Molecular Structure of Hydrazoic Acid with Hydrogen-Bonded Tetramers in Nearly Planar Layers
Jürgen Evers; Michael Göbel; Burkhard Krumm; Franz Martin; Sergey Medvedyev; Gilbert Oehlinger; Franz Xaver Steemann; Ivan Troyan; Thomas M. Klapötke; Mikhail I. Eremets; Journal of the American Chemical Society 133 (2011) 12100–12105; doi:10.1021/ja2027053

data_4106499
_publ_contact_author_address
;
Department Chemie
Ludwig-Maximilians Universit\"at
Butenandtstra\&se 5-13 (Haus D)
D-81377 M\"unchen
Bundesrepublik Deutschland
;
_publ_contact_author_email       tmk@cup.uni-muenchen.de
_publ_contact_author_fax         +49-89-2180-77491
_publ_contact_author_name        'Thomas M. Klapo\"tke'
_publ_contact_author_phone       +49-89-2180-77492
_publ_section_title
;
 Molecular Structure of Hydrazoic Acid with Hydrogen-Bonded Tetramers in
 Nearly Planar Layers
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              12100
_journal_page_last               12105
_journal_paper_doi               10.1021/ja2027053
_journal_volume                  133
_journal_year                    2011
_chemical_formula_moiety         'H N3'
_chemical_formula_sum            'H N3'
_chemical_formula_weight         43.028
_chemical_name_common            'hydrazoic acid'
_chemical_name_systematic        'hydrogen azide'
_space_group_IT_number           9
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date
;
'Sun Nov 29 04:44:09 2009'
;
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 119.57(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            16
_cell_length_a                   11.607(2)
_cell_length_b                   11.6091(12)
_cell_length_c                   6.7825(14)
_cell_measurement_reflns_used    2995
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      32.3985
_cell_measurement_theta_min      4.9052
_cell_volume                     794.9(3)
_computing_cell_refinement
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET)
(compiled May  6 2009,17:20:42)
;
_computing_data_collection
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CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET)
(compiled May  6 2009,17:20:42)
;
_computing_data_reduction
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CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET)
(compiled May  6 2009,17:20:42)
;
_computing_molecular_graphics
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'ORTEP (M. N. Burnett, C. K. Johnson, ORTEP-III: Oak Ridge Thermal Ellipsoid
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_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-97
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 15.9809
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_details
;
  1 omega    0.00  101.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       30.0000   70.0000    0.0000 101

  2 omega    0.00  101.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       30.0000   70.0000  120.0000 101

  3 omega    0.00  101.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       30.0000   70.0000  240.0000 101

  4 omega  -41.00   60.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       30.0000  -70.0000    0.0000 101

  5 omega  -41.00   60.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       30.0000  -70.0000  120.0000 101

  6 omega  -41.00   60.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       30.0000  -70.0000  240.0000 101

;
_diffrn_measurement_device       'CCD camera on \k-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       omega-scan
_diffrn_orient_matrix_UB_11      -0.0142039012
_diffrn_orient_matrix_UB_12      0.0462182988
_diffrn_orient_matrix_UB_13      0.0533393058
_diffrn_orient_matrix_UB_21      -0.0502407984
_diffrn_orient_matrix_UB_22      -0.0337648295
_diffrn_orient_matrix_UB_23      0.0026983646
_diffrn_orient_matrix_UB_31      0.0473089463
_diffrn_orient_matrix_UB_32      -0.0219209301
_diffrn_orient_matrix_UB_33      0.1081001480
_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     0.71069
_diffrn_reflns_av_R_equivalents  0.0277
_diffrn_reflns_av_sigmaI/netI    0.0184
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            3973
_diffrn_reflns_theta_full        26.49
_diffrn_reflns_theta_max         26.49
_diffrn_reflns_theta_min         4.93
_diffrn_source_current           40
_diffrn_source_type              'Spellman generator'
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    0.120
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.26973
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET)
(compiled May  6 2009,17:20:42)
empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.4384(4)
_exptl_crystal_description       capillary
_exptl_crystal_F_000             352
_exptl_crystal_size_max          0.02
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.124
_refine_diff_density_min         -0.108
_refine_diff_density_rms         0.025
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     125
_refine_ls_number_reflns         828
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0244
_refine_ls_R_factor_gt           0.0208
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0347P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0494
_refine_ls_wR_factor_ref         0.0504
_reflns_number_gt                752
_reflns_number_total             828
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ja2027053_si_001.cif
_cod_data_source_block           ex558_4_Cc_HN3
_cod_original_cell_volume        794.8(2)
_cod_database_code               4106499