Structure Revision of Circumdatins A and B, Benzodiazepine Alkaloids Produced by Marine Fungus Aspergillus ostianus, by X-ray Crystallography
Ryuhei Ookura; Keijiro Kito; Takashi Ooi; Michio Namikoshi; Takenori Kusumi; Journal of Organic Chemistry 73 (2008) 4245–4247; doi:10.1021/jo800348d

data_4023446
_publ_section_title
;
 Structure Revision of Circumdatins A and B, Benzodiazepine
 Alkaloids Produced by Marine Fungus Aspergillus ostianus,
 by X-ray Crystallography
;
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              4245
_journal_page_last               4247
_journal_paper_doi               10.1021/jo800348d
_journal_volume                  73
_journal_year                    2008
_chemical_absolute_configuration unk
_chemical_formula_moiety         '2(C20 H17 N3 O4), H2 O '
_chemical_formula_sum            'C40 H36 N6 O9'
_chemical_formula_weight         744.76
_chemical_melting_point_gt       471
_chemical_melting_point_lt       472
_chemical_name_common            'circumdatin B '
_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'
_audit_creation_date             2008-01-26
_audit_creation_method           'by CrystalStructure 3.6.0'
_cell_angle_alpha                90
_cell_angle_beta                 93.195(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.6004(8)
_cell_length_b                   8.4072(6)
_cell_length_c                   21.327(2)
_cell_measurement_reflns_used    10214
_cell_measurement_temperature    173.1
_cell_measurement_theta_max      27.9
_cell_measurement_theta_min      3.1
_cell_volume                     1718.7(2)
_computing_cell_refinement       PROCESS-AUTO
_computing_data_collection       PROCESS-AUTO
_computing_data_reduction        CrystalStructure
_computing_publication_material  'CrystalStructure 3.6.0'
_computing_structure_refinement  CRYSTALS
_computing_structure_solution    SIR97
_diffrn_detector_area_resol_mean 10.00
_diffrn_measured_fraction_theta_full 0.9961
_diffrn_measured_fraction_theta_max 0.9961
_diffrn_measurement_device_type  'Rigaku RAXIS-RAPID'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.089
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            17516
_diffrn_reflns_theta_full        27.87
_diffrn_reflns_theta_max         27.87
_exptl_absorpt_coefficient_mu    0.104
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.439
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             780.00
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.63
_refine_diff_density_min         -0.57
_refine_ls_extinction_coef       21(12)
_refine_ls_extinction_method
'Larson (1970) Crystallographic Computing eq. 22'
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_hydrogen_treatment    refall
_refine_ls_number_parameters     542
_refine_ls_number_reflns         4360
_refine_ls_R_factor_gt           0.0480
_refine_ls_shift/su_max          0.0010
_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         0.1070
_reflns_number_gt                2044
_reflns_number_total             4360
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            jo800348d-File002.cif
_cod_data_source_block           '_compound_2'
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_absolute_configuration' value 'unk ' changed to 'unk'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_original_formula_sum        'C40 H36 N6 O9 '
_cod_database_code               4023446