Endo-Selective Enyne Ring-Closing Metathesis Promoted by Stereogenic-at-Mo Monoalkoxide and Monoaryloxide Complexes. Efficient Synthesis of Cyclic Dienes Not Accessible through Reactions with Ru Carbenes
Yeon-Ju Lee; Richard R. Schrock; Amir H. Hoveyda; Journal of the American Chemical Society 131 (2009) 10652–10661; doi:10.1021/ja904098h

data_4104780
_publ_section_title
;
 Endo-Selective Enyne Ring-Closing Metathesis Promoted by
 Stereogenic-at-Mo Monoalkoxide and Monoaryloxide Complexes. Efficient
 Synthesis of Cyclic Dienes Not Accessible through Reactions with Ru
 Carbenes
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              10652
_journal_page_last               10661
_journal_paper_doi               10.1021/ja904098h
_journal_volume                  131
_journal_year                    2009
_chemical_formula_moiety         'C46 H50 Mo N2 O'
_chemical_formula_sum            'C46 H50 Mo N2 O'
_chemical_formula_weight         742.82
_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   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 106.856(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   43.321(7)
_cell_length_b                   12.988(2)
_cell_length_c                   14.383(2)
_cell_measurement_reflns_used    9913
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.32
_cell_measurement_theta_min      2.11
_cell_volume                     7745(2)
_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 0.989
_diffrn_measured_fraction_theta_max 0.989
_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  0.0476
_diffrn_reflns_av_sigmaI/netI    0.0359
_diffrn_reflns_limit_h_max       57
_diffrn_reflns_limit_h_min       -56
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            58663
_diffrn_reflns_theta_full        28.37
_diffrn_reflns_theta_max         28.37
_diffrn_reflns_theta_min         1.64
_exptl_absorpt_coefficient_mu    0.375
_exptl_absorpt_correction_T_max  0.9888
_exptl_absorpt_correction_T_min  0.9599
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.274
_exptl_crystal_density_method    none
_exptl_crystal_description       block
_exptl_crystal_F_000             3120
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.760
_refine_diff_density_min         -0.675
_refine_diff_density_rms         0.076
_refine_ls_extinction_coef       na
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_matrix_type           full
_refine_ls_number_parameters     592
_refine_ls_number_reflns         9584
_refine_ls_number_restraints     50
_refine_ls_restrained_S_all      1.076
_refine_ls_R_factor_all          0.0480
_refine_ls_R_factor_gt           0.0370
_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^)+(0.0367P)^2^+9.7751P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0796
_refine_ls_wR_factor_ref         0.0842
_reflns_number_gt                8121
_reflns_number_total             9584
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja904098h_si_003.cif
_cod_data_source_block           C46H50MoN2O
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4104780