(11<i>R</i>,13<i>R</i>)-13-(Tetralin-1-ylamino)-4,5-epoxy-11,13-dihydrocostunolide
Nasim, Shama; Parkin, Sean; Crooks, Peter A.; Acta Crystallographica Section E 64 (2008) o639–; doi:10.1107/S1600536808003322

data_2217783
_publ_section_title
(11<i>R</i>,13<i>R</i>)-13-(Tetralin-1-ylamino)-4,5-epoxy-11,13-dihydrocostunolide
_journal_coeditor_code           HG2376
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o639
_journal_paper_doi               10.1107/S1600536808003322
_journal_volume                  64
_journal_year                    2008
_chemical_formula_iupac          'C25 H33 N O3'
_chemical_formula_moiety         'C25 H33 N O3'
_chemical_formula_sum            'C25 H33 N O3'
_chemical_formula_weight         395.52
_chemical_name_common
;
(11R,13R)-13-(Tetralin-1-ylamino)-4,5-epoxy-11,13-dihydrocostunolide
;
_chemical_name_systematic
;
(12R)-4,8-dimethyl-12-[(1'R)-1',2',3',4'-tetrahydro-1'-naphthyl)aminomethyl]-
3,14-dioxatricyclo[9.3.0.0^2,4^]tetradec-7-en-13-one
;
_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                   8.4952(13)
_cell_length_b                   13.1852(19)
_cell_length_c                   18.771(3)
_cell_measurement_reflns_used    9023
_cell_measurement_temperature    90.0(2)
_cell_measurement_theta_max      68.57
_cell_measurement_theta_min      4.09
_cell_volume                     2102.6(6)
_computing_cell_refinement       'APEX2 (Bruker Nonius, 2004)'
_computing_data_collection       'APEX2 (Bruker Nonius, 2004)'
_computing_data_reduction        'APEX2 (Bruker Nonius, 2004)'
_computing_molecular_graphics    'XP in SHELXTL (Sheldrick, 2008)'
_computing_publication_material
;
SHELXL97 (Sheldrick, 2008) and local procedures
;
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      90.0(2)
_diffrn_detector_area_resol_mean 18
_diffrn_measured_fraction_theta_full .996
_diffrn_measured_fraction_theta_max .996
_diffrn_measurement_device_type  'Bruker 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  0.0326
_diffrn_reflns_av_sigmaI/netI    0.0179
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            26461
_diffrn_reflns_theta_full        68.63
_diffrn_reflns_theta_max         68.63
_diffrn_reflns_theta_min         4.10
_exptl_absorpt_coefficient_mu    0.638
_exptl_absorpt_correction_T_max  0.894
_exptl_absorpt_correction_T_min  0.782
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS in APEX2; Bruker Nonius, 2004)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.249
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'cut block'
_exptl_crystal_F_000             856
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.18
_refine_diff_density_max         .336
_refine_diff_density_min         -.221
_refine_ls_abs_structure_details 'Flack (1983)'
_refine_ls_abs_structure_Flack   0.06(5)
_refine_ls_extinction_coef       0.0147(7)
_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   1.060
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     269
_refine_ls_number_reflns         3849
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.0432
_refine_ls_R_factor_gt           0.0429
_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^)+(0.0627P)^2^+0.7419P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1098
_refine_ls_wR_factor_ref         0.1100
_reflns_number_gt                3813
_reflns_number_total             3849
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            hg2376.cif
_cod_data_source_block           I
_cod_database_code               2217783
_cod_database_fobs_code          2217783