Cyclometalated N-Heterocyclic Carbene Complexes of Ruthenium for Access to Electron-Rich Silylene Complexes That Bind the Lewis Acids CuOTf and AgOTf.
Liu, Hsueh-Ju; Raynaud, Christophe; Eisenstein, Odile; Tilley, T. Don; Journal of the American Chemical Society 136 (2014) 11473–11482; doi:10.1021/ja5054237

data_4122539
_publ_section_title
;
 Cyclometalated N-Heterocyclic Carbene Complexes of Ruthenium for Access
 to Electron-Rich Silylene Complexes That Bind the Lewis Acids CuOTf and
 AgOTf.
;
_journal_issue                   32
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              11473
_journal_page_last               11482
_journal_paper_doi               10.1021/ja5054237
_journal_volume                  136
_journal_year                    2014
_chemical_formula_moiety         'C52 H67 Br N2 O Ru Si, C2.5'
_chemical_formula_sum            'C54.5 H67 Br N2 O Ru Si'
_chemical_formula_weight         975.17
_chemical_name_common            hj4057
_chemical_name_systematic
; 
 ? 
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014
_cell_angle_alpha                90
_cell_angle_beta                 109.314(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   46.2094(15)
_cell_length_b                   12.0283(4)
_cell_length_c                   19.2661(6)
_cell_measurement_reflns_used    9978
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.30
_cell_measurement_theta_min      2.20
_cell_volume                     10105.8(6)
_computing_cell_refinement       'Bruker APEX2 v. 2011.4'
_computing_data_collection       'Bruker APEX2 v. 2011.4'
_computing_data_reduction        'Bruker APEX2 v. 2011.4'
_computing_molecular_graphics    ORTEP-32
_computing_publication_material  WinGX
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_solution    SIR-92
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.366
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0762
_diffrn_reflns_av_unetI/netI     0.0566
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       55
_diffrn_reflns_limit_h_min       -55
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            64370
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.378
_diffrn_reflns_theta_min         1.756
_diffrn_source                   'microfocus sealed tube'
_exptl_absorpt_coefficient_mu    1.163
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6170
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.282
_exptl_crystal_description       block
_exptl_crystal_F_000             4072
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.060
_exptl_crystal_size_min          0.020
_refine_diff_density_max         1.068
_refine_diff_density_min         -0.992
_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     622
_refine_ls_number_reflns         9287
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0658
_refine_ls_R_factor_gt           0.0394
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0312P)^2^+27.7119P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0849
_refine_ls_wR_factor_ref         0.0963
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6915
_reflns_number_total             9287
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja5054237_si_005.cif
_cod_data_source_block           shelx
_cod_original_formula_sum        'C54.50 H67 Br N2 O Ru Si'
_cod_database_code               4122539
_shelx_estimated_absorpt_t_min   0.893
_shelx_estimated_absorpt_t_max   0.977
_shelxl_version_number           2014-3
_shelx_res_checksum              75180
_shelx_hkl_checksum              27213