Generation of Alkyl Radical through Direct Excitation of Boracene-Based Alkylborate.
Sato, Yukiya; Nakamura, Kei; Sumida, Yuto; Hashizume, Daisuke; Hosoya, Takamitsu; Ohmiya, Hirohisa; Journal of the American Chemical Society 142 (2020) 9938–9943; doi:10.1021/jacs.0c04456

data_4135004
_publ_section_title
;
 Generation of Alkyl Radical through Direct Excitation of Boracene-Based
 Alkylborate.
;
_journal_issue                   22
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              9938
_journal_page_last               9943
_journal_paper_doi               10.1021/jacs.0c04456
_journal_volume                  142
_journal_year                    2020
_chemical_formula_moiety         'C34 H44 B Li O5, C30 H36 B Li O4'
_chemical_formula_sum            'C64 H80 B2 Li2 O9'
_chemical_formula_weight         1028.78
_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   mixed
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/1
_cell_angle_alpha                90
_cell_angle_beta                 96.6693(11)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.82397(12)
_cell_length_b                   16.16979(18)
_cell_length_c                   32.6888(4)
_cell_measurement_reflns_used    104115
_cell_measurement_temperature    90
_cell_measurement_theta_max      32.683
_cell_measurement_theta_min      1.906
_cell_volume                     5682.52(11)
_computing_cell_refinement       'CrysAlisPro 1.171.39.9f (Rigaku OD, 2015)'
_computing_data_collection       CrystalClear
_computing_data_reduction        'CrysAlisPro 1.171.39.9f (Rigaku OD, 2015)'
_computing_molecular_graphics    SV
_computing_publication_material  'SHELXL-2018/1 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2018/1 (Sheldrick, 2018)'
_computing_structure_solution    SHELXT
_diffrn_ambient_temperature      90
_diffrn_detector_area_resol_mean 7.31
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Rigaku AFC-8 with Saturn70 CCD'
_diffrn_measurement_method       \w-scan
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0573
_diffrn_reflns_av_unetI/netI     0.0208
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       42
_diffrn_reflns_limit_l_min       -42
_diffrn_reflns_number            224284
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.485
_diffrn_reflns_theta_min         1.778
_diffrn_source                   'Fine-focus rotating anode'
_exptl_absorpt_coefficient_mu    0.077
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.92851
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 CrysAlisPro 1.171.39.9f (Rigaku Oxford Diffraction, 2015)
 Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.203
_exptl_crystal_description       block
_exptl_crystal_F_000             2208
_exptl_crystal_size_max          0.152
_exptl_crystal_size_mid          0.117
_exptl_crystal_size_min          0.112
_refine_diff_density_max         0.925
_refine_diff_density_min         -0.310
_refine_diff_density_rms         0.042
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     726
_refine_ls_number_reflns         13012
_refine_ls_number_restraints     26
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0570
_refine_ls_R_factor_gt           0.0456
_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^)+(0.0490P)^2^+2.9119P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1082
_refine_ls_wR_factor_ref         0.1152
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10809
_reflns_number_total             13012
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja0c04456_si_002.cif
_cod_data_source_block           YS019
_cod_depositor_comments
;Adding full bibliography for 4135004.cif.

 Adding full bibliography for 4135004.cif.
;
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4135004
_shelx_shelxl_version_number     2018/1
_shelx_estimated_absorpt_t_min   0.988
_shelx_estimated_absorpt_t_max   0.991
_shelx_res_checksum              93061
_shelx_hkl_checksum              59935