Ruthenium-Catalyzed [2 + 2 + 2] Cocyclization of Diene-yne
Daisuke Tanaka; Yoshihiro Sato; Miwako Mori; Journal of the American Chemical Society 129 (2007) 7730–7731; doi:10.1021/ja071954t

data_4109576
_publ_contact_author_address
;
Health Scieces University of Hokkaido
Ishikari-Tobetsu
Hokkaido 061-0293
Japan
;
_publ_contact_author_email       mori@pharm.hokudai.ac.jp
_publ_contact_author_fax         +81-11-787-6045
_publ_contact_author_name        'Dr Miwako Mori'
_publ_contact_author_phone       +81-11-787-6045
_publ_section_title
;
 Ruthenium-Catalyzed [2 + 2 + 2] Cocyclization of Diene-yne
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              7730
_journal_page_last               7731
_journal_paper_doi               10.1021/ja071954t
_journal_volume                  129
_journal_year                    2007
_chemical_formula_moiety         'C26 H32 N2 O4 S2 '
_chemical_formula_sum            'C26 H32 N2 O4 S2'
_chemical_formula_weight         500.67
_chemical_melting_point          492(1)
_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'
_audit_creation_date             2006-11-14
_audit_creation_method           'by CrystalStructure 3.8.0'
_cell_angle_alpha                79.995(2)
_cell_angle_beta                 80.8101(19)
_cell_angle_gamma                85.537(3)
_cell_formula_units_Z            2
_cell_length_a                   6.28801(17)
_cell_length_b                   12.0898(4)
_cell_length_c                   16.3874(5)
_cell_measurement_reflns_used    8110
_cell_measurement_temperature    93.1
_cell_measurement_theta_max      68.2
_cell_measurement_theta_min      4.3
_cell_volume                     1209.48(6)
_computing_cell_refinement       'PROCESS-AUTO (Rigaku, 1998)'
_computing_data_collection       'PROCESS-AUTO (Rigaku, 1998)'
_computing_data_reduction        'CrystalStructure (R/MSC, Rigaku, 2005)'
_computing_molecular_graphics    'ORTEP (Johnson, 1976)'
_computing_publication_material  'CrystalStructure (R/MSC, Rigaku, 2005)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'PATTY (Beurskens, 1994)'
_diffrn_detector_area_resol_mean 10.00
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'Rigaku RAXIS-RAPID'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54187
_diffrn_reflns_av_R_equivalents  0.043
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            25744
_diffrn_reflns_theta_full        68.25
_diffrn_reflns_theta_max         68.25
_exptl_absorpt_coefficient_mu    2.292
_exptl_absorpt_correction_T_max  0.934
_exptl_absorpt_correction_T_min  0.667
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
    Higashi, T. (1995). Program for Absorption Correction.
    Rigaku Corporation, Tokyo, Japan.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.375
_exptl_crystal_description       platelet
_exptl_crystal_F_000             532.00
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.51
_refine_diff_density_min         -0.35
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.111
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     312
_refine_ls_number_reflns         4374
_refine_ls_R_factor_gt           0.0362
_refine_ls_shift/su_max          0.0010
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0498P)^2^+0.5921P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0999
_reflns_number_gt                3981
_reflns_number_total             4374
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            ja071954tsi20070320_072222.cif
_cod_data_source_block           '_SC0065raplt'
_cod_original_formula_sum        'C26 H32 N2 O4 S2 '
_cod_database_code               4109576