Ultrathin covalent and cuprophilic interaction-assembled copper-sulfur monolayer in organic metal chalcogenide for oriented photoconductivity
Liu, Guang-Ning; Xu, Rang-Dong; Li, Ming-Kun; Sun, Yiqiang; Zhou, Meng-Jie; Cai, Rui-Yun; You, Zuo-Jiang; Jiang, Xiao-Ming; Li, Cuncheng; Chemical Communications  (2022) –; doi:10.1039/D2CC00145D

data_7129619
_publ_section_title
;
 Ultrathin covalent and cuprophilic interaction-assembled copper-sulfur
 monolayer in organic metal chalcogenide for oriented photoconductivity
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D2CC00145D
_journal_year                    2022
_chemical_formula_moiety         'C5 H3 Cl Cu N S'
_chemical_formula_sum            'C5 H3 Cl Cu N S'
_chemical_formula_weight         208.13
_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     dual
_audit_creation_date             2020-06-23
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-10-16 deposited with the CCDC.	2022-01-25 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 99.156(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.6065(5)
_cell_length_b                   5.9981(3)
_cell_length_c                   7.4480(3)
_cell_measurement_reflns_used    1842
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.8650
_cell_measurement_theta_min      2.9520
_cell_volume                     600.11(4)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46e (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    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0355
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.906
_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    -51.00  33.00   1.00    1.03    --   16.17 -57.00  90.00   84
  2  \w     -3.00  85.00   1.00    1.03    --   16.17  37.00-120.00   88
  3  \w    -51.00  33.00   1.00    1.03    --   16.17 -57.00   0.00   84
  4  \w    -25.00  22.00   1.00    1.03    --  -16.64 -99.00   0.00   47
  5  \w     -1.00  83.00   1.00    1.03    --   16.17  57.00 120.00   84
  6  \w    -53.00 -28.00   1.00    1.03    --   16.17 -37.00 150.00   25
  7  \w     35.00  88.00   1.00    1.03    --   16.17 178.00 -30.00   53
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0379458000
_diffrn_orient_matrix_UB_12      -0.0811318000
_diffrn_orient_matrix_UB_13      -0.0218846000
_diffrn_orient_matrix_UB_21      -0.0351210000
_diffrn_orient_matrix_UB_22      0.0858045000
_diffrn_orient_matrix_UB_23      -0.0270117000
_diffrn_orient_matrix_UB_31      0.0107614000
_diffrn_orient_matrix_UB_32      -0.0060744000
_diffrn_orient_matrix_UB_33      -0.0899703000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0353
_diffrn_reflns_av_unetI/netI     0.0329
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.906
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            5660
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.906
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.173
_diffrn_reflns_theta_min         3.033
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    4.312
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.72033
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46e (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear yellowish yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    2.304
_exptl_crystal_description       block
_exptl_crystal_F_000             408
_exptl_crystal_preparation       photoconductivity
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.617
_refine_diff_density_min         -0.370
_refine_diff_density_rms         0.098
_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     82
_refine_ls_number_reflns         1468
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0458
_refine_ls_R_factor_gt           0.0325
_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^)+(0.0355P)^2^+0.4124P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0722
_refine_ls_wR_factor_ref         0.0802
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1187
_reflns_number_total             1468
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc00145d2.cif
_cod_data_source_block           '[Cu(CMP)]n'
_cod_database_code               7129619
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C H N O'
_shelx_estimated_absorpt_t_max   0.479
_shelx_estimated_absorpt_t_min   0.277
_reflns_odcompleteness_completeness 99.63
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C3(H3), C4(H4)
;
_olex2_date_sample_data_collection 2019-11-08
_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 1.394
_oxdiff_exptl_absorpt_empirical_full_min 0.835