Enolphosphato-Phosphines: A New Class of P,O Ligands
Xavier Morise; Pierre Braunstein; Richard Welter; Inorganic Chemistry 42 (2003) 7752–7765; doi:10.1021/ic030032y

data_4312551
_publ_contact_author_address
;
Institut Le Bel, rue Blaise Pascal, 67000 STRASBOURG, FRANCE
;
_publ_contact_author_email       morise@chimie.u-strasbg.fr
_publ_contact_author_fax         0390245001
_publ_contact_author_name
;
Xavier Morise
;
_publ_contact_author_phone       0390241316
_publ_section_title
;
 Enolphosphato-Phosphines: A New Class of P,O Ligands
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              7752
_journal_page_last               7765
_journal_paper_doi               10.1021/ic030032y
_journal_volume                  42
_journal_year                    2003
_chemical_formula_moiety         'C48 H52 Cl4 O8 P4 Pd2, C4 H10 O'
_chemical_formula_sum            'C52 H62 Cl4 O9 P4 Pd2'
_chemical_formula_weight         1309.50
_chemical_name_systematic
;
   ?
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.0000(10)
_cell_angle_beta                 96.923(3)
_cell_angle_gamma                90.0000(10)
_cell_formula_units_Z            4
_cell_length_a                   24.9753(4)
_cell_length_b                   9.8367(3)
_cell_length_c                   23.6794(4)
_cell_measurement_reflns_used    6981
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      1.4
_cell_volume                     5775.0(2)
_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    'PLATON 98 (Spek, 1998)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       '\p 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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0470
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            6593
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         1.64
_exptl_absorpt_coefficient_mu    0.970
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.506
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2664
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.218
_refine_diff_density_min         -1.205
_refine_diff_density_rms         0.260
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.288
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     311
_refine_ls_number_reflns         6593
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.287
_refine_ls_R_factor_all          0.0636
_refine_ls_R_factor_gt           0.0501
_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^)+(0.0832P)^2^+11.4128P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1599
_refine_ls_wR_factor_ref         0.1742
_reflns_number_gt                5492
_reflns_number_total             6593
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic030032y_3.cif
_cod_data_source_block           st585
_cod_database_code               4312551