Crystal structures of two charge‒transfer complexes of benzo[1,2-<i>c</i>:3,4-<i>c</i>':5,6-<i>c</i>'']trithiophene (<i>D</i>~3<i>h~</i>-BTT)
Qin, Qian; Mague, Joel T.; Gould, Haley E.; Vasquez, Samuel E.; Heyer, Anthony E.; Acta Crystallographica Section E 75 (2019) 1573–1577; doi:10.1107/S2056989019013161

data_2243608
_publ_section_title
;
 Crystal structures of two charge--transfer complexes of
 benzo[1,2-<i>c</i>:3,4-<i>c</i>':5,6-<i>c</i>'']trithiophene
 (<i>D</i>~3<i>h~</i>-BTT)
;
_journal_coeditor_code           ZL2760
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              1573
_journal_page_last               1577
_journal_paper_doi               10.1107/S2056989019013161
_journal_volume                  75
_journal_year                    2019
_chemical_absolute_configuration unk
_chemical_formula_iupac          'C12 H6 S3, C60, C7 H8'
_chemical_formula_moiety         'C12 H6 S3, C60, C7 H8'
_chemical_formula_sum            'C79 H14 S3'
_chemical_formula_weight         1059.08
_chemical_name_systematic
;
Benzo[1,2-<i>c</i>:3,4-<i>c</i>':5,6-<i>c</i>'']trithiophene--\
buckminsterfullerene--toluene
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                90
_cell_angle_beta                 108.816(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.0139(6)
_cell_length_b                   17.4327(10)
_cell_length_c                   13.0286(8)
_cell_measurement_reflns_used    9987
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      74.4850
_cell_measurement_theta_min      3.5840
_cell_volume                     2152.8(2)
_computing_cell_refinement
;
<i>SAINT</i> (Bruker, 2016)
;
_computing_data_collection
;
<i>APEX3</i> (Bruker, 2016)
;
_computing_data_reduction
;
<i>SAINT</i>  (Bruker, 2016)
;
_computing_molecular_graphics
;
<i>DIAMOND</i> (Brandenburg & Putz, 2012)
;
_computing_publication_material
;
<i>SHELXTL</i> (Sheldrick, 2008)
;
_computing_structure_refinement
;
<i>SHELXL2018/1</i> (Sheldrick, 2015<i>b</i>)
;
_computing_structure_solution
;
<i>SHELXT</i> (Sheldrick, 2015<i>a</i>)
;
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 10.4167
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device_type  'Bruker D8 VENTURE PHOTON 100 CMOS'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0346
_diffrn_reflns_av_unetI/netI     0.0435
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            16787
_diffrn_reflns_theta_full        68.000
_diffrn_reflns_theta_max         74.477
_diffrn_reflns_theta_min         3.584
_diffrn_source                   'INCOATEC I\mS micro--focus source'
_exptl_absorpt_coefficient_mu    2.046
_exptl_absorpt_correction_T_max  0.94
_exptl_absorpt_correction_T_min  0.76
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(<i>SADABS</i>; Krause <i>et al.</i>, 2015)
;
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.634
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1072
_exptl_crystal_size_max          0.325
_exptl_crystal_size_mid          0.297
_exptl_crystal_size_min          0.029
_refine_diff_density_max         0.326
_refine_diff_density_min         -0.259
_refine_ls_abs_structure_details
;
 Refined as an inversion twin
;
_refine_ls_abs_structure_Flack   0.36(2)
_refine_ls_extinction_coef       0.0009(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method
;
<i>SHELXL2018/1</i> (Sheldrick, 2015<i>b</i>)
;
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1307
_refine_ls_number_reflns         7520
_refine_ls_number_restraints     3769
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0449
_refine_ls_R_factor_gt           0.0417
_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^)+(0.0640P)^2^+0.8700P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1085
_refine_ls_wR_factor_ref         0.1122
_reflns_number_gt                7066
_reflns_number_total             7520
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            zl2760sup1.cif
_cod_data_source_block           II
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               2243608
_shelx_estimated_absorpt_t_min   0.556
_shelx_estimated_absorpt_t_max   0.943
_shelx_hkl_checksum              13198
_shelx_res_checksum              82174
_cod_database_fobs_code 2243608