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_4113498
_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            'C50 H65 N O2 W'
_chemical_formula_weight         895.88
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 113.5690(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   22.2675(15)
_cell_length_b                   19.8014(14)
_cell_length_c                   22.5546(15)
_cell_measurement_temperature    293(2)
_cell_volume                     9115.3(11)
_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 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0686
_diffrn_reflns_av_sigmaI/netI    0.0619
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            15311
_diffrn_reflns_theta_full        21.50
_diffrn_reflns_theta_max         21.50
_diffrn_reflns_theta_min         2.09
_exptl_absorpt_coefficient_mu    2.572
_exptl_absorpt_correction_T_max  0.4624
_exptl_absorpt_correction_T_min  0.3419
_exptl_absorpt_correction_type   empirical
_exptl_crystal_density_diffrn    1.306
_exptl_crystal_F_000             3696
_refine_diff_density_max         1.411
_refine_diff_density_min         -2.103
_refine_diff_density_rms         0.119
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.397
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     482
_refine_ls_number_reflns         5241
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.397
_refine_ls_R_factor_all          0.1026
_refine_ls_R_factor_gt           0.0887
_refine_ls_shift/su_max          0.014
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0182P)^2^+189.8251P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1437
_refine_ls_wR_factor_ref         0.1478
_reflns_number_gt                4697
_reflns_number_total             5241
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0210603_s1.cif
_cod_data_source_block           Compound16
_cod_depositor_comments
;

2021-08-29
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C400 H520 N8 O16 W8'
_cod_original_formula_units_Z            1
_cod_database_code               4113498