Structure and absolute configuration assignments of ochracines F–L, chamigrane and cadinane sesquiterpenes from the basidiomycete Steccherinum ochraceum HFG119
Zhao, Zhen-Zhu; Zhao, Qi-Lu; Feng, Wei-Sheng; He, Hai-Rong; Li, Meng; Xue, Gui-Min; Chen, He-Ping; Liu, Ji-Kai; RSC Advances 11 (2021) 18693–18701; doi:10.1039/D1RA03320D

data_7242906
_publ_section_title
;
 Structure and absolute configuration assignments of ochracines F--L,
 chamigrane and cadinane sesquiterpenes from the basidiomycete
 Steccherinum ochraceum HFG119
;
_journal_issue                   31
_journal_name_full               'RSC Advances'
_journal_page_first              18693
_journal_page_last               18701
_journal_paper_doi               10.1039/D1RA03320D
_journal_volume                  11
_journal_year                    2021
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C15 H22 O4, 1.5(H2 O)'
_chemical_formula_sum            'C15 H25 O5.5'
_chemical_formula_weight         293.35
_chemical_name_systematic        'Ochracine F'
_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
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2020-01-06 deposited with the CCDC.	2021-05-12 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 108.863(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   6.1285(5)
_cell_length_b                   32.973(3)
_cell_length_c                   7.7602(6)
_cell_measurement_reflns_used    9991
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      70.14
_cell_measurement_theta_min      2.68
_cell_volume                     1483.9(2)
_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 0.943
_diffrn_measured_fraction_theta_max 0.926
_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  0.0459
_diffrn_reflns_av_unetI/netI     0.0549
_diffrn_reflns_Laue_measured_fraction_full 0.943
_diffrn_reflns_Laue_measured_fraction_max 0.926
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       38
_diffrn_reflns_limit_k_min       -39
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            13461
_diffrn_reflns_point_group_measured_fraction_full 0.874
_diffrn_reflns_point_group_measured_fraction_max 0.854
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         70.138
_diffrn_reflns_theta_min         2.680
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.819
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.313
_exptl_crystal_description       plate
_exptl_crystal_F_000             636
_exptl_crystal_size_max          1.140
_exptl_crystal_size_mid          0.520
_exptl_crystal_size_min          0.030
_exptl_transmission_factor_max   0.5856
_exptl_transmission_factor_min   0.1987
_refine_diff_density_max         0.415
_refine_diff_density_min         -0.349
_refine_diff_density_rms         0.081
_refine_ls_abs_structure_details
;
 Flack x determined using 1976 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.14(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     404
_refine_ls_number_reflns         4805
_refine_ls_number_restraints     10
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0615
_refine_ls_R_factor_gt           0.0579
_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^)+(0.0816P)^2^+2.1251P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1595
_refine_ls_wR_factor_ref         0.1664
_reflns_Friedel_coverage         0.811
_reflns_Friedel_fraction_full    0.802
_reflns_Friedel_fraction_max     0.779
_reflns_number_gt                4627
_reflns_number_total             4805
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1ra03320d2.cif
_cod_data_source_block           cu_lzz40_0m
_cod_depositor_comments
;

2024-12-16
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C30 H50 O11'
_cod_original_formula_weight         586.70
_cod_original_formula_moiety         '2(C15 H22 O4), 3(H2 O)'
_cod_original_formula_units_Z            2
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               7242906
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.455
_shelx_estimated_absorpt_t_max   0.976
_shelx_res_checksum              95949