BEDT-TTF radical-cation salts with tris(oxalato)chromate and guest additives.
Blundell, Toby J.; Ogar, Joseph O.; Brannan, Michael J.; Rusbridge, Elizabeth K.; Wallis, John D.; Akutsu, Hiroki; Nakazawa, Yasuhiro; Imajo, Shusaku; Martin, Lee; RSC advances 14 (2024) 18444–18452; doi:10.1039/d4ra03425b

data_7248852
_publ_section_title
;
 BEDT-TTF radical-cation salts with tris(oxalato)chromate and guest
 additives.
;
_journal_issue                   26
_journal_name_full               'RSC advances'
_journal_page_first              18444
_journal_page_last               18452
_journal_paper_doi               10.1039/d4ra03425b
_journal_volume                  14
_journal_year                    2024
_chemical_formula_moiety         'C6 Cr O12, 4(C10 H8 S8), C6 H5 O, H3 O'
_chemical_formula_sum            'C52 H40 Cr O14 S32'
_chemical_formula_weight         1966.76
_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
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2024-04-18
_audit_creation_method
;
Olex2 1.5-beta
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2024-04-18 deposited with the CCDC.	2024-05-30 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 93.139(7)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.3270(2)
_cell_length_b                   19.9211(4)
_cell_length_c                   35.3072(7)
_cell_measurement_reflns_used    29921
_cell_measurement_temperature    298
_cell_measurement_theta_max      27.47
_cell_measurement_theta_min      2.04
_cell_volume                     7252.7(3)
_computing_cell_refinement       'RAPID AUTO'
_computing_data_collection       'RAPID AUTO (Rigaku, ????)'
_computing_data_reduction        'RAPID AUTO'
_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 Version 2018/2 (Sheldrick, 2014)'
_diffrn_ambient_temperature      298.15
_diffrn_detector_area_resol_mean 10.000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0356
_diffrn_reflns_av_unetI/netI     0.0251
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       -45
_diffrn_reflns_number            34185
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.464
_diffrn_reflns_theta_min         2.125
_exptl_absorpt_coefficient_mu    1.141
_exptl_absorpt_correction_T_max  0.843
_exptl_absorpt_correction_T_min  0.426
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSCOR (Rigaku, 1995)'
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.801
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             4000
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.914
_refine_diff_density_min         -0.431
_refine_diff_density_rms         0.084
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     498
_refine_ls_number_reflns         8299
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0457
_refine_ls_R_factor_gt           0.0391
_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^)+(0.0619P)^2^+5.4666P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1050
_refine_ls_wR_factor_ref         0.1097
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7129
_reflns_number_total             8299
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4ra03425b1.cif
_cod_data_source_block           m191031a
_cod_original_cell_volume        7252.7(2)
_cod_database_code               7248852
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.848
_shelx_estimated_absorpt_t_min   0.764
_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
 O8-H8A = O8-H8B
 1 with sigma of 0.02
 O8-H8A \\sim O8-H8B \\sim O8-H8A_$1
 with sigma of 0.001
3. Others
 Sof(C7B)=Sof(H7BA)=Sof(H7BB)=Sof(C8B)=Sof(H8BA)=Sof(H8BB)=1-FVAR(1)
 Sof(C7A)=Sof(H7AA)=Sof(H7AB)=Sof(C8A)=Sof(H8AA)=Sof(H8AB)=FVAR(1)
 Sof(C9B)=Sof(H9BA)=Sof(H9BB)=Sof(C10B)=Sof(H10C)=Sof(H10D)=1-FVAR(2)
 Sof(C9A)=Sof(H9AA)=Sof(H9AB)=Sof(C10A)=Sof(H10A)=Sof(H10B)=FVAR(2)
 Fixed Sof: O7(0.5) H7(0.5)
4.a Secondary CH2 refined with riding coordinates:
 C7A(H7AA,H7AB), C8A(H8AA,H8AB), C7B(H7BA,H7BB), C8B(H8BA,H8BB), C9A(H9AA,
 H9AB), C10A(H10A,H10B), C9B(H9BA,H9BB), C10B(H10C,H10D), C17(H17A,H17B),
 C18(H18A,H18B), C19(H19A,H19B), C20(H20A,H20B)
4.b Aromatic/amide H refined with riding coordinates:
 C24(H24), C26(H26), C27(H27)
4.c Idealised tetrahedral OH refined as rotating group:
 O7(H7)
;
_shelx_res_checksum              93401
_olex2_submission_special_instructions 'No special instructions were received'