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_1573420
_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   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2024-10-27
_audit_creation_method
;
Olex2 1.5
(compiled 2024.01.12 svn.r2f8d729c for OlexSys, GUI svn.r6928)
;
_cell_angle_alpha                94.801(3)
_cell_angle_beta                 90.106(3)
_cell_angle_gamma                99.151(4)
_cell_formula_units_Z            2
_cell_length_a                   6.6582(3)
_cell_length_b                   8.2694(4)
_cell_length_c                   32.8995(9)
_cell_measurement_reflns_used    9320
_cell_measurement_temperature    263.15
_cell_measurement_theta_max      31.1540
_cell_measurement_theta_min      1.8610
_cell_volume                     1781.88(13)
_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      263.15
_diffrn_detector                 CCD
_diffrn_detector_area_resol_mean 7.111
_diffrn_detector_type            'Rigaku Saturn724+ area detector'
_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   -110.00  70.00   0.30    6.00    --  -20.00  45.00   0.00  600
  2  \w   -110.00  70.00   0.30    6.00    --  -20.00  45.00  90.00  600
  3  \w   -110.00  70.00   0.30    6.00    --  -20.00  45.00 180.00  600
  4  \w   -110.00  70.00   0.30    6.00    --  -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      -0.0078420000
_diffrn_orient_matrix_UB_12      0.0842918000
_diffrn_orient_matrix_UB_13      -0.0006468000
_diffrn_orient_matrix_UB_21      0.0124514000
_diffrn_orient_matrix_UB_22      0.0119371000
_diffrn_orient_matrix_UB_23      0.0215145000
_diffrn_orient_matrix_UB_31      0.1069088000
_diffrn_orient_matrix_UB_32      0.0188544000
_diffrn_orient_matrix_UB_33      -0.0022166000
_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  0.1166
_diffrn_reflns_av_unetI/netI     0.1211
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_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            20565
_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         27.481
_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    0.836
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.91523
_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    1.674
_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         0.850
_refine_diff_density_min         -0.433
_refine_diff_density_rms         0.105
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.962
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     438
_refine_ls_number_reflns         8170
_refine_ls_number_restraints     24
_refine_ls_restrained_S_all      0.962
_refine_ls_R_factor_all          0.1209
_refine_ls_R_factor_gt           0.0584
_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^)+(0.0443P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1049
_refine_ls_wR_factor_ref         0.1266
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4627
_reflns_number_total             8170
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            rac-DMCh-EDT-TTF_PF6_263K.cif
_cod_data_source_block           rac-dmch-et_pf6-thf-2_autored
_cod_database_code               1573420
_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
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 S5-C13A \\sim S5-C13B
 with sigma of 0.02
 C14-C13A \\sim C14-C13B
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C13B \\sim C13A: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08 within 1.7A
4. Rigid body (RIGU) restrains
 C13B, S5, C11, C14, S6
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(H14C)=Sof(H14D)=Sof(C13B)=Sof(H13C)=Sof(H13D)=1-FVAR(1)
 Sof(H14A)=Sof(H14B)=Sof(C13A)=Sof(H13A)=Sof(H13B)=FVAR(1)
6.a Ternary CH refined with riding coordinates:
 C18(H18), C4(H4), C3(H3), C17(H17)
6.b Secondary CH2 refined with riding coordinates:
 C20(H20A,H20B), C6(H6A,H6B), C5(H5A,H5B), C27(H27A,H27B), C28(H28A,H28B),
 C19(H19A,H19B), C14(H14A,H14B), C14(H14C,H14D), C13A(H13A,H13B), C13B(H13C,
 H13D)
6.c Idealised Me refined as rotating group:
 C15(H15A,H15B,H15C), C16(H16A,H16B,H16C), C2(H2A,H2B,H2C), C1(H1A,H1B,H1C)
;
_shelx_res_checksum              17517
_shelx_hkl_checksum              90619
_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 1.746
_oxdiff_exptl_absorpt_empirical_full_min 0.822