Dammarane-Type Triterpenoids from Gentianella azurea.
Huang, Yu-Jie; Lu, Hui; Yu, Xue-Li; Zhang, Shu-Wei; Wang, Wen-Qiong; Fen, Lin-Yin; Xuan, Li-Jiang; Journal of natural products 77 (2014) 1201–; doi:10.1021/np500077z

data_1516021
_publ_section_title
;
 Dammarane-Type Triterpenoids from Gentianella azurea.
;
_journal_issue                   5
_journal_name_full               'Journal of natural products'
_journal_page_first              1201
_journal_paper_doi               10.1021/np500077z
_journal_volume                  77
_journal_year                    2014
_chemical_absolute_configuration ad
_chemical_formula_sum            'C36.5 H63 O12'
_chemical_formula_weight         693.87
_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-2013
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   7.31720(10)
_cell_length_b                   23.8986(3)
_cell_length_c                   40.6627(5)
_cell_measurement_reflns_used    9692
_cell_measurement_temperature    140(2)
_cell_measurement_theta_max      69.24
_cell_measurement_theta_min      3.70
_cell_volume                     7110.72(16)
_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 0.975
_diffrn_measured_fraction_theta_max 0.965
_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  0.0534
_diffrn_reflns_av_unetI/netI     0.0454
_diffrn_reflns_Laue_measured_fraction_full 0.975
_diffrn_reflns_Laue_measured_fraction_max 0.965
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       49
_diffrn_reflns_limit_l_min       -48
_diffrn_reflns_number            48526
_diffrn_reflns_point_group_measured_fraction_full 0.963
_diffrn_reflns_point_group_measured_fraction_max 0.948
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         69.650
_diffrn_reflns_theta_min         2.144
_exptl_absorpt_coefficient_mu    0.784
_exptl_absorpt_correction_T_max  0.7532
_exptl_absorpt_correction_T_min  0.6377
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.296
_exptl_crystal_description       prism
_exptl_crystal_F_000             3024
_exptl_crystal_size_max          0.350
_exptl_crystal_size_mid          0.040
_exptl_crystal_size_min          0.020
_refine_diff_density_max         0.189
_refine_diff_density_min         -0.173
_refine_diff_density_rms         0.039
_refine_ls_abs_structure_details
; 
 Flack x determined using 4830 quotients [(I+)-(I-)]/[(I+)+(I-)] 
 (Parsons and Flack (2004), Acta Cryst. A60, s61). 
;
_refine_ls_abs_structure_Flack   -0.05(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     912
_refine_ls_number_reflns         12683
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0382
_refine_ls_R_factor_gt           0.0344
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0510P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0860
_refine_ls_wR_factor_ref         0.0890
_reflns_Friedel_coverage         0.751
_reflns_Friedel_fraction_full    0.946
_reflns_Friedel_fraction_max     0.926
_reflns_number_gt                11789
_reflns_number_total             12683
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            np500077z_si_003.cif
_cod_data_source_block           cu_dm13353_0m
_cod_depositor_comments
'Adding full bibliography for 1516020--1516024.cif.'
_cod_original_formula_sum        'C36.50 H63 O12'
_cod_database_code               1516021
_shelx_estimated_absorpt_t_min   0.771
_shelx_estimated_absorpt_t_max   0.984
_shelxl_version_number           2013-4
_shelx_res_checksum              92886
_shelx_hkl_checksum              64454