Copper diaryl-dithiocarbamate complexes and their application as single source precursors (SSPs) for copper sulfide nanomaterials
Sarker, Jagodish C.; Xu, Xiang; Alam, Firoz; Nash, Rosie; Boonrungsiman, Suwimon; Pugh, David; Cockcroft, Jeremy K.; Lewis, David J.; Hogarth, Graeme; New Journal of Chemistry 47 (2023) 12718–12727; doi:10.1039/D3NJ01918G

data_7062573
_publ_section_title
;
 Copper diaryl-dithiocarbamate complexes and their application as single
 source precursors (SSPs) for copper sulfide nanomaterials
;
_journal_issue                   27
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              12718
_journal_page_last               12727
_journal_paper_doi               10.1039/D3NJ01918G
_journal_volume                  47
_journal_year                    2023
_chemical_formula_moiety         'C30 H28 Cu N2 S4'
_chemical_formula_sum            'C30 H28 Cu N2 S4'
_chemical_formula_weight         608.32
_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     iterative
_audit_creation_date             2023-04-25
_audit_creation_method
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_audit_update_record
;
2023-04-25 deposited with the CCDC.	2023-06-12 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 97.231(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.1900(6)
_cell_length_b                   17.2006(6)
_cell_length_c                   14.9006(5)
_cell_measurement_reflns_used    5017
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      69.7120
_cell_measurement_theta_min      4.7250
_cell_volume                     2845.2(2)
_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 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.5 (Bourhis et al., 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.963
_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    -89.00  89.00   0.50    6.00    --    0.00  10.00 -60.00  356
  2  \w   -179.00  -1.00   0.50   24.00    --  -90.00  58.00-104.95  356
  3  \w   -179.00  -1.00   0.50   24.00    --  -90.00  56.00-173.49  356
  4  \w   -179.00  -1.00   0.50   24.00    --  -90.00  58.00 -25.55  356
  5  \w    -91.00  -4.00   0.50   24.00    --  -90.00  58.00 -33.11  174
  6  \w    -91.00  -4.00   0.50   24.00    --  -90.00  58.00 -33.11  174
  7  \w    -64.00 -38.00   0.50   24.00    --  -90.00  10.00 150.00   52
  8  \w   -144.00-100.00   0.50   24.00    --  -90.00  30.00 -90.00   88
  9  \w    -45.00 -10.00   0.50   24.00    --  -90.00  30.00 -90.00   70
 10  \w   -144.00 -60.00   0.50   24.00    --  -90.00  58.00-104.95  168
 11  \w   -123.00 -97.00   0.50   24.00    --  -90.00  51.00  95.07   52
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC11 (RCD3): quarter-chi single'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0200805000
_diffrn_orient_matrix_UB_12      0.0847658000
_diffrn_orient_matrix_UB_13      0.0320184000
_diffrn_orient_matrix_UB_21      0.1372697000
_diffrn_orient_matrix_UB_22      -0.0125117000
_diffrn_orient_matrix_UB_23      0.0090794000
_diffrn_orient_matrix_UB_31      0.0004960000
_diffrn_orient_matrix_UB_32      0.0262395000
_diffrn_orient_matrix_UB_33      -0.0987591000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0899
_diffrn_reflns_av_unetI/netI     0.0703
_diffrn_reflns_Laue_measured_fraction_full 0.986
_diffrn_reflns_Laue_measured_fraction_max 0.963
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            21888
_diffrn_reflns_point_group_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.963
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         70.449
_diffrn_reflns_theta_min         3.943
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.994
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.43535
_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            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.420
_exptl_crystal_description       'Fragment (from block)'
_exptl_crystal_F_000             1260
_exptl_crystal_size_max          0.07
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.717
_refine_diff_density_min         -0.589
_refine_diff_density_rms         0.103
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     338
_refine_ls_number_reflns         5239
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.1000
_refine_ls_R_factor_gt           0.0667
_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^)+(0.0772P)^2^+5.8252P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1519
_refine_ls_wR_factor_ref         0.1698
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3704
_reflns_number_total             5239
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3nj01918g2.cif
_cod_data_source_block           compound_2b
_cod_database_code               7062573
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C30 H30 Cu N2 S4 '
_chemical_oxdiff_usercomment     JCS_04
_shelx_estimated_absorpt_t_max   0.961
_shelx_estimated_absorpt_t_min   0.767
_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),
 C18(H18), C19(H19), C21(H21), C22(H22), C25(H25), C26(H26), C28(H28), C29(H29)
2.b Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C15(H15A,H15B,H15C), C23(H23A,H23B,H23C), C30(H30A,H30B,H30C)
;
_shelx_res_checksum              41868
_shelx_hkl_checksum              2649
_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 1.937
_oxdiff_exptl_absorpt_empirical_full_min 0.549