Alkylidene and Metalacyclic Complexes of Tungsten that Contain a Chiral Biphenoxide Ligand. Synthesis, Asymmetric Ring-Closing Metathesis, and Mechanistic Investigations
W. C. Peter Tsang; Kai C. Hultzsch; John B. Alexander; Peter J. Bonitatebus; Richard R. Schrock; Amir H. Hoveyda; Journal of the American Chemical Society 125 (2003) 2652–2666; doi:10.1021/ja0210603

data_4113499
_publ_section_title
;
 Alkylidene and Metalacyclic Complexes of Tungsten that Contain a Chiral
 Biphenoxide Ligand. Synthesis, Asymmetric Ring-Closing Metathesis, and
 Mechanistic Investigations
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              2652
_journal_page_last               2666
_journal_paper_doi               10.1021/ja0210603
_journal_volume                  125
_journal_year                    2003
_chemical_formula_sum            'C45 H63 N O3 W'
_chemical_formula_weight         849.81
_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                75.914(3)
_cell_angle_beta                 80.904(2)
_cell_angle_gamma                65.334(2)
_cell_formula_units_Z            2
_cell_length_a                   10.1880(16)
_cell_length_b                   10.8869(17)
_cell_length_c                   21.512(3)
_cell_measurement_temperature    293(2)
_cell_volume                     2098.8(6)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.962
_diffrn_measured_fraction_theta_max 0.962
_diffrn_measurement_device_type  'CCD area detector'
_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     0.71073
_diffrn_reflns_av_R_equivalents  0.0321
_diffrn_reflns_av_sigmaI/netI    0.0241
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            8327
_diffrn_reflns_theta_full        23.34
_diffrn_reflns_theta_max         23.34
_diffrn_reflns_theta_min         2.47
_exptl_absorpt_coefficient_mu    2.790
_exptl_absorpt_correction_T_max  0.5958
_exptl_absorpt_correction_T_min  0.3937
_exptl_absorpt_correction_type   empirical
_exptl_crystal_density_diffrn    1.345
_exptl_crystal_F_000             876
_refine_diff_density_max         1.304
_refine_diff_density_min         -0.876
_refine_diff_density_rms         0.083
_refine_ls_extinction_coef       0.0018(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.118
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     452
_refine_ls_number_reflns         5863
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.118
_refine_ls_R_factor_all          0.0292
_refine_ls_R_factor_gt           0.0281
_refine_ls_shift/su_max          0.014
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0401P)^2^+3.0035P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0701
_refine_ls_wR_factor_ref         0.0708
_reflns_number_gt                5688
_reflns_number_total             5863
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0210603_s2.cif
_cod_data_source_block           Compound14
_cod_original_cell_volume        2098.7(6)
_cod_database_code               4113499