#------------------------------------------------------------------------------
#$Date: 2016-03-25 23:10:29 +0200 (Fri, 25 Mar 2016) $
#$Revision: 180028 $
#$URL: svn://www.crystallography.net/cod/cif/7/03/22/7032240.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_7032240
loop_
_publ_author_name
'Guńka, Piotr A'
'Kraszewski, Karol'
'Chen, Yu-Sheng'
'Zachara, Janusz'
_publ_section_title
;
 The structure and energetics of arsenic(iii) oxide intercalated by ionic
 azides.
;
_journal_issue                   33
_journal_name_full               'Dalton transactions'
_journal_page_first              12776
_journal_page_last               12783
_journal_paper_doi               10.1039/c4dt01569j
_journal_volume                  43
_journal_year                    2014
_chemical_formula_moiety         '2(As2 O3), N3, NH4'
_chemical_formula_sum            'As4 H4 N4 O6'
_chemical_formula_weight         455.76
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      hexagonal
_space_group_IT_number           191
_space_group_name_Hall           '-P 6 2'
_space_group_name_H-M_alt        'P 6/m m m'
_symmetry_space_group_name_Hall  '-P 6 2'
_symmetry_space_group_name_H-M   'P 6/m m m'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     iterative
_audit_creation_date             2014-04-09
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2014.03.20 svn.r2918 for OlexSys, GUI svn.r4816)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            1
_cell_length_a                   5.2354(3)
_cell_length_b                   5.2354(3)
_cell_length_c                   9.6787(5)
_cell_measurement_reflns_used    3746
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      29.1840
_cell_measurement_theta_min      4.1760
_cell_volume                     229.75(2)
_computing_cell_refinement
'CrysAlisPro, Agilent Technologies, Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) (compiled Feb 1 2013,16:14:44)'
_computing_data_collection
'CrysAlisPro, Agilent Technologies, Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) (compiled Feb 1 2013,16:14:44)'
_computing_data_reduction
'CrysAlisPro, Agilent Technologies, Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) (compiled Feb 1 2013,16:14:44)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2013)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 10.3347
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      0.1419900000
_diffrn_orient_matrix_UB_12      0.1277204000
_diffrn_orient_matrix_UB_13      0.0019393000
_diffrn_orient_matrix_UB_21      0.0656406000
_diffrn_orient_matrix_UB_22      -0.0899021000
_diffrn_orient_matrix_UB_23      -0.0042678000
_diffrn_orient_matrix_UB_31      -0.0000610000
_diffrn_orient_matrix_UB_32      0.0086422000
_diffrn_orient_matrix_UB_33      -0.0731431000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0493
_diffrn_reflns_av_unetI/netI     0.0135
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            7048
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.396
_diffrn_reflns_theta_min         4.211
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    14.432
_exptl_absorpt_correction_T_max  0.734
_exptl_absorpt_correction_T_min  0.160
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
'CrysAlisPro, Agilent Technologies, Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) (compiled Feb 1 2013,16:14:44) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    3.294
_exptl_crystal_description       plate
_exptl_crystal_F_000             212
_exptl_crystal_size_max          0.2032
_exptl_crystal_size_mid          0.1744
_exptl_crystal_size_min          0.0162
_refine_diff_density_max         0.456
_refine_diff_density_min         -0.386
_refine_diff_density_rms         0.092
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.220
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     15
_refine_ls_number_reflns         171
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.220
_refine_ls_R_factor_all          0.0192
_refine_ls_R_factor_gt           0.0155
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0187P)²+0.1827P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0379
_refine_ls_wR_factor_ref         0.0388
_reflns_Friedel_coverage         0.000
_reflns_number_gt                158
_reflns_number_total             171
_reflns_threshold_expression     'I > 2σ(I)'
_iucr_refine_instructions_details
;
TITL
CELL 0.71073 5.235406 5.235406 9.678698 90 90 120
ZERR 1 0.000262 0.000262 0.000537 0 0 0
LATT 1
SYMM -Y+X,+X,+Z
SYMM -Y,+X-Y,+Z
SYMM -X,-Y,+Z
SYMM +Y-X,-X,+Z
SYMM +Y,-X+Y,+Z
SYMM -Y+X,-Y,-Z
SYMM -X,-X+Y,-Z
SYMM +Y,+X,-Z
SYMM -Y,-X,-Z
SYMM +Y-X,+Y,-Z
SYMM +X,+X-Y,-Z

SFAC As H N O
UNIT 4.00008 4.00008 4.00008 6

L.S. 10
PLAN  20
rem DFIX 0.901 0.000001 N1 H1b N1 H1a
bond $H
more -3
fmap 2
acta
REM <HKL>/home/piogun/struct/pg42_As2O3_NH4N3_final/pg42.hkl</HKL>

WGHT    0.018700    0.182700
FVAR       2.60657
AS1   1    0.333333    0.666667    0.277364    10.16667    0.01085    0.01085 =
         0.02320    0.00000    0.00000    0.00542
O1    4    0.500000    1.000000    0.178211    10.25000    0.01543    0.00807 =
         0.02737    0.00000    0.00000    0.00403
N1    3    0.000000    0.000000    0.000000    10.04167    0.02592    0.02592 =
         0.02622    0.00000    0.00000    0.01296
H1A   2   10.000000   10.000000   10.093090    10.04167   -1.50000
H1B   2   10.000000   10.162621    9.969529    10.12500   -1.50000
N2    3    0.000000    0.000000    0.500000    10.04167    0.01853    0.01853 =
         0.03751    0.00000    0.00000    0.00927
N3    3    0.000000    0.000000    0.378792    10.08333    0.04795    0.04795 =
         0.02889    0.00000    0.00000    0.02397
HKLF 4

REM
REM R1 =  0.0155 for     158 Fo > 4sig(Fo)  and  0.0192 for all     171 data
REM     15 parameters refined using      0 restraints

END

WGHT      0.0186      0.1836

REM Highest difference peak  0.456,  deepest hole -0.386,  1-sigma level  0.092
Q1    1   0.4519  0.9038  0.2053  10.50000  0.05    0.37
Q2    1   0.2831  0.7169  0.3470  10.50000  0.05    0.34
Q3    1   0.1685  0.3369  0.0000  10.25000  0.05    0.30
Q4    1   0.2138  0.4275  0.5000  10.25000  0.05    0.25
Q5    1   0.5000  1.0000  0.2903  10.25000  0.05    0.24
Q6    1   0.1602  0.3204 -0.1131  10.50000  0.05    0.22
Q7    1   0.3149  0.0000  0.3530  10.50000  0.05    0.21
Q8    1   0.7363  1.0000  0.2792  10.50000  0.05    0.21
Q9    1   0.2545  0.5089  0.0000  10.25000  0.05    0.19
Q10   1   0.1786  0.3573  0.3178  10.50000  0.05    0.18
Q11   1   0.0822  0.1644  0.2828  10.50000  0.05    0.16
Q12   1   0.2214  0.2214  0.1789  10.50000  0.05    0.15
Q13   1   0.0000  0.3029 -0.0484  10.50000  0.05    0.15
Q14   1   0.1280  0.2560  0.1914  10.50000  0.05    0.14
Q15   1   0.3333  0.6667  0.5000  10.08333  0.05    0.14
Q16   1   0.5843  1.1686  0.1111  10.50000  0.05    0.14
Q17   1   0.3431  0.1715  0.4065  10.50000  0.05    0.13
Q18   1   0.6813  1.0866  0.1365  11.00000  0.05    0.13
Q19   1   0.4652  1.2326  0.1135  10.50000  0.05    0.13
Q20   1   0.0956  0.1913  0.3674  10.50000  0.05    0.12
;
_cod_duplicate_entry             7032246
_cod_data_source_file            allP.cif
_cod_data_source_block           pg42
_cod_original_cell_volume        229.75(3)
_cod_database_code               7032240
#BEGIN Tags that were not found in dictionaries:
_shelxl_version_number           2014-1
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_reflns_odcompleteness_completeness 99.25
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All N(H,H) groups
2. Others
 Fixed Sof: H1A(0.04167) H1B(0.125)
 Fixed X: H1A(0) H1B(0)
 Fixed Y: H1A(0) H1B(0.162621)
 Fixed Z: H1A(0.09309) H1B(-0.030471)
;
_shelx_res_checksum              39837
#END Tags that were not found in dictionaries
loop_
_space_group_symop_operation_xyz
'x, y, z'
'x-y, x, z'
'-y, x-y, z'
'-x, -y, z'
'-x+y, -x, z'
'y, -x+y, z'
'x-y, -y, -z'
'-x, -x+y, -z'
'y, x, -z'
'-y, -x, -z'
'-x+y, y, -z'
'x, x-y, -z'
'-x, -y, -z'
'-x+y, -x, -z'
'y, -x+y, -z'
'x, y, -z'
'x-y, x, -z'
'-y, x-y, -z'
'-x+y, y, z'
'x, x-y, z'
'-y, -x, z'
'y, x, z'
'x-y, -y, z'
'-x, -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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
As1 As 0.3333 0.6667 0.27736(4) 0.01497(17) Uani 1 6 d S T P
O1 O 0.5000 1.0000 0.1782(3) 0.0178(5) Uani 1 4 d S T P
N1 N 0.0000 0.0000 0.0000 0.0260(18) Uani 1 24 d S T P
H1A H 0.0000 0.0000 0.0931 0.039 Uiso 0.5 12 d RS T P
H1B H 0.0000 0.1626 -0.0305 0.039 Uiso 0.25 2 d RS T P
N2 N 0.0000 0.0000 0.5000 0.0249(18) Uani 1 24 d S T P
N3 N 0.0000 0.0000 0.3788(7) 0.0416(18) Uani 1 12 d S T P
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
As1 0.01085(19) 0.01085(19) 0.0232(3) 0.000 0.000 0.00542(10)
O1 0.0154(9) 0.0081(11) 0.0274(11) 0.000 0.000 0.0040(5)
N1 0.026(3) 0.026(3) 0.026(4) 0.000 0.000 0.0130(14)
N2 0.019(3) 0.019(3) 0.038(5) 0.000 0.000 0.0093(13)
N3 0.048(3) 0.048(3) 0.029(3) 0.000 0.000 0.0240(14)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
As As 0.0499 2.0058 '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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
0 0 1 0.0152 0.0031 0.0010 0.9990 0.0025 -0.0041 -0.0731
0 0 -1 0.0010 -0.0031 -0.0010 -0.9990 -0.0025 0.0041 0.0731
1 0 0 0.0936 0.9983 0.0005 -0.0132 0.1418 0.0655 0.0009
-1 0 0 0.0818 -0.9983 -0.0005 0.0132 -0.1418 -0.0655 -0.0009
0 1 0 0.0788 -0.0008 0.9988 -0.0094 0.1274 -0.0898 0.0093
0 -1 0 0.0977 0.0008 -0.9988 0.0094 -0.1274 0.0898 -0.0093
1 -1 0 0.0634 0.9991 -0.9983 -0.0038 0.0143 0.1553 -0.0084
-1 1 0 0.1109 -0.9991 0.9983 0.0038 -0.0143 -0.1553 0.0084
-2 1 0 0.1112 -1.9974 0.9979 0.0170 -0.1561 -0.2209 0.0075
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
O1 As1 O1 93.95(9) . 3_665
O1 As1 O1 93.95(9) . 2_655
O1 As1 O1 93.95(9) 3_665 2_655
As1 O1 As1 115.17(14) 2_665 .
H1A N1 H1B 109.106(1) . .
N3 N2 N3 180.0 13_556 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
As1 O1 1.7903(14) .
As1 O1 1.7903(14) 2_655
As1 O1 1.7903(14) 3_665
O1 As1 1.7903(14) 2_665
N1 H1A 0.90099(5) .
N1 H1B 0.90102(4) .
N2 N3 1.173(7) 13_556
N2 N3 1.173(7) .
