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_4114894
_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            'C24 H21 Cl2 N O5 S'
_chemical_formula_weight         506.38
_space_group_IT_number           2
_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                100.1930(10)
_cell_angle_beta                 97.8050(10)
_cell_angle_gamma                109.7160(10)
_cell_formula_units_Z            2
_cell_length_a                   8.1787(5)
_cell_length_b                   11.8767(7)
_cell_length_c                   13.1547(8)
_cell_measurement_temperature    173(2)
_cell_volume                     1157.24(12)
_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 0.974
_diffrn_measured_fraction_theta_max 0.974
_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  0.0163
_diffrn_reflns_av_sigmaI/netI    0.0291
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            9078
_diffrn_reflns_theta_full        29.17
_diffrn_reflns_theta_max         29.17
_diffrn_reflns_theta_min         1.61
_exptl_absorpt_coefficient_mu    0.408
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   (SADABS)
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.453
_exptl_crystal_description       plate
_exptl_crystal_F_000             524
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.8
_refine_diff_density_max         0.830
_refine_diff_density_min         -0.616
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.702
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     300
_refine_ls_number_reflns         6096
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.702
_refine_ls_R_factor_all          0.0615
_refine_ls_R_factor_gt           0.0502
_refine_ls_shift/su_max          0.118
_refine_ls_shift/su_mean         0.015
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1720P)^2^+0.3234P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1491
_refine_ls_wR_factor_ref         0.1644
_reflns_number_gt                4778
_reflns_number_total             6096
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0264100_s2_2.cif
_cod_data_source_block           7bg2Cl2
_cod_database_code               4114894