A free boratriptycene-type Lewis superacid
Henkelmann, Marcel; Omlor, Andreas; Bolte, Michael; Schunemann, Volker; Lerner, Hans-Wolfram; Noga, Jozef; Hrobarik, Peter; Wagner, Matthias; Chemical Science  (2021) –; doi:10.1039/D1SC06404E

data_1565587
_publ_section_title
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 A free boratriptycene-type Lewis superacid
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_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/D1SC06404E
_journal_year                    2021
_chemical_formula_moiety         'C24 B F20, C16 H15 B2 Fe N4'
_chemical_formula_sum            'C40 H15 B3 F20 Fe N4'
_chemical_formula_weight         1019.84
_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   mixed
_atom_sites_solution_primary     direct
_audit_creation_method           SHELXL-2018/3
_audit_update_record
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2021-11-03 deposited with the CCDC.	2021-12-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 105.884(3)
_cell_angle_gamma                90
_cell_formula_units_Z            12
_cell_length_a                   46.3281(16)
_cell_length_b                   18.1515(6)
_cell_length_c                   14.1178(5)
_cell_measurement_reflns_used    45368
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      25.86
_cell_measurement_theta_min      3.12
_cell_volume                     11418.7(7)
_computing_cell_refinement       'X-Area (Stoe & Cie, 2001)'
_computing_data_collection       'X-Area (Stoe & Cie, 2001)'
_computing_data_reduction        'X-Area (Stoe & Cie, 2001)'
_computing_molecular_graphics    'XP in SHELXTL-Plus (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'STOE IPDS II two-circle-diffractometer'
_diffrn_measurement_method       \w
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0533
_diffrn_reflns_av_unetI/netI     0.0610
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       55
_diffrn_reflns_limit_h_min       -55
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            63766
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.027
_diffrn_reflns_theta_min         3.118
_diffrn_source                   'Genix 3D I\mS microfocus X-ray source'
_exptl_absorpt_coefficient_mu    0.535
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.513
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'X-Area (Stoe & Cie, 2001)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.780
_exptl_crystal_description       plate
_exptl_crystal_F_000             6048
_exptl_crystal_size_max          0.180
_exptl_crystal_size_mid          0.130
_exptl_crystal_size_min          0.070
_refine_diff_density_max         0.763
_refine_diff_density_min         -0.460
_refine_diff_density_rms         0.074
_refine_ls_abs_structure_details
; 
 Refined as an inversion twin. 
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_refine_ls_abs_structure_Flack   0.55(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1850
_refine_ls_number_reflns         20126
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0988
_refine_ls_R_factor_gt           0.0619
_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^)+(0.0692P)^2^+46.9565P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1371
_refine_ls_wR_factor_ref         0.1589
_reflns_Friedel_coverage         0.999
_reflns_Friedel_fraction_full    0.998
_reflns_Friedel_fraction_max     0.998
_reflns_number_gt                14890
_reflns_number_total             20126
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1sc06404e3.cif
_cod_data_source_block           wa2927
_cod_original_sg_symbol_H-M      'C c'
_cod_database_code               1565587
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.910
_shelx_estimated_absorpt_t_max   0.964
_shelx_res_checksum              74233
_shelx_hkl_checksum              12904