Application of Chiral Amine-Imine Ligands in Palladium-Catalyzed Polyketone Synthesis: Effect of Ligand Backbone on the Polymer Stereochemistry
Axet, M. Rosa; Amoroso, Francesco; Bottari, Giovanni; D’Amora, Angela; Zangrando, Ennio; Faraone, Felice; Drommi, Dario; Saporita, Maria; Carfagna, Carla; Natanti, Paolo; Seraglia, Roberta; Milani, Barbara; Organometallics 28 (2009) 4464–; doi:10.1021/om900300w

data_4069611
_publ_section_title
;
 Application of Chiral Amine-Imine Ligands in Palladium-Catalyzed
 Polyketone Synthesis: Effect of Ligand Backbone on the Polymer
 Stereochemistry
;
_journal_issue                   15
_journal_name_full               Organometallics
_journal_page_first              4464
_journal_paper_doi               10.1021/om900300w
_journal_volume                  28
_journal_year                    2009
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C32 H25 Cl N2 Pd, C H Cl3'
_chemical_formula_sum            'C33 H26 Cl4 N2 Pd'
_chemical_formula_weight         698.76
_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                 110.62(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   8.250(3)
_cell_length_b                   20.859(4)
_cell_length_c                   9.051(3)
_cell_measurement_temperature    293(2)
_cell_volume                     1457.8(8)
_computing_cell_refinement       'Denzo (Otwinowski & Minor 1997)'
_computing_data_collection       'Nonius Xpress'
_computing_data_reduction
'Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_molecular_graphics    'Ortep3/windows (Farrugia,1997)'
_computing_publication_material  'Wingx 1.70.00 (Farrugia, 1999)'
_computing_structure_refinement  'SHELX97 (Sheldrick, 1998)'
_computing_structure_solution    'SHELX97 (Sheldrick, 1998)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.808
_diffrn_measured_fraction_theta_max 0.808
_diffrn_measurement_device_type  'image plate dip1030'
_diffrn_measurement_method       'laser scanner'
_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  0.0690
_diffrn_reflns_av_sigmaI/netI    0.2290
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            18537
_diffrn_reflns_theta_full        26.76
_diffrn_reflns_theta_max         26.76
_diffrn_reflns_theta_min         1.95
_exptl_absorpt_coefficient_mu    1.030
_exptl_absorpt_correction_T_max  0.8292
_exptl_absorpt_correction_T_min  0.6850
_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            yellow
_exptl_crystal_density_diffrn    1.592
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             704
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.452
_refine_diff_density_min         -0.739
_refine_diff_density_rms         0.084
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.10(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.822
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     361
_refine_ls_number_reflns         4159
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.822
_refine_ls_R_factor_all          0.1440
_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^)+(0.0567P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1353
_refine_ls_wR_factor_ref         0.1600
_reflns_number_gt                1943
_reflns_number_total             4159
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om900300w_si_003.cif
_cod_data_source_block           S2a
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               4069611