Pentacyclic spermidine alkaloids with radioprotective and anti-inflammatory activities from <i>Orychophragmus violaceus</i>.
Xu, Zan-Xin; Li, Bin; Tian, Ying; Li, Min; Dong, Jun-Xing; Zhang, Guang-Jie; Organic & biomolecular chemistry 19 (2021) 9844–9848; doi:10.1039/d1ob01973b

data_7158364
_publ_section_title
;
 Pentacyclic spermidine alkaloids with radioprotective and
 anti-inflammatory activities from <i>Orychophragmus violaceus</i>.
;
_journal_issue                   45
_journal_name_full               'Organic &amp; biomolecular chemistry'
_journal_page_first              9844
_journal_page_last               9848
_journal_paper_doi               10.1039/d1ob01973b
_journal_volume                  19
_journal_year                    2021
_chemical_formula_moiety         'C25 H34 N3 O4, C H4 O, Cl'
_chemical_formula_sum            'C26 H38 Cl N3 O5'
_chemical_formula_weight         508.04
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2020-06-30
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-12-21 deposited with the CCDC.	2021-10-29 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 99.650(4)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   17.4753(17)
_cell_length_b                   11.4632(11)
_cell_length_c                   26.206(2)
_cell_measurement_reflns_used    9837
_cell_measurement_temperature    190(2)
_cell_measurement_theta_max      53.88
_cell_measurement_theta_min      2.98
_cell_volume                     5175.4(8)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      189.99
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.34139
_diffrn_reflns_av_R_equivalents  0.0606
_diffrn_reflns_av_unetI/netI     0.0315
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            33846
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        53.594
_diffrn_reflns_theta_max         54.370
_diffrn_reflns_theta_min         2.976
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.069
_exptl_absorpt_correction_T_max  0.3012
_exptl_absorpt_correction_T_min  0.1954
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1241 before and 0.0746 after correction.
The Ratio of minimum to maximum transmission is 0.6487.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.304
_exptl_crystal_description       block
_exptl_crystal_F_000             2176
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.280
_refine_diff_density_min         -0.286
_refine_diff_density_rms         0.039
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     318
_refine_ls_number_reflns         4750
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0451
_refine_ls_R_factor_gt           0.0360
_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^)+(0.0365P)^2^+4.5638P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0879
_refine_ls_wR_factor_ref         0.0951
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4000
_reflns_number_total             4750
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1ob01973b2.cif
_cod_data_source_block           20200627li_znz8277_0m_a
_cod_depositor_comments          'Adding full bibliography for 7158364.cif.'
_cod_original_cell_volume        5175.3(9)
_cod_database_code               7158364
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.919
_shelx_estimated_absorpt_t_min   0.882
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups, All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2.a Ternary CH refined with riding coordinates:
 C12(H12), C15(H15)
2.b Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B), C6(H6A,H6B),
 C7(H7A,H7B), C9(H9A,H9B), C10(H10A,H10B), C13(H13A,H13B), C14(H14A,H14B),
 C22(H22A,H22B), C23(H23A,H23B), N2(H2C,H2D)
2.c Aromatic/amide H refined with riding coordinates:
 C18(H18), C20(H20), C21(H21), N1(H1)
2.d Idealised Me refined as rotating group:
 C26(H26A,H26B,H26C)
2.e Idealised tetrahedral OH refined as rotating group:
 O5(H5)
;
_shelx_res_checksum              74081
_shelx_hkl_checksum              73640
_olex2_submission_special_instructions 'No special instructions were received'