Pyrone and isocoumarin derivatives from the endophytic fungus <i>Cytospora rhizophorae</i>.
Liu, Hongxin; Zhang, Yanjiang; Chen, Yuchan; Liu, Zhaoming; Tan, Haibo; Zhang, Weimin; Organic & biomolecular chemistry 20 (2022) 4900–4904; doi:10.1039/d2ob00846g

data_7158730
_publ_section_title
;
 Pyrone and isocoumarin derivatives from the endophytic fungus
 <i>Cytospora rhizophorae</i>.
;
_journal_issue                   24
_journal_name_full               'Organic &amp; biomolecular chemistry'
_journal_page_first              4900
_journal_page_last               4904
_journal_paper_doi               10.1039/d2ob00846g
_journal_volume                  20
_journal_year                    2022
_chemical_formula_moiety         'C23 H24 O7'
_chemical_formula_sum            'C23 H24 O7'
_chemical_formula_weight         412.42
_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_block_doi                 10.5517/ccdc.csd.cc2896tm
_audit_creation_date             2020-08-14
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-07-04 deposited with the CCDC.	2022-06-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 96.603(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.2709(5)
_cell_length_b                   15.7729(5)
_cell_length_c                   10.1394(3)
_cell_measurement_reflns_used    1679
_cell_measurement_temperature    106.6(8)
_cell_measurement_theta_max      68.6950
_cell_measurement_theta_min      3.6100
_cell_volume                     1949.44(12)
_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      106.6(8)
_diffrn_detector                 'Pilatus3R 200K-A'
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.964
_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    -27.00  17.00   0.50    2.00    --    0.00 -82.00-180.00   88
  2  \w    -22.00   6.00   0.50    2.00    --    0.00 -82.00 120.00   56
  3  \w    -30.00  29.00   0.50    2.00    --    0.00 -82.00 -30.00  118
  4  \w     -8.00  26.00   0.50    2.00    --    0.00 -82.00 -90.00   68
  5  \w     67.00 102.00   0.50   10.00    --   88.70 -77.00-120.00   70
  6  \w     91.00 118.00   0.50   10.00    --   88.70  82.00 -90.00   54
  7  \w      2.00 107.00   0.50   10.00    --   88.70 -45.00 -60.00  210
  8  \w      6.00  98.00   0.50   10.00    --   88.70 -61.00-180.00  184
  9  \w     72.00  99.00   0.50   10.00    --   88.70 -61.00  60.00   54
 10  \w      7.00  34.00   0.50   10.00    --   88.70 -77.00-120.00   54
 11  \w    132.00 160.00   0.50   10.00    --   88.70  82.00 -90.00   56
 12  \w     -1.00 116.00   0.50   10.00    --   88.70 -77.00-180.00  234
 13  \w     93.00 118.00   0.50   10.00    --   88.70 -77.00  60.00   50
 14  \w     72.00 177.00   0.50   10.00    --   88.70  15.00  90.00  210
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Pro: Kappa single'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0847133000
_diffrn_orient_matrix_UB_12      0.0689316000
_diffrn_orient_matrix_UB_13      -0.0226446000
_diffrn_orient_matrix_UB_21      -0.0927906000
_diffrn_orient_matrix_UB_22      0.0659796000
_diffrn_orient_matrix_UB_23      -0.0233539000
_diffrn_orient_matrix_UB_31      0.0131664000
_diffrn_orient_matrix_UB_32      0.0208333000
_diffrn_orient_matrix_UB_33      0.1495202000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0734
_diffrn_reflns_av_unetI/netI     0.0925
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.964
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -6
_diffrn_reflns_number            10730
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.964
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         70.908
_diffrn_reflns_theta_min         3.626
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'MicroMax 007 (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.864
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.91822
_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 light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.405
_exptl_crystal_description       needle
_exptl_crystal_F_000             872
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.270
_refine_diff_density_min         -0.219
_refine_diff_density_rms         0.057
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.983
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     277
_refine_ls_number_reflns         3628
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.983
_refine_ls_R_factor_all          0.1025
_refine_ls_R_factor_gt           0.0529
_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^)+(0.0612P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1169
_refine_ls_wR_factor_ref         0.1377
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2209
_reflns_number_total             3628
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2ob00846g2.cif
_cod_data_source_block           zhangyanjiang_zyj-a761-44_collect
_cod_depositor_comments          'Adding full bibliography for 7158730.cif.'
_cod_database_code               7158730
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.975
_shelx_estimated_absorpt_t_min   0.813
_reflns_odcompleteness_completeness 99.91
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     64.99
_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.a Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C8(H8A,H8B), C9(H9A,H9B), C10(H10A,H10B)
2.b Aromatic/amide H refined with riding coordinates:
 C7'(H7'), C12'(H12')
2.c Idealised Me refined as rotating group:
 C11'(H11A,H11B,H11C), C13'(H13A,H13B,H13C), C12(H12A,H12B,H12C), C11(H11D,
 H11E,H11F)
2.d Idealised tetrahedral OH refined as rotating group:
 O28(H28), O29(H29)
;
_shelx_res_checksum              20364
_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 1.582
_oxdiff_exptl_absorpt_empirical_full_min 0.849