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_4104749
_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 syn
_chemical_formula_moiety         'C28 H29 Cl N2 O8'
_chemical_formula_sum            'C28 H29 Cl N2 O8'
_chemical_formula_weight         557.00
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      15
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_cell_angle_alpha                90.0000
_cell_angle_beta                 125.6197(11)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            8
_cell_length_a                   28.0108(10)
_cell_length_b                   12.6124(2)
_cell_length_c                   18.5089(6)
_cell_measurement_reflns_used    40898
_cell_measurement_temperature    80.1
_cell_measurement_theta_max      72.1
_cell_measurement_theta_min      1.8
_cell_volume                     5315.5(3)
_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    SIR92
_diffrn_ambient_temperature      80
_diffrn_detector_area_resol_mean 10.00
_diffrn_measured_fraction_theta_full 0.954
_diffrn_measured_fraction_theta_max 0.954
_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  0.063
_diffrn_reflns_limit_h_max       38
_diffrn_reflns_limit_h_min       -38
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            26379
_diffrn_reflns_theta_full        30.54
_diffrn_reflns_theta_max         30.54
_diffrn_source                   'rotating anode'
_diffrn_source_type              'Rigaku MM-007HF'
_exptl_absorpt_coefficient_mu    0.198
_exptl_absorpt_correction_T_max  0.961
_exptl_absorpt_correction_T_min  0.799
_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    1.392
_exptl_crystal_description       prism
_exptl_crystal_F_000             2336.00
_exptl_crystal_recrystallization_method 'dichloromethane, hexane'
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         67.70
_refine_diff_density_min         -8.52
_refine_ls_extinction_coef       -36(6)
_refine_ls_extinction_method
'Larson (1970) Crystallographic Computing eq. 22'
_refine_ls_goodness_of_fit_ref   3.837
_refine_ls_hydrogen_treatment    mixed
_refine_ls_number_parameters     492
_refine_ls_number_reflns         15621
_refine_ls_R_factor_gt           0.0818
_refine_ls_shift/su_max          0.0000
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 1.0'
_refine_ls_weighting_scheme      unit
_refine_ls_wR_factor_ref         0.0825
_reflns_number_gt                15397
_reflns_number_total             7755
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            ja902939t_si_003.cif
_cod_data_source_block           '__SYP_131008_21'
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4104749