# Electronic Supplementary Material (ESI) for ChemComm.
# This journal is © The Royal Society of Chemistry 2021

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_shelx
_database_code_depnum_ccdc_archive 'CCDC 2015241'
loop_
_audit_author_name
_audit_author_address
'Valentin Weippert'
;LMU Munich
Germany
;
_audit_update_record             
;
2020-07-09 deposited with the CCDC.	2020-12-21 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'As14 Ba Ge8'
_chemical_formula_sum            'As14 Ba Ge8'
_chemical_formula_weight         1766.94

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
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'
Ba Ba -0.3244 2.2819 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      cubic
_space_group_IT_number           217
_space_group_name_H-M_alt        'I -4 3 m'
_space_group_name_Hall           'I -4 2 3'

_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'-x, y, -z'
'x, -y, -z'
'z, x, y'
'z, -x, -y'
'-z, -x, y'
'-z, x, -y'
'y, z, x'
'-y, z, -x'
'y, -z, -x'
'-y, -z, x'
'y, x, z'
'-y, -x, z'
'y, -x, -z'
'-y, x, -z'
'x, z, y'
'-x, z, -y'
'-x, -z, y'
'x, -z, -y'
'z, y, x'
'z, -y, -x'
'-z, y, -x'
'-z, -y, x'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'-x+1/2, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'z+1/2, x+1/2, y+1/2'
'z+1/2, -x+1/2, -y+1/2'
'-z+1/2, -x+1/2, y+1/2'
'-z+1/2, x+1/2, -y+1/2'
'y+1/2, z+1/2, x+1/2'
'-y+1/2, z+1/2, -x+1/2'
'y+1/2, -z+1/2, -x+1/2'
'-y+1/2, -z+1/2, x+1/2'
'y+1/2, x+1/2, z+1/2'
'-y+1/2, -x+1/2, z+1/2'
'y+1/2, -x+1/2, -z+1/2'
'-y+1/2, x+1/2, -z+1/2'
'x+1/2, z+1/2, y+1/2'
'-x+1/2, z+1/2, -y+1/2'
'-x+1/2, -z+1/2, y+1/2'
'x+1/2, -z+1/2, -y+1/2'
'z+1/2, y+1/2, x+1/2'
'z+1/2, -y+1/2, -x+1/2'
'-z+1/2, y+1/2, -x+1/2'
'-z+1/2, -y+1/2, x+1/2'

_cell_length_a                   10.3145(2)
_cell_length_b                   10.3145(2)
_cell_length_c                   10.3145(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1097.35(6)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    5587
_cell_measurement_theta_min      5.586
_cell_measurement_theta_max      71.848

_exptl_crystal_description       block
_exptl_crystal_colour            black
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    5.348
_exptl_crystal_F_000             1548
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.134
_exptl_crystal_size_mid          0.087
_exptl_crystal_size_min          0.054
_exptl_absorpt_coefficient_mu    33.493
_shelx_estimated_absorpt_T_min   0.094
_shelx_estimated_absorpt_T_max   0.265
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.1886
_exptl_absorpt_correction_T_max  0.3437
_exptl_absorpt_process_details   
;
Additional spherical absorption correction
 applied with mu*r =  0.8000  (Bruker, 2016)
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'I\m S'
_diffrn_radiation_monochromator  'Goebel Mirror'
_diffrn_measurement_device_type  'Bruker D8 Quest'
_diffrn_measurement_method       'combined φ ω scan'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            8373
_diffrn_reflns_av_unetI/netI     0.0113
_diffrn_reflns_av_R_equivalents  0.0408
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         2.793
_diffrn_reflns_theta_max         29.952
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measured_fraction_theta_full 0.984
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_Laue_measured_fraction_full 0.984
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_point_group_measured_fraction_full 0.986
_reflns_number_total             329
_reflns_number_gt                325
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.741
_reflns_Friedel_fraction_max     0.993
_reflns_Friedel_fraction_full    0.989

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;

_computing_data_collection       'APEX3 (Bruker, 2016)'
_computing_cell_refinement       'APEX3 (Bruker, 2016)'
_computing_data_reduction        'APEX3 (Bruker, 2016)'
_computing_structure_solution    'SUPERFLIP (Palatinus & Chapuis, 2007)'
_computing_structure_refinement  'SHELXL (Sheldrick, 2015)'
_computing_molecular_graphics    'DIAMOND 3 (Brandenburg, 2014)'
_computing_publication_material  
;
PLATON V. 91007 (Spek, 2009)
STRUCTURETIDY (Gelato, Parthé, 1987)
;
_refine_special_details          
;
 Refined as a 2-component inversion twin.
 Ge2:As2 ratio fixed to 50:50 based on elemental analysis.
 Ba1 refined as a split position, changing the Wyckoff position
 from 2a to 8c. Consequently the occupancy of the Ba1 split 
 position is fixed to 0.25.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0161P)²+0.0356P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   .
_refine_ls_hydrogen_treatment    undef
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.22(12)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         329
_refine_ls_number_parameters     16
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0132
_refine_ls_R_factor_gt           0.0123
_refine_ls_wR_factor_ref         0.0303
_refine_ls_wR_factor_gt          0.0301
_refine_ls_goodness_of_fit_ref   1.330
_refine_ls_restrained_S_all      1.330
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000


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
Ba1 Ba 0.47998(18) 0.47998(18) 0.47998(18) 0.0503(13) Uani 0.25 6 d S T P . .
Ge1 Ge 0.250000 0.500000 0.000000 0.01077(15) Uani 1 4 d S T P . .
Ge2 Ge 0.21902(5) 0.21902(5) 0.21902(5) 0.01339(18) Uani 0.5 6 d S T P . .
As1 As 0.38499(3) 0.38499(3) 0.15708(5) 0.01151(13) Uani 1 2 d S T P . .
As2 As 0.21902(5) 0.21902(5) 0.21902(5) 0.01339(18) Uani 0.5 6 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
Ba1 0.0503(13) 0.0503(13) 0.0503(13) -0.0092(7) -0.0092(7) -0.0092(7)
Ge1 0.0129(3) 0.00973(18) 0.00973(18) 0.000 0.000 0.000
Ge2 0.01339(18) 0.01339(18) 0.01339(18) 0.00172(19) 0.00172(19) 0.00172(19)
As1 0.01216(16) 0.01216(16) 0.0102(2) 0.00053(12) 0.00053(12) 0.00034(16)
As2 0.01339(18) 0.01339(18) 0.01339(18) 0.00172(19) 0.00172(19) 0.00172(19)

_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ba1 Ba1 0.584(5) 4_566 ?
Ba1 Ba1 0.584(5) 3_656 ?
Ba1 Ba1 0.584(5) 2_665 ?
Ba1 As1 3.607(3) . ?
Ba1 As1 3.607(3) 9 ?
Ba1 As1 3.607(3) 5 ?
Ba1 Ge2 3.8087(11) 26 ?
Ba1 Ge2 3.8087(11) 28 ?
Ba1 Ge2 3.8087(11) 27 ?
Ba1 As1 3.8695(6) 6_566 ?
Ba1 As1 3.8695(6) 10_656 ?
Ba1 As1 3.8695(6) 2_665 ?
Ge1 As1 2.4435(3) 36_554 ?
Ge1 As1 2.4435(3) 34 ?
Ge1 As1 2.4435(3) 4_565 ?
Ge1 As1 2.4435(3) . ?
As1 As2 2.5038(8) . ?

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
_geom_angle_publ_flag
Ba1 Ba1 Ba1 60.0 4_566 3_656 ?
Ba1 Ba1 Ba1 59.998(1) 4_566 2_665 ?
Ba1 Ba1 Ba1 59.998(1) 3_656 2_665 ?
Ba1 Ba1 As1 147.664(10) 4_566 . ?
Ba1 Ba1 As1 147.664(10) 3_656 . ?
Ba1 Ba1 As1 112.59(3) 2_665 . ?
Ba1 Ba1 As1 147.664(10) 4_566 9 ?
Ba1 Ba1 As1 112.59(3) 3_656 9 ?
Ba1 Ba1 As1 147.664(10) 2_665 9 ?
As1 Ba1 As1 54.88(5) . 9 ?
Ba1 Ba1 As1 112.59(3) 4_566 5 ?
Ba1 Ba1 As1 147.664(10) 3_656 5 ?
Ba1 Ba1 As1 147.664(10) 2_665 5 ?
As1 Ba1 As1 54.88(5) . 5 ?
As1 Ba1 As1 54.88(5) 9 5 ?
Ba1 Ba1 Ge2 85.60(4) 4_566 26 ?
Ba1 Ba1 Ge2 85.60(4) 3_656 26 ?
Ba1 Ba1 Ge2 139.65(5) 2_665 26 ?
As1 Ba1 Ge2 107.75(7) . 26 ?
As1 Ba1 Ge2 62.09(3) 9 26 ?
As1 Ba1 Ge2 62.09(3) 5 26 ?
Ba1 Ba1 Ge2 139.65(5) 4_566 28 ?
Ba1 Ba1 Ge2 85.60(4) 3_656 28 ?
Ba1 Ba1 Ge2 85.60(4) 2_665 28 ?
As1 Ba1 Ge2 62.09(3) . 28 ?
As1 Ba1 Ge2 62.09(3) 9 28 ?
As1 Ba1 Ge2 107.76(7) 5 28 ?
Ge2 Ba1 Ge2 114.04(4) 26 28 ?
Ba1 Ba1 Ge2 85.60(4) 4_566 27 ?
Ba1 Ba1 Ge2 139.65(5) 3_656 27 ?
Ba1 Ba1 Ge2 85.60(4) 2_665 27 ?
As1 Ba1 Ge2 62.09(3) . 27 ?
As1 Ba1 Ge2 107.76(7) 9 27 ?
As1 Ba1 Ge2 62.09(3) 5 27 ?
Ge2 Ba1 Ge2 114.04(4) 26 27 ?
Ge2 Ba1 Ge2 114.04(4) 28 27 ?
Ba1 Ba1 As1 59.40(5) 4_566 6_566 ?
Ba1 Ba1 As1 110.74(4) 3_656 6_566 ?
Ba1 Ba1 As1 110.74(4) 2_665 6_566 ?
As1 Ba1 As1 101.32(5) . 6_566 ?
As1 Ba1 As1 101.32(5) 9 6_566 ?
As1 Ba1 As1 53.19(2) 5 6_566 ?
Ge2 Ba1 As1 59.807(9) 26 6_566 ?
Ge2 Ba1 As1 160.94(9) 28 6_566 ?
Ge2 Ba1 As1 59.807(9) 27 6_566 ?
Ba1 Ba1 As1 110.74(4) 4_566 10_656 ?
Ba1 Ba1 As1 59.40(5) 3_656 10_656 ?
Ba1 Ba1 As1 110.74(4) 2_665 10_656 ?
As1 Ba1 As1 101.32(5) . 10_656 ?
As1 Ba1 As1 53.19(2) 9 10_656 ?
As1 Ba1 As1 101.32(5) 5 10_656 ?
Ge2 Ba1 As1 59.807(9) 26 10_656 ?
Ge2 Ba1 As1 59.807(9) 28 10_656 ?
Ge2 Ba1 As1 160.94(9) 27 10_656 ?
As1 Ba1 As1 119.346(13) 6_566 10_656 ?
Ba1 Ba1 As1 110.74(4) 4_566 2_665 ?
Ba1 Ba1 As1 110.74(4) 3_656 2_665 ?
Ba1 Ba1 As1 59.40(5) 2_665 2_665 ?
As1 Ba1 As1 53.19(2) . 2_665 ?
As1 Ba1 As1 101.32(5) 9 2_665 ?
As1 Ba1 As1 101.32(5) 5 2_665 ?
Ge2 Ba1 As1 160.94(9) 26 2_665 ?
Ge2 Ba1 As1 59.807(9) 28 2_665 ?
Ge2 Ba1 As1 59.807(9) 27 2_665 ?
As1 Ba1 As1 119.346(13) 6_566 2_665 ?
As1 Ba1 As1 119.346(13) 10_656 2_665 ?
As1 Ge1 As1 110.53(2) 36_554 34 ?
As1 Ge1 As1 108.946(11) 36_554 4_565 ?
As1 Ge1 As1 108.946(11) 34 4_565 ?
As1 Ge1 As1 108.946(11) 36_554 . ?
As1 Ge1 As1 108.946(11) 34 . ?
As1 Ge1 As1 110.53(2) 4_565 . ?
Ge1 As1 Ge1 96.525(17) 30 . ?
Ge1 As1 As2 96.405(18) 30 . ?
Ge1 As1 As2 96.405(18) . . ?
Ge1 As1 Ba1 129.426(12) 30 . ?
Ge1 As1 Ba1 129.426(12) . . ?
As2 As1 Ba1 97.80(4) . . ?
Ge1 As1 Ba1 126.945(19) 30 2_665 ?
Ge1 As1 Ba1 126.945(19) . 2_665 ?
As2 As1 Ba1 105.82(5) . 2_665 ?
Ba1 As1 Ba1 8.01(7) . 2_665 ?
As1 As2 As1 83.19(3) . 9 ?
As1 As2 As1 83.19(3) . 5 ?
As1 As2 As1 83.20(3) 9 5 ?
As1 As2 Ba1 124.87(5) . 26_554 ?
As1 As2 Ba1 132.34(3) 9 26_554 ?
As1 As2 Ba1 132.34(3) 5 26_554 ?
As1 As2 Ba1 132.34(3) . 28_455 ?
As1 As2 Ba1 132.34(3) 9 28_455 ?
As1 As2 Ba1 124.87(5) 5 28_455 ?
Ba1 As2 Ba1 8.79(8) 26_554 28_455 ?
As1 As2 Ba1 132.34(3) . 27_545 ?
As1 As2 Ba1 124.87(5) 9 27_545 ?
As1 As2 Ba1 132.34(3) 5 27_545 ?
Ba1 As2 Ba1 8.79(8) 26_554 27_545 ?
Ba1 As2 Ba1 8.79(8) 28_455 27_545 ?

_refine_diff_density_max         0.597
_refine_diff_density_min         -0.598
_refine_diff_density_rms         0.159

_shelx_res_file                  
;
TITL nochmal in I-43m
    shelx.res
    created by SHELXL-2018/3 at 10:21:46 on 09-Jul-2020
CELL 0.71073  10.314500  10.314500  10.314500  90.000000  90.000000  90.000000
ZERR   2      0.000200   0.000200   0.000200   0.000000   0.000000   0.000000
LATT -2
SYMM -x,-y,z
SYMM -x,y,-z
SYMM x,-y,-z
SYMM z,x,y
SYMM z,-x,-y
SYMM -z,-x,y
SYMM -z,x,-y
SYMM y,z,x
SYMM -y,z,-x
SYMM y,-z,-x
SYMM -y,-z,x
SYMM y,x,z
SYMM -y,-x,z
SYMM y,-x,-z
SYMM -y,x,-z
SYMM x,z,y
SYMM -x,z,-y
SYMM -x,-z,y
SYMM x,-z,-y
SYMM z,y,x
SYMM z,-y,-x
SYMM -z,y,-x
SYMM -z,-y,x
SFAC Ge As Ba
UNIT  16 28 2
L.S.   10
FMAP   2
SIZE 0.054 0.087 0.134
TWIN
ACTA
EADP AS2 GE2
EXYZ AS2 GE2
PLAN   20
WGHT    0.016100    0.035600
BASF   0.21963
FVAR       0.06985
BA1   3    0.479979    0.479979    0.479979    10.04167    0.05035    0.05035 =
         0.05035   -0.00921   -0.00921   -0.00921
GE1   1    0.250000    0.500000    0.000000    10.25000    0.01286    0.00973 =
         0.00973    0.00000    0.00000    0.00000
GE2   1    0.219022    0.219022    0.219022    10.08333    0.01339    0.01339 =
         0.01339    0.00172    0.00172    0.00172
AS1   2    0.384986    0.384986    0.157076    10.50000    0.01216    0.01216 =
         0.01021    0.00053    0.00053    0.00034
AS2   2    0.219022    0.219022    0.219022    10.08333    0.01339    0.01339 =
         0.01339    0.00172    0.00172    0.00172

HKLF  4




REM  nochmal in I-43m
REM wR2 = 0.0303, GooF = S = 1.330, Restrained GooF = 1.330 for all data
REM R1 = 0.0123 for 325 Fo > 4sig(Fo) and 0.0132 for all 329 data
REM 16 parameters refined using 0 restraints

END

WGHT      0.0161      0.0356

REM Highest difference peak  0.597,  deepest hole -0.598,  1-sigma level  0.159
Q1    1   0.3283  0.4466  0.0688  11.00000  0.05    0.60
Q2    1   0.3007  0.3007  0.1707  10.50000  0.05    0.59
Q3    1   0.5000  0.5000  0.0349  10.25000  0.05    0.53
Q4    1   0.5000  0.5000  0.0000  10.12500  0.05    0.49
Q5    1   0.1282  0.4113  0.1282  10.50000  0.05    0.44
Q6    1   0.2996  0.2729  0.2996  10.50000  0.05    0.42
Q7    1   0.3194  0.3194  0.0700  10.50000  0.05    0.41
Q8    1   0.4214  0.5786  0.3235  10.50000  0.05    0.39
Q9    1   0.4301  0.3645  0.5699  10.50000  0.05    0.38
Q10   1   0.4428  0.4428  0.2511  10.50000  0.05    0.38
Q11   1   0.3996  0.3996  0.5611  10.50000  0.05    0.37
Q12   1   0.3589  0.6411  0.0679  10.50000  0.05    0.33
Q13   1   0.4562  0.4305  0.2239  11.00000  0.05    0.29
Q14   1   0.4587  0.2630  0.2630  10.50000  0.05    0.28
Q15   1   0.4638  0.4638  0.1907  10.50000  0.05    0.27
Q16   1   0.3057  0.4533  0.1810  11.00000  0.05    0.24
Q17   1   0.1256  0.1256  0.3111  10.50000  0.05    0.22
Q18   1   0.2951  0.4658  0.2322  11.00000  0.05    0.21
Q19   1   0.4232  0.3397  0.4232  10.50000  0.05    0.19
Q20   1   0.3286  0.5810  0.0461  11.00000  0.05    0.18
;
_shelx_res_checksum              60999

# start Validation Reply Form
_vrf_PLAT911_shelx               
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L=    0.600          2 Report
RESPONSE: Reflections concealed by beam stop.
;
# end Validation Reply Form
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_shelx_CCDC1
_database_code_depnum_ccdc_archive 'CCDC 2017129'
loop_
_audit_author_name
_audit_author_address
'Valentin Weippert'
;LMU Munich
Germany
;
_audit_update_record             
;
2020-07-17 deposited with the CCDC.	2020-12-21 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'As14 Ba Ge8'
_chemical_formula_sum            'As14 Ba Ge8'
_chemical_formula_weight         1766.94

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
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'
Ba Ba -0.3244 2.2819 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      cubic
_space_group_IT_number           217
_space_group_name_H-M_alt        'I -4 3 m'
_space_group_name_Hall           'I -4 2 3'

_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'-x, y, -z'
'x, -y, -z'
'z, x, y'
'z, -x, -y'
'-z, -x, y'
'-z, x, -y'
'y, z, x'
'-y, z, -x'
'y, -z, -x'
'-y, -z, x'
'y, x, z'
'-y, -x, z'
'y, -x, -z'
'-y, x, -z'
'x, z, y'
'-x, z, -y'
'-x, -z, y'
'x, -z, -y'
'z, y, x'
'z, -y, -x'
'-z, y, -x'
'-z, -y, x'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'-x+1/2, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'z+1/2, x+1/2, y+1/2'
'z+1/2, -x+1/2, -y+1/2'
'-z+1/2, -x+1/2, y+1/2'
'-z+1/2, x+1/2, -y+1/2'
'y+1/2, z+1/2, x+1/2'
'-y+1/2, z+1/2, -x+1/2'
'y+1/2, -z+1/2, -x+1/2'
'-y+1/2, -z+1/2, x+1/2'
'y+1/2, x+1/2, z+1/2'
'-y+1/2, -x+1/2, z+1/2'
'y+1/2, -x+1/2, -z+1/2'
'-y+1/2, x+1/2, -z+1/2'
'x+1/2, z+1/2, y+1/2'
'-x+1/2, z+1/2, -y+1/2'
'-x+1/2, -z+1/2, y+1/2'
'x+1/2, -z+1/2, -y+1/2'
'z+1/2, y+1/2, x+1/2'
'z+1/2, -y+1/2, -x+1/2'
'-z+1/2, y+1/2, -x+1/2'
'-z+1/2, -y+1/2, x+1/2'

_cell_length_a                   10.3060(2)
_cell_length_b                   10.3060(2)
_cell_length_c                   10.3060(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1094.64(6)
_cell_formula_units_Z            2
_cell_measurement_temperature    218(2)
_cell_measurement_reflns_used    9982
_cell_measurement_theta_min      5.590
_cell_measurement_theta_max      89.110

_exptl_crystal_description       block
_exptl_crystal_colour            black
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    5.361
_exptl_crystal_F_000             1548
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.119
_exptl_crystal_size_mid          0.111
_exptl_crystal_size_min          0.059
_exptl_absorpt_coefficient_mu    33.576
_shelx_estimated_absorpt_T_min   0.109
_shelx_estimated_absorpt_T_max   0.242
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.1855
_exptl_absorpt_correction_T_max  0.3554
_exptl_absorpt_process_details   
;
Additional spherical absorption correction
 applied with mu*r =  0.8000  (Bruker, 2016)
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      218(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       'combined φ ω scan'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            17101
_diffrn_reflns_av_unetI/netI     0.0098
_diffrn_reflns_av_R_equivalents  0.0355
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         2.795
_diffrn_reflns_theta_max         36.956
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measured_fraction_theta_full 0.952
_diffrn_reflns_Laue_measured_fraction_max 0.981
_diffrn_reflns_Laue_measured_fraction_full 0.952
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_point_group_measured_fraction_full 0.953
_reflns_number_total             540
_reflns_number_gt                536
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.776
_reflns_Friedel_fraction_max     0.983
_reflns_Friedel_fraction_full    0.955

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;

_computing_data_collection       'APEX3 (Bruker, 2016)'
_computing_cell_refinement       'APEX3 (Bruker, 2016)'
_computing_data_reduction        'APEX3 (Bruker, 2016)'
_computing_structure_solution    'SUPERFLIP (Palatinus & Chapuis, 2007)'
_computing_structure_refinement  'SHELXL (Sheldrick, 2015)'
_computing_molecular_graphics    'DIAMOND 3 (Brandenburg, 2014)'
_computing_publication_material  
;
PLATON V. 91007 (Spek, 2009)
STRUCTURETIDY (Gelato, Parthé, 1987)
;
_refine_special_details          
;
 Refined as a 2-component inversion twin.
 Ge2:As2 ratio fixed to 50:50 based on elemental analysis.
 Ba1 refined as a split position, changing the Wyckoff position
 from 2a to 8c. Consequently the occupancy of the Ba1 split 
 position is fixed to 0.25.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+6.5139P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   .
_refine_ls_hydrogen_treatment    undef
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.42(15)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         540
_refine_ls_number_parameters     16
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0120
_refine_ls_R_factor_gt           0.0116
_refine_ls_wR_factor_ref         0.0374
_refine_ls_wR_factor_gt          0.0373
_refine_ls_goodness_of_fit_ref   1.418
_refine_ls_restrained_S_all      1.418
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

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
Ba1 Ba 0.01986(18) 0.01986(18) 0.01986(18) 0.0446(12) Uani 0.25 6 d S T P . .
Ge1 Ge 0.250000 0.500000 0.000000 0.00792(11) Uani 1 4 d S T P . .
Ge2 Ge 0.28102(5) 0.28102(5) 0.28102(5) 0.01021(15) Uani 0.5 6 d S T P . .
As1 As 0.11512(4) 0.11512(4) 0.34292(5) 0.00855(9) Uani 1 2 d S T P . .
As2 As 0.28102(5) 0.28102(5) 0.28102(5) 0.01021(15) Uani 0.5 6 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
Ba1 0.0446(12) 0.0446(12) 0.0446(12) -0.0092(6) -0.0092(6) -0.0092(6)
Ge1 0.0098(3) 0.00699(15) 0.00699(15) 0.000 0.000 0.000
Ge2 0.01021(15) 0.01021(15) 0.01021(15) 0.00186(17) 0.00186(17) 0.00186(17)
As1 0.00894(12) 0.00894(12) 0.00776(18) 0.00054(10) 0.00054(10) 0.00035(14)
As2 0.01021(15) 0.01021(15) 0.01021(15) 0.00186(17) 0.00186(17) 0.00186(17)

_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ba1 Ba1 0.579(5) 4 ?
Ba1 Ba1 0.579(5) 3 ?
Ba1 Ba1 0.579(5) 2 ?
Ba1 As1 3.607(3) . ?
Ba1 As1 3.607(3) 9 ?
Ba1 As1 3.607(3) 5 ?
Ba1 Ge2 3.8054(12) 26_554 ?
Ba1 Ge2 3.8054(12) 28_455 ?
Ba1 Ge2 3.8054(12) 27_545 ?
Ba1 As1 3.8672(5) 10 ?
Ba1 As1 3.8672(5) 6 ?
Ba1 As1 3.8672(5) 2 ?
Ge1 As1 2.4415(3) 27 ?
Ge1 As1 2.4415(3) 9 ?
Ge1 As1 2.4415(3) 26_554 ?
Ge1 As1 2.4415(3) 11_565 ?
As1 As2 2.5008(8) . ?

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
_geom_angle_publ_flag
Ba1 Ba1 Ba1 60.002(1) 4 3 ?
Ba1 Ba1 Ba1 60.002(1) 4 2 ?
Ba1 Ba1 Ba1 60.002(1) 3 2 ?
Ba1 Ba1 As1 147.679(10) 4 . ?
Ba1 Ba1 As1 147.679(10) 3 . ?
Ba1 Ba1 As1 112.63(3) 2 . ?
Ba1 Ba1 As1 147.680(10) 4 9 ?
Ba1 Ba1 As1 112.64(3) 3 9 ?
Ba1 Ba1 As1 147.680(10) 2 9 ?
As1 Ba1 As1 54.80(5) . 9 ?
Ba1 Ba1 As1 112.64(3) 4 5 ?
Ba1 Ba1 As1 147.680(10) 3 5 ?
Ba1 Ba1 As1 147.680(10) 2 5 ?
As1 Ba1 As1 54.80(5) . 5 ?
As1 Ba1 As1 54.80(5) 9 5 ?
Ba1 Ba1 Ge2 85.64(4) 4 26_554 ?
Ba1 Ba1 Ge2 85.64(4) 3 26_554 ?
Ba1 Ba1 Ge2 139.70(5) 2 26_554 ?
As1 Ba1 Ge2 107.67(8) . 26_554 ?
As1 Ba1 Ge2 62.07(3) 9 26_554 ?
As1 Ba1 Ge2 62.07(3) 5 26_554 ?
Ba1 Ba1 Ge2 139.70(5) 4 28_455 ?
Ba1 Ba1 Ge2 85.64(4) 3 28_455 ?
Ba1 Ba1 Ge2 85.64(4) 2 28_455 ?
As1 Ba1 Ge2 62.07(3) . 28_455 ?
As1 Ba1 Ge2 62.07(3) 9 28_455 ?
As1 Ba1 Ge2 107.67(8) 5 28_455 ?
Ge2 Ba1 Ge2 114.01(4) 26_554 28_455 ?
Ba1 Ba1 Ge2 85.64(4) 4 27_545 ?
Ba1 Ba1 Ge2 139.70(5) 3 27_545 ?
Ba1 Ba1 Ge2 85.64(4) 2 27_545 ?
As1 Ba1 Ge2 62.07(3) . 27_545 ?
As1 Ba1 Ge2 107.67(8) 9 27_545 ?
As1 Ba1 Ge2 62.07(3) 5 27_545 ?
Ge2 Ba1 Ge2 114.01(4) 26_554 27_545 ?
Ge2 Ba1 Ge2 114.01(4) 28_455 27_545 ?
Ba1 Ba1 As1 110.76(4) 4 10 ?
Ba1 Ba1 As1 59.42(5) 3 10 ?
Ba1 Ba1 As1 110.76(4) 2 10 ?
As1 Ba1 As1 101.28(6) . 10 ?
As1 Ba1 As1 53.21(3) 9 10 ?
As1 Ba1 As1 101.28(6) 5 10 ?
Ge2 Ba1 As1 59.804(9) 26_554 10 ?
Ge2 Ba1 As1 59.804(9) 28_455 10 ?
Ge2 Ba1 As1 160.88(10) 27_545 10 ?
Ba1 Ba1 As1 59.42(5) 4 6 ?
Ba1 Ba1 As1 110.76(4) 3 6 ?
Ba1 Ba1 As1 110.76(4) 2 6 ?
As1 Ba1 As1 101.28(6) . 6 ?
As1 Ba1 As1 101.28(6) 9 6 ?
As1 Ba1 As1 53.21(3) 5 6 ?
Ge2 Ba1 As1 59.804(9) 26_554 6 ?
Ge2 Ba1 As1 160.88(10) 28_455 6 ?
Ge2 Ba1 As1 59.804(9) 27_545 6 ?
As1 Ba1 As1 119.340(14) 10 6 ?
Ba1 Ba1 As1 110.76(4) 4 2 ?
Ba1 Ba1 As1 110.76(4) 3 2 ?
Ba1 Ba1 As1 59.42(5) 2 2 ?
As1 Ba1 As1 53.21(3) . 2 ?
As1 Ba1 As1 101.28(6) 9 2 ?
As1 Ba1 As1 101.28(6) 5 2 ?
Ge2 Ba1 As1 160.88(10) 26_554 2 ?
Ge2 Ba1 As1 59.804(9) 28_455 2 ?
Ge2 Ba1 As1 59.804(9) 27_545 2 ?
As1 Ba1 As1 119.340(14) 10 2 ?
As1 Ba1 As1 119.340(14) 6 2 ?
As1 Ge1 As1 108.915(12) 27 9 ?
As1 Ge1 As1 110.59(2) 27 26_554 ?
As1 Ge1 As1 108.915(12) 9 26_554 ?
As1 Ge1 As1 108.915(12) 27 11_565 ?
As1 Ge1 As1 110.59(2) 9 11_565 ?
As1 Ge1 As1 108.915(12) 26_554 11_565 ?
Ge1 As1 Ge1 96.527(17) 5 26 ?
Ge1 As1 As2 96.436(18) 5 . ?
Ge1 As1 As2 96.436(18) 26 . ?
Ge1 As1 Ba1 129.399(12) 5 . ?
Ge1 As1 Ba1 129.399(12) 26 . ?
As2 As1 Ba1 97.86(4) . . ?
Ge1 As1 Ba1 126.93(2) 5 2 ?
Ge1 As1 Ba1 126.93(2) 26 2 ?
As2 As1 Ba1 105.80(5) . 2 ?
Ba1 As1 Ba1 7.94(8) . 2 ?
As1 As2 As1 83.19(3) 9 5 ?
As1 As2 As1 83.19(3) 9 . ?
As1 As2 As1 83.19(3) 5 . ?
As1 As2 Ba1 124.92(5) 9 27 ?
As1 As2 Ba1 132.33(3) 5 27 ?
As1 As2 Ba1 132.33(3) . 27 ?
As1 As2 Ba1 132.33(3) 9 28 ?
As1 As2 Ba1 124.92(5) 5 28 ?
As1 As2 Ba1 132.33(3) . 28 ?
Ba1 As2 Ba1 8.72(8) 27 28 ?
As1 As2 Ba1 132.33(3) 9 26 ?
As1 As2 Ba1 132.33(3) 5 26 ?
As1 As2 Ba1 124.92(5) . 26 ?
Ba1 As2 Ba1 8.72(8) 27 26 ?
Ba1 As2 Ba1 8.72(8) 28 26 ?

_refine_diff_density_max         0.870
_refine_diff_density_min         -0.436
_refine_diff_density_rms         0.157

_shelx_res_file                  
;
TITL 218 in I-43m
    shelx.res
    created by SHELXL-2018/3 at 15:33:47 on 16-Jul-2020
CELL 0.71073  10.306000  10.306000  10.306000  90.000000  90.000000  90.000000
ZERR   2      0.000200   0.000200   0.000200   0.000000   0.000000   0.000000
LATT -2
SYMM -x,-y,z
SYMM -x,y,-z
SYMM x,-y,-z
SYMM z,x,y
SYMM z,-x,-y
SYMM -z,-x,y
SYMM -z,x,-y
SYMM y,z,x
SYMM -y,z,-x
SYMM y,-z,-x
SYMM -y,-z,x
SYMM y,x,z
SYMM -y,-x,z
SYMM y,-x,-z
SYMM -y,x,-z
SYMM x,z,y
SYMM -x,z,-y
SYMM -x,-z,y
SYMM x,-z,-y
SYMM z,y,x
SYMM z,-y,-x
SYMM -z,y,-x
SYMM -z,-y,x
SFAC Ge As Ba
UNIT  16 28 2
L.S.   10
FMAP   2
TWIN
TEMP -55
ACTA
SIZE 0.059 0.111 0.119
EADP AS2 GE2
EXYZ AS2 GE2
PLAN   20
WGHT    0.000000    6.513900
BASF   0.42211
FVAR       0.09435
BA1   3    0.019858    0.019858    0.019858    10.04167    0.04465    0.04465 =
         0.04465   -0.00923   -0.00923   -0.00923
GE1   1    0.250000    0.500000    0.000000    10.25000    0.00978    0.00699 =
         0.00699    0.00000    0.00000    0.00000
GE2   1    0.281022    0.281022    0.281022    10.08333    0.01021    0.01021 =
         0.01021    0.00186    0.00186    0.00186
AS1   2    0.115117    0.115117    0.342916    10.50000    0.00894    0.00894 =
         0.00776    0.00054    0.00054    0.00035
AS2   2    0.281022    0.281022    0.281022    10.08333    0.01021    0.01021 =
         0.01021    0.00186    0.00186    0.00186

HKLF  4




REM  218 in I-43m
REM wR2 = 0.0374, GooF = S = 1.418, Restrained GooF = 1.418 for all data
REM R1 = 0.0116 for 536 Fo > 4sig(Fo) and 0.0120 for all 540 data
REM 16 parameters refined using 0 restraints

END

WGHT      0.0000      6.5140

REM Highest difference peak  0.870,  deepest hole -0.436,  1-sigma level  0.157
Q1    1   0.0614  0.0000  0.0000  10.25000  0.05    0.87
Q2    1   0.0505  0.0505  0.0505  10.16667  0.05    0.79
Q3    1  -0.0240  0.0240  0.0240  10.16667  0.05    0.67
Q4    1   0.0000  0.0000  0.1440  10.25000  0.05    0.66
Q5    1   0.1066  0.1066 -0.0654  10.50000  0.05    0.63
Q6    1   0.0935  0.0935  0.0658  10.50000  0.05    0.51
Q7    1  -0.0540  0.0540  0.0540  10.16667  0.05    0.49
Q8    1   0.1065  0.0380  0.1065  10.50000  0.05    0.48
Q9    1   0.2211  0.2211  0.2211  10.16667  0.05    0.44
Q10   1   0.0502  0.1624  0.1624  10.50000  0.05    0.43
Q11   1   0.1007  0.0783 -0.0160  11.00000  0.05    0.42
Q12   1   0.3234  0.4080  0.3844  11.00000  0.05    0.40
Q13   1   0.1585  0.0503  0.0503  10.50000  0.05    0.37
Q14   1   0.0260  0.0260  0.2488  10.50000  0.05    0.37
Q15   1  -0.0300  0.0300  0.2432  10.50000  0.05    0.30
Q16   1  -0.0306  0.0802  0.2475  11.00000  0.05    0.30
Q17   1   0.1137  0.1137  0.2810  10.50000  0.05    0.29
Q18   1   0.0000  0.0000  0.3162  10.25000  0.05    0.29
Q19   1   0.2941  0.3723  0.3723  10.50000  0.05    0.29
Q20   1   0.1429  0.1049  0.1049  10.50000  0.05    0.28
;
_shelx_res_checksum              13360

# start Validation Reply Form
_vrf_PLAT919_shelx               
;
PROBLEM: Reflection # Likely Affected by the Beamstop ...          1 Check 
RESPONSE: Concealed by beam stop.
;
_vrf_STRVA01_shelx               
;
PROBLEM: Flack test results are ambiguous.
RESPONSE: Inversion twin with aprox. 50:50 ratio, absolute configuration
 not of interest.
;
_vrf_PLAT911_shelx               
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L=    0.600          6 Report
RESPONSE: Concealed by beam stop.
;
_vrf_PLAT913_shelx               
;
PROBLEM: Missing # of Very Strong Reflections in FCF ....          5 Note  
RESPONSE: Concealed by beam stop.
;
_vrf_PLAT934_shelx               
;
PROBLEM: Number of (Iobs-Icalc)/Sigma(W) > 10 Outliers ..          1 Check 
RESPONSE: Due to the formation of ice during measurement.
;
# end Validation Reply Form

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_shelx_CCDC2
_database_code_depnum_ccdc_archive 'CCDC 2017128'
loop_
_audit_author_name
_audit_author_address
'Valentin Weippert'
;LMU Munich
Germany
;
_audit_update_record             
;
2020-07-17 deposited with the CCDC.	2020-12-21 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'As14 Ba Ge8'
_chemical_formula_sum            'As14 Ba Ge8'
_chemical_formula_weight         1766.94

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
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'
Ba Ba -0.3244 2.2819 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      cubic
_space_group_IT_number           217
_space_group_name_H-M_alt        'I -4 3 m'
_space_group_name_Hall           'I -4 2 3'

_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'-x, y, -z'
'x, -y, -z'
'z, x, y'
'z, -x, -y'
'-z, -x, y'
'-z, x, -y'
'y, z, x'
'-y, z, -x'
'y, -z, -x'
'-y, -z, x'
'y, x, z'
'-y, -x, z'
'y, -x, -z'
'-y, x, -z'
'x, z, y'
'-x, z, -y'
'-x, -z, y'
'x, -z, -y'
'z, y, x'
'z, -y, -x'
'-z, y, -x'
'-z, -y, x'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'-x+1/2, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'z+1/2, x+1/2, y+1/2'
'z+1/2, -x+1/2, -y+1/2'
'-z+1/2, -x+1/2, y+1/2'
'-z+1/2, x+1/2, -y+1/2'
'y+1/2, z+1/2, x+1/2'
'-y+1/2, z+1/2, -x+1/2'
'y+1/2, -z+1/2, -x+1/2'
'-y+1/2, -z+1/2, x+1/2'
'y+1/2, x+1/2, z+1/2'
'-y+1/2, -x+1/2, z+1/2'
'y+1/2, -x+1/2, -z+1/2'
'-y+1/2, x+1/2, -z+1/2'
'x+1/2, z+1/2, y+1/2'
'-x+1/2, z+1/2, -y+1/2'
'-x+1/2, -z+1/2, y+1/2'
'x+1/2, -z+1/2, -y+1/2'
'z+1/2, y+1/2, x+1/2'
'z+1/2, -y+1/2, -x+1/2'
'-z+1/2, y+1/2, -x+1/2'
'-z+1/2, -y+1/2, x+1/2'

_cell_length_a                   10.3052(2)
_cell_length_b                   10.3052(2)
_cell_length_c                   10.3052(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1094.38(6)
_cell_formula_units_Z            2
_cell_measurement_temperature    189(2)
_cell_measurement_reflns_used    9979
_cell_measurement_theta_min      5.591
_cell_measurement_theta_max      89.118

_exptl_crystal_description       block
_exptl_crystal_colour            black
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    5.362
_exptl_crystal_F_000             1548
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.119
_exptl_crystal_size_mid          0.111
_exptl_crystal_size_min          0.059
_exptl_absorpt_coefficient_mu    33.584
_shelx_estimated_absorpt_T_min   0.108
_shelx_estimated_absorpt_T_max   0.242
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.1829
_exptl_absorpt_correction_T_max  0.3555
_exptl_absorpt_process_details   
;
Additional spherical absorption correction
 applied with mu*r =  0.8000  (Bruker, 2016)
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      189(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       'combined φ ω scan'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            17257
_diffrn_reflns_av_unetI/netI     0.0100
_diffrn_reflns_av_R_equivalents  0.0373
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         2.795
_diffrn_reflns_theta_max         36.959
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measured_fraction_theta_full 0.960
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_Laue_measured_fraction_full 0.960
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_point_group_measured_fraction_full 0.958
_reflns_number_total             541
_reflns_number_gt                537
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.774
_reflns_Friedel_fraction_max     0.983
_reflns_Friedel_fraction_full    0.955

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;

_computing_data_collection       'APEX3 (Bruker, 2016)'
_computing_cell_refinement       'APEX3 (Bruker, 2016)'
_computing_data_reduction        'APEX3 (Bruker, 2016)'
_computing_structure_solution    'SUPERFLIP (Palatinus & Chapuis, 2007)'
_computing_structure_refinement  'SHELXL (Sheldrick, 2015)'
_computing_molecular_graphics    'DIAMOND 3 (Brandenburg, 2014)'
_computing_publication_material  
;
PLATON V. 91007 (Spek, 2009)
STRUCTURETIDY (Gelato, Parthé, 1987)
;
_refine_special_details          
;
 Refined as a 2-component inversion twin.
 Ge2:As2 ratio fixed to 50:50 based on elemental analysis.
 Ba1 refined as a split position, changing the Wyckoff position
 from 2a to 8c. Consequently the occupancy of the Ba1 split 
 position is fixed to 0.25.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+6.5987P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   .
_refine_ls_hydrogen_treatment    undef
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.61(14)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         541
_refine_ls_number_parameters     16
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0119
_refine_ls_R_factor_gt           0.0119
_refine_ls_wR_factor_ref         0.0366
_refine_ls_wR_factor_gt          0.0366
_refine_ls_goodness_of_fit_ref   1.431
_refine_ls_restrained_S_all      1.431
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

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
Ba1 Ba 0.01981(17) 0.01981(17) 0.01981(17) 0.0417(12) Uani 0.25 6 d S T P . .
Ge1 Ge 0.250000 0.500000 0.000000 0.00687(11) Uani 1 4 d S T P . .
Ge2 Ge 0.28105(5) 0.28105(5) 0.28105(5) 0.00895(15) Uani 0.5 6 d S T P . .
As1 As 0.11513(4) 0.11513(4) 0.34287(5) 0.00742(9) Uani 1 2 d S T P . .
As2 As 0.28105(5) 0.28105(5) 0.28105(5) 0.00895(15) Uani 0.5 6 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
Ba1 0.0417(12) 0.0417(12) 0.0417(12) -0.0091(6) -0.0091(6) -0.0091(6)
Ge1 0.0085(2) 0.00603(15) 0.00603(15) 0.000 0.000 0.000
Ge2 0.00895(15) 0.00895(15) 0.00895(15) 0.00170(16) 0.00170(16) 0.00170(16)
As1 0.00781(12) 0.00781(12) 0.00662(18) 0.00045(10) 0.00045(10) 0.00030(13)
As2 0.00895(15) 0.00895(15) 0.00895(15) 0.00170(16) 0.00170(16) 0.00170(16)

_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ba1 Ba1 0.577(5) 4 ?
Ba1 Ba1 0.577(5) 3 ?
Ba1 Ba1 0.577(5) 2 ?
Ba1 As1 3.607(3) 9 ?
Ba1 As1 3.607(3) 5 ?
Ba1 As1 3.607(3) . ?
Ba1 Ge2 3.8048(12) 27_545 ?
Ba1 Ge2 3.8048(12) 28_455 ?
Ba1 Ge2 3.8048(12) 26_554 ?
Ba1 As1 3.8666(5) 10 ?
Ba1 As1 3.8666(5) 6 ?
Ba1 As1 3.8666(5) 2 ?
Ge1 As1 2.4416(3) 27 ?
Ge1 As1 2.4416(3) 9 ?
Ge1 As1 2.4416(3) 26_554 ?
Ge1 As1 2.4416(3) 11_565 ?
As1 As2 2.5006(8) . ?

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
_geom_angle_publ_flag
Ba1 Ba1 Ba1 59.995(1) 4 3 ?
Ba1 Ba1 Ba1 59.995(1) 4 2 ?
Ba1 Ba1 Ba1 59.995(1) 3 2 ?
Ba1 Ba1 As1 147.687(9) 4 9 ?
Ba1 Ba1 As1 112.65(3) 3 9 ?
Ba1 Ba1 As1 147.687(9) 2 9 ?
Ba1 Ba1 As1 112.65(3) 4 5 ?
Ba1 Ba1 As1 147.687(9) 3 5 ?
Ba1 Ba1 As1 147.687(9) 2 5 ?
As1 Ba1 As1 54.78(5) 9 5 ?
Ba1 Ba1 As1 147.686(9) 4 . ?
Ba1 Ba1 As1 147.686(9) 3 . ?
Ba1 Ba1 As1 112.65(3) 2 . ?
As1 Ba1 As1 54.78(5) 9 . ?
As1 Ba1 As1 54.78(5) 5 . ?
Ba1 Ba1 Ge2 85.65(4) 4 27_545 ?
Ba1 Ba1 Ge2 139.71(5) 3 27_545 ?
Ba1 Ba1 Ge2 85.65(4) 2 27_545 ?
As1 Ba1 Ge2 107.64(7) 9 27_545 ?
As1 Ba1 Ge2 62.06(3) 5 27_545 ?
As1 Ba1 Ge2 62.06(3) . 27_545 ?
Ba1 Ba1 Ge2 139.71(5) 4 28_455 ?
Ba1 Ba1 Ge2 85.65(4) 3 28_455 ?
Ba1 Ba1 Ge2 85.65(4) 2 28_455 ?
As1 Ba1 Ge2 62.06(3) 9 28_455 ?
As1 Ba1 Ge2 107.64(7) 5 28_455 ?
As1 Ba1 Ge2 62.06(3) . 28_455 ?
Ge2 Ba1 Ge2 114.00(4) 27_545 28_455 ?
Ba1 Ba1 Ge2 85.65(4) 4 26_554 ?
Ba1 Ba1 Ge2 85.65(4) 3 26_554 ?
Ba1 Ba1 Ge2 139.71(5) 2 26_554 ?
As1 Ba1 Ge2 62.06(3) 9 26_554 ?
As1 Ba1 Ge2 62.06(3) 5 26_554 ?
As1 Ba1 Ge2 107.64(7) . 26_554 ?
Ge2 Ba1 Ge2 114.00(4) 27_545 26_554 ?
Ge2 Ba1 Ge2 114.00(4) 28_455 26_554 ?
Ba1 Ba1 As1 110.76(4) 4 10 ?
Ba1 Ba1 As1 59.43(5) 3 10 ?
Ba1 Ba1 As1 110.76(4) 2 10 ?
As1 Ba1 As1 53.22(2) 9 10 ?
As1 Ba1 As1 101.27(5) 5 10 ?
As1 Ba1 As1 101.27(5) . 10 ?
Ge2 Ba1 As1 160.86(9) 27_545 10 ?
Ge2 Ba1 As1 59.803(9) 28_455 10 ?
Ge2 Ba1 As1 59.803(9) 26_554 10 ?
Ba1 Ba1 As1 59.43(5) 4 6 ?
Ba1 Ba1 As1 110.76(4) 3 6 ?
Ba1 Ba1 As1 110.76(4) 2 6 ?
As1 Ba1 As1 101.27(5) 9 6 ?
As1 Ba1 As1 53.22(2) 5 6 ?
As1 Ba1 As1 101.27(5) . 6 ?
Ge2 Ba1 As1 59.803(9) 27_545 6 ?
Ge2 Ba1 As1 160.86(9) 28_455 6 ?
Ge2 Ba1 As1 59.803(9) 26_554 6 ?
As1 Ba1 As1 119.338(13) 10 6 ?
Ba1 Ba1 As1 110.76(4) 4 2 ?
Ba1 Ba1 As1 110.76(4) 3 2 ?
Ba1 Ba1 As1 59.43(5) 2 2 ?
As1 Ba1 As1 101.27(5) 9 2 ?
As1 Ba1 As1 101.27(5) 5 2 ?
As1 Ba1 As1 53.22(2) . 2 ?
Ge2 Ba1 As1 59.803(9) 27_545 2 ?
Ge2 Ba1 As1 59.803(9) 28_455 2 ?
Ge2 Ba1 As1 160.86(9) 26_554 2 ?
As1 Ba1 As1 119.338(13) 10 2 ?
As1 Ba1 As1 119.338(13) 6 2 ?
As1 Ge1 As1 108.905(12) 27 9 ?
As1 Ge1 As1 110.61(2) 27 26_554 ?
As1 Ge1 As1 108.905(12) 9 26_554 ?
As1 Ge1 As1 108.905(12) 27 11_565 ?
As1 Ge1 As1 110.61(2) 9 11_565 ?
As1 Ge1 As1 108.905(12) 26_554 11_565 ?
Ge1 As1 Ge1 96.511(17) 26 5 ?
Ge1 As1 As2 96.430(18) 26 . ?
Ge1 As1 As2 96.430(18) 5 . ?
Ge1 As1 Ba1 129.400(12) 26 . ?
Ge1 As1 Ba1 129.400(12) 5 . ?
As2 As1 Ba1 97.89(3) . . ?
Ge1 As1 Ba1 126.940(19) 26 2 ?
Ge1 As1 Ba1 126.940(19) 5 2 ?
As2 As1 Ba1 105.81(5) . 2 ?
Ba1 As1 Ba1 7.92(7) . 2 ?
As1 As2 As1 83.16(3) 9 5 ?
As1 As2 As1 83.16(3) 9 . ?
As1 As2 As1 83.16(3) 5 . ?
As1 As2 Ba1 124.95(5) 9 27 ?
As1 As2 Ba1 132.34(3) 5 27 ?
As1 As2 Ba1 132.34(3) . 27 ?
As1 As2 Ba1 132.34(3) 9 28 ?
As1 As2 Ba1 124.95(5) 5 28 ?
As1 As2 Ba1 132.34(3) . 28 ?
Ba1 As2 Ba1 8.70(8) 27 28 ?
As1 As2 Ba1 132.34(3) 9 26 ?
As1 As2 Ba1 132.34(3) 5 26 ?
As1 As2 Ba1 124.95(5) . 26 ?
Ba1 As2 Ba1 8.70(8) 27 26 ?
Ba1 As2 Ba1 8.70(8) 28 26 ?

_refine_diff_density_max         1.105
_refine_diff_density_min         -0.741
_refine_diff_density_rms         0.179

_shelx_res_file                  
;
TITL 189 in I-43m
    shelx.res
    created by SHELXL-2018/3 at 15:31:08 on 16-Jul-2020
CELL 0.71073  10.305200  10.305200  10.305200  90.000000  90.000000  90.000000
ZERR   2      0.000200   0.000200   0.000200   0.000000   0.000000   0.000000
LATT -2
SYMM -x,-y,z
SYMM -x,y,-z
SYMM x,-y,-z
SYMM z,x,y
SYMM z,-x,-y
SYMM -z,-x,y
SYMM -z,x,-y
SYMM y,z,x
SYMM -y,z,-x
SYMM y,-z,-x
SYMM -y,-z,x
SYMM y,x,z
SYMM -y,-x,z
SYMM y,-x,-z
SYMM -y,x,-z
SYMM x,z,y
SYMM -x,z,-y
SYMM -x,-z,y
SYMM x,-z,-y
SYMM z,y,x
SYMM z,-y,-x
SYMM -z,y,-x
SYMM -z,-y,x
SFAC Ge As Ba
UNIT  16 28 2
L.S.   10
FMAP   2
TWIN
TEMP -84
ACTA
SIZE 0.059 0.111 0.119
EADP AS2 GE2
EXYZ AS2 GE2
PLAN   20
WGHT    0.000000    6.598700
BASF   0.61160
FVAR       0.08116
BA1   3    0.019809    0.019809    0.019809    10.04167    0.04169    0.04169 =
         0.04169   -0.00913   -0.00913   -0.00913
GE1   1    0.250000    0.500000    0.000000    10.25000    0.00854    0.00603 =
         0.00603    0.00000    0.00000    0.00000
GE2   1    0.281053    0.281053    0.281053    10.08333    0.00895    0.00895 =
         0.00895    0.00170    0.00170    0.00170
AS1   2    0.115133    0.115133    0.342869    10.50000    0.00781    0.00781 =
         0.00662    0.00045    0.00045    0.00030
AS2   2    0.281053    0.281053    0.281053    10.08333    0.00895    0.00895 =
         0.00895    0.00170    0.00170    0.00170

HKLF  4




REM  189 in I-43m
REM wR2 = 0.0366, GooF = S = 1.431, Restrained GooF = 1.431 for all data
REM R1 = 0.0119 for 537 Fo > 4sig(Fo) and 0.0119 for all 541 data
REM 16 parameters refined using 0 restraints

END

WGHT      0.0000      6.5990

REM Highest difference peak  1.105,  deepest hole -0.741,  1-sigma level  0.179
Q1    1   0.0000  0.0487  0.0000  10.25000  0.05    1.10
Q2    1   0.0509  0.0509  0.0509  10.16667  0.05    0.72
Q3    1   0.0000  0.0000  0.1364  10.25000  0.05    0.70
Q4    1  -0.0545  0.0545  0.0545  10.16667  0.05    0.61
Q5    1   0.1132  0.1132 -0.0626  10.50000  0.05    0.53
Q6    1   0.1357  0.1074  0.1074  10.50000  0.05    0.53
Q7    1  -0.0410  0.1030  0.1339  11.00000  0.05    0.51
Q8    1  -0.0659  0.1464  0.0659  10.50000  0.05    0.48
Q9    1   0.0955  0.0955  0.0955  10.16667  0.05    0.48
Q10   1   0.0908  0.0908  0.1637  10.50000  0.05    0.46
Q11   1   0.3104  0.4077  0.4077  10.50000  0.05    0.46
Q12   1   0.1414 -0.0343  0.0343  10.50000  0.05    0.45
Q13   1   0.1247  0.0587 -0.0160  11.00000  0.05    0.45
Q14   1   0.1176  0.0312  0.1176  10.50000  0.05    0.43
Q15   1   0.1764  0.0925 -0.0218  11.00000  0.05    0.43
Q16   1   0.1614  0.0545  0.0545  10.50000  0.05    0.42
Q17   1   0.0595 -0.0595  0.2243  10.50000  0.05    0.42
Q18   1   0.0000  0.0000  0.4640  10.25000  0.05    0.42
Q19   1   0.0561  0.0561  0.3162  10.50000  0.05    0.42
Q20   1   0.1182 -0.0096  0.1512  11.00000  0.05    0.38
;
_shelx_res_checksum              76716


# start Validation Reply Form
_vrf_PLAT919_shelx               
;
PROBLEM: Reflection # Likely Affected by the Beamstop ...          1 Check 
RESPONSE: Concealed by beam stop.
;
_vrf_STRVA01_shelx               
;
PROBLEM: Flack test results are ambiguous.
RESPONSE: Inversion twin with aprox. 50:50 ratio, absolute configuration
 not of interest.
;
_vrf_PLAT907_shelx               
;
PROBLEM: Flack x > 0.5, Structure Needs to be Inverted? .       0.61 Check 
RESPONSE: This refinement is based on the same crystal used for
the measurements at 103, 143 and 218K presented in this paper.
They yield a Flack paramter of 0.41(14). Consequently the
structure for this refinement was not inverted.
;
_vrf_PLAT911_shelx               
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L=    0.600          5 Report
RESPONSE: Concealed by beam stop.
;
_vrf_PLAT918_shelx               
;
PROBLEM: Reflection(s) with I(obs) much Smaller I(calc) .          1 Check 
RESPONSE: Partially concealed by beam stop.
;
_vrf_PLAT934_shelx               
;
PROBLEM: Number of (Iobs-Icalc)/Sigma(W) > 10 Outliers ..          1 Check 
RESPONSE: Due to the formation of ice during measurement.
;
# end Validation Reply Form
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_shelx_CCDC3
_database_code_depnum_ccdc_archive 'CCDC 2017126'
loop_
_audit_author_name
_audit_author_address
'Valentin Weippert'
;LMU Munich
Germany
;
_audit_update_record             
;
2020-07-17 deposited with the CCDC.	2020-12-21 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'As14 Ba Ge8'
_chemical_formula_sum            'As14 Ba Ge8'
_chemical_formula_weight         1766.94

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
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'
Ba Ba -0.3244 2.2819 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      cubic
_space_group_IT_number           217
_space_group_name_H-M_alt        'I -4 3 m'
_space_group_name_Hall           'I -4 2 3'

_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'-x, y, -z'
'x, -y, -z'
'z, x, y'
'z, -x, -y'
'-z, -x, y'
'-z, x, -y'
'y, z, x'
'-y, z, -x'
'y, -z, -x'
'-y, -z, x'
'y, x, z'
'-y, -x, z'
'y, -x, -z'
'-y, x, -z'
'x, z, y'
'-x, z, -y'
'-x, -z, y'
'x, -z, -y'
'z, y, x'
'z, -y, -x'
'-z, y, -x'
'-z, -y, x'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'-x+1/2, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'z+1/2, x+1/2, y+1/2'
'z+1/2, -x+1/2, -y+1/2'
'-z+1/2, -x+1/2, y+1/2'
'-z+1/2, x+1/2, -y+1/2'
'y+1/2, z+1/2, x+1/2'
'-y+1/2, z+1/2, -x+1/2'
'y+1/2, -z+1/2, -x+1/2'
'-y+1/2, -z+1/2, x+1/2'
'y+1/2, x+1/2, z+1/2'
'-y+1/2, -x+1/2, z+1/2'
'y+1/2, -x+1/2, -z+1/2'
'-y+1/2, x+1/2, -z+1/2'
'x+1/2, z+1/2, y+1/2'
'-x+1/2, z+1/2, -y+1/2'
'-x+1/2, -z+1/2, y+1/2'
'x+1/2, -z+1/2, -y+1/2'
'z+1/2, y+1/2, x+1/2'
'z+1/2, -y+1/2, -x+1/2'
'-z+1/2, y+1/2, -x+1/2'
'-z+1/2, -y+1/2, x+1/2'

_cell_length_a                   10.2967(2)
_cell_length_b                   10.2967(2)
_cell_length_c                   10.2967(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1091.68(6)
_cell_formula_units_Z            2
_cell_measurement_temperature    103(2)
_cell_measurement_reflns_used    9953
_cell_measurement_theta_min      5.595
_cell_measurement_theta_max      89.211

_exptl_crystal_description       block
_exptl_crystal_colour            black
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    5.375
_exptl_crystal_F_000             1548
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.119
_exptl_crystal_size_mid          0.111
_exptl_crystal_size_min          0.059
_exptl_absorpt_coefficient_mu    33.667
_shelx_estimated_absorpt_T_min   0.108
_shelx_estimated_absorpt_T_max   0.241
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.4348
_exptl_absorpt_correction_T_max  0.7489
_exptl_absorpt_process_details   
;
Additional spherical absorption correction
 applied with mu*r =  0.2000  (Bruker, 2016)
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      103(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       'combined φ ω scan'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            17494
_diffrn_reflns_av_unetI/netI     0.0105
_diffrn_reflns_av_R_equivalents  0.0395
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         2.798
_diffrn_reflns_theta_max         36.995
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measured_fraction_theta_full 0.984
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_Laue_measured_fraction_full 0.984
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_point_group_measured_fraction_full 0.986
_reflns_number_total             547
_reflns_number_gt                542
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.776
_reflns_Friedel_fraction_max     0.996
_reflns_Friedel_fraction_full    0.989

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;

_computing_data_collection       'APEX3 (Bruker, 2016)'
_computing_cell_refinement       'APEX3 (Bruker, 2016)'
_computing_data_reduction        'APEX3 (Bruker, 2016)'
_computing_structure_solution    'SUPERFLIP (Palatinus & Chapuis, 2007)'
_computing_structure_refinement  'SHELXL (Sheldrick, 2015)'
_computing_molecular_graphics    'DIAMOND 3 (Brandenburg, 2014)'
_computing_publication_material  
;
PLATON V. 91007 (Spek, 2009)
STRUCTURETIDY (Gelato, Parthé, 1987)
;
_refine_special_details          
;
 Refined as a 2-component inversion twin.
 Ge2:As2 ratio fixed to 50:50 based on elemental analysis.
 Ba1 refined as a split position, changing the Wyckoff position
 from 2a to 8c. Consequently the occupancy of the Ba1 split 
 position is fixed to 0.25.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+7.8597P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   .
_refine_ls_hydrogen_treatment    undef
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.45(13)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         547
_refine_ls_number_parameters     16
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0121
_refine_ls_R_factor_gt           0.0119
_refine_ls_wR_factor_ref         0.0346
_refine_ls_wR_factor_gt          0.0345
_refine_ls_goodness_of_fit_ref   1.351
_refine_ls_restrained_S_all      1.351
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

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
Ba1 Ba 0.01987(15) 0.01987(15) 0.01987(15) 0.0340(10) Uani 0.25 6 d S T P . .
Ge1 Ge 0.250000 0.500000 0.000000 0.00409(10) Uani 1 4 d S T P . .
Ge2 Ge 0.28112(5) 0.28112(5) 0.28112(5) 0.00593(14) Uani 0.5 6 d S T P . .
As1 As 0.11514(3) 0.11514(3) 0.34284(5) 0.00459(8) Uani 1 2 d S T P . .
As2 As 0.28112(5) 0.28112(5) 0.28112(5) 0.00593(14) Uani 0.5 6 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
Ba1 0.0340(10) 0.0340(10) 0.0340(10) -0.0089(5) -0.0089(5) -0.0089(5)
Ge1 0.0054(2) 0.00345(14) 0.00345(14) 0.000 0.000 0.000
Ge2 0.00593(14) 0.00593(14) 0.00593(14) 0.00172(15) 0.00172(15) 0.00172(15)
As1 0.00481(11) 0.00481(11) 0.00413(17) 0.00043(10) 0.00043(10) 0.00028(13)
As2 0.00593(14) 0.00593(14) 0.00593(14) 0.00172(15) 0.00172(15) 0.00172(15)

_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ba1 Ba1 0.579(4) 4 ?
Ba1 Ba1 0.579(4) 3 ?
Ba1 Ba1 0.579(4) 2 ?
Ba1 As1 3.603(2) . ?
Ba1 As1 3.603(2) 9 ?
Ba1 As1 3.603(2) 5 ?
Ba1 Ge2 3.8002(11) 26_554 ?
Ba1 Ge2 3.8002(11) 28_455 ?
Ba1 Ge2 3.8002(11) 27_545 ?
Ba1 As1 3.8632(5) 6 ?
Ba1 As1 3.8632(5) 10 ?
Ba1 As1 3.8632(5) 2 ?
Ge1 As1 2.4398(3) 27 ?
Ge1 As1 2.4398(3) 9 ?
Ge1 As1 2.4398(3) 26_554 ?
Ge1 As1 2.4398(3) 11_565 ?
As1 As2 2.4992(8) . ?

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
_geom_angle_publ_flag
Ba1 Ba1 Ba1 60.002(1) 4 3 ?
Ba1 Ba1 Ba1 60.002(1) 4 2 ?
Ba1 Ba1 Ba1 60.002(1) 3 2 ?
Ba1 Ba1 As1 147.682(8) 4 . ?
Ba1 Ba1 As1 147.682(8) 3 . ?
Ba1 Ba1 As1 112.64(2) 2 . ?
Ba1 Ba1 As1 147.682(8) 4 9 ?
Ba1 Ba1 As1 112.64(2) 3 9 ?
Ba1 Ba1 As1 147.682(8) 2 9 ?
As1 Ba1 As1 54.79(4) . 9 ?
Ba1 Ba1 As1 112.64(2) 4 5 ?
Ba1 Ba1 As1 147.682(8) 3 5 ?
Ba1 Ba1 As1 147.682(8) 2 5 ?
As1 Ba1 As1 54.79(4) . 5 ?
As1 Ba1 As1 54.79(4) 9 5 ?
Ba1 Ba1 Ge2 85.63(3) 4 26_554 ?
Ba1 Ba1 Ge2 85.63(3) 3 26_554 ?
Ba1 Ba1 Ge2 139.69(4) 2 26_554 ?
As1 Ba1 Ge2 107.67(6) . 26_554 ?
As1 Ba1 Ge2 62.07(3) 9 26_554 ?
As1 Ba1 Ge2 62.07(3) 5 26_554 ?
Ba1 Ba1 Ge2 139.69(4) 4 28_455 ?
Ba1 Ba1 Ge2 85.63(3) 3 28_455 ?
Ba1 Ba1 Ge2 85.63(3) 2 28_455 ?
As1 Ba1 Ge2 62.07(3) . 28_455 ?
As1 Ba1 Ge2 62.07(3) 9 28_455 ?
As1 Ba1 Ge2 107.67(6) 5 28_455 ?
Ge2 Ba1 Ge2 114.01(3) 26_554 28_455 ?
Ba1 Ba1 Ge2 85.63(3) 4 27_545 ?
Ba1 Ba1 Ge2 139.69(4) 3 27_545 ?
Ba1 Ba1 Ge2 85.63(3) 2 27_545 ?
As1 Ba1 Ge2 62.07(3) . 27_545 ?
As1 Ba1 Ge2 107.67(6) 9 27_545 ?
As1 Ba1 Ge2 62.07(3) 5 27_545 ?
Ge2 Ba1 Ge2 114.01(3) 26_554 27_545 ?
Ge2 Ba1 Ge2 114.01(3) 28_455 27_545 ?
Ba1 Ba1 As1 59.41(4) 4 6 ?
Ba1 Ba1 As1 110.75(3) 3 6 ?
Ba1 Ba1 As1 110.75(3) 2 6 ?
As1 Ba1 As1 101.29(5) . 6 ?
As1 Ba1 As1 101.29(5) 9 6 ?
As1 Ba1 As1 53.23(2) 5 6 ?
Ge2 Ba1 As1 59.806(8) 26_554 6 ?
Ge2 Ba1 As1 160.90(8) 28_455 6 ?
Ge2 Ba1 As1 59.806(8) 27_545 6 ?
Ba1 Ba1 As1 110.75(3) 4 10 ?
Ba1 Ba1 As1 59.41(4) 3 10 ?
Ba1 Ba1 As1 110.75(3) 2 10 ?
As1 Ba1 As1 101.29(5) . 10 ?
As1 Ba1 As1 53.23(2) 9 10 ?
As1 Ba1 As1 101.29(5) 5 10 ?
Ge2 Ba1 As1 59.806(8) 26_554 10 ?
Ge2 Ba1 As1 59.806(8) 28_455 10 ?
Ge2 Ba1 As1 160.90(8) 27_545 10 ?
As1 Ba1 As1 119.343(11) 6 10 ?
Ba1 Ba1 As1 110.75(3) 4 2 ?
Ba1 Ba1 As1 110.75(3) 3 2 ?
Ba1 Ba1 As1 59.41(4) 2 2 ?
As1 Ba1 As1 53.23(2) . 2 ?
As1 Ba1 As1 101.29(5) 9 2 ?
As1 Ba1 As1 101.29(5) 5 2 ?
Ge2 Ba1 As1 160.90(8) 26_554 2 ?
Ge2 Ba1 As1 59.806(8) 28_455 2 ?
Ge2 Ba1 As1 59.806(8) 27_545 2 ?
As1 Ba1 As1 119.343(11) 6 2 ?
As1 Ba1 As1 119.343(11) 10 2 ?
As1 Ge1 As1 108.903(11) 27 9 ?
As1 Ge1 As1 110.61(2) 27 26_554 ?
As1 Ge1 As1 108.903(11) 9 26_554 ?
As1 Ge1 As1 108.903(11) 27 11_565 ?
As1 Ge1 As1 110.61(2) 9 11_565 ?
As1 Ge1 As1 108.903(11) 26_554 11_565 ?
Ge1 As1 Ge1 96.501(16) 5 26 ?
Ge1 As1 As2 96.414(17) 5 . ?
Ge1 As1 As2 96.414(17) 26 . ?
Ge1 As1 Ba1 129.406(11) 5 . ?
Ge1 As1 Ba1 129.406(11) 26 . ?
As2 As1 Ba1 97.91(3) . . ?
Ge1 As1 Ba1 126.936(17) 5 2 ?
Ge1 As1 Ba1 126.936(17) 26 2 ?
As2 As1 Ba1 105.86(4) . 2 ?
Ba1 As1 Ba1 7.95(6) . 2 ?
As1 As2 As1 83.12(3) . 9 ?
As1 As2 As1 83.12(3) . 5 ?
As1 As2 As1 83.12(3) 9 5 ?
As1 As2 Ba1 124.96(4) . 26 ?
As1 As2 Ba1 132.38(2) 9 26 ?
As1 As2 Ba1 132.38(2) 5 26 ?
As1 As2 Ba1 132.38(2) . 28 ?
As1 As2 Ba1 132.38(2) 9 28 ?
As1 As2 Ba1 124.96(4) 5 28 ?
Ba1 As2 Ba1 8.74(7) 26 28 ?
As1 As2 Ba1 132.38(2) . 27 ?
As1 As2 Ba1 124.96(4) 9 27 ?
As1 As2 Ba1 132.38(2) 5 27 ?
Ba1 As2 Ba1 8.74(7) 26 27 ?
Ba1 As2 Ba1 8.74(7) 28 27 ?

_refine_diff_density_max         1.266
_refine_diff_density_min         -0.524
_refine_diff_density_rms         0.166

_shelx_res_file                  
;
TITL 103 in I-43m
    shelx.res
    created by SHELXL-2018/3 at 15:38:30 on 16-Jul-2020
CELL 0.71073  10.296700  10.296700  10.296700  90.000000  90.000000  90.000000
ZERR   2      0.000200   0.000200   0.000200   0.000000   0.000000   0.000000
LATT -2
SYMM -x,-y,z
SYMM -x,y,-z
SYMM x,-y,-z
SYMM z,x,y
SYMM z,-x,-y
SYMM -z,-x,y
SYMM -z,x,-y
SYMM y,z,x
SYMM -y,z,-x
SYMM y,-z,-x
SYMM -y,-z,x
SYMM y,x,z
SYMM -y,-x,z
SYMM y,-x,-z
SYMM -y,x,-z
SYMM x,z,y
SYMM -x,z,-y
SYMM -x,-z,y
SYMM x,-z,-y
SYMM z,y,x
SYMM z,-y,-x
SYMM -z,y,-x
SYMM -z,-y,x
SFAC Ge As Ba
UNIT  16 28 2
L.S.   10
FMAP   2
TWIN
TEMP -170
ACTA
SIZE 0.059 0.111 0.119
EADP AS2 GE2
EXYZ AS2 GE2
PLAN   20
WGHT    0.000000    7.859700
BASF   0.44959
FVAR       0.06167
BA1   3    0.019873    0.019873    0.019873    10.04167    0.03396    0.03396 =
         0.03396   -0.00891   -0.00891   -0.00891
GE1   1    0.250000    0.500000    0.000000    10.25000    0.00537    0.00345 =
         0.00345    0.00000    0.00000    0.00000
GE2   1    0.281121    0.281121    0.281121    10.08333    0.00593    0.00593 =
         0.00593    0.00172    0.00172    0.00172
AS1   2    0.115136    0.115136    0.342840    10.50000    0.00481    0.00481 =
         0.00413    0.00043    0.00043    0.00028
AS2   2    0.281121    0.281121    0.281121    10.08333    0.00593    0.00593 =
         0.00593    0.00172    0.00172    0.00172

HKLF  4




REM  103 in I-43m
REM wR2 = 0.0346, GooF = S = 1.351, Restrained GooF = 1.351 for all data
REM R1 = 0.0119 for 542 Fo > 4sig(Fo) and 0.0121 for all 547 data
REM 16 parameters refined using 0 restraints

END

WGHT      0.0000      7.8585

REM Highest difference peak  1.266,  deepest hole -0.524,  1-sigma level  0.166
Q1    1   0.0599  0.0000  0.0000  10.25000  0.05    1.27
Q2    1   0.0538  0.0538  0.0538  10.16667  0.05    1.09
Q3    1  -0.0591  0.0591  0.0591  10.16667  0.05    0.84
Q4    1   0.1107  0.1107 -0.0672  10.50000  0.05    0.67
Q5    1   0.1145  0.0328  0.1145  10.50000  0.05    0.61
Q6    1  -0.0738  0.0738  0.1331  10.50000  0.05    0.55
Q7    1   0.1664  0.0000  0.0000  10.25000  0.05    0.51
Q8    1   0.1172  0.0596 -0.0128  11.00000  0.05    0.50
Q9    1   0.1209  0.1209  0.1209  10.16667  0.05    0.47
Q10   1   0.0537 -0.0537  0.2336  10.50000  0.05    0.47
Q11   1   0.0497  0.1595  0.1595  10.50000  0.05    0.42
Q12   1   0.1568  0.0586  0.0586  10.50000  0.05    0.42
Q13   1   0.0573  0.0573  0.3180  10.50000  0.05    0.41
Q14   1   0.0721  0.0721  0.1780  10.50000  0.05    0.40
Q15   1   0.4280  0.3999  0.3047  11.00000  0.05    0.38
Q16   1   0.0401  0.0401  0.2425  10.50000  0.05    0.38
Q17   1   0.1889 -0.0218  0.0849  11.00000  0.05    0.35
Q18   1   0.0241  0.0899  0.1841  11.00000  0.05    0.34
Q19   1   0.2400  0.0224  0.2400  10.50000  0.05    0.33
Q20   1   0.0758  0.1025  0.1771  11.00000  0.05    0.33
;
_shelx_res_checksum              60324

# start Validation Reply Form
_vrf_PLAT919_shelx               
;
PROBLEM: Reflection # Likely Affected by the Beamstop ...          1 Check 
RESPONSE: Concealed by beam stop.
;
_vrf_STRVA01_shelx               
;
PROBLEM: Flack test results are ambiguous.
RESPONSE: inversion twin with aprox. 50:50 ratio, absolute configuration
 not of interest.
;
_vrf_PLAT094_shelx               
;
PROBLEM: Ratio of Maximum / Minimum Residual Density ....       2.42 Report
RESPONSE: Result of Barium disorder.
;
_vrf_PLAT911_shelx               
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L=    0.600          2 Report
RESPONSE: Concealed by beam stop.
;
_vrf_PLAT934_shelx               
;
PROBLEM: Number of (Iobs-Icalc)/Sigma(W) > 10 Outliers ..          1 Check 
RESPONSE: Due to the formation of ice during measurement.
;
_vrf_PLAT971_shelx               
;
PROBLEM: Check Calcd Resid. Dens.  0.52A   From Ba1             1.53 eA-3  
RESPONSE: Result of Barium disorder.
;
# end Validation Reply Form
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_shelx_CCDC4
_database_code_depnum_ccdc_archive 'CCDC 2017127'
loop_
_audit_author_name
_audit_author_address
'Valentin Weippert'
;LMU Munich
Germany
;
_audit_update_record             
;
2020-07-17 deposited with the CCDC.	2020-12-21 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'As14 Ba Ge8'
_chemical_formula_sum            'As14 Ba Ge8'
_chemical_formula_weight         1766.94

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
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'
Ba Ba -0.3244 2.2819 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      cubic
_space_group_IT_number           217
_space_group_name_H-M_alt        'I -4 3 m'
_space_group_name_Hall           'I -4 2 3'

_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'-x, y, -z'
'x, -y, -z'
'z, x, y'
'z, -x, -y'
'-z, -x, y'
'-z, x, -y'
'y, z, x'
'-y, z, -x'
'y, -z, -x'
'-y, -z, x'
'y, x, z'
'-y, -x, z'
'y, -x, -z'
'-y, x, -z'
'x, z, y'
'-x, z, -y'
'-x, -z, y'
'x, -z, -y'
'z, y, x'
'z, -y, -x'
'-z, y, -x'
'-z, -y, x'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'-x+1/2, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'z+1/2, x+1/2, y+1/2'
'z+1/2, -x+1/2, -y+1/2'
'-z+1/2, -x+1/2, y+1/2'
'-z+1/2, x+1/2, -y+1/2'
'y+1/2, z+1/2, x+1/2'
'-y+1/2, z+1/2, -x+1/2'
'y+1/2, -z+1/2, -x+1/2'
'-y+1/2, -z+1/2, x+1/2'
'y+1/2, x+1/2, z+1/2'
'-y+1/2, -x+1/2, z+1/2'
'y+1/2, -x+1/2, -z+1/2'
'-y+1/2, x+1/2, -z+1/2'
'x+1/2, z+1/2, y+1/2'
'-x+1/2, z+1/2, -y+1/2'
'-x+1/2, -z+1/2, y+1/2'
'x+1/2, -z+1/2, -y+1/2'
'z+1/2, y+1/2, x+1/2'
'z+1/2, -y+1/2, -x+1/2'
'-z+1/2, y+1/2, -x+1/2'
'-z+1/2, -y+1/2, x+1/2'

_cell_length_a                   10.3018(2)
_cell_length_b                   10.3018(2)
_cell_length_c                   10.3018(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1093.30(6)
_cell_formula_units_Z            2
_cell_measurement_temperature    143(2)
_cell_measurement_reflns_used    9914
_cell_measurement_theta_min      5.592
_cell_measurement_theta_max      90.793

_exptl_crystal_description       block
_exptl_crystal_colour            black
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    5.367
_exptl_crystal_F_000             1548
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.119
_exptl_crystal_size_mid          0.111
_exptl_crystal_size_min          0.059
_exptl_absorpt_coefficient_mu    33.617
_shelx_estimated_absorpt_T_min   0.108
_shelx_estimated_absorpt_T_max   0.242
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.1886
_exptl_absorpt_correction_T_max  0.3555
_exptl_absorpt_process_details   
;
Additional spherical absorption correction
 applied with mu*r =  0.8000  (Bruker, 2016)
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      143(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       'combined φ ω scan'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            17366
_diffrn_reflns_av_unetI/netI     0.0100
_diffrn_reflns_av_R_equivalents  0.0358
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         2.796
_diffrn_reflns_theta_max         36.974
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measured_fraction_theta_full 0.968
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_Laue_measured_fraction_full 0.968
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_point_group_measured_fraction_full 0.962
_reflns_number_total             542
_reflns_number_gt                538
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.771
_reflns_Friedel_fraction_max     0.983
_reflns_Friedel_fraction_full    0.955

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;

_computing_data_collection       'APEX3 (Bruker, 2016)'
_computing_cell_refinement       'APEX3 (Bruker, 2016)'
_computing_data_reduction        'APEX3 (Bruker, 2016)'
_computing_structure_solution    'SUPERFLIP (Palatinus & Chapuis, 2007)'
_computing_structure_refinement  'SHELXL (Sheldrick, 2015)'
_computing_molecular_graphics    'DIAMOND 3 (Brandenburg, 2014)'
_computing_publication_material  
;
PLATON V. 91007 (Spek, 2009)
STRUCTURETIDY (Gelato, Parthé, 1987)
;
_refine_special_details          
;
 Refined as a 2-component inversion twin.
 Ge2:As2 ratio fixed to 50:50 based on elemental analysis.
 Ba1 refined as a split position, changing the Wyckoff position
 from 2a to 8c. Consequently the occupancy of the Ba1 split 
 position is fixed to 0.25.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+6.3372P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   .
_refine_ls_hydrogen_treatment    undef
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.41(14)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         542
_refine_ls_number_parameters     16
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0119
_refine_ls_R_factor_gt           0.0117
_refine_ls_wR_factor_ref         0.0364
_refine_ls_wR_factor_gt          0.0364
_refine_ls_goodness_of_fit_ref   1.468
_refine_ls_restrained_S_all      1.468
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

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
Ba1 Ba 0.01979(16) 0.01979(16) 0.01979(16) 0.0388(11) Uani 0.25 6 d S T P . .
Ge1 Ge 0.250000 0.500000 0.000000 0.00598(11) Uani 1 4 d S T P . .
Ge2 Ge 0.28107(5) 0.28107(5) 0.28107(5) 0.00799(14) Uani 0.5 6 d S T P . .
As1 As 0.11513(3) 0.11513(3) 0.34287(5) 0.00649(9) Uani 1 2 d S T P . .
As2 As 0.28107(5) 0.28107(5) 0.28107(5) 0.00799(14) Uani 0.5 6 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
Ba1 0.0388(11) 0.0388(11) 0.0388(11) -0.0092(5) -0.0092(5) -0.0092(5)
Ge1 0.0075(2) 0.00524(15) 0.00524(15) 0.000 0.000 0.000
Ge2 0.00799(14) 0.00799(14) 0.00799(14) 0.00174(16) 0.00174(16) 0.00174(16)
As1 0.00677(12) 0.00677(12) 0.00593(17) 0.00044(10) 0.00044(10) 0.00032(13)
As2 0.00799(14) 0.00799(14) 0.00799(14) 0.00174(16) 0.00174(16) 0.00174(16)

_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ba1 Ba1 0.577(5) 4 ?
Ba1 Ba1 0.577(5) 3 ?
Ba1 Ba1 0.577(5) 2 ?
Ba1 As1 3.607(2) . ?
Ba1 As1 3.607(2) 9 ?
Ba1 As1 3.607(2) 5 ?
Ba1 Ge2 3.8032(11) 26_554 ?
Ba1 Ge2 3.8032(11) 28_455 ?
Ba1 Ge2 3.8032(11) 27_545 ?
Ba1 As1 3.8654(5) 10 ?
Ba1 As1 3.8654(5) 6 ?
Ba1 As1 3.8654(5) 2 ?
Ge1 As1 2.4408(3) 27 ?
Ge1 As1 2.4408(3) 9 ?
Ge1 As1 2.4408(3) 26_554 ?
Ge1 As1 2.4408(3) 11_565 ?
As1 As2 2.5000(8) . ?

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
_geom_angle_publ_flag
Ba1 Ba1 Ba1 60.001(1) 4 3 ?
Ba1 Ba1 Ba1 60.001(1) 4 2 ?
Ba1 Ba1 Ba1 60.001(1) 3 2 ?
Ba1 Ba1 As1 147.686(9) 4 . ?
Ba1 Ba1 As1 147.686(9) 3 . ?
Ba1 Ba1 As1 112.65(3) 2 . ?
Ba1 Ba1 As1 147.685(9) 4 9 ?
Ba1 Ba1 As1 112.65(3) 3 9 ?
Ba1 Ba1 As1 147.685(9) 2 9 ?
As1 Ba1 As1 54.77(4) . 9 ?
Ba1 Ba1 As1 112.65(3) 4 5 ?
Ba1 Ba1 As1 147.685(9) 3 5 ?
Ba1 Ba1 As1 147.685(9) 2 5 ?
As1 Ba1 As1 54.77(4) . 5 ?
As1 Ba1 As1 54.77(4) 9 5 ?
Ba1 Ba1 Ge2 85.65(4) 4 26_554 ?
Ba1 Ba1 Ge2 85.65(4) 3 26_554 ?
Ba1 Ba1 Ge2 139.71(4) 2 26_554 ?
As1 Ba1 Ge2 107.63(7) . 26_554 ?
As1 Ba1 Ge2 62.06(3) 9 26_554 ?
As1 Ba1 Ge2 62.06(3) 5 26_554 ?
Ba1 Ba1 Ge2 139.71(4) 4 28_455 ?
Ba1 Ba1 Ge2 85.65(4) 3 28_455 ?
Ba1 Ba1 Ge2 85.65(4) 2 28_455 ?
As1 Ba1 Ge2 62.06(3) . 28_455 ?
As1 Ba1 Ge2 62.06(3) 9 28_455 ?
As1 Ba1 Ge2 107.63(7) 5 28_455 ?
Ge2 Ba1 Ge2 113.99(3) 26_554 28_455 ?
Ba1 Ba1 Ge2 85.65(4) 4 27_545 ?
Ba1 Ba1 Ge2 139.71(4) 3 27_545 ?
Ba1 Ba1 Ge2 85.65(4) 2 27_545 ?
As1 Ba1 Ge2 62.06(3) . 27_545 ?
As1 Ba1 Ge2 107.63(7) 9 27_545 ?
As1 Ba1 Ge2 62.06(3) 5 27_545 ?
Ge2 Ba1 Ge2 113.99(3) 26_554 27_545 ?
Ge2 Ba1 Ge2 113.99(3) 28_455 27_545 ?
Ba1 Ba1 As1 110.77(4) 4 10 ?
Ba1 Ba1 As1 59.43(4) 3 10 ?
Ba1 Ba1 As1 110.77(4) 2 10 ?
As1 Ba1 As1 101.26(5) . 10 ?
As1 Ba1 As1 53.22(2) 9 10 ?
As1 Ba1 As1 101.26(5) 5 10 ?
Ge2 Ba1 As1 59.801(8) 26_554 10 ?
Ge2 Ba1 As1 59.801(8) 28_455 10 ?
Ge2 Ba1 As1 160.85(8) 27_545 10 ?
Ba1 Ba1 As1 59.43(4) 4 6 ?
Ba1 Ba1 As1 110.77(4) 3 6 ?
Ba1 Ba1 As1 110.77(4) 2 6 ?
As1 Ba1 As1 101.26(5) . 6 ?
As1 Ba1 As1 101.26(5) 9 6 ?
As1 Ba1 As1 53.22(2) 5 6 ?
Ge2 Ba1 As1 59.801(8) 26_554 6 ?
Ge2 Ba1 As1 160.85(8) 28_455 6 ?
Ge2 Ba1 As1 59.801(8) 27_545 6 ?
As1 Ba1 As1 119.336(12) 10 6 ?
Ba1 Ba1 As1 110.77(4) 4 2 ?
Ba1 Ba1 As1 110.77(4) 3 2 ?
Ba1 Ba1 As1 59.43(4) 2 2 ?
As1 Ba1 As1 53.22(2) . 2 ?
As1 Ba1 As1 101.26(5) 9 2 ?
As1 Ba1 As1 101.26(5) 5 2 ?
Ge2 Ba1 As1 160.85(8) 26_554 2 ?
Ge2 Ba1 As1 59.801(8) 28_455 2 ?
Ge2 Ba1 As1 59.801(8) 27_545 2 ?
As1 Ba1 As1 119.336(12) 10 2 ?
As1 Ba1 As1 119.336(12) 6 2 ?
As1 Ge1 As1 108.908(11) 27 9 ?
As1 Ge1 As1 110.60(2) 27 26_554 ?
As1 Ge1 As1 108.908(11) 9 26_554 ?
As1 Ge1 As1 108.908(11) 27 11_565 ?
As1 Ge1 As1 110.60(2) 9 11_565 ?
As1 Ge1 As1 108.908(11) 26_554 11_565 ?
Ge1 As1 Ge1 96.511(16) 5 26 ?
Ge1 As1 As2 96.425(18) 5 . ?
Ge1 As1 As2 96.425(18) 26 . ?
Ge1 As1 Ba1 129.400(11) 5 . ?
Ge1 As1 Ba1 129.400(11) 26 . ?
As2 As1 Ba1 97.90(3) . . ?
Ge1 As1 Ba1 126.942(18) 5 2 ?
Ge1 As1 Ba1 126.942(18) 26 2 ?
As2 As1 Ba1 105.81(5) . 2 ?
Ba1 As1 Ba1 7.91(7) . 2 ?
As1 As2 As1 83.15(3) . 5 ?
As1 As2 As1 83.15(3) . 9 ?
As1 As2 As1 83.15(3) 5 9 ?
As1 As2 Ba1 132.35(3) . 27 ?
As1 As2 Ba1 132.35(3) 5 27 ?
As1 As2 Ba1 124.96(5) 9 27 ?
As1 As2 Ba1 132.35(3) . 28 ?
As1 As2 Ba1 124.96(5) 5 28 ?
As1 As2 Ba1 132.35(3) 9 28 ?
Ba1 As2 Ba1 8.70(7) 27 28 ?
As1 As2 Ba1 124.96(5) . 26 ?
As1 As2 Ba1 132.35(3) 5 26 ?
As1 As2 Ba1 132.35(3) 9 26 ?
Ba1 As2 Ba1 8.70(7) 27 26 ?
Ba1 As2 Ba1 8.70(7) 28 26 ?

_refine_diff_density_max         0.840
_refine_diff_density_min         -0.688
_refine_diff_density_rms         0.207

_shelx_res_file                  
;
TITL 143 in I-43m
    shelx.res
    created by SHELXL-2018/3 at 15:35:23 on 16-Jul-2020
CELL 0.71073  10.301800  10.301800  10.301800  90.000000  90.000000  90.000000
ZERR   2      0.000200   0.000200   0.000200   0.000000   0.000000   0.000000
LATT -2
SYMM -x,-y,z
SYMM -x,y,-z
SYMM x,-y,-z
SYMM z,x,y
SYMM z,-x,-y
SYMM -z,-x,y
SYMM -z,x,-y
SYMM y,z,x
SYMM -y,z,-x
SYMM y,-z,-x
SYMM -y,-z,x
SYMM y,x,z
SYMM -y,-x,z
SYMM y,-x,-z
SYMM -y,x,-z
SYMM x,z,y
SYMM -x,z,-y
SYMM -x,-z,y
SYMM x,-z,-y
SYMM z,y,x
SYMM z,-y,-x
SYMM -z,y,-x
SYMM -z,-y,x
SFAC Ge As Ba
UNIT  16 28 2
L.S.   10
FMAP   2
TWIN
TEMP -130
ACTA
SIZE 0.059 0.111 0.119
EADP AS2 GE2
EXYZ AS2 GE2
PLAN   20
WGHT    0.000000    6.337200
BASF   0.40933
FVAR       0.08064
BA1   3    0.019790    0.019790    0.019790    10.04167    0.03884    0.03884 =
         0.03884   -0.00921   -0.00921   -0.00921
GE1   1    0.250000    0.500000    0.000000    10.25000    0.00747    0.00524 =
         0.00524    0.00000    0.00000    0.00000
GE2   1    0.281073    0.281073    0.281073    10.08333    0.00799    0.00799 =
         0.00799    0.00174    0.00174    0.00174
AS1   2    0.115130    0.115130    0.342870    10.50000    0.00677    0.00677 =
         0.00593    0.00044    0.00044    0.00032
AS2   2    0.281073    0.281073    0.281073    10.08333    0.00799    0.00799 =
         0.00799    0.00174    0.00174    0.00174

HKLF  4




REM  143 in I-43m
REM wR2 = 0.0364, GooF = S = 1.468, Restrained GooF = 1.468 for all data
REM R1 = 0.0117 for 538 Fo > 4sig(Fo) and 0.0119 for all 542 data
REM 16 parameters refined using 0 restraints

END

WGHT      0.0000      6.3370

REM Highest difference peak  0.840,  deepest hole -0.688,  1-sigma level  0.207
Q1    1   0.0596  0.0000  0.0000  10.25000  0.05    0.84
Q2    1   0.0000  0.0000  0.1475  10.25000  0.05    0.78
Q3    1  -0.0577  0.2204  0.0577  10.50000  0.05    0.75
Q4    1   0.1819 -0.0580  0.0580  10.50000  0.05    0.74
Q5    1   0.1342 -0.0594  0.1018  11.00000  0.05    0.70
Q6    1  -0.0630  0.1519  0.0630  10.50000  0.05    0.68
Q7    1  -0.0571  0.0849  0.1828  11.00000  0.05    0.68
Q8    1  -0.0603  0.0603  0.0603  10.16667  0.05    0.61
Q9    1   0.1431 -0.0304  0.0304  10.50000  0.05    0.59
Q10   1   0.0000  0.0000  0.4824  10.25000  0.05    0.55
Q11   1   0.1183  0.0318  0.1183  10.50000  0.05    0.53
Q12   1   0.1223  0.1223  0.1223  10.16667  0.05    0.49
Q13   1   0.0508  0.0508  0.0508  10.16667  0.05    0.49
Q14   1   0.3700  0.3700  0.1051  10.50000  0.05    0.49
Q15   1   0.1860  0.2119  0.3165  11.00000  0.05    0.48
Q16   1   0.0115  0.2409  0.2409  10.50000  0.05    0.45
Q17   1   0.2210  0.1624  0.3002  11.00000  0.05    0.44
Q18   1   0.0528  0.0528  0.3147  10.50000  0.05    0.42
Q19   1   0.1680  0.0542  0.0542  10.50000  0.05    0.40
Q20   1   0.2181  0.2181  0.4846  10.50000  0.05    0.39
;
_shelx_res_checksum              71252

# start Validation Reply Form
_vrf_PLAT919_shelx               
;
PROBLEM: Reflection # Likely Affected by the Beamstop ...          1 Check 
RESPONSE: Concealed by beam stop.
;
_vrf_STRVA01_shelx               
;
PROBLEM: Flack test results are ambiguous.
RESPONSE: Inversion twin with aprox. 50:50 ratio, absolute configuration
 not of interest.
;
_vrf_PLAT911_shelx               
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L=    0.600          4 Report
RESPONSE: Concealed by beam stop.
;
_vrf_PLAT934_shelx               
;
PROBLEM: Number of (Iobs-Icalc)/Sigma(W) > 10 Outliers ..          1 Check 
RESPONSE: Due to the formation of ice during measurement.
;
# end Validation Reply Form
