(±)-Rhytidhymarins A and B, two pairs of new isocoumarin derivatives from endophytic fungus Rhytidhysteron sp. BZM-9
Zhang, Sha; Kang, Feng-Hua; Tan, Jian-Bing; Chen, De-Kun; Kuang, Min; Wang, Wen-Xuan; Xu, Kang-Ping; Zou, Zhen-xing; New Journal of Chemistry 45 (2021) 12700–12704; doi:10.1039/D1NJ01993G

data_7060794
_publ_section_title
;
 (+-)-Rhytidhymarins A and B, two pairs of new isocoumarin derivatives
 from endophytic fungus Rhytidhysteron sp. BZM-9
;
_journal_issue                   28
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              12700
_journal_page_last               12704
_journal_paper_doi               10.1039/D1NJ01993G
_journal_volume                  45
_journal_year                    2021
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C12 H14 O5'
_chemical_formula_sum            'C12 H14 O5'
_chemical_formula_weight         238.23
_space_group_crystal_system      tetragonal
_space_group_IT_number           94
_space_group_name_Hall           'P 4n 2n'
_space_group_name_H-M_alt        'P 42 21 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-05-24
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2021-05-26 deposited with the CCDC.	2021-06-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   18.0572(4)
_cell_length_b                   18.0572(4)
_cell_length_c                   6.7365(2)
_cell_measurement_reflns_used    2447
_cell_measurement_temperature    101(2)
_cell_measurement_theta_max      73.6430
_cell_measurement_theta_min      5.4800
_cell_volume                     2196.52(9)
_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 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      101(2)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  -3.00   0.20    0.63    --    0.00 -82.00-120.00  150
  2  \w    -31.00  28.00   0.20    0.63    --    0.00 -82.00  30.00  295
  3  \w      7.00  86.00   0.20    2.51    --   95.80 -61.00 120.00  395
  4  \w     92.00 118.00   0.20    2.51    --   95.80 -61.00 120.00  130
  5  \w     87.00 164.00   0.20    2.51    --   95.80  82.00-150.00  385
  6  \w     96.00 175.00   0.20    2.51    --   95.80  45.00   0.00  395
;
_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      -0.0118559000
_diffrn_orient_matrix_UB_12      -0.0829560000
_diffrn_orient_matrix_UB_13      -0.0421096000
_diffrn_orient_matrix_UB_21      0.0183339000
_diffrn_orient_matrix_UB_22      -0.0180315000
_diffrn_orient_matrix_UB_23      0.2178913000
_diffrn_orient_matrix_UB_31      -0.0826159000
_diffrn_orient_matrix_UB_32      0.0078679000
_diffrn_orient_matrix_UB_33      0.0543417000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0279
_diffrn_reflns_av_unetI/netI     0.0343
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -5
_diffrn_reflns_number            5270
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        67.045
_diffrn_reflns_theta_max         67.045
_diffrn_reflns_theta_min         3.461
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.950
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.67657
_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    1.441
_exptl_crystal_description       block
_exptl_crystal_F_000             1008
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.240
_refine_diff_density_min         -0.280
_refine_diff_density_rms         0.061
_refine_ls_abs_structure_details
;
 Flack x determined using 686 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.02(13)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.179
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     160
_refine_ls_number_reflns         1964
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.179
_refine_ls_R_factor_all          0.0653
_refine_ls_R_factor_gt           0.0633
_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^)+(0.0211P)^2^+4.4834P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1455
_refine_ls_wR_factor_ref         0.1464
_reflns_Friedel_coverage         0.662
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.999
_reflns_number_gt                1887
_reflns_number_total             1964
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1nj01993g2.cif
_cod_data_source_block           zhangxiao_bmz-9-1_collect
_cod_depositor_comments
;
Adding full bibliography for 7060793--7060794.cif.

2025-03-29
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C96 H112 O40'
_cod_original_formula_weight         1905.85
_cod_original_formula_moiety         '8(C12 H14 O5)'
_cod_original_formula_units_Z            1
_cod_original_cell_volume        2196.52(12)
_cod_database_code               7060794
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C99 H90 N9 O9 '
_shelx_estimated_absorpt_t_max   0.981
_shelx_estimated_absorpt_t_min   0.928
_reflns_odcompleteness_completeness 99.92
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2.a Ternary CH refined with riding coordinates:
 C009(H009)
2.b Aromatic/amide H refined with riding coordinates:
 C008(H008)
2.c Idealised Me refined as rotating group:
 C00F(H00A,H00B,H00C), C00G(H00D,H00E,H00F), C00H(H00G,H00H,H00I)
2.d Idealised tetrahedral OH refined as rotating group:
 O001(H001), O003(H003), O005(H005)
;
_shelx_res_checksum              12593
_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 1.500
_oxdiff_exptl_absorpt_empirical_full_min 0.753