# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2017

####################################################################### 
# 
# 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_Ba4Si3Se9Cl2
_database_code_depnum_ccdc_archive 'CCDC 1516718'
_audit_update_record             
;
2016-11-11 deposited with the CCDC.
2017-01-27 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'Ba4 Cl2 Se9 Si3'
_chemical_formula_weight         1415.17

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'
Cl Cl 0.1484 0.1585 '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'
Ba Ba -0.3244 2.2819 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Hexagonal
_symmetry_space_group_name_H-M   P63

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

_cell_length_a                   10.0024(16)
_cell_length_b                   10.0024(16)
_cell_length_c                   12.406(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_volume                     1074.9(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    3715
_cell_measurement_theta_min      2.3501
_cell_measurement_theta_max      27.4700

_exptl_crystal_description       block
_exptl_crystal_colour            dark-red
_exptl_crystal_size_max          0.2000
_exptl_crystal_size_mid          0.2000
_exptl_crystal_size_min          0.2000
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    4.373
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1212
_exptl_absorpt_coefficient_mu    22.864
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.5611
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(2)
_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  CCD
_diffrn_measurement_device       
;
Saturn724+ (2x2 bin mode)
;
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            6731
_diffrn_reflns_av_R_equivalents  0.0373
_diffrn_reflns_av_sigmaI/netI    0.0391
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         2.35
_diffrn_reflns_theta_max         27.49
_reflns_number_total             1639
_reflns_number_gt                1564
_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)+(0.0118P)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       0.00383(15)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.057(13)
_refine_ls_number_reflns         1639
_refine_ls_number_parameters     56
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0194
_refine_ls_R_factor_gt           0.0186
_refine_ls_wR_factor_ref         0.0383
_refine_ls_wR_factor_gt          0.0382
_refine_ls_goodness_of_fit_ref   1.009
_refine_ls_restrained_S_all      1.009
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.001

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
Ba1 Ba 0.67132(3) 0.92077(3) 0.91768(3) 0.01952(9) Uani 1 1 d . . .
Ba2 Ba 0.3333 0.6667 1.22473(5) 0.01701(14) Uani 1 3 d S . .
Si1 Si 0.55280(15) 0.88150(15) 0.58187(12) 0.0127(3) Uani 1 1 d . . .
Se1 Se 0.75636(6) 1.06603(6) 0.66724(5) 0.01778(13) Uani 1 1 d . . .
Se2 Se 0.66139(6) 1.11476(6) 1.14786(5) 0.01604(13) Uani 1 1 d . . .
Se3 Se 0.91057(6) 1.33721(6) 0.90464(5) 0.01674(12) Uani 1 1 d . . .
Cl1 Cl 0.3333 0.6667 0.9717(2) 0.0207(5) Uani 1 3 d S . .
Cl2 Cl 1.0000 1.0000 0.9186(4) 0.0477(9) Uani 1 3 d S . .

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 0.01958(17) 0.01943(16) 0.0199(2) 0.00409(16) 0.00413(15) 0.01002(13)
Ba2 0.02053(18) 0.02053(18) 0.0100(3) 0.000 0.000 0.01026(9)
Si1 0.0149(7) 0.0132(7) 0.0091(8) -0.0012(6) -0.0007(6) 0.0064(6)
Se1 0.0179(3) 0.0171(3) 0.0129(3) -0.0024(2) -0.0030(2) 0.0047(2)
Se2 0.0166(3) 0.0174(3) 0.0136(3) 0.0040(2) 0.0000(2) 0.0082(2)
Se3 0.0197(3) 0.0244(3) 0.0082(3) 0.0000(2) -0.0010(2) 0.0126(2)
Cl1 0.0204(7) 0.0204(7) 0.0212(14) 0.000 0.000 0.0102(4)
Cl2 0.0201(7) 0.0201(7) 0.103(3) 0.000 0.000 0.0101(3)

_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 Cl2 2.9717(6) . ?
Ba1 Cl1 3.1219(8) . ?
Ba1 Se1 3.3543(10) . ?
Ba1 Se3 3.4369(8) 2_765 ?
Ba1 Se2 3.4816(9) . ?
Ba1 Se1 3.5550(10) 6_655 ?
Ba1 Se3 3.6042(8) 3_575 ?
Ba1 Se3 3.6243(8) . ?
Ba1 Ba2 4.7909(8) 4_674 ?
Ba2 Cl1 3.138(3) . ?
Ba2 Se3 3.2924(8) 4_675 ?
Ba2 Se3 3.2924(8) 6_655 ?
Ba2 Se3 3.2924(8) 5_455 ?
Ba2 Se1 3.2956(7) 4_675 ?
Ba2 Se1 3.2956(7) 5_455 ?
Ba2 Se1 3.2956(7) 6_655 ?
Ba2 Ba1 4.7909(8) 4_675 ?
Ba2 Ba1 4.7909(8) 5_455 ?
Ba2 Ba1 4.7909(8) 6_655 ?
Si1 Se1 2.2171(15) . ?
Si1 Se3 2.2139(17) 6_654 ?
Si1 Se2 2.3112(15) 4_674 ?
Si1 Se2 2.3207(15) 6_654 ?
Se1 Ba2 3.2956(7) 4_674 ?
Se1 Ba1 3.5550(10) 5_564 ?
Se2 Si1 2.3112(15) 4_675 ?
Se2 Si1 2.3207(15) 5_565 ?
Se3 Si1 2.2139(17) 5_565 ?
Se3 Ba2 3.2924(8) 4_674 ?
Se3 Ba1 3.4369(8) 3_675 ?
Se3 Ba1 3.6042(8) 2_775 ?
Cl1 Ba1 3.1219(8) 2_665 ?
Cl1 Ba1 3.1219(8) 3_565 ?
Cl2 Ba1 2.9717(6) 3_675 ?
Cl2 Ba1 2.9717(6) 2_765 ?

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
Cl2 Ba1 Cl1 145.04(4) . . ?
Cl2 Ba1 Se1 83.16(8) . . ?
Cl1 Ba1 Se1 119.24(5) . . ?
Cl2 Ba1 Se3 74.615(11) . 2_765 ?
Cl1 Ba1 Se3 73.597(12) . 2_765 ?
Se1 Ba1 Se3 105.489(17) . 2_765 ?
Cl2 Ba1 Se2 100.62(7) . . ?
Cl1 Ba1 Se2 87.51(4) . . ?
Se1 Ba1 Se2 126.158(19) . . ?
Se3 Ba1 Se2 127.509(19) 2_765 . ?
Cl2 Ba1 Se1 79.17(8) . 6_655 ?
Cl1 Ba1 Se1 73.91(4) . 6_655 ?
Se1 Ba1 Se1 161.149(19) . 6_655 ?
Se3 Ba1 Se1 63.468(16) 2_765 6_655 ?
Se2 Ba1 Se1 64.32(2) . 6_655 ?
Cl2 Ba1 Se3 142.650(14) . 3_575 ?
Cl1 Ba1 Se3 71.239(12) . 3_575 ?
Se1 Ba1 Se3 80.802(15) . 3_575 ?
Se3 Ba1 Se3 142.347(16) 2_765 3_575 ?
Se2 Ba1 Se3 63.942(15) . 3_575 ?
Se1 Ba1 Se3 117.486(17) 6_655 3_575 ?
Cl2 Ba1 Se3 71.759(11) . . ?
Cl1 Ba1 Se3 140.287(15) . . ?
Se1 Ba1 Se3 65.299(15) . . ?
Se3 Ba1 Se3 145.920(15) 2_765 . ?
Se2 Ba1 Se3 65.327(15) . . ?
Se1 Ba1 Se3 114.409(17) 6_655 . ?
Se3 Ba1 Se3 70.898(17) 3_575 . ?
Cl2 Ba1 Ba2 104.96(5) . 4_674 ?
Cl1 Ba1 Ba2 109.61(2) . 4_674 ?
Se1 Ba1 Ba2 43.424(11) . 4_674 ?
Se3 Ba1 Ba2 147.281(18) 2_765 4_674 ?
Se2 Ba1 Ba2 85.095(19) . 4_674 ?
Se1 Ba1 Ba2 149.246(13) 6_655 4_674 ?
Se3 Ba1 Ba2 43.373(11) 3_575 4_674 ?
Se3 Ba1 Ba2 43.361(11) . 4_674 ?
Cl1 Ba2 Se3 132.678(15) . 4_675 ?
Cl1 Ba2 Se3 132.678(15) . 6_655 ?
Se3 Ba2 Se3 79.09(2) 4_675 6_655 ?
Cl1 Ba2 Se3 132.678(15) . 5_455 ?
Se3 Ba2 Se3 79.09(2) 4_675 5_455 ?
Se3 Ba2 Se3 79.09(2) 6_655 5_455 ?
Cl1 Ba2 Se1 77.502(15) . 4_675 ?
Se3 Ba2 Se1 69.853(16) 4_675 4_675 ?
Se3 Ba2 Se1 86.502(15) 6_655 4_675 ?
Se3 Ba2 Se1 147.73(2) 5_455 4_675 ?
Cl1 Ba2 Se1 77.502(15) . 5_455 ?
Se3 Ba2 Se1 86.502(15) 4_675 5_455 ?
Se3 Ba2 Se1 147.73(2) 6_655 5_455 ?
Se3 Ba2 Se1 69.853(16) 5_455 5_455 ?
Se1 Ba2 Se1 115.452(11) 4_675 5_455 ?
Cl1 Ba2 Se1 77.502(15) . 6_655 ?
Se3 Ba2 Se1 147.73(2) 4_675 6_655 ?
Se3 Ba2 Se1 69.853(16) 6_655 6_655 ?
Se3 Ba2 Se1 86.502(15) 5_455 6_655 ?
Se1 Ba2 Se1 115.452(11) 4_675 6_655 ?
Se1 Ba2 Se1 115.452(11) 5_455 6_655 ?
Cl1 Ba2 Ba1 119.976(10) . 4_675 ?
Se3 Ba2 Ba1 49.095(11) 4_675 4_675 ?
Se3 Ba2 Ba1 48.745(11) 6_655 4_675 ?
Se3 Ba2 Ba1 107.35(2) 5_455 4_675 ?
Se1 Ba2 Ba1 44.398(16) 4_675 4_675 ?
Se1 Ba2 Ba1 133.582(12) 5_455 4_675 ?
Se1 Ba2 Ba1 110.456(11) 6_655 4_675 ?
Cl1 Ba2 Ba1 119.976(10) . 5_455 ?
Se3 Ba2 Ba1 48.745(11) 4_675 5_455 ?
Se3 Ba2 Ba1 107.35(2) 6_655 5_455 ?
Se3 Ba2 Ba1 49.095(11) 5_455 5_455 ?
Se1 Ba2 Ba1 110.456(11) 4_675 5_455 ?
Se1 Ba2 Ba1 44.398(16) 5_455 5_455 ?
Se1 Ba2 Ba1 133.582(12) 6_655 5_455 ?
Ba1 Ba2 Ba1 97.213(13) 4_675 5_455 ?
Cl1 Ba2 Ba1 119.976(10) . 6_655 ?
Se3 Ba2 Ba1 107.35(2) 4_675 6_655 ?
Se3 Ba2 Ba1 49.095(11) 6_655 6_655 ?
Se3 Ba2 Ba1 48.745(11) 5_455 6_655 ?
Se1 Ba2 Ba1 133.582(12) 4_675 6_655 ?
Se1 Ba2 Ba1 110.456(11) 5_455 6_655 ?
Se1 Ba2 Ba1 44.398(16) 6_655 6_655 ?
Ba1 Ba2 Ba1 97.213(13) 4_675 6_655 ?
Ba1 Ba2 Ba1 97.213(13) 5_455 6_655 ?
Se1 Si1 Se3 112.25(6) . 6_654 ?
Se1 Si1 Se2 106.87(6) . 4_674 ?
Se3 Si1 Se2 112.06(6) 6_654 4_674 ?
Se1 Si1 Se2 101.48(6) . 6_654 ?
Se3 Si1 Se2 115.57(6) 6_654 6_654 ?
Se2 Si1 Se2 107.77(6) 4_674 6_654 ?
Si1 Se1 Ba2 105.64(4) . 4_674 ?
Si1 Se1 Ba1 98.82(4) . . ?
Ba2 Se1 Ba1 92.179(19) 4_674 . ?
Si1 Se1 Ba1 90.51(5) . 5_564 ?
Ba2 Se1 Ba1 90.750(18) 4_674 5_564 ?
Ba1 Se1 Ba1 169.067(19) . 5_564 ?
Si1 Se2 Si1 108.65(7) 4_675 5_565 ?
Si1 Se2 Ba1 90.20(4) 4_675 . ?
Si1 Se2 Ba1 86.92(4) 5_565 . ?
Si1 Se3 Ba2 126.19(4) 5_565 4_674 ?
Si1 Se3 Ba1 93.70(4) 5_565 3_675 ?
Ba2 Se3 Ba1 139.98(2) 4_674 3_675 ?
Si1 Se3 Ba1 88.66(4) 5_565 2_775 ?
Ba2 Se3 Ba1 87.881(13) 4_674 2_775 ?
Ba1 Se3 Ba1 97.158(16) 3_675 2_775 ?
Si1 Se3 Ba1 85.00(4) 5_565 . ?
Ba2 Se3 Ba1 87.544(13) 4_674 . ?
Ba1 Se3 Ba1 93.556(14) 3_675 . ?
Ba1 Se3 Ba1 167.883(18) 2_775 . ?
Ba1 Cl1 Ba1 115.52(3) 2_665 . ?
Ba1 Cl1 Ba1 115.52(3) 2_665 3_565 ?
Ba1 Cl1 Ba1 115.52(3) . 3_565 ?
Ba1 Cl1 Ba2 102.41(5) 2_665 . ?
Ba1 Cl1 Ba2 102.41(5) . . ?
Ba1 Cl1 Ba2 102.41(5) 3_565 . ?
Ba1 Cl2 Ba1 119.999(1) 3_675 . ?
Ba1 Cl2 Ba1 119.999(1) 3_675 2_765 ?
Ba1 Cl2 Ba1 119.998(1) . 2_765 ?

_diffrn_measured_fraction_theta_max 0.995
_diffrn_reflns_theta_full        27.49
_diffrn_measured_fraction_theta_full 0.995
_refine_diff_density_max         1.447
_refine_diff_density_min         -0.607
_refine_diff_density_rms         0.144
####################################################################### 
# 
# 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_Ba4Ge3S9Cl2
_database_code_depnum_ccdc_archive 'CCDC 1516717'
_audit_update_record             
;
2016-11-11 deposited with the CCDC.
2017-01-27 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'Ba4 Cl2 Ge3 S9'
_chemical_formula_weight         1126.57

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 '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'
Ba Ba -0.3244 2.2819 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Hexagonal
_symmetry_space_group_name_H-M   P63

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

_cell_length_a                   9.8200(4)
_cell_length_b                   9.8200(4)
_cell_length_c                   12.0544(12)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_volume                     1006.70(12)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    2956
_cell_measurement_theta_min      2.3949
_cell_measurement_theta_max      27.4277

_exptl_crystal_description       block
_exptl_crystal_colour            'light yellow'
_exptl_crystal_size_max          0.2000
_exptl_crystal_size_mid          0.2000
_exptl_crystal_size_min          0.2000
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    3.717
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             996
_exptl_absorpt_coefficient_mu    13.288
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.8082
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_detector       CCD
_diffrn_measurement_device       
;
Mercury70 (2x2 bin mode)
;
_diffrn_measurement_device_type  ?
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            7891
_diffrn_reflns_av_R_equivalents  0.0292
_diffrn_reflns_av_sigmaI/netI    0.0252
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         2.93
_diffrn_reflns_theta_max         27.43
_reflns_number_total             1480
_reflns_number_gt                1424
_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)+(0.0072P)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       0.00254(11)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.024(12)
_refine_ls_number_reflns         1480
_refine_ls_number_parameters     56
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0179
_refine_ls_R_factor_gt           0.0161
_refine_ls_wR_factor_ref         0.0278
_refine_ls_wR_factor_gt          0.0274
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_restrained_S_all      1.011
_refine_ls_shift/su_max          0.010
_refine_ls_shift/su_mean         0.002

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
Ba1 Ba 0.67101(2) 0.92154(2) 0.02475(2) 0.02027(7) Uani 1 1 d . . .
Ba2 Ba 0.6667 1.3333 0.20788(3) 0.01497(9) Uani 1 3 d S . .
Ge1 Ge 0.88408(4) 1.33218(4) -0.14327(3) 0.01275(9) Uani 1 1 d . . .
S1 S 0.91345(10) 1.33908(10) 0.03490(10) 0.01782(19) Uani 1 1 d . . .
S2 S 0.74987(10) 1.06989(10) 0.26941(8) 0.0168(2) Uani 1 1 d . . .
S3 S 0.66524(10) 1.11660(10) -0.20703(9) 0.0172(2) Uani 1 1 d . . .
Cl1 Cl 0.3333 0.6667 -0.03169(14) 0.0190(4) Uani 1 3 d S . .
Cl2 Cl 1.0000 1.0000 0.0008(3) 0.0581(10) Uani 1 3 d S . .

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 0.01763(11) 0.01907(11) 0.02410(15) -0.00449(12) -0.00418(12) 0.00916(9)
Ba2 0.01662(11) 0.01662(11) 0.0117(2) 0.000 0.000 0.00831(6)
Ge1 0.01173(17) 0.01447(18) 0.0124(2) 0.00054(17) 0.00204(17) 0.00677(14)
S1 0.0185(4) 0.0256(4) 0.0117(5) 0.0007(5) 0.0023(4) 0.0128(4)
S2 0.0156(4) 0.0147(4) 0.0158(6) 0.0031(4) 0.0033(4) 0.0044(3)
S3 0.0158(4) 0.0168(4) 0.0185(6) -0.0042(4) 0.0006(4) 0.0078(4)
Cl1 0.0174(5) 0.0174(5) 0.0221(10) 0.000 0.000 0.0087(2)
Cl2 0.0177(5) 0.0177(5) 0.139(3) 0.000 0.000 0.0088(2)

_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 Cl2 2.9369(4) . ?
Ba1 Cl1 3.0697(4) . ?
Ba1 S2 3.2082(11) . ?
Ba1 S1 3.3629(9) 2_765 ?
Ba1 S3 3.4040(11) . ?
Ba1 S1 3.5145(9) 3_575 ?
Ba1 S2 3.5315(11) 6_654 ?
Ba1 S1 3.5684(9) . ?
Ba1 Ba2 4.6261(3) . ?
Ba2 Cl1 3.1393(17) 4_675 ?
Ba2 S2 3.1661(9) . ?
Ba2 S2 3.1661(9) 2_775 ?
Ba2 S2 3.1661(9) 3_575 ?
Ba2 S1 3.1761(10) . ?
Ba2 S1 3.1761(10) 3_575 ?
Ba2 S1 3.1761(10) 2_775 ?
Ba2 Ba1 4.6261(3) 2_775 ?
Ba2 Ba1 4.6261(3) 3_575 ?
Ge1 S2 2.1609(9) 5_564 ?
Ge1 S1 2.1636(12) . ?
Ge1 S3 2.2674(10) . ?
Ge1 S3 2.2635(10) 2_775 ?
S1 Ba1 3.3629(9) 3_675 ?
S1 Ba1 3.5145(9) 2_775 ?
S2 Ge1 2.1609(9) 6_655 ?
S2 Ba1 3.5315(11) 5_565 ?
S3 Ge1 2.2635(10) 3_575 ?
Cl1 Ba1 3.0697(4) 2_665 ?
Cl1 Ba1 3.0697(4) 3_565 ?
Cl1 Ba2 3.1393(17) 4_674 ?
Cl2 Ba1 2.9369(4) 3_675 ?
Cl2 Ba1 2.9369(4) 2_765 ?

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
Cl2 Ba1 Cl1 142.21(3) . . ?
Cl2 Ba1 S2 89.26(6) . . ?
Cl1 Ba1 S2 119.41(3) . . ?
Cl2 Ba1 S1 74.959(16) . 2_765 ?
Cl1 Ba1 S1 73.098(16) . 2_765 ?
S2 Ba1 S1 107.75(3) . 2_765 ?
Cl2 Ba1 S3 95.58(5) . . ?
Cl1 Ba1 S3 87.81(3) . . ?
S2 Ba1 S3 124.55(2) . . ?
S1 Ba1 S3 126.87(3) 2_765 . ?
Cl2 Ba1 S1 143.163(16) . 3_575 ?
Cl1 Ba1 S1 70.943(16) . 3_575 ?
S2 Ba1 S1 79.87(3) . 3_575 ?
S1 Ba1 S1 141.88(2) 2_765 3_575 ?
S3 Ba1 S1 63.96(2) . 3_575 ?
Cl2 Ba1 S2 75.69(6) . 6_654 ?
Cl1 Ba1 S2 72.08(3) . 6_654 ?
S2 Ba1 S2 163.74(3) . 6_654 ?
S1 Ba1 S2 62.80(2) 2_765 6_654 ?
S3 Ba1 S2 64.19(2) . 6_654 ?
S1 Ba1 S2 115.91(2) 3_575 6_654 ?
Cl2 Ba1 S1 71.789(15) . . ?
Cl1 Ba1 S1 140.585(18) . . ?
S2 Ba1 S1 64.90(2) . . ?
S1 Ba1 S1 145.91(2) 2_765 . ?
S3 Ba1 S1 64.58(2) . . ?
S1 Ba1 S1 71.72(3) 3_575 . ?
S2 Ba1 S1 114.63(2) 6_654 . ?
Cl2 Ba1 Ba2 107.90(3) . . ?
Cl1 Ba1 Ba2 109.885(14) . . ?
S2 Ba1 Ba2 43.112(17) . . ?
S1 Ba1 Ba2 149.35(2) 2_765 . ?
S3 Ba1 Ba2 83.671(18) . . ?
S1 Ba1 Ba2 43.301(17) 3_575 . ?
S2 Ba1 Ba2 147.836(16) 6_654 . ?
S1 Ba1 Ba2 43.253(16) . . ?
Cl1 Ba2 S2 76.45(2) 4_675 . ?
Cl1 Ba2 S2 76.45(2) 4_675 2_775 ?
S2 Ba2 S2 114.688(15) . 2_775 ?
Cl1 Ba2 S2 76.45(2) 4_675 3_575 ?
S2 Ba2 S2 114.688(15) . 3_575 ?
S2 Ba2 S2 114.688(15) 2_775 3_575 ?
Cl1 Ba2 S1 131.04(2) 4_675 . ?
S2 Ba2 S1 70.24(2) . . ?
S2 Ba2 S1 85.91(2) 2_775 . ?
S2 Ba2 S1 150.55(3) 3_575 . ?
Cl1 Ba2 S1 131.04(2) 4_675 3_575 ?
S2 Ba2 S1 85.91(2) . 3_575 ?
S2 Ba2 S1 150.55(3) 2_775 3_575 ?
S2 Ba2 S1 70.24(2) 3_575 3_575 ?
S1 Ba2 S1 81.57(3) . 3_575 ?
Cl1 Ba2 S1 131.04(2) 4_675 2_775 ?
S2 Ba2 S1 150.55(3) . 2_775 ?
S2 Ba2 S1 70.24(2) 2_775 2_775 ?
S2 Ba2 S1 85.91(2) 3_575 2_775 ?
S1 Ba2 S1 81.57(3) . 2_775 ?
S1 Ba2 S1 81.57(3) 3_575 2_775 ?
Cl1 Ba2 Ba1 118.504(6) 4_675 . ?
S2 Ba2 Ba1 43.829(19) . . ?
S2 Ba2 Ba1 133.784(17) 2_775 . ?
S2 Ba2 Ba1 111.398(16) 3_575 . ?
S1 Ba2 Ba1 50.340(16) . . ?
S1 Ba2 Ba1 49.367(16) 3_575 . ?
S1 Ba2 Ba1 110.46(2) 2_775 . ?
Cl1 Ba2 Ba1 118.504(6) 4_675 2_775 ?
S2 Ba2 Ba1 111.398(16) . 2_775 ?
S2 Ba2 Ba1 43.829(19) 2_775 2_775 ?
S2 Ba2 Ba1 133.784(17) 3_575 2_775 ?
S1 Ba2 Ba1 49.367(16) . 2_775 ?
S1 Ba2 Ba1 110.46(2) 3_575 2_775 ?
S1 Ba2 Ba1 50.340(16) 2_775 2_775 ?
Ba1 Ba2 Ba1 99.114(8) . 2_775 ?
Cl1 Ba2 Ba1 118.504(6) 4_675 3_575 ?
S2 Ba2 Ba1 133.784(17) . 3_575 ?
S2 Ba2 Ba1 111.398(16) 2_775 3_575 ?
S2 Ba2 Ba1 43.829(19) 3_575 3_575 ?
S1 Ba2 Ba1 110.46(2) . 3_575 ?
S1 Ba2 Ba1 50.340(16) 3_575 3_575 ?
S1 Ba2 Ba1 49.367(16) 2_775 3_575 ?
Ba1 Ba2 Ba1 99.114(8) . 3_575 ?
Ba1 Ba2 Ba1 99.114(8) 2_775 3_575 ?
S2 Ge1 S1 112.47(4) 5_564 . ?
S2 Ge1 S3 102.45(4) 5_564 . ?
S1 Ge1 S3 114.52(4) . . ?
S2 Ge1 S3 106.59(4) 5_564 2_775 ?
S1 Ge1 S3 111.76(4) . 2_775 ?
S3 Ge1 S3 108.38(5) . 2_775 ?
Ge1 S1 Ba2 124.23(4) . . ?
Ge1 S1 Ba1 94.63(3) . 3_675 ?
Ba2 S1 Ba1 140.98(4) . 3_675 ?
Ge1 S1 Ba1 88.80(3) . 2_775 ?
Ba2 S1 Ba1 87.33(2) . 2_775 ?
Ba1 S1 Ba1 97.83(2) 3_675 2_775 ?
Ge1 S1 Ba1 85.88(3) . . ?
Ba2 S1 Ba1 86.41(2) . . ?
Ba1 S1 Ba1 93.78(2) 3_675 . ?
Ba1 S1 Ba1 167.58(3) 2_775 . ?
Ge1 S2 Ba2 108.26(3) 6_655 . ?
Ge1 S2 Ba1 98.82(3) 6_655 . ?
Ba2 S2 Ba1 93.06(3) . . ?
Ge1 S2 Ba1 90.09(3) 6_655 5_565 ?
Ba2 S2 Ba1 92.70(2) . 5_565 ?
Ba1 S2 Ba1 167.30(3) . 5_565 ?
Ge1 S3 Ge1 109.84(4) . 3_575 ?
Ge1 S3 Ba1 88.42(3) . . ?
Ge1 S3 Ba1 90.02(3) 3_575 . ?
Ba1 Cl1 Ba1 115.24(2) 2_665 . ?
Ba1 Cl1 Ba1 115.24(2) 2_665 3_565 ?
Ba1 Cl1 Ba1 115.24(2) . 3_565 ?
Ba1 Cl1 Ba2 102.80(3) 2_665 4_674 ?
Ba1 Cl1 Ba2 102.80(3) . 4_674 ?
Ba1 Cl1 Ba2 102.80(3) 3_565 4_674 ?
Ba1 Cl2 Ba1 119.05(2) 3_675 2_765 ?
Ba1 Cl2 Ba1 119.05(2) 3_675 . ?
Ba1 Cl2 Ba1 119.05(2) 2_765 . ?

_diffrn_measured_fraction_theta_max 0.980
_diffrn_reflns_theta_full        27.43
_diffrn_measured_fraction_theta_full 0.980
_refine_diff_density_max         0.826
_refine_diff_density_min         -0.745
_refine_diff_density_rms         0.095
####################################################################### 
# 
# 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_Ba4Ge3Se9Cl2
_database_code_depnum_ccdc_archive 'CCDC 1516719'
_audit_update_record             
;
2016-11-11 deposited with the CCDC.
2017-01-27 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'Ba4 Cl2 Ge3 Se9'
_chemical_formula_weight         1548.67

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Cl Cl 0.1484 0.1585 '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'
Ba Ba -0.3244 2.2819 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Hexagonal
_symmetry_space_group_name_H-M   P63

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

_cell_length_a                   10.0924(6)
_cell_length_b                   10.0924(6)
_cell_length_c                   12.5117(14)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_volume                     1103.66(15)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    3419
_cell_measurement_theta_min      2.3303
_cell_measurement_theta_max      27.4547

_exptl_crystal_description       block
_exptl_crystal_colour            dark-red
_exptl_crystal_size_max          0.2000
_exptl_crystal_size_mid          0.2000
_exptl_crystal_size_min          0.2000
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    4.660
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1320
_exptl_absorpt_coefficient_mu    26.111
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.6542
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_detector       CCD
_diffrn_measurement_device       
;
Mercury70 (2x2 bin mode)
;
_diffrn_measurement_device_type  ?
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            8456
_diffrn_reflns_av_R_equivalents  0.0396
_diffrn_reflns_av_sigmaI/netI    0.0326
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         2.33
_diffrn_reflns_theta_max         27.43
_reflns_number_total             1663
_reflns_number_gt                1619
_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)+(0.0112P)²+0.5958P] 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       0.00036(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.057(16)
_refine_ls_number_reflns         1663
_refine_ls_number_parameters     56
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0227
_refine_ls_R_factor_gt           0.0213
_refine_ls_wR_factor_ref         0.0404
_refine_ls_wR_factor_gt          0.0400
_refine_ls_goodness_of_fit_ref   1.081
_refine_ls_restrained_S_all      1.081
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.001

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
Ba1 Ba 0.67186(4) 0.92080(4) 0.03296(3) 0.02055(10) Uani 1 1 d . . .
Ba2 Ba 0.6667 1.3333 -0.15982(5) 0.01721(14) Uani 1 3 d S . .
Ge1 Ge 0.67013(7) 0.55581(7) 0.19805(5) 0.01302(14) Uani 1 1 d . . .
Se2 Se 0.69024(7) 0.76491(7) 0.28567(5) 0.01780(14) Uani 1 1 d . . .
Se4 Se 0.66243(7) 1.10918(7) 0.26591(5) 0.01747(14) Uani 1 1 d . . .
Se1 Se 0.65954(7) 0.57527(7) 0.01534(5) 0.01877(14) Uani 1 1 d . . .
Cl7 Cl 0.3333 0.6667 0.0885(2) 0.0194(6) Uani 1 3 d S . .
Cl8 Cl 1.0000 1.0000 0.0402(3) 0.0419(8) Uani 1 3 d S . .

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 0.0195(2) 0.0206(2) 0.02209(18) 0.00492(16) 0.00457(16) 0.01044(17)
Ba2 0.0199(2) 0.0199(2) 0.0119(3) 0.000 0.000 0.00994(11)
Ge1 0.0159(3) 0.0136(3) 0.0108(3) -0.0011(2) 0.0002(2) 0.0083(3)
Se2 0.0247(3) 0.0168(3) 0.0155(3) -0.0038(2) -0.0004(3) 0.0131(3)
Se4 0.0167(3) 0.0183(3) 0.0169(3) 0.0048(3) -0.0002(2) 0.0083(3)
Se1 0.0274(3) 0.0200(3) 0.0106(3) -0.0015(2) 0.0004(2) 0.0132(3)
Cl7 0.0182(9) 0.0182(9) 0.0218(13) 0.000 0.000 0.0091(4)
Cl8 0.0209(9) 0.0209(9) 0.084(2) 0.000 0.000 0.0104(4)

_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 Cl8 2.9945(4) . ?
Ba1 Cl7 3.1577(7) . ?
Ba1 Se2 3.3776(8) 5_564 ?
Ba1 Se1 3.4338(8) . ?
Ba1 Se4 3.5071(8) . ?
Ba1 Se2 3.5775(8) . ?
Ba1 Se1 3.6202(8) 2_665 ?
Ba1 Se1 3.6906(7) 3_675 ?
Ba1 Ba2 4.8346(5) . ?
Ba2 Cl7 3.149(3) 4_674 ?
Ba2 Se2 3.2942(6) 5_564 ?
Ba2 Se2 3.2942(6) 6_664 ?
Ba2 Se2 3.2942(6) 4_674 ?
Ba2 Se1 3.3085(7) 3_675 ?
Ba2 Se1 3.3085(8) 2_665 ?
Ba2 Se1 3.3085(7) 1_565 ?
Ba2 Ba1 4.8346(5) 2_775 ?
Ba2 Ba1 4.8346(5) 3_575 ?
Ge1 Se2 2.2952(9) . ?
Ge1 Se1 2.3014(8) . ?
Ge1 Se4 2.3852(9) 3_565 ?
Ge1 Se4 2.3958(8) 2_765 ?
Se2 Ba2 3.2942(6) 4_675 ?
Se2 Ba1 3.3776(8) 6_655 ?
Se4 Ge1 2.3852(9) 2_665 ?
Se4 Ge1 2.3958(8) 3_675 ?
Se1 Ba2 3.3085(7) 1_545 ?
Se1 Ba1 3.6202(8) 3_565 ?
Se1 Ba1 3.6906(7) 2_765 ?
Cl7 Ba2 3.149(3) 4_675 ?
Cl7 Ba1 3.1577(7) 2_665 ?
Cl7 Ba1 3.1577(7) 3_565 ?
Cl8 Ba1 2.9945(4) 3_675 ?
Cl8 Ba1 2.9945(4) 2_765 ?

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
Cl8 Ba1 Cl7 144.41(4) . . ?
Cl8 Ba1 Se2 83.61(8) . 5_564 ?
Cl7 Ba1 Se2 120.95(5) . 5_564 ?
Cl8 Ba1 Se1 75.326(14) . . ?
Cl7 Ba1 Se1 73.392(14) . . ?
Se2 Ba1 Se1 105.587(18) 5_564 . ?
Cl8 Ba1 Se4 99.00(7) . . ?
Cl7 Ba1 Se4 86.89(4) . . ?
Se2 Ba1 Se4 126.065(19) 5_564 . ?
Se1 Ba1 Se4 127.363(19) . . ?
Cl8 Ba1 Se2 78.30(7) . . ?
Cl7 Ba1 Se2 73.81(4) . . ?
Se2 Ba1 Se2 161.47(2) 5_564 . ?
Se1 Ba1 Se2 66.022(15) . . ?
Se4 Ba1 Se2 61.663(17) . . ?
Cl8 Ba1 Se1 143.336(17) . 2_665 ?
Cl7 Ba1 Se1 70.814(15) . 2_665 ?
Se2 Ba1 Se1 80.284(16) 5_564 2_665 ?
Se1 Ba1 Se1 140.85(2) . 2_665 ?
Se4 Ba1 Se1 65.915(16) . 2_665 ?
Se2 Ba1 Se1 116.951(17) . 2_665 ?
Cl8 Ba1 Se1 71.429(13) . 3_675 ?
Cl7 Ba1 Se1 140.819(16) . 3_675 ?
Se2 Ba1 Se1 62.941(15) 5_564 3_675 ?
Se1 Ba1 Se1 145.728(18) . 3_675 ?
Se4 Ba1 Se1 67.094(16) . 3_675 ?
Se2 Ba1 Se1 113.953(18) . 3_675 ?
Se1 Ba1 Se1 71.91(2) 2_665 3_675 ?
Cl8 Ba1 Ba2 105.78(4) . . ?
Cl7 Ba1 Ba2 109.64(2) . . ?
Se2 Ba1 Ba2 42.885(12) 5_564 . ?
Se1 Ba1 Ba2 146.314(17) . . ?
Se4 Ba1 Ba2 86.149(16) . . ?
Se2 Ba1 Ba2 147.664(15) . . ?
Se1 Ba1 Ba2 43.162(11) 2_665 . ?
Se1 Ba1 Ba2 43.120(11) 3_675 . ?
Cl7 Ba2 Se2 78.050(15) 4_674 5_564 ?
Cl7 Ba2 Se2 78.050(15) 4_674 6_664 ?
Se2 Ba2 Se2 115.829(10) 5_564 6_664 ?
Cl7 Ba2 Se2 78.050(15) 4_674 4_674 ?
Se2 Ba2 Se2 115.829(10) 5_564 4_674 ?
Se2 Ba2 Se2 115.829(10) 6_664 4_674 ?
Cl7 Ba2 Se1 131.484(13) 4_674 3_675 ?
Se2 Ba2 Se1 68.157(15) 5_564 3_675 ?
Se2 Ba2 Se1 86.290(16) 6_664 3_675 ?
Se2 Ba2 Se1 148.02(2) 4_674 3_675 ?
Cl7 Ba2 Se1 131.484(13) 4_674 2_665 ?
Se2 Ba2 Se1 86.290(16) 5_564 2_665 ?
Se2 Ba2 Se1 148.02(2) 6_664 2_665 ?
Se2 Ba2 Se1 68.156(15) 4_674 2_665 ?
Se1 Ba2 Se1 80.90(2) 3_675 2_665 ?
Cl7 Ba2 Se1 131.484(13) 4_674 1_565 ?
Se2 Ba2 Se1 148.02(2) 5_564 1_565 ?
Se2 Ba2 Se1 68.156(15) 6_664 1_565 ?
Se2 Ba2 Se1 86.290(16) 4_674 1_565 ?
Se1 Ba2 Se1 80.90(2) 3_675 1_565 ?
Se1 Ba2 Se1 80.90(2) 2_665 1_565 ?
Cl7 Ba2 Ba1 119.927(8) 4_674 . ?
Se2 Ba2 Ba1 44.248(13) 5_564 . ?
Se2 Ba2 Ba1 134.513(14) 6_664 . ?
Se2 Ba2 Ba1 108.975(12) 4_674 . ?
Se1 Ba2 Ba1 49.682(12) 3_675 . ?
Se1 Ba2 Ba1 48.463(13) 2_665 . ?
Se1 Ba2 Ba1 108.585(19) 1_565 . ?
Cl7 Ba2 Ba1 119.927(8) 4_674 2_775 ?
Se2 Ba2 Ba1 108.975(12) 5_564 2_775 ?
Se2 Ba2 Ba1 44.248(13) 6_664 2_775 ?
Se2 Ba2 Ba1 134.513(13) 4_674 2_775 ?
Se1 Ba2 Ba1 48.463(13) 3_675 2_775 ?
Se1 Ba2 Ba1 108.585(19) 2_665 2_775 ?
Se1 Ba2 Ba1 49.682(12) 1_565 2_775 ?
Ba1 Ba2 Ba1 97.276(11) . 2_775 ?
Cl7 Ba2 Ba1 119.927(8) 4_674 3_575 ?
Se2 Ba2 Ba1 134.513(13) 5_564 3_575 ?
Se2 Ba2 Ba1 108.975(12) 6_664 3_575 ?
Se2 Ba2 Ba1 44.248(13) 4_674 3_575 ?
Se1 Ba2 Ba1 108.585(19) 3_675 3_575 ?
Se1 Ba2 Ba1 49.682(12) 2_665 3_575 ?
Se1 Ba2 Ba1 48.463(13) 1_565 3_575 ?
Ba1 Ba2 Ba1 97.276(11) . 3_575 ?
Ba1 Ba2 Ba1 97.276(11) 2_775 3_575 ?
Se2 Ge1 Se1 112.49(3) . . ?
Se2 Ge1 Se4 106.69(3) . 3_565 ?
Se1 Ge1 Se4 111.69(3) . 3_565 ?
Se2 Ge1 Se4 100.68(3) . 2_765 ?
Se1 Ge1 Se4 115.85(3) . 2_765 ?
Se4 Ge1 Se4 108.57(4) 3_565 2_765 ?
Ge1 Se2 Ba2 103.97(3) . 4_675 ?
Ge1 Se2 Ba1 97.28(3) . 6_655 ?
Ba2 Se2 Ba1 92.868(19) 4_675 6_655 ?
Ge1 Se2 Ba1 88.97(3) . . ?
Ba2 Se2 Ba1 91.492(19) 4_675 . ?
Ba1 Se2 Ba1 171.29(2) 6_655 . ?
Ge1 Se4 Ge1 107.64(4) 2_665 3_675 ?
Ge1 Se4 Ba1 89.52(2) 2_665 . ?
Ge1 Se4 Ba1 86.65(2) 3_675 . ?
Ge1 Se1 Ba2 125.16(3) . 1_545 ?
Ge1 Se1 Ba1 92.48(2) . . ?
Ba2 Se1 Ba1 142.08(2) 1_545 . ?
Ge1 Se1 Ba1 88.09(2) . 3_565 ?
Ba2 Se1 Ba1 88.375(16) 1_545 3_565 ?
Ba1 Se1 Ba1 98.25(2) . 3_565 ?
Ge1 Se1 Ba1 83.72(2) . 2_765 ?
Ba2 Se1 Ba1 87.198(15) 1_545 2_765 ?
Ba1 Se1 Ba1 93.316(18) . 2_765 ?
Ba1 Se1 Ba1 166.10(2) 3_565 2_765 ?
Ba2 Cl7 Ba1 102.71(5) 4_675 2_665 ?
Ba2 Cl7 Ba1 102.71(5) 4_675 . ?
Ba1 Cl7 Ba1 115.30(3) 2_665 . ?
Ba2 Cl7 Ba1 102.71(5) 4_675 3_565 ?
Ba1 Cl7 Ba1 115.30(3) 2_665 3_565 ?
Ba1 Cl7 Ba1 115.30(3) . 3_565 ?
Ba1 Cl8 Ba1 119.910(8) 3_675 . ?
Ba1 Cl8 Ba1 119.910(9) 3_675 2_765 ?
Ba1 Cl8 Ba1 119.910(8) . 2_765 ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        27.43
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.599
_refine_diff_density_min         -0.596
_refine_diff_density_rms         0.136
