Ethyl 4-(3-hydroxy-6-methyl-4-oxo-4<i>H</i>-pyran-2-ylmethyl)piperazine-1-carboxylate
Ocak, Nazan; Işık, Şamil; Dilsiz Aytemir, Mutlu; Acta Crystallographica Section E 60 (2004) o561–o563; doi:10.1107/S1600536804005720

data_2203469
_publ_section_title
;Ethyl
 4-(3-hydroxy-6-methyl-4-oxo-4<i>H</i>-pyran-2-ylmethyl)piperazine-1-carboxylate
;
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o561
_journal_page_last               o563
_journal_paper_doi               10.1107/S1600536804005720
_journal_volume                  60
_journal_year                    2004
_chemical_formula_iupac          'C14 H20 N2 O5'
_chemical_formula_moiety         'C14 H20 N2 O5'
_chemical_formula_sum            'C14 H20 N2 O5'
_chemical_formula_weight         296.32
_chemical_name_systematic
;Ethyl
 4-(3-hydroxy-6-methyl-4-oxo-4H-pyran-2-ylmethyl)piperazine-1-carboxylate
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 95.513(8)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   24.069(3)
_cell_length_b                   6.1796(4)
_cell_length_c                   19.788(2)
_cell_measurement_reflns_used    15639
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      29.56
_cell_measurement_theta_min      1.70
_cell_volume                     2929.6(5)
_computing_cell_refinement       X-AREA
_computing_data_collection       'X-AREA (Stoe & Cie, 2002)'
_computing_data_reduction        'X-RED32 (Stoe & Cie, 2002)'
_computing_molecular_graphics    'ORTEPIII (Burnett & Johnson, 1996)'
_computing_publication_material
'WinGX (Farrugia, 1997) and PARST (Nardelli, 1995)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 6.67
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'STOE IPDS-II'
_diffrn_measurement_method       'w scans'
_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  0.0741
_diffrn_reflns_av_sigmaI/netI    0.0351
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            16025
_diffrn_reflns_theta_full        25.99
_diffrn_reflns_theta_max         25.99
_diffrn_reflns_theta_min         1.70
_diffrn_standards_decay_%        'not measurement'
_diffrn_standards_interval_time  30
_diffrn_standards_number         1
_exptl_absorpt_coefficient_mu    0.102
_exptl_absorpt_correction_T_max  0.9700
_exptl_absorpt_correction_T_min  0.9373
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'X-RED32 (Stoe & Cie, 2002)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.344
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism.
_exptl_crystal_F_000             1264
_exptl_crystal_size_max          0.600
_exptl_crystal_size_mid          0.553
_exptl_crystal_size_min          0.320
_refine_diff_density_max         0.367
_refine_diff_density_min         -0.333
_refine_ls_extinction_coef       0.0072(13)
_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   1.099
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     191
_refine_ls_number_reflns         2888
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.099
_refine_ls_R_factor_all          0.0560
_refine_ls_R_factor_gt           0.0491
_refine_ls_shift/su_max          <0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0946P)^2^+0.909P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1553
_refine_ls_wR_factor_ref         0.1621
_reflns_number_gt                2388
_reflns_number_total             2888
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            na6300.cif
_cod_data_source_block           I
_cod_original_cell_volume        2929.7(5)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               2203469
_cod_database_fobs_code          2203469