Formation of (Alkenylphosphonio)phenylruthenium Complexes from Diphenylacetylene and a [CpRu(dppm)] Cation: Experimental Evidence for the Equilibrium between η1-Disubstituted Vinylidene and η2-Internal Alkyne
Mutoh, Yuichiro; Kimura, Yusuke; Ikeda, Yousuke; Tsuchida, Noriko; Takano, Keiko; Ishii, Youichi; Organometallics 31 (2012) 5150–; doi:10.1021/om3004948

data_4078880
_publ_section_title
;
 Formation of (Alkenylphosphonio)phenylruthenium Complexes from
 Diphenylacetylene and a [CpRu(dppm)] Cation: Experimental Evidence for
 the Equilibrium between \h1-Disubstituted Vinylidene and \h2-Internal
 Alkyne
;
_journal_issue                   14
_journal_name_full               Organometallics
_journal_page_first              5150
_journal_paper_doi               10.1021/om3004948
_journal_volume                  31
_journal_year                    2012
_chemical_formula_moiety         'C76 H49 B F24 P2 Ru'
_chemical_formula_sum            'C76 H49 B F24 P2 Ru'
_chemical_formula_weight         1592.01
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                69.419(4)
_cell_angle_beta                 84.293(5)
_cell_angle_gamma                78.708(5)
_cell_formula_units_Z            4
_cell_length_a                   16.690(2)
_cell_length_b                   18.527(2)
_cell_length_c                   24.597(3)
_cell_measurement_reflns_used    18388
_cell_measurement_temperature    113
_cell_measurement_theta_max      30.80
_cell_measurement_theta_min      1.90
_cell_volume                     6978.6(14)
_computing_cell_refinement       CrystalClear
_computing_data_collection       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_reduction        CrystalClear
_computing_molecular_graphics    'CrystalStructure 4.0'
_computing_publication_material  'CrystalStructure 4.0 (Rigaku, 2010)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR92 (Altomare, et al., 1994)'
_diffrn_ambient_temperature      113
_diffrn_detector_area_resol_mean 7.314
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Rigaku Mercury70'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0567
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            105492
_diffrn_reflns_theta_full        27.51
_diffrn_reflns_theta_max         27.50
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.379
_exptl_absorpt_correction_T_max  0.981
_exptl_absorpt_correction_T_min  0.793
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'REQAB (Rigaku, 1998)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.515
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             3200.00
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.050
_refine_diff_density_max         1.590
_refine_diff_density_min         -1.140
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.090
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     1927
_refine_ls_number_reflns         31948
_refine_ls_number_restraints     0
_refine_ls_R_factor_gt           0.0598
_refine_ls_shift/su_max          0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0614P)^2^+10.0985P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.1594
_reflns_number_gt                23793
_reflns_number_total             31948
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            om3004948_si_002.cif
_cod_data_source_block           CpRudppmPhPh_vinylidene_4
_cod_original_cell_volume        6978.7(14)
_cod_database_code               4078880