Cytotoxic Compounds from the Stem Bark of Two subsp. of <i>Bersama abyssinica</i>.
Nyamboki, Divinah K.; Bedane, Kibrom G.; Hassan, Khadija; Brieger, Lukas; Strohmann, Carsten; Spiteller, Michael; Matasyoh, Josphat C.; Journal of natural products 84 (2021) 1453–1458; doi:10.1021/acs.jnatprod.0c01141

data_1562545
_publ_section_title
;
 Cytotoxic Compounds from the Stem Bark of Two subsp. of <i>Bersama
 abyssinica</i>.
;
_journal_issue                   5
_journal_name_full               'Journal of natural products'
_journal_page_first              1453
_journal_page_last               1458
_journal_paper_doi               10.1021/acs.jnatprod.0c01141
_journal_volume                  84
_journal_year                    2021
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C26 H34 O9, C H4 O'
_chemical_formula_sum            'C27 H38 O10'
_chemical_formula_weight         522.57
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-11-13
_audit_creation_method
;
Olex2 1.3-alpha
(compiled 2019.10.31 svn.r3677 for OlexSys, GUI svn.r5972)
;
_cell_angle_alpha                90
_cell_angle_beta                 102.657(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   7.1585(3)
_cell_length_b                   16.5713(8)
_cell_length_c                   10.8248(4)
_cell_measurement_reflns_used    1770
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      74.49
_cell_measurement_theta_min      4.19
_cell_volume                     1252.89(9)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics    'Olex2 1.3-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-alpha (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'XT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.0
_diffrn_detector                 'Bruker D8 VENTURE area detector'
_diffrn_detector_area_resol_mean 10.4167
_diffrn_detector_type            'CPAD PHOTON II area detector'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'HELIOS mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0224
_diffrn_reflns_av_unetI/netI     0.0107
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            42139
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         74.970
_diffrn_reflns_theta_min         4.186
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_type              'Incoatec I\ms'
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.877
_exptl_absorpt_correction_T_max  0.5879
_exptl_absorpt_correction_T_min  0.5164
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0776 before and 0.0384 after correction.
The Ratio of minimum to maximum transmission is 0.8784.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.385
_exptl_crystal_description       block
_exptl_crystal_F_000             560
_exptl_crystal_size_max          0.276
_exptl_crystal_size_mid          0.163
_exptl_crystal_size_min          0.078
_refine_diff_density_max         0.261
_refine_diff_density_min         -0.139
_refine_diff_density_rms         0.036
_refine_ls_abs_structure_details
;
 Flack x determined using 2417 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.04(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     342
_refine_ls_number_reflns         5098
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0250
_refine_ls_R_factor_gt           0.0250
_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^)+(0.0455P)^2^+0.2209P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0697
_refine_ls_wR_factor_ref         0.0698
_reflns_Friedel_coverage         0.909
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.975
_reflns_number_gt                5087
_reflns_number_total             5098
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            np0c01141_si_003.cif
_cod_data_source_block           b1666_0m
_cod_depositor_comments
'Adding full bibliography for 1562544--1562546.cif.'
_cod_database_code               1562545
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.935
_shelx_estimated_absorpt_t_min   0.794
_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 Ternary CH refined with riding coordinates:
 C20(H20), C22(H22), C6(H6A), C7(H7A), C14(H14), C15(H15)
2.b Secondary CH2 refined with riding coordinates:
 C12(H12A,H12B), C21(H21A,H21B), C13(H13A,H13B), C17(H17A,H17B), C23(H23A,
 H23B), C8(H8A,H8B), C16(H16A,H16B)
2.c Aromatic/amide H refined with riding coordinates:
 C24(H24), C5(H5), C2(H2), C3(H3A)
2.d Idealised Me refined as rotating group:
 C27(H27A,H27B,H27C), C11(H11A,H11B,H11C), C26(H26A,H26B,H26C)
2.e Idealised tetrahedral OH refined as rotating group:
 O6(H6), O3(H3), O4(H4), O7(H7), O10(H10)
;
_shelx_res_checksum              16183
_shelx_hkl_checksum              838
_olex2_submission_special_instructions 'No special instructions were received'