Introduction of new guest molecules into BEDT-TTF radical-cation salts with tris(oxalato)ferrate
Blundell, Toby J.; Rusbridge, Elizabeth K.; Pemberton, Rebecca E.; Brannan, Michael J.; Morritt, Alexander L.; Ogar, Joseph O.; Wallis, John D.; Akutsu, Hiroki; Nakazawa, Yasuhiro; Imajo, Shusaku; Martin, Lee; CrystEngComm 26 (2024) 1962–1975; doi:10.1039/D4CE00099D

data_1571183
_publ_section_title
;
 Introduction of new guest molecules into BEDT-TTF radical-cation salts
 with tris(oxalato)ferrate
;
_journal_issue                   14
_journal_name_full               CrystEngComm
_journal_page_first              1962
_journal_page_last               1975
_journal_paper_doi               10.1039/D4CE00099D
_journal_volume                  26
_journal_year                    2024
_chemical_formula_moiety         '4(C10 H8 S8), C10 H5 Fe O12'
_chemical_formula_sum            'C50 H37 Fe O12 S32'
_chemical_formula_weight         1911.56
_space_group_crystal_system      monoclinic
_space_group_IT_number           13
_space_group_name_Hall           '-P 2yac'
_space_group_name_H-M_alt        'P 1 2/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2024-02-28
_audit_creation_method
;
Olex2 1.5-beta
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2024-02-28 deposited with the CCDC.	2024-03-04 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 108.849(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   24.9368(6)
_cell_length_b                   19.4844(3)
_cell_length_c                   31.8267(10)
_cell_measurement_reflns_used    10924
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      71.5970
_cell_measurement_theta_min      3.6590
_cell_volume                     14634.6(7)
_computing_cell_refinement       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.5-beta (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-beta (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      293.00
_diffrn_detector_area_resol_mean 15.9832
_diffrn_detector_type            Sapphire3
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.976
_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   -101.00 -17.00   1.00   15.00    --  -33.50 -57.00-150.00   84
  2  \w      1.00  76.00   1.00   15.00    --   36.58 -99.00-120.00   75
  3  \w    -31.00  53.00   1.00   15.00    --   36.58 -57.00-180.00   84
  4  \w     22.00  90.00   1.00   15.00    --   36.58-125.00  30.00   68
  5  \w    -33.00  56.00   1.00   15.00    --   36.58 -37.00-120.00   89
  6  \w     20.00 104.00   1.00   15.00    --   36.58  57.00 150.00   84
  7  \w    104.00 175.00   1.00   60.00    --  108.00 111.00-120.00   71
  8  \w     39.00  65.00   1.00   60.00    --  108.00 -30.00-150.00   26
  9  \w    103.00 175.00   1.00   60.00    --  108.00  45.00 -60.00   72
 10  \w     38.00 109.00   1.00   60.00    --  108.00-111.00 120.00   71
 11  \w     41.00 123.00   1.00   60.00    --  108.00 -45.00 -60.00   82
 12  \w     78.00 114.00   1.00   60.00    --  108.00 -30.00-150.00   36
 13  \w     63.00  95.00   1.00   60.00    --  108.00 -77.00   0.00   32
 14  \w     39.00 129.00   1.00   60.00    --  108.00 -30.00 120.00   90
 15  \w     38.00  63.00   1.00   15.00    --   36.58 -77.00 -90.00   25
 16  \w     60.00 106.00   1.00   60.00    --  108.00 -94.00  90.00   46
 17  \w     20.00 104.00   1.00   15.00    --   36.58  57.00 -30.00   84
 18  \w     20.00 104.00   1.00   15.00    --   36.58  57.00-150.00   84
 19  \w     20.00 104.00   1.00   15.00    --   36.58  57.00  60.00   84
 20  \w    -31.00  53.00   1.00   15.00    --   36.58 -57.00  90.00   84
 21  \w    -18.00  63.00   1.00   15.00    --   36.58 -77.00   0.00   81
 22  \w    -31.00  53.00   1.00   15.00    --   36.58 -57.00  60.00   84
 23  \w     70.00 178.00   1.00   60.00    --  108.00  15.00-120.00  108
 24  \w     39.00  76.00   1.00   60.00    --  108.00 -94.00-120.00   37
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0581
_diffrn_reflns_av_unetI/netI     0.0625
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.976
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            100690
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.976
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.088
_diffrn_reflns_theta_min         3.547
_exptl_absorpt_coefficient_mu    10.671
_exptl_absorpt_correction_T_max  0.905
_exptl_absorpt_correction_T_min  0.715
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.67a (Rigaku Oxford Diffraction, 2019)
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            'clear black'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.735
_exptl_crystal_description       'black block'
_exptl_crystal_F_000             7768
_exptl_crystal_size_max          0.273
_exptl_crystal_size_mid          0.126
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.018
_refine_diff_density_min         -0.354
_refine_diff_density_rms         0.098
_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     1751
_refine_ls_number_reflns         28103
_refine_ls_number_restraints     1425
_refine_ls_restrained_S_all      0.939
_refine_ls_R_factor_all          0.1527
_refine_ls_R_factor_gt           0.0706
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0942P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1774
_refine_ls_wR_factor_ref         0.2294
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12543
_reflns_number_total             28103
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4ce00099d1.cif
_cod_data_source_block           ekr_37_01_sq
_cod_depositor_comments
'Adding full bibliography for 1571179--1571183.cif.'
_cod_database_code               1571183
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.567
_shelx_estimated_absorpt_t_min   0.159
_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 O(H) groups
2. Restrained distances
 S1E-C1E \\sim S1E-C11E \\sim S2E-C2E \\sim S2E-C12E
 with sigma of 0.02
 S8E-C10E \\sim S7E-C9E
 with sigma of 0.02
 S7C-C11C \\sim S7C-C9C \\sim S8C-C12C \\sim S8C-C10C
 with sigma of 0.02
 C9C-C10C \\sim C12C-C11C
 with sigma of 0.02
 C11E-C12E \\sim C1E-C2E
 with sigma of 0.02
3. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Sof(C11E)=Sof(H11A)=Sof(H11B)=Sof(C12E)=Sof(H12A)=Sof(H12B)=1-FVAR(1)
 Sof(C1E)=Sof(H1EA)=Sof(H1EB)=Sof(C2E)=Sof(H2EA)=Sof(H2EB)=FVAR(1)
 Sof(C11C)=Sof(H11C)=Sof(H11D)=Sof(C12C)=Sof(H12C)=Sof(H12D)=1-FVAR(2)
 Sof(C9C)=Sof(H9CA)=Sof(H9CB)=Sof(C10C)=Sof(H10C)=Sof(H10D)=FVAR(2)
5.a Secondary CH2 refined with riding coordinates:
 C1E(H1EA,H1EB), C2E(H2EA,H2EB), C9E(H9EA,H9EB), C10E(H10A,H10B), C11E(H11A,
 H11B), C12E(H12A,H12B), C1C(H1CA,H1CB), C2C(H2CA,H2CB), C9C(H9CA,H9CB),
 C10C(H10C,H10D), C11C(H11C,H11D), C12C(H12C,H12D), C16(H16A,H16B), C26(H26A,
 H26B), C1A(H1AA,H1AB), C2A(H2AA,H2AB), C9A(H9AA,H9AB), C10A(H10E,H10F),
 C1B(H1BA,H1BB), C2B(H2BA,H2BB), C9B(H9BA,H9BB), C10B(H10G,H10H), C1F(H1FA,
 H1FB), C2F(H2FA,H2FB), C9F(H9FA,H9FB), C10F(H10I,H10J), C1G(H1GA,H1GB),
 C2G(H2GA,H2GB), C9G(H9GA,H9GB), C10G(H10K,H10L), C1D(H1DA,H1DB), C2D(H2DA,
 H2DB), C9D(H9DA,H9DB), C10D(H10M,H10N), C1H(H1HA,H1HB), C2H(H2HA,H2HB),
 C9H(H9HA,H9HB), C10H(H10O,H10P)
5.b Aromatic/amide H refined with riding coordinates:
 C11(H11), C14(H14), C21(H21), C24(H24)
5.c Idealised tetrahedral OH refined as rotating group:
 O4(H4), O16(H16)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 216 electrons were
found in a volume of 1076\%A^3 in 1 void per unit cell.
This is consistent with the presence of 
8[C2H6O] per Unit Cell 
which account for 208 electrons 
per unit cell.
;
_shelx_res_checksum              68724
_shelx_fab_checksum              48333
_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
;