Synthesis, Structure, and Reductive Elimination Chemistry of Three-Coordinate Arylpalladium Amido Complexes
Makoto Yamashita; John F. Hartwig; Journal of the American Chemical Society 126 (2004) 5344–5345; doi:10.1021/ja0315107

data_4112520
_publ_section_title
;
 Synthesis, Structure, and Reductive Elimination Chemistry of
 Three-Coordinate Arylpalladium Amido Complexes
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              5344
_journal_page_last               5345
_journal_paper_doi               10.1021/ja0315107
_journal_volume                  126
_journal_year                    2004
_chemical_formula_sum            'C67.5 H53 F12 Fe N O P2 Pd'
_chemical_formula_weight         1346.30
_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                73.57(3)
_cell_angle_beta                 71.97(3)
_cell_angle_gamma                81.58(3)
_cell_formula_units_Z            2
_cell_length_a                   13.525(3)
_cell_length_b                   15.326(3)
_cell_length_c                   15.580(3)
_cell_measurement_temperature    173(2)
_cell_volume                     2939.4(12)
_computing_cell_refinement       Denzo
_computing_data_collection       'Nonius Collect'
_computing_data_reduction        Denzo
_computing_molecular_graphics    XP
_computing_publication_material  XCIF
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Nonius KappaCCD'
_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  0.0396
_diffrn_reflns_av_sigmaI/netI    0.0697
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            20270
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         2.41
_exptl_absorpt_coefficient_mu    0.691
_exptl_absorpt_correction_T_max  0.8742
_exptl_absorpt_correction_T_min  0.8463
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.521
_exptl_crystal_description       block
_exptl_crystal_F_000             1366
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.023
_refine_diff_density_min         -0.671
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     782
_refine_ls_number_reflns         11466
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0781
_refine_ls_R_factor_gt           0.0485
_refine_ls_shift/su_max          0.131
_refine_ls_shift/su_mean         0.005
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0800P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1253
_refine_ls_wR_factor_ref         0.1388
_reflns_number_gt                8352
_reflns_number_total             11466
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0315107si20031204_112343_5.cif
_cod_data_source_block           complex4
_cod_original_cell_volume        2939.2(10)
_cod_original_formula_sum        'C67.50 H53 F12 Fe N O P2 Pd'
_cod_database_code               4112520