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_1508432
_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_formula_moiety         'C4 H12 P, 0.5(C2 N10)'
_chemical_formula_sum            'C5 H12 N5 P'
_chemical_formula_weight         173.17
_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_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
   Universit\''at Innsbruck
   Innrain 52
   A-6020 Innsbruck
   Austria
;
_audit_creation_date             2008-09-05T20:11:55-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 93.941(17)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   5.9035(9)
_cell_length_b                   13.388(2)
_cell_length_c                   11.3173(19)
_cell_measurement_reflns_used    2186
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      28.3182
_cell_measurement_theta_min      3.4538
_cell_volume                     892.4(2)
_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_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR2002 (Burla et al., 2003)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean 10.3822
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.887
_diffrn_measurement_device_type  'Oxford diffraction GEMINI R ULTRA'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0855102029
_diffrn_orient_matrix_UB_12      0.008828715
_diffrn_orient_matrix_UB_13      -0.0456619928
_diffrn_orient_matrix_UB_21      0.0782496997
_diffrn_orient_matrix_UB_22      -0.0117098339
_diffrn_orient_matrix_UB_23      -0.042434602
_diffrn_orient_matrix_UB_31      -0.0329004845
_diffrn_orient_matrix_UB_32      -0.0509577316
_diffrn_orient_matrix_UB_33      0.0017383075
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.021
_diffrn_reflns_av_unetI/netI     0.0481
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            3626
_diffrn_reflns_theta_full        25.3
_diffrn_reflns_theta_max         28.3182
_diffrn_reflns_theta_min         3.4538
_exptl_absorpt_coefficient_mu    0.257
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.92318
_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            orange-yellow
_exptl_crystal_density_diffrn    1.289
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'fragment of a plate'
_exptl_crystal_F_000             368
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.267
_refine_diff_density_min         -0.242
_refine_diff_density_rms         0.043
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.08
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     104
_refine_ls_number_reflns         1760
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.08
_refine_ls_R_factor_all          0.0391
_refine_ls_R_factor_gt           0.0303
_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^)+(0.0469P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0793
_refine_ls_wR_factor_ref         0.0816
_reflns_number_gt                1461
_reflns_number_total             1760
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file
C5H12N5P_P21_c_CCDC846913_crystals-02-00127-s001_DC177.cif
_cod_data_source_block           VA19_chateigner_1508432
_cod_database_code               1508432