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#$Date: 2025-08-19 00:06:14 +0300 (Tue, 19 Aug 2025) $
#$Revision: 301780 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/55/80/1558002.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_1558002
loop_
_publ_author_name
'Ahmadi, Mohsen'
'Correia, Jevy'
'Chrysochos, Nicolas'
'Schulzke, Carola'
_publ_section_title
;
 A Mixed-Valence Tetra-Nuclear Nickel Dithiolene Complex: Synthesis,
 Crystal Structure, and the Lability of Its Nickel Sulfur Bonds
;
_journal_issue                   4
_journal_name_full               Inorganics
_journal_page_first              27
_journal_paper_doi               10.3390/inorganics8040027
_journal_volume                  8
_journal_year                    2020
_chemical_formula_moiety         'C12 H10 O3 S2'
_chemical_formula_sum            'C12 H10 O3 S2'
_chemical_formula_weight         266.32
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 107.77(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   30.240(6)
_cell_length_b                   3.9413(8)
_cell_length_c                   20.418(4)
_cell_measurement_reflns_used    8779
_cell_measurement_temperature    170(2)
_cell_measurement_theta_max      51.4
_cell_measurement_theta_min      6.3
_cell_volume                     2317.4(9)
_computing_cell_refinement       'X-Area by STOE & Cie GmbH 2010'
_computing_data_collection       'X-Area by STOE & Cie GmbH 2010'
_computing_data_reduction        'X-Area by STOE & Cie GmbH 2010'
_computing_molecular_graphics    'XP Version 5.1 by Bruker AXS 1998'
_computing_publication_material  'CIFTAB (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXT-2014 (Sheldrick, 2013)'
_diffrn_ambient_temperature      170(2)
_diffrn_detector_area_resol_mean 6.67
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'STOE IPDS2T'
_diffrn_measurement_method       ω
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1321
_diffrn_reflns_av_unetI/netI     0.0997
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_k_max       3
_diffrn_reflns_limit_k_min       -4
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            7984
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.678
_diffrn_reflns_theta_min         3.994
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.451
_exptl_absorpt_correction_T_max  0.8861
_exptl_absorpt_correction_T_min  0.3773
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'face indexed'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.527
_exptl_crystal_description       needle
_exptl_crystal_F_000             1104
_exptl_crystal_size_max          0.495
_exptl_crystal_size_mid          0.174
_exptl_crystal_size_min          0.043
_refine_diff_density_max         0.281
_refine_diff_density_min         -0.378
_refine_diff_density_rms         0.077
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.940
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     155
_refine_ls_number_reflns         2175
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.940
_refine_ls_R_factor_all          0.0944
_refine_ls_R_factor_gt           0.0501
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0583P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1103
_refine_ls_wR_factor_ref         0.1292
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1364
_reflns_number_total             2175
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            mac45a.cif
_cod_data_source_block           MAC45a
_cod_original_cell_volume        2317.5(9)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               1558002
_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   0.808
_shelx_estimated_absorpt_t_max   0.981
_shelxl_version_number           2013-3
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'
'-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
S1 S 0.58882(3) 0.3529(3) 0.34235(5) 0.0382(3) Uani 1 1 d . . . . .
S2 S 0.68470(3) 0.2658(3) 0.43166(5) 0.0368(3) Uani 1 1 d . . . . .
O1 O 0.65582(10) 0.0840(8) 0.30106(14) 0.0531(8) Uani 1 1 d . . . . .
O2 O 0.56548(9) 0.7764(7) 0.50151(13) 0.0435(7) Uani 1 1 d . . . . .
O3 O 0.52474(8) 0.6537(7) 0.39249(13) 0.0398(7) Uani 1 1 d . . . . .
C1 C 0.64521(15) 0.2122(10) 0.34860(19) 0.0398(9) Uani 1 1 d . . . . .
C2 C 0.60163(13) 0.4827(9) 0.42842(18) 0.0332(8) Uani 1 1 d . . . . .
C3 C 0.64543(13) 0.4352(9) 0.47035(18) 0.0308(8) Uani 1 1 d . . . . .
C4 C 0.56311(13) 0.6532(9) 0.44662(19) 0.0333(9) Uani 1 1 d . . . . .
C5 C 0.48419(13) 0.8278(11) 0.4006(2) 0.0429(10) Uani 1 1 d . . . . .
H5A H 0.4941 1.0295 0.4304 0.052 Uiso 1 1 calc R U . . .
H5B H 0.4669 0.6744 0.4225 0.052 Uiso 1 1 calc R U . . .
C6 C 0.45402(15) 0.9328(12) 0.3317(2) 0.0509(11) Uani 1 1 d . . . . .
H6A H 0.4719 1.0741 0.3093 0.076 Uiso 1 1 calc R U . . .
H6B H 0.4276 1.0627 0.3366 0.076 Uiso 1 1 calc R U . . .
H6C H 0.4427 0.7308 0.3036 0.076 Uiso 1 1 calc R U . . .
C7 C 0.66548(13) 0.5035(9) 0.54473(18) 0.0320(8) Uani 1 1 d . . . . .
C8 C 0.70830(13) 0.6638(10) 0.56955(18) 0.0343(9) Uani 1 1 d . . . . .
H8 H 0.7241 0.7362 0.5382 0.041 Uiso 1 1 calc R U . . .
C9 C 0.72839(14) 0.7196(10) 0.63965(19) 0.0388(9) Uani 1 1 d . . . . .
H9 H 0.7579 0.8256 0.6563 0.047 Uiso 1 1 calc R U . . .
C10 C 0.70490(14) 0.6191(11) 0.6849(2) 0.0407(10) Uani 1 1 d . . . . .
H10 H 0.7178 0.6648 0.7327 0.049 Uiso 1 1 calc R U . . .
C11 C 0.66273(14) 0.4525(10) 0.66094(19) 0.0388(9) Uani 1 1 d . . . . .
H11 H 0.6472 0.3802 0.6926 0.047 Uiso 1 1 calc R U . . .
C12 C 0.64292(13) 0.3903(10) 0.59147(19) 0.0364(9) Uani 1 1 d . . . . .
H12 H 0.6143 0.2718 0.5755 0.044 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'
O O 0.0106 0.0060 '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
_geom_angle_publ_flag
C2 S1 C1 96.10(19) . . ?
C3 S2 C1 97.27(19) . . ?
C4 O3 C5 117.0(3) . . ?
O1 C1 S1 123.8(3) . . ?
O1 C1 S2 123.3(3) . . ?
S1 C1 S2 112.9(2) . . ?
C3 C2 C4 126.5(3) . . ?
C3 C2 S1 117.9(3) . . ?
C4 C2 S1 115.6(3) . . ?
C2 C3 C7 129.8(3) . . ?
C2 C3 S2 115.8(3) . . ?
C7 C3 S2 114.3(3) . . ?
O2 C4 O3 124.0(3) . . ?
O2 C4 C2 125.9(3) . . ?
O3 C4 C2 110.0(3) . . ?
O3 C5 C6 108.5(3) . . ?
O3 C5 H5A 110.0 . . ?
C6 C5 H5A 110.0 . . ?
O3 C5 H5B 110.0 . . ?
C6 C5 H5B 110.0 . . ?
H5A C5 H5B 108.4 . . ?
C5 C6 H6A 109.5 . . ?
C5 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
C5 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C8 C7 C12 119.2(3) . . ?
C8 C7 C3 120.1(3) . . ?
C12 C7 C3 120.5(3) . . ?
C7 C8 C9 120.8(4) . . ?
C7 C8 H8 119.6 . . ?
C9 C8 H8 119.6 . . ?
C10 C9 C8 119.3(4) . . ?
C10 C9 H9 120.3 . . ?
C8 C9 H9 120.3 . . ?
C11 C10 C9 120.3(4) . . ?
C11 C10 H10 119.9 . . ?
C9 C10 H10 119.9 . . ?
C12 C11 C10 120.7(4) . . ?
C12 C11 H11 119.6 . . ?
C10 C11 H11 119.6 . . ?
C11 C12 C7 119.5(4) . . ?
C11 C12 H12 120.3 . . ?
C7 C12 H12 120.3 . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
S1 C2 1.756(4) . ?
S1 C1 1.761(4) . ?
S2 C3 1.747(4) . ?
S2 C1 1.764(4) . ?
O1 C1 1.221(5) . ?
O2 C4 1.203(4) . ?
O3 C4 1.336(4) . ?
O3 C5 1.458(4) . ?
C2 C3 1.353(5) . ?
C2 C4 1.487(5) . ?
C3 C7 1.478(5) . ?
C5 C6 1.484(6) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C7 C8 1.390(5) . ?
C7 C12 1.404(5) . ?
C8 C9 1.391(5) . ?
C8 H8 0.9500 . ?
C9 C10 1.384(6) . ?
C9 H9 0.9500 . ?
C10 C11 1.384(5) . ?
C10 H10 0.9500 . ?
C11 C12 1.383(5) . ?
C11 H11 0.9500 . ?
C12 H12 0.9500 . ?
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 PubChem 12650108
