Synthesis and characterization of palladium(II) complexes with new diphosphonium-diphosphine and diphosphine ligands. Production of low molecular weight alternating polyketones via catalytic CO/ethene copolymerisation.
Bianchini, Claudio; Brüggeller, Peter; Claver, Carmen; Czermak, Georg; Dumfort, Alexander; Meli, Andrea; Oberhauser, Werner; Garcia Suarez, Eduardo J.; Dalton transactions (Cambridge, England : 2003)  (2006) 2964–2973; doi:10.1039/b601154c

data_7007177
_publ_section_title
;
 Synthesis and characterization of palladium(II) complexes with new
 diphosphonium-diphosphine and diphosphine ligands. Production of low
 molecular weight alternating polyketones via catalytic CO/ethene
 copolymerisation.
;
_journal_issue                   24
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2964
_journal_page_last               2973
_journal_paper_doi               10.1039/b601154c
_journal_year                    2006
_chemical_formula_moiety         'C61 H62 Cl2 O8 P4 Pd, 2(C3 H6 O), 2(F6 P)'
_chemical_formula_sum            'C67 H74 Cl2 F12 O10 P6 Pd'
_chemical_formula_weight         1630.41
_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_date             2005-10-05T15:59:56-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 91.8346(9)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.3205(2)
_cell_length_b                   20.4675(3)
_cell_length_c                   24.5985(3)
_cell_measurement_temperature    243(2)
_cell_volume                     7206.24(17)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      243(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0451
_diffrn_reflns_av_unetI/netI     0.0522
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            46151
_diffrn_reflns_theta_full        25.42
_diffrn_reflns_theta_max         25.42
_diffrn_reflns_theta_min         1.29
_exptl_absorpt_coefficient_mu    0.552
_exptl_absorpt_correction_T_max  0.950
_exptl_absorpt_correction_T_min  0.910
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Otwinowski et al, 1997'
_exptl_crystal_density_diffrn    1.503
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3336
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.630
_refine_diff_density_min         -0.451
_refine_diff_density_rms         0.070
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     895
_refine_ls_number_reflns         13017
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.017
_refine_ls_R_factor_all          0.1017
_refine_ls_R_factor_gt           0.0477
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0967P)^2^+4.38P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1497
_refine_ls_wR_factor_ref         0.1685
_reflns_number_gt                6216
_reflns_number_total             13308
_reflns_threshold_expression     >3sigma(I)
_cod_data_source_file            b601154c.txt
_cod_data_source_block           papo
_cod_original_cell_volume        7206.25(17)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7007177