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_4130019
_publ_section_title
;
 Stable Borocyclic Radicals via Frustrated Lewis Pair Hydrogenations.
;
_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         'C26 H8 B F10 O2'
_chemical_formula_sum            'C26 H8 B F10 O2'
_chemical_formula_weight         553.16
_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                 99.583(4)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   13.1089(10)
_cell_length_b                   23.2919(19)
_cell_length_c                   14.0746(9)
_cell_measurement_reflns_used    5086
_cell_measurement_temperature    149(2)
_cell_measurement_theta_max      27.61
_cell_measurement_theta_min      2.48
_cell_volume                     4237.4(5)
_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    'SIR2004 (Burla et al., 2007)'
_diffrn_ambient_temperature      149(2)
_diffrn_measured_fraction_theta_full 0.9997
_diffrn_measured_fraction_theta_max 0.9997
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1378
_diffrn_reflns_av_unetI/netI     0.1596
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            38155
_diffrn_reflns_theta_full        24.9996
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.58
_exptl_absorpt_coefficient_mu    0.168
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6051
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0760 before and 0.0583 after correction.
The Ratio of minimum to maximum transmission is 0.8116.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_density_diffrn    1.7340
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plates
_exptl_crystal_F_000             2202.0884
_refine_diff_density_max         1.1537
_refine_diff_density_min         -0.8985
_refine_diff_density_rms         0.2086
_refine_ls_d_res_high            0.8409
_refine_ls_d_res_low             12.9260
_refine_ls_goodness_of_fit_ref   1.0764
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    32
_refine_ls_number_parameters     702
_refine_ls_number_reflns         7466
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0764
_refine_ls_R_factor_all          0.1681
_refine_ls_R_factor_gt           0.0862
_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^)+(0.1500P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2303
_refine_ls_wR_factor_ref         0.2790
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              15
_reflns_limit_h_min              -15
_reflns_limit_k_max              27
_reflns_limit_k_min              0
_reflns_limit_l_max              16
_reflns_limit_l_min              0
_reflns_number_gt                3830
_reflns_number_total             7466
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            3-LEL024_0m.cif
_cod_data_source_block           LEL024_0m
_cod_original_cell_volume        4237.4(6)
_cod_database_code               4130019
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C24(H24), C25(H25), C26(H26), C27(H27), C28(H28), C29(H29),
 C33(H33), C34(H34), C50(H50), C51(H51), C52(H52), C53(H53), C54(H54), C55(H55)
;
_olex2_submission_special_instructions 'No special instructions were received'