Anti-inflammatory fusicoccane-type diterpenoids from the phytopathogenic fungus Alternaria brassicicola.
Li, Fengli; Sun, Weiguang; Guan, Jiankun; Lu, Yuanyuan; Lin, Shuang; Zhang, Sitian; Gao, Weixi; Liu, Junjun; Du, Guang; Wang, Jianping; Zhu, Hucheng; Qi, Changxing; Hu, Zhengxi; Zhang, Yonghui; Organic & biomolecular chemistry 16 (2018) 8751–8760; doi:10.1039/c8ob02353k

data_7156544
_publ_section_title
;
 Anti-inflammatory fusicoccane-type diterpenoids from the phytopathogenic
 fungus Alternaria brassicicola.
;
_journal_issue                   45
_journal_name_full               'Organic &amp; biomolecular chemistry'
_journal_page_first              8751
_journal_page_last               8760
_journal_paper_doi               10.1039/c8ob02353k
_journal_volume                  16
_journal_year                    2018
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C21 H32 O5'
_chemical_formula_sum            'C21 H32 O5'
_chemical_formula_weight         364.46
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2018-08-07 deposited with the CCDC.
2018-10-18 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 92.5190(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   6.3056(2)
_cell_length_b                   17.1631(6)
_cell_length_c                   17.9081(7)
_cell_measurement_reflns_used    9924
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      69.71
_cell_measurement_theta_min      3.57
_cell_volume                     1936.21(12)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.979
_diffrn_measured_fraction_theta_max 0.951
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0592
_diffrn_reflns_av_unetI/netI     0.0662
_diffrn_reflns_Laue_measured_fraction_full 0.979
_diffrn_reflns_Laue_measured_fraction_max 0.951
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            15901
_diffrn_reflns_point_group_measured_fraction_full 0.863
_diffrn_reflns_point_group_measured_fraction_max 0.832
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         70.267
_diffrn_reflns_theta_min         3.568
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.708
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.250
_exptl_crystal_description       prism
_exptl_crystal_F_000             792
_exptl_crystal_size_max          1.050
_exptl_crystal_size_mid          0.420
_exptl_crystal_size_min          0.150
_exptl_transmission_factor_max   0.7533
_exptl_transmission_factor_min   0.4258
_refine_diff_density_max         0.714
_refine_diff_density_min         -0.610
_refine_diff_density_rms         0.149
_refine_ls_abs_structure_details
;
 Flack x determined using 2223 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.24(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.089
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     485
_refine_ls_number_reflns         6140
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.088
_refine_ls_R_factor_all          0.0716
_refine_ls_R_factor_gt           0.0705
_refine_ls_shift/su_max          0.010
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1667P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1996
_refine_ls_wR_factor_ref         0.2013
_reflns_Friedel_coverage         0.689
_reflns_Friedel_fraction_full    0.739
_reflns_Friedel_fraction_max     0.704
_reflns_number_gt                5897
_reflns_number_total             6140
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8ob02353k2.cif
_cod_data_source_block           cu_zyh_lyy3262_0m
_cod_depositor_comments
'Adding full bibliography for 7156543--7156546.cif.'
_cod_database_code               7156544
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.523
_shelx_estimated_absorpt_t_max   0.901
_shelx_res_checksum              2300