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_4078879
_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         'C82 H63 B F24 P2 Ru'
_chemical_formula_sum            'C82 H63 B F24 P2 Ru'
_chemical_formula_weight         1678.19
_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                82.693(4)
_cell_angle_beta                 87.357(4)
_cell_angle_gamma                75.420(4)
_cell_formula_units_Z            2
_cell_length_a                   10.7153(16)
_cell_length_b                   18.425(3)
_cell_length_c                   19.554(3)
_cell_measurement_reflns_used    10782
_cell_measurement_temperature    123
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      3.03
_cell_volume                     3705.5(10)
_computing_cell_refinement       CrystalClear
_computing_data_collection       'CrystalClear (Rigaku Corp., 2000)'
_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    'Il Milione (Burla, et al., 2007)'
_diffrn_ambient_temperature      123
_diffrn_detector_area_resol_mean 7.314
_diffrn_measured_fraction_theta_full 0.956
_diffrn_measured_fraction_theta_max 0.956
_diffrn_measurement_device_type  'Rigaku Mercury70'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0546
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            27555
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.48
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.361
_exptl_absorpt_correction_T_max  0.820
_exptl_absorpt_correction_T_min  0.601
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'REQAB (Rigaku, 1998)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.504
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1700.00
_exptl_crystal_size_max          0.800
_exptl_crystal_size_mid          0.550
_exptl_crystal_size_min          0.550
_refine_diff_density_max         1.330
_refine_diff_density_min         -1.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.984
_refine_ls_hydrogen_treatment    mixed
_refine_ls_number_parameters     1040
_refine_ls_number_reflns         16231
_refine_ls_number_restraints     0
_refine_ls_R_factor_gt           0.0508
_refine_ls_shift/su_max          0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0715P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.1390
_reflns_number_gt                12949
_reflns_number_total             16231
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            om3004948_si_002.cif
_cod_data_source_block           CpRudppmPhPh_alkene_3
_cod_database_code               4078879