A Mixed-Valence Tetra-Nuclear Nickel Dithiolene Complex: Synthesis, Crystal Structure, and the Lability of Its Nickel Sulfur Bonds
Ahmadi, Mohsen; Correia, Jevy; Chrysochos, Nicolas; Schulzke, Carola; Inorganics 8 (2020) 27–; doi:10.3390/inorganics8040027

data_1558002
_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       \w
_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/[\s^2^(Fo^2^)+(0.0583P)^2^] where P=(Fo^2^+2Fc^2^)/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 > 2\s(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_estimated_absorpt_t_min   0.808
_shelx_estimated_absorpt_t_max   0.981
_shelxl_version_number           2013-3
_shelx_res_checksum              39596
_shelx_hkl_checksum              3985