Discovery of an Oxepine-Containing Diketopiperazine Derivative Active against Concanavalin A-Induced Hepatitis.
Qi, Changxing; Tan, Xiaosheng; Shi, Zhengyi; Feng, Hao; Sun, Lingjuan; Hu, Zhengxi; Chen, Gang; Zhang, Yonghui; Journal of natural products 83 (2020) 2672–2678; doi:10.1021/acs.jnatprod.0c00558

data_1559007
_publ_section_title
;
 Discovery of an Oxepine-Containing Diketopiperazine Derivative Active
 against Concanavalin A-Induced Hepatitis.
;
_journal_issue                   9
_journal_name_full               'Journal of natural products'
_journal_page_first              2672
_journal_page_last               2678
_journal_paper_doi               10.1021/acs.jnatprod.0c00558
_journal_volume                  83
_journal_year                    2020
_chemical_absolute_configuration ad
_chemical_formula_sum            'C27 H31 N3 O5'
_chemical_formula_weight         477.55
_space_group_crystal_system      monoclinic
_space_group_IT_number           5
_space_group_name_Hall           'C 2y'
_space_group_name_H-M_alt        'C 1 2 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 106.69
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   35.8230(2)
_cell_length_b                   6.493
_cell_length_c                   11.16740(10)
_cell_measurement_reflns_used    24156
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      73.55
_cell_measurement_theta_min      2.572
_cell_volume                     2488.10(3)
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  CCD
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0256
_diffrn_reflns_av_unetI/netI     0.0150
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       44
_diffrn_reflns_limit_h_min       -44
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            29453
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         73.951
_diffrn_reflns_theta_min         2.575
_exptl_absorpt_coefficient_mu    0.721
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.275
_exptl_crystal_description       block
_exptl_crystal_F_000             1016
_exptl_crystal_size_max          0.220
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.180
_exptl_transmission_factor_max   0.864
_exptl_transmission_factor_min   0.864
_refine_diff_density_max         0.131
_refine_diff_density_min         -0.196
_refine_diff_density_rms         0.037
_refine_ls_abs_structure_details
;
 Flack x determined using 2160 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.06(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     320
_refine_ls_number_reflns         4920
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0254
_refine_ls_R_factor_gt           0.0252
_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^)+(0.0388P)^2^+0.7225P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0665
_refine_ls_wR_factor_ref         0.0666
_reflns_Friedel_coverage         0.810
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.967
_reflns_number_gt                4872
_reflns_number_total             4920
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            np0c00558_si_002.cif
_cod_data_source_block           1_a
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_chemical_absolute_configuration' value 'AD' was changed
to 'ad' in accordance with the
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas 

 Adding full bibliography for 1559007.cif.
;
_cod_original_cell_volume        2488.07(3)
_cod_original_sg_symbol_H-M      'C 2'
_cod_database_code               1559007
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.857
_shelx_estimated_absorpt_t_max   0.881
_shelx_res_checksum              44768
_shelx_hkl_checksum              40777