11α,12β-Acetonyltenacissoside F acetone solvate: a new polyoxypregnane glycoside from the stems of <i>Marsdenia tenacissima</i>
Qi-Fa Li; Xiao-Ling Wang; Kai-Bei Yu; Shu-Lin Peng; Li-Sheng Ding; Acta Crystallographica Section E 62 (2006) o5255–o5256; doi:10.1107/S1600536806042048

data_2210992
_publ_section_title
;
 11\a,12\b-Acetonyltenacissoside F acetone solvate: a new
 polyoxypregnane glycoside from the stems of <i>Marsdenia
 tenacissima</i>
;
_journal_coeditor_code           FL2058
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o5255
_journal_page_last               o5256
_journal_paper_doi               10.1107/S1600536806042048
_journal_volume                  62
_journal_year                    2006
_chemical_formula_iupac          'C38 H60 O12, C3 H6 O'
_chemical_formula_moiety         'C38 H60 O12, C3 H6 O'
_chemical_formula_sum            'C41 H66 O13'
_chemical_formula_weight         766.94
_chemical_melting_point          375.0(10)
_chemical_name_systematic
;
11\a,12\b-acetonyltenacigenin B 3-O-6-deoxy
-3-O-methyl-\b-D-allopyranosyl-(1\\rightarrow4)-\b-D-oleandropyranoside
acetone solvate
;
_space_group_IT_number           1
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  'P 1'
_symmetry_space_group_name_H-M   'P 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                74.57(2)
_cell_angle_beta                 81.76(2)
_cell_angle_gamma                79.03(2)
_cell_formula_units_Z            1
_cell_length_a                   6.3280(10)
_cell_length_b                   10.558(2)
_cell_length_c                   17.553(4)
_cell_measurement_reflns_used    28
_cell_measurement_temperature    288(2)
_cell_measurement_theta_max      14.23
_cell_measurement_theta_min      4.75
_cell_volume                     1104.5(4)
_computing_cell_refinement       XSCANS
_computing_data_collection       'XSCANS (Siemens, 1994)'
_computing_data_reduction        'SHELXTL (Siemens, 1997)'
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      288(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Siemens P4'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0122
_diffrn_reflns_av_sigmaI/netI    0.0343
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            4887
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         1.21
_diffrn_standards_decay_%        5.57
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.085
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.153
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             416
_exptl_crystal_size_max          0.54
_exptl_crystal_size_mid          0.54
_exptl_crystal_size_min          0.50
_refine_diff_density_max         0.222
_refine_diff_density_min         -0.227
_refine_ls_extinction_coef       0.023(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL97
_refine_ls_goodness_of_fit_ref   0.965
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     523
_refine_ls_number_reflns         4316
_refine_ls_number_restraints     15
_refine_ls_restrained_S_all      0.967
_refine_ls_R_factor_all          0.0559
_refine_ls_R_factor_gt           0.0412
_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^)+(0.063P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0976
_refine_ls_wR_factor_ref         0.1026
_reflns_number_gt                3221
_reflns_number_total             4316
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            fl2058.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
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_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_chemical_melting_point' value '374--376' was changed to '375.0(10)'
- the average value was taken and precision was estimated.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 

The following automatic conversions were performed:

'_chemical_melting_point' value '374--376' was changed to '375.0(10)'
- the average value was taken and precision was
estimated.

'_symmetry_cell_setting' value 'Triclinic' changed to
'triclinic' 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_database_code               2210992
_cod_database_fobs_code          2210992