The supramolecular structure of <i>N</i>-(6-amino-3,4-dihydro-3-methyl-5-nitroso-4-oxopyrimidin-2-yl)glycylglycinate contains a unique O—H···N(nitroso) hydrogen bond
Low, John Nicolson; Quesada, Antonio; Glidewell, Christopher; Fontecha, M. Angeles; Arranz, Paloma; Godino, M. Luz; López, Rafael; Acta Crystallographica Section E 58 (2002) o942–o945; doi:10.1107/S1600536802013405

data_2201282
_publ_section_title
;The supramolecular structure of
 <i>N</i>-(6-amino-3,4-dihydro-3-methyl-5-nitroso-4-oxopyrimidin-2-yl)glycylglycinate
 contains a unique O---H&#x00B7;&#x00B7;&#x00B7;N(nitroso) hydrogen bond
;
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o942
_journal_page_last               o945
_journal_paper_doi               10.1107/S1600536802013405
_journal_volume                  58
_journal_year                    2002
_chemical_formula_iupac          'C9 H12 N6 O5'
_chemical_formula_moiety         'C9 H12 N6 O5'
_chemical_formula_sum            'C9 H12 N6 O5'
_chemical_formula_weight         284.25
_chemical_name_systematic
;
N-(6-amino-3,4-dihydro-3-methyl-5-nitroso-4-oxopyrimidin-2-yl)glycylglycinate
;
_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                81.208(5)
_cell_angle_beta                 88.722(3)
_cell_angle_gamma                76.169(4)
_cell_formula_units_Z            2
_cell_length_a                   7.4727(6)
_cell_length_b                   8.2356(4)
_cell_length_c                   9.6678(8)
_cell_measurement_reflns_used    2321
_cell_measurement_temperature    150.0(10)
_cell_measurement_theta_max      26.42
_cell_measurement_theta_min      2.80
_cell_volume                     570.87(7)
_computing_cell_refinement       'DENZO-SMN (Otwinowski & Minor, 1997)'
_computing_data_collection       'KappaCCD Server Software (Nonius, 1997)'
_computing_data_reduction        DENZO-SMN
_computing_molecular_graphics
'ORTEPII (Johnson, 1976) and PLATON (Spek, 2002)'
_computing_publication_material
'SHELXL97 and WordPerfect macro PRPKAPPA (Ferguson, 1999)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      150.0(10)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       '\f scans, and \w scans with \k offsets'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed X-ray tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0551
_diffrn_reflns_av_sigmaI/netI    0.0470
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            9202
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         26.42
_diffrn_reflns_theta_min         2.80
_diffrn_standards_decay_%        negligible
_exptl_absorpt_coefficient_mu    0.137
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            pink
_exptl_crystal_density_diffrn    1.654
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       lath
_exptl_crystal_F_000             296
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.206
_refine_diff_density_min         -0.290
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     182
_refine_ls_number_reflns         2321
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0622
_refine_ls_R_factor_gt           0.0444
_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^)+(0.0708P)^2^+0.0612P] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1117
_refine_ls_wR_factor_ref         0.1215
_reflns_number_gt                1775
_reflns_number_total             2321
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            bt6170.cif
_cod_data_source_block           I
_cod_database_code               2201282
_cod_database_fobs_code          2201282