Palladium-Assisted Formation of Carbon−Carbon Bonds. Part 10.1Insertion Reactions of Isocyanides into the Pd−C Bond of Orthopalladated Primary Amines. Synthesis of 2-R-Aminoisoindolinium Salts (R =tBu, 2,6-Xylyl)
Vicente, José; Saura-Llamas, Isabel; Grünwald, Claus; Alcaraz, Carmen; Jones, Peter G.; Bautista, Delia; Organometallics 21 (2002) 3587–; doi:10.1021/om020365n

data_4076975
_publ_section_title
;
 Palladium-Assisted Formation of Carbon&#x2212;Carbon Bonds. Part
 10.1Insertion Reactions of Isocyanides into the Pd&#x2212;C Bond of
 Orthopalladated Primary Amines. Synthesis of 2-R-Aminoisoindolinium Salts
 (R =tBu, 2,6-Xylyl)
;
_journal_issue                   17
_journal_name_full               Organometallics
_journal_page_first              3587
_journal_paper_doi               10.1021/om020365n
_journal_volume                  21
_journal_year                    2002
_chemical_formula_sum            'C17 H17 F3 N2 O3 S'
_chemical_formula_weight         386.39
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 100.052(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.5482(12)
_cell_length_b                   11.9641(14)
_cell_length_c                   13.9946(16)
_cell_measurement_reflns_used    3926
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      28
_cell_measurement_theta_min      2
_cell_volume                     1739.0(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Siemens XP'
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      143(2)
_diffrn_detector_area_resol_mean 8.192
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker SMART 1000 CCD'
_diffrn_measurement_method       \w-scan
_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  0.0567
_diffrn_reflns_av_sigmaI/netI    0.0663
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            14177
_diffrn_reflns_theta_full        30.00
_diffrn_reflns_theta_max         30.03
_diffrn_reflns_theta_min         2.24
_exptl_absorpt_coefficient_mu    0.237
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.476
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       tablet
_exptl_crystal_F_000             800
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.362
_refine_diff_density_min         -0.396
_refine_diff_density_rms         0.059
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.927
_refine_ls_hydrogen_treatment    'NH free, methyls rigid, others riding''
_refine_ls_matrix_type           full
_refine_ls_number_parameters     245
_refine_ls_number_reflns         5073
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.927
_refine_ls_R_factor_all          0.0705
_refine_ls_R_factor_gt           0.0390
_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^)+(0.0476P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0883
_refine_ls_wR_factor_ref         0.0967
_reflns_number_gt                3284
_reflns_number_total             5073
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om020365n.cif
_cod_data_source_block           10.OTf
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4076975