Synthesis and Structure of the First Heterodinuclear PCP−Pincer−CDP Complex with a Pd−Au d8−d10Pseudo-Closed-Shell Interaction
Reitsamer, Christian; Schuh, Walter; Kopacka, Holger; Wurst, Klaus; Peringer, Paul; Organometallics 28 (2009) 6617–; doi:10.1021/om900686r

data_4070256
_publ_section_title
;
 Synthesis and Structure of the First Heterodinuclear
 PCP&#x2212;Pincer&#x2212;CDP Complex with a Pd&#x2212;Au
 d8&#x2212;d10Pseudo-Closed-Shell Interaction
;
_journal_issue                   22
_journal_name_full               Organometallics
_journal_page_first              6617
_journal_paper_doi               10.1021/om900686r
_journal_volume                  28
_journal_year                    2009
_chemical_formula_sum            'C53 H52 Au Cl3 O2 P4 Pd'
_chemical_formula_weight         1254.54
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 90.620(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.6502(1)
_cell_length_b                   20.0992(3)
_cell_length_c                   20.2354(2)
_cell_measurement_reflns_used    73785
_cell_measurement_temperature    233(2)
_cell_measurement_theta_max      27.0
_cell_measurement_theta_min      1.0
_cell_volume                     5144.73(10)
_computing_data_collection       COLLECT
_computing_data_reduction        'DENZO and SCALEPACK'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      233(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Nonius KappaCCD'
_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  0.0373
_diffrn_reflns_av_sigmaI/netI    0.0290
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            36708
_diffrn_reflns_theta_full        27.00
_diffrn_reflns_theta_max         27.00
_diffrn_reflns_theta_min         1.90
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.517
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.620
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2488
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.861
_refine_diff_density_min         -0.621
_refine_diff_density_rms         0.085
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     604
_refine_ls_number_reflns         11206
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.0321
_refine_ls_R_factor_gt           0.0273
_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^)+(0.0213P)^2^+8.7405P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0644
_refine_ls_wR_factor_ref         0.0663
_reflns_number_gt                10209
_reflns_number_total             11206
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om900686r_si_001.cif
_cod_data_source_block           p200
_cod_original_sg_symbol_H-M      P21/n
_cod_database_code               4070256