Palladium Complexes of a Novel Family of P,N-Chelates, the 2-(2-Pyridyl)phospholes: Synthesis, Structural Characterization, and Catalytic Activity for Olefin/CO Copolymerization
Sauthier, Mathieu; Leca, François; Toupet, Loïc; Réau, Régis; Organometallics 21 (2002) 1591–; doi:10.1021/om011034y

data_4076751
_publ_section_title
;
 Palladium Complexes of a Novel Family of P,N-Chelates, the
 2-(2-Pyridyl)phospholes: Synthesis, Structural Characterization, and
 Catalytic Activity for Olefin/CO Copolymerization
;
_journal_issue                   8
_journal_name_full               Organometallics
_journal_page_first              1591
_journal_paper_doi               10.1021/om011034y
_journal_volume                  21
_journal_year                    2002
_chemical_formula_sum            'C46 H20 Cl2 F12 N2 P2 Pd S2 Sb2'
_chemical_formula_weight         1375.50
_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                108.886(2)
_cell_angle_beta                 108.480(3)
_cell_angle_gamma                90.104(3)
_cell_formula_units_Z            2
_cell_length_a                   13.655(10)
_cell_length_b                   14.991(2)
_cell_length_c                   16.835(2)
_cell_measurement_temperature    293(2)
_cell_volume                     3071(2)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.967
_diffrn_measured_fraction_theta_max 0.967
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0213
_diffrn_reflns_av_sigmaI/netI    0.0582
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            13496
_diffrn_reflns_theta_full        26.97
_diffrn_reflns_theta_max         26.97
_diffrn_reflns_theta_min         1.36
_exptl_absorpt_coefficient_mu    1.435
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.487
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1324
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.33
_exptl_crystal_size_min          0.33
_refine_diff_density_max         1.570
_refine_diff_density_min         -0.971
_refine_diff_density_rms         0.137
_refine_ls_extinction_coef       0.0000(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.964
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     645
_refine_ls_number_reflns         12920
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.964
_refine_ls_R_factor_all          0.1363
_refine_ls_R_factor_gt           0.0735
_refine_ls_shift/su_max          1.925
_refine_ls_shift/su_mean         0.040
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1741P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2112
_refine_ls_wR_factor_ref         0.2535
_reflns_number_gt                7587
_reflns_number_total             12920
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om011034y.cif
_cod_data_source_block           ms
_cod_depositor_comments
;
The following automatic conversions were performed:
'_atom_site_symetry_multiplicity' tag replaced with
'_atom_site_symmetry_multiplicity'.

Automatic conversion script
Id: cif_correct_tags 1440 2010-10-19 06:21:57Z saulius 

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.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4076751