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_1516020
_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 H60 O12'
_chemical_formula_weight         684.84
_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                 116.3950(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   15.2751(3)
_cell_length_b                   8.0457(2)
_cell_length_c                   15.9079(3)
_cell_measurement_reflns_used    7115
_cell_measurement_temperature    140(2)
_cell_measurement_theta_max      69.18
_cell_measurement_theta_min      3.23
_cell_volume                     1751.25(7)
_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 0.992
_diffrn_measured_fraction_theta_max 0.977
_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  0.0333
_diffrn_reflns_av_unetI/netI     0.0400
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.977
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            12092
_diffrn_reflns_point_group_measured_fraction_full 0.751
_diffrn_reflns_point_group_measured_fraction_max 0.735
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         69.571
_diffrn_reflns_theta_min         3.230
_exptl_absorpt_coefficient_mu    0.791
_exptl_absorpt_correction_T_max  0.7532
_exptl_absorpt_correction_T_min  0.5520
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.299
_exptl_crystal_description       block
_exptl_crystal_F_000             744
_exptl_crystal_size_max          0.290
_exptl_crystal_size_mid          0.160
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.553
_refine_diff_density_min         -0.286
_refine_diff_density_rms         0.054
_refine_ls_abs_structure_details
; 
 Flack x determined using 1339 quotients [(I+)-(I-)]/[(I+)+(I-)] 
 (Parsons and Flack (2004), Acta Cryst. A60, s61). 
;
_refine_ls_abs_structure_Flack   0.11(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     447
_refine_ls_number_reflns         4840
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0472
_refine_ls_R_factor_gt           0.0468
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1008P)^2^+0.4717P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1362
_refine_ls_wR_factor_ref         0.1368
_reflns_Friedel_coverage         0.398
_reflns_Friedel_fraction_full    0.469
_reflns_Friedel_fraction_max     0.453
_reflns_number_gt                4759
_reflns_number_total             4840
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            np500077z_si_004.cif
_cod_data_source_block           cu_dm13474_0m
_cod_depositor_comments
'Adding full bibliography for 1516020--1516024.cif.'
_cod_database_code               1516020
_shelx_estimated_absorpt_t_min   0.803
_shelx_estimated_absorpt_t_max   0.925
_shelxl_version_number           2013-4
_shelx_res_checksum              58047
_shelx_hkl_checksum              12558