A chemically induced, room temperature, single source precursor to CuS (covellite) nanomaterials: synthesis and reactivity of [Cu(S<sub>2</sub>CNHBz)]<sub><i>n</i></sub>.
Huang, Siqiao; Xu, Xiang; Sarker, Jagodish C.; Pugh, David; Hogarth, Graeme; Dalton transactions (Cambridge, England : 2003) 53 (2024) 17140–17145; doi:10.1039/d4dt02366h

data_7717179
_publ_section_title
;
 A chemically induced, room temperature, single source precursor to CuS
 (covellite) nanomaterials: synthesis and reactivity of
 [Cu(S<sub>2</sub>CNHBz)]<sub><i>n</i></sub>.
;
_journal_issue                   42
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              17140
_journal_page_last               17145
_journal_paper_doi               10.1039/d4dt02366h
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C44 H38 Cu N P2 S2'
_chemical_formula_sum            'C44 H38 Cu N P2 S2'
_chemical_formula_weight         770.35
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-I 2ya'
_space_group_name_H-M_alt        'I 1 2/a 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2023-01-11
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2024-08-19 deposited with the CCDC.	2024-10-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 116.023(3)
_cell_angle_gamma                90
_cell_formula_units_Z            24
_cell_length_a                   38.4141(11)
_cell_length_b                   15.0917(4)
_cell_length_c                   44.0156(12)
_cell_measurement_reflns_used    30562
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      33.4250
_cell_measurement_theta_min      2.3390
_cell_volume                     22930.3(12)
_computing_cell_refinement       'CrysAlisPro 1.171.42.76a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.76a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.76a (Rigaku OD, 2022)'
_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_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 1.000
_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    -55.00  -6.00   0.50    7.00    --  -15.18 118.00 116.00   98
  2  \w     12.00  58.00   0.50    7.00    --   17.84-118.00  30.00   92
  3  \w     21.00  63.00   0.50    7.00    --  -15.18  19.00  30.00   84
  4  \w    -93.00 -17.00   0.50    7.00    --  -15.18 -19.00-120.00  152
  5  \w     21.00  63.00   0.50    7.00    --  -15.18  19.00-180.00   84
  6  \w     21.00  63.00   0.50    7.00    --  -15.18  19.00-120.00   84
  7  \w    -18.00  39.00   0.50    7.00    --   17.84 -77.00  30.00  114
  8  \w      6.00  62.00   0.50    7.00    --   17.84  57.00   0.00  112
  9  \w     31.00  62.00   0.50    7.00    --   17.84  57.00 -60.00   62
 10  \w      6.00  51.00   0.50    7.00    --   17.84  57.00  60.00   90
 11  \w      0.00  25.00   0.50    7.00    --   17.84 -99.00  30.00   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'ROD, Synergy Custom system, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0057071000
_diffrn_orient_matrix_UB_12      0.0425383000
_diffrn_orient_matrix_UB_13      -0.0030196000
_diffrn_orient_matrix_UB_21      0.0195135000
_diffrn_orient_matrix_UB_22      -0.0145257000
_diffrn_orient_matrix_UB_23      0.0067407000
_diffrn_orient_matrix_UB_31      -0.0028776000
_diffrn_orient_matrix_UB_32      -0.0138428000
_diffrn_orient_matrix_UB_33      -0.0163240000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0950
_diffrn_reflns_av_unetI/netI     0.0842
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       54
_diffrn_reflns_limit_h_min       -54
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       62
_diffrn_reflns_limit_l_min       -62
_diffrn_reflns_number            178339
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.509
_diffrn_reflns_theta_min         1.940
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.797
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.63661
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.76a (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.339
_exptl_crystal_description       block
_exptl_crystal_F_000             9600
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.496
_refine_diff_density_min         -0.485
_refine_diff_density_rms         0.085
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.992
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1351
_refine_ls_number_reflns         35000
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.992
_refine_ls_R_factor_all          0.1047
_refine_ls_R_factor_gt           0.0538
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0385P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0983
_refine_ls_wR_factor_ref         0.1153
_reflns_Friedel_coverage         0.000
_reflns_number_gt                21940
_reflns_number_total             35000
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt02366h2.cif
_cod_data_source_block           Compound_2
_cod_depositor_comments
'Adding full bibliography for 7717179--7717181.cif.'
_cod_database_code               7717179
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C44 H44 N S2 Cu P2'
_chemical_oxdiff_usercomment     GH-Cu-PPh3
_shelx_estimated_absorpt_t_max   0.925
_shelx_estimated_absorpt_t_min   0.925
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
2.a Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C46(H46A,H46B), C90(H90A,H90B)
2.b Aromatic/amide H refined with riding coordinates:
 N1(H1), C4(H4), C5(H5), C6(H6), C7(H7), C8(H8), C10(H10), C11(H11), C12(H12),
 C13(H13), C14(H14), C16(H16), C17(H17), C18(H18), C19(H19), C20(H20), C22(H22),
  C23(H23), C24(H24), C25(H25), C26(H26), C28(H28), C29(H29), C30(H30),
 C31(H31), C32(H32), C34(H34), C35(H35), C36(H36), C37(H37), C38(H38), C40(H40),
  C41(H41), C42(H42), C43(H43), C44(H44), N2(H2), C48(H48), C49(H49), C50(H50),
 C51(H51), C52(H52), C54(H54), C55(H55), C56(H56), C57(H57), C58(H58), C60(H60),
  C61(H61), C62(H62), C63(H63), C64(H64), C66(H66), C67(H67), C68(H68),
 C69(H69), C70(H70), C72(H72), C73(H73), C74(H74), C75(H75), C76(H76), C78(H78),
  C79(H79), C80(H80), C81(H81), C82(H82), C84(H84), C85(H85), C86(H86),
 C87(H87), C88(H88), N3(H3), C92(H92), C93(H93), C94(H94), C95(H95), C96(H96),
 C98(H98), C99(H99), C100(H100), C101(H101), C102(H102), C104(H104), C105(H105),
  C106(H106), C107(H107), C108(H108), C110(H110), C111(H111), C112(H112),
 C113(H113), C114(H114), C116(H116), C117(H117), C118(H118), C119(H119),
 C120(H120), C122(H122), C123(H123), C124(H124), C125(H125), C126(H126),
 C128(H128), C129(H129), C130(H130), C131(H131), C132(H132)
;
_shelx_res_checksum              44346
_shelx_hkl_checksum              87764
_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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 3.221
_oxdiff_exptl_absorpt_empirical_full_min 0.428