Synthetic, Structural, and Mechanistic Aspects of an Amine Activation Process Mediated at a Zwitterionic Pd(II) Center
Connie C. Lu; Jonas C. Peters; Journal of the American Chemical Society 126 (2004) 15818–15832; doi:10.1021/ja046415s

data_4113244
_publ_section_title
;
 Synthetic, Structural, and Mechanistic Aspects of an Amine Activation
 Process Mediated at a Zwitterionic Pd(II) Center
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              15818
_journal_page_last               15832
_journal_paper_doi               10.1021/ja046415s
_journal_volume                  126
_journal_year                    2004
_chemical_formula_sum            'C52 H60 B N P2 Pd'
_chemical_formula_weight         878.16
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_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                 107.570(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.9776(11)
_cell_length_b                   19.4418(16)
_cell_length_c                   18.1205(15)
_cell_measurement_reflns_used    6911
_cell_measurement_temperature    98
_cell_measurement_theta_max      28.67
_cell_measurement_theta_min      2.40
_cell_volume                     4358.7(6)
_computing_cell_refinement       'Bruker SMART v5.606, Bruker SAINT v6.29'
_computing_data_collection       'Bruker SMART v5.054'
_computing_data_reduction        'Bruker SAINT v6.29'
_computing_molecular_graphics    'Diamond, Bruker SHELXTL v6.12'
_computing_publication_material  'Bruker SHELXTL v6.12'
_computing_structure_refinement  'SHELX-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELX-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      98
_diffrn_measured_fraction_theta_full 0.941
_diffrn_measured_fraction_theta_max 0.941
_diffrn_measurement_device_type  'Bruker SMART 1000 ccd'
_diffrn_measurement_method       '\w scans at 7 fixed \f values'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0721
_diffrn_reflns_av_sigmaI/netI    0.0550
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            77250
_diffrn_reflns_theta_full        28.50
_diffrn_reflns_theta_max         28.50
_diffrn_reflns_theta_min         1.58
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  'first 75 scans recollected at end of runs'
_exptl_absorpt_coefficient_mu    0.536
_exptl_absorpt_correction_T_max  0.9604
_exptl_absorpt_correction_T_min  0.9191
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   XPREP
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.338
_exptl_crystal_description       tabular
_exptl_crystal_F_000             1840
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.10
_refine_diff_density_max         4.140
_refine_diff_density_min         -1.681
_refine_diff_density_rms         0.105
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.745
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     515
_refine_ls_number_reflns         10404
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.745
_refine_ls_R_factor_all          0.0777
_refine_ls_R_factor_gt           0.0497
_refine_ls_shift/su_max          0.027
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.02P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0953
_refine_ls_wR_factor_ref         0.0987
_reflns_number_gt                7523
_reflns_number_total             10404
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja046415ssi20040707_052035_3.cif
_cod_data_source_block           complex8
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4113244