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_4108855
_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         'C73 H70 N O11 P7 Ru '
_chemical_formula_sum            'C73 H70 N O11 P7 Ru'
_chemical_formula_weight         1455.24
_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'
_cell_angle_alpha                85.009(5)
_cell_angle_beta                 82.014(4)
_cell_angle_gamma                84.929(5)
_cell_formula_units_Z            2
_cell_length_a                   9.8148(18)
_cell_length_b                   16.692(3)
_cell_length_c                   20.779(4)
_cell_measurement_reflns_used    8778
_cell_measurement_temperature    123.1
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.0
_cell_volume                     3348.3(11)
_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 0.964
_diffrn_measured_fraction_theta_max 0.964
_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  0.035
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            25710
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_exptl_absorpt_coefficient_mu    0.464
_exptl_absorpt_correction_T_max  0.831
_exptl_absorpt_correction_T_min  0.634
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.443
_exptl_crystal_description       prism
_exptl_crystal_F_000             1504.00
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.60
_exptl_crystal_size_min          0.40
_refine_diff_density_max         0.93
_refine_diff_density_min         -0.73
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.089
_refine_ls_hydrogen_treatment    refall
_refine_ls_number_parameters     839
_refine_ls_number_reflns         14803
_refine_ls_R_factor_gt           0.0608
_refine_ls_shift/su_max          0.0010
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0493P)^2^+6.5148P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.1369
_reflns_number_gt                12427
_reflns_number_total             14803
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            ja8080567_si_002_3.cif
_cod_data_source_block           5a_(PPN)[Ru(P3O9)(=C=CPhMe)]
_cod_original_cell_volume        3348.5(11)
_cod_original_formula_sum        'C73 H70 N O11 P7 Ru '
_cod_database_code               4108855