Synthetic Study of Dragmacidin E: Construction of the Core Structure Using Pd-Catalyzed Cascade Cyclization and Rh-Catalyzed Aminoacetoxylation.
Inoue, Naoya; Nakano, Shun-Ichi; Harada, Shingo; Hamada, Yasumasa; Nemoto, Tetsuhiro; The Journal of organic chemistry 82 (2017) 2787–2793; doi:10.1021/acs.joc.7b00083

data_4032200
_publ_section_title
;
 Synthetic Study of Dragmacidin E: Construction of the Core Structure
 Using Pd-Catalyzed Cascade Cyclization and Rh-Catalyzed
 Aminoacetoxylation.
;
_journal_issue                   5
_journal_name_full               'The Journal of organic chemistry'
_journal_page_first              2787
_journal_page_last               2793
_journal_paper_doi               10.1021/acs.joc.7b00083
_journal_volume                  82
_journal_year                    2017
_chemical_formula_moiety         'C26 H28 N6 O6 S, C4 H8 O2'
_chemical_formula_sum            'C30 H36 N6 O8 S'
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_space_group_name_Hall           '-P 2ybc'
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_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
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_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.0000
_cell_angle_beta                 99.3754(17)
_cell_angle_gamma                90.0000
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_cell_length_b                   19.2205(5)
_cell_length_c                   9.7931(3)
_cell_measurement_reflns_used    21533
_cell_measurement_temperature    93
_cell_measurement_theta_max      68.28
_cell_measurement_theta_min      3.50
_cell_volume                     3153.57(16)
_computing_cell_refinement       'RAPID AUTO'
_computing_data_collection       'RAPID AUTO (Rigaku, ????)'
_computing_data_reduction        'RAPID AUTO'
_computing_molecular_graphics    'CrystalStructure 4.2.2'
_computing_publication_material  'CrystalStructure 4.2.2 (Rigaku, 2016)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'Il Milione (Burla, et al., 2007)'
_diffrn_ambient_temperature      93
_diffrn_detector_area_resol_mean 10.000
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Cu K\a'
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_diffrn_reflns_av_R_equivalents  0.1178
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_diffrn_reflns_limit_h_max       20
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_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
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_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            32833
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_diffrn_reflns_theta_max         68.250
_diffrn_reflns_theta_min         3.500
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_exptl_absorpt_correction_T_min  0.548
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSCOR (Rigaku, 1995)'
_exptl_crystal_colour            colorless
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_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
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_refine_ls_extinction_method     none
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_refine_ls_number_reflns         5749
_refine_ls_number_restraints     0
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_refine_ls_R_factor_gt           0.0714
_refine_ls_shift/su_max          0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0619P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1451
_refine_ls_wR_factor_ref         0.1556
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_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            jo7b00083_si_002.cif
_cod_data_source_block           sh161130inoue2
_cod_depositor_comments          'Adding full bibliography for 4032200.cif.'
_cod_original_cell_volume        3153.57(15)
_cod_database_code               4032200