Selective C-H Activation α to Primary Amines. Bridging Metallaaziridines for Catalytic, Intramolecular α-Alkylation
Jason A. Bexrud; Patrick Eisenberger; David C. Leitch; Philippa R. Payne; Laurel L. Schafer; Journal of the American Chemical Society 131 (2009) 2116–2118; doi:10.1021/ja808862w

data_4103923
_publ_section_title
;
 Selective C-H Activation \a to Primary Amines. Bridging Metallaaziridines
 for Catalytic, Intramolecular \a-Alkylation
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              2116
_journal_page_last               2118
_journal_paper_doi               10.1021/ja808862w
_journal_volume                  131
_journal_year                    2009
_chemical_formula_moiety         'C83 H88 N6 O3 Ti2'
_chemical_formula_sum            'C83 H88 N6 O3 Ti2'
_chemical_formula_weight         1313.39
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           9
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 c 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                 110.135(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   56.082(3)
_cell_length_b                   13.3274(8)
_cell_length_c                   21.6153(12)
_cell_measurement_reflns_used    9925
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      25.018
_cell_measurement_theta_min      2.343
_cell_volume                     15168.5(15)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0306
_diffrn_reflns_av_sigmaI/netI    0.0428
_diffrn_reflns_limit_h_max       57
_diffrn_reflns_limit_h_min       -66
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            49297
_diffrn_reflns_theta_full        25.02
_diffrn_reflns_theta_max         25.02
_diffrn_reflns_theta_min         1.80
_exptl_absorpt_coefficient_mu    0.261
_exptl_absorpt_correction_T_max  0.9803
_exptl_absorpt_correction_T_min  0.7805
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.150
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             5568
_exptl_crystal_size_max          1.00
_exptl_crystal_size_mid          0.70
_exptl_crystal_size_min          0.40
_refine_diff_density_max         0.629
_refine_diff_density_min         -0.209
_refine_diff_density_rms         0.047
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.001(12)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           fullcycle
_refine_ls_number_parameters     1659
_refine_ls_number_reflns         23228
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.0498
_refine_ls_R_factor_gt           0.0409
_refine_ls_shift/su_max          0.017
_refine_ls_shift/su_mean         0.004
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0718P)^2^+4.8695P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1090
_refine_ls_wR_factor_ref         0.1154
_reflns_number_gt                20420
_reflns_number_total             23228
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja808862w_si_002.cif
_cod_data_source_block           ls152_0m
_cod_database_code               4103923