Crystal structure of the cytotoxic macrocyclic trichothecene Isororidin A.
Asmaey, Mostafa A.; Kalofolias, Dimitris A.; Charavgi, Maria Despoina; Abdel-Rahim, Ismail R; Chrysina, Evangelia D.; Abatis, Dennis; Acta crystallographica. Section C, Structural chemistry 80 (2024) –; doi:10.1107/S2053229624006144

data_2312550
_publ_section_title
;
 Crystal structure of the cytotoxic macrocyclic trichothecene Isororidin
 A.
;
_journal_coeditor_code           UX3006
_journal_issue                   8
_journal_name_full
'Acta crystallographica. Section C, Structural chemistry'
_journal_paper_doi               10.1107/S2053229624006144
_journal_volume                  80
_journal_year                    2024
_chemical_absolute_configuration ad
_chemical_formula_iupac          'C29 H40 O9'
_chemical_formula_moiety         'C29 H40 O9'
_chemical_formula_sum            'C29 H40 O9'
_chemical_formula_weight         532.61
_chemical_name_common
;
Isororidin A
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     difmap
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.2707(4)
_cell_length_b                   15.2236(6)
_cell_length_c                   20.0806(8)
_cell_measurement_reflns_used    9959
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      74.91
_cell_measurement_theta_min      4.4
_cell_volume                     2834.0(2)
_computing_cell_refinement
;
SAINT (Bruker, 2021)
;
_computing_data_collection
;
APEX2 (Bruker, 2021)
;
_computing_data_reduction
;
SORTAV (Blessing, 1995)
;
_computing_structure_refinement
;
SHELXL2018 (Sheldrick, 2015<i>b</i>)
;
_computing_structure_solution
;
SHELXT (Sheldrick, 2015<i>a</i>)
;
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'APEX-II CCD'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEXII'
_diffrn_measurement_method       '\f or \w oscillation scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0552
_diffrn_reflns_av_unetI/netI     0.0211
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            101717
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         72.097
_diffrn_reflns_theta_min         3.643
_diffrn_source                   'sealed x-ray tube'
_exptl_absorpt_coefficient_mu    0.758
_exptl_absorpt_correction_T_max  0.754
_exptl_absorpt_correction_T_min  0.673
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Bruker, 2021)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.248
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Irregular
_exptl_crystal_F_000             1144
_exptl_crystal_size_max          0.079
_exptl_crystal_size_mid          0.055
_exptl_crystal_size_min          0.042
_refine_diff_density_max         0.337
_refine_diff_density_min         -0.220
_refine_ls_abs_structure_details
;
Flack <i>x</i> determined using 2264 quotients [(I+)-(I-)]/[(I+)+(I-)]
(Parsons <i>et al.</i>,  2013)
;
_refine_ls_abs_structure_Flack   -0.02(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     349
_refine_ls_number_reflns         5548
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.0422
_refine_ls_R_factor_gt           0.0407
_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^)+(0.0618P)^2^+1.0952P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1079
_refine_ls_wR_factor_ref         0.1091
_reflns_number_gt                5338
_reflns_number_total             5548
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ux3006.cif
_cod_data_source_block           I
_cod_database_code               2312550
_shelx_estimated_absorpt_t_min   0.943
_shelx_estimated_absorpt_t_max   0.969
_shelx_hkl_checksum              11977
_shelx_res_checksum              85079