Evidence for Radical Fragmentations from Persistent Singlet Carbenes
Xavier Cattoën; Karinne Miqueu; Heinz Gornitzka; Didier Bourissou; Guy Bertrand; Journal of the American Chemical Society 127 (2005) 3292–3293; doi:10.1021/ja050028g

data_4111539
_publ_section_title
;
 Evidence for Radical Fragmentations from Persistent Singlet Carbenes
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              3292
_journal_page_last               3293
_journal_paper_doi               10.1021/ja050028g
_journal_volume                  127
_journal_year                    2005
_chemical_formula_sum            'C39 H52 B N3'
_chemical_formula_weight         573.65
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 97.558(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.0301(19)
_cell_length_b                   9.5538(15)
_cell_length_c                   31.063(5)
_cell_measurement_reflns_used    9336
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      26.438
_cell_measurement_theta_min      1.984
_cell_volume                     3539.2(10)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      193(2)
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'Bruker CCD detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0365
_diffrn_reflns_av_sigmaI/netI    0.0399
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            17188
_diffrn_reflns_theta_full        24.71
_diffrn_reflns_theta_max         24.71
_diffrn_reflns_theta_min         5.10
_exptl_absorpt_coefficient_mu    0.062
_exptl_absorpt_correction_T_max  1.000000
_exptl_absorpt_correction_T_min  0.707205
_exptl_absorpt_correction_type   semi-empirical
_exptl_absorpt_process_details   'SABABS (Bruker-AXS)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.077
_exptl_crystal_description       block
_exptl_crystal_F_000             1248
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.6
_refine_diff_density_max         0.201
_refine_diff_density_min         -0.153
_refine_diff_density_rms         0.030
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     394
_refine_ls_number_reflns         5960
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.074
_refine_ls_R_factor_all          0.0629
_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
'calc w=1/[\s^2^(Fo^2^)+(0.0335P)^2^+1.2906P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1056
_refine_ls_wR_factor_ref         0.1122
_reflns_number_gt                4793
_reflns_number_total             5960
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja050028gsi20050104_104737.cif
_cod_data_source_block           1b
_cod_original_cell_volume        3539.1(10)
_cod_database_code               4111539