Capsisteroids A–F, Withanolides from the Leaves of Solanum capsicoides
Chen, Bo-Wei; Chen, Yih Yang; Lin, You-Cheng; Huang, Chiung-Yao; Chokkalingam, Uvarani; Hwang, Tsong-Long; Chiang, Michael, Y.; Liu, Ho-Yih; Sheu, Jyh-Horng; RSC Adv.  (2015) –; doi:10.1039/C5RA12014D

data_7222458
_publ_section_title
;
 Capsisteroids A--F, Withanolides from the Leaves of Solanum capsicoides
;
_journal_name_full               'RSC Adv.'
_journal_paper_doi               10.1039/C5RA12014D
_journal_year                    2015
_chemical_absolute_configuration rm
_chemical_compound_source        'leaves from Solanum capsicoides'
_chemical_formula_moiety         'C28 H42 O6 2.5(H2 O)'
_chemical_formula_sum            'C28 H47 O8.5'
_chemical_formula_weight         519.65
_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   mixed
_audit_creation_method           SHELXL-2014/6
_audit_update_record
;
2015-08-18 deposited with the CCDC.
2015-09-24 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.5227(4)
_cell_length_b                   9.6240(6)
_cell_length_c                   37.396(2)
_cell_measurement_reflns_used    9856
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      66.1844
_cell_measurement_theta_min      3.1902
_cell_volume                     2707.4(3)
_computing_cell_refinement       'SAINT V7.68A (Bruker AXS, 2009)'
_computing_data_collection       'APEX2 (Bruker AXS, 2010)'
_computing_data_reduction        'SAINT V7.68A (Bruker AXS, 2009)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.3333
_diffrn_measured_fraction_theta_full 0.920
_diffrn_measured_fraction_theta_max 0.950
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0520
_diffrn_reflns_av_unetI/netI     0.0550
_diffrn_reflns_Laue_measured_fraction_full 0.920
_diffrn_reflns_Laue_measured_fraction_max 0.950
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       44
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            13445
_diffrn_reflns_point_group_measured_fraction_full 0.921
_diffrn_reflns_point_group_measured_fraction_max 0.952
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         66.257
_diffrn_reflns_theta_min         2.363
_exptl_absorpt_coefficient_mu    0.758
_exptl_absorpt_correction_T_max  0.9492
_exptl_absorpt_correction_T_min  0.7735
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2008/1 (Bruker AXS)'
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.275
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Lamellar
_exptl_crystal_F_000             1132
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: methanol and water 4:1'
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.416
_refine_diff_density_min         -0.443
_refine_diff_density_rms         0.096
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.3(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.113
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     344
_refine_ls_number_reflns         4384
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.112
_refine_ls_R_factor_all          0.0943
_refine_ls_R_factor_gt           0.0936
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0528P)^2^+14.3446P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2351
_refine_ls_wR_factor_ref         0.2355
_reflns_Friedel_coverage         0.728
_reflns_Friedel_fraction_full    0.921
_reflns_Friedel_fraction_max     0.954
_reflns_number_gt                4291
_reflns_number_total             4384
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5ra12014d2.cif
_cod_data_source_block           CU_130829LT_0M
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_absolute_configuration' value 'RM' changed to 'rm'
according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

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

Automatic conversion script
Id: cif_fix_values 3271 2015-04-21 07:52:19Z andrius 
;
_cod_original_formula_sum        'C28 H47 O8.50'
_cod_database_code               7222458
_shelxl_version_number           2014/6
_shelx_res_checksum              97078
_shelx_hkl_checksum              8359