#------------------------------------------------------------------------------
#$Date: 2021-04-06 12:47:06 +0300 (Tue, 06 Apr 2021) $
#$Revision: 263910 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/56/15/1561511.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_1561511
loop_
_publ_author_name
'Khatun, Mansura'
'Stoyko, Stanislav S.'
'Mar, Arthur'
_publ_section_title
;
 Ternary arsenides ATt3As3 (A=K, Rb; Tt=Ge, Sn) with layered structures
;
_journal_name_full               'Journal of Solid State Chemistry'
_journal_page_first              229
_journal_page_last               235
_journal_paper_doi               10.1016/j.jssc.2016.03.035
_journal_volume                  238
_journal_year                    2016
_chemical_formula_structural     'K Sn3 As3'
_chemical_formula_sum            'As3 K Sn3'
_chemical_formula_weight         619.93
_chemical_name_common            'potassium tin arsenide (1/3/3)'
_chemical_name_systematic        'potassium tin arsenide (1/3/3)'
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_Hall           '-P 2ac 2n'
_space_group_name_H-M_alt        'P n m a'
_atom_sites_solution_hydrogens   .
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.1990(12)
_cell_length_b                   4.0840(5)
_cell_length_c                   19.240(2)
_cell_measurement_reflns_used    2802
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      31.47
_cell_measurement_theta_min      2.91
_cell_volume                     801.40(16)
_computing_cell_refinement       'Bruker SAINT 7.68A (Bruker, 2009)'
_computing_data_collection       'Bruker APEX 2 (Bruker, 2008)'
_computing_data_reduction        'Bruker SAINT 7.68A'
_computing_molecular_graphics    'ATOMS 5.1 (Dowty, 1999)'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device_type  'Bruker PLATFORM/SMART APEX II CCD'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0792
_diffrn_reflns_av_unetI/netI     0.0460
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            10718
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         33.249
_diffrn_reflns_theta_min         2.117
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    21.981
_exptl_absorpt_correction_T_max  0.6969
_exptl_absorpt_correction_T_min  0.1333
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'Bruker SHELXTL (Sheldrick, 2013)'
_exptl_crystal_colour            grey
_exptl_crystal_density_diffrn    5.138
_exptl_crystal_description       needle
_exptl_crystal_F_000             1072
_exptl_crystal_size_max          0.155
_exptl_crystal_size_mid          0.040
_exptl_crystal_size_min          0.021
_refine_diff_density_max         2.085
_refine_diff_density_min         -2.176
_refine_diff_density_rms         0.397
_refine_ls_extinction_coef       0.00083(12)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     44
_refine_ls_number_reflns         1697
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.020
_refine_ls_R_factor_all          0.0553
_refine_ls_R_factor_gt           0.0341
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0353P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0680
_refine_ls_wR_factor_ref         0.0745
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1313
_reflns_number_total             1697
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            mmc12.cif
_cod_data_source_block           KSn3As3
_cod_original_cell_volume        801.41(16)
_cod_database_code               1561511
_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.
;
_shelx_estimated_absorpt_t_min   0.132
_shelx_estimated_absorpt_t_max   0.655
_shelxl_version_number           2013-4
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
K K 0.21476(19) 0.2500 0.45854(11) 0.0196(4) Uani 1 2 d S T P . .
Sn1 Sn 0.32879(5) 0.2500 0.14869(3) 0.01055(12) Uani 1 2 d S T P . .
Sn2 Sn 0.39021(5) 0.2500 0.75813(3) 0.01116(12) Uani 1 2 d S T P . .
Sn3 Sn 0.51891(5) 0.2500 0.62159(3) 0.01258(12) Uani 1 2 d S T P . .
As1 As 0.01512(8) 0.2500 0.62022(4) 0.01045(16) Uani 1 2 d S T P . .
As2 As 0.12616(8) 0.2500 0.06768(4) 0.01172(17) Uani 1 2 d S T P . .
As3 As 0.27428(8) 0.2500 0.28142(4) 0.01133(16) Uani 1 2 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
K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
As As 0.0499 2.0058 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Sn Sn -0.6537 1.4246 '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
As2 K As2 75.16(4) 2_565 2
As2 K As1 164.42(7) 2_565 5_556
As2 K As1 104.073(19) 2 5_556
As2 K As1 104.073(19) 2_565 5_566
As2 K As1 164.42(7) 2 5_566
As1 K As1 72.37(4) 5_556 5_566
As2 K As3 122.17(5) 2_565 .
As2 K As3 122.17(5) 2 .
As1 K As3 71.79(4) 5_556 .
As1 K As3 71.79(4) 5_566 .
As2 K As1 74.97(4) 2_565 .
As2 K As1 74.97(4) 2 .
As1 K As1 89.73(4) 5_556 .
As1 K As1 89.73(4) 5_566 .
As3 K As1 156.89(6) . .
As2 K Sn3 64.70(3) 2_565 5_666
As2 K Sn3 103.89(5) 2 5_666
As1 K Sn3 129.46(6) 5_556 5_666
As1 K Sn3 89.39(3) 5_566 5_666
As3 K Sn3 57.70(3) . 5_666
As1 K Sn3 138.10(4) . 5_666
As2 K Sn3 103.89(5) 2_565 5_656
As2 K Sn3 64.70(3) 2 5_656
As1 K Sn3 89.39(3) 5_556 5_656
As1 K Sn3 129.46(6) 5_566 5_656
As3 K Sn3 57.70(3) . 5_656
As1 K Sn3 138.10(4) . 5_656
Sn3 K Sn3 66.35(4) 5_666 5_656
As2 K K 127.58(2) 2_565 1_545
As2 K K 52.42(2) 2 1_545
As1 K K 53.82(2) 5_556 1_545
As1 K K 126.18(2) 5_566 1_545
As3 K K 90.0 . 1_545
As1 K K 90.0 . 1_545
Sn3 K K 123.177(18) 5_666 1_545
Sn3 K K 56.824(18) 5_656 1_545
As2 K K 52.42(2) 2_565 1_565
As2 K K 127.58(2) 2 1_565
As1 K K 126.18(2) 5_556 1_565
As1 K K 53.82(2) 5_566 1_565
As3 K K 90.0 . 1_565
As1 K K 90.0 . 1_565
Sn3 K K 56.824(18) 5_666 1_565
Sn3 K K 123.177(18) 5_656 1_565
K K K 180.0 1_545 1_565
As2 Sn1 As3 114.74(3) . .
As2 Sn1 As1 110.83(3) . 2_564
As3 Sn1 As1 109.28(2) . 2_564
As2 Sn1 As1 110.83(3) . 2_554
As3 Sn1 As1 109.28(2) . 2_554
As1 Sn1 As1 100.99(3) 2_564 2_554
As1 Sn2 As3 98.76(3) 6_657 2
As1 Sn2 As3 98.76(3) 6_657 2_565
As3 Sn2 As3 99.24(3) 2 2_565
As1 Sn2 Sn3 124.89(3) 6_657 .
As3 Sn2 Sn3 115.42(2) 2 .
As3 Sn2 Sn3 115.42(2) 2_565 .
As2 Sn3 As2 96.99(3) 2 2_565
As2 Sn3 Sn2 95.61(2) 2 .
As2 Sn3 Sn2 95.61(2) 2_565 .
As2 Sn3 K 130.36(4) 2 5_666
As2 Sn3 K 80.10(3) 2_565 5_666
Sn2 Sn3 K 134.02(3) . 5_666
As2 Sn3 K 80.10(3) 2 5_656
As2 Sn3 K 130.36(4) 2_565 5_656
Sn2 Sn3 K 134.02(3) . 5_656
K Sn3 K 66.35(4) 5_666 5_656
Sn1 As1 Sn1 100.99(3) 2_565 2
Sn1 As1 Sn2 96.07(3) 2_565 6_557
Sn1 As1 Sn2 96.07(3) 2 6_557
Sn1 As1 K 162.55(4) 2_565 5_556
Sn1 As1 K 92.46(2) 2 5_556
Sn2 As1 K 93.49(4) 6_557 5_556
Sn1 As1 K 92.46(2) 2_565 5_566
Sn1 As1 K 162.55(4) 2 5_566
Sn2 As1 K 93.49(4) 6_557 5_566
K As1 K 72.37(4) 5_556 5_566
Sn1 As1 K 81.01(3) 2_565 .
Sn1 As1 K 81.01(3) 2 .
Sn2 As1 K 175.35(4) 6_557 .
K As1 K 90.27(4) 5_556 .
K As1 K 90.27(5) 5_566 .
Sn1 As2 Sn3 101.78(3) . 2_554
Sn1 As2 Sn3 101.78(3) . 2_564
Sn3 As2 Sn3 96.99(3) 2_554 2_564
Sn1 As2 K 89.47(4) . 2_554
Sn3 As2 K 92.57(2) 2_554 2_554
Sn3 As2 K 163.38(4) 2_564 2_554
Sn1 As2 K 89.47(4) . 2_564
Sn3 As2 K 163.38(4) 2_554 2_564
Sn3 As2 K 92.57(2) 2_564 2_564
K As2 K 75.16(4) 2_554 2_564
Sn1 As3 Sn2 88.27(3) . 2_554
Sn1 As3 Sn2 88.27(3) . 2_564
Sn2 As3 Sn2 99.24(3) 2_554 2_564
Sn1 As3 K 177.82(5) . .
Sn2 As3 K 93.14(3) 2_554 .
Sn2 As3 K 93.14(3) 2_564 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
K As2 3.3484(17) 2_565
K As2 3.3484(17) 2
K As1 3.4588(17) 5_556
K As1 3.4588(17) 5_566
K As3 3.462(2) .
K As1 3.718(2) .
K Sn3 3.7316(18) 5_666
K Sn3 3.7316(18) 5_656
K K 4.0840(5) 1_545
K K 4.0840(5) 1_565
Sn1 As2 2.5885(10) .
Sn1 As3 2.6134(10) .
Sn1 As1 2.6466(6) 2_564
Sn1 As1 2.6466(6) 2_554
Sn2 As1 2.6649(10) 6_657
Sn2 As3 2.6805(7) 2
Sn2 As3 2.6805(7) 2_565
Sn2 Sn3 2.9366(8) .
Sn3 As2 2.7267(7) 2
Sn3 As2 2.7267(7) 2_565
Sn3 K 3.7316(18) 5_666
Sn3 K 3.7316(18) 5_656
As1 Sn1 2.6466(6) 2_565
As1 Sn1 2.6466(6) 2
As1 Sn2 2.6649(10) 6_557
As1 K 3.4587(17) 5_556
As1 K 3.4587(17) 5_566
As2 Sn3 2.7267(7) 2_554
As2 Sn3 2.7267(7) 2_564
As2 K 3.3483(17) 2_554
As2 K 3.3483(17) 2_564
As3 Sn2 2.6805(7) 2_554
As3 Sn2 2.6805(7) 2_564
