Addressing the Poly- to Oligo-ketone Selectivity in Styrene Carbonylation Catalyzed by Palladium/bpy Complexes. Effect of the 6-Alkyl Substitution
D’Amora, Angela; Fanfoni, Lidia; Cozzula, Daniela; Guidolin, Nicol; Zangrando, Ennio; Felluga, Fulvia; Gladiali, Serafino; Benedetti, Fabio; Milani, Barbara; Organometallics 29 (2010) 4472–; doi:10.1021/om100585x

data_4066709
_publ_section_title
;
 Addressing the Poly- to Oligo-ketone Selectivity in Styrene Carbonylation
 Catalyzed by Palladium/bpy Complexes. Effect of the 6-Alkyl Substitution
;
_journal_issue                   20
_journal_name_full               Organometallics
_journal_page_first              4472
_journal_paper_doi               10.1021/om100585x
_journal_volume                  29
_journal_year                    2010
_chemical_formula_moiety         'C28 H30 Cl N4 Pd2 1+, P F6 1-'
_chemical_formula_sum            'C28 H30 Cl F6 N4 P Pd2'
_chemical_formula_weight         815.78
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-I 2ya'
_symmetry_space_group_name_H-M   'I 1 2/a 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                 93.66(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.868(3)
_cell_length_b                   16.494(4)
_cell_length_c                   16.664(4)
_cell_measurement_temperature    100(2)
_cell_volume                     2981.0(13)
_computing_cell_refinement       'Denzo (Otwinowski & Minor 1997)'
_computing_data_reduction
'Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_molecular_graphics    'Ortep3/windows (Farrugia,1997)'
_computing_publication_material  'Wingx 1.80.05 (Farrugia, 1999)'
_computing_structure_refinement  'SHELX97 (Sheldrick, 1998)'
_computing_structure_solution    'SHELX97 (Sheldrick, 1998)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.943
_diffrn_measured_fraction_theta_max 0.943
_diffrn_measurement_device_type  'CCD MarResearch'
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_radiation_monochromator  Si111
_diffrn_radiation_source         'Elettra Synchrotron, Trieste (Italy)'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     1.00000
_diffrn_reflns_av_R_equivalents  0.0650
_diffrn_reflns_av_sigmaI/netI    0.0689
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            7242
_diffrn_reflns_theta_full        26.61
_diffrn_reflns_theta_max         26.61
_diffrn_reflns_theta_min         2.45
_exptl_absorpt_coefficient_mu    3.381
_exptl_absorpt_correction_T_max  0.9475
_exptl_absorpt_correction_T_min  0.8163
_exptl_absorpt_correction_type   refdelf
_exptl_absorpt_process_details
;
Parkin S,Moezzi B & Hope H, (1995) J. Appl. Cryst. 28, 53-56
Linear fit to sin(theta)/lambda - 12 parameters
;
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.818
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1616
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.635
_refine_diff_density_min         -0.403
_refine_diff_density_rms         0.096
_refine_ls_extinction_coef       0.0005(5)
_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   1.098
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     193
_refine_ls_number_reflns         1061
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.098
_refine_ls_R_factor_all          0.0681
_refine_ls_R_factor_gt           0.0621
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1134P)^2^+6.1100P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1652
_refine_ls_wR_factor_ref         0.1717
_reflns_number_gt                885
_reflns_number_total             1061
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            om100585x_si_003.cif
_cod_data_source_block           3a'
_cod_original_sg_symbol_H-M      'I 2/a'
_cod_database_code               4066709