Crystal and molecular structure of jatrophane diterpenoid (2<i>R</i>,3<i>R</i>,4<i>S</i>,5<i>R</i>,7<i>S</i>,8<i>S</i>,9<i>S</i>,13<i>S</i>,14<i>S</i>,15<i>R</i>)-2,3,8,9-tetraacetoxy-5,14-bis(benzoyloxy)-15-hydroxy-7-(isobutanoyloxy)jatropha-6(17),11(<i>E</i>)-diene
Yang, Hequn; Zhao, Jiangyu; Talipov, Samat; Izotova, Lidiya; Aisa, Hadji Akbar; Ibragimov, Bakhtiyar; Acta Crystallographica Section E 75 (2019) 1884–1887; doi:10.1107/S205698901901541X

data_2243205
_publ_section_title
;
 Crystal and molecular structure of jatrophane diterpenoid
 (2<i>R</i>,3<i>R</i>,4<i>S</i>,5<i>R</i>,7<i>S</i>,8<i>S</i>,9<i>S</i>,13<i>S</i>,14<i>S</i>,15<i>R</i>)-2,3,8,9-tetraacetoxy-5,14-bis(benzoyloxy)-15-hydroxy-7-(isobutanoyloxy)jatropha-6(17),11(<i>E</i>)-diene
;
_journal_coeditor_code           FY2141
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              1884
_journal_page_last               1887
_journal_paper_doi               10.1107/S205698901901541X
_journal_volume                  75
_journal_year                    2019
_chemical_absolute_configuration rm
_chemical_formula_iupac          'C46 H56 O15'
_chemical_formula_moiety         'C46 H56 O15'
_chemical_formula_sum            'C46 H56 O15'
_chemical_formula_weight         848.90
_chemical_melting_point          166
_chemical_name_common            jatrophan
_chemical_name_systematic
(2<i>R</i>,3<i>R</i>,4<i>S</i>,5<i>R</i>,7<i>S</i>,8<i>S</i>,9<i>S</i>,13<i>S</i>,14<i>S</i>,15<i>R</i>)-2,3,8,9-Tetraacetoxy-5,14-bis(benzoyloxy)-15-hydroxy-7-(isobutanoyloxy)jatropha-6(17),11(<i>E</i>)-diene
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.9730(5)
_cell_length_b                   20.9171(9)
_cell_length_c                   23.9201(11)
_cell_measurement_reflns_used    5355
_cell_measurement_temperature    104(2)
_cell_measurement_theta_max      69.5640
_cell_measurement_theta_min      4.2370
_cell_volume                     4489.5(4)
_computing_cell_refinement
;
CrysAlis PRO (Agilent, 2014)
;
_computing_data_collection
;
CrysAlis PRO (Agilent, 2014)
;
_computing_data_reduction
;
CrysAlis PRO (Agilent, 2014)
;
_computing_molecular_graphics
;
XP (Siemens, 1994)
;
_computing_publication_material
;
XP (Siemens, 1994)
;
_computing_structure_refinement
;
SHELXL2018 (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      104(7)
_diffrn_detector_area_resol_mean 10.2576
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Agilent Xcalibur Ruby'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0584
_diffrn_reflns_av_unetI/netI     0.0422
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            37870
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.461
_diffrn_reflns_theta_min         3.696
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.778
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.74820
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(CrysAlis PRO; Agilent, 2014)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.256
_exptl_crystal_density_meas      1.256
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1808
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.258
_refine_diff_density_min         -0.186
_refine_ls_abs_structure_details
;
Flack <i>x</i> determined using 2403 quotients
[(<i>I</i>^+^)-(<i>I</i>^-^)]/[(<i>I</i>^+^)+(<i>I</i>^-^)]
(Parsons <i>et al.</i>,  2013)
;
_refine_ls_abs_structure_Flack   -0.06(11)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     587
_refine_ls_number_reflns         9301
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.016
_refine_ls_R_factor_all          0.0793
_refine_ls_R_factor_gt           0.0563
_refine_ls_shift/su_max          0.010
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0710P)^2^+1.4583P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1360
_refine_ls_wR_factor_ref         0.1534
_reflns_number_gt                7007
_reflns_number_total             9301
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            fy2141sup1.cif
_cod_data_source_block           I
_cod_database_code               2243205
_cod_database_fobs_code          2243205
_shelx_estimated_absorpt_t_min   0.830
_shelx_estimated_absorpt_t_max   0.925
_shelx_hkl_checksum              24620
_shelx_res_checksum              94960