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_1516022
_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 H68 O15.5'
_chemical_formula_weight         754.90
_chemical_name_systematic
; 
 ? 
;
_space_group_crystal_system      triclinic
_space_group_IT_number           1
_space_group_name_Hall           'P 1'
_space_group_name_H-M_alt        'P 1'
_symmetry_space_group_name_Hall  'P 1'
_symmetry_space_group_name_H-M   'P 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                85.657(2)
_cell_angle_beta                 88.636(2)
_cell_angle_gamma                77.863(2)
_cell_formula_units_Z            2
_cell_length_a                   7.1558(3)
_cell_length_b                   12.8203(4)
_cell_length_c                   21.0330(7)
_cell_measurement_reflns_used    9002
_cell_measurement_temperature    140(2)
_cell_measurement_theta_max      68.79
_cell_measurement_theta_min      4.22
_cell_volume                     1880.95(12)
_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 0.956
_diffrn_measured_fraction_theta_max 0.940
_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  0.0442
_diffrn_reflns_av_unetI/netI     0.0656
_diffrn_reflns_Laue_measured_fraction_full 0.956
_diffrn_reflns_Laue_measured_fraction_max 0.940
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            23575
_diffrn_reflns_point_group_measured_fraction_full 0.765
_diffrn_reflns_point_group_measured_fraction_max 0.749
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         69.252
_diffrn_reflns_theta_min         3.535
_exptl_absorpt_coefficient_mu    0.855
_exptl_absorpt_correction_T_max  0.75
_exptl_absorpt_correction_T_min  0.49
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_density_diffrn    1.333
_exptl_crystal_description       block
_exptl_crystal_F_000             822
_exptl_crystal_size_max          0.230
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.080
_refine_diff_density_max         0.540
_refine_diff_density_min         -0.289
_refine_diff_density_rms         0.068
_refine_ls_abs_structure_details
; 
 Flack x determined using 3825 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   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     966
_refine_ls_number_reflns         10540
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0479
_refine_ls_R_factor_gt           0.0477
_refine_ls_shift/su_max          0.036
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0836P)^2^+0.4499P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1226
_refine_ls_wR_factor_ref         0.1230
_reflns_Friedel_coverage         0.593
_reflns_Friedel_fraction_full    0.573
_reflns_Friedel_fraction_max     0.558
_reflns_number_gt                10436
_reflns_number_total             10540
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            np500077z_si_006.cif
_cod_data_source_block           cu_dm13492_0m
_cod_depositor_comments
;
Adding full bibliography for 1516020--1516024.cif.

2019-02-22
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C73 H136 O31'
_cod_original_formula_weight         1509.81
_cod_original_formula_units_Z            1
_cod_database_code               1516022
_shelx_estimated_absorpt_t_min   0.828
_shelx_estimated_absorpt_t_max   0.935
_shelxl_version_number           2013-4
_shelx_res_checksum              22472
_shelx_hkl_checksum              31791