Tandem Processes Identified from Reaction Screening: Nucleophilic Addition to Aryl N-Phosphinylimines Employing La(III)-TFAA Activation
Hidenori Kinoshita; Oscar J. Ingham; Winnie W. Ong; Aaron B. Beeler; John A. Porco; Journal of the American Chemical Society 132 (2010) 6412–6418; doi:10.1021/ja100346w

data_4102383
_publ_section_title
;
 Tandem Processes Identified from Reaction Screening: Nucleophilic
 Addition to Aryl N-Phosphinylimines Employing La(III)-TFAA Activation
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              6412
_journal_page_last               6418
_journal_paper_doi               10.1021/ja100346w
_journal_volume                  132
_journal_year                    2010
_chemical_formula_moiety         'C28 H26 F3 N O4'
_chemical_formula_sum            'C28 H26 F3 N O4'
_chemical_formula_weight         497.50
_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                90.235(12)
_cell_angle_beta                 115.124(11)
_cell_angle_gamma                105.603(11)
_cell_formula_units_Z            2
_cell_length_a                   10.320(3)
_cell_length_b                   11.387(4)
_cell_length_c                   12.207(4)
_cell_measurement_reflns_used    3714
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      23.88
_cell_measurement_theta_min      2.45
_cell_volume                     1239.3(7)
_computing_cell_refinement       'Bruker SAINT+'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT+'
_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      173(2)
_diffrn_measured_fraction_theta_full 0.973
_diffrn_measured_fraction_theta_max 0.973
_diffrn_measurement_device_type  'Bruker X8 APEX II diffractometer'
_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  0.0320
_diffrn_reflns_av_sigmaI/netI    0.0549
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            18829
_diffrn_reflns_theta_full        28.50
_diffrn_reflns_theta_max         28.50
_diffrn_reflns_theta_min         1.86
_exptl_absorpt_coefficient_mu    0.104
_exptl_absorpt_correction_T_max  0.9796
_exptl_absorpt_correction_T_min  0.9404
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.333
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             520
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.214
_refine_diff_density_min         -0.323
_refine_diff_density_rms         0.047
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.082
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     470
_refine_ls_number_reflns         6124
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.082
_refine_ls_R_factor_all          0.0833
_refine_ls_R_factor_gt           0.0462
_refine_ls_shift/su_max          1.113
_refine_ls_shift/su_mean         0.030
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0590P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1134
_refine_ls_wR_factor_ref         0.1236
_reflns_number_gt                3683
_reflns_number_total             6124
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja100346w_si_005.cif
_cod_data_source_block           Compound_86
_cod_original_cell_volume        1239.4(7)
_cod_database_code               4102383