Concise synthesis of the oxapentacyclic core of cortistatin A.
Yu, Fangmiao; Li, Guozhi; Gao, Peng; Gong, Hongju; Liu, Yinghua; Wu, Yongming; Cheng, Bin; Zhai, Hongbin; Organic letters 12 (2010) 5135–5137; doi:10.1021/ol102058f

data_1503258
_publ_section_title
;
 Concise synthesis of the oxapentacyclic core of cortistatin A.
;
_journal_issue                   22
_journal_name_full               'Organic letters'
_journal_page_first              5135
_journal_page_last               5137
_journal_paper_doi               10.1021/ol102058f
_journal_volume                  12
_journal_year                    2010
_chemical_formula_sum            'C21 H28 O5'
_chemical_formula_weight         360.43
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                94.782(2)
_cell_angle_beta                 107.021(2)
_cell_angle_gamma                102.586(2)
_cell_formula_units_Z            2
_cell_length_a                   7.3454(9)
_cell_length_b                   10.6476(13)
_cell_length_c                   12.4508(16)
_cell_measurement_reflns_used    2067
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      54.093
_cell_measurement_theta_min      5.666
_cell_volume                     897.39(19)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0930
_diffrn_reflns_av_sigmaI/netI    0.0754
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            4714
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         25.50
_diffrn_reflns_theta_min         1.98
_exptl_absorpt_coefficient_mu    0.094
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.18072
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.334
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             388
_exptl_crystal_size_max          0.408
_exptl_crystal_size_mid          0.364
_exptl_crystal_size_min          0.195
_refine_diff_density_max         0.326
_refine_diff_density_min         -0.298
_refine_diff_density_rms         0.065
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.991
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     238
_refine_ls_number_reflns         3285
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.991
_refine_ls_R_factor_all          0.0691
_refine_ls_R_factor_gt           0.0561
_refine_ls_shift/su_max          0.028
_refine_ls_shift/su_mean         0.005
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0979P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1515
_refine_ls_wR_factor_ref         0.1596
_reflns_number_gt                2513
_reflns_number_total             3285
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ol102058f_si_002.cif
_cod_data_source_block           cd201365
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               1503258