The First Carbodiphosphorane Complex with Two Palladium Centers Attached to the CDP Carbon: Assembly of a Single-Stranded di-Pd Helicate by the PCP Pincer ligand C(dppm)2
Reitsamer, Christian; Schuh, Walter; Kopacka, Holger; Wurst, Klaus; Ellmerer, Ernst P.; Peringer, Paul; Organometallics 30 (2011) 4220–; doi:10.1021/om2002975

data_4064732
_publ_section_title
;
 The First Carbodiphosphorane Complex with Two Palladium Centers Attached
 to the CDP Carbon: Assembly of a Single-Stranded di-Pd Helicate by the
 PCP Pincer ligand C(dppm)2
;
_journal_issue                   15
_journal_name_full               Organometallics
_journal_page_first              4220
_journal_paper_doi               10.1021/om2002975
_journal_volume                  30
_journal_year                    2011
_chemical_formula_sum            'C53 H49 Cl9 P4 Pd2'
_chemical_formula_weight         1341.65
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 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                 104.255(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   12.9599(4)
_cell_length_b                   16.8199(5)
_cell_length_c                   13.9015(6)
_cell_measurement_reflns_used    29334
_cell_measurement_temperature    233(2)
_cell_measurement_theta_max      25.0
_cell_measurement_theta_min      1.0
_cell_volume                     2937.00(18)
_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  0.0400
_diffrn_reflns_av_sigmaI/netI    0.0563
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            15499
_diffrn_reflns_theta_full        24.00
_diffrn_reflns_theta_max         24.00
_diffrn_reflns_theta_min         1.93
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.165
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.517
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1344
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.933
_refine_diff_density_min         -0.497
_refine_diff_density_rms         0.101
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.01(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    'constr, refined at C2 (bond restraint)'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     615
_refine_ls_number_reflns         9011
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0691
_refine_ls_R_factor_gt           0.0555
_refine_ls_shift/su_max          0.033
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0804P)^2^+4.8015P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1382
_refine_ls_wR_factor_ref         0.1469
_reflns_number_gt                7773
_reflns_number_total             9011
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om2002975_si_001.cif
_cod_data_source_block           p186
_cod_original_sg_symbol_H-M      P21
_cod_database_code               4064732