Cytotoxic trichothecene-type sesquiterpenes from the sponge-derived fungus Stachybotrys chartarum with tyrosine kinase inhibition
Li, Yong; Liu, Dong; Cheng, Zhongbin; Proksch, Peter; Lin, Wenhan; RSC Advances 7 (2017) 7259–; doi:10.1039/C6RA26956G

data_7236280
_publ_section_title
;
 Cytotoxic trichothecene-type sesquiterpenes from the sponge-derived
 fungus Stachybotrys chartarum with tyrosine kinase inhibition
;
_journal_issue                   12
_journal_name_full               'RSC Advances'
_journal_page_first              7259
_journal_paper_doi               10.1039/C6RA26956G
_journal_volume                  7
_journal_year                    2017
_chemical_absolute_configuration unk
_chemical_formula_moiety         'C15 H22 O4'
_chemical_formula_sum            'C15 H22 O4'
_chemical_formula_weight         266.34
_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'
_symmetry_Int_Tables_number      19
_atom_sites_solution_primary     direct
_audit_creation_date             2016-11-11
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2016-11-11 deposited with the CCDC.
2017-01-09 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   6.4486(3)
_cell_length_b                   11.3707(10)
_cell_length_c                   17.7648(15)
_cell_measurement_reflns_used    2202
_cell_measurement_temperature    98.8
_cell_measurement_theta_max      71.5643
_cell_measurement_theta_min      3.8803
_cell_volume                     1302.61(17)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine (Bourhis et al., 2015)'
_computing_structure_solution    'XS (Sheldrick, 2008)'
_diffrn_ambient_temperature      98.8
_diffrn_detector_area_resol_mean 16.0971
_diffrn_measured_fraction_theta_full 0.9819
_diffrn_measured_fraction_theta_max 0.9819
_diffrn_measurement_details
;
  1 omega  -27.00   -1.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  128.0000  -28.0000 26

  2 omega    2.00   28.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   52.0000   94.0000 26

  3 omega  -60.00   26.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      -42.5000   77.0000  -90.0000 86

  4 omega  -20.00   18.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      -42.5000   37.0000    0.0000 38

  5 omega -112.00  -32.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      -42.5000  -52.0000   85.0000 80

  6 omega  -45.00   19.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      -42.5000   37.0000 -150.0000 64

  7 omega   56.00   98.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -45.0000   90.0000 42

  8 omega   91.00  178.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000   45.0000   30.0000 87

  9 omega   59.00  164.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000   15.0000 -180.0000 105

 10 omega   47.00   85.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -45.0000 -150.0000 38

 11 omega   41.00   89.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -45.0000  150.0000 48

 12 omega  112.00  177.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  111.0000  120.0000 65

 13 omega   50.00   82.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -45.0000   60.0000 32
;
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.1414924000
_diffrn_orient_matrix_UB_12      0.0929040000
_diffrn_orient_matrix_UB_13      0.0364829000
_diffrn_orient_matrix_UB_21      0.0557342000
_diffrn_orient_matrix_UB_22      -0.0478711000
_diffrn_orient_matrix_UB_23      0.0784247000
_diffrn_orient_matrix_UB_31      0.1845060000
_diffrn_orient_matrix_UB_32      0.0859673000
_diffrn_orient_matrix_UB_33      0.0042630000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0191
_diffrn_reflns_av_unetI/netI     0.0324
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            4098
_diffrn_reflns_theta_full        71.8036
_diffrn_reflns_theta_max         71.80
_diffrn_reflns_theta_min         4.62
_diffrn_source                   'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.792
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.92921
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    1.3580
_exptl_crystal_F_000             577.9299
_exptl_crystal_recrystallization_method 'Vapour deposition'
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.3969
_refine_diff_density_min         -0.2546
_refine_diff_density_rms         0.0536
_refine_ls_abs_structure_details
'Flack, H. D. (1983). Acta Cryst. A39, 876-881.'
_refine_ls_abs_structure_Flack   0.2(2)
_refine_ls_d_res_high            0.8115
_refine_ls_d_res_low             9.5769
_refine_ls_goodness_of_fit_ref   1.0502
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    34
_refine_ls_number_parameters     176
_refine_ls_number_reflns         2490
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0502
_refine_ls_R_factor_all          0.0419
_refine_ls_R_factor_gt           0.0404
_refine_ls_shift/su_max          0.0002
_refine_ls_shift/su_mean         0.0001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0682P)^2^+0.2180P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1036
_refine_ls_wR_factor_ref         0.1049
_reflns_Friedel_coverage         0.970
_reflns_limit_h_max              7
_reflns_limit_h_min              -7
_reflns_limit_k_max              13
_reflns_limit_k_min              -13
_reflns_limit_l_max              21
_reflns_limit_l_min              -21
_reflns_number_gt                2391
_reflns_number_total             2490
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            c6ra26956g2.cif
_cod_data_source_block           exp_1485
_cod_original_sg_symbol_Hall     ' P 2ac 2ab'
_cod_database_code               7236280
_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
2.a Ternary CH refined with riding coordinates:
 C11(H11), C9(H9)
2.b Secondary CH2 refined with riding coordinates:
 C3(H3a,H3b), C5(H5a,H5b), C15(H15a,H15b), C10(H10a,H10b)
2.c Aromatic/amide H refined with riding coordinates:
 C1(H1)
2.d Idealised Me refined as rotating group:
 C14(H14a,H14b,H14c), C13(H13a,H13b,H13c), C12(H12a,H12b,H12c)
2.e Idealised tetrahedral OH refined as rotating group:
 O3(H3), O4(H4)
;
_olex2_submission_special_instructions 'No special instructions were received'