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_7062575
_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 O4 S4'
_chemical_formula_sum            'C30 H28 Cu N2 O4 S4'
_chemical_formula_weight         672.32
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     dual
_audit_creation_date             2019-02-25
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2023-04-25 deposited with the CCDC.	2023-06-12 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 99.4430(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.7567(2)
_cell_length_b                   19.5651(2)
_cell_length_c                   16.5460(2)
_cell_measurement_reflns_used    27999
_cell_measurement_temperature    150.0
_cell_measurement_theta_max      72.6120
_cell_measurement_theta_min      4.4820
_cell_volume                     3115.68(8)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_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_environment      N~2~
_diffrn_ambient_temperature      150.0
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2031
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.988
_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    -70.00 -23.00   1.00    7.50    --  -43.17 -38.00 150.00   47
  2  \w    -55.00 -23.00   1.00    7.50    --  -43.17 -38.00  30.00   32
  3  \w    -57.00 -17.00   1.00    7.50    --  -43.17 -57.00   0.00   40
  4  \w   -116.00 -89.00   1.00    7.50    --  -43.17 -77.00-150.00   27
  5  \w   -116.00 -12.00   1.00    7.50    --  -43.17 -77.00 120.00  104
  6  \w   -116.00 -69.00   1.00    7.50    --  -43.17 -38.00  30.00   47
  7  \w   -110.00 -83.00   1.00    7.50    --  -43.17 -57.00   0.00   27
  8  \w    -41.00 -16.00   1.00    7.50    --  -43.17 -77.00  60.00   25
  9  \w   -115.00 -89.00   1.00    7.50    --  -43.17 -38.00 150.00   26
 10  \w    -60.00 -12.00   1.00    7.50    --  -43.17 -77.00-150.00   48
 11  \w    -51.00 -17.00   1.00    7.50    --  -43.17 -57.00-120.00   34
 12  \w   -108.00 -57.00   1.00    7.50    --  -43.17 -57.00-120.00   51
 13  \w    -73.00  31.00   1.00    7.50    --  -43.17  77.00 120.00  104
 14  \w    -85.00 -12.00   1.00    7.50    --  -43.17 -77.00 -30.00   73
 15  \w     23.00  66.00   1.00    7.50    --   43.17-125.00  60.00   43
 16  \w      1.00  68.00   1.00    7.50    --   43.17 -99.00 -90.00   67
 17  \w     26.00 103.00   1.00   30.00    --  104.25 -94.00   0.00   77
 18  \w     75.00 139.00   1.00   30.00    --  104.25  69.00-121.46   64
 19  \w     34.00 123.00   1.00   30.00    --  104.25-133.00 -60.15   89
 20  \w     78.00 105.00   1.00   30.00    --  104.25  57.00  43.01   27
 21  \w     75.00 101.00   1.00   30.00    --  104.25  69.00-132.66   26
 22  \w     74.00 166.00   1.00   30.00    --  104.25  73.00-111.26   92
 23  \w    131.00 173.00   1.00   30.00    --  104.25 125.00  60.00   42
 24  \w     73.00  99.00   1.00   30.00    --  104.25  77.00-180.00   26
 25  \w    113.00 178.00   1.00   30.00    --  104.25  77.00-180.00   65
 26  \w     77.00 169.00   1.00   30.00    --  104.25  61.00 -30.00   92
 27  \w     73.00 177.00   1.00   30.00    --  104.25  77.00 150.00  104
 28  \w     76.00 102.00   1.00   30.00    --  104.25  65.00 178.46   26
 29  \w     77.00 108.00   1.00   30.00    --  104.25  61.00  90.00   31
 30  \w    148.00 174.00   1.00   30.00    --  104.25  61.00  90.00   26
 31  \w     73.00  99.00   1.00   30.00    --  104.25  77.00 120.00   26
 32  \w     73.00  99.00   1.00   30.00    --  104.25  77.00  53.93   26
 33  \w    148.00 175.00   1.00   30.00    --  104.25  65.00 -58.75   27
 34  \w     77.00 106.00   1.00   30.00    --  104.25  61.00-150.00   29
 35  \w     73.00  99.00   1.00   30.00    --  104.25  77.00 -30.00   26
 36  \w     77.00 103.00   1.00   30.00    --  104.25  61.00 120.00   26
 37  \w     77.00 171.00   1.00   30.00    --  104.25  61.00  60.00   94
 38  \w     73.00  99.00   1.00   30.00    --  104.25  77.00 -60.00   26
 39  \w     23.00  84.00   1.00   30.00    --  104.25 -94.00  90.00   61
 40  \w     74.00  99.00   1.00   30.00    --  104.25  74.00  11.37   25
 41  \w     73.00 178.00   1.00   30.00    --  104.25  77.00   0.00  105
 42  \w     73.00  99.00   1.00   30.00    --  104.25  77.00 -90.00   26
 43  \w     73.00  99.00   1.00   30.00    --  104.25  77.00  30.00   26
 44  \w     77.00 139.00   1.00   30.00    --  104.25  61.00 150.00   62
 45  \w     73.00 170.00   1.00   30.00    --  104.25  77.00  90.00   97
 46  \w     77.00 104.00   1.00   30.00    --  104.25  61.00   0.00   27
 47  \w     56.00 117.00   1.00   30.00    --  104.25-125.00-180.00   61
 48  \w    128.00 175.00   1.00   30.00    --  104.25 114.00 -49.00   47
 49  \w     76.00 172.00   1.00   30.00    --  104.25  63.00 -83.06   96
 50  \w     76.00 102.00   1.00   30.00    --  104.25  65.00 -58.75   26
 51  \w    113.00 143.00   1.00   30.00    --  104.25  65.00-141.77   30
 52  \w     76.00 105.00   1.00   30.00    --  104.25  65.00-141.77   29
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0163909000
_diffrn_orient_matrix_UB_12      -0.0065295000
_diffrn_orient_matrix_UB_13      -0.0907392000
_diffrn_orient_matrix_UB_21      0.0266726000
_diffrn_orient_matrix_UB_22      -0.0772457000
_diffrn_orient_matrix_UB_23      0.0117878000
_diffrn_orient_matrix_UB_31      -0.1569306000
_diffrn_orient_matrix_UB_32      -0.0138051000
_diffrn_orient_matrix_UB_33      -0.0232454000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0416
_diffrn_reflns_av_unetI/netI     0.0200
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            51710
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.921
_diffrn_reflns_theta_min         3.526
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.804
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.553
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'metallic brownish orange'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   brownish
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.433
_exptl_crystal_description       needle
_exptl_crystal_F_000             1388
_exptl_crystal_size_max          0.283
_exptl_crystal_size_mid          0.043
_exptl_crystal_size_min          0.032
_refine_diff_density_max         0.473
_refine_diff_density_min         -0.373
_refine_diff_density_rms         0.057
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     482
_refine_ls_number_reflns         6144
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.076
_refine_ls_R_factor_all          0.0338
_refine_ls_R_factor_gt           0.0300
_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^)+(0.0390P)^2^+1.7392P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0761
_refine_ls_wR_factor_ref         0.0786
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5600
_reflns_number_total             6144
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3nj01918g2.cif
_cod_data_source_block           Compound_2c
_cod_database_code               7062575
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C30  H28  Cu1  N2  O4  S4'
_chemical_oxdiff_usercomment
'JCS-19 - metallic looking needles most of which are not single crystals!'
_shelx_estimated_absorpt_t_max   0.888
_shelx_estimated_absorpt_t_min   0.412
_reflns_odcompleteness_completeness 99.93
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.49
_olex2_refinement_description
;
;
_shelx_res_checksum              24113
_shelx_hkl_checksum              64487
_olex2_date_sample_data_collection 2019-02-22
_olex2_exptl_crystal_mounting_method '0.3um nylon loop from Hampton Research'
_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 1.921
_oxdiff_exptl_absorpt_empirical_full_min 0.657