Formation of P-C Bonds under Unexpectedly Mild Conditions. Phosphoryl Migration and Metal Coordination of Diphenylphosphinomethyl-oxazolines and -thiazolines
Roberto Pattacini; Günter Margraf; Abdelatif Messaoudi; Nicola Oberbeckmann-Winter; Pierre Braunstein; Inorganic Chemistry 47 (2008) 9886–9897; doi:10.1021/ic800934h

data_4306000
_publ_contact_author_address
;Laboratoire de Chimie de Coordination
CNRS-Universit\'e Louis Pasteur
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)390241322
_publ_contact_author_name        'Dr. Pierre Braunstein'
_publ_contact_author_phone       +33(0)390241308
_publ_section_title
;
Formation of P-C Bonds under Unexpectedly Mild Conditions. Phosphoryl
Migration and Metal Coordination of Diphenylphosphinomethyl-oxazolines and
-thiazolines
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              9886
_journal_page_last               9897
_journal_paper_doi               10.1021/ic800934h
_journal_volume                  47
_journal_year                    2008
_chemical_formula_moiety         'C28 H25 N O1.32 P2'
_chemical_formula_sum            'C28 H25 N O1.32 P2'
_chemical_formula_weight         458.55
_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                80.151(6)
_cell_angle_beta                 76.242(7)
_cell_angle_gamma                77.920(5)
_cell_formula_units_Z            2
_cell_length_a                   8.7124(10)
_cell_length_b                   11.4999(13)
_cell_length_c                   12.6509(10)
_cell_measurement_reflns_used    2644
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      26.022
_cell_measurement_theta_min      0.998
_cell_volume                     1194.0(2)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_molecular_graphics    Ortep3
_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 0.996
_diffrn_measured_fraction_theta_max 0.996
_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  0.0455
_diffrn_reflns_av_sigmaI/netI    0.1114
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            6272
_diffrn_reflns_theta_full        25.05
_diffrn_reflns_theta_max         25.05
_diffrn_reflns_theta_min         1.67
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.204
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.275
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             481
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.344
_refine_diff_density_min         -0.300
_refine_diff_density_rms         0.070
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.105
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     298
_refine_ls_number_reflns         4218
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.105
_refine_ls_R_factor_all          0.1363
_refine_ls_R_factor_gt           0.0722
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0619P)^2^+0.1971P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1304
_refine_ls_wR_factor_ref         0.1611
_reflns_number_gt                2607
_reflns_number_total             4218
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic800934h_si_003.cif
_cod_data_source_block           Compound1ox
_cod_database_code               4306000