Electronic structure of (MePh~3~P)~2~[Ni^II^(bdtCl~2~)~2~]·2(CH~3~)~2~SO and (MePh~3~P)[Ni^III^(bdtCl~2~)~2~] (bdtCl~2~ = 3,6-dichlorobenzene-1,2-dithiolate)
Adamko Koziskova, Julia; Chen, Yu-Sheng; Grass, Su-Yin; Chuang, Yu-Chun; Hsu, I-Jui; Wang, Yu; Lutz, Martin; Volkov, Anatoliy; Herich, Peter; Vénosová, Barbora; Jelemenská, Ingrid; Bučinský, Lukáš; Breza, Martin; Kožíšek, Jozef; Acta Crystallographica Section B 77 (2021) 919–929; doi:10.1107/S2052520621011495

data_2108904
_publ_section_title
;
 Electronic structure of
 (MePh~3~P)~2~[Ni^II^(bdtCl~2~)~2~]&#x00B7;2(CH~3~)~2~SO and
 (MePh~3~P)[Ni^III^(bdtCl~2~)~2~] (bdtCl~2~ =
 3,6-dichlorobenzene-1,2-dithiolate)
;
_journal_coeditor_code           px5045
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section B'
_journal_page_first              919
_journal_page_last               929
_journal_paper_doi               10.1107/S2052520621011495
_journal_volume                  77
_journal_year                    2021
_chemical_formula_moiety
'C12 H4 Cl4 Ni S4, 2(C2 H6 O S), 2(C19 H18 P)'
_chemical_formula_sum            'C54 H52 Cl4 Ni O2 P2 S6'
_chemical_formula_weight         1187.76
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-06-29
_audit_creation_method
;
Olex2 1.2
(compiled 2018.04.26 svn.r3504 for OlexSys, GUI svn.r5492)
;
_cell_angle_alpha                90
_cell_angle_beta                 90.6510(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   13.87880(10)
_cell_length_b                   11.57650(10)
_cell_length_c                   16.43870(10)
_cell_measurement_reflns_used    564441
_cell_measurement_temperature    100(1)
_cell_measurement_theta_max      39.74
_cell_measurement_theta_min      2.05
_cell_volume                     2641.00(3)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100
_diffrn_detector                 HPAD
_diffrn_detector_area_resol_mean 5.81
_diffrn_detector_type            'Dectris 300K Pilatus3R'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.972
_diffrn_measurement_details      ' 7604 frames, detector distance = 40 mm'
_diffrn_measurement_device       '4-circle diffractometer'
_diffrn_measurement_device_type  'STOE STADIVARI'
_diffrn_measurement_method       'rotation method, \w scans'
_diffrn_radiation_collimation    '0.6 mm diameter'
_diffrn_radiation_monochromator  'Graded multilayer mirror'
_diffrn_radiation_polarisn_norm  270
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Ag K\a'
_diffrn_radiation_wavelength     0.56083
_diffrn_reflns_av_R_equivalents  0.0460
_diffrn_reflns_av_unetI/netI     0.0231
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.972
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            423226
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.972
_diffrn_reflns_theta_full        19.664
_diffrn_reflns_theta_max         39.840
_diffrn_reflns_theta_min         2.049
_diffrn_source                   'Incoatec HB I\ms 2.0'
_diffrn_source_current           0.880
_diffrn_source_power             0.044
_diffrn_source_target            Ag
_diffrn_source_type              'Incoatec Ag tube'
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    0.47
_exptl_absorpt_correction_T_max  0.9849
_exptl_absorpt_correction_T_min  0.9343
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
;
STOE X-Red32, absorption correction by Gaussian integration, analogous to
P. Coppens, "The Evaluation of Absorption and Extinction in Single-Crystal
Structure Analysis", published in
F. R. Ahmed (Editor), "Crystallographic Computing",
Munksgaard, Copenhagen (1970), 255 - 270
;
_exptl_crystal_colour            yellow-brown
_exptl_crystal_density_diffrn    1.494
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1228
_exptl_crystal_size_max          0.320
_exptl_crystal_size_mid          0.180
_exptl_crystal_size_min          0.050
_refine_diff_density_max         1.140
_refine_diff_density_min         -0.759
_refine_diff_density_rms         0.088
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.998
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     316
_refine_ls_number_reflns         32089
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.998
_refine_ls_R_factor_all          0.0651
_refine_ls_R_factor_gt           0.0328
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0475P)^2^+0.4625P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0841
_refine_ls_wR_factor_ref         0.0983
_reflns_Friedel_coverage         0.000
_reflns_number_gt                21588
_reflns_number_total             32089
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            px5045sup1.cif
_cod_data_source_block           1_100K
_cod_database_code               2108904
_publcif_datablock.id            {8d763239-83ac-4687-accf-bd38c7560f0c}
_shelx_shelxl_version_number     2016/6
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C9(H9), C10(H10), C11(H11), C12(H12), C13(H13), C15(H15),
 C16(H16), C17(H17), C18(H18), C19(H19), C21(H21), C22(H22), C23(H23), C24(H24),
  C25(H25)
2.b Idealised Me refined as rotating group:
 C26(H26A,H26B,H26C), C27(H27A,H27B,H27C), C7(H7A,H7B,H7C)
;
_shelx_res_checksum              48701
_shelx_hkl_checksum              96261
_olex2_submission_special_instructions 'No special instructions were received'
_cod_database_fobs_code 2108904