Synthesis and reactivity studies of palladium(II) complexes containing the N-phosphorylated iminophosphorane-phosphine ligands Ph2PCH2P{=NP(=O)(OR)2}Ph2 (R=Et, Ph): application to the catalytic synthesis of 2,3-dimethylfuran.
Cadierno, Victorio; Díez, Josefina; García-Alvarez, Joaquín; Gimeno, José; Nebra, Noel; Rubio-García, Javier; Dalton transactions (Cambridge, England : 2003)  (2006) 5593–5604; doi:10.1039/b609359k

data_7007700
_publ_section_title
;
 Synthesis and reactivity studies of palladium(II) complexes containing
 the N-phosphorylated iminophosphorane-phosphine ligands
 Ph2PCH2P{=NP(=O)(OR)2}Ph2 (R=Et, Ph): application to the catalytic
 synthesis of 2,3-dimethylfuran.
;
_journal_issue                   47
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              5593
_journal_page_last               5604
_journal_paper_doi               10.1039/b609359k
_journal_year                    2006
_chemical_formula_moiety         'C58 H64 N2 O6 P6 Pd, 2(F6 Sb), 2(C H2 Cl2)'
_chemical_formula_sum            'C60 H68 Cl4 F12 N2 O6 P6 Pd Sb2'
_chemical_formula_weight         1818.68
_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                82.941(2)
_cell_angle_beta                 86.073(2)
_cell_angle_gamma                75.890(2)
_cell_formula_units_Z            2
_cell_length_a                   12.5698(4)
_cell_length_b                   13.6979(4)
_cell_length_c                   21.3980(7)
_cell_measurement_reflns_used    13845
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      69.996
_cell_measurement_theta_min      3.34
_cell_volume                     3543.22(19)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'PLATON (Spek, 2005)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'DIRDIF-99 (Beurskens, 1999)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.861
_diffrn_measured_fraction_theta_max 0.861
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.0426
_diffrn_reflns_av_sigmaI/netI    0.0495
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            26848
_diffrn_reflns_theta_full        70.03
_diffrn_reflns_theta_max         70.03
_diffrn_reflns_theta_min         2.08
_exptl_absorpt_coefficient_mu    11.403
_exptl_absorpt_correction_T_max  0.0962
_exptl_absorpt_correction_T_min  0.0378
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
'XABS(Parkin S,Moezzi B & Hope H, 1995)'
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.705
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1808
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.06
_refine_diff_density_max         3.170
_refine_diff_density_min         -2.479
_refine_diff_density_rms         0.155
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     818
_refine_ls_number_reflns         11585
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0805
_refine_ls_R_factor_gt           0.0631
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1023P)^2^+16.5267P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1667
_refine_ls_wR_factor_ref         0.1800
_reflns_number_gt                9083
_reflns_number_total             11585
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b609359k.txt
_cod_data_source_block           9
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from
2010-06-29.

'_exptl_absorpt_correction_type' value 'Empirical' changed to
'empirical' according to
'/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7007700