8β-Acetoxy-14α-benzoyloxy-<i>N</i>-ethyl-3α,10β,13β,15α-tetrahydroxy-1α,6α,16β-trimethoxy-4β-(methoxymethylene)aconitane: aconifine from <i>Aconitum karakolicum Rapaics</i>
Tashkhodjaev, Bakhodir; Sultankhodjaev, Mukhlis N.; Acta Crystallographica Section E 65 (2009) o1543–o1544; doi:10.1107/S1600536809021436

data_2222518
_publ_section_title
;8\b-Acetoxy-14\a-benzoyloxy-<i>N</i>-ethyl-3\a,10\b,13\b,15\a-tetrahydroxy-1\a,6\a,16\b-trimethoxy-4\b-(methoxymethylene)aconitane:
 aconifine from <i>Aconitum karakolicum Rapaics</i>
;
_journal_coeditor_code           ZL2215
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o1543
_journal_page_last               o1544
_journal_paper_doi               10.1107/S1600536809021436
_journal_volume                  65
_journal_year                    2009
_chemical_formula_iupac          'C34 H47 N O12'
_chemical_formula_moiety         'C34 H47 N O12'
_chemical_formula_sum            'C34 H47 N O12'
_chemical_formula_weight         661.73
_chemical_melting_point          472(2)
_chemical_name_common            akonifine
_chemical_name_systematic
;
8\b-Acetoxy-14\a-benzoyloxy-<i>N</i>-ethyl-3\a,10\b,13\b,15\a-tetrahydroxy-
1\a,6\a,16\b-trimethoxy-4\b-(methoxymethylene)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                   12.0213(3)
_cell_length_b                   15.4938(6)
_cell_length_c                   17.1038(4)
_cell_measurement_reflns_used    11111
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      75.48
_cell_measurement_theta_min      3.67
_cell_volume                     3185.68(16)
_computing_cell_refinement
;
CrysAlisPro (Oxford Diffraction, 2009)
;
_computing_data_collection
;
CrysAlisPro (Oxford Diffraction, 2009)
;
_computing_data_reduction
;
CrysAlisPro (Oxford Diffraction, 2009)
;
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      300(2)
_diffrn_detector_area_resol_mean 10.2576
_diffrn_measured_fraction_theta_full 0.977
_diffrn_measured_fraction_theta_max 0.977
_diffrn_measurement_device       Xcalibur
_diffrn_measurement_device_type  'Oxford Diffraction Xcalibur Ruby'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Cu) X-ray Source'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0236
_diffrn_reflns_av_sigmaI/netI    0.0240
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            11111
_diffrn_reflns_theta_full        75.78
_diffrn_reflns_theta_max         75.63
_diffrn_reflns_theta_min         3.85
_exptl_absorpt_coefficient_mu    0.867
_exptl_absorpt_correction_T_max  0.81066
_exptl_absorpt_correction_T_min  0.76706
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(CrysAlisPro; Oxford Diffraction, 2009)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.380
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prizmatic
_exptl_crystal_F_000             1416
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.357
_refine_diff_density_min         -0.222
_refine_ls_abs_structure_details 'Flack (1983), 2633 Friedel pairs'
_refine_ls_abs_structure_Flack   0.04(10)
_refine_ls_extinction_coef       0.00043(12)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL97 (Sheldrick, 2008)'
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     451
_refine_ls_number_reflns         6334
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.0380
_refine_ls_R_factor_gt           0.0365
_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^)+(0.0771P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0975
_refine_ls_wR_factor_ref         0.0984
_reflns_number_gt                6050
_reflns_number_total             6334
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            zl2215.cif
_cod_data_source_block           I
_cod_database_code               2222518
_cod_database_fobs_code          2222518