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_7158138
_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         '2(C13 H18 O6), H2 O'
_chemical_formula_sum            'C26 H38 O13'
_chemical_formula_weight         558.56
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_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                 100.7810(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   23.3741(4)
_cell_length_b                   13.2115(2)
_cell_length_c                   17.7270(3)
_cell_measurement_reflns_used    15666
_cell_measurement_temperature    99.9(6)
_cell_measurement_theta_max      73.6780
_cell_measurement_theta_min      4.2090
_cell_volume                     5377.60(15)
_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(6)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.985
_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  -2.00   0.50    0.50    --    0.00 -82.00  60.00   62
  2  \w    -15.00  59.00   0.50    0.50    --    0.00  38.00  60.00  148
  3  \w      9.00  87.00   0.50    0.50    --    0.00  38.00-120.00  156
  4  \w    -88.00 -14.00   0.50    0.50    --    0.00 -19.00  90.00  148
  5  \w     13.00  49.00   0.50    1.50    --   95.20 -82.00 120.00   72
  6  \w     88.00 126.00   0.50    1.50    --   95.20 -82.00 120.00   76
  7  \w     78.00 184.00   0.50    1.50    --   95.20  44.00 -78.88  212
  8  \w     73.00 100.00   0.50    1.50    --   95.20  61.00 -90.00   54
  9  \w    135.00 184.00   0.50    1.50    --   95.20  77.00  90.00   98
 10  \w      7.00 126.00   0.50    1.50    --   95.20 -82.00  60.00  238
 11  \w     73.00 183.00   0.50    1.50    --   95.20  61.00 -30.00  220
 12  \w      7.00  95.00   0.50    1.50    --   95.20 -61.00-180.00  176
 13  \w      9.00  63.00   0.50    1.50    --   95.20 -61.00 -90.00  108
 14  \w     64.00 112.00   0.50    1.50    --   95.20 -61.00 -90.00   96
 15  \w     66.00 101.00   0.50    1.50    --   95.20 -82.00-180.00   70
 16  \w     16.00 119.00   0.50    1.50    --   95.20 -82.00 -90.00  206
 17  \w     79.00 162.00   0.50    1.50    --   95.20  30.00  60.00  166
 18  \w     10.00 119.00   0.50    1.50    --   95.20 -61.00  60.00  218
 19  \w     79.00 185.00   0.50    1.50    --   95.20  30.00  30.00  212
 20  \w    134.00 172.00   0.50    1.50    --   95.20  71.00 -92.33   76
 21  \w     82.00 107.00   0.50    1.50    --   95.20 -82.00-150.00   50
 22  \w     69.00  96.00   0.50    1.50    --   95.20  71.00 -92.33   54
;
_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      -0.0622270000
_diffrn_orient_matrix_UB_12      -0.0359912000
_diffrn_orient_matrix_UB_13      -0.0335943000
_diffrn_orient_matrix_UB_21      0.0237999000
_diffrn_orient_matrix_UB_22      -0.1053429000
_diffrn_orient_matrix_UB_23      -0.0152650000
_diffrn_orient_matrix_UB_31      -0.0077374000
_diffrn_orient_matrix_UB_32      -0.0350252000
_diffrn_orient_matrix_UB_33      0.0803493000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0311
_diffrn_reflns_av_unetI/netI     0.0215
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            29267
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.159
_diffrn_reflns_theta_min         3.850
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.939
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.77694
_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 yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.380
_exptl_crystal_description       block
_exptl_crystal_F_000             2384
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.693
_refine_diff_density_min         -0.417
_refine_diff_density_rms         0.059
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.081
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     386
_refine_ls_number_reflns         5403
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.081
_refine_ls_R_factor_all          0.0734
_refine_ls_R_factor_gt           0.0701
_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^)+(0.0857P)^2^+12.4774P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1920
_refine_ls_wR_factor_ref         0.1945
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4974
_reflns_number_total             5403
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1ob00869b2.cif
_cod_data_source_block           zahngwenjun_sh31-10_collect
_cod_depositor_comments
'Adding full bibliography for 7158134--7158138.cif.'
_cod_database_code               7158138
_shelx_shelxl_version_number     2018/1
_chemical_oxdiff_formula         'C216 H352 N16 O80 '
_shelx_estimated_absorpt_t_max   0.955
_shelx_estimated_absorpt_t_min   0.912
_reflns_odcompleteness_completeness 99.96
_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, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups, All O(H,H) groups
2. Others
 Sof(H00a)=Sof(H00i)=Sof(H00j)=Sof(C0)=Sof(H0)=Sof(C1)=Sof(H1a)=Sof(H1b)=
 Sof(H1c)=1-FVAR(1)
 Sof(H00C)=Sof(H00g)=Sof(H00h)=Sof(C011)=Sof(H011)=Sof(C013)=Sof(H01a)=
 Sof(H01b)=Sof(H01c)=FVAR(1)
3.a Free rotating group:
 O00D(H00z,H)
3.b Ternary CH refined with riding coordinates:
 C010(H010), C011(H011), C0(H0)
3.c Secondary CH2 refined with riding coordinates:
 C00R(H00q,H00r), C00S(H00s,H00t), C00U(H00g,H00h), C00U(H00i,H00j), C00W(H00k,
 H00m), C00X(H00n,H00o), C00Z(H00x,H00y)
3.d Aromatic/amide H refined with riding coordinates:
 C00J(H00p), C00L(H00L)
3.e Tetrahedral OH refined with riding coordinates:
 O00C(H00C), O00C(H00a)
3.f Idealised Me refined as rotating group:
 C00T(H00d,H00e,H00f), C00Y(H00u,H00v,H00w), C012(H01d,H01e,H01f), C013(H01a,
 H01b,H01c), C1(H1a,H1b,H1c)
3.g Idealised tetrahedral OH refined as rotating group:
 O002(H002), O004(H004), O005(H005), O007(H007), O008(H008), O009(H009),
 O00B(H00B)
;
_shelx_res_checksum              25415
_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 1.455
_oxdiff_exptl_absorpt_empirical_full_min 0.726