Short Total Synthesis of (+)-Madindolines A and B
Hirose, Tomoyasu; Sunazuka, Toshiaki; Shirahata, Tatsuya; Yamamoto, Daisuke; Harigaya, Yoshihiro; Kuwajima, Isao; Ōmura, Satoshi; Organic Letters 4 (2002) 501–; doi:10.1021/ol017058i

data_1507434
_publ_section_title
;
 Short Total Synthesis of (+)-Madindolines A and B
;
_journal_issue                   4
_journal_name_full               'Organic Letters'
_journal_page_first              501
_journal_paper_doi               10.1021/ol017058i
_journal_volume                  4
_journal_year                    2002
_chemical_formula_moiety         'C22 H27 N O4 '
_chemical_formula_sum            'C22 H27 N O4'
_chemical_formula_weight         369.46
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      4
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_cell_angle_alpha                90
_cell_angle_beta                 91.30(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   7.639(4)
_cell_length_b                   9.002(4)
_cell_length_c                   14.719(3)
_cell_measurement_reflns_used    20
_cell_measurement_temperature    296.2
_cell_measurement_theta_max      29.2
_cell_measurement_theta_min      28.2
_cell_volume                     1011.9(7)
_computing_cell_refinement       'MSC/AFC Diffractometer Control'
_computing_data_collection       'MSC/AFC Diffractometer Control'
_computing_data_reduction        'teXsan Ver. 1.10'
_computing_publication_material  'teXsan Ver. 1.10'
_computing_structure_refinement  'teXsan Ver. 1.10'
_computing_structure_solution    SHELXS97
_diffrn_measured_fraction_theta_full 0.9678
_diffrn_measured_fraction_theta_max 0.9678
_diffrn_measurement_device_type  'Rigaku AFC5R'
_diffrn_measurement_method       \w-2\q
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.024
_diffrn_reflns_limit_h_max       0
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            2050
_diffrn_reflns_theta_full        67.63
_diffrn_reflns_theta_max         67.63
_diffrn_standards_decay_%        0.08
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.670
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.213
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.200
_refine_diff_density_max         0.40
_refine_diff_density_min         -0.32
_refine_ls_abs_structure_Flack   4.86645
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   4.573
_refine_ls_hydrogen_treatment    noref
_refine_ls_number_parameters     245
_refine_ls_number_reflns         1098
_refine_ls_R_factor_gt           0.0981
_refine_ls_shift/su_max          2.1344
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^) + (0.00100(Max(Fo^2^,0) + 2Fc^2^)/3)^2^]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.1207
_reflns_number_gt                1098
_reflns_number_total             1894
_reflns_threshold_expression     F^2^>3.0\s(F^2^)
_cod_data_source_file            ol017058i_s2.cif
_cod_data_source_block           mdlb-2
_cod_original_cell_volume        1011.8(6)
_cod_original_formula_sum        'C22 H27 N O4 '
_cod_database_code               1507434