Palladium-Catalyzed Deallylation of Allyl Ethers with a Xanthene Phosphole Ligand. Experimental and DFT Mechanistic Studies
Mora, Guilhem; Piechaczyk, Olivier; Le Goff, Xavier F.; Le Floch, Pascal; Organometallics 27 (2008) 2565–; doi:10.1021/om800051n

data_4071237
_publ_section_title
;
 Palladium-Catalyzed Deallylation of Allyl Ethers with a Xanthene
 Phosphole Ligand. Experimental and DFT Mechanistic Studies
;
_journal_issue                   11
_journal_name_full               Organometallics
_journal_page_first              2565
_journal_paper_doi               10.1021/om800051n
_journal_volume                  27
_journal_year                    2008
_chemical_formula_moiety
'C50 H41 O P2 Pd, 1/2C6 H6 O, C H2 Cl2, 2(F6 P)'
_chemical_formula_sum            'C54 H46 Cl2 F6 O1.5 P3 Pd'
_chemical_formula_weight         1103.12
_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                90.00
_cell_angle_beta                 126.804(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   34.860(1)
_cell_length_b                   15.184(1)
_cell_length_c                   23.014(1)
_cell_measurement_reflns_used    10298
_cell_measurement_temperature    150.0(1)
_cell_measurement_theta_max      30.034
_cell_measurement_theta_min      0.998
_cell_volume                     9753.7(8)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150.0(1)
_diffrn_measured_fraction_theta_full .994
_diffrn_measured_fraction_theta_max .994
_diffrn_measurement_device_type  KappaCCD
_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     0.71069
_diffrn_reflns_av_R_equivalents  0.0226
_diffrn_reflns_av_sigmaI/netI    0.0360
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -49
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            31782
_diffrn_reflns_theta_full        30.06
_diffrn_reflns_theta_max         30.06
_diffrn_reflns_theta_min         1.53
_exptl_absorpt_coefficient_mu    0.652
_exptl_absorpt_correction_T_max  0.9085
_exptl_absorpt_correction_T_min  0.8698
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.502
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             4488
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.708
_refine_diff_density_min         -1.230
_refine_diff_density_rms         .085
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.009
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     645
_refine_ls_number_reflns         14239
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.009
_refine_ls_R_factor_all          0.0725
_refine_ls_R_factor_gt           0.0534
_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^)+(0.0922P)^2^+21.1243P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1498
_refine_ls_wR_factor_ref         0.1688
_reflns_number_gt                10853
_reflns_number_total             14239
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om800051n-file005.cif
_cod_data_source_block           gm433
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      'C2/c     '
_cod_original_formula_sum        'C54 H46 Cl2 F6 O1.50 P3 Pd'
_cod_database_code               4071237