1,4,4-Trimethyl-9-phenyl-8-oxa-9-azabicyclo[3.2.2]non-6-en-2-one
Russi, Silvia; Pardo, Helena; Heinzen, Horacio; Dias, Eduardo; Moyna, Patrick; Mariezcurrena, Raúl A.; Suescun, Leopoldo; Mombrú, Alvaro W.; Acta Crystallographica Section C 56 (2000) 672–673; doi:10.1107/S0108270100002729

data_2011070
_publ_section_title
;
 1,4,4-Trimethyl-9-phenyl-8-oxa-9-azabicyclo[3.2.2]non-6-en-2-one
;
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              672
_journal_page_last               673
_journal_paper_doi               10.1107/S0108270100002729
_journal_volume                  56
_journal_year                    2000
_chemical_formula_moiety         'C16 H19 N O2'
_chemical_formula_sum            'C16 H19 N O2'
_chemical_formula_weight         257.32
_chemical_melting_point          330.0(10)
_chemical_name_systematic
N-Phenyl-8-oxa-9-aza-1,4,4-trimethylbicyclo[3.2.2]non-6-en-one
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 92.746(11)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.417(3)
_cell_length_b                   8.263(2)
_cell_length_c                   16.5049(12)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.40
_cell_measurement_theta_min      20.17
_cell_volume                     1419.0(5)
_computing_cell_refinement       'MSC/AFC Diffractometer Software'
_computing_data_collection
'MSC/AFC Diffractometer Software  (Molecular Structure Corporation, 1993)'
_computing_data_reduction        'MSC/AFC Diffractometer Software'
_computing_molecular_graphics    'ZORTEP (Zsolnai & Pritzkow, 1995)'
_computing_publication_material
;
PLATON (Spek, 1990) and CSD (Allen & Kennard, 1993)
;
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Rigaku AFC7S'
_diffrn_measurement_method       \q/2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     .71069
_diffrn_reflns_av_R_equivalents  .0173
_diffrn_reflns_av_sigmaI/netI    .0494
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            3571
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         2.26
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    .079
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  .9638
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details
'MSC/AFC Diffractometer Software (Molecular Structure Corporation, 1993)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.205
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prismatic
_exptl_crystal_F_000             552
_exptl_crystal_size_max          .20
_exptl_crystal_size_mid          .17
_exptl_crystal_size_min          .13
_refine_diff_density_max         .145
_refine_diff_density_min         -.181
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     230
_refine_ls_number_reflns         3254
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          .0989
_refine_ls_R_factor_gt           .0422
_refine_ls_shift/su_max          <0.001
_refine_ls_shift/su_mean         .000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.0692P)^2^+0.0281P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         .1393
_reflns_number_gt                1819
_reflns_number_total             3254
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            sx1097.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value '329-331 K' was changed to
'330.0(10)' - the average value was taken and precision was
estimated.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 

The following automatic conversions were performed:

'_chemical_melting_point' value '329-331 K' was changed to
'330.0(10)' - the average value was taken and precision was
estimated.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2011070
_cod_database_fobs_code          2011070