# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2015

####################################################################### 
# 
# 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_c
_database_code_depnum_ccdc_archive 'CCDC 1422758'
_audit_update_record             
;
2015-09-07 deposited with the CCDC.
2015-11-03 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'Ga Ge3 Na Se8'
_chemical_formula_weight         942.16

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Na Na 0.0362 0.0249 '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'
Se Se -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   P21/c

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

_cell_length_a                   7.2329(14)
_cell_length_b                   11.889(2)
_cell_length_c                   17.550(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 101.75(3)
_cell_angle_gamma                90.00
_cell_volume                     1477.5(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    153.1500
_cell_measurement_reflns_used    5538
_cell_measurement_theta_min      2.0831
_cell_measurement_theta_max      31.4970

_exptl_crystal_description       Prism
_exptl_crystal_colour            orange
_exptl_crystal_size_max          0.6000
_exptl_crystal_size_mid          0.1800
_exptl_crystal_size_min          0.0420
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    4.235
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1640
_exptl_absorpt_coefficient_mu    27.542
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.2832
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_process_details   'face indexed'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      153.1500
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini ultra'
_diffrn_measurement_method       dtprofit.ref
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            12334
_diffrn_reflns_av_R_equivalents  0.2088
_diffrn_reflns_av_sigmaI/netI    0.1990
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         2.88
_diffrn_reflns_theta_max         26.37
_reflns_number_total             3006
_reflns_number_gt                1836
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0200P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   none
_refine_ls_hydrogen_treatment    none
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.00051(11)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         3006
_refine_ls_number_parameters     119
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0881
_refine_ls_R_factor_gt           0.0664
_refine_ls_wR_factor_ref         0.1145
_refine_ls_wR_factor_gt          0.1044
_refine_ls_goodness_of_fit_ref   0.897
_refine_ls_restrained_S_all      0.897
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Na Na 0.2576(8) 0.5657(6) 0.3257(3) 0.0430(19) Uani 1 1 d . . .
Ge1 Ge 0.54335(18) 0.23592(12) 0.35235(7) 0.0107(3) Uani 0.75 1 d P . .
Ga1 Ga 0.54335(18) 0.23592(12) 0.35235(7) 0.0107(3) Uani 0.25 1 d P . .
Ge2 Ge 0.25116(19) 0.29082(12) 0.16209(7) 0.0121(3) Uani 0.75 1 d P . .
Ga2 Ga 0.25116(19) 0.29082(12) 0.16209(7) 0.0121(3) Uani 0.25 1 d P . .
Ge3 Ge 0.31289(19) 0.18912(12) 0.00552(7) 0.0122(4) Uani 0.75 1 d P . .
Ga3 Ga 0.31289(19) 0.18912(12) 0.00552(7) 0.0122(4) Uani 0.25 1 d P . .
Ge4 Ge 0.03486(19) 0.24061(12) 0.32465(7) 0.0116(3) Uani 0.75 1 d P . .
Ga4 Ga 0.03486(19) 0.24061(12) 0.32465(7) 0.0116(3) Uani 0.25 1 d P . .
Se1 Se 0.07287(19) 0.39682(11) 0.41184(7) 0.0142(3) Uani 1 1 d . . .
Se2 Se 0.32103(19) 0.10368(11) 0.12875(7) 0.0142(3) Uani 1 1 d . . .
Se3 Se 0.2388(2) 0.37542(12) 0.03835(7) 0.0191(4) Uani 1 1 d . . .
Se4 Se 0.49222(18) 0.37739(11) 0.25466(7) 0.0138(3) Uani 1 1 d . . .
Se5 Se 0.20344(17) 0.61304(11) 0.15469(7) 0.0133(3) Uani 1 1 d . . .
Se6 Se 0.28822(17) 0.10976(11) 0.34034(7) 0.0126(3) Uani 1 1 d . . .
Se7 Se 0.61509(19) 0.33102(13) 0.47580(7) 0.0175(4) Uani 1 1 d . . .
Se8 Se 0.05000(19) 0.80952(13) 0.30652(7) 0.0171(4) Uani 1 1 d . . .


_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
Na Se1 2.987(6) . ?
Na Se5 3.000(6) . ?
Na Se2 3.023(6) 2_655 ?
Na Se4 3.211(7) . ?
Na Se8 3.250(7) . ?
Ge1 Se6 2.3540(19) . ?
Ge1 Se5 2.3656(19) 2_645 ?
Ge1 Se4 2.3763(18) . ?
Ge1 Se7 2.4049(18) . ?
Ge2 Se4 2.363(2) . ?
Ge2 Se8 2.3636(19) 2_545 ?
Ge2 Se3 2.3783(17) . ?
Ge2 Se2 2.3808(19) . ?
Ge3 Se7 2.3604(18) 4_565 ?
Ge3 Se1 2.366(2) 4_565 ?
Ge3 Se3 2.3772(19) . ?
Ge3 Se2 2.3793(16) . ?
Ge4 Se6 2.3767(19) . ?
Ge4 Se5 2.3785(18) 2_545 ?
Ge4 Se1 2.3863(18) . ?
Ge4 Se8 2.4025(18) 2_545 ?
Se1 Ga3 2.366(2) 4_566 ?
Se1 Ge3 2.366(2) 4_566 ?
Se2 Na 3.023(6) 2_645 ?
Se5 Ga1 2.3656(19) 2_655 ?
Se5 Ge1 2.3656(19) 2_655 ?
Se5 Ga4 2.3785(18) 2 ?
Se5 Ge4 2.3785(18) 2 ?
Se7 Ga3 2.3603(18) 4_566 ?
Se7 Ge3 2.3603(18) 4_566 ?
Se8 Ga2 2.3636(19) 2 ?
Se8 Ge2 2.3636(19) 2 ?
Se8 Ga4 2.4025(18) 2 ?
Se8 Ge4 2.4025(18) 2 ?

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
Se1 Na Se5 130.7(2) . . ?
Se1 Na Se2 119.8(2) . 2_655 ?
Se5 Na Se2 98.95(15) . 2_655 ?
Se1 Na Se4 93.1(2) . . ?
Se5 Na Se4 73.37(13) . . ?
Se2 Na Se4 67.83(13) 2_655 . ?
Se1 Na Se8 114.03(18) . . ?
Se5 Na Se8 76.45(15) . . ?
Se2 Na Se8 108.3(2) 2_655 . ?
Se4 Na Se8 148.34(18) . . ?
Se6 Ge1 Se5 101.71(7) . 2_645 ?
Se6 Ge1 Se4 112.48(7) . . ?
Se5 Ge1 Se4 114.07(7) 2_645 . ?
Se6 Ge1 Se7 113.68(7) . . ?
Se5 Ge1 Se7 108.07(7) 2_645 . ?
Se4 Ge1 Se7 106.89(7) . . ?
Se4 Ge2 Se8 112.63(7) . 2_545 ?
Se4 Ge2 Se3 109.20(7) . . ?
Se8 Ge2 Se3 107.94(8) 2_545 . ?
Se4 Ge2 Se2 114.34(7) . . ?
Se8 Ge2 Se2 113.39(8) 2_545 . ?
Se3 Ge2 Se2 98.12(6) . . ?
Se7 Ge3 Se1 112.59(7) 4_565 4_565 ?
Se7 Ge3 Se3 114.37(8) 4_565 . ?
Se1 Ge3 Se3 113.65(7) 4_565 . ?
Se7 Ge3 Se2 107.76(7) 4_565 . ?
Se1 Ge3 Se2 109.03(7) 4_565 . ?
Se3 Ge3 Se2 98.19(6) . . ?
Se6 Ge4 Se5 97.50(7) . 2_545 ?
Se6 Ge4 Se1 116.73(7) . . ?
Se5 Ge4 Se1 113.02(7) 2_545 . ?
Se6 Ge4 Se8 112.00(7) . 2_545 ?
Se5 Ge4 Se8 108.17(7) 2_545 2_545 ?
Se1 Ge4 Se8 108.82(7) . 2_545 ?
Ga3 Se1 Ge3 0.00(8) 4_566 4_566 ?
Ga3 Se1 Ge4 94.70(7) 4_566 . ?
Ge3 Se1 Ge4 94.70(7) 4_566 . ?
Ga3 Se1 Na 107.54(13) 4_566 . ?
Ge3 Se1 Na 107.54(13) 4_566 . ?
Ge4 Se1 Na 101.76(14) . . ?
Ge3 Se2 Ge2 81.79(6) . . ?
Ge3 Se2 Na 98.10(13) . 2_645 ?
Ge2 Se2 Na 109.12(15) . 2_645 ?
Ge3 Se3 Ge2 81.89(6) . . ?
Ge2 Se4 Ge1 99.93(7) . . ?
Ge2 Se4 Na 101.32(13) . . ?
Ge1 Se4 Na 103.31(11) . . ?
Ga1 Se5 Ge1 0.00(8) 2_655 2_655 ?
Ga1 Se5 Ga4 101.94(7) 2_655 2 ?
Ge1 Se5 Ga4 101.94(7) 2_655 2 ?
Ga1 Se5 Ge4 101.94(7) 2_655 2 ?
Ge1 Se5 Ge4 101.94(7) 2_655 2 ?
Ga4 Se5 Ge4 0.00(6) 2 2 ?
Ga1 Se5 Na 102.91(13) 2_655 . ?
Ge1 Se5 Na 102.91(13) 2_655 . ?
Ga4 Se5 Na 85.30(14) 2 . ?
Ge4 Se5 Na 85.30(14) 2 . ?
Ge1 Se6 Ge4 99.51(7) . . ?
Ga3 Se7 Ge3 0.00(7) 4_566 4_566 ?
Ga3 Se7 Ge1 96.42(7) 4_566 . ?
Ge3 Se7 Ge1 96.42(7) 4_566 . ?
Ga2 Se8 Ge2 0.00(7) 2 2 ?
Ga2 Se8 Ga4 97.10(7) 2 2 ?
Ge2 Se8 Ga4 97.10(7) 2 2 ?
Ga2 Se8 Ge4 97.10(7) 2 2 ?
Ge2 Se8 Ge4 97.10(7) 2 2 ?
Ga4 Se8 Ge4 0.00(9) 2 2 ?
Ga2 Se8 Na 108.67(12) 2 . ?
Ge2 Se8 Na 108.67(12) 2 . ?
Ga4 Se8 Na 79.50(12) 2 . ?
Ge4 Se8 Na 79.50(12) 2 . ?

_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full        26.37
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max         2.878
_refine_diff_density_min         -2.460
_refine_diff_density_rms         0.571
####################################################################### 
# 
# 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_b
_database_code_depnum_ccdc_archive 'CCDC 1422759'
_audit_update_record             
;
2015-09-07 deposited with the CCDC.
2015-11-03 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'Ga3 Ge7 K3 S20'
_chemical_formula_weight         1475.79

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'
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'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   P21/c

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

_cell_length_a                   6.7665(4)
_cell_length_b                   37.527(2)
_cell_length_c                   6.6796(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.802(5)
_cell_angle_gamma                90.00
_cell_volume                     1695.94(18)
_cell_formula_units_Z            2
_cell_measurement_temperature    153.1500
_cell_measurement_reflns_used    2287
_cell_measurement_theta_min      3.3550
_cell_measurement_theta_max      28.6190

_exptl_crystal_description       Prism
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.890
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1388
_exptl_absorpt_coefficient_mu    10.053
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.31192
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   'face indexed'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      153.1500
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini ultra'
_diffrn_measurement_method       dtprofit.ref
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            9264
_diffrn_reflns_av_R_equivalents  0.0678
_diffrn_reflns_av_sigmaI/netI    0.0754
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_k_max       46
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_theta_min         3.42
_diffrn_reflns_theta_max         26.37
_reflns_number_total             3451
_reflns_number_gt                2815
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0400P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   none
_refine_ls_hydrogen_treatment    none
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.0013(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         3451
_refine_ls_number_parameters     152
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0710
_refine_ls_R_factor_gt           0.0564
_refine_ls_wR_factor_ref         0.1156
_refine_ls_wR_factor_gt          0.1086
_refine_ls_goodness_of_fit_ref   1.145
_refine_ls_restrained_S_all      1.145
_refine_ls_shift/su_max          0.001
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
K1 K 0.0164(5) 0.83414(9) 0.2039(4) 0.1042(11) Uani 1 1 d . . .
K2 K 0.5000 0.0000 0.5000 0.1159(18) Uani 1 2 d S . .
Ga1 Ga 0.41240(10) 0.09260(2) 0.26720(12) 0.0216(2) Uani 0.30 1 d P . .
Ge1 Ge 0.41240(10) 0.09260(2) 0.26720(12) 0.0216(2) Uani 0.70 1 d P . .
Ga2 Ga 0.08693(10) 0.03590(2) 0.02280(12) 0.0217(2) Uani 0.30 1 d P . .
Ge2 Ge 0.08693(10) 0.03590(2) 0.02280(12) 0.0217(2) Uani 0.70 1 d P . .
Ga3 Ga 0.09013(10) 0.60402(2) 0.18828(12) 0.0210(2) Uani 0.30 1 d P . .
Ge3 Ge 0.09013(10) 0.60402(2) 0.18828(12) 0.0210(2) Uani 0.70 1 d P . .
Ga4 Ga 0.60074(10) 0.17850(2) 0.27195(11) 0.0211(2) Uani 0.30 1 d P . .
Ge4 Ge 0.60074(10) 0.17850(2) 0.27195(11) 0.0211(2) Uani 0.70 1 d P . .
Ga5 Ga 0.38383(11) 0.25929(2) 0.08604(12) 0.0236(2) Uani 0.30 1 d P . .
Ge5 Ge 0.38383(11) 0.25929(2) 0.08604(12) 0.0236(2) Uani 0.70 1 d P . .
S1 S 0.4302(3) 0.14129(6) 0.0757(3) 0.0280(5) Uani 1 1 d . . .
S2 S 0.1691(2) 0.41331(6) -0.0101(3) 0.0296(5) Uani 1 1 d . . .
S3 S 0.6583(2) 0.41408(6) -0.0078(3) 0.0281(5) Uani 1 1 d . . .
S4 S 0.4077(3) 0.04568(6) 0.0548(3) 0.0340(5) Uani 1 1 d . . .
S5 S 0.6622(3) 0.22830(6) 0.1054(3) 0.0304(5) Uani 1 1 d . . .
S6 S 0.4745(3) 0.31661(6) 0.0769(3) 0.0320(5) Uani 1 1 d . . .
S7 S 0.0937(3) 0.58534(6) 0.5046(3) 0.0289(5) Uani 1 1 d . . .
S8 S 0.0308(3) 0.49740(6) 0.2507(3) 0.0293(5) Uani 1 1 d . . .
S9 S 0.0785(3) 0.66309(6) 0.2002(3) 0.0311(5) Uani 1 1 d . . .
S10 S 0.1765(3) 0.25421(7) 0.3377(3) 0.0369(5) Uani 1 1 d . . .


_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
K1 S10 3.281(4) 2 ?
K1 S9 3.337(4) 4_576 ?
K1 S7 3.346(4) 4_575 ?
K1 S9 3.398(4) 4_575 ?
K1 S1 3.648(4) 3_565 ?
K1 S6 3.707(4) 2 ?
K1 S6 3.782(4) 2_655 ?
K1 Ga3 4.007(3) 4_576 ?
K2 S3 3.398(2) 4_566 ?
K2 S3 3.398(2) 2_645 ?
K2 S4 3.482(2) 3_656 ?
K2 S4 3.482(2) . ?
K2 S8 3.6117(19) 2_645 ?
K2 S8 3.6117(19) 4_566 ?
K2 Ga1 3.8497(8) . ?
K2 Ga1 3.8497(8) 3_656 ?
K2 Ge1 3.8497(8) 3_656 ?
Ga1 S1 2.234(2) . ?
Ga1 S3 2.2406(19) 4_566 ?
Ga1 S2 2.2455(19) 4_566 ?
Ga1 S4 2.261(2) . ?
Ga2 S4 2.2084(18) . ?
Ga2 S7 2.228(2) 2_545 ?
Ga2 S8 2.234(2) 4_565 ?
Ga2 S8 2.246(2) 2_545 ?
Ga2 Ge2 2.9544(16) 3 ?
Ga2 Ga2 2.9544(16) 3 ?
Ga3 S2 2.204(2) 3_565 ?
Ga3 S3 2.2066(19) 3_665 ?
Ga3 S9 2.220(2) . ?
Ga3 S7 2.226(2) . ?
Ga3 K1 4.007(3) 4_575 ?
Ga4 S5 2.217(2) . ?
Ga4 S1 2.227(2) . ?
Ga4 S6 2.227(2) 4_566 ?
Ga4 S9 2.2516(19) 2_645 ?
Ga5 S10 2.213(2) . ?
Ga5 S5 2.216(2) . ?
Ga5 S10 2.216(2) 4_565 ?
Ga5 S6 2.238(2) . ?
S1 K1 3.648(4) 3_565 ?
S2 Ge3 2.2040(19) 3_565 ?
S2 Ga3 2.2040(19) 3_565 ?
S2 Ga1 2.2455(19) 4_565 ?
S2 Ge1 2.2455(19) 4_565 ?
S3 Ge3 2.2066(19) 3_665 ?
S3 Ga3 2.2066(19) 3_665 ?
S3 Ga1 2.2406(19) 4_565 ?
S3 Ge1 2.2406(19) 4_565 ?
S3 K2 3.398(2) 2_655 ?
S6 Ge4 2.227(2) 4_565 ?
S6 Ga4 2.227(2) 4_565 ?
S6 K1 3.707(4) 2_545 ?
S6 K1 3.782(4) 2_645 ?
S7 Ge2 2.228(2) 2 ?
S7 Ga2 2.228(2) 2 ?
S7 K1 3.346(4) 4_576 ?
S8 Ge2 2.234(2) 4_566 ?
S8 Ga2 2.234(2) 4_566 ?
S8 Ge2 2.246(2) 2 ?
S8 Ga2 2.246(2) 2 ?
S8 K2 3.6117(19) 2_655 ?
S9 Ge4 2.2516(19) 2_655 ?
S9 Ga4 2.2516(19) 2_655 ?
S9 K1 3.337(4) 4_575 ?
S9 K1 3.398(4) 4_576 ?
S10 Ge5 2.216(2) 4_566 ?
S10 Ga5 2.216(2) 4_566 ?
S10 K1 3.281(4) 2_545 ?

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
S10 K1 S9 99.03(9) 2 4_576 ?
S10 K1 S7 148.88(11) 2 4_575 ?
S9 K1 S7 110.41(10) 4_576 4_575 ?
S10 K1 S9 89.92(9) 2 4_575 ?
S9 K1 S9 165.23(13) 4_576 4_575 ?
S7 K1 S9 63.66(7) 4_575 4_575 ?
S10 K1 S1 82.08(8) 2 3_565 ?
S9 K1 S1 126.34(12) 4_576 3_565 ?
S7 K1 S1 72.62(8) 4_575 3_565 ?
S9 K1 S1 66.32(7) 4_575 3_565 ?
S10 K1 S6 60.92(7) 2 2 ?
S9 K1 S6 73.40(7) 4_576 2 ?
S7 K1 S6 117.61(12) 4_575 2 ?
S9 K1 S6 121.35(10) 4_575 2 ?
S1 K1 S6 60.45(7) 3_565 2 ?
S10 K1 S6 103.46(11) 2 2_655 ?
S9 K1 S6 61.28(7) 4_576 2_655 ?
S7 K1 S6 99.45(9) 4_575 2_655 ?
S9 K1 S6 105.31(10) 4_575 2_655 ?
S1 K1 S6 170.25(10) 3_565 2_655 ?
S6 K1 S6 129.24(9) 2 2_655 ?
S10 K1 Ga3 129.99(9) 2 4_576 ?
S9 K1 Ga3 33.64(5) 4_576 4_576 ?
S7 K1 Ga3 77.28(7) 4_575 4_576 ?
S9 K1 Ga3 140.00(10) 4_575 4_576 ?
S1 K1 Ga3 111.10(10) 3_565 4_576 ?
S6 K1 Ga3 83.46(7) 2 4_576 ?
S6 K1 Ga3 71.68(6) 2_655 4_576 ?
S3 K2 S3 180.00(2) 4_566 2_645 ?
S3 K2 S4 115.31(5) 4_566 3_656 ?
S3 K2 S4 64.69(5) 2_645 3_656 ?
S3 K2 S4 64.69(5) 4_566 . ?
S3 K2 S4 115.31(5) 2_645 . ?
S4 K2 S4 180.00(6) 3_656 . ?
S3 K2 S8 74.88(5) 4_566 2_645 ?
S3 K2 S8 105.12(5) 2_645 2_645 ?
S4 K2 S8 103.56(4) 3_656 2_645 ?
S4 K2 S8 76.44(4) . 2_645 ?
S3 K2 S8 105.12(5) 4_566 4_566 ?
S3 K2 S8 74.88(5) 2_645 4_566 ?
S4 K2 S8 76.44(4) 3_656 4_566 ?
S4 K2 S8 103.56(4) . 4_566 ?
S8 K2 S8 180.00(6) 2_645 4_566 ?
S3 K2 Ga1 35.32(3) 4_566 . ?
S3 K2 Ga1 144.68(3) 2_645 . ?
S4 K2 Ga1 144.52(4) 3_656 . ?
S4 K2 Ga1 35.48(4) . . ?
S8 K2 Ga1 88.19(4) 2_645 . ?
S8 K2 Ga1 91.81(4) 4_566 . ?
S3 K2 Ga1 144.68(3) 4_566 3_656 ?
S3 K2 Ga1 35.32(3) 2_645 3_656 ?
S4 K2 Ga1 35.48(4) 3_656 3_656 ?
S4 K2 Ga1 144.52(4) . 3_656 ?
S8 K2 Ga1 91.81(4) 2_645 3_656 ?
S8 K2 Ga1 88.19(4) 4_566 3_656 ?
Ga1 K2 Ga1 180.000(10) . 3_656 ?
S3 K2 Ge1 144.68(3) 4_566 3_656 ?
S3 K2 Ge1 35.32(3) 2_645 3_656 ?
S4 K2 Ge1 35.48(4) 3_656 3_656 ?
S4 K2 Ge1 144.52(4) . 3_656 ?
S8 K2 Ge1 91.81(4) 2_645 3_656 ?
S8 K2 Ge1 88.19(4) 4_566 3_656 ?
Ga1 K2 Ge1 180.000(10) . 3_656 ?
Ga1 K2 Ge1 0.000(10) 3_656 3_656 ?
S1 Ga1 S3 115.47(8) . 4_566 ?
S1 Ga1 S2 120.40(8) . 4_566 ?
S3 Ga1 S2 95.11(7) 4_566 4_566 ?
S1 Ga1 S4 106.13(9) . . ?
S3 Ga1 S4 109.73(8) 4_566 . ?
S2 Ga1 S4 109.55(8) 4_566 . ?
S1 Ga1 K2 163.76(6) . . ?
S3 Ga1 K2 61.27(6) 4_566 . ?
S2 Ga1 K2 75.72(6) 4_566 . ?
S4 Ga1 K2 63.34(6) . . ?
S4 Ga2 S7 114.02(9) . 2_545 ?
S4 Ga2 S8 109.11(8) . 4_565 ?
S7 Ga2 S8 108.18(8) 2_545 4_565 ?
S4 Ga2 S8 113.52(8) . 2_545 ?
S7 Ga2 S8 113.06(8) 2_545 2_545 ?
S8 Ga2 S8 97.47(7) 4_565 2_545 ?
S4 Ga2 Ge2 123.43(7) . 3 ?
S7 Ga2 Ge2 122.26(6) 2_545 3 ?
S8 Ga2 Ge2 48.91(6) 4_565 3 ?
S8 Ga2 Ge2 48.56(5) 2_545 3 ?
S4 Ga2 Ga2 123.43(7) . 3 ?
S7 Ga2 Ga2 122.26(6) 2_545 3 ?
S8 Ga2 Ga2 48.91(6) 4_565 3 ?
S8 Ga2 Ga2 48.56(5) 2_545 3 ?
Ge2 Ga2 Ga2 0.00(3) 3 3 ?
S2 Ga3 S3 103.19(8) 3_565 3_665 ?
S2 Ga3 S9 106.59(8) 3_565 . ?
S3 Ga3 S9 110.80(8) 3_665 . ?
S2 Ga3 S7 114.70(8) 3_565 . ?
S3 Ga3 S7 115.04(8) 3_665 . ?
S9 Ga3 S7 106.29(9) . . ?
S2 Ga3 K1 69.24(8) 3_565 4_575 ?
S3 Ga3 K1 79.95(7) 3_665 4_575 ?
S9 Ga3 K1 56.39(7) . 4_575 ?
S7 Ga3 K1 161.51(8) . 4_575 ?
S5 Ga4 S1 109.43(8) . . ?
S5 Ga4 S6 117.80(8) . 4_566 ?
S1 Ga4 S6 112.82(8) . 4_566 ?
S5 Ga4 S9 94.04(8) . 2_645 ?
S1 Ga4 S9 112.26(8) . 2_645 ?
S6 Ga4 S9 109.09(8) 4_566 2_645 ?
S10 Ga5 S5 117.25(8) . . ?
S10 Ga5 S10 98.47(8) . 4_565 ?
S5 Ga5 S10 116.91(9) . 4_565 ?
S10 Ga5 S6 106.29(9) . . ?
S5 Ga5 S6 105.84(8) . . ?
S10 Ga5 S6 111.73(9) 4_565 . ?
Ga4 S1 Ga1 101.97(8) . . ?
Ga4 S1 K1 124.17(10) . 3_565 ?
Ga1 S1 K1 116.67(8) . 3_565 ?
Ge3 S2 Ga3 0.00(5) 3_565 3_565 ?
Ge3 S2 Ga1 101.44(8) 3_565 4_565 ?
Ga3 S2 Ga1 101.44(8) 3_565 4_565 ?
Ge3 S2 Ge1 101.44(8) 3_565 4_565 ?
Ga3 S2 Ge1 101.44(8) 3_565 4_565 ?
Ga1 S2 Ge1 0.00(5) 4_565 4_565 ?
Ge3 S3 Ga3 0.00(5) 3_665 3_665 ?
Ge3 S3 Ga1 99.81(8) 3_665 4_565 ?
Ga3 S3 Ga1 99.81(8) 3_665 4_565 ?
Ge3 S3 Ge1 99.81(8) 3_665 4_565 ?
Ga3 S3 Ge1 99.81(8) 3_665 4_565 ?
Ga1 S3 Ge1 0.00(5) 4_565 4_565 ?
Ge3 S3 K2 123.11(8) 3_665 2_655 ?
Ga3 S3 K2 123.11(8) 3_665 2_655 ?
Ga1 S3 K2 83.41(6) 4_565 2_655 ?
Ge1 S3 K2 83.41(6) 4_565 2_655 ?
Ga2 S4 Ga1 101.26(8) . . ?
Ga2 S4 K2 99.51(8) . . ?
Ga1 S4 K2 81.18(7) . . ?
Ga5 S5 Ga4 107.84(8) . . ?
Ge4 S6 Ga4 0.00(4) 4_565 4_565 ?
Ge4 S6 Ga5 102.29(8) 4_565 . ?
Ga4 S6 Ga5 102.29(8) 4_565 . ?
Ge4 S6 K1 134.73(9) 4_565 2_545 ?
Ga4 S6 K1 134.73(9) 4_565 2_545 ?
Ga5 S6 K1 84.97(8) . 2_545 ?
Ge4 S6 K1 88.90(8) 4_565 2_645 ?
Ga4 S6 K1 88.90(8) 4_565 2_645 ?
Ga5 S6 K1 113.90(9) . 2_645 ?
K1 S6 K1 129.24(9) 2_545 2_645 ?
Ga3 S7 Ge2 100.68(8) . 2 ?
Ga3 S7 Ga2 100.68(8) . 2 ?
Ge2 S7 Ga2 0.00(4) 2 2 ?
Ga3 S7 K1 95.37(9) . 4_576 ?
Ge2 S7 K1 134.10(10) 2 4_576 ?
Ga2 S7 K1 134.10(10) 2 4_576 ?
Ge2 S8 Ga2 0.00(4) 4_566 4_566 ?
Ge2 S8 Ge2 82.53(7) 4_566 2 ?
Ga2 S8 Ge2 82.53(7) 4_566 2 ?
Ge2 S8 Ga2 82.53(7) 4_566 2 ?
Ga2 S8 Ga2 82.53(7) 4_566 2 ?
Ge2 S8 Ga2 0.00(4) 2 2 ?
Ge2 S8 K2 104.58(7) 4_566 2_655 ?
Ga2 S8 K2 104.58(7) 4_566 2_655 ?
Ge2 S8 K2 128.12(8) 2 2_655 ?
Ga2 S8 K2 128.12(8) 2 2_655 ?
Ga3 S9 Ge4 102.98(8) . 2_655 ?
Ga3 S9 Ga4 102.98(8) . 2_655 ?
Ge4 S9 Ga4 0.00(6) 2_655 2_655 ?
Ga3 S9 K1 89.98(9) . 4_575 ?
Ge4 S9 K1 100.49(10) 2_655 4_575 ?
Ga4 S9 K1 100.49(10) 2_655 4_575 ?
Ga3 S9 K1 94.06(9) . 4_576 ?
Ge4 S9 K1 92.44(9) 2_655 4_576 ?
Ga4 S9 K1 92.44(9) 2_655 4_576 ?
K1 S9 K1 165.23(13) 4_575 4_576 ?
Ga5 S10 Ge5 100.76(8) . 4_566 ?
Ga5 S10 Ga5 100.76(8) . 4_566 ?
Ge5 S10 Ga5 0.00(5) 4_566 4_566 ?
Ga5 S10 K1 96.45(10) . 2_545 ?
Ge5 S10 K1 121.28(11) 4_566 2_545 ?
Ga5 S10 K1 121.28(11) 4_566 2_545 ?

_diffrn_measured_fraction_theta_max 0.994
_diffrn_reflns_theta_full        26.37
_diffrn_measured_fraction_theta_full 0.994
_refine_diff_density_max         1.808
_refine_diff_density_min         -1.222
_refine_diff_density_rms         0.245
####################################################################### 
# 
# 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_a
_database_code_depnum_ccdc_archive 'CCDC 1422760'
_audit_update_record             
;
2015-09-07 deposited with the CCDC.
2015-11-03 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'Ga3 Ge7 K3 Se20'
_chemical_formula_weight         2413.79

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'
Ge Ge 0.1547 1.8001 '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'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   P21/c

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

_cell_length_a                   7.0520(4)
_cell_length_b                   39.033(2)
_cell_length_c                   6.9488(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.433(5)
_cell_angle_gamma                90.00
_cell_volume                     1912.67(19)
_cell_formula_units_Z            2
_cell_measurement_temperature    153.1500
_cell_measurement_reflns_used    2293
_cell_measurement_theta_min      3.8900
_cell_measurement_theta_max      27.7420

_exptl_crystal_description       Prism
_exptl_crystal_colour            orange
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    4.191
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2108
_exptl_absorpt_coefficient_mu    26.854
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.49894
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   'face indexed'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      153.1500
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini ultra'
_diffrn_measurement_method       dtprofit.ref
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            13485
_diffrn_reflns_av_R_equivalents  0.0887
_diffrn_reflns_av_sigmaI/netI    0.0852
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -47
_diffrn_reflns_limit_k_max       48
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_theta_min         3.56
_diffrn_reflns_theta_max         26.37
_reflns_number_total             3915
_reflns_number_gt                3031
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0400P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   none
_refine_ls_hydrogen_treatment    none
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.00142(11)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         3915
_refine_ls_number_parameters     152
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0708
_refine_ls_R_factor_gt           0.0502
_refine_ls_wR_factor_ref         0.1160
_refine_ls_wR_factor_gt          0.1048
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_restrained_S_all      1.033
_refine_ls_shift/su_max          0.001
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
K1 K 0.0363(9) 0.83429(13) 0.1945(8) 0.129(2) Uani 1 1 d . . .
K2 K 0.5000 0.0000 0.5000 0.122(3) Uani 1 2 d S . .
Ga1 Ga 0.41506(13) 0.09195(3) 0.27271(17) 0.0168(3) Uani 0.30 1 d P . .
Ge1 Ge 0.41506(13) 0.09195(3) 0.27271(17) 0.0168(3) Uani 0.70 1 d P . .
Ga2 Ga 0.08860(13) 0.03581(3) 0.02505(17) 0.0175(3) Uani 0.30 1 d P . .
Ge2 Ge 0.08860(13) 0.03581(3) 0.02505(17) 0.0175(3) Uani 0.70 1 d P . .
Ga3 Ga 0.08905(12) 0.60397(3) 0.18171(17) 0.0167(3) Uani 0.30 1 d P . .
Ge3 Ge 0.08905(12) 0.60397(3) 0.18171(17) 0.0167(3) Uani 0.70 1 d P . .
Ga4 Ga 0.59998(13) 0.17838(2) 0.28343(17) 0.0174(3) Uani 0.30 1 d P . .
Ge4 Ge 0.59998(13) 0.17838(2) 0.28343(17) 0.0174(3) Uani 0.70 1 d P . .
Ga5 Ga 0.37485(13) 0.25996(3) 0.09974(17) 0.0197(3) Uani 0.30 1 d P . .
Ge5 Ge 0.37485(13) 0.25996(3) 0.09974(17) 0.0197(3) Uani 0.70 1 d P . .
Se1 Se 0.43327(14) 0.14110(3) 0.07577(17) 0.0236(3) Uani 1 1 d . . .
Se2 Se 0.16931(13) 0.41529(3) 0.00000(18) 0.0246(3) Uani 1 1 d . . .
Se3 Se 0.65711(13) 0.41389(3) 0.00816(17) 0.0242(3) Uani 1 1 d . . .
Se4 Se 0.41715(13) 0.04520(3) 0.0519(2) 0.0309(3) Uani 1 1 d . . .
Se5 Se 0.66183(13) 0.22956(3) 0.11694(18) 0.0238(3) Uani 1 1 d . . .
Se6 Se 0.46297(15) 0.31859(3) 0.09200(18) 0.0272(3) Uani 1 1 d . . .
Se7 Se 0.10017(14) 0.58550(3) 0.50407(17) 0.0254(3) Uani 1 1 d . . .
Se8 Se 0.03259(14) 0.49695(3) 0.24383(17) 0.0250(3) Uani 1 1 d . . .
Se9 Se 0.07129(13) 0.66449(3) 0.18851(18) 0.0235(3) Uani 1 1 d . . .
Se10 Se 0.16064(14) 0.25471(3) 0.35370(19) 0.0320(3) Uani 1 1 d . . .


_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
K1 Se10 3.418(5) 2 ?
K1 Se7 3.430(5) 4_575 ?
K1 Se9 3.440(5) 4_576 ?
K1 Se9 3.527(5) 4_575 ?
K1 Se6 3.869(6) 2_655 ?
K1 Se6 3.880(6) 2 ?
K1 Se1 3.914(6) 3_565 ?
K1 Se5 3.936(7) 3_665 ?
K2 Se3 3.5392(11) 4_566 ?
K2 Se3 3.5392(11) 2_645 ?
K2 Se4 3.6225(14) . ?
K2 Se4 3.6225(14) 3_656 ?
K2 Se8 3.7194(11) 2_645 ?
K2 Se8 3.7194(11) 4_566 ?
K2 Ga1 3.9648(11) . ?
K2 Ga1 3.9648(11) 3_656 ?
K2 Ge1 3.9648(11) 3_656 ?
Ga1 Se1 2.3607(15) . ?
Ga1 Se3 2.3665(15) 4_566 ?
Ga1 Se2 2.3704(15) 4_566 ?
Ga1 Se4 2.3841(15) . ?
Ga2 Se4 2.3518(13) . ?
Ga2 Se7 2.3601(14) 2_545 ?
Ga2 Se8 2.3661(15) 4_565 ?
Ga2 Se8 2.3731(16) 2_545 ?
Ga3 Se2 2.3333(14) 3_565 ?
Ga3 Se3 2.3382(14) 3_665 ?
Ga3 Se7 2.3539(16) . ?
Ga3 Se9 2.3660(14) . ?
Ga4 Se5 2.3509(14) . ?
Ga4 Se1 2.3570(15) . ?
Ga4 Se6 2.3615(17) 4_566 ?
Ga4 Se9 2.3873(13) 2_645 ?
Ga5 Se10 2.3406(16) . ?
Ga5 Se10 2.3439(16) 4_565 ?
Ga5 Se5 2.3484(13) . ?
Ga5 Se6 2.3721(14) . ?
Se1 K1 3.914(6) 3_565 ?
Se2 Ge3 2.3333(14) 3_565 ?
Se2 Ga3 2.3333(14) 3_565 ?
Se2 Ga1 2.3704(15) 4_565 ?
Se2 Ge1 2.3704(15) 4_565 ?
Se3 Ge3 2.3382(14) 3_665 ?
Se3 Ga3 2.3382(14) 3_665 ?
Se3 Ga1 2.3665(15) 4_565 ?
Se3 Ge1 2.3665(15) 4_565 ?
Se3 K2 3.5392(11) 2_655 ?
Se5 K1 3.936(7) 3_665 ?
Se6 Ge4 2.3615(17) 4_565 ?
Se6 Ga4 2.3615(17) 4_565 ?
Se6 K1 3.869(6) 2_645 ?
Se6 K1 3.880(6) 2_545 ?
Se7 Ge2 2.3601(14) 2 ?
Se7 Ga2 2.3601(14) 2 ?
Se7 K1 3.430(5) 4_576 ?
Se8 Ge2 2.3661(15) 4_566 ?
Se8 Ga2 2.3661(15) 4_566 ?
Se8 Ge2 2.3731(16) 2 ?
Se8 Ga2 2.3731(16) 2 ?
Se8 K2 3.7194(11) 2_655 ?
Se9 Ge4 2.3873(13) 2_655 ?
Se9 Ga4 2.3873(13) 2_655 ?
Se9 K1 3.440(5) 4_575 ?
Se9 K1 3.527(5) 4_576 ?
Se10 Ge5 2.3439(16) 4_566 ?
Se10 Ga5 2.3439(16) 4_566 ?
Se10 K1 3.418(5) 2_545 ?

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
Se10 K1 Se7 147.80(17) 2 4_575 ?
Se10 K1 Se9 97.83(12) 2 4_576 ?
Se7 K1 Se9 111.33(14) 4_575 4_576 ?
Se10 K1 Se9 86.91(12) 2 4_575 ?
Se7 K1 Se9 65.97(9) 4_575 4_575 ?
Se9 K1 Se9 171.7(2) 4_576 4_575 ?
Se10 K1 Se6 105.22(15) 2 2_655 ?
Se7 K1 Se6 99.81(12) 4_575 2_655 ?
Se9 K1 Se6 63.97(10) 4_576 2_655 ?
Se9 K1 Se6 108.30(17) 4_575 2_655 ?
Se10 K1 Se6 61.62(9) 2 2 ?
Se7 K1 Se6 114.45(18) 4_575 2 ?
Se9 K1 Se6 71.28(11) 4_576 2 ?
Se9 K1 Se6 117.00(15) 4_575 2 ?
Se6 K1 Se6 131.04(14) 2_655 2 ?
Se10 K1 Se1 80.47(11) 2 3_565 ?
Se7 K1 Se1 72.78(11) 4_575 3_565 ?
Se9 K1 Se1 121.97(18) 4_576 3_565 ?
Se9 K1 Se1 65.40(10) 4_575 3_565 ?
Se6 K1 Se1 171.61(14) 2_655 3_565 ?
Se6 K1 Se1 57.00(9) 2 3_565 ?
Se10 K1 Se5 65.91(10) 2 3_665 ?
Se7 K1 Se5 107.02(14) 4_575 3_665 ?
Se9 K1 Se5 121.48(17) 4_576 3_665 ?
Se9 K1 Se5 54.43(9) 4_575 3_665 ?
Se6 K1 Se5 67.34(11) 2_655 3_665 ?
Se6 K1 Se5 127.33(12) 2 3_665 ?
Se1 K1 Se5 110.53(13) 3_565 3_665 ?
Se3 K2 Se3 180.000(11) 4_566 2_645 ?
Se3 K2 Se4 66.40(3) 4_566 . ?
Se3 K2 Se4 113.60(3) 2_645 . ?
Se3 K2 Se4 113.60(3) 4_566 3_656 ?
Se3 K2 Se4 66.40(3) 2_645 3_656 ?
Se4 K2 Se4 180.00(3) . 3_656 ?
Se3 K2 Se8 76.07(2) 4_566 2_645 ?
Se3 K2 Se8 103.93(2) 2_645 2_645 ?
Se4 K2 Se8 76.22(2) . 2_645 ?
Se4 K2 Se8 103.78(2) 3_656 2_645 ?
Se3 K2 Se8 103.93(2) 4_566 4_566 ?
Se3 K2 Se8 76.07(2) 2_645 4_566 ?
Se4 K2 Se8 103.78(2) . 4_566 ?
Se4 K2 Se8 76.22(2) 3_656 4_566 ?
Se8 K2 Se8 180.0 2_645 4_566 ?
Se3 K2 Ga1 36.21(2) 4_566 . ?
Se3 K2 Ga1 143.79(2) 2_645 . ?
Se4 K2 Ga1 36.27(2) . . ?
Se4 K2 Ga1 143.73(2) 3_656 . ?
Se8 K2 Ga1 88.81(2) 2_645 . ?
Se8 K2 Ga1 91.19(2) 4_566 . ?
Se3 K2 Ga1 143.79(2) 4_566 3_656 ?
Se3 K2 Ga1 36.21(2) 2_645 3_656 ?
Se4 K2 Ga1 143.73(2) . 3_656 ?
Se4 K2 Ga1 36.27(2) 3_656 3_656 ?
Se8 K2 Ga1 91.19(2) 2_645 3_656 ?
Se8 K2 Ga1 88.81(2) 4_566 3_656 ?
Ga1 K2 Ga1 180.00(3) . 3_656 ?
Se3 K2 Ge1 143.79(2) 4_566 3_656 ?
Se3 K2 Ge1 36.21(2) 2_645 3_656 ?
Se4 K2 Ge1 143.73(2) . 3_656 ?
Se4 K2 Ge1 36.27(2) 3_656 3_656 ?
Se8 K2 Ge1 91.19(2) 2_645 3_656 ?
Se8 K2 Ge1 88.81(2) 4_566 3_656 ?
Ga1 K2 Ge1 180.00(3) . 3_656 ?
Ga1 K2 Ge1 0.000(12) 3_656 3_656 ?
Se1 Ga1 Se3 115.91(5) . 4_566 ?
Se1 Ga1 Se2 121.76(5) . 4_566 ?
Se3 Ga1 Se2 93.15(6) 4_566 4_566 ?
Se1 Ga1 Se4 104.38(6) . . ?
Se3 Ga1 Se4 111.30(5) 4_566 . ?
Se2 Ga1 Se4 110.23(5) 4_566 . ?
Se1 Ga1 K2 163.31(5) . . ?
Se3 Ga1 K2 62.05(3) 4_566 . ?
Se2 Ga1 K2 74.68(4) 4_566 . ?
Se4 Ga1 K2 64.02(4) . . ?
Se4 Ga2 Se7 115.69(6) . 2_545 ?
Se4 Ga2 Se8 107.93(5) . 4_565 ?
Se7 Ga2 Se8 106.43(6) 2_545 4_565 ?
Se4 Ga2 Se8 113.92(6) . 2_545 ?
Se7 Ga2 Se8 112.18(6) 2_545 2_545 ?
Se8 Ga2 Se8 98.90(5) 4_565 2_545 ?
Se2 Ga3 Se3 101.34(6) 3_565 3_665 ?
Se2 Ga3 Se7 115.88(6) 3_565 . ?
Se3 Ga3 Se7 115.18(6) 3_665 . ?
Se2 Ga3 Se9 106.93(5) 3_565 . ?
Se3 Ga3 Se9 110.48(5) 3_665 . ?
Se7 Ga3 Se9 106.75(6) . . ?
Se5 Ga4 Se1 108.47(6) . . ?
Se5 Ga4 Se6 118.88(6) . 4_566 ?
Se1 Ga4 Se6 112.41(6) . 4_566 ?
Se5 Ga4 Se9 92.83(5) . 2_645 ?
Se1 Ga4 Se9 112.92(6) . 2_645 ?
Se6 Ga4 Se9 109.93(6) 4_566 2_645 ?
Se10 Ga5 Se10 96.46(5) . 4_565 ?
Se10 Ga5 Se5 118.57(6) . . ?
Se10 Ga5 Se5 117.65(6) 4_565 . ?
Se10 Ga5 Se6 105.80(6) . . ?
Se10 Ga5 Se6 112.75(6) 4_565 . ?
Se5 Ga5 Se6 105.24(5) . . ?
Ga4 Se1 Ga1 100.13(6) . . ?
Ga4 Se1 K1 123.95(9) . 3_565 ?
Ga1 Se1 K1 115.34(8) . 3_565 ?
Ge3 Se2 Ga3 0.00(5) 3_565 3_565 ?
Ge3 Se2 Ga1 99.95(6) 3_565 4_565 ?
Ga3 Se2 Ga1 99.95(6) 3_565 4_565 ?
Ge3 Se2 Ge1 99.95(6) 3_565 4_565 ?
Ga3 Se2 Ge1 99.95(6) 3_565 4_565 ?
Ga1 Se2 Ge1 0.00(6) 4_565 4_565 ?
Ge3 Se3 Ga3 0.00(7) 3_665 3_665 ?
Ge3 Se3 Ga1 97.61(6) 3_665 4_565 ?
Ga3 Se3 Ga1 97.61(6) 3_665 4_565 ?
Ge3 Se3 Ge1 97.61(6) 3_665 4_565 ?
Ga3 Se3 Ge1 97.61(6) 3_665 4_565 ?
Ga1 Se3 Ge1 0.00(6) 4_565 4_565 ?
Ge3 Se3 K2 121.00(5) 3_665 2_655 ?
Ga3 Se3 K2 121.00(5) 3_665 2_655 ?
Ga1 Se3 K2 81.74(4) 4_565 2_655 ?
Ge1 Se3 K2 81.74(4) 4_565 2_655 ?
Ga2 Se4 Ga1 99.17(5) . . ?
Ga2 Se4 K2 98.32(5) . . ?
Ga1 Se4 K2 79.71(5) . . ?
Ga5 Se5 Ga4 106.95(5) . . ?
Ga5 Se5 K1 139.59(10) . 3_665 ?
Ga4 Se5 K1 80.54(8) . 3_665 ?
Ge4 Se6 Ga4 0.00(5) 4_565 4_565 ?
Ge4 Se6 Ga5 100.25(5) 4_565 . ?
Ga4 Se6 Ga5 100.25(5) 4_565 . ?
Ge4 Se6 K1 87.81(9) 4_565 2_645 ?
Ga4 Se6 K1 87.81(9) 4_565 2_645 ?
Ga5 Se6 K1 112.50(9) . 2_645 ?
Ge4 Se6 K1 135.89(9) 4_565 2_545 ?
Ga4 Se6 K1 135.89(9) 4_565 2_545 ?
Ga5 Se6 K1 84.55(9) . 2_545 ?
K1 Se6 K1 131.04(14) 2_645 2_545 ?
Ga3 Se7 Ge2 98.94(6) . 2 ?
Ga3 Se7 Ga2 98.94(6) . 2 ?
Ge2 Se7 Ga2 0.00(5) 2 2 ?
Ga3 Se7 K1 94.82(10) . 4_576 ?
Ge2 Se7 K1 135.03(13) 2 4_576 ?
Ga2 Se7 K1 135.03(13) 2 4_576 ?
Ge2 Se8 Ga2 0.00(5) 4_566 4_566 ?
Ge2 Se8 Ge2 81.10(5) 4_566 2 ?
Ga2 Se8 Ge2 81.10(5) 4_566 2 ?
Ge2 Se8 Ga2 81.10(5) 4_566 2 ?
Ga2 Se8 Ga2 81.10(5) 4_566 2 ?
Ge2 Se8 Ga2 0.00(5) 2 2 ?
Ge2 Se8 K2 104.51(4) 4_566 2_655 ?
Ga2 Se8 K2 104.51(4) 4_566 2_655 ?
Ge2 Se8 K2 127.79(5) 2 2_655 ?
Ga2 Se8 K2 127.79(5) 2 2_655 ?
Ga3 Se9 Ge4 100.18(5) . 2_655 ?
Ga3 Se9 Ga4 100.18(5) . 2_655 ?
Ge4 Se9 Ga4 0.00(7) 2_655 2_655 ?
Ga3 Se9 K1 89.84(9) . 4_575 ?
Ge4 Se9 K1 98.09(12) 2_655 4_575 ?
Ga4 Se9 K1 98.09(12) 2_655 4_575 ?
Ga3 Se9 K1 92.15(9) . 4_576 ?
Ge4 Se9 K1 89.47(12) 2_655 4_576 ?
Ga4 Se9 K1 89.47(12) 2_655 4_576 ?
K1 Se9 K1 171.7(2) 4_575 4_576 ?
Ga5 Se10 Ge5 98.93(5) . 4_566 ?
Ga5 Se10 Ga5 98.93(5) . 4_566 ?
Ge5 Se10 Ga5 0.00(6) 4_566 4_566 ?
Ga5 Se10 K1 96.35(11) . 2_545 ?
Ge5 Se10 K1 123.54(11) 4_566 2_545 ?
Ga5 Se10 K1 123.54(11) 4_566 2_545 ?

_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full        26.37
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max         1.418
_refine_diff_density_min         -1.559
_refine_diff_density_rms         0.321
