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_4109575
_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         'C24 H28 N2 O4 S2, C7 H8 '
_chemical_formula_sum            'C31 H36 N2 O4 S2'
_chemical_formula_weight         564.76
_chemical_melting_point          468(2)
_space_group_IT_number           60
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      60
_symmetry_space_group_name_Hall  '-P 2n 2ab'
_symmetry_space_group_name_H-M   'P b c n'
_audit_creation_date             2006-11-01
_audit_creation_method           'by CrystalStructure 3.8.0'
_cell_angle_alpha                90.0000
_cell_angle_beta                 90.0000
_cell_angle_gamma                90.0000
_cell_formula_units_Z            8
_cell_length_a                   30.7329(5)
_cell_length_b                   12.1699(2)
_cell_length_c                   15.1349(2)
_cell_measurement_reflns_used    43683
_cell_measurement_temperature    93.1
_cell_measurement_theta_max      68.4
_cell_measurement_theta_min      3.3
_cell_volume                     5660.70(15)
_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    'SIR2002 (Burla, 2003)'
_diffrn_detector_area_resol_mean 10.00
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.069
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            68671
_diffrn_reflns_theta_full        68.25
_diffrn_reflns_theta_max         68.25
_exptl_absorpt_coefficient_mu    2.023
_exptl_absorpt_correction_T_max  0.817
_exptl_absorpt_correction_T_min  0.605
_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    1.325
_exptl_crystal_description       block
_exptl_crystal_F_000             2400.00
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.36
_refine_diff_density_min         -0.27
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.106
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     356
_refine_ls_number_reflns         5177
_refine_ls_R_factor_gt           0.0495
_refine_ls_shift/su_max          0.0010
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0657P)^2^+2.2828P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.1457
_reflns_number_gt                3629
_reflns_number_total             5177
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            ja071954tsi20070320_072202.cif
_cod_data_source_block           '_SC0064raplt'
_cod_original_cell_volume        5660.71(15)
_cod_original_formula_sum        'C31 H36 N2 O4 S2 '
_cod_database_code               4109575