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_4076976
_publ_section_title
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 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            'C12 H16 Br F N2 Pd'
_chemical_formula_weight         393.58
_chemical_name_systematic
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 ? 
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_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                80.825(5)
_cell_angle_beta                 82.462(4)
_cell_angle_gamma                76.751(4)
_cell_formula_units_Z            2
_cell_length_a                   5.3580(3)
_cell_length_b                   10.0813(6)
_cell_length_c                   13.6049(8)
_cell_measurement_reflns_used    62
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      12.5
_cell_measurement_theta_min      5.4
_cell_volume                     702.73(7)
_computing_cell_refinement       'Siemens XSCANS'
_computing_data_collection       'Siemens XSCANS'
_computing_data_reduction        'Siemens XSCANS'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens 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 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Siemens P4'
_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  0.0088
_diffrn_reflns_av_sigmaI/netI    0.0138
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       1
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            2626
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.05
_diffrn_standards_decay_%        1.6
_diffrn_standards_interval_count 247
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    4.155
_exptl_absorpt_correction_T_max  0.914
_exptl_absorpt_correction_T_min  0.654
_exptl_absorpt_correction_type   Psi-scans
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.860
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             384
_exptl_crystal_size_max          0.44
_exptl_crystal_size_mid          0.44
_exptl_crystal_size_min          0.34
_refine_diff_density_max         0.415
_refine_diff_density_min         -0.608
_refine_diff_density_rms         0.066
_refine_ls_extinction_coef       0.0097(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    'H1, H2 free,rigid methyls, others riding''
_refine_ls_matrix_type           full
_refine_ls_number_parameters     166
_refine_ls_number_reflns         2473
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.0241
_refine_ls_R_factor_gt           0.0213
_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^)+(0.0218P)^2^+0.9315P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0488
_refine_ls_wR_factor_ref         0.0500
_reflns_number_gt                2309
_reflns_number_total             2473
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om020365n.cif
_cod_data_source_block           3d
_cod_depositor_comments
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The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
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_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4076976