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_4312550
_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         'C23 H26 N2 O P Pd, B F4'
_chemical_formula_sum            'C23 H26 B F4 N2 O P Pd'
_chemical_formula_weight         570.64
_chemical_name_systematic
;
   ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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                99.023(5)
_cell_angle_beta                 104.466(5)
_cell_angle_gamma                95.540(5)
_cell_formula_units_Z            2
_cell_length_a                   10.172(5)
_cell_length_b                   11.129(5)
_cell_length_c                   11.190(5)
_cell_measurement_reflns_used    15949
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      40.250
_cell_measurement_theta_min      0.998
_cell_volume                     1199.2(10)
_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      173(2)
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_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     0.71069
_diffrn_reflns_av_R_equivalents  0.0295
_diffrn_reflns_av_sigmaI/netI    0.0501
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            16951
_diffrn_reflns_theta_full        40.32
_diffrn_reflns_theta_max         40.32
_diffrn_reflns_theta_min         1.87
_exptl_absorpt_coefficient_mu    0.890
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.580
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             576
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.669
_refine_diff_density_min         -1.811
_refine_diff_density_rms         0.126
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     291
_refine_ls_number_reflns         14964
_refine_ls_number_restraints     11
_refine_ls_restrained_S_all      1.017
_refine_ls_R_factor_all          0.0517
_refine_ls_R_factor_gt           0.0436
_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^)+(0.0616P)^2^+0.7600P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1171
_refine_ls_wR_factor_ref         0.1227
_reflns_number_gt                13091
_reflns_number_total             14964
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic030032y_2.cif
_cod_data_source_block           cristal
_cod_database_code               4312550