Formation of Vinylidenes from Internal Alkynes at a Cyclotriphosphato Ruthenium Complex
Yousuke Ikeda; Takafumi Yamaguchi; Keiichiro Kanao; Kazuhiro Kimura; Sou Kamimura; Yuichiro Mutoh; Yoshiaki Tanabe; Youichi Ishii; Journal of the American Chemical Society 130 (2008) 16856–16857; doi:10.1021/ja8080567

data_4108854
_publ_section_title
;
 Formation of Vinylidenes from Internal Alkynes at a Cyclotriphosphato
 Ruthenium Complex
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              16856
_journal_page_last               16857
_journal_paper_doi               10.1021/ja8080567
_journal_volume                  130
_journal_year                    2008
_chemical_formula_moiety         'C66 H70 N O13 P7 Ru '
_chemical_formula_sum            'C66 H70 N O13 P7 Ru'
_chemical_formula_weight         1403.16
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_cell_angle_alpha                90.0000
_cell_angle_beta                 90.293(3)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            4
_cell_length_a                   17.828(3)
_cell_length_b                   18.996(4)
_cell_length_c                   19.444(4)
_cell_measurement_reflns_used    19509
_cell_measurement_temperature    123.1
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.1
_cell_volume                     6585(2)
_computing_cell_refinement       CrystalClear
_computing_data_collection       CrystalClear
_computing_data_reduction        CrystalStructure
_computing_publication_material  'CrystalStructure 3.8'
_computing_structure_refinement  SHELXL
_computing_structure_solution    SIR97
_diffrn_detector_area_resol_mean 7.31
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Rigaku Mercury'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.033
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            49689
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_exptl_absorpt_coefficient_mu    0.471
_exptl_absorpt_correction_T_max  0.790
_exptl_absorpt_correction_T_min  0.642
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.415
_exptl_crystal_description       prism
_exptl_crystal_F_000             2904.00
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.50
_exptl_crystal_size_min          0.50
_refine_diff_density_max         2.16
_refine_diff_density_min         -0.65
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.089
_refine_ls_hydrogen_treatment    refall
_refine_ls_number_parameters     794
_refine_ls_number_reflns         14949
_refine_ls_R_factor_gt           0.0490
_refine_ls_shift/su_max          0.0020
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0687P)^2^+10.5128P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.1380
_reflns_number_gt                12983
_reflns_number_total             14949
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            ja8080567_si_002_2.cif
_cod_data_source_block           2_(PPN)[Ru(P3O9)(CH3OH)(dppe)]
_cod_original_formula_sum        'C66 H70 N O13 P7 Ru '
_cod_database_code               4108854