Fusidane-Type Antibiotics from the Marine-Derived Fungus <i>Simplicillium</i> sp. SCSIO 41513.
Cheng, Xia; Liang, Xiao; Yao, Fei-Hua; Liu, Xiao-Bo; Qi, Shu-Hua; Journal of natural products 84 (2021) 2945–2952; doi:10.1021/acs.jnatprod.1c00776

data_1565514
_publ_section_title
;
 Fusidane-Type Antibiotics from the Marine-Derived Fungus
 <i>Simplicillium</i> sp. SCSIO 41513.
;
_journal_issue                   11
_journal_name_full               'Journal of natural products'
_journal_page_first              2945
_journal_page_last               2952
_journal_paper_doi               10.1021/acs.jnatprod.1c00776
_journal_volume                  84
_journal_year                    2021
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C29 H42 O7, 2(H2 O)'
_chemical_formula_sum            'C29 H46 O9'
_chemical_formula_weight         538.66
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2020-06-15
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-04-30 deposited with the CCDC.	2021-06-16 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.1557(2)
_cell_length_b                   13.7018(3)
_cell_length_c                   27.1770(7)
_cell_measurement_reflns_used    7014
_cell_measurement_temperature    105.9(5)
_cell_measurement_theta_max      74.2360
_cell_measurement_theta_min      3.2510
_cell_volume                     2664.60(12)
_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_environment      N~2~
_diffrn_ambient_temperature      105.9(5)
_diffrn_detector                 'Pilatus3R 200K-A'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.981
_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    -14.00  31.00   0.50    1.03    --    0.00 -82.00 -60.00   90
  2  \w    -15.00  35.00   0.50    1.03    --    0.00  29.00  33.74  100
  3  \w     44.00  79.00   0.50    1.03    --   32.00  75.00-119.70   70
  4  \w     47.00 119.00   0.50    4.12    --   95.80 -61.00-120.00  144
  5  \w     10.00  37.00   0.50    4.12    --   95.80 -61.00 -30.00   54
  6  \w     46.00  72.00   0.50    4.12    --   95.80 -61.00 -30.00   52
  7  \w    134.00 185.00   0.50    4.12    --   95.80  61.00  60.00  102
  8  \w     51.00 117.00   0.50    4.12    --   95.80 -77.00 -90.00  132
  9  \w     75.00 185.00   0.50    4.12    --   95.80  15.00-180.00  220
 10  \w      7.00  44.00   0.50    4.12    --   95.80 -77.00 -90.00   74
 11  \w      6.00  31.00   0.50    4.12    --   95.80 -61.00-120.00   50
 12  \w     22.00 112.00   0.50    4.12    --   95.80 -15.00   0.00  180
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Pro: Kappa single'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0048367000
_diffrn_orient_matrix_UB_12      -0.0919449000
_diffrn_orient_matrix_UB_13      -0.0326529000
_diffrn_orient_matrix_UB_21      0.0862431000
_diffrn_orient_matrix_UB_22      -0.0584361000
_diffrn_orient_matrix_UB_23      0.0427934000
_diffrn_orient_matrix_UB_31      -0.1970292000
_diffrn_orient_matrix_UB_32      -0.0278497000
_diffrn_orient_matrix_UB_33      0.0178817000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0325
_diffrn_reflns_av_unetI/netI     0.0333
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.981
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            12105
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.963
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.356
_diffrn_reflns_theta_min         3.252
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'MicroMax 007 (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.807
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.55648
_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 light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.343
_exptl_crystal_description       plate
_exptl_crystal_F_000             1168
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.645
_refine_diff_density_min         -0.369
_refine_diff_density_rms         0.071
_refine_ls_abs_structure_details
;
 Flack x determined using 1973 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.04(11)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     361
_refine_ls_number_reflns         5218
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0505
_refine_ls_R_factor_gt           0.0485
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0857P)^2^+1.0600P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1323
_refine_ls_wR_factor_ref         0.1338
_reflns_Friedel_coverage         0.714
_reflns_Friedel_fraction_full    0.995
_reflns_Friedel_fraction_max     0.937
_reflns_number_gt                4924
_reflns_number_total             5218
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            np1c00776_si_003.cif
_cod_data_source_block           chengxia_cx-28_collect
_cod_database_code               1565514
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C112 H168 N12 O28 '
_shelx_estimated_absorpt_t_max   0.984
_shelx_estimated_absorpt_t_min   0.855
_reflns_odcompleteness_completeness 99.93
_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, All O(H,H) groups
2.a Free rotating group:
 O1(H1C,H1D), O2(H2C,H2D)
2.b Ternary CH refined with riding coordinates:
 C13(H13), C7(H7), C9(H9), C4(H4), C16(H16), C5(H5), C3(H3), C11(H11)
2.c Secondary CH2 refined with riding coordinates:
 C22(H22A,H22B), C6(H6A,H6B), C1(H1A,H1B), C23(H23A,H23B), C2(H2A,H2B),
 C15(H15A,H15B), C12(H12A,H12B)
2.d Aromatic/amide H refined with riding coordinates:
 C24(H24)
2.e Idealised Me refined as rotating group:
 C19(H19A,H19B,H19C), C29(H29A,H29B,H29C), C18(H18A,H18B,H18C), C28(H28A,H28B,
 H28C), C26(H26A,H26B,H26C)
2.f Idealised tetrahedral OH refined as rotating group:
 O29(H29), O31(H31), O26(H26)
;
_shelx_res_checksum              86172
_shelx_hkl_checksum              53518
_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 1.651
_oxdiff_exptl_absorpt_empirical_full_min 0.787