Mechanistic Analysis of Gold(I)-Catalyzed Intramolecular Allene Hydroalkoxylation Reveals an Off-Cycle Bis(gold) Vinyl Species and Reversible C-O Bond Formation
Timothy J. Brown; Dieter Weber; Michel R. Gagné; Ross A. Widenhoefer; Journal of the American Chemical Society 134 (2012) 9134–9137; doi:10.1021/ja303844h

data_4118035
_publ_contact_author_address
;Department of Chemistry
Duke University
Campus Box 90346
Durham, NC 27708-0346
;
_publ_contact_author_email       rwidenho@chem.duke.edu
_publ_contact_author_fax         '1 (919) 6601605'
_publ_contact_author_name        'Ross A. Widenhoefer'
_publ_contact_author_phone       '1 (919) 6601533'
_publ_section_title
;
 Mechanistic Analysis of Gold(I)-Catalyzed Intramolecular Allene
 Hydroalkoxylation Reveals an Off-Cycle Bis(gold) Vinyl Species and
 Reversible C-O Bond Formation
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              9134
_journal_page_last               9137
_journal_paper_doi               10.1021/ja303844h
_journal_volume                  134
_journal_year                    2012
_chemical_formula_sum            'C38 H44 Au O P'
_chemical_formula_weight         744.67
_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                78.881(4)
_cell_angle_beta                 78.768(4)
_cell_angle_gamma                67.199(5)
_cell_formula_units_Z            2
_cell_length_a                   10.4836(10)
_cell_length_b                   12.0170(12)
_cell_length_c                   13.9089(13)
_cell_measurement_reflns_used    4663
_cell_measurement_temperature    110
_cell_measurement_theta_max      31.80
_cell_measurement_theta_min      2.23
_cell_volume                     1571.0(3)
_computing_cell_refinement       SAINT
_computing_data_collection       Apex2
_computing_data_reduction        SAINT
_computing_molecular_graphics    NRCVAX
_computing_publication_material  cif2tables.py
_computing_structure_refinement  XL
_computing_structure_solution    XS
_diffrn_ambient_temperature      110
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.930
_diffrn_measurement_device_type  'Bruker-Nonius Kappa Axis X8 Apex2'
_diffrn_measurement_method       'omega and phi 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  0.0471
_diffrn_reflns_av_sigmaI/netI    0.0490
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            29017
_diffrn_reflns_theta_full        36.32
_diffrn_reflns_theta_max         37.93
_diffrn_reflns_theta_min         1.85
_exptl_absorpt_coefficient_mu    4.762
_exptl_absorpt_correction_T_max  0.7730
_exptl_absorpt_correction_T_min  0.2517
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   TWINABS
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.574
_exptl_crystal_description       plate
_exptl_crystal_F_000             748
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.06
_refine_diff_density_max         5.034
_refine_diff_density_min         -2.020
_refine_diff_density_rms         0.175
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.119
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     377
_refine_ls_number_reflns         29017
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.119
_refine_ls_R_factor_all          0.0516
_refine_ls_R_factor_gt           0.0415
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0835P)^2^+40.5672P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1061
_refine_ls_wR_factor_ref         0.1167
_reflns_number_gt                25686
_reflns_number_total             29017
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja303844h_si_001.cif
_cod_data_source_block           x11039
_cod_database_code               4118035