Carbon Monoxide-Promoted Carbene Insertion into the Aryl Substituent of an N-Heterocyclic Carbene Ligand: Buchner Reaction in a Ruthenium Carbene Complex
Brandon R. Galan; Milan Gembicky; Paulina M. Dominiak; Jerome B. Keister; Steven T. Diver; Journal of the American Chemical Society 127 (2005) 15702–15703; doi:10.1021/ja0545618

data_4112053
_publ_section_title
;
 Carbon Monoxide-Promoted Carbene Insertion into the Aryl Substituent of
 an N-Heterocyclic Carbene Ligand: Buchner Reaction in a Ruthenium Carbene
 Complex
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              15702
_journal_page_last               15703
_journal_paper_doi               10.1021/ja0545618
_journal_volume                  127
_journal_year                    2005
_chemical_formula_sum            'C49.27 H65 Cl5.95 N2 O2.11 P Ru'
_chemical_formula_weight         1062.02
_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                 99.5360(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   14.3169(3)
_cell_length_b                   21.9313(4)
_cell_length_c                   33.6130(7)
_cell_measurement_temperature    90(2)
_cell_volume                     10408.2(4)
_computing_cell_refinement       'APEX2 (Bruker, 2004)'
_computing_data_collection       'APEX2 (Bruker, 2004)'
_computing_data_reduction        'SAINT-Plus (Bruker, 2004)'
_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      90(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Bruker SMART APEX2'
_diffrn_measurement_method       'omega scan'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0190
_diffrn_reflns_av_sigmaI/netI    0.0137
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       44
_diffrn_reflns_limit_l_min       -45
_diffrn_reflns_number            81739
_diffrn_reflns_theta_full        28.69
_diffrn_reflns_theta_max         28.69
_diffrn_reflns_theta_min         1.23
_exptl_absorpt_coefficient_mu    0.679
_exptl_absorpt_correction_T_max  0.91
_exptl_absorpt_correction_T_min  0.83
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS v2.10; Sheldrick, 1996)'
_exptl_crystal_density_diffrn    1.358
_exptl_crystal_F_000             4413.3
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.689
_refine_diff_density_min         -1.081
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     642
_refine_ls_number_reflns         13318
_refine_ls_number_restraints     31
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0381
_refine_ls_R_factor_gt           0.0341
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0339P)^2^+28.6466P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0833
_refine_ls_wR_factor_ref         0.0862
_reflns_number_gt                12115
_reflns_number_total             13318
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0545618si20050715_120239.cif
_cod_data_source_block           benzylidene
_cod_database_code               4112053