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

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_3
_database_code_depnum_ccdc_archive 'CCDC 1017826'
_audit_update_record             
;
2014-10-08 deposited with the CCDC.
2015-02-02 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C30 H46 Ge2 N4 Se3'
_chemical_formula_sum            'C30 H46 Ge2 N4 Se3'

_chemical_formula_weight         844.81

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'
Ge Ge 0.1547 1.8001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Se Se -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/c'
_symmetry_space_group_name_hall  '-P 2ybc'

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

_cell_length_a                   16.736(3)
_cell_length_b                   11.336(2)
_cell_length_c                   18.978(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 106.354(3)
_cell_angle_gamma                90.00
_cell_volume                     3454.8(10)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    6084
_cell_measurement_theta_min      1.27
_cell_measurement_theta_max      25.000

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.461
_exptl_crystal_size_mid          0.387
_exptl_crystal_size_min          0.266
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.565
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1626.6
_exptl_absorpt_coefficient_mu    4.511
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.136
_exptl_absorpt_correction_T_max  0.301
_exptl_absorpt_process_details   '(SADABS; Bruker, 2000)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      100(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            17739
_diffrn_reflns_av_R_equivalents  0.0461
_diffrn_reflns_av_sigmaI/netI    0.0495
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         1.27
_diffrn_reflns_theta_max         25.00
_reflns_number_total             6084
_reflns_number_gt                4972
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_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)+(0.0766P)²+2.5113P] 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         6068
_refine_ls_number_parameters     361
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0545
_refine_ls_R_factor_gt           0.0419
_refine_ls_wR_factor_ref         0.1329
_refine_ls_wR_factor_gt          0.1169
_refine_ls_goodness_of_fit_ref   1.088
_refine_ls_restrained_S_all      1.088
_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
Ge2 Ge 0.18502(3) 0.32023(4) 0.27971(3) 0.01864(15) Uani 1 1 d . . .
Ge1 Ge 0.35340(3) 0.21125(4) 0.43005(3) 0.01864(15) Uani 1 1 d . . .
Se1 Se 0.27427(4) 0.08330(5) 0.46641(3) 0.03325(18) Uani 1 1 d . . .
Se2 Se 0.13576(4) 0.42340(5) 0.35582(3) 0.03575(18) Uani 1 1 d . . .
Se3 Se 0.32450(6) 0.27888(8) 0.31183(5) 0.0265(3) Uani 0.607(2) 1 d P . .
N2 N 0.4010(3) 0.3365(4) 0.4948(2) 0.0202(9) Uani 1 1 d . . .
N3 N 0.1206(3) 0.1896(3) 0.2348(2) 0.0202(9) Uani 1 1 d . . .
C7 C 0.4827(3) 0.3248(4) 0.5269(3) 0.0224(11) Uani 1 1 d . . .
N4 N 0.1736(2) 0.3701(3) 0.1820(2) 0.0191(9) Uani 1 1 d . . .
N1 N 0.4655(3) 0.1639(3) 0.4455(2) 0.0192(9) Uani 1 1 d . . .
C17 C 0.0206(3) 0.1329(4) 0.1218(3) 0.0265(12) Uani 1 1 d . . .
H17 H -0.0026 0.0853 0.1508 0.032 Uiso 1 1 calc R . .
C22 C 0.1244(3) 0.2988(4) 0.1301(3) 0.0200(11) Uani 1 1 d . . .
C16 C 0.0876(3) 0.2021(4) 0.1613(3) 0.0209(11) Uani 1 1 d . . .
C1 C 0.5213(3) 0.2273(4) 0.4968(3) 0.0220(11) Uani 1 1 d . . .
C6 C 0.5244(3) 0.3989(5) 0.5844(3) 0.0275(12) Uani 1 1 d . . .
H6 H 0.4904 0.4550 0.5973 0.033 Uiso 1 1 calc R . .
C2 C 0.6055(3) 0.2026(5) 0.5158(3) 0.0284(12) Uani 1 1 d . . .
H2 H 0.6199 0.1445 0.4870 0.034 Uiso 1 1 calc R . .
C20 C 0.0680(4) 0.2564(5) -0.0063(3) 0.0318(13) Uani 1 1 d . . .
H20 H 0.0778 0.2768 -0.0506 0.038 Uiso 1 1 calc R . .
C21 C 0.1170(3) 0.3128(5) 0.0546(3) 0.0255(12) Uani 1 1 d . . .
H21 H 0.1516 0.3705 0.0443 0.031 Uiso 1 1 calc R . .
C19 C 0.0067(4) 0.1744(5) -0.0109(3) 0.0346(14) Uani 1 1 d . . .
H19 H -0.0222 0.1503 -0.0581 0.042 Uiso 1 1 calc R . .
C18 C -0.0176(3) 0.1228(5) 0.0460(3) 0.0322(13) Uani 1 1 d . . .
H18 H -0.0651 0.0759 0.0324 0.039 Uiso 1 1 calc R . .
C4 C 0.6751(4) 0.3391(5) 0.6197(3) 0.0362(14) Uani 1 1 d . . .
H4 H 0.7266 0.3582 0.6518 0.043 Uiso 1 1 calc R . .
C5 C 0.6085(4) 0.4043(5) 0.6264(3) 0.0355(14) Uani 1 1 d . . .
H5 H 0.6206 0.4598 0.6640 0.043 Uiso 1 1 calc R . .
C3 C 0.6747(4) 0.2492(5) 0.5711(3) 0.0372(14) Uani 1 1 d . . .
H3 H 0.7259 0.2142 0.5748 0.045 Uiso 1 1 calc R . .
C9 C 0.3484(3) 0.4312(4) 0.5088(3) 0.0245(12) Uani 1 1 d . . .
H9A H 0.3132 0.4591 0.4621 0.029 Uiso 1 1 calc R . .
H9B H 0.3840 0.4962 0.5318 0.029 Uiso 1 1 calc R . .
C8 C 0.4847(3) 0.0530(4) 0.4135(3) 0.0242(11) Uani 1 1 d . . .
H8A H 0.4433 -0.0055 0.4159 0.029 Uiso 1 1 calc R . .
H8B H 0.5384 0.0245 0.4429 0.029 Uiso 1 1 calc R . .
C23 C 0.0955(3) 0.0967(4) 0.2767(3) 0.0269(12) Uani 1 1 d . . .
H23A H 0.0355 0.0999 0.2673 0.032 Uiso 1 1 calc R . .
H23B H 0.1200 0.1127 0.3286 0.032 Uiso 1 1 calc R . .
C24 C 0.2162(3) 0.4720(4) 0.1624(3) 0.0228(11) Uani 1 1 d . . .
H24A H 0.2463 0.4468 0.1282 0.027 Uiso 1 1 calc R . .
H24B H 0.2569 0.5005 0.2063 0.027 Uiso 1 1 calc R . .
C11 C 0.2927(3) 0.3982(5) 0.5574(3) 0.0274(12) Uani 1 1 d . . .
H11 H 0.2542 0.3364 0.5324 0.033 Uiso 1 1 calc R . .
C25 C 0.1197(4) -0.0283(5) 0.2607(3) 0.0320(13) Uani 1 1 d . . .
H25 H 0.0885 -0.0488 0.2103 0.038 Uiso 1 1 calc R . .
C26 C 0.1581(4) 0.5747(4) 0.1277(3) 0.0291(12) Uani 1 1 d . . .
H26 H 0.1127 0.5442 0.0872 0.035 Uiso 1 1 calc R . .
C10 C 0.4870(4) 0.0643(5) 0.3331(3) 0.0384(15) Uani 1 1 d . . .
H10 H 0.4320 0.0899 0.3032 0.046 Uiso 1 1 calc R . .
C28 C 0.2123(4) -0.0396(5) 0.2676(3) 0.0386(15) Uani 1 1 d . . .
H28A H 0.2440 -0.0161 0.3160 0.058 Uiso 1 1 calc R . .
H28B H 0.2263 0.0103 0.2319 0.058 Uiso 1 1 calc R . .
H28C H 0.2251 -0.1200 0.2592 0.058 Uiso 1 1 calc R . .
C27 C 0.0933(4) -0.1124(5) 0.3132(4) 0.0441(16) Uani 1 1 d . . .
H27A H 0.1254 -0.0962 0.3627 0.066 Uiso 1 1 calc R . .
H27B H 0.1025 -0.1924 0.3009 0.066 Uiso 1 1 calc R . .
H27C H 0.0352 -0.1011 0.3088 0.066 Uiso 1 1 calc R . .
C15 C 0.2422(4) 0.5053(6) 0.5647(4) 0.0445(16) Uani 1 1 d . . .
H15A H 0.2077 0.4870 0.5960 0.067 Uiso 1 1 calc R . .
H15B H 0.2077 0.5280 0.5171 0.067 Uiso 1 1 calc R . .
H15C H 0.2790 0.5690 0.5857 0.067 Uiso 1 1 calc R . .
C14 C 0.3412(4) 0.3518(6) 0.6315(3) 0.0476(18) Uani 1 1 d . . .
H14A H 0.3718 0.4152 0.6605 0.071 Uiso 1 1 calc R . .
H14B H 0.3792 0.2920 0.6253 0.071 Uiso 1 1 calc R . .
H14C H 0.3034 0.3188 0.6560 0.071 Uiso 1 1 calc R . .
C29 C 0.1215(5) 0.6309(6) 0.1841(4) 0.0531(19) Uani 1 1 d . . .
H29A H 0.1082 0.5707 0.2145 0.080 Uiso 1 1 calc R . .
H29B H 0.0719 0.6734 0.1595 0.080 Uiso 1 1 calc R . .
H29C H 0.1613 0.6844 0.2141 0.080 Uiso 1 1 calc R . .
C30 C 0.2079(5) 0.6656(6) 0.0975(5) 0.063(2) Uani 1 1 d . . .
H30A H 0.1702 0.7171 0.0638 0.095 Uiso 1 1 calc R . .
H30B H 0.2424 0.6254 0.0725 0.095 Uiso 1 1 calc R . .
H30C H 0.2422 0.7110 0.1373 0.095 Uiso 1 1 calc R . .
C12 C 0.5044(6) -0.0579(7) 0.3072(4) 0.078(3) Uani 1 1 d . . .
H12A H 0.5042 -0.0541 0.2566 0.117 Uiso 1 1 calc R . .
H12B H 0.4621 -0.1118 0.3122 0.117 Uiso 1 1 calc R . .
H12C H 0.5578 -0.0848 0.3364 0.117 Uiso 1 1 calc R . .
C13 C 0.5505(5) 0.1536(7) 0.3250(4) 0.066(2) Uani 1 1 d . . .
H13A H 0.5493 0.2205 0.3558 0.099 Uiso 1 1 calc R . .
H13B H 0.5377 0.1787 0.2748 0.099 Uiso 1 1 calc R . .
H13C H 0.6049 0.1187 0.3395 0.099 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
Ge2 N3 1.888(4) . ?
Ge2 N4 1.897(4) . ?
Ge2 Se2 2.1917(8) . ?
Ge2 Se3 2.2890(11) . ?
Ge1 N1 1.893(4) . ?
Ge1 N2 1.900(4) . ?
Ge1 Se1 2.2019(8) . ?
Ge1 Se3 2.2899(10) . ?
N2 C7 1.337(7) . ?
N2 C9 1.459(6) . ?
N3 C16 1.356(6) . ?
N3 C23 1.451(6) . ?
C7 C6 1.398(7) . ?
C7 C1 1.474(7) . ?
N4 C22 1.358(6) . ?
N4 C24 1.460(6) . ?
N1 C1 1.352(7) . ?
N1 C8 1.471(6) . ?
C17 C16 1.400(7) . ?
C17 C18 1.404(8) . ?
C17 H17 0.9300 . ?
C22 C21 1.412(7) . ?
C22 C16 1.462(7) . ?
C1 C2 1.381(7) . ?
C6 C5 1.411(8) . ?
C6 H6 0.9300 . ?
C2 C3 1.427(8) . ?
C2 H2 0.9300 . ?
C20 C19 1.369(8) . ?
C20 C21 1.372(8) . ?
C20 H20 0.9300 . ?
C21 H21 0.9300 . ?
C19 C18 1.387(8) . ?
C19 H19 0.9300 . ?
C18 H18 0.9300 . ?
C4 C5 1.373(8) . ?
C4 C3 1.373(8) . ?
C4 H4 0.9300 . ?
C5 H5 0.9300 . ?
C3 H3 0.9300 . ?
C9 C11 1.531(7) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C8 C10 1.542(7) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C23 C25 1.528(7) . ?
C23 H23A 0.9700 . ?
C23 H23B 0.9700 . ?
C24 C26 1.541(7) . ?
C24 H24A 0.9700 . ?
C24 H24B 0.9700 . ?
C11 C14 1.506(8) . ?
C11 C15 1.508(8) . ?
C11 H11 0.9800 . ?
C25 C28 1.524(8) . ?
C25 C27 1.532(7) . ?
C25 H25 0.9800 . ?
C26 C29 1.515(8) . ?
C26 C30 1.534(8) . ?
C26 H26 0.9800 . ?
C10 C13 1.507(10) . ?
C10 C12 1.525(8) . ?
C10 H10 0.9800 . ?
C28 H28A 0.9600 . ?
C28 H28B 0.9600 . ?
C28 H28C 0.9600 . ?
C27 H27A 0.9600 . ?
C27 H27B 0.9600 . ?
C27 H27C 0.9600 . ?
C15 H15A 0.9600 . ?
C15 H15B 0.9600 . ?
C15 H15C 0.9600 . ?
C14 H14A 0.9600 . ?
C14 H14B 0.9600 . ?
C14 H14C 0.9600 . ?
C29 H29A 0.9600 . ?
C29 H29B 0.9600 . ?
C29 H29C 0.9600 . ?
C30 H30A 0.9600 . ?
C30 H30B 0.9600 . ?
C30 H30C 0.9600 . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 0.9600 . ?
C13 H13A 0.9600 . ?
C13 H13B 0.9600 . ?
C13 H13C 0.9600 . ?

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
N3 Ge2 N4 84.53(17) . . ?
N3 Ge2 Se2 116.32(12) . . ?
N4 Ge2 Se2 122.15(12) . . ?
N3 Ge2 Se3 111.68(13) . . ?
N4 Ge2 Se3 97.82(12) . . ?
Se2 Ge2 Se3 118.58(4) . . ?
N1 Ge1 N2 83.98(17) . . ?
N1 Ge1 Se1 114.96(12) . . ?
N2 Ge1 Se1 117.98(12) . . ?
N1 Ge1 Se3 99.97(12) . . ?
N2 Ge1 Se3 108.55(12) . . ?
Se1 Ge1 Se3 123.21(4) . . ?
Ge2 Se3 Ge1 104.34(4) . . ?
C7 N2 C9 125.6(4) . . ?
C7 N2 Ge1 114.1(3) . . ?
C9 N2 Ge1 120.2(3) . . ?
C16 N3 C23 122.9(4) . . ?
C16 N3 Ge2 113.5(3) . . ?
C23 N3 Ge2 122.5(3) . . ?
N2 C7 C6 121.1(5) . . ?
N2 C7 C1 113.7(4) . . ?
C6 C7 C1 125.2(5) . . ?
C22 N4 C24 121.8(4) . . ?
C22 N4 Ge2 113.9(3) . . ?
C24 N4 Ge2 124.2(3) . . ?
C1 N1 C8 124.4(4) . . ?
C1 N1 Ge1 114.5(3) . . ?
C8 N1 Ge1 120.1(3) . . ?
C16 C17 C18 131.2(5) . . ?
C16 C17 H17 114.4 . . ?
C18 C17 H17 114.4 . . ?
N4 C22 C21 122.1(4) . . ?
N4 C22 C16 113.0(4) . . ?
C21 C22 C16 124.7(5) . . ?
N3 C16 C17 121.7(5) . . ?
N3 C16 C22 113.5(4) . . ?
C17 C16 C22 124.6(5) . . ?
N1 C1 C2 121.8(5) . . ?
N1 C1 C7 112.9(5) . . ?
C2 C1 C7 125.3(5) . . ?
C7 C6 C5 131.8(5) . . ?
C7 C6 H6 114.1 . . ?
C5 C6 H6 114.1 . . ?
C1 C2 C3 132.4(5) . . ?
C1 C2 H2 113.8 . . ?
C3 C2 H2 113.8 . . ?
C19 C20 C21 129.1(5) . . ?
C19 C20 H20 115.5 . . ?
C21 C20 H20 115.5 . . ?
C20 C21 C22 131.5(5) . . ?
C20 C21 H21 114.2 . . ?
C22 C21 H21 114.2 . . ?
C20 C19 C18 128.0(5) . . ?
C20 C19 H19 116.0 . . ?
C18 C19 H19 116.0 . . ?
C19 C18 C17 127.9(5) . . ?
C19 C18 H18 116.0 . . ?
C17 C18 H18 116.0 . . ?
C5 C4 C3 127.7(5) . . ?
C5 C4 H4 116.2 . . ?
C3 C4 H4 116.2 . . ?
C4 C5 C6 129.1(5) . . ?
C4 C5 H5 115.4 . . ?
C6 C5 H5 115.4 . . ?
C4 C3 C2 128.2(6) . . ?
C4 C3 H3 115.9 . . ?
C2 C3 H3 115.9 . . ?
N2 C9 C11 115.5(4) . . ?
N2 C9 H9A 108.4 . . ?
C11 C9 H9A 108.4 . . ?
N2 C9 H9B 108.4 . . ?
C11 C9 H9B 108.4 . . ?
H9A C9 H9B 107.5 . . ?
N1 C8 C10 114.0(4) . . ?
N1 C8 H8A 108.7 . . ?
C10 C8 H8A 108.7 . . ?
N1 C8 H8B 108.7 . . ?
C10 C8 H8B 108.7 . . ?
H8A C8 H8B 107.6 . . ?
N3 C23 C25 115.4(4) . . ?
N3 C23 H23A 108.4 . . ?
C25 C23 H23A 108.4 . . ?
N3 C23 H23B 108.4 . . ?
C25 C23 H23B 108.4 . . ?
H23A C23 H23B 107.5 . . ?
N4 C24 C26 114.3(4) . . ?
N4 C24 H24A 108.7 . . ?
C26 C24 H24A 108.7 . . ?
N4 C24 H24B 108.7 . . ?
C26 C24 H24B 108.7 . . ?
H24A C24 H24B 107.6 . . ?
C14 C11 C15 111.3(5) . . ?
C14 C11 C9 112.9(5) . . ?
C15 C11 C9 108.1(5) . . ?
C14 C11 H11 108.1 . . ?
C15 C11 H11 108.1 . . ?
C9 C11 H11 108.1 . . ?
C28 C25 C23 112.4(4) . . ?
C28 C25 C27 111.4(5) . . ?
C23 C25 C27 107.8(5) . . ?
C28 C25 H25 108.4 . . ?
C23 C25 H25 108.4 . . ?
C27 C25 H25 108.4 . . ?
C29 C26 C30 110.6(5) . . ?
C29 C26 C24 110.4(5) . . ?
C30 C26 C24 108.8(5) . . ?
C29 C26 H26 109.0 . . ?
C30 C26 H26 109.0 . . ?
C24 C26 H26 109.0 . . ?
C13 C10 C12 112.0(6) . . ?
C13 C10 C8 111.7(5) . . ?
C12 C10 C8 107.7(5) . . ?
C13 C10 H10 108.5 . . ?
C12 C10 H10 108.5 . . ?
C8 C10 H10 108.5 . . ?
C25 C28 H28A 109.5 . . ?
C25 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C25 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C25 C27 H27A 109.5 . . ?
C25 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
C25 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C11 C15 H15A 109.5 . . ?
C11 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C11 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C11 C14 H14A 109.5 . . ?
C11 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C11 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C26 C29 H29A 109.5 . . ?
C26 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
C26 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C26 C30 H30A 109.5 . . ?
C26 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
C26 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C10 C12 H12A 109.5 . . ?
C10 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C10 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C10 C13 H13A 109.5 . . ?
C10 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C10 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 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
N3 Ge2 Se3 Ge1 -91.57(13) . . . . ?
N4 Ge2 Se3 Ge1 -178.76(12) . . . . ?
Se2 Ge2 Se3 Ge1 47.88(5) . . . . ?
N1 Ge1 Se3 Ge2 173.59(12) . . . . ?
N2 Ge1 Se3 Ge2 -99.46(13) . . . . ?
Se1 Ge1 Se3 Ge2 44.75(5) . . . . ?
N1 Ge1 N2 C7 -8.6(3) . . . . ?
Se1 Ge1 N2 C7 106.5(3) . . . . ?
Se3 Ge1 N2 C7 -107.2(3) . . . . ?
N1 Ge1 N2 C9 174.4(4) . . . . ?
Se1 Ge1 N2 C9 -70.5(4) . . . . ?
Se3 Ge1 N2 C9 75.9(3) . . . . ?
N4 Ge2 N3 C16 -10.0(3) . . . . ?
Se2 Ge2 N3 C16 113.3(3) . . . . ?
Se3 Ge2 N3 C16 -106.2(3) . . . . ?
N4 Ge2 N3 C23 -178.3(4) . . . . ?
Se2 Ge2 N3 C23 -55.0(4) . . . . ?
Se3 Ge2 N3 C23 85.4(4) . . . . ?
C9 N2 C7 C6 6.9(7) . . . . ?
Ge1 N2 C7 C6 -169.8(4) . . . . ?
C9 N2 C7 C1 -174.3(4) . . . . ?
Ge1 N2 C7 C1 9.0(5) . . . . ?
N3 Ge2 N4 C22 3.6(3) . . . . ?
Se2 Ge2 N4 C22 -114.1(3) . . . . ?
Se3 Ge2 N4 C22 114.8(3) . . . . ?
N3 Ge2 N4 C24 -173.4(4) . . . . ?
Se2 Ge2 N4 C24 68.9(4) . . . . ?
Se3 Ge2 N4 C24 -62.2(4) . . . . ?
N2 Ge1 N1 C1 6.5(3) . . . . ?
Se1 Ge1 N1 C1 -111.7(3) . . . . ?
Se3 Ge1 N1 C1 114.3(3) . . . . ?
N2 Ge1 N1 C8 175.4(4) . . . . ?
Se1 Ge1 N1 C8 57.3(4) . . . . ?
Se3 Ge1 N1 C8 -76.8(3) . . . . ?
C24 N4 C22 C21 5.4(7) . . . . ?
Ge2 N4 C22 C21 -171.7(4) . . . . ?
C24 N4 C22 C16 -180.0(4) . . . . ?
Ge2 N4 C22 C16 2.9(5) . . . . ?
C23 N3 C16 C17 6.5(7) . . . . ?
Ge2 N3 C16 C17 -161.8(4) . . . . ?
C23 N3 C16 C22 -177.7(4) . . . . ?
Ge2 N3 C16 C22 14.0(5) . . . . ?
C18 C17 C16 N3 -173.1(5) . . . . ?
C18 C17 C16 C22 11.7(9) . . . . ?
N4 C22 C16 N3 -11.1(6) . . . . ?
C21 C22 C16 N3 163.4(5) . . . . ?
N4 C22 C16 C17 164.5(5) . . . . ?
C21 C22 C16 C17 -21.0(8) . . . . ?
C8 N1 C1 C2 10.3(7) . . . . ?
Ge1 N1 C1 C2 178.6(4) . . . . ?
C8 N1 C1 C7 -171.6(4) . . . . ?
Ge1 N1 C1 C7 -3.3(5) . . . . ?
N2 C7 C1 N1 -3.8(6) . . . . ?
C6 C7 C1 N1 175.0(5) . . . . ?
N2 C7 C1 C2 174.3(5) . . . . ?
C6 C7 C1 C2 -7.0(8) . . . . ?
N2 C7 C6 C5 179.9(5) . . . . ?
C1 C7 C6 C5 1.3(9) . . . . ?
N1 C1 C2 C3 -174.2(5) . . . . ?
C7 C1 C2 C3 7.9(9) . . . . ?
C19 C20 C21 C22 5.3(11) . . . . ?
N4 C22 C21 C20 -175.5(5) . . . . ?
C16 C22 C21 C20 10.5(9) . . . . ?
C21 C20 C19 C18 -4.2(11) . . . . ?
C20 C19 C18 C17 -7.6(11) . . . . ?
C16 C17 C18 C19 5.7(10) . . . . ?
C3 C4 C5 C6 -2.5(10) . . . . ?
C7 C6 C5 C4 3.4(10) . . . . ?
C5 C4 C3 C2 0.7(10) . . . . ?
C1 C2 C3 C4 -3.6(10) . . . . ?
C7 N2 C9 C11 -103.3(6) . . . . ?
Ge1 N2 C9 C11 73.2(5) . . . . ?
C1 N1 C8 C10 -108.1(6) . . . . ?
Ge1 N1 C8 C10 84.1(5) . . . . ?
C16 N3 C23 C25 67.7(6) . . . . ?
Ge2 N3 C23 C25 -125.0(4) . . . . ?
C22 N4 C24 C26 70.6(6) . . . . ?
Ge2 N4 C24 C26 -112.6(4) . . . . ?
N2 C9 C11 C14 57.4(6) . . . . ?
N2 C9 C11 C15 -179.0(5) . . . . ?
N3 C23 C25 C28 53.2(6) . . . . ?
N3 C23 C25 C27 176.4(5) . . . . ?
N4 C24 C26 C29 68.5(6) . . . . ?
N4 C24 C26 C30 -170.0(5) . . . . ?
N1 C8 C10 C13 58.7(7) . . . . ?
N1 C8 C10 C12 -178.0(6) . . . . ?

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         0.973
_refine_diff_density_min         -0.763
_refine_diff_density_rms         0.155
_vrf_PLAT029_1                   
;
PROBLEM: Site occupancy factor(sof) is low (0.61) for the bridging selenium atom due to a disorder
Author Response:
The disorder on the bridging selenium atom could not be fixed because other site(s) was/were not identified with the current dataset. Although the presence of residual sulfur can not be ruled out, assigning this site to sulfur gives the ADP for sulfur as NPD and worsens the R-factors. Also, the data collected for the crystals grown from other solvents such as benzene and tetrahydrofuran were not good enough to model the structure even up to this level. This was the best crystal and detaset we could obtain for this compound.

;
# end validation form
_exptl_crystal_recrystallization_method 'cooling saturated solution'
_chemical_properties_physical    Moisture-sensitive
####################################################################### 
# 
# 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_4
_database_code_depnum_ccdc_archive 'CCDC 1028134'
_audit_update_record             
;
2014-10-08 deposited with the CCDC.
2015-02-02 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C30 H46 Ge2 N4 S3'
_chemical_formula_sum            'C30 H46 Ge2 N4 S3'

_chemical_formula_weight         704.14

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'
Ge Ge 0.1547 1.8001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   'P 21/c'
_symmetry_space_group_name_hall  '-P 2ybc'

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

_cell_length_a                   16.400(4)
_cell_length_b                   11.364(3)
_cell_length_c                   18.733(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 106.005(4)
_cell_angle_gamma                90.00
_cell_volume                     3355.9(15)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    3366
_cell_measurement_theta_min      2.58
_cell_measurement_theta_max      25.000

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.474
_exptl_crystal_size_mid          0.339
_exptl_crystal_size_min          0.255
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.394
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1464.0
_exptl_absorpt_coefficient_mu    2.003
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.447
_exptl_absorpt_correction_T_max  0.600
_exptl_absorpt_process_details   '(SADABS; Bruker, 2000)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      150(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            17191
_diffrn_reflns_av_R_equivalents  0.0503
_diffrn_reflns_av_sigmaI/netI    0.0602
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         1.29
_diffrn_reflns_theta_max         25.00
_reflns_number_total             5904
_reflns_number_gt                4692
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_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)+(0.0481P)²+0.0000P] 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         5903
_refine_ls_number_parameters     360
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0599
_refine_ls_R_factor_gt           0.0426
_refine_ls_wR_factor_ref         0.0981
_refine_ls_wR_factor_gt          0.0921
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_restrained_S_all      1.025
_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 0.35207(2) 0.28950(3) 0.43036(2) 0.01917(12) Uani 1 1 d . . .
Ge2 Ge 0.18557(2) 0.17880(3) 0.28259(2) 0.01919(12) Uani 1 1 d . . .
S3 S 0.32319(6) 0.22066(8) 0.31522(6) 0.0261(2) Uani 1 1 d . . .
S2 S 0.13786(6) 0.07887(8) 0.35481(6) 0.0276(2) Uani 1 1 d . . .
S1 S 0.27474(6) 0.40886(8) 0.46535(6) 0.0251(2) Uani 1 1 d . . .
N1 N 0.46605(18) 0.3382(2) 0.44486(17) 0.0207(7) Uani 1 1 d . . .
N2 N 0.40083(19) 0.1653(2) 0.49477(17) 0.0201(7) Uani 1 1 d . . .
N3 N 0.11972(18) 0.3096(2) 0.23745(17) 0.0206(7) Uani 1 1 d . . .
N4 N 0.17393(18) 0.1304(2) 0.18346(17) 0.0185(7) Uani 1 1 d . . .
C7 C 0.4846(2) 0.1768(3) 0.5268(2) 0.0204(8) Uani 1 1 d . . .
C17 C 0.0189(2) 0.3680(3) 0.1246(2) 0.0242(9) Uani 1 1 d . . .
H17 H -0.0053 0.4144 0.1543 0.029 Uiso 1 1 calc R . .
C22 C 0.1249(2) 0.2024(3) 0.1317(2) 0.0194(8) Uani 1 1 d . . .
C16 C 0.0872(2) 0.2987(3) 0.1636(2) 0.0198(8) Uani 1 1 d . . .
C9 C 0.3469(2) 0.0695(3) 0.5092(2) 0.0227(9) Uani 1 1 d . . .
H9A H 0.3831 0.0047 0.5322 0.027 Uiso 1 1 calc R . .
H9B H 0.3110 0.0418 0.4621 0.027 Uiso 1 1 calc R . .
C27 C 0.2155(3) 0.5382(3) 0.2714(2) 0.0327(10) Uani 1 1 d . . .
H27A H 0.2278 0.6163 0.2577 0.049 Uiso 1 1 calc R . .
H27B H 0.2308 0.4821 0.2390 0.049 Uiso 1 1 calc R . .
H27C H 0.2475 0.5228 0.3218 0.049 Uiso 1 1 calc R . .
C18 C -0.0182(2) 0.3787(3) 0.0498(2) 0.0291(10) Uani 1 1 d . . .
H18 H -0.0661 0.4265 0.0368 0.035 Uiso 1 1 calc R . .
C6 C 0.5286(2) 0.1027(3) 0.5849(2) 0.0269(9) Uani 1 1 d . . .
H6 H 0.4947 0.0469 0.5992 0.032 Uiso 1 1 calc R . .
C21 C 0.1171(2) 0.1883(3) 0.0559(2) 0.0250(9) Uani 1 1 d . . .
H21 H 0.1516 0.1299 0.0451 0.030 Uiso 1 1 calc R . .
C24 C 0.2183(2) 0.0284(3) 0.1622(2) 0.0256(9) Uani 1 1 d . . .
H24A H 0.2603 -0.0003 0.2059 0.031 Uiso 1 1 calc R . .
H24B H 0.2480 0.0543 0.1269 0.031 Uiso 1 1 calc R . .
C1 C 0.5231(2) 0.2749(3) 0.4951(2) 0.0190(8) Uani 1 1 d . . .
C10 C 0.4837(3) 0.4394(3) 0.3308(2) 0.0331(10) Uani 1 1 d . . .
H10 H 0.4274 0.4126 0.3020 0.040 Uiso 1 1 calc R . .
C23 C 0.0948(2) 0.4035(3) 0.2813(2) 0.0257(9) Uani 1 1 d . . .
H23A H 0.1196 0.3870 0.3336 0.031 Uiso 1 1 calc R . .
H23B H 0.0336 0.4017 0.2721 0.031 Uiso 1 1 calc R . .
C3 C 0.6784(2) 0.2531(3) 0.5663(2) 0.0322(10) Uani 1 1 d . . .
H3 H 0.7307 0.2862 0.5676 0.039 Uiso 1 1 calc R . .
C11 C 0.2908(2) 0.1024(3) 0.5585(2) 0.0269(9) Uani 1 1 d . . .
H11 H 0.2515 0.1636 0.5327 0.032 Uiso 1 1 calc R . .
C20 C 0.0671(2) 0.2458(3) -0.0057(2) 0.0292(9) Uani 1 1 d . . .
H20 H 0.0767 0.2256 -0.0508 0.035 Uiso 1 1 calc R . .
C8 C 0.4834(2) 0.4491(3) 0.4116(2) 0.0256(9) Uani 1 1 d . . .
H8A H 0.5381 0.4786 0.4403 0.031 Uiso 1 1 calc R . .
H8B H 0.4409 0.5064 0.4153 0.031 Uiso 1 1 calc R . .
C2 C 0.6100(2) 0.3003(3) 0.5140(2) 0.0292(9) Uani 1 1 d . . .
H2 H 0.6243 0.3604 0.4860 0.035 Uiso 1 1 calc R . .
C5 C 0.6128(3) 0.0983(3) 0.6244(2) 0.0327(10) Uani 1 1 d . . .
H5 H 0.6260 0.0422 0.6620 0.039 Uiso 1 1 calc R . .
C19 C 0.0046(3) 0.3294(3) -0.0094(2) 0.0336(10) Uani 1 1 d . . .
H19 H -0.0250 0.3550 -0.0566 0.040 Uiso 1 1 calc R . .
C26 C 0.1589(2) -0.0730(3) 0.1279(2) 0.0266(9) Uani 1 1 d . . .
H26 H 0.1095 -0.0397 0.0915 0.032 Uiso 1 1 calc R . .
C4 C 0.6811(3) 0.1641(3) 0.6169(2) 0.0333(10) Uani 1 1 d . . .
H4 H 0.7339 0.1465 0.6492 0.040 Uiso 1 1 calc R . .
C25 C 0.1212(3) 0.5278(3) 0.2647(2) 0.0298(10) Uani 1 1 d . . .
H25 H 0.0897 0.5481 0.2137 0.036 Uiso 1 1 calc R . .
C14 C 0.3390(3) 0.1513(4) 0.6336(2) 0.0412(12) Uani 1 1 d . . .
H14A H 0.3744 0.0908 0.6621 0.062 Uiso 1 1 calc R . .
H14B H 0.2995 0.1779 0.6596 0.062 Uiso 1 1 calc R . .
H14C H 0.3737 0.2160 0.6268 0.062 Uiso 1 1 calc R . .
C15 C 0.2381(3) -0.0044(4) 0.5668(2) 0.0398(11) Uani 1 1 d . . .
H15A H 0.2097 -0.0349 0.5185 0.060 Uiso 1 1 calc R . .
H15B H 0.1967 0.0183 0.5918 0.060 Uiso 1 1 calc R . .
H15C H 0.2745 -0.0639 0.5952 0.060 Uiso 1 1 calc R . .
C28 C 0.0941(3) 0.6123(3) 0.3172(3) 0.0406(12) Uani 1 1 d . . .
H28A H 0.1230 0.5924 0.3677 0.061 Uiso 1 1 calc R . .
H28B H 0.0340 0.6063 0.3099 0.061 Uiso 1 1 calc R . .
H28C H 0.1083 0.6914 0.3072 0.061 Uiso 1 1 calc R . .
C29 C 0.1279(3) -0.1369(4) 0.1856(3) 0.0437(12) Uani 1 1 d . . .
H29A H 0.0864 -0.1944 0.1619 0.066 Uiso 1 1 calc R . .
H29B H 0.1028 -0.0816 0.2120 0.066 Uiso 1 1 calc R . .
H29C H 0.1748 -0.1754 0.2198 0.066 Uiso 1 1 calc R . .
C13 C 0.4985(4) 0.5615(4) 0.3027(3) 0.0613(16) Uani 1 1 d . . .
H13A H 0.5515 0.5922 0.3327 0.092 Uiso 1 1 calc R . .
H13B H 0.4532 0.6130 0.3059 0.092 Uiso 1 1 calc R . .
H13C H 0.5002 0.5562 0.2520 0.092 Uiso 1 1 calc R . .
C30 C 0.2032(3) -0.1566(4) 0.0871(3) 0.0549(15) Uani 1 1 d . . .
H30A H 0.2531 -0.1880 0.1214 0.082 Uiso 1 1 calc R . .
H30B H 0.2189 -0.1146 0.0484 0.082 Uiso 1 1 calc R . .
H30C H 0.1655 -0.2197 0.0657 0.082 Uiso 1 1 calc R . .
C12 C 0.5484(3) 0.3521(4) 0.3188(3) 0.0527(13) Uani 1 1 d . . .
H12A H 0.6043 0.3782 0.3449 0.079 Uiso 1 1 calc R . .
H12B H 0.5438 0.3463 0.2667 0.079 Uiso 1 1 calc R . .
H12C H 0.5380 0.2763 0.3373 0.079 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 N2 1.886(3) . ?
Ge1 N1 1.896(3) . ?
Ge1 S1 2.0824(10) . ?
Ge1 S3 2.2192(12) . ?
Ge2 N3 1.894(3) . ?
Ge2 N4 1.895(3) . ?
Ge2 S2 2.0774(11) . ?
Ge2 S3 2.2212(11) . ?
N1 C1 1.339(4) . ?
N1 C8 1.468(4) . ?
N2 C7 1.345(4) . ?
N2 C9 1.474(4) . ?
N3 C16 1.345(5) . ?
N3 C23 1.472(4) . ?
N4 C22 1.351(4) . ?
N4 C24 1.480(4) . ?
C7 C6 1.407(5) . ?
C7 C1 1.484(5) . ?
C17 C18 1.371(5) . ?
C17 C16 1.400(5) . ?
C17 H17 0.9300 . ?
C22 C21 1.399(5) . ?
C22 C16 1.462(5) . ?
C9 C11 1.518(5) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C27 C25 1.522(5) . ?
C27 H27A 0.9600 . ?
C27 H27B 0.9600 . ?
C27 H27C 0.9600 . ?
C18 C19 1.383(6) . ?
C18 H18 0.9300 . ?
C6 C5 1.376(5) . ?
C6 H6 0.9300 . ?
C21 C20 1.381(5) . ?
C21 H21 0.9300 . ?
C24 C26 1.531(5) . ?
C24 H24A 0.9700 . ?
C24 H24B 0.9700 . ?
C1 C2 1.401(5) . ?
C10 C12 1.513(6) . ?
C10 C8 1.520(5) . ?
C10 C13 1.527(5) . ?
C10 H10 0.9800 . ?
C23 C25 1.534(5) . ?
C23 H23A 0.9700 . ?
C23 H23B 0.9700 . ?
C3 C4 1.378(6) . ?
C3 C2 1.379(5) . ?
C3 H3 0.9300 . ?
C11 C14 1.517(5) . ?
C11 C15 1.523(5) . ?
C11 H11 0.9800 . ?
C20 C19 1.385(5) . ?
C20 H20 0.9300 . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C2 H2 0.9300 . ?
C5 C4 1.386(6) . ?
C5 H5 0.9300 . ?
C19 H19 0.9300 . ?
C26 C29 1.502(6) . ?
C26 C30 1.523(5) . ?
C26 H26 0.9800 . ?
C4 H4 0.9300 . ?
C25 C28 1.526(5) . ?
C25 H25 0.9800 . ?
C14 H14A 0.9600 . ?
C14 H14B 0.9600 . ?
C14 H14C 0.9600 . ?
C15 H15A 0.9600 . ?
C15 H15B 0.9600 . ?
C15 H15C 0.9600 . ?
C28 H28A 0.9600 . ?
C28 H28B 0.9600 . ?
C28 H28C 0.9600 . ?
C29 H29A 0.9600 . ?
C29 H29B 0.9600 . ?
C29 H29C 0.9600 . ?
C13 H13A 0.9600 . ?
C13 H13B 0.9600 . ?
C13 H13C 0.9600 . ?
C30 H30A 0.9600 . ?
C30 H30B 0.9600 . ?
C30 H30C 0.9600 . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 0.9600 . ?

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
N2 Ge1 N1 84.23(12) . . ?
N2 Ge1 S1 118.28(10) . . ?
N1 Ge1 S1 115.26(9) . . ?
N2 Ge1 S3 107.30(9) . . ?
N1 Ge1 S3 100.36(10) . . ?
S1 Ge1 S3 123.39(4) . . ?
N3 Ge2 N4 84.21(12) . . ?
N3 Ge2 S2 116.68(10) . . ?
N4 Ge2 S2 121.68(9) . . ?
N3 Ge2 S3 111.46(9) . . ?
N4 Ge2 S3 98.74(9) . . ?
S2 Ge2 S3 118.33(4) . . ?
Ge1 S3 Ge2 105.74(4) . . ?
C1 N1 C8 125.5(3) . . ?
C1 N1 Ge1 114.4(2) . . ?
C8 N1 Ge1 119.2(2) . . ?
C7 N2 C9 125.5(3) . . ?
C7 N2 Ge1 114.4(2) . . ?
C9 N2 Ge1 120.0(2) . . ?
C16 N3 C23 123.3(3) . . ?
C16 N3 Ge2 113.7(2) . . ?
C23 N3 Ge2 122.1(2) . . ?
C22 N4 C24 121.4(3) . . ?
C22 N4 Ge2 114.0(2) . . ?
C24 N4 Ge2 124.5(2) . . ?
N2 C7 C6 122.0(3) . . ?
N2 C7 C1 112.9(3) . . ?
C6 C7 C1 125.1(3) . . ?
C18 C17 C16 130.4(4) . . ?
C18 C17 H17 114.8 . . ?
C16 C17 H17 114.8 . . ?
N4 C22 C21 121.9(3) . . ?
N4 C22 C16 113.2(3) . . ?
C21 C22 C16 124.7(3) . . ?
N3 C16 C17 121.2(3) . . ?
N3 C16 C22 113.4(3) . . ?
C17 C16 C22 125.2(4) . . ?
N2 C9 C11 115.2(3) . . ?
N2 C9 H9A 108.5 . . ?
C11 C9 H9A 108.5 . . ?
N2 C9 H9B 108.5 . . ?
C11 C9 H9B 108.5 . . ?
H9A C9 H9B 107.5 . . ?
C25 C27 H27A 109.5 . . ?
C25 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
C25 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C17 C18 C19 130.0(4) . . ?
C17 C18 H18 115.0 . . ?
C19 C18 H18 115.0 . . ?
C5 C6 C7 131.5(4) . . ?
C5 C6 H6 114.3 . . ?
C7 C6 H6 114.3 . . ?
C20 C21 C22 131.3(4) . . ?
C20 C21 H21 114.3 . . ?
C22 C21 H21 114.3 . . ?
N4 C24 C26 113.6(3) . . ?
N4 C24 H24A 108.9 . . ?
C26 C24 H24A 108.9 . . ?
N4 C24 H24B 108.9 . . ?
C26 C24 H24B 108.9 . . ?
H24A C24 H24B 107.7 . . ?
N1 C1 C2 122.1(3) . . ?
N1 C1 C7 113.2(3) . . ?
C2 C1 C7 124.7(3) . . ?
C12 C10 C8 113.0(3) . . ?
C12 C10 C13 111.1(4) . . ?
C8 C10 C13 108.7(3) . . ?
C12 C10 H10 108.0 . . ?
C8 C10 H10 108.0 . . ?
C13 C10 H10 108.0 . . ?
N3 C23 C25 114.6(3) . . ?
N3 C23 H23A 108.6 . . ?
C25 C23 H23A 108.6 . . ?
N3 C23 H23B 108.6 . . ?
C25 C23 H23B 108.6 . . ?
H23A C23 H23B 107.6 . . ?
C4 C3 C2 129.8(4) . . ?
C4 C3 H3 115.1 . . ?
C2 C3 H3 115.1 . . ?
C14 C11 C9 113.9(3) . . ?
C14 C11 C15 111.3(3) . . ?
C9 C11 C15 108.8(3) . . ?
C14 C11 H11 107.5 . . ?
C9 C11 H11 107.5 . . ?
C15 C11 H11 107.5 . . ?
C21 C20 C19 128.9(4) . . ?
C21 C20 H20 115.6 . . ?
C19 C20 H20 115.6 . . ?
N1 C8 C10 114.5(3) . . ?
N1 C8 H8A 108.6 . . ?
C10 C8 H8A 108.6 . . ?
N1 C8 H8B 108.6 . . ?
C10 C8 H8B 108.6 . . ?
H8A C8 H8B 107.6 . . ?
C3 C2 C1 132.2(4) . . ?
C3 C2 H2 113.9 . . ?
C1 C2 H2 113.9 . . ?
C6 C5 C4 130.2(4) . . ?
C6 C5 H5 114.9 . . ?
C4 C5 H5 114.9 . . ?
C18 C19 C20 126.7(4) . . ?
C18 C19 H19 116.7 . . ?
C20 C19 H19 116.7 . . ?
C29 C26 C30 111.3(3) . . ?
C29 C26 C24 111.3(3) . . ?
C30 C26 C24 110.1(3) . . ?
C29 C26 H26 108.0 . . ?
C30 C26 H26 108.0 . . ?
C24 C26 H26 108.0 . . ?
C3 C4 C5 126.3(4) . . ?
C3 C4 H4 116.9 . . ?
C5 C4 H4 116.9 . . ?
C27 C25 C28 111.6(3) . . ?
C27 C25 C23 113.1(3) . . ?
C28 C25 C23 107.5(3) . . ?
C27 C25 H25 108.2 . . ?
C28 C25 H25 108.2 . . ?
C23 C25 H25 108.2 . . ?
C11 C14 H14A 109.5 . . ?
C11 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C11 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C11 C15 H15A 109.5 . . ?
C11 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C11 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C25 C28 H28A 109.5 . . ?
C25 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C25 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C26 C29 H29A 109.5 . . ?
C26 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
C26 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C10 C13 H13A 109.5 . . ?
C10 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C10 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C26 C30 H30A 109.5 . . ?
C26 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
C26 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C10 C12 H12A 109.5 . . ?
C10 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C10 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
N2 Ge1 S3 Ge2 99.69(10) . . . . ?
N1 Ge1 S3 Ge2 -173.19(9) . . . . ?
S1 Ge1 S3 Ge2 -43.39(6) . . . . ?
N3 Ge2 S3 Ge1 90.04(11) . . . . ?
N4 Ge2 S3 Ge1 177.22(8) . . . . ?
S2 Ge2 S3 Ge1 -49.42(6) . . . . ?
N2 Ge1 N1 C1 -5.7(3) . . . . ?
S1 Ge1 N1 C1 112.9(2) . . . . ?
S3 Ge1 N1 C1 -112.3(2) . . . . ?
N2 Ge1 N1 C8 -175.7(3) . . . . ?
S1 Ge1 N1 C8 -57.1(3) . . . . ?
S3 Ge1 N1 C8 77.7(3) . . . . ?
N1 Ge1 N2 C7 8.5(3) . . . . ?
S1 Ge1 N2 C7 -107.1(2) . . . . ?
S3 Ge1 N2 C7 107.6(2) . . . . ?
N1 Ge1 N2 C9 -174.5(3) . . . . ?
S1 Ge1 N2 C9 69.9(3) . . . . ?
S3 Ge1 N2 C9 -75.4(3) . . . . ?
N4 Ge2 N3 C16 9.2(3) . . . . ?
S2 Ge2 N3 C16 -113.5(2) . . . . ?
S3 Ge2 N3 C16 106.3(2) . . . . ?
N4 Ge2 N3 C23 179.1(3) . . . . ?
S2 Ge2 N3 C23 56.4(3) . . . . ?
S3 Ge2 N3 C23 -83.8(3) . . . . ?
N3 Ge2 N4 C22 -2.9(2) . . . . ?
S2 Ge2 N4 C22 115.0(2) . . . . ?
S3 Ge2 N4 C22 -113.8(2) . . . . ?
N3 Ge2 N4 C24 172.9(3) . . . . ?
S2 Ge2 N4 C24 -69.2(3) . . . . ?
S3 Ge2 N4 C24 62.1(3) . . . . ?
C9 N2 C7 C6 -6.9(5) . . . . ?
Ge1 N2 C7 C6 169.8(3) . . . . ?
C9 N2 C7 C1 173.8(3) . . . . ?
Ge1 N2 C7 C1 -9.4(4) . . . . ?
C24 N4 C22 C21 -3.5(5) . . . . ?
Ge2 N4 C22 C21 172.5(3) . . . . ?
C24 N4 C22 C16 -179.4(3) . . . . ?
Ge2 N4 C22 C16 -3.4(4) . . . . ?
C23 N3 C16 C17 -8.3(5) . . . . ?
Ge2 N3 C16 C17 161.4(3) . . . . ?
C23 N3 C16 C22 177.0(3) . . . . ?
Ge2 N3 C16 C22 -13.2(4) . . . . ?
C18 C17 C16 N3 173.2(4) . . . . ?
C18 C17 C16 C22 -12.8(6) . . . . ?
N4 C22 C16 N3 10.9(4) . . . . ?
C21 C22 C16 N3 -164.9(3) . . . . ?
N4 C22 C16 C17 -163.5(3) . . . . ?
C21 C22 C16 C17 20.7(6) . . . . ?
C7 N2 C9 C11 103.6(4) . . . . ?
Ge1 N2 C9 C11 -73.0(4) . . . . ?
C16 C17 C18 C19 -4.6(7) . . . . ?
N2 C7 C6 C5 179.2(4) . . . . ?
C1 C7 C6 C5 -1.7(7) . . . . ?
N4 C22 C21 C20 175.2(4) . . . . ?
C16 C22 C21 C20 -9.4(6) . . . . ?
C22 N4 C24 C26 -72.4(4) . . . . ?
Ge2 N4 C24 C26 112.1(3) . . . . ?
C8 N1 C1 C2 -9.2(6) . . . . ?
Ge1 N1 C1 C2 -178.5(3) . . . . ?
C8 N1 C1 C7 171.3(3) . . . . ?
Ge1 N1 C1 C7 2.0(4) . . . . ?
N2 C7 C1 N1 4.8(4) . . . . ?
C6 C7 C1 N1 -174.4(3) . . . . ?
N2 C7 C1 C2 -174.6(3) . . . . ?
C6 C7 C1 C2 6.1(6) . . . . ?
C16 N3 C23 C25 -66.9(4) . . . . ?
Ge2 N3 C23 C25 124.2(3) . . . . ?
N2 C9 C11 C14 -56.4(4) . . . . ?
N2 C9 C11 C15 178.8(3) . . . . ?
C22 C21 C20 C19 -5.6(7) . . . . ?
C1 N1 C8 C10 107.8(4) . . . . ?
Ge1 N1 C8 C10 -83.3(4) . . . . ?
C12 C10 C8 N1 -58.6(5) . . . . ?
C13 C10 C8 N1 177.6(3) . . . . ?
C4 C3 C2 C1 -0.1(7) . . . . ?
N1 C1 C2 C3 175.4(4) . . . . ?
C7 C1 C2 C3 -5.2(7) . . . . ?
C7 C6 C5 C4 -2.4(7) . . . . ?
C17 C18 C19 C20 7.4(7) . . . . ?
C21 C20 C19 C18 3.9(7) . . . . ?
N4 C24 C26 C29 -73.0(4) . . . . ?
N4 C24 C26 C30 163.1(4) . . . . ?
C2 C3 C4 C5 2.3(7) . . . . ?
C6 C5 C4 C3 0.8(7) . . . . ?
N3 C23 C25 C27 -53.8(5) . . . . ?
N3 C23 C25 C28 -177.4(3) . . . . ?

_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         0.774
_refine_diff_density_min         -0.359
_refine_diff_density_rms         0.093
