Ruthenium(II)-Catalyzed [2 + 2 + 2] Cycloaddition of 1,6-Diynes with Tricarbonyl Compounds
Yoshihiko Yamamoto; Hideyuki Takagishi; Kenji Itoh; Journal of the American Chemical Society 124 (2002) 6844–6845; doi:10.1021/ja0264100

data_4114893
_publ_section_title
;
 Ruthenium(II)-Catalyzed [2 + 2 + 2] Cycloaddition of 1,6-Diynes with
 Tricarbonyl Compounds
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              6844
_journal_page_last               6845
_journal_paper_doi               10.1021/ja0264100
_journal_volume                  124
_journal_year                    2002
_chemical_formula_sum            'C20 H26 O9'
_chemical_formula_weight         410.41
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_symmetry_cell_setting           triclinic
_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
_audit_creation_method           SHELXL-97
_cell_angle_alpha                95.1660(10)
_cell_angle_beta                 106.8200(10)
_cell_angle_gamma                96.2770(10)
_cell_formula_units_Z            2
_cell_length_a                   8.9287(5)
_cell_length_b                   9.9445(5)
_cell_length_c                   12.4010(7)
_cell_measurement_temperature    173(2)
_cell_volume                     1039.07(10)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.975
_diffrn_measured_fraction_theta_max 0.975
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0233
_diffrn_reflns_av_sigmaI/netI    0.0250
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            8184
_diffrn_reflns_theta_full        29.15
_diffrn_reflns_theta_max         29.15
_diffrn_reflns_theta_min         1.73
_exptl_absorpt_coefficient_mu    0.104
_exptl_absorpt_correction_type   enpirical
_exptl_absorpt_process_details   (sadabs)
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.312
_exptl_crystal_F_000             436
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.7
_refine_diff_density_max         0.681
_refine_diff_density_min         -0.331
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.811
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     267
_refine_ls_number_reflns         5468
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.811
_refine_ls_R_factor_all          0.0625
_refine_ls_R_factor_gt           0.0557
_refine_ls_shift/su_max          0.588
_refine_ls_shift/su_mean         0.026
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1765
_refine_ls_wR_factor_ref         0.1911
_reflns_number_gt                4549
_reflns_number_total             5468
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0264100_s2_1.cif
_cod_data_source_block           4c
_cod_database_code               4114893