5-Amino-3-ethoxy-1,8,8-trimethyl-2-azabicyclo[2.2.2]octa-2,5-diene-4,6-dicarbonitrile
Chantrapromma, Suchada; Suwunwong, Thitipone; Ruanwas, Pumsak; Boonnak, Nawong; Fun, Hoong-Kun; Acta Crystallographica Section E 68 (2012) o2606–o2607; doi:10.1107/S1600536812032990

data_2236595
_publ_section_title
;
 5-Amino-3-ethoxy-1,8,8-trimethyl-2-azabicyclo[2.2.2]octa-2,5-diene-4,6-dicarbonitrile
;
_journal_coeditor_code           RZ2787
_journal_issue                   9
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o2606
_journal_page_last               o2607
_journal_paper_doi               10.1107/S1600536812032990
_journal_volume                  68
_journal_year                    2012
_chemical_formula_iupac          'C14 H18 N4 O'
_chemical_formula_moiety         'C14 H18 N4 O'
_chemical_formula_sum            'C14 H18 N4 O'
_chemical_formula_weight         258.32
_chemical_name_systematic
5-Amino-3-ethoxy-1,8,8-trimethyl-2-azabicyclo[2.2.2]octa-2,5-diene-4,6-dicarbonitrile
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                62.9450(10)
_cell_angle_beta                 85.3820(10)
_cell_angle_gamma                89.3390(10)
_cell_formula_units_Z            4
_cell_length_a                   9.11150(10)
_cell_length_b                   12.4407(2)
_cell_length_c                   13.4945(2)
_cell_measurement_reflns_used    6248
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.55
_cell_measurement_theta_min      1.75
_cell_volume                     1357.29(4)
_computing_cell_refinement       'SAINT (Bruker, 2009)'
_computing_data_collection       'APEX2 (Bruker, 2009)'
_computing_data_reduction        'SAINT (Bruker, 2009)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material
'SHELXTL (Sheldrick, 2008) and PLATON (Spek, 2009)'
_computing_structure_refinement  'SHELXTL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXTL (Sheldrick, 2008)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEXII CCD area-detector'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0411
_diffrn_reflns_av_sigmaI/netI    0.0397
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            23432
_diffrn_reflns_theta_full        27.55
_diffrn_reflns_theta_max         27.55
_diffrn_reflns_theta_min         1.70
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.083
_exptl_absorpt_correction_T_max  0.9926
_exptl_absorpt_correction_T_min  0.9699
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2009)'
_exptl_crystal_colour            Colourles
_exptl_crystal_density_diffrn    1.264
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             552
_exptl_crystal_size_max          0.37
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.391
_refine_diff_density_min         -0.256
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     367
_refine_ls_number_reflns         6248
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0627
_refine_ls_R_factor_gt           0.0474
_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^)+(0.0415P)^2^+0.6407P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1010
_refine_ls_wR_factor_ref         0.1088
_reflns_number_gt                5008
_reflns_number_total             6248
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            rz2787.cif
_cod_data_source_block           I
_cod_original_cell_volume        1357.30(4)
_cod_database_code               2236595
_cod_database_fobs_code          2236595