Sensitivities of Some Imidazole-1-sulfonyl Azide Salts
Niko Fischer; Ethan D. Goddard-Borger; Robert Greiner; Thomas M. Klapötke; Brian W. Skelton; Jörg Stierstorfer; Journal of Organic Chemistry 77 (2012) 1760–1764; doi:10.1021/jo202264r

data_4026960
_publ_contact_author_address
;
   Department of Chemistry
   University of Western Australia
   35 Stirling Highway
   Crawley
   Western Australia 6009
   Australia
;
_publ_contact_author_email       bws@crystal.uwa.edu.au
_publ_contact_author_fax         (+61)_08_6488_1118
_publ_contact_author_name        'Skelton, B. W.'
_publ_contact_author_phone       (+61)_08_6488_7107
_publ_section_title
;
 Sensitivities of Some Imidazole-1-sulfonyl Azide Salts
;
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              1760
_journal_page_last               1764
_journal_paper_doi               10.1021/jo202264r
_journal_volume                  77
_journal_year                    2012
_chemical_formula_moiety         'C3 H4 N5 O2 S, Cl'
_chemical_formula_sum            'C3 H4 Cl N5 O2 S'
_chemical_formula_weight         209.62
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_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             2007-06-08T19:57:37-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 100.049(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.4067(2)
_cell_length_b                   9.2983(3)
_cell_length_c                   11.9830(3)
_cell_measurement_reflns_used    7032
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      34.369
_cell_measurement_theta_min      2.7792
_cell_volume                     812.61(4)
_computing_cell_refinement
;
        CrysAlis RED, Oxford Diffraction Ltd.,
        Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET)
        (compiled May  8 2007,13:10:02)
;
_computing_data_collection
;
        CrysAlis CCD, Oxford Diffraction Ltd.,
        Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET)
        (compiled May  8 2007,13:10:02)
;
_computing_data_reduction
;
        CrysAlis RED, Oxford Diffraction Ltd.,
        Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET)
        (compiled May  8 2007,13:10:02)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 16.0009
_diffrn_measured_fraction_theta_full 0.99
_diffrn_measured_fraction_theta_max 0.972
_diffrn_measurement_device_type
;
 Oxford Diffraction Xcalibur diffractometer
;
_diffrn_measurement_method       '\p and \w scans'
_diffrn_orient_matrix_UB_11      0.0692337738
_diffrn_orient_matrix_UB_12      0.0007571259
_diffrn_orient_matrix_UB_13      -0.0340779324
_diffrn_orient_matrix_UB_21      -0.0221255093
_diffrn_orient_matrix_UB_22      0.0723266059
_diffrn_orient_matrix_UB_23      -0.0152777463
_diffrn_orient_matrix_UB_31      0.0644944257
_diffrn_orient_matrix_UB_32      0.0241492843
_diffrn_orient_matrix_UB_33      0.0470659144
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0357
_diffrn_reflns_av_unetI/netI     0.046
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            16883
_diffrn_reflns_theta_full        34
_diffrn_reflns_theta_max         34.46
_diffrn_reflns_theta_min         2.79
_exptl_absorpt_coefficient_mu    0.694
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.98582
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
        CrysAlis RED, Oxford Diffraction Ltd.,
        Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET)
        (compiled May  8 2007,13:10:02)
        empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.713
_exptl_crystal_description       plate
_exptl_crystal_F_000             424
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.482
_refine_diff_density_min         -0.428
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.985
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     109
_refine_ls_number_reflns         3335
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.985
_refine_ls_R_factor_all          0.0462
_refine_ls_R_factor_gt           0.0291
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0458P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0771
_refine_ls_wR_factor_ref         0.0813
_reflns_number_gt                2336
_reflns_number_total             3335
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            jo202264r_si_003.cif
_cod_data_source_block           edg601
_cod_original_sg_symbol_Hall     -P_2ybc
_cod_database_code               4026960