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#$Date: 2021-09-07 09:45:48 +0300 (Tue, 07 Sep 2021) $
#$Revision: 268996 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/56/45/1564551.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.
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data_1564551
loop_
_publ_author_name
'Rodina, Tatyana A.'
'Loseva, Olga V.'
'Smolentsev, Anton I.'
'Antzutkin, Oleg N.'
'Ivanov, Alexander V.'
_publ_section_title
;
 Crystal structure, solid-state 13C and 15N NMR characterisation,
 chemisorption activity and thermal behaviour of new mercury(II)
 dipropyldithiocarbamate: Binuclear, pseudo-binuclear and heteronuclear
 complexes of [Hg2(PrDtc)4], [Hg(PrDtc)2]2 and [Au(PrDtc)2]2[Hg2Cl6]
;
_journal_name_full               'Inorganica Chimica Acta'
_journal_page_first              119630
_journal_paper_doi               10.1016/j.ica.2020.119630
_journal_volume                  508
_journal_year                    2020
_chemical_formula_moiety         'C28 H56 Hg2 N4 S8'
_chemical_formula_sum            'C28 H56 Hg2 N4 S8'
_chemical_formula_weight         1106.42
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_cell_angle_alpha                90
_cell_angle_beta                 108.247(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.4211(5)
_cell_length_b                   14.8838(8)
_cell_length_c                   12.3249(7)
_cell_measurement_reflns_used    6352
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.50
_cell_measurement_theta_min      3.24
_cell_volume                     1989.75(18)
_computing_cell_refinement       'SAINT (Bruker, 2004)'
_computing_data_collection       'APEX2 (Bruker, 2004)'
_computing_data_reduction        'SAINT (Bruker, 2004)'
_computing_molecular_graphics    'SHELXTL (Bruker, 2004)'
_computing_publication_material  'SHELXTL (Bruker, 2004)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXS-2013/1 (Sheldrick, 2013)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 25
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker Nonius X8Apex CCD area-detector'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0265
_diffrn_reflns_av_unetI/netI     0.0311
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            13514
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.250
_diffrn_reflns_theta_max         27.545
_diffrn_reflns_theta_min         1.877
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    8.151
_exptl_absorpt_correction_T_max  0.2712
_exptl_absorpt_correction_T_min  0.1504
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 2004)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.847
_exptl_crystal_description       prism
_exptl_crystal_F_000             1080
_exptl_crystal_size_max          0.370
_exptl_crystal_size_mid          0.300
_exptl_crystal_size_min          0.220
_refine_diff_density_max         1.398
_refine_diff_density_min         -1.563
_refine_diff_density_rms         0.104
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     194
_refine_ls_number_reflns         4567
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.070
_refine_ls_R_factor_all          0.0318
_refine_ls_R_factor_gt           0.0240
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0201P)²+1.2036P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0510
_refine_ls_wR_factor_ref         0.0526
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3930
_reflns_number_total             4567
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ICA-2020-508-119630.cif
_cod_data_source_block           1
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               1564551
_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_min   0.152
_shelx_estimated_absorpt_t_max   0.267
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -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 0.18229(2) 0.48556(2) 0.59613(2) 0.02772(5) Uani 1 1 d . . . . .
S1 S 0.19950(8) 0.48019(6) 0.79859(7) 0.02533(18) Uani 1 1 d . . . . .
S2 S 0.35926(7) 0.36117(6) 0.71388(8) 0.02831(19) Uani 1 1 d . . . . .
S3 S 0.20021(7) 0.56517(5) 0.43160(7) 0.02250(17) Uani 1 1 d . . . . .
S4 S -0.00632(6) 0.63519(5) 0.50913(6) 0.01880(16) Uani 1 1 d . . . . .
N1 N 0.3501(2) 0.35881(18) 0.9258(2) 0.0194(5) Uani 1 1 d . . . . .
N2 N 0.0505(2) 0.69437(17) 0.3266(2) 0.0168(5) Uani 1 1 d . . . . .
C1 C 0.3096(2) 0.3949(2) 0.8223(3) 0.0176(6) Uani 1 1 d . . . . .
C2 C 0.3084(3) 0.3889(2) 1.0208(3) 0.0238(7) Uani 1 1 d . . . . .
H2A H 0.310380 0.337347 1.072095 0.029 Uiso 1 1 calc R U . . .
H2B H 0.221927 0.409634 0.990178 0.029 Uiso 1 1 calc R U . . .
C3 C 0.3867(3) 0.4644(2) 1.0896(3) 0.0290(8) Uani 1 1 d . . . . .
H3A H 0.472694 0.443226 1.123326 0.035 Uiso 1 1 calc R U . . .
H3B H 0.387208 0.515514 1.038359 0.035 Uiso 1 1 calc R U . . .
C4 C 0.3375(4) 0.4952(3) 1.1835(4) 0.0429(10) Uani 1 1 d . . . . .
H4A H 0.254176 0.519346 1.149835 0.064 Uiso 1 1 calc R U . . .
H4B H 0.391442 0.542065 1.228570 0.064 Uiso 1 1 calc R U . . .
H4C H 0.335028 0.444218 1.233006 0.064 Uiso 1 1 calc R U . . .
C5 C 0.4379(3) 0.2840(2) 0.9522(3) 0.0245(7) Uani 1 1 d . . . . .
H5A H 0.488446 0.287054 1.033638 0.029 Uiso 1 1 calc R U . . .
H5B H 0.493881 0.289331 0.905358 0.029 Uiso 1 1 calc R U . . .
C6 C 0.3716(3) 0.1939(2) 0.9285(3) 0.0293(8) Uani 1 1 d . . . . .
H6A H 0.310033 0.190946 0.969851 0.035 Uiso 1 1 calc R U . . .
H6B H 0.327129 0.188639 0.845757 0.035 Uiso 1 1 calc R U . . .
C7 C 0.4614(3) 0.1163(2) 0.9658(3) 0.0352(9) Uani 1 1 d . . . . .
H7A H 0.522966 0.119480 0.925617 0.053 Uiso 1 1 calc R U . . .
H7B H 0.416436 0.059306 0.947522 0.053 Uiso 1 1 calc R U . . .
H7C H 0.502755 0.119831 1.048373 0.053 Uiso 1 1 calc R U . . .
C8 C 0.0766(2) 0.63781(19) 0.4136(3) 0.0152(6) Uani 1 1 d . . . . .
C9 C 0.1272(3) 0.7003(2) 0.2504(3) 0.0212(7) Uani 1 1 d . . . . .
H9A H 0.077644 0.727140 0.176878 0.025 Uiso 1 1 calc R U . . .
H9B H 0.150714 0.638827 0.234472 0.025 Uiso 1 1 calc R U . . .
C10 C 0.2436(3) 0.7559(2) 0.2998(3) 0.0262(7) Uani 1 1 d . . . . .
H10A H 0.221035 0.816678 0.319001 0.031 Uiso 1 1 calc R U . . .
H10B H 0.295995 0.727421 0.371134 0.031 Uiso 1 1 calc R U . . .
C11 C 0.3160(3) 0.7636(3) 0.2157(3) 0.0353(9) Uani 1 1 d . . . . .
H11A H 0.338157 0.703414 0.196397 0.053 Uiso 1 1 calc R U . . .
H11B H 0.391144 0.798580 0.250212 0.053 Uiso 1 1 calc R U . . .
H11C H 0.265329 0.793759 0.146136 0.053 Uiso 1 1 calc R U . . .
C12 C -0.0596(3) 0.7526(2) 0.2942(3) 0.0230(7) Uani 1 1 d . . . . .
H12A H -0.114074 0.734875 0.339227 0.028 Uiso 1 1 calc R U . . .
H12B H -0.105568 0.742806 0.212525 0.028 Uiso 1 1 calc R U . . .
C13 C -0.0297(3) 0.8514(2) 0.3133(3) 0.0258(7) Uani 1 1 d . . . . .
H13A H -0.106862 0.886319 0.283507 0.031 Uiso 1 1 calc R U . . .
H13B H 0.025429 0.868838 0.268817 0.031 Uiso 1 1 calc R U . . .
C14 C 0.0319(3) 0.8764(2) 0.4379(3) 0.0333(8) Uani 1 1 d . . . . .
H14A H -0.021343 0.858568 0.482965 0.050 Uiso 1 1 calc R U . . .
H14B H 0.045288 0.941526 0.444120 0.050 Uiso 1 1 calc R U . . .
H14C H 0.111247 0.845391 0.466753 0.050 Uiso 1 1 calc R U . . .
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'
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
S3 Hg1 S1 150.95(3) . .
S3 Hg1 S4 99.73(3) . 3_566
S1 Hg1 S4 106.16(3) . 3_566
S3 Hg1 S2 121.67(3) . .
S1 Hg1 S2 68.49(3) . .
S4 Hg1 S2 96.72(3) 3_566 .
S3 Hg1 S4 65.31(2) . .
S1 Hg1 S4 101.84(2) . .
S4 Hg1 S4 88.83(2) 3_566 .
S2 Hg1 S4 169.86(2) . .
C1 S1 Hg1 91.03(11) . .
C1 S2 Hg1 81.11(10) . .
C8 S3 Hg1 97.68(10) . .
C8 S4 Hg1 99.90(10) . 3_566
C8 S4 Hg1 77.19(10) . .
Hg1 S4 Hg1 91.17(2) 3_566 .
C1 N1 C2 122.8(3) . .
C1 N1 C5 122.0(3) . .
C2 N1 C5 115.2(3) . .
C8 N2 C9 121.8(2) . .
C8 N2 C12 123.4(2) . .
C9 N2 C12 114.8(2) . .
N1 C1 S2 122.7(2) . .
N1 C1 S1 118.1(2) . .
S2 C1 S1 119.23(18) . .
N1 C2 C3 113.0(3) . .
N1 C2 H2A 109.0 . .
C3 C2 H2A 109.0 . .
N1 C2 H2B 109.0 . .
C3 C2 H2B 109.0 . .
H2A C2 H2B 107.8 . .
C4 C3 C2 111.0(3) . .
C4 C3 H3A 109.4 . .
C2 C3 H3A 109.4 . .
C4 C3 H3B 109.4 . .
C2 C3 H3B 109.4 . .
H3A C3 H3B 108.0 . .
C3 C4 H4A 109.5 . .
C3 C4 H4B 109.5 . .
H4A C4 H4B 109.5 . .
C3 C4 H4C 109.5 . .
H4A C4 H4C 109.5 . .
H4B C4 H4C 109.5 . .
N1 C5 C6 111.2(2) . .
N1 C5 H5A 109.4 . .
C6 C5 H5A 109.4 . .
N1 C5 H5B 109.4 . .
C6 C5 H5B 109.4 . .
H5A C5 H5B 108.0 . .
C7 C6 C5 111.4(3) . .
C7 C6 H6A 109.4 . .
C5 C6 H6A 109.4 . .
C7 C6 H6B 109.4 . .
C5 C6 H6B 109.4 . .
H6A C6 H6B 108.0 . .
C6 C7 H7A 109.5 . .
C6 C7 H7B 109.5 . .
H7A C7 H7B 109.5 . .
C6 C7 H7C 109.5 . .
H7A C7 H7C 109.5 . .
H7B C7 H7C 109.5 . .
N2 C8 S4 122.3(2) . .
N2 C8 S3 117.9(2) . .
S4 C8 S3 119.77(17) . .
N2 C9 C10 113.4(3) . .
N2 C9 H9A 108.9 . .
C10 C9 H9A 108.9 . .
N2 C9 H9B 108.9 . .
C10 C9 H9B 108.9 . .
H9A C9 H9B 107.7 . .
C11 C10 C9 111.2(3) . .
C11 C10 H10A 109.4 . .
C9 C10 H10A 109.4 . .
C11 C10 H10B 109.4 . .
C9 C10 H10B 109.4 . .
H10A C10 H10B 108.0 . .
C10 C11 H11A 109.5 . .
C10 C11 H11B 109.5 . .
H11A C11 H11B 109.5 . .
C10 C11 H11C 109.5 . .
H11A C11 H11C 109.5 . .
H11B C11 H11C 109.5 . .
N2 C12 C13 113.4(2) . .
N2 C12 H12A 108.9 . .
C13 C12 H12A 108.9 . .
N2 C12 H12B 108.9 . .
C13 C12 H12B 108.9 . .
H12A C12 H12B 107.7 . .
C12 C13 C14 114.0(3) . .
C12 C13 H13A 108.8 . .
C14 C13 H13A 108.8 . .
C12 C13 H13B 108.8 . .
C14 C13 H13B 108.8 . .
H13A C13 H13B 107.7 . .
C13 C14 H14A 109.5 . .
C13 C14 H14B 109.5 . .
H14A C14 H14B 109.5 . .
C13 C14 H14C 109.5 . .
H14A C14 H14C 109.5 . .
H14B C14 H14C 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Hg1 S3 2.4121(8) .
Hg1 S1 2.4421(9) .
Hg1 S4 2.7055(8) 3_566
Hg1 S2 2.7897(8) .
Hg1 S4 3.0501(8) .
S1 C1 1.746(3) .
S2 C1 1.683(3) .
S3 C8 1.736(3) .
S4 C8 1.727(3) .
N1 C1 1.327(4) .
N1 C2 1.465(4) .
N1 C5 1.465(4) .
N2 C8 1.322(4) .
N2 C9 1.474(4) .
N2 C12 1.475(4) .
C2 C3 1.518(5) .
C2 H2A 0.9900 .
C2 H2B 0.9900 .
C3 C4 1.508(5) .
C3 H3A 0.9900 .
C3 H3B 0.9900 .
C4 H4A 0.9800 .
C4 H4B 0.9800 .
C4 H4C 0.9800 .
C5 C6 1.522(5) .
C5 H5A 0.9900 .
C5 H5B 0.9900 .
C6 C7 1.518(4) .
C6 H6A 0.9900 .
C6 H6B 0.9900 .
C7 H7A 0.9800 .
C7 H7B 0.9800 .
C7 H7C 0.9800 .
C9 C10 1.522(4) .
C9 H9A 0.9900 .
C9 H9B 0.9900 .
C10 C11 1.519(4) .
C10 H10A 0.9900 .
C10 H10B 0.9900 .
C11 H11A 0.9800 .
C11 H11B 0.9800 .
C11 H11C 0.9800 .
C12 C13 1.511(4) .
C12 H12A 0.9900 .
C12 H12B 0.9900 .
C13 C14 1.521(5) .
C13 H13A 0.9900 .
C13 H13B 0.9900 .
C14 H14A 0.9800 .
C14 H14B 0.9800 .
C14 H14C 0.9800 .
