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_7226574
_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 H32 O6'
_chemical_formula_weight         404.48
_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'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.7367(5)
_cell_length_b                   11.1799(5)
_cell_length_c                   16.8458(9)
_cell_measurement_reflns_used    2453
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      62.8670
_cell_measurement_theta_min      4.8520
_cell_volume                     2022.09(17)
_computing_cell_refinement       'CrysAlis PRO '
_computing_data_collection       'CrysAlis PRO '
_computing_data_reduction        'CrysAlis PRO '
_computing_molecular_graphics    'OLEX2 (Dolomanov <i>et al.</i>, 2009)'
_computing_publication_material  'XP (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0282
_diffrn_reflns_av_unetI/netI     0.0330
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            5049
_diffrn_reflns_point_group_measured_fraction_full 0.907
_diffrn_reflns_point_group_measured_fraction_max 0.907
_diffrn_reflns_theta_full        62.580
_diffrn_reflns_theta_max         62.580
_diffrn_reflns_theta_min         4.747
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.774
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.927
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.329
_exptl_crystal_description       block
_exptl_crystal_F_000             872
_exptl_crystal_size_max          0.43
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.23
_refine_diff_density_max         0.844
_refine_diff_density_min         -0.608
_refine_diff_density_rms         0.073
_refine_ls_abs_structure_details
;
 Flack x determined using 976 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.11(14)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     266
_refine_ls_number_reflns         2932
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0662
_refine_ls_R_factor_gt           0.0633
_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^)+(0.1125P)^2^+2.0762P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1777
_refine_ls_wR_factor_ref         0.1817
_reflns_Friedel_coverage         0.581
_reflns_Friedel_fraction_full    0.785
_reflns_Friedel_fraction_max     0.785
_reflns_number_gt                2782
_reflns_number_total             2932
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6ra18676a2.cif
_cod_data_source_block           ZPW
_cod_database_code               7226574
_shelx_shelxl_version_number     2014/7
_shelx_res_checksum              73403