# Electronic Supplementary Material (ESI) for Inorganic Chemistry Frontiers.
# This journal is © the Partner Organisations 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_a
_database_code_depnum_ccdc_archive 'CCDC 1470886'
_audit_update_record             
;
2016-03-28 deposited with the CCDC.
2016-12-16 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C4.50 H0 Cu5.25 Ge3 N3 Se9.75'
_chemical_formula_weight         1417.29

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 '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           Hexagonal
_symmetry_space_group_name_H-M   R3c

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'-x+y, y, z+1/2'
'x, x-y, z+1/2'
'-y, -x, z+1/2'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'-x+y+2/3, y+1/3, z+5/6'
'x+2/3, x-y+1/3, z+5/6'
'-y+2/3, -x+1/3, z+5/6'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x+y+1/3, y+2/3, z+7/6'
'x+1/3, x-y+2/3, z+7/6'
'-y+1/3, -x+2/3, z+7/6'

_cell_length_a                   13.2540(6)
_cell_length_b                   13.2540(6)
_cell_length_c                   30.366(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_volume                     4619.7(5)
_cell_formula_units_Z            8
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    9850
_cell_measurement_theta_min      3.07
_cell_measurement_theta_max      30.37

_exptl_crystal_description       cubic
_exptl_crystal_colour            black
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    4.076
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             5022
_exptl_absorpt_coefficient_mu    23.944
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  0.1237
_exptl_absorpt_correction_T_max  0.1237
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      296(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 area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            20220
_diffrn_reflns_av_R_equivalents  0.0371
_diffrn_reflns_av_sigmaI/netI    0.0186
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_theta_min         3.80
_diffrn_reflns_theta_max         25.00
_reflns_number_total             1712
_reflns_number_gt                1706
_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)+(0.0005P)²+54.6222P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.00
_refine_ls_number_reflns         1712
_refine_ls_number_parameters     105
_refine_ls_number_restraints     85
_refine_ls_R_factor_all          0.0163
_refine_ls_R_factor_gt           0.0149
_refine_ls_wR_factor_ref         0.0370
_refine_ls_wR_factor_gt          0.0363
_refine_ls_goodness_of_fit_ref   1.176
_refine_ls_restrained_S_all      1.147
_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
Se5 Se 0.65442(5) 0.49553(4) 0.640486(15) 0.00695(12) Uani 1 1 d U . .
Se2 Se 0.38153(5) 0.33480(5) 0.719355(17) 0.00827(13) Uani 1 1 d U . .
Se4 Se 0.33709(5) 0.37464(4) 0.600132(17) 0.00779(12) Uani 1 1 d U . .
Ge1 Ge 0.46021(4) 0.46487(4) 0.66032(2) 0.00552(10) Uani 1 1 d U . .
Cu3 Cu 0.75022(6) 0.55625(7) 0.71411(2) 0.01396(17) Uani 1 1 d U . .
Cu2 Cu 0.53981(6) 0.41869(6) 0.77247(2) 0.01346(17) Uani 1 1 d U . .
Ge2 Ge 0.6667 0.3333 0.66736(3) 0.00724(19) Uani 1 3 d SU . .
Cu1 Cu 0.6667 0.3333 0.83769(4) 0.0108(2) Uani 1 3 d SU . .
Se1 Se 0.6667 0.3333 0.74398(4) 0.01177(16) Uani 1 3 d SU . .
Se3 Se 0.83972(4) 0.51648(5) 0.844195(15) 0.00725(12) Uani 1 1 d U . .
N1 N 0.3333 0.6667 0.8324(3) 0.0107(14) Uani 1 3 d SU . .
C1 C 0.2855(5) 0.5458(4) 0.84849(17) 0.0137(11) Uani 1 1 d U . .
N2 N 0.2552(4) 0.4535(4) 0.77549(16) 0.0172(10) Uani 1 1 d U . .
C2 C 0.3208(5) 0.4772(5) 0.81844(19) 0.0150(12) Uani 1 1 d U . .

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
Se5 0.0066(3) 0.0064(3) 0.0083(3) 0.00071(19) 0.0004(2) 0.0036(2)
Se2 0.0088(3) 0.0078(3) 0.0084(3) 0.0014(2) 0.0012(2) 0.0042(2)
Se4 0.0084(3) 0.0072(3) 0.0072(3) -0.0003(2) -0.0018(2) 0.0035(2)
Ge1 0.0063(2) 0.0060(2) 0.00509(19) 0.0000(2) -0.0003(2) 0.00368(16)
Cu3 0.0117(3) 0.0193(4) 0.0135(3) -0.0061(3) -0.0026(3) 0.0097(3)
Cu2 0.0114(4) 0.0130(4) 0.0117(3) 0.0017(3) -0.0014(3) 0.0029(3)
Ge2 0.0062(3) 0.0062(3) 0.0093(4) 0.000 0.000 0.00309(13)
Cu1 0.0087(3) 0.0087(3) 0.0151(5) 0.000 0.000 0.00436(17)
Se1 0.0123(2) 0.0123(2) 0.0107(3) 0.000 0.000 0.00615(11)
Se3 0.0078(3) 0.0062(2) 0.0079(3) 0.00004(19) -0.00116(19) 0.0036(2)
N1 0.0086(17) 0.0086(17) 0.015(4) 0.000 0.000 0.0043(9)
C1 0.015(2) 0.009(2) 0.017(3) -0.001(2) 0.002(2) 0.006(2)
N2 0.014(2) 0.018(2) 0.023(2) -0.0060(18) 0.0000(18) 0.0101(19)
C2 0.017(3) 0.011(2) 0.018(3) 0.000(2) -0.002(2) 0.008(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
Se5 Ge2 2.3796(6) . ?
Se5 Ge1 2.4713(8) . ?
Se5 Cu3 2.4973(9) . ?
Se2 Ge1 2.3399(8) . ?
Se2 Cu3 2.3935(9) 2_655 ?
Se2 Cu2 2.4301(9) . ?
Se4 Ge1 2.3414(8) . ?
Se4 Cu3 2.3732(9) 11_454 ?
Se4 Cu2 2.4448(9) 11_454 ?
Ge1 Se3 2.3556(8) 11_454 ?
Cu3 Se4 2.3732(9) 17_554 ?
Cu3 Se2 2.3935(9) 3_665 ?
Cu3 Se1 2.7397(9) . ?
Cu3 Ge2 2.9495(9) . ?
Cu3 Cu2 3.0261(10) . ?
Cu2 Se3 2.4407(9) 2_655 ?
Cu2 Se4 2.4447(9) 17_554 ?
Cu2 Se1 2.5995(9) . ?
Ge2 Se1 2.3265(14) . ?
Ge2 Se5 2.3796(6) 3_665 ?
Ge2 Se5 2.3796(6) 2_655 ?
Ge2 Cu3 2.9494(9) 3_665 ?
Ge2 Cu3 2.9495(9) 2_655 ?
Cu1 Se3 2.3717(5) 3_665 ?
Cu1 Se3 2.3717(6) . ?
Cu1 Se3 2.3717(5) 2_655 ?
Cu1 Se1 2.8456(15) . ?
Se1 Cu2 2.5995(9) 3_665 ?
Se1 Cu2 2.5995(9) 2_655 ?
Se1 Cu3 2.7397(9) 3_665 ?
Se1 Cu3 2.7397(9) 2_655 ?
Se3 Ge1 2.3555(8) 17_554 ?
Se3 Cu2 2.4407(8) 3_665 ?
N1 C1 1.481(6) 3_565 ?
N1 C1 1.481(6) 2_665 ?
N1 C1 1.481(6) . ?
C1 C2 1.517(7) . ?
N2 C2 1.511(7) . ?

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
Ge2 Se5 Ge1 107.68(2) . . ?
Ge2 Se5 Cu3 74.38(3) . . ?
Ge1 Se5 Cu3 98.90(3) . . ?
Ge1 Se2 Cu3 108.86(3) . 2_655 ?
Ge1 Se2 Cu2 101.92(3) . . ?
Cu3 Se2 Cu2 81.13(3) 2_655 . ?
Ge1 Se4 Cu3 101.01(3) . 11_454 ?
Ge1 Se4 Cu2 100.81(3) . 11_454 ?
Cu3 Se4 Cu2 77.80(3) 11_454 11_454 ?
Se2 Ge1 Se4 106.36(2) . . ?
Se2 Ge1 Se3 113.86(3) . 11_454 ?
Se4 Ge1 Se3 117.58(3) . 11_454 ?
Se2 Ge1 Se5 110.59(3) . . ?
Se4 Ge1 Se5 107.24(3) . . ?
Se3 Ge1 Se5 100.91(2) 11_454 . ?
Se4 Cu3 Se2 117.91(4) 17_554 3_665 ?
Se4 Cu3 Se5 118.45(3) 17_554 . ?
Se2 Cu3 Se5 118.26(3) 3_665 . ?
Se4 Cu3 Se1 101.16(4) 17_554 . ?
Se2 Cu3 Se1 97.36(3) 3_665 . ?
Se5 Cu3 Se1 94.74(3) . . ?
Se4 Cu3 Ge2 135.37(4) 17_554 . ?
Se2 Cu3 Ge2 99.87(3) 3_665 . ?
Se5 Cu3 Ge2 50.99(2) . . ?
Se1 Cu3 Ge2 48.10(3) . . ?
Se4 Cu3 Cu2 52.15(2) 17_554 . ?
Se2 Cu3 Cu2 135.02(3) 3_665 . ?
Se5 Cu3 Cu2 99.39(3) . . ?
Se1 Cu3 Cu2 53.32(3) . . ?
Ge2 Cu3 Cu2 84.66(3) . . ?
Se2 Cu2 Se3 112.64(3) . 2_655 ?
Se2 Cu2 Se4 115.60(4) . 17_554 ?
Se3 Cu2 Se4 120.85(3) 2_655 17_554 ?
Se2 Cu2 Se1 100.27(3) . . ?
Se3 Cu2 Se1 99.67(3) 2_655 . ?
Se4 Cu2 Se1 103.29(3) 17_554 . ?
Se2 Cu2 Cu3 102.22(3) . . ?
Se3 Cu2 Cu3 141.78(3) 2_655 . ?
Se4 Cu2 Cu3 50.04(2) 17_554 . ?
Se1 Cu2 Cu3 57.69(3) . . ?
Se1 Ge2 Se5 110.05(2) . 3_665 ?
Se1 Ge2 Se5 110.05(2) . 2_655 ?
Se5 Ge2 Se5 108.88(2) 3_665 2_655 ?
Se1 Ge2 Se5 110.05(2) . . ?
Se5 Ge2 Se5 108.88(2) 3_665 . ?
Se5 Ge2 Se5 108.88(2) 2_655 . ?
Se1 Ge2 Cu3 61.23(2) . 3_665 ?
Se5 Ge2 Cu3 54.63(2) 3_665 3_665 ?
Se5 Ge2 Cu3 103.38(2) 2_655 3_665 ?
Se5 Ge2 Cu3 147.42(2) . 3_665 ?
Se1 Ge2 Cu3 61.23(2) . . ?
Se5 Ge2 Cu3 103.38(2) 3_665 . ?
Se5 Ge2 Cu3 147.42(2) 2_655 . ?
Se5 Ge2 Cu3 54.63(2) . . ?
Cu3 Ge2 Cu3 98.77(3) 3_665 . ?
Se1 Ge2 Cu3 61.23(2) . 2_655 ?
Se5 Ge2 Cu3 147.42(2) 3_665 2_655 ?
Se5 Ge2 Cu3 54.63(2) 2_655 2_655 ?
Se5 Ge2 Cu3 103.38(2) . 2_655 ?
Cu3 Ge2 Cu3 98.77(3) 3_665 2_655 ?
Cu3 Ge2 Cu3 98.77(3) . 2_655 ?
Se3 Cu1 Se3 119.313(9) 3_665 . ?
Se3 Cu1 Se3 119.313(9) 3_665 2_655 ?
Se3 Cu1 Se3 119.313(9) . 2_655 ?
Se3 Cu1 Se1 94.78(3) 3_665 . ?
Se3 Cu1 Se1 94.78(3) . . ?
Se3 Cu1 Se1 94.78(3) 2_655 . ?
Ge2 Se1 Cu2 109.44(3) . 3_665 ?
Ge2 Se1 Cu2 109.44(3) . 2_655 ?
Cu2 Se1 Cu2 109.50(3) 3_665 2_655 ?
Ge2 Se1 Cu2 109.44(3) . . ?
Cu2 Se1 Cu2 109.50(3) 3_665 . ?
Cu2 Se1 Cu2 109.50(3) 2_655 . ?
Ge2 Se1 Cu3 70.67(3) . 3_665 ?
Cu2 Se1 Cu3 68.99(2) 3_665 3_665 ?
Cu2 Se1 Cu3 71.91(2) 2_655 3_665 ?
Cu2 Se1 Cu3 178.32(3) . 3_665 ?
Ge2 Se1 Cu3 70.67(3) . 2_655 ?
Cu2 Se1 Cu3 178.31(3) 3_665 2_655 ?
Cu2 Se1 Cu3 68.99(2) 2_655 2_655 ?
Cu2 Se1 Cu3 71.91(2) . 2_655 ?
Cu3 Se1 Cu3 109.61(3) 3_665 2_655 ?
Ge2 Se1 Cu3 70.67(3) . . ?
Cu2 Se1 Cu3 71.91(2) 3_665 . ?
Cu2 Se1 Cu3 178.31(3) 2_655 . ?
Cu2 Se1 Cu3 68.99(2) . . ?
Cu3 Se1 Cu3 109.61(3) 3_665 . ?
Cu3 Se1 Cu3 109.61(3) 2_655 . ?
Ge2 Se1 Cu1 180.0 . . ?
Cu2 Se1 Cu1 70.56(3) 3_665 . ?
Cu2 Se1 Cu1 70.56(3) 2_655 . ?
Cu2 Se1 Cu1 70.56(3) . . ?
Cu3 Se1 Cu1 109.33(3) 3_665 . ?
Cu3 Se1 Cu1 109.33(3) 2_655 . ?
Cu3 Se1 Cu1 109.33(3) . . ?
Ge1 Se3 Cu1 107.78(3) 17_554 . ?
Ge1 Se3 Cu2 103.55(3) 17_554 3_665 ?
Cu1 Se3 Cu2 81.80(4) . 3_665 ?
C1 N1 C1 109.6(4) 3_565 2_665 ?
C1 N1 C1 109.6(4) 3_565 . ?
C1 N1 C1 109.6(4) 2_665 . ?
N1 C1 C2 110.8(5) . . ?
N2 C2 C1 109.0(4) . . ?

_diffrn_measured_fraction_theta_max 0.945
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.945
_refine_diff_density_max         1.775
_refine_diff_density_min         -0.681
_refine_diff_density_rms         0.100
####################################################################### 
# 
# 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_ay7_sq_d
_database_code_depnum_ccdc_archive 'CCDC 1470883'
_audit_update_record             
;
2016-03-28 deposited with the CCDC.
2016-12-16 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         '??Cu8Se13?? ??Ge2Se2??3'
_chemical_formula_sum            'Cu32 Ge24 Se76'
_chemical_formula_weight         9776.40

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Cu Cu 0.3201 1.2651 '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           cubic
_symmetry_space_group_name_H-M   Im-3
_symmetry_space_group_name_Hall  '-I 2 2 3'

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

_cell_length_a                   23.5208(17)
_cell_length_b                   23.5208(17)
_cell_length_c                   23.5208(17)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     13012.4(16)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    7110
_cell_measurement_theta_min      2.4492
_cell_measurement_theta_max      20.9101

_exptl_crystal_description       cubic
_exptl_crystal_colour            black
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.495
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             8560
_exptl_absorpt_coefficient_mu    15.912
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.204
_exptl_absorpt_correction_T_max  0.222
_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 area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            49106
_diffrn_reflns_av_R_equivalents  0.1363
_diffrn_reflns_av_sigmaI/netI    0.0505
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         2.12
_diffrn_reflns_theta_max         22.47
_reflns_number_total             1539
_reflns_number_gt                1074
_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)+(0.0716P)²+538.2859P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         1539
_refine_ls_number_parameters     54
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1220
_refine_ls_R_factor_gt           0.0771
_refine_ls_wR_factor_ref         0.1987
_refine_ls_wR_factor_gt          0.1782
_refine_ls_goodness_of_fit_ref   1.086
_refine_ls_restrained_S_all      1.086
_refine_ls_shift/su_max          0.002
_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
Se1 Se -0.20100(10) 0.35902(10) 0.86293(9) 0.0820(8) Uani 1 1 d . . .
Se2 Se -0.2500 0.2500 0.7500 0.0691(14) Uani 1 6 d S . .
Se11 Se -0.18116(16) 0.5000 0.78432(12) 0.0866(11) Uani 1 2 d S . .
Se15 Se -0.30329(10) 0.40457(10) 0.73045(11) 0.0909(8) Uani 1 1 d . . .
Se16 Se -0.2084(2) 0.5000 0.63675(13) 0.1066(14) Uani 1 2 d S . .
Ge1 Ge -0.20945(11) 0.56711(9) 0.71287(9) 0.0770(8) Uani 1 1 d . . .
Cu1 Cu -0.16346(11) 0.30524(11) 0.78353(11) 0.0776(8) Uani 1 1 d . . .
Cu23 Cu -0.31190(11) 0.31190(11) 0.68810(11) 0.0839(14) 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
Se1 0.0919(17) 0.0845(16) 0.0697(15) -0.0090(12) 0.0033(12) -0.0176(12)
Se2 0.0691(14) 0.0691(14) 0.0691(14) 0.0013(15) -0.0013(15) 0.0013(15)
Se11 0.123(3) 0.084(2) 0.0529(18) 0.000 0.0011(18) 0.000
Se15 0.0902(17) 0.0746(15) 0.1078(19) 0.0008(14) 0.0001(14) 0.0139(13)
Se16 0.194(4) 0.071(2) 0.054(2) 0.000 0.001(2) 0.000
Ge1 0.1057(19) 0.0548(13) 0.0705(15) 0.0005(11) 0.0084(13) -0.0034(12)
Cu1 0.0777(18) 0.0811(18) 0.0741(17) -0.0009(14) 0.0016(14) -0.0024(14)
Cu23 0.0839(14) 0.0839(14) 0.0839(14) 0.0093(14) -0.0093(14) 0.0093(14)

_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
Se1 Ge1 2.319(3) 20_556 ?
Se1 Cu1 2.423(3) . ?
Se1 Cu1 2.427(3) 43 ?
Se2 Cu23 2.522(4) 37_456 ?
Se2 Cu23 2.522(4) . ?
Se2 Cu1 2.540(3) 43 ?
Se2 Cu1 2.540(3) 37_456 ?
Se2 Cu1 2.540(3) . ?
Se2 Cu1 2.540(3) 12_566 ?
Se2 Cu1 2.540(3) 7_456 ?
Se2 Cu1 2.540(3) 48_445 ?
Se11 Ge1 2.400(3) 28_565 ?
Se11 Ge1 2.400(3) . ?
Se15 Ge1 2.342(4) 28_565 ?
Se15 Cu23 2.405(3) . ?
Se15 Cu1 2.423(4) 43 ?
Se16 Ge1 2.387(3) . ?
Se16 Ge1 2.387(3) 28_565 ?
Ge1 Se1 2.319(3) 22_465 ?
Ge1 Se15 2.342(4) 28_565 ?
Cu1 Se15 2.423(4) 48_445 ?
Cu1 Se1 2.427(3) 48_445 ?
Cu1 Cu23 2.893(4) 37_456 ?
Cu1 Cu1 2.963(4) 43 ?
Cu1 Cu1 2.963(4) 48_445 ?
Cu23 Se15 2.405(3) 12_566 ?
Cu23 Se15 2.405(3) 7_456 ?
Cu23 Cu1 2.893(4) 43 ?
Cu23 Cu1 2.893(4) 37_456 ?
Cu23 Cu1 2.893(4) 48_445 ?

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
Ge1 Se1 Cu1 103.19(12) 20_556 . ?
Ge1 Se1 Cu1 98.58(12) 20_556 43 ?
Cu1 Se1 Cu1 75.32(13) . 43 ?
Cu23 Se2 Cu23 180.00(10) 37_456 . ?
Cu23 Se2 Cu1 110.28(6) 37_456 43 ?
Cu23 Se2 Cu1 69.72(6) . 43 ?
Cu23 Se2 Cu1 110.28(6) 37_456 37_456 ?
Cu23 Se2 Cu1 69.72(6) . 37_456 ?
Cu1 Se2 Cu1 108.65(6) 43 37_456 ?
Cu23 Se2 Cu1 69.72(6) 37_456 . ?
Cu23 Se2 Cu1 110.28(6) . . ?
Cu1 Se2 Cu1 71.35(6) 43 . ?
Cu1 Se2 Cu1 180.00(7) 37_456 . ?
Cu23 Se2 Cu1 69.72(6) 37_456 12_566 ?
Cu23 Se2 Cu1 110.28(6) . 12_566 ?
Cu1 Se2 Cu1 71.35(6) 43 12_566 ?
Cu1 Se2 Cu1 71.35(6) 37_456 12_566 ?
Cu1 Se2 Cu1 108.65(6) . 12_566 ?
Cu23 Se2 Cu1 69.72(6) 37_456 7_456 ?
Cu23 Se2 Cu1 110.28(6) . 7_456 ?
Cu1 Se2 Cu1 180.0 43 7_456 ?
Cu1 Se2 Cu1 71.35(6) 37_456 7_456 ?
Cu1 Se2 Cu1 108.65(6) . 7_456 ?
Cu1 Se2 Cu1 108.65(6) 12_566 7_456 ?
Cu23 Se2 Cu1 110.28(6) 37_456 48_445 ?
Cu23 Se2 Cu1 69.72(6) . 48_445 ?
Cu1 Se2 Cu1 108.65(6) 43 48_445 ?
Cu1 Se2 Cu1 108.65(6) 37_456 48_445 ?
Cu1 Se2 Cu1 71.35(6) . 48_445 ?
Cu1 Se2 Cu1 180.0 12_566 48_445 ?
Cu1 Se2 Cu1 71.35(6) 7_456 48_445 ?
Ge1 Se11 Ge1 82.26(14) 28_565 . ?
Ge1 Se15 Cu23 105.30(11) 28_565 . ?
Ge1 Se15 Cu1 97.77(12) 28_565 43 ?
Cu23 Se15 Cu1 73.64(13) . 43 ?
Ge1 Se16 Ge1 82.79(14) . 28_565 ?
Se1 Ge1 Se15 118.28(12) 22_465 28_565 ?
Se1 Ge1 Se16 111.82(14) 22_465 . ?
Se15 Ge1 Se16 109.27(16) 28_565 . ?
Se1 Ge1 Se11 111.00(14) 22_465 . ?
Se15 Ge1 Se11 108.95(14) 28_565 . ?
Se16 Ge1 Se11 95.02(11) . . ?
Se1 Cu1 Se15 118.16(13) . 48_445 ?
Se1 Cu1 Se1 113.83(11) . 48_445 ?
Se15 Cu1 Se1 114.55(13) 48_445 48_445 ?
Se1 Cu1 Se2 102.38(11) . . ?
Se15 Cu1 Se2 102.56(11) 48_445 . ?
Se1 Cu1 Se2 102.26(11) 48_445 . ?
Se1 Cu1 Cu23 104.27(10) . 37_456 ?
Se15 Cu1 Cu23 52.90(10) 48_445 37_456 ?
Se1 Cu1 Cu23 139.52(12) 48_445 37_456 ?
Se2 Cu1 Cu23 54.84(9) . 37_456 ?
Se1 Cu1 Cu1 52.41(10) . 43 ?
Se15 Cu1 Cu1 140.97(13) 48_445 43 ?
Se1 Cu1 Cu1 101.92(15) 48_445 43 ?
Se2 Cu1 Cu1 54.33(3) . 43 ?
Cu23 Cu1 Cu1 90.34(7) 37_456 43 ?
Se1 Cu1 Cu1 137.25(15) . 48_445 ?
Se15 Cu1 Cu1 102.82(11) 48_445 48_445 ?
Se1 Cu1 Cu1 52.27(11) 48_445 48_445 ?
Se2 Cu1 Cu1 54.33(3) . 48_445 ?
Cu23 Cu1 Cu1 90.34(7) 37_456 48_445 ?
Cu1 Cu1 Cu1 88.29(13) 43 48_445 ?
Se15 Cu23 Se15 114.63(9) 12_566 . ?
Se15 Cu23 Se15 114.63(9) 12_566 7_456 ?
Se15 Cu23 Se15 114.63(9) . 7_456 ?
Se15 Cu23 Se2 103.62(12) 12_566 . ?
Se15 Cu23 Se2 103.62(12) . . ?
Se15 Cu23 Se2 103.62(12) 7_456 . ?
Se15 Cu23 Cu1 102.23(9) 12_566 43 ?
Se15 Cu23 Cu1 53.46(8) . 43 ?
Se15 Cu23 Cu1 141.66(12) 7_456 43 ?
Se2 Cu23 Cu1 55.44(9) . 43 ?
Se15 Cu23 Cu1 53.46(8) 12_566 37_456 ?
Se15 Cu23 Cu1 141.66(12) . 37_456 ?
Se15 Cu23 Cu1 102.23(9) 7_456 37_456 ?
Se2 Cu23 Cu1 55.44(9) . 37_456 ?
Cu1 Cu23 Cu1 90.99(13) 43 37_456 ?
Se15 Cu23 Cu1 141.66(12) 12_566 48_445 ?
Se15 Cu23 Cu1 102.23(9) . 48_445 ?
Se15 Cu23 Cu1 53.46(8) 7_456 48_445 ?
Se2 Cu23 Cu1 55.44(9) . 48_445 ?
Cu1 Cu23 Cu1 90.99(13) 43 48_445 ?
Cu1 Cu23 Cu1 90.99(13) 37_456 48_445 ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Ge1 Se16 Ge1 Se1 131.74(11) 28_565 . . 22_465 ?
Ge1 Se16 Ge1 Se15 -95.36(14) 28_565 . . 28_565 ?
Ge1 Se16 Ge1 Se11 16.73(18) 28_565 . . . ?
Ge1 Se11 Ge1 Se1 -132.35(10) 28_565 . . 22_465 ?
Ge1 Se11 Ge1 Se15 95.70(12) 28_565 . . 28_565 ?
Ge1 Se11 Ge1 Se16 -16.66(18) 28_565 . . . ?
Ge1 Se1 Cu1 Se15 -38.86(17) 20_556 . . 48_445 ?
Cu1 Se1 Cu1 Se15 -134.42(14) 43 . . 48_445 ?
Ge1 Se1 Cu1 Se1 -177.60(13) 20_556 . . 48_445 ?
Cu1 Se1 Cu1 Se1 86.84(18) 43 . . 48_445 ?
Ge1 Se1 Cu1 Se2 72.86(12) 20_556 . . . ?
Cu1 Se1 Cu1 Se2 -22.70(8) 43 . . . ?
Ge1 Se1 Cu1 Cu23 16.40(16) 20_556 . . 37_456 ?
Cu1 Se1 Cu1 Cu23 -79.16(11) 43 . . 37_456 ?
Ge1 Se1 Cu1 Cu1 95.56(13) 20_556 . . 43 ?
Ge1 Se1 Cu1 Cu1 122.91(16) 20_556 . . 48_445 ?
Cu1 Se1 Cu1 Cu1 27.35(18) 43 . . 48_445 ?
Cu23 Se2 Cu1 Se1 -98.86(10) 37_456 . . . ?
Cu23 Se2 Cu1 Se1 81.14(10) . . . . ?
Cu1 Se2 Cu1 Se1 22.12(7) 43 . . . ?
Cu1 Se2 Cu1 Se1 153(100) 37_456 . . . ?
Cu1 Se2 Cu1 Se1 -39.84(16) 12_566 . . . ?
Cu1 Se2 Cu1 Se1 -157.88(7) 7_456 . . . ?
Cu1 Se2 Cu1 Se1 140.17(16) 48_445 . . . ?
Cu23 Se2 Cu1 Se15 24.09(8) 37_456 . . 48_445 ?
Cu23 Se2 Cu1 Se15 -155.91(8) . . . 48_445 ?
Cu1 Se2 Cu1 Se15 145.06(13) 43 . . 48_445 ?
Cu1 Se2 Cu1 Se15 -84(100) 37_456 . . 48_445 ?
Cu1 Se2 Cu1 Se15 83.11(9) 12_566 . . 48_445 ?
Cu1 Se2 Cu1 Se15 -34.94(13) 7_456 . . 48_445 ?
Cu1 Se2 Cu1 Se15 -96.89(9) 48_445 . . 48_445 ?
Cu23 Se2 Cu1 Se1 143.04(11) 37_456 . . 48_445 ?
Cu23 Se2 Cu1 Se1 -36.96(11) . . . 48_445 ?
Cu1 Se2 Cu1 Se1 -95.99(16) 43 . . 48_445 ?
Cu1 Se2 Cu1 Se1 35(100) 37_456 . . 48_445 ?
Cu1 Se2 Cu1 Se1 -157.94(10) 12_566 . . 48_445 ?
Cu1 Se2 Cu1 Se1 84.01(16) 7_456 . . 48_445 ?
Cu1 Se2 Cu1 Se1 22.06(10) 48_445 . . 48_445 ?
Cu23 Se2 Cu1 Cu23 180.0 . . . 37_456 ?
Cu1 Se2 Cu1 Cu23 120.98(7) 43 . . 37_456 ?
Cu1 Se2 Cu1 Cu23 -108(100) 37_456 . . 37_456 ?
Cu1 Se2 Cu1 Cu23 59.02(7) 12_566 . . 37_456 ?
Cu1 Se2 Cu1 Cu23 -59.02(7) 7_456 . . 37_456 ?
Cu1 Se2 Cu1 Cu23 -120.98(7) 48_445 . . 37_456 ?
Cu23 Se2 Cu1 Cu1 -120.98(7) 37_456 . . 43 ?
Cu23 Se2 Cu1 Cu1 59.02(7) . . . 43 ?
Cu1 Se2 Cu1 Cu1 131(100) 37_456 . . 43 ?
Cu1 Se2 Cu1 Cu1 -61.95(14) 12_566 . . 43 ?
Cu1 Se2 Cu1 Cu1 180.0 7_456 . . 43 ?
Cu1 Se2 Cu1 Cu1 118.05(14) 48_445 . . 43 ?
Cu23 Se2 Cu1 Cu1 120.98(7) 37_456 . . 48_445 ?
Cu23 Se2 Cu1 Cu1 -59.02(7) . . . 48_445 ?
Cu1 Se2 Cu1 Cu1 -118.05(14) 43 . . 48_445 ?
Cu1 Se2 Cu1 Cu1 13(100) 37_456 . . 48_445 ?
Cu1 Se2 Cu1 Cu1 180.0 12_566 . . 48_445 ?
Cu1 Se2 Cu1 Cu1 61.95(14) 7_456 . . 48_445 ?
Ge1 Se15 Cu23 Se15 -179.08(14) 28_565 . . 12_566 ?
Cu1 Se15 Cu23 Se15 87.16(19) 43 . . 12_566 ?
Ge1 Se15 Cu23 Se15 -43.5(2) 28_565 . . 7_456 ?
Cu1 Se15 Cu23 Se15 -137.2(2) 43 . . 7_456 ?
Ge1 Se15 Cu23 Se2 68.73(11) 28_565 . . . ?
Cu1 Se15 Cu23 Se2 -25.04(9) 43 . . . ?
Ge1 Se15 Cu23 Cu1 93.77(12) 28_565 . . 43 ?
Ge1 Se15 Cu23 Cu1 119.4(2) 28_565 . . 37_456 ?
Cu1 Se15 Cu23 Cu1 25.6(2) 43 . . 37_456 ?
Ge1 Se15 Cu23 Cu1 11.73(17) 28_565 . . 48_445 ?
Cu1 Se15 Cu23 Cu1 -82.04(15) 43 . . 48_445 ?
Cu23 Se2 Cu23 Se15 46(100) 37_456 . . 12_566 ?
Cu1 Se2 Cu23 Se15 -95.61(9) 43 . . 12_566 ?
Cu1 Se2 Cu23 Se15 24.39(9) 37_456 . . 12_566 ?
Cu1 Se2 Cu23 Se15 -155.61(9) . . . 12_566 ?
Cu1 Se2 Cu23 Se15 -35.61(9) 12_566 . . 12_566 ?
Cu1 Se2 Cu23 Se15 84.39(9) 7_456 . . 12_566 ?
Cu1 Se2 Cu23 Se15 144.39(9) 48_445 . . 12_566 ?
Cu23 Se2 Cu23 Se15 166(100) 37_456 . . . ?
Cu1 Se2 Cu23 Se15 24.39(9) 43 . . . ?
Cu1 Se2 Cu23 Se15 144.39(9) 37_456 . . . ?
Cu1 Se2 Cu23 Se15 -35.61(9) . . . . ?
Cu1 Se2 Cu23 Se15 84.39(9) 12_566 . . . ?
Cu1 Se2 Cu23 Se15 -155.61(9) 7_456 . . . ?
Cu1 Se2 Cu23 Se15 -95.61(9) 48_445 . . . ?
Cu23 Se2 Cu23 Se15 -74(100) 37_456 . . 7_456 ?
Cu1 Se2 Cu23 Se15 144.39(9) 43 . . 7_456 ?
Cu1 Se2 Cu23 Se15 -95.61(9) 37_456 . . 7_456 ?
Cu1 Se2 Cu23 Se15 84.39(9) . . . 7_456 ?
Cu1 Se2 Cu23 Se15 -155.61(9) 12_566 . . 7_456 ?
Cu1 Se2 Cu23 Se15 -35.61(9) 7_456 . . 7_456 ?
Cu1 Se2 Cu23 Se15 24.39(9) 48_445 . . 7_456 ?
Cu23 Se2 Cu23 Cu1 142(100) 37_456 . . 43 ?
Cu1 Se2 Cu23 Cu1 120.0 37_456 . . 43 ?
Cu1 Se2 Cu23 Cu1 -60.0 . . . 43 ?
Cu1 Se2 Cu23 Cu1 60.0 12_566 . . 43 ?
Cu1 Se2 Cu23 Cu1 180.0 7_456 . . 43 ?
Cu1 Se2 Cu23 Cu1 -120.0 48_445 . . 43 ?
Cu23 Se2 Cu23 Cu1 22(100) 37_456 . . 37_456 ?
Cu1 Se2 Cu23 Cu1 -120.0 43 . . 37_456 ?
Cu1 Se2 Cu23 Cu1 180.0 . . . 37_456 ?
Cu1 Se2 Cu23 Cu1 -60.0 12_566 . . 37_456 ?
Cu1 Se2 Cu23 Cu1 60.0 7_456 . . 37_456 ?
Cu1 Se2 Cu23 Cu1 120.0 48_445 . . 37_456 ?
Cu23 Se2 Cu23 Cu1 -98(100) 37_456 . . 48_445 ?
Cu1 Se2 Cu23 Cu1 120.0 43 . . 48_445 ?
Cu1 Se2 Cu23 Cu1 -120.0 37_456 . . 48_445 ?
Cu1 Se2 Cu23 Cu1 60.0 . . . 48_445 ?
Cu1 Se2 Cu23 Cu1 180.0 12_566 . . 48_445 ?
Cu1 Se2 Cu23 Cu1 -60.0 7_456 . . 48_445 ?

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        22.47
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         0.709
_refine_diff_density_min         -0.768
_refine_diff_density_rms         0.160

loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 -0.050 -0.028 -0.021 6945 2033 ' '
_platon_squeeze_details          ?

####################################################################### 
# 
# 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_scs_sq_d
_database_code_depnum_ccdc_archive 'CCDC 1470884'
_audit_update_record             
;
2016-03-28 deposited with the CCDC.
2016-12-16 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            CuSnSe
_chemical_melting_point          ?
_chemical_formula_moiety         'Cu32 Se76 Sn24'
_chemical_formula_sum            'Cu32 Se76 Sn24'
_chemical_formula_weight         10883.60

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 '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'
Sn Sn -0.6537 1.4246 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           cubic
_symmetry_space_group_name_H-M   'I m -3'
_symmetry_space_group_name_Hall  '-I 2 2 3'

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

_cell_length_a                   24.0523(5)
_cell_length_b                   24.0523(5)
_cell_length_c                   24.0523(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     13914.6(9)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    1077
_cell_measurement_theta_min      3.5800
_cell_measurement_theta_max      20.4120

_exptl_crystal_description       cubic
_exptl_crystal_colour            black
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.13
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.598
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             9424.0
_exptl_absorpt_coefficient_mu    14.442
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  0.176
_exptl_absorpt_correction_T_max  0.153
_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 area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            6497
_diffrn_reflns_av_R_equivalents  0.0567
_diffrn_reflns_av_sigmaI/netI    0.0783
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_theta_min         3.17
_diffrn_reflns_theta_max         25.00
_reflns_number_total             2219
_reflns_number_gt                1147
_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)+(0.0872P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         2210
_refine_ls_number_parameters     54
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1130
_refine_ls_R_factor_gt           0.0610
_refine_ls_wR_factor_ref         0.1789
_refine_ls_wR_factor_gt          0.1658
_refine_ls_goodness_of_fit_ref   0.985
_refine_ls_restrained_S_all      0.985
_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
Sn1 Sn 0.07110(4) 0.29471(5) 0.20514(5) 0.0711(4) Uani 1 1 d . . .
Se4 Se 0.2500 0.2500 0.2500 0.0580(9) Uani 1 6 d S . .
Se5 Se 0.14687(6) 0.36417(7) 0.19098(7) 0.0732(5) Uani 1 1 d . . .
Se2 Se 0.0000 0.32924(11) 0.27738(10) 0.0792(7) Uani 1 2 d S . .
Se6 Se 0.09716(7) 0.19683(7) 0.22878(8) 0.0817(6) Uani 1 1 d . . .
Se1 Se 0.0000 0.29396(13) 0.12462(11) 0.0984(10) Uani 1 2 d S . .
Cu7 Cu 0.19627(8) 0.33885(8) 0.27632(8) 0.0771(6) Uani 1 1 d . . .
Cu8 Cu 0.18900(9) 0.18900(9) 0.18900(9) 0.0821(11) 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
Sn1 0.0541(7) 0.0876(9) 0.0716(8) 0.0089(6) 0.0003(5) 0.0001(6)
Se4 0.0580(9) 0.0580(9) 0.0580(9) -0.0014(10) -0.0014(10) -0.0014(10)
Se5 0.0578(10) 0.0771(11) 0.0846(12) 0.0148(9) 0.0067(8) 0.0056(8)
Se2 0.0688(15) 0.0987(19) 0.0701(16) 0.0002(13) 0.000 0.000
Se6 0.0687(11) 0.0775(12) 0.0988(14) 0.0040(10) -0.0012(10) -0.0083(9)
Se1 0.0767(17) 0.156(3) 0.0627(16) 0.0117(16) 0.000 0.000
Cu7 0.0859(15) 0.0755(13) 0.0699(13) 0.0064(11) -0.0003(10) 0.0029(11)
Cu8 0.0821(11) 0.0821(11) 0.0821(11) -0.0056(11) -0.0056(11) -0.0056(11)

_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
Sn1 Se5 2.4957(19) . ?
Sn1 Se6 2.502(2) . ?
Sn1 Se2 2.576(2) . ?
Sn1 Se1 2.584(2) . ?
Se4 Cu8 2.541(4) . ?
Se4 Cu8 2.541(4) 37 ?
Se4 Cu7 2.576(2) 9 ?
Se4 Cu7 2.576(2) 41 ?
Se4 Cu7 2.576(2) . ?
Se4 Cu7 2.576(2) 37 ?
Se4 Cu7 2.576(2) 45 ?
Se4 Cu7 2.576(2) 5 ?
Se5 Cu7 2.449(3) . ?
Se5 Cu7 2.458(3) 41 ?
Se2 Sn1 2.576(2) 28 ?
Se6 Cu8 2.415(2) . ?
Se6 Cu7 2.457(3) 45 ?
Se1 Sn1 2.584(2) 28 ?
Cu7 Se6 2.457(3) 41 ?
Cu7 Se5 2.458(3) 45 ?
Cu7 Cu8 2.960(3) 37 ?
Cu7 Cu7 2.970(3) 41 ?
Cu7 Cu7 2.970(3) 45 ?
Cu8 Se6 2.415(2) 9 ?
Cu8 Se6 2.415(2) 5 ?
Cu8 Cu7 2.960(3) 41 ?
Cu8 Cu7 2.960(3) 45 ?
Cu8 Cu7 2.960(3) 37 ?

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
Se5 Sn1 Se6 118.56(7) . . ?
Se5 Sn1 Se2 111.17(8) . . ?
Se6 Sn1 Se2 108.45(8) . . ?
Se5 Sn1 Se1 112.69(8) . . ?
Se6 Sn1 Se1 109.24(9) . . ?
Se2 Sn1 Se1 93.93(7) . . ?
Cu8 Se4 Cu8 180.00(15) . 37 ?
Cu8 Se4 Cu7 109.34(5) . 9 ?
Cu8 Se4 Cu7 70.66(5) 37 9 ?
Cu8 Se4 Cu7 70.66(5) . 41 ?
Cu8 Se4 Cu7 109.34(5) 37 41 ?
Cu7 Se4 Cu7 70.40(5) 9 41 ?
Cu8 Se4 Cu7 109.34(5) . . ?
Cu8 Se4 Cu7 70.66(5) 37 . ?
Cu7 Se4 Cu7 109.60(5) 9 . ?
Cu7 Se4 Cu7 70.40(5) 41 . ?
Cu8 Se4 Cu7 70.66(5) . 37 ?
Cu8 Se4 Cu7 109.34(5) 37 37 ?
Cu7 Se4 Cu7 70.40(5) 9 37 ?
Cu7 Se4 Cu7 109.60(5) 41 37 ?
Cu7 Se4 Cu7 180.0 . 37 ?
Cu8 Se4 Cu7 70.66(5) . 45 ?
Cu8 Se4 Cu7 109.34(5) 37 45 ?
Cu7 Se4 Cu7 180.00(9) 9 45 ?
Cu7 Se4 Cu7 109.60(5) 41 45 ?
Cu7 Se4 Cu7 70.40(5) . 45 ?
Cu7 Se4 Cu7 109.60(5) 37 45 ?
Cu8 Se4 Cu7 109.34(5) . 5 ?
Cu8 Se4 Cu7 70.66(5) 37 5 ?
Cu7 Se4 Cu7 109.60(5) 9 5 ?
Cu7 Se4 Cu7 180.00(9) 41 5 ?
Cu7 Se4 Cu7 109.60(5) . 5 ?
Cu7 Se4 Cu7 70.40(5) 37 5 ?
Cu7 Se4 Cu7 70.40(5) 45 5 ?
Cu7 Se5 Cu7 74.51(10) . 41 ?
Cu7 Se5 Sn1 94.21(8) . . ?
Cu7 Se5 Sn1 101.11(8) 41 . ?
Sn1 Se2 Sn1 83.21(9) 28 . ?
Cu8 Se6 Cu7 74.82(10) . 45 ?
Cu8 Se6 Sn1 102.27(7) . . ?
Cu7 Se6 Sn1 94.38(8) 45 . ?
Sn1 Se1 Sn1 82.89(9) . 28 ?
Se5 Cu7 Se6 114.87(10) . 41 ?
Se5 Cu7 Se5 114.56(9) . 45 ?
Se6 Cu7 Se5 114.79(10) 41 45 ?
Se5 Cu7 Se4 104.11(8) . . ?
Se6 Cu7 Se4 102.48(8) 41 . ?
Se5 Cu7 Se4 103.84(8) 45 . ?
Se5 Cu7 Cu8 138.16(9) . 37 ?
Se6 Cu7 Cu8 51.94(8) 41 37 ?
Se5 Cu7 Cu8 105.88(8) 45 37 ?
Se4 Cu7 Cu8 54.12(7) . 37 ?
Se5 Cu7 Cu7 52.89(8) . 41 ?
Se6 Cu7 Cu7 105.10(9) 41 41 ?
Se5 Cu7 Cu7 138.53(12) 45 41 ?
Se4 Cu7 Cu7 54.80(2) . 41 ?
Cu8 Cu7 Cu7 89.52(5) 37 41 ?
Se5 Cu7 Cu7 106.26(11) . 45 ?
Se6 Cu7 Cu7 137.28(10) 41 45 ?
Se5 Cu7 Cu7 52.60(7) 45 45 ?
Se4 Cu7 Cu7 54.80(2) . 45 ?
Cu8 Cu7 Cu7 89.52(5) 37 45 ?
Cu7 Cu7 Cu7 90.28(10) 41 45 ?
Se6 Cu8 Se6 113.76(7) 9 . ?
Se6 Cu8 Se6 113.76(7) 9 5 ?
Se6 Cu8 Se6 113.76(7) . 5 ?
Se6 Cu8 Se4 104.73(9) 9 . ?
Se6 Cu8 Se4 104.73(9) . . ?
Se6 Cu8 Se4 104.73(9) 5 . ?
Se6 Cu8 Cu7 53.24(6) 9 41 ?
Se6 Cu8 Cu7 105.95(7) . 41 ?
Se6 Cu8 Cu7 139.37(9) 5 41 ?
Se4 Cu8 Cu7 55.22(7) . 41 ?
Se6 Cu8 Cu7 139.37(9) 9 45 ?
Se6 Cu8 Cu7 53.24(6) . 45 ?
Se6 Cu8 Cu7 105.95(7) 5 45 ?
Se4 Cu8 Cu7 55.22(7) . 45 ?
Cu7 Cu8 Cu7 90.69(10) 41 45 ?
Se6 Cu8 Cu7 105.95(7) 9 37 ?
Se6 Cu8 Cu7 139.37(9) . 37 ?
Se6 Cu8 Cu7 53.24(6) 5 37 ?
Se4 Cu8 Cu7 55.22(7) . 37 ?
Cu7 Cu8 Cu7 90.69(10) 41 37 ?
Cu7 Cu8 Cu7 90.69(10) 45 37 ?

_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max         0.749
_refine_diff_density_min         -0.844
_refine_diff_density_rms         0.174
# SQUEEZE RESULTS (APPEND TO CIF)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 -0.047 -0.030 -0.032 7467 2179 ' '
_platon_squeeze_details          ?
####################################################################### 
# 
# 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_sq_d_sq_d
_database_code_depnum_ccdc_archive 'CCDC 1470885'
_audit_update_record             
;
2016-10-17 deposited with the CCDC.
2016-12-16 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            1c
_chemical_melting_point          'C12 H Cl3 Cu32 Ge24 N12 Ni6 S72'
_chemical_formula_moiety         'C12 H Cl3 Cu32 Ge24 N12 Ni6 S72'
_chemical_formula_sum            'C12 H Cl3 Cu32 Ge24 N12 Ni6 S72'
_chemical_formula_weight         6855.29

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 '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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 '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'

_symmetry_cell_setting           cubic
_symmetry_space_group_name_H-M   'I m -3'
_symmetry_space_group_name_Hall  '-I 2 2 3'

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

_cell_length_a                   22.7454(6)
_cell_length_b                   22.7454(6)
_cell_length_c                   22.7454(6)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     11767.4(5)
_cell_formula_units_Z            2
_cell_measurement_temperature    273(2)
_cell_measurement_reflns_used    9459
_cell_measurement_theta_min      2.53
_cell_measurement_theta_max      26.23

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.935
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             8976
_exptl_absorpt_coefficient_mu    6.986
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      273(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 area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            29719
_diffrn_reflns_av_R_equivalents  0.0662
_diffrn_reflns_av_sigmaI/netI    0.0276
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_theta_min         2.83
_diffrn_reflns_theta_max         24.97
_reflns_number_total             1870
_reflns_number_gt                1382
_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)+(0.1000P)²+400.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         1870
_refine_ls_number_parameters     71
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0955
_refine_ls_R_factor_gt           0.0782
_refine_ls_wR_factor_ref         0.2156
_refine_ls_wR_factor_gt          0.2023
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_restrained_S_all      1.056
_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
Ge1 Ge 0.22562(5) 0.27084(5) 0.43402(5) 0.0454(4) Uani 1 1 d . . .
Cu1 Cu 0.31922(6) 0.31922(6) 0.31922(6) 0.0508(7) Uani 1 3 d S . .
Cu2 Cu 0.30072(7) 0.18296(7) 0.33713(7) 0.0553(5) Uani 1 1 d . . .
S1 S 0.20719(19) 0.19912(16) 0.5000 0.0461(9) Uani 1 2 d S . .
S6 S 0.31361(13) 0.25940(14) 0.39735(13) 0.0524(8) Uani 1 1 d . . .
S7 S 0.2245(2) 0.34418(17) 0.5000 0.0582(12) Uani 1 2 d S . .
S8 S 0.15146(13) 0.27896(14) 0.37358(14) 0.0528(8) Uani 1 1 d . . .
Ni2 Ni 0.19707(14) 0.5000 0.0000 0.0482(8) Uani 1 4 d S . .
Cl1 Cl 0.0000 0.5000 0.0000 0.101(5) Uani 1 8 d S . .
N1 N 0.2677(7) 0.5000 0.0612(7) 0.090(6) Uani 1 2 d S . .
C1 C 0.3240(12) 0.5000 0.0281(11) 0.120(11) Uani 1 2 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
Ge1 0.0509(7) 0.0405(7) 0.0449(7) -0.0010(5) -0.0021(5) -0.0007(5)
Cu1 0.0508(7) 0.0508(7) 0.0508(7) -0.0037(6) -0.0037(6) -0.0037(6)
Cu2 0.0569(9) 0.0570(9) 0.0518(9) -0.0027(7) 0.0006(7) -0.0044(7)
S1 0.055(2) 0.0302(18) 0.053(2) 0.000 0.000 0.0028(17)
S6 0.0520(17) 0.0578(18) 0.0473(16) 0.0005(13) -0.0028(13) -0.0001(14)
S7 0.095(4) 0.0286(19) 0.051(2) 0.000 0.000 0.003(2)
S8 0.0492(16) 0.0573(18) 0.0521(17) 0.0012(14) -0.0010(14) 0.0001(14)
Ni2 0.0512(17) 0.0483(16) 0.0451(16) 0.000 0.000 0.000
Cl1 0.045(5) 0.187(15) 0.071(7) 0.000 0.000 0.000
N1 0.047(9) 0.17(2) 0.053(9) 0.000 -0.023(8) 0.000
C1 0.083(17) 0.21(4) 0.068(14) 0.000 -0.019(13) 0.000

_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
Ge1 S6 2.184(3) . ?
Ge1 S8 2.184(3) . ?
Ge1 S7 2.244(3) . ?
Ge1 S1 2.256(3) . ?
Cu1 S6 2.242(3) 9 ?
Cu1 S6 2.242(3) 5 ?
Cu1 S6 2.242(3) . ?
Cu2 S6 2.233(3) . ?
Cu2 S8 2.238(3) 45 ?
Cu2 S8 2.238(3) 5 ?
S1 Ge1 2.256(3) 26_556 ?
S7 Ge1 2.244(3) 26_556 ?
S8 Cu2 2.238(3) 41 ?
S8 Cu2 2.238(3) 9 ?
Ni2 N1 2.126(14) . ?
Ni2 N1 2.126(14) 26 ?
N1 C1 1.48(3) . ?
C1 C1 1.28(5) 26 ?

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
S6 Ge1 S8 118.53(12) . . ?
S6 Ge1 S7 110.74(17) . . ?
S8 Ge1 S7 110.46(15) . . ?
S6 Ge1 S1 109.77(14) . . ?
S8 Ge1 S1 109.65(14) . . ?
S7 Ge1 S1 95.20(11) . . ?
S6 Cu1 S6 119.45(3) 9 5 ?
S6 Cu1 S6 119.45(3) 9 . ?
S6 Cu1 S6 119.45(3) 5 . ?
S6 Cu2 S8 118.86(13) . 45 ?
S6 Cu2 S8 120.98(13) . 5 ?
S8 Cu2 S8 118.97(9) 45 5 ?
Ge1 S1 Ge1 83.41(14) 26_556 . ?
Ge1 S6 Cu2 101.94(13) . . ?
Ge1 S6 Cu1 106.41(13) . . ?
Cu2 S6 Cu1 89.64(13) . . ?
Ge1 S7 Ge1 83.95(15) . 26_556 ?
Ge1 S8 Cu2 101.75(13) . 41 ?
Ge1 S8 Cu2 105.59(14) . 9 ?
Cu2 S8 Cu2 90.92(13) 41 9 ?
N1 Ni2 N1 81.8(10) . 26 ?
C1 N1 Ni2 108.6(13) . . ?
C1 C1 N1 120.5(11) 26 . ?

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        24.97
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         1.025
_refine_diff_density_min         -1.152
_refine_diff_density_rms         0.203

# SQUEEZE RESULTS (APPEND TO CIF)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 -0.002 -0.001 -0.001 2462 533 ' '
2 -0.064 0.497 0.494 2462 533 ' '
3 0.250 0.250 0.250 11 2 ' '
4 0.250 0.250 0.750 11 2 ' '
5 0.250 0.750 0.250 11 2 ' '
6 0.250 0.750 0.750 11 2 ' '
7 0.750 0.250 0.250 11 2 ' '
8 0.750 0.250 0.750 11 2 ' '
9 0.750 0.750 0.250 11 2 ' '
10 0.750 0.750 0.750 11 2 ' '
_platon_squeeze_details          ?
