(11<i>R</i>)-13-(Benzylamino)-4,5-epoxy-11,13-dihydrocostunolide
Nasim, Shama; Parkin, Sean; Crooks, Peter A.; Acta Crystallographica Section E 63 (2007) o3922–o3922; doi:10.1107/S1600536807041712

data_2215153
_publ_section_title
;
 (11<i>R</i>)-13-(Benzylamino)-4,5-epoxy-11,13-dihydrocostunolide
;
_journal_coeditor_code           HG2279
_journal_issue                   9
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o3922
_journal_page_last               o3922
_journal_paper_doi               10.1107/S1600536807041712
_journal_volume                  63
_journal_year                    2007
_chemical_formula_iupac          'C22 H29 N O3'
_chemical_formula_moiety         'C22 H29 N O3'
_chemical_formula_sum            'C22 H29 N O3'
_chemical_formula_weight         355.46
_chemical_name_systematic
;
(11R)-13-(Benzylamino)-4,5-epoxy-11,13-dihydrocostunolide
;
_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                   8.3772(6)
_cell_length_b                   13.7441(10)
_cell_length_c                   16.9684(12)
_cell_measurement_reflns_used    7188
_cell_measurement_temperature    90.0(2)
_cell_measurement_theta_max      68.01
_cell_measurement_theta_min      4.14
_cell_volume                     1953.7(2)
_computing_cell_refinement       APEX2
_computing_data_collection       'APEX2 (Bruker--Nonius, 2004)'
_computing_data_reduction        APEX2
_computing_molecular_graphics    'XP in SHELXTL/PC (Sheldrick, 1995)'
_computing_publication_material
;
SHELXL97 (Sheldrick, 1997) and local procedures
;
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      90.0(2)
_diffrn_detector_area_resol_mean 18
_diffrn_measured_fraction_theta_full .995
_diffrn_measured_fraction_theta_max .995
_diffrn_measurement_device_type  'X8 Proteum'
_diffrn_measurement_method       '\w and \f'
_diffrn_radiation_monochromator  'Helios multilayer optics'
_diffrn_radiation_source         'fine-focus rotating anode'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0425
_diffrn_reflns_av_sigmaI/netI    0.0306
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            21942
_diffrn_reflns_theta_full        68.01
_diffrn_reflns_theta_max         68.01
_diffrn_reflns_theta_min         4.14
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_exptl_absorpt_coefficient_mu    0.631
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.208
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             768
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.08
_refine_diff_density_max         .258
_refine_diff_density_min         -.193
_refine_ls_abs_structure_details 'Flack (1983), with 0000 Friedel pairs'
_refine_ls_abs_structure_Flack   0.13(6)
_refine_ls_extinction_coef       0.0055(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL97 (Sheldrick, 1997)'
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     241
_refine_ls_number_reflns         3531
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.079
_refine_ls_R_factor_all          0.0371
_refine_ls_R_factor_gt           0.0363
_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^)+(0.0636P)^2^+0.2363P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0949
_refine_ls_wR_factor_ref         0.0960
_reflns_number_gt                3446
_reflns_number_total             3531
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            hg2279.cif
_cod_data_source_block           I
_cod_database_code               2215153
_cod_database_fobs_code          2215153