Paxdaphnine B: a 1,19-bisnor-daphniphyllum alkaloid
Yong-Bin Lu; Ning-Chuan Kong; Yuan-Yuan Feng; Xiao-Jiang Hao; Yang Lu; Acta Crystallographica Section E 63 (2007) o589–o591; doi:10.1107/S1600536806055826

data_2212372
_publ_section_title
;
 Paxdaphnine B: a 1,19-bisnor-daphniphyllum alkaloid
;
_journal_coeditor_code           SJ2204
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o589
_journal_page_last               o591
_journal_paper_doi               10.1107/S1600536806055826
_journal_volume                  63
_journal_year                    2007
_chemical_formula_iupac          'C21 H31 N O3'
_chemical_formula_moiety         'C21 H31 N O3'
_chemical_formula_sum            'C21 H31 N O3'
_chemical_formula_weight         345.47
_chemical_name_common            'Paxdaphnine B '
_chemical_name_systematic
;
methyl
5-ethyl-2-methoxy-6-azapentacyclo[9.5.1.0^1,5^.0^2,8^.0^14,17^]heptadec-
11(17)-ene-15-carboxylate
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 94.619(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.7500(15)
_cell_length_b                   24.717(3)
_cell_length_c                   9.605(2)
_cell_measurement_reflns_used    3431
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      25.44
_cell_measurement_theta_min      2.13
_cell_volume                     1833.9(6)
_computing_cell_refinement       'SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_collection       'DENZO (Otwinowski & Minor, 1997)'
_computing_data_reduction        SCALEPACK
_computing_molecular_graphics    'PLATON (Spek, 2003)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      295(2)
_diffrn_detector_area_resol_mean 0
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device_type  'MAC DIP 2030K'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.035
_diffrn_reflns_av_sigmaI/netI    0.0297
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            10725
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.44
_diffrn_reflns_theta_min         2.13
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.082
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.251
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             752
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.161
_refine_diff_density_min         -0.181
_refine_ls_extinction_coef       0.134(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL97
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     464
_refine_ls_number_reflns         3431
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0584
_refine_ls_R_factor_gt           0.0516
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0864P)^2^+0.2863P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1295
_refine_ls_wR_factor_ref         0.1367
_reflns_number_gt                3019
_reflns_number_total             3431
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            sj2204.cif
_cod_data_source_block           I
_cod_original_cell_volume        1833.9(5)
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               2212372
_cod_database_fobs_code          2212372