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_4130020
_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         'C20 H30 Co, C26 H8 B F10 O2'
_chemical_formula_sum            'C46 H38 B Co F10 O2'
_chemical_formula_weight         882.55
_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                 97.057(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.0423(8)
_cell_length_b                   16.9039(13)
_cell_length_c                   21.2807(14)
_cell_measurement_reflns_used    5902
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      25.87
_cell_measurement_theta_min      2.27
_cell_volume                     3942.1(5)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_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 0.9975
_diffrn_measured_fraction_theta_max 0.9975
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0534
_diffrn_reflns_av_unetI/netI     0.0598
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            33408
_diffrn_reflns_theta_full        27.5395
_diffrn_reflns_theta_max         27.54
_diffrn_reflns_theta_min         1.86
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.523
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6999
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0571 before and 0.0483 after correction.
The Ratio of minimum to maximum transmission is 0.9387.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.4869
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1810.6491
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.6236
_refine_diff_density_min         -0.6416
_refine_diff_density_rms         0.1294
_refine_ls_d_res_high            0.7686
_refine_ls_d_res_low             10.9586
_refine_ls_goodness_of_fit_ref   1.0642
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    18
_refine_ls_number_parameters     540
_refine_ls_number_reflns         9073
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0642
_refine_ls_R_factor_all          0.0886
_refine_ls_R_factor_gt           0.0524
_refine_ls_shift/su_max          0.0003
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0628P)^2^+3.1891P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1267
_refine_ls_wR_factor_ref         0.1459
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              14
_reflns_limit_h_min              -14
_reflns_limit_k_max              21
_reflns_limit_k_min              0
_reflns_limit_l_max              27
_reflns_limit_l_min              0
_reflns_number_gt                6171
_reflns_number_total             9073
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            11-LEL062_0m.cif
_cod_data_source_block           LEL062_0m
_cod_database_code               4130020
_olex2_refinement_description
;
1. Others
 Fixed Uiso: H43c(0.052599) H43b(0.052599) H43a(0.052599) H36a(0.055778)
 H36c(0.055778) H36b(0.055778) H34a(0.044671) H34b(0.044671) H34c(0.044671)
 H33c(0.044046) H33b(0.044046) H33a(0.044046) H44a(0.051994) H44b(0.051994)
 H44c(0.051994) H45c(0.054802) H45a(0.054802) H45b(0.054802) H46a(0.051273)
 H46b(0.051273) H46c(0.051273) H42b(0.050713) H42a(0.050713) H42c(0.050713)
 H32b(0.0519) H32a(0.0519) H32c(0.0519) H35a(0.05377) H35c(0.05377)
 H35b(0.05377) H8(0.02649) H7(0.032773) H6(0.033202) H5(0.029461) H4(0.030206)
 H3(0.033719) H2(0.033509) H1(0.0279)
2.a Me refined with riding coordinates:
 C44(H44a,H44b,H44c), C43(H43a,H43b,H43c), C42(H42a,H42b,H42c), C46(H46a,H46b,
 H46c), C45(H45a,H45b,H45c), C35(H35a,H35b,H35c), C34(H34a,H34b,H34c), C33(H33a,
 H33b,H33c), C32(H32a,H32b,H32c), C36(H36a,H36b,H36c)
2.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C8(H8), C7(H7), C6(H6), C5(H5), C4(H4)
;
_olex2_submission_special_instructions 'No special instructions were received'