Molecular Conductors Based on Dimethylcyclohexene-Fused Tetrathiafulvalene
Fujisaki, Masahiro; Naito, Ryoya; Shirahata, Takashi; Kawasugi, Yoshitaka; Tajima, Naoya; Misaki, Yohji; Chemistry 6 (2024) 1509–1522; doi:10.3390/chemistry6060091

data_1573423
_publ_section_title
;
 Molecular Conductors Based on Dimethylcyclohexene-Fused
 Tetrathiafulvalene
;
_journal_issue                   6
_journal_name_full               Chemistry
_journal_page_first              1509
_journal_page_last               1522
_journal_paper_doi               10.3390/chemistry6060091
_journal_volume                  6
_journal_year                    2024
_chemical_formula_moiety         '2(C14 H16 S6), F6 P'
_chemical_formula_sum            'C28 H32 F6 P S12'
_chemical_formula_weight         898.22
_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   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2024-11-20
_audit_creation_method
;
Olex2 1.5
(compiled 2024.01.12 svn.r2f8d729c for OlexSys, GUI svn.r6928)
;
_cell_angle_alpha                94.785(2)
_cell_angle_beta                 90.361(2)
_cell_angle_gamma                99.344(2)
_cell_formula_units_Z            2
_cell_length_a                   6.6189(2)
_cell_length_b                   8.1402(2)
_cell_length_c                   32.8895(8)
_cell_measurement_reflns_used    18912
_cell_measurement_temperature    100.15
_cell_measurement_theta_max      31.1300
_cell_measurement_theta_min      2.5320
_cell_volume                     1742.10(8)
_computing_cell_refinement       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_collection       'CrystalClear-SM Expert 2.1 b46 (Rigaku, 2016)'
_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, 2018)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100.15
_diffrn_detector                 CCD
_diffrn_detector_area_resol_mean 7.111
_diffrn_detector_type            'Rigaku Saturn724+ area detector'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_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   -110.00  70.00   0.30    5.00    --  -20.00  45.00   0.00  600
  2  \w   -110.00  70.00   0.30    5.00    --  -20.00  45.00  90.00  600
  3  \w   -110.00  70.00   0.30    5.00    --  -20.00  45.00 180.00  600
  4  \w   -110.00  70.00   0.30    5.00    --  -20.00  45.00 270.00  600
;
_diffrn_measurement_device       'AFC11 SATURN724+ Right'
_diffrn_measurement_device_type  'Rigaku Varimax with Saturn'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0458297000
_diffrn_orient_matrix_UB_12      0.0611235000
_diffrn_orient_matrix_UB_13      -0.0091555000
_diffrn_orient_matrix_UB_21      -0.0084042000
_diffrn_orient_matrix_UB_22      0.0423670000
_diffrn_orient_matrix_UB_23      0.0194993000
_diffrn_orient_matrix_UB_31      0.0981255000
_diffrn_orient_matrix_UB_32      0.0482150000
_diffrn_orient_matrix_UB_33      -0.0021224000
_diffrn_radiation_collimation    0.3
_diffrn_radiation_monochromator  'multi-layer mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0543
_diffrn_reflns_av_unetI/netI     0.0552
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       42
_diffrn_reflns_limit_l_min       -42
_diffrn_reflns_number            28964
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.485
_diffrn_reflns_theta_min         1.864
_diffrn_source                   'rotating anode X-ray generator'
_diffrn_source_current           24.0
_diffrn_source_power             1.2
_diffrn_source_target            Mo
_diffrn_source_type              'MicroMax 007'
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    0.855
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.95176
_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            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.712
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             922
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.701
_refine_diff_density_min         -0.397
_refine_diff_density_rms         0.093
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     500
_refine_ls_number_reflns         8026
_refine_ls_number_restraints     107
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0620
_refine_ls_R_factor_gt           0.0409
_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^)+(0.0333P)^2^+0.8222P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0792
_refine_ls_wR_factor_ref         0.0860
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6213
_reflns_number_total             8026
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            rac-DMCh-EDT-TTF_PF6_100K.cif
_cod_data_source_block           rac-dmch-et_pf6-thf-1_autored
_cod_database_code               1573423
_shelx_shelxl_version_number     2019/2
_chemical_oxdiff_formula         C28H32PF6S12
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
2. Restrained distances
 C6-C4 \\sim C6-C4A
 with sigma of 0.02
 C18-C17 \\sim C18-C17A
 with sigma of 0.02
 C18-C17 \\sim C18A-C17
 with sigma of 0.02
 C17-C18A \\sim C17A-C18A
 with sigma of 0.02
 C2-C4 \\sim C2-C4A
 with sigma of 0.02
 C19-C17 \\sim C19-C17A
 with sigma of 0.02
 C16-C18 \\sim C16-C18A
 with sigma of 0.02
 C1-C3 \\sim C1-C3A
 with sigma of 0.02
 C15-C17 \\sim C15-C17A
 with sigma of 0.02
 C4-C3 \\sim C4A-C3
 with sigma of 0.02
 C5-C3 \\sim C5-C3A
 with sigma of 0.02
 C20-C18 \\sim C20-C18A
 with sigma of 0.02
 C4-C3 \\sim C4-C3A
 with sigma of 0.02
 C3-C4A \\sim C3A-C4A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C4A \\sim C4: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08 within 1.7A
C3A \\sim C3: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08 within 1.7A
4. Rigid body (RIGU) restrains
 C4A, C6, C8, C3A, C5, C7, C3, C4, C2, C1
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(H5BC)=Sof(H5BD)=Sof(H6BC)=Sof(H6BD)=Sof(C4A)=Sof(H4A)=Sof(C3A)=Sof(H3A)=1-
 FVAR(1)
 Sof(H5AA)=Sof(H5AB)=Sof(H6AA)=Sof(H6AB)=Sof(C4)=Sof(H4)=Sof(C3)=Sof(H3)=FVAR(1)
 Sof(H20C)=Sof(H20D)=Sof(H19C)=Sof(H19D)=Sof(C18A)=Sof(H18A)=Sof(C17A)=
 Sof(H17A)=1-FVAR(2)
 Sof(H20A)=Sof(H20B)=Sof(H19A)=Sof(H19B)=Sof(C18)=Sof(H18)=Sof(C17)=Sof(H17)=
 FVAR(2)
6.a Ternary CH refined with riding coordinates:
 C4(H4), C18(H18), C3(H3), C17(H17), C4A(H4A), C3A(H3A), C18A(H18A), C17A(H17A)
6.b Secondary CH2 refined with riding coordinates:
 C28(H28A,H28B), C5(H5AA,H5AB), C5(H5BC,H5BD), C27(H27A,H27B), C20(H20A,H20B),
 C20(H20C,H20D), C6(H6AA,H6AB), C6(H6BC,H6BD), C19(H19A,H19B), C19(H19C,H19D),
 C14(H14A,H14B), C13(H13A,H13B)
;
_shelx_res_checksum              96672
_shelx_hkl_checksum              37778
_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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.083
_oxdiff_exptl_absorpt_empirical_full_min 0.927