# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2018

####################################################################### 
# 
# 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 1810961'
_audit_update_record             
;
2017-12-13 deposited with the CCDC.
2018-03-14 downloaded from the CCDC.
;


_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C18 H34 S2 Si4'
_chemical_formula_sum            'C18 H34 S2 Si4'
_chemical_formula_weight         426.93

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'
Si Si 0.0817 0.0704 '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           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                   6.6294(5)
_cell_length_b                   6.7581(5)
_cell_length_c                   14.6108(11)
_cell_angle_alpha                85.8080(10)
_cell_angle_beta                 81.3960(10)
_cell_angle_gamma                79.9180(10)
_cell_volume                     636.49(8)
_cell_formula_units_Z            1
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    5081
_cell_measurement_theta_min      2.824
_cell_measurement_theta_max      30.445

_exptl_crystal_description       plate
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.114
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             230
_exptl_absorpt_coefficient_mu    0.398
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8733
_exptl_absorpt_correction_T_max  0.9613
_exptl_absorpt_process_details   'SADABS (Bruker, 2008)'

_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  'Bruker SMART APEXII'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         .
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  .
_diffrn_standards_decay_%        0
_diffrn_reflns_number            6151
_diffrn_reflns_av_R_equivalents  0.0107
_diffrn_reflns_av_sigmaI/netI    0.0133
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         3.07
_diffrn_reflns_theta_max         27.00
_reflns_number_total             2763
_reflns_number_gt                2566
_reflns_threshold_expression     I>2σ(I)

_computing_data_collection       'APEX2 (Bruker, 2008)'
_computing_cell_refinement       'SAINT (Bruker, 2008)'
_computing_data_reduction        'SAINT (Bruker, 2008)'
_computing_structure_solution    'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXTL (Sheldrick, 2008)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'

_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)+(0.0377P)²+0.1923P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         2763
_refine_ls_number_parameters     135
_refine_ls_number_restraints     30
_refine_ls_R_factor_all          0.0278
_refine_ls_R_factor_gt           0.0257
_refine_ls_wR_factor_ref         0.0724
_refine_ls_wR_factor_gt          0.0704
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_restrained_S_all      1.097
_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
S1 S 0.31850(5) 0.54599(5) 0.38429(2) 0.02986(10) Uani 1 1 d . A .
Si1 Si 0.04582(5) 0.31865(5) 0.28259(2) 0.02401(10) Uani 1 1 d . A .
Si2 Si 0.27814(6) 0.19539(6) 0.15479(3) 0.03151(11) Uani 1 1 d D . .
C1 C 0.43243(18) 0.44612(18) 0.48009(8) 0.0244(2) Uani 1 1 d . . .
C2 C 0.3757(2) 0.2630(2) 0.50713(9) 0.0308(3) Uani 1 1 d . . .
C3 C 0.2433(2) 0.2050(2) 0.45001(9) 0.0312(3) Uani 1 1 d . A .
C4 C 0.19587(19) 0.34189(19) 0.37901(8) 0.0261(2) Uani 1 1 d . . .
C5 C -0.1351(2) 0.1374(2) 0.32510(11) 0.0368(3) Uani 1 1 d . . .
H5A H -0.2342 0.1932 0.3773 0.055 Uiso 1 1 calc R A .
H5B H -0.0559 0.0095 0.3454 0.055 Uiso 1 1 calc R . .
H5C H -0.2099 0.1144 0.2749 0.055 Uiso 1 1 calc R . .
C6 C -0.0972(2) 0.5731(2) 0.25146(11) 0.0361(3) Uani 1 1 d . . .
H6A H -0.1978 0.6218 0.3046 0.054 Uiso 1 1 calc R A .
H6B H -0.1699 0.5637 0.1986 0.054 Uiso 1 1 calc R . .
H6C H 0.0011 0.6669 0.2349 0.054 Uiso 1 1 calc R . .
H2 H 0.420(3) 0.187(3) 0.5561(12) 0.039(4) Uiso 1 1 d . . .
H3 H 0.192(3) 0.082(3) 0.4582(11) 0.036(4) Uiso 1 1 d . . .
C7A C 0.120(2) 0.260(3) 0.0562(8) 0.0798(12) Uani 0.202(11) 1 d PD A 1
H7AA H 0.2041 0.2126 -0.0016 0.120 Uiso 0.202(11) 1 calc PR A 1
H7AB H 0.0779 0.4064 0.0503 0.120 Uiso 0.202(11) 1 calc PR A 1
H7AC H -0.0026 0.1952 0.0686 0.120 Uiso 0.202(11) 1 calc PR A 1
C8A C 0.372(2) -0.0818(7) 0.1591(12) 0.0546(10) Uani 0.202(11) 1 d PD A 1
H8AA H 0.4680 -0.1182 0.1028 0.082 Uiso 0.202(11) 1 calc PR A 1
H8AB H 0.2540 -0.1530 0.1633 0.082 Uiso 0.202(11) 1 calc PR A 1
H8AC H 0.4434 -0.1198 0.2134 0.082 Uiso 0.202(11) 1 calc PR A 1
C9A C 0.5048(17) 0.332(2) 0.1311(14) 0.0451(6) Uani 0.202(11) 1 d PD A 1
H9AA H 0.5802 0.3011 0.0694 0.068 Uiso 0.202(11) 1 calc PR A 1
H9AB H 0.5971 0.2891 0.1779 0.068 Uiso 0.202(11) 1 calc PR A 1
H9AC H 0.4557 0.4773 0.1335 0.068 Uiso 0.202(11) 1 calc PR A 1
C7B C 0.1376(5) 0.1689(10) 0.0563(2) 0.0798(12) Uani 0.798(11) 1 d PD A 2
H7BA H 0.2364 0.1109 0.0045 0.120 Uiso 0.798(11) 1 calc PR A 2
H7BB H 0.0673 0.3015 0.0365 0.120 Uiso 0.798(11) 1 calc PR A 2
H7BC H 0.0352 0.0804 0.0760 0.120 Uiso 0.798(11) 1 calc PR A 2
C8B C 0.4203(6) -0.0595(4) 0.1904(3) 0.0546(10) Uani 0.798(11) 1 d PD A 2
H8BB H 0.5283 -0.1081 0.1398 0.082 Uiso 0.798(11) 1 calc PR A 2
H8BC H 0.3227 -0.1546 0.2040 0.082 Uiso 0.798(11) 1 calc PR A 2
H8BD H 0.4838 -0.0481 0.2458 0.082 Uiso 0.798(11) 1 calc PR A 2
C9B C 0.4740(5) 0.3648(5) 0.1191(3) 0.0451(6) Uani 0.798(11) 1 d PD A 2
H9BB H 0.5780 0.3044 0.0696 0.068 Uiso 0.798(11) 1 calc PR A 2
H9BC H 0.5415 0.3832 0.1724 0.068 Uiso 0.798(11) 1 calc PR A 2
H9BD H 0.4051 0.4957 0.0965 0.068 Uiso 0.798(11) 1 calc PR A 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
S1 C1 1.7276(12) . ?
S1 C4 1.7310(13) . ?
Si1 C4 1.8723(13) . ?
Si1 C5 1.8724(14) . ?
Si1 C6 1.8726(14) . ?
Si1 Si2 2.3388(5) . ?
Si2 C7B 1.863(2) . ?
Si2 C8A 1.867(4) . ?
Si2 C9B 1.8707(19) . ?
Si2 C9A 1.875(4) . ?
Si2 C7A 1.886(4) . ?
Si2 C8B 1.891(2) . ?
C1 C2 1.3700(18) . ?
C1 C1 1.455(2) 2_666 ?
C2 C3 1.4167(19) . ?
C2 H2 0.906(17) . ?
C3 C4 1.3732(18) . ?
C3 H3 0.943(17) . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C7A H7AA 0.9800 . ?
C7A H7AB 0.9800 . ?
C7A H7AC 0.9800 . ?
C8A H8AA 0.9800 . ?
C8A H8AB 0.9800 . ?
C8A H8AC 0.9800 . ?
C9A H9AA 0.9800 . ?
C9A H9AB 0.9800 . ?
C9A H9AC 0.9800 . ?
C7B H7BA 0.9800 . ?
C7B H7BB 0.9800 . ?
C7B H7BC 0.9800 . ?
C8B H8BB 0.9800 . ?
C8B H8BC 0.9800 . ?
C8B H8BD 0.9800 . ?
C9B H9BB 0.9800 . ?
C9B H9BC 0.9800 . ?
C9B H9BD 0.9800 . ?

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
C1 S1 C4 93.71(6) . . ?
C4 Si1 C5 107.19(6) . . ?
C4 Si1 C6 108.91(6) . . ?
C5 Si1 C6 111.71(7) . . ?
C4 Si1 Si2 108.54(4) . . ?
C5 Si1 Si2 110.51(5) . . ?
C6 Si1 Si2 109.87(5) . . ?
C7B Si2 C9B 110.35(14) . . ?
C7B Si2 C9A 117.9(7) . . ?
C8A Si2 C9A 109.6(3) . . ?
C8A Si2 C7A 108.5(3) . . ?
C9A Si2 C7A 108.1(3) . . ?
C7B Si2 C8B 109.38(13) . . ?
C9B Si2 C8B 107.88(11) . . ?
C7B Si2 Si1 110.56(12) . . ?
C8A Si2 Si1 115.8(4) . . ?
C9B Si2 Si1 110.50(14) . . ?
C9A Si2 Si1 111.7(6) . . ?
C7A Si2 Si1 102.7(5) . . ?
C8B Si2 Si1 108.10(11) . . ?
C2 C1 C1 129.27(14) . 2_666 ?
C2 C1 S1 109.87(9) . . ?
C1 C1 S1 120.85(12) 2_666 . ?
C1 C2 C3 113.06(12) . . ?
C1 C2 H2 123.1(11) . . ?
C3 C2 H2 123.9(11) . . ?
C4 C3 C2 114.53(12) . . ?
C4 C3 H3 121.4(10) . . ?
C2 C3 H3 124.0(10) . . ?
C3 C4 S1 108.81(9) . . ?
C3 C4 Si1 128.88(10) . . ?
S1 C4 Si1 122.10(7) . . ?
Si1 C5 H5A 109.5 . . ?
Si1 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
Si1 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
Si1 C6 H6A 109.5 . . ?
Si1 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
Si1 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
Si2 C7A H7AA 109.5 . . ?
Si2 C7A H7AB 109.5 . . ?
Si2 C7A H7AC 109.5 . . ?
Si2 C8A H8AA 109.5 . . ?
Si2 C8A H8AB 109.5 . . ?
Si2 C8A H8AC 109.5 . . ?
Si2 C9A H9AA 109.5 . . ?
Si2 C9A H9AB 109.5 . . ?
Si2 C9A H9AC 109.5 . . ?
Si2 C7B H7BA 109.5 . . ?
Si2 C7B H7BB 109.5 . . ?
H7BA C7B H7BB 109.5 . . ?
Si2 C7B H7BC 109.5 . . ?
H7BA C7B H7BC 109.5 . . ?
H7BB C7B H7BC 109.5 . . ?
Si2 C8B H8BB 109.5 . . ?
Si2 C8B H8BC 109.5 . . ?
H8BB C8B H8BC 109.5 . . ?
Si2 C8B H8BD 109.5 . . ?
H8BB C8B H8BD 109.5 . . ?
H8BC C8B H8BD 109.5 . . ?
Si2 C9B H9BB 109.5 . . ?
Si2 C9B H9BC 109.5 . . ?
H9BB C9B H9BC 109.5 . . ?
Si2 C9B H9BD 109.5 . . ?
H9BB C9B H9BD 109.5 . . ?
H9BC C9B H9BD 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
C4 Si1 Si2 C7B 180.0(2) . . . . ?
C5 Si1 Si2 C7B 62.7(2) . . . . ?
C6 Si1 Si2 C7B -61.0(2) . . . . ?
C4 Si1 Si2 C8A 79.7(6) . . . . ?
C5 Si1 Si2 C8A -37.6(6) . . . . ?
C6 Si1 Si2 C8A -161.3(6) . . . . ?
C4 Si1 Si2 C9B -57.54(14) . . . . ?
C5 Si1 Si2 C9B -174.82(14) . . . . ?
C6 Si1 Si2 C9B 61.46(14) . . . . ?
C4 Si1 Si2 C9A -46.7(5) . . . . ?
C5 Si1 Si2 C9A -164.0(5) . . . . ?
C6 Si1 Si2 C9A 72.3(5) . . . . ?
C4 Si1 Si2 C7A -162.3(6) . . . . ?
C5 Si1 Si2 C7A 80.4(6) . . . . ?
C6 Si1 Si2 C7A -43.3(6) . . . . ?
C4 Si1 Si2 C8B 60.30(18) . . . . ?
C5 Si1 Si2 C8B -56.98(18) . . . . ?
C6 Si1 Si2 C8B 179.30(18) . . . . ?
C4 S1 C1 C2 -0.56(10) . . . . ?
C4 S1 C1 C1 179.04(13) . . . 2_666 ?
C1 C1 C2 C3 -178.99(16) 2_666 . . . ?
S1 C1 C2 C3 0.56(15) . . . . ?
C1 C2 C3 C4 -0.27(18) . . . . ?
C2 C3 C4 S1 -0.16(15) . . . . ?
C2 C3 C4 Si1 174.66(10) . . . . ?
C1 S1 C4 C3 0.40(10) . . . . ?
C1 S1 C4 Si1 -174.84(8) . . . . ?
C5 Si1 C4 C3 26.43(14) . . . . ?
C6 Si1 C4 C3 147.44(12) . . . . ?
Si2 Si1 C4 C3 -92.96(12) . . . . ?
C5 Si1 C4 S1 -159.36(8) . . . . ?
C6 Si1 C4 S1 -38.34(10) . . . . ?
Si2 Si1 C4 S1 81.26(8) . . . . ?

_diffrn_measured_fraction_theta_max 0.992
_diffrn_reflns_theta_full        27.00
_diffrn_measured_fraction_theta_full 0.992
_refine_diff_density_max         0.335
_refine_diff_density_min         -0.243
_refine_diff_density_rms         0.040
####################################################################### 
# 
# 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_z
_database_code_depnum_ccdc_archive 'CCDC 1810964'
_audit_update_record             
;
2017-12-13 deposited with the CCDC.
2018-03-14 downloaded from the CCDC.
;


_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C20 H22 Ge2 S4'
_chemical_formula_sum            'C20 H22 Ge2 S4'
_chemical_formula_weight         535.80

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'
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                   7.6171(3)
_cell_length_b                   8.9311(4)
_cell_length_c                   16.6999(7)
_cell_angle_alpha                90.00
_cell_angle_beta                 96.6462(6)
_cell_angle_gamma                90.00
_cell_volume                     1128.44(8)
_cell_formula_units_Z            2
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    8646
_cell_measurement_theta_min      2.456
_cell_measurement_theta_max      30.485

_exptl_crystal_description       prism
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.577
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             540
_exptl_absorpt_coefficient_mu    3.036
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5819
_exptl_absorpt_correction_T_max  0.7511
_exptl_absorpt_process_details   'SADABS (Bruker, 2008)'


_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  'Bruker SMART APEX II'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         .
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  .
_diffrn_standards_decay_%        0
_diffrn_reflns_number            12365
_diffrn_reflns_av_R_equivalents  0.0159
_diffrn_reflns_av_sigmaI/netI    0.0123
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         2.46
_diffrn_reflns_theta_max         29.00
_reflns_number_total             3001
_reflns_number_gt                2844
_reflns_threshold_expression     I>2σ(I)

_computing_data_collection       'APEX2 (Bruker, 2008)'
_computing_cell_refinement       'SAINT (Bruker, 2008)'
_computing_data_reduction        'SAINT (Bruker, 2008)'
_computing_structure_solution    'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXTL (Sheldrick, 2008)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'

_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)+(0.0308P)²+0.5358P] 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         3001
_refine_ls_number_parameters     120
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0200
_refine_ls_R_factor_gt           0.0187
_refine_ls_wR_factor_ref         0.0544
_refine_ls_wR_factor_gt          0.0536
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_restrained_S_all      1.070
_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
Ge1 Ge 0.438304(18) 0.598485(16) 0.456243(8) 0.01655(5) Uani 1 1 d . . .
S1 S 0.91863(6) 0.50950(5) 0.11718(2) 0.03231(10) Uani 1 1 d . . .
S2 S 0.73349(4) 0.66426(4) 0.33927(2) 0.02047(8) Uani 1 1 d . . .
C1 C 0.5116(2) 0.79171(18) 0.50324(10) 0.0293(3) Uani 1 1 d . . .
H1A H 0.4862 0.7951 0.5594 0.044 Uiso 1 1 calc R . .
H1B H 0.4467 0.8719 0.4726 0.044 Uiso 1 1 calc R . .
H1C H 0.6387 0.8052 0.5013 0.044 Uiso 1 1 calc R . .
C2 C 0.1829(2) 0.5801(2) 0.43397(11) 0.0323(4) Uani 1 1 d . . .
H2A H 0.1289 0.5973 0.4837 0.049 Uiso 1 1 calc R . .
H2B H 0.1527 0.4794 0.4136 0.049 Uiso 1 1 calc R . .
H2C H 0.1384 0.6544 0.3934 0.049 Uiso 1 1 calc R . .
C11 C 1.0987(2) 0.6111(2) 0.09854(10) 0.0335(4) Uani 1 1 d . . .
H11 H 1.1693 0.5888 0.0568 0.040 Uiso 1 1 calc R . .
C12 C 1.1292(3) 0.7274(2) 0.15017(11) 0.0387(4) Uani 1 1 d U . .
H12 H 1.2248 0.7951 0.1483 0.046 Uiso 1 1 calc R . .
C13 C 1.0042(2) 0.73949(19) 0.20805(10) 0.0296(3) Uani 1 1 d U . .
H13 H 1.0060 0.8147 0.2483 0.035 Uiso 1 1 calc R . .
C14 C 0.8781(2) 0.62312(17) 0.19626(8) 0.0212(3) Uani 1 1 d . . .
C21 C 0.7331(2) 0.59161(16) 0.24315(8) 0.0205(3) Uani 1 1 d . . .
C22 C 0.5850(2) 0.5064(2) 0.22403(9) 0.0318(4) Uani 1 1 d . . .
H22 H 0.5592 0.4560 0.1739 0.038 Uiso 1 1 calc R . .
C23 C 0.4736(2) 0.5007(2) 0.28663(9) 0.0309(4) Uani 1 1 d . . .
H23 H 0.3660 0.4460 0.2823 0.037 Uiso 1 1 calc R . .
C24 C 0.53556(18) 0.58107(16) 0.35375(8) 0.0191(3) Uani 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ge1 C2 1.9448(16) . ?
Ge1 C24 1.9484(14) . ?
Ge1 C1 1.9505(16) . ?
Ge1 Ge1 2.4075(3) 3_666 ?
S1 C11 1.7029(18) . ?
S1 C14 1.7214(15) . ?
S2 C24 1.7227(14) . ?
S2 C21 1.7309(14) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
C11 C12 1.352(3) . ?
C11 H11 0.9500 . ?
C12 C13 1.437(2) . ?
C12 H12 0.9500 . ?
C13 C14 1.413(2) . ?
C13 H13 0.9500 . ?
C14 C21 1.454(2) . ?
C21 C22 1.367(2) . ?
C22 C23 1.421(2) . ?
C22 H22 0.9500 . ?
C23 C24 1.368(2) . ?
C23 H23 0.9500 . ?

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
C2 Ge1 C24 107.39(7) . . ?
C2 Ge1 C1 112.64(8) . . ?
C24 Ge1 C1 107.69(6) . . ?
C2 Ge1 Ge1 111.47(6) . 3_666 ?
C24 Ge1 Ge1 108.27(4) . 3_666 ?
C1 Ge1 Ge1 109.20(5) . 3_666 ?
C11 S1 C14 92.61(8) . . ?
C24 S2 C21 93.48(7) . . ?
Ge1 C1 H1A 109.5 . . ?
Ge1 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
Ge1 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
Ge1 C2 H2A 109.5 . . ?
Ge1 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
Ge1 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
C12 C11 S1 112.04(13) . . ?
C12 C11 H11 124.0 . . ?
S1 C11 H11 124.0 . . ?
C11 C12 C13 114.09(16) . . ?
C11 C12 H12 123.0 . . ?
C13 C12 H12 123.0 . . ?
C14 C13 C12 110.08(14) . . ?
C14 C13 H13 125.0 . . ?
C12 C13 H13 125.0 . . ?
C13 C14 C21 127.87(13) . . ?
C13 C14 S1 111.18(11) . . ?
C21 C14 S1 120.92(11) . . ?
C22 C21 C14 129.76(14) . . ?
C22 C21 S2 109.78(11) . . ?
C14 C21 S2 120.45(11) . . ?
C21 C22 C23 113.23(14) . . ?
C21 C22 H22 123.4 . . ?
C23 C22 H22 123.4 . . ?
C24 C23 C22 113.91(14) . . ?
C24 C23 H23 123.0 . . ?
C22 C23 H23 123.0 . . ?
C23 C24 S2 109.61(11) . . ?
C23 C24 Ge1 129.16(11) . . ?
S2 C24 Ge1 121.12(8) . . ?

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
C14 S1 C11 C12 0.20(16) . . . . ?
S1 C11 C12 C13 -0.3(2) . . . . ?
C11 C12 C13 C14 0.3(2) . . . . ?
C12 C13 C14 C21 177.84(16) . . . . ?
C12 C13 C14 S1 -0.17(19) . . . . ?
C11 S1 C14 C13 -0.01(13) . . . . ?
C11 S1 C14 C21 -178.17(13) . . . . ?
C13 C14 C21 C22 162.26(18) . . . . ?
S1 C14 C21 C22 -19.9(2) . . . . ?
C13 C14 C21 S2 -18.8(2) . . . . ?
S1 C14 C21 S2 159.06(9) . . . . ?
C24 S2 C21 C22 -0.14(13) . . . . ?
C24 S2 C21 C14 -179.29(12) . . . . ?
C14 C21 C22 C23 179.17(16) . . . . ?
S2 C21 C22 C23 0.1(2) . . . . ?
C21 C22 C23 C24 0.0(2) . . . . ?
C22 C23 C24 S2 -0.07(19) . . . . ?
C22 C23 C24 Ge1 -176.22(13) . . . . ?
C21 S2 C24 C23 0.12(13) . . . . ?
C21 S2 C24 Ge1 176.63(9) . . . . ?
C2 Ge1 C24 C23 -31.33(17) . . . . ?
C1 Ge1 C24 C23 -152.89(15) . . . . ?
Ge1 Ge1 C24 C23 89.15(15) 3_666 . . . ?
C2 Ge1 C24 S2 152.91(9) . . . . ?
C1 Ge1 C24 S2 31.35(11) . . . . ?
Ge1 Ge1 C24 S2 -86.60(8) 3_666 . . . ?

_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        29.00
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         0.583
_refine_diff_density_min         -0.551
_refine_diff_density_rms         0.066
####################################################################### 
# 
# 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_CCDC1
_database_code_depnum_ccdc_archive 'CCDC 1810963'
_audit_update_record             
;
2017-12-13 deposited with the CCDC.
2018-03-14 downloaded from the CCDC.
;


_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C20 H22 S4 Si2'
_chemical_formula_sum            'C20 H22 S4 Si2'
_chemical_formula_weight         446.80

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'
Si Si 0.0817 0.0704 '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   '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                   7.6131(4)
_cell_length_b                   8.7828(4)
_cell_length_c                   16.7001(8)
_cell_angle_alpha                90.00
_cell_angle_beta                 95.931(1)
_cell_angle_gamma                90.00
_cell_volume                     1110.66(9)
_cell_formula_units_Z            2
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    7958
_cell_measurement_theta_min      2.453
_cell_measurement_theta_max      30.475

_exptl_crystal_description       prism
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.336
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             468
_exptl_absorpt_coefficient_mu    0.539
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8771
_exptl_absorpt_correction_T_max  0.8999
_exptl_absorpt_process_details   'SADABS (Bruker, 2008)'

_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  'Bruker SMART APEX II'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         .
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  .
_diffrn_standards_decay_%        0
_diffrn_reflns_number            12179
_diffrn_reflns_av_R_equivalents  0.0155
_diffrn_reflns_av_sigmaI/netI    0.0126
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         2.45
_diffrn_reflns_theta_max         29.00
_reflns_number_total             2951
_reflns_number_gt                2732
_reflns_threshold_expression     I>2σ(I)

_computing_data_collection       'APEX2 (Bruker, 2008)'
_computing_cell_refinement       'SAINT (Bruker, 2008)'
_computing_data_reduction        'SAINT (Bruker, 2008)'
_computing_structure_solution    'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXTL (Sheldrick, 2008)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'

_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)+(0.0473P)²+0.5675P] 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         2951
_refine_ls_number_parameters     120
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0307
_refine_ls_R_factor_gt           0.0284
_refine_ls_wR_factor_ref         0.0860
_refine_ls_wR_factor_gt          0.0838
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_restrained_S_all      1.076
_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
Si1 Si 0.43832(4) 0.59609(4) 0.45739(2) 0.01742(10) Uani 1 1 d . . .
S1 S 0.90863(5) 0.51313(5) 0.11619(2) 0.03208(11) Uani 1 1 d . . .
S2 S 0.73215(4) 0.66233(4) 0.343052(19) 0.02107(10) Uani 1 1 d . . .
C1 C 0.5042(2) 0.78551(17) 0.50266(9) 0.0277(3) Uani 1 1 d . . .
H1A H 0.4697 0.7909 0.5575 0.042 Uiso 1 1 calc R . .
H1B H 0.4449 0.8668 0.4700 0.042 Uiso 1 1 calc R . .
H1C H 0.6324 0.7979 0.5042 0.042 Uiso 1 1 calc R . .
C2 C 0.19369(18) 0.5730(2) 0.43875(10) 0.0306(3) Uani 1 1 d . . .
H2A H 0.1413 0.5837 0.4896 0.046 Uiso 1 1 calc R . .
H2B H 0.1661 0.4719 0.4160 0.046 Uiso 1 1 calc R . .
H2C H 0.1453 0.6512 0.4009 0.046 Uiso 1 1 calc R . .
C11 C 1.0942(2) 0.6119(2) 0.09895(9) 0.0324(3) Uani 1 1 d . . .
H11 H 1.1637 0.5900 0.0563 0.039 Uiso 1 1 calc R . .
C12 C 1.1306(2) 0.7250(2) 0.15312(11) 0.0381(4) Uani 1 1 d U . .
H12 H 1.2292 0.7911 0.1523 0.046 Uiso 1 1 calc R . .
C13 C 1.0062(2) 0.73596(19) 0.21208(9) 0.0306(3) Uani 1 1 d U . .
H13 H 1.0119 0.8089 0.2542 0.037 Uiso 1 1 calc R . .
C14 C 0.87486(18) 0.62334(16) 0.19853(8) 0.0211(3) Uani 1 1 d . . .
C21 C 0.72892(18) 0.59246(15) 0.24609(8) 0.0206(3) Uani 1 1 d . . .
C22 C 0.5786(2) 0.50905(19) 0.22662(9) 0.0297(3) Uani 1 1 d . . .
H22 H 0.5514 0.4604 0.1760 0.036 Uiso 1 1 calc R . .
C23 C 0.4675(2) 0.50273(19) 0.28988(9) 0.0290(3) Uani 1 1 d . . .
H23 H 0.3584 0.4492 0.2854 0.035 Uiso 1 1 calc R . .
C24 C 0.53157(17) 0.58096(15) 0.35822(8) 0.0195(2) 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
Si1 C2 1.8673(14) . ?
Si1 C24 1.8730(13) . ?
Si1 C1 1.8741(15) . ?
Si1 Si1 2.3409(7) 3_666 ?
S1 C11 1.7072(17) . ?
S1 C14 1.7225(14) . ?
S2 C24 1.7282(13) . ?
S2 C21 1.7295(13) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
C11 C12 1.353(2) . ?
C11 H11 0.9500 . ?
C12 C13 1.438(2) . ?
C12 H12 0.9500 . ?
C13 C14 1.408(2) . ?
C13 H13 0.9500 . ?
C14 C21 1.4564(18) . ?
C21 C22 1.369(2) . ?
C22 C23 1.421(2) . ?
C22 H22 0.9500 . ?
C23 C24 1.3775(19) . ?
C23 H23 0.9500 . ?

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
C2 Si1 C24 107.91(7) . . ?
C2 Si1 C1 112.61(7) . . ?
C24 Si1 C1 108.04(6) . . ?
C2 Si1 Si1 110.71(6) . 3_666 ?
C24 Si1 Si1 108.75(5) . 3_666 ?
C1 Si1 Si1 108.73(5) . 3_666 ?
C11 S1 C14 92.49(7) . . ?
C24 S2 C21 93.62(6) . . ?
Si1 C1 H1A 109.5 . . ?
Si1 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
Si1 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
Si1 C2 H2A 109.5 . . ?
Si1 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
Si1 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
C12 C11 S1 112.11(12) . . ?
C12 C11 H11 123.9 . . ?
S1 C11 H11 123.9 . . ?
C11 C12 C13 113.76(15) . . ?
C11 C12 H12 123.1 . . ?
C13 C12 H12 123.1 . . ?
C14 C13 C12 110.48(14) . . ?
C14 C13 H13 124.8 . . ?
C12 C13 H13 124.8 . . ?
C13 C14 C21 127.76(12) . . ?
C13 C14 S1 111.15(10) . . ?
C21 C14 S1 121.06(11) . . ?
C22 C21 C14 129.50(13) . . ?
C22 C21 S2 110.05(10) . . ?
C14 C21 S2 120.44(10) . . ?
C21 C22 C23 113.05(13) . . ?
C21 C22 H22 123.5 . . ?
C23 C22 H22 123.5 . . ?
C24 C23 C22 114.16(13) . . ?
C24 C23 H23 122.9 . . ?
C22 C23 H23 122.9 . . ?
C23 C24 S2 109.12(10) . . ?
C23 C24 Si1 129.33(10) . . ?
S2 C24 Si1 121.44(7) . . ?

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
C14 S1 C11 C12 -0.14(15) . . . . ?
S1 C11 C12 C13 0.0(2) . . . . ?
C11 C12 C13 C14 0.2(2) . . . . ?
C12 C13 C14 C21 177.72(15) . . . . ?
C12 C13 C14 S1 -0.28(18) . . . . ?
C11 S1 C14 C13 0.24(13) . . . . ?
C11 S1 C14 C21 -177.91(12) . . . . ?
C13 C14 C21 C22 164.08(16) . . . . ?
S1 C14 C21 C22 -18.1(2) . . . . ?
C13 C14 C21 S2 -17.2(2) . . . . ?
S1 C14 C21 S2 160.60(8) . . . . ?
C24 S2 C21 C22 -0.22(12) . . . . ?
C24 S2 C21 C14 -179.15(11) . . . . ?
C14 C21 C22 C23 178.99(14) . . . . ?
S2 C21 C22 C23 0.20(18) . . . . ?
C21 C22 C23 C24 -0.1(2) . . . . ?
C22 C23 C24 S2 -0.12(17) . . . . ?
C22 C23 C24 Si1 -176.45(12) . . . . ?
C21 S2 C24 C23 0.19(11) . . . . ?
C21 S2 C24 Si1 176.87(8) . . . . ?
C2 Si1 C24 C23 -28.12(16) . . . . ?
C1 Si1 C24 C23 -150.13(14) . . . . ?
Si1 Si1 C24 C23 92.02(14) 3_666 . . . ?
C2 Si1 C24 S2 155.94(9) . . . . ?
C1 Si1 C24 S2 33.92(10) . . . . ?
Si1 Si1 C24 S2 -83.92(8) 3_666 . . . ?

_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        29.00
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         0.531
_refine_diff_density_min         -0.511
_refine_diff_density_rms         0.063
####################################################################### 
# 
# 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_p-1
_database_code_depnum_ccdc_archive 'CCDC 1810962'
_audit_update_record             
;
2017-12-13 deposited with the CCDC.
2018-03-14 downloaded from the CCDC.
;
_audit_creation_date             2016-01-19
_audit_creation_method           
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_chemical_name_common            ?
_chemical_name_systematic        
;
 ? 
;
_chemical_formula_moiety         'C18 H34 Ge4 S2'
_chemical_formula_sum            'C18 H34 Ge4 S2'
_chemical_formula_weight         604.93
_chemical_melting_point          ?
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'
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'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 'x, y, z'
2 '-x, -y, -z'

_cell_length_a                   6.7760(10)
_cell_length_b                   8.4190(13)
_cell_length_c                   12.5300(19)
_cell_angle_alpha                90.805(2)
_cell_angle_beta                 94.883(2)
_cell_angle_gamma                112.136(2)
_cell_volume                     658.89(17)
_cell_formula_units_Z            1
_cell_measurement_reflns_used    3385
_cell_measurement_temperature    170
_cell_measurement_theta_max      30.248
_cell_measurement_theta_min      2.615
_exptl_absorpt_coefficient_mu    4.676
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.5588
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0994 before and 0.0260 after correction.
The Ratio of minimum to maximum transmission is 0.7490.
The λ/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.525
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             302
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.26
_exptl_special_details           
;
 ? 
;
_diffrn_reflns_av_R_equivalents  0.0173
_diffrn_reflns_av_unetI/netI     0.0256
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            7182
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         29.00
_diffrn_reflns_theta_min         2.62
_diffrn_ambient_temperature      170
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_decay_%        ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_number         ?
_reflns_number_gt                2883
_reflns_number_total             3464
_reflns_threshold_expression     >2sigma(I)
_computing_cell_refinement       'SAINT v7.60A (Bruker, 2009)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT v7.60A (Bruker, 2009)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XH (Sheldrick, 2008)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_refine_diff_density_max         1.204
_refine_diff_density_min         -0.466
_refine_diff_density_rms         0.100
_refine_ls_extinction_coef       ?
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.099
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     114
_refine_ls_number_reflns         3464
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0408
_refine_ls_R_factor_gt           0.0302
_refine_ls_restrained_S_all      1.099
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0486P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0782
_refine_ls_wR_factor_ref         0.0814
_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. 
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3)
2.b Idealised Me refined as rotating group:
 C5(H5A,H5B,H5C), C6(H6A,H6B,H6C), C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C9(H9A,
 H9B,H9C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
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_calc_flag
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_refinement_flags_posn
Ge1 Ge 0.26349(4) 0.74446(3) 0.323418(19) 0.02551(8) Uani 1 d . . .
Ge2 Ge 0.21787(4) 0.46703(3) 0.24623(2) 0.03040(9) Uani 1 d . . .
S1 S -0.03203(9) 0.84566(8) 0.14204(5) 0.03083(14) Uani 1 d . . .
C1 C 0.2178(4) 0.8742(3) 0.20259(19) 0.0264(5) Uani 1 d . . .
C2 C 0.3712(4) 0.9850(3) 0.1462(2) 0.0331(5) Uani 1 d . . .
H2 H 0.5200 1.0177 0.1663 0.040 Uiso 1 calc . . R
C3 C 0.2900(4) 1.0471(3) 0.0551(2) 0.0328(5) Uani 1 d . . .
H3 H 0.3783 1.1251 0.0086 0.039 Uiso 1 calc . . R
C4 C 0.0705(4) 0.9828(3) 0.04108(19) 0.0256(5) Uani 1 d . . .
C5 C 0.0595(5) 0.7346(4) 0.4263(2) 0.0414(6) Uani 1 d . . .
H5A H -0.0860 0.6665 0.3944 0.062 Uiso 1 calc . . GR
H5B H 0.0705 0.8512 0.4452 0.062 Uiso 1 calc . . GR
H5C H 0.0914 0.6812 0.4910 0.062 Uiso 1 calc . . GR
C6 C 0.5575(4) 0.8765(4) 0.3840(2) 0.0380(6) Uani 1 d . . .
H6A H 0.5859 0.8292 0.4520 0.057 Uiso 1 calc . . GR
H6B H 0.5763 0.9967 0.3968 0.057 Uiso 1 calc . . GR
H6C H 0.6574 0.8699 0.3337 0.057 Uiso 1 calc . . GR
C7 C -0.0836(5) 0.3268(4) 0.2137(3) 0.0623(10) Uani 1 d . . .
H7A H -0.1519 0.2996 0.2806 0.094 Uiso 1 calc . . GR
H7B H -0.0992 0.2201 0.1751 0.094 Uiso 1 calc . . GR
H7C H -0.1523 0.3897 0.1690 0.094 Uiso 1 calc . . GR
C8 C 0.3522(6) 0.5078(4) 0.1128(3) 0.0531(8) Uani 1 d . . .
H8A H 0.2742 0.5560 0.0621 0.080 Uiso 1 calc . . GR
H8B H 0.3493 0.3991 0.0821 0.080 Uiso 1 calc . . GR
H8C H 0.5010 0.5887 0.1270 0.080 Uiso 1 calc . . GR
C9 C 0.3507(7) 0.3476(5) 0.3424(3) 0.0645(10) Uani 1 d . . .
H9A H 0.5011 0.4212 0.3621 0.097 Uiso 1 calc . . GR
H9B H 0.3424 0.2411 0.3061 0.097 Uiso 1 calc . . GR
H9C H 0.2753 0.3205 0.4072 0.097 Uiso 1 calc . . GR


_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 Ge2 2.4141(5) . ?
Ge1 C1 1.950(2) . ?
Ge1 C5 1.949(3) . ?
Ge1 C6 1.957(3) . ?
Ge2 C7 1.939(3) . ?
Ge2 C8 1.944(3) . ?
Ge2 C9 1.950(3) . ?
S1 C1 1.723(2) . ?
S1 C4 1.733(2) . ?
C1 C2 1.365(3) . ?
C2 H2 0.9500 . ?
C2 C3 1.416(4) . ?
C3 H3 0.9500 . ?
C3 C4 1.372(3) . ?
C4 C4 1.452(5) 2_575 ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?

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
C1 Ge1 Ge2 105.24(7) . . ?
C1 Ge1 C6 104.46(11) . . ?
C5 Ge1 Ge2 113.70(9) . . ?
C5 Ge1 C1 108.73(11) . . ?
C5 Ge1 C6 111.09(13) . . ?
C6 Ge1 Ge2 112.93(9) . . ?
C7 Ge2 Ge1 110.50(11) . . ?
C7 Ge2 C8 108.55(16) . . ?
C7 Ge2 C9 109.48(17) . . ?
C8 Ge2 Ge1 106.80(9) . . ?
C8 Ge2 C9 110.13(16) . . ?
C9 Ge2 Ge1 111.32(11) . . ?
C1 S1 C4 93.37(11) . . ?
S1 C1 Ge1 123.34(13) . . ?
C2 C1 Ge1 126.81(18) . . ?
C2 C1 S1 109.51(18) . . ?
C1 C2 H2 122.8 . . ?
C1 C2 C3 114.4(2) . . ?
C3 C2 H2 122.8 . . ?
C2 C3 H3 123.5 . . ?
C4 C3 C2 112.9(2) . . ?
C4 C3 H3 123.5 . . ?
C3 C4 S1 109.78(18) . . ?
C3 C4 C4 129.3(3) . 2_575 ?
C4 C4 S1 120.9(2) 2_575 . ?
Ge1 C5 H5A 109.5 . . ?
Ge1 C5 H5B 109.5 . . ?
Ge1 C5 H5C 109.5 . . ?
H5A C5 H5B 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
Ge1 C6 H6A 109.5 . . ?
Ge1 C6 H6B 109.5 . . ?
Ge1 C6 H6C 109.5 . . ?
H6A C6 H6B 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
Ge2 C7 H7A 109.5 . . ?
Ge2 C7 H7B 109.5 . . ?
Ge2 C7 H7C 109.5 . . ?
H7A C7 H7B 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
Ge2 C8 H8A 109.5 . . ?
Ge2 C8 H8B 109.5 . . ?
Ge2 C8 H8C 109.5 . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
Ge2 C9 H9A 109.5 . . ?
Ge2 C9 H9B 109.5 . . ?
Ge2 C9 H9C 109.5 . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 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
Ge1 C1 C2 C3 173.51(18) . . . . ?
Ge2 Ge1 C1 S1 77.69(14) . . . . ?
Ge2 Ge1 C1 C2 -94.9(2) . . . . ?
S1 C1 C2 C3 0.1(3) . . . . ?
C1 Ge1 Ge2 C7 -77.88(15) . . . . ?
C1 Ge1 Ge2 C8 40.00(14) . . . . ?
C1 Ge1 Ge2 C9 160.25(15) . . . . ?
C1 S1 C4 C3 0.0(2) . . . . ?
C1 S1 C4 C4 -179.1(3) . . . 2_575 ?
C1 C2 C3 C4 -0.1(3) . . . . ?
C2 C3 C4 S1 0.1(3) . . . . ?
C2 C3 C4 C4 179.1(3) . . . 2_575 ?
C4 S1 C1 Ge1 -173.73(14) . . . . ?
C4 S1 C1 C2 0.0(2) . . . . ?
C5 Ge1 Ge2 C7 41.00(17) . . . . ?
C5 Ge1 Ge2 C8 158.89(15) . . . . ?
C5 Ge1 Ge2 C9 -80.87(16) . . . . ?
C5 Ge1 C1 S1 -44.46(18) . . . . ?
C5 Ge1 C1 C2 143.0(2) . . . . ?
C6 Ge1 Ge2 C7 168.77(16) . . . . ?
C6 Ge1 Ge2 C8 -73.35(15) . . . . ?
C6 Ge1 Ge2 C9 46.90(16) . . . . ?
C6 Ge1 C1 S1 -163.14(15) . . . . ?
C6 Ge1 C1 C2 24.3(2) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
