The crystal structure of 1-methyl-2-nitro-1H-imidazole 3-oxide, C4H5N3O3
Yuan, Jun; Wu, Bingheng; Wang, Yong; Wang, Jianlong; Cao, Duanlin; Chen, Lizhen; Zeitschrift für Kristallographie - New Crystal Structures 237 (2022) 267–268; doi:10.1515/ncrs-2021-0481

data_8105200
_publ_section_title
;
 The crystal structure of 1-methyl-2-nitro-1H-imidazole 3-oxide, C4H5N3O3
;
_journal_issue                   2
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              267
_journal_page_last               268
_journal_paper_doi               10.1515/ncrs-2021-0481
_journal_volume                  237
_journal_year                    2022
_chemical_formula_moiety         'C4 H5 N3 O3'
_chemical_formula_sum            'C4 H5 N3 O3'
_chemical_formula_weight         143.11
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_cell_angle_alpha                90
_cell_angle_beta                 90.12(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.4556(2)
_cell_length_b                   7.0609(3)
_cell_length_c                   9.5928(4)
_cell_measurement_reflns_used    3290
_cell_measurement_temperature    140
_cell_measurement_theta_max      26.156
_cell_measurement_theta_min      3.212
_cell_volume                     572.73(4)
_computing_cell_refinement       'SAINT V8.40A (?, 2016)'
_computing_data_reduction        'SAINT V8.40A (?, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_exptl_absorpt_coefficient_mu    0.143
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6989
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
 wR2(int) was 0.0964 before and 0.0453 after correction.
 The Ratio of minimum to maximum transmission is 0.9376.
 The \l/2 correction factor is Not present.
_exptl_absorpt_special_details     ?
_exptl_crystal_colour              yellow
_exptl_crystal_colour_primary      yellow
_exptl_crystal_density_diffrn      1.660
_exptl_crystal_density_meas        ?
_exptl_crystal_density_method      ?
_exptl_crystal_description         block
_exptl_crystal_F_000               296
_exptl_crystal_size_max            0.18
_exptl_crystal_size_mid            0.15
_exptl_crystal_size_min            0.11
_exptl_transmission_factor_max     ?
_exptl_transmission_factor_min     ?
_diffrn_reflns_av_R_equivalents    0.0346
_diffrn_reflns_av_unetI/netI       0.0250
_diffrn_reflns_Laue_measured_fraction_full  0.992
_diffrn_reflns_Laue_measured_fraction_max  0.990
_diffrn_reflns_limit_h_max         10
_diffrn_reflns_limit_h_min         -10
_diffrn_reflns_limit_k_max         8
_diffrn_reflns_limit_k_min         -8
_diffrn_reflns_limit_l_max         11
_diffrn_reflns_limit_l_min         -11
_diffrn_reflns_number              6195
_diffrn_reflns_point_group_measured_fraction_full  0.992
_diffrn_reflns_point_group_measured_fraction_max  0.990
_diffrn_reflns_theta_full          25.242
_diffrn_reflns_theta_max           26.430
_diffrn_reflns_theta_min           3.208
_diffrn_ambient_temperature        140.0
_diffrn_detector_area_resol_mean   ?
_diffrn_measured_fraction_theta_full  0.992
_diffrn_measured_fraction_theta_max  0.990
_diffrn_measurement_device_type    'Bruker APEX-II CCD'
_diffrn_measurement_method         '\f and \w scans'
_diffrn_radiation_type             MoK\a
_diffrn_radiation_wavelength       0.71073
_diffrn_source                     ?
_diffrn_standards_number           0
_reflns_Friedel_coverage           0.000
_reflns_Friedel_fraction_full      .
_reflns_Friedel_fraction_max       .
_reflns_number_gt                  1011
_reflns_number_total               1157
_reflns_special_details

 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_refine_diff_density_max         0.263
_refine_diff_density_min         -0.262
_refine_diff_density_rms         0.042
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.084
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     92
_refine_ls_number_reflns         1157
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.084
_refine_ls_R_factor_all          0.0407
_refine_ls_R_factor_gt           0.0339
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0454P)^2^+0.2100P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0854
_refine_ls_wR_factor_ref         0.0914
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            suppl_j_ncrs-2021-0481_suppl.cif
_cod_data_source_block           2
_cod_database_code               8105200
_shelx_estimated_absorpt_t_max   0.984
_shelx_estimated_absorpt_t_min   0.975
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C4(H4), C3(H3)
2.b Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C)
;