Total Synthesis and Biological Evaluation of Cortistatins A and J and Analogues Thereof
K. C. Nicolaou; Xiao-Shui Peng; Ya-Ping Sun; Damien Polet; Bin Zou; Chek Shik Lim; David Y.-K. Chen; Journal of the American Chemical Society 131 (2009) 10587–10597; doi:10.1021/ja902939t

data_4104751
_publ_section_title
;
 Total Synthesis and Biological Evaluation of Cortistatins A and J and
 Analogues Thereof
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              10587
_journal_page_last               10597
_journal_paper_doi               10.1021/ja902939t
_journal_volume                  131
_journal_year                    2009
_chemical_absolute_configuration unk
_chemical_formula_moiety         'C15 H18 O3'
_chemical_formula_sum            'C15 H18 O3'
_chemical_formula_weight         246.31
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_cell_angle_alpha                90.0000
_cell_angle_beta                 108.844(3)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            3
_cell_length_a                   11.7346(7)
_cell_length_b                   9.0075(4)
_cell_length_c                   11.8751(8)
_cell_measurement_reflns_used    22079
_cell_measurement_temperature    93.1
_cell_measurement_theta_max      72.1
_cell_measurement_theta_min      1.8
_cell_volume                     1187.91(12)
_computing_cell_refinement       PROCESS
_computing_data_collection       PROCESS
_computing_data_reduction        CrystalStructure
_computing_publication_material  'CrystalStructure 3.8'
_computing_structure_refinement  CRYSTALS
_computing_structure_solution    SHELXS97
_diffrn_ambient_temperature      93
_diffrn_detector_area_resol_mean 10.00
_diffrn_measured_fraction_theta_full 0.898
_diffrn_measured_fraction_theta_max 0.898
_diffrn_measurement_device_type  'Rigaku RAXIS-SPIDER'
_diffrn_measurement_method       \w
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.099
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            32091
_diffrn_reflns_theta_full        55.73
_diffrn_reflns_theta_max         55.73
_diffrn_source                   'rotating anode'
_diffrn_source_type              'Rigaku MM-007HF'
_exptl_absorpt_coefficient_mu    0.071
_exptl_absorpt_correction_T_max  0.986
_exptl_absorpt_correction_T_min  0.979
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
    Higashi, T. (1999). Program for Absorption Correction.
    Rigaku Corporation, Tokyo, Japan.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.033
_exptl_crystal_description       prism
_exptl_crystal_F_000             396.00
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.58
_exptl_crystal_size_min          0.60
_refine_diff_density_max         102.00
_refine_diff_density_min         -10.10
_refine_ls_extinction_coef       40(4)
_refine_ls_extinction_method
'Larson (1970) Crystallographic Computing eq. 22'
_refine_ls_goodness_of_fit_ref   6.121
_refine_ls_hydrogen_treatment    refall
_refine_ls_number_parameters     362
_refine_ls_number_reflns         16663
_refine_ls_R_factor_gt           0.0725
_refine_ls_shift/su_max          2.4823
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 1.0'
_refine_ls_weighting_scheme      unit
_refine_ls_wR_factor_ref         0.0778
_reflns_number_gt                16255
_reflns_number_total             14061
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            ja902939t_si_005.cif
_cod_data_source_block           '__SYP_131008'
_cod_original_cell_volume        1187.92(12)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4104751