Alternative Mechanisms of the Alkyne to Vinylidene Isomerization Promoted by Half-Sandwich Ruthenium Complexes. X-ray Crystal Structures of [Cp*RuCCHCOOMe(dippe)][BPh4] and [Cp*RuH(C\τbCCOOMe)(dippe)][BPh4] (dippe = 1,2-bis(diisopropylphosphino)ethane; Cp* = C5Me5)
Isaac de los Ríos; Manuel Jiménez Tenorio; M. Carmen Puerta; Pedro Valerga; Journal of the American Chemical Society 119 (1997) 6529–6538; doi:10.1021/ja9701220

data_4116990
_publ_contact_author
;
    M.Carmen Puerta
    Departamento de Qu=A1mica Inorg=A0nica
    Facultad de Ciencias. Universidad de C=A0diz.
    Apartado 40. Puerto Real 11510. SPAIN.
;
_publ_contact_author_email       ' carmen.puerta@uca.es '
_publ_contact_author_fax         ' 34-956-834924 '
_publ_contact_author_phone       ' 34-956-830828 '
_publ_section_title
;
 Alternative Mechanisms of the Alkyne to Vinylidene Isomerization Promoted
 by Half-Sandwich Ruthenium Complexes. X-ray Crystal Structures of
 [Cp*RuCCHCOOMe(dippe)][BPh4] and [Cp*RuH(C\\tbCCOOMe)(dippe)][BPh4]
 (dippe = 1,2-bis(diisopropylphosphino)ethane; Cp* = C5Me5)
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              6529
_journal_page_last               6538
_journal_paper_doi               10.1021/ja9701220
_journal_volume                  119
_journal_year                    1997
_chemical_formula_sum            'C52 H71 B O2 P2 Ru'
_chemical_formula_weight         901.96
_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'
_audit_creation_date             'Tue Mar 25 10:07:30 1997'
_audit_creation_method           'from TEXRAY.INF file'
_cell_angle_alpha                95.81(2)
_cell_angle_beta                 91.09(1)
_cell_angle_gamma                94.36(1)
_cell_formula_units_Z            2
_cell_length_a                   13.275(2)
_cell_length_b                   14.672(3)
_cell_length_c                   12.172(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    290.2
_cell_measurement_theta_max      18.4
_cell_measurement_theta_min      12.4
_cell_volume                     2350.9(7)
_computing_cell_refinement       'MSC/AFC Diffractometer Control'
_computing_data_collection       'MSC/AFC Diffractometer Control'
_computing_data_reduction        teXsan
_computing_publication_material  teXsan
_computing_structure_refinement  teXsan
_diffrn_ambient_temperature      290.2
_diffrn_measurement_device       AFC6S
_diffrn_measurement_method       'omega/2-theta scans'
_diffrn_orient_matrix_UB_11      -0.07277
_diffrn_orient_matrix_UB_12      0.00474
_diffrn_orient_matrix_UB_13      0.01781
_diffrn_orient_matrix_UB_21      -0.01888
_diffrn_orient_matrix_UB_22      -0.01202
_diffrn_orient_matrix_UB_23      -0.08037
_diffrn_orient_matrix_UB_31      -0.00778
_diffrn_orient_matrix_UB_32      -0.06749
_diffrn_orient_matrix_UB_33      0.00689
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'X-ray tube'
_diffrn_radiation_type           MoKalpha
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  5.23
_diffrn_reflns_number            7516
_diffrn_reflns_theta_max         25.05
_diffrn_standards_decay_%        -1.20
_diffrn_standards_interval_count 100
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.430
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.861
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   psi-scan
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.274
_exptl_crystal_density_meas      0.000
_exptl_crystal_description       irregular
_exptl_crystal_F_000             956.00
_exptl_crystal_size_max          0.280
_exptl_crystal_size_mid          0.170
_exptl_crystal_size_min          0.100
_refine_diff_density_max         -0.80
_refine_diff_density_min         0.95
_refine_ls_extinction_coef       0.00000
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_obs   1.687
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     495
_refine_ls_number_reflns         4322
_refine_ls_number_restraints     0
_refine_ls_R_factor_obs          0.0579
_refine_ls_shift/esd_max         5.7045
_refine_ls_structure_factor_coef F
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_obs         0.0695
_reflns_number_observed          4322
_reflns_number_total             7516
_reflns_observed_criterion       3.00
_cod_data_source_file            ja9701220_1.cif
_cod_data_source_block           '[Ru(Cp*)(C_CHCOOMe)(dippe)][BPh4]'
_cod_original_sg_symbol_H-M      'P -1 '
_cod_original_formula_sum        'C52 H71 B O2 P2 Ru '
_cod_database_code               4116990