Ethylene Transposition: Ruthenium Hydride Catalyzed Intramolecular trans-Silylvinylation of Internal Alkynes.
Liu, Shasha; Zhao, Jinbo; Kaminsky, Lauren; Wilson, Robert J.; Marino, Nadia; Clark, Daniel A.; Organic letters 16 (2014) 4456–; doi:10.1021/ol5020027

data_1517401
_publ_section_title
;
 Ethylene Transposition: Ruthenium Hydride Catalyzed Intramolecular
 trans-Silylvinylation of Internal Alkynes.
;
_journal_issue                   17
_journal_name_full               'Organic letters'
_journal_page_first              4456
_journal_paper_doi               10.1021/ol5020027
_journal_volume                  16
_journal_year                    2014
_chemical_formula_moiety         'C15 H19 N O3 Si'
_chemical_formula_sum            'C15 H19 N O3 Si'
_chemical_formula_weight         289.40
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 97.843(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.6235(4)
_cell_length_b                   10.0558(3)
_cell_length_c                   12.9667(4)
_cell_measurement_reflns_used    8560
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      66.21
_cell_measurement_theta_min      4.80
_cell_volume                     1501.42(8)
_computing_cell_refinement       'Bruker SAINT (Bruker, 2011)'
_computing_data_collection       'Bruker APEX2 (Bruker, 2011)'
_computing_data_reduction        'Bruker SAINT (Bruker, 2011)'
_computing_molecular_graphics    'SHELXP-97 (Sheldrick, 2008)'
_computing_publication_material  'Bruker SHELXTL(Bruker,2011)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      90(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0238
_diffrn_reflns_av_sigmaI/netI    0.0183
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            12072
_diffrn_reflns_theta_full        65.06
_diffrn_reflns_theta_max         65.06
_diffrn_reflns_theta_min         4.79
_exptl_absorpt_coefficient_mu    1.443
_exptl_absorpt_correction_T_max  0.9580
_exptl_absorpt_correction_T_min  0.9314
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS SHELXL-97 (Sheldrick, 2008)'
_exptl_crystal_colour            COLOURLESS
_exptl_crystal_density_diffrn    1.280
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       BLOCK
_exptl_crystal_F_000             616
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.296
_refine_diff_density_min         -0.286
_refine_diff_density_rms         0.043
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.142
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     213
_refine_ls_number_reflns         2551
_refine_ls_number_restraints     129
_refine_ls_restrained_S_all      1.129
_refine_ls_R_factor_all          0.0395
_refine_ls_R_factor_gt           0.0374
_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^)+(0.0458P)^2^+0.7908P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0980
_refine_ls_wR_factor_ref         0.0997
_reflns_number_gt                2402
_reflns_number_total             2551
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ol5020027_si_004.cif
_cod_data_source_block           p21n
_cod_depositor_comments
'Adding full bibliography for 1517399--1517401.cif.'
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               1517401