Linear α-Olefins Obtained with Palladium(II) Complexes Bearing a Partially Oxidized Tetraphosphane
Oberhauser, Werner; Manca, Gabriele; Ienco, Andrea; Strabler, Christof; Prock, Johannes; Weninger, Alexander; Gutmann, Rene; Brüggeller, Peter; Organometallics 33 (2014) 4067–; doi:10.1021/om500573q

data_4084113
_publ_section_title
;
 Linear \a-Olefins Obtained with Palladium(II) Complexes Bearing a
 Partially Oxidized Tetraphosphane
;
_journal_issue                   15
_journal_name_full               Organometallics
_journal_page_first              4067
_journal_paper_doi               10.1021/om500573q
_journal_volume                  33
_journal_year                    2014
_chemical_formula_moiety         'C54 H50 Cl2 O2 P4 Pd2, 3.425(C2 H4 Cl2)'
_chemical_formula_sum            'C60.85 H58 Cl8.85 O2 P4 Pd2'
_chemical_formula_weight         1471.69
_chemical_name_systematic        '[Pd2Cl2(Me)2(1,3-trans-dppcbO2)]'
_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                108.414(1)
_cell_angle_beta                 105.187(1)
_cell_angle_gamma                91.546(1)
_cell_formula_units_Z            4
_cell_length_a                   15.5968(3)
_cell_length_b                   17.3262(5)
_cell_length_c                   26.5022(6)
_cell_measurement_reflns_used    73444
_cell_measurement_temperature    203(2)
_cell_measurement_theta_max      26.022
_cell_measurement_theta_min      0.998
_cell_volume                     6510.5(3)
_computing_cell_refinement       'Denzo and Scalepack'
_computing_data_collection       'Kappa CCD'
_computing_data_reduction        'Denzo and Scalepack'
_computing_molecular_graphics    'SHELXTL-NT V6.1'
_computing_publication_material  'SHELXTL-NT V6.1'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      203(2)
_diffrn_measured_fraction_theta_full 1.00
_diffrn_measurement_device_type  'Kappa CCD'
_diffrn_measurement_method       'phi- and omega-scans'
_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  0.0340
_diffrn_reflns_av_sigmaI/netI    0.0673
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            47620
_diffrn_reflns_theta_full        26.01
_diffrn_reflns_theta_max         26.01
_diffrn_reflns_theta_min         1.69
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  120
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.054
_exptl_absorpt_correction_T_max  0.910
_exptl_absorpt_correction_T_min  0.701
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Otwinowski et al, 1997'
_exptl_crystal_colour            'light brown'
_exptl_crystal_density_diffrn    1.502
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2966.2
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.090
_refine_diff_density_max         1.330
_refine_diff_density_min         -0.780
_refine_diff_density_rms         0.090
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1436
_refine_ls_number_reflns         25431
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0631
_refine_ls_R_factor_gt           0.0478
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0701P)^2^+4.5083P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1259
_refine_ls_wR_factor_ref         0.1626
_reflns_number_gt                18133
_reflns_number_total             25639
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om500573q_si_002.cif
_cod_data_source_block           1
_cod_depositor_comments
;
Adding full bibliography for 4084113--4084116.cif.

2026-05-15
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_weight         2943.38
_cod_original_formula_moiety
'2(C54 H50 Cl2 O2 P4 Pd2), 2.85(C2 Cl2), 4(C2 H4 Cl2)'
_cod_original_formula_units_Z            2
_cod_original_formula_sum        'C121.70 H116 Cl17.70 O4 P8 Pd4'
_cod_database_code               4084113
_diffrn_measured_fraction        0.997