A Cationic AgI(PNPtBu) Species Acting as PNP Transfer Agent: Facile Synthesis of Pd(PNPtBu)(alkyl) Complexes and Their Reactivity Compared to PCPtBuAnalogues
van der Vlugt, Jarl Ivar; Siegler, Maxime A.; Janssen, Michèle; Vogt, Dieter; Spek, Anthony L.; Organometallics 28 (2009) 7025–; doi:10.1021/om900862w

data_4070490
_publ_section_title
;
 A Cationic AgI(PNPtBu) Species Acting as PNP Transfer Agent: Facile
 Synthesis of Pd(PNPtBu)(alkyl) Complexes and Their Reactivity Compared to
 PCPtBuAnalogues
;
_journal_issue                   24
_journal_name_full               Organometallics
_journal_page_first              7025
_journal_paper_doi               10.1021/om900862w
_journal_volume                  28
_journal_year                    2009
_chemical_formula_moiety         'C46 H86 Au2 N2 P4, 2(B F4)'
_chemical_formula_sum            'C46 H86 Au2 B2 F8 N2 P4'
_chemical_formula_weight         1358.60
_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   difmap
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 112.254(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   13.7230(4)
_cell_length_b                   14.4624(6)
_cell_length_c                   14.6730(4)
_cell_measurement_reflns_used    18348
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.50
_cell_measurement_theta_min      1.60
_cell_volume                     2695.20(16)
_computing_cell_refinement       'PEAKREF (Schreurs, 2005)'
_computing_data_collection       'COLLECT (Nonius, 1999)'
_computing_data_reduction        'EVALCCD (Duisenberg et al., 2003)'
_computing_molecular_graphics    'PLATON (Spek, 2003)'
_computing_publication_material  'PLATON (Spek, 2003)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'DIRDIF08 (Beurskens et al., 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Nonius KappaCCD diffractometer'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0356
_diffrn_reflns_av_sigmaI/netI    0.0251
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            39614
_diffrn_reflns_theta_full        26.50
_diffrn_reflns_theta_max         26.50
_diffrn_reflns_theta_min         1.60
_exptl_absorpt_coefficient_mu    5.616
_exptl_absorpt_correction_T_max  0.680
_exptl_absorpt_correction_T_min  0.333
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2006)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.674
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1352
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.867
_refine_diff_density_min         -0.552
_refine_diff_density_rms         0.098
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     301
_refine_ls_number_reflns         5573
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0334
_refine_ls_R_factor_gt           0.0210
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0115P)^2^+3.9898P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0373
_refine_ls_wR_factor_ref         0.0402
_reflns_number_gt                4669
_reflns_number_total             5573
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            om900862w_si_002.cif
_cod_data_source_block           Comp-2
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4070490