Synthetic, spectroscopic, structural, and electrochemical investigations of ferricenium derivatives with weakly coordinating anions: ion pairing, substituent, and solvent effects.
Khan, Firoz Shah Tuglak; Waldbusser, Amy L.; Carrasco, Maria C.; Pourhadi, Hadi; Hematian, Shabnam; Dalton transactions (Cambridge, England : 2003) 50 (2021) 7433–7455; doi:10.1039/d1dt01192h

data_7707251
_publ_section_title
;
 Synthetic, spectroscopic, structural, and electrochemical investigations
 of ferricenium derivatives with weakly coordinating anions: ion pairing,
 substituent, and solvent effects.
;
_journal_issue                   21
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              7433
_journal_page_last               7455
_journal_paper_doi               10.1039/d1dt01192h
_journal_volume                  50
_journal_year                    2021
_chemical_formula_moiety         'C24 B F20, C20 H30 Fe'
_chemical_formula_sum            'C44 H30 B F20 Fe'
_chemical_formula_weight         1005.34
_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     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2021-04-21 deposited with the CCDC.	2021-04-27 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.297(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   16.5730(4)
_cell_length_b                   19.8456(5)
_cell_length_c                   24.3129(5)
_cell_measurement_reflns_used    21997
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.2590
_cell_measurement_theta_min      3.5060
_cell_volume                     7996.4(3)
_computing_cell_refinement       'CrysAlisPro 1.171.39.29c (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.29c (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.29c (Rigaku OD, 2017)'
_computing_molecular_graphics    'SHELXTL v6.10 (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL v6.10 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXS-2018/3 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1066
_diffrn_reflns_av_unetI/netI     0.0900
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            135211
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        24.999
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         2.217
_diffrn_source                   'fine-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    0.505
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.962
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.67a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.670
_exptl_crystal_description       block
_exptl_crystal_F_000             4040
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.526
_refine_diff_density_min         -0.383
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.973
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1213
_refine_ls_number_reflns         14294
_refine_ls_number_restraints     24
_refine_ls_restrained_S_all      0.973
_refine_ls_R_factor_all          0.0750
_refine_ls_R_factor_gt           0.0463
_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^)+(0.0565P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1044
_refine_ls_wR_factor_ref         0.1102
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9740
_reflns_number_total             14294
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt01192h2.cif
_cod_data_source_block           Me10FcBArF20
_cod_depositor_comments
'Adding full bibliography for 7707245--7707255.cif.'
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7707251
_shelx_shelxl_version_number     2018/3
_twin_information
;
Twin law determination (relative to component 1)
Matrix 1 is taken from component 1 (  16.578   19.846   24.319    90.00    90.30    90.05)
Matrix 2 is taken from component 2 (  16.565   19.855   24.339    89.88    90.17    90.14)
Twin analysis: Component 1 with component 2
TL  =UB[1]-1*UB[2]:  -1.0008  -0.0014  -0.0046     0.0003  -0.9995  -0.0085     0.0021  -0.0153   0.9991   det 0.999564
TL-1=UB[2]*UB[1]-1:  -0.9992   0.0015  -0.0046    -0.0003  -1.0004  -0.0086     0.0021  -0.0153   1.0007   det 1.000436
Rot= 179.9869 deg around the following vectors: 
Reciprocal space (hkl): -0.0031 -0.0051 1.0000
Direct space (uvw)    : 0.0010 -0.0076 1.0000

BASF refines to 0.3351(7)
;
_oxdiff_exptl_absorpt_empirical_full_min 0.933
_oxdiff_exptl_absorpt_empirical_full_max 1.078
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_shelx_res_checksum              50109
_shelx_hkl_checksum              35756