# 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_1093j
_audit_block_doi                 10.5517/ccdc.csd.cc1kp3w7
_database_code_depnum_ccdc_archive 'CCDC 1450269'
loop_
_citation_id
_citation_doi
_citation_year
1 10.1021/acs.organomet.6b00482 2016
_audit_update_record             
;
2016-01-27 deposited with the CCDC.
2018-03-23 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C30 H58 Ge Si8'
_chemical_formula_weight         716.07

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'
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   C2/c

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

_cell_length_a                   13.843(3)
_cell_length_b                   17.869(4)
_cell_length_c                   17.503(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 101.50(3)
_cell_angle_gamma                90.00
_cell_volume                     4242.5(15)
_cell_formula_units_Z            4
_cell_measurement_temperature    200(2)
_cell_measurement_reflns_used    4237
_cell_measurement_theta_min      4.734
_cell_measurement_theta_max      51.200

_exptl_crystal_description       blocks
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.121
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1528
_exptl_absorpt_coefficient_mu    0.966
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7225
_exptl_absorpt_correction_T_max  0.8303
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      200(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  'SMART APEX'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            14538
_diffrn_reflns_av_R_equivalents  0.0618
_diffrn_reflns_av_sigmaI/netI    0.0659
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         1.88
_diffrn_reflns_theta_max         26.37
_reflns_number_total             4326
_reflns_number_gt                3428
_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)+(0.0478P)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         4326
_refine_ls_number_parameters     185
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0557
_refine_ls_R_factor_gt           0.0439
_refine_ls_wR_factor_ref         0.1073
_refine_ls_wR_factor_gt          0.1023
_refine_ls_goodness_of_fit_ref   0.984
_refine_ls_restrained_S_all      0.984
_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 0.5000 0.245308(19) 0.2500 0.03562(13) Uani 1 2 d S . .
Si1 Si 0.61339(5) 0.17247(4) 0.19486(4) 0.03703(18) Uani 1 1 d . . .
Si2 Si 0.57852(5) 0.05102(4) 0.23298(4) 0.0418(2) Uani 1 1 d . . .
Si3 Si 0.56391(5) 0.18845(4) 0.05965(4) 0.0448(2) Uani 1 1 d . . .
Si4 Si 0.77553(6) 0.21254(6) 0.23994(5) 0.0610(3) Uani 1 1 d . . .
C1 C 0.47248(18) 0.34851(13) 0.21478(14) 0.0400(6) Uani 1 1 d . . .
C2 C 0.43424(18) 0.40155(14) 0.15263(14) 0.0401(6) Uani 1 1 d . . .
C3 C 0.3502(2) 0.38678(17) 0.09756(15) 0.0556(7) Uani 1 1 d . . .
H3 H 0.3151 0.3415 0.1006 0.067 Uiso 1 1 calc R . .
C4 C 0.3163(2) 0.43682(19) 0.03810(17) 0.0665(9) Uani 1 1 d . . .
H4 H 0.2571 0.4266 0.0017 0.080 Uiso 1 1 calc R . .
C5 C 0.3679(2) 0.50118(18) 0.03139(17) 0.0625(8) Uani 1 1 d . . .
H5 H 0.3454 0.5350 -0.0102 0.075 Uiso 1 1 calc R . .
C6 C 0.4521(2) 0.51643(16) 0.08512(16) 0.0601(8) Uani 1 1 d . . .
H6 H 0.4881 0.5609 0.0806 0.072 Uiso 1 1 calc R . .
C7 C 0.4848(2) 0.46738(15) 0.14584(16) 0.0510(7) Uani 1 1 d . . .
H7 H 0.5426 0.4789 0.1833 0.061 Uiso 1 1 calc R . .
C8 C 0.5787(2) -0.01893(15) 0.15240(16) 0.0608(8) Uani 1 1 d . . .
H8A H 0.6449 -0.0218 0.1406 0.091 Uiso 1 1 calc R . .
H8B H 0.5317 -0.0031 0.1057 0.091 Uiso 1 1 calc R . .
H8C H 0.5596 -0.0682 0.1690 0.091 Uiso 1 1 calc R . .
C9 C 0.6727(2) 0.01947(17) 0.32008(16) 0.0615(8) Uani 1 1 d . . .
H9A H 0.6555 -0.0306 0.3358 0.092 Uiso 1 1 calc R . .
H9B H 0.6736 0.0545 0.3633 0.092 Uiso 1 1 calc R . .
H9C H 0.7380 0.0181 0.3065 0.092 Uiso 1 1 calc R . .
C10 C 0.6370(2) 0.12805(19) 0.00465(16) 0.0662(9) Uani 1 1 d . . .
H10A H 0.6253 0.0753 0.0150 0.099 Uiso 1 1 calc R . .
H10B H 0.7073 0.1393 0.0215 0.099 Uiso 1 1 calc R . .
H10C H 0.6167 0.1379 -0.0513 0.099 Uiso 1 1 calc R . .
C11 C 0.5788(3) 0.28803(18) 0.03173(18) 0.0685(9) Uani 1 1 d . . .
H11A H 0.5542 0.2941 -0.0244 0.103 Uiso 1 1 calc R . .
H11B H 0.6488 0.3017 0.0446 0.103 Uiso 1 1 calc R . .
H11C H 0.5414 0.3205 0.0603 0.103 Uiso 1 1 calc R . .
C12 C 0.4312(2) 0.16206(18) 0.02990(17) 0.0656(9) Uani 1 1 d . . .
H12A H 0.4093 0.1698 -0.0263 0.098 Uiso 1 1 calc R . .
H12B H 0.3916 0.1933 0.0580 0.098 Uiso 1 1 calc R . .
H12C H 0.4229 0.1093 0.0424 0.098 Uiso 1 1 calc R . .
C13 C 0.8172(2) 0.1988(2) 0.34707(18) 0.0817(11) Uani 1 1 d . . .
H13A H 0.8270 0.1453 0.3584 0.123 Uiso 1 1 calc R . .
H13B H 0.7671 0.2184 0.3742 0.123 Uiso 1 1 calc R . .
H13C H 0.8794 0.2256 0.3650 0.123 Uiso 1 1 calc R . .
C14 C 0.8591(3) 0.1593(4) 0.1887(3) 0.151(3) Uani 1 1 d . . .
H14A H 0.9272 0.1758 0.2076 0.227 Uiso 1 1 calc R . .
H14B H 0.8403 0.1684 0.1325 0.227 Uiso 1 1 calc R . .
H14C H 0.8537 0.1057 0.1991 0.227 Uiso 1 1 calc R . .
C15 C 0.7832(4) 0.3140(2) 0.2195(3) 0.1229(18) Uani 1 1 d . . .
H15A H 0.7344 0.3411 0.2425 0.184 Uiso 1 1 calc R . .
H15B H 0.7698 0.3221 0.1630 0.184 Uiso 1 1 calc R . .
H15C H 0.8494 0.3323 0.2422 0.184 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 C1 1.958(2) 2_655 ?
Ge1 C1 1.958(2) . ?
Ge1 Si1 2.3861(8) . ?
Ge1 Si1 2.3861(8) 2_655 ?
Si1 Si4 2.3381(12) . ?
Si1 Si3 2.3461(11) . ?
Si1 Si2 2.3488(11) . ?
Si2 C9 1.884(3) . ?
Si2 C8 1.885(3) . ?
Si2 Si2 2.3660(16) 2_655 ?
Si3 C11 1.868(3) . ?
Si3 C12 1.868(3) . ?
Si3 C10 1.872(3) . ?
Si4 C15 1.855(4) . ?
Si4 C14 1.859(4) . ?
Si4 C13 1.865(3) . ?
C1 C1 1.314(5) 2_655 ?
C1 C2 1.460(3) . ?
C2 C3 1.380(3) . ?
C2 C7 1.386(4) . ?
C3 C4 1.381(4) . ?
C4 C5 1.371(4) . ?
C5 C6 1.371(4) . ?
C6 C7 1.382(4) . ?

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 C1 39.21(13) 2_655 . ?
C1 Ge1 Si1 122.60(8) 2_655 . ?
C1 Ge1 Si1 119.27(8) . . ?
C1 Ge1 Si1 119.27(8) 2_655 2_655 ?
C1 Ge1 Si1 122.61(8) . 2_655 ?
Si1 Ge1 Si1 113.88(4) . 2_655 ?
Si4 Si1 Si3 111.75(5) . . ?
Si4 Si1 Si2 115.14(4) . . ?
Si3 Si1 Si2 111.34(4) . . ?
Si4 Si1 Ge1 111.17(4) . . ?
Si3 Si1 Ge1 104.97(4) . . ?
Si2 Si1 Ge1 101.54(4) . . ?
C9 Si2 C8 107.65(14) . . ?
C9 Si2 Si1 110.99(10) . . ?
C8 Si2 Si1 111.66(10) . . ?
C9 Si2 Si2 108.57(11) . 2_655 ?
C8 Si2 Si2 109.08(11) . 2_655 ?
Si1 Si2 Si2 108.83(3) . 2_655 ?
C11 Si3 C12 108.76(15) . . ?
C11 Si3 C10 108.38(15) . . ?
C12 Si3 C10 108.29(15) . . ?
C11 Si3 Si1 110.77(11) . . ?
C12 Si3 Si1 108.88(11) . . ?
C10 Si3 Si1 111.69(10) . . ?
C15 Si4 C14 110.0(3) . . ?
C15 Si4 C13 107.71(18) . . ?
C14 Si4 C13 108.7(2) . . ?
C15 Si4 Si1 108.78(15) . . ?
C14 Si4 Si1 109.16(14) . . ?
C13 Si4 Si1 112.50(12) . . ?
C1 C1 C2 139.06(14) 2_655 . ?
C1 C1 Ge1 70.39(7) 2_655 . ?
C2 C1 Ge1 149.87(18) . . ?
C3 C2 C7 118.2(2) . . ?
C3 C2 C1 121.7(2) . . ?
C7 C2 C1 120.0(2) . . ?
C2 C3 C4 121.0(3) . . ?
C5 C4 C3 120.2(3) . . ?
C4 C5 C6 119.6(3) . . ?
C5 C6 C7 120.3(3) . . ?
C6 C7 C2 120.7(3) . . ?

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
C1 Ge1 Si1 Si4 26.55(9) 2_655 . . . ?
C1 Ge1 Si1 Si4 72.45(9) . . . . ?
Si1 Ge1 Si1 Si4 -130.08(4) 2_655 . . . ?
C1 Ge1 Si1 Si3 -94.44(9) 2_655 . . . ?
C1 Ge1 Si1 Si3 -48.54(8) . . . . ?
Si1 Ge1 Si1 Si3 108.93(3) 2_655 . . . ?
C1 Ge1 Si1 Si2 149.51(8) 2_655 . . . ?
C1 Ge1 Si1 Si2 -164.59(8) . . . . ?
Si1 Ge1 Si1 Si2 -7.114(18) 2_655 . . . ?
Si4 Si1 Si2 C9 19.55(12) . . . . ?
Si3 Si1 Si2 C9 148.08(11) . . . . ?
Ge1 Si1 Si2 C9 -100.65(11) . . . . ?
Si4 Si1 Si2 C8 -100.57(12) . . . . ?
Si3 Si1 Si2 C8 27.96(12) . . . . ?
Ge1 Si1 Si2 C8 139.23(11) . . . . ?
Si4 Si1 Si2 Si2 138.97(5) . . . 2_655 ?
Si3 Si1 Si2 Si2 -92.50(6) . . . 2_655 ?
Ge1 Si1 Si2 Si2 18.77(5) . . . 2_655 ?
Si4 Si1 Si3 C11 -56.15(13) . . . . ?
Si2 Si1 Si3 C11 173.54(12) . . . . ?
Ge1 Si1 Si3 C11 64.46(12) . . . . ?
Si4 Si1 Si3 C12 -175.70(12) . . . . ?
Si2 Si1 Si3 C12 53.98(12) . . . . ?
Ge1 Si1 Si3 C12 -55.09(12) . . . . ?
Si4 Si1 Si3 C10 64.77(12) . . . . ?
Si2 Si1 Si3 C10 -65.54(12) . . . . ?
Ge1 Si1 Si3 C10 -174.62(12) . . . . ?
Si3 Si1 Si4 C15 61.73(17) . . . . ?
Si2 Si1 Si4 C15 -169.95(17) . . . . ?
Ge1 Si1 Si4 C15 -55.19(17) . . . . ?
Si3 Si1 Si4 C14 -58.3(2) . . . . ?
Si2 Si1 Si4 C14 70.0(2) . . . . ?
Ge1 Si1 Si4 C14 -175.2(2) . . . . ?
Si3 Si1 Si4 C13 -179.01(13) . . . . ?
Si2 Si1 Si4 C13 -50.70(14) . . . . ?
Ge1 Si1 Si4 C13 64.06(14) . . . . ?
Si1 Ge1 C1 C1 -106.9(2) . . . 2_655 ?
Si1 Ge1 C1 C1 97.7(2) 2_655 . . 2_655 ?
C1 Ge1 C1 C2 169.7(6) 2_655 . . . ?
Si1 Ge1 C1 C2 62.8(4) . . . . ?
Si1 Ge1 C1 C2 -92.6(4) 2_655 . . . ?
C1 C1 C2 C3 -155.8(4) 2_655 . . . ?
Ge1 C1 C2 C3 39.1(5) . . . . ?
C1 C1 C2 C7 26.9(6) 2_655 . . . ?
Ge1 C1 C2 C7 -138.2(3) . . . . ?
C7 C2 C3 C4 -1.1(4) . . . . ?
C1 C2 C3 C4 -178.5(3) . . . . ?
C2 C3 C4 C5 2.1(5) . . . . ?
C3 C4 C5 C6 -1.5(5) . . . . ?
C4 C5 C6 C7 -0.2(5) . . . . ?
C5 C6 C7 C2 1.2(4) . . . . ?
C3 C2 C7 C6 -0.5(4) . . . . ?
C1 C2 C7 C6 176.9(2) . . . . ?

_diffrn_measured_fraction_theta_max 0.994
_diffrn_reflns_theta_full        26.37
_diffrn_measured_fraction_theta_full 0.994
_refine_diff_density_max         0.701
_refine_diff_density_min         -0.303
_refine_diff_density_rms         0.071

# SQUEEZE RESULTS (APPEND TO CIF)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.000 0.313 0.250 50 0 ' '
2 0.000 0.687 0.750 50 0 ' '
3 0.250 0.250 0.000 9 0 ' '
4 0.250 0.750 0.500 9 0 ' '
5 0.500 0.813 0.250 50 0 ' '
6 0.500 0.187 0.750 50 0 ' '
7 0.750 0.750 0.000 9 0 ' '
8 0.750 0.250 0.500 9 0 ' '
_platon_squeeze_details          
;
;

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

data_1125j
_database_code_depnum_ccdc_archive 'CCDC 1450272'
_audit_update_record             
;
2016-01-27 deposited with the CCDC.
2018-03-23 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C32 H60 Ge3 Si6'
_chemical_formula_weight         831.11

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'
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   P2(1)/n

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

_cell_length_a                   9.7468(19)
_cell_length_b                   27.980(6)
_cell_length_c                   16.054(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 98.41(3)
_cell_angle_gamma                90.00
_cell_volume                     4331.2(15)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    12314
_cell_measurement_theta_min      4.454
_cell_measurement_theta_max      52.522

_exptl_crystal_description       blocks
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.275
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1728
_exptl_absorpt_coefficient_mu    2.254
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5324
_exptl_absorpt_correction_T_max  0.8060
_exptl_absorpt_process_details   SADABS

_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  'SMART APEX'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            33865
_diffrn_reflns_av_R_equivalents  0.0508
_diffrn_reflns_av_sigmaI/netI    0.0513
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         1.46
_diffrn_reflns_theta_max         26.37
_reflns_number_total             8800
_reflns_number_gt                7207
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker XSCANS'
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_reduction        'Bruker SHELXTL'
_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)+(0.0451P)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         8800
_refine_ls_number_parameters     386
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0543
_refine_ls_R_factor_gt           0.0423
_refine_ls_wR_factor_ref         0.0826
_refine_ls_wR_factor_gt          0.0791
_refine_ls_goodness_of_fit_ref   0.974
_refine_ls_restrained_S_all      0.974
_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 0.87522(3) 0.133985(10) 0.623457(18) 0.01420(8) Uani 1 1 d . . .
Ge2 Ge 0.96986(3) 0.215792(10) 0.645688(19) 0.01706(8) Uani 1 1 d . . .
Ge3 Ge 0.74682(3) 0.075999(10) 0.812042(18) 0.01566(8) Uani 1 1 d . . .
Si2 Si 0.99359(7) 0.06026(3) 0.65985(5) 0.01608(17) Uani 1 1 d . . .
Si1 Si 0.98540(7) 0.05954(3) 0.80401(5) 0.01663(17) Uani 1 1 d . . .
Si6 Si 0.81645(8) 0.28177(3) 0.65818(5) 0.02410(19) Uani 1 1 d . . .
Si5 Si 1.20355(8) 0.23159(3) 0.70763(5) 0.02038(18) Uani 1 1 d . . .
Si3 Si 0.72521(8) 0.13072(3) 0.92295(5) 0.02174(18) Uani 1 1 d . . .
Si4 Si 0.62403(8) 0.00342(3) 0.82851(5) 0.02037(18) Uani 1 1 d . . .
C3 C 0.5705(3) 0.13270(10) 0.56481(18) 0.0183(6) Uani 1 1 d . . .
C8 C 0.5697(3) 0.17663(10) 0.52377(19) 0.0243(7) Uani 1 1 d . . .
H8 H 0.6396 0.1995 0.5421 0.029 Uiso 1 1 calc R . .
C4 C 0.4683(3) 0.09940(11) 0.53525(18) 0.0232(7) Uani 1 1 d . . .
H4 H 0.4674 0.0691 0.5619 0.028 Uiso 1 1 calc R . .
C7 C 0.4685(3) 0.18720(12) 0.4568(2) 0.0342(8) Uani 1 1 d . . .
H7 H 0.4683 0.2175 0.4299 0.041 Uiso 1 1 calc R . .
C6 C 0.3674(3) 0.15392(14) 0.4286(2) 0.0403(9) Uani 1 1 d . . .
H6 H 0.2978 0.1613 0.3826 0.048 Uiso 1 1 calc R . .
C5 C 0.3679(3) 0.11011(12) 0.4674(2) 0.0336(8) Uani 1 1 d . . .
H5 H 0.2992 0.0871 0.4476 0.040 Uiso 1 1 calc R . .
C1 C 0.6794(3) 0.12104(9) 0.63783(18) 0.0161(6) Uani 1 1 d . . .
C11 C 0.8842(3) 0.13203(9) 0.42840(17) 0.0164(6) Uani 1 1 d . . .
C2 C 0.6422(3) 0.10104(9) 0.70660(17) 0.0154(6) Uani 1 1 d . . .
H2 H 0.5446 0.0983 0.7043 0.018 Uiso 1 1 calc R . .
C9 C 0.9068(3) 0.15725(9) 0.51031(17) 0.0154(6) Uani 1 1 d . . .
C10 C 0.9658(3) 0.20024(9) 0.52527(17) 0.0184(6) Uani 1 1 d . . .
H10 H 1.0000 0.2200 0.4847 0.022 Uiso 1 1 calc R . .
C12 C 0.9675(3) 0.14130(10) 0.36661(19) 0.0248(7) Uani 1 1 d . . .
H12 H 1.0424 0.1632 0.3780 0.030 Uiso 1 1 calc R . .
C16 C 0.7770(3) 0.09898(10) 0.40991(19) 0.0235(7) Uani 1 1 d . . .
H16 H 0.7210 0.0912 0.4517 0.028 Uiso 1 1 calc R . .
C13 C 0.9425(3) 0.11907(11) 0.2890(2) 0.0323(8) Uani 1 1 d . . .
H13 H 1.0008 0.1255 0.2478 0.039 Uiso 1 1 calc R . .
C17 C 1.0342(3) 0.00274(10) 0.86329(18) 0.0247(7) Uani 1 1 d . . .
H17A H 1.1342 -0.0027 0.8665 0.037 Uiso 1 1 calc R . .
H17B H 0.9836 -0.0241 0.8340 0.037 Uiso 1 1 calc R . .
H17C H 1.0103 0.0053 0.9203 0.037 Uiso 1 1 calc R . .
C20 C 1.1693(3) 0.05869(10) 0.62628(19) 0.0239(7) Uani 1 1 d . . .
H20A H 1.2075 0.0263 0.6340 0.036 Uiso 1 1 calc R . .
H20B H 1.2307 0.0812 0.6605 0.036 Uiso 1 1 calc R . .
H20C H 1.1617 0.0677 0.5668 0.036 Uiso 1 1 calc R . .
C19 C 0.8858(3) 0.01234(10) 0.59979(19) 0.0241(7) Uani 1 1 d . . .
H19A H 0.8885 0.0163 0.5394 0.036 Uiso 1 1 calc R . .
H19B H 0.7897 0.0149 0.6107 0.036 Uiso 1 1 calc R . .
H19C H 0.9230 -0.0191 0.6179 0.036 Uiso 1 1 calc R . .
C28 C 1.2201(3) 0.24853(11) 0.82083(19) 0.0314(7) Uani 1 1 d . . .
H28A H 1.1747 0.2243 0.8515 0.047 Uiso 1 1 calc R . .
H28B H 1.1759 0.2796 0.8261 0.047 Uiso 1 1 calc R . .
H28C H 1.3185 0.2506 0.8445 0.047 Uiso 1 1 calc R . .
C25 C 0.4382(3) 0.01761(11) 0.8353(2) 0.0311(7) Uani 1 1 d . . .
H25A H 0.3859 -0.0122 0.8371 0.047 Uiso 1 1 calc R . .
H25B H 0.3989 0.0363 0.7859 0.047 Uiso 1 1 calc R . .
H25C H 0.4327 0.0361 0.8865 0.047 Uiso 1 1 calc R . .
C27 C 1.3151(3) 0.17881(11) 0.6948(2) 0.0318(8) Uani 1 1 d . . .
H27A H 1.4127 0.1875 0.7112 0.048 Uiso 1 1 calc R . .
H27B H 1.3001 0.1685 0.6359 0.048 Uiso 1 1 calc R . .
H27C H 1.2910 0.1527 0.7307 0.048 Uiso 1 1 calc R . .
C18 C 1.1037(3) 0.10779(10) 0.85434(19) 0.0264(7) Uani 1 1 d . . .
H18A H 1.0939 0.1104 0.9140 0.040 Uiso 1 1 calc R . .
H18B H 1.0790 0.1383 0.8261 0.040 Uiso 1 1 calc R . .
H18C H 1.2000 0.0998 0.8491 0.040 Uiso 1 1 calc R . .
C15 C 0.7511(3) 0.07737(10) 0.33193(19) 0.0279(7) Uani 1 1 d . . .
H15 H 0.6764 0.0554 0.3201 0.033 Uiso 1 1 calc R . .
C32 C 0.6826(3) 0.26653(12) 0.7265(2) 0.0393(9) Uani 1 1 d . . .
H32A H 0.7281 0.2608 0.7842 0.059 Uiso 1 1 calc R . .
H32B H 0.6326 0.2377 0.7049 0.059 Uiso 1 1 calc R . .
H32C H 0.6171 0.2931 0.7262 0.059 Uiso 1 1 calc R . .
C14 C 0.8331(3) 0.08744(11) 0.27101(19) 0.0303(7) Uani 1 1 d . . .
H14 H 0.8146 0.0728 0.2172 0.036 Uiso 1 1 calc R . .
C26 C 0.6304(3) -0.03474(10) 0.7331(2) 0.0284(7) Uani 1 1 d . . .
H26A H 0.5758 -0.0638 0.7373 0.043 Uiso 1 1 calc R . .
H26B H 0.7268 -0.0434 0.7297 0.043 Uiso 1 1 calc R . .
H26C H 0.5918 -0.0169 0.6825 0.043 Uiso 1 1 calc R . .
C24 C 0.6934(3) -0.03135(11) 0.9251(2) 0.0344(8) Uani 1 1 d . . .
H24A H 0.6940 -0.0111 0.9749 0.052 Uiso 1 1 calc R . .
H24B H 0.7882 -0.0419 0.9212 0.052 Uiso 1 1 calc R . .
H24C H 0.6345 -0.0593 0.9298 0.052 Uiso 1 1 calc R . .
C30 C 0.9180(3) 0.33463(11) 0.7039(2) 0.0404(9) Uani 1 1 d . . .
H30A H 0.8542 0.3604 0.7135 0.061 Uiso 1 1 calc R . .
H30B H 0.9795 0.3456 0.6647 0.061 Uiso 1 1 calc R . .
H30C H 0.9735 0.3256 0.7575 0.061 Uiso 1 1 calc R . .
C31 C 0.7272(4) 0.30119(11) 0.5522(2) 0.0388(8) Uani 1 1 d . . .
H31A H 0.6753 0.3307 0.5582 0.058 Uiso 1 1 calc R . .
H31B H 0.6630 0.2761 0.5283 0.058 Uiso 1 1 calc R . .
H31C H 0.7964 0.3069 0.5148 0.058 Uiso 1 1 calc R . .
C29 C 1.2626(3) 0.28213(11) 0.6456(2) 0.0361(8) Uani 1 1 d . . .
H29A H 1.3600 0.2894 0.6664 0.054 Uiso 1 1 calc R . .
H29B H 1.2056 0.3104 0.6518 0.054 Uiso 1 1 calc R . .
H29C H 1.2532 0.2731 0.5860 0.054 Uiso 1 1 calc R . .
C21 C 0.5422(4) 0.14971(14) 0.9228(3) 0.0558(11) Uani 1 1 d . . .
H21A H 0.4858 0.1219 0.9330 0.084 Uiso 1 1 calc R . .
H21B H 0.5062 0.1638 0.8680 0.084 Uiso 1 1 calc R . .
H21C H 0.5381 0.1734 0.9672 0.084 Uiso 1 1 calc R . .
C23 C 0.8316(4) 0.18489(11) 0.9106(2) 0.0420(9) Uani 1 1 d . . .
H23A H 0.7977 0.2116 0.9414 0.063 Uiso 1 1 calc R . .
H23B H 0.8242 0.1931 0.8508 0.063 Uiso 1 1 calc R . .
H23C H 0.9287 0.1784 0.9331 0.063 Uiso 1 1 calc R . .
C22 C 0.7917(5) 0.10067(13) 1.0247(2) 0.0647(14) Uani 1 1 d . . .
H22A H 0.7977 0.1240 1.0706 0.097 Uiso 1 1 calc R . .
H22B H 0.8840 0.0874 1.0218 0.097 Uiso 1 1 calc R . .
H22C H 0.7284 0.0748 1.0350 0.097 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 C1 1.989(3) . ?
Ge1 C9 1.995(3) . ?
Ge1 Si2 2.3937(9) . ?
Ge1 Ge2 2.4741(6) . ?
Ge2 C10 1.976(3) . ?
Ge2 Si5 2.3895(10) . ?
Ge2 Si6 2.4025(9) . ?
Ge3 C2 1.973(3) . ?
Ge3 Si3 2.3809(9) . ?
Ge3 Si4 2.3913(9) . ?
Ge3 Si1 2.3925(9) . ?
Si2 C20 1.869(3) . ?
Si2 C19 1.880(3) . ?
Si2 Si1 2.3275(12) . ?
Si1 C17 1.878(3) . ?
Si1 C18 1.880(3) . ?
Si6 C30 1.869(3) . ?
Si6 C32 1.872(3) . ?
Si6 C31 1.875(3) . ?
Si5 C27 1.863(3) . ?
Si5 C28 1.862(3) . ?
Si5 C29 1.868(3) . ?
Si3 C21 1.861(3) . ?
Si3 C23 1.863(3) . ?
Si3 C22 1.867(4) . ?
Si4 C24 1.872(3) . ?
Si4 C25 1.872(3) . ?
Si4 C26 1.875(3) . ?
C3 C8 1.394(4) . ?
C3 C4 1.396(4) . ?
C3 C1 1.498(4) . ?
C8 C7 1.381(4) . ?
C4 C5 1.386(4) . ?
C7 C6 1.383(5) . ?
C6 C5 1.374(5) . ?
C1 C2 1.334(4) . ?
C11 C16 1.394(4) . ?
C11 C12 1.395(4) . ?
C11 C9 1.480(4) . ?
C9 C10 1.340(4) . ?
C12 C13 1.381(4) . ?
C16 C15 1.380(4) . ?
C13 C14 1.384(4) . ?
C15 C14 1.380(4) . ?

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 C9 116.33(11) . . ?
C1 Ge1 Si2 104.54(8) . . ?
C9 Ge1 Si2 111.73(8) . . ?
C1 Ge1 Ge2 119.71(7) . . ?
C9 Ge1 Ge2 74.07(8) . . ?
Si2 Ge1 Ge2 127.29(3) . . ?
C10 Ge2 Si5 109.22(8) . . ?
C10 Ge2 Si6 109.10(8) . . ?
Si5 Ge2 Si6 112.96(3) . . ?
C10 Ge2 Ge1 72.63(8) . . ?
Si5 Ge2 Ge1 122.94(2) . . ?
Si6 Ge2 Ge1 119.97(3) . . ?
C2 Ge3 Si3 108.80(8) . . ?
C2 Ge3 Si4 101.09(8) . . ?
Si3 Ge3 Si4 111.28(3) . . ?
C2 Ge3 Si1 113.99(8) . . ?
Si3 Ge3 Si1 110.93(4) . . ?
Si4 Ge3 Si1 110.40(3) . . ?
C20 Si2 C19 107.58(13) . . ?
C20 Si2 Si1 116.90(11) . . ?
C19 Si2 Si1 113.94(10) . . ?
C20 Si2 Ge1 112.27(10) . . ?
C19 Si2 Ge1 106.03(10) . . ?
Si1 Si2 Ge1 99.49(4) . . ?
C17 Si1 C18 107.21(14) . . ?
C17 Si1 Si2 117.94(10) . . ?
C18 Si1 Si2 108.24(10) . . ?
C17 Si1 Ge3 108.17(9) . . ?
C18 Si1 Ge3 112.25(10) . . ?
Si2 Si1 Ge3 103.11(4) . . ?
C30 Si6 C32 108.93(17) . . ?
C30 Si6 C31 106.01(16) . . ?
C32 Si6 C31 109.09(16) . . ?
C30 Si6 Ge2 109.91(11) . . ?
C32 Si6 Ge2 111.68(11) . . ?
C31 Si6 Ge2 111.04(11) . . ?
C27 Si5 C28 109.91(15) . . ?
C27 Si5 C29 108.12(15) . . ?
C28 Si5 C29 109.77(16) . . ?
C27 Si5 Ge2 110.09(10) . . ?
C28 Si5 Ge2 113.24(10) . . ?
C29 Si5 Ge2 105.51(11) . . ?
C21 Si3 C23 108.41(17) . . ?
C21 Si3 C22 109.9(2) . . ?
C23 Si3 C22 109.39(19) . . ?
C21 Si3 Ge3 111.85(13) . . ?
C23 Si3 Ge3 109.40(11) . . ?
C22 Si3 Ge3 107.89(12) . . ?
C24 Si4 C25 107.30(15) . . ?
C24 Si4 C26 109.24(15) . . ?
C25 Si4 C26 108.42(14) . . ?
C24 Si4 Ge3 114.01(10) . . ?
C25 Si4 Ge3 109.29(10) . . ?
C26 Si4 Ge3 108.45(10) . . ?
C8 C3 C4 118.3(3) . . ?
C8 C3 C1 121.1(2) . . ?
C4 C3 C1 120.6(2) . . ?
C7 C8 C3 120.7(3) . . ?
C5 C4 C3 120.6(3) . . ?
C8 C7 C6 120.3(3) . . ?
C5 C6 C7 119.8(3) . . ?
C6 C5 C4 120.3(3) . . ?
C2 C1 C3 119.4(2) . . ?
C2 C1 Ge1 123.6(2) . . ?
C3 C1 Ge1 116.87(19) . . ?
C16 C11 C12 117.9(3) . . ?
C16 C11 C9 121.0(2) . . ?
C12 C11 C9 121.1(2) . . ?
C1 C2 Ge3 133.6(2) . . ?
C10 C9 C11 126.3(2) . . ?
C10 C9 Ge1 104.4(2) . . ?
C11 C9 Ge1 129.07(19) . . ?
C9 C10 Ge2 108.6(2) . . ?
C13 C12 C11 120.9(3) . . ?
C15 C16 C11 121.1(3) . . ?
C12 C13 C14 120.4(3) . . ?
C16 C15 C14 120.3(3) . . ?
C15 C14 C13 119.4(3) . . ?

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
C1 Ge1 Ge2 C10 -114.15(12) . . . . ?
C9 Ge1 Ge2 C10 -2.54(11) . . . . ?
Si2 Ge1 Ge2 C10 102.92(9) . . . . ?
C1 Ge1 Ge2 Si5 143.83(10) . . . . ?
C9 Ge1 Ge2 Si5 -104.57(8) . . . . ?
Si2 Ge1 Ge2 Si5 0.89(4) . . . . ?
C1 Ge1 Ge2 Si6 -11.71(10) . . . . ?
C9 Ge1 Ge2 Si6 99.90(8) . . . . ?
Si2 Ge1 Ge2 Si6 -154.64(4) . . . . ?
C1 Ge1 Si2 C20 165.96(13) . . . . ?
C9 Ge1 Si2 C20 39.33(13) . . . . ?
Ge2 Ge1 Si2 C20 -46.78(11) . . . . ?
C1 Ge1 Si2 C19 48.74(13) . . . . ?
C9 Ge1 Si2 C19 -77.89(13) . . . . ?
Ge2 Ge1 Si2 C19 -164.00(10) . . . . ?
C1 Ge1 Si2 Si1 -69.69(9) . . . . ?
C9 Ge1 Si2 Si1 163.68(8) . . . . ?
Ge2 Ge1 Si2 Si1 77.57(4) . . . . ?
C20 Si2 Si1 C17 -70.68(15) . . . . ?
C19 Si2 Si1 C17 55.90(15) . . . . ?
Ge1 Si2 Si1 C17 168.27(10) . . . . ?
C20 Si2 Si1 C18 51.16(15) . . . . ?
C19 Si2 Si1 C18 177.74(14) . . . . ?
Ge1 Si2 Si1 C18 -69.89(10) . . . . ?
C20 Si2 Si1 Ge3 170.24(10) . . . . ?
C19 Si2 Si1 Ge3 -63.17(11) . . . . ?
Ge1 Si2 Si1 Ge3 49.20(4) . . . . ?
C2 Ge3 Si1 C17 -140.49(13) . . . . ?
Si3 Ge3 Si1 C17 96.30(11) . . . . ?
Si4 Ge3 Si1 C17 -27.53(11) . . . . ?
C2 Ge3 Si1 C18 101.42(14) . . . . ?
Si3 Ge3 Si1 C18 -21.79(11) . . . . ?
Si4 Ge3 Si1 C18 -145.62(11) . . . . ?
C2 Ge3 Si1 Si2 -14.85(9) . . . . ?
Si3 Ge3 Si1 Si2 -138.06(4) . . . . ?
Si4 Ge3 Si1 Si2 98.11(4) . . . . ?
C10 Ge2 Si6 C30 -115.36(15) . . . . ?
Si5 Ge2 Si6 C30 6.31(13) . . . . ?
Ge1 Ge2 Si6 C30 164.13(13) . . . . ?
C10 Ge2 Si6 C32 123.62(15) . . . . ?
Si5 Ge2 Si6 C32 -114.70(13) . . . . ?
Ge1 Ge2 Si6 C32 43.11(13) . . . . ?
C10 Ge2 Si6 C31 1.62(15) . . . . ?
Si5 Ge2 Si6 C31 123.29(12) . . . . ?
Ge1 Ge2 Si6 C31 -78.89(12) . . . . ?
C10 Ge2 Si5 C27 -58.23(14) . . . . ?
Si6 Ge2 Si5 C27 -179.84(11) . . . . ?
Ge1 Ge2 Si5 C27 23.10(12) . . . . ?
C10 Ge2 Si5 C28 178.29(14) . . . . ?
Si6 Ge2 Si5 C28 56.68(12) . . . . ?
Ge1 Ge2 Si5 C28 -100.38(11) . . . . ?
C10 Ge2 Si5 C29 58.21(15) . . . . ?
Si6 Ge2 Si5 C29 -63.40(12) . . . . ?
Ge1 Ge2 Si5 C29 139.54(12) . . . . ?
C2 Ge3 Si3 C21 47.16(17) . . . . ?
Si4 Ge3 Si3 C21 -63.37(16) . . . . ?
Si1 Ge3 Si3 C21 173.30(15) . . . . ?
C2 Ge3 Si3 C23 -72.97(15) . . . . ?
Si4 Ge3 Si3 C23 176.51(13) . . . . ?
Si1 Ge3 Si3 C23 53.18(13) . . . . ?
C2 Ge3 Si3 C22 168.11(18) . . . . ?
Si4 Ge3 Si3 C22 57.59(17) . . . . ?
Si1 Ge3 Si3 C22 -65.74(17) . . . . ?
C2 Ge3 Si4 C24 -179.45(14) . . . . ?
Si3 Ge3 Si4 C24 -64.06(13) . . . . ?
Si1 Ge3 Si4 C24 59.56(13) . . . . ?
C2 Ge3 Si4 C25 -59.39(13) . . . . ?
Si3 Ge3 Si4 C25 55.99(11) . . . . ?
Si1 Ge3 Si4 C25 179.62(11) . . . . ?
C2 Ge3 Si4 C26 58.63(13) . . . . ?
Si3 Ge3 Si4 C26 174.01(11) . . . . ?
Si1 Ge3 Si4 C26 -62.36(11) . . . . ?
C4 C3 C8 C7 1.4(4) . . . . ?
C1 C3 C8 C7 -179.7(3) . . . . ?
C8 C3 C4 C5 -0.7(4) . . . . ?
C1 C3 C4 C5 -179.7(3) . . . . ?
C3 C8 C7 C6 -1.0(5) . . . . ?
C8 C7 C6 C5 -0.1(5) . . . . ?
C7 C6 C5 C4 0.8(5) . . . . ?
C3 C4 C5 C6 -0.4(5) . . . . ?
C8 C3 C1 C2 134.6(3) . . . . ?
C4 C3 C1 C2 -46.5(4) . . . . ?
C8 C3 C1 Ge1 -48.2(3) . . . . ?
C4 C3 C1 Ge1 130.8(2) . . . . ?
C9 Ge1 C1 C2 173.3(2) . . . . ?
Si2 Ge1 C1 C2 49.6(2) . . . . ?
Ge2 Ge1 C1 C2 -100.7(2) . . . . ?
C9 Ge1 C1 C3 -3.8(2) . . . . ?
Si2 Ge1 C1 C3 -127.57(18) . . . . ?
Ge2 Ge1 C1 C3 82.1(2) . . . . ?
C3 C1 C2 Ge3 175.1(2) . . . . ?
Ge1 C1 C2 Ge3 -2.0(4) . . . . ?
Si3 Ge3 C2 C1 106.2(3) . . . . ?
Si4 Ge3 C2 C1 -136.6(3) . . . . ?
Si1 Ge3 C2 C1 -18.1(3) . . . . ?
C16 C11 C9 C10 -153.3(3) . . . . ?
C12 C11 C9 C10 25.3(4) . . . . ?
C16 C11 C9 Ge1 33.0(4) . . . . ?
C12 C11 C9 Ge1 -148.3(2) . . . . ?
C1 Ge1 C9 C10 119.41(18) . . . . ?
Si2 Ge1 C9 C10 -120.67(17) . . . . ?
Ge2 Ge1 C9 C10 3.70(16) . . . . ?
C1 Ge1 C9 C11 -65.9(2) . . . . ?
Si2 Ge1 C9 C11 54.0(2) . . . . ?
Ge2 Ge1 C9 C11 178.4(2) . . . . ?
C11 C9 C10 Ge2 -179.6(2) . . . . ?
Ge1 C9 C10 Ge2 -4.7(2) . . . . ?
Si5 Ge2 C10 C9 123.47(17) . . . . ?
Si6 Ge2 C10 C9 -112.61(18) . . . . ?
Ge1 Ge2 C10 C9 3.85(16) . . . . ?
C16 C11 C12 C13 1.3(4) . . . . ?
C9 C11 C12 C13 -177.4(3) . . . . ?
C12 C11 C16 C15 -2.2(4) . . . . ?
C9 C11 C16 C15 176.4(3) . . . . ?
C11 C12 C13 C14 0.6(5) . . . . ?
C11 C16 C15 C14 1.3(4) . . . . ?
C16 C15 C14 C13 0.6(5) . . . . ?
C12 C13 C14 C15 -1.6(5) . . . . ?

_diffrn_measured_fraction_theta_max 0.995
_diffrn_reflns_theta_full        26.37
_diffrn_measured_fraction_theta_full 0.995
_refine_diff_density_max         0.804
_refine_diff_density_min         -0.434
_refine_diff_density_rms         0.097

# SQUEEZE RESULTS (APPEND TO CIF)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.113 0.488 0.961 12 0 ' '
2 0.386 0.988 0.539 11 0 ' '
3 0.614 0.012 0.461 12 0 ' '
4 0.886 0.512 0.039 11 0 ' '
_platon_squeeze_details          
;
;


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

data_1136j
_database_code_depnum_ccdc_archive 'CCDC 1450273'
_audit_update_record             
;
2016-01-27 deposited with the CCDC.
2018-03-23 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C30 H58 Ge Si8'
_chemical_formula_weight         716.07

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'
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   P2(1)/n

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

_cell_length_a                   10.786(3)
_cell_length_b                   35.733(10)
_cell_length_c                   10.841(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 96.252(5)
_cell_angle_gamma                90.00
_cell_volume                     4153(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9843
_cell_measurement_theta_min      4.371
_cell_measurement_theta_max      52.538

_exptl_crystal_description       blocks
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.15
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.145
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1528
_exptl_absorpt_coefficient_mu    0.986
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7303
_exptl_absorpt_correction_T_max  0.8662
_exptl_absorpt_process_details   SADABS

_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  'SMART APEX'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            32831
_diffrn_reflns_av_R_equivalents  0.0620
_diffrn_reflns_av_sigmaI/netI    0.0557
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -44
_diffrn_reflns_limit_k_max       44
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         1.97
_diffrn_reflns_theta_max         26.57
_reflns_number_total             8603
_reflns_number_gt                7091
_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)+(0.0735P)²+5.4970P] 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_coef       none
_refine_ls_number_reflns         8603
_refine_ls_number_parameters     368
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0785
_refine_ls_R_factor_gt           0.0647
_refine_ls_wR_factor_ref         0.1510
_refine_ls_wR_factor_gt          0.1449
_refine_ls_goodness_of_fit_ref   1.097
_refine_ls_restrained_S_all      1.097
_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 0.78877(3) 0.079001(10) 0.19036(3) 0.01794(12) Uani 1 1 d . . .
Si1 Si 0.60170(9) 0.04729(3) 0.22366(9) 0.0200(2) Uani 1 1 d . . .
Si2 Si 0.88406(10) 0.13509(3) 0.28340(9) 0.0194(2) Uani 1 1 d . . .
Si3 Si 0.82552(10) 0.16457(3) 0.08870(9) 0.0217(2) Uani 1 1 d . . .
Si4 Si 0.81070(10) 0.10564(3) -0.00917(9) 0.0203(2) Uani 1 1 d . . .
Si5 Si 0.81004(12) 0.16246(3) 0.45954(10) 0.0289(3) Uani 1 1 d . . .
Si6 Si 1.09910(11) 0.12513(3) 0.34005(11) 0.0291(3) Uani 1 1 d . . .
Si7 Si 0.95513(13) 0.21046(3) 0.01317(11) 0.0332(3) Uani 1 1 d . . .
Si8 Si 0.61964(11) 0.18704(3) 0.07613(11) 0.0291(3) Uani 1 1 d . . .
C1 C 0.8315(3) 0.02538(10) 0.2278(3) 0.0193(7) Uani 1 1 d . . .
C2 C 0.7204(3) 0.00812(10) 0.2367(3) 0.0197(7) Uani 1 1 d . . .
C3 C 0.6982(3) -0.03240(10) 0.2477(3) 0.0197(7) Uani 1 1 d . . .
C4 C 0.6117(3) -0.04601(10) 0.3248(3) 0.0223(8) Uani 1 1 d . . .
H4 H 0.5680 -0.0288 0.3711 0.027 Uiso 1 1 calc R . .
C5 C 0.5892(4) -0.08375(11) 0.3345(4) 0.0281(9) Uani 1 1 d . . .
H5 H 0.5312 -0.0923 0.3881 0.034 Uiso 1 1 calc R . .
C6 C 0.6507(4) -0.10931(11) 0.2665(4) 0.0290(9) Uani 1 1 d . . .
H6 H 0.6353 -0.1354 0.2735 0.035 Uiso 1 1 calc R . .
C7 C 0.7349(4) -0.09648(11) 0.1881(4) 0.0299(9) Uani 1 1 d . . .
H7 H 0.7767 -0.1138 0.1406 0.036 Uiso 1 1 calc R . .
C8 C 0.7582(4) -0.05851(11) 0.1789(4) 0.0267(8) Uani 1 1 d . . .
H8 H 0.8161 -0.0501 0.1248 0.032 Uiso 1 1 calc R . .
C9 C 0.9575(3) 0.00874(10) 0.2450(3) 0.0197(7) Uani 1 1 d . . .
C10 C 0.9947(4) -0.01367(10) 0.3481(3) 0.0234(8) Uani 1 1 d . . .
H10 H 0.9353 -0.0207 0.4024 0.028 Uiso 1 1 calc R . .
C11 C 1.1166(4) -0.02581(11) 0.3722(4) 0.0298(9) Uani 1 1 d . . .
H11 H 1.1407 -0.0406 0.4435 0.036 Uiso 1 1 calc R . .
C12 C 1.2040(4) -0.01639(12) 0.2921(4) 0.0339(10) Uani 1 1 d . . .
H12 H 1.2881 -0.0244 0.3093 0.041 Uiso 1 1 calc R . .
C13 C 1.1680(4) 0.00452(12) 0.1882(4) 0.0352(10) Uani 1 1 d . . .
H13 H 1.2265 0.0101 0.1313 0.042 Uiso 1 1 calc R . .
C14 C 1.0472(4) 0.01747(11) 0.1660(4) 0.0276(9) Uani 1 1 d . . .
H14 H 1.0245 0.0327 0.0952 0.033 Uiso 1 1 calc R . .
C15 C 0.5280(4) 0.05555(12) 0.3706(4) 0.0315(9) Uani 1 1 d . . .
H15A H 0.4852 0.0798 0.3657 0.047 Uiso 1 1 calc R . .
H15B H 0.5927 0.0555 0.4414 0.047 Uiso 1 1 calc R . .
H15C H 0.4676 0.0356 0.3811 0.047 Uiso 1 1 calc R . .
C16 C 0.4743(4) 0.04214(12) 0.0925(4) 0.0304(9) Uani 1 1 d . . .
H16A H 0.4339 0.0177 0.0982 0.046 Uiso 1 1 calc R . .
H16B H 0.5099 0.0439 0.0133 0.046 Uiso 1 1 calc R . .
H16C H 0.4126 0.0621 0.0975 0.046 Uiso 1 1 calc R . .
C17 C 0.9552(4) 0.09135(12) -0.0793(4) 0.0264(8) Uani 1 1 d . . .
H17A H 0.9502 0.0647 -0.1007 0.040 Uiso 1 1 calc R . .
H17B H 1.0285 0.0958 -0.0193 0.040 Uiso 1 1 calc R . .
H17C H 0.9623 0.1061 -0.1543 0.040 Uiso 1 1 calc R . .
C18 C 0.6739(4) 0.09781(12) -0.1293(4) 0.0306(9) Uani 1 1 d . . .
H18A H 0.6847 0.1126 -0.2035 0.046 Uiso 1 1 calc R . .
H18B H 0.5970 0.1055 -0.0958 0.046 Uiso 1 1 calc R . .
H18C H 0.6685 0.0712 -0.1513 0.046 Uiso 1 1 calc R . .
C19 C 0.6372(5) 0.15932(13) 0.4652(5) 0.0418(11) Uani 1 1 d . . .
H19A H 0.6164 0.1689 0.5452 0.063 Uiso 1 1 calc R . .
H19B H 0.6107 0.1332 0.4556 0.063 Uiso 1 1 calc R . .
H19C H 0.5943 0.1743 0.3979 0.063 Uiso 1 1 calc R . .
C20 C 0.8838(6) 0.14022(14) 0.6060(4) 0.0484(13) Uani 1 1 d . . .
H20A H 0.8497 0.1515 0.6774 0.073 Uiso 1 1 calc R . .
H20B H 0.9742 0.1442 0.6132 0.073 Uiso 1 1 calc R . .
H20C H 0.8660 0.1133 0.6040 0.073 Uiso 1 1 calc R . .
C21 C 0.8551(5) 0.21316(11) 0.4648(4) 0.0370(10) Uani 1 1 d . . .
H21A H 0.8200 0.2255 0.3881 0.055 Uiso 1 1 calc R . .
H21B H 0.9462 0.2153 0.4731 0.055 Uiso 1 1 calc R . .
H21C H 0.8227 0.2252 0.5360 0.055 Uiso 1 1 calc R . .
C22 C 1.1164(4) 0.08415(11) 0.4476(4) 0.0338(10) Uani 1 1 d . . .
H22A H 1.2050 0.0801 0.4750 0.051 Uiso 1 1 calc R . .
H22B H 1.0817 0.0618 0.4044 0.051 Uiso 1 1 calc R . .
H22C H 1.0716 0.0891 0.5199 0.051 Uiso 1 1 calc R . .
C23 C 1.1746(5) 0.16693(14) 0.4213(6) 0.0557(15) Uani 1 1 d . . .
H23A H 1.1314 0.1730 0.4938 0.084 Uiso 1 1 calc R . .
H23B H 1.1695 0.1883 0.3644 0.084 Uiso 1 1 calc R . .
H23C H 1.2623 0.1613 0.4483 0.084 Uiso 1 1 calc R . .
C24 C 1.1888(4) 0.11441(14) 0.2052(5) 0.0419(12) Uani 1 1 d . . .
H24A H 1.2783 0.1143 0.2333 0.063 Uiso 1 1 calc R . .
H24B H 1.1710 0.1336 0.1410 0.063 Uiso 1 1 calc R . .
H24C H 1.1638 0.0898 0.1711 0.063 Uiso 1 1 calc R . .
C25 C 0.8647(6) 0.23945(17) -0.1092(6) 0.0686(19) Uani 1 1 d . . .
H25A H 0.7998 0.2534 -0.0723 0.103 Uiso 1 1 calc R . .
H25B H 0.8258 0.2231 -0.1749 0.103 Uiso 1 1 calc R . .
H25C H 0.9211 0.2570 -0.1445 0.103 Uiso 1 1 calc R . .
C26 C 1.0875(5) 0.18947(15) -0.0654(6) 0.0582(16) Uani 1 1 d . . .
H26A H 1.1366 0.2096 -0.0977 0.087 Uiso 1 1 calc R . .
H26B H 1.0532 0.1734 -0.1340 0.087 Uiso 1 1 calc R . .
H26C H 1.1410 0.1746 -0.0052 0.087 Uiso 1 1 calc R . .
C27 C 1.0202(9) 0.2404(2) 0.1426(6) 0.111(4) Uani 1 1 d . . .
H27A H 1.0795 0.2582 0.1128 0.166 Uiso 1 1 calc R . .
H27B H 1.0632 0.2248 0.2082 0.166 Uiso 1 1 calc R . .
H27C H 0.9526 0.2542 0.1756 0.166 Uiso 1 1 calc R . .
C28 C 0.6121(5) 0.23128(13) 0.1674(4) 0.0416(11) Uani 1 1 d . . .
H28A H 0.6635 0.2505 0.1334 0.062 Uiso 1 1 calc R . .
H28B H 0.6433 0.2266 0.2544 0.062 Uiso 1 1 calc R . .
H28C H 0.5254 0.2399 0.1624 0.062 Uiso 1 1 calc R . .
C29 C 0.5594(5) 0.19732(15) -0.0894(4) 0.0456(12) Uani 1 1 d . . .
H29A H 0.4700 0.2029 -0.0948 0.068 Uiso 1 1 calc R . .
H29B H 0.5728 0.1755 -0.1411 0.068 Uiso 1 1 calc R . .
H29C H 0.6039 0.2189 -0.1187 0.068 Uiso 1 1 calc R . .
C30 C 0.5100(4) 0.15161(13) 0.1326(5) 0.0403(11) Uani 1 1 d . . .
H30A H 0.5459 0.1416 0.2128 0.061 Uiso 1 1 calc R . .
H30B H 0.4971 0.1312 0.0722 0.061 Uiso 1 1 calc R . .
H30C H 0.4299 0.1636 0.1421 0.061 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 C1 2.002(4) . ?
Ge1 Si1 2.3758(12) . ?
Ge1 Si4 2.3984(12) . ?
Ge1 Si2 2.4217(12) . ?
Si1 C16 1.876(4) . ?
Si1 C15 1.879(4) . ?
Si1 C2 1.892(4) . ?
Si2 Si5 2.3605(15) . ?
Si2 Si6 2.3608(16) . ?
Si2 Si3 2.3818(15) . ?
Si3 Si8 2.3512(16) . ?
Si3 Si4 2.3557(16) . ?
Si3 Si7 2.3586(16) . ?
Si4 C17 1.878(4) . ?
Si4 C18 1.880(4) . ?
Si5 C20 1.873(5) . ?
Si5 C19 1.875(5) . ?
Si5 C21 1.875(4) . ?
Si6 C22 1.869(4) . ?
Si6 C23 1.875(5) . ?
Si6 C24 1.878(5) . ?
Si7 C27 1.841(6) . ?
Si7 C25 1.872(5) . ?
Si7 C26 1.895(5) . ?
Si8 C28 1.871(5) . ?
Si8 C29 1.877(5) . ?
Si8 C30 1.880(5) . ?
C1 C2 1.361(5) . ?
C1 C9 1.476(5) . ?
C2 C3 1.475(5) . ?
C3 C8 1.397(5) . ?
C3 C4 1.406(5) . ?
C4 C5 1.376(5) . ?
C5 C6 1.387(6) . ?
C6 C7 1.387(6) . ?
C7 C8 1.385(6) . ?
C9 C14 1.395(5) . ?
C9 C10 1.398(5) . ?
C10 C11 1.382(6) . ?
C11 C12 1.390(6) . ?
C12 C13 1.373(6) . ?
C13 C14 1.379(6) . ?

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 Si1 72.15(11) . . ?
C1 Ge1 Si4 121.30(10) . . ?
Si1 Ge1 Si4 119.68(4) . . ?
C1 Ge1 Si2 129.02(11) . . ?
Si1 Ge1 Si2 131.33(4) . . ?
Si4 Ge1 Si2 88.17(4) . . ?
C16 Si1 C15 108.4(2) . . ?
C16 Si1 C2 114.71(17) . . ?
C15 Si1 C2 113.49(18) . . ?
C16 Si1 Ge1 119.73(14) . . ?
C15 Si1 Ge1 119.90(14) . . ?
C2 Si1 Ge1 77.59(11) . . ?
Si5 Si2 Si6 105.15(6) . . ?
Si5 Si2 Si3 116.95(6) . . ?
Si6 Si2 Si3 117.09(6) . . ?
Si5 Si2 Ge1 120.95(5) . . ?
Si6 Si2 Ge1 110.12(5) . . ?
Si3 Si2 Ge1 86.42(4) . . ?
Si8 Si3 Si4 105.18(6) . . ?
Si8 Si3 Si7 109.52(6) . . ?
Si4 Si3 Si7 118.61(6) . . ?
Si8 Si3 Si2 111.10(6) . . ?
Si4 Si3 Si2 90.12(5) . . ?
Si7 Si3 Si2 120.34(6) . . ?
C17 Si4 C18 107.63(19) . . ?
C17 Si4 Si3 114.01(14) . . ?
C18 Si4 Si3 117.04(14) . . ?
C17 Si4 Ge1 115.14(13) . . ?
C18 Si4 Ge1 114.75(14) . . ?
Si3 Si4 Ge1 87.54(5) . . ?
C20 Si5 C19 106.2(3) . . ?
C20 Si5 C21 107.4(2) . . ?
C19 Si5 C21 108.2(2) . . ?
C20 Si5 Si2 111.10(16) . . ?
C19 Si5 Si2 115.27(15) . . ?
C21 Si5 Si2 108.40(16) . . ?
C22 Si6 C23 108.8(2) . . ?
C22 Si6 C24 107.5(2) . . ?
C23 Si6 C24 107.1(3) . . ?
C22 Si6 Si2 107.99(15) . . ?
C23 Si6 Si2 111.48(18) . . ?
C24 Si6 Si2 113.77(15) . . ?
C27 Si7 C25 110.2(4) . . ?
C27 Si7 C26 109.2(4) . . ?
C25 Si7 C26 105.1(3) . . ?
C27 Si7 Si3 109.3(2) . . ?
C25 Si7 Si3 110.4(2) . . ?
C26 Si7 Si3 112.63(17) . . ?
C28 Si8 C29 108.1(2) . . ?
C28 Si8 C30 109.4(2) . . ?
C29 Si8 C30 106.2(2) . . ?
C28 Si8 Si3 110.68(17) . . ?
C29 Si8 Si3 110.41(17) . . ?
C30 Si8 Si3 112.01(15) . . ?
C2 C1 C9 127.9(3) . . ?
C2 C1 Ge1 105.2(3) . . ?
C9 C1 Ge1 126.9(3) . . ?
C1 C2 C3 127.1(3) . . ?
C1 C2 Si1 104.7(3) . . ?
C3 C2 Si1 128.2(3) . . ?
C8 C3 C4 117.6(3) . . ?
C8 C3 C2 121.6(3) . . ?
C4 C3 C2 120.8(3) . . ?
C5 C4 C3 121.2(4) . . ?
C4 C5 C6 120.4(4) . . ?
C7 C6 C5 119.4(4) . . ?
C8 C7 C6 120.3(4) . . ?
C7 C8 C3 121.1(4) . . ?
C14 C9 C10 117.4(4) . . ?
C14 C9 C1 121.5(3) . . ?
C10 C9 C1 120.8(3) . . ?
C11 C10 C9 121.0(4) . . ?
C10 C11 C12 120.1(4) . . ?
C13 C12 C11 119.6(4) . . ?
C12 C13 C14 120.2(4) . . ?
C13 C14 C9 121.5(4) . . ?

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
C1 Ge1 Si1 C16 -114.71(19) . . . . ?
Si4 Ge1 Si1 C16 1.70(16) . . . . ?
Si2 Ge1 Si1 C16 118.59(16) . . . . ?
C1 Ge1 Si1 C15 107.0(2) . . . . ?
Si4 Ge1 Si1 C15 -136.62(17) . . . . ?
Si2 Ge1 Si1 C15 -19.73(18) . . . . ?
C1 Ge1 Si1 C2 -3.17(15) . . . . ?
Si4 Ge1 Si1 C2 113.24(12) . . . . ?
Si2 Ge1 Si1 C2 -129.87(12) . . . . ?
C1 Ge1 Si2 Si5 -89.95(14) . . . . ?
Si1 Ge1 Si2 Si5 10.84(8) . . . . ?
Si4 Ge1 Si2 Si5 140.01(6) . . . . ?
C1 Ge1 Si2 Si6 33.01(14) . . . . ?
Si1 Ge1 Si2 Si6 133.80(6) . . . . ?
Si4 Ge1 Si2 Si6 -97.03(5) . . . . ?
C1 Ge1 Si2 Si3 150.58(13) . . . . ?
Si1 Ge1 Si2 Si3 -108.62(5) . . . . ?
Si4 Ge1 Si2 Si3 20.55(4) . . . . ?
Si5 Si2 Si3 Si8 -37.68(8) . . . . ?
Si6 Si2 Si3 Si8 -163.78(6) . . . . ?
Ge1 Si2 Si3 Si8 85.42(6) . . . . ?
Si5 Si2 Si3 Si4 -144.03(6) . . . . ?
Si6 Si2 Si3 Si4 89.87(6) . . . . ?
Ge1 Si2 Si3 Si4 -20.93(4) . . . . ?
Si5 Si2 Si3 Si7 92.18(8) . . . . ?
Si6 Si2 Si3 Si7 -33.92(9) . . . . ?
Ge1 Si2 Si3 Si7 -144.71(6) . . . . ?
Si8 Si3 Si4 C17 152.67(14) . . . . ?
Si7 Si3 Si4 C17 29.82(16) . . . . ?
Si2 Si3 Si4 C17 -95.39(14) . . . . ?
Si8 Si3 Si4 C18 25.84(17) . . . . ?
Si7 Si3 Si4 C18 -97.01(17) . . . . ?
Si2 Si3 Si4 C18 137.77(16) . . . . ?
Si8 Si3 Si4 Ge1 -90.82(5) . . . . ?
Si7 Si3 Si4 Ge1 146.33(6) . . . . ?
Si2 Si3 Si4 Ge1 21.12(4) . . . . ?
C1 Ge1 Si4 C17 -41.2(2) . . . . ?
Si1 Ge1 Si4 C17 -127.38(15) . . . . ?
Si2 Ge1 Si4 C17 94.68(15) . . . . ?
C1 Ge1 Si4 C18 84.6(2) . . . . ?
Si1 Ge1 Si4 C18 -1.60(16) . . . . ?
Si2 Ge1 Si4 C18 -139.54(15) . . . . ?
C1 Ge1 Si4 Si3 -156.64(13) . . . . ?
Si1 Ge1 Si4 Si3 117.17(5) . . . . ?
Si2 Ge1 Si4 Si3 -20.76(4) . . . . ?
Si6 Si2 Si5 C20 -39.7(2) . . . . ?
Si3 Si2 Si5 C20 -171.5(2) . . . . ?
Ge1 Si2 Si5 C20 85.6(2) . . . . ?
Si6 Si2 Si5 C19 -160.51(18) . . . . ?
Si3 Si2 Si5 C19 67.67(19) . . . . ?
Ge1 Si2 Si5 C19 -35.22(19) . . . . ?
Si6 Si2 Si5 C21 78.10(17) . . . . ?
Si3 Si2 Si5 C21 -53.71(18) . . . . ?
Ge1 Si2 Si5 C21 -156.60(17) . . . . ?
Si5 Si2 Si6 C22 74.77(16) . . . . ?
Si3 Si2 Si6 C22 -153.50(16) . . . . ?
Ge1 Si2 Si6 C22 -57.03(16) . . . . ?
Si5 Si2 Si6 C23 -44.7(2) . . . . ?
Si3 Si2 Si6 C23 87.0(2) . . . . ?
Ge1 Si2 Si6 C23 -176.5(2) . . . . ?
Si5 Si2 Si6 C24 -165.97(17) . . . . ?
Si3 Si2 Si6 C24 -34.24(19) . . . . ?
Ge1 Si2 Si6 C24 62.23(18) . . . . ?
Si8 Si3 Si7 C27 90.9(4) . . . . ?
Si4 Si3 Si7 C27 -148.4(4) . . . . ?
Si2 Si3 Si7 C27 -39.6(4) . . . . ?
Si8 Si3 Si7 C25 -30.4(2) . . . . ?
Si4 Si3 Si7 C25 90.3(2) . . . . ?
Si2 Si3 Si7 C25 -160.9(2) . . . . ?
Si8 Si3 Si7 C26 -147.5(2) . . . . ?
Si4 Si3 Si7 C26 -26.8(2) . . . . ?
Si2 Si3 Si7 C26 82.0(2) . . . . ?
Si4 Si3 Si8 C28 172.93(17) . . . . ?
Si7 Si3 Si8 C28 -58.56(18) . . . . ?
Si2 Si3 Si8 C28 76.78(18) . . . . ?
Si4 Si3 Si8 C29 -67.48(19) . . . . ?
Si7 Si3 Si8 C29 61.0(2) . . . . ?
Si2 Si3 Si8 C29 -163.62(19) . . . . ?
Si4 Si3 Si8 C30 50.60(18) . . . . ?
Si7 Si3 Si8 C30 179.11(17) . . . . ?
Si2 Si3 Si8 C30 -45.55(18) . . . . ?
Si1 Ge1 C1 C2 4.5(2) . . . . ?
Si4 Ge1 C1 C2 -109.9(2) . . . . ?
Si2 Ge1 C1 C2 133.7(2) . . . . ?
Si1 Ge1 C1 C9 -174.2(3) . . . . ?
Si4 Ge1 C1 C9 71.4(3) . . . . ?
Si2 Ge1 C1 C9 -45.0(4) . . . . ?
C9 C1 C2 C3 -9.6(6) . . . . ?
Ge1 C1 C2 C3 171.8(3) . . . . ?
C9 C1 C2 Si1 173.1(3) . . . . ?
Ge1 C1 C2 Si1 -5.5(3) . . . . ?
C16 Si1 C2 C1 121.8(3) . . . . ?
C15 Si1 C2 C1 -112.9(3) . . . . ?
Ge1 Si1 C2 C1 4.6(2) . . . . ?
C16 Si1 C2 C3 -55.4(4) . . . . ?
C15 Si1 C2 C3 69.9(4) . . . . ?
Ge1 Si1 C2 C3 -172.7(3) . . . . ?
C1 C2 C3 C8 -40.9(6) . . . . ?
Si1 C2 C3 C8 135.8(3) . . . . ?
C1 C2 C3 C4 141.6(4) . . . . ?
Si1 C2 C3 C4 -41.8(5) . . . . ?
C8 C3 C4 C5 1.5(6) . . . . ?
C2 C3 C4 C5 179.2(3) . . . . ?
C3 C4 C5 C6 -0.9(6) . . . . ?
C4 C5 C6 C7 -0.2(6) . . . . ?
C5 C6 C7 C8 0.6(6) . . . . ?
C6 C7 C8 C3 0.1(6) . . . . ?
C4 C3 C8 C7 -1.1(6) . . . . ?
C2 C3 C8 C7 -178.8(4) . . . . ?
C2 C1 C9 C14 137.8(4) . . . . ?
Ge1 C1 C9 C14 -43.8(5) . . . . ?
C2 C1 C9 C10 -48.2(6) . . . . ?
Ge1 C1 C9 C10 130.2(3) . . . . ?
C14 C9 C10 C11 1.7(6) . . . . ?
C1 C9 C10 C11 -172.6(3) . . . . ?
C9 C10 C11 C12 -1.2(6) . . . . ?
C10 C11 C12 C13 -1.0(6) . . . . ?
C11 C12 C13 C14 2.8(7) . . . . ?
C12 C13 C14 C9 -2.3(7) . . . . ?
C10 C9 C14 C13 0.1(6) . . . . ?
C1 C9 C14 C13 174.3(4) . . . . ?

_diffrn_measured_fraction_theta_max 0.990
_diffrn_reflns_theta_full        26.57
_diffrn_measured_fraction_theta_full 0.990
_refine_diff_density_max         1.158
_refine_diff_density_min         -0.457
_refine_diff_density_rms         0.109

# SQUEEZE RESULTS (APPEND TO CIF)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.237 0.695 0.769 11 1 ' '
2 0.208 0.717 0.342 8 0 ' '
3 0.263 0.195 0.731 11 1 ' '
4 0.291 0.217 0.158 8 0 ' '
5 0.708 0.783 0.842 8 0 ' '
6 0.737 0.805 0.269 11 1 ' '
7 0.763 0.305 0.231 11 1 ' '
8 0.791 0.283 0.658 8 0 ' '
_platon_squeeze_details          
;
;

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

data_1098j
_database_code_depnum_ccdc_archive 'CCDC 1450270'
_audit_update_record             
;
2016-01-27 deposited with the CCDC.
2018-03-23 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C26 H68 Ge Si10'
_chemical_formula_weight         734.29

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0817 0.0704 '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           orthorhombic
_symmetry_space_group_name_H-M   Fddd

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

_cell_length_a                   18.093(4)
_cell_length_b                   30.534(6)
_cell_length_c                   32.837(7)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     18141(6)
_cell_formula_units_Z            16
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    23899
_cell_measurement_theta_min      4.535
_cell_measurement_theta_max      52.507

_exptl_crystal_description       plates
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.52
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.40
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.075
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             6336
_exptl_absorpt_coefficient_mu    0.954
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6367
_exptl_absorpt_correction_T_max  0.7014
_exptl_absorpt_process_details   SADABS

_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  'SMART APEX'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            35050
_diffrn_reflns_av_R_equivalents  0.0229
_diffrn_reflns_av_sigmaI/netI    0.0137
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_k_min       -38
_diffrn_reflns_limit_k_max       38
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_theta_min         1.82
_diffrn_reflns_theta_max         26.37
_reflns_number_total             4631
_reflns_number_gt                4432
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker XSCANS'
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_reduction        'Bruker SHELXTL'
_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)+(0.0374P)²+16.6155P] 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         4631
_refine_ls_number_parameters     179
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0230
_refine_ls_R_factor_gt           0.0220
_refine_ls_wR_factor_ref         0.0602
_refine_ls_wR_factor_gt          0.0597
_refine_ls_goodness_of_fit_ref   1.078
_refine_ls_restrained_S_all      1.078
_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 0.3750 0.3750 0.027901(5) 0.01412(6) Uani 1 2 d S . .
Si1 Si 0.417647(17) 0.313262(10) -0.010851(9) 0.01670(8) Uani 1 1 d . . .
Si2 Si 0.539616(17) 0.321967(10) 0.011302(10) 0.01755(8) Uani 1 1 d . . .
Si3 Si 0.611643(19) 0.357187(11) -0.038318(10) 0.02068(8) Uani 1 1 d . . .
Si4 Si 0.596463(19) 0.257973(11) 0.035525(10) 0.02163(8) Uani 1 1 d . . .
Si5 Si 0.467404(18) 0.426493(10) 0.105235(9) 0.01797(8) Uani 1 1 d . . .
C1 C 0.46353(6) 0.38560(4) 0.06233(3) 0.0165(2) Uani 1 1 d . . .
C2 C 0.52610(7) 0.36323(4) 0.05377(4) 0.0190(2) Uani 1 1 d . . .
H2 H 0.5675 0.3688 0.0708 0.023 Uiso 1 1 calc R . .
C3 C 0.37472(7) 0.26009(4) 0.00575(4) 0.0248(3) Uani 1 1 d . . .
H3A H 0.3220 0.2601 -0.0012 0.037 Uiso 1 1 calc R . .
H3B H 0.3805 0.2567 0.0353 0.037 Uiso 1 1 calc R . .
H3C H 0.3993 0.2357 -0.0082 0.037 Uiso 1 1 calc R . .
C4 C 0.40639(7) 0.31739(4) -0.06769(4) 0.0237(3) Uani 1 1 d . . .
H4A H 0.4315 0.2927 -0.0808 0.036 Uiso 1 1 calc R . .
H4B H 0.4281 0.3449 -0.0773 0.036 Uiso 1 1 calc R . .
H4C H 0.3537 0.3167 -0.0746 0.036 Uiso 1 1 calc R . .
C5 C 0.56108(8) 0.40756(4) -0.05553(5) 0.0313(3) Uani 1 1 d . . .
H5A H 0.5949 0.4265 -0.0708 0.047 Uiso 1 1 calc R . .
H5B H 0.5424 0.4234 -0.0317 0.047 Uiso 1 1 calc R . .
H5C H 0.5196 0.3991 -0.0730 0.047 Uiso 1 1 calc R . .
C6 C 0.62929(8) 0.32065(5) -0.08304(4) 0.0319(3) Uani 1 1 d . . .
H6A H 0.6581 0.3366 -0.1035 0.048 Uiso 1 1 calc R . .
H6B H 0.5821 0.3114 -0.0949 0.048 Uiso 1 1 calc R . .
H6C H 0.6570 0.2948 -0.0741 0.048 Uiso 1 1 calc R . .
C7 C 0.70268(8) 0.37470(6) -0.01657(5) 0.0392(4) Uani 1 1 d . . .
H7A H 0.7313 0.3488 -0.0088 0.059 Uiso 1 1 calc R . .
H7B H 0.6942 0.3930 0.0075 0.059 Uiso 1 1 calc R . .
H7C H 0.7301 0.3915 -0.0370 0.059 Uiso 1 1 calc R . .
C8 C 0.59946(9) 0.21639(5) -0.00644(4) 0.0327(3) Uani 1 1 d . . .
H8A H 0.6220 0.1893 0.0037 0.049 Uiso 1 1 calc R . .
H8B H 0.6288 0.2278 -0.0291 0.049 Uiso 1 1 calc R . .
H8C H 0.5491 0.2103 -0.0158 0.049 Uiso 1 1 calc R . .
C9 C 0.69331(8) 0.26980(5) 0.05273(5) 0.0372(3) Uani 1 1 d . . .
H9A H 0.7152 0.2432 0.0642 0.056 Uiso 1 1 calc R . .
H9B H 0.6925 0.2928 0.0736 0.056 Uiso 1 1 calc R . .
H9C H 0.7228 0.2797 0.0295 0.056 Uiso 1 1 calc R . .
C10 C 0.54405(8) 0.23416(5) 0.07956(4) 0.0342(3) Uani 1 1 d . . .
H10A H 0.4947 0.2252 0.0705 0.051 Uiso 1 1 calc R . .
H10B H 0.5394 0.2562 0.1011 0.051 Uiso 1 1 calc R . .
H10C H 0.5706 0.2086 0.0901 0.051 Uiso 1 1 calc R . .
C11 C 0.52530(8) 0.47424(4) 0.08939(4) 0.0296(3) Uani 1 1 d . . .
H11A H 0.5025 0.4886 0.0659 0.044 Uiso 1 1 calc R . .
H11B H 0.5749 0.4640 0.0820 0.044 Uiso 1 1 calc R . .
H11C H 0.5289 0.4951 0.1120 0.044 Uiso 1 1 calc R . .
C12 C 0.51330(8) 0.40154(5) 0.15089(4) 0.0303(3) Uani 1 1 d . . .
H12A H 0.5600 0.3879 0.1426 0.045 Uiso 1 1 calc R . .
H12B H 0.4808 0.3793 0.1627 0.045 Uiso 1 1 calc R . .
H12C H 0.5231 0.4244 0.1711 0.045 Uiso 1 1 calc R . .
C13 C 0.37379(7) 0.44627(5) 0.12041(4) 0.0270(3) Uani 1 1 d . . .
H13A H 0.3788 0.4704 0.1399 0.041 Uiso 1 1 calc R . .
H13B H 0.3462 0.4222 0.1330 0.041 Uiso 1 1 calc R . .
H13C H 0.3472 0.4566 0.0962 0.041 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 C1 1.9870(11) 2 ?
Ge1 C1 1.9870(11) . ?
Ge1 Si1 2.4016(5) 2 ?
Ge1 Si1 2.4017(5) . ?
Si1 C3 1.8805(13) . ?
Si1 C4 1.8819(13) . ?
Si1 Si2 2.3387(6) . ?
Si2 C2 1.8953(12) . ?
Si2 Si4 2.3470(6) . ?
Si2 Si3 2.3473(5) . ?
Si3 C6 1.8716(14) . ?
Si3 C7 1.8733(15) . ?
Si3 C5 1.8767(14) . ?
Si4 C8 1.8747(14) . ?
Si4 C10 1.8759(14) . ?
Si4 C9 1.8762(15) . ?
Si5 C13 1.8658(14) . ?
Si5 C11 1.8691(13) . ?
Si5 C12 1.8755(14) . ?
Si5 C1 1.8839(12) . ?
C1 C2 1.3518(17) . ?

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 C1 110.65(7) 2 . ?
C1 Ge1 Si1 99.81(4) 2 2 ?
C1 Ge1 Si1 115.63(3) . 2 ?
C1 Ge1 Si1 115.63(3) 2 . ?
C1 Ge1 Si1 99.81(4) . . ?
Si1 Ge1 Si1 116.01(2) 2 . ?
C3 Si1 C4 107.50(6) . . ?
C3 Si1 Si2 113.43(5) . . ?
C4 Si1 Si2 113.77(4) . . ?
C3 Si1 Ge1 113.04(4) . . ?
C4 Si1 Ge1 115.99(4) . . ?
Si2 Si1 Ge1 92.817(16) . . ?
C2 Si2 Si1 100.53(4) . . ?
C2 Si2 Si4 111.14(4) . . ?
Si1 Si2 Si4 115.106(19) . . ?
C2 Si2 Si3 106.13(4) . . ?
Si1 Si2 Si3 111.10(2) . . ?
Si4 Si2 Si3 111.92(2) . . ?
C6 Si3 C7 108.62(7) . . ?
C6 Si3 C5 109.60(7) . . ?
C7 Si3 C5 108.03(7) . . ?
C6 Si3 Si2 111.48(5) . . ?
C7 Si3 Si2 110.75(5) . . ?
C5 Si3 Si2 108.29(5) . . ?
C8 Si4 C10 108.59(7) . . ?
C8 Si4 C9 108.95(7) . . ?
C10 Si4 C9 108.34(7) . . ?
C8 Si4 Si2 109.11(5) . . ?
C10 Si4 Si2 111.25(5) . . ?
C9 Si4 Si2 110.55(5) . . ?
C13 Si5 C11 109.31(7) . . ?
C13 Si5 C12 108.66(7) . . ?
C11 Si5 C12 106.93(7) . . ?
C13 Si5 C1 112.36(6) . . ?
C11 Si5 C1 109.25(6) . . ?
C12 Si5 C1 110.19(6) . . ?
C2 C1 Si5 117.33(9) . . ?
C2 C1 Ge1 118.33(9) . . ?
Si5 C1 Ge1 124.30(6) . . ?
C1 C2 Si2 126.64(9) . . ?

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
C1 Ge1 Si1 C3 -13.19(6) 2 . . . ?
C1 Ge1 Si1 C3 105.48(6) . . . . ?
Si1 Ge1 Si1 C3 -129.58(5) 2 . . . ?
C1 Ge1 Si1 C4 111.61(6) 2 . . . ?
C1 Ge1 Si1 C4 -129.71(6) . . . . ?
Si1 Ge1 Si1 C4 -4.77(5) 2 . . . ?
C1 Ge1 Si1 Si2 -130.17(4) 2 . . . ?
C1 Ge1 Si1 Si2 -11.49(3) . . . . ?
Si1 Ge1 Si1 Si2 113.449(14) 2 . . . ?
C3 Si1 Si2 C2 -105.08(6) . . . . ?
C4 Si1 Si2 C2 131.63(6) . . . . ?
Ge1 Si1 Si2 C2 11.56(4) . . . . ?
C3 Si1 Si2 Si4 14.40(5) . . . . ?
C4 Si1 Si2 Si4 -108.90(5) . . . . ?
Ge1 Si1 Si2 Si4 131.04(2) . . . . ?
C3 Si1 Si2 Si3 142.92(5) . . . . ?
C4 Si1 Si2 Si3 19.62(5) . . . . ?
Ge1 Si1 Si2 Si3 -100.44(2) . . . . ?
C2 Si2 Si3 C6 -179.39(6) . . . . ?
Si1 Si2 Si3 C6 -71.00(6) . . . . ?
Si4 Si2 Si3 C6 59.21(6) . . . . ?
C2 Si2 Si3 C7 59.54(7) . . . . ?
Si1 Si2 Si3 C7 167.93(6) . . . . ?
Si4 Si2 Si3 C7 -61.86(6) . . . . ?
C2 Si2 Si3 C5 -58.74(6) . . . . ?
Si1 Si2 Si3 C5 49.65(5) . . . . ?
Si4 Si2 Si3 C5 179.86(5) . . . . ?
C2 Si2 Si4 C8 174.23(6) . . . . ?
Si1 Si2 Si4 C8 60.81(5) . . . . ?
Si3 Si2 Si4 C8 -67.30(6) . . . . ?
C2 Si2 Si4 C10 54.45(7) . . . . ?
Si1 Si2 Si4 C10 -58.97(6) . . . . ?
Si3 Si2 Si4 C10 172.92(6) . . . . ?
C2 Si2 Si4 C9 -65.97(7) . . . . ?
Si1 Si2 Si4 C9 -179.39(6) . . . . ?
Si3 Si2 Si4 C9 52.51(6) . . . . ?
C13 Si5 C1 C2 -168.33(10) . . . . ?
C11 Si5 C1 C2 70.19(11) . . . . ?
C12 Si5 C1 C2 -47.01(11) . . . . ?
C13 Si5 C1 Ge1 13.97(9) . . . . ?
C11 Si5 C1 Ge1 -107.52(8) . . . . ?
C12 Si5 C1 Ge1 135.28(7) . . . . ?
C1 Ge1 C1 C2 131.29(11) 2 . . . ?
Si1 Ge1 C1 C2 -116.20(9) 2 . . . ?
Si1 Ge1 C1 C2 9.00(10) . . . . ?
C1 Ge1 C1 Si5 -51.02(5) 2 . . . ?
Si1 Ge1 C1 Si5 61.48(7) 2 . . . ?
Si1 Ge1 C1 Si5 -173.31(6) . . . . ?
Si5 C1 C2 Si2 -177.45(6) . . . . ?
Ge1 C1 C2 Si2 0.40(15) . . . . ?
Si1 Si2 C2 C1 -9.83(11) . . . . ?
Si4 Si2 C2 C1 -132.14(10) . . . . ?
Si3 Si2 C2 C1 105.95(11) . . . . ?

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        26.37
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         0.492
_refine_diff_density_min         -0.201
_refine_diff_density_rms         0.051

# SQUEEZE RESULTS (APPEND TO CIF)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.875 0.072 0.375 16 0 ' '
2 0.375 0.072 0.875 16 0 ' '
3 0.625 0.125 0.125 154 3 ' '
4 0.125 0.125 0.625 154 3 ' '
5 0.625 0.125 0.295 20 0 ' '
6 0.125 0.125 0.455 19 0 ' '
7 0.125 0.125 0.795 20 0 ' '
8 0.625 0.125 0.955 19 0 ' '
9 0.375 0.178 0.375 16 0 ' '
10 0.875 0.178 0.875 16 0 ' '
11 0.625 0.322 0.125 16 0 ' '
12 0.125 0.322 0.625 16 0 ' '
13 0.375 0.375 0.375 154 3 ' '
14 0.875 0.375 0.875 154 3 ' '
15 0.875 0.375 0.045 20 0 ' '
16 0.375 0.375 0.205 19 0 ' '
17 0.375 0.375 0.545 20 0 ' '
18 0.875 0.375 0.705 19 0 ' '
19 0.125 0.428 0.125 16 0 ' '
20 0.625 0.428 0.625 16 0 ' '
21 0.375 0.572 0.375 16 0 ' '
22 0.875 0.572 0.875 16 0 ' '
23 0.125 0.625 0.125 154 3 ' '
24 0.625 0.625 0.625 154 3 ' '
25 0.125 0.625 0.295 20 0 ' '
26 0.625 0.625 0.455 19 0 ' '
27 0.625 0.625 0.795 20 0 ' '
28 0.125 0.625 0.955 19 0 ' '
29 0.875 0.678 0.375 16 0 ' '
30 0.375 0.678 0.875 16 0 ' '
31 0.125 0.822 0.125 16 0 ' '
32 0.625 0.822 0.625 16 0 ' '
33 0.875 0.875 0.375 154 3 ' '
34 0.375 0.875 0.875 154 3 ' '
35 0.375 0.875 0.045 20 0 ' '
36 0.875 0.875 0.205 19 0 ' '
37 0.875 0.875 0.545 20 0 ' '
38 0.375 0.875 0.705 19 0 ' '
39 0.625 0.928 0.125 16 0 ' '
40 0.125 0.928 0.625 16 0 ' '
_platon_squeeze_details          
;
;


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

data_1026j
_database_code_depnum_ccdc_archive 'CCDC 1450265'
_audit_update_record             
;
2016-01-27 deposited with the CCDC.
2018-03-23 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C32 H60 Ge Si8'
_chemical_formula_weight         742.11

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'
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   P2(1)/n

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

_cell_length_a                   9.7118(19)
_cell_length_b                   27.874(6)
_cell_length_c                   16.028(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 98.49(3)
_cell_angle_gamma                90.00
_cell_volume                     4291.5(15)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    12204
_cell_measurement_theta_min      4.597
_cell_measurement_theta_max      52.507

_exptl_crystal_description       plates
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.149
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1584
_exptl_absorpt_coefficient_mu    0.957
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7623
_exptl_absorpt_correction_T_max  0.9104
_exptl_absorpt_process_details   SADABS

_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  'SMART APEX'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            34044
_diffrn_reflns_av_R_equivalents  0.0543
_diffrn_reflns_av_sigmaI/netI    0.0515
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         1.46
_diffrn_reflns_theta_max         26.37
_reflns_number_total             8740
_reflns_number_gt                8275
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker XSCANS'
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_reduction        'Bruker SHELXTL'
_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)+(0.0275P)²+15.7250P] 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         8740
_refine_ls_number_parameters     386
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0933
_refine_ls_R_factor_gt           0.0871
_refine_ls_wR_factor_ref         0.1548
_refine_ls_wR_factor_gt          0.1525
_refine_ls_goodness_of_fit_ref   1.394
_refine_ls_restrained_S_all      1.394
_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 0.37634(5) 0.135301(18) 0.62430(3) 0.01166(13) Uani 1 1 d . . .
Si1 Si 0.49292(14) 0.06096(5) 0.65997(8) 0.0140(3) Uani 1 1 d . . .
Si2 Si 0.48133(14) 0.06005(5) 0.80394(8) 0.0140(3) Uani 1 1 d . . .
Si3 Si 0.24524(14) 0.07677(5) 0.81035(8) 0.0137(3) Uani 1 1 d . . .
Si4 Si 0.22608(15) 0.13002(5) 0.92125(9) 0.0194(3) Uani 1 1 d . . .
Si5 Si 0.12566(15) 0.00474(5) 0.82816(9) 0.0177(3) Uani 1 1 d . . .
Si6 Si 0.46961(14) 0.21610(5) 0.64093(8) 0.0152(3) Uani 1 1 d . . .
Si7 Si 0.69921(14) 0.23179(5) 0.70506(9) 0.0175(3) Uani 1 1 d . . .
Si8 Si 0.31889(15) 0.28137(5) 0.65530(9) 0.0207(3) Uani 1 1 d . . .
C1 C 0.3845(5) 0.01327(19) 0.5984(3) 0.0218(11) Uani 1 1 d . . .
H1A H 0.3848 0.0183 0.5379 0.033 Uiso 1 1 calc R . .
H1B H 0.2887 0.0150 0.6107 0.033 Uiso 1 1 calc R . .
H1C H 0.4235 -0.0184 0.6145 0.033 Uiso 1 1 calc R . .
C2 C 0.6703(5) 0.05837(19) 0.6274(3) 0.0215(11) Uani 1 1 d . . .
H2A H 0.7061 0.0255 0.6338 0.032 Uiso 1 1 calc R . .
H2B H 0.7332 0.0800 0.6630 0.032 Uiso 1 1 calc R . .
H2C H 0.6644 0.0683 0.5683 0.032 Uiso 1 1 calc R . .
C3 C 0.6023(5) 0.1079(2) 0.8544(3) 0.0245(12) Uani 1 1 d . . .
H3A H 0.5958 0.1097 0.9148 0.037 Uiso 1 1 calc R . .
H3B H 0.5761 0.1389 0.8279 0.037 Uiso 1 1 calc R . .
H3C H 0.6981 0.1001 0.8469 0.037 Uiso 1 1 calc R . .
C4 C 0.5328(6) 0.00285(19) 0.8631(3) 0.0216(11) Uani 1 1 d . . .
H4A H 0.6323 -0.0031 0.8634 0.032 Uiso 1 1 calc R . .
H4B H 0.4790 -0.0240 0.8353 0.032 Uiso 1 1 calc R . .
H4C H 0.5138 0.0058 0.9212 0.032 Uiso 1 1 calc R . .
C5 C 0.2974(9) 0.1004(2) 1.0223(4) 0.052(2) Uani 1 1 d . . .
H5A H 0.3071 0.1241 1.0679 0.078 Uiso 1 1 calc R . .
H5B H 0.3888 0.0866 1.0177 0.078 Uiso 1 1 calc R . .
H5C H 0.2340 0.0749 1.0346 0.078 Uiso 1 1 calc R . .
C6 C 0.0425(7) 0.1485(3) 0.9249(5) 0.050(2) Uani 1 1 d . . .
H6A H -0.0122 0.1204 0.9366 0.075 Uiso 1 1 calc R . .
H6B H 0.0028 0.1624 0.8704 0.075 Uiso 1 1 calc R . .
H6C H 0.0404 0.1724 0.9695 0.075 Uiso 1 1 calc R . .
C7 C 0.3305(7) 0.1855(2) 0.9079(4) 0.0357(15) Uani 1 1 d . . .
H7A H 0.2884 0.2130 0.9327 0.054 Uiso 1 1 calc R . .
H7B H 0.3313 0.1914 0.8477 0.054 Uiso 1 1 calc R . .
H7C H 0.4261 0.1811 0.9363 0.054 Uiso 1 1 calc R . .
C8 C 0.1941(6) -0.0299(2) 0.9260(4) 0.0328(14) Uani 1 1 d . . .
H8A H 0.1323 -0.0570 0.9321 0.049 Uiso 1 1 calc R . .
H8B H 0.1980 -0.0089 0.9754 0.049 Uiso 1 1 calc R . .
H8C H 0.2877 -0.0418 0.9218 0.049 Uiso 1 1 calc R . .
C9 C -0.0621(5) 0.0181(2) 0.8343(4) 0.0269(13) Uani 1 1 d . . .
H9A H -0.1019 0.0369 0.7848 0.040 Uiso 1 1 calc R . .
H9B H -0.0689 0.0365 0.8856 0.040 Uiso 1 1 calc R . .
H9C H -0.1136 -0.0121 0.8356 0.040 Uiso 1 1 calc R . .
C10 C 0.1325(6) -0.03431(19) 0.7338(3) 0.0239(12) Uani 1 1 d . . .
H10A H 0.0751 -0.0629 0.7377 0.036 Uiso 1 1 calc R . .
H10B H 0.2290 -0.0440 0.7318 0.036 Uiso 1 1 calc R . .
H10C H 0.0969 -0.0165 0.6824 0.036 Uiso 1 1 calc R . .
C11 C 0.1453(5) 0.10139(17) 0.7094(3) 0.0154(10) Uani 1 1 d . . .
H11 H 0.0473 0.0987 0.7074 0.019 Uiso 1 1 calc R . .
C12 C 0.1808(5) 0.12180(17) 0.6398(3) 0.0149(10) Uani 1 1 d . . .
C13 C 0.0718(5) 0.13256(18) 0.5666(3) 0.0171(10) Uani 1 1 d . . .
C14 C -0.0291(5) 0.0983(2) 0.5373(3) 0.0205(11) Uani 1 1 d . . .
H14 H -0.0290 0.0681 0.5649 0.025 Uiso 1 1 calc R . .
C15 C -0.1294(6) 0.1079(2) 0.4682(3) 0.0299(14) Uani 1 1 d . . .
H15 H -0.1966 0.0842 0.4485 0.036 Uiso 1 1 calc R . .
C16 C -0.1321(6) 0.1515(2) 0.4280(4) 0.0345(15) Uani 1 1 d . . .
H16 H -0.2013 0.1581 0.3811 0.041 Uiso 1 1 calc R . .
C17 C -0.0329(6) 0.1860(2) 0.4567(4) 0.0319(14) Uani 1 1 d . . .
H17 H -0.0347 0.2163 0.4295 0.038 Uiso 1 1 calc R . .
C18 C 0.0681(5) 0.17627(19) 0.5245(3) 0.0206(11) Uani 1 1 d . . .
H18 H 0.1365 0.1999 0.5427 0.025 Uiso 1 1 calc R . .
C19 C 0.4074(5) 0.15803(17) 0.5101(3) 0.0117(9) Uani 1 1 d . . .
C20 C 0.4664(5) 0.20143(18) 0.5255(3) 0.0167(10) Uani 1 1 d . . .
H20 H 0.5007 0.2214 0.4851 0.020 Uiso 1 1 calc R . .
C21 C 0.3830(5) 0.13274(17) 0.4279(3) 0.0150(10) Uani 1 1 d . . .
C22 C 0.2760(5) 0.09984(19) 0.4097(3) 0.0217(11) Uani 1 1 d . . .
H22 H 0.2200 0.0921 0.4516 0.026 Uiso 1 1 calc R . .
C23 C 0.2495(6) 0.0781(2) 0.3318(3) 0.0253(12) Uani 1 1 d . . .
H23 H 0.1741 0.0563 0.3201 0.030 Uiso 1 1 calc R . .
C24 C 0.3320(6) 0.0880(2) 0.2703(3) 0.0270(13) Uani 1 1 d . . .
H24 H 0.3131 0.0734 0.2163 0.032 Uiso 1 1 calc R . .
C25 C 0.4426(7) 0.1196(2) 0.2886(4) 0.0309(14) Uani 1 1 d . . .
H25 H 0.5014 0.1258 0.2475 0.037 Uiso 1 1 calc R . .
C26 C 0.4681(6) 0.14218(18) 0.3660(3) 0.0218(11) Uani 1 1 d . . .
H26 H 0.5432 0.1642 0.3774 0.026 Uiso 1 1 calc R . .
C27 C 0.8132(6) 0.1789(2) 0.6946(4) 0.0292(13) Uani 1 1 d . . .
H27A H 0.7965 0.1671 0.6363 0.044 Uiso 1 1 calc R . .
H27B H 0.7921 0.1534 0.7329 0.044 Uiso 1 1 calc R . .
H27C H 0.9111 0.1883 0.7089 0.044 Uiso 1 1 calc R . .
C28 C 0.7141(6) 0.2490(2) 0.8190(3) 0.0275(13) Uani 1 1 d . . .
H28A H 0.8126 0.2520 0.8429 0.041 Uiso 1 1 calc R . .
H28B H 0.6704 0.2243 0.8498 0.041 Uiso 1 1 calc R . .
H28C H 0.6671 0.2798 0.8240 0.041 Uiso 1 1 calc R . .
C29 C 0.1851(6) 0.2661(2) 0.7245(4) 0.0359(15) Uani 1 1 d . . .
H29A H 0.1186 0.2926 0.7237 0.054 Uiso 1 1 calc R . .
H29B H 0.2312 0.2608 0.7824 0.054 Uiso 1 1 calc R . .
H29C H 0.1355 0.2369 0.7035 0.054 Uiso 1 1 calc R . .
C30 C 0.7622(6) 0.2824(2) 0.6440(4) 0.0323(14) Uani 1 1 d . . .
H30A H 0.8601 0.2891 0.6657 0.049 Uiso 1 1 calc R . .
H30B H 0.7062 0.3111 0.6501 0.049 Uiso 1 1 calc R . .
H30C H 0.7536 0.2736 0.5843 0.049 Uiso 1 1 calc R . .
C31 C 0.4196(7) 0.3351(2) 0.7007(4) 0.0371(15) Uani 1 1 d . . .
H31A H 0.4855 0.3449 0.6630 0.056 Uiso 1 1 calc R . .
H31B H 0.4708 0.3270 0.7562 0.056 Uiso 1 1 calc R . .
H31C H 0.3552 0.3616 0.7064 0.056 Uiso 1 1 calc R . .
C32 C 0.2271(7) 0.3009(2) 0.5493(4) 0.0343(15) Uani 1 1 d . . .
H32A H 0.1689 0.3290 0.5562 0.052 Uiso 1 1 calc R . .
H32B H 0.1684 0.2747 0.5235 0.052 Uiso 1 1 calc R . .
H32C H 0.2960 0.3093 0.5128 0.052 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 C12 1.987(5) . ?
Ge1 C19 2.001(5) . ?
Ge1 Si1 2.3899(15) . ?
Ge1 Si6 2.4276(15) . ?
Si1 C2 1.874(5) . ?
Si1 C1 1.882(5) . ?
Si1 Si2 2.3271(19) . ?
Si2 C3 1.880(5) . ?
Si2 C4 1.884(5) . ?
Si2 Si3 2.3568(19) . ?
Si3 C11 1.889(5) . ?
Si3 Si4 2.3441(19) . ?
Si3 Si5 2.358(2) . ?
Si4 C5 1.858(6) . ?
Si4 C6 1.865(6) . ?
Si4 C7 1.879(6) . ?
Si5 C10 1.873(5) . ?
Si5 C8 1.878(6) . ?
Si5 C9 1.878(5) . ?
Si6 C20 1.891(5) . ?
Si6 Si7 2.354(2) . ?
Si6 Si8 2.367(2) . ?
Si7 C27 1.867(6) . ?
Si7 C30 1.871(6) . ?
Si7 C28 1.873(6) . ?
Si8 C31 1.876(6) . ?
Si8 C29 1.878(6) . ?
Si8 C32 1.880(6) . ?
C11 C12 1.342(7) . ?
C12 C13 1.490(7) . ?
C13 C18 1.391(7) . ?
C13 C14 1.399(7) . ?
C14 C15 1.389(7) . ?
C15 C16 1.374(9) . ?
C16 C17 1.390(9) . ?
C17 C18 1.379(7) . ?
C19 C20 1.346(7) . ?
C19 C21 1.483(6) . ?
C21 C22 1.384(7) . ?
C21 C26 1.407(7) . ?
C22 C23 1.377(7) . ?
C23 C24 1.387(8) . ?
C24 C25 1.386(8) . ?
C25 C26 1.380(8) . ?

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
C12 Ge1 C19 116.7(2) . . ?
C12 Ge1 Si1 103.51(14) . . ?
C19 Ge1 Si1 111.31(14) . . ?
C12 Ge1 Si6 120.67(14) . . ?
C19 Ge1 Si6 72.70(14) . . ?
Si1 Ge1 Si6 128.48(5) . . ?
C2 Si1 C1 107.0(2) . . ?
C2 Si1 Si2 117.20(18) . . ?
C1 Si1 Si2 114.01(18) . . ?
C2 Si1 Ge1 112.91(18) . . ?
C1 Si1 Ge1 106.16(17) . . ?
Si2 Si1 Ge1 98.98(6) . . ?
C3 Si2 C4 106.3(2) . . ?
C3 Si2 Si1 107.49(19) . . ?
C4 Si2 Si1 117.38(18) . . ?
C3 Si2 Si3 113.03(18) . . ?
C4 Si2 Si3 109.44(18) . . ?
Si1 Si2 Si3 103.35(7) . . ?
C11 Si3 Si4 109.35(16) . . ?
C11 Si3 Si2 114.50(16) . . ?
Si4 Si3 Si2 110.18(8) . . ?
C11 Si3 Si5 102.30(16) . . ?
Si4 Si3 Si5 110.59(7) . . ?
Si2 Si3 Si5 109.67(7) . . ?
C5 Si4 C6 109.3(4) . . ?
C5 Si4 C7 109.1(3) . . ?
C6 Si4 C7 108.1(3) . . ?
C5 Si4 Si3 108.6(2) . . ?
C6 Si4 Si3 112.4(2) . . ?
C7 Si4 Si3 109.3(2) . . ?
C10 Si5 C8 109.0(3) . . ?
C10 Si5 C9 107.9(3) . . ?
C8 Si5 C9 106.6(3) . . ?
C10 Si5 Si3 108.69(18) . . ?
C8 Si5 Si3 114.8(2) . . ?
C9 Si5 Si3 109.7(2) . . ?
C20 Si6 Si7 110.19(17) . . ?
C20 Si6 Si8 109.89(17) . . ?
Si7 Si6 Si8 111.97(7) . . ?
C20 Si6 Ge1 74.92(16) . . ?
Si7 Si6 Ge1 122.30(7) . . ?
Si8 Si6 Ge1 119.84(7) . . ?
C27 Si7 C30 107.7(3) . . ?
C27 Si7 C28 109.2(3) . . ?
C30 Si7 C28 109.4(3) . . ?
C27 Si7 Si6 110.49(19) . . ?
C30 Si7 Si6 105.9(2) . . ?
C28 Si7 Si6 113.9(2) . . ?
C31 Si8 C29 108.6(3) . . ?
C31 Si8 C32 105.6(3) . . ?
C29 Si8 C32 108.8(3) . . ?
C31 Si8 Si6 110.9(2) . . ?
C29 Si8 Si6 112.0(2) . . ?
C32 Si8 Si6 110.7(2) . . ?
C12 C11 Si3 134.7(4) . . ?
C11 C12 C13 120.0(4) . . ?
C11 C12 Ge1 123.5(4) . . ?
C13 C12 Ge1 116.4(3) . . ?
C18 C13 C14 118.0(5) . . ?
C18 C13 C12 121.5(5) . . ?
C14 C13 C12 120.5(4) . . ?
C15 C14 C13 120.6(5) . . ?
C16 C15 C14 120.5(5) . . ?
C15 C16 C17 119.5(5) . . ?
C18 C17 C16 120.1(5) . . ?
C17 C18 C13 121.3(5) . . ?
C20 C19 C21 126.7(4) . . ?
C20 C19 Ge1 103.6(3) . . ?
C21 C19 Ge1 129.6(3) . . ?
C19 C20 Si6 108.6(4) . . ?
C22 C21 C26 118.4(5) . . ?
C22 C21 C19 121.2(4) . . ?
C26 C21 C19 120.3(4) . . ?
C23 C22 C21 121.1(5) . . ?
C22 C23 C24 120.5(5) . . ?
C25 C24 C23 119.1(5) . . ?
C26 C25 C24 120.7(5) . . ?
C25 C26 C21 120.2(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
C12 Ge1 Si1 C2 166.6(2) . . . . ?
C19 Ge1 Si1 C2 40.5(2) . . . . ?
Si6 Ge1 Si1 C2 -43.9(2) . . . . ?
C12 Ge1 Si1 C1 49.7(2) . . . . ?
C19 Ge1 Si1 C1 -76.5(2) . . . . ?
Si6 Ge1 Si1 C1 -160.90(18) . . . . ?
C12 Ge1 Si1 Si2 -68.67(16) . . . . ?
C19 Ge1 Si1 Si2 165.15(15) . . . . ?
Si6 Ge1 Si1 Si2 80.76(8) . . . . ?
C2 Si1 Si2 C3 51.2(3) . . . . ?
C1 Si1 Si2 C3 177.3(3) . . . . ?
Ge1 Si1 Si2 C3 -70.45(19) . . . . ?
C2 Si1 Si2 C4 -68.5(3) . . . . ?
C1 Si1 Si2 C4 57.6(3) . . . . ?
Ge1 Si1 Si2 C4 169.8(2) . . . . ?
C2 Si1 Si2 Si3 170.9(2) . . . . ?
C1 Si1 Si2 Si3 -63.0(2) . . . . ?
Ge1 Si1 Si2 Si3 49.31(7) . . . . ?
C3 Si2 Si3 C11 100.9(3) . . . . ?
C4 Si2 Si3 C11 -140.8(2) . . . . ?
Si1 Si2 Si3 C11 -14.99(19) . . . . ?
C3 Si2 Si3 Si4 -22.8(2) . . . . ?
C4 Si2 Si3 Si4 95.48(19) . . . . ?
Si1 Si2 Si3 Si4 -138.72(7) . . . . ?
C3 Si2 Si3 Si5 -144.8(2) . . . . ?
C4 Si2 Si3 Si5 -26.5(2) . . . . ?
Si1 Si2 Si3 Si5 99.32(8) . . . . ?
C11 Si3 Si4 C5 170.0(3) . . . . ?
Si2 Si3 Si4 C5 -63.3(3) . . . . ?
Si5 Si3 Si4 C5 58.1(3) . . . . ?
C11 Si3 Si4 C6 48.9(3) . . . . ?
Si2 Si3 Si4 C6 175.6(3) . . . . ?
Si5 Si3 Si4 C6 -63.0(3) . . . . ?
C11 Si3 Si4 C7 -71.1(3) . . . . ?
Si2 Si3 Si4 C7 55.6(2) . . . . ?
Si5 Si3 Si4 C7 177.0(2) . . . . ?
C11 Si3 Si5 C10 59.2(3) . . . . ?
Si4 Si3 Si5 C10 175.6(2) . . . . ?
Si2 Si3 Si5 C10 -62.7(2) . . . . ?
C11 Si3 Si5 C8 -178.5(3) . . . . ?
Si4 Si3 Si5 C8 -62.1(2) . . . . ?
Si2 Si3 Si5 C8 59.6(2) . . . . ?
C11 Si3 Si5 C9 -58.6(3) . . . . ?
Si4 Si3 Si5 C9 57.8(2) . . . . ?
Si2 Si3 Si5 C9 179.5(2) . . . . ?
C12 Ge1 Si6 C20 -113.8(2) . . . . ?
C19 Ge1 Si6 C20 -2.6(2) . . . . ?
Si1 Ge1 Si6 C20 101.24(17) . . . . ?
C12 Ge1 Si6 Si7 141.52(18) . . . . ?
C19 Ge1 Si6 Si7 -107.20(16) . . . . ?
Si1 Ge1 Si6 Si7 -3.39(11) . . . . ?
C12 Ge1 Si6 Si8 -9.27(19) . . . . ?
C19 Ge1 Si6 Si8 102.01(15) . . . . ?
Si1 Ge1 Si6 Si8 -154.19(7) . . . . ?
C20 Si6 Si7 C27 -58.8(3) . . . . ?
Si8 Si6 Si7 C27 178.6(2) . . . . ?
Ge1 Si6 Si7 C27 25.7(2) . . . . ?
C20 Si6 Si7 C30 57.6(3) . . . . ?
Si8 Si6 Si7 C30 -65.0(2) . . . . ?
Ge1 Si6 Si7 C30 142.1(2) . . . . ?
C20 Si6 Si7 C28 177.9(3) . . . . ?
Si8 Si6 Si7 C28 55.2(2) . . . . ?
Ge1 Si6 Si7 C28 -97.6(2) . . . . ?
C20 Si6 Si8 C31 -114.4(3) . . . . ?
Si7 Si6 Si8 C31 8.4(3) . . . . ?
Ge1 Si6 Si8 C31 162.0(2) . . . . ?
C20 Si6 Si8 C29 124.1(3) . . . . ?
Si7 Si6 Si8 C29 -113.1(2) . . . . ?
Ge1 Si6 Si8 C29 40.5(2) . . . . ?
C20 Si6 Si8 C32 2.5(3) . . . . ?
Si7 Si6 Si8 C32 125.3(2) . . . . ?
Ge1 Si6 Si8 C32 -81.1(2) . . . . ?
Si4 Si3 C11 C12 106.3(5) . . . . ?
Si2 Si3 C11 C12 -17.9(6) . . . . ?
Si5 Si3 C11 C12 -136.5(5) . . . . ?
Si3 C11 C12 C13 173.4(4) . . . . ?
Si3 C11 C12 Ge1 -2.4(7) . . . . ?
C19 Ge1 C12 C11 172.4(4) . . . . ?
Si1 Ge1 C12 C11 49.7(4) . . . . ?
Si6 Ge1 C12 C11 -102.7(4) . . . . ?
C19 Ge1 C12 C13 -3.7(4) . . . . ?
Si1 Ge1 C12 C13 -126.3(3) . . . . ?
Si6 Ge1 C12 C13 81.3(4) . . . . ?
C11 C12 C13 C18 135.0(5) . . . . ?
Ge1 C12 C13 C18 -48.8(6) . . . . ?
C11 C12 C13 C14 -46.1(7) . . . . ?
Ge1 C12 C13 C14 130.0(4) . . . . ?
C18 C13 C14 C15 0.0(7) . . . . ?
C12 C13 C14 C15 -178.9(5) . . . . ?
C13 C14 C15 C16 -0.8(8) . . . . ?
C14 C15 C16 C17 0.5(9) . . . . ?
C15 C16 C17 C18 0.5(9) . . . . ?
C16 C17 C18 C13 -1.3(9) . . . . ?
C14 C13 C18 C17 1.0(8) . . . . ?
C12 C13 C18 C17 179.9(5) . . . . ?
C12 Ge1 C19 C20 119.8(3) . . . . ?
Si1 Ge1 C19 C20 -121.7(3) . . . . ?
Si6 Ge1 C19 C20 3.6(3) . . . . ?
C12 Ge1 C19 C21 -64.6(5) . . . . ?
Si1 Ge1 C19 C21 53.9(4) . . . . ?
Si6 Ge1 C19 C21 179.2(4) . . . . ?
C21 C19 C20 Si6 179.6(4) . . . . ?
Ge1 C19 C20 Si6 -4.6(4) . . . . ?
Si7 Si6 C20 C19 123.2(3) . . . . ?
Si8 Si6 C20 C19 -112.9(3) . . . . ?
Ge1 Si6 C20 C19 3.8(3) . . . . ?
C20 C19 C21 C22 -152.9(5) . . . . ?
Ge1 C19 C21 C22 32.4(7) . . . . ?
C20 C19 C21 C26 26.4(7) . . . . ?
Ge1 C19 C21 C26 -148.3(4) . . . . ?
C26 C21 C22 C23 -2.5(8) . . . . ?
C19 C21 C22 C23 176.8(5) . . . . ?
C21 C22 C23 C24 1.6(8) . . . . ?
C22 C23 C24 C25 0.7(9) . . . . ?
C23 C24 C25 C26 -2.0(9) . . . . ?
C24 C25 C26 C21 1.0(9) . . . . ?
C22 C21 C26 C25 1.2(8) . . . . ?
C19 C21 C26 C25 -178.1(5) . . . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        26.37
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.798
_refine_diff_density_min         -0.766
_refine_diff_density_rms         0.106

# SQUEEZE RESULTS (APPEND TO CIF)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.119 0.012 0.461 11 1 ' '
2 0.381 0.512 0.039 11 1 ' '
3 0.619 0.488 0.961 11 1 ' '
4 0.881 0.988 0.539 11 1 ' '
_platon_squeeze_details          
;
;


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

data_1103j
_database_code_depnum_ccdc_archive 'CCDC 1450271'
_audit_update_record             
;
2016-01-27 deposited with the CCDC.
2018-03-23 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C30 H58 Ge3 Si6'
_chemical_formula_weight         805.07

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'
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   P2(1)/n

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

_cell_length_a                   10.817(3)
_cell_length_b                   35.902(9)
_cell_length_c                   10.823(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 96.083(5)
_cell_angle_gamma                90.00
_cell_volume                     4179.6(19)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    5995
_cell_measurement_theta_min      4.400
_cell_measurement_theta_max      5.375

_exptl_crystal_description       blocks
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.04
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.279
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1672
_exptl_absorpt_coefficient_mu    2.333
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6278
_exptl_absorpt_correction_T_max  0.9124
_exptl_absorpt_process_details   SADABS

_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  'SMART APEX'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            33243
_diffrn_reflns_av_R_equivalents  0.0948
_diffrn_reflns_av_sigmaI/netI    0.0859
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -44
_diffrn_reflns_limit_k_max       44
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         1.98
_diffrn_reflns_theta_max         26.38
_reflns_number_total             8542
_reflns_number_gt                6742
_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)+(0.0756P)²+15.8027P] 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         8542
_refine_ls_number_parameters     368
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.1116
_refine_ls_R_factor_gt           0.0894
_refine_ls_wR_factor_ref         0.1923
_refine_ls_wR_factor_gt          0.1831
_refine_ls_goodness_of_fit_ref   1.182
_refine_ls_restrained_S_all      1.183
_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 0.71222(7) 0.07847(2) 0.31188(7) 0.01506(19) Uani 1 1 d . . .
Ge2 Ge 0.61640(7) 0.13517(2) 0.21571(7) 0.0170(2) Uani 1 1 d . . .
Ge3 Ge 0.67454(7) 0.16474(2) 0.42025(7) 0.0175(2) Uani 1 1 d . . .
Si1 Si 0.89908(18) 0.04722(6) 0.27731(19) 0.0180(4) Uani 1 1 d . . .
Si2 Si 0.68965(18) 0.10415(6) 0.51221(18) 0.0176(4) Uani 1 1 d . . .
Si3 Si 0.3991(2) 0.12551(6) 0.1570(2) 0.0257(5) Uani 1 1 d . . .
Si4 Si 0.6956(2) 0.16304(6) 0.03935(19) 0.0253(5) Uani 1 1 d . . .
Si5 Si 0.8816(2) 0.18772(6) 0.4313(2) 0.0251(5) Uani 1 1 d . . .
Si6 Si 0.5395(2) 0.20998(6) 0.4956(2) 0.0253(5) Uani 1 1 d . . .
C1 C 0.6685(6) 0.02567(19) 0.2727(6) 0.0151(14) Uani 1 1 d . . .
C2 C 0.7807(7) 0.00813(19) 0.2638(6) 0.0172(15) Uani 1 1 d . . .
C3 C 0.8026(6) -0.0323(2) 0.2537(7) 0.0186(15) Uani 1 1 d . . .
C4 C 0.8891(6) -0.0458(2) 0.1760(6) 0.0189(15) Uani 1 1 d . . .
H4 H 0.9331 -0.0286 0.1302 0.023 Uiso 1 1 calc R . .
C5 C 0.9108(7) -0.0831(2) 0.1650(7) 0.0265(17) Uani 1 1 d . . .
H5 H 0.9682 -0.0915 0.1105 0.032 Uiso 1 1 calc R . .
C6 C 0.8497(7) -0.1089(2) 0.2330(8) 0.0267(18) Uani 1 1 d . . .
H6 H 0.8651 -0.1348 0.2256 0.032 Uiso 1 1 calc R . .
C7 C 0.7662(7) -0.0960(2) 0.3115(8) 0.0293(18) Uani 1 1 d . . .
H7 H 0.7248 -0.1132 0.3598 0.035 Uiso 1 1 calc R . .
C8 C 0.7428(7) -0.0587(2) 0.3202(8) 0.0266(18) Uani 1 1 d . . .
H8 H 0.6837 -0.0505 0.3733 0.032 Uiso 1 1 calc R . .
C9 C 0.5438(7) 0.0090(2) 0.2537(6) 0.0190(15) Uani 1 1 d . . .
C10 C 0.5074(7) -0.0139(2) 0.1512(7) 0.0222(16) Uani 1 1 d . . .
H10 H 0.5672 -0.0215 0.0981 0.027 Uiso 1 1 calc R . .
C11 C 0.3861(7) -0.0255(2) 0.1269(8) 0.0274(18) Uani 1 1 d . . .
H11 H 0.3626 -0.0404 0.0559 0.033 Uiso 1 1 calc R . .
C12 C 0.2984(7) -0.0156(2) 0.2038(8) 0.0308(19) Uani 1 1 d . . .
H12 H 0.2147 -0.0236 0.1856 0.037 Uiso 1 1 calc R . .
C13 C 0.3326(8) 0.0060(2) 0.3086(8) 0.033(2) Uani 1 1 d . . .
H13 H 0.2728 0.0121 0.3635 0.040 Uiso 1 1 calc R . .
C14 C 0.4530(7) 0.0183(2) 0.3326(7) 0.0223(16) Uani 1 1 d . . .
H14 H 0.4753 0.0335 0.4035 0.027 Uiso 1 1 calc R . .
C15 C 1.0255(7) 0.0423(2) 0.4075(7) 0.0258(17) Uani 1 1 d . . .
H15A H 1.0661 0.0181 0.4018 0.039 Uiso 1 1 calc R . .
H15B H 0.9900 0.0441 0.4870 0.039 Uiso 1 1 calc R . .
H15C H 1.0867 0.0623 0.4023 0.039 Uiso 1 1 calc R . .
C16 C 0.9715(8) 0.0561(2) 0.1299(8) 0.0296(19) Uani 1 1 d . . .
H16A H 1.0155 0.0800 0.1362 0.044 Uiso 1 1 calc R . .
H16B H 0.9064 0.0569 0.0597 0.044 Uiso 1 1 calc R . .
H16C H 1.0304 0.0361 0.1168 0.044 Uiso 1 1 calc R . .
C17 C 0.8251(7) 0.0957(2) 0.6316(7) 0.0267(18) Uani 1 1 d . . .
H17A H 0.8102 0.1079 0.7096 0.040 Uiso 1 1 calc R . .
H17B H 0.9007 0.1059 0.6020 0.040 Uiso 1 1 calc R . .
H17C H 0.8353 0.0688 0.6455 0.040 Uiso 1 1 calc R . .
C18 C 0.5457(7) 0.0898(2) 0.5827(7) 0.0224(16) Uani 1 1 d . . .
H18A H 0.5523 0.0636 0.6071 0.034 Uiso 1 1 calc R . .
H18B H 0.4729 0.0933 0.5216 0.034 Uiso 1 1 calc R . .
H18C H 0.5366 0.1052 0.6560 0.034 Uiso 1 1 calc R . .
C19 C 0.3281(8) 0.1671(3) 0.0717(9) 0.045(2) Uani 1 1 d . . .
H19A H 0.3629 0.1697 -0.0079 0.067 Uiso 1 1 calc R . .
H19B H 0.3464 0.1895 0.1218 0.067 Uiso 1 1 calc R . .
H19C H 0.2378 0.1637 0.0565 0.067 Uiso 1 1 calc R . .
C20 C 0.3101(7) 0.1158(3) 0.2927(8) 0.035(2) Uani 1 1 d . . .
H20A H 0.2217 0.1129 0.2637 0.053 Uiso 1 1 calc R . .
H20B H 0.3209 0.1366 0.3516 0.053 Uiso 1 1 calc R . .
H20C H 0.3412 0.0928 0.3339 0.053 Uiso 1 1 calc R . .
C21 C 0.3821(7) 0.0838(2) 0.0516(8) 0.0287(19) Uani 1 1 d . . .
H21A H 0.4193 0.0620 0.0955 0.043 Uiso 1 1 calc R . .
H21B H 0.4245 0.0886 -0.0225 0.043 Uiso 1 1 calc R . .
H21C H 0.2937 0.0791 0.0268 0.043 Uiso 1 1 calc R . .
C22 C 0.6247(9) 0.1404(3) -0.1076(7) 0.041(2) Uani 1 1 d U . .
H22A H 0.5340 0.1429 -0.1135 0.061 Uiso 1 1 calc R . .
H22B H 0.6472 0.1140 -0.1069 0.061 Uiso 1 1 calc R . .
H22C H 0.6557 0.1526 -0.1792 0.061 Uiso 1 1 calc R . .
C23 C 0.8689(8) 0.1600(3) 0.0357(8) 0.038(2) Uani 1 1 d . . .
H23A H 0.8901 0.1673 -0.0467 0.057 Uiso 1 1 calc R . .
H23B H 0.8965 0.1344 0.0535 0.057 Uiso 1 1 calc R . .
H23C H 0.9104 0.1768 0.0985 0.057 Uiso 1 1 calc R . .
C24 C 0.6487(8) 0.2136(2) 0.0346(8) 0.034(2) Uani 1 1 d . . .
H24A H 0.6768 0.2254 -0.0391 0.051 Uiso 1 1 calc R . .
H24B H 0.6870 0.2262 0.1095 0.051 Uiso 1 1 calc R . .
H24C H 0.5580 0.2155 0.0311 0.051 Uiso 1 1 calc R . .
C25 C 0.9902(8) 0.1525(2) 0.3730(9) 0.036(2) Uani 1 1 d . . .
H25A H 1.0691 0.1646 0.3603 0.055 Uiso 1 1 calc R . .
H25B H 0.9527 0.1421 0.2940 0.055 Uiso 1 1 calc R . .
H25C H 1.0054 0.1324 0.4341 0.055 Uiso 1 1 calc R . .
C26 C 0.8876(8) 0.2320(2) 0.3409(8) 0.034(2) Uani 1 1 d . . .
H26A H 0.8299 0.2501 0.3708 0.052 Uiso 1 1 calc R . .
H26B H 0.8638 0.2269 0.2526 0.052 Uiso 1 1 calc R . .
H26C H 0.9723 0.2421 0.3520 0.052 Uiso 1 1 calc R . .
C27 C 0.9423(8) 0.1977(2) 0.5965(7) 0.033(2) Uani 1 1 d . . .
H27A H 0.9373 0.1751 0.6464 0.049 Uiso 1 1 calc R . .
H27B H 0.8923 0.2174 0.6293 0.049 Uiso 1 1 calc R . .
H27C H 1.0291 0.2058 0.6002 0.049 Uiso 1 1 calc R . .
C28 C 0.6310(9) 0.2417(3) 0.6075(10) 0.050(3) Uani 1 1 d . . .
H28A H 0.7002 0.2525 0.5679 0.076 Uiso 1 1 calc R . .
H28B H 0.6637 0.2276 0.6813 0.076 Uiso 1 1 calc R . .
H28C H 0.5771 0.2618 0.6319 0.076 Uiso 1 1 calc R . .
C29 C 0.4655(13) 0.2379(3) 0.3618(10) 0.072(4) Uani 1 1 d . . .
H29A H 0.4177 0.2213 0.3027 0.108 Uiso 1 1 calc R . .
H29B H 0.5301 0.2504 0.3204 0.108 Uiso 1 1 calc R . .
H29C H 0.4098 0.2565 0.3923 0.108 Uiso 1 1 calc R . .
C30 C 0.4150(8) 0.1887(2) 0.5802(9) 0.039(2) Uani 1 1 d . . .
H30A H 0.3642 0.2085 0.6115 0.059 Uiso 1 1 calc R . .
H30B H 0.4532 0.1739 0.6501 0.059 Uiso 1 1 calc R . .
H30C H 0.3624 0.1727 0.5234 0.059 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 C1 1.988(7) . ?
Ge1 Si1 2.376(2) . ?
Ge1 Si2 2.392(2) . ?
Ge1 Ge2 2.4644(11) . ?
Ge2 Si4 2.393(2) . ?
Ge2 Si3 2.394(2) . ?
Ge2 Ge3 2.4758(11) . ?
Ge3 Si5 2.378(2) . ?
Ge3 Si6 2.385(2) . ?
Ge3 Si2 2.391(2) . ?
Si1 C15 1.865(8) . ?
Si1 C16 1.878(8) . ?
Si1 C2 1.895(7) . ?
Si2 C17 1.873(7) . ?
Si2 C18 1.877(7) . ?
Si3 C20 1.872(9) . ?
Si3 C19 1.876(9) . ?
Si3 C21 1.879(8) . ?
Si4 C22 1.876(9) . ?
Si4 C23 1.882(9) . ?
Si4 C24 1.883(8) . ?
Si5 C26 1.871(8) . ?
Si5 C27 1.872(8) . ?
Si5 C25 1.880(9) . ?
Si6 C28 1.869(9) . ?
Si6 C30 1.870(9) . ?
Si6 C29 1.870(10) . ?
C1 C2 1.380(10) . ?
C1 C9 1.471(10) . ?
C2 C3 1.478(10) . ?
C3 C8 1.389(10) . ?
C3 C4 1.408(9) . ?
C4 C5 1.368(10) . ?
C5 C6 1.392(11) . ?
C6 C7 1.385(11) . ?
C7 C8 1.369(11) . ?
C9 C10 1.403(10) . ?
C9 C14 1.408(10) . ?
C10 C11 1.375(10) . ?
C11 C12 1.373(12) . ?
C12 C13 1.391(12) . ?
C13 C14 1.375(11) . ?

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 Si1 72.7(2) . . ?
C1 Ge1 Si2 121.07(19) . . ?
Si1 Ge1 Si2 119.67(7) . . ?
C1 Ge1 Ge2 128.1(2) . . ?
Si1 Ge1 Ge2 130.56(6) . . ?
Si2 Ge1 Ge2 89.18(6) . . ?
Si4 Ge2 Si3 105.85(9) . . ?
Si4 Ge2 Ge1 120.82(6) . . ?
Si3 Ge2 Ge1 110.47(6) . . ?
Si4 Ge2 Ge3 117.09(7) . . ?
Si3 Ge2 Ge3 116.66(6) . . ?
Ge1 Ge2 Ge3 85.47(4) . . ?
Si5 Ge3 Si6 110.74(8) . . ?
Si5 Ge3 Si2 105.79(8) . . ?
Si6 Ge3 Si2 119.64(8) . . ?
Si5 Ge3 Ge2 110.03(6) . . ?
Si6 Ge3 Ge2 119.42(7) . . ?
Si2 Ge3 Ge2 88.95(6) . . ?
C15 Si1 C16 108.6(4) . . ?
C15 Si1 C2 115.1(3) . . ?
C16 Si1 C2 113.6(3) . . ?
C15 Si1 Ge1 119.5(3) . . ?
C16 Si1 Ge1 119.5(3) . . ?
C2 Si1 Ge1 77.5(2) . . ?
C17 Si2 C18 107.3(3) . . ?
C17 Si2 Ge3 116.7(3) . . ?
C18 Si2 Ge3 113.3(3) . . ?
C17 Si2 Ge1 114.5(3) . . ?
C18 Si2 Ge1 115.5(2) . . ?
Ge3 Si2 Ge1 88.99(7) . . ?
C20 Si3 C19 108.5(4) . . ?
C20 Si3 C21 107.6(4) . . ?
C19 Si3 C21 109.1(4) . . ?
C20 Si3 Ge2 113.0(3) . . ?
C19 Si3 Ge2 110.8(3) . . ?
C21 Si3 Ge2 107.8(3) . . ?
C22 Si4 C23 106.0(4) . . ?
C22 Si4 C24 108.0(4) . . ?
C23 Si4 C24 108.7(4) . . ?
C22 Si4 Ge2 110.3(3) . . ?
C23 Si4 Ge2 115.7(3) . . ?
C24 Si4 Ge2 107.8(3) . . ?
C26 Si5 C27 108.0(4) . . ?
C26 Si5 C25 109.7(4) . . ?
C27 Si5 C25 106.4(4) . . ?
C26 Si5 Ge3 110.7(3) . . ?
C27 Si5 Ge3 110.3(3) . . ?
C25 Si5 Ge3 111.6(3) . . ?
C28 Si6 C30 106.9(4) . . ?
C28 Si6 C29 109.2(6) . . ?
C30 Si6 C29 109.0(5) . . ?
C28 Si6 Ge3 109.6(3) . . ?
C30 Si6 Ge3 112.9(3) . . ?
C29 Si6 Ge3 109.1(3) . . ?
C2 C1 C9 127.2(6) . . ?
C2 C1 Ge1 105.0(5) . . ?
C9 C1 Ge1 127.7(5) . . ?
C1 C2 C3 127.1(6) . . ?
C1 C2 Si1 104.4(5) . . ?
C3 C2 Si1 128.4(5) . . ?
C8 C3 C4 116.9(7) . . ?
C8 C3 C2 122.9(7) . . ?
C4 C3 C2 120.2(6) . . ?
C5 C4 C3 121.2(7) . . ?
C4 C5 C6 120.7(7) . . ?
C7 C6 C5 118.6(7) . . ?
C8 C7 C6 120.5(8) . . ?
C7 C8 C3 122.1(7) . . ?
C10 C9 C14 117.6(7) . . ?
C10 C9 C1 121.7(6) . . ?
C14 C9 C1 120.4(6) . . ?
C11 C10 C9 120.7(7) . . ?
C12 C11 C10 120.8(7) . . ?
C11 C12 C13 119.8(7) . . ?
C14 C13 C12 119.9(8) . . ?
C13 C14 C9 121.1(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
C1 Ge1 Ge2 Si4 -90.8(3) . . . . ?
Si1 Ge1 Ge2 Si4 9.31(11) . . . . ?
Si2 Ge1 Ge2 Si4 139.06(9) . . . . ?
C1 Ge1 Ge2 Si3 33.4(3) . . . . ?
Si1 Ge1 Ge2 Si3 133.52(9) . . . . ?
Si2 Ge1 Ge2 Si3 -96.73(8) . . . . ?
C1 Ge1 Ge2 Ge3 150.2(2) . . . . ?
Si1 Ge1 Ge2 Ge3 -109.68(8) . . . . ?
Si2 Ge1 Ge2 Ge3 20.07(5) . . . . ?
Si4 Ge2 Ge3 Si5 -36.10(10) . . . . ?
Si3 Ge2 Ge3 Si5 -162.98(9) . . . . ?
Ge1 Ge2 Ge3 Si5 86.36(7) . . . . ?
Si4 Ge2 Ge3 Si6 93.57(10) . . . . ?
Si3 Ge2 Ge3 Si6 -33.31(10) . . . . ?
Ge1 Ge2 Ge3 Si6 -143.97(7) . . . . ?
Si4 Ge2 Ge3 Si2 -142.54(8) . . . . ?
Si3 Ge2 Ge3 Si2 90.58(8) . . . . ?
Ge1 Ge2 Ge3 Si2 -20.08(5) . . . . ?
C1 Ge1 Si1 C15 -115.4(4) . . . . ?
Si2 Ge1 Si1 C15 1.0(3) . . . . ?
Ge2 Ge1 Si1 C15 118.8(3) . . . . ?
C1 Ge1 Si1 C16 106.7(4) . . . . ?
Si2 Ge1 Si1 C16 -136.9(3) . . . . ?
Ge2 Ge1 Si1 C16 -19.1(3) . . . . ?
C1 Ge1 Si1 C2 -3.5(3) . . . . ?
Si2 Ge1 Si1 C2 112.9(2) . . . . ?
Ge2 Ge1 Si1 C2 -129.4(2) . . . . ?
Si5 Ge3 Si2 C17 27.2(3) . . . . ?
Si6 Ge3 Si2 C17 -98.5(3) . . . . ?
Ge2 Ge3 Si2 C17 137.8(3) . . . . ?
Si5 Ge3 Si2 C18 152.6(3) . . . . ?
Si6 Ge3 Si2 C18 26.8(3) . . . . ?
Ge2 Ge3 Si2 C18 -96.9(3) . . . . ?
Si5 Ge3 Si2 Ge1 -89.89(8) . . . . ?
Si6 Ge3 Si2 Ge1 144.35(8) . . . . ?
Ge2 Ge3 Si2 Ge1 20.65(5) . . . . ?
C1 Ge1 Si2 C17 84.8(4) . . . . ?
Si1 Ge1 Si2 C17 -2.0(3) . . . . ?
Ge2 Ge1 Si2 C17 -139.8(3) . . . . ?
C1 Ge1 Si2 C18 -40.7(4) . . . . ?
Si1 Ge1 Si2 C18 -127.5(3) . . . . ?
Ge2 Ge1 Si2 C18 94.7(3) . . . . ?
C1 Ge1 Si2 Ge3 -156.2(2) . . . . ?
Si1 Ge1 Si2 Ge3 117.01(8) . . . . ?
Ge2 Ge1 Si2 Ge3 -20.75(5) . . . . ?
Si4 Ge2 Si3 C20 -164.7(3) . . . . ?
Ge1 Ge2 Si3 C20 62.9(3) . . . . ?
Ge3 Ge2 Si3 C20 -32.5(3) . . . . ?
Si4 Ge2 Si3 C19 -42.8(4) . . . . ?
Ge1 Ge2 Si3 C19 -175.2(3) . . . . ?
Ge3 Ge2 Si3 C19 89.4(4) . . . . ?
Si4 Ge2 Si3 C21 76.4(3) . . . . ?
Ge1 Ge2 Si3 C21 -56.0(3) . . . . ?
Ge3 Ge2 Si3 C21 -151.3(3) . . . . ?
Si3 Ge2 Si4 C22 -40.7(4) . . . . ?
Ge1 Ge2 Si4 C22 85.7(4) . . . . ?
Ge3 Ge2 Si4 C22 -172.7(3) . . . . ?
Si3 Ge2 Si4 C23 -161.0(3) . . . . ?
Ge1 Ge2 Si4 C23 -34.6(3) . . . . ?
Ge3 Ge2 Si4 C23 67.0(3) . . . . ?
Si3 Ge2 Si4 C24 77.0(3) . . . . ?
Ge1 Ge2 Si4 C24 -156.6(3) . . . . ?
Ge3 Ge2 Si4 C24 -55.0(3) . . . . ?
Si6 Ge3 Si5 C26 -57.7(3) . . . . ?
Si2 Ge3 Si5 C26 171.3(3) . . . . ?
Ge2 Ge3 Si5 C26 76.5(3) . . . . ?
Si6 Ge3 Si5 C27 61.8(3) . . . . ?
Si2 Ge3 Si5 C27 -69.3(3) . . . . ?
Ge2 Ge3 Si5 C27 -164.0(3) . . . . ?
Si6 Ge3 Si5 C25 179.8(3) . . . . ?
Si2 Ge3 Si5 C25 48.7(3) . . . . ?
Ge2 Ge3 Si5 C25 -46.0(3) . . . . ?
Si5 Ge3 Si6 C28 -25.6(4) . . . . ?
Si2 Ge3 Si6 C28 97.8(4) . . . . ?
Ge2 Ge3 Si6 C28 -154.9(4) . . . . ?
Si5 Ge3 Si6 C30 -144.6(4) . . . . ?
Si2 Ge3 Si6 C30 -21.3(4) . . . . ?
Ge2 Ge3 Si6 C30 86.0(4) . . . . ?
Si5 Ge3 Si6 C29 94.0(5) . . . . ?
Si2 Ge3 Si6 C29 -142.6(5) . . . . ?
Ge2 Ge3 Si6 C29 -35.4(5) . . . . ?
Si1 Ge1 C1 C2 4.9(4) . . . . ?
Si2 Ge1 C1 C2 -109.8(4) . . . . ?
Ge2 Ge1 C1 C2 133.4(4) . . . . ?
Si1 Ge1 C1 C9 -173.6(6) . . . . ?
Si2 Ge1 C1 C9 71.7(6) . . . . ?
Ge2 Ge1 C1 C9 -45.2(7) . . . . ?
C9 C1 C2 C3 -10.8(12) . . . . ?
Ge1 C1 C2 C3 170.7(6) . . . . ?
C9 C1 C2 Si1 172.4(6) . . . . ?
Ge1 C1 C2 Si1 -6.1(5) . . . . ?
C15 Si1 C2 C1 122.0(5) . . . . ?
C16 Si1 C2 C1 -111.9(5) . . . . ?
Ge1 Si1 C2 C1 5.0(4) . . . . ?
C15 Si1 C2 C3 -54.7(7) . . . . ?
C16 Si1 C2 C3 71.4(7) . . . . ?
Ge1 Si1 C2 C3 -171.7(6) . . . . ?
C1 C2 C3 C8 -39.8(11) . . . . ?
Si1 C2 C3 C8 136.2(7) . . . . ?
C1 C2 C3 C4 141.5(7) . . . . ?
Si1 C2 C3 C4 -42.5(10) . . . . ?
C8 C3 C4 C5 1.2(11) . . . . ?
C2 C3 C4 C5 -179.9(7) . . . . ?
C3 C4 C5 C6 -1.4(11) . . . . ?
C4 C5 C6 C7 0.2(12) . . . . ?
C5 C6 C7 C8 1.2(12) . . . . ?
C6 C7 C8 C3 -1.4(13) . . . . ?
C4 C3 C8 C7 0.2(11) . . . . ?
C2 C3 C8 C7 -178.6(7) . . . . ?
C2 C1 C9 C10 -46.7(11) . . . . ?
Ge1 C1 C9 C10 131.5(6) . . . . ?
C2 C1 C9 C14 139.2(8) . . . . ?
Ge1 C1 C9 C14 -42.6(9) . . . . ?
C14 C9 C10 C11 2.4(11) . . . . ?
C1 C9 C10 C11 -171.9(7) . . . . ?
C9 C10 C11 C12 -1.6(11) . . . . ?
C10 C11 C12 C13 -0.7(12) . . . . ?
C11 C12 C13 C14 2.0(12) . . . . ?
C12 C13 C14 C9 -1.1(12) . . . . ?
C10 C9 C14 C13 -1.0(11) . . . . ?
C1 C9 C14 C13 173.3(7) . . . . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        26.38
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         2.036
_refine_diff_density_min         -0.997
_refine_diff_density_rms         0.167

# SQUEEZE RESULTS (APPEND TO CIF)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.165 0.198 0.811 37 5 ' '
2 0.198 0.207 0.354 21 3 ' '
3 0.167 0.914 0.100 8 1 ' '
4 0.334 0.698 0.689 37 5 ' '
5 0.302 0.707 0.146 21 2 ' '
6 0.333 0.414 0.400 8 1 ' '
7 0.666 0.302 0.311 37 5 ' '
8 0.698 0.293 0.854 21 3 ' '
9 0.667 0.586 0.600 8 1 ' '
10 0.834 0.802 0.189 37 5 ' '
11 0.802 0.793 0.646 21 3 ' '
12 0.833 0.086 0.900 8 1 ' '
_platon_squeeze_details          
;
;

