Engineering of CdS-chain arrays assembled through S⋯S interactions in 1D semiconductive coordination polymers.
Nishibe, Asuka; Akiyoshi, Ryohei; Saeki, Akinori; Ogasawara, Kazuyoshi; Tsuruoka, Takaaki; Tanaka, Daisuke; Chemical communications (Cambridge, England) 60 (2024) 1277–1280; doi:10.1039/d3cc05689a

data_7132560
_publ_section_title
;
 Engineering of CdS-chain arrays assembled through S&#x22ef;S interactions
 in 1D semiconductive coordination polymers.
;
_journal_issue                   10
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              1277
_journal_page_last               1280
_journal_paper_doi               10.1039/d3cc05689a
_journal_volume                  60
_journal_year                    2024
_chemical_formula_moiety         '3(C4.667 H4.667 Cd0.333 O0.667 S0.667)'
_chemical_formula_sum            'C14 H14 Cd O2 S2'
_chemical_formula_weight         390.77
_space_group_crystal_system      orthorhombic
_space_group_IT_number           45
_space_group_name_Hall           'I 2 -2c'
_space_group_name_H-M_alt        'I b a 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-12-17
_audit_creation_method
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_audit_update_record
;
2023-12-16 deposited with the CCDC.	2023-12-29 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            12
_cell_length_a                   35.4228(10)
_cell_length_b                   16.8199(4)
_cell_length_c                   7.2761(2)
_cell_measurement_reflns_used    2774
_cell_measurement_temperature    293
_cell_measurement_theta_max      75.5400
_cell_measurement_theta_min      2.9100
_cell_volume                     4335.2(2)
_computing_cell_refinement       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_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    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      293
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.975
_diffrn_measured_fraction_theta_max 0.928
_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   -173.00 -69.00   0.50    0.92    -- -105.02  -6.00-165.00  208
  2  \w     -6.00  19.00   0.50    2.48    --  -46.17   6.00  10.00   50
  3  \w    -61.00  27.00   0.50    2.48    --  -46.17  57.00  90.00  176
  4  \w    -29.00   0.00   0.50    2.48    --   46.17 -19.00 -60.00   58
  5  \w    -21.00   6.00   0.50    2.48    --   46.17  -6.00-165.00   54
  6  \w     32.00  71.00   0.50    0.92    --  105.02 -61.00-180.00   78
  7  \w    102.00 127.00   0.50    0.92    --  105.02-146.00-128.00   50
  8  \w     39.00  89.00   0.50    0.92    --  105.02-146.00-128.00  100
  9  \w     56.00 117.00   0.50    0.92    --  105.02-139.00 -42.00  122
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'XtaLAB Synergy, Single source at home/near, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0094552000
_diffrn_orient_matrix_UB_12      -0.0893721000
_diffrn_orient_matrix_UB_13      -0.0041535000
_diffrn_orient_matrix_UB_21      0.0423286000
_diffrn_orient_matrix_UB_22      0.0197033000
_diffrn_orient_matrix_UB_23      0.0170889000
_diffrn_orient_matrix_UB_31      -0.0032693000
_diffrn_orient_matrix_UB_32      -0.0033630000
_diffrn_orient_matrix_UB_33      0.2110049000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0404
_diffrn_reflns_av_unetI/netI     0.0520
_diffrn_reflns_Laue_measured_fraction_full 0.975
_diffrn_reflns_Laue_measured_fraction_max 0.928
_diffrn_reflns_limit_h_max       44
_diffrn_reflns_limit_h_min       -44
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -3
_diffrn_reflns_number            6597
_diffrn_reflns_point_group_measured_fraction_full 0.730
_diffrn_reflns_point_group_measured_fraction_max 0.685
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.040
_diffrn_reflns_theta_min         2.495
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    14.758
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.88345
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.93a (Rigaku Oxford Diffraction, 2020)
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    1.796
_exptl_crystal_description       needle
_exptl_crystal_F_000             2328
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.082
_refine_diff_density_min         -0.730
_refine_diff_density_rms         0.113
_refine_ls_abs_structure_details
;
 Classical Flack method preferred over Parsons because s.u. lower.
;
_refine_ls_abs_structure_Flack   -0.01(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.007
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     261
_refine_ls_number_reflns         3100
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.011
_refine_ls_R_factor_all          0.0605
_refine_ls_R_factor_gt           0.0429
_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^)+(0.0619P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1066
_refine_ls_wR_factor_ref         0.1175
_reflns_Friedel_coverage         0.360
_reflns_Friedel_fraction_full    0.438
_reflns_Friedel_fraction_max     0.397
_reflns_number_gt                2336
_reflns_number_total             3100
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc05689a2.cif
_cod_data_source_block           an103_2_autored
_cod_depositor_comments
'Adding full bibliography for 7132559--7132561.cif.'
_cod_database_code               7132560
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C H Cd S O'
_chemical_oxdiff_usercomment     '300 K'
_shelx_estimated_absorpt_t_max   0.590
_shelx_estimated_absorpt_t_min   0.096
_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
C21 \\sim O3: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
within 2A
3.a Aromatic/amide H refined with riding coordinates:
 C12(H12), C16(H16), C13(H13), C5(H5), C6(H6), C17(H17), C9(H9), C3(H3),
 C19(H19), C20(H20), C10(H10), C2(H2)
3.b Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C21(H21A,H21B,H21C), C14(H14A,H14B,H14C)
;
_shelx_res_checksum              1376
_shelx_hkl_checksum              18155
_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 1.194
_oxdiff_exptl_absorpt_empirical_full_min 0.697