Metal–organic polyhedron from a flexible tetrakis(thiobenzyl-carboxylate)-tetrathiafulvalene
Cheret, Yohan; Avarvari, Narcis; Zigon, Nicolas; CrystEngComm 26 (2024) 2072–2077; doi:10.1039/D3CE01251D

data_7248225
_publ_section_title
;
 Metal--organic polyhedron from a flexible
 tetrakis(thiobenzyl-carboxylate)-tetrathiafulvalene
;
_journal_issue                   15
_journal_name_full               CrystEngComm
_journal_page_first              2072
_journal_page_last               2077
_journal_paper_doi               10.1039/D3CE01251D
_journal_volume                  26
_journal_year                    2024
_chemical_formula_moiety         'C38 H28 O8 S8, 2(C2 H6 O S)'
_chemical_formula_sum            'C42 H40 O10 S10'
_chemical_formula_weight         1025.34
_chemical_name_systematic
'4,4',4'',4'''-(([2,2'-bi(1,3-dithiolylidene)]-4,4',5,5'-tetrayltetrakis(sulfanediyl))tetrakis(methylene))tetrabenzoic acid, dimethylsufoxide solvate'
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2024-01-16
_audit_creation_method
;
Olex2 1.3-ac4
(compiled 2019.04.23 svn.r3594 for Rigaku Oxford Diffraction, GUI svn.r5739)
;
_audit_update_record
;
2024-01-24 deposited with the CCDC.	2024-02-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.723(6)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   21.7980(12)
_cell_length_b                   6.3399(5)
_cell_length_c                   16.8128(10)
_cell_measurement_reflns_used    3032
_cell_measurement_temperature    250.00(10)
_cell_measurement_theta_max      71.8470
_cell_measurement_theta_min      4.0220
_cell_volume                     2323.3(3)
_computing_cell_refinement       'CrysAlisPro 1.171.41.118a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.118a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.118a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      250.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.1990
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.968
_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    -34.00  26.00   1.00    5.00    --   42.94 -19.00  90.00   60
  2  \w    -11.00  14.00   1.00    5.00    --   42.94 -19.00 120.00   25
  3  \w    -32.00  27.00   1.00    5.00    --   42.94 -19.00 -30.00   59
  4  \w    -28.00  42.00   1.00    5.00    --   42.94 -38.00  60.00   70
  5  \w     45.00  71.00   1.00   20.00    --  103.00 -61.00 120.00   26
  6  \w     95.00 158.00   1.00   20.00    --  103.00  77.00  60.00   63
  7  \w     40.00  67.00   1.00   20.00    --  103.00 -61.00 -30.00   27
  8  \w     59.00 104.00   1.00   20.00    --  103.00 -77.00  60.00   45
  9  \w     33.00  71.00   1.00   20.00    --  103.00 -61.00  30.00   38
 10  \w     84.00 158.00   1.00   20.00    --  103.00  77.00-180.00   74
 11  \w     41.00  67.00   1.00   20.00    --  103.00 -61.00-180.00   26
 12  \w     88.00 158.00   1.00   20.00    --  103.00  45.00 120.00   70
 13  \w     85.00 128.00   1.00   20.00    --  103.00  61.00 -30.00   43
 14  \w     35.00  60.00   1.00   20.00    --  103.00 -61.00 150.00   25
 15  \w    132.00 157.00   1.00   20.00    --  103.00 104.00-102.00   25
 16  \w     85.00 110.00   1.00   20.00    --  103.00 104.00-102.00   25
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'SuperNova, Single source at offset/far, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0605878000
_diffrn_orient_matrix_UB_12      0.0582158000
_diffrn_orient_matrix_UB_13      -0.0429371000
_diffrn_orient_matrix_UB_21      -0.0290803000
_diffrn_orient_matrix_UB_22      -0.2058792000
_diffrn_orient_matrix_UB_23      0.0300049000
_diffrn_orient_matrix_UB_31      -0.0218837000
_diffrn_orient_matrix_UB_32      0.1151757000
_diffrn_orient_matrix_UB_33      0.0752060000
_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  0.0336
_diffrn_reflns_av_unetI/netI     0.0415
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.968
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            9432
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.968
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.270
_diffrn_reflns_theta_min         4.056
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.867
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.33101
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.118a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.466
_exptl_crystal_description       plate
_exptl_crystal_F_000             1064
_exptl_crystal_preparation       'slow evap in DMSO'
_exptl_crystal_recrystallization_method 'slow evap in DMSO'
_exptl_crystal_size_max          0.65
_exptl_crystal_size_mid          0.206
_exptl_crystal_size_min          0.178
_refine_diff_density_max         0.435
_refine_diff_density_min         -0.280
_refine_diff_density_rms         0.061
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     400
_refine_ls_number_reflns         4439
_refine_ls_number_restraints     26
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0790
_refine_ls_R_factor_gt           0.0582
_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^)+(0.0949P)^2^+0.4509P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1550
_refine_ls_wR_factor_ref         0.1759
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3228
_reflns_number_total             4439
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3ce01251d2.cif
_cod_data_source_block           cy063_auto
_cod_depositor_comments
'Adding full bibliography for 7248225--7248227.cif.'
_cod_database_code               7248225
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C42 H36 O8 S8'
_shelx_estimated_absorpt_t_max   0.478
_shelx_estimated_absorpt_t_min   0.144
_diffrn_oxdiff_digest_frames
;
012050f1527d01dfd5a4a4947752e3221800027c972
;
_diffrn_oxdiff_digest_hkl
;
019d157a3f1fb2d0dbcf0d0533f06898206ca9
;
_reflns_odcompleteness_completeness 99.54
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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, All O(H) groups
2. Same fragment restrains
{O5A, S5A, C20A, C21A} sigma for 1-2: 0.02, 1-3: 0.04
as
{O5B, S5B, C20B, C21B}
{O1A, O2A, C1A, C2A, C3A, C4A, C5A, C6A, C7A} sigma for 1-2: 0.02, 1-3: 0.04
as
{O1B, O2B, C1B, C2B, C3B, C4B, C5B, C6B, C7B}
3. Others
 Fixed Sof: O5A(0.5) S5A(0.5) C20A(0.5) H20A(0.5) H20B(0.5) H20C(0.5)
 C21A(0.5) H21A(0.5) H21B(0.5) H21C(0.5) O5B(0.5) S5B(0.5) C20B(0.5) H20D(0.5)
 H20E(0.5) H20F(0.5) C21B(0.5) H21D(0.5) H21E(0.5) H21F(0.5) H8AA(0.5)
 H8AB(0.5) H8BC(0.5) H8BD(0.5) O1A(0.5) O2A(0.5) H2A(0.5) C1A(0.5) C2A(0.5)
 C3A(0.5) H3A(0.5) C4A(0.5) H4A(0.5) C5A(0.5) C6A(0.5) H6A(0.5) C7A(0.5)
 H7A(0.5) O1B(0.5) O2B(0.5) H2B(0.5) C1B(0.5) C2B(0.5) C3B(0.5) H3B(0.5)
 C4B(0.5) H4B(0.5) C5B(0.5) C6B(0.5) H6B(0.5) C7B(0.5) H7B(0.5)
4.a Secondary CH2 refined with riding coordinates:
 C12(H12A,H12B), C8(H8AA,H8AB), C8(H8BC,H8BD)
4.b Me refined with riding coordinates:
 C20A(H20A,H20B,H20C), C21A(H21A,H21B,H21C), C20B(H20D,H20E,H20F), C21B(H21D,
 H21E,H21F)
4.c Aromatic/amide H refined with riding coordinates:
 C15(H15), C14(H14), C17(H17), C18(H18), C3A(H3A), C4A(H4A), C6A(H6A),
 C7A(H7A), C3B(H3B), C4B(H4B), C6B(H6B), C7B(H7B)
4.d Idealised tetrahedral OH refined as rotating group:
 O4(H4), O2A(H2A), O2B(H2B)
;
_olex2_exptl_crystal_mounting_method 'paraffin oil'
_olex2_submission_original_sample_id CY_063
_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 3.391
_oxdiff_exptl_absorpt_empirical_full_min 0.457