The New Pentacyclic Saponine Ecdysantherin [3β-Hydroxy-20-methylpregn-5,14-dien-16-one-(18–20)-lactone] from <i>Ecdysanthera rosea Hook</i>. <i>et Arn</i>. (<i>Apocynaceae</i>) of Vietnam
Luger, P.; Weber, M.; Dung, N. X.; Ky, P. T.; The, C. L.; Acta Crystallographica Section C 52 (1996) 1574–1576; doi:10.1107/S0108270195017045

data_2005011
_publ_contact_author
;
     Prof. Dr. Peter Luger
     Institut f\"ur Kristallographie
     Fachbereich Chemie der Freien Universit\"at
     Takustrasse 6
     14195 Berlin
     Germany
;
_publ_section_title
;
 The New Pentacyclic Saponine Ecdysantherin
 [3\b-Hydroxy-20-methylpregn-5,14-dien-16-one-(18--20)-lactone] from
 <i>Ecdysanthera rosea Hook</i>. <i>et Arn</i>. (<i>Apocynaceae</i>) of
 Vietnam
;
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              1574
_journal_page_last               1576
_journal_paper_doi               10.1107/S0108270195017045
_journal_volume                  52
_journal_year                    1996
_chemical_formula_moiety         'C21 H26 O4'
_chemical_formula_sum            'C21 H26 O4'
_chemical_formula_weight         342.42
_chemical_melting_point          240.5(5)
_chemical_name_common
;
3\b-hydroxy-20methyl-pregn-5,14-dien-16-on(18--20) lactone
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   6.0860(10)
_cell_length_b                   11.9900(10)
_cell_length_c                   23.831(2)
_cell_measurement_reflns_used    90
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      30
_cell_measurement_theta_min      20
_cell_volume                     1739.0(4)
_computing_cell_refinement       'STOE software'
_computing_data_collection       'STOE software'
_computing_data_reduction        'in-house program'
_computing_molecular_graphics    'SCHAKAL88 (Keller, 1988)'
_computing_publication_material  SHELXL-93
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1985)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'STOE four-circle, MicroVAX-controlled'
_diffrn_measurement_method       \w/2\q
_diffrn_radiation_monochromator  none
_diffrn_radiation_source         xray_tube
_diffrn_radiation_type           'Cu K\a, Ni filter'
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0547
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            1525
_diffrn_reflns_theta_max         59.99
_diffrn_reflns_theta_min         3.71
_diffrn_standards_decay_%        3
_diffrn_standards_interval_time  90
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.718
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.308
_exptl_crystal_density_meas      ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             736
_exptl_crystal_size_max          0.43
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.215
_refine_diff_density_min         -0.194
_refine_ls_abs_structure_details 'Flack (1983)'
_refine_ls_abs_structure_Flack   '0.1(7) (indeterminate)'
_refine_ls_extinction_coef       0.0014(4)
_refine_ls_extinction_method     'SHELXL-93 (Sheldrick, 1993)'
_refine_ls_goodness_of_fit_all   1.052
_refine_ls_goodness_of_fit_obs   1.103
_refine_ls_hydrogen_treatment    'noref (riding)'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     230
_refine_ls_number_reflns         1520
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.122
_refine_ls_restrained_S_obs      1.103
_refine_ls_R_factor_all          0.0909
_refine_ls_R_factor_obs          0.0436
_refine_ls_shift/esd_max         0.000
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0523P)^2^+1.1728P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1323
_refine_ls_wR_factor_obs         0.1081
_reflns_number_observed          1121
_reflns_number_total             1525
_reflns_observed_criterion       >2sigma(F)
_cod_data_source_file            jz1101.cif
_cod_data_source_block           kd42
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value '240-241' was changed to '240.5(5)' -
the average value was taken and precision was estimated.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc w =
1/[\s^2^(Fo^2^)+(0.0523P)^2^+1.1728P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to 'w =
1/[\s^2^(Fo^2^)+(0.0523P)^2^+1.1728P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_database_code               2005011