An Unusual Reduction of an Imine Bond: The Isolation of a Stable π-Iminium Intermediate
Eric W. Ainscough; Andrew M. Brodie; Anthony K. Burrell; Steven M. F. Kennedy; Journal of the American Chemical Society 123 (2001) 10391–10392; doi:10.1021/ja0109996

data_4115727
_publ_section_title
;
 An Unusual Reduction of an Imine Bond: The Isolation of a Stable
 \p-Iminium Intermediate
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              10391
_journal_page_last               10392
_journal_paper_doi               10.1021/ja0109996
_journal_volume                  123
_journal_year                    2001
_chemical_formula_sum            'C39 H30 Cl2 N O2 P2 W'
_chemical_formula_weight         861.33
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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
_audit_creation_method           SHELXL-97
_cell_angle_alpha                68.9950(10)
_cell_angle_beta                 85.7360(10)
_cell_angle_gamma                71.9260(10)
_cell_formula_units_Z            2
_cell_length_a                   11.0236(2)
_cell_length_b                   12.0855(2)
_cell_length_c                   16.6620(3)
_cell_measurement_reflns_used    8198
_cell_measurement_temperature    203(2)
_cell_measurement_theta_max      27.47
_cell_measurement_theta_min      1.31
_cell_volume                     1968.35(6)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      203(2)
_diffrn_measured_fraction_theta_full 0.000
_diffrn_measured_fraction_theta_max 0.947
_diffrn_measurement_device_type  'Siemens SMART CCD area-detector'
_diffrn_measurement_method       '\w 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  0.0195
_diffrn_reflns_av_sigmaI/netI    0.0255
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            19519
_diffrn_reflns_theta_full        0.50
_diffrn_reflns_theta_max         27.47
_diffrn_reflns_theta_min         1.31
_exptl_absorpt_coefficient_mu    3.183
_exptl_absorpt_correction_T_max  0.5280
_exptl_absorpt_correction_T_min  0.3284
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(Blessing, 1995)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.453
_exptl_crystal_description       plate
_exptl_crystal_F_000             850
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.23
_refine_diff_density_max         1.360
_refine_diff_density_min         -0.748
_refine_diff_density_rms         0.077
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     424
_refine_ls_number_reflns         8557
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.0218
_refine_ls_R_factor_gt           0.0206
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0273P)^2^+1.7704P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0531
_refine_ls_wR_factor_ref         0.0538
_reflns_number_gt                8198
_reflns_number_total             8557
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0109996_2.cif
_cod_data_source_block           sk10
_cod_database_code               4115727