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_4324867
_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 H50 Cl2 N2 O2 P4 Pt, 2.5(C H2 Cl2)'
_chemical_formula_sum            'C58.5 H55 Cl7 N2 O2 P4 Pt'
_chemical_formula_weight         1385.16
_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                107.918(2)
_cell_angle_beta                 107.738(2)
_cell_angle_gamma                90.299(3)
_cell_formula_units_Z            4
_cell_length_a                   17.0905(5)
_cell_length_b                   18.0349(8)
_cell_length_c                   24.3921(10)
_cell_measurement_reflns_used    14986
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      26.373
_cell_measurement_theta_min      0.998
_cell_volume                     6772.8(5)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Bruker AXS BV, 1997-2004)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_molecular_graphics    ORTEP
_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 0.989
_diffrn_measured_fraction_theta_max 0.989
_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  0.0364
_diffrn_reflns_av_sigmaI/netI    0.1247
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            38965
_diffrn_reflns_theta_full        26.36
_diffrn_reflns_theta_max         26.36
_diffrn_reflns_theta_min         1.19
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    2.480
_exptl_absorpt_correction_T_max  0.777
_exptl_absorpt_correction_T_min  0.681
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'L. Spek, J. Appl.Cryst. 2003, 36, 7, B. Blessing, Acta Cryst, 1995, A51, 33'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.358
_exptl_crystal_description       prism
_exptl_crystal_F_000             2772
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_platon_squeeze_details
;
;
_refine_diff_density_max         1.591
_refine_diff_density_min         -1.472
_refine_diff_density_rms         0.160
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.952
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1342
_refine_ls_number_reflns         27358
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.952
_refine_ls_R_factor_all          0.1238
_refine_ls_R_factor_gt           0.0656
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1043P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1677
_refine_ls_wR_factor_ref         0.1859
_reflns_number_gt                15000
_reflns_number_total             27358
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic1024422_si_003_3.cif
_cod_data_source_block           compound6
_cod_original_formula_sum        'C58.50 H55 Cl7 N2 O2 P4 Pt'
_cod_database_code               4324867