Anthelmintic flavonoids and other compounds from <i>Combretum glutinosum</i> Perr. ex DC (Combretaceae) leaves
Toklo, Placide M.; Yayi Ladekan, Eléonore; Linden, Anthony; Hounzangbe-Adote, Sylvie; Kouam, Siméon F.; Gbenou, Joachim D.; Acta Crystallographica Section C 77 (2021) –; doi:10.1107/S2053229621007841

data_2022413
_publ_section_title
;
 Anthelmintic flavonoids and other compounds from <i>Combretum
 glutinosum</i> Perr. ex DC (Combretaceae) leaves
;
_journal_coeditor_code           OV3154
_journal_issue                   9
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first
;
;
_journal_paper_doi               10.1107/S2053229621007841
_journal_volume                  77
_journal_year                    2021
_chemical_absolute_configuration ad
_chemical_formula_iupac          'C30 H50 O3'
_chemical_formula_moiety         'C30 H50 O3'
_chemical_formula_sum            'C30 H50 O3'
_chemical_formula_weight         458.70
_chemical_name_common            (20S,24R)-ocotillone
_chemical_name_systematic
(5<i>R</i>,8<i>R</i>,9<i>R</i>,10<i>R</i>,13<i>R</i>,14<i>R</i>,17<i>S</i>)-17-[(2<i>S</i>,5<i>R</i>)-5-(2-Hydroxypropan-2-yl)-2-methyloxolan-2-yl]-4,4,8,10,14-pentamethyl-1,2,5,6,7,9,11,12,13,15,16,17-dodecahydrocyclopenta[<i>a</i>]phenanthren-3-one
_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     dual
_atom_sites_solution_secondary   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                   6.37386(6)
_cell_length_b                   12.10746(11)
_cell_length_c                   33.8928(3)
_cell_measurement_reflns_used    21446
_cell_measurement_temperature    160(2)
_cell_measurement_theta_max      76.2410
_cell_measurement_theta_min      2.5630
_cell_volume                     2615.55(4)
_computing_cell_refinement
;
CrysAlis PRO (Rigaku Oxford Diffraction, 2021)
;
_computing_data_collection
;
CrysAlis PRO (Rigaku Oxford Diffraction, 2021)
;
_computing_data_reduction
;
CrysAlis PRO (Rigaku Oxford Diffraction, 2021)
;
_computing_molecular_graphics
;
OLEX2 (Dolomanov <i>et al.</i>,  2009) and Mercury (Macrae <i>et
al.</i>,  2020)
;
_computing_publication_material
;
SHELXL2018 (Sheldrick, 2015b) and PLATON (Spek, 2020)
;
_computing_structure_refinement
;
SHELXL2018 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT2018 (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      160(2)
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 10.3801
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device       'four-circle \k-geometry diffractometer'
_diffrn_measurement_device_type  'Oxford Diffraction SuperNova dual radiation'
_diffrn_measurement_method       '\w scans'
_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  0.0181
_diffrn_reflns_av_unetI/netI     0.0119
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -42
_diffrn_reflns_number            26797
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.248
_diffrn_reflns_theta_min         2.607
_diffrn_source                   'micro-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    0.557
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.614
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model (Coppens <i>et al</i>., 1965)
plus an empirical absorption correction using spherical harmonics
(CrysAlis PRO; Rigaku Oxford Diffraction, 2021)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.165
_exptl_crystal_description       plate
_exptl_crystal_F_000             1016
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.225
_refine_diff_density_min         -0.143
_refine_ls_abs_structure_details
;
Flack <i>x</i> determined using 2226 quotients [(I+)-(I-)]/[(I+)+(I-)]
(Parsons <i>et al.</i>,  2013)
;
_refine_ls_abs_structure_Flack   -0.07(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     310
_refine_ls_number_reflns         5424
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0330
_refine_ls_R_factor_gt           0.0322
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0576P)^2^+0.4171P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0883
_refine_ls_wR_factor_ref         0.0892
_reflns_number_gt                5324
_reflns_number_total             5424
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ov3154sup1.cif
_cod_data_source_block           3
_cod_database_code               2022413
_shelx_hkl_checksum              52101
_shelx_res_checksum              95148
_cod_database_fobs_code 2022413