#------------------------------------------------------------------------------
#$Date: 2021-04-06 12:42:09 +0300 (Tue, 06 Apr 2021) $
#$Revision: 263908 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/56/15/1561509.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_1561509
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 Ge3 As3'
_chemical_formula_sum            'As3 Ge3 K'
_chemical_formula_weight         481.63
_chemical_name_common            'potassium germanium arsenide (1/3/3)'
_chemical_name_systematic        'potassium germanium 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                   9.9931(11)
_cell_length_b                   3.7664(4)
_cell_length_c                   18.607(2)
_cell_measurement_reflns_used    2151
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      27.03
_cell_measurement_theta_min      2.19
_cell_volume                     700.33(13)
_computing_cell_refinement       'Bruker SAINT 8.34A (Bruker, 2013)'
_computing_data_collection       'Bruker APEX 2 (Bruker, 2008)'
_computing_data_reduction        'Bruker SAINT 8.34A'
_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      193(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_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  0.0780
_diffrn_reflns_av_unetI/netI     0.0428
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       5
_diffrn_reflns_limit_k_min       -5
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            9750
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         33.047
_diffrn_reflns_theta_min         2.189
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    27.330
_exptl_absorpt_correction_T_max  0.5963
_exptl_absorpt_correction_T_min  0.1217
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'Bruker SHELXTL (Sheldrick, 2013)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    4.568
_exptl_crystal_description       needle
_exptl_crystal_F_000             856
_exptl_crystal_size_max          0.288
_exptl_crystal_size_mid          0.027
_exptl_crystal_size_min          0.024
_refine_diff_density_max         1.955
_refine_diff_density_min         -2.330
_refine_diff_density_rms         0.342
_refine_ls_extinction_coef       0.0012(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   1.084
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     44
_refine_ls_number_reflns         1497
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.084
_refine_ls_R_factor_all          0.0626
_refine_ls_R_factor_gt           0.0386
_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)+(0.0360P)²+6.8843P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0879
_refine_ls_wR_factor_ref         0.0961
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1092
_reflns_number_total             1497
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            mmc8.cif
_cod_data_source_block           KGe3As3unsplit
_cod_original_cell_volume        700.34(13)
_cod_database_code               1561509
_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   0.047
_shelx_estimated_absorpt_t_max   0.560
_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 0.2202(3) 0.2500 0.45727(18) 0.0713(12) Uani 1 2 d S T P . .
Ge1 Ge 0.30819(9) 0.2500 0.15689(5) 0.01194(19) Uani 1 2 d S T P . .
Ge2 Ge 0.41421(9) 0.2500 0.75660(5) 0.01276(19) Uani 1 2 d S T P . .
Ge3 Ge 0.52037(10) 0.2500 0.63181(5) 0.0165(2) Uani 1 2 d S T P . .
As1 As 0.04405(8) 0.2500 0.63048(4) 0.01128(18) Uani 1 2 d S T P . .
As2 As 0.11350(9) 0.2500 0.07913(5) 0.01413(19) Uani 1 2 d S T P . .
As3 As 0.23867(9) 0.2500 0.28121(5) 0.01278(19) 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'
Ge Ge 0.1547 1.8001 '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'
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
As3 K As2 129.91(8) . 2_565
As3 K As2 129.91(8) . 2
As2 K As2 67.64(6) 2_565 2
As3 K Ge3 60.06(6) . 5_666
As2 K Ge3 70.40(5) 2_565 5_666
As2 K Ge3 104.22(9) 2 5_666
As3 K Ge3 60.06(6) . 5_656
As2 K Ge3 104.22(9) 2_565 5_656
As2 K Ge3 70.40(5) 2 5_656
Ge3 K Ge3 62.94(6) 5_666 5_656
As3 K As1 65.91(6) . 5_556
As2 K As1 161.27(11) 2_565 5_556
As2 K As1 111.70(3) 2 5_556
Ge3 K As1 125.93(10) 5_666 5_556
Ge3 K As1 92.60(5) 5_656 5_556
As3 K As1 65.91(6) . 5_566
As2 K As1 111.70(3) 2_565 5_566
As2 K As1 161.27(11) 2 5_566
Ge3 K As1 92.60(5) 5_666 5_566
Ge3 K As1 125.93(10) 5_656 5_566
As1 K As1 62.47(6) 5_556 5_566
As3 K As1 154.57(11) . .
As2 K As1 69.35(6) 2_565 .
As2 K As1 69.35(6) 2 .
Ge3 K As1 138.39(7) 5_666 .
Ge3 K As1 138.39(7) 5_656 .
As1 K As1 92.63(8) 5_556 .
As1 K As1 92.63(8) 5_566 .
As3 K K 90.0 . 1_565
As2 K K 56.18(3) 2_565 1_565
As2 K K 123.82(3) 2 1_565
Ge3 K K 58.53(3) 5_666 1_565
Ge3 K K 121.47(3) 5_656 1_565
As1 K K 121.24(3) 5_556 1_565
As1 K K 58.76(3) 5_566 1_565
As1 K K 90.0 . 1_565
As3 K K 90.0 . 1_545
As2 K K 123.82(3) 2_565 1_545
As2 K K 56.18(3) 2 1_545
Ge3 K K 121.47(3) 5_666 1_545
Ge3 K K 58.53(3) 5_656 1_545
As1 K K 58.76(3) 5_556 1_545
As1 K K 121.24(3) 5_566 1_545
As1 K K 90.0 . 1_545
K K K 180.0 1_565 1_545
As3 Ge1 As2 109.92(5) . .
As3 Ge1 As1 111.50(3) . 2_564
As2 Ge1 As1 111.40(3) . 2_564
As3 Ge1 As1 111.50(3) . 2_554
As2 Ge1 As1 111.40(3) . 2_554
As1 Ge1 As1 100.86(5) 2_564 2_554
As3 Ge2 As3 99.48(4) 2 2_565
As3 Ge2 As1 99.64(4) 2 6_657
As3 Ge2 As1 99.64(4) 2_565 6_657
As3 Ge2 Ge3 115.22(3) 2 .
As3 Ge2 Ge3 115.22(3) 2_565 .
As1 Ge2 Ge3 123.75(5) 6_657 .
As2 Ge3 As2 97.26(5) 2 2_565
As2 Ge3 Ge2 97.69(4) 2 .
As2 Ge3 Ge2 97.69(4) 2_565 .
As2 Ge3 K 126.54(6) 2 5_666
As2 Ge3 K 79.15(5) 2_565 5_666
Ge2 Ge3 K 135.77(5) . 5_666
As2 Ge3 K 79.15(5) 2 5_656
As2 Ge3 K 126.54(6) 2_565 5_656
Ge2 Ge3 K 135.77(5) . 5_656
K Ge3 K 62.94(6) 5_666 5_656
Ge1 As1 Ge1 100.86(5) 2_565 2
Ge1 As1 Ge2 98.42(3) 2_565 6_557
Ge1 As1 Ge2 98.42(3) 2 6_557
Ge1 As1 K 158.40(4) 2_565 5_556
Ge1 As1 K 97.49(4) 2 5_556
Ge2 As1 K 90.03(6) 6_557 5_556
Ge1 As1 K 97.49(4) 2_565 5_566
Ge1 As1 K 158.40(4) 2 5_566
Ge2 As1 K 90.03(6) 6_557 5_566
K As1 K 62.47(6) 5_556 5_566
Ge1 As1 K 83.50(4) 2_565 .
Ge1 As1 K 83.50(4) 2 .
Ge2 As1 K 176.95(7) 6_557 .
K As1 K 87.37(8) 5_556 .
K As1 K 87.37(8) 5_566 .
Ge1 As2 Ge3 101.23(4) . 2_554
Ge1 As2 Ge3 101.23(4) . 2_564
Ge3 As2 Ge3 97.26(5) 2_554 2_564
Ge1 As2 K 90.34(7) . 2_554
Ge3 As2 K 96.07(4) 2_554 2_554
Ge3 As2 K 160.26(5) 2_564 2_554
Ge1 As2 K 90.34(7) . 2_564
Ge3 As2 K 160.26(5) 2_554 2_564
Ge3 As2 K 96.07(4) 2_564 2_564
K As2 K 67.64(6) 2_554 2_564
Ge1 As3 Ge2 90.02(4) . 2_554
Ge1 As3 Ge2 90.02(4) . 2_564
Ge2 As3 Ge2 99.48(4) 2_554 2_564
Ge1 As3 K 166.50(7) . .
Ge2 As3 K 98.66(5) 2_554 .
Ge2 As3 K 98.66(5) 2_564 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
K As3 3.281(3) .
K As2 3.384(3) 2_565
K As2 3.384(3) 2
K Ge3 3.607(3) 5_666
K Ge3 3.607(3) 5_656
K As1 3.632(3) 5_556
K As1 3.632(3) 5_566
K As1 3.673(4) .
K K 3.7664(4) 1_565
K K 3.7664(4) 1_545
Ge1 As3 2.4153(12) .
Ge1 As2 2.4246(13) .
Ge1 As1 2.4430(8) 2_564
Ge1 As1 2.4430(8) 2_554
Ge2 As3 2.4678(8) 2
Ge2 As3 2.4678(8) 2_565
Ge2 As1 2.4694(13) 6_657
Ge2 Ge3 2.5529(14) .
Ge3 As2 2.5093(9) 2
Ge3 As2 2.5093(9) 2_565
Ge3 K 3.607(3) 5_666
Ge3 K 3.607(3) 5_656
As1 Ge1 2.4430(8) 2_565
As1 Ge1 2.4430(8) 2
As1 Ge2 2.4694(13) 6_557
As1 K 3.632(3) 5_556
As1 K 3.632(3) 5_566
As2 Ge3 2.5093(9) 2_554
As2 Ge3 2.5093(9) 2_564
As2 K 3.384(3) 2_554
As2 K 3.384(3) 2_564
As3 Ge2 2.4678(8) 2_554
As3 Ge2 2.4678(8) 2_564
