Preparation, Spectroscopic Characterization and Theoretical Study of a Three-Dimensional Conjugated 70 π-Electron Thiophene 6-mer Radical Cation π-Dimer
Fujiwara, Toshihiro; Muranaka, Atsuya; Nishinaga, Tohru; Aoyagi, Shinobu; Kobayashi, Nagao; Uchiyama, Masanobu; Otani, Hiroyuki; Iyoda, Masahiko; Journal of the American Chemical Society  (2020) –; doi:10.1021/jacs.9b13573

data_4134264
_publ_section_title
;
 Preparation, Spectroscopic Characterization and Theoretical Study of a
 Three-Dimensional Conjugated 70 \p-Electron Thiophene 6-mer Radical
 Cation \p-Dimer
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_paper_doi               10.1021/jacs.9b13573
_journal_year                    2020
_chemical_formula_sum            'C53 H50 Cl2 F6 S6 Sb'
_chemical_formula_weight         1185.94
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2017/1
_cell_angle_alpha                90
_cell_angle_beta                 93.824(7)
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   14.1298(16)
_cell_length_b                   38.475(4)
_cell_length_c                   38.518(4)
_cell_measurement_reflns_used    445902
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      14.091
_cell_measurement_theta_min      0.616
_cell_volume                     20893(4)
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_diffrn_ambient_temperature      90(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'SPring-8 BL02B1'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.4139
_diffrn_reflns_av_R_equivalents  0.2880
_diffrn_reflns_av_unetI/netI     0.1314
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       45
_diffrn_reflns_limit_k_min       -45
_diffrn_reflns_limit_l_max       45
_diffrn_reflns_limit_l_min       -45
_diffrn_reflns_number            430240
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        14.091
_diffrn_reflns_theta_max         14.091
_diffrn_reflns_theta_min         0.616
_exptl_absorpt_coefficient_mu    0.220
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.508
_exptl_crystal_description       plate
_exptl_crystal_F_000             9648
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.02
_refine_diff_density_max         3.144
_refine_diff_density_min         -1.543
_refine_diff_density_rms         0.195
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.830
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2449
_refine_ls_number_reflns         35642
_refine_ls_number_restraints     1566
_refine_ls_restrained_S_all      1.814
_refine_ls_R_factor_all          0.2195
_refine_ls_R_factor_gt           0.1667
_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^)+(0.1000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3627
_refine_ls_wR_factor_ref         0.3857
_reflns_Friedel_coverage         0.000
_reflns_number_gt                21952
_reflns_number_total             35642
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b13573_si_002.cif
_cod_data_source_block           shelx
_cod_original_cell_volume        20894(4)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4134264
_shelx_shelxl_version_number     2017/1
_shelx_res_checksum              68788