Resorcylic Acid Lactones from an Ilyonectria sp.
Zhou, Jia; Gao, Ying; Chang, Jin-Ling; Yu, Heng-Yi; Chen, Juan; Zhou, Ming; Meng, Xiang-Gao; Ruan, Han-Li; Journal of Natural Products  (2020) –; doi:10.1021/acs.jnatprod.9b01167

data_1557887
_publ_section_title
;
 Resorcylic Acid Lactones from an Ilyonectria sp.
;
_journal_name_full               'Journal of Natural Products'
_journal_paper_doi               10.1021/acs.jnatprod.9b01167
_journal_year                    2020
_chemical_formula_moiety         'C18 H20 O7, 1.5(H2 O)'
_chemical_formula_sum            'C18 H22 O8.5'
_chemical_formula_weight         374.35
_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   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2019-06-11
_audit_creation_method
; 
Olex2 1.2 
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506) 
;
_cell_angle_alpha                90
_cell_angle_beta                 94.614(17)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   5.3318(16)
_cell_length_b                   22.504(6)
_cell_length_c                   15.235(4)
_cell_measurement_reflns_used    1110
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      41.30
_cell_measurement_theta_min      3.51
_cell_volume                     1822.1(9)
_computing_cell_refinement       'SAINT v7.68A (Bruker, 2009)'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'SAINT v7.68A (Bruker, 2009)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.955
_diffrn_measured_fraction_theta_max 0.955
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.2149
_diffrn_reflns_av_unetI/netI     0.2584
_diffrn_reflns_Laue_measured_fraction_full 0.955
_diffrn_reflns_Laue_measured_fraction_max 0.955
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            13927
_diffrn_reflns_point_group_measured_fraction_full 0.941
_diffrn_reflns_point_group_measured_fraction_max 0.941
_diffrn_reflns_theta_full        58.209
_diffrn_reflns_theta_max         58.208
_diffrn_reflns_theta_min         3.511
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.926
_exptl_absorpt_correction_T_max  0.7513
_exptl_absorpt_correction_T_min  0.5371
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.365
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             792
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.431
_refine_diff_density_min         -0.381
_refine_diff_density_rms         0.112
_refine_ls_abs_structure_details
; 
 Flack x determined using 705 quotients [(I+)-(I-)]/[(I+)+(I-)] 
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). 
;
_refine_ls_abs_structure_Flack   -0.5(5)
_refine_ls_extinction_coef       0.038(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     478
_refine_ls_number_reflns         4805
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.1925
_refine_ls_R_factor_gt           0.1078
_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^)+(0.1168P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2324
_refine_ls_wR_factor_ref         0.2825
_reflns_Friedel_coverage         0.913
_reflns_Friedel_fraction_full    0.925
_reflns_Friedel_fraction_max     0.925
_reflns_number_gt                2600
_reflns_number_total             4805
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            np9b01167_si_010.cif
_cod_data_source_block           cu_190310c_0m
_cod_depositor_comments
;

2022-03-31
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C36 H44 O17'
_cod_original_formula_weight         748.71
_cod_original_formula_moiety         '2(C18 H20 O7), 2(H2 O), O'
_cod_original_formula_units_Z            2
_cod_database_code               1557887
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.982
_shelx_estimated_absorpt_t_min   0.913
_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 Free rotating group: 
 O1W(H1WA,H1WB), O2W(H2WA,H2WB) 
2.b Ternary CH refined with riding coordinates: 
 C2(H2), C4(H4), C5(H5), C8(H8), C2B(H2B), C4B(H4B), C5B(H5B), C8B(H8B) 
2.c Secondary CH2 refined with riding coordinates: 
 C3(H3A,H3B), C9(H9A,H9B), C11(H11A,H11B), C3B(H3BA,H3BB), C9B(H9BA,H9BB), 
 C11B(H11C,H11D) 
2.d Aromatic/amide H refined with riding coordinates: 
 C6(H6), C7(H7), C13(H13), C15(H15), C6B(H6B), C7B(H7B), C13B(H13B), C15B(H15B) 
2.e Idealised Me refined as rotating group: 
 C1(H1A,H1B,H1C), C1B(H1BA,H1BB,H1BC) 
2.f Idealised tetrahedral OH refined as rotating group: 
 O3(H3), O6(H6A), O7(H7A), O3B(H3BC), O6B(H6BA), O7B(H7BA) 
;
_olex2_submission_special_instructions 'No special instructions were received'