#------------------------------------------------------------------------------
#$Date: 2016-03-25 23:10:29 +0200 (Fri, 25 Mar 2016) $
#$Revision: 180028 $
#$URL: svn://www.crystallography.net/cod/cif/7/03/22/7032244.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_7032244
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                   5.2469(12)
_cell_length_b                   5.2469(12)
_cell_length_c                   9.560(2)
_cell_measurement_reflns_used    758
_cell_measurement_temperature    15(2)
_cell_measurement_theta_max      26.42
_cell_measurement_theta_min      2.44
_cell_volume                     227.93(9)
_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 (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS-1997 (Sheldrick, 2008)'
_diffrn_ambient_temperature      15(2)
_diffrn_detector                 'APEXII CCD area detector'
_diffrn_detector_type            'Bruker APEXII'
_diffrn_measured_fraction_theta_full 0.814
_diffrn_measured_fraction_theta_max 0.859
_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  0.0244
_diffrn_reflns_av_unetI/netI     0.0188
_diffrn_reflns_Laue_measured_fraction_full 0.814
_diffrn_reflns_Laue_measured_fraction_max 0.859
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       4
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            799
_diffrn_reflns_point_group_measured_fraction_full 0.814
_diffrn_reflns_point_group_measured_fraction_max 0.859
_diffrn_reflns_theta_full        13.443
_diffrn_reflns_theta_max         15.970
_diffrn_reflns_theta_min         2.706
_diffrn_source                   synchrotron
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.851
_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    3.474
_exptl_crystal_description       plate
_exptl_crystal_F_000             220
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.37
_exptl_crystal_size_min          0.003
_refine_diff_density_max         2.266
_refine_diff_density_min         -1.190
_refine_diff_density_rms         0.186
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.183
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     15
_refine_ls_number_reflns         158
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.183
_refine_ls_R_factor_all          0.0365
_refine_ls_R_factor_gt           0.0348
_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)+(0.0387P)²+2.0883P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0904
_refine_ls_wR_factor_ref         0.0910
_reflns_Friedel_coverage         0.000
_reflns_number_gt                148
_reflns_number_total             158
_reflns_threshold_expression     'I > 2σ(I)'
_cod_duplicate_entry             7032250
_cod_data_source_file            allP.cif
_cod_data_source_block           int_15k
_cod_original_cell_volume        227.93(12)
_cod_database_code               7032244
#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: As1(0) O1(0) K1(0) N1(0) N2(0)
 Fixed U23: As1(0) O1(0) K1(0) N1(0) N2(0)
 Fixed X: As1(0.3333) O1(0) K1(0) N1(0) N2(0)
 Fixed Y: As1(0.6667) O1(0.5) K1(0) N1(0) N2(0)
 Fixed Z: K1(0) N1(0.5)
;
#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
As1 As 0.3333 0.6667 0.27174(13) 0.0156(4) Uani 1 6 d S T P
O1 O 0.0000 0.5000 0.1708(7) 0.0185(11) Uani 1 4 d S T P
K1 K 0.0000 0.0000 0.0000 0.0216(10) Uani 1 24 d S T P
N1 N 0.0000 0.0000 0.5000 0.034(6) Uani 1 24 d S T P
N2 N 0.0000 0.0000 0.381(3) 0.059(6) Uani 1 12 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
O1 As1 O1 93.8(2) . 3_565
O1 As1 O1 93.8(2) 3_565 2_665
O1 As1 O1 93.8(2) . 2_665
As1 O1 As1 115.0(4) . 4_565
As1 O1 K1 106.49(4) . .
As1 O1 K1 106.49(4) 4_565 .
As1 O1 K1 106.49(4) . 1_565
As1 O1 K1 106.49(4) 4_565 1_565
K1 O1 K1 116.2(2) . 1_565
O1 K1 O1 85.35(14) 2_665 15_655
O1 K1 O1 50.23(6) 14 13_565
O1 K1 O1 94.65(14) 3_455 1_545
O1 K1 O1 129.77(6) 2 15_655
O1 K1 O1 116.2(2) . 1_545
O1 K1 O1 63.8(2) 15 3_455
O1 K1 O1 116.2(2) 13 13_565
O1 K1 O1 50.23(6) 2 3_455
O1 K1 O1 94.65(14) 2_665 1_545
O1 K1 O1 180.0 14_445 2_665
O1 K1 O1 180.0 2 14
O1 K1 O1 50.23(6) 14_445 15
O1 K1 O1 85.35(14) 3 14
O1 K1 O1 129.77(6) 2_665 15
O1 K1 O1 116.2(2) 14_445 14
O1 K1 O1 50.23(6) 14_445 13
O1 K1 O1 50.23(6) 2_665 .
O1 K1 O1 129.77(6) 2_665 13
O1 K1 O1 94.65(14) 3 2
O1 K1 O1 94.65(14) 15 13
O1 K1 O1 180.0 13 .
O1 K1 O1 129.77(6) 14_445 3
O1 K1 O1 94.65(14) 15 14
O1 K1 O1 50.23(6) 2_665 3
O1 K1 O1 63.8(2) 14_445 2
O1 K1 O1 180.0 15 3
O1 K1 O1 85.35(14) 15 2
O1 K1 O1 129.77(6) . 15_655
O1 K1 O1 129.77(6) 14_445 .
O1 K1 O1 50.23(6) 14 15_655
O1 K1 O1 85.35(14) 3_455 13_565
O1 K1 O1 94.65(14) 2_665 3_455
O1 K1 O1 85.35(14) 15 .
O1 K1 O1 129.77(6) 13 3_455
O1 K1 O1 63.8(2) . 13_565
O1 K1 O1 50.23(6) . 3_455
O1 K1 O1 94.65(14) 3 .
O1 K1 O1 129.77(6) 14 3_455
O1 K1 O1 129.77(6) 14 1_545
O1 K1 O1 85.35(14) 14_445 1_545
O1 K1 O1 116.2(2) 2_665 2
O1 K1 O1 129.77(6) 15 1_545
O1 K1 O1 63.8(2) 3 15_655
O1 K1 O1 50.23(6) 3 1_545
O1 K1 O1 85.35(14) 13 2
O1 K1 O1 50.23(6) 2 1_545
O1 K1 O1 63.8(2) 13 1_545
O1 K1 O1 85.35(14) 15_655 1_545
O1 K1 O1 94.65(14) . 2
O1 K1 O1 94.65(14) 14_445 13_565
O1 K1 O1 85.35(14) 14_445 3_455
O1 K1 O1 50.23(6) 15 13_565
O1 K1 O1 63.8(2) 2_665 14
O1 K1 O1 129.77(6) 3 13_565
O1 K1 O1 85.35(14) 2_665 13_565
O1 K1 O1 129.77(6) 2 13_565
O1 K1 O1 94.65(14) 13 14
O1 K1 O1 94.65(14) 15_655 13_565
O1 K1 O1 116.2(2) 3 3_455
O1 K1 O1 180.0 1_545 13_565
O1 K1 O1 85.35(14) . 14
O1 K1 O1 94.65(14) 14_445 15_655
O1 K1 O1 180.0 15_655 3_455
O1 K1 O1 85.35(14) 13 3
O1 K1 O1 50.23(6) 13 15_655
O1 K1 O1 116.2(2) 15 15_655
N2 N1 N2 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 1.796(4) .
As1 O1 1.796(4) 3_565
As1 O1 1.796(4) 2_665
O1 As1 1.796(4) 4_565
O1 K1 3.090(3) .
O1 K1 3.090(3) 1_565
K1 O1 3.090(3) 15_655
K1 O1 3.090(3) 3
K1 O1 3.090(3) 3_455
K1 O1 3.090(3) 2
K1 O1 3.090(3) 13_565
K1 O1 3.090(3) 14
K1 O1 3.090(3) 13
K1 O1 3.090(3) 14_445
K1 O1 3.090(3) 1_545
K1 O1 3.090(3) 15
K1 O1 3.090(3) 2_665
N1 N2 1.14(3) 13_556
N1 N2 1.14(3) .
