A Cation-Captured Palladium(0) Anion: Synthesis, Structure, and Bonding of [PdBr(PPh3)2]−Ligated by an N-Heterocyclic Phosphenium Cation
Caputo, Christine A.; Brazeau, Allison L.; Hynes, Zachery; Price, Jacquelyn T.; Tuononen, Heikki M.; Jones, Nathan D.; Organometallics 28 (2009) 5261–; doi:10.1021/om9006278

data_4070143
_publ_section_title
;
 A Cation-Captured Palladium(0) Anion: Synthesis, Structure, and Bonding
 of [PdBr(PPh3)2]&#x2212;Ligated by an N-Heterocyclic Phosphenium Cation
;
_journal_issue                   17
_journal_name_full               Organometallics
_journal_page_first              5261
_journal_paper_doi               10.1021/om9006278
_journal_volume                  28
_journal_year                    2009
_chemical_formula_moiety         'C56 H54 N2 P3 Pd, C4 H4 O, C F3 O3 S'
_chemical_formula_sum            'C61 H62 F3 N2 O4 P3 Pd S'
_chemical_formula_weight         1175.50
_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                88.19(3)
_cell_angle_beta                 80.10(3)
_cell_angle_gamma                82.02(3)
_cell_formula_units_Z            2
_cell_length_a                   12.465(3)
_cell_length_b                   14.141(3)
_cell_length_c                   16.332(3)
_cell_measurement_reflns_used    16488
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      30.03
_cell_measurement_theta_min      2.04
_cell_volume                     2808.4(11)
_computing_cell_refinement       'Bruker SMART (Bruker, 1997)'
_computing_data_collection       'Bruker SMART (Bruker, 1997)'
_computing_data_reduction        'Bruker SMART (Bruker, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL (Bruker, 1997)'
_computing_publication_material  'Bruker SHELXTL (Bruker, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full .981
_diffrn_measured_fraction_theta_max .981
_diffrn_measurement_device_type
'Bruker PLATFORM diffractometer/SMART 1000 CCD area detector'
_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  0.0395
_diffrn_reflns_av_sigmaI/netI    0.0817
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            24701
_diffrn_reflns_theta_full        30.10
_diffrn_reflns_theta_max         30.10
_diffrn_reflns_theta_min         2.06
_exptl_absorpt_coefficient_mu    0.512
_exptl_absorpt_correction_T_max  0.9749
_exptl_absorpt_correction_T_min  0.8936
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.390
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1216
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.05
_refine_diff_density_max         .919
_refine_diff_density_min         -1.460
_refine_diff_density_rms         .113
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.100
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     580
_refine_ls_number_reflns         16211
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.100
_refine_ls_R_factor_all          0.0971
_refine_ls_R_factor_gt           0.0571
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0756P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1369
_refine_ls_wR_factor_ref         0.1569
_reflns_number_gt                10982
_reflns_number_total             16211
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om9006278_si_002.cif
_cod_data_source_block           3.THF
_cod_original_cell_volume        2808.5(10)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4070143