<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_1559198
_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 H14 O5'
_chemical_formula_sum            'C20 H14 O5'
_chemical_formula_weight         334.31
_space_group_crystal_system      orthorhombic
_space_group_IT_number           56
_space_group_name_Hall           '-P 2ab 2ac'
_space_group_name_H-M_alt        'P c c n'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2020-08-31
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   22.7722(9)
_cell_length_b                   21.0367(12)
_cell_length_c                   6.7533(3)
_cell_measurement_reflns_used    2383
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      73.1380
_cell_measurement_theta_min      5.7110
_cell_volume                     3235.2(3)
_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 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.00(10)
_diffrn_measured_fraction_theta_full 0.992
_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  11.15   0.35    8.00    --    0.00 -77.00 150.00  109
  2  \w    -32.00  18.05   0.35    8.00    --    0.00 -82.00 120.00  143
  3  \w    -32.00  29.25   0.35    8.00    --    0.00 -82.00-180.00  175
  4  \w      6.00 107.15   0.35   50.00    --   94.60 -30.00   0.00  289
  5  \w    148.00 177.75   0.35   50.00    --   94.60  82.00-120.00   85
  6  \w     91.00 129.15   0.35   50.00    --   94.60  82.00-120.00  109
  7  \w      5.00  32.30   0.35   50.00    --   94.60 -15.00   0.00   78
  8  \w      6.00 109.25   0.35   50.00    --   94.60 -30.00 120.00  295
  9  \w      5.00  77.10   0.35   50.00    --   94.60 -61.00   0.00  206
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa single'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0653
_diffrn_reflns_av_unetI/netI     0.0787
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.964
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            10668
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.964
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.948
_diffrn_reflns_theta_min         3.882
_exptl_absorpt_coefficient_mu    0.823
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.51866
_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            'dark red'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.373
_exptl_crystal_description       needle
_exptl_crystal_F_000             1392
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.252
_refine_diff_density_min         -0.288
_refine_diff_density_rms         0.062
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     230
_refine_ls_number_reflns         3175
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0901
_refine_ls_R_factor_gt           0.0609
_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^)+(0.1022P)^2^+0.1348P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1687
_refine_ls_wR_factor_ref         0.1896
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2097
_reflns_number_total             3175
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            np0c00719_si_008.cif
_cod_data_source_block           fangzhuangjie_29t-8_collect
_cod_database_code               1559198
_shelx_shelxl_version_number     2018/1
_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:
 C21(H21a,H21b)
2.b Aromatic/amide H refined with riding coordinates:
 C12(H12), C5(H5), C16(H16), C14(H14), C7(H7), C6(H6)
2.c Idealised Me refined as rotating group:
 C22(H22a,H22b,H22c)
2.d Idealised tetrahedral OH refined as rotating group:
 O20(H20), O24(H24), O19(H19)
;
_shelx_res_checksum              55398
_shelx_hkl_checksum              7889
_shelx_fab_checksum              74717
_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
;