'C3 H3 Cl Hg N2 S2'
_chemical_formula_sum            'C3 H3 Cl Hg N2 S2'
_chemical_formula_weight         367.23
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_atom_sites_solution_hydrogens   geom
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.794(8)
_cell_length_b                   4.0798(17)
_cell_length_c                   10.093(4)
_cell_measurement_reflns_used    8942
_cell_measurement_temperature    291(2)
_cell_measurement_theta_max      0.8917
_cell_measurement_theta_min      0.6571
_cell_volume                     773.9(6)
_computing_cell_refinement       'Bruker SMART [1]'
_computing_data_collection       'Bruker SMART [1]'
_computing_data_reduction        'Bruker SAINT [1]'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)[2]'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)[2]'
_computing_structure_refinement  'SHELXL (Sheldrick, 2015)[3]'
_computing_structure_solution    'SHELXS (Sheldrick, 2015)[3]'
_diffrn_ambient_temperature      291.15
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0533
_diffrn_reflns_av_unetI/netI     0.0707
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       5
_diffrn_reflns_limit_k_min       -5
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            5143
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.278
_diffrn_reflns_theta_min         2.962
_exptl_absorpt_coefficient_mu    20.685
_exptl_absorpt_correction_T_max  0.4185
_exptl_absorpt_correction_T_min  0.1315
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    3.152
_exptl_crystal_description       block
_exptl_crystal_F_000             656
_exptl_crystal_size_max          0.165
_exptl_crystal_size_mid          0.092
_exptl_crystal_size_min          0.051
_exptl_transmission_factor_max   0.8714
_exptl_transmission_factor_min   0.5892
_refine_diff_density_max         1.789
_refine_diff_density_min         -1.745
_refine_diff_density_rms         0.230
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.09(2)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     84
_refine_ls_number_reflns         1849
_refine_ls_number_restraints     43
_refine_ls_restrained_S_all      1.009
_refine_ls_R_factor_all          0.0693
_refine_ls_R_factor_gt           0.0437
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0410P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0922
_refine_ls_wR_factor_ref         0.1024
_reflns_Friedel_coverage         0.898
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.990
_reflns_number_gt                1354
_reflns_number_total             1849
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            suppl_ncrs-2017-0277_suppl.cif
_cod_data_source_block           a
_cod_original_cell_volume        773.8(6)
_cod_database_code               8106212
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_max   0.418
_shelx_estimated_absorpt_t_min   0.132
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.91(2)
 0.09(2)
2. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups
3. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.02 and sigma
for terminal atoms of 0.04
4.a Idealised Me refined as rotating group:
 C3(H3A,H3B,H3C)
;
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z+1/2'
'x+1/2, -y+1/2, z'
'-x+1/2, y+1/2, z+1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Hg1 Hg 1.05409(4) 1.19998(15) 0.01403(8) 0.0499(2) Uani 1 1 d . U . . .
Cl1 Cl 1.1325(3) 1.5467(15) 0.1282(6) 0.0642(14) Uani 1 1 d . U . . .
S1 S 0.8364(3) 0.5636(13) 0.0571(4) 0.0497(12) Uani 1 1 d . U . . .
S2 S 0.9645(3) 0.8633(13) -0.0819(5) 0.0513(13) Uani 1 1 d . U . . .
N1 N 0.9365(10) 0.869(4) 0.1863(16) 0.050(4) Uani 1 1 d . U . . .
N2 N 0.8866(10) 0.760(4) 0.2774(16) 0.051(4) Uani 1 1 d . U . . .
C1 C 0.9193(13) 0.776(4) 0.0618(18) 0.045(4) Uani 1 1 d . U . . .
C2 C 0.8300(11) 0.601(4) 0.2295(18) 0.042(4) Uani 1 1 d . U . . .
C3 C 0.7713(13) 0.476(5) 0.311(2) 0.060(6) Uani 1 1 d . U . . .
H3A H 0.774175 0.241065 0.315337 0.090 Uiso 1 1 calc GR . . . .
H3B H 0.726778 0.538356 0.271805 0.090 Uiso 1 1 calc GR . . . .
H3C H 0.774689 0.565630 0.398478 0.090 Uiso 1 1 calc GR . . . .
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'
Cl Cl 0.1484 0.1585 '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'
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'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
Cl1 Hg1 S2 173.2(2) . .
Cl1 Hg1 N2 98.1(4) . 2_774
S2 Hg1 N2 88.1(4) . 2_774
C2 S1 C1 89.5(9) . .
C1 S2 Hg1 97.3(7) . .
C1 N1 N2 111.4(17) . .
N1 N2 Hg1 107.1(12) . 2_775
C2 N2 Hg1 133.9(13) . 2_775
C2 N2 N1 117.0(16) . .
S2 C1 S1 120.7(11) . .
N1 C1 S1 111.7(16) . .
N1 C1 S2 127.4(18) . .
N2 C2 S1 110.3(14) . .
N2 C2 C3 124.4(18) . .
C3 C2 S1 125.3(16) . .
C2 C3 H3A 109.5 . .
C2 C3 H3B 109.5 . .
C2 C3 H3C 109.5 . .
H3A C3 H3B 109.5 . .
H3A C3 H3C 109.5 . .
H3B C3 H3C 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Hg1 Cl1 2.345(5) .
Hg1 S2 2.379(6) .
Hg1 N2 2.640(17) 2_774
S1 C1 1.78(2) .
S1 C2 1.751(19) .
S2 C1 1.72(2) .
N1 N2 1.39(2) .
N1 C1 1.35(2) .
N2 C2 1.34(3) .
C2 C3 1.47(3) .
C3 H3A 0.9600 .
C3 H3B 0.9600 .
C3 H3C 0.9600 .
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
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
Hg1 S2 C1 S1 172.2(11) . . . .
Hg1 S2 C1 N1 -3(2) . . . .
Hg1 N2 C2 S1 -159.9(11) 2_775 . . .
Hg1 N2 C2 C3 20(3) 2_775 . . .
N1 N2 C2 S1 2(2) . . . .
N1 N2 C2 C3 -178.6(19) . . . .
N2 N1 C1 S1 3(2) . . . .
N2 N1 C1 S2 178.5(15) . . . .
C1 S1 C2 N2 -0.1(15) . . . .
C1 S1 C2 C3 -179.7(19) . . . .
C1 N1 N2 Hg1 163.2(14) . . . 2_775
C1 N1 N2 C2 -3(3) . . . .
C2 S1 C1 S2 -177.6(13) . . . .
C2 S1 C1 N1 -1.6(16) . . . .
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.91(2)
2 0.09(2)
