Isomerization of Terminal Epoxides by a [Pd-H] Catalyst: A Combined Experimental and Theoretical Mechanistic Study
Devendra J. Vyas; Evgeny Larionov; Céline Besnard; Laure Guénée; Clément Mazet; Journal of the American Chemical Society 135 (2013) 6177–6183; doi:10.1021/ja400325w

data_4119613
_publ_contact_author_name
;
;
_publ_section_title
;
 Isomerization of Terminal Epoxides by a [Pd-H] Catalyst: A Combined
 Experimental and Theoretical Mechanistic Study
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              6177
_journal_page_last               6183
_journal_paper_doi               10.1021/ja400325w
_journal_volume                  135
_journal_year                    2013
_chemical_formula_moiety         'C45 H104 P6 Pd2, 2(C F3 O3 S)'
_chemical_formula_sum            'C47 H104 F6 O6 P6 Pd2 S2'
_chemical_formula_weight         1342.04
_chemical_name_systematic
;
 ? 
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2012-06-28
_audit_creation_method
;
  Olex2 1.2-beta
  (compiled May  9 2012 12:37:22, GUI svn.r4230)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 94.181(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.9673(5)
_cell_length_b                   28.4151(8)
_cell_length_c                   15.1131(5)
_cell_measurement_temperature    180(2)
_cell_volume                     6410.5(4)
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
SHELXL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution
;
XS, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_diffrn_ambient_temperature      180.15
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.968
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0619
_diffrn_reflns_av_unetI/netI     0.0815
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            28575
_diffrn_reflns_theta_full        67.00
_diffrn_reflns_theta_max         74.28
_diffrn_reflns_theta_min         2.96
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    7.034
_exptl_absorpt_correction_T_max  0.7537
_exptl_absorpt_correction_T_min  0.5930
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2009/1 (Bruker,2010) was used for absorption correction.
wR2(int) was 0.0802 before and 0.0675 after correction.
The Ratio of minimum to maximum transmission is 0.7868.
The \l/2 correction factor is Not present.
;
_exptl_crystal_density_diffrn    1.391
_exptl_crystal_description       platelet
_exptl_crystal_F_000             2808
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.03
_refine_diff_density_max         2.154
_refine_diff_density_min         -1.332
_refine_diff_density_rms         0.132
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     718
_refine_ls_number_reflns         12650
_refine_ls_number_restraints     250
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0926
_refine_ls_R_factor_gt           0.0693
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1081P)^2^+10.4056P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1845
_refine_ls_wR_factor_ref         0.2060
_reflns_number_gt                9386
_reflns_number_total             12650
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja400325w_si_002.cif
_cod_data_source_block           free
_cod_database_code               4119613