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_4130021
_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         'C28 H8 B F10 O2, C10 H10 Co'
_chemical_formula_sum            'C38 H18 B Co F10 O2'
_chemical_formula_weight         766.31
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_Int_Tables_number      15
_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                 117.857(7)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   25.3133(18)
_cell_length_b                   15.9662(18)
_cell_length_c                   16.4000(13)
_cell_measurement_reflns_used    4229
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      22.61
_cell_measurement_theta_min      2.37
_cell_volume                     5860.1(10)
_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      150.01
_diffrn_measured_fraction_theta_full 0.9978
_diffrn_measured_fraction_theta_max 0.9978
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1050
_diffrn_reflns_av_unetI/netI     0.0925
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            47154
_diffrn_reflns_theta_full        27.5294
_diffrn_reflns_theta_max         27.53
_diffrn_reflns_theta_min         1.57
_exptl_absorpt_coefficient_mu    0.689
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6930
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0666 before and 0.0568 after correction.
The Ratio of minimum to maximum transmission is 0.9295.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            block
_exptl_crystal_density_diffrn    1.7370
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       brown
_exptl_crystal_F_000             3077.1367
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.8184
_refine_diff_density_min         -0.8246
_refine_diff_density_rms         0.1988
_refine_ls_d_res_high            0.7689
_refine_ls_d_res_low             12.9976
_refine_ls_goodness_of_fit_ref   1.0326
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    36
_refine_ls_number_parameters     468
_refine_ls_number_reflns         6735
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0326
_refine_ls_R_factor_all          0.1099
_refine_ls_R_factor_gt           0.0470
_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^)+(0.0195P)^2^+7.1369P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0727
_refine_ls_wR_factor_ref         0.0905
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              28
_reflns_limit_h_min              -32
_reflns_limit_k_max              20
_reflns_limit_k_min              0
_reflns_limit_l_max              21
_reflns_limit_l_min              0
_reflns_number_gt                4044
_reflns_number_total             6735
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            10-LEL073_monoc.cif
_cod_data_source_block           LEL073_monoc
_cod_database_code               4130021
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Ternary CH refined with riding coordinates:
 C38(H38), C37(H37), C36(H36), C35(H35), C34(H34), C33(H33), C32(H32),
 C31(H31), C30(H30), C29(H29)
2.b Aromatic/amide H refined with riding coordinates:
 C8(H8), C9(H9), C10(H10), C3(H3), C2(H2), C1(H1), C7(H7), C6(H6)
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_olex2_submission_special_instructions 'No special instructions were received'