Antiproliferative Cardiac Glycosides from the Latex of Antiaris toxicaria.
Liu, Qian; Tang, Jin-Shan; Hu, Meng-Jie; Liu, Jie; Chen, Hai-Feng; Gao, Hao; Wang, Guang-Hui; Li, Shun-Lin; Hao, Xiao-Jiang; Zhang, Xiao-Kun; Yao, Xin-Sheng; Journal of natural products 76 (2013) 1771–1780; doi:10.1021/np4005147

data_1512277
_publ_section_title
;
 Antiproliferative Cardiac Glycosides from the Latex of Antiaris
 toxicaria.
;
_journal_issue                   9
_journal_name_full               'Journal of natural products'
_journal_page_first              1771
_journal_page_last               1780
_journal_paper_doi               10.1021/np4005147
_journal_volume                  76
_journal_year                    2013
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C29 H42 O10, 2(H2 O)'
_chemical_formula_sum            'C29 H46 O12'
_chemical_formula_weight         586.66
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2013-04-06
_audit_creation_method
;
  Olex2 1.1
  (compiled Nov  1 2011 20:42:30, GUI svn.r3906)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.99910(10)
_cell_length_b                   10.3062(2)
_cell_length_c                   30.5548(5)
_cell_measurement_reflns_used    4550
_cell_measurement_temperature    173.0
_cell_measurement_theta_max      62.6919
_cell_measurement_theta_min      4.2863
_cell_volume                     2833.85(8)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET)
(compiled Jan 20 2011,15:58:25)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET)
(compiled Jan 20 2011,15:58:25)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET)
(compiled Jan 20 2011,15:58:25)
;
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
SHELXL, G.M. Sheldrick, Acta Cryst.
2008). A64, 112-122
;
_computing_structure_solution
;
SHELXS, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_diffrn_ambient_temperature      173.0
_diffrn_detector_area_resol_mean 16.0288
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_details
;
  1 omega   71.00   99.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       33.1184   38.0000 -120.0000 28

  2 omega   61.00  101.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       33.1184   77.0000 -120.0000 40

  3 omega   14.00   47.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       33.1184   38.0000 -120.0000 33

  4 omega  -11.00   72.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       33.1184 -116.0000  -33.0000 83

  5 omega  -21.00    5.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      -64.0000   45.0000 -180.0000 26

  6 omega   45.00  119.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       90.5000  -77.0000  -90.0000 74

  7 omega   23.00   68.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       90.5000  -45.0000    0.0000 45

  8 omega   67.00  131.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       90.5000   45.0000  -30.0000 64

  9 omega   81.00  156.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       90.5000  111.0000   30.0000 75

 10 omega   27.00   54.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       90.5000  -45.0000  -60.0000 27

 11 omega   65.00  128.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       90.5000  -92.0000  153.0000 63
;
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0270619000
_diffrn_orient_matrix_UB_12      0.1451214000
_diffrn_orient_matrix_UB_13      -0.0092286000
_diffrn_orient_matrix_UB_21      -0.1663425000
_diffrn_orient_matrix_UB_22      -0.0276527000
_diffrn_orient_matrix_UB_23      -0.0073669000
_diffrn_orient_matrix_UB_31      -0.0299637000
_diffrn_orient_matrix_UB_32      0.0231577000
_diffrn_orient_matrix_UB_33      0.0490008000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.0196
_diffrn_reflns_av_unetI/netI     0.0286
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            7292
_diffrn_reflns_theta_full        62.78
_diffrn_reflns_theta_max         62.78
_diffrn_reflns_theta_min         4.53
_diffrn_source                   'Enhance Ultra (Cu) X-ray Source'
_diffrn_source_current           n/a
_diffrn_source_voltage           n/a
_exptl_absorpt_coefficient_mu    0.887
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.85039
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET)
(compiled Jan 20 2011,15:58:25)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.375
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1264
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.335
_refine_diff_density_min         -0.414
_refine_diff_density_rms         0.046
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.10(18)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.103
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     383
_refine_ls_number_reflns         4070
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.103
_refine_ls_R_factor_all          0.0385
_refine_ls_R_factor_gt           0.0369
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0606P)^2^+0.8491P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1029
_refine_ls_wR_factor_ref         0.1044
_reflns_number_gt                3908
_reflns_number_total             4070
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            np4005147_si_002.cif
_cod_data_source_block           antiaroside_J
_cod_database_code               1512277
_reflns_odcompleteness_completeness 99.54
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     62.30