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_2108905
_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         '2(C6 H2 Cl2 Ni0.5 S2), C19 H18 P'
_chemical_formula_sum            'C31 H22 Cl4 Ni P S4'
_chemical_formula_weight         754.20
_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
_atom_sites_solution_primary     dual
_audit_creation_date             2021-06-18
_audit_creation_method
;
Olex2 1.2
(compiled 2018.04.26 svn.r3504 for OlexSys, GUI svn.r5492)
;
_cell_angle_alpha                90
_cell_angle_beta                 93.0540(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.36640(10)
_cell_length_b                   14.48490(10)
_cell_length_c                   15.97120(10)
_cell_measurement_reflns_used    1181142
_cell_measurement_temperature    100(1)
_cell_measurement_theta_max      39.15
_cell_measurement_theta_min      1.96
_cell_volume                     3087.81(4)
_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(1)
_diffrn_detector                 HPAD
_diffrn_detector_area_resol_mean 5.81
_diffrn_detector_type            'Dectris 300K Pilatus3R'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.977
_diffrn_measurement_details      ' 12602 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  0.0303
_diffrn_reflns_av_unetI/netI     0.0134
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.977
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            653883
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.977
_diffrn_reflns_theta_full        19.664
_diffrn_reflns_theta_max         39.171
_diffrn_reflns_theta_min         2.015
_diffrn_source                   'Incoatec HB I\ms 2.0'
_diffrn_source_current           0.600
_diffrn_source_power             0.030
_diffrn_source_target            Ag
_diffrn_source_type              'Incoatec Ag tube'
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    0.68
_exptl_absorpt_correction_T_max  0.8344
_exptl_absorpt_correction_T_min  0.2619
_exptl_absorpt_correction_type   multi-scan
_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.
Afterwards scaling of reflection intensities was performed within STOE LANA.
J. Koziskova, F. Hahn, J. Richter, J. Kozisek, "Comparison of different
absorption corrections on the model structure of tetrakis(\m~2~-acetato)-
diaqua-di-copper(II)", Acta Chimica Slovaca, vol. 9, no. 2, 2016, pp. 136 - 140.
Finally a spherical absorption correction was done within STOE LANA.
;
_exptl_crystal_colour            black-green
_exptl_crystal_density_diffrn    1.622
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1532
_exptl_crystal_size_max          0.230
_exptl_crystal_size_mid          0.157
_exptl_crystal_size_min          0.030
_refine_diff_density_max         0.833
_refine_diff_density_min         -0.736
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     375
_refine_ls_number_reflns         36081
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0492
_refine_ls_R_factor_gt           0.0264
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0343P)^2^+0.6067P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0669
_refine_ls_wR_factor_ref         0.0789
_reflns_Friedel_coverage         0.000
_reflns_number_gt                25847
_reflns_number_total             36081
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            px5045sup1.cif
_cod_data_source_block           2_100K
_cod_database_code               2108905
_publcif_datablock.id            {b21184cc-7883-4726-aa91-bc6a77e40453}
_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:
 C3(H3), C4(H4), C9(H9), C10(H10), C15(H15), C16(H16), C17(H17), C18(H18),
 C19(H19), C21(H21), C22(H22), C23(H23), C24(H24), C25(H25), C27(H27), C28(H28),
  C29(H29), C30(H30), C31(H31)
2.b Idealised Me refined as rotating group:
 C13(H13A,H13B,H13C)
;
_shelx_res_checksum              13033
_shelx_hkl_checksum              6427
_olex2_submission_special_instructions 'No special instructions were received'
_cod_database_fobs_code 2108905