Ethyl <i>N</i>-(2-benzylamino-6-benzyloxy-5-nitrosopyrimidin-4-yl)glycinate: sheets built from a three-centre N—H···(N,O), and two-centre C—H···O and C—H···π(arene) hydrogen bonds
Low, John N.; Glidewell, Christopher; Quesada, Antonio; Nogueras, Manuel; Sánchez, Adolfo; Acta Crystallographica Section C 58 (2002) o425–o427; doi:10.1107/S0108270102009575

data_2012827
_publ_section_title
;
 Ethyl
 <i>N</i>-(2-benzylamino-6-benzyloxy-5-nitrosopyrimidin-4-yl)glycinate:
 sheets built from a three-centre N---H&#x00B7;&#x00B7;&#x00B7;(N,O),
 and two-centre C---H&#x00B7;&#x00B7;&#x00B7;O and
 C---H&#x00B7;&#x00B7;&#x00B7;\p(arene) hydrogen bonds
;
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              o425
_journal_page_last               o427
_journal_paper_doi               10.1107/S0108270102009575
_journal_volume                  58
_journal_year                    2002
_chemical_formula_iupac          'C22 H23 N5 O4'
_chemical_formula_moiety         'C22 H23 N5 O4'
_chemical_formula_sum            'C22 H23 N5 O4'
_chemical_formula_weight         421.45
_chemical_melting_point          396
_chemical_name_systematic
;
Ethyl  N-[2-benzylamino-6-benzyloxy-5-nitrosopyrimidin-4-yl]glycinate
;
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 97.5860(11)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.2278(8)
_cell_length_b                   15.8992(5)
_cell_length_c                   8.5558(3)
_cell_measurement_reflns_used    4644
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      25.00
_cell_measurement_theta_min      2.99
_cell_volume                     2053.31(14)
_computing_cell_refinement       'DENZO--SMN (Otwinowski & Minor, 1997)'
_computing_data_collection       'KappaCCD Server Software (Nonius, 1997)'
_computing_data_reduction        DENZO--SMN
_computing_molecular_graphics    'PLATON (Spek, 2002)'
_computing_publication_material  'SHELXL97 and PRPKAPPA (Ferguson, 1999)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1997
_diffrn_reflns_av_sigmaI/netI    0.1304
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            24714
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.99
_diffrn_standards_decay_%        negligible
_exptl_absorpt_coefficient_mu    0.096
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.363
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             888
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.282
_refine_diff_density_min         -0.280
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     281
_refine_ls_number_reflns         3619
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.1684
_refine_ls_R_factor_gt           0.0689
_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^)+(0.0658P)^2^+1.1859P] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1373
_refine_ls_wR_factor_ref         0.1761
_reflns_number_gt                1861
_reflns_number_total             3619
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            na1576.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2012827
_cod_database_fobs_code          2012827