# Electronic Supplementary Material (ESI) for RSC Advances.
# This journal is © The Royal Society of Chemistry 2016

####################################################################### 
# 
# 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_3096
_database_code_depnum_ccdc_archive 'CCDC 1473572'
_audit_update_record             
;
2016-04-26 deposited with the CCDC.
2016-07-25 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'Ga2.40 Ge1.60 K2.40 Se8'
_chemical_formula_weight         1009.2

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'
Se Se -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ga Ga 0.2307 1.6083 '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'

_space_group_crystal_system      tetragonal
_space_group_IT_number           140
_space_group_name_H-M_alt        'I 4/m c m'
_space_group_name_Hall           '-I 4 2c'

_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'
'-y, x, z'
'x, -y, -z+1/2'
'-x, -y, z'
'-y, -x, -z+1/2'
'y, x, -z+1/2'
'y, -x, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z+1/2'
'-y+1/2, x+1/2, z+1/2'
'x+1/2, -y+1/2, -z+1'
'-x+1/2, -y+1/2, z+1/2'
'-y+1/2, -x+1/2, -z+1'
'y+1/2, x+1/2, -z+1'
'y+1/2, -x+1/2, z+1/2'
'-x+1/2, y+1/2, -z+1'
'-x, -y, -z'
'y, -x, -z'
'-x, y, z-1/2'
'x, y, -z'
'y, x, z-1/2'
'-y, -x, z-1/2'
'-y, x, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z+1/2'
'y+1/2, -x+1/2, -z+1/2'
'-x+1/2, y+1/2, z'
'x+1/2, y+1/2, -z+1/2'
'y+1/2, x+1/2, z'
'-y+1/2, -x+1/2, z'
'-y+1/2, x+1/2, -z+1/2'
'x+1/2, -y+1/2, z'

_cell_length_a                   8.1208(8)
_cell_length_b                   8.1208(8)
_cell_length_c                   6.2080(8)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     409.40(9)
_cell_formula_units_Z            1
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    25
_cell_measurement_theta_min      7.5
_cell_measurement_theta_max      15

_exptl_crystal_description       bar
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    4.093
_exptl_crystal_F_000             736
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.039
_exptl_crystal_size_mid          0.008
_exptl_crystal_size_min          0.006
_exptl_absorpt_coefficient_mu    25.170
_shelx_estimated_absorpt_T_min   0.295
_shelx_estimated_absorpt_T_max   0.789
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.679
_exptl_absorpt_correction_T_max  0.780
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            377
_diffrn_reflns_av_unetI/netI     0.0149
_diffrn_reflns_av_R_equivalents  0.0169
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_limit_l_max       5
_diffrn_reflns_theta_min         3.548
_diffrn_reflns_theta_max         24.728
_diffrn_reflns_theta_full        24.728
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             111
_reflns_number_gt                106
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_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.
;

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SMART'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0195P)²+8.8948P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   .
_refine_ls_hydrogen_treatment    undef
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         111
_refine_ls_number_parameters     9
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0242
_refine_ls_R_factor_gt           0.0235
_refine_ls_wR_factor_ref         0.0559
_refine_ls_wR_factor_gt          0.0554
_refine_ls_goodness_of_fit_ref   1.180
_refine_ls_restrained_S_all      1.180
_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
Se Se 0.65828(10) 0.15828(10) 0.0000 0.0173(4) Uani 1 4 d S T P . .
Ga Ga 0.5000 0.0000 0.2500 0.0121(5) Uani 0.6 8 d S T P . .
Ge Ge 0.5000 0.0000 0.2500 0.0121(5) Uani 0.4 8 d S T P . .
K1 K 1.0000 0.0000 0.2500 0.097(5) Uani 0.6 8 d S T P . .


_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
Se Ge 2.3901(9) 17_655 ?
Se Ga 2.3901(9) 17_655 ?
Se Ga 2.3901(9) . ?
Se K1 3.4295(4) 25_655 ?
Se K1 3.4295(4) . ?
Se K1 3.4295(4) 9_454 ?
Se K1 3.4295(4) 17_755 ?
Ga Se 2.3902(9) 17_655 ?
Ga Se 2.3902(9) 26 ?
Ga Se 2.3902(9) 10_545 ?
K1 K1 3.1040(4) 17_756 ?
K1 K1 3.1040(4) 17_755 ?
K1 Se 3.4295(4) 10_645 ?
K1 Se 3.4295(4) 2_645 ?
K1 Se 3.4295(4) 25_655 ?
K1 Se 3.4295(4) 26 ?
K1 Se 3.4295(4) 18_665 ?
K1 Se 3.4295(4) 9_545 ?
K1 Se 3.4295(4) 17_755 ?

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
Ge Se Ga 0.0 17_655 17_655 ?
Ge Se Ga 81.0 17_655 . ?
Ga Se Ga 80.98(4) 17_655 . ?
Ge Se K1 121.833(16) 17_655 25_655 ?
Ga Se K1 121.833(16) 17_655 25_655 ?
Ga Se K1 86.546(7) . 25_655 ?
Ge Se K1 121.833(16) 17_655 . ?
Ga Se K1 121.833(16) 17_655 . ?
Ga Se K1 86.546(7) . . ?
K1 Se K1 113.686(18) 25_655 . ?
Ge Se K1 86.546(7) 17_655 9_454 ?
Ga Se K1 86.546(7) 17_655 9_454 ?
Ga Se K1 121.833(16) . 9_454 ?
K1 Se K1 53.813(10) 25_655 9_454 ?
K1 Se K1 144.22(3) . 9_454 ?
Ge Se K1 86.546(7) 17_655 17_755 ?
Ga Se K1 86.546(7) 17_655 17_755 ?
Ga Se K1 121.833(16) . 17_755 ?
K1 Se K1 144.22(3) 25_655 17_755 ?
K1 Se K1 53.813(10) . 17_755 ?
K1 Se K1 113.686(18) 9_454 17_755 ?
Se Ga Se 99.02(4) . 17_655 ?
Se Ga Se 114.937(19) . 26 ?
Se Ga Se 114.937(19) 17_655 26 ?
Se Ga Se 114.937(19) . 10_545 ?
Se Ga Se 114.937(19) 17_655 10_545 ?
Se Ga Se 99.02(4) 26 10_545 ?
K1 K1 K1 180.0 17_756 17_755 ?
K1 K1 Se 63.093(5) 17_756 10_645 ?
K1 K1 Se 116.907(5) 17_755 10_645 ?
K1 K1 Se 116.907(5) 17_756 2_645 ?
K1 K1 Se 63.093(5) 17_755 2_645 ?
Se K1 Se 144.23(3) 10_645 2_645 ?
K1 K1 Se 63.093(5) 17_756 25_655 ?
K1 K1 Se 116.907(5) 17_755 25_655 ?
Se K1 Se 78.183(4) 10_645 25_655 ?
Se K1 Se 135.98(3) 2_645 25_655 ?
K1 K1 Se 63.093(5) 17_756 26 ?
K1 K1 Se 116.907(5) 17_755 26 ?
Se K1 Se 126.187(10) 10_645 26 ?
Se K1 Se 66.313(18) 2_645 26 ?
Se K1 Se 78.183(4) 25_655 26 ?
K1 K1 Se 116.907(5) 17_756 18_665 ?
K1 K1 Se 63.093(5) 17_755 18_665 ?
Se K1 Se 66.313(18) 10_645 18_665 ?
Se K1 Se 126.187(10) 2_645 18_665 ?
Se K1 Se 71.97(3) 25_655 18_665 ?
Se K1 Se 144.23(3) 26 18_665 ?
K1 K1 Se 63.093(5) 17_756 9_545 ?
K1 K1 Se 116.907(5) 17_755 9_545 ?
Se K1 Se 78.183(4) 10_645 9_545 ?
Se K1 Se 71.97(3) 2_645 9_545 ?
Se K1 Se 126.187(10) 25_655 9_545 ?
Se K1 Se 78.183(4) 26 9_545 ?
Se K1 Se 135.98(3) 18_665 9_545 ?
K1 K1 Se 116.907(5) 17_756 17_755 ?
K1 K1 Se 63.093(5) 17_755 17_755 ?
Se K1 Se 71.97(3) 10_645 17_755 ?
Se K1 Se 78.183(4) 2_645 17_755 ?
Se K1 Se 144.23(4) 25_655 17_755 ?
Se K1 Se 135.98(3) 26 17_755 ?
Se K1 Se 78.183(4) 18_665 17_755 ?
Se K1 Se 66.313(18) 9_545 17_755 ?
K1 K1 Se 116.907(5) 17_756 . ?
K1 K1 Se 63.093(5) 17_755 . ?
Se K1 Se 135.98(3) 10_645 . ?
Se K1 Se 78.182(4) 2_645 . ?
Se K1 Se 66.313(18) 25_655 . ?
Se K1 Se 71.97(3) 26 . ?
Se K1 Se 78.183(4) 18_665 . ?
Se K1 Se 144.22(3) 9_545 . ?
Se K1 Se 126.187(10) 17_755 . ?

_refine_diff_density_max         1.391
_refine_diff_density_min         -1.104
_refine_diff_density_rms         0.180



####################################################################### 
# 
# 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_121213a
_database_code_depnum_ccdc_archive 'CCDC 1473573'
_audit_update_record             
;
2016-04-26 deposited with the CCDC.
2016-07-25 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'Ga2.40 K2.40 Se8 Si1.60'
_chemical_formula_weight         932.31

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'
Ga Ga 0.2307 1.6083 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Se Se -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      tetragonal
_space_group_IT_number           140
_space_group_name_H-M_alt        'I 4/m c m'
_space_group_name_Hall           '-I 4 2c'

_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'
'-y, x, z'
'y, -x, z'
'-x, y, -z+1/2'
'x, -y, -z+1/2'
'y, x, -z+1/2'
'-y, -x, -z+1/2'
'x+1/2, y+1/2, z+1/2'
'-x+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'
'-x+1/2, y+1/2, -z+1'
'x+1/2, -y+1/2, -z+1'
'y+1/2, x+1/2, -z+1'
'-y+1/2, -x+1/2, -z+1'
'-x, -y, -z'
'x, y, -z'
'y, -x, -z'
'-y, x, -z'
'x, -y, z-1/2'
'-x, y, z-1/2'
'-y, -x, z-1/2'
'y, x, z-1/2'
'-x+1/2, -y+1/2, -z+1/2'
'x+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'
'x+1/2, -y+1/2, z'
'-x+1/2, y+1/2, z'
'-y+1/2, -x+1/2, z'
'y+1/2, x+1/2, z'

_cell_length_a                   8.1999(4)
_cell_length_b                   8.1999(4)
_cell_length_c                   6.1460(7)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     413.25(6)
_cell_formula_units_Z            1
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    25
_cell_measurement_theta_min      7.5
_cell_measurement_theta_max      15

_exptl_crystal_description       bar
_exptl_crystal_colour            brown
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    3.746
_exptl_crystal_F_000             298
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.029
_exptl_crystal_size_mid          0.007
_exptl_crystal_size_min          0.005
_exptl_absorpt_coefficient_mu    22.199
_shelx_estimated_absorpt_T_min   0.672
_shelx_estimated_absorpt_T_max   0.929
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.883
_exptl_absorpt_correction_T_max  0.928
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            341
_diffrn_reflns_av_unetI/netI     0.0524
_diffrn_reflns_av_R_equivalents  0.0743
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       3
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_limit_l_max       3
_diffrn_reflns_theta_min         3.514
_diffrn_reflns_theta_max         24.631
_diffrn_reflns_theta_full        24.631
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             111
_reflns_number_gt                102
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_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.
;

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SMART'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0779P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   .
_refine_ls_hydrogen_treatment    undef
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         111
_refine_ls_number_parameters     9
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0526
_refine_ls_R_factor_gt           0.0501
_refine_ls_wR_factor_ref         0.1364
_refine_ls_wR_factor_gt          0.1326
_refine_ls_goodness_of_fit_ref   1.145
_refine_ls_restrained_S_all      1.145
_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
Se Se 0.34508(15) 0.15492(15) 0.0000 0.0375(10) Uani 1 4 d S T P . .
Ga Ga 0.5000 0.0000 0.2500 0.0252(11) Uani 0.58 8 d S T P . .
Si Si 0.5000 0.0000 0.2500 0.0252(11) Uani 0.4 8 d S T P . .
K K 0.0000 0.0000 0.2500 0.130(7) Uani 0.6 8 d S T P . .


_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
Se Si 2.3639(13) 17_655 ?
Se Ga 2.3639(13) . ?
Se Ga 2.3639(13) 17_655 ?
Se K 3.4614(6) 25 ?
Se K 3.4614(6) 17 ?
Se K 3.4614(6) . ?
Se K 3.4614(6) 9_554 ?
Ga Se 2.3639(13) 27 ?
Ga Se 2.3639(13) 17_655 ?
Ga Se 2.3639(13) 11_545 ?
K K 3.0730(4) 17_556 ?
K K 3.0730(4) 17 ?
K Se 3.4614(6) 17 ?
K Se 3.4614(6) 25 ?
K Se 3.4614(6) 19 ?
K Se 3.4614(6) 11_545 ?
K Se 3.4614(6) 9_445 ?
K Se 3.4614(6) 3 ?
K Se 3.4614(6) 27_455 ?

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
Si Se Ga 81.1 17_655 . ?
Si Se Ga 0.0 17_655 17_655 ?
Ga Se Ga 81.08(6) . 17_655 ?
Si Se K 122.05(2) 17_655 25 ?
Ga Se K 87.338(9) . 25 ?
Ga Se K 122.05(2) 17_655 25 ?
Si Se K 87.338(8) 17_655 17 ?
Ga Se K 122.05(2) . 17 ?
Ga Se K 87.338(8) 17_655 17 ?
K Se K 142.85(5) 25 17 ?
Si Se K 122.05(2) 17_655 . ?
Ga Se K 87.338(8) . . ?
Ga Se K 122.05(2) 17_655 . ?
K Se K 113.76(3) 25 . ?
K Se K 52.705(10) 17 . ?
Si Se K 87.338(8) 17_655 9_554 ?
Ga Se K 122.05(2) . 9_554 ?
Ga Se K 87.338(8) 17_655 9_554 ?
K Se K 52.705(10) 25 9_554 ?
K Se K 113.76(3) 17 9_554 ?
K Se K 142.85(5) . 9_554 ?
Se Ga Se 114.99(3) 27 17_655 ?
Se Ga Se 98.92(6) 27 11_545 ?
Se Ga Se 114.99(3) 17_655 11_545 ?
Se Ga Se 114.99(3) 27 . ?
Se Ga Se 98.92(6) 17_655 . ?
Se Ga Se 114.99(3) 11_545 . ?
K K K 180.0 17_556 17 ?
K K Se 116.353(5) 17_556 . ?
K K Se 63.647(5) 17 . ?
K K Se 116.353(5) 17_556 17 ?
K K Se 63.648(5) 17 17 ?
Se K Se 127.295(10) . 17 ?
K K Se 63.648(6) 17_556 25 ?
K K Se 116.353(5) 17 25 ?
Se K Se 66.24(3) . 25 ?
Se K Se 142.85(5) 17 25 ?
K K Se 116.353(5) 17_556 19 ?
K K Se 63.648(5) 17 19 ?
Se K Se 78.637(5) . 19 ?
Se K Se 78.636(4) 17 19 ?
Se K Se 136.94(5) 25 19 ?
K K Se 63.648(5) 17_556 11_545 ?
K K Se 116.353(5) 17 11_545 ?
Se K Se 70.33(4) . 11_545 ?
Se K Se 136.94(5) 17 11_545 ?
Se K Se 78.636(4) 25 11_545 ?
Se K Se 66.24(3) 19 11_545 ?
K K Se 63.648(5) 17_556 9_445 ?
K K Se 116.352(6) 17 9_445 ?
Se K Se 142.85(5) . 9_445 ?
Se K Se 66.24(3) 17 9_445 ?
Se K Se 127.295(11) 25 9_445 ?
Se K Se 70.33(4) 19 9_445 ?
Se K Se 78.636(4) 11_545 9_445 ?
K K Se 116.352(5) 17_556 3 ?
K K Se 63.648(5) 17 3 ?
Se K Se 78.635(5) . 3 ?
Se K Se 78.636(4) 17 3 ?
Se K Se 70.33(4) 25 3 ?
Se K Se 127.295(11) 19 3 ?
Se K Se 142.85(5) 11_545 3 ?
Se K Se 136.94(5) 9_445 3 ?
K K Se 63.648(5) 17_556 27_455 ?
K K Se 116.352(6) 17 27_455 ?
Se K Se 136.94(5) . 27_455 ?
Se K Se 70.33(4) 17 27_455 ?
Se K Se 78.636(4) 25 27_455 ?
Se K Se 142.85(5) 19 27_455 ?
Se K Se 127.295(11) 11_545 27_455 ?
Se K Se 78.636(4) 9_445 27_455 ?
Se K Se 66.24(3) 3 27_455 ?

_refine_diff_density_max         1.052
_refine_diff_density_min         -0.831
_refine_diff_density_rms         0.270



####################################################################### 
# 
# 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_I4-mcm_a
_database_code_depnum_ccdc_archive 'CCDC 1476383'
_audit_update_record             
;
2016-04-26 deposited with the CCDC.
2016-07-25 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'Ga2.40 Ge1.60 K2.40 S8'
_chemical_formula_weight         633.82

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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ga Ga 0.2307 1.6083 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      tetragonal
_space_group_IT_number           140
_space_group_name_H-M_alt        'I 4/m c m'
_space_group_name_Hall           '-I 4 2c'

_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'
'-y, x, z'
'y, -x, z'
'-x, y, -z+1/2'
'x, -y, -z+1/2'
'y, x, -z+1/2'
'-y, -x, -z+1/2'
'x+1/2, y+1/2, z+1/2'
'-x+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'
'-x+1/2, y+1/2, -z+1'
'x+1/2, -y+1/2, -z+1'
'y+1/2, x+1/2, -z+1'
'-y+1/2, -x+1/2, -z+1'
'-x, -y, -z'
'x, y, -z'
'y, -x, -z'
'-y, x, -z'
'x, -y, z-1/2'
'-x, y, z-1/2'
'-y, -x, z-1/2'
'y, x, z-1/2'
'-x+1/2, -y+1/2, -z+1/2'
'x+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'
'x+1/2, -y+1/2, z'
'-x+1/2, y+1/2, z'
'-y+1/2, -x+1/2, z'
'y+1/2, x+1/2, z'

_cell_length_a                   7.8824(9)
_cell_length_b                   7.8824(9)
_cell_length_c                   5.9557(7)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     370.04(10)
_cell_formula_units_Z            1
_cell_measurement_temperature    273(2)
_cell_measurement_reflns_used    25
_cell_measurement_theta_min      7.5
_cell_measurement_theta_max      15

_exptl_crystal_description       bar
_exptl_crystal_colour            pink
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.844
_exptl_crystal_F_000             392
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.048
_exptl_crystal_size_mid          0.006
_exptl_crystal_size_min          0.004
_exptl_absorpt_coefficient_mu    9.303
_shelx_estimated_absorpt_T_min   0.499
_shelx_estimated_absorpt_T_max   0.936
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.935
_exptl_absorpt_correction_T_max  0.963
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      273(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            2185
_diffrn_reflns_av_unetI/netI     0.0175
_diffrn_reflns_av_R_equivalents  0.0411
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -6
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_theta_min         3.656
_diffrn_reflns_theta_max         27.481
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             131
_reflns_number_gt                124
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_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.
;

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SMART'
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0244P)²+0.3237P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   .
_refine_ls_hydrogen_treatment    undef
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         131
_refine_ls_number_parameters     9
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0237
_refine_ls_R_factor_gt           0.0208
_refine_ls_wR_factor_ref         0.0465
_refine_ls_wR_factor_gt          0.0455
_refine_ls_goodness_of_fit_ref   1.192
_refine_ls_restrained_S_all      1.192
_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
Ga Ga 0.5000 1.0000 0.7500 0.0170(3) Uani 0.6 8 d S T P . .
Ge Ge 0.5000 1.0000 0.7500 0.0170(3) Uani 0.4 8 d S T P . .
S2 S 0.34758(10) 0.84758(10) 0.5000 0.0234(3) Uani 1 4 d S T P . .
K3 K 0.5000 0.5000 0.2500 0.113(3) Uani 0.6 8 d S T P . .


_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
Ga S2 2.2592(9) 27_466 ?
Ga S2 2.2592(9) 11_655 ?
Ga S2 2.2592(9) 17_676 ?
Ga S2 2.2592(9) . ?
Ga Ge 2.9779(4) 17_676 ?
Ga Ge 2.9778(4) 17_677 ?
Ga Ga 2.9778(4) 17_677 ?
Ga Ga 2.9779(4) 17_676 ?
Ga K3 3.9412(5) 17_676 ?
Ga K3 3.9412(5) 9_455 ?
Ga K3 3.9412(5) 9 ?
Ga K3 3.9412(5) 17_666 ?
S2 Ge 2.2592(9) 17_676 ?
S2 Ga 2.2592(9) 17_676 ?
S2 K3 3.3416(5) 25_565 ?
S2 K3 3.3416(5) . ?
S2 K3 3.3416(5) 9_455 ?
S2 K3 3.3416(5) 17_666 ?
K3 K3 2.9779(4) 17_666 ?
K3 K3 2.9779(4) 17_665 ?
K3 S2 3.3417(5) 27_455 ?
K3 S2 3.3417(5) 19_566 ?
K3 S2 3.3417(5) 25_565 ?
K3 S2 3.3417(5) 11_654 ?
K3 S2 3.3417(5) 3_655 ?
K3 S2 3.3417(5) 17_666 ?
K3 S2 3.3417(5) 9_544 ?
K3 Ga 3.9412(5) 9_544 ?
K3 Ge 3.9412(5) 17_676 ?

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
S2 Ga S2 97.54(4) 27_466 11_655 ?
S2 Ga S2 115.74(2) 27_466 17_676 ?
S2 Ga S2 115.74(2) 11_655 17_676 ?
S2 Ga S2 115.74(2) 27_466 . ?
S2 Ga S2 115.74(2) 11_655 . ?
S2 Ga S2 97.54(4) 17_676 . ?
S2 Ga Ge 131.23(2) 27_466 17_676 ?
S2 Ga Ge 131.23(2) 11_655 17_676 ?
S2 Ga Ge 48.77(2) 17_676 17_676 ?
S2 Ga Ge 48.77(2) . 17_676 ?
S2 Ga Ge 48.77(2) 27_466 17_677 ?
S2 Ga Ge 48.77(2) 11_655 17_677 ?
S2 Ga Ge 131.23(2) 17_676 17_677 ?
S2 Ga Ge 131.23(2) . 17_677 ?
Ge Ga Ge 180.0 17_676 17_677 ?
S2 Ga Ga 48.77(2) 27_466 17_677 ?
S2 Ga Ga 48.77(2) 11_655 17_677 ?
S2 Ga Ga 131.23(2) 17_676 17_677 ?
S2 Ga Ga 131.23(2) . 17_677 ?
Ge Ga Ga 180.0 17_676 17_677 ?
Ge Ga Ga 0.0 17_677 17_677 ?
S2 Ga Ga 131.23(2) 27_466 17_676 ?
S2 Ga Ga 131.23(2) 11_655 17_676 ?
S2 Ga Ga 48.77(2) 17_676 17_676 ?
S2 Ga Ga 48.77(2) . 17_676 ?
Ge Ga Ga 0.0 17_676 17_676 ?
Ge Ga Ga 180.0 17_677 17_676 ?
Ga Ga Ga 180.0 17_677 17_676 ?
S2 Ga K3 57.872(11) 27_466 17_676 ?
S2 Ga K3 122.128(11) 11_655 17_676 ?
S2 Ga K3 57.872(11) 17_676 17_676 ?
S2 Ga K3 122.128(11) . 17_676 ?
Ge Ga K3 90.0 17_676 17_676 ?
Ge Ga K3 90.0 17_677 17_676 ?
Ga Ga K3 90.0 17_677 17_676 ?
Ga Ga K3 90.0 17_676 17_676 ?
S2 Ga K3 57.872(11) 27_466 9_455 ?
S2 Ga K3 122.128(11) 11_655 9_455 ?
S2 Ga K3 122.128(11) 17_676 9_455 ?
S2 Ga K3 57.872(11) . 9_455 ?
Ge Ga K3 90.0 17_676 9_455 ?
Ge Ga K3 90.0 17_677 9_455 ?
Ga Ga K3 90.0 17_677 9_455 ?
Ga Ga K3 90.0 17_676 9_455 ?
K3 Ga K3 90.0 17_676 9_455 ?
S2 Ga K3 122.128(11) 27_466 9 ?
S2 Ga K3 57.872(11) 11_655 9 ?
S2 Ga K3 57.872(11) 17_676 9 ?
S2 Ga K3 122.128(11) . 9 ?
Ge Ga K3 90.0 17_676 9 ?
Ge Ga K3 90.0 17_677 9 ?
Ga Ga K3 90.0 17_677 9 ?
Ga Ga K3 90.0 17_676 9 ?
K3 Ga K3 90.0 17_676 9 ?
K3 Ga K3 180.0 9_455 9 ?
S2 Ga K3 122.128(11) 27_466 17_666 ?
S2 Ga K3 57.872(11) 11_655 17_666 ?
S2 Ga K3 122.128(11) 17_676 17_666 ?
S2 Ga K3 57.872(11) . 17_666 ?
Ge Ga K3 90.0 17_676 17_666 ?
Ge Ga K3 90.0 17_677 17_666 ?
Ga Ga K3 90.0 17_677 17_666 ?
Ga Ga K3 90.0 17_676 17_666 ?
K3 Ga K3 180.0 17_676 17_666 ?
K3 Ga K3 90.0 9_455 17_666 ?
K3 Ga K3 90.0 9 17_666 ?
Ga S2 Ge 82.5 . 17_676 ?
Ga S2 Ga 82.46(4) . 17_676 ?
Ge S2 Ga 0.0 17_676 17_676 ?
Ga S2 K3 122.579(17) . 25_565 ?
Ge S2 K3 87.201(7) 17_676 25_565 ?
Ga S2 K3 87.201(7) 17_676 25_565 ?
Ga S2 K3 122.579(17) . . ?
Ge S2 K3 87.201(7) 17_676 . ?
Ga S2 K3 87.201(7) 17_676 . ?
K3 S2 K3 113.02(2) 25_565 . ?
Ga S2 K3 87.201(7) . 9_455 ?
Ge S2 K3 122.579(17) 17_676 9_455 ?
Ga S2 K3 122.579(17) 17_676 9_455 ?
K3 S2 K3 52.919(10) 25_565 9_455 ?
K3 S2 K3 142.01(4) . 9_455 ?
Ga S2 K3 87.201(7) . 17_666 ?
Ge S2 K3 122.579(17) 17_676 17_666 ?
Ga S2 K3 122.579(17) 17_676 17_666 ?
K3 S2 K3 142.01(4) 25_565 17_666 ?
K3 S2 K3 52.919(10) . 17_666 ?
K3 S2 K3 113.02(2) 9_455 17_666 ?
K3 K3 K3 180.0 17_666 17_665 ?
K3 K3 S2 63.540(5) 17_666 . ?
K3 K3 S2 116.460(5) 17_665 . ?
K3 K3 S2 116.460(5) 17_666 27_455 ?
K3 K3 S2 63.540(5) 17_665 27_455 ?
S2 K3 S2 137.86(4) . 27_455 ?
K3 K3 S2 63.540(5) 17_666 19_566 ?
K3 K3 S2 116.460(5) 17_665 19_566 ?
S2 K3 S2 78.549(4) . 19_566 ?
S2 K3 S2 142.01(4) 27_455 19_566 ?
K3 K3 S2 116.460(5) 17_666 25_565 ?
K3 K3 S2 63.540(5) 17_665 25_565 ?
S2 K3 S2 66.98(2) . 25_565 ?
S2 K3 S2 78.549(4) 27_455 25_565 ?
S2 K3 S2 137.86(4) 19_566 25_565 ?
K3 K3 S2 116.459(5) 17_666 11_654 ?
K3 K3 S2 63.541(5) 17_665 11_654 ?
S2 K3 S2 69.85(3) . 11_654 ?
S2 K3 S2 127.081(9) 27_455 11_654 ?
S2 K3 S2 66.98(2) 19_566 11_654 ?
S2 K3 S2 78.549(4) 25_565 11_654 ?
K3 K3 S2 63.541(5) 17_666 3_655 ?
K3 K3 S2 116.459(5) 17_665 3_655 ?
S2 K3 S2 78.549(4) . 3_655 ?
S2 K3 S2 66.98(2) 27_455 3_655 ?
S2 K3 S2 127.081(9) 19_566 3_655 ?
S2 K3 S2 69.85(3) 25_565 3_655 ?
S2 K3 S2 142.01(4) 11_654 3_655 ?
K3 K3 S2 63.540(5) 17_666 17_666 ?
K3 K3 S2 116.460(5) 17_665 17_666 ?
S2 K3 S2 127.081(10) . 17_666 ?
S2 K3 S2 69.85(3) 27_455 17_666 ?
S2 K3 S2 78.549(4) 19_566 17_666 ?
S2 K3 S2 142.01(4) 25_565 17_666 ?
S2 K3 S2 137.86(4) 11_654 17_666 ?
S2 K3 S2 78.549(4) 3_655 17_666 ?
K3 K3 S2 116.460(5) 17_666 9_544 ?
K3 K3 S2 63.541(5) 17_665 9_544 ?
S2 K3 S2 142.01(4) . 9_544 ?
S2 K3 S2 78.549(4) 27_455 9_544 ?
S2 K3 S2 69.85(3) 19_566 9_544 ?
S2 K3 S2 127.081(9) 25_565 9_544 ?
S2 K3 S2 78.549(4) 11_654 9_544 ?
S2 K3 S2 137.86(4) 3_655 9_544 ?
S2 K3 S2 66.98(2) 17_666 9_544 ?
K3 K3 Ga 90.0 17_666 9_544 ?
K3 K3 Ga 90.0 17_665 9_544 ?
S2 K3 Ga 111.072(18) . 9_544 ?
S2 K3 Ga 111.072(18) 27_455 9_544 ?
S2 K3 Ga 34.927(16) 19_566 9_544 ?
S2 K3 Ga 145.073(16) 25_565 9_544 ?
S2 K3 Ga 68.928(18) 11_654 9_544 ?
S2 K3 Ga 145.073(16) 3_655 9_544 ?
S2 K3 Ga 68.928(18) 17_666 9_544 ?
S2 K3 Ga 34.927(16) 9_544 9_544 ?
K3 K3 Ge 90.0 17_666 17_676 ?
K3 K3 Ge 90.0 17_665 17_676 ?
S2 K3 Ge 34.927(16) . 17_676 ?
S2 K3 Ge 145.073(16) 27_455 17_676 ?
S2 K3 Ge 68.928(18) 19_566 17_676 ?
S2 K3 Ge 68.928(18) 25_565 17_676 ?
S2 K3 Ge 34.927(16) 11_654 17_676 ?
S2 K3 Ge 111.072(18) 3_655 17_676 ?
S2 K3 Ge 145.073(16) 17_666 17_676 ?
S2 K3 Ge 111.072(18) 9_544 17_676 ?
Ga K3 Ge 90.0 9_544 17_676 ?

_refine_diff_density_max         0.746
_refine_diff_density_min         -0.608
_refine_diff_density_rms         0.110



####################################################################### 
# 
# 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_I4-mcm
_database_code_depnum_ccdc_archive 'CCDC 1476384'
_audit_update_record             
;
2016-04-26 deposited with the CCDC.
2016-07-25 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'Ga2.4 K2.4 S8 Si1.6'
_chemical_formula_weight         562.60

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ga Ga 0.2307 1.6083 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      tetragonal
_space_group_IT_number           140
_space_group_name_H-M_alt        'I 4/m c m'
_space_group_name_Hall           '-I 4 2c'

_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'
'-y, x, z'
'y, -x, z'
'-x, y, -z+1/2'
'x, -y, -z+1/2'
'y, x, -z+1/2'
'-y, -x, -z+1/2'
'x+1/2, y+1/2, z+1/2'
'-x+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'
'-x+1/2, y+1/2, -z+1'
'x+1/2, -y+1/2, -z+1'
'y+1/2, x+1/2, -z+1'
'-y+1/2, -x+1/2, -z+1'
'-x, -y, -z'
'x, y, -z'
'y, -x, -z'
'-y, x, -z'
'x, -y, z-1/2'
'-x, y, z-1/2'
'-y, -x, z-1/2'
'y, x, z-1/2'
'-x+1/2, -y+1/2, -z+1/2'
'x+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'
'x+1/2, -y+1/2, z'
'-x+1/2, y+1/2, z'
'-y+1/2, -x+1/2, z'
'y+1/2, x+1/2, z'

_cell_length_a                   7.8910(7)
_cell_length_b                   7.8910(7)
_cell_length_c                   5.8660(5)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     365.26(7)
_cell_formula_units_Z            1
_cell_measurement_temperature    273(2)
_cell_measurement_reflns_used    25
_cell_measurement_theta_min      7.5
_cell_measurement_theta_max      15

_exptl_crystal_description       bar
_exptl_crystal_colour            pale
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.558
_exptl_crystal_F_000             270
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.063
_exptl_crystal_size_mid          0.010
_exptl_crystal_size_min          0.005
_exptl_absorpt_coefficient_mu    6.328
_shelx_estimated_absorpt_T_min   0.691
_shelx_estimated_absorpt_T_max   0.969
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.927
_exptl_absorpt_correction_T_max  0.969
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      273(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            2003
_diffrn_reflns_av_unetI/netI     0.0093
_diffrn_reflns_av_R_equivalents  0.0269
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -6
_diffrn_reflns_limit_l_max       6
_diffrn_reflns_theta_min         3.652
_diffrn_reflns_theta_max         24.874
_diffrn_reflns_theta_full        24.874
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measured_fraction_theta_full 0.981
_diffrn_reflns_Laue_measured_fraction_max 0.981
_diffrn_reflns_Laue_measured_fraction_full 0.981
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_point_group_measured_fraction_full 0.981
_reflns_number_total             101
_reflns_number_gt                98
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_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.
;

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0427P)²+1.1681P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   .
_refine_ls_hydrogen_treatment    undef
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         101
_refine_ls_number_parameters     9
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0250
_refine_ls_R_factor_gt           0.0247
_refine_ls_wR_factor_ref         0.0720
_refine_ls_wR_factor_gt          0.0717
_refine_ls_goodness_of_fit_ref   1.245
_refine_ls_restrained_S_all      1.245
_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
Ga Ga 0.5000 0.0000 0.2500 0.0182(5) Uani 0.6 8 d S T P . .
Si Si 0.5000 0.0000 0.2500 0.0182(5) Uani 0.4 8 d S T P . .
S S 0.64982(14) 0.14982(14) 0.5000 0.0294(6) Uani 1 4 d S T P . .
K K 0.5000 0.5000 0.7500 0.132(4) Uani 0.6 8 d S T P . .


_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
Ga S 2.2240(12) . ?
Ga S 2.2240(12) 27 ?
Ga S 2.2240(12) 11_544 ?
Ga S 2.2240(12) 17_656 ?
Ga Ga 2.9330(3) 17_655 ?
Ga Ga 2.9330(3) 17_656 ?
Ga K 3.9455(4) 17_666 ?
Ga K 3.9455(4) 9_444 ?
Ga K 3.9455(4) 9_544 ?
Ga K 3.9455(4) 17_656 ?
S Si 2.2240(12) 17_656 ?
S Ga 2.2240(12) 17_656 ?
S K 3.3442(6) 25_656 ?
S K 3.3442(6) . ?
S K 3.3442(6) 9_544 ?
S K 3.3442(6) 17_666 ?
K K 2.9330(2) 17_667 ?
K K 2.9330(3) 17_666 ?
K S 3.3442(6) 19_566 ?
K S 3.3442(6) 27_566 ?
K S 3.3442(6) 25_656 ?
K S 3.3442(6) 3_655 ?
K S 3.3442(6) 11_545 ?
K S 3.3442(6) 17_666 ?
K S 3.3442(6) 9_455 ?
K Ga 3.9455(4) 17_666 ?
K Ga 3.9455(4) 9 ?

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
S Ga S 115.77(3) . 27 ?
S Ga S 115.77(3) . 11_544 ?
S Ga S 97.49(6) 27 11_544 ?
S Ga S 97.49(6) . 17_656 ?
S Ga S 115.77(3) 27 17_656 ?
S Ga S 115.77(3) 11_544 17_656 ?
S Ga Ga 131.25(3) . 17_655 ?
S Ga Ga 48.75(3) 27 17_655 ?
S Ga Ga 48.75(3) 11_544 17_655 ?
S Ga Ga 131.25(3) 17_656 17_655 ?
S Ga Ga 48.75(3) . 17_656 ?
S Ga Ga 131.25(3) 27 17_656 ?
S Ga Ga 131.25(3) 11_544 17_656 ?
S Ga Ga 48.75(3) 17_656 17_656 ?
Ga Ga Ga 180.0 17_655 17_656 ?
S Ga K 57.887(15) . 17_666 ?
S Ga K 122.114(15) 27 17_666 ?
S Ga K 57.887(15) 11_544 17_666 ?
S Ga K 122.114(15) 17_656 17_666 ?
Ga Ga K 90.0 17_655 17_666 ?
Ga Ga K 90.0 17_656 17_666 ?
S Ga K 122.113(15) . 9_444 ?
S Ga K 122.114(15) 27 9_444 ?
S Ga K 57.886(15) 11_544 9_444 ?
S Ga K 57.886(15) 17_656 9_444 ?
Ga Ga K 90.0 17_655 9_444 ?
Ga Ga K 90.0 17_656 9_444 ?
K Ga K 90.0 17_666 9_444 ?
S Ga K 57.887(15) . 9_544 ?
S Ga K 57.887(15) 27 9_544 ?
S Ga K 122.114(15) 11_544 9_544 ?
S Ga K 122.114(15) 17_656 9_544 ?
Ga Ga K 90.0 17_655 9_544 ?
Ga Ga K 90.0 17_656 9_544 ?
K Ga K 90.0 17_666 9_544 ?
K Ga K 180.0 9_444 9_544 ?
S Ga K 122.113(15) . 17_656 ?
S Ga K 57.886(15) 27 17_656 ?
S Ga K 122.113(15) 11_544 17_656 ?
S Ga K 57.886(15) 17_656 17_656 ?
Ga Ga K 90.0 17_655 17_656 ?
Ga Ga K 90.0 17_656 17_656 ?
K Ga K 180.0 17_666 17_656 ?
K Ga K 90.0 9_444 17_656 ?
K Ga K 90.0 9_544 17_656 ?
Ga S Si 82.5 . 17_656 ?
Ga S Ga 82.51(6) . 17_656 ?
Si S Ga 0.0 17_656 17_656 ?
Ga S K 122.72(2) . 25_656 ?
Si S K 87.831(7) 17_656 25_656 ?
Ga S K 87.831(7) 17_656 25_656 ?
Ga S K 122.72(2) . . ?
Si S K 87.831(7) 17_656 . ?
Ga S K 87.831(7) 17_656 . ?
K S K 113.07(3) 25_656 . ?
Ga S K 87.831(7) . 9_544 ?
Si S K 122.72(2) 17_656 9_544 ?
Ga S K 122.72(2) 17_656 9_544 ?
K S K 52.018(11) 25_656 9_544 ?
K S K 140.94(5) . 9_544 ?
Ga S K 87.831(7) . 17_666 ?
Si S K 122.72(2) 17_656 17_666 ?
Ga S K 122.72(2) 17_656 17_666 ?
K S K 140.94(5) 25_656 17_666 ?
K S K 52.018(11) . 17_666 ?
K S K 113.07(3) 9_544 17_666 ?
K K K 180.0 17_667 17_666 ?
K K S 116.009(5) 17_667 19_566 ?
K K S 63.991(5) 17_666 19_566 ?
K K S 63.991(5) 17_667 27_566 ?
K K S 116.009(5) 17_666 27_566 ?
S K S 140.94(5) 19_566 27_566 ?
K K S 63.991(5) 17_667 25_656 ?
K K S 116.009(5) 17_666 25_656 ?
S K S 138.59(5) 19_566 25_656 ?
S K S 78.913(4) 27_566 25_656 ?
K K S 116.009(5) 17_667 3_655 ?
K K S 63.991(6) 17_666 3_655 ?
S K S 127.981(11) 19_566 3_655 ?
S K S 66.93(3) 27_566 3_655 ?
S K S 68.57(4) 25_656 3_655 ?
K K S 63.991(5) 17_667 11_545 ?
K K S 116.009(5) 17_666 11_545 ?
S K S 66.93(3) 19_566 11_545 ?
S K S 127.981(11) 27_566 11_545 ?
S K S 78.913(4) 25_656 11_545 ?
S K S 140.94(5) 3_655 11_545 ?
K K S 116.009(5) 17_667 17_666 ?
K K S 63.991(5) 17_666 17_666 ?
S K S 78.913(4) 19_566 17_666 ?
S K S 68.57(4) 27_566 17_666 ?
S K S 140.94(5) 25_656 17_666 ?
S K S 78.913(4) 3_655 17_666 ?
S K S 138.59(5) 11_545 17_666 ?
K K S 63.991(5) 17_667 9_455 ?
K K S 116.009(5) 17_666 9_455 ?
S K S 68.57(4) 19_566 9_455 ?
S K S 78.913(4) 27_566 9_455 ?
S K S 127.981(11) 25_656 9_455 ?
S K S 138.59(5) 3_655 9_455 ?
S K S 78.913(4) 11_545 9_455 ?
S K S 66.93(3) 17_666 9_455 ?
K K S 116.009(5) 17_667 . ?
K K S 63.991(5) 17_666 . ?
S K S 78.913(4) 19_566 . ?
S K S 138.59(5) 27_566 . ?
S K S 66.93(3) 25_656 . ?
S K S 78.914(4) 3_655 . ?
S K S 68.56(4) 11_545 . ?
S K S 127.981(11) 17_666 . ?
S K S 140.94(5) 9_455 . ?
K K Ga 90.0 17_667 17_666 ?
K K Ga 90.0 17_666 17_666 ?
S K Ga 110.70(2) 19_566 17_666 ?
S K Ga 34.28(2) 27_566 17_666 ?
S K Ga 110.70(2) 25_656 17_666 ?
S K Ga 69.30(2) 3_655 17_666 ?
S K Ga 145.72(2) 11_545 17_666 ?
S K Ga 34.28(2) 17_666 17_666 ?
S K Ga 69.30(2) 9_455 17_666 ?
S K Ga 145.72(2) . 17_666 ?
K K Ga 90.0 17_667 9 ?
K K Ga 90.0 17_666 9 ?
S K Ga 145.72(2) 19_566 9 ?
S K Ga 69.30(2) 27_566 9 ?
S K Ga 34.28(2) 25_656 9 ?
S K Ga 34.28(2) 3_655 9 ?
S K Ga 110.70(2) 11_545 9 ?
S K Ga 110.70(2) 17_666 9 ?
S K Ga 145.72(2) 9_455 9 ?
S K Ga 69.30(2) . 9 ?
Ga K Ga 90.0 17_666 9 ?

_refine_diff_density_max         1.104
_refine_diff_density_min         -1.037
_refine_diff_density_rms         0.120



