Total Synthesis and Structure Revision of the (-)-Maduropeptin Chromophore
Kazuo Komano; Satoshi Shimamura; Yutaro Norizuki; Donglin Zhao; Chizuko Kabuto; Itaru Sato; Masahiro Hirama; Journal of the American Chemical Society 131 (2009) 12072–12073; doi:10.1021/ja905397p

data_4104956
_publ_section_title
;
 Total Synthesis and Structure Revision of the (-)-Maduropeptin
 Chromophore
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              12072
_journal_page_last               12073
_journal_paper_doi               10.1021/ja905397p
_journal_volume                  131
_journal_year                    2009
_chemical_absolute_configuration syn
_chemical_formula_moiety         'C38 H40 Cl N O11 '
_chemical_formula_sum            'C38 H40 Cl N O11'
_chemical_formula_weight         722.19
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      19
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_cell_angle_alpha                90.0000
_cell_angle_beta                 90.0000
_cell_angle_gamma                90.0000
_cell_formula_units_Z            4
_cell_length_a                   8.817(3)
_cell_length_b                   17.774(6)
_cell_length_c                   22.892(8)
_cell_measurement_reflns_used    12831
_cell_measurement_temperature    173.1
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.1
_cell_volume                     3587(2)
_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    SIR92
_diffrn_detector_area_resol_mean 7.31
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_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  0.091
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            55487
_diffrn_reflns_theta_full        27.41
_diffrn_reflns_theta_max         27.41
_exptl_absorpt_coefficient_mu    0.169
_exptl_absorpt_correction_T_max  0.983
_exptl_absorpt_correction_T_min  0.699
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.337
_exptl_crystal_description       needle
_exptl_crystal_F_000             1520.00
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.77
_refine_diff_density_min         -0.80
_refine_ls_abs_structure_details
'Flack, H. D. (1983), Acta Cryst. A39, 876-881.  3514 Friedel Pairs'
_refine_ls_abs_structure_Flack   -0.00(9)
_refine_ls_extinction_coef       79(78)
_refine_ls_extinction_method
'Larson (1970) Crystallographic Computing eq. 22'
_refine_ls_goodness_of_fit_ref   0.901
_refine_ls_hydrogen_treatment    refall
_refine_ls_number_parameters     502
_refine_ls_number_reflns         8044
_refine_ls_R_factor_gt           0.0564
_refine_ls_shift/su_max          0.0196
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     'w = 1/[1.0000\s(Fo^2^)]/(4Fo^2^)'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0762
_reflns_number_gt                3218
_reflns_number_total             8044
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            ja905397p_si_001.cif
_cod_data_source_block           '_komano070227'
_cod_original_cell_volume        3588(2)
_cod_original_formula_sum        'C38 H40 Cl N O11 '
_cod_database_code               4104956