#------------------------------------------------------------------------------
#$Date: 2018-09-01 16:16:27 +0300 (Sat, 01 Sep 2018) $
#$Revision: 210300 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/31/02/4310261.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_4310261
loop_
_publ_author_name
'Klapötke, Thomas M.'
'Krumm, Burkhard'
'Galvez-Ruiz, Juan-Carlos'
'Nöth, Heinrich'
_publ_section_title
;
 Highly Sensitive Ammonium Tetraazidoaurates(III)
;
_journal_coden_ASTM              INOCAJ
_journal_issue                   26
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              9625
_journal_page_last               9627
_journal_paper_doi               10.1021/ic051543i
_journal_volume                  44
_journal_year                    2005
_chemical_formula_sum            'C4 H12 Au N13'
_chemical_formula_weight         439.23
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                94.14(3)
_cell_angle_beta                 93.63(3)
_cell_angle_gamma                110.42(3)
_cell_formula_units_Z            4
_cell_length_a                   9.973(2)
_cell_length_b                   10.246(2)
_cell_length_c                   13.625(3)
_cell_measurement_temperature    293(2)
_cell_volume                     1295.5(5)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.732
_diffrn_measured_fraction_theta_max 0.732
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0253
_diffrn_reflns_av_sigmaI/netI    0.0489
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            6751
_diffrn_reflns_theta_full        29.13
_diffrn_reflns_theta_max         29.13
_diffrn_reflns_theta_min         1.51
_exptl_absorpt_coefficient_mu    11.364
_exptl_crystal_density_diffrn    2.252
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             824
_refine_diff_density_max         2.582
_refine_diff_density_min         -2.929
_refine_diff_density_rms         0.221
_refine_ls_extinction_coef       0.0007(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.954
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     326
_refine_ls_number_reflns         5103
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.954
_refine_ls_R_factor_all          0.0700
_refine_ls_R_factor_gt           0.0444
_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)+(0.0822P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1116
_refine_ls_wR_factor_ref         0.1240
_reflns_number_gt                3569
_reflns_number_total             5103
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic051543isi20050909_081010.cif
_cod_data_source_block           auabs
_cod_original_cell_volume        1295.7(4)
_cod_database_code               4310261
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
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
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Au1 Au 0.56039(4) 0.02502(4) 0.37930(3) 0.03282(15) Uani 1 1 d . . .
Au2 Au 0.46660(4) 0.00573(4) 0.12479(3) 0.03486(15) Uani 1 1 d . . .
N1 N 0.3441(7) -0.0439(7) 0.3724(5) 0.0218(16) Uani 1 1 d . . .
N16 N 0.6738(11) 0.0502(10) 0.1298(7) 0.048(3) Uani 1 1 d . . .
N7 N 0.7805(8) 0.0716(10) 0.3864(7) 0.041(2) Uani 1 1 d . . .
N17 N 0.7353(8) -0.0301(9) 0.1374(6) 0.036(2) Uani 1 1 d . . .
N20 N 0.4836(9) -0.2629(9) 0.1465(7) 0.042(2) Uani 1 1 d . . .
N13 N 0.5001(10) 0.2065(11) 0.0945(8) 0.051(3) Uani 1 1 d . . .
N26 N 0.8764(8) -0.3362(9) 0.3835(6) 0.037(2) Uani 1 1 d . . .
N8 N 0.8501(10) 0.1798(10) 0.3579(6) 0.039(2) Uani 1 1 d . . .
N5 N 0.5224(8) 0.2884(9) 0.3801(6) 0.036(2) Uani 1 1 d . . .
N23 N 0.1701(10) -0.1252(11) 0.1348(7) 0.046(2) Uani 1 1 d . . .
N2 N 0.2786(9) 0.0338(8) 0.3751(6) 0.0367(19) Uani 1 1 d . . .
N14 N 0.6244(12) 0.2844(11) 0.0924(7) 0.049(2) Uani 1 1 d . . .
N4 N 0.6006(10) 0.2259(10) 0.3598(8) 0.048(2) Uani 1 1 d . . .
N25 N 0.1660(9) 0.3388(9) 0.1162(6) 0.039(2) Uani 1 1 d . . .
N10 N 0.5507(9) -0.1735(10) 0.3977(8) 0.049(2) Uani 1 1 d . . .
N11 N 0.4336(10) -0.2659(10) 0.3848(7) 0.042(2) Uani 1 1 d . . .
N22 N 0.2548(11) -0.0093(11) 0.1192(8) 0.057(3) Uani 1 1 d . . .
N19 N 0.4045(10) -0.1971(10) 0.1521(8) 0.049(2) Uani 1 1 d . . .
N18 N 0.8056(10) -0.0966(11) 0.1455(9) 0.066(3) Uani 1 1 d . . .
N3 N 0.2019(10) 0.0952(10) 0.3749(8) 0.057(3) Uani 1 1 d . . .
N12 N 0.3275(10) -0.3601(10) 0.3730(8) 0.053(3) Uani 1 1 d . . .
N24 N 0.0832(11) -0.2251(12) 0.1503(8) 0.059(3) Uani 1 1 d . . .
N9 N 0.9261(10) 0.2835(11) 0.3319(8) 0.056(3) Uani 1 1 d . . .
N6 N 0.4522(10) 0.3553(10) 0.3980(8) 0.055(3) Uani 1 1 d . . .
C3 C 0.2595(12) 0.3464(12) 0.2083(8) 0.053(3) Uani 1 1 d . . .
H3A H 0.2042 0.3382 0.2642 0.079 Uiso 1 1 calc R . .
H3B H 0.3381 0.4344 0.2167 0.079 Uiso 1 1 calc R . .
H3C H 0.2963 0.2714 0.2031 0.079 Uiso 1 1 calc R . .
N21 N 0.5448(11) -0.3411(9) 0.1420(8) 0.061(3) Uani 1 1 d . . .
C2 C 0.2513(12) 0.3532(13) 0.0273(8) 0.051(3) Uani 1 1 d . . .
H2A H 0.1904 0.3499 -0.0310 0.076 Uiso 1 1 calc R . .
H2B H 0.2874 0.2779 0.0204 0.076 Uiso 1 1 calc R . .
H2C H 0.3303 0.4409 0.0361 0.076 Uiso 1 1 calc R . .
C5 C 0.8029(11) -0.4019(13) 0.4682(8) 0.056(3) Uani 1 1 d . . .
H5A H 0.7089 -0.3957 0.4665 0.084 Uiso 1 1 calc R . .
H5B H 0.8579 -0.3539 0.5289 0.084 Uiso 1 1 calc R . .
H5C H 0.7944 -0.4984 0.4642 0.084 Uiso 1 1 calc R . .
N15 N 0.7379(13) 0.3635(11) 0.0899(9) 0.073(3) Uani 1 1 d . . .
C1 C 0.0472(12) 0.2013(11) 0.1041(10) 0.065(4) Uani 1 1 d . . .
H1A H -0.0092 0.1933 0.1594 0.097 Uiso 1 1 calc R . .
H1B H 0.0863 0.1279 0.1008 0.097 Uiso 1 1 calc R . .
H1C H -0.0125 0.1936 0.0443 0.097 Uiso 1 1 calc R . .
C8 C 1.0217(11) -0.3493(14) 0.3880(9) 0.059(3) Uani 1 1 d . . .
H8A H 1.0775 -0.2986 0.4477 0.088 Uiso 1 1 calc R . .
H8B H 1.0697 -0.3114 0.3319 0.088 Uiso 1 1 calc R . .
H8C H 1.0110 -0.4462 0.3872 0.088 Uiso 1 1 calc R . .
C4 C 0.1046(14) 0.4539(12) 0.1270(9) 0.061(3) Uani 1 1 d . . .
H4A H 0.0489 0.4421 0.1829 0.091 Uiso 1 1 calc R . .
H4B H 0.0443 0.4499 0.0683 0.091 Uiso 1 1 calc R . .
H4C H 0.1816 0.5431 0.1369 0.091 Uiso 1 1 calc R . .
C7 C 0.7933(12) -0.4126(14) 0.2885(8) 0.063(4) Uani 1 1 d . . .
H7A H 0.6991 -0.4070 0.2850 0.094 Uiso 1 1 calc R . .
H7B H 0.7852 -0.5090 0.2857 0.094 Uiso 1 1 calc R . .
H7C H 0.8424 -0.3709 0.2339 0.094 Uiso 1 1 calc R . .
C6 C 0.8935(15) -0.1867(13) 0.3890(11) 0.074(4) Uani 1 1 d . . .
H6A H 0.8006 -0.1781 0.3867 0.110 Uiso 1 1 calc R . .
H6B H 0.9424 -0.1455 0.3342 0.110 Uiso 1 1 calc R . .
H6C H 0.9486 -0.1393 0.4498 0.110 Uiso 1 1 calc R . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Au Au -2.0133 8.8022 '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
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N4 Au1 N1 99.7(3) . . ?
N4 Au1 N10 171.6(4) . . ?
N1 Au1 N10 88.6(3) . . ?
N4 Au1 N7 86.9(4) . . ?
N1 Au1 N7 173.3(3) . . ?
N10 Au1 N7 84.7(4) . . ?
N16 Au2 N19 99.5(4) . . ?
N16 Au2 N13 88.3(4) . . ?
N19 Au2 N13 172.2(4) . . ?
N16 Au2 N22 171.4(4) . . ?
N19 Au2 N22 89.0(4) . . ?
N13 Au2 N22 83.2(4) . . ?
N2 N1 Au1 122.5(6) . . ?
N17 N16 Au2 126.4(9) . . ?
N8 N7 Au1 116.6(7) . . ?
N18 N17 N16 173.7(10) . . ?
N21 N20 N19 171.4(11) . . ?
N14 N13 Au2 117.4(8) . . ?
C6 N26 C5 110.6(9) . . ?
C6 N26 C7 110.8(10) . . ?
C5 N26 C7 109.8(8) . . ?
C6 N26 C8 109.3(9) . . ?
C5 N26 C8 107.9(8) . . ?
C7 N26 C8 108.3(8) . . ?
N9 N8 N7 175.5(11) . . ?
N6 N5 N4 176.3(10) . . ?
N24 N23 N22 173.4(11) . . ?
N3 N2 N1 172.2(10) . . ?
N15 N14 N13 176.1(12) . . ?
N5 N4 Au1 124.3(7) . . ?
C1 N25 C3 108.4(9) . . ?
C1 N25 C2 109.3(8) . . ?
C3 N25 C2 110.4(8) . . ?
C1 N25 C4 109.4(9) . . ?
C3 N25 C4 108.8(8) . . ?
C2 N25 C4 110.5(9) . . ?
N11 N10 Au1 117.5(7) . . ?
N12 N11 N10 175.1(10) . . ?
N23 N22 Au2 114.4(7) . . ?
N20 N19 Au2 122.1(8) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Au1 N4 1.996(9) . ?
Au1 N1 2.015(6) . ?
Au1 N10 2.037(10) . ?
Au1 N7 2.071(7) . ?
Au2 N16 1.950(10) . ?
Au2 N19 2.021(10) . ?
Au2 N13 2.043(10) . ?
Au2 N22 2.059(10) . ?
N1 N2 1.193(10) . ?
N16 N17 1.191(11) . ?
N7 N8 1.192(13) . ?
N17 N18 1.141(12) . ?
N20 N21 1.165(12) . ?
N20 N19 1.206(12) . ?
N13 N14 1.221(14) . ?
N26 C6 1.477(14) . ?
N26 C5 1.483(13) . ?
N26 C7 1.496(13) . ?
N26 C8 1.500(12) . ?
N8 N9 1.164(13) . ?
N5 N6 1.163(11) . ?
N5 N4 1.202(12) . ?
N23 N24 1.131(14) . ?
N23 N22 1.236(14) . ?
N2 N3 1.147(12) . ?
N14 N15 1.144(14) . ?
N25 C1 1.481(12) . ?
N25 C3 1.497(12) . ?
N25 C2 1.510(13) . ?
N25 C4 1.510(13) . ?
N10 N11 1.212(12) . ?
N11 N12 1.150(12) . ?
