Studies of a bola-type bis(dithiafulvene) molecular system: synthesis, crystal structure, and electrochemical properties
Afzali, Azedeh; Tabasi, Zahra A.; Zhang, Baiyu H.; Zhao, Yuming; New Journal of Chemistry 46 (2022) 18133–18145; doi:10.1039/D2NJ01796B

data_7061734
_publ_section_title
;
 Studies of a bola-type bis(dithiafulvene) molecular system: synthesis,
 crystal structure, and electrochemical properties
;
_journal_issue                   38
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              18133
_journal_page_last               18145
_journal_paper_doi               10.1039/D2NJ01796B
_journal_volume                  46
_journal_year                    2022
_chemical_formula_moiety         'C27 H28 O2 S8'
_chemical_formula_sum            'C27 H28 O2 S8'
_chemical_formula_weight         640.97
_space_group_crystal_system      monoclinic
_space_group_IT_number           13
_space_group_name_Hall           '-P 2yc'
_space_group_name_H-M_alt        'P 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2020-10-13
_audit_creation_method
;
Olex2 1.3
(compiled 2020.07.31 svn.rc2a77460 for OlexSys, GUI svn.r6145)
;
_audit_update_record
;
2022-03-11 deposited with the CCDC.	2022-08-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 98.392(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   21.3010(5)
_cell_length_b                   5.21057(12)
_cell_length_c                   13.0620(3)
_cell_measurement_reflns_used    6189
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      75.8650
_cell_measurement_theta_min      2.0910
_cell_volume                     1434.23(6)
_computing_cell_refinement       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_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_environment      N~2~
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.984
_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    -24.00  64.00   0.50    0.07    --   47.45 -61.00 -67.00  176
  2  \w     35.00  79.00   0.50    0.27    --  107.75 -61.00 -67.00   88
  3  \w     35.00  79.00   0.50    0.27    --  107.75 -61.00-120.00   88
  4  \w     35.00  79.00   0.50    0.27    --  107.75 -61.00-180.00   88
  5  \w     35.00 106.00   0.50    0.27    --  107.75 -94.00-180.00  142
  6  \w     35.00  79.00   0.50    0.27    --  107.75 -61.00 -30.00   88
  7  \w     35.00 106.00   0.50    0.27    --  107.75 -94.00  30.00  142
  8  \w     35.00 131.00   0.50    0.27    --  107.75 -77.00  30.00  192
  9  \w     94.00 178.00   0.50    0.27    --  107.75  15.00   0.00  168
 10  \w     95.00 178.00   0.50    0.27    --  107.75 125.00   0.00  166
 11  \w     95.00 178.00   0.50    0.27    --  107.75 125.00 120.00  166
 12  \w     91.00 178.00   0.50    0.27    --  107.75  61.00  71.00  174
 13  \w     85.00 178.00   0.50    0.27    --  107.75  77.00 120.00  186
 14  \w     31.00 120.00   0.50    0.07    --   47.45  61.00  71.00  178
 15  \w     35.00  79.00   0.50    0.27    --  107.75 -61.00 150.00   88
 16  \w     35.00 106.00   0.50    0.27    --  107.75 -94.00 120.00  142
 17  \w     35.00 112.00   0.50    0.27    --  107.75-125.00 150.00  154
 18  \w     35.00 106.00   0.50    0.27    --  107.75 -94.00 -60.00  142
 19  \w     35.00 111.00   0.50    0.07    --   47.45  37.00  30.00  152
 20  \w    -16.00  28.00   0.50    0.07    --  -47.45  19.00  60.00   88
 21  \w    -43.00 -14.00   0.50    0.27    --  -86.25  45.00 -90.00   58
 22  \w    -43.00 -14.00   0.50    0.27    --  -86.25  45.00-120.00   58
 23  \w    -59.00  25.00   0.50    0.07    --  -47.45  57.00   0.00  168
 24  \w    -64.00  25.00   0.50    0.07    --  -47.45  61.00  71.00  178
 25  \w    -65.00 -13.00   0.50    0.27    --  -86.25  61.00  71.00  104
 26  \w   -120.00 -31.00   0.50    0.07    --  -47.45 -61.00 -67.00  178
 27  \w   -120.00 -32.00   0.50    0.07    --  -47.45 -57.00-150.00  176
 28  \w   -159.00 -70.00   0.50    0.27    --  -86.25 -61.00 -67.00  178
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0143447000
_diffrn_orient_matrix_UB_12      -0.2111430000
_diffrn_orient_matrix_UB_13      -0.0758371000
_diffrn_orient_matrix_UB_21      -0.0705336000
_diffrn_orient_matrix_UB_22      -0.0053782000
_diffrn_orient_matrix_UB_23      -0.0476014000
_diffrn_orient_matrix_UB_31      0.0127082000
_diffrn_orient_matrix_UB_32      0.2071010000
_diffrn_orient_matrix_UB_33      -0.0786599000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0745
_diffrn_reflns_av_unetI/netI     0.0402
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -5
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            18250
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.412
_diffrn_reflns_theta_min         2.097
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    5.970
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.47409
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.84a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'light yellow'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.484
_exptl_crystal_description       block
_exptl_crystal_F_000             668
_exptl_crystal_size_max          0.232
_exptl_crystal_size_mid          0.179
_exptl_crystal_size_min          0.039
_refine_diff_density_max         1.106
_refine_diff_density_min         -0.581
_refine_diff_density_rms         0.112
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.102
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     170
_refine_ls_number_reflns         3013
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.102
_refine_ls_R_factor_all          0.0658
_refine_ls_R_factor_gt           0.0631
_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^)+(0.0863P)^2^+4.5688P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1733
_refine_ls_wR_factor_ref         0.1752
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2765
_reflns_number_total             3013
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2nj01796b2.cif
_cod_data_source_block           a12c1
_cod_depositor_comments
'Adding full bibliography for 7061734--7061735.cif.'
_cod_database_code               7061734
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C31H36O2S8
_shelx_estimated_absorpt_t_max   0.801
_shelx_estimated_absorpt_t_min   0.338
_reflns_odcompleteness_completeness 99.97
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     74.33
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Fixed Sof: H14A(0.5) H14B(0.5)
3.a Secondary CH2 refined with riding coordinates:
 C13(H13A,H13B), C14(H14A,H14B)
3.b Aromatic/amide H refined with riding coordinates:
 C6(H6), C8(H8), C9(H9), C11(H11), C12(H12)
3.c Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C), C5(H5A,H5B,H5C)
;
_shelx_res_checksum              56612
_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
;
_oxdiff_exptl_absorpt_empirical_full_max 1.895
_oxdiff_exptl_absorpt_empirical_full_min 0.495