One- and Two-Electron Reduction of Triarylborane-Based Helical Donor-Acceptor Compounds
Jia, Xiangqing; Nitsch, Jörn; Wu, Zhu; Friedrich, Alexandra; Krebs, Johannes; Krummenacher, Ivo; Fantuzzi, Felipe; Braunschweig, Holger; Moos, Michael; Lambert, Christoph; Engels, Bernd; Marder, Todd B.; Chemical Science  (2021) –; doi:10.1039/D1SC02409D

data_1564259
_publ_section_title
;
 One- and Two-Electron Reduction of Triarylborane-Based Helical
 Donor-Acceptor Compounds
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/D1SC02409D
_journal_year                    2021
_chemical_formula_moiety         'C54 H48 B N, C12 H24 K O6'
_chemical_formula_sum            'C66 H72 B K N O6'
_chemical_formula_weight         1025.15
_chemical_name_systematic
'13-(dimesitylboryl)-N,N-di-p-tolyldibenzo[c,g]phenanthren-8-amine (3-B(Mes)2-[5]helix-12-N(p-Tol)2) monoanion'
_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   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2020-11-13 deposited with the CCDC.	2021-07-27 downloaded from the CCDC.
;
_cell_angle_alpha                73.438(9)
_cell_angle_beta                 86.260(12)
_cell_angle_gamma                86.518(8)
_cell_formula_units_Z            2
_cell_length_a                   8.842(3)
_cell_length_b                   13.762(6)
_cell_length_c                   24.038(12)
_cell_measurement_reflns_used    6206
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      20.95
_cell_measurement_theta_min      2.31
_cell_volume                     2795(2)
_computing_cell_refinement       'Saint+ ver. V8.37A (Bruker AXS)'
_computing_data_collection       'APEX2 ver. 2014.9 (Bruker AXS)'
_computing_data_reduction        'Saint+ ver. V8.37A (Bruker AXS)'
_computing_molecular_graphics    'ShelXLe (Huebschle et all, 2011)'
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'CCD area detector (APEX2 CCD)'
_diffrn_detector_area_resol_mean 10.24
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker X8-APEX II'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'multi-layer mirror'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1598
_diffrn_reflns_av_unetI/netI     0.1156
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            99934
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         26.403
_diffrn_reflns_theta_min         2.311
_diffrn_source                   'rotating-anode (Nonius FR-591)'
_exptl_absorpt_coefficient_mu    0.148
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.7003
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SadAbs 2016/2 (Bruker AXS)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.218
_exptl_crystal_description       needle
_exptl_crystal_F_000             1094
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Tetrahydrofuran'
_exptl_crystal_size_max          0.216
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.059
_refine_diff_density_max         0.248
_refine_diff_density_min         -0.254
_refine_diff_density_rms         0.057
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.996
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     684
_refine_ls_number_reflns         11400
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.996
_refine_ls_R_factor_all          0.1467
_refine_ls_R_factor_gt           0.0580
_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^)+(0.0422P)^2^+0.9681P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1019
_refine_ls_wR_factor_ref         0.1311
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5926
_reflns_number_total             11400
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1sc02409d2.cif
_cod_data_source_block           cmpd_2K1
_cod_database_code               1564259
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.969
_shelx_estimated_absorpt_t_max   0.991
_shelx_res_checksum              86767
_shelx_hkl_checksum              75915