Ruthenium-catalyzed cyclization/transfer hydrogenation of 1,6-diynes: Unprecedented mode of alcohol activation via metallacyclopentatriene
Ken Yamashita; Yuki Nagashima; Yoshihiko Yamamoto; Hisao Nishiyama; Chem.Commun. 47 (2011) 11552–; doi:10.1039/c1cc13744a

data_7106952
_publ_section_title
;
 Ruthenium-catalyzed cyclization/transfer hydrogenation of 1,6-diynes:
 Unprecedented mode of alcohol activation via metallacyclopentatriene
;
_journal_name_full               Chem.Commun.
_journal_page_first              11552
_journal_paper_doi               10.1039/c1cc13744a
_journal_volume                  47
_journal_year                    2011
_chemical_formula_sum            'C28 H31 Cl O Ru'
_chemical_formula_weight         520.05
_chemical_name_systematic
;
?
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_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            4
_cell_length_a                   7.2976(5)
_cell_length_b                   14.8834(11)
_cell_length_c                   23.5529(17)
_cell_measurement_reflns_used    6234
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      28.24
_cell_measurement_theta_min      2.21
_cell_volume                     2558.2(3)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_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      153(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK_a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0729
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            6358
_diffrn_reflns_theta_full        28.31
_diffrn_reflns_theta_max         28.31
_diffrn_reflns_theta_min         1.62
_exptl_absorpt_coefficient_mu    0.734
_exptl_absorpt_correction_T_max  1.000000
_exptl_absorpt_correction_T_min  0.623506
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS '
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.350
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1072
_exptl_crystal_size_max          0.80
_exptl_crystal_size_mid          0.50
_exptl_crystal_size_min          0.15
_platon_squeeze_details
;
;
_refine_diff_density_max         0.899
_refine_diff_density_min         -1.439
_refine_diff_density_rms         0.118
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.16(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.128
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     286
_refine_ls_number_reflns         6358
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.128
_refine_ls_R_factor_all          0.0660
_refine_ls_R_factor_gt           0.0567
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[_s^2^(Fo^2^)+(0.0313P)^2^+6.8872P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1305
_refine_ls_wR_factor_ref         0.1339
_reflns_number_gt                5582
_reflns_number_total             6358
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c1cc13744a.txt
_cod_data_source_block           ky161
_cod_original_sg_symbol_H-M      P2(1)2(1)2(1)
_cod_database_code               7106952