<i>S</i>-Bridged Thioether and Structure-Diversified Angucyclinone Derivatives from the South China Sea-Derived <i>Micromonospora echinospora</i> SCSIO 04089.
Fang, Zhuangjie; Jiang, Xiaodong; Zhang, Qingbo; Zhang, Liping; Zhang, Wenjun; Yang, Chunfang; Zhang, Haibo; Zhu, Yiguang; Zhang, Changsheng; Journal of natural products  (2020) –; doi:10.1021/acs.jnatprod.0c00719

data_1559202
_publ_section_title
;
 <i>S</i>-Bridged Thioether and Structure-Diversified Angucyclinone
 Derivatives from the South China Sea-Derived <i>Micromonospora
 echinospora</i> SCSIO 04089.
;
_journal_name_full               'Journal of natural products'
_journal_paper_doi               10.1021/acs.jnatprod.0c00719
_journal_year                    2020
_chemical_formula_moiety         'C20 H16 O7'
_chemical_formula_sum            'C20 H16 O7'
_chemical_formula_weight         368.33
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2020-04-16
_audit_creation_method
;
Olex2 1.3
(compiled 2020.02.04 svn.rd84adfe8 for OlexSys, GUI svn.r6032)
;
_cell_angle_alpha                90
_cell_angle_beta                 102.198(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.4014(3)
_cell_length_b                   9.5711(3)
_cell_length_c                   19.3229(5)
_cell_measurement_reflns_used    3879
_cell_measurement_temperature    99.9(6)
_cell_measurement_theta_max      73.6120
_cell_measurement_theta_min      4.6900
_cell_volume                     1699.45(9)
_computing_cell_refinement       'CrysAlisPro 1.171.39.33c (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.33c (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.33c (Rigaku OD, 2017)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine 1.3 (Bourhis et al., 2015)'
_computing_structure_solution    'olex2.solve 1.3 (Bourhis et al., 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      99.9(6)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.964
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
--------------------------------------------------------------------------
  1  \w    -27.00   6.00   0.50    1.50    --    0.00 -82.00  30.00   66
  2  \w    -23.00  29.00   0.50    1.50    --    0.00 -82.00 -30.00  104
  3  \w    -11.00  16.00   0.50    1.50    --    0.00  38.00  90.00   54
  4  \w     31.00  87.00   0.50    1.50    --    0.00  38.00  90.00  112
  5  \w    -33.00   0.00   0.50    1.50    --    0.00 -82.00-150.00   66
  6  \w      7.00  99.00   0.50    5.00    --   95.20 -45.00 -90.00  184
  7  \w      6.00  55.00   0.50    5.00    --   95.20 -45.00-120.00   98
  8  \w     82.00 108.00   0.50    5.00    --   95.20  30.00-150.00   52
  9  \w    121.00 168.00   0.50    5.00    --   95.20  30.00-150.00   94
 10  \w     23.00  89.00   0.50    5.00    --   95.20 -30.00 120.00  132
 11  \w     17.00 127.00   0.50    5.00    --   95.20 -82.00  60.00  220
 12  \w     16.00  90.00   0.50    5.00    --   95.20 -30.00 -90.00  148
 13  \w     37.00 116.00   0.50    5.00    --   95.20 -15.00  30.00  158
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa single'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0642209000
_diffrn_orient_matrix_UB_12      -0.0478848000
_diffrn_orient_matrix_UB_13      -0.0763144000
_diffrn_orient_matrix_UB_21      0.1033358000
_diffrn_orient_matrix_UB_22      0.0999692000
_diffrn_orient_matrix_UB_23      -0.0277633000
_diffrn_orient_matrix_UB_31      0.1152374000
_diffrn_orient_matrix_UB_32      -0.1168645000
_diffrn_orient_matrix_UB_33      0.0073919000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0381
_diffrn_reflns_av_unetI/netI     0.0418
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.964
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            8474
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.964
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.235
_diffrn_reflns_theta_min         4.683
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.927
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.58286
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.33c (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear yellowish brown'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.440
_exptl_crystal_description       plate
_exptl_crystal_F_000             768
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.275
_refine_diff_density_min         -0.300
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     249
_refine_ls_number_reflns         3335
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.075
_refine_ls_R_factor_all          0.0551
_refine_ls_R_factor_gt           0.0478
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0877P)^2^+0.2859P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1342
_refine_ls_wR_factor_ref         0.1400
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2844
_reflns_number_total             3335
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            np0c00719_si_006.cif
_cod_data_source_block           fangzhuangjie_29t-0_collect
_cod_database_code               1559202
_shelx_shelxl_version_number     2018/1
_chemical_oxdiff_formula         'C80 H64 O28 '
_reflns_odcompleteness_completeness 99.85
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2.a Secondary CH2 refined with riding coordinates:
 C22(H22A,H22B)
2.b Aromatic/amide H refined with riding coordinates:
 C15(H15), C8(H8), C13(H13), C7(H7), C6(H6)
2.c Idealised Me refined as rotating group:
 C19(H19A,H19B,H19C), C23(H23A,H23B,H23C)
2.d Idealised tetrahedral OH refined as rotating group:
 O27(H27), O21(H21), O26(H26)
;
_shelx_res_checksum              34699
_shelx_hkl_checksum              98786
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.077
_oxdiff_exptl_absorpt_empirical_full_min 0.625