C‒H Bond Amination by Photochemically Generated Transient Borylnitrenes at Room Temperature: A Combined Experimental and Theoretical Investigation of the Insertion Mechanism and Influence of Substituents
Filthaus, Matthias; Schwertmann, Larissa; Neuhaus, Patrik; Seidel, Rüdiger W.; Oppel, Iris M.; Bettinger, Holger F.; Organometallics 31 (2012) 3894–; doi:10.1021/om300063y

data_4078229
_publ_section_title
;
 C--H Bond Amination by Photochemically Generated Transient Borylnitrenes
 at Room Temperature: A Combined Experimental and Theoretical
 Investigation of the Insertion Mechanism and Influence of Substituents
;
_journal_issue                   10
_journal_name_full               Organometallics
_journal_page_first              3894
_journal_paper_doi               10.1021/om300063y
_journal_volume                  31
_journal_year                    2012
_chemical_formula_sum            'C16 H18 B N5 O4 S2'
_chemical_formula_weight         419.28
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           5
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C 2y'
_symmetry_space_group_name_H-M   'C 1 2 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 102.626(18)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   20.875(5)
_cell_length_b                   8.8602(17)
_cell_length_c                   5.2408(11)
_cell_measurement_reflns_used    1350
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      36.6
_cell_measurement_theta_min      3.00
_cell_volume                     945.9(4)
_computing_cell_refinement       'CrysAlis RED Oxford diffraction'
_computing_data_collection       'CrysAlis CCD Oxford diffraction'
_computing_data_reduction        'CrysAlis RED Oxford diffraction'
_computing_molecular_graphics    SHELXL-97
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      153(2)
_diffrn_detector_area_resol_mean 8.4171
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  '560 frames in \w and 15 sec'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0664
_diffrn_reflns_av_sigmaI/netI    0.0716
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       6
_diffrn_reflns_limit_l_min       -6
_diffrn_reflns_number            4253
_diffrn_reflns_theta_full        25.99
_diffrn_reflns_theta_max         25.99
_diffrn_reflns_theta_min         3.78
_exptl_absorpt_coefficient_mu    0.316
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.472
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             436
_exptl_crystal_size_max          0.426
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.102
_refine_diff_density_max         0.639
_refine_diff_density_min         -0.290
_refine_diff_density_rms         0.068
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.1(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     138
_refine_ls_number_reflns         1674
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0820
_refine_ls_R_factor_gt           0.0641
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0956P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1573
_refine_ls_wR_factor_ref         0.1649
_reflns_number_gt                1293
_reflns_number_total             1674
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om300063y_si_001.cif
_cod_data_source_block           6c
_cod_original_cell_volume        945.9(3)
_cod_original_sg_symbol_H-M      C2
_cod_database_code               4078229