Unprecedented Formation of μ-Vinylidene Complexes from Phospharuthenocene and Acyl Chloride via Activation of the CO Double Bond
Ogasawara, Masamichi; Sakamoto, Takeshi; Ito, Azumi; Ge, Yonghui; Nakajima, Kiyohiko; Takahashi, Tamotsu; Hayashi, Tamio; Organometallics 26 (2007) 6698–; doi:10.1021/om701063k

data_4074103
_publ_section_title
;
 Unprecedented Formation of \m-Vinylidene Complexes from
 Phospharuthenocene and Acyl Chloride via Activation of the C&#xE5FB;O
 Double Bond
;
_journal_issue                   27
_journal_name_full               Organometallics
_journal_page_first              6698
_journal_paper_doi               10.1021/om701063k
_journal_volume                  26
_journal_year                    2007
_chemical_formula_moiety         'C34 H53 O1.50 P2 Ru '
_chemical_formula_sum            'C34 H53 O1.5 P2 Ru'
_chemical_formula_weight         648.81
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yab'
_symmetry_space_group_name_H-M   'P 1 21/a 1'
_cell_angle_alpha                90.0000
_cell_angle_beta                 90.759(13)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            4
_cell_length_a                   11.897(3)
_cell_length_b                   16.879(4)
_cell_length_c                   17.761(6)
_cell_measurement_reflns_used    23568
_cell_measurement_temperature    298.1
_cell_measurement_theta_max      27.6
_cell_measurement_theta_min      3.1
_cell_volume                     3566.3(17)
_computing_cell_refinement       PROCESS-AUTO
_computing_data_collection       PROCESS-AUTO
_computing_data_reduction        CrystalStructure
_computing_publication_material  'CrystalStructure 3.8'
_computing_structure_refinement  SHELXL
_computing_structure_solution    SIR2004
_diffrn_detector_area_resol_mean 10.00
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Rigaku RAXIS-RAPID'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.078
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            33753
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_exptl_absorpt_coefficient_mu    0.553
_exptl_absorpt_correction_T_max  0.967
_exptl_absorpt_correction_T_min  0.879
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
    Higashi, T. (1999). Program for Absorption Correction.
    Rigaku Corporation, Tokyo, Japan.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.208
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1372.00
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.21
_refine_diff_density_min         -0.45
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.994
_refine_ls_hydrogen_treatment    mixed
_refine_ls_number_parameters     400
_refine_ls_number_reflns         8159
_refine_ls_R_factor_gt           0.0615
_refine_ls_shift/su_max          0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.1500P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.2074
_reflns_number_gt                6047
_reflns_number_total             8159
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            om701063k-file003.cif
_cod_data_source_block           '_tt77'
_cod_original_cell_volume        3566.2(17)
_cod_original_formula_sum        'C34 H53 O1.50 P2 Ru '
_cod_database_code               4074103