Directedortho-C–H Silylation Coupled withtrans-Selective Hydrogenation of Arylalkynes Catalyzed by Ruthenium Complexes of a Xanthene-BasedSi,O,Si-Chelate Ligand, “Xantsil”
Komuro, Takashi; Kitano, Takeo; Yamahira, Nobukazu; Ohta, Keisuke; Okawara, Satoshi; Mager, Nathalie; Okazaki, Masaaki; Tobita, Hiromi; Organometallics 35 (2016) 1209–; doi:10.1021/acs.organomet.5b01013

data_4086473
_publ_section_title
;
 Directedortho-C--H Silylation Coupled withtrans-Selective Hydrogenation
 of Arylalkynes Catalyzed by Ruthenium Complexes of a
 Xanthene-BasedSi,O,Si-Chelate Ligand, &#x201C;Xantsil&#x201D;
;
_journal_issue                   9
_journal_name_full               Organometallics
_journal_page_first              1209
_journal_paper_doi               10.1021/acs.organomet.5b01013
_journal_volume                  35
_journal_year                    2016
_chemical_formula_moiety         'C22 H22 Si'
_chemical_formula_sum            'C22 H22 Si'
_chemical_formula_weight         314.49
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      19
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   8.176(4)
_cell_length_b                   20.602(11)
_cell_length_c                   21.311(12)
_cell_measurement_reflns_used    9222
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.0
_cell_volume                     3590(3)
_computing_cell_refinement       CrystalClear
_computing_data_collection       CrystalClear
_computing_data_reduction        CrystalStructure
_computing_molecular_graphics
;
'ORTEP-3', 'Yadokari-XG 2009 (Wakita, Nemoto, et al., 2009)'
;
_computing_publication_material
;
'Yadokari-XG 2009 (Wakita, Nemoto, et al., 2009)'
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean 7.31
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Rigaku Saturn70 CCD'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.107
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            46013
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         3.03
_exptl_absorpt_coefficient_mu    0.129
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.790
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
'Jacobson, R. (1998) Private communication' 
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.164
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1344
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.983
_refine_diff_density_min         -0.254
_refine_diff_density_rms         0.062
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.19(19)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.809
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     419
_refine_ls_number_reflns         8220
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.809
_refine_ls_R_factor_all          0.1148
_refine_ls_R_factor_gt           0.0523
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0250P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0978
_refine_ls_wR_factor_ref         0.1180
_reflns_number_gt                3629
_reflns_number_total             8220
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            om5b01013_si_002.cif
_cod_data_source_block           compound-2d
_cod_depositor_comments
'Adding full bibliography for 4086472--4086473.cif.'
_cod_database_code               4086473