Generation of Boryl-nitroxide Radicals from a Boraalkene via the Nitroso Ene Reaction
Chen, Chaohuang; Daniliuc, Constantin Gabriel; Klabunde, Sina; Hansen, Michael Ryan; Kehr, Gerald; Erker, Gerhard; Chemical Science  (2022) –; doi:10.1039/D2SC02485C

data_1567495
_publ_section_title
;
 Generation of Boryl-nitroxide Radicals from a Boraalkene via the Nitroso
 Ene Reaction
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/D2SC02485C
_journal_year                    2022
_chemical_formula_sum            'C39 H39 B F5 N3 O'
_chemical_formula_weight         671.54
_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'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           'APEX3 v2019.11-0'
_audit_update_record
;
2022-03-11 deposited with the CCDC.	2022-08-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 110.1980(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.5547(5)
_cell_length_b                   10.2914(4)
_cell_length_c                   20.8535(8)
_cell_measurement_reflns_used    9980
_cell_measurement_temperature    100.(2)
_cell_measurement_theta_max      26.7050
_cell_measurement_theta_min      2.2359
_cell_volume                     3334.4(2)
_computing_cell_refinement       'SAINT V8.40B (Bruker Nano, Inc., 2019)'
_computing_data_collection       'Bruker APEX3 v2019.11-0 Photon III'
_computing_data_reduction        'SAINT V8.40B (Bruker Nano, Inc., 2019)'
_computing_molecular_graphics    'shelXle (C.B. Huebschle, rev 994)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100.(2)
_diffrn_detector_area_resol_mean 7.3910
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device       'Bruker D8 Venture Photon III Diffractometer'
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       'phi/omega scans'
_diffrn_radiation_monochromator  'MX mirror'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0749
_diffrn_reflns_av_unetI/netI     0.0284
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            87549
_diffrn_reflns_theta_full        25.24
_diffrn_reflns_theta_max         26.81
_diffrn_reflns_theta_min         2.24
_diffrn_source                   MoK\a
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_type              'micro focus tube'
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    0.099
_exptl_absorpt_correction_T_max  0.99
_exptl_absorpt_correction_T_min  0.94
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 - Bruker AXS area detector scaling and absorption
correction. Reference: Krause, L., Herbst-Irmer, R., Sheldrick G.M.
& Stalke D., J. Appl. Cryst. 48 (2015) 3-10.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.338
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1408
_exptl_crystal_size_max          0.416
_exptl_crystal_size_mid          0.168
_exptl_crystal_size_min          0.131
_refine_diff_density_max         0.329
_refine_diff_density_min         -0.235
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.092
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     453
_refine_ls_number_reflns         7108
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.092
_refine_ls_R_factor_all          0.0597
_refine_ls_R_factor_gt           0.0480
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0313P)^2^+2.7168P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0973
_refine_ls_wR_factor_ref         0.1025
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6054
_reflns_number_total             7108
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2sc02485c6.cif
_cod_data_source_block           8_erk10033
_cod_database_code               1567495
_shelx_res_checksum              62104
_shelx_hkl_checksum              39467