Cyclic C-Amino Phosphorus Ylides as a Source of Bidentate Heteroditopic Ligands (Phosphine/Aminocarbene) for Transition Metals
Joan Vignolle; Bruno Donnadieu; Didier Bourissou; Michèle Soleilhavoup; Guy Bertrand; Journal of the American Chemical Society 128 (2006) 14810–14811; doi:10.1021/ja0662725

data_4111122
_publ_contact_author             'Prof G. Bertrand'
_publ_contact_author_address
;
University of California
UCR-CNRS Joint Research Lab
(UMR 2282) 
Department of Chemistry
Riverside, CA 92521 USA 
;
_publ_contact_author_email       ' guy.bertrand@ucr.edu '
_publ_contact_author_fax         951-827-4713
_publ_section_title
;
 Cyclic C-Amino Phosphorus Ylides as a Source of Bidentate Heteroditopic
 Ligands (Phosphine/Aminocarbene) for Transition Metals
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              14810
_journal_page_last               14811
_journal_paper_doi               10.1021/ja0662725
_journal_volume                  128
_journal_year                    2006
_chemical_formula_sum            'C68 H56 F6 N2 O6 P2 Pd2 S2'
_chemical_formula_weight         1450.01
_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                98.194(2)
_cell_angle_beta                 94.660(2)
_cell_angle_gamma                100.156(2)
_cell_formula_units_Z            2
_cell_length_a                   13.0253(4)
_cell_length_b                   14.6703(5)
_cell_length_c                   17.4565(6)
_cell_measurement_reflns_used    6788
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      29.33
_cell_measurement_theta_min      2.29
_cell_volume                     3230.46(19)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'Sir 97'
_diffrn_ambient_temperature      90(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.0331
_diffrn_reflns_av_sigmaI/netI    0.0347
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            46671
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         1.19
_exptl_absorpt_coefficient_mu    0.741
_exptl_absorpt_correction_T_max  0.9131
_exptl_absorpt_correction_T_min  0.5366
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.491
_exptl_crystal_density_meas      0
_exptl_crystal_description       'prism frag'
_exptl_crystal_F_000             1468
_exptl_crystal_size_max          0.96
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.13
_refine_diff_density_max         1.052
_refine_diff_density_min         -1.042
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     919
_refine_ls_number_reflns         13196
_refine_ls_number_restraints     94
_refine_ls_restrained_S_all      1.123
_refine_ls_R_factor_all          0.0426
_refine_ls_R_factor_gt           0.0313
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0389P)^2^+2.5014P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0806
_refine_ls_wR_factor_ref         0.0856
_reflns_number_gt                10647
_reflns_number_total             13196
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0662725si20060829_022032_4.cif
_cod_data_source_block           7
_cod_database_code               4111122