Synthesis of nitrogen heterocycles via alpha-aminoalkyl radicals generated from alpha-silyl secondary amines under visible light irradiation
Kazunari Nakajima; Mai Kitagawa; Yuya Ashida; Yoshihiro Miyake; Yoshiaki Nishibayashi; Chem.Commun. 50 (2014) 8900–; doi:10.1039/C4cc03000A

data_7115388
_publ_section_title
;
 Synthesis of nitrogen heterocycles via alpha-aminoalkyl radicals
 generated from alpha-silyl secondary amines under visible light
 irradiation
;
_journal_name_full               Chem.Commun.
_journal_page_first              8900
_journal_paper_doi               10.1039/C4cc03000A
_journal_volume                  50
_journal_year                    2014
_chemical_formula_moiety         'C19 H19 N O3'
_chemical_formula_sum            'C19 H19 N O3'
_chemical_formula_weight         309.36
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                96.837(5)
_cell_angle_beta                 105.663(5)
_cell_angle_gamma                109.836(5)
_cell_formula_units_Z            2
_cell_length_a                   7.9490(18)
_cell_length_b                   9.913(3)
_cell_length_c                   11.241(3)
_cell_measurement_reflns_used    2191
_cell_measurement_temperature    93
_cell_measurement_theta_max      27.43
_cell_measurement_theta_min      3.23
_cell_volume                     780.3(4)
_computing_cell_refinement       'RAPID AUTO'
_computing_data_collection       'RAPID AUTO (Rigaku, ????)'
_computing_data_reduction        'RAPID AUTO'
_computing_molecular_graphics    'CrystalStructure 4.0'
_computing_publication_material  'CrystalStructure 4.0 (Rigaku, 2010)'
_computing_structure_refinement  'CRYSTALS (Carruthers, et al., 1999)'
_computing_structure_solution    SIR97
_diffrn_ambient_temperature      93
_diffrn_detector_area_resol_mean 10.000
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0501
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            7619
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.089
_exptl_absorpt_correction_T_max  0.991
_exptl_absorpt_correction_T_min  0.561
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSCOR (Rigaku, 1995)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.317
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             328.00
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.391
_refine_diff_density_min         -0.289
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.914
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     227
_refine_ls_number_reflns         3541
_refine_ls_R_factor_gt           0.0579
_refine_ls_shift/su_max          0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[0.0023Fo^2^ + 2.0000\s(Fo^2^)]/(4Fo^2^)'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.1583
_reflns_number_gt                2722
_reflns_number_total             3541
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            c4cc03000a2.cif
_cod_data_source_block           20131125
_cod_original_cell_volume        780.3(3)
_cod_database_code               7115388