A new key intermediate in the synthesis of 6-oxopiperidine-2-carboxylate derivatives
Lenda, Fatimazohra; Guenoun, Farhate; Tasi, Bouchra; Ben larbi, Najib; Martinez, Jean; Lamaty, Frederic; Allouchi, Hassan; Acta Crystallographica Section E 60 (2004) o1038–o1039; doi:10.1107/S1600536804011626

data_2203747
_publ_section_title
;
 A new key intermediate in the synthesis of
 6-oxopiperidine-2-carboxylate derivatives
;
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o1038
_journal_page_last               o1039
_journal_paper_doi               10.1107/S1600536804011626
_journal_volume                  60
_journal_year                    2004
_chemical_formula_iupac          'C14 H15 N5 O3'
_chemical_formula_moiety         'C14 H15 N5 O3'
_chemical_formula_structural     'C14 H15 N5 O3'
_chemical_formula_sum            'C14 H15 N5 O3'
_chemical_formula_weight         301.31
_chemical_name_systematic
;
6-oxo-5-(5-phenyltetrazol-2-yl)piperidine-2-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'
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 102.7960(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.7980(6)
_cell_length_b                   10.8334(3)
_cell_length_c                   10.9142(3)
_cell_measurement_temperature    296(2)
_cell_volume                     1475.63(9)
_computing_data_collection       'KappaCCD Server Software (Nonius, 1998)'
_computing_data_reduction        'Denzo (Otwinowski & Miror, 1997)'
_computing_molecular_graphics
;
ORTEP-3 for Windows (Farrugia, 1997) and CAMERON (Watkin et al., 1993)
;
_computing_publication_material  'WinGX (Farugia, 1999)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0198
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            5170
_diffrn_reflns_theta_full        25.01
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         3.82
_exptl_absorpt_coefficient_mu    0.099
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.356
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             632
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.164
_refine_diff_density_min         -0.147
_refine_ls_extinction_coef       0.026(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL97
_refine_ls_goodness_of_fit_ref   1.04
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     204
_refine_ls_number_reflns         2563
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.04
_refine_ls_R_factor_gt           0.044
_refine_ls_shift/su_max          0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0438P)^2^+0.1856P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.1083
_reflns_number_gt                1777
_reflns_number_total             2563
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            dn6134.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2203747
_cod_database_fobs_code          2203747