# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2014

#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_l

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C24 H40 Ge4 N4 O6 S10'
_chemical_formula_weight         1091.56

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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ge Ge 0.1547 1.8001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_H-M   'I 41/a  '
_symmetry_space_group_name_Hall  '-I 4ad  '

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y+3/4, x+1/4, z+1/4'
'-x+1/2, -y, z+1/2'
'y+3/4, -x+3/4, z+3/4'
'x+1/2, y+1/2, z+1/2'
'-y+5/4, x+3/4, z+3/4'
'-x+1, -y+1/2, z+1'
'y+5/4, -x+5/4, z+5/4'
'-x, -y, -z'
'y-3/4, -x-1/4, -z-1/4'
'x-1/2, y, -z-1/2'
'-y-3/4, x-3/4, -z-3/4'
'-x+1/2, -y+1/2, -z+1/2'
'y-1/4, -x+1/4, -z+1/4'
'x, y+1/2, -z'
'-y-1/4, x-1/4, -z-1/4'

_cell_length_a                   10.9355(8)
_cell_length_b                   10.9355(8)
_cell_length_c                   34.918(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     4175.6(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    223(2)
_cell_measurement_reflns_used    5651
_cell_measurement_theta_min      3.5
_cell_measurement_theta_max      27.5

_exptl_crystal_description       Block
_exptl_crystal_colour            Yellow
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.736
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2192
_exptl_absorpt_coefficient_mu    3.392
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.3831
_exptl_absorpt_correction_T_max  0.5502
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication '
_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      223(2)
_diffrn_radiation_wavelength     0.71075
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Rigaku Saturn'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean 14.63
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            8020
_diffrn_reflns_av_R_equivalents  0.0326
_diffrn_reflns_av_sigmaI/netI    0.0330
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_limit_l_max       45
_diffrn_reflns_theta_min         3.46
_diffrn_reflns_theta_max         27.48
_reflns_number_total             2388
_reflns_number_gt                2055
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrystalClear (Rigaku Corporation, 1999)'
_computing_cell_refinement       'CrystalClear (Rigaku Corporation, 1999)'
_computing_data_reduction        'CrystalClear (Rigaku Corporation, 1999)'
_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)+(0.0457P)²+2.8245P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         2388
_refine_ls_number_parameters     112
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0511
_refine_ls_R_factor_gt           0.0397
_refine_ls_wR_factor_ref         0.0961
_refine_ls_wR_factor_gt          0.0909
_refine_ls_goodness_of_fit_ref   1.127
_refine_ls_restrained_S_all      1.127
_refine_ls_shift/su_max          0.015
_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 0.57776(3) -0.10153(3) 0.660776(9) 0.02044(13) Uani 1 1 d . . .
S1 S 0.65707(8) 0.03457(8) 0.69647(2) 0.0281(2) Uani 1 1 d . . .
S2 S 0.5000 -0.2500 0.69822(3) 0.0219(2) Uani 1 2 d S . .
S3 S 0.42509(7) -0.02245(7) 0.62634(2) 0.02364(19) Uani 1 1 d . . .
N1 N 0.7727(3) 0.0835(3) 0.54520(7) 0.0274(6) Uani 1 1 d . . .
C1 C 0.7760(3) 0.2045(3) 0.55006(10) 0.0321(8) Uani 1 1 d . . .
H1 H 0.8517 0.2441 0.5529 0.039 Uiso 1 1 calc R . .
C2 C 0.6702(3) 0.2717(3) 0.55090(10) 0.0323(8) Uani 1 1 d . . .
H2 H 0.6738 0.3566 0.5549 0.039 Uiso 1 1 calc R . .
C3 C 0.5580(3) 0.2148(3) 0.54593(8) 0.0245(7) Uani 1 1 d . . .
C4 C 0.5578(3) 0.0882(3) 0.54092(9) 0.0289(7) Uani 1 1 d . . .
H4 H 0.4834 0.0463 0.5378 0.035 Uiso 1 1 calc R . .
C5 C 0.6657(3) 0.0253(3) 0.54051(9) 0.0299(8) Uani 1 1 d . . .
H5 H 0.6649 -0.0599 0.5369 0.036 Uiso 1 1 calc R . .
C6 C 0.8873(3) 0.0123(4) 0.54476(11) 0.0371(9) Uani 1 1 d . . .
H6A H 0.9564 0.0676 0.5427 0.056 Uiso 1 1 calc R . .
H6B H 0.8869 -0.0430 0.5230 0.056 Uiso 1 1 calc R . .
H6C H 0.8940 -0.0344 0.5683 0.056 Uiso 1 1 calc R . .
O1 O 0.8607(3) 0.1449(3) 0.63456(9) 0.0544(8) Uani 1 1 d . . .
O2 O 1.0000 0.2500 0.49094(10) 0.0407(9) Uani 1 2 d S . .


_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 S1 2.1262(9) . ?
Ge1 S3 2.2317(8) . ?
Ge1 S3 2.2383(8) 14_656 ?
Ge1 S2 2.2513(7) . ?
S2 Ge1 2.2513(7) 7_544 ?
S3 Ge1 2.2383(8) 12_657 ?
N1 C1 1.334(5) . ?
N1 C5 1.343(4) . ?
N1 C6 1.475(4) . ?
C1 C2 1.371(5) . ?
C1 H1 0.9400 . ?
C2 C3 1.387(5) . ?
C2 H2 0.9400 . ?
C3 C4 1.395(5) . ?
C3 C3 1.485(7) 7_554 ?
C4 C5 1.366(5) . ?
C4 H4 0.9400 . ?
C5 H5 0.9400 . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C6 H6C 0.9700 . ?

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
S1 Ge1 S3 110.47(3) . . ?
S1 Ge1 S3 107.01(3) . 14_656 ?
S3 Ge1 S3 112.01(2) . 14_656 ?
S1 Ge1 S2 108.57(3) . . ?
S3 Ge1 S2 108.04(3) . . ?
S3 Ge1 S2 110.70(3) 14_656 . ?
Ge1 S2 Ge1 109.00(4) . 7_544 ?
Ge1 S3 Ge1 107.29(3) . 12_657 ?
C1 N1 C5 120.6(3) . . ?
C1 N1 C6 120.1(3) . . ?
C5 N1 C6 119.3(3) . . ?
N1 C1 C2 120.8(3) . . ?
N1 C1 H1 119.6 . . ?
C2 C1 H1 119.6 . . ?
C1 C2 C3 120.2(3) . . ?
C1 C2 H2 119.9 . . ?
C3 C2 H2 119.9 . . ?
C2 C3 C4 117.6(3) . . ?
C2 C3 C3 121.6(4) . 7_554 ?
C4 C3 C3 120.9(4) . 7_554 ?
C5 C4 C3 120.0(3) . . ?
C5 C4 H4 120.0 . . ?
C3 C4 H4 120.0 . . ?
N1 C5 C4 120.9(3) . . ?
N1 C5 H5 119.6 . . ?
C4 C5 H5 119.6 . . ?
N1 C6 H6A 109.5 . . ?
N1 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
N1 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?

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
S1 Ge1 S2 Ge1 -177.79(3) . . . 7_544 ?
S3 Ge1 S2 Ge1 62.38(2) . . . 7_544 ?
S3 Ge1 S2 Ge1 -60.61(2) 14_656 . . 7_544 ?
S1 Ge1 S3 Ge1 178.88(4) . . . 12_657 ?
S3 Ge1 S3 Ge1 59.69(3) 14_656 . . 12_657 ?
S2 Ge1 S3 Ge1 -62.49(4) . . . 12_657 ?
C5 N1 C1 C2 0.9(5) . . . . ?
C6 N1 C1 C2 -179.4(3) . . . . ?
N1 C1 C2 C3 -1.3(5) . . . . ?
C1 C2 C3 C4 1.3(5) . . . . ?
C1 C2 C3 C3 -178.8(2) . . . 7_554 ?
C2 C3 C4 C5 -0.9(5) . . . . ?
C3 C3 C4 C5 179.1(2) 7_554 . . . ?
C1 N1 C5 C4 -0.6(5) . . . . ?
C6 N1 C5 C4 179.7(3) . . . . ?
C3 C4 C5 N1 0.6(5) . . . . ?

_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full        27.48
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max         0.555
_refine_diff_density_min         -0.440
_refine_diff_density_rms         0.115
_database_code_depnum_ccdc_archive 'CCDC 961237'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_1'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C24 H40 Ge4 N4 O6 S10'
_chemical_formula_weight         1091.56

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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ge Ge 0.1547 1.8001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'C 2/c  '
_symmetry_space_group_name_Hall  '-C 2yc '

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

_cell_length_a                   9.2968(15)
_cell_length_b                   21.035(3)
_cell_length_c                   21.516(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 101.997(5)
_cell_angle_gamma                90.00
_cell_volume                     4115.7(12)
_cell_formula_units_Z            4
_cell_measurement_temperature    223(2)
_cell_measurement_reflns_used    7762
_cell_measurement_theta_min      3.4
_cell_measurement_theta_max      27.5

_exptl_crystal_description       Block
_exptl_crystal_colour            Orange
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.05
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.762
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2192
_exptl_absorpt_coefficient_mu    3.442
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5049
_exptl_absorpt_correction_T_max  0.8467
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication '
_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      223(2)
_diffrn_radiation_wavelength     0.71075
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Rigaku Saturn'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean 14.63
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            10142
_diffrn_reflns_av_R_equivalents  0.0981
_diffrn_reflns_av_sigmaI/netI    0.1177
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         3.42
_diffrn_reflns_theta_max         25.00
_reflns_number_total             3600
_reflns_number_gt                2349
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrystalClear (Rigaku Corporation, 1999)'
_computing_cell_refinement       'CrystalClear (Rigaku Corporation, 1999)'
_computing_data_reduction        'CrystalClear (Rigaku Corporation, 1999)'
_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)+(0.0306P)²+15.8000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         3600
_refine_ls_number_parameters     221
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1454
_refine_ls_R_factor_gt           0.0876
_refine_ls_wR_factor_ref         0.1465
_refine_ls_wR_factor_gt          0.1293
_refine_ls_goodness_of_fit_ref   1.184
_refine_ls_restrained_S_all      1.184
_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 0.65051(12) 0.54049(5) 0.31758(5) 0.0306(3) Uani 1 1 d . . .
Ge2 Ge 0.63107(11) 0.66121(5) 0.19839(5) 0.0294(3) Uani 1 1 d . . .
S1 S 0.7965(3) 0.48179(15) 0.38255(13) 0.0512(9) Uani 1 1 d . . .
S2 S 0.5000 0.47835(17) 0.2500 0.0335(9) Uani 1 2 d S . .
S3 S 0.7864(3) 0.60118(13) 0.26719(11) 0.0342(7) Uani 1 1 d . . .
S4 S 0.5184(3) 0.60024(13) 0.37187(10) 0.0322(6) Uani 1 1 d . . .
S5 S 0.7532(3) 0.72197(13) 0.14961(13) 0.0429(7) Uani 1 1 d . . .
S6 S 0.5000 0.72373(17) 0.2500 0.0350(9) Uani 1 2 d S . .
N1 N 0.8572(9) 0.5747(5) 0.6189(4) 0.053(3) Uani 1 1 d . . .
N2 N 0.9590(9) 0.7963(5) 0.3899(4) 0.044(2) Uani 1 1 d . . .
C1 C 0.8521(13) 0.5563(6) 0.5586(5) 0.059(4) Uani 1 1 d . . .
H1 H 0.8332 0.5135 0.5473 0.071 Uiso 1 1 calc R . .
C2 C 0.8737(12) 0.5988(6) 0.5134(5) 0.050(3) Uani 1 1 d . . .
H2 H 0.8696 0.5848 0.4716 0.060 Uiso 1 1 calc R . .
C3 C 0.9015(11) 0.6621(6) 0.5284(5) 0.042(3) Uani 1 1 d . . .
C4 C 0.9081(12) 0.6794(6) 0.5915(5) 0.051(3) Uani 1 1 d . . .
H4 H 0.9275 0.7218 0.6042 0.061 Uiso 1 1 calc R . .
C5 C 0.8863(11) 0.6340(7) 0.6357(5) 0.058(4) Uani 1 1 d . . .
H5 H 0.8924 0.6461 0.6782 0.069 Uiso 1 1 calc R . .
C6 C 0.8932(13) 0.7415(6) 0.3715(5) 0.052(3) Uani 1 1 d . . .
H6 H 0.8593 0.7333 0.3280 0.063 Uiso 1 1 calc R . .
C7 C 0.8741(13) 0.6963(6) 0.4160(5) 0.052(3) Uani 1 1 d . . .
H7 H 0.8279 0.6575 0.4021 0.063 Uiso 1 1 calc R . .
C8 C 0.9221(11) 0.7073(5) 0.4807(5) 0.035(3) Uani 1 1 d . . .
C9 C 0.9911(14) 0.7645(5) 0.4959(5) 0.058(4) Uani 1 1 d . . .
H9 H 1.0288 0.7739 0.5390 0.069 Uiso 1 1 calc R . .
C10 C 1.0073(13) 0.8086(6) 0.4508(5) 0.058(4) Uani 1 1 d . . .
H10 H 1.0530 0.8477 0.4634 0.070 Uiso 1 1 calc R . .
C11 C 0.8394(14) 0.5264(7) 0.6673(5) 0.073(4) Uani 1 1 d . . .
H11A H 0.8158 0.5476 0.7040 0.110 Uiso 1 1 calc R . .
H11B H 0.9302 0.5027 0.6802 0.110 Uiso 1 1 calc R . .
H11C H 0.7605 0.4975 0.6493 0.110 Uiso 1 1 calc R . .
C12 C 0.9781(12) 0.8429(5) 0.3415(5) 0.051(3) Uani 1 1 d . . .
H12A H 1.0185 0.8819 0.3621 0.076 Uiso 1 1 calc R . .
H12B H 0.8837 0.8516 0.3139 0.076 Uiso 1 1 calc R . .
H12C H 1.0449 0.8258 0.3165 0.076 Uiso 1 1 calc R . .
O1 O 0.6922(8) 0.8600(4) 0.2186(3) 0.052(2) Uani 1 1 d . . .
O2 O 0.9090(18) 0.0473(5) 0.5184(5) 0.154(6) Uani 1 1 d . . .
O3 O 0.6587(17) 0.1037(5) 0.4350(7) 0.174(7) Uani 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ge1 S1 2.129(3) . ?
Ge1 S2 2.221(2) . ?
Ge1 S3 2.229(3) . ?
Ge1 S4 2.247(3) . ?
Ge2 S5 2.126(3) . ?
Ge2 S3 2.232(3) . ?
Ge2 S4 2.233(3) 2_655 ?
Ge2 S6 2.238(2) . ?
S2 Ge1 2.221(2) 2_655 ?
S4 Ge2 2.233(3) 2_655 ?
S6 Ge2 2.238(2) 2_655 ?
N1 C5 1.312(15) . ?
N1 C1 1.346(13) . ?
N1 C11 1.488(13) . ?
N2 C10 1.319(12) . ?
N2 C6 1.326(13) . ?
N2 C12 1.468(12) . ?
C1 C2 1.365(14) . ?
C1 H1 0.9400 . ?
C2 C3 1.383(15) . ?
C2 H2 0.9400 . ?
C3 C4 1.393(14) . ?
C3 C8 1.441(14) . ?
C4 C5 1.392(15) . ?
C4 H4 0.9400 . ?
C5 H5 0.9400 . ?
C6 C7 1.387(14) . ?
C6 H6 0.9400 . ?
C7 C8 1.390(13) . ?
C7 H7 0.9400 . ?
C8 C9 1.371(14) . ?
C9 C10 1.373(14) . ?
C9 H9 0.9400 . ?
C10 H10 0.9400 . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C11 H11C 0.9700 . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C12 H12C 0.9700 . ?

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
S1 Ge1 S2 108.51(12) . . ?
S1 Ge1 S3 107.64(12) . . ?
S2 Ge1 S3 111.23(9) . . ?
S1 Ge1 S4 109.02(10) . . ?
S2 Ge1 S4 109.35(9) . . ?
S3 Ge1 S4 111.02(10) . . ?
S5 Ge2 S3 109.24(11) . . ?
S5 Ge2 S4 109.39(10) . 2_655 ?
S3 Ge2 S4 110.47(11) . 2_655 ?
S5 Ge2 S6 107.06(12) . . ?
S3 Ge2 S6 110.31(8) . . ?
S4 Ge2 S6 110.29(9) 2_655 . ?
Ge1 S2 Ge1 107.92(16) 2_655 . ?
Ge1 S3 Ge2 107.03(11) . . ?
Ge2 S4 Ge1 107.44(10) 2_655 . ?
Ge2 S6 Ge2 108.03(16) 2_655 . ?
C5 N1 C1 120.2(10) . . ?
C5 N1 C11 120.2(11) . . ?
C1 N1 C11 119.5(11) . . ?
C10 N2 C6 120.6(10) . . ?
C10 N2 C12 120.5(10) . . ?
C6 N2 C12 118.9(9) . . ?
N1 C1 C2 121.2(12) . . ?
N1 C1 H1 119.4 . . ?
C2 C1 H1 119.4 . . ?
C1 C2 C3 120.8(11) . . ?
C1 C2 H2 119.6 . . ?
C3 C2 H2 119.6 . . ?
C2 C3 C4 116.6(11) . . ?
C2 C3 C8 120.9(10) . . ?
C4 C3 C8 122.5(11) . . ?
C5 C4 C3 120.2(12) . . ?
C5 C4 H4 119.9 . . ?
C3 C4 H4 119.9 . . ?
N1 C5 C4 121.0(11) . . ?
N1 C5 H5 119.5 . . ?
C4 C5 H5 119.5 . . ?
N2 C6 C7 120.4(10) . . ?
N2 C6 H6 119.8 . . ?
C7 C6 H6 119.8 . . ?
C6 C7 C8 121.1(10) . . ?
C6 C7 H7 119.5 . . ?
C8 C7 H7 119.5 . . ?
C9 C8 C7 115.0(10) . . ?
C9 C8 C3 122.2(10) . . ?
C7 C8 C3 122.8(10) . . ?
C8 C9 C10 122.6(11) . . ?
C8 C9 H9 118.7 . . ?
C10 C9 H9 118.7 . . ?
N2 C10 C9 120.3(11) . . ?
N2 C10 H10 119.8 . . ?
C9 C10 H10 119.8 . . ?
N1 C11 H11A 109.5 . . ?
N1 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
N1 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
N2 C12 H12A 109.5 . . ?
N2 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
N2 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?

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
S1 Ge1 S2 Ge1 -179.73(10) . . . 2_655 ?
S3 Ge1 S2 Ge1 -61.50(8) . . . 2_655 ?
S4 Ge1 S2 Ge1 61.47(8) . . . 2_655 ?
S1 Ge1 S3 Ge2 179.18(11) . . . . ?
S2 Ge1 S3 Ge2 60.43(13) . . . . ?
S4 Ge1 S3 Ge2 -61.58(13) . . . . ?
S5 Ge2 S3 Ge1 178.88(11) . . . . ?
S4 Ge2 S3 Ge1 -60.74(13) 2_655 . . . ?
S6 Ge2 S3 Ge1 61.47(14) . . . . ?
S1 Ge1 S4 Ge2 179.56(13) . . . 2_655 ?
S2 Ge1 S4 Ge2 -61.95(14) . . . 2_655 ?
S3 Ge1 S4 Ge2 61.15(14) . . . 2_655 ?
S5 Ge2 S6 Ge2 179.71(10) . . . 2_655 ?
S3 Ge2 S6 Ge2 -61.53(8) . . . 2_655 ?
S4 Ge2 S6 Ge2 60.79(8) 2_655 . . 2_655 ?
C5 N1 C1 C2 -1.3(18) . . . . ?
C11 N1 C1 C2 -177.4(11) . . . . ?
N1 C1 C2 C3 0.0(19) . . . . ?
C1 C2 C3 C4 0.9(17) . . . . ?
C1 C2 C3 C8 -179.1(10) . . . . ?
C2 C3 C4 C5 -0.5(16) . . . . ?
C8 C3 C4 C5 179.5(10) . . . . ?
C1 N1 C5 C4 1.8(17) . . . . ?
C11 N1 C5 C4 177.9(10) . . . . ?
C3 C4 C5 N1 -0.9(17) . . . . ?
C10 N2 C6 C7 0.1(18) . . . . ?
C12 N2 C6 C7 179.6(10) . . . . ?
N2 C6 C7 C8 0.4(19) . . . . ?
C6 C7 C8 C9 -1.5(17) . . . . ?
C6 C7 C8 C3 178.6(11) . . . . ?
C2 C3 C8 C9 -160.3(11) . . . . ?
C4 C3 C8 C9 19.8(17) . . . . ?
C2 C3 C8 C7 19.7(17) . . . . ?
C4 C3 C8 C7 -160.3(11) . . . . ?
C7 C8 C9 C10 2.1(19) . . . . ?
C3 C8 C9 C10 -178.0(11) . . . . ?
C6 N2 C10 C9 0.5(18) . . . . ?
C12 N2 C10 C9 -179.0(11) . . . . ?
C8 C9 C10 N2 -2(2) . . . . ?

_diffrn_measured_fraction_theta_max 0.994
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.994
_refine_diff_density_max         0.702
_refine_diff_density_min         -0.561
_refine_diff_density_rms         0.136
_database_code_depnum_ccdc_archive 'CCDC 1000266'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_2

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C25 H32 Ge4 N4 O S10'
_chemical_formula_weight         1015.51

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'
O O 0.0106 0.0060 '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'
Ge Ge 0.1547 1.8001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1  '
_symmetry_space_group_name_Hall  '-P 1  '

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   10.0424(8)
_cell_length_b                   11.5726(12)
_cell_length_c                   17.4356(18)
_cell_angle_alpha                79.485(14)
_cell_angle_beta                 74.554(13)
_cell_angle_gamma                74.835(14)
_cell_volume                     1871.2(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    223(2)
_cell_measurement_reflns_used    7612
_cell_measurement_theta_min      3.0
_cell_measurement_theta_max      27.5

_exptl_crystal_description       Block
_exptl_crystal_colour            Red
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.802
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1012
_exptl_absorpt_coefficient_mu    3.769
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.4408
_exptl_absorpt_correction_T_max  0.7525
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication '
_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      223(2)
_diffrn_radiation_wavelength     0.71075
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Rigaku Saturn'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean 14.63
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            14823
_diffrn_reflns_av_R_equivalents  0.0696
_diffrn_reflns_av_sigmaI/netI    0.1026
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         3.08
_diffrn_reflns_theta_max         25.00
_reflns_number_total             6534
_reflns_number_gt                4232
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrystalClear (Rigaku Corporation, 1999)'
_computing_cell_refinement       'CrystalClear (Rigaku Corporation, 1999)'
_computing_data_reduction        'CrystalClear (Rigaku Corporation, 1999)'
_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)+(0.0076P)²+14.4300P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         6534
_refine_ls_number_parameters     404
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1332
_refine_ls_R_factor_gt           0.0784
_refine_ls_wR_factor_ref         0.1308
_refine_ls_wR_factor_gt          0.1116
_refine_ls_goodness_of_fit_ref   1.084
_refine_ls_restrained_S_all      1.084
_refine_ls_shift/su_max          0.047
_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 -0.04513(11) 0.14554(10) 0.69008(6) 0.0311(3) Uani 1 1 d . . .
Ge2 Ge 0.26450(11) 0.27840(10) 0.63397(6) 0.0305(3) Uani 1 1 d . . .
Ge3 Ge 0.26188(11) 0.00872(10) 0.77497(6) 0.0315(3) Uani 1 1 d . . .
Ge4 Ge 0.02564(11) 0.29360(10) 0.83414(6) 0.0322(3) Uani 1 1 d . . .
S1 S -0.2150(3) 0.1212(3) 0.64842(17) 0.0442(7) Uani 1 1 d . . .
S2 S 0.0943(3) 0.2386(2) 0.58872(15) 0.0331(6) Uani 1 1 d . . .
S3 S 0.0931(3) -0.0304(2) 0.72893(15) 0.0359(7) Uani 1 1 d . . .
S4 S -0.1458(3) 0.2591(3) 0.78971(16) 0.0371(7) Uani 1 1 d . . .
S5 S 0.3816(3) 0.3806(3) 0.53921(16) 0.0402(7) Uani 1 1 d . . .
S6 S 0.4025(3) 0.1068(2) 0.67800(15) 0.0336(6) Uani 1 1 d . . .
S7 S 0.1671(3) 0.3914(2) 0.73617(15) 0.0336(6) Uani 1 1 d . . .
S8 S 0.3869(3) -0.1556(3) 0.81919(17) 0.0434(7) Uani 1 1 d . . .
S9 S 0.1586(3) 0.1179(2) 0.87790(15) 0.0332(6) Uani 1 1 d . . .
S10 S -0.0662(3) 0.3984(3) 0.93164(16) 0.0448(7) Uani 1 1 d . . .
N1 N 1.3418(12) 0.4577(11) 0.3416(6) 0.060(3) Uani 1 1 d . . .
N2 N 0.7748(10) 0.1668(9) 0.4513(5) 0.047(2) Uani 1 1 d . . .
N3 N 0.9923(10) -0.2500(8) 0.8688(5) 0.043(2) Uani 1 1 d . . .
N4 N 0.4315(8) 0.2540(8) 0.9248(6) 0.040(2) Uani 1 1 d . . .
C1 C 1.2121(14) 0.5187(13) 0.3766(8) 0.066(4) Uani 1 1 d . . .
H1 H 1.1968 0.5977 0.3870 0.079 Uiso 1 1 calc R . .
C2 C 1.1041(12) 0.4597(11) 0.3961(7) 0.053(3) Uani 1 1 d . . .
H2 H 1.0136 0.5005 0.4196 0.063 Uiso 1 1 calc R . .
C3 C 1.1237(11) 0.3417(11) 0.3824(6) 0.046(3) Uani 1 1 d . . .
C4 C 1.2590(12) 0.2823(12) 0.3473(7) 0.057(3) Uani 1 1 d . . .
H4 H 1.2761 0.2030 0.3370 0.068 Uiso 1 1 calc R . .
C5 C 1.3699(13) 0.3427(13) 0.3273(7) 0.057(3) Uani 1 1 d . . .
H5 H 1.4618 0.3037 0.3046 0.068 Uiso 1 1 calc R . .
C6 C 0.7545(12) 0.2853(12) 0.4455(7) 0.058(4) Uani 1 1 d . . .
H6 H 0.6619 0.3306 0.4575 0.069 Uiso 1 1 calc R . .
C7 C 0.8613(11) 0.3441(10) 0.4231(7) 0.051(3) Uani 1 1 d . . .
H7 H 0.8406 0.4279 0.4189 0.062 Uiso 1 1 calc R . .
C8 C 1.0020(12) 0.2804(10) 0.4061(6) 0.046(3) Uani 1 1 d . . .
C9 C 1.0241(12) 0.1542(11) 0.4150(7) 0.049(3) Uani 1 1 d . . .
H9 H 1.1161 0.1072 0.4059 0.059 Uiso 1 1 calc R . .
C10 C 0.9126(13) 0.1001(12) 0.4368(7) 0.057(3) Uani 1 1 d . . .
H10 H 0.9295 0.0165 0.4420 0.068 Uiso 1 1 calc R . .
C11 C 1.4595(15) 0.5242(15) 0.3210(8) 0.089(5) Uani 1 1 d . . .
H11A H 1.5057 0.5081 0.3647 0.133 Uiso 1 1 calc R . .
H11B H 1.4208 0.6092 0.3115 0.133 Uiso 1 1 calc R . .
H11C H 1.5269 0.4976 0.2736 0.133 Uiso 1 1 calc R . .
C12 C 0.6564(13) 0.1035(11) 0.4755(7) 0.062(4) Uani 1 1 d . . .
H12A H 0.6670 0.0469 0.5223 0.092 Uiso 1 1 calc R . .
H12B H 0.6579 0.0613 0.4326 0.092 Uiso 1 1 calc R . .
H12C H 0.5679 0.1613 0.4872 0.092 Uiso 1 1 calc R . .
C13 C 0.9949(11) -0.1642(10) 0.9087(6) 0.043(3) Uani 1 1 d . . .
H13 H 1.0748 -0.1706 0.9280 0.051 Uiso 1 1 calc R . .
C14 C 0.8826(10) -0.0645(9) 0.9230(6) 0.036(3) Uani 1 1 d . . .
H14 H 0.8865 -0.0058 0.9519 0.043 Uiso 1 1 calc R . .
C15 C 0.7652(10) -0.0550(10) 0.8931(6) 0.034(3) Uani 1 1 d . . .
C16 C 0.7633(11) -0.1453(10) 0.8518(6) 0.040(3) Uani 1 1 d . . .
H16 H 0.6846 -0.1415 0.8321 0.048 Uiso 1 1 calc R . .
C17 C 0.8783(13) -0.2408(11) 0.8399(7) 0.055(3) Uani 1 1 d . . .
H17 H 0.8771 -0.3005 0.8111 0.065 Uiso 1 1 calc R . .
C18 C 0.5048(11) 0.2100(10) 0.9826(6) 0.039(3) Uani 1 1 d . . .
H18 H 0.4816 0.2481 1.0285 0.047 Uiso 1 1 calc R . .
C19 C 0.6129(10) 0.1095(9) 0.9737(6) 0.036(3) Uani 1 1 d . . .
H19 H 0.6630 0.0792 1.0136 0.043 Uiso 1 1 calc R . .
C20 C 0.6470(10) 0.0540(9) 0.9064(6) 0.033(2) Uani 1 1 d . . .
C21 C 0.5689(10) 0.1012(10) 0.8471(6) 0.036(3) Uani 1 1 d . . .
H21 H 0.5889 0.0638 0.8011 0.043 Uiso 1 1 calc R . .
C22 C 0.4638(11) 0.2021(11) 0.8583(7) 0.045(3) Uani 1 1 d . . .
H22 H 0.4136 0.2354 0.8187 0.054 Uiso 1 1 calc R . .
C23 C 1.1148(12) -0.3497(10) 0.8534(7) 0.053(3) Uani 1 1 d . . .
H23A H 1.1184 -0.3797 0.8048 0.079 Uiso 1 1 calc R . .
H23B H 1.1074 -0.4130 0.8973 0.079 Uiso 1 1 calc R . .
H23C H 1.1997 -0.3223 0.8478 0.079 Uiso 1 1 calc R . .
C24 C 0.3116(12) 0.3603(11) 0.9380(8) 0.067(4) Uani 1 1 d . . .
H24A H 0.3080 0.4110 0.8881 0.100 Uiso 1 1 calc R . .
H24B H 0.3245 0.4048 0.9757 0.100 Uiso 1 1 calc R . .
H24C H 0.2244 0.3338 0.9586 0.100 Uiso 1 1 calc R . .
C25 C 0.4247(16) 0.4772(14) 0.1179(11) 0.101(6) Uani 1 1 d . . .
H25A H 0.4312 0.5280 0.0675 0.152 Uiso 1 1 calc R . .
H25B H 0.5141 0.4215 0.1185 0.152 Uiso 1 1 calc R . .
H25C H 0.4009 0.5261 0.1606 0.152 Uiso 1 1 calc R . .
O1 O 0.3255(14) 0.4169(11) 0.1275(10) 0.132(5) Uani 1 1 d . . .
H1A H 0.2576 0.4613 0.1115 0.198 Uiso 1 1 calc R . .


_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 S1 2.122(3) . ?
Ge1 S4 2.229(3) . ?
Ge1 S2 2.241(3) . ?
Ge1 S3 2.247(3) . ?
Ge2 S5 2.119(3) . ?
Ge2 S2 2.240(3) . ?
Ge2 S6 2.242(3) . ?
Ge2 S7 2.257(3) . ?
Ge3 S8 2.126(3) . ?
Ge3 S3 2.232(3) . ?
Ge3 S6 2.238(3) . ?
Ge3 S9 2.246(3) . ?
Ge4 S10 2.132(3) . ?
Ge4 S4 2.216(3) . ?
Ge4 S9 2.248(3) . ?
Ge4 S7 2.249(3) . ?
N1 C5 1.341(16) . ?
N1 C1 1.349(15) . ?
N1 C11 1.505(16) . ?
N2 C6 1.321(15) . ?
N2 C10 1.378(14) . ?
N2 C12 1.485(14) . ?
N3 C13 1.322(14) . ?
N3 C17 1.342(14) . ?
N3 C23 1.453(13) . ?
N4 C22 1.328(13) . ?
N4 C18 1.352(12) . ?
N4 C24 1.482(13) . ?
C1 C2 1.366(16) . ?
C1 H1 0.9300 . ?
C2 C3 1.383(16) . ?
C2 H2 0.9300 . ?
C3 C4 1.384(15) . ?
C3 C8 1.499(16) . ?
C4 C5 1.401(16) . ?
C4 H4 0.9300 . ?
C5 H5 0.9300 . ?
C6 C7 1.352(15) . ?
C6 H6 0.9300 . ?
C7 C8 1.392(14) . ?
C7 H7 0.9300 . ?
C8 C9 1.404(15) . ?
C9 C10 1.358(16) . ?
C9 H9 0.9300 . ?
C10 H10 0.9300 . ?
C11 H11A 0.9600 . ?
C11 H11B 0.9600 . ?
C11 H11C 0.9600 . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 0.9600 . ?
C13 C14 1.392(14) . ?
C13 H13 0.9300 . ?
C14 C15 1.384(13) . ?
C14 H14 0.9300 . ?
C15 C16 1.380(14) . ?
C15 C20 1.494(14) . ?
C16 C17 1.373(15) . ?
C16 H16 0.9300 . ?
C17 H17 0.9300 . ?
C18 C19 1.367(14) . ?
C18 H18 0.9300 . ?
C19 C20 1.361(13) . ?
C19 H19 0.9300 . ?
C20 C21 1.409(13) . ?
C21 C22 1.358(14) . ?
C21 H21 0.9300 . ?
C22 H22 0.9300 . ?
C23 H23A 0.9600 . ?
C23 H23B 0.9600 . ?
C23 H23C 0.9600 . ?
C24 H24A 0.9600 . ?
C24 H24B 0.9600 . ?
C24 H24C 0.9600 . ?
C25 O1 1.318(16) . ?
C25 H25A 0.9600 . ?
C25 H25B 0.9600 . ?
C25 H25C 0.9600 . ?
O1 H1A 0.8200 . ?

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
S1 Ge1 S4 105.64(11) . . ?
S1 Ge1 S2 108.53(11) . . ?
S4 Ge1 S2 111.52(11) . . ?
S1 Ge1 S3 112.46(12) . . ?
S4 Ge1 S3 112.41(10) . . ?
S2 Ge1 S3 106.29(10) . . ?
S5 Ge2 S2 107.76(11) . . ?
S5 Ge2 S6 111.93(11) . . ?
S2 Ge2 S6 110.51(11) . . ?
S5 Ge2 S7 107.89(12) . . ?
S2 Ge2 S7 110.20(10) . . ?
S6 Ge2 S7 108.52(10) . . ?
S8 Ge3 S3 109.62(12) . . ?
S8 Ge3 S6 108.98(11) . . ?
S3 Ge3 S6 110.96(10) . . ?
S8 Ge3 S9 107.66(11) . . ?
S3 Ge3 S9 108.77(11) . . ?
S6 Ge3 S9 110.78(11) . . ?
S10 Ge4 S4 109.13(12) . . ?
S10 Ge4 S9 108.65(11) . . ?
S4 Ge4 S9 109.88(11) . . ?
S10 Ge4 S7 109.85(12) . . ?
S4 Ge4 S7 110.91(10) . . ?
S9 Ge4 S7 108.39(10) . . ?
Ge2 S2 Ge1 109.08(11) . . ?
Ge3 S3 Ge1 108.57(12) . . ?
Ge4 S4 Ge1 107.88(11) . . ?
Ge3 S6 Ge2 107.16(11) . . ?
Ge4 S7 Ge2 109.30(12) . . ?
Ge3 S9 Ge4 109.13(11) . . ?
C5 N1 C1 123.6(12) . . ?
C5 N1 C11 119.9(12) . . ?
C1 N1 C11 116.4(13) . . ?
C6 N2 C10 117.8(11) . . ?
C6 N2 C12 122.8(10) . . ?
C10 N2 C12 119.3(10) . . ?
C13 N3 C17 119.2(10) . . ?
C13 N3 C23 119.9(10) . . ?
C17 N3 C23 120.8(11) . . ?
C22 N4 C18 121.0(9) . . ?
C22 N4 C24 120.4(9) . . ?
C18 N4 C24 118.6(10) . . ?
N1 C1 C2 117.3(14) . . ?
N1 C1 H1 121.4 . . ?
C2 C1 H1 121.4 . . ?
C1 C2 C3 122.8(12) . . ?
C1 C2 H2 118.6 . . ?
C3 C2 H2 118.6 . . ?
C2 C3 C4 117.9(12) . . ?
C2 C3 C8 120.7(10) . . ?
C4 C3 C8 121.5(12) . . ?
C3 C4 C5 119.4(13) . . ?
C3 C4 H4 120.3 . . ?
C5 C4 H4 120.3 . . ?
N1 C5 C4 119.0(11) . . ?
N1 C5 H5 120.5 . . ?
C4 C5 H5 120.5 . . ?
N2 C6 C7 123.4(11) . . ?
N2 C6 H6 118.3 . . ?
C7 C6 H6 118.3 . . ?
C6 C7 C8 120.6(11) . . ?
C6 C7 H7 119.7 . . ?
C8 C7 H7 119.7 . . ?
C7 C8 C9 116.2(11) . . ?
C7 C8 C3 122.4(10) . . ?
C9 C8 C3 121.4(10) . . ?
C10 C9 C8 120.6(11) . . ?
C10 C9 H9 119.7 . . ?
C8 C9 H9 119.7 . . ?
C9 C10 N2 121.3(12) . . ?
C9 C10 H10 119.3 . . ?
N2 C10 H10 119.3 . . ?
N1 C11 H11A 109.5 . . ?
N1 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
N1 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
N2 C12 H12A 109.5 . . ?
N2 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
N2 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
N3 C13 C14 122.5(11) . . ?
N3 C13 H13 118.8 . . ?
C14 C13 H13 118.8 . . ?
C15 C14 C13 118.3(11) . . ?
C15 C14 H14 120.9 . . ?
C13 C14 H14 120.9 . . ?
C16 C15 C14 118.8(10) . . ?
C16 C15 C20 123.2(10) . . ?
C14 C15 C20 118.0(10) . . ?
C17 C16 C15 119.6(10) . . ?
C17 C16 H16 120.2 . . ?
C15 C16 H16 120.2 . . ?
N3 C17 C16 121.7(12) . . ?
N3 C17 H17 119.2 . . ?
C16 C17 H17 119.2 . . ?
N4 C18 C19 120.2(10) . . ?
N4 C18 H18 119.9 . . ?
C19 C18 H18 119.9 . . ?
C20 C19 C18 119.9(9) . . ?
C20 C19 H19 120.1 . . ?
C18 C19 H19 120.1 . . ?
C19 C20 C21 119.0(9) . . ?
C19 C20 C15 122.2(9) . . ?
C21 C20 C15 118.8(9) . . ?
C22 C21 C20 118.8(10) . . ?
C22 C21 H21 120.6 . . ?
C20 C21 H21 120.6 . . ?
N4 C22 C21 121.0(10) . . ?
N4 C22 H22 119.5 . . ?
C21 C22 H22 119.5 . . ?
N3 C23 H23A 109.5 . . ?
N3 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
N3 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
N4 C24 H24A 109.5 . . ?
N4 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
N4 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
O1 C25 H25A 109.5 . . ?
O1 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
O1 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C25 O1 H1A 109.5 . . ?

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
S5 Ge2 S2 Ge1 -174.77(12) . . . . ?
S6 Ge2 S2 Ge1 62.65(14) . . . . ?
S7 Ge2 S2 Ge1 -57.29(14) . . . . ?
S1 Ge1 S2 Ge2 175.53(12) . . . . ?
S4 Ge1 S2 Ge2 59.56(14) . . . . ?
S3 Ge1 S2 Ge2 -63.28(14) . . . . ?
S8 Ge3 S3 Ge1 176.42(12) . . . . ?
S6 Ge3 S3 Ge1 -63.16(14) . . . . ?
S9 Ge3 S3 Ge1 58.94(13) . . . . ?
S1 Ge1 S3 Ge3 -178.08(12) . . . . ?
S4 Ge1 S3 Ge3 -58.99(14) . . . . ?
S2 Ge1 S3 Ge3 63.29(14) . . . . ?
S10 Ge4 S4 Ge1 -178.59(12) . . . . ?
S9 Ge4 S4 Ge1 -59.56(14) . . . . ?
S7 Ge4 S4 Ge1 60.26(14) . . . . ?
S1 Ge1 S4 Ge4 -178.23(12) . . . . ?
S2 Ge1 S4 Ge4 -60.50(14) . . . . ?
S3 Ge1 S4 Ge4 58.77(14) . . . . ?
S8 Ge3 S6 Ge2 179.88(12) . . . . ?
S3 Ge3 S6 Ge2 59.08(15) . . . . ?
S9 Ge3 S6 Ge2 -61.85(14) . . . . ?
S5 Ge2 S6 Ge3 -178.56(12) . . . . ?
S2 Ge2 S6 Ge3 -58.45(14) . . . . ?
S7 Ge2 S6 Ge3 62.49(14) . . . . ?
S10 Ge4 S7 Ge2 179.60(12) . . . . ?
S4 Ge4 S7 Ge2 -59.68(14) . . . . ?
S9 Ge4 S7 Ge2 61.03(14) . . . . ?
S5 Ge2 S7 Ge4 174.96(11) . . . . ?
S2 Ge2 S7 Ge4 57.56(13) . . . . ?
S6 Ge2 S7 Ge4 -63.57(13) . . . . ?
S8 Ge3 S9 Ge4 179.69(12) . . . . ?
S3 Ge3 S9 Ge4 -61.60(14) . . . . ?
S6 Ge3 S9 Ge4 60.61(14) . . . . ?
S10 Ge4 S9 Ge3 -178.19(12) . . . . ?
S4 Ge4 S9 Ge3 62.49(14) . . . . ?
S7 Ge4 S9 Ge3 -58.86(14) . . . . ?
C5 N1 C1 C2 -1.9(18) . . . . ?
C11 N1 C1 C2 -179.7(10) . . . . ?
N1 C1 C2 C3 0.9(18) . . . . ?
C1 C2 C3 C4 -0.1(17) . . . . ?
C1 C2 C3 C8 179.0(10) . . . . ?
C2 C3 C4 C5 0.2(17) . . . . ?
C8 C3 C4 C5 -178.9(10) . . . . ?
C1 N1 C5 C4 2.0(19) . . . . ?
C11 N1 C5 C4 179.8(10) . . . . ?
C3 C4 C5 N1 -1.1(17) . . . . ?
C10 N2 C6 C7 2.8(18) . . . . ?
C12 N2 C6 C7 -179.6(11) . . . . ?
N2 C6 C7 C8 -1(2) . . . . ?
C6 C7 C8 C9 -0.9(17) . . . . ?
C6 C7 C8 C3 -179.0(11) . . . . ?
C2 C3 C8 C7 16.8(16) . . . . ?
C4 C3 C8 C7 -164.0(11) . . . . ?
C2 C3 C8 C9 -161.1(11) . . . . ?
C4 C3 C8 C9 18.1(16) . . . . ?
C7 C8 C9 C10 1.7(17) . . . . ?
C3 C8 C9 C10 179.8(10) . . . . ?
C8 C9 C10 N2 -0.4(18) . . . . ?
C6 N2 C10 C9 -1.9(17) . . . . ?
C12 N2 C10 C9 -179.6(10) . . . . ?
C17 N3 C13 C14 0.8(15) . . . . ?
C23 N3 C13 C14 177.8(9) . . . . ?
N3 C13 C14 C15 -0.9(14) . . . . ?
C13 C14 C15 C16 1.1(13) . . . . ?
C13 C14 C15 C20 -178.2(8) . . . . ?
C14 C15 C16 C17 -1.3(15) . . . . ?
C20 C15 C16 C17 177.9(9) . . . . ?
C13 N3 C17 C16 -1.0(15) . . . . ?
C23 N3 C17 C16 -178.0(10) . . . . ?
C15 C16 C17 N3 1.3(16) . . . . ?
C22 N4 C18 C19 -0.9(15) . . . . ?
C24 N4 C18 C19 177.7(10) . . . . ?
N4 C18 C19 C20 0.2(15) . . . . ?
C18 C19 C20 C21 -0.4(15) . . . . ?
C18 C19 C20 C15 179.2(9) . . . . ?
C16 C15 C20 C19 147.4(10) . . . . ?
C14 C15 C20 C19 -33.3(13) . . . . ?
C16 C15 C20 C21 -33.0(14) . . . . ?
C14 C15 C20 C21 146.3(9) . . . . ?
C19 C20 C21 C22 1.3(15) . . . . ?
C15 C20 C21 C22 -178.3(9) . . . . ?
C18 N4 C22 C21 1.8(16) . . . . ?
C24 N4 C22 C21 -176.7(10) . . . . ?
C20 C21 C22 N4 -2.1(15) . . . . ?

_diffrn_measured_fraction_theta_max 0.992
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.992
_refine_diff_density_max         0.841
_refine_diff_density_min         -0.669
_refine_diff_density_rms         0.142

#######################end
_database_code_depnum_ccdc_archive 'CCDC 1000267'
