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_7062574
_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         'C51 H44 Cu N P2 S2'
_chemical_formula_sum            'C51 H44 Cu N P2 S2'
_chemical_formula_weight         860.47
_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             2023-04-24
_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                 105.406(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.9452(4)
_cell_length_b                   12.0938(2)
_cell_length_c                   19.1076(5)
_cell_measurement_reflns_used    15087
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.9840
_cell_measurement_theta_min      1.9590
_cell_volume                     4220.61(17)
_computing_cell_refinement       'CrysAlisPro 1.171.41.105a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.105a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.105a (Rigaku OD, 2021)'
_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_temperature      100(2)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10
_diffrn_detector_dtime           0.000
_diffrn_detector_type            'Rigaku, HyPix 6000'
_diffrn_measured_fraction_theta_full 0.905
_diffrn_measured_fraction_theta_max 0.873
_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   -100.00  79.00   0.50   60.00    --  -10.60  -4.00 -43.00  358
  2  \w   -100.00  24.00   0.50   60.00    --  -10.60 -60.00-120.00  248
  3  \w    -45.00  79.00   0.50   60.00    --  -10.60  60.00-150.00  248
  4  \w    -50.00  33.00   0.50   60.00    --  -10.60  38.00  60.00  166
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_details 'Rigaku, AFC12 \k goniometer'
_diffrn_measurement_device_type
;
Rigaku FRE+ equipped with VHF Varimax confocal mirrors 
and an AFC12 goniometer and HyPix 6000 detector
;
_diffrn_measurement_method       'profile data from \w-scans'
_diffrn_measurement_specimen_support 'MiTeGen MicroLoop'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0338036000
_diffrn_orient_matrix_UB_12      0.0024878000
_diffrn_orient_matrix_UB_13      0.0093168000
_diffrn_orient_matrix_UB_21      -0.0190624000
_diffrn_orient_matrix_UB_22      0.0023997000
_diffrn_orient_matrix_UB_23      -0.0373272000
_diffrn_orient_matrix_UB_31      -0.0021828000
_diffrn_orient_matrix_UB_32      -0.0585447000
_diffrn_orient_matrix_UB_33      -0.0011636000
_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  0.2796
_diffrn_reflns_av_unetI/netI     0.1529
_diffrn_reflns_Laue_measured_fraction_full 0.905
_diffrn_reflns_Laue_measured_fraction_max 0.873
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            51312
_diffrn_reflns_point_group_measured_fraction_full 0.905
_diffrn_reflns_point_group_measured_fraction_max 0.873
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.718
_diffrn_reflns_theta_min         2.020
_diffrn_source                   'Rotating Anode'
_diffrn_source_current           55.0
_diffrn_source_power             2.475
_diffrn_source_target            Mo
_diffrn_source_type              'Rigaku FRE+'
_diffrn_source_voltage           45.0
_exptl_absorpt_coefficient_mu    0.730
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.09021
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.105a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.354
_exptl_crystal_description       rod
_exptl_crystal_F_000             1792
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.025
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.410
_refine_diff_density_min         -0.792
_refine_diff_density_rms         0.143
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     504
_refine_ls_number_reflns         9554
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.1370
_refine_ls_R_factor_gt           0.0835
_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^)+(0.0799P)^2^+13.0086P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1870
_refine_ls_wR_factor_ref         0.2147
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6148
_reflns_number_total             9554
_reflns_threshold_expression     'I > 2\s(I)'
_twin_special_details
;
Component 2 rotated by -178.2117\% 
around [0.00 1.00 -0.00] (reciprocal) or [-0.00 1.00 -0.00] (direct)
;
_cod_data_source_file            d3nj01918g2.cif
_cod_data_source_block           Compound_4
_cod_database_code               7062574
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C51 H44 N Cu P2 S2'
_chemical_oxdiff_usercomment     JCS_194
_shelx_estimated_absorpt_t_max   0.986
_shelx_estimated_absorpt_t_min   0.769
_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. Uiso/Uaniso restraints and constraints
Uanis(C40) \\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.01
Uanis(C34) = Uanis(C40) = Uanis(C46)
3.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C6(H6), C7(H7), C10(H10), C11(H11), C13(H13), C14(H14),
 C17(H17), C18(H18), C19(H19), C20(H20), C21(H21), C23(H23), C24(H24), C25(H25),
  C26(H26), C27(H27), C29(H29), C30(H30), C31(H31), C32(H32), C33(H33),
 C35(H35), C36(H36), C37(H37), C38(H38), C39(H39), C41(H41), C42(H42), C43(H43),
  C44(H44), C45(H45), C47(H47), C48(H48), C49(H49), C50(H50), C51(H51)
3.b Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C15(H15A,H15B,H15C)
;
_shelx_res_checksum              86403
_shelx_hkl_checksum              78668
_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 7.042
_oxdiff_exptl_absorpt_empirical_full_min 0.162
_oxdiff_twin_integration_method  simultaneous
_oxdiff_twin_items               2