(1α,8β)-6β-Benzoyloxy-6-dehydroxyheteratisine from <i>Aconitum zeravschanicum</i>
Tashkhodjaev, Bakhodir; Salimov, Bakhodir T.; Acta Crystallographica Section E 65 (2009) o1682–o1683; doi:10.1107/S1600536809023873

data_2222522
_publ_section_title
;
 (1\a,8\b)-6\b-Benzoyloxy-6-dehydroxyheteratisine from <i>Aconitum
 zeravschanicum</i>
;
_journal_coeditor_code           ZL2222
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o1682
_journal_page_last               o1683
_journal_paper_doi               10.1107/S1600536809023873
_journal_volume                  65
_journal_year                    2009
_chemical_formula_moiety         'C29 H37 N O6'
_chemical_formula_sum            'C29 H37 N O6'
_chemical_formula_weight         495.60
_chemical_melting_point          486(2)
_chemical_name_common
;
6-benzoylheteratisine and
1\a-Methoxy-6\b-benzoyloxy-8\b-hydroxy-\D^13,14^-oxy-\D^17,19^---<i>N</i>-\
ethylaconanon-14: 6-benzoylheteratisine
;
_chemical_name_systematic
;
(1\a,8\b)-6\b-Benzoyloxy-6-dehydroxyheteratisine
;
_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                   10.039(5)
_cell_length_b                   14.107(8)
_cell_length_c                   17.512(6)
_cell_measurement_reflns_used    30
_cell_measurement_temperature    300(2)
_cell_measurement_theta_max      20
_cell_measurement_theta_min      10
_cell_volume                     2480(2)
_computing_cell_refinement       'STADI4 (Stoe & Cie, 1997)'
_computing_data_collection       'STADI4 (Stoe & Cie, 1997)'
_computing_data_reduction        'X-RED (Stoe & Cie, 1997)'
_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_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Stoe Stadi-4 four-circle'
_diffrn_measurement_method
; Scan width (omega) = 1.56 - 1.68, scan ratio 2theta:omega = 1.00
  I(Net) and sigma(I) calculated according to Blessing (1987)
;
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0548
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            2481
_diffrn_reflns_theta_full        24.99
_diffrn_reflns_theta_max         24.99
_diffrn_reflns_theta_min         1.85
_diffrn_standards_decay_%        6.8
_diffrn_standards_interval_count 200
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.092
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.327
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prizmatic
_exptl_crystal_F_000             1064
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.215
_refine_diff_density_min         -0.205
_refine_ls_extinction_coef       0.0056(10)
_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   1.215
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     330
_refine_ls_number_reflns         2481
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.215
_refine_ls_R_factor_all          0.1187
_refine_ls_R_factor_gt           0.0671
_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^)+(0.0342P)^2^+1.8083P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1174
_refine_ls_wR_factor_ref         0.1421
_reflns_number_gt                1667
_reflns_number_total             2481
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            zl2222.cif
_cod_data_source_block           I
_cod_original_cell_volume        2480.(2)
_cod_database_code               2222522
_cod_database_fobs_code          2222522