Talatisamine, a C~19~-diterpenoid alkaloid from Chinese traditional herbal `Chuanwu'
Lei, Jun; Luo, Ya-Jun; Bian, Qing-Quan; Wang, Xiong-Qing; Acta Crystallographica Section E 67 (2011) o3145–o3146; doi:10.1107/S1600536811044242

data_2232999
_publ_section_title
;
 Talatisamine, a C~19~-diterpenoid alkaloid from Chinese traditional
 herbal `Chuanwu'
;
_journal_coeditor_code           XU5344
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o3145
_journal_page_last               o3146
_journal_paper_doi               10.1107/S1600536811044242
_journal_volume                  67
_journal_year                    2011
_chemical_formula_iupac          'C24 H39 N O5'
_chemical_formula_moiety         'C24 H39 N O5'
_chemical_formula_sum            'C24 H39 N O5'
_chemical_formula_weight         421.56
_chemical_name_systematic
;
(1<i>S</i>,4<i>S</i>,5<i>R</i>,7<i>S</i>,8<i>S</i>,9<i>R</i>,10<i>R</i>,
11<i>S</i>,13<i>S</i>,14<i>S</i>,16<i>S</i>,17<i>R</i>)-<i>N</i>-methyl-
8,14-dihydroxy-1,16-trimethoxy-4-(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                   9.7124(4)
_cell_length_b                   13.9401(7)
_cell_length_c                   16.3729(8)
_cell_measurement_reflns_used    2165
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      29.0535
_cell_measurement_theta_min      2.8797
_cell_volume                     2216.76(18)
_computing_cell_refinement       'CrysAlis CCD (Oxford Diffraction, 2009)'
_computing_data_collection       'CrysAlis CCD (Oxford Diffraction, 2009)'
_computing_data_reduction        'CrysAlis RED (Oxford Diffraction, 2009)'
_computing_molecular_graphics    'OLEX2 (Dolomanov <i>et al.</i>, 2009)'
_computing_publication_material  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293.0
_diffrn_detector_area_resol_mean 16.0874
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Oxford Diffraction Xcalibur Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0260
_diffrn_reflns_av_sigmaI/netI    0.0354
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            6644
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         2.89
_exptl_absorpt_coefficient_mu    0.087
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.263
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             920
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.35
_refine_diff_density_max         0.147
_refine_diff_density_min         -0.147
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     277
_refine_ls_number_reflns         2572
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0592
_refine_ls_R_factor_gt           0.0439
_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^)+(0.0403P)^2^+0.3082P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0889
_refine_ls_wR_factor_ref         0.0967
_reflns_number_gt                2068
_reflns_number_total             2572
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            xu5344.cif
_cod_data_source_block           I
_cod_original_cell_volume        2216.77(17)
_cod_database_code               2232999
_cod_database_fobs_code          2232999