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_1571179
_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), C7 H8, C6 Fe O12, 0.5(H6 O2)'
_chemical_formula_sum            'C53 H43 Fe O13 S32'
_chemical_formula_weight         1969.64
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 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                90
_cell_angle_beta                 94.106(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.2478(6)
_cell_length_b                   19.9069(14)
_cell_length_c                   35.264(2)
_cell_measurement_reflns_used    3718
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      71.7990
_cell_measurement_theta_min      4.4050
_cell_volume                     7175.5(8)
_computing_cell_refinement       'CrysAlisPro 1.171.41.119a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.119a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.119a (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 0.995
_diffrn_measured_fraction_theta_max 0.970
_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    -57.00  34.00   1.00   10.00    --  -33.50  77.00-120.00   91
  2  \w    -68.00 -41.00   1.00   10.00    --  -33.50-178.00 -60.00   27
  3  \w     28.00  53.00   1.00   10.00    --   36.58 -57.00-120.00   25
  4  \w     65.00  96.00   1.00   10.00    --   36.58 178.00-120.00   31
  5  \w    -27.00   9.00   1.00   10.00    --   36.58 -57.00-120.00   36
  6  \w     57.00  88.00   1.00   10.00    --   36.58-178.00  90.00   31
  7  \w     17.00  56.00   1.00   10.00    --   36.58  37.00 150.00   39
  8  \w     60.00 103.00   1.00   10.00    --   36.58  37.00 150.00   43
  9  \w     57.00  86.00   1.00   40.00    --  108.00 -45.00 -90.00   29
 10  \w     93.00 148.00   1.00   40.00    --  108.00  45.00 -30.00   55
 11  \w    104.00 172.00   1.00   40.00    --  108.00 111.00-180.00   68
 12  \w    119.00 151.00   1.00   40.00    --  108.00 111.00-150.00   32
 13  \w     61.00 105.00   1.00   40.00    --  108.00 -94.00  30.00   44
 14  \w     38.00 129.00   1.00   40.00    --  108.00 -30.00  90.00   91
 15  \w     52.00  77.00   1.00   40.00    --  108.00 -94.00-180.00   25
 16  \w     97.00 123.00   1.00   40.00    --  108.00 -45.00 -90.00   26
 17  \w     54.00 125.00   1.00   40.00    --  108.00 -45.00-180.00   71
 18  \w     39.00  84.00   1.00   40.00    --  108.00 -94.00 120.00   45
 19  \w    -93.00 -66.00   1.00   10.00    --  -33.50 -57.00  90.00   27
 20  \w    -50.00 -23.00   1.00   10.00    --  -33.50 -57.00  90.00   27
 21  \w    -50.00 -24.00   1.00   10.00    --  -33.50 -57.00 120.00   26
 22  \w     54.00  87.00   1.00   10.00    --   36.58-125.00 -60.00   33
 23  \w     39.00  90.00   1.00   10.00    --   36.58-125.00  90.00   51
 24  \w     17.00  42.00   1.00   10.00    --   36.58  37.00  30.00   25
;
_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  0.0904
_diffrn_reflns_av_unetI/netI     0.1384
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.970
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       43
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            14834
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.970
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.171
_diffrn_reflns_theta_min         4.442
_exptl_absorpt_coefficient_mu    10.914
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.68242
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.119a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear dark black'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.823
_exptl_crystal_description       block
_exptl_crystal_F_000             4012
_exptl_crystal_size_max          0.132
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.047
_refine_diff_density_max         1.295
_refine_diff_density_min         -0.685
_refine_diff_density_rms         0.162
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     452
_refine_ls_number_reflns         6875
_refine_ls_number_restraints     330
_refine_ls_restrained_S_all      1.017
_refine_ls_R_factor_all          0.1218
_refine_ls_R_factor_gt           0.0862
_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^)+(0.0729P)^2^+51.1098P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2072
_refine_ls_wR_factor_ref         0.2425
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4418
_reflns_number_total             6875
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4ce00099d1.cif
_cod_data_source_block           rp5b_2_auto
_cod_depositor_comments
'Adding full bibliography for 1571179--1571183.cif.'
_cod_database_code               1571179
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.628
_shelx_estimated_absorpt_t_min   0.327
_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
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 O7-H7B_$1 = O7-H7C_$1 = O7-H7A_$1
 0.84 with sigma of 0.02
3. Restrained planarity
 O7, H7A, H7B, H7C
 with sigma of 0.1
4. 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
5. Others
 Fixed Sof: H28A(0.5) H28B(0.5) H28C(0.5) H7A(0.5) H7B(0.5) H7C(0.5)
6.a Free rotating group:
 O7(H7A,H7B,H7C)
6.b Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C9(H9A,H9B), C10(H10A,H10B), C11(H11A,H11B),
 C12(H12A,H12B), C19(H19A,H19B), C20(H20A,H20B)
6.c Aromatic/amide H refined with riding coordinates:
 C24(H24), C25(H25), C26(H26)
6.d Idealised Me refined with everything fixed:
 C28(H28A,H28B,H28C)
;
_shelx_res_checksum              71796
_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
;