Synthesis and Crystal Structures of New 5,5'-Azotetrazolates
Laus, Gerhard; Kahlenberg, Volker; Wurst, Klaus; Schottenberger, Herwig; Fischer, Niko; Stierstorfer, Jοrg; Klapοtke, Thomas M.; Crystals 2 (2012) 127–136; doi:10.3390/cryst2010127

data_1508433
_publ_section_title
;
 Synthesis and Crystal Structures of New 5,5'-Azotetrazolates
;
_journal_issue                   1
_journal_name_full               Crystals
_journal_page_first              127
_journal_page_last               136
_journal_paper_doi               10.3390/cryst2010127
_journal_volume                  2
_journal_year                    2012
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C3 H9 O S, 0.5(C2 N10)'
_chemical_formula_sum            'C4 H9 N5 O S'
_chemical_formula_weight         175.23
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_author_name               'V. Kahlenberg'
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.3
_audit_contact_author_address
;
  Institut f\"ur Mineralogie und Petrographie
  Leopold-Franzens-Universit\"at Innsbruck
  Innrain 52
  A-6020 Innsbruck
  Austria
;
_audit_contact_author_email      Volker.Kahlenberg@uibk.ac.at
_audit_contact_author_fax        '+43 512 507 2926'
_audit_contact_author_phone      '+43 512 507 5503'
_audit_creation_date             2008-09-06T17:22:40-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 102.036(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   5.2452(2)
_cell_length_b                   14.0290(4)
_cell_length_c                   10.7735(4)
_cell_measurement_reflns_used    4513
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      28.3777
_cell_measurement_theta_min      3.4811
_cell_measurement_wavelength     0.71073
_cell_volume                     775.34(5)
_computing_cell_refinement
;
        CrysAlis RED, Oxford Diffraction Ltd.,
        Version 1.171.32.24 (release 21-04-2008 CrysAlis171 .NET)
        (compiled Apr 21 2008,18:23:10)
;
_computing_data_collection
;
        CrysAlis CCD, Oxford Diffraction Ltd.,
        Version 1.171.32.24 (release 21-04-2008 CrysAlis171 .NET)
        (compiled Apr 21 2008,18:23:10)
;
_computing_data_reduction
;
        CrysAlis RED, Oxford Diffraction Ltd.,
        Version 1.171.32.24 (release 21-04-2008 CrysAlis171 .NET)
        (compiled Apr 21 2008,18:23:10)
;
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR2002 (Burla et al., 2002)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean 10.3822
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.887
_diffrn_measurement_device_type  'Oxford Diffraction Gemini-R Ultra'
_diffrn_measurement_method       '\w (1\% width)'
_diffrn_orient_matrix_UB_11      0.0409523065
_diffrn_orient_matrix_UB_12      0.0338672607
_diffrn_orient_matrix_UB_13      0.0490492421
_diffrn_orient_matrix_UB_21      0.1100552823
_diffrn_orient_matrix_UB_22      -0.0286493873
_diffrn_orient_matrix_UB_23      0.0250338583
_diffrn_orient_matrix_UB_31      0.0729066483
_diffrn_orient_matrix_UB_32      0.0243096861
_diffrn_orient_matrix_UB_33      -0.038735024
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0207
_diffrn_reflns_av_unetI/netI     0.036
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            6332
_diffrn_reflns_theta_full        25.3
_diffrn_reflns_theta_max         28.3777
_diffrn_reflns_theta_min         3.4811
_exptl_absorpt_coefficient_mu    0.368
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.95841
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
        CrysAlis RED, Oxford Diffraction Ltd.,
        Version 1.171.32.24 (release 21-04-2008 CrysAlis171 .NET)
        (compiled Apr 21 2008,18:23:10)
        Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.501
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'isometric fragment'
_exptl_crystal_F_000             368
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.337
_refine_diff_density_min         -0.308
_refine_diff_density_rms         0.046
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     103
_refine_ls_number_reflns         1723
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0312
_refine_ls_R_factor_gt           0.0276
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0342P)^2^+0.3450P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0703
_refine_ls_wR_factor_ref         0.0717
_reflns_number_gt                1573
_reflns_number_total             1723
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file
C4H9N5OS_P21_n_CCDC846914_crystals-02-00127-s001_DC178.cif
_cod_data_source_block           messung_od_chateigner_1508433
_cod_database_code               1508433
_audit_contact_author            'V. Kahlenberg'