Crystal structure of sepaconitine, a C~19~-diterpenoid alkaloid from the roots of <i>Aconitum sinomontanum</i> Nakai
Shi, Xin-Wei; Lu, Qiang-Qiang; Zhou, Jun-Hui; Cui, Xin-Ai; Acta Crystallographica Section E 71 (2015) o550–o551; doi:10.1107/S205698901501258X

data_2240907
_publ_section_title
;
 Crystal structure of sepaconitine, a C~19~-diterpenoid alkaloid from the
 roots of <i>Aconitum sinomontanum</i> Nakai
;
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o550
_journal_page_last               o551
_journal_paper_doi               10.1107/S205698901501258X
_journal_volume                  71
_journal_year                    2015
_chemical_formula_iupac          'C30 H42 N2 O8'
_chemical_formula_moiety         'C30 H42 N2 O8'
_chemical_formula_sum            'C30 H42 N2 O8'
_chemical_formula_weight         558.66
_chemical_melting_point_gt       250
_chemical_melting_point_lt       252
_chemical_name_common
;
Sepaconitine
;
_chemical_name_systematic
;
(1\a,14\a,16\b)-20-Ethyl-8,9,10-trihydroxy-1,14,16-trimethoxyaconitan-4-yl
2-aminobenzoate
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.6917(5)
_cell_length_b                   16.0510(7)
_cell_length_c                   18.3549(7)
_cell_measurement_reflns_used    2628
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      64.24
_cell_measurement_theta_min      3.66
_cell_volume                     2855.3(2)
_computing_cell_refinement
;
SAINT (Bruker, 2002)
;
_computing_data_collection
;
SMART (Bruker, 2002)
;
_computing_data_reduction
;
SAINT (Bruker, 2002)
;
_computing_molecular_graphics
;
SHELXTL (Sheldrick, 2008)
;
_computing_publication_material
;
SHELXTL (Sheldrick, 2008)
;
_computing_structure_refinement
;
SHELXTL (Sheldrick, 2008)
;
_computing_structure_solution
;
SHELXTL (Sheldrick, 2008)
;
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device_type  'Bruker SMART CCD area-detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0291
_diffrn_reflns_av_sigmaI/netI    0.0434
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            8125
_diffrn_reflns_theta_full        64.99
_diffrn_reflns_theta_max         64.99
_diffrn_reflns_theta_min         3.66
_exptl_absorpt_coefficient_mu    0.771
_exptl_absorpt_correction_T_max  0.8131
_exptl_absorpt_correction_T_min  0.7905
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Bruker, 2002)
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.300
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1200
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.28
_refine_diff_density_max         0.463
_refine_diff_density_min         -0.192
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     388
_refine_ls_number_reflns         4528
_refine_ls_number_restraints     60
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.0548
_refine_ls_R_factor_gt           0.0461
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0752P)^2^+0.0411P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1197
_refine_ls_wR_factor_ref         0.1259
_reflns_number_gt                3831
_reflns_number_total             4528
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            hg5447sup1.cif
_cod_data_source_block           I
_cod_database_code               2240907
_cod_database_fobs_code          2240907