Mechanistic and Preparative Studies of Radical Chain Homolytic Substitution Reactions of N-Heterocyclic Carbene Boranes and Disulfides
Xiangcheng Pan; Anne-Laure Vallet; Stéphane Schweizer; Karim Dahbi; Bernard Delpech; Nicolas Blanchard; Bernadette Graff; Steven J. Geib; Dennis P. Curran; Jacques Lalevée; Emmanuel Lacôte; Journal of the American Chemical Society 135 (2013) 10484–10491; doi:10.1021/ja403627k

data_4120110
_publ_section_title
;
 Mechanistic and Preparative Studies of Radical Chain Homolytic
 Substitution Reactions of N-Heterocyclic Carbene Boranes and Disulfides
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              10484
_journal_page_last               10491
_journal_paper_doi               10.1021/ja403627k
_journal_volume                  135
_journal_year                    2013
_chemical_formula_sum            'C12 H15 B N6 S'
_chemical_formula_weight         286.17
_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_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_method           SHELXL-2012
_cell_angle_alpha                90
_cell_angle_beta                 112.055(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.3754(10)
_cell_length_b                   7.8232(4)
_cell_length_c                   12.4708(8)
_cell_measurement_temperature    150(2)
_cell_volume                     1480.70(16)
_computing_structure_refinement  'SHELXL-2012 (Sheldrick, 2012)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.952
_diffrn_measured_fraction_theta_max 0.951
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0369
_diffrn_reflns_av_unetI/netI     0.0403
_diffrn_reflns_Laue_measured_fraction_full 0.952
_diffrn_reflns_Laue_measured_fraction_max 0.951
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -5
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            7455
_diffrn_reflns_point_group_measured_fraction_full 0.952
_diffrn_reflns_point_group_measured_fraction_max 0.951
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         67.856
_diffrn_reflns_theta_min         2.911
_exptl_absorpt_coefficient_mu    1.928
_exptl_absorpt_correction_T_max  .952
_exptl_absorpt_correction_T_min  .715
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker Sadabs'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.284
_exptl_crystal_description       plate
_exptl_crystal_F_000             600
_exptl_crystal_size_max          0.180
_exptl_crystal_size_mid          0.140
_exptl_crystal_size_min          0.020
_refine_diff_density_max         0.668
_refine_diff_density_min         -0.369
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.563
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     219
_refine_ls_number_reflns         2565
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.563
_refine_ls_R_factor_all          0.0625
_refine_ls_R_factor_gt           0.0558
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0680P)^2^]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1430
_refine_ls_wR_factor_ref         0.1470
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2227
_reflns_number_total             2565
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja403627k_si_003.cif
_cod_data_source_block           xp_me_sptb_0ma
_cod_depositor_comments
;
The following automatic conversions were performed:

'_atom_sites_solution_primary' value 'direct methods' was changed to
'direct'.

Automatic conversion script
Id: cif_fix_values 6452 2018-10-05 10:23:21Z andrius 
;
_cod_database_code               4120110
_shelx_estimated_absorpt_t_min   0.723
_shelx_estimated_absorpt_t_max   0.962
_shelxl_version_number           2012-9
_shelx_res_checksum              32230