Stable Borocyclic Radicals via Frustrated Lewis Pair Hydrogenations.
Longobardi, Lauren E.; Liu, Lei; Grimme, Stefan; Stephan, Douglas W.; Journal of the American Chemical Society 138 (2016) 2500–2503; doi:10.1021/jacs.5b12823

data_4130018
_publ_section_title
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 Stable Borocyclic Radicals via Frustrated Lewis Pair Hydrogenations.
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_journal_issue                   8
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              2500
_journal_page_last               2503
_journal_paper_doi               10.1021/jacs.5b12823
_journal_volume                  138
_journal_year                    2016
_chemical_formula_moiety         'C20 H8 B F5 O2'
_chemical_formula_sum            'C20 H8 B F5 O2'
_chemical_formula_weight         386.10
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_Int_Tables_number      14
_audit_creation_date             2015-12-07
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_cell_angle_alpha                90
_cell_angle_beta                 97.455(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.047(2)
_cell_length_b                   14.854(5)
_cell_length_c                   15.221(6)
_cell_measurement_reflns_used    1856
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      25.47
_cell_measurement_theta_min      2.70
_cell_volume                     1579.8(9)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine (Bourhis et al., 2015)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150.03
_diffrn_measured_fraction_theta_full 0.9881
_diffrn_measured_fraction_theta_max 0.9881
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0967
_diffrn_reflns_av_unetI/netI     0.1042
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            13656
_diffrn_reflns_theta_full        24.9981
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.92
_exptl_absorpt_coefficient_mu    0.143
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.5692
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.1045 before and 0.0821 after correction.
The Ratio of minimum to maximum transmission is 0.7634.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.6232
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             776.6446
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.7486
_refine_diff_density_min         -0.5896
_refine_diff_density_rms         0.1596
_refine_ls_d_res_high            0.8409
_refine_ls_d_res_low             10.5867
_refine_ls_goodness_of_fit_ref   1.0968
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    8
_refine_ls_number_parameters     252
_refine_ls_number_reflns         2748
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0968
_refine_ls_R_factor_all          0.1157
_refine_ls_R_factor_gt           0.0772
_refine_ls_shift/su_max          0.0000
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0990P)^2^+3.0659P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1990
_refine_ls_wR_factor_ref         0.2236
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              8
_reflns_limit_h_min              -8
_reflns_limit_k_max              17
_reflns_limit_k_min              0
_reflns_limit_l_max              18
_reflns_limit_l_min              0
_reflns_number_gt                1811
_reflns_number_total             2748
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            4-LEL059_0m.cif
_cod_data_source_block           LEL059_0m
_cod_original_cell_volume        1579.7(9)
_cod_database_code               4130018
_olex2_refinement_description
;
1. Others
 Fixed Uiso: H2(0.03451) H1(0.02827) H3(0.03344) H4(0.02914) H5(0.03047)
 H8(0.02901) H6(0.03645) H7(0.0384)
2.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C1(H1), C3(H3), C4(H4), C5(H5), C8(H8), C6(H6), C7(H7)
;
_olex2_submission_special_instructions 'No special instructions were received'