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_1571181
_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), C6 Fe O12, C7 H6 O, H3 O'
_chemical_formula_sum            'C53 H41 Fe O14 S32'
_chemical_formula_weight         1983.63
_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
_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                89.485(5)
_cell_angle_beta                 86.524(6)
_cell_angle_gamma                62.861(9)
_cell_formula_units_Z            2
_cell_length_a                   10.2331(10)
_cell_length_b                   11.1922(9)
_cell_length_c                   35.2191(14)
_cell_measurement_reflns_used    7965
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      71.8160
_cell_measurement_theta_min      4.3870
_cell_volume                     3582.2(6)
_computing_cell_refinement       'CrysAlisPro 1.171.42.38a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.42.38a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.42.38a (Rigaku OD, 2021)'
_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      150.15
_diffrn_detector_area_resol_mean 15.9832
_diffrn_detector_type            Sapphire3
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.963
_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     19.00 103.00   1.00   15.00    --   35.96  57.00-150.00   84
  3  \w     22.00  89.00   1.00   15.00    --   35.96-125.00  30.00   67
  4  \w     15.00 106.00   1.00   15.00    --   35.96  19.00 -90.00   91
  5  \w     34.00  84.00   1.00   15.00    --   35.96-125.00 -90.00   50
  6  \w     46.00  85.00   1.00   15.00    --   35.96-118.00 135.00   39
  7  \w     95.00 130.00   1.00   60.00    --  108.00  61.00 150.00   35
  8  \w     42.00  93.00   1.00   60.00    --  108.00 -45.00  60.00   51
  9  \w    107.00 167.00   1.00   60.00    --  108.00 111.00 120.00   60
 10  \w     87.00 157.00   1.00   60.00    --  108.00  30.00 120.00   70
 11  \w     46.00  84.00   1.00   60.00    --  108.00 -94.00  30.00   38
 12  \w     52.00  99.00   1.00   60.00    --  108.00 -94.00  90.00   47
 13  \w     76.00 102.00   1.00   60.00    --  108.00 -94.00 -60.00   26
 14  \w    150.00 175.00   1.00   60.00    --  108.00  61.00 150.00   25
 15  \w    102.00 173.00   1.00   60.00    --  108.00  77.00  60.00   71
 16  \w     94.00 170.00   1.00   60.00    --  108.00  61.00-150.00   76
 17  \w    -26.00   0.00   1.00   15.00    --  -33.50  57.00 -90.00   26
 18  \w    -17.00  12.00   1.00   15.00    --  -33.50  37.00 150.00   29
 19  \w     66.00 103.00   1.00   15.00    --   36.58  37.00 150.00   37
 20  \w    -30.00  49.00   1.00   15.00    --   36.58 -57.00   0.00   79
 21  \w     21.00  63.00   1.00   15.00    --   36.58  37.00 150.00   42
 22  \w    -31.00   9.00   1.00   15.00    --   36.58 -57.00  90.00   40
 23  \w     20.00  85.00   1.00   15.00    --   36.58  57.00 -30.00   65
 24  \w    138.00 170.00   1.00   60.00    --  108.00  77.00-180.00   32
 25  \w    102.00 127.00   1.00   60.00    --  108.00  77.00-180.00   25
 26  \w     38.00 119.00   1.00   60.00    --  108.00 -30.00 120.00   81
 27  \w     91.00 125.00   1.00   60.00    --  108.00  45.00 -30.00   34
 28  \w    131.00 157.00   1.00   60.00    --  108.00  45.00 -30.00   26
 29  \w     53.00  79.00   1.00   60.00    --  108.00 -94.00  60.00   26
 30  \w     49.00 109.00   1.00   60.00    --  108.00-111.00   0.00   60
 31  \w    108.00 133.00   1.00   60.00    --  108.00 111.00 150.00   25
 32  \w     43.00 111.00   1.00   60.00    --  108.00 -61.00-150.00   68
 33  \w     80.00 109.00   1.00   60.00    --  108.00-111.00-120.00   29
 34  \w     61.00  90.00   1.00   60.00    --  108.00 -94.00 150.00   29
 35  \w    113.00 139.00   1.00   60.00    --  108.00 111.00  30.00   26
 36  \w     46.00  80.00   1.00   60.00    --  108.00 -94.00-150.00   34
 37  \w     39.00  64.00   1.00   60.00    --  108.00 -30.00  30.00   25
 38  \w    -70.00 -35.00   1.00   15.00    --  -33.50 178.00 150.00   35
 39  \w     66.00  92.00   1.00   15.00    --   35.96 178.00-180.00   26
 40  \w    -17.00   9.00   1.00   15.00    --   35.96 -77.00-180.00   26
 41  \w     80.00 106.00   1.00   60.00    --  108.00-111.00  90.00   26
 42  \w     97.00 123.00   1.00   60.00    --  108.00  45.00-150.00   26
 43  \w    132.00 162.00   1.00   60.00    --  108.00  45.00-150.00   30
 44  \w     81.00 106.00   1.00   60.00    --  108.00 -94.00-180.00   25
 45  \w     46.00  72.00   1.00   60.00    --  108.00 -94.00-180.00   26
 46  \w    112.00 145.00   1.00   60.00    --  108.00 111.00  90.00   33
 47  \w     79.00 105.00   1.00   60.00    --  108.00 -94.00-120.00   26
 48  \w     83.00 109.00   1.00   60.00    --  108.00-111.00-180.00   26
 49  \w     50.00  76.00   1.00   60.00    --  108.00-111.00  90.00   26
;
_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  0.0916
_diffrn_reflns_av_unetI/netI     0.1241
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.963
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       42
_diffrn_reflns_limit_l_min       -43
_diffrn_reflns_number            30593
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.963
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.415
_diffrn_reflns_theta_min         4.440
_exptl_absorpt_coefficient_mu    10.948
_exptl_absorpt_correction_T_max  0.605
_exptl_absorpt_correction_T_min  0.366
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.38a (Rigaku Oxford Diffraction, 2021)
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    1.839
_exptl_crystal_description       'black block'
_exptl_crystal_F_000             2018
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.869
_refine_diff_density_min         -2.038
_refine_diff_density_rms         0.390
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.514
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     942
_refine_ls_number_reflns         13666
_refine_ls_number_restraints     1474
_refine_ls_restrained_S_all      1.443
_refine_ls_R_factor_all          0.1749
_refine_ls_R_factor_gt           0.1359
_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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3833
_refine_ls_wR_factor_ref         0.4348
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9309
_reflns_number_total             13666
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4ce00099d1.cif
_cod_data_source_block           rp3a_abs
_cod_depositor_comments
'Adding full bibliography for 1571179--1571183.cif.'
_cod_original_cell_volume        3582.2(5)
_cod_database_code               1571181
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.560
_shelx_estimated_absorpt_t_min   0.309
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All O(H,H,H) groups
2. Restrained distances
 O14-H14A = O14-H14C = O14-H14B
 0.84 with sigma of 0.02
 H14A-H14B = H14B-H14C
 1.37 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08 within 2A
Uanis(C3D) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
5. Others
 Sof(C11B)=Sof(H11C)=Sof(H11D)=Sof(C12B)=Sof(H12C)=Sof(H12D)=1-FVAR(1)
 Sof(C1B)=Sof(H1BA)=Sof(H1BB)=Sof(C2B)=Sof(H2BA)=Sof(H2BB)=FVAR(1)
 Sof(C11D)=Sof(H11A)=Sof(H11B)=Sof(C12D)=Sof(H12A)=Sof(H12B)=1-FVAR(2)
 Sof(C9D)=Sof(H9DA)=Sof(H9DB)=Sof(C10D)=Sof(H10A)=Sof(H10B)=FVAR(2)
6.a Free rotating group:
 O14(H14A,H14B,H14C)
6.b Secondary CH2 refined with riding coordinates:
 C1C(H1CA,H1CB), C1D(H1DA,H1DB), C2C(H2CA,H2CB), C2D(H2DA,H2DB), C9C(H9CA,
 H9CB), C9D(H9DA,H9DB), C10C(H10E,H10F), C10D(H10A,H10B), C11D(H11A,H11B),
 C12D(H12A,H12B), C1B(H1BA,H1BB), C2B(H2BA,H2BB), C9B(H9BA,H9BB), C10B(H10C,
 H10D), C11B(H11C,H11D), C12B(H12C,H12D), C1A(H1AA,H1AB), C2A(H2AA,H2AB),
 C9A(H9AA,H9AB), C10A(H10G,H10H)
6.c Aromatic/amide H refined with riding coordinates:
 C8(H8), C9(H9), C10(H10), C11(H11), C12(H12), C13(H13)
;
_shelx_res_checksum              41730
_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
;