The 2:1 salt-type adduct formed between 6-amino-3-methyl-5-nitrosopyrimidine-2,4(1<i>H</i>,3<i>H</i>)-dione and piperidine: sheets containing 20 independent hydrogen bonds
Orozco, Fabián; Insuasty, Braulio; Cobo, Justo; Glidewell, Christopher; Acta Crystallographica Section C 65 (2009) o257–o260; doi:10.1107/S0108270109014279

data_2017099
_publ_section_title
;
 The 2:1 salt-type adduct formed between
 6-amino-3-methyl-5-nitrosopyrimidine-2,4(1<i>H</i>,3<i>H</i>)-dione
 and piperidine: sheets containing 20 independent hydrogen bonds
;
_journal_coeditor_code           GG3200
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              o257
_journal_page_last               o260
_journal_paper_doi               10.1107/S0108270109014279
_journal_volume                  65
_journal_year                    2009
_chemical_formula_iupac          'C5 H12 N + , C5 H5 N4 O3 - , C5 H6 N4 O3'
_chemical_formula_moiety         'C5 H12 N + , C5 H5 N4 O3 - , C5 H6 N4 O3'
_chemical_formula_sum            'C15 H23 N9 O6'
_chemical_formula_weight         425.42
_chemical_name_systematic
;
Piperidinium
6-amino-3-methyl-5-nitroso-2,4-dioxo-1,2,3,tetrahydropyrimidin-1-ide
6-amino-3-methyl-5-nitrosopyrimidine-2,4(1<i>H</i>,3<i>H</i>)-dione
;
_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
_cell_angle_alpha                87.815(10)
_cell_angle_beta                 74.095(10)
_cell_angle_gamma                89.987(16)
_cell_formula_units_Z            4
_cell_length_a                   9.3287(19)
_cell_length_b                   13.1352(10)
_cell_length_c                   16.2814(19)
_cell_measurement_reflns_used    8768
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.50
_cell_measurement_theta_min      3.08
_cell_volume                     1917.2(5)
_computing_cell_refinement       'DIRAX/LSQ (Duisenberg <i>et al.</i>,  2000)'
_computing_data_collection       'COLLECT (Nonius, 1999)'
_computing_data_reduction        'EVALCCD (Duisenberg <i>et al.</i>,  2003)'
_computing_molecular_graphics    'PLATON (Spek, 2009)'
_computing_publication_material
'SHELXL97 (Sheldrick, 2008) and PLATON (Spek, 2009)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR2004 (Burla <i>et al.</i>,  2005)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 9.091
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker Nonius KappaCCD area-detector'
_diffrn_measurement_method       '\f and \w'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Bruker-Nonius FR591 rotating anode'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1071
_diffrn_reflns_av_sigmaI/netI    0.1388
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            44265
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         3.08
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.116
_exptl_absorpt_correction_T_max  0.975
_exptl_absorpt_correction_T_min  0.922
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2003)'
_exptl_crystal_colour            red-violet
_exptl_crystal_density_diffrn    1.474
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             896
_exptl_crystal_size_max          0.41
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.537
_refine_diff_density_min         -0.410
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     545
_refine_ls_number_reflns         8768
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.2202
_refine_ls_R_factor_gt           0.0688
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0865P)^2^+1.0774P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1484
_refine_ls_wR_factor_ref         0.2163
_reflns_number_gt                3414
_reflns_number_total             8768
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            gg3200.cif
_cod_data_source_block           I
_cod_database_code               2017099
_cod_database_fobs_code          2017099