Synthesis, bridgehead functionalization, and photoisomerization of 9,10-diboratatriptycene dianions.
Prey, Sven E.; Gilmer, Jannik; Teichmann, Samira V.; Čaić, Luis; Wenisch, Mischa; Bolte, Michael; Virovets, Alexander; Lerner, Hans-Wolfram; Fantuzzi, Felipe; Wagner, Matthias; Chemical science 14 (2023) 5316–5322; doi:10.1039/d3sc00555k

data_1568570
_publ_section_title
;
 Synthesis, bridgehead functionalization, and photoisomerization of
 9,10-diboratatriptycene dianions.
;
_journal_issue                   20
_journal_name_full               'Chemical science'
_journal_page_first              5316
_journal_page_last               5322
_journal_paper_doi               10.1039/d3sc00555k
_journal_volume                  14
_journal_year                    2023
_chemical_formula_moiety         'C48 H64 B2 K2 O6'
_chemical_formula_sum            'C48 H64 B2 K2 O6'
_chemical_formula_weight         836.81
_chemical_properties_physical    Moisture-sensitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2023-01-25 deposited with the CCDC.	2023-03-03 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 102.177(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.4510(3)
_cell_length_b                   27.0259(12)
_cell_length_c                   18.2350(7)
_cell_measurement_reflns_used    36650
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      26.38
_cell_measurement_theta_min      2.26
_cell_volume                     4552.8(3)
_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 0.999
_diffrn_measured_fraction_theta_max 0.994
_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  0.0520
_diffrn_reflns_av_unetI/netI     0.0432
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            45836
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.977
_diffrn_reflns_theta_min         2.330
_diffrn_source                   'Genix 3D I\mS microfocus X-ray source'
_exptl_absorpt_coefficient_mu    0.255
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.445
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'X-Area (Stoe & Cie, 2001)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.221
_exptl_crystal_description       plate
_exptl_crystal_F_000             1792
_exptl_crystal_size_max          0.240
_exptl_crystal_size_mid          0.140
_exptl_crystal_size_min          0.080
_refine_diff_density_max         0.237
_refine_diff_density_min         -0.222
_refine_diff_density_rms         0.045
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     529
_refine_ls_number_reflns         8880
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0731
_refine_ls_R_factor_gt           0.0500
_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^)+(0.0545P)^2^+0.6924P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1032
_refine_ls_wR_factor_ref         0.1114
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6884
_reflns_number_total             8880
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sc00555k3.cif
_cod_data_source_block           wa3232
_cod_depositor_comments
'Adding full bibliography for 1568566--1568570.cif.'
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               1568570
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.941
_shelx_estimated_absorpt_t_max   0.980
_shelx_res_checksum              59663
_shelx_hkl_checksum              1640