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_4112518
_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            'C71 H60 F12 Fe N O P Pd'
_chemical_formula_weight         1364.42
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 103.70(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.979(3)
_cell_length_b                   17.638(4)
_cell_length_c                   24.486(5)
_cell_measurement_temperature    173(2)
_cell_volume                     6285(2)
_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 0.993
_diffrn_measured_fraction_theta_max 0.993
_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  0.0710
_diffrn_reflns_av_sigmaI/netI    0.1168
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            27821
_diffrn_reflns_theta_full        28.26
_diffrn_reflns_theta_max         28.26
_diffrn_reflns_theta_min         2.26
_exptl_absorpt_coefficient_mu    0.623
_exptl_absorpt_correction_T_max  0.9404
_exptl_absorpt_correction_T_min  0.8856
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.442
_exptl_crystal_description       plate
_exptl_crystal_F_000             2784
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.619
_refine_diff_density_min         -0.660
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.004
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     849
_refine_ls_number_reflns         15448
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.004
_refine_ls_R_factor_all          0.1332
_refine_ls_R_factor_gt           0.0536
_refine_ls_shift/su_max          0.337
_refine_ls_shift/su_mean         0.016
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0500P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1004
_refine_ls_wR_factor_ref         0.1213
_reflns_number_gt                8467
_reflns_number_total             15448
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0315107si20031204_112343_3.cif
_cod_data_source_block           complex2c
_cod_database_code               4112518