Enantioselective Intramolecular [2 + 2 + 2] Cycloaddition of Enediynes for the Synthesis of Chiral Cyclohexa-1,3-dienes
Takanori Shibata; Hiroshi Kurokawa; Kazumasa Kanda; Journal of Organic Chemistry 72 (2007) 6521–6525; doi:10.1021/jo070762d

data_4024123
_publ_section_title
;
 Enantioselective Intramolecular [2 + 2 + 2] Cycloaddition
 of Enediynes for the Synthesis of Chiral Cyclohexa-1,3-dienes
;
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              6521
_journal_page_last               6525
_journal_paper_doi               10.1021/jo070762d
_journal_volume                  72
_journal_year                    2007
_chemical_absolute_configuration 'CHOOSE rm ad rmad syn or unk'
_chemical_formula_moiety         'C36 H32 O8 S4 '
_chemical_formula_sum            'C36 H32 O8 S4'
_chemical_formula_weight         720.88
_space_group_IT_number           1
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      1
_symmetry_space_group_name_Hall  'P 1'
_symmetry_space_group_name_H-M   'P 1'
_audit_creation_date             2006-12-22
_audit_creation_method           'by CrystalStructure 3.7.0'
_cell_angle_alpha                74.3751(9)
_cell_angle_beta                 83.9217(9)
_cell_angle_gamma                74.2005(8)
_cell_formula_units_Z            4
_cell_length_a                   12.4320(2)
_cell_length_b                   16.2601(3)
_cell_length_c                   17.7369(3)
_cell_measurement_reflns_used    31524
_cell_measurement_temperature    173.1
_cell_measurement_theta_max      68.2
_cell_measurement_theta_min      3.4
_cell_volume                     3320.44(10)
_computing_cell_refinement       PROCESS-AUTO
_computing_data_collection       PROCESS-AUTO
_computing_data_reduction        CrystalStructure
_computing_publication_material  'CrystalStructure 3.7.0'
_computing_structure_refinement  CRYSTALS
_computing_structure_solution    SIR92
_diffrn_detector_area_resol_mean 10.00
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_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  0.090
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            61807
_diffrn_reflns_theta_full        68.23
_diffrn_reflns_theta_max         68.23
_exptl_absorpt_coefficient_mu    3.080
_exptl_absorpt_correction_T_max  0.397
_exptl_absorpt_correction_T_min  0.307
_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    1.442
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1504.00
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.90
_refine_diff_density_min         -0.91
_refine_ls_abs_structure_details
'Flack, H. D. (1983), Acta Cryst. A39, 876-881.  9883 Friedel Pairs'
_refine_ls_abs_structure_Flack   0.056(18)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   6.390
_refine_ls_hydrogen_treatment    refall
_refine_ls_number_parameters     1858
_refine_ls_number_reflns         19665
_refine_ls_R_factor_gt           0.0482
_refine_ls_shift/su_max          0.2855
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 1.0'
_refine_ls_weighting_scheme      unit
_refine_ls_wR_factor_ref         0.0556
_reflns_number_gt                19605
_reflns_number_total             21853
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            jo070762dsi20070411_024029.cif
_cod_data_source_block           '_kuro3-off'
_cod_original_formula_sum        'C36 H32 O8 S4 '
_cod_database_code               4024123