Crystal structure of 3-bromo-4-dimethylamino-1-methyl-1,2,4-triazol-5(4<i>H</i>)-one
Laus, Gerhard; Gelbrich, Thomas; Wurst, Klaus; Schottenberger, Herwig; Acta Crystallographica Section E 71 (2015) o23–; doi:10.1107/S205698901402636X

data_2240278
_publ_section_title
;
 Crystal structure of
 3-bromo-4-dimethylamino-1-methyl-1,2,4-triazol-5(4<i>H</i>)-one
;
_journal_coeditor_code           FJ2686
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o23
_journal_paper_doi               10.1107/S205698901402636X
_journal_volume                  71
_journal_year                    2015
_chemical_formula_iupac          'C5 H9 Br N4 O'
_chemical_formula_moiety         'C5 H9 Br N4 O'
_chemical_formula_sum            'C5 H9 Br N4 O'
_chemical_formula_weight         221.07
_chemical_name_systematic
;
3-Bromo-4-dimethylamino-1-methyl-1,2,4-triazol-5(4<i>H</i>)-one
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           12
_space_group_name_Hall           '-C 2y'
_space_group_name_H-M_alt        'C 1 2/m 1'
_symmetry_space_group_name_Hall  '-C 2y'
_symmetry_space_group_name_H-M   'C 1 2/m 1'
_atom_sites_solution_hydrogens   difmap
_audit_creation_method           SHELXL-2014/6
_cell_angle_alpha                90
_cell_angle_beta                 93.869(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.1993(6)
_cell_length_b                   6.9377(4)
_cell_length_c                   7.8771(7)
_cell_measurement_reflns_used    3066
_cell_measurement_temperature    233(2)
_cell_measurement_theta_max      25.0
_cell_measurement_theta_min      1.0
_cell_volume                     828.73(9)
_computing_cell_refinement
;
DENZO (Otwinowski & Minor, 1997) and COLLECT (Hooft, 1998)
;
_computing_data_collection
;
DENZO (Otwinowski & Minor, 1997) and COLLECT (Hooft, 1998)
;
_computing_data_reduction
;
DENZO (Otwinowski & Minor, 1997) and COLLECT (Hooft, 1998)
;
_computing_molecular_graphics
;
Mercury (Macrae <i>et al.</i>,  2006) and ORTEP-3 for Windows (Farrugia,
2012)
;
_computing_publication_material
;
publCIF (Westrip, 2010)
;
_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2008)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      233(2)
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0339
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            2310
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.048
_diffrn_reflns_theta_min         2.592
_exptl_absorpt_coefficient_mu    4.911
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.772
_exptl_crystal_density_method    none
_exptl_crystal_description       prism
_exptl_crystal_F_000             440
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.496
_refine_diff_density_min         -0.442
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     75
_refine_ls_number_reflns         806
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.0334
_refine_ls_R_factor_gt           0.0283
_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^)+(0.0330P)^2^+0.5344P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0631
_refine_ls_wR_factor_ref         0.0650
_reflns_number_gt                734
_reflns_number_total             806
_reflns_threshold_expression     I>2\s(I)
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_cod_data_source_block           I
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_cod_database_fobs_code          2240278
_shelx_hkl_checksum              58751
_shelx_res_checksum              37343
_shelxl_version_number           2014/6