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_7717181
_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         'C42 H36 Cu Fe N P2 S2'
_chemical_formula_sum            'C42 H36 Cu Fe N P2 S2'
_chemical_formula_weight         800.17
_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             2022-11-08
_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                95.408(3)
_cell_angle_beta                 93.201(3)
_cell_angle_gamma                92.636(3)
_cell_formula_units_Z            4
_cell_length_a                   11.9613(4)
_cell_length_b                   16.1413(5)
_cell_length_c                   18.9872(6)
_cell_measurement_reflns_used    10048
_cell_measurement_temperature    150.01(10)
_cell_measurement_theta_max      72.1970
_cell_measurement_theta_min      3.4440
_cell_volume                     3639.0(2)
_computing_cell_refinement       'CrysAlisPro 1.171.41.123a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.41.123a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.41.123a (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      150.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 15.9832
_diffrn_detector_type            Sapphire3
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.974
_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    -18.00  36.00   1.00    7.50    --  -33.50  37.00  60.00   54
  2  \w    -42.00 -14.00   1.00    7.50    --  -33.50 -37.00-120.00   28
  3  \w    -97.00 -59.00   1.00    7.50    --  -33.50 -37.00-120.00   38
  4  \w    -53.00 -23.00   1.00    7.50    --  -33.50  37.00  60.00   30
  5  \w     20.00  74.00   1.00    7.50    --   36.21 -99.00  30.00   54
  6  \w    -35.00  62.00   1.00    7.50    --   36.21 -19.00 -30.00   97
  7  \w    -30.00  10.00   1.00    7.50    --   36.21 -57.00-120.00   40
  8  \w     22.00  63.00   1.00    7.50    --   36.21 -77.00 -90.00   41
  9  \w      1.00  74.00   1.00    7.50    --   36.21 -99.00-150.00   73
 10  \w      8.00  97.00   1.00    7.50    --   36.21  19.00-180.00   89
 11  \w     61.00  88.00   1.00    7.50    --   36.21 178.00  30.00   27
 12  \w     71.00 108.00   1.00    7.50    --   36.21-178.00-150.00   37
 13  \w     16.00  53.00   1.00    7.50    --   36.21 -57.00-120.00   37
 14  \w     93.00 129.00   1.00   30.00    --  108.00 -30.00 -90.00   36
 15  \w     39.00  66.00   1.00   30.00    --  108.00-111.00-120.00   27
 16  \w     39.00  91.00   1.00   30.00    --  108.00 -30.00 -90.00   52
 17  \w     42.00 125.00   1.00   30.00    --  108.00 -61.00-180.00   83
 18  \w     87.00 159.00   1.00   30.00    --  108.00  30.00-180.00   72
 19  \w     37.00 137.00   1.00   30.00    --  108.00 -15.00 150.00  100
 20  \w     83.00 109.00   1.00   30.00    --  108.00-111.00 120.00   26
 21  \w     47.00  95.00   1.00   30.00    --  108.00 -94.00  30.00   48
 22  \w     77.00 109.00   1.00   30.00    --  108.00-111.00   0.00   32
 23  \w     59.00 108.00   1.00   30.00    --  108.00 -30.00  90.00   49
 24  \w     64.00 106.00   1.00   30.00    --  108.00 -94.00-120.00   42
 25  \w     38.00 129.00   1.00   30.00    --  108.00 -30.00   0.00   91
 26  \w     79.00 106.00   1.00   30.00    --  108.00 -94.00 150.00   27
 27  \w     42.00  69.00   1.00   30.00    --  108.00 -94.00 150.00   27
 28  \w     42.00 126.00   1.00   30.00    --  108.00 -61.00 -90.00   84
 29  \w    104.00 139.00   1.00   30.00    --  108.00 111.00  90.00   35
 30  \w     84.00 109.00   1.00   30.00    --  108.00-111.00 -90.00   25
 31  \w     46.00 133.00   1.00   30.00    --  108.00 -77.00  60.00   87
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0146994000
_diffrn_orient_matrix_UB_12      0.0937460000
_diffrn_orient_matrix_UB_13      0.0182729000
_diffrn_orient_matrix_UB_21      -0.0616574000
_diffrn_orient_matrix_UB_22      0.0042111000
_diffrn_orient_matrix_UB_23      -0.0729105000
_diffrn_orient_matrix_UB_31      -0.1125475000
_diffrn_orient_matrix_UB_32      -0.0202325000
_diffrn_orient_matrix_UB_33      0.0318866000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0379
_diffrn_reflns_av_unetI/netI     0.0549
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.974
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            26444
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.974
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.258
_diffrn_reflns_theta_min         3.438
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    6.061
_exptl_absorpt_correction_T_max  0.819
_exptl_absorpt_correction_T_min  0.645
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.123a (Rigaku Oxford Diffraction, 2022)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.461
_exptl_crystal_description       block
_exptl_crystal_F_000             1648
_exptl_crystal_size_max          0.367
_exptl_crystal_size_mid          0.284
_exptl_crystal_size_min          0.174
_refine_diff_density_max         0.759
_refine_diff_density_min         -0.426
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     929
_refine_ls_number_reflns         14004
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0623
_refine_ls_R_factor_gt           0.0463
_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^)+(0.0652P)^2^+0.7254P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1207
_refine_ls_wR_factor_ref         0.1292
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11014
_reflns_number_total             14004
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt02366h2.cif
_cod_data_source_block           Compound_3
_cod_depositor_comments
'Adding full bibliography for 7717179--7717181.cif.'
_cod_database_code               7717181
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'Cu Fe P2 S2 C40 H40 N4'
_shelx_estimated_absorpt_t_max   0.419
_shelx_estimated_absorpt_t_min   0.214
_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. Uiso/Uaniso restraints and constraints
Uanis(C85) \\sim Ueq, Uanis(C86) \\sim Ueq, Uanis(C87) \\sim Ueq: with sigma of
0.02 and sigma for terminal atoms of 0.01
3. Others
 Sof(C85)=Sof(H85)=Sof(C86)=Sof(H86)=Sof(C87)=Sof(H87)=Sof(C88)=Sof(H88)=
 Sof(C89)=Sof(H89)=1-FVAR(1)
 Sof(C80)=Sof(H80)=Sof(C81)=Sof(H81)=Sof(C82)=Sof(H82)=Sof(C83)=Sof(H83)=
 Sof(C84)=Sof(H84)=FVAR(1)
4.a Secondary CH2 refined with riding coordinates:
 C36(H36A,H36B), C78(H78A,H78B)
4.b Aromatic/amide H refined with riding coordinates:
 N1(H1), C2(H2A), C3(H3), C4(H4), C5(H5), C7(H7), C8(H8), C9(H9), C10(H10),
 C12(H12), C13(H13), C14(H14), C15(H15), C16(H16), C18(H18), C19(H19), C20(H20),
  C21(H21), C22(H22), C24(H24), C25(H25), C26(H26), C27(H27), C28(H28),
 C30(H30), C31(H31), C32(H32), C33(H33), C34(H34), C38(H38), C39(H39), C40(H40),
  C41(H41), C42(H42), N2(H2), C44(H44), C45(H45), C46(H46), C47(H47), 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),
  C80(H80), C81(H81), C82(H82), C83(H83), C84(H84), C85(H85), C86(H86),
 C87(H87), C88(H88), C89(H89)
;
_shelx_res_checksum              82190
_shelx_hkl_checksum              48886
_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 1.245
_oxdiff_exptl_absorpt_empirical_full_min 0.683