Walrobsins A and B, Two Anti-inflammatory Limonoids from Root Barks of Walsura robusta.
An, Fa-Liang; Sun, Dong-Mei; Li, Rui-Jun; Zhou, Miao-Miao; Yang, Ming-Hua; Yin, Yong; Kong, Ling-Yi; Luo, Jun; Organic letters 19 (2017) 4568–4571; doi:10.1021/acs.orglett.7b02173

data_1547051
_publ_section_title
;
 Walrobsins A and B, Two Anti-inflammatory Limonoids from Root Barks of
 Walsura robusta.
;
_journal_issue                   17
_journal_name_full               'Organic letters'
_journal_page_first              4568
_journal_page_last               4571
_journal_paper_doi               10.1021/acs.orglett.7b02173
_journal_volume                  19
_journal_year                    2017
_chemical_absolute_configuration ad
_chemical_formula_sum            'C33 H42 O8'
_chemical_formula_weight         566.66
_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   geom
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.54080(10)
_cell_length_b                   16.31220(10)
_cell_length_c                   18.8674(2)
_cell_measurement_reflns_used    15892
_cell_measurement_temperature    289(2)
_cell_measurement_theta_max      69.9690
_cell_measurement_theta_min      4.6270
_cell_volume                     2936.36(5)
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      289(2)
_diffrn_detector_area_resol_mean 5.2169
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0278
_diffrn_reflns_av_unetI/netI     0.0199
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            26402
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         70.079
_diffrn_reflns_theta_min         3.582
_diffrn_source                   'micro-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    0.739
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.75453
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.282
_exptl_crystal_description       block
_exptl_crystal_F_000             1216
_exptl_crystal_size_max          0.350
_exptl_crystal_size_mid          0.320
_exptl_crystal_size_min          0.260
_refine_diff_density_max         0.744
_refine_diff_density_min         -0.389
_refine_diff_density_rms         0.051
_refine_ls_abs_structure_details
;
 Flack x determined using 2310 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.04(5)
_refine_ls_extinction_coef       0.0049(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     379
_refine_ls_number_reflns         5502
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0452
_refine_ls_R_factor_gt           0.0441
_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^)+(0.0949P)^2^+0.4999P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1301
_refine_ls_wR_factor_ref         0.1339
_reflns_Friedel_coverage         0.761
_reflns_Friedel_fraction_full    0.996
_reflns_Friedel_fraction_max     0.979
_reflns_number_gt                5396
_reflns_number_total             5502
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ol7b02173_si_002.cif
_cod_data_source_block           shelxl
_cod_database_code               1547051
_shelx_estimated_absorpt_t_min   0.782
_shelx_estimated_absorpt_t_max   0.831
_shelxl_version_number           2013-4
_shelx_res_checksum              74848
_shelx_hkl_checksum              47751