Enol Ethers as Substrates for EfficientZ- and Enantioselective Ring-Opening/Cross-Metathesis Reactions Promoted by Stereogenic-at-Mo Complexes: Utility in Chemical Synthesis and Mechanistic Attributes
Miao Yu; Ismail Ibrahem; Masayuki Hasegawa; Richard R. Schrock; Amir H. Hoveyda; Journal of the American Chemical Society 134 (2012) 2788–2799; doi:10.1021/ja210946z

data_4117439
_publ_section_title
;
 Enol Ethers as Substrates for EfficientZ- and Enantioselective
 Ring-Opening/Cross-Metathesis Reactions Promoted by Stereogenic-at-Mo
 Complexes: Utility in Chemical Synthesis and Mechanistic Attributes
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              2788
_journal_page_last               2799
_journal_paper_doi               10.1021/ja210946z
_journal_volume                  134
_journal_year                    2012
_chemical_formula_moiety
'[Mo (C26H33Br2SiO2) (C12H17N) (C6H8N) (C10H12)] (C5H12)'
_chemical_formula_sum            'C59 H82 Br2 Mo N2 O2 Si'
_chemical_formula_weight         1135.12
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 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                 100.5680(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   11.1036(9)
_cell_length_b                   12.5845(11)
_cell_length_c                   20.5049(17)
_cell_measurement_reflns_used    9867
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.86
_cell_measurement_theta_min      2.28
_cell_volume                     2816.6(4)
_computing_cell_refinement       'Bruker SAINT'
_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, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker SMART APEX CCD'
_diffrn_measurement_method       '0.3 deg wide \w exposures'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0232
_diffrn_reflns_av_sigmaI/netI    0.0524
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            33266
_diffrn_reflns_theta_full        28.00
_diffrn_reflns_theta_max         28.00
_diffrn_reflns_theta_min         1.95
_exptl_absorpt_coefficient_mu    1.714
_exptl_absorpt_correction_T_max  0.9504
_exptl_absorpt_correction_T_min  0.6738
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.338
_exptl_crystal_density_method    none
_exptl_crystal_description       plate
_exptl_crystal_F_000             1184
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.773
_refine_diff_density_min         -0.251
_refine_diff_density_rms         0.061
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.007(3)
_refine_ls_extinction_coef       na
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.941
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     611
_refine_ls_number_reflns         13252
_refine_ls_number_restraints     597
_refine_ls_restrained_S_all      0.925
_refine_ls_R_factor_all          0.0257
_refine_ls_R_factor_gt           0.0237
_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^)+(0.0000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0531
_refine_ls_wR_factor_ref         0.0535
_reflns_number_gt                12440
_reflns_number_total             13252
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja210946z_si_004.cif
_cod_data_source_block           C59H82Br2MoN2O2Si
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               4117439