Ethyl 6-amino-5-cyano-4-isopropyl-2-methyl-4<i>H</i>-pyran-3-carboxylate
Messaâd, Mehdi; Hamdi, Besma; Chabchoub, Fakher; Ben Salah, Abdelhamid; Salem, Mansour; Acta Crystallographica Section E 65 (2009) o39–; doi:10.1107/S160053680804052X

data_2220474
_publ_section_title
;
 Ethyl
 6-amino-5-cyano-4-isopropyl-2-methyl-4<i>H</i>-pyran-3-carboxylate
;
_journal_coeditor_code           DN2412
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o39
_journal_paper_doi               10.1107/S160053680804052X
_journal_volume                  65
_journal_year                    2009
_chemical_formula_iupac          'C13 H18 N2 O3'
_chemical_formula_moiety         'C13 H18 N2 O3'
_chemical_formula_sum            'C13 H18 N2 O3'
_chemical_formula_weight         250.29
_chemical_name_systematic
;
Ethyl 6-amino-5-cyano-4-isopropyl-2-methyl-4<i>H</i>-pyran-3-carboxylate
;
_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           SHELXL97
_cell_angle_alpha                65.6520(10)
_cell_angle_beta                 69.6790(10)
_cell_angle_gamma                76.1050(10)
_cell_formula_units_Z            2
_cell_length_a                   8.08560(10)
_cell_length_b                   9.3193(2)
_cell_length_c                   10.4563(2)
_cell_measurement_reflns_used    2132
_cell_measurement_temperature    296
_cell_measurement_theta_max      21.20
_cell_measurement_theta_min      2.30
_cell_volume                     668.80(2)
_computing_cell_refinement       'SAINT (Bruker, 1998)'
_computing_data_collection       'SMART (Bruker, 1998)'
_computing_data_reduction        'SAINT (Bruker, 1998)'
_computing_molecular_graphics
;
ORTEPIII (Burnett & Johnson, 1996), ORTEP-3 for Windows (Farrugia,
1997) and
PLATON (Spek, 2003)
;
_computing_publication_material  'WinGX (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker SMART CCD area-detector'
_diffrn_measurement_method       '\f and \w'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0266
_diffrn_reflns_av_sigmaI/netI    0.0240
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            17876
_diffrn_reflns_theta_full        32.11
_diffrn_reflns_theta_max         32.11
_diffrn_reflns_theta_min         2.23
_exptl_absorpt_coefficient_mu    0.089
_exptl_absorpt_correction_T_max  0.982
_exptl_absorpt_correction_T_min  0.959
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 1998)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.243
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             268
_exptl_crystal_size_max          0.44
_exptl_crystal_size_mid          0.36
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.235
_refine_diff_density_min         -0.237
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     167
_refine_ls_number_reflns         4664
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0671
_refine_ls_R_factor_gt           0.0461
_refine_ls_shift/su_max          0.009
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.0801P)^2^+0.0260P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1271
_refine_ls_wR_factor_ref         0.1428
_reflns_number_gt                3324
_reflns_number_total             4664
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            dn2412.cif
_cod_data_source_block           I
_cod_database_code               2220474
_cod_database_fobs_code          2220474