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_1557885
_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_absolute_configuration ad
_chemical_formula_moiety         'C20 H25 Cl O6, 0.5(C H4 O), 0.5(H2 O)'
_chemical_formula_sum            'C20.5 H28 Cl O7'
_chemical_formula_weight         421.87
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2019-04-25
_audit_creation_method
; 
Olex2 1.2 
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506) 
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   13.1677(4)
_cell_length_b                   15.9113(4)
_cell_length_c                   20.4458(6)
_cell_measurement_reflns_used    8022
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      63.29
_cell_measurement_theta_min      3.52
_cell_volume                     4283.7(2)
_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    'XM (Sheldrick, 2008)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_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  0.1709
_diffrn_reflns_av_unetI/netI     0.1059
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            36853
_diffrn_reflns_point_group_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        64.989
_diffrn_reflns_theta_max         64.989
_diffrn_reflns_theta_min         3.520
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.910
_exptl_absorpt_correction_T_max  0.7535
_exptl_absorpt_correction_T_min  0.4500
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.308
_exptl_crystal_description       block
_exptl_crystal_F_000             1792
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.748
_refine_diff_density_min         -0.860
_refine_diff_density_rms         0.172
_refine_ls_abs_structure_details
; 
 Flack x determined using 1491 quotients [(I+)-(I-)]/[(I+)+(I-)] 
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). 
;
_refine_ls_abs_structure_Flack   0.128(19)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.334
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     527
_refine_ls_number_reflns         7189
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.334
_refine_ls_R_factor_all          0.1315
_refine_ls_R_factor_gt           0.1123
_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^)+(0.1000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2542
_refine_ls_wR_factor_ref         0.2631
_reflns_Friedel_coverage         0.788
_reflns_Friedel_fraction_full    0.983
_reflns_Friedel_fraction_max     0.983
_reflns_number_gt                5039
_reflns_number_total             7189
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            np9b01167_si_003.cif
_cod_data_source_block           cu_190422b_0m
_cod_depositor_comments
;

2022-05-28
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_moiety     '2(C20 H25 Cl O6), C H4 O, H2 O'
_cod_original_formula_sum        'C41 H56 Cl2 O14'
_cod_original_formula_units_Z    4
_cod_original_formula_weight     843.75
_cod_database_code               1557885
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.832
_shelx_estimated_absorpt_t_min   0.803
_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) 
2.b Ternary CH refined with riding coordinates: 
 C2(H2), C10(H10), C2A(H2A), C10A(H10A) 
2.c Secondary CH2 refined with riding coordinates: 
 C3(H3A,H3B), C6(H6A,H6B), C7(H7A,H7B), C8(H8A,H8B), C9(H9A,H9B), C11(H11A, 
 H11B), C13(H13A,H13B), C3A(H3AA,H3AB), C6A(H6AA,H6AB), C7A(H7AA,H7AB), 
 C8A(H8AA,H8AB), C9A(H9AA,H9AB), C11A(H11C,H11D), C13A(H13C,H13D) 
2.d Aromatic/amide H refined with riding coordinates: 
 C4(H4), C5(H5), C17(H17), C4A(H4A), C5A(H5AA), C17A(H17A) 
2.e Idealised Me refined as rotating group: 
 C1(H1A,H1B,H1C), C1A(H1AA,H1AB,H1AC), C1S(H1SA,H1SB,H1SC) 
2.f Idealised tetrahedral OH refined as rotating group: 
 O3(H3), O5(H5A), O6(H6), O3A(H3AC), O5A(H5AB), O6A(H6AC), O1S(H1S) 
;
_shelx_res_checksum              69041
_shelx_hkl_checksum              85220
_olex2_submission_special_instructions 'No special instructions were received'