#------------------------------------------------------------------------------
#$Date: 2016-03-21 18:22:36 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178810 $
#$URL: svn://www.crystallography.net/cod/cif/4/10/64/4106499.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4106499
loop_
_publ_author_name
'Jürgen Evers'
'Michael Göbel'
'Burkhard Krumm'
'Franz Martin'
'Sergey Medvedyev'
'Gilbert Oehlinger'
'Franz Xaver Steemann'
'Ivan Troyan'
'Thomas M. Klapötke'
'Mikhail I. Eremets'
_publ_contact_author_address
;
Department Chemie
Ludwig-Maximilians Universität
Butenandtstraße 5-13 (Haus D)
D-81377 München
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. Klapoẗke'
_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
;
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
;
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
;
'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-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 κ-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/[σ²(Fo²)+(0.0347P)²+0.0000P] where P=(Fo²+2Fc²)/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     >2σ(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
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'x, -y, z+1/2'
'x+1/2, y+1/2, z'
'x+1/2, -y+1/2, z+1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
N5 N 0.27915(16) -0.21653(12) 0.4929(2) 0.0235(3) Uani 1 1 d
N8 N 0.44035(14) -0.41058(11) 0.9965(2) 0.0224(3) Uani 1 1 d
N2 N 0.31124(15) 0.07526(15) 0.4876(2) 0.0223(3) Uani 1 1 d
N6 N 0.18872(19) -0.17458(13) 0.4819(3) 0.0340(5) Uani 1 1 d
N11 N 0.14929(13) -0.44664(12) 1.0013(2) 0.0242(3) Uani 1 1 d
N10 N 0.11706(16) -0.34499(13) 0.9996(3) 0.0327(4) Uani 1 1 d
N4 N 0.38330(15) -0.24969(15) 0.5068(3) 0.0325(4) Uani 1 1 d
N1 N 0.21151(17) 0.10834(14) 0.4920(3) 0.0294(4) Uani 1 1 d
N7 N 0.47012(15) -0.51109(12) 0.9811(2) 0.0282(3) Uani 1 1 d
N12 N 0.18930(15) -0.53459(13) 1.0021(3) 0.0350(4) Uani 1 1 d
N9 N 0.40121(17) -0.32402(13) 1.0087(3) 0.0332(4) Uani 1 1 d
N3 N 0.39697(18) 0.03443(15) 0.4841(3) 0.0330(4) Uani 1 1 d
H4 H 0.387(3) -0.3147(19) 0.502(4) 0.037(6) Uiso 1 1 d
H1 H 0.217(3) 0.1827(18) 0.490(4) 0.037(6) Uiso 1 1 d
H7 H 0.543(3) -0.5136(19) 0.984(4) 0.035(6) Uiso 1 1 d
H10 H 0.047(3) -0.343(2) 0.998(5) 0.048(7) Uiso 1 1 d
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
N5 0.0274(8) 0.0174(7) 0.0282(6) -0.0003(5) 0.0157(5) -0.0019(5)
N8 0.0212(6) 0.0243(7) 0.0252(7) 0.0013(5) 0.0141(5) -0.0020(6)
N2 0.0249(8) 0.0175(7) 0.0252(6) -0.0023(4) 0.0129(5) -0.0031(5)
N6 0.0340(11) 0.0275(11) 0.0449(10) -0.0028(7) 0.0229(8) 0.0006(7)
N11 0.0204(7) 0.0257(7) 0.0281(7) -0.0014(5) 0.0133(5) -0.0023(6)
N10 0.0298(10) 0.0221(6) 0.0539(9) -0.0020(6) 0.0265(8) -0.0026(6)
N4 0.0313(9) 0.0192(7) 0.0550(10) 0.0005(7) 0.0274(7) 0.0007(7)
N1 0.0290(9) 0.0203(7) 0.0460(9) -0.0009(7) 0.0239(7) -0.0008(7)
N7 0.0290(9) 0.0215(6) 0.0429(8) -0.0033(6) 0.0245(7) 0.0001(6)
N12 0.0337(9) 0.0285(10) 0.0453(10) -0.0019(7) 0.0214(8) 0.0038(8)
N9 0.0340(10) 0.0247(11) 0.0480(10) 0.0020(7) 0.0256(8) 0.0026(7)
N3 0.0298(9) 0.0285(10) 0.0455(9) -0.0026(7) 0.0224(8) 0.0029(7)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
N6 N5 N4 172.64(18)
N9 N8 N7 172.56(18)
N3 N2 N1 172.9(2)
N12 N11 N10 173.00(18)
N11 N10 H10 109.2(18)
N5 N4 H4 113(2)
N2 N1 H1 103.2(18)
N8 N7 H7 110.7(15)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
N5 N6 1.126(3)
N5 N4 1.227(2)
N8 N9 1.1226(18)
N8 N7 1.2360(18)
N2 N3 1.113(3)
N2 N1 1.234(2)
N11 N12 1.121(2)
N11 N10 1.236(2)
N10 H10 0.81(3)
N4 H4 0.76(2)
N1 H1 0.87(2)
N7 H7 0.84(3)
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N4 H4 N7 0.76(2) 2.27(2) 2.989(2) 157(3) 2_544
N1 H1 N10 0.87(2) 2.23(2) 2.968(2) 143(2) 2_554
N1 H1 N9 0.87(2) 2.64(3) 3.299(2) 133(2) 2_554
N7 H7 N1 0.84(3) 2.22(3) 2.988(2) 152(2) 4_545
N10 H10 N4 0.81(3) 2.21(3) 2.950(2) 153(2) 4_445
