Total Synthesis of Cortistatins A and J
Shuji Yamashita; Kentaro Iso; Kazuki Kitajima; Masafumi Himuro; Masahiro Hirama; Journal of Organic Chemistry 76 (2011) 2408–2425; doi:10.1021/jo2002616

data_4026224
_publ_section_title
;
 Total Synthesis of Cortistatins A and J
;
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              2408
_journal_page_last               2425
_journal_paper_doi               10.1021/jo2002616
_journal_volume                  76
_journal_year                    2011
_chemical_absolute_configuration 'CHOOSE rm ad rmad syn or unk'
_chemical_formula_moiety         'C26 H27 Br O4 '
_chemical_formula_sum            'C26 H27 Br O4'
_chemical_formula_weight         483.40
_space_group_IT_number           5
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      5
_symmetry_space_group_name_Hall  'C 2y'
_symmetry_space_group_name_H-M   'C 1 2 1'
_cell_angle_alpha                90.0000
_cell_angle_beta                 92.777(11)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            4
_cell_length_a                   21.235(17)
_cell_length_b                   8.271(7)
_cell_length_c                   13.904(11)
_cell_measurement_reflns_used    3628
_cell_measurement_temperature    173.1
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.0
_cell_volume                     2439(3)
_computing_cell_refinement       CrystalClear
_computing_data_collection       CrystalClear
_computing_data_reduction        CrystalStructure
_computing_publication_material  'CrystalStructure 3.8'
_computing_structure_refinement  CRYSTALS
_computing_structure_solution    SHELXS97
_diffrn_detector_area_resol_mean 7.31
_diffrn_measured_fraction_theta_full 0.978
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measurement_device_type  'Rigaku Saturn'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.052
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            17216
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_exptl_absorpt_coefficient_mu    1.718
_exptl_absorpt_correction_T_max  0.918
_exptl_absorpt_correction_T_min  0.751
_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    1.316
_exptl_crystal_description       prism
_exptl_crystal_F_000             1000.00
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.05
_refine_diff_density_max         3.03
_refine_diff_density_min         -0.94
_refine_ls_abs_structure_details
'Flack, H. D. (1983), Acta Cryst. A39, 876-881.  2528 Friedel Pairs'
_refine_ls_abs_structure_Flack   0.006(19)
_refine_ls_extinction_coef       446(44)
_refine_ls_extinction_method
'Larson (1970) Crystallographic Computing eq. 22'
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_hydrogen_treatment    refall
_refine_ls_number_parameters     309
_refine_ls_number_reflns         5457
_refine_ls_R_factor_gt           0.0687
_refine_ls_shift/su_max          0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[0.0012Fo^2^ + 1.0000\s(Fo^2^)]/(4Fo^2^)'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.1967
_reflns_number_gt                2539
_reflns_number_total             5457
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            jo2002616_si_001.cif
_cod_data_source_block           '__a'
_cod_original_formula_sum        'C26 H27 Br O4 '
_cod_database_code               4026224