Unexpected Metal-Induced Isomerisms and Phosphoryl Migrations in Pt(II) and Pd(II) Complexes of the Functional Phosphine 2-(Bis(diphenylphosphino)methyl)-oxazoline
Shuanming Zhang; Roberto Pattacini; Pierre Braunstein; Inorganic Chemistry 50 (2011) 3511–3522; doi:10.1021/ic1024422

data_4324865
_publ_contact_author_address
;Laboratoire de Chimie de Coordination
UMR 7177 CNRS
Universit\'e de Strasbourg
Institut Le Bel - 4 rue Blaise Pascal, 
CS 90032, F-67081 STRASBOURG cedex
France
;
_publ_contact_author_email       braunst@chimie.u-strasbg.fr
_publ_contact_author_fax         '+33 (0)3 68 85 13 22'
_publ_contact_author_name        'Dr. Pierre Braunstein'
_publ_contact_author_phone       '+33 (0)3 68 85 13 08'
_publ_section_title
;
 Unexpected Metal-Induced Isomerisms and Phosphoryl Migrations in Pt(II)
 and Pd(II) Complexes of the Functional Phosphine
 2-(Bis(diphenylphosphino)methyl)-oxazoline
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3511
_journal_page_last               3522
_journal_paper_doi               10.1021/ic1024422
_journal_volume                  50
_journal_year                    2011
_chemical_formula_moiety         'C56 H48 N2 O2 P4 Pd, 4(C H2 Cl2)'
_chemical_formula_sum            'C60 H56 Cl8 N2 O2 P4 Pd'
_chemical_formula_weight         1350.95
_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                75.682(2)
_cell_angle_beta                 73.222(2)
_cell_angle_gamma                74.038(2)
_cell_formula_units_Z            1
_cell_length_a                   9.8705(5)
_cell_length_b                   12.5788(5)
_cell_length_c                   13.3436(6)
_cell_measurement_reflns_used    4852
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.32
_cell_measurement_theta_min      0.998
_cell_volume                     1499.46(12)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_molecular_graphics    ORTEP-3
_computing_publication_material  PLATON
_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 0.994
_diffrn_measured_fraction_theta_max 0.994
_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     0.71073
_diffrn_reflns_av_R_equivalents  0.0693
_diffrn_reflns_av_sigmaI/netI    0.0727
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            15842
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.62
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.817
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.496
_exptl_crystal_description       prism
_exptl_crystal_F_000             688
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.601
_refine_diff_density_min         -0.934
_refine_diff_density_rms         0.090
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     349
_refine_ls_number_reflns         6862
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0712
_refine_ls_R_factor_gt           0.0474
_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^)+(0.0409P)^2^+0.9573P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1014
_refine_ls_wR_factor_ref         0.1107
_reflns_number_gt                5287
_reflns_number_total             6862
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic1024422_si_003_1.cif
_cod_data_source_block           compound3b
_cod_database_code               4324865