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_1565584
_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         'C16 H16 B2 Fe N4'
_chemical_formula_sum            'C16 H16 B2 Fe N4'
_chemical_formula_weight         341.80
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2021-11-03 deposited with the CCDC.	2021-12-06 downloaded from the CCDC.
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_cell_angle_alpha                98.677(9)
_cell_angle_beta                 90.081(8)
_cell_angle_gamma                106.197(8)
_cell_formula_units_Z            2
_cell_length_a                   7.5278(8)
_cell_length_b                   8.0007(9)
_cell_length_c                   12.8810(14)
_cell_measurement_reflns_used    5235
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      25.99
_cell_measurement_theta_min      3.3
_cell_volume                     735.70(14)
_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_publication_material  SHELXL
_computing_structure_refinement  'SHELXL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.978
_diffrn_measured_fraction_theta_max 0.971
_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  0.0680
_diffrn_reflns_av_unetI/netI     0.0639
_diffrn_reflns_Laue_measured_fraction_full 0.978
_diffrn_reflns_Laue_measured_fraction_max 0.971
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            5235
_diffrn_reflns_point_group_measured_fraction_full 0.978
_diffrn_reflns_point_group_measured_fraction_max 0.971
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.612
_diffrn_reflns_theta_min         3.307
_diffrn_source                   'Genix 3D I\mS microfocus X-ray source'
_exptl_absorpt_coefficient_mu    1.026
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.583
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'X-Area (Stoe & Cie, 2001)'
_exptl_crystal_colour            'light brown'
_exptl_crystal_density_diffrn    1.543
_exptl_crystal_description       block
_exptl_crystal_F_000             352
_exptl_crystal_size_max          0.290
_exptl_crystal_size_mid          0.220
_exptl_crystal_size_min          0.140
_refine_diff_density_max         2.377
_refine_diff_density_min         -1.101
_refine_diff_density_rms         0.155
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     216
_refine_ls_number_reflns         2688
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.0853
_refine_ls_R_factor_gt           0.0793
_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^)+(0.1603P)^2^+0.4775P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2082
_refine_ls_wR_factor_ref         0.2155
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2349
_reflns_number_total             2688
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1sc06404e3.cif
_cod_data_source_block           wa2798
_cod_database_code               1565584
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.755
_shelx_estimated_absorpt_t_max   0.870
_shelx_res_checksum              10653
_shelx_hkl_checksum              20969