Palladium and Platinum Complexes of a Benzannulated N-Heterocyclic Plumbylene with an Unusual Bonding Mode
Dennis Heitmann; Tania Pape; Alexander Hepp; Christian Mück-Lichtenfeld; Stefan Grimme; F. Ekkehardt Hahn; Journal of the American Chemical Society 133 (2011) 11118–11120; doi:10.1021/ja204955f

data_4106465
_publ_section_title
;
 Palladium and Platinum Complexes of a Benzannulated N-Heterocyclic
 Plumbylene with an Unusual Bonding Mode
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              11118
_journal_page_last               11120
_journal_paper_doi               10.1021/ja204955f
_journal_volume                  133
_journal_year                    2011
_chemical_formula_sum            'C82 H83 N2 P3 Pb Pd'
_chemical_formula_weight         1503.00
_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                79.2470(10)
_cell_angle_beta                 81.7380(10)
_cell_angle_gamma                84.0190(10)
_cell_formula_units_Z            2
_cell_length_a                   13.4081(5)
_cell_length_b                   13.6329(6)
_cell_length_c                   19.9252(8)
_cell_measurement_reflns_used    900
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      22.5
_cell_measurement_theta_min      1
_cell_volume                     3529.8(2)
_computing_cell_refinement       'APEX2(Bruker AXS, 2007)'
_computing_data_collection       'APEX2(Bruker AXS, 2007)'
_computing_data_reduction        'SAINT,SADABS (Bruker AXS, 2007 )'
_computing_molecular_graphics
;
ORTEP3,L.J. Farrugia, J. Appl. Cryst. (1997) 30, 565
;
_computing_structure_refinement
;
SHELXL-97, G. M. Sheldrick, Acta Cryst. (2008) A64, 112-122
;
_computing_structure_solution
;
SHELXS-97 , G. M. Sheldrick, Acta Cryst. (2008) A64, 112-122
;
_diffrn_ambient_temperature      153(2)
_diffrn_detector_area_resol_mean 80
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'Omega and Phi scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0211
_diffrn_reflns_av_sigmaI/netI    0.0345
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            41843
_diffrn_reflns_theta_full        30.00
_diffrn_reflns_theta_max         30.00
_diffrn_reflns_theta_min         1.05
_exptl_absorpt_coefficient_mu    2.749
_exptl_absorpt_correction_T_max  0.8748
_exptl_absorpt_correction_T_min  0.6832
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
 Corrections were done with the SADABS program, utilizing the none merged
 raw data obtained from the integration process. Integration and final cell
 refinement were done with SAINT.

 SADABS reports ratio of Tmin/Tmax = 0.785111  

;
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.414
_exptl_crystal_description       'transparent prism'
_exptl_crystal_F_000             1524
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.05
_refine_diff_density_max         2.226
_refine_diff_density_min         -3.815
_refine_diff_density_rms         0.129
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.919
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     728
_refine_ls_number_reflns         20410
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      0.919
_refine_ls_R_factor_all          0.0501
_refine_ls_R_factor_gt           0.0392
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0816P)^2^+4.3273P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1059
_refine_ls_wR_factor_ref         0.1154
_reflns_number_gt                17152
_reflns_number_total             20410
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja204955f_si_002.cif
_cod_data_source_block           sad
_cod_database_code               4106465