Au(I)-Catalyzed Cyclization of Enynes Bearing an Olefinic Cycle
Sang Ick Lee; Soo Min Kim; Mi Ra Choi; Sun Young Kim; Young Keun Chung; Won-Sik Han; Sang Ook Kang; Journal of Organic Chemistry 71 (2006) 9366–9372; doi:10.1021/jo061254r

data_4022130
_publ_section_title
;
 Au(I)-Catalyzed Cyclization of Enynes Bearing an Olefinic Cycle
;
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              9366
_journal_page_last               9372
_journal_paper_doi               10.1021/jo061254r
_journal_volume                  71
_journal_year                    2006
_chemical_formula_sum            'C27 H30 N2 O4 S2'
_chemical_formula_weight         510.16
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 97.708(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.5935(4)
_cell_length_b                   9.6906(6)
_cell_length_c                   19.9797(12)
_cell_measurement_temperature    293(2)
_cell_volume                     2608.1(2)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_molecular_graphics    ORTEP32
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.974
_diffrn_measured_fraction_theta_max 0.974
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       '95mm CCD camera on \k-goniostat'
_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  0.0380
_diffrn_reflns_av_sigmaI/netI    0.0600
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            9776
_diffrn_reflns_theta_full        27.46
_diffrn_reflns_theta_max         27.46
_diffrn_reflns_theta_min         1.51
_exptl_absorpt_coefficient_mu    0.060
_exptl_crystal_colour            white
_exptl_crystal_density_diffrn    0.324
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       cubic
_exptl_crystal_F_000             268
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.495
_refine_diff_density_min         -0.608
_refine_diff_density_rms         0.193
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.142
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     319
_refine_ls_number_reflns         5816
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.142
_refine_ls_R_factor_all          0.1211
_refine_ls_R_factor_gt           0.0658
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1109P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1686
_refine_ls_wR_factor_ref         0.2152
_reflns_number_gt                3508
_reflns_number_total             5816
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo061254rsi20060620_095210.cif
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4022130