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_4116991
_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           19
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      19
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_audit_creation_date             'Tue Mar 25 11:29:13 1997'
_audit_creation_method           'from TEXRAY.INF file'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.167(7)
_cell_length_b                   28.707(4)
_cell_length_c                   10.257(6)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    290.2
_cell_measurement_theta_max      17.7
_cell_measurement_theta_min      12.7
_cell_volume                     4760(4)
_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 scans with profile analysis'
_diffrn_orient_matrix_UB_11      -0.00261
_diffrn_orient_matrix_UB_12      -0.03480
_diffrn_orient_matrix_UB_13      -0.00218
_diffrn_orient_matrix_UB_21      0.06128
_diffrn_orient_matrix_UB_22      -0.00156
_diffrn_orient_matrix_UB_23      0.01255
_diffrn_orient_matrix_UB_31      -0.00797
_diffrn_orient_matrix_UB_32      -0.00058
_diffrn_orient_matrix_UB_33      0.09666
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'X-ray tube'
_diffrn_radiation_type           MoKalpha
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  15.04
_diffrn_reflns_number            3880
_diffrn_reflns_theta_max         25.06
_diffrn_standards_decay_%        -5.40
_diffrn_standards_interval_count 100
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.425
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.917
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   psi-scan
_exptl_crystal_colour            'colorless plate'
_exptl_crystal_density_diffrn    1.258
_exptl_crystal_density_meas      0.000
_exptl_crystal_description       plate
_exptl_crystal_F_000             1912.00
_exptl_crystal_size_max          0.450
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.080
_refine_diff_density_max         -0.94
_refine_diff_density_min         0.60
_refine_ls_extinction_coef       0.00000
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_obs   1.535
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     383
_refine_ls_number_reflns         2821
_refine_ls_number_restraints     0
_refine_ls_R_factor_obs          0.0642
_refine_ls_shift/esd_max         14.6130
_refine_ls_structure_factor_coef F
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_obs         0.0727
_reflns_number_observed          2821
_reflns_number_total             3880
_reflns_observed_criterion       3.00
_cod_data_source_file            ja9701220_2.cif
_cod_data_source_block           '[RU(CP*)(H)(CCCOOME)(DIPPE)][BPH4]'
_cod_original_cell_volume        4760(5)
_cod_original_sg_symbol_H-M      'P 21 21 21 '
_cod_original_formula_sum        'C52 H71 B O2 P2 Ru '
_cod_database_code               4116991