Anti-glioma trichobamide A with an unprecedented tetrahydro-5H-furo[2,3-b]pyrrol-5-one functionality from ascidian-derived fungus Trichobotrys effuse 4729
Chen, Senhua; Shen, Hongjie; Zhang, Panpan; Cheng, Hongwei; Dai, Xingliang; Liu, Lan; Chemical Communications  (2019) –; doi:10.1039/C8CC08970A

data_7122773
_publ_section_title
;
 Anti-glioma trichobamide A with an unprecedented
 tetrahydro-5H-furo[2,3-b]pyrrol-5-one functionality from ascidian-derived
 fungus Trichobotrys effuse 4729
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/C8CC08970A
_journal_year                    2019
_chemical_absolute_configuration ad
_chemical_compound_source        'Ascidian-derived fungi'
_chemical_formula_moiety         'C H Cl3, C35 H41 N O5'
_chemical_formula_sum            'C36 H42 Cl3 N O5'
_chemical_formula_weight         675.06
_chemical_name_systematic        'Compound 1'
_space_group_crystal_system      orthorhombic
_space_group_IT_number           18
_space_group_name_Hall           'P 2 2ab'
_space_group_name_H-M_alt        'P 21 21 2'
_symmetry_space_group_name_Hall  'P 2 2ab'
_symmetry_space_group_name_H-M   'P 21 21 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2018-03-13
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2018-03-14 deposited with the CCDC.
2019-01-08 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.04610(10)
_cell_length_b                   28.6830(2)
_cell_length_c                   7.87240(10)
_cell_measurement_reflns_used    17666
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      73.7240
_cell_measurement_theta_min      4.2370
_cell_volume                     3397.47(5)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'SIR2004 (Burla et al., 2007)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'multiwire proportional'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0542
_diffrn_reflns_av_unetI/netI     0.0369
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            25248
_diffrn_reflns_theta_full        74.12
_diffrn_reflns_theta_max         74.12
_diffrn_reflns_theta_min         3.32
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    2.788
_exptl_absorpt_correction_T_max  0.8506
_exptl_absorpt_correction_T_min  0.2139
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.320
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1424
_exptl_crystal_recrystallization_method 'Vapour deposition'
_exptl_crystal_size_max          0.8
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.594
_refine_diff_density_min         -0.538
_refine_diff_density_rms         0.052
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.005(13)
_refine_ls_extinction_coef       0.00086(14)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     420
_refine_ls_number_reflns         6774
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0439
_refine_ls_R_factor_gt           0.0424
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0641P)^2^+1.4806P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1118
_refine_ls_wR_factor_ref         0.1137
_reflns_number_gt                6540
_reflns_number_total             6774
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c8cc08970a2.cif
_cod_data_source_block           aa
_cod_database_code               7122773
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C1'(H1'), C17(H17), C12(H12), C13(H13), C9(H9), C15(H15), C6(H6), C18(H18),
 C14(H14), C11(H11), C3(H3)
2.b Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B), C10(H10A,H10B), C25(H25A,H25B)
2.c Aromatic/amide H refined with riding coordinates:
 N1(H1), C31(H31), C4(H4), C22(H22), C28(H28), C30(H30), C2(H2), C27(H27)
2.d Idealised Me refined as rotating group:
 C34(H34A,H34B,H34C), C32(H32A,H32B,H32C), C33(H33A,H33B,H33C), C35(H35A,H35B,
 H35C), C21(H21A,H21B,H21C)
;
_olex2_submission_special_instructions 'No special instructions were received'