Palladium complexes derived from N,N-bidentate NH-iminophosphorane ligands: synthesis and use as catalysts in the Sonogashira reaction.
Alajarin, Mateo; Lopez-Leonardo, Carmen; Llamas-Lorente, Pilar; Raja, Rosalia; Bautista, Delia; Orenes, Raul-Angel; Dalton transactions (Cambridge, England : 2003) 41 (2012) 12259–12269; doi:10.1039/c2dt31290e

data_7030182
_publ_section_title
;
 Palladium complexes derived from N,N-bidentate NH-iminophosphorane
 ligands: synthesis and use as catalysts in the Sonogashira reaction.
;
_journal_issue                   39
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              12259
_journal_page_last               12269
_journal_paper_doi               10.1039/c2dt31290e
_journal_volume                  41
_journal_year                    2012
_chemical_formula_sum            'C32 H35 Cl8 N2 P Pd'
_chemical_formula_weight         868.59
_chemical_name_systematic
;
?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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                 92.837(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.0275(6)
_cell_length_b                   14.4426(16)
_cell_length_c                   25.536(2)
_cell_measurement_reflns_used    99
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      12.44
_cell_measurement_theta_min      5.48
_cell_volume                     3693.7(5)
_computing_cell_refinement       'Siemens XSCANS'
_computing_data_collection       'Siemens XSCANS'
_computing_data_reduction        'Siemens XSCANS'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Siemens P4'
_diffrn_measurement_method       \w-scan
_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  0.0347
_diffrn_reflns_av_sigmaI/netI    0.0517
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       1
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            6676
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.00
_diffrn_standards_decay_%        1.2
_diffrn_standards_interval_count 247
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.150
_exptl_absorpt_correction_T_max  0.83033
_exptl_absorpt_correction_T_min  0.70268
_exptl_absorpt_correction_type   Psi-scans
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.562
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       lath
_exptl_crystal_F_000             1752
_exptl_crystal_size_max          0.44
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.529
_refine_diff_density_min         -0.526
_refine_diff_density_rms         0.088
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.937
_refine_ls_hydrogen_treatment    'NH free, others riding'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     403
_refine_ls_number_reflns         6467
_refine_ls_number_restraints     38
_refine_ls_restrained_S_all      0.934
_refine_ls_R_factor_all          0.0562
_refine_ls_R_factor_gt           0.0362
_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^)+(0.0485P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0824
_refine_ls_wR_factor_ref         0.0881
_reflns_number_gt                4809
_reflns_number_total             6467
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2dt31290e.txt
_cod_data_source_block           plame_compound_u,l-12
_cod_original_cell_volume        3693.7(6)
_cod_original_sg_symbol_H-M      'P 2(1)/c'
_cod_database_code               7030182