Gelstriamine A, a Triamino Monoterpene Indole Alkaloid with a Caged 6/5/7/6/6/5 Scaffold and Analgesic Alkaloids from <i>Gelsemium elegans</i> Stems.
Jin, Pengfei; Zhan, Guanqun; Zheng, Guijuan; Liu, Junjun; Peng, Xiang; Huang, Lang; Gao, Biao; Yuan, Xinghua; Yao, Guangmin; Journal of natural products 84 (2021) 1326–1334; doi:10.1021/acs.jnatprod.1c00062

data_1562349
_publ_section_title
;
 Gelstriamine A, a Triamino Monoterpene Indole Alkaloid with a Caged
 6/5/7/6/6/5 Scaffold and Analgesic Alkaloids from <i>Gelsemium
 elegans</i> Stems.
;
_journal_issue                   4
_journal_name_full               'Journal of natural products'
_journal_page_first              1326
_journal_page_last               1334
_journal_paper_doi               10.1021/acs.jnatprod.1c00062
_journal_volume                  84
_journal_year                    2021
_chemical_formula_moiety         'C17 H16 N2'
_chemical_formula_sum            'C17 H16 N2'
_chemical_formula_weight         248.32
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2021-03-19
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_cell_angle_alpha                90
_cell_angle_beta                 114.1490(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   15.9907(2)
_cell_length_b                   11.36670(10)
_cell_length_c                   15.9469(2)
_cell_measurement_reflns_used    4856
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      69.70
_cell_measurement_theta_min      2.17
_cell_volume                     2644.87(6)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.3 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      173.0
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'multiwire proportional'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0386
_diffrn_reflns_av_unetI/netI     0.0168
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            67744
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         73.974
_diffrn_reflns_theta_min         3.028
_exptl_absorpt_coefficient_mu    0.570
_exptl_absorpt_correction_T_max  0.9244
_exptl_absorpt_correction_T_min  0.9043
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   'SADABS, Sheldrick,2008'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.247
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1056
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.181
_refine_diff_density_min         -0.220
_refine_diff_density_rms         0.041
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     343
_refine_ls_number_reflns         5333
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0380
_refine_ls_R_factor_gt           0.0362
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0371P)^2^+1.0728P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0871
_refine_ls_wR_factor_ref         0.0884
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5052
_reflns_number_total             5333
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            np1c00062_si_002.cif
_cod_data_source_block           12
_cod_original_cell_volume        2644.86(6)
_cod_database_code               1562349
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.924
_shelx_estimated_absorpt_t_min   0.904
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
2.a Riding coordinates:
 N1(H1), N1A(H1A)
2.b Secondary CH2 refined with riding coordinates:
 C4'(H4'A,H4'B), C5'(H5'A,H5'B), C6'(H6'A,H6'B), C7'(H7'A,H7'B), C4'B(H4'C,
 H4'D), C5'B(H5'C,H5'D), C6'B(H6'C,H6'D), C7'B(H7'C,H7'D)
2.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C6(H6), C7(H7), C3'(H3'), C8'(H8'), C3B(H3B),
 C4B(H4B), C5B(H5B), C6B(H6B), C7B(H7B), C3'B(H3'B), C8'B(H8'B)
;
_shelx_res_checksum              12792
_shelx_hkl_checksum              30298
_olex2_submission_special_instructions 'No special instructions were received'