Diaryl dithiocarbamates: synthesis, oxidation to thiuram disulfides, Co(iii) complexes [Co(S2CNAr2)3] and their use as single source precursors to CoS2
Sarker, Jagodish C.; Nash, Rosie; Boonrungsiman, Suwimon; Pugh, David; Hogarth, Graeme; Dalton Transactions  (2022) –; doi:10.1039/D2DT01767A

data_7710991
_publ_section_title
;
 Diaryl dithiocarbamates: synthesis, oxidation to thiuram disulfides,
 Co(iii) complexes [Co(S2CNAr2)3] and their use as single source
 precursors to CoS2
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT01767A
_journal_year                    2022
_chemical_formula_moiety         'C30 H28 N2 O4 S4'
_chemical_formula_sum            'C30 H28 N2 O4 S4'
_chemical_formula_weight         608.78
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2021-03-25
_audit_creation_method
;
Olex2 1.3
(compiled 2020.02.04 svn.rd84adfe8 for OlexSys, GUI svn.r6032)
;
_audit_update_record
;
2022-05-27 deposited with the CCDC.	2022-08-08 downloaded from the CCDC.
;
_cell_angle_alpha                68.656(5)
_cell_angle_beta                 89.217(5)
_cell_angle_gamma                64.833(6)
_cell_formula_units_Z            1
_cell_length_a                   8.5740(6)
_cell_length_b                   9.6486(6)
_cell_length_c                   11.1360(5)
_cell_measurement_reflns_used    9503
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      31.7650
_cell_measurement_theta_min      2.0720
_cell_volume                     765.65(10)
_computing_cell_refinement       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.3 (Bourhis et al., 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'hybrid pixel detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -84.00  35.00   0.50    1.00    --    5.00 -38.00 150.00  238
  2  \w    -95.00  25.00   0.50    1.00    --   -5.80 -38.00 -30.00  240
  3  \w    -95.00  24.00   0.50    1.00    --   -5.80 -57.00  90.00  238
  4  \w    -95.00  25.00   0.50    1.00    --   -5.80 -60.00-120.00  240
  5  \w    -84.00  53.00   0.50    1.00    --    5.00 -19.00 -30.00  274
  6  \w    -36.00  13.00   0.50    1.00    --   -5.80  38.00 -90.00   98
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'Rigaku FRE+ diffractometer equipped with VHF Varimax confocal mirrors and an AFC12 goniometer and HyPix 6000HE detector'
_diffrn_measurement_method       'profile data from \w-scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0271160000
_diffrn_orient_matrix_UB_12      0.0694376000
_diffrn_orient_matrix_UB_13      -0.0608156000
_diffrn_orient_matrix_UB_21      -0.0618817000
_diffrn_orient_matrix_UB_22      0.0506889000
_diffrn_orient_matrix_UB_23      0.0279436000
_diffrn_orient_matrix_UB_31      0.0634895000
_diffrn_orient_matrix_UB_32      0.0207762000
_diffrn_orient_matrix_UB_33      0.0182184000
_diffrn_radiation_monochromator  'Confocal mirrors, VHF Varimax'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0222
_diffrn_reflns_av_unetI/netI     0.0147
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            17250
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.478
_diffrn_reflns_theta_min         2.540
_diffrn_source                   'Rotating Anode'
_diffrn_source_type              'Rigaku FRE+'
_exptl_absorpt_coefficient_mu    0.347
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.79195
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'light yellow'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.320
_exptl_crystal_description       block
_exptl_crystal_F_000             318
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.796
_refine_diff_density_min         -0.253
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     183
_refine_ls_number_reflns         3512
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0498
_refine_ls_R_factor_gt           0.0465
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0746P)^2^+0.8541P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1252
_refine_ls_wR_factor_ref         0.1287
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3236
_reflns_number_total             3512
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt01767a2.cif
_cod_data_source_block           Compound_2c
_cod_original_cell_volume        765.65(9)
_cod_database_code               7710991
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C30 H28 N2 O4 S4'
_chemical_oxdiff_usercomment     JCS_86
_shelx_estimated_absorpt_t_max   0.973
_shelx_estimated_absorpt_t_min   0.874
_reflns_odcompleteness_completeness 99.94
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.42
_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), C6(H6), C7(H7), C10(H10), C11(H11), C13(H13), C14(H14)
2.b Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C15(H15A,H15B,H15C)
;
_shelx_res_checksum              12878
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.267
_oxdiff_exptl_absorpt_empirical_full_min 0.742