Lignans and [11]-chaetoglobosins from <i>Pseudeurotium bakeri</i> and their immunosuppressive activity.
Duan, Fangfang; Qin, Chunlun; Sang, Zihuan; Wei, Xiaoyi; Ruan, Hanli; Organic & biomolecular chemistry 22 (2024) 2271–2278; doi:10.1039/d3ob02109b

data_7159818
_publ_section_title
;
 Lignans and [11]-chaetoglobosins from <i>Pseudeurotium bakeri</i> and
 their immunosuppressive activity.
;
_journal_issue                   11
_journal_name_full               'Organic &amp; biomolecular chemistry'
_journal_page_first              2271
_journal_page_last               2278
_journal_paper_doi               10.1039/d3ob02109b
_journal_volume                  22
_journal_year                    2024
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C18 H20 O5, 2(H2 O)'
_chemical_formula_sum            'C18 H24 O7'
_chemical_formula_weight         352.37
_space_group_crystal_system      triclinic
_space_group_IT_number           1
_space_group_name_Hall           'P 1'
_space_group_name_H-M_alt        'P 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2024-01-30
_audit_creation_method
; 
Olex2 1.5 
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817) 
;
_audit_update_record
;
2024-01-30 deposited with the CCDC.	2024-02-19 downloaded from the CCDC.
;
_cell_angle_alpha                70.9980(10)
_cell_angle_beta                 85.0370(10)
_cell_angle_gamma                87.5120(10)
_cell_formula_units_Z            2
_cell_length_a                   7.8560(6)
_cell_length_b                   9.6968(7)
_cell_length_c                   12.0012(9)
_cell_measurement_reflns_used    9117
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      72.25
_cell_measurement_theta_min      3.40
_cell_volume                     861.06(11)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX3 Bruker-AXS, Madison WI'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'XM  (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.0
_diffrn_detector                 'Bruker Photon III 28 detector'
_diffrn_detector_area_resol_mean ' 7.39 for PHOTON III'
_diffrn_detector_type            'Bruker Photon III 28'
_diffrn_measured_fraction_theta_full 0.890
_diffrn_measured_fraction_theta_max 0.930
_diffrn_measurement_device       'Bruker D8 Venture'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'Metaljet Helios MX'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     1.34139
_diffrn_radiation_xray_symbol    'Ga K\a'
_diffrn_reflns_av_R_equivalents  0.0739
_diffrn_reflns_av_unetI/netI     0.1307
_diffrn_reflns_Laue_measured_fraction_full 0.890
_diffrn_reflns_Laue_measured_fraction_max 0.930
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            47380
_diffrn_reflns_point_group_measured_fraction_full 0.841
_diffrn_reflns_point_group_measured_fraction_max 0.869
_diffrn_reflns_theta_full        53.594
_diffrn_reflns_theta_max         72.365
_diffrn_reflns_theta_min         3.399
_diffrn_source                   'METALJET liquid metal X-ray source'
_diffrn_source_current           3.57
_diffrn_source_power             0.24972149999999999
_diffrn_source_target            Ga
_diffrn_source_type              'Sealed X-ray tube'
_diffrn_source_voltage           69.95
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.557
_exptl_absorpt_correction_T_max  0.3859
_exptl_absorpt_correction_T_min  0.2666
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, Sheldrick,2014'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.359
_exptl_crystal_description       block
_exptl_crystal_F_000             376
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.711
_refine_diff_density_min         -0.541
_refine_diff_density_rms         0.122
_refine_ls_abs_structure_details
; 
 Flack x determined using 3754 quotients [(I+)-(I-)]/[(I+)+(I-)] 
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). 
;
_refine_ls_abs_structure_Flack   0.19(18)
_refine_ls_extinction_coef       0.81(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.088
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     456
_refine_ls_number_reflns         8985
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.088
_refine_ls_R_factor_all          0.0813
_refine_ls_R_factor_gt           0.0778
_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^)+(0.1849P)^2^+0.0419P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2146
_refine_ls_wR_factor_ref         0.2382
_reflns_Friedel_coverage         0.870
_reflns_Friedel_fraction_full    0.792
_reflns_Friedel_fraction_max     0.809
_reflns_number_gt                8760
_reflns_number_total             8985
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3ob02109b2.cif
_cod_data_source_block           220225a_0m
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_diffrn_radiation_probe' value 'X-ray' was changed to
'x-ray' in accordance with the
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/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 8170 2020-07-09 18:12:32Z antanas 

 Adding full bibliography for 7159816--7159818.cif.
;
_cod_database_code               7159818
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.983
_shelx_estimated_absorpt_t_min   0.946
_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, All O(H,H) groups 
2.a Riding coordinates: 
 O1(H1), O1'(H1'), O2(H2), O2'(H2'), O1A(H1A), O1B(H1B), O2A(H2AA), O2B(H2B), 
 O1W(H1WA,H1WB), O2W(H2WA,H2WB), O3W(H3WA,H3WB), O4W(H4WA,H4WB) 
2.b Ternary CH refined with riding coordinates: 
 C8'(H8'), C8B(H8B) 
2.c Secondary CH2 refined with riding coordinates: 
 C7(H7A,H7B), C7'(H7'A,H7'B), C7A(H7AA,H7AB), C7B(H7BA,H7BB) 
2.d Aromatic/amide H refined with riding coordinates: 
 C2(H2A), C2'(H2'A), C4(H4), C4'(H4'), C6(H6), C2A(H2AB), C2B(H2BA), C4A(H4A), 
 C4B(H4B), C6A(H6A) 
2.e Idealised Me refined as rotating group: 
 C9(H9A,H9B,H9C), C9'(H9'A,H9'B,H9'C), C9A(H9AA,H9AB,H9AC), C9B(H9BA,H9BB,H9BC) 
;
_shelx_res_checksum              43616
_olex2_submission_special_instructions 'No special instructions were received'