Structures and absolute configurations of phomalones from the coral-associated fungus Parengyodontium album sp. SCSIO 40430.
Wang, Lu; Huang, Yanbing; Zhang, Liping; Liu, Zhiwen; Liu, Wei; Xu, Huixin; Zhang, Qingbo; Zhang, Haibo; Yan, Yan; Liu, Zhiyong; Zhang, Tianyu; Zhang, Wenjun; Zhang, Changsheng; Organic & biomolecular chemistry 19 (2021) 6030–6037; doi:10.1039/d1ob00869b

data_7158137
_publ_section_title
;
 Structures and absolute configurations of phomalones from the
 coral-associated fungus Parengyodontium album sp. SCSIO 40430.
;
_journal_issue                   27
_journal_name_full               'Organic &amp; biomolecular chemistry'
_journal_page_first              6030
_journal_page_last               6037
_journal_paper_doi               10.1039/d1ob00869b
_journal_volume                  19
_journal_year                    2021
_chemical_formula_moiety         'C13 H13.84 O4'
_chemical_formula_sum            'C13 H14 O4'
_chemical_formula_weight         234.24
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-03-19
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-03-22 deposited with the CCDC.	2021-06-21 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 99.215(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.1797(3)
_cell_length_b                   5.27290(10)
_cell_length_c                   17.2041(4)
_cell_measurement_reflns_used    5498
_cell_measurement_temperature    99.98(16)
_cell_measurement_theta_max      78.8090
_cell_measurement_theta_min      5.1980
_cell_volume                     1090.63(4)
_computing_cell_refinement       'CrysAlisPro 1.171.39.33c (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.33c (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.33c (Rigaku OD, 2017)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      99.98(16)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -33.00  31.00   0.40    1.07    --    0.00 -82.00  60.00  160
  2  \w    -33.00  31.00   0.40    1.07    --    0.00 -82.00-150.00  160
  3  \w    -33.00  31.00   0.40    1.07    --    0.00 -82.00   0.00  160
  4  \w    -33.00  31.00   0.40    1.07    --    0.00 -82.00 120.00  160
  5  \w     17.00 129.00   0.40    4.29    --  106.20 -15.00  60.00  280
  6  \w     17.00 129.00   0.40    4.29    --  106.20 -61.00 -60.00  280
  7  \w     88.00 196.00   0.40    4.29    --  106.20  82.00  60.00  270
  8  \w     90.00 196.00   0.40    4.29    --  106.20  30.00-120.00  265
  9  \w     17.00 125.00   0.40    4.29    --  106.20 -45.00 -60.00  270
 10  \w     90.00 196.00   0.40    4.29    --  106.20  30.00-180.00  265
 11  \w     92.00 160.80   0.40    4.29    --  106.20  15.00 -30.00  172
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa single'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0615608000
_diffrn_orient_matrix_UB_12      -0.1073379000
_diffrn_orient_matrix_UB_13      0.0782874000
_diffrn_orient_matrix_UB_21      -0.0966782000
_diffrn_orient_matrix_UB_22      0.0845421000
_diffrn_orient_matrix_UB_23      0.0417854000
_diffrn_orient_matrix_UB_31      -0.0573422000
_diffrn_orient_matrix_UB_32      -0.2581995000
_diffrn_orient_matrix_UB_33      -0.0188155000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0222
_diffrn_reflns_av_unetI/netI     0.0187
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.978
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       4
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            6947
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.978
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         79.170
_diffrn_reflns_theta_min         3.677
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.878
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.70151
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.33c (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.427
_exptl_crystal_description       needle
_exptl_crystal_F_000             496
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.249
_refine_diff_density_min         -0.233
_refine_diff_density_rms         0.051
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.125
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     177
_refine_ls_number_reflns         2311
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.128
_refine_ls_R_factor_all          0.0502
_refine_ls_R_factor_gt           0.0487
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0523P)^2^+0.8040P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1253
_refine_ls_wR_factor_ref         0.1263
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2204
_reflns_number_total             2311
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1ob00869b2.cif
_cod_data_source_block           huangyanbing_sh31-fr1-m2_collect
_cod_depositor_comments
'Adding full bibliography for 7158134--7158138.cif.'
_cod_database_code               7158137
_shelx_shelxl_version_number     2018/1
_chemical_oxdiff_formula         'C52 H56 O16 '
_reflns_odcompleteness_completeness 99.88
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     71.98
_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
2. Restrained distances
 C10A-C11A
 1.5 with sigma of 0.02
 C17-C10A
 1.5 with sigma of 0.02
3. Others
 Sof(H17a)=Sof(H17b)=Sof(H17c)=FVAR(1)
 Sof(C10A)=Sof(H10A)=1-FVAR(2)
 Sof(C10)=Sof(H10)=FVAR(2)
 Sof(C11A)=Sof(H11c)=Sof(H11d)=1-FVAR(3)
 Sof(C11)=Sof(H11a)=Sof(H11b)=FVAR(3)
4.a Ternary CH refined with riding coordinates:
 C10(H10), C10A(H10A)
4.b Secondary CH2 refined with riding coordinates:
 C6(H6a,H6b), C5(H5a,H5b), C11(H11a,H11b), C11A(H11c,H11d)
4.c Aromatic/amide H refined with riding coordinates:
 C2(H2)
4.d Idealised Me refined as rotating group:
 C17(H17a,H17b,H17c), C15(H15a,H15b,H15c)
;
_shelx_res_checksum              54349
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.321
_oxdiff_exptl_absorpt_empirical_full_min 0.498