(11<i>SR</i>,13<i>RS</i>)-12-Oxa-9-azatetracyclo[7.4.1.0^2,7^.0^11,13^]tetradeca-2(7),3,5-trien-8-one
Gallucci, Judith C.; Dura, Robert D.; Paquette, Leo A.; Acta Crystallographica Section E 63 (2007) o3417–o3417; doi:10.1107/S160053680703228X

data_2214645
_publ_section_title
(11<i>SR</i>,13<i>RS</i>)-12-Oxa-9-azatetracyclo[7.4.1.0^2,7^.0^11,13^]tetradeca-2(7),3,5-trien-8-one
_journal_coeditor_code           FL2141
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o3417
_journal_page_last               o3417
_journal_paper_doi               10.1107/S160053680703228X
_journal_volume                  63
_journal_year                    2007
_chemical_formula_iupac          'C13 H13 N1 O2'
_chemical_formula_moiety         'C13 H13 N1 O2'
_chemical_formula_sum            'C13 H13 N O2'
_chemical_formula_weight         215.24
_chemical_name_systematic
;
(11<i>SR</i>,13<i>RS</i>)-12-Oxa-9-
azatetracyclo[7.4.1.0^2,7^.0^11,13^]tetradeca-2(7),3,5-trien-8-one
;
_space_group_IT_number           9
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.3
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 101.364(11)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.1597(10)
_cell_length_b                   16.533(3)
_cell_length_c                   8.7277(10)
_cell_measurement_reflns_used    1207
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      2.037
_cell_volume                     1012.9(3)
_computing_cell_refinement       'SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 1999)'
_computing_data_reduction
'SCALEPACK and DENZO (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'SHELXTL (Bruker, 1999)'
_computing_publication_material  'WinGX (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  'Nonius KappaCCD area-detector'
_diffrn_measurement_method       '\f and \w'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.032
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            10172
_diffrn_reflns_theta_full        27.47
_diffrn_reflns_theta_max         27.47
_diffrn_reflns_theta_min         2.46
_exptl_absorpt_coefficient_mu    0.096
_exptl_absorpt_correction_T_max  0.989
_exptl_absorpt_correction_T_min  0.933
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SCALEPACK; Otwinowski & Minor, 1997)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.412
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'arrowhead-shaped chunk'
_exptl_crystal_F_000             456
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.191
_refine_diff_density_min         -0.179
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     145
_refine_ls_number_reflns         1166
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.014
_refine_ls_R_factor_all          0.0429
_refine_ls_R_factor_gt           0.038
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0754P)^2^+0.2542P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0972
_refine_ls_wR_factor_ref         0.1051
_reflns_number_gt                1069
_reflns_number_total             1166
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            fl2141.cif
_cod_data_source_block           I
_cod_original_cell_volume        1012.8(3)
_cod_original_sg_symbol_H-M      'C c'
_cod_original_formula_sum        'C13 H13 N1 O2'
_cod_database_code               2214645
_cod_database_fobs_code          2214645