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_1502003
_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 ad
_chemical_formula_moiety         'C32 H56 O7, 7(H2 O)'
_chemical_formula_sum            'C32 H70 O14'
_chemical_formula_weight         678.90
_space_group_IT_number           5
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C 2y'
_symmetry_space_group_name_H-M   'C 1 2 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_cell_angle_alpha                90
_cell_angle_beta                 105.051(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   50.084(4)
_cell_length_b                   5.9938(6)
_cell_length_c                   13.2247(10)
_cell_measurement_reflns_used    0
_cell_measurement_temperature    173
_cell_measurement_theta_max      0
_cell_measurement_theta_min      0
_cell_volume                     3833.8(6)
_computing_cell_refinement       'SAINT (Siemens ,1995)'
_computing_data_collection       'SMART (Siemens, 1993)'
_computing_data_reduction        'SAINT (Siemens ,1995)'
_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    'SHELXS 86 (Sheldrick, 1986)'
_diffrn_ambient_temperature      173
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.966
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Bruker SMART'
_diffrn_measurement_method       '\f & \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54180
_diffrn_reflns_av_R_equivalents  0.069
_diffrn_reflns_limit_h_max       58
_diffrn_reflns_limit_h_min       -59
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            23579
_diffrn_reflns_theta_full        32.828
_diffrn_reflns_theta_max         66.997
_diffrn_reflns_theta_min         1.827
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.749
_exptl_absorpt_correction_T_max  0.99
_exptl_absorpt_correction_T_min  0.93
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.18
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1456
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.010
_refine_diff_density_max         0.70
_refine_diff_density_min         -0.70
_refine_ls_abs_structure_details 'Flack (1983), 0 Friedel-pairs'
_refine_ls_abs_structure_Flack   0.2(3)
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9263
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     443
_refine_ls_number_reflns         4707
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.1040
_refine_ls_R_factor_gt           0.0833
_refine_ls_shift/su_max          0.0012236
_refine_ls_shift/su_mean         0.0000568
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] 
 where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ 
 A~i~ are: 
 1.25 1.00 0.699 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1160
_refine_ls_wR_factor_gt          0.0862
_refine_ls_wR_factor_ref         0.0862
_reflns_limit_h_max              56
_reflns_limit_h_min              -59
_reflns_limit_k_max              6
_reflns_limit_k_min              -7
_reflns_limit_l_max              15
_reflns_limit_l_min              0
_reflns_number_gt                4707
_reflns_number_total             6224
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   0.00
_oxford_diffrn_Wilson_scale      0.00
_oxford_refine_ls_r_factor_ref   0.0833
_oxford_refine_ls_scale          0.2546(8)
_oxford_reflns_number_all        6198
_oxford_reflns_threshold_expression_ref I>2.0\s(I)
_cod_data_source_file            ol200047v_si_002.cif
_cod_data_source_block           2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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_sg_symbol_H-M      'C 2'
_cod_database_code               1502003