Rh-catalyzed cyclization of diynes and enynes initiated by carbonyl-directed activation of aromatic and vinylic C-H bonds.
Tsuchikama, Kyoji; Kuwata, Yusuke; Tahara, Yu-ki; Yoshinami, Yusuke; Shibata, Takanori; Organic letters 9 (2007) 3097–3099; doi:10.1021/ol0711669

data_1516660
_publ_section_title
;
 Rh-catalyzed cyclization of diynes and enynes initiated by
 carbonyl-directed activation of aromatic and vinylic C-H bonds.
;
_journal_issue                   16
_journal_name_full               'Organic letters'
_journal_page_first              3097
_journal_page_last               3099
_journal_paper_doi               10.1021/ol0711669
_journal_volume                  9
_journal_year                    2007
_chemical_formula_moiety         'C28 H27 N O3 S '
_chemical_formula_sum            'C28 H27 N O3 S'
_chemical_formula_weight         457.59
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_cell_angle_alpha                90.0000
_cell_angle_beta                 95.1550(17)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            4
_cell_length_a                   11.1671(6)
_cell_length_b                   16.1513(9)
_cell_length_c                   13.1889(7)
_cell_measurement_reflns_used    17643
_cell_measurement_temperature    123.1
_cell_measurement_theta_max      27.4
_cell_measurement_theta_min      3.1
_cell_volume                     2369.2(2)
_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 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Rigaku RAXIS-RAPID'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.032
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            22720
_diffrn_reflns_theta_full        27.43
_diffrn_reflns_theta_max         27.43
_exptl_absorpt_coefficient_mu    0.167
_exptl_absorpt_correction_T_max  0.905
_exptl_absorpt_correction_T_min  0.721
_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    1.283
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             968.00
_exptl_crystal_size_max          0.80
_exptl_crystal_size_mid          0.60
_exptl_crystal_size_min          0.60
_refine_diff_density_max         0.36
_refine_diff_density_min         -0.31
_refine_ls_extinction_coef       -227(25)
_refine_ls_extinction_method
'Larson (1970) Crystallographic Computing eq. 22'
_refine_ls_goodness_of_fit_ref   0.989
_refine_ls_hydrogen_treatment    refall
_refine_ls_number_parameters     326
_refine_ls_number_reflns         4335
_refine_ls_R_factor_gt           0.0389
_refine_ls_shift/su_max          0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[0.0024Fo^2^ + 1.0000\s(Fo^2^)]/(4Fo^2^)'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.1207
_reflns_number_gt                4311
_reflns_number_total             5395
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            ol0711669si20070518_083738.cif
_cod_data_source_block           '_kama568'
_cod_original_formula_sum        'C28 H27 N O3 S '
_cod_database_code               1516660