Tridentate Assembling Ligands Based on Oxazoline and Phosphorus Donors in Dinuclear Pd(I)-Pd(I) Complexes
Jing Zhang; Roberto Pattacini; Pierre Braunstein; Inorganic Chemistry 48 (2009) 11954–11962; doi:10.1021/ic9018579

data_4303898
_publ_contact_author_address
;Laboratoire de Chimie de Coordination
CNRS-Universit\'e de Strasbourg
Institut Le Bel - 4 rue Blaise Pascal
67070 Strasbourg Cedex - France
;
_publ_contact_author_email       braunst@chimie.u-strasbg.fr
_publ_contact_author_fax         +33(0)368851322
_publ_contact_author_name        'Dr. Pierre Braunstein'
_publ_contact_author_phone       +33(0)368851308
_publ_section_title
;
Tridentate Assembling Ligands Based on Oxazoline and Phosphorus Donors in
Dinuclear Pd(I)-Pd(I) Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              11954
_journal_page_last               11962
_journal_paper_doi               10.1021/ic9018579
_journal_volume                  48
_journal_year                    2009
_chemical_formula_moiety         'C22 H33 Cl N2 O4 P Pd, 0.5(C2 H3 N), B F4'
_chemical_formula_sum            'C23 H34.5 B Cl F4 N2.5 O4 P Pd'
_chemical_formula_weight         669.66
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_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                97.809(4)
_cell_angle_beta                 109.390(4)
_cell_angle_gamma                97.814(6)
_cell_formula_units_Z            4
_cell_length_a                   11.580(1)
_cell_length_b                   16.228(2)
_cell_length_c                   16.892(2)
_cell_measurement_reflns_used    19500
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      30.034
_cell_measurement_theta_min      0.998
_cell_volume                     2910.3(6)
_computing_cell_refinement       'Denzo (Nonius B.V., 1998)'
_computing_data_collection       'Collect (Nonius B.V., 1998)'
_computing_data_reduction        'Denzo (Nonius B.V., 1998)'
_computing_molecular_graphics    'ATOMS V6 (Dowty, 2001)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       CCD
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0389
_diffrn_reflns_av_sigmaI/netI    0.0409
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            34106
_diffrn_reflns_theta_full        27.00
_diffrn_reflns_theta_max         27.00
_diffrn_reflns_theta_min         1.29
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.842
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.528
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1364
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.244
_refine_diff_density_min         -0.961
_refine_diff_density_rms         0.154
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.140
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     723
_refine_ls_number_reflns         12691
_refine_ls_number_restraints     82
_refine_ls_restrained_S_all      1.146
_refine_ls_R_factor_all          0.0403
_refine_ls_R_factor_gt           0.0313
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0463P)^2^+1.6005P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0855
_refine_ls_wR_factor_ref         0.0967
_reflns_number_gt                10988
_reflns_number_total             12691
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic9018579_si_002.cif
_cod_data_source_block           compound3
_cod_database_code               4303898