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_4070144
_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 Br N2 P3 Pd, 0.35(C8 H16 O2)'
_chemical_formula_sum            'C58.8 H59.6 Br N2 O0.7 P3 Pd'
_chemical_formula_weight         1084.70
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 129.64(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   34.230(7)
_cell_length_b                   17.143(3)
_cell_length_c                   24.015(5)
_cell_measurement_reflns_used    13703
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      25.03
_cell_measurement_theta_min      2.04
_cell_volume                     10852(6)
_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 .997
_diffrn_measured_fraction_theta_max .997
_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  0.0736
_diffrn_reflns_av_sigmaI/netI    0.1039
_diffrn_reflns_limit_h_max       40
_diffrn_reflns_limit_h_min       -40
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            18051
_diffrn_reflns_theta_full        25.07
_diffrn_reflns_theta_max         25.07
_diffrn_reflns_theta_min         2.08
_exptl_absorpt_coefficient_mu    1.206
_exptl_absorpt_correction_T_max  0.9567
_exptl_absorpt_correction_T_min  0.8398
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.328
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             4464
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.04
_refine_diff_density_max         .841
_refine_diff_density_min         -.879
_refine_diff_density_rms         .102
_refine_ls_extinction_coef       0.00051(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     496
_refine_ls_number_reflns         9606
_refine_ls_number_restraints     20
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.1380
_refine_ls_R_factor_gt           0.0645
_refine_ls_shift/su_max          0.080
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1036P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1634
_refine_ls_wR_factor_ref         0.2020
_reflns_number_gt                5169
_reflns_number_total             9606
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om9006278_si_003.cif
_cod_data_source_block           4.THF
_cod_original_cell_volume        10853(4)
_cod_original_sg_symbol_H-M      C2/c
_cod_original_formula_sum        'C58.80 H59.60 Br N2 O.70 P3 Pd'
_cod_database_code               4070144