Synthesis and reactivity of an unexpected highly sensitive 1-carboxymethyl-3-diazonio-5-nitrimino-1,2,4-triazole
Klapötke, Thomas M.; Nordheider, Andreas; Stierstorfer, Jörg; New Journal of Chemistry 36 (2012) 1463–; doi:10.1039/c2nj40044h

data_7052903
_publ_section_title
;
 Synthesis and reactivity of an unexpected highly sensitive
 1-carboxymethyl-3-diazonio-5-nitrimino-1,2,4-triazole
;
_journal_issue                   7
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              1463
_journal_paper_doi               10.1039/c2nj40044h
_journal_volume                  36
_journal_year                    2012
_chemical_formula_moiety         'C4 H4 N8 O4'
_chemical_formula_sum            'C4 H4 N8 O4'
_chemical_formula_weight         228.15
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_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
_audit_creation_date
;
'Wed Sep 29 23:52:48 2010'
;
_audit_creation_method           SHELXL-97
_audit_update_record             30.9.2010
_cell_angle_alpha                90.00
_cell_angle_beta                 98.873(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.3123(7)
_cell_length_b                   6.8821(5)
_cell_length_c                   12.2305(9)
_cell_measurement_reflns_used    1516
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      33.7518
_cell_measurement_theta_min      4.1715
_cell_volume                     857.61(11)
_computing_cell_refinement
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.27p5 beta (release 01-04-2005 CrysAlis171 .NET)
(compiled Apr 1 2005,17:53:34)
;
_computing_data_collection
;
CrysAlis CCD, Oxford Diffraction Ltd.,
Version 1.171.27p5 beta (release 01-04-2005 CrysAlis171 .NET)
(compiled Apr 1 2005,17:53:34)
;
_computing_data_reduction
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.27p5 beta (release 01-04-2005 CrysAlis171 .NET)
(compiled Apr 1 2005,17:53:34)
;
_computing_molecular_graphics
;
'ORTEP (M. N. Burnett, C. K. Johnson, ORTEP-III: Oak Ridge Thermal Ellipsoid
;
_computing_publication_material
'PLATON (A. L. Spek, Acta Crystallogr, Sect. A, 1990, 46, C34, 1995 version).'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    SIR-92
_diffrn_ambient_temperature      173
_diffrn_detector_area_resol_mean 15.9809
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device       'CCD camera on \k-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       omega-scan
_diffrn_orient_matrix_UB_11      -0.0320430045
_diffrn_orient_matrix_UB_12      -0.0126760475
_diffrn_orient_matrix_UB_13      -0.0552976719
_diffrn_orient_matrix_UB_21      -0.0614808033
_diffrn_orient_matrix_UB_22      0.0170774204
_diffrn_orient_matrix_UB_23      0.0174695740
_diffrn_orient_matrix_UB_31      0.0063436865
_diffrn_orient_matrix_UB_32      0.1009839870
_diffrn_orient_matrix_UB_33      -0.0099073426
_diffrn_radiation_collimation    0.5
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0286
_diffrn_reflns_av_sigmaI/netI    0.0479
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            4250
_diffrn_reflns_theta_full        25.98
_diffrn_reflns_theta_max         25.98
_diffrn_reflns_theta_min         4.18
_diffrn_source_current           40
_diffrn_source_type              'Spellman generator'
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    0.156
_exptl_absorpt_correction_T_max  0.9800
_exptl_absorpt_correction_T_min  0.9561
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;SCALE3 ABSPACK - An Oxford Diffraction program (1.0.4,gui:1.0.3)
(C) 2005 Oxford Diffraction Ltd.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.767
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             464
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.170
_refine_diff_density_min         -0.216
_refine_diff_density_rms         0.039
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.859
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     161
_refine_ls_number_reflns         1677
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.859
_refine_ls_R_factor_all          0.0557
_refine_ls_R_factor_gt           0.0330
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0665
_refine_ls_wR_factor_ref         0.0705
_reflns_number_gt                1124
_reflns_number_total             1677
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2nj40044h.txt
_cod_data_source_block           fx441
_cod_original_sg_symbol_Hall     '-P 2ybc '
_cod_database_code               7052903