Curtachalasins, immunosuppressive agents from the endophytic fungus Xylaria cf. curta.
Wang, Wen-Xuan; Cheng, Gui-Guang; Li, Zheng-Hui; Ai, Hong-Lian; He, Juan; Li, Jing; Feng, Tao; Liu, Ji-Kai; Organic & biomolecular chemistry 17 (2019) 7985–7994; doi:10.1039/c9ob01552c

data_7157030
_publ_section_title
;
 Curtachalasins, immunosuppressive agents from the endophytic fungus
 Xylaria cf. curta.
;
_journal_issue                   34
_journal_name_full               'Organic &amp; biomolecular chemistry'
_journal_page_first              7985
_journal_page_last               7994
_journal_paper_doi               10.1039/c9ob01552c
_journal_volume                  17
_journal_year                    2019
_chemical_absolute_configuration ad
_chemical_formula_sum            'C31 H40 Cl3 N O9'
_chemical_formula_weight         676.99
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   mixed
_audit_update_record
;
2019-07-08 deposited with the CCDC.    2019-08-07 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 101.5590(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   8.1478(3)
_cell_length_b                   12.7979(4)
_cell_length_c                   15.6927(5)
_cell_measurement_reflns_used    9906
_cell_measurement_temperature    150.(2)
_cell_measurement_theta_max      79.2188
_cell_measurement_theta_min      2.8742
_cell_volume                     1603.17(9)
_computing_cell_refinement       'SAINT V8.38A (Bruker AXS Inc., 2017)'
_computing_data_reduction        'SAINT V8.38A (Bruker AXS Inc., 2017)'
_computing_molecular_graphics    'shelXle (C.B. Huebschle, rev 833)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      150.(2)
_diffrn_detector_area_resol_mean 7.3910
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.1664
_diffrn_reflns_av_unetI/netI     0.0663
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            45142
_diffrn_reflns_theta_full        79.56
_diffrn_reflns_theta_max         79.56
_diffrn_reflns_theta_min         2.87
_exptl_absorpt_coefficient_mu    3.049
_exptl_absorpt_correction_T_max  0.69
_exptl_absorpt_correction_T_min  0.44
_exptl_absorpt_process_details
;
;
_exptl_crystal_colour            'light colourless'
_exptl_crystal_density_diffrn    1.402
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       BLOCK
_exptl_crystal_F_000             712
_exptl_crystal_size_max          0.326
_exptl_crystal_size_mid          0.135
_exptl_crystal_size_min          0.129
_refine_diff_density_max         0.656
_refine_diff_density_min         -0.410
_refine_ls_abs_structure_details
;

Classical Flack method preferred over Parsons because s.u. lower.
;
_refine_ls_abs_structure_Flack   0.05(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.101
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     450
_refine_ls_number_reflns         6825
_refine_ls_number_restraints     88
_refine_ls_restrained_S_all      1.123
_refine_ls_R_factor_all          0.0725
_refine_ls_R_factor_gt           0.0710
_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^)+(0.1083P)^2^+1.0092P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1882
_refine_ls_wR_factor_ref         0.1900
_reflns_number_gt                6590
_reflns_number_total             6825
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9ob01552c2.cif
_cod_data_source_block           LE1094
_cod_depositor_comments
'Adding full bibliography for 7157030--7157031.cif.'
_cod_database_code               7157030
_shelx_res_checksum              3426