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_1562546
_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 H30 O6, H2 O'
_chemical_formula_sum            'C26 H32 O7'
_chemical_formula_weight         456.51
_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   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2019-11-06
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 105.607(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.1262(8)
_cell_length_b                   14.4026(7)
_cell_length_c                   13.3342(8)
_cell_measurement_reflns_used    5796
_cell_measurement_temperature    100
_cell_measurement_theta_max      74.46
_cell_measurement_theta_min      3.44
_cell_volume                     2242.9(2)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (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 0.996
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       '\f and \w 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  0.0643
_diffrn_reflns_av_unetI/netI     0.0477
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            41245
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.976
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         74.996
_diffrn_reflns_theta_min         3.441
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.800
_exptl_absorpt_correction_T_max  0.5879
_exptl_absorpt_correction_T_min  0.4680
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1560 before and 0.0798 after correction. The Ratio of minimum to maximum transmission is 0.7961. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.352
_exptl_crystal_description       needle
_exptl_crystal_F_000             976
_exptl_crystal_size_max          0.452
_exptl_crystal_size_mid          0.147
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.186
_refine_diff_density_min         -0.215
_refine_diff_density_rms         0.039
_refine_ls_abs_structure_details
;
 Flack x determined using 3519 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.08(13)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     625
_refine_ls_number_reflns         9034
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0483
_refine_ls_R_factor_gt           0.0428
_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^)+(0.0540P)^2^+0.6983P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1056
_refine_ls_wR_factor_ref         0.1108
_reflns_Friedel_coverage         0.880
_reflns_Friedel_fraction_full    0.995
_reflns_Friedel_fraction_max     0.953
_reflns_number_gt                8280
_reflns_number_total             9034
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            np0c01141_si_001.cif
_cod_data_source_block           b1658_0m
_cod_depositor_comments
'Adding full bibliography for 1562544--1562546.cif.'
_cod_database_code               1562546
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.939
_shelx_estimated_absorpt_t_min   0.714
_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
2.a Ternary CH refined with riding coordinates:
 C29(H29), C38(H38), C39(H39), C33(H33), C10(H10), C9(H9), C3(H3), C5(H5)
2.b Secondary CH2 refined with riding coordinates:
 C11(H11A,H11B), C37(H37A,H37B), C6(H6A,H6B), C12(H12A,H12B), C34(H34A,H34B),
 C41(H41A,H41B), C36(H36A,H36B), C14(H14A,H14B), C30(H30A,H30B), C40(H40A,H40B),
  C4(H4A,H4B), C15(H15A,H15B)
2.c Aromatic/amide H refined with riding coordinates:
 C23(H23), C50(H50), C18(H18), C44(H44), C26(H26), C49(H49), C52(H52), C24(H24)
2.d Idealised Me refined as rotating group:
 C47(H47A,H47B,H47C), C27(H27A,H27B,H27C), C21(H21A,H21B,H21C), C35(H35A,H35B,
 H35C), C1(H1A,H1B,H1C), C13(H13A,H13B,H13C)
;
_shelx_res_checksum              52722
_shelx_hkl_checksum              43695
_olex2_submission_special_instructions 'No special instructions were received'