Structural modification of oridonin via DAST induced rearrangement
Luo, Dong-Dong; Peng, Kai; Yang, Jia-Yu; Piyachaturawat, Pawinee; Saengsawang, Witchuda; Ao, Lei; Zhao, Wan-Zhou; Tang, Yu; Wan, Sheng-Biao; RSC Advances 8 (2018) 29548–; doi:10.1039/C8RA05728A

data_7231394
_publ_section_title
;
 Structural modification of oridonin via DAST induced rearrangement
;
_journal_issue                   52
_journal_name_full               'RSC Advances'
_journal_page_first              29548
_journal_paper_doi               10.1039/C8RA05728A
_journal_volume                  8
_journal_year                    2018
_chemical_absolute_configuration syn
_chemical_formula_sum            'C31 H34 O8'
_chemical_formula_weight         534.58
_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_block_doi                 10.5517/ccdc.csd.cc1qcvrp
_audit_creation_method           SHELXL-2016/4
_audit_update_record
;
2018-01-30 deposited with the CCDC.
2018-08-10 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.3902(4)
_cell_length_b                   8.3748(5)
_cell_length_c                   43.293(3)
_cell_measurement_reflns_used    10740
_cell_measurement_temperature    150.01(10)
_cell_measurement_theta_max      70.7750
_cell_measurement_theta_min      4.0820
_cell_volume                     2679.5(3)
_computing_structure_refinement  'SHELXL-2016/4 (Sheldrick, 2016)'
_diffrn_ambient_temperature      150.01(10)
_diffrn_detector_area_resol_mean 16.0450
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.964
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0411
_diffrn_reflns_av_unetI/netI     0.0300
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.964
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       52
_diffrn_reflns_limit_l_min       -52
_diffrn_reflns_number            17966
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.956
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.657
_diffrn_reflns_theta_min         4.085
_diffrn_source                   'micro-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    0.782
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.83891
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.325
_exptl_crystal_description       block
_exptl_crystal_F_000             1136
_exptl_crystal_size_max          0.160
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.090
_refine_diff_density_max         0.298
_refine_diff_density_min         -0.264
_refine_diff_density_rms         0.061
_refine_ls_abs_structure_details
;
 Flack x determined using 1855 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.17(11)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.159
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     364
_refine_ls_number_reflns         5085
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.159
_refine_ls_R_factor_all          0.0564
_refine_ls_R_factor_gt           0.0506
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0251P)^2^+3.5299P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1164
_refine_ls_wR_factor_ref         0.1218
_reflns_Friedel_coverage         0.706
_reflns_Friedel_fraction_full    0.996
_reflns_Friedel_fraction_max     0.944
_reflns_number_gt                4899
_reflns_number_total             5085
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8ra05728a2.cif
_cod_data_source_block           shelx
_cod_database_code               7231394
_shelx_shelxl_version_number     2016/4
_shelx_estimated_absorpt_t_min   0.885
_shelx_estimated_absorpt_t_max   0.933
_shelx_res_checksum              31298