A Triad Molecular Conductor: Simultaneous Control of Charge and Molecular Arrangements
kinoshita, Naoya; Maruyama, Atsuya; Shirahata, Takashi; Naito, Toshio; Misaki, Yohji; Chemical Communications  (2023) –; doi:10.1039/D3CC03198E

data_7132196
_publ_section_title
;
 A Triad Molecular Conductor: Simultaneous Control of Charge and Molecular
 Arrangements
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D3CC03198E
_journal_year                    2023
_chemical_formula_moiety         'C24 H16 S16 Se4, F6 P'
_chemical_formula_sum            'C24 H16 F6 P S16 Se4'
_chemical_formula_weight         1278.14
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-10-03
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2023-10-06 deposited with the CCDC.	2023-10-10 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 109.992(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.2588(3)
_cell_length_b                   28.5988(6)
_cell_length_c                   12.6211(3)
_cell_measurement_reflns_used    8468
_cell_measurement_temperature    120
_cell_measurement_theta_max      30.1620
_cell_measurement_theta_min      2.0270
_cell_volume                     3818.96(17)
_computing_cell_refinement       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.49 (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 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      120
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.997
_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      1.00  27.00   0.25   16.00    --    5.00  76.00-120.00  104
  2  \w     27.00  60.00   0.25   16.00    --  -15.00  76.00 150.00  132
  3  \w    -54.00 -11.00   0.25   16.00    --  -15.00  76.00 -30.00  172
  4  \w     11.00  73.00   0.25   16.00    --  -15.00  76.00 -30.00  248
  5  \w    -58.00  14.00   0.25   16.00    --  -15.00  76.00 150.00  288
  6  \w    -69.00  33.00   0.25   16.00    --  -15.00  38.00 120.00  408
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC11 (RINC): Kappa single'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0570363000
_diffrn_orient_matrix_UB_12      0.0036357000
_diffrn_orient_matrix_UB_13      -0.0458121000
_diffrn_orient_matrix_UB_21      -0.0113025000
_diffrn_orient_matrix_UB_22      -0.0244372000
_diffrn_orient_matrix_UB_23      -0.0035296000
_diffrn_orient_matrix_UB_31      -0.0334199000
_diffrn_orient_matrix_UB_32      0.0020621000
_diffrn_orient_matrix_UB_33      0.0382930000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0501
_diffrn_reflns_av_unetI/netI     0.0386
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       -37
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            15296
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.484
_diffrn_reflns_theta_min         2.052
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    4.814
_exptl_absorpt_correction_T_max  0.729
_exptl_absorpt_correction_T_min  0.179
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.49 (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            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    2.223
_exptl_crystal_description       plate
_exptl_crystal_F_000             2484
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.349
_refine_diff_density_min         -0.506
_refine_diff_density_rms         0.117
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     233
_refine_ls_number_reflns         4379
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0400
_refine_ls_R_factor_gt           0.0347
_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^)+(0.0501P)^2^+5.8990P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0903
_refine_ls_wR_factor_ref         0.0930
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3923
_reflns_number_total             4379
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc03198e2.cif
_cod_data_source_block           exp_06-120k
_cod_database_code               7132196
_shelx_shelxl_version_number     2019/3
_chemical_oxdiff_formula         'C24 H16 F6 P1 S16 Se4'
_shelx_estimated_absorpt_t_max   0.869
_shelx_estimated_absorpt_t_min   0.291
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C5(H5A,H5B), C6(H6A,H6B), C13(H13A,H13B)
2.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C12(H12)
;
_shelx_res_checksum              1614
_shelx_hkl_checksum              84736
_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 1.884
_oxdiff_exptl_absorpt_empirical_full_min 0.478