Viridicatumtoxins: Expanding on a Rare Tetracycline Antibiotic Scaffold.
Shang, Zhuo; Salim, Angela A.; Khalil, Zeinab; Quezada, Michelle; Bernhardt, Paul V.; Capon, Robert J.; The Journal of organic chemistry 80 (2015) 12501–12508; doi:10.1021/acs.joc.5b02367

data_4031757
_publ_section_title
;
 Viridicatumtoxins: Expanding on a Rare Tetracycline Antibiotic Scaffold.
;
_journal_issue                   24
_journal_name_full               'The Journal of organic chemistry'
_journal_page_first              12501
_journal_page_last               12508
_journal_paper_doi               10.1021/acs.joc.5b02367
_journal_volume                  80
_journal_year                    2015
_chemical_absolute_configuration ad
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C30 H31 N1 O10, 2(C H4 O),0.5(H2 O)'
_chemical_formula_sum            'C32 H40 N O12.5'
_chemical_formula_weight         638.65
_space_group_IT_number           5
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      5
_symmetry_space_group_name_Hall  'C 2y'
_symmetry_space_group_name_H-M   'C 1 2 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.4
_audit_creation_date             2014-12-05T12:53:44-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 105.700(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   30.1333(7)
_cell_length_b                   7.7644(2)
_cell_length_c                   12.9297(3)
_cell_measurement_reflns_used    10134
_cell_measurement_temperature    190(2)
_cell_measurement_theta_max      62.37
_cell_measurement_theta_min      4.021
_cell_measurement_wavelength     1.54184
_cell_volume                     2912.26(13)
_computing_cell_refinement
;
        Department of Chemistry
        University of Anywhere
        Sometown
        Somewhere, UK
;
_computing_data_collection
;
        Department of Chemistry
        University of Anywhere
        Sometown
        Somewhere, UK
;
_computing_data_reduction
;
        Department of Chemistry
        University of Anywhere
        Sometown
        Somewhere, UK
;
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR92 (Giacovazzo et al, 1993)'
_diffrn_ambient_temperature      190(2)
_diffrn_detector_area_resol_mean 16.0696
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0509593
_diffrn_orient_matrix_UB_12      -0.0050097
_diffrn_orient_matrix_UB_13      0.0655929
_diffrn_orient_matrix_UB_21      0.0114797
_diffrn_orient_matrix_UB_22      -0.1137773
_diffrn_orient_matrix_UB_23      -0.0869479
_diffrn_orient_matrix_UB_31      0.0095832
_diffrn_orient_matrix_UB_32      0.1624358
_diffrn_orient_matrix_UB_33      -0.0588355
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0413
_diffrn_reflns_av_unetI/netI     0.0357
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            16514
_diffrn_reflns_theta_full        62.46
_diffrn_reflns_theta_max         62.46
_diffrn_reflns_theta_min         3.55
_exptl_absorpt_coefficient_mu    0.944
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.60316
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
        Department of Chemistry
        University of Anywhere
        Sometown
        Somewhere, UK
;
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_density_diffrn    1.457
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1356
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.488
_refine_diff_density_min         -0.694
_refine_diff_density_rms         0.061
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.05(19)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     417
_refine_ls_number_reflns         4539
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.069
_refine_ls_R_factor_all          0.0484
_refine_ls_R_factor_gt           0.0466
_refine_ls_shift/su_max          0.011
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0970P)^2^+1.5867P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1326
_refine_ls_wR_factor_ref         0.1348
_reflns_number_gt                4334
_reflns_number_total             4539
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            jo5b02367_si_001.cif
_cod_data_source_block           1257rc2
_cod_depositor_comments          'Adding full bibliography for 4031757.cif.'
_cod_original_cell_volume        2912.26(12)
_cod_original_formula_sum        'C32 H40 N O12.50'
_cod_database_code               4031757