Phosphido Pincer Complexes of Palladium as New Efficient Catalysts for Allylation of Aldehydes
Mazzeo, Mina; Lamberti, Marina; Massa, Antonio; Scettri, Arrigo; Pellecchia, Claudio; Peters, Jonas C.; Organometallics 27 (2008) 5741–; doi:10.1021/om8008537

data_4072406
_publ_contact_author             'Mina Mazzeo'
_publ_section_title
;
 Phosphido Pincer Complexes of Palladium as New Efficient Catalysts for
 Allylation of Aldehydes
;
_journal_issue                   22
_journal_name_full               Organometallics
_journal_page_first              5741
_journal_paper_doi               10.1021/om8008537
_journal_volume                  27
_journal_year                    2008
_chemical_formula_moiety         'C24 H36 Cl P3 Pd'
_chemical_formula_sum            'C24 H36 Cl P3 Pd'
_chemical_formula_weight         559.29
_chemical_name_systematic
'bis(2-di-iso-propylphosphinophenyl)phosphidepalladiumchloride   '
_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                 102.12(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.310(4)
_cell_length_b                   11.988(5)
_cell_length_c                   15.352(7)
_cell_measurement_reflns_used    8015
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      39.91
_cell_measurement_theta_min      2.19
_cell_volume                     2574.9(18)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.879
_diffrn_measured_fraction_theta_max 0.879
_diffrn_measurement_device_type  'CCD area detector'
_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  0.1122
_diffrn_reflns_av_sigmaI/netI    0.0917
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            48836
_diffrn_reflns_theta_full        40.75
_diffrn_reflns_theta_max         40.75
_diffrn_reflns_theta_min         1.77
_exptl_absorpt_coefficient_mu    1.020
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.443
_exptl_crystal_density_meas      0
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1152
_refine_diff_density_max         3.118
_refine_diff_density_min         -1.119
_refine_diff_density_rms         0.172
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.209
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     270
_refine_ls_number_reflns         14690
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.209
_refine_ls_R_factor_all          0.0895
_refine_ls_R_factor_gt           0.0469
_refine_ls_shift/su_max          0.038
_refine_ls_shift/su_mean         0.004
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0866
_refine_ls_wR_factor_ref         0.0961
_reflns_number_gt                9220
_reflns_number_total             14690
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om8008537_si_002.cif
_cod_data_source_block           mm03
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_cell_volume        2574.7(17)
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               4072406