Ruthenium Allenylidene/Alkenylcarbyne Complexes Triggering Keto−Enol Tautomerism: An Alternative Approach to γ-Keto Vinylidenes from Simple Ketones and 1,3-Dicarbonyl Compounds
Bustelo, Emilio; Jiménez-Tenorio, Manuel; Puerta, M. Carmen; Valerga, Pedro; Organometallics 25 (2006) 4019–; doi:10.1021/om060453y

data_4074192
_publ_section_title
;
 Ruthenium Allenylidene/Alkenylcarbyne Complexes Triggering
 Keto&#x2212;Enol Tautomerism:&#x00A0; An Alternative Approach to \g-Keto
 Vinylidenes from Simple Ketones and 1,3-Dicarbonyl Compounds
;
_journal_issue                   16
_journal_name_full               Organometallics
_journal_page_first              4019
_journal_paper_doi               10.1021/om060453y
_journal_volume                  25
_journal_year                    2006
_chemical_formula_moiety         'C36 H59 O P2 Ru; B F4'
_chemical_formula_sum            'C36 H59 B F4 O P2 Ru'
_chemical_formula_weight         757.65
_chemical_name_common
'[(\h^5^-C~5~Me~5~)Ru(dippe){=C=CHCHPhCH~2~COCH~3~}][BF~4~]'
_chemical_name_systematic
;{1,2-bis(diisopropylphosphino)ethane}-(pentahapto-pentamethylcyclopentadienyl)
-{(1-phenyl-3-acetyl)butyl-vinylidene}-ruthenium (II) tetrafluorborate
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_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                 93.15(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.780(3)
_cell_length_b                   11.933(2)
_cell_length_c                   20.543(4)
_cell_measurement_reflns_used    5906
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      24.968
_cell_measurement_theta_min      2.355
_cell_volume                     3617.7(12)
_computing_cell_refinement       'Bruker SAINT +'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT +, SADABS, XPREP'
_computing_molecular_graphics    'ORTEP-3 vers. 1.08 (L.J. Faruggia, 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Bruker SMART APEX CCD area detector'
_diffrn_measurement_method       '1700 omega scan frames, 0.3 deg, 10 sec'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0283
_diffrn_reflns_av_sigmaI/netI    0.0356
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            16201
_diffrn_reflns_theta_full        25.06
_diffrn_reflns_theta_max         25.06
_diffrn_reflns_theta_min         1.97
_diffrn_source                   'fine-focus sealed tube'
_diffrn_source_type              'Bruker SMART APEX'
_diffrn_standards_decay_%        0.0010
_exptl_absorpt_coefficient_mu    0.570
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.750
_exptl_absorpt_correction_type   'semi-empirical from equiv.(prg.SADABS)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.391
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1592
_exptl_crystal_size_max          0.43
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.24
_refine_diff_density_max         0.763
_refine_diff_density_min         -0.714
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     560
_refine_ls_number_reflns         6341
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.0672
_refine_ls_R_factor_gt           0.0616
_refine_ls_shift/su_max          0.085
_refine_ls_shift/su_mean         0.005
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0385P)^2^+14.0484P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1282
_refine_ls_wR_factor_ref         0.1314
_reflns_number_gt                5893
_reflns_number_total             6341
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om060453ysi20060523_020930.cif
_cod_data_source_block           pv0604
_cod_original_cell_volume        3617.5(13)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4074192