Diffusion and Overhauser NMR Studies on Dicationic Palladium Complexes of BINAP
Nama, Devendrababu; Schott, Daniele; Pregosin, Paul S.; Veiros, L. F.; Calhorda, M. J.; Organometallics 25 (2006) 4596–; doi:10.1021/om0603518

data_4075538
_publ_section_title
;
 Diffusion and Overhauser NMR Studies on Dicationic Palladium Complexes of
 BINAP
;
_journal_issue                   19
_journal_name_full               Organometallics
_journal_page_first              4596
_journal_paper_doi               10.1021/om0603518
_journal_volume                  25
_journal_year                    2006
_chemical_formula_moiety         'C95H73NOP4Pd2, 2(C4H8O), 2(CF3O3S)'
_chemical_formula_sum            'C105 H89 F6 N O9 P4 Pd2 S2'
_chemical_formula_weight         2023.57
_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
_cell_angle_alpha                80.1980(10)
_cell_angle_beta                 83.5970(10)
_cell_angle_gamma                75.7990(10)
_cell_formula_units_Z            2
_cell_length_a                   12.6336(9)
_cell_length_b                   13.1083(9)
_cell_length_c                   30.389(2)
_cell_measurement_temperature    200(2)
_cell_volume                     4794.7(6)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Ortep32 for Windows'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'Bruker Apex with CCD'
_diffrn_measurement_method       'phi and omega 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  0.0426
_diffrn_reflns_av_sigmaI/netI    0.0721
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            49678
_diffrn_reflns_theta_full        28.36
_diffrn_reflns_theta_max         28.36
_diffrn_reflns_theta_min         1.85
_exptl_absorpt_coefficient_mu    0.555
_exptl_absorpt_correction_T_max  0.9067
_exptl_absorpt_correction_T_min  0.7574
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'Blessing, 1995'
_exptl_crystal_colour            orange-red
_exptl_crystal_density_diffrn    1.402
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'irregular shaped crystal'
_exptl_crystal_F_000             2072
_exptl_crystal_size_max          0.53
_exptl_crystal_size_mid          0.33
_exptl_crystal_size_min          0.18
_refine_diff_density_max         2.623
_refine_diff_density_min         -0.835
_refine_diff_density_rms         0.156
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1236
_refine_ls_number_reflns         23674
_refine_ls_number_restraints     224
_refine_ls_restrained_S_all      1.077
_refine_ls_R_factor_all          0.1065
_refine_ls_R_factor_gt           0.0763
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1243P)^2^+8.4496P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2088
_refine_ls_wR_factor_ref         0.2294
_reflns_number_gt                16677
_reflns_number_total             23674
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om0603518si20060420_114113.cif
_cod_data_source_block           binap_Pd
_cod_original_sg_symbol_Hall     -P1
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4075538