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_7707245
_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, C16 H36 N'
_chemical_formula_sum            'C40 H36 B F20 N'
_chemical_formula_weight         921.51
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 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
;
2020-11-22 deposited with the CCDC.	2021-04-27 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 130.542(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   23.9161(5)
_cell_length_b                   12.8024(3)
_cell_length_c                   17.3043(4)
_cell_measurement_reflns_used    18606
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.6860
_cell_measurement_theta_min      2.0700
_cell_volume                     4026.3(2)
_computing_cell_refinement       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_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    'SHELXT-2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 10.3321
_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  0.0181
_diffrn_reflns_av_unetI/netI     0.0156
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            35854
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.500
_diffrn_reflns_theta_min         2.365
_diffrn_source                   'fine-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    0.153
_exptl_absorpt_correction_T_max  0.965
_exptl_absorpt_correction_T_min  0.939
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.53 (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            colorless
_exptl_crystal_density_diffrn    1.520
_exptl_crystal_description       block
_exptl_crystal_F_000             1872
_exptl_crystal_size_max          0.565
_exptl_crystal_size_mid          0.523
_exptl_crystal_size_min          0.320
_refine_diff_density_max         0.192
_refine_diff_density_min         -0.163
_refine_diff_density_rms         0.034
_refine_ls_abs_structure_details
;
 Flack x determined using 4114 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.02(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     563
_refine_ls_number_reflns         9127
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0265
_refine_ls_R_factor_gt           0.0247
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0343P)^2^+1.2191P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0610
_refine_ls_wR_factor_ref         0.0621
_reflns_Friedel_coverage         0.973
_reflns_Friedel_fraction_full    0.991
_reflns_Friedel_fraction_max     0.974
_reflns_number_gt                8759
_reflns_number_total             9127
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt01192h2.cif
_cod_data_source_block           '[(nBu)4N][B(C6F5)4]'
_cod_depositor_comments
'Adding full bibliography for 7707245--7707255.cif.'
_cod_original_cell_volume        4026.33(18)
_cod_original_sg_symbol_H-M      'C c'
_cod_database_code               7707245
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.919
_shelx_estimated_absorpt_t_max   0.953
_oxdiff_exptl_absorpt_empirical_full_min 0.967
_oxdiff_exptl_absorpt_empirical_full_max 1.037
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_shelx_res_checksum              12427
_shelx_hkl_checksum              71024