6-Formyl-2-naphthyl <i>cis</i>-1,5,7-trimethyl-2,4-dioxo-3-azabicyclo[3.3.1]nonane-7-carboxylate
Xu, Sheng-guang; Wang, Chun-hua; Liu, Jun-shen; Liu, Xi-guang; Li, Long; Acta Crystallographica Section E 66 (2010) o245–; doi:10.1107/S1600536809054786

data_2224653
_publ_section_title
;
 6-Formyl-2-naphthyl
 <i>cis</i>-1,5,7-trimethyl-2,4-dioxo-3-azabicyclo[3.3.1]nonane-7-carboxylate
;
_journal_coeditor_code           HB5273
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o245
_journal_paper_doi               10.1107/S1600536809054786
_journal_volume                  66
_journal_year                    2010
_chemical_formula_iupac          'C23 H23 N O5'
_chemical_formula_moiety         'C23 H23 N O5'
_chemical_formula_sum            'C23 H23 N O5'
_chemical_formula_weight         393.42
_chemical_name_systematic
;
6-Formyl-2-naphthyl
<i>cis</i>-1,5,7-trimethyl-2,4-dioxo-3-azabicyclo[3.3.1]nonane-7-carboxylate
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_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                 121.124(9)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.896(2)
_cell_length_b                   11.692(2)
_cell_length_c                   16.636(2)
_cell_measurement_reflns_used    4643
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      27.57
_cell_measurement_theta_min      2.47
_cell_volume                     1980.8(6)
_computing_cell_refinement       'SAINT (Bruker, 2004)'
_computing_data_collection       'APEX2 (Bruker, 2004)'
_computing_data_reduction        'SAINT (Bruker, 2004)'
_computing_molecular_graphics    'XP in SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEXII CCD'
_diffrn_measurement_method       '\f and \w scan'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0180
_diffrn_reflns_av_sigmaI/netI    0.0217
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            10443
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         2.00
_exptl_absorpt_coefficient_mu    0.093
_exptl_absorpt_correction_T_max  0.9816
_exptl_absorpt_correction_T_min  0.9744
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2004)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.319
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             832
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.191
_refine_diff_density_min         -0.215
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     265
_refine_ls_number_reflns         3897
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0467
_refine_ls_R_factor_gt           0.0378
_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^)+(0.0518P)^2^+0.4083P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0972
_refine_ls_wR_factor_ref         0.1050
_reflns_number_gt                3217
_reflns_number_total             3897
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            hb5273.cif
_cod_data_source_block           I
_cod_original_cell_volume        1980.8(5)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2224653
_cod_database_fobs_code          2224653