Synthesis and Structures of Polyiodide Radical Cation Salts of Donors Combining Tetrathiafulvalene with Multiple Thiophene or Oligo-thiophene Substituents.
Short, Jonni; Blundell, Toby J.; Yang, Songjie; Sahin, Onur; Shakespeare, Yiana; Smith, Emma Louise; Martin, Lee; Wallis, John D.; CrystEngComm  (2020) –; doi:10.1039/D0CE00954G

data_7241256
_publ_section_title
;
 Synthesis and Structures of Polyiodide Radical Cation Salts of Donors
 Combining Tetrathiafulvalene with Multiple Thiophene or Oligo-thiophene
 Substituents.
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/D0CE00954G
_journal_year                    2020
_chemical_formula_moiety         '2(I3), C24 H14 S12'
_chemical_formula_sum            'C24 H14 I6 S12'
_chemical_formula_weight         1448.47
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2020-06-02
_audit_creation_method
;
Olex2 1.3
(compiled 2020.02.04 svn.rd84adfe8 for OlexSys, GUI svn.r6032)
;
_audit_update_record
;
2020-06-23 deposited with the CCDC.	2020-09-15 downloaded from the CCDC.
;
_cell_angle_alpha                90.663(5)
_cell_angle_beta                 102.294(6)
_cell_angle_gamma                93.878(5)
_cell_formula_units_Z            2
_cell_length_a                   10.2097(6)
_cell_length_b                   10.9057(6)
_cell_length_c                   17.3954(12)
_cell_measurement_reflns_used    3819
_cell_measurement_temperature    150.01(10)
_cell_measurement_theta_max      28.2670
_cell_measurement_theta_min      3.3990
_cell_volume                     1887.5(2)
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      150.15
_diffrn_detector_area_resol_mean 15.9832
_diffrn_detector_type            Sapphire3
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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    -25.00  23.00   1.00  120.00    --  -16.16 -99.00 120.00   48
  2  \w      0.00  84.00   1.00  120.00    --   16.24  57.00 -60.00   84
  3  \w    -51.00  33.00   1.00  120.00    --   16.24 -57.00 120.00   84
  4  \w      0.00  84.00   1.00  120.00    --   16.24  57.00  30.00   84
  5  \w      0.00  82.00   1.00  120.00    --   16.24  57.00 120.00   82
  6  \w     -3.00  55.00   1.00  120.00    --   16.24  37.00 -90.00   58
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0513
_diffrn_reflns_av_unetI/netI     0.0749
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            15448
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.025
_diffrn_reflns_theta_max         25.025
_diffrn_reflns_theta_min         3.295
_exptl_absorpt_coefficient_mu    5.621
_exptl_absorpt_correction_T_max  0.940
_exptl_absorpt_correction_T_min  0.474
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
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    2.549
_exptl_crystal_description       plank
_exptl_crystal_F_000             1336
_exptl_crystal_preparation       'electrical insulator'
_exptl_crystal_recrystallization_method
'Diffusion of iodine/hexane into donor/DCM'
_exptl_crystal_size_max          0.565
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.022
_refine_diff_density_max         1.253
_refine_diff_density_min         -0.932
_refine_diff_density_rms         0.200
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.177
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     416
_refine_ls_number_reflns         6654
_refine_ls_number_restraints     302
_refine_ls_restrained_S_all      1.152
_refine_ls_R_factor_all          0.0828
_refine_ls_R_factor_gt           0.0620
_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^)+(0.0253P)^2^+2.6514P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0948
_refine_ls_wR_factor_ref         0.1011
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5517
_reflns_number_total             6654
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0ce00954g2.cif
_cod_data_source_block           19ci5i2
_cod_database_code               7241256
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.886
_shelx_estimated_absorpt_t_min   0.143
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 S12B-C21 \\sim S12A-C21
 with sigma of 0.02
 C22B-C21 \\sim C22A-C21
 with sigma of 0.02
 S12B-C24B \\sim S12A-C24A
 with sigma of 0.02
 C22B-C23B \\sim C22A-C23A
 with sigma of 0.02
 C23A-C24A \\sim C23B-C24B
 with sigma of 0.02
3. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
4. Others
 Sof(S12B)=Sof(C22B)=Sof(H22B)=Sof(C23B)=Sof(H23B)=Sof(C24B)=Sof(H24B)=1-FVAR(1)
 Sof(S12A)=Sof(C22A)=Sof(H22A)=Sof(C23A)=Sof(H23A)=Sof(C24A)=Sof(H24A)=FVAR(1)
5.a Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C8(H8A,H8B)
5.b Aromatic/amide H refined with riding coordinates:
 C10(H10), C11(H11), C14(H14), C15(H15), C16(H16), C18(H18), C19(H19),
 C22B(H22B), C23B(H23B), C24B(H24B), C22A(H22A), C23A(H23A), C24A(H24A)
;
_shelx_res_checksum              33589
_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
;