Limonoids and Triterpenoids as 11β-HSD1 Inhibitors from Walsura robusta.
Wang, Guo-Cai; Yu, Jin-Hai; Shen, Yu; Leng, Ying; Zhang, Hua; Yue, Jian-Min; Journal of natural products 79 (2016) 899–906; doi:10.1021/acs.jnatprod.5b00952

data_1542618
_publ_section_title
;
 Limonoids and Triterpenoids as 11\b-HSD1 Inhibitors from Walsura robusta.
;
_journal_issue                   4
_journal_name_full               'Journal of natural products'
_journal_page_first              899
_journal_page_last               906
_journal_paper_doi               10.1021/acs.jnatprod.5b00952
_journal_volume                  79
_journal_year                    2016
_chemical_absolute_configuration ad
_chemical_formula_sum            'C27 H32 O8'
_chemical_formula_weight         484.52
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 103.8820(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   7.50130(10)
_cell_length_b                   11.6919(2)
_cell_length_c                   14.6190(2)
_cell_measurement_reflns_used    8380
_cell_measurement_temperature    140(2)
_cell_measurement_theta_max      69.30
_cell_measurement_theta_min      3.11
_cell_volume                     1244.70(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      140(2)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.978
_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  0.0486
_diffrn_reflns_av_unetI/netI     0.0572
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.978
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            9728
_diffrn_reflns_point_group_measured_fraction_full 0.939
_diffrn_reflns_point_group_measured_fraction_max 0.922
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         69.460
_diffrn_reflns_theta_min         3.114
_exptl_absorpt_coefficient_mu    0.784
_exptl_absorpt_correction_T_max  0.7532
_exptl_absorpt_correction_T_min  0.4701
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.293
_exptl_crystal_description       prism
_exptl_crystal_F_000             516
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.284
_refine_diff_density_min         -0.254
_refine_diff_density_rms         0.058
_refine_ls_abs_structure_details
; 
 Flack x determined using 1880 quotients [(I+)-(I-)]/[(I+)+(I-)] 
 (Parsons and Flack (2004), Acta Cryst. A60, s61). 
;
_refine_ls_abs_structure_Flack   -0.01(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     324
_refine_ls_number_reflns         4294
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.0424
_refine_ls_R_factor_gt           0.0423
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0716P)^2^+0.1051P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1051
_refine_ls_wR_factor_ref         0.1053
_reflns_Friedel_coverage         0.791
_reflns_Friedel_fraction_full    0.884
_reflns_Friedel_fraction_max     0.860
_reflns_number_gt                4269
_reflns_number_total             4294
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            np5b00952_si_003.cif
_cod_data_source_block           cu_dm14138_0m
_cod_depositor_comments
'Adding full bibliography for 1542618--1542619.cif.'
_cod_database_code               1542618
_shelx_estimated_absorpt_t_min   0.828
_shelx_estimated_absorpt_t_max   0.926
_shelxl_version_number           2013-4
_shelx_res_checksum              98099
_shelx_hkl_checksum              64888