Triple-Negative Breast Cancer Cells Exhibit Differential Sensitivity to Cardenolides from <i>Calotropis gigantea</i>.
Pederson, Petra J.; Cai, Shengxin; Carver, Chase; Powell, Douglas R.; Risinger, April L.; Grkovic, Tanja; O'Keefe, Barry R; Mooberry, Susan L.; Cichewicz, Robert H.; Journal of natural products 83 (2020) 2269–2280; doi:10.1021/acs.jnatprod.0c00423

data_1558566
_publ_section_title
;
 Triple-Negative Breast Cancer Cells Exhibit Differential Sensitivity to
 Cardenolides from <i>Calotropis gigantea</i>.
;
_journal_issue                   7
_journal_name_full               'Journal of natural products'
_journal_page_first              2269
_journal_page_last               2280
_journal_paper_doi               10.1021/acs.jnatprod.0c00423
_journal_volume                  83
_journal_year                    2020
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C57 H56 Br4 O13, 3(C H Cl3)'
_chemical_formula_sum            'C60 H59 Br4 Cl9 O13'
_chemical_formula_weight         1626.76
_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
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                90
_cell_angle_beta                 95.260(4)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   14.1567(17)
_cell_length_b                   6.2892(7)
_cell_length_c                   37.652(5)
_cell_measurement_reflns_used    9705
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.40
_cell_measurement_theta_min      2.50
_cell_volume                     3338.2(7)
_computing_cell_refinement       'SAINT (Bruker, 2016)'
_computing_data_collection       'APEX3 (Bruker, 2018)'
_computing_data_reduction        'SAINT (Bruker, 2016)'
_computing_molecular_graphics    'Mercury (CCDC, 2018)'
_computing_publication_material  'SHELXL-2018/3 (Sheldrick, 2015b)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2015b)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015a)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       '\k--geometry diffractometer'
_diffrn_measurement_device_type  'Bruker Photon II cmos'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'multilayer mirror'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0834
_diffrn_reflns_av_unetI/netI     0.0469
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       48
_diffrn_reflns_limit_l_min       -48
_diffrn_reflns_number            128169
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.124
_diffrn_reflns_theta_min         2.076
_diffrn_source                   'microfocus sealed tube'
_diffrn_source_type              'Incoatec I\mS 3.0'
_exptl_absorpt_coefficient_mu    2.831
_exptl_absorpt_correction_T_max  0.4912
_exptl_absorpt_correction_T_min  0.4256
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
 SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D., 
 J. Appl. Cryst. 48 (2015) 3-10 
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.618
_exptl_crystal_description       block
_exptl_crystal_F_000             1632
_exptl_crystal_size_max          0.128
_exptl_crystal_size_mid          0.082
_exptl_crystal_size_min          0.038
_refine_diff_density_max         0.858
_refine_diff_density_min         -0.904
_refine_diff_density_rms         0.087
_refine_ls_abs_structure_details
; 
 Flack x determined using 4806 quotients [(I+)-(I-)]/[(I+)+(I-)] 
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). 
;
_refine_ls_abs_structure_Flack   -0.002(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.009
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     780
_refine_ls_number_reflns         14702
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.009
_refine_ls_R_factor_all          0.0600
_refine_ls_R_factor_gt           0.0435
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0520P)^2^+4.9000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1006
_refine_ls_wR_factor_ref         0.1113
_reflns_Friedel_coverage         0.830
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.999
_reflns_number_gt                12380
_reflns_number_total             14702
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            np0c00423_si_005.cif
_cod_data_source_block           compound_4_deriv
_cod_depositor_comments
'Adding full bibliography for 1558566--1558571.cif.'
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               1558566
_shelx_estimated_absorpt_t_min   0.713
_shelx_estimated_absorpt_t_max   0.900
_shelx_res_checksum              15082
_shelx_hkl_checksum              42859