1,2-Dimethyl-4-nitro-5-morpholinoimidazole and its hydrate: a case of a centrosymmetric‒noncentrosymmetric ambiguity
Kubicki, Maciej; Borowiak, Teresa; Dutkiewicz, Grzegorz; Sobiak, Stanisław; Weidlich, Iwona; Acta Crystallographica Section B 59 (2003) 487–491; doi:10.1107/S010876810301070X

data_2103935
_publ_contact_author
;
Teresa Borowiak
Faculty of Chemistry
Adam Mickiewicz University
Grunwaldzka 6
60-780 Pozna\'n
Poland
;
_publ_section_title
;
 1,2-Dimethyl-4-nitro-5-morpholinoimidazole and its hydrate: a case of
 a centrosymmetric--noncentrosymmetric ambiguity
;
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section B'
_journal_page_first              487
_journal_page_last               491
_journal_paper_doi               10.1107/S010876810301070X
_journal_volume                  59
_journal_year                    2003
_chemical_formula_moiety         'C9 H14 N4 O3, H2 O'
_chemical_formula_sum            'C9 H16 N4 O4'
_chemical_formula_weight         244.26
_chemical_name_systematic
;
1,2-Dimethyl-4-nitro-5-morpholine-imidazole hydrate
;
_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
_audit_creation_method           SHELXL-97
_cell_angle_alpha                95.319(8)
_cell_angle_beta                 92.235(9)
_cell_angle_gamma                90.777(8)
_cell_formula_units_Z            4
_cell_length_a                   10.1972(11)
_cell_length_b                   10.2908(9)
_cell_length_c                   11.1812(12)
_cell_measurement_reflns_used    2644
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      20
_cell_measurement_theta_min      5
_cell_volume                     1167.2(2)
_computing_cell_refinement       'CrysAlisCCD v.158'
_computing_data_collection       'CrysAlisCCD v.158'
_computing_data_reduction        'CrysAlisRed v.158'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'KUMA KM4CCD \k-craddle diffractometer'
_diffrn_measurement_method       \w-scan
_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  0.011
_diffrn_reflns_av_sigmaI/netI    0.0268
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            6520
_diffrn_reflns_theta_full        27.00
_diffrn_reflns_theta_max         27.00
_diffrn_reflns_theta_min         3.46
_exptl_absorpt_coefficient_mu    0.114
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.437
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             520
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.181
_refine_diff_density_min         -0.226
_refine_ls_extinction_coef       0.150(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.089
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     444
_refine_ls_number_reflns         4860
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.089
_refine_ls_R_factor_all          0.0464
_refine_ls_R_factor_gt           0.0404
_refine_ls_shift/su_max          0.014
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0601P)^2^+0.1765P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1078
_refine_ls_wR_factor_ref         0.1130
_reflns_number_gt                4180
_reflns_number_total             4860
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            sn0030.cif
_cod_data_source_block           2
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               2103935
_cod_database_fobs_code          2103935