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_4115726
_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_moiety         'C42 H33 B Cl4 F4 N O3 P2 W'
_chemical_formula_sum            'C42 H33 B Cl4 F4 N O3 P2 W'
_chemical_formula_weight         1074.09
_chemical_name_systematic
; 
 ? 
;
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_symmetry_space_group_name_Hall  '-P 1'
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_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                95.6520(10)
_cell_angle_beta                 105.2640(10)
_cell_angle_gamma                111.0940(10)
_cell_formula_units_Z            2
_cell_length_a                   10.91880(10)
_cell_length_b                   12.88350(10)
_cell_length_c                   17.43280(10)
_cell_measurement_reflns_used    8192
_cell_measurement_temperature    203(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      1.24
_cell_volume                     2155.81(4)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'XPMA (Zsolnai, 1994)'
_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 0.948
_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
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_diffrn_reflns_av_sigmaI/netI    0.0290
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            21461
_diffrn_reflns_theta_full        0.50
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         1.24
_exptl_absorpt_coefficient_mu    3.058
_exptl_absorpt_correction_T_max  0.7296
_exptl_absorpt_correction_T_min  0.5397
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(Blessing, 1995)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.655
_exptl_crystal_description       shard
_exptl_crystal_F_000             1058
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_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.11
_refine_diff_density_max         1.504
_refine_diff_density_min         -1.323
_refine_diff_density_rms         0.092
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     523
_refine_ls_number_reflns         9391
_refine_ls_number_restraints     0
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_refine_ls_R_factor_all          0.0328
_refine_ls_R_factor_gt           0.0279
_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^)+(0.0291P)^2^+3.9877P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0661
_refine_ls_wR_factor_ref         0.0693
_reflns_number_gt                8582
_reflns_number_total             9391
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0109996_1.cif
_cod_data_source_block           sk14
_cod_original_cell_volume        2155.80(3)
_cod_database_code               4115726