Synthesis, Isolation, Characterization, and Reactivity of High-Energy Stereogenic-at-Ru Carbenes: Stereochemical Inversion through Olefin Metathesis and Other Pathways
R. Kashif M. Khan; Adil R. Zhugralin; Sebastian Torker; Robert V. O'Brien; Pamela J. Lombardi; Amir H. Hoveyda; Journal of the American Chemical Society 134 (2012) 12438–12441; doi:10.1021/ja3056722

data_4118439
_publ_section_title
;
 Synthesis, Isolation, Characterization, and Reactivity of High-Energy
 Stereogenic-at-Ru Carbenes: Stereochemical Inversion through Olefin
 Metathesis and Other Pathways
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              12438
_journal_page_last               12441
_journal_paper_doi               10.1021/ja3056722
_journal_volume                  134
_journal_year                    2012
_chemical_formula_sum            'C54 H51 Cl4 I N2 O2 Ru'
_chemical_formula_weight         1129.74
_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                 90.318(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   12.6693(18)
_cell_length_b                   15.589(2)
_cell_length_c                   12.7899(18)
_cell_measurement_reflns_used    4587
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      22.92
_cell_measurement_theta_min      2.26
_cell_volume                     2526.0(6)
_computing_cell_refinement       'Bruker SMART'
_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, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      193(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0274
_diffrn_reflns_av_sigmaI/netI    0.0544
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            19260
_diffrn_reflns_theta_full        28.38
_diffrn_reflns_theta_max         28.38
_diffrn_reflns_theta_min         1.59
_exptl_absorpt_coefficient_mu    1.175
_exptl_absorpt_correction_T_max  0.9436
_exptl_absorpt_correction_T_min  0.8916
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            wine
_exptl_crystal_density_diffrn    1.485
_exptl_crystal_density_meas      0
_exptl_crystal_description       block
_exptl_crystal_F_000             1140
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.020
_refine_diff_density_min         -0.777
_refine_diff_density_rms         0.098
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.02(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     582
_refine_ls_number_reflns         10888
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0641
_refine_ls_R_factor_gt           0.0504
_refine_ls_shift/su_max          0.108
_refine_ls_shift/su_mean         0.006
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0693P)^2^+0.4488P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1223
_refine_ls_wR_factor_ref         0.1328
_reflns_number_gt                8903
_reflns_number_total             10888
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja3056722_si_001.cif
_cod_data_source_block           az01
_cod_database_code               4118439