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_4111540
_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            'C20 H42 N4'
_chemical_formula_weight         338.58
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_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                 105.034(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.795(3)
_cell_length_b                   12.267(3)
_cell_length_c                   16.109(4)
_cell_measurement_reflns_used    2195
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      25.567
_cell_measurement_theta_min      2.440
_cell_volume                     2251.0(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  0.0640
_diffrn_reflns_av_sigmaI/netI    0.0723
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            9075
_diffrn_reflns_theta_full        22.71
_diffrn_reflns_theta_max         22.71
_diffrn_reflns_theta_min         5.10
_exptl_absorpt_coefficient_mu    0.059
_exptl_absorpt_correction_T_max  1.000000
_exptl_absorpt_correction_T_min  0.650222
_exptl_absorpt_correction_type   semi-empirical
_exptl_absorpt_process_details   'SADABS (Bruker-AXS)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    0.999
_exptl_crystal_description       plate
_exptl_crystal_F_000             760
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.5
_refine_diff_density_max         0.198
_refine_diff_density_min         -0.148
_refine_diff_density_rms         0.036
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.981
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     229
_refine_ls_number_reflns         2986
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.981
_refine_ls_R_factor_all          0.0983
_refine_ls_R_factor_gt           0.0521
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0717P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1164
_refine_ls_wR_factor_ref         0.1353
_reflns_number_gt                1874
_reflns_number_total             2986
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja050028gsi20050104_104749.cif
_cod_data_source_block           5
_cod_original_cell_volume        2251.1(9)
_cod_database_code               4111540