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_7159817
_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         'C40 H45 F3 N2 O6, C1 H1 Cl3'
_chemical_formula_sum            'C41 H46 Cl3 F3 N2 O6'
_chemical_formula_weight         826.15
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2022-03-17
_audit_creation_method
; 
Olex2 1.3 
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408) 
;
_audit_update_record
;
2023-12-25 deposited with the CCDC.	2024-02-19 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 101.029(4)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   14.4485(12)
_cell_length_b                   8.6090(7)
_cell_length_c                   16.5929(14)
_cell_measurement_reflns_used    9650
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      59.03
_cell_measurement_theta_min      2.36
_cell_volume                     2025.8(3)
_computing_cell_refinement
'SAINT V8.40B Bruker-AXS, Madison WI for PHOTON III'
_computing_data_collection       'Bruker APEX3 Bruker-AXS, Madison WI'
_computing_data_reduction
'SAINT V8.40B Bruker-AXS, Madison WI for PHOTON III'
_computing_molecular_graphics
'Bruker SHELXTL Bruker-AXS, Madison WI and local programs'
_computing_publication_material  'Bruker SHELXTL Bruker-AXS, Madison WI'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_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 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device       'Bruker D8 Venture'
_diffrn_measurement_device_type  'Bruker Photon III'
_diffrn_measurement_method       'Profile data from \q/2\q 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  0.1448
_diffrn_reflns_av_unetI/netI     0.0687
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            91830
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        52.499
_diffrn_reflns_theta_max         52.499
_diffrn_reflns_theta_min         2.360
_diffrn_source                   'METALJET liquid metal X-ray source'
_diffrn_source_current           3.57
_diffrn_source_power             0.2497215
_diffrn_source_target            Ga
_diffrn_source_type              'Sealed X-ray tube'
_diffrn_source_voltage           69.95
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.697
_exptl_absorpt_correction_T_max  0.6750
_exptl_absorpt_correction_T_min  0.5355
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 - Bruker AXS, Madison WI for PHOTON III'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.354
_exptl_crystal_description       needle
_exptl_crystal_F_000             864
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.643
_refine_diff_density_min         -0.596
_refine_diff_density_rms         0.105
_refine_ls_abs_structure_details
; 
 Flack x determined using 2126 quotients [(I+)-(I-)]/[(I+)+(I-)] 
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). 
;
_refine_ls_abs_structure_Flack   0.11(3)
_refine_ls_extinction_coef       0.020(3)
_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   1.058
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     515
_refine_ls_number_reflns         6992
_refine_ls_number_restraints     13
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.1005
_refine_ls_R_factor_gt           0.0889
_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^)+(0.1810P)^2^+0.2977P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2401
_refine_ls_wR_factor_ref         0.2500
_reflns_Friedel_coverage         0.864
_reflns_Friedel_fraction_full    0.997
_reflns_Friedel_fraction_max     0.997
_reflns_number_gt                5613
_reflns_number_total             6992
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3ob02109b2.cif
_cod_data_source_block           220301j_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               7159817
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.967
_shelx_estimated_absorpt_t_min   0.849
_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. Restrained distances 
 Cl2S-C1S = Cl1S-C1S = Cl3S-C1S = Cl2T-C1T = Cl3T-C1T = Cl1T-C1T 
 1.73 with sigma of 0.02 
 Cl3S-C1S \\sim Cl3T-C1T 
 with sigma of 0.02 
 Cl1S-Cl2S \\sim Cl1T-Cl2T 
 with sigma of 0.04 
 Cl1S-C1S \\sim Cl1T-C1T 
 with sigma of 0.02 
 Cl2S-C1S \\sim Cl2T-C1T 
 with sigma of 0.02 
 Cl3S-Cl1S \\sim Cl3T-Cl1T 
 with sigma of 0.04 
 Cl3S-Cl2S \\sim Cl3T-Cl2T 
 with sigma of 0.04 
3. Uiso/Uaniso restraints and constraints 
Uanis(C1S) = Uanis(C1T) 
Uanis(Cl2S) = Uanis(Cl1T) 
Uanis(Cl3S) = Uanis(Cl3T) 
Uanis(Cl1S) = Uanis(Cl2T) 
4. Others 
 Sof(C1T)=Sof(H1T)=Sof(Cl1T)=Sof(Cl2T)=Sof(Cl3T)=1-FVAR(1) 
 Sof(C1S)=Sof(H1S)=Sof(Cl1S)=Sof(Cl2S)=Sof(Cl3S)=FVAR(1) 
5.a Ternary CH refined with riding coordinates: 
 C3(H3), C4(H4), C5(H5), C8(H8), C16(H16), C18(H18), C19(H19), C1S(H1S), 
 C1T(H1T) 
5.b Secondary CH2 refined with riding coordinates: 
 C10(H10A,H10B), C15(H15A,H15B), C17(H17A,H17B), C20(H20A,H20B) 
5.c Aromatic/amide H refined with riding coordinates: 
 C2"(H2"), C2'(H2'), C3"(H3"), C4"(H4"), C5"(H5"), C5'(H5'), C6"(H6"), 
 C6'(H6'), C7(H7), C7'(H7'), C8'(H8'), C13(H13), C14(H14), N1'(H1'), N2(H2) 
5.d Idealised Me refined as rotating group: 
 C9"(H9"A,H9"B,H9"C), C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C22(H22A,H22B, 
 H22C), C23(H23A,H23B,H23C) 
;
_olex2_submission_special_instructions 'No special instructions were received'