Phyteumosides A and B: new saponins with unique triterpenoid aglycons from Phyteuma orbiculare L.
Abbet, Christian; Neuburger, Markus; Wagner, Trixie; Quitschau, Melanie; Hamburger, Matthias; Potterat, Olivier; Organic letters 13 (2011) 1354–1357; doi:10.1021/ol200047v

data_1502002
_publ_section_title
;
 Phyteumosides A and B: new saponins with unique triterpenoid aglycons
 from Phyteuma orbiculare L.
;
_journal_issue                   6
_journal_name_full               'Organic letters'
_journal_page_first              1354
_journal_page_last               1357
_journal_paper_doi               10.1021/ol200047v
_journal_volume                  13
_journal_year                    2011
_chemical_absolute_configuration unk
_chemical_formula_moiety         'C32 H52 O6, 2.38(H2 O)'
_chemical_formula_sum            'C32 H56.76 O8.38'
_chemical_formula_weight         571.77
_space_group_IT_number           18
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ac'
_symmetry_space_group_name_H-M   'P 21 2 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   6.4777(15)
_cell_length_b                   16.504(5)
_cell_length_c                   29.762(7)
_cell_measurement_reflns_used    1279
_cell_measurement_temperature    123
_cell_measurement_theta_max      21
_cell_measurement_theta_min      3
_cell_volume                     3181.8(14)
_computing_cell_refinement       'Apex2 (Bruker AXS, 2006)'
_computing_data_collection       'Apex2 (Bruker AXS, 2006)'
_computing_data_reduction        'Apex2 (Bruker AXS, 2006)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'Superflip (Palatinus & Chapuis, 2007)'
_diffrn_ambient_temperature      123
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Bruker Kappa Apex2'
_diffrn_measurement_method       '\f & \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.122
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            10935
_diffrn_reflns_theta_full        25.201
_diffrn_reflns_theta_max         27.098
_diffrn_reflns_theta_min         2.395
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.085
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.99
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.193
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1248
_exptl_crystal_size_max          0.270
_exptl_crystal_size_mid          0.090
_exptl_crystal_size_min          0.010
_refine_diff_density_max         1.02
_refine_diff_density_min         -1.12
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9538
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     373
_refine_ls_number_reflns         3968
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.1551
_refine_ls_R_factor_gt           0.0880
_refine_ls_shift/su_max          0.0041952
_refine_ls_shift/su_mean         0.0004427
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[\s^2^(F^2^) + ( 0.11P)^2^ + 3.27P] 
 ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2294
_refine_ls_wR_factor_gt          0.1988
_refine_ls_wR_factor_ref         0.2294
_reflns_limit_h_max              8
_reflns_limit_h_min              0
_reflns_limit_k_max              21
_reflns_limit_k_min              0
_reflns_limit_l_max              38
_reflns_limit_l_min              0
_reflns_number_gt                2173
_reflns_number_total             3995
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.14
_oxford_diffrn_Wilson_scale      29.24
_oxford_refine_ls_r_factor_ref   0.1551
_oxford_refine_ls_scale          0.1952(3)
_oxford_reflns_number_all        3968
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_cod_data_source_file            ol200047v_si_002.cif
_cod_data_source_block           1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_cell_volume        3181.9(14)
_cod_database_code               1502002