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_2108906
_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             2021-11-11
_audit_creation_method
;
Olex2 1.2
(compiled 2018.04.26 svn.r3504 for OlexSys, GUI svn.r5492)
;
_cell_angle_alpha                90
_cell_angle_beta                 93.3640(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.37850(10)
_cell_length_b                   14.4463(2)
_cell_length_c                   15.9474(2)
_cell_measurement_reflns_used    590779
_cell_measurement_temperature    15(2)
_cell_measurement_theta_max      27.996
_cell_measurement_theta_min      1.519
_cell_volume                     3076.84(6)
_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      15(2)
_diffrn_detector                 'Bruker PHOTON 2 area detector'
_diffrn_detector_type            'Charge-integrating Pixel Array Detector'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker D8 goniometer'
_diffrn_measurement_method       'omega and phi scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.30996
_diffrn_reflns_av_R_equivalents  0.0501
_diffrn_reflns_av_unetI/netI     0.0331
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       40
_diffrn_reflns_limit_h_min       -37
_diffrn_reflns_limit_k_max       43
_diffrn_reflns_limit_k_min       -42
_diffrn_reflns_limit_l_max       48
_diffrn_reflns_limit_l_min       -46
_diffrn_reflns_number            831499
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        10.718
_diffrn_reflns_theta_max         27.996
_diffrn_reflns_theta_min         1.519
_diffrn_source                   synchrotron
_diffrn_source_type              'Incoatec I\ms'
_exptl_absorpt_coefficient_mu    1.325
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.8937
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0490 before and 0.0490 after correction.
The Ratio of minimum to maximum transmission is 0.8937.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            black-green
_exptl_crystal_density_diffrn    1.628
_exptl_crystal_description       plate
_exptl_crystal_F_000             1532
_exptl_crystal_size_max          0.093
_exptl_crystal_size_mid          0.047
_exptl_crystal_size_min          0.026
_exptl_transmission_factor_max   1.0000
_exptl_transmission_factor_min   0.8937
_refine_diff_density_max         2.465
_refine_diff_density_min         -3.179
_refine_diff_density_rms         0.124
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     374
_refine_ls_number_reflns         88732
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0550
_refine_ls_R_factor_gt           0.0319
_refine_ls_shift/su_max          0.010
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0408P)^2^+0.1535P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0782
_refine_ls_wR_factor_ref         0.0845
_reflns_Friedel_coverage         0.000
_reflns_number_gt                64088
_reflns_number_total             89538
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            px5045sup1.cif
_cod_data_source_block           2_15K
_cod_database_code               2108906
_publcif_datablock.id            {91ac6347-1e47-407e-87b9-e2972bcc1d1a}
_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              97804
_shelx_hkl_checksum              33425
_olex2_submission_special_instructions 'No special instructions were received'
_publcif_info_exptl_table_max_cols 5
_publcif_info_exptl_table_use_headnotes n
_publcif_funding_html
'<span class="funder"><span class="fundref-name" data-id="501100005357">Agent&uacute;ra na Podporu V&yacute;skumu a V&yacute;voja</span><span class="fundref-subname" data-id=""></span> (<span class="fundref-grant-group"><span class="fundref-grant-type">grant</span> No. <span class="fundref-grant-id">APVV-20-0213</span></span>); </span><span class="funder"><span class="fundref-name" data-id="501100006109">Vedeck&aacute; Grantov&aacute; Agent&uacute;ra MVVa SR a SAV</span><span class="fundref-subname" data-id=""></span> (<span class="fundref-grant-group"><span class="fundref-grant-type">grant</span> No. <span class="fundref-grant-id">1/0718/19</span></span>); </span><span class="funder"><span class="fundref-name" data-id="501100005357">Agent&uacute;ra na Podporu V&yacute;skumu a V&yacute;voja</span><span class="fundref-subname" data-id=""></span> (<span class="fundref-grant-group"><span class="fundref-grant-type">grant</span> No. <span class="fundref-grant-id">APVV-19-0087</span></span>); </span><span class="funder"><span class="fundref-name" data-id="501100008530">European Regional Development Fund</span><span class="fundref-subname" data-id=""></span> (<span class="fundref-grant-group"><span class="fundref-grant-type">grant</span> No. <span class="fundref-grant-id">26230120002</span></span>); </span><span class="funder"><span class="fundref-name" data-id="">Research and Development Operational Programme </span><span class="fundref-subname" data-id=""></span> (<span class="fundref-grant-group"><span class="fundref-grant-type">grant</span> No. <span class="fundref-grant-id">ITMS 26240220084</span></span>).</span>'
_cod_database_fobs_code 2108906