8β-Acetoxy-14α-benzoyloxy-<i>N</i>-methyl-13β,15α-dihydroxy-1α,6α,16β-trimethoxy-4β-(methoxymethyl)aconitane: hypaconitine isolated from `fuzi'
Zheng, Ling-Li; Li, Yan; Zi, Tie-Ying; Yuan, Ming-Yong; Acta Crystallographica Section E 66 (2010) o2787–o2788; doi:10.1107/S1600536810039887

data_2227839
_publ_section_title
;
 8\b-Acetoxy-14\a-benzoyloxy-<i>N</i>-methyl-13\b,15\a-dihydroxy-1\a,6\a,16\b-trimethoxy-4\b-(methoxymethyl)aconitane:
 hypaconitine isolated from `fuzi'
;
_journal_coeditor_code           NG5034
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o2787
_journal_page_last               o2788
_journal_paper_doi               10.1107/S1600536810039887
_journal_volume                  66
_journal_year                    2010
_chemical_formula_iupac          'C33 H45 N O10'
_chemical_formula_moiety         'C33 H45 N O10'
_chemical_formula_sum            'C33 H45 N O10'
_chemical_formula_weight         615.70
_chemical_name_common            hypaconitine
_chemical_name_systematic
;
8\b-Acetoxy-14\a-benzoyloxy-<i>N</i>-methyl-13\b,15\a-dihydroxy-
1\a,6\a,16\b-trimethoxy-4\b-(methoxymethyl)aconitane
;
_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                   12.457(2)
_cell_length_b                   15.689(3)
_cell_length_c                   15.771(3)
_cell_measurement_reflns_used    11109
_cell_measurement_temperature    113(2)
_cell_measurement_theta_max      27.9
_cell_measurement_theta_min      1.3
_cell_volume                     3082.3(10)
_computing_cell_refinement       'CrystalClear (Rigaku/MSC, 2005)'
_computing_data_collection       'CrystalClear (Rigaku/MSC, 2005)'
_computing_data_reduction        'CrystalClear (Rigaku/MSC, 2005)'
_computing_molecular_graphics    'ORTEP03 (Farrugia, 1997)'
_computing_publication_material  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      113(2)
_diffrn_detector_area_resol_mean 14.63
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Rigaku Saturn CCD area-detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  multiplayer
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0403
_diffrn_reflns_av_sigmaI/netI    0.0304
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            28410
_diffrn_reflns_theta_full        27.87
_diffrn_reflns_theta_max         27.87
_diffrn_reflns_theta_min         1.83
_exptl_absorpt_coefficient_mu    0.098
_exptl_absorpt_correction_T_max  0.9798
_exptl_absorpt_correction_T_min  0.9694
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(CrystalClear; Rigaku/MSC, 2005)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.327
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1320
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.29
_exptl_crystal_size_min          0.21
_refine_diff_density_max         0.247
_refine_diff_density_min         -0.211
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     406
_refine_ls_number_reflns         4094
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.0387
_refine_ls_R_factor_gt           0.0353
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0542P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0816
_refine_ls_wR_factor_ref         0.0834
_reflns_number_gt                3805
_reflns_number_total             4094
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            ng5034.cif
_cod_data_source_block           I
_cod_database_code               2227839
_cod_database_fobs_code          2227839