Intramolecular Cyclization of Ruthenium Vinylidene Complexes with a Tethering Vinyl Group: Facile Cleavage and Reconstruction of the C-C Double Bond
Cheng-Wei Cheng; Yi-Chun Kuo; Shu-Hao Chang; Ying-Chih Lin; Yi-Hong Liu; Yu Wang; Journal of the American Chemical Society 129 (2007) 14974–14980; doi:10.1021/ja074951p

data_4110252
_publ_section_title
;
 Intramolecular Cyclization of Ruthenium Vinylidene Complexes with a
 Tethering Vinyl Group: Facile Cleavage and Reconstruction of the C-C
 Double Bond
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              14974
_journal_page_last               14980
_journal_paper_doi               10.1021/ja074951p
_journal_volume                  129
_journal_year                    2007
_chemical_formula_sum            'C59 H51 F6 O3 P3 Ru'
_chemical_formula_weight         1115.98
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 104.8960(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.5383(2)
_cell_length_b                   15.3990(3)
_cell_length_c                   20.8194(4)
_cell_measurement_reflns_used    61371
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      1
_cell_volume                     5123.96(16)
_computing_cell_refinement       'HKL Denzo & Scalepack (Otwinowski & Minor)'
_computing_data_collection       'COLLECT (Nonius BV)'
_computing_data_reduction        'HKL Denzo & Scalepack (Otwinowski & Minor)'
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      295(2)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       CCD
_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  0.0823
_diffrn_reflns_av_sigmaI/netI    0.0854
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            33285
_diffrn_reflns_theta_full        27.46
_diffrn_reflns_theta_max         27.46
_diffrn_reflns_theta_min         1.67
_exptl_absorpt_coefficient_mu    0.467
_exptl_absorpt_correction_T_max  0.9548
_exptl_absorpt_correction_T_min  0.9123
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
multi-scan from symmetry-related measurements 
 Sortav (Blessing 1995) 
;
_exptl_crystal_density_diffrn    1.447
_exptl_crystal_F_000             2288
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.625
_refine_diff_density_min         -0.582
_refine_diff_density_rms         0.071
_refine_ls_extinction_coef       0.00015(9)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.997
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     659
_refine_ls_number_reflns         11596
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.997
_refine_ls_R_factor_all          0.1145
_refine_ls_R_factor_gt           0.0527
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0471P)^2^+4.3814P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1050
_refine_ls_wR_factor_ref         0.1291
_reflns_number_gt                6942
_reflns_number_total             11596
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja074951psi20070705_042614.cif
_cod_data_source_block           ic12260
_cod_original_cell_volume        5123.96(15)
_cod_database_code               4110252