Lithocarpic Acids A-N, 3,4-seco-Cycloartane Derivatives from the Cupules of Lithocarpus polystachyus.
Wang, Hongmin; Ning, Ruonan; Shen, Yu; Chen, Zhenhua; Li, Jinlong; Zhang, Rujun; Leng, Ying; Zhao, Weimin; Journal of natural products 77 (2014) 1910–; doi:10.1021/np500379f

data_1517373
_publ_section_title
;
 Lithocarpic Acids A-N, 3,4-seco-Cycloartane Derivatives from the Cupules
 of Lithocarpus polystachyus.
;
_journal_issue                   8
_journal_name_full               'Journal of natural products'
_journal_page_first              1910
_journal_paper_doi               10.1021/np500379f
_journal_volume                  77
_journal_year                    2014
_chemical_absolute_configuration ad
_chemical_formula_sum            'C31 H50.5 N0.5 O4.5'
_chemical_formula_weight         502.21
_chemical_name_systematic
; 
 ? 
;
_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                 98.4080(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.5653(2)
_cell_length_b                   7.60490(10)
_cell_length_c                   23.1068(3)
_cell_measurement_reflns_used    7436
_cell_measurement_temperature    140(2)
_cell_measurement_theta_max      69.02
_cell_measurement_theta_min      3.54
_cell_volume                     2879.65(6)
_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 0.974
_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  0.0306
_diffrn_reflns_av_unetI/netI     0.0372
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.974
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            22035
_diffrn_reflns_point_group_measured_fraction_full 0.842
_diffrn_reflns_point_group_measured_fraction_max 0.821
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         69.698
_diffrn_reflns_theta_min         3.541
_exptl_absorpt_coefficient_mu    0.594
_exptl_absorpt_correction_T_max  0.7432
_exptl_absorpt_correction_T_min  0.6516
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.158
_exptl_crystal_description       block
_exptl_crystal_F_000             1104
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.250
_exptl_crystal_size_min          0.200
_refine_diff_density_max         0.404
_refine_diff_density_min         -0.309
_refine_diff_density_rms         0.051
_refine_ls_abs_structure_details
; 
 Flack x determined using 2804 quotients [(I+)-(I-)]/[(I+)+(I-)] 
 (Parsons and Flack (2004), Acta Cryst. A60, s61). 
;
_refine_ls_abs_structure_Flack   0.08(11)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.928
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     686
_refine_ls_number_reflns         8927
_refine_ls_number_restraints     91
_refine_ls_restrained_S_all      0.930
_refine_ls_R_factor_all          0.0576
_refine_ls_R_factor_gt           0.0545
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1244P)^2^+0.7567P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1537
_refine_ls_wR_factor_ref         0.1582
_reflns_Friedel_coverage         0.560
_reflns_Friedel_fraction_full    0.665
_reflns_Friedel_fraction_max     0.641
_reflns_number_gt                8294
_reflns_number_total             8927
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            np500379f_si_002.cif
_cod_data_source_block           cu_dm13373_0m
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'MULTI-SCAN' changed to
'multi-scan' according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 

 Adding full bibliography for 1517372--1517374.cif.

2019-08-10
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C62 H101 N O9'
_cod_original_formula_weight         1004.43
_cod_original_formula_units_Z            2
_cod_database_code               1517373
_shelx_estimated_absorpt_t_min   0.842
_shelx_estimated_absorpt_t_max   0.890
_shelxl_version_number           2013-4
_shelx_res_checksum              51853
_shelx_hkl_checksum              91122