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_4086472
_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         'C35 H51 O2 P Ru Si2'
_chemical_formula_sum            'C35 H51 O2 P Ru Si2'
_chemical_formula_weight         691.98
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                106.2466(19)
_cell_angle_beta                 100.4617(16)
_cell_angle_gamma                100.808(2)
_cell_formula_units_Z            4
_cell_length_a                   10.0512(7)
_cell_length_b                   18.7660(12)
_cell_length_c                   19.7903(14)
_cell_measurement_reflns_used    65638
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.4
_cell_measurement_theta_min      1.1
_cell_volume                     3410.1(4)
_computing_cell_refinement       PROCESS-AUTO
_computing_data_collection       PROCESS-AUTO
_computing_data_reduction        'teXsan Ver.1.11'
_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      150(2)
_diffrn_detector_area_resol_mean 10.00
_diffrn_measured_fraction_theta_full 0.978
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measurement_device_type  'Rigaku RAXIS-RAPID Imaging Plate'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating-anode X-ray tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0919
_diffrn_reflns_av_sigmaI/netI    0.0752
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            42248
_diffrn_reflns_theta_full        27.40
_diffrn_reflns_theta_max         27.40
_diffrn_reflns_theta_min         1.11
_exptl_absorpt_coefficient_mu    0.606
_exptl_absorpt_correction_T_max  0.926687
_exptl_absorpt_correction_T_min  0.857851
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
; 
HIGASHI, T. (1999). Shape - Program to obtain Crystal Shape using CCD camera.
Rigaku Corporation, Tokyo, Japan. 
HIGASHI, T. (1999). Numabs - Numerical Absorption Correction,
Rigaku Corporation, Tokyo, Japan. 
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.348
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1456
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.924
_refine_diff_density_min         -1.339
_refine_diff_density_rms         0.243
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.213
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     752
_refine_ls_number_reflns         15159
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.213
_refine_ls_R_factor_all          0.0970
_refine_ls_R_factor_gt           0.0746
_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^)+(0.0637P)^2^+10.7554P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1598
_refine_ls_wR_factor_ref         0.1747
_reflns_number_gt                12557
_reflns_number_total             15159
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            om5b01013_si_002.cif
_cod_data_source_block           compound-1-Cyp
_cod_depositor_comments
'Adding full bibliography for 4086472--4086473.cif.'
_cod_database_code               4086472