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_2103934
_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_sum            'C9 H14 N4 O3'
_chemical_formula_weight         226.24
_chemical_name_systematic
;
1,2-Dimethyl-4-nitro-5-morpholine-imidazole
;
_space_group_IT_number           11
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yb'
_symmetry_space_group_name_H-M   'P 1 21/m 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 112.23(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   8.589(2)
_cell_length_b                   6.6750(10)
_cell_length_c                   10.657(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      15
_cell_measurement_theta_min      8
_cell_volume                     565.6(2)
_computing_cell_refinement       'KUMA KM4 software (Kuma Diffraction, 1991)'
_computing_data_collection       'KUMA KM4 software (Kuma Diffraction, 1991)'
_computing_data_reduction        'KUMA KM4 software (Kuma Diffraction, 1991)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device       'KM4 four-circle diffractometer'
_diffrn_measurement_method       \w/2\Q
_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  0.0330
_diffrn_reflns_av_sigmaI/netI    0.0184
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            1140
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.69
_diffrn_standards_decay_%        2
_diffrn_standards_interval_count 100
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.102
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.329
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             240
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.189
_refine_diff_density_min         -0.162
_refine_ls_extinction_coef       0.68(2)
_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     94
_refine_ls_number_reflns         1068
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.089
_refine_ls_R_factor_all          0.0548
_refine_ls_R_factor_gt           0.0454
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0120P)^2^+0.2500P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0884
_refine_ls_wR_factor_ref         0.0908
_reflns_number_gt                908
_reflns_number_total             1068
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            sn0030.cif
_cod_data_source_block           1
_cod_original_cell_volume        565.57(19)
_cod_original_sg_symbol_H-M      P2~1~/m
_cod_database_code               2103934
_cod_database_fobs_code          2103934