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_7710994
_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         'C17 H11 N S2'
_chemical_formula_sum            'C17 H11 N S2'
_chemical_formula_weight         293.39
_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             2020-08-26
_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                72.472(2)
_cell_angle_beta                 81.6840(10)
_cell_angle_gamma                74.729(2)
_cell_formula_units_Z            12
_cell_length_a                   11.5301(2)
_cell_length_b                   15.3915(3)
_cell_length_c                   25.5188(5)
_cell_measurement_reflns_used    22365
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      32.9670
_cell_measurement_theta_min      2.0010
_cell_volume                     4155.45(15)
_computing_cell_refinement       'CrysAlisPro 1.171.40.82a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.82a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.82a (Rigaku OD, 2020)'
_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_temperature      100(2)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_dtime           0.000
_diffrn_detector_type            'Rigaku, HyPix 6000'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.997
_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   9.00   0.50    5.00    --  -13.40 -60.00 -90.00  186
  2  \w    -17.00  11.00   0.50    5.00    --  -13.40  57.00 -30.00   56
  3  \w     43.00  76.00   0.50    5.00    --  -13.40  57.00 -30.00   66
  4  \w    -81.00 -55.00   0.50    5.00    --  -13.40 -60.00 -30.00   52
  5  \w    -17.00  10.00   0.50    5.00    --  -13.40 -60.00 -30.00   54
  6  \w    -89.00  11.00   0.50    5.00    --  -13.40 -60.00 150.00  200
  7  \w    -88.00 -39.00   0.50    5.00    --  -13.40 -60.00  90.00   98
  8  \w    -38.00 -13.00   0.50    5.00    --  -13.40 -60.00  90.00   50
  9  \w    -80.00   9.00   0.50    5.00    --  -13.40 -60.00-150.00  178
 10  \w    -41.00 -16.00   0.50    5.00    --  -13.40 -60.00 -60.00   50
 11  \w   -103.00   7.00   0.50    5.00    --  -13.40 -57.00  30.00  220
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_details 'Rigaku, AFC12 \k goniometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RCD3): Kappa single'
_diffrn_measurement_method       '\w scans'
_diffrn_measurement_specimen_support 'MiTeGen MicroLoop'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0038666000
_diffrn_orient_matrix_UB_12      0.0298744000
_diffrn_orient_matrix_UB_13      0.0157805000
_diffrn_orient_matrix_UB_21      0.0383590000
_diffrn_orient_matrix_UB_22      0.0218128000
_diffrn_orient_matrix_UB_23      -0.0213294000
_diffrn_orient_matrix_UB_31      -0.0509974000
_diffrn_orient_matrix_UB_32      0.0331861000
_diffrn_orient_matrix_UB_33      -0.0122462000
_diffrn_radiation_collimation    0.2
_diffrn_radiation_monochromator  'Confocal mirrors, VHF Varimax'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_radiation_xray_symbol    K-L~3~
_diffrn_reflns_av_R_equivalents  0.0698
_diffrn_reflns_av_unetI/netI     0.0808
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            81514
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.509
_diffrn_reflns_theta_min         1.963
_diffrn_source                   'Rotating Anode'
_diffrn_source_current           55.0
_diffrn_source_power             2.475
_diffrn_source_target            Mo
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_diffrn_source_voltage           45.0
_exptl_absorpt_coefficient_mu    0.371
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.37363
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.82a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'light green'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.407
_exptl_crystal_description       block
_exptl_crystal_F_000             1824
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.630
_refine_diff_density_min         -0.669
_refine_diff_density_rms         0.085
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1081
_refine_ls_number_reflns         25303
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.015
_refine_ls_R_factor_all          0.0835
_refine_ls_R_factor_gt           0.0523
_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^)+(0.0516P)^2^+1.3853P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1130
_refine_ls_wR_factor_ref         0.1271
_reflns_Friedel_coverage         0.000
_reflns_number_gt                18288
_reflns_number_total             25303
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt01767a2.cif
_cod_data_source_block           Compound_2h
_cod_database_code               7710994
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C51 H36 N4 S2'
_chemical_oxdiff_usercomment     JCS_121
_reflns_odcompleteness_completeness 99.73
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     30.44
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C10(H10), C11(H11), C12(H12),
 C13(H13), C15(H15), C16(H16), C19(H19), C20(H20), C21(H21), C22(H22), C23(H23),
  C26(H26), C27(H27), C29(H29), C30(H30), C31(H31), C32(H32), C36(H36),
 C37(H37), C38(H38), C39(H39), C40(H40), C44(H44), C45(H45), C46(H46), C47(H47),
  C49(H49), C50(H50), C53(H53), C54(H54), C55(H55), C56(H56), C57(H57),
 C60(H60), C61(H61), C63(H63), C64(H64), C65(H65), C66(H66), C70(H70), C71(H71),
  C72(H72), C73(H73), C74(H74), C77(H77), C78(H78), C80(H80), C81(H81),
 C82(H82), C83(H83), C87(H87), C88(H88), C89(H89), C90(H90), C91(H91), C95(H95),
  C96(H96), C97(H97), C98(H98), C100(H100), C101(H101)
;
_shelx_res_checksum              26152
_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 3.181
_oxdiff_exptl_absorpt_empirical_full_min 0.327