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_4078878
_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         'C79 H52 B F24 P2 Ru'
_chemical_formula_sum            'C79 H52 B F24 P2 Ru'
_chemical_formula_weight         1631.07
_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                73.738(4)
_cell_angle_beta                 88.468(5)
_cell_angle_gamma                87.523(5)
_cell_formula_units_Z            2
_cell_length_a                   12.728(3)
_cell_length_b                   15.881(3)
_cell_length_c                   18.128(3)
_cell_measurement_reflns_used    7667
_cell_measurement_temperature    123
_cell_measurement_theta_max      27.50
_cell_measurement_theta_min      3.02
_cell_volume                     3514.0(12)
_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    'Il Milione (Burla, et al., 2007)'
_diffrn_ambient_temperature      123
_diffrn_detector_area_resol_mean 7.314
_diffrn_measured_fraction_theta_full 0.971
_diffrn_measured_fraction_theta_max 0.971
_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  0.0697
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            27678
_diffrn_reflns_theta_full        27.51
_diffrn_reflns_theta_max         27.51
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.378
_exptl_absorpt_correction_T_max  0.975
_exptl_absorpt_correction_T_min  0.510
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'REQAB (Rigaku, 1998)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.541
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             1642.00
_exptl_crystal_size_max          0.180
_exptl_crystal_size_mid          0.152
_exptl_crystal_size_min          0.067
_refine_diff_density_max         1.150
_refine_diff_density_min         -0.690
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     991
_refine_ls_number_reflns         15707
_refine_ls_number_restraints     0
_refine_ls_R_factor_gt           0.0739
_refine_ls_shift/su_max          0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0496P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.1780
_reflns_number_gt                10268
_reflns_number_total             15707
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            om3004948_si_002.cif
_cod_data_source_block           CpRu(dppm)PhPh_alkyne_2
_cod_original_cell_volume        3514.0(11)
_cod_database_code               4078878