#------------------------------------------------------------------------------
#$Date: 2016-03-25 23:10:29 +0200 (Fri, 25 Mar 2016) $
#$Revision: 180028 $
#$URL: svn://www.crystallography.net/cod/cif/7/03/22/7032247.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_7032247
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, K'
_chemical_formula_sum            'As4 K N3 O6'
_chemical_formula_weight         476.81
_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_primary     direct
_audit_creation_date             2014-05-26
_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                   5.2425(10)
_cell_length_b                   5.2425(10)
_cell_length_c                   9.4865(17)
_cell_measurement_reflns_used    974
_cell_measurement_temperature    45(2)
_cell_measurement_theta_max      26.443
_cell_measurement_theta_min      4.397
_cell_volume                     225.79(7)
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL-1997 (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS-1997 (Sheldrick, 2008)'
_diffrn_ambient_temperature      45(2)
_diffrn_detector                 'APEXII CCD area detector'
_diffrn_detector_type            'Bruker APEXII'
_diffrn_measured_fraction_theta_full 0.795
_diffrn_measured_fraction_theta_max 0.846
_diffrn_measurement_details
'0.5 degree frames measured for 0.3 seconds each'
_diffrn_measurement_device       'three-circle goniometer with fixed chi'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ scans'
_diffrn_radiation_monochromator  'silicon 1 1 1 and 3 1 1'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.38745
_diffrn_reflns_av_R_equivalents  0.0236
_diffrn_reflns_av_unetI/netI     0.0194
_diffrn_reflns_Laue_measured_fraction_full 0.795
_diffrn_reflns_Laue_measured_fraction_max 0.846
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       4
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            775
_diffrn_reflns_point_group_measured_fraction_full 0.795
_diffrn_reflns_point_group_measured_fraction_max 0.846
_diffrn_reflns_theta_full        13.443
_diffrn_reflns_theta_max         15.999
_diffrn_reflns_theta_min         2.711
_diffrn_source                   synchrotron
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.872
_exptl_absorpt_correction_T_max  0.8878
_exptl_absorpt_correction_T_min  0.7213
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0703 before and 0.0455 after correction.
The Ratio of minimum to maximum transmission is 0.8125.
The λ/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    3.507
_exptl_crystal_description       plate
_exptl_crystal_F_000             220
_exptl_crystal_size_max          0.047
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.003
_refine_diff_density_max         1.007
_refine_diff_density_min         -0.658
_refine_diff_density_rms         0.111
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.356
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     15
_refine_ls_number_reflns         154
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.356
_refine_ls_R_factor_all          0.0225
_refine_ls_R_factor_gt           0.0220
_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)+(0.0100P)²+0.7703P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0538
_refine_ls_wR_factor_ref         0.0539
_reflns_Friedel_coverage         0.000
_reflns_number_gt                149
_reflns_number_total             154
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            allP.cif
_cod_data_source_block           int_45k
_cod_original_cell_volume        225.79(10)
_cod_database_code               7032247
#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.
;
_olex2_refinement_description
;
1. Others
 Fixed U13: O1(0) N2(0) As1(0) N3(0) K1(0)
 Fixed U23: O1(0) N2(0) As1(0) N3(0) K1(0)
 Fixed X: O1(0.5) N2(0) As1(0.3333) N3(0) K1(0)
 Fixed Y: O1(1) N2(0) As1(0.6667) N3(0) K1(0)
 Fixed Z: N2(0.5) K1(0)
;
#END Tags that were not found in dictionaries
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'-x, -y, z'
'y, -x+y, z'
'x-y, x, z'
'y, x, -z'
'x-y, -y, -z'
'-x, -x+y, -z'
'-y, -x, -z'
'-x+y, y, -z'
'x, x-y, -z'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'x, y, -z'
'-y, x-y, -z'
'-x+y, -x, -z'
'-y, -x, z'
'-x+y, y, z'
'x, x-y, 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
O1 O 0.5000 1.0000 0.1703(4) 0.0126(7) Uani 1 4 d S T P
N2 N 0.0000 0.0000 0.5000 0.024(3) Uani 1 24 d S T P
As1 As 0.3333 0.6667 0.27167(8) 0.0104(2) Uani 1 6 d S T P
N3 N 0.0000 0.0000 0.3776(16) 0.038(3) Uani 1 12 d S T P
K1 K 0.0000 0.0000 0.0000 0.0165(6) Uani 1 24 d S T P
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
N N 0.0000 0.0010 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0010 0.0020 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
K K 0.0710 0.0740 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
As As 0.2730 0.6850 '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
As1 O1 As1 115.1(2) 4_675 .
As1 O1 K1 106.34(2) . 1_565
As1 O1 K1 106.34(2) 4_675 1_665
As1 O1 K1 106.34(2) 4_675 1_565
As1 O1 K1 106.34(2) . 1_665
K1 O1 K1 116.71(12) 1_565 1_665
N3 N2 N3 180.0 13_556 .
O1 As1 O1 93.92(14) 2_665 .
O1 As1 O1 93.92(14) 2_665 3_565
O1 As1 O1 93.92(14) . 3_565
O1 As1 K1 107.15(11) 3_565 1_565
O1 As1 K1 48.01(5) . 1_665
O1 As1 K1 48.01(5) 3_565 1_665
O1 As1 K1 107.15(11) 2_665 1_665
O1 As1 K1 48.01(5) . 1_565
O1 As1 K1 107.15(11) . .
O1 As1 K1 48.01(5) 3_565 .
O1 As1 K1 48.01(5) 2_665 1_565
O1 As1 K1 48.01(5) 2_665 .
K1 As1 K1 82.505(16) 1_565 1_665
K1 As1 K1 82.505(16) 1_565 .
K1 As1 K1 82.505(16) . 1_665
O1 K1 O1 116.71(12) 3_565 3_455
O1 K1 O1 95.00(8) 3_565 1_445
O1 K1 O1 63.29(12) 1_545 13_665
O1 K1 O1 95.00(8) 14_455 13_665
O1 K1 O1 85.00(8) 14_455 1_445
O1 K1 O1 85.00(8) 3_565 13_665
O1 K1 O1 129.61(4) 3_455 13_665
O1 K1 O1 95.00(8) 1_545 3_455
O1 K1 O1 50.39(4) 2_665 1_445
O1 K1 O1 50.39(4) 3_455 1_445
O1 K1 O1 129.61(4) 13_565 2_655
O1 K1 O1 95.00(8) 2_665 3_455
O1 K1 O1 129.61(4) 15_655 2_655
O1 K1 O1 129.61(4) 2_665 13_665
O1 K1 O1 95.00(8) 15_545 14_455
O1 K1 O1 85.00(8) 15_545 2_655
O1 K1 O1 116.71(12) 14_445 14_455
O1 K1 O1 116.71(12) 1_545 1_445
O1 K1 O1 50.39(4) 13_565 14_455
O1 K1 O1 63.29(12) 14_445 2_655
O1 K1 O1 50.39(4) 15_655 14_455
O1 K1 O1 180.0 2_655 14_455
O1 K1 O1 85.00(8) 14_445 3_455
O1 K1 O1 180.0 15_545 3_565
O1 K1 O1 85.00(8) 15_545 1_445
O1 K1 O1 63.29(12) 3_565 15_655
O1 K1 O1 50.39(4) 14_445 13_665
O1 K1 O1 180.0 14_445 2_665
O1 K1 O1 85.00(8) 13_565 3_455
O1 K1 O1 50.39(4) 15_545 14_445
O1 K1 O1 95.00(8) 2_655 1_445
O1 K1 O1 85.00(8) 2_665 15_655
O1 K1 O1 180.0 15_655 3_455
O1 K1 O1 129.61(4) 3_565 14_445
O1 K1 O1 50.39(4) 15_655 13_665
O1 K1 O1 85.00(8) 13_565 2_665
O1 K1 O1 95.00(8) 3_565 2_655
O1 K1 O1 129.61(4) 15_545 1_545
O1 K1 O1 63.29(12) 13_565 1_445
O1 K1 O1 85.00(8) 1_545 15_655
O1 K1 O1 50.39(4) 1_545 2_655
O1 K1 O1 50.39(4) 3_565 1_545
O1 K1 O1 95.00(8) 15_545 13_665
O1 K1 O1 50.39(4) 3_565 2_665
O1 K1 O1 116.71(12) 2_665 2_655
O1 K1 O1 85.00(8) 14_445 1_545
O1 K1 O1 116.71(12) 13_565 13_665
O1 K1 O1 95.00(8) 1_545 2_665
O1 K1 O1 50.39(4) 3_455 2_655
O1 K1 O1 50.39(4) 15_545 13_565
O1 K1 O1 85.00(8) 2_655 13_665
O1 K1 O1 116.71(12) 15_545 15_655
O1 K1 O1 85.00(8) 3_565 14_455
O1 K1 O1 129.61(4) 3_565 13_565
O1 K1 O1 129.61(4) 14_445 1_445
O1 K1 O1 95.00(8) 14_445 15_655
O1 K1 O1 129.61(4) 1_545 14_455
O1 K1 O1 95.00(8) 14_445 13_565
O1 K1 O1 129.61(4) 15_655 1_445
O1 K1 O1 95.00(8) 13_565 15_655
O1 K1 O1 63.29(12) 2_665 14_455
O1 K1 O1 180.00(12) 1_545 13_565
O1 K1 O1 180.0 13_665 1_445
O1 K1 O1 63.29(12) 15_545 3_455
O1 K1 O1 129.61(4) 3_455 14_455
O1 K1 O1 129.61(4) 15_545 2_665
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
O1 As1 1.793(2) 4_675
O1 As1 1.793(2) .
O1 K1 3.079(2) 1_565
O1 K1 3.079(2) 1_665
N2 N3 1.161(16) 13_556
N2 N3 1.161(16) .
As1 O1 1.793(2) 2_665
As1 O1 1.793(2) 3_565
As1 K1 3.9753(7) 1_565
As1 K1 3.9753(7) .
As1 K1 3.9753(7) 1_665
K1 O1 3.079(2) 15_545
K1 O1 3.079(2) 13_665
K1 O1 3.079(2) 3_565
K1 O1 3.079(2) 13_565
K1 O1 3.079(2) 15_655
K1 O1 3.079(2) 1_545
K1 O1 3.079(2) 2_655
K1 O1 3.079(2) 14_455
K1 O1 3.079(2) 2_665
K1 O1 3.079(2) 14_445
K1 O1 3.079(2) 3_455
K1 O1 3.079(2) 1_445
