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_4084114
_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, C H2 Cl2, 0.8(O)'
_chemical_formula_sum            'C55 H52 Cl4 O2.8 P4 Pd2'
_chemical_formula_weight         1236.25
_chemical_name_systematic        '[Pd2Cl2(Me)2(2,3-trans-dppcbO2)]'
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 109.0463(9)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   14.3998(6)
_cell_length_b                   43.289(2)
_cell_length_c                   18.0032(7)
_cell_measurement_reflns_used    62544
_cell_measurement_temperature    243(2)
_cell_measurement_theta_max      26.022
_cell_measurement_theta_min      0.998
_cell_volume                     10608.0(8)
_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      243(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  0.0433
_diffrn_reflns_av_sigmaI/netI    0.0840
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       52
_diffrn_reflns_limit_k_min       -53
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            29045
_diffrn_reflns_theta_full        26.07
_diffrn_reflns_theta_max         26.07
_diffrn_reflns_theta_min         1.52
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  120
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.043
_exptl_absorpt_correction_T_max  0.885
_exptl_absorpt_correction_T_min  0.725
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Otwinowski et al, 1997'
_exptl_crystal_colour            'light brown'
_exptl_crystal_density_diffrn    1.548
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             4995.2
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.070
_refine_diff_density_min         -0.780
_refine_diff_density_rms         0.080
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.979
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1229
_refine_ls_number_reflns         18513
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0671
_refine_ls_R_factor_gt           0.0490
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0959P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1361
_refine_ls_wR_factor_ref         0.1812
_reflns_number_gt                11037
_reflns_number_total             21028
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om500573q_si_002.cif
_cod_data_source_block           3
_cod_depositor_comments
'Adding full bibliography for 4084113--4084116.cif.'
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_original_formula_sum        'C55 H52 Cl4 O2.80 P4 Pd2'
_cod_database_code               4084114
_diffrn_measured_fraction        0.998