Epibisdehydroneotuberostemonine J
Jin, Lu; Zhang, Rong-Rong; Tian, Hai-Yan; But, Paul Pui-Hay; Jiang, Ren-Wang; Acta Crystallographica Section E 69 (2013) o1369–o1370; doi:10.1107/S1600536813021077

data_2238586
_publ_section_title
;
 Epibisdehydroneotuberostemonine J
;
_journal_coeditor_code           ZL2558
_journal_issue                   9
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o1369
_journal_page_last               o1370
_journal_paper_doi               10.1107/S1600536813021077
_journal_volume                  69
_journal_year                    2013
_chemical_formula_iupac          'C22 H29 N O4'
_chemical_formula_moiety         'C22 H29 N O4'
_chemical_formula_sum            'C22 H29 N O4'
_chemical_formula_weight         371.46
_chemical_name_common            'Epibisdehydroneotuberostemonine J'
_chemical_name_systematic
(9<i>R</i>,10<i>R</i>,11<i>S</i>,14<i>S</i>,15<i>R</i>)-3-[(2<i>S</i>,5<i>S</i>)-4,5-dimethyloxolan-2-yl]-10-ethyl-14-methyl-12-oxa-4-azatetracyclo[7.6.1.0^4,16^.0^11,15^]hexadeca-1(16),2-dien-13-one
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_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
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 92.521(18)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   6.3596(19)
_cell_length_b                   18.495(3)
_cell_length_c                   8.3875(15)
_cell_measurement_reflns_used    2449
_cell_measurement_temperature    291(2)
_cell_measurement_theta_max      24.0
_cell_measurement_theta_min      2.2
_cell_volume                     985.6(4)
_computing_cell_refinement       'SMART and SAINT (Bruker, 1998)'
_computing_data_collection       'SMART (Bruker, 1998)'
_computing_data_reduction        'SAINT and XPREP (Bruker, 1998)'
_computing_molecular_graphics    'XP in SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      291(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker SMART 1000 CCD'
_diffrn_measurement_method       'omega scan'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0224
_diffrn_reflns_av_sigmaI/netI    0.0503
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -1
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            2449
_diffrn_reflns_theta_full        24.99
_diffrn_reflns_theta_max         24.99
_diffrn_reflns_theta_min         2.20
_exptl_absorpt_coefficient_mu    0.085
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.8314
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2004)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.252
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             400
_exptl_crystal_size_max          0.43
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.127
_refine_diff_density_min         -0.130
_refine_ls_extinction_coef       0.013(2)
_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   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     245
_refine_ls_number_reflns         1914
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0767
_refine_ls_R_factor_gt           0.0448
_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^)+(0.0368P)^2^+0.0285P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0818
_refine_ls_wR_factor_ref         0.0932
_reflns_number_gt                1383
_reflns_number_total             1914
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            zl2558.cif
_cod_data_source_block           I
_cod_database_code               2238586
_cod_database_fobs_code          2238586