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_7158134
_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         'C11.95 H13.91 O4'
_chemical_formula_sum            'C12 H14 O4'
_chemical_formula_weight         222.23
_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                 115.015(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.6505(4)
_cell_length_b                   4.35190(10)
_cell_length_c                   17.2668(5)
_cell_measurement_reflns_used    2179
_cell_measurement_temperature    99.9(5)
_cell_measurement_theta_max      73.6490
_cell_measurement_theta_min      6.4150
_cell_volume                     1065.72(6)
_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      99.9(5)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.963
_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    -14.00  31.00   0.50    1.00    --    0.00 -82.00 -30.00   90
  2  \w    -29.00  31.00   0.50    1.00    --    0.00 -82.00-150.00  120
  3  \w     -1.00  28.00   0.50    1.00    --    0.00 -82.00 120.00   58
  4  \w    -30.00  -3.00   0.50    1.00    --    0.00 -82.00 120.00   54
  5  \w    160.00 185.00   0.50    4.00    --   95.20  15.00 120.00   50
  6  \w     77.00 109.00   0.50    4.00    --   95.20 -45.00 -90.00   64
  7  \w     97.00 123.00   0.50    4.00    --   95.20  15.00 120.00   52
  8  \w      9.00 100.00   0.50    4.00    --   95.20 -45.00  30.00  182
  9  \w     79.00 181.00   0.50    4.00    --   95.20  61.00 150.00  204
 10  \w    133.00 183.00   0.50    4.00    --   95.20  82.00  30.00  100
 11  \w      7.00  73.00   0.50    4.00    --   95.20 -45.00 -90.00  132
 12  \w     17.00 106.00   0.50    4.00    --   95.20 -30.00  30.00  178
;
_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      -0.0974018000
_diffrn_orient_matrix_UB_12      -0.0728837000
_diffrn_orient_matrix_UB_13      -0.0722647000
_diffrn_orient_matrix_UB_21      0.0135230000
_diffrn_orient_matrix_UB_22      0.2590769000
_diffrn_orient_matrix_UB_23      -0.0545677000
_diffrn_orient_matrix_UB_31      0.0461568000
_diffrn_orient_matrix_UB_32      -0.2300031000
_diffrn_orient_matrix_UB_33      -0.0385916000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0236
_diffrn_reflns_av_unetI/netI     0.0384
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.963
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       3
_diffrn_reflns_limit_k_min       -5
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            4622
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.963
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.018
_diffrn_reflns_theta_min         5.175
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.865
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.87085
_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 yellowish white'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    white
_exptl_crystal_density_diffrn    1.385
_exptl_crystal_description       block
_exptl_crystal_F_000             472
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.874
_refine_diff_density_min         -0.269
_refine_diff_density_rms         0.053
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     151
_refine_ls_number_reflns         2097
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.077
_refine_ls_R_factor_all          0.0554
_refine_ls_R_factor_gt           0.0475
_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^)+(0.0682P)^2^+0.5610P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1307
_refine_ls_wR_factor_ref         0.1367
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1783
_reflns_number_total             2097
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1ob00869b2.cif
_cod_data_source_block           zhangwenjun_sh31-19_collect
_cod_depositor_comments
'Adding full bibliography for 7158134--7158138.cif.'
_cod_database_code               7158134
_shelx_shelxl_version_number     2018/1
_chemical_oxdiff_formula         'C44 H52 O20 '
_shelx_estimated_absorpt_t_max   0.958
_shelx_estimated_absorpt_t_min   0.846
_reflns_odcompleteness_completeness 99.77
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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
2. Others
 Sof(H16a)=Sof(H16b)=Sof(H16c)=Sof(H2a)=Sof(H2b)=FVAR(1)
 Sof(C1)=Sof(H1)=FVAR(2)
3.a Ternary CH refined with riding coordinates:
 C1(H1)
3.b Secondary CH2 refined with riding coordinates:
 C14(H14a,H14b), C2(H2a,H2b)
3.c Aromatic/amide H refined with riding coordinates:
 C6(H6)
3.d Idealised Me refined as rotating group:
 C15(H15a,H15b,H15c), C16(H16a,H16b,H16c)
3.e Idealised tetrahedral OH refined as rotating group:
 O12(H12), O11(H11)
;
_shelx_res_checksum              68900
_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 1.338
_oxdiff_exptl_absorpt_empirical_full_min 0.788