Structures and inhibitory activity against breast cancer cells of new bufadienolides from the eggs of toad Bufo bufo gargarizans
Zhang, Peng-Wei; Tian, Hai-Yan; Nie, Qiu-Lin; Wang, Lei; Zhou, Shi-Wen; Ye, Wen-Cai; Zhang, Dong-Mei; Jiang, Ren-Wang; RSC Adv.  (2016) –; doi:10.1039/C6RA18676A

data_7226573
_publ_section_title
;
 Structures and inhibitory activity against breast cancer cells of new
 bufadienolides from the eggs of toad Bufo bufo gargarizans
;
_journal_name_full               'RSC Adv.'
_journal_paper_doi               10.1039/C6RA18676A
_journal_year                    2016
_chemical_absolute_configuration rm
_chemical_formula_sum            'C23 H36 O8'
_chemical_formula_weight         440.52
_space_group_crystal_system      monoclinic
_space_group_IT_number           5
_space_group_name_Hall           'C 2y'
_space_group_name_H-M_alt        'C 1 2 1'
_symmetry_space_group_name_Hall  'C 2y'
_symmetry_space_group_name_H-M   'C 1 2 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2016-06-24 deposited with the CCDC.
2016-09-12 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 104.253(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.8755(3)
_cell_length_b                   10.7481(2)
_cell_length_c                   18.0005(4)
_cell_measurement_reflns_used    2311
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      62.7878
_cell_measurement_theta_min      5.0660
_cell_volume                     2226.84(9)
_computing_cell_refinement       'CrysAlis PRO '
_computing_data_collection       'CrysAlis PRO '
_computing_data_reduction        'CrysAlis PRO '
_computing_molecular_graphics    'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.969
_diffrn_measured_fraction_theta_max 0.969
_diffrn_measurement_device_type  'Agilent Gemini S ultra'
_diffrn_measurement_method       'omega scan'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0140
_diffrn_reflns_av_unetI/netI     0.0207
_diffrn_reflns_Laue_measured_fraction_full 0.969
_diffrn_reflns_Laue_measured_fraction_max 0.969
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            3396
_diffrn_reflns_point_group_measured_fraction_full 0.719
_diffrn_reflns_point_group_measured_fraction_max 0.719
_diffrn_reflns_theta_full        62.876
_diffrn_reflns_theta_max         62.876
_diffrn_reflns_theta_min         5.070
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.813
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.910
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.314
_exptl_crystal_description       block
_exptl_crystal_F_000             952
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.260
_refine_diff_density_min         -0.308
_refine_diff_density_rms         0.034
_refine_ls_abs_structure_details
;
 Flack x determined using 711 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.09(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.085
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     290
_refine_ls_number_reflns         2590
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.084
_refine_ls_R_factor_all          0.0383
_refine_ls_R_factor_gt           0.0376
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0662P)^2^+0.6039P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1018
_refine_ls_wR_factor_ref         0.1029
_reflns_Friedel_coverage         0.401
_reflns_Friedel_fraction_full    0.438
_reflns_Friedel_fraction_max     0.438
_reflns_number_gt                2522
_reflns_number_total             2590
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6ra18676a2.cif
_cod_data_source_block           tb13
_cod_database_code               7226573
_shelx_shelxl_version_number     2014/7
_shelx_res_checksum              63109