# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2023

####################################################################### 
# 
# 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_sh4473_a
_database_code_depnum_ccdc_archive 'CCDC 2288211'
loop_
_audit_author_name
_audit_author_address
'Bernd Morgenstern'
;Universitaet des Saarlandes
Germany
;
_audit_update_record             
;
2023-08-11 deposited with the CCDC.	2023-10-20 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C32 H44 Si2 Sn2'
_chemical_formula_sum            'C32 H44 Si2 Sn2'
_chemical_formula_weight         722.23

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'
Sn Sn -0.6537 1.4246 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           41
_space_group_name_H-M_alt        'A b a 2'
_space_group_name_Hall           'A 2 -2ac'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   16.7596(8)
_cell_length_b                   21.3357(10)
_cell_length_c                   8.6837(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     3105.1(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    133(2)
_cell_measurement_reflns_used    9713
_cell_measurement_theta_min      2.26
_cell_measurement_theta_max      26.70

_exptl_crystal_description       plate
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.545
_exptl_crystal_F_000             1456
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.243
_exptl_crystal_size_mid          0.123
_exptl_crystal_size_min          0.094
_exptl_absorpt_coefficient_mu    1.705
_shelx_estimated_absorpt_T_min   0.682
_shelx_estimated_absorpt_T_max   0.856
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6908
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_process_details   
;
 SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D.,
 J. Appl. Cryst. 48 (2015) 3-10
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      133(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'INCOATEC I\^A?S microfocus sealed tube'
_diffrn_measurement_device_type  'Bruker AXS D8 Venture, Photon II'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            51606
_diffrn_reflns_av_unetI/netI     0.0113
_diffrn_reflns_av_R_equivalents  0.0260
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_theta_min         2.263
_diffrn_reflns_theta_max         26.697
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             3285
_reflns_number_gt                3255
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.869
_reflns_Friedel_fraction_max     0.999
_reflns_Friedel_fraction_full    0.999

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'APEX 3 (Bruker Nano, Inc., 2019)'
_computing_cell_refinement       'SAINT V8.40A (Bruker Nano, Inc., 2019)'
_computing_data_reduction        'SAINT V8.40A (Bruker Nano, Inc., 2019)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    ?
_computing_publication_material  'SHELXL-2018/3 (Sheldrick, 2018)'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0166P)²+1.1439P] 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_abs_structure_details 
;
 Flack x determined using 1500 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.003(5)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         3285
_refine_ls_number_parameters     169
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0114
_refine_ls_R_factor_gt           0.0112
_refine_ls_wR_factor_ref         0.0304
_refine_ls_wR_factor_gt          0.0303
_refine_ls_goodness_of_fit_ref   1.106
_refine_ls_restrained_S_all      1.105
_refine_ls_shift/su_max          0.002
_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Sn1 Sn 0.41114(2) 0.44940(2) 0.46624(2) 0.01909(5) Uani 1 1 d . . . . .
Si1 Si 0.60627(3) 0.35984(3) 0.34260(7) 0.01758(11) Uani 1 1 d . . . . .
C1 C 0.51545(10) 0.35700(7) 0.4694(3) 0.0188(3) Uani 1 1 d . . . . .
C2 C 0.43603(13) 0.33315(9) 0.4370(2) 0.0190(5) Uani 1 1 d . . . . .
C4 C 0.44004(14) 0.36224(10) 0.6923(3) 0.0220(4) Uani 1 1 d . . . . .
C3 C 0.39011(13) 0.33768(10) 0.5740(3) 0.0204(4) Uani 1 1 d . . . . .
C5 C 0.51588(13) 0.37426(10) 0.6287(3) 0.0202(4) Uani 1 1 d . . . . .
C7 C 0.30488(13) 0.31700(11) 0.5948(3) 0.0266(5) Uani 1 1 d . . . . .
H7A H 0.276556 0.320386 0.496414 0.040 Uiso 1 1 calc R U . . .
H7B H 0.278827 0.343781 0.671457 0.040 Uiso 1 1 calc R U . . .
H7C H 0.303801 0.273374 0.630042 0.040 Uiso 1 1 calc R U . . .
C6 C 0.40810(13) 0.30129(12) 0.2920(3) 0.0272(5) Uani 1 1 d . . . . .
H6A H 0.349973 0.296459 0.295098 0.041 Uiso 1 1 calc R U . . .
H6B H 0.433167 0.259927 0.283854 0.041 Uiso 1 1 calc R U . . .
H6C H 0.422977 0.326758 0.202529 0.041 Uiso 1 1 calc R U . . .
C9 C 0.58534(13) 0.39967(13) 0.7193(3) 0.0262(5) Uani 1 1 d . . . . .
H9A H 0.624419 0.418076 0.648569 0.039 Uiso 1 1 calc R U . . .
H9B H 0.610419 0.365576 0.777389 0.039 Uiso 1 1 calc R U . . .
H9C H 0.566364 0.431896 0.790893 0.039 Uiso 1 1 calc R U . . .
C8 C 0.41771(14) 0.36925(15) 0.8582(3) 0.0335(6) Uani 1 1 d . . . . .
H8A H 0.359509 0.367682 0.868486 0.050 Uiso 1 1 calc R U . . .
H8B H 0.437361 0.409550 0.896848 0.050 Uiso 1 1 calc R U . . .
H8C H 0.441614 0.335112 0.917971 0.050 Uiso 1 1 calc R U . . .
C10 C 0.58531(14) 0.32900(12) 0.1456(3) 0.0276(5) Uani 1 1 d . . . . .
H10A H 0.544724 0.355156 0.095919 0.041 Uiso 1 1 calc R U . . .
H10B H 0.565805 0.285802 0.153117 0.041 Uiso 1 1 calc R U . . .
H10C H 0.634403 0.329831 0.084322 0.041 Uiso 1 1 calc R U . . .
C11 C 0.68557(13) 0.31058(11) 0.4339(3) 0.0298(6) Uani 1 1 d . . . . .
H11A H 0.666014 0.267573 0.445850 0.045 Uiso 1 1 calc R U . . .
H11B H 0.699057 0.327825 0.535186 0.045 Uiso 1 1 calc R U . . .
H11C H 0.733201 0.310549 0.368395 0.045 Uiso 1 1 calc R U . . .
C12 C 0.64652(13) 0.44031(10) 0.3132(3) 0.0194(4) Uani 1 1 d . . . . .
C13 C 0.71323(13) 0.46844(11) 0.3849(3) 0.0252(5) Uani 1 1 d . . . . .
H13 H 0.744825 0.449832 0.463436 0.030 Uiso 1 1 calc R U . . .
C14 C 0.72547(13) 0.52876(11) 0.3212(3) 0.0291(5) Uani 1 1 d . . . . .
H14 H 0.766197 0.557464 0.349759 0.035 Uiso 1 1 calc R U . . .
C15 C 0.66681(16) 0.53871(10) 0.2083(3) 0.0275(5) Uani 1 1 d . . . . .
H15 H 0.669618 0.571257 0.125619 0.033 Uiso 1 1 calc R U . . .
C16 C 0.61811(14) 0.48442(10) 0.2035(3) 0.0229(4) Uani 1 1 d . . . . .
H16 H 0.573573 0.478470 0.137391 0.027 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Sn1 C2 2.5278(19) . ?
Sn1 C3 2.585(2) . ?
Sn1 C15 2.605(2) 2_665 ?
Sn1 C1 2.6350(17) . ?
Sn1 C14 2.654(2) 2_665 ?
Si1 C12 1.862(2) . ?
Si1 C10 1.866(3) . ?
Si1 C11 1.871(2) . ?
Si1 C1 1.880(2) . ?
C1 C5 1.431(3) . ?
C1 C2 1.452(3) . ?
C2 C3 1.420(3) . ?
C2 C6 1.506(3) . ?
C4 C5 1.410(3) . ?
C4 C3 1.425(3) . ?
C4 C8 1.496(3) . ?
C3 C7 1.506(3) . ?
C5 C9 1.506(3) . ?
C12 C13 1.414(3) . ?
C12 C16 1.421(3) . ?
C13 C14 1.416(3) . ?
C14 C15 1.404(4) . ?
C15 C16 1.418(3) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2 Sn1 C3 32.23(7) . . ?
C2 Sn1 C15 95.27(7) . 2_665 ?
C3 Sn1 C15 109.43(7) . 2_665 ?
C2 Sn1 C1 32.59(6) . . ?
C3 Sn1 C1 52.90(7) . . ?
C15 Sn1 C1 114.49(8) 2_665 . ?
C2 Sn1 C14 105.48(7) . 2_665 ?
C3 Sn1 C14 102.48(7) . 2_665 ?
C15 Sn1 C14 30.96(8) 2_665 2_665 ?
C1 Sn1 C14 135.12(7) . 2_665 ?
C12 Si1 C10 105.52(11) . . ?
C12 Si1 C11 108.58(10) . . ?
C10 Si1 C11 108.91(11) . . ?
C12 Si1 C1 113.79(8) . . ?
C10 Si1 C1 111.91(11) . . ?
C11 Si1 C1 108.00(11) . . ?
C5 C1 C2 106.38(19) . . ?
C5 C1 Si1 123.62(15) . . ?
C2 C1 Si1 129.8(2) . . ?
C5 C1 Sn1 79.68(12) . . ?
C2 C1 Sn1 69.64(10) . . ?
Si1 C1 Sn1 120.47(10) . . ?
C3 C2 C1 108.1(2) . . ?
C3 C2 C6 124.25(19) . . ?
C1 C2 C6 127.2(2) . . ?
C3 C2 Sn1 76.09(12) . . ?
C1 C2 Sn1 77.77(10) . . ?
C6 C2 Sn1 118.41(14) . . ?
C5 C4 C3 108.3(2) . . ?
C5 C4 C8 125.8(2) . . ?
C3 C4 C8 125.8(2) . . ?
C2 C3 C4 108.11(19) . . ?
C2 C3 C7 126.5(2) . . ?
C4 C3 C7 125.3(2) . . ?
C2 C3 Sn1 71.68(11) . . ?
C4 C3 Sn1 80.90(12) . . ?
C7 C3 Sn1 116.29(14) . . ?
C4 C5 C1 109.13(18) . . ?
C4 C5 C9 123.9(2) . . ?
C1 C5 C9 127.0(2) . . ?
C13 C12 C16 106.22(19) . . ?
C13 C12 Si1 128.13(17) . . ?
C16 C12 Si1 125.52(17) . . ?
C12 C13 C14 109.1(2) . . ?
C15 C14 C13 108.0(2) . . ?
C15 C14 Sn1 72.60(13) . 2_665 ?
C13 C14 Sn1 81.32(13) . 2_665 ?
C14 C15 C16 107.5(2) . . ?
C14 C15 Sn1 76.45(14) . 2_665 ?
C16 C15 Sn1 79.42(14) . 2_665 ?
C15 C16 C12 109.2(2) . . ?

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 Si1 C1 C5 -64.34(19) . . . . ?
C10 Si1 C1 C5 176.15(16) . . . . ?
C11 Si1 C1 C5 56.28(18) . . . . ?
C12 Si1 C1 C2 121.76(17) . . . . ?
C10 Si1 C1 C2 2.3(2) . . . . ?
C11 Si1 C1 C2 -117.61(19) . . . . ?
C12 Si1 C1 Sn1 33.80(16) . . . . ?
C10 Si1 C1 Sn1 -85.71(13) . . . . ?
C11 Si1 C1 Sn1 154.42(12) . . . . ?
C5 C1 C2 C3 1.3(2) . . . . ?
Si1 C1 C2 C3 175.99(15) . . . . ?
Sn1 C1 C2 C3 -70.76(14) . . . . ?
C5 C1 C2 C6 -171.4(2) . . . . ?
Si1 C1 C2 C6 3.3(3) . . . . ?
Sn1 C1 C2 C6 116.5(2) . . . . ?
C5 C1 C2 Sn1 72.05(13) . . . . ?
Si1 C1 C2 Sn1 -113.25(16) . . . . ?
C1 C2 C3 C4 -1.6(2) . . . . ?
C6 C2 C3 C4 171.4(2) . . . . ?
Sn1 C2 C3 C4 -73.53(15) . . . . ?
C1 C2 C3 C7 -178.49(19) . . . . ?
C6 C2 C3 C7 -5.5(3) . . . . ?
Sn1 C2 C3 C7 109.6(2) . . . . ?
C1 C2 C3 Sn1 71.91(13) . . . . ?
C6 C2 C3 Sn1 -115.1(2) . . . . ?
C5 C4 C3 C2 1.3(2) . . . . ?
C8 C4 C3 C2 -174.2(2) . . . . ?
C5 C4 C3 C7 178.24(19) . . . . ?
C8 C4 C3 C7 2.7(4) . . . . ?
C5 C4 C3 Sn1 -65.88(15) . . . . ?
C8 C4 C3 Sn1 118.5(2) . . . . ?
C3 C4 C5 C1 -0.5(2) . . . . ?
C8 C4 C5 C1 175.1(2) . . . . ?
C3 C4 C5 C9 -179.0(2) . . . . ?
C8 C4 C5 C9 -3.5(4) . . . . ?
C2 C1 C5 C4 -0.5(2) . . . . ?
Si1 C1 C5 C4 -175.59(14) . . . . ?
Sn1 C1 C5 C4 64.55(15) . . . . ?
C2 C1 C5 C9 178.0(2) . . . . ?
Si1 C1 C5 C9 2.9(3) . . . . ?
Sn1 C1 C5 C9 -117.0(2) . . . . ?
C10 Si1 C12 C13 -135.2(2) . . . . ?
C11 Si1 C12 C13 -18.5(2) . . . . ?
C1 Si1 C12 C13 101.8(2) . . . . ?
C10 Si1 C12 C16 40.1(2) . . . . ?
C11 Si1 C12 C16 156.76(19) . . . . ?
C1 Si1 C12 C16 -82.9(2) . . . . ?
C16 C12 C13 C14 0.2(2) . . . . ?
Si1 C12 C13 C14 176.26(17) . . . . ?
C12 C13 C14 C15 -0.4(3) . . . . ?
C12 C13 C14 Sn1 68.05(17) . . . 2_665 ?
C13 C14 C15 C16 0.4(3) . . . . ?
Sn1 C14 C15 C16 -74.10(17) 2_665 . . . ?
C13 C14 C15 Sn1 74.46(17) . . . 2_665 ?
C14 C15 C16 C12 -0.2(3) . . . . ?
Sn1 C15 C16 C12 -72.22(16) 2_665 . . . ?
C13 C12 C16 C15 0.0(3) . . . . ?
Si1 C12 C16 C15 -176.17(16) . . . . ?

_refine_diff_density_max         0.189
_refine_diff_density_min         -0.315
_refine_diff_density_rms         0.042


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

data_sh4524_a
_database_code_depnum_ccdc_archive 'CCDC 2288213'
loop_
_audit_author_name
_audit_author_address
'Bernd Morgenstern'
;Universitaet des Saarlandes
Germany
;
_audit_update_record             
;
2023-09-14 deposited with the CCDC.	2023-10-20 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2019/1
_shelx_SHELXL_version_number     2019/1
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         '2(C16 H22 Ge2)'
_chemical_formula_sum            'C32 H44 Ge4'
_chemical_formula_weight         719.03

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ge Ge 0.1547 1.8001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           5
_space_group_name_H-M_alt        'C 2'
_space_group_name_Hall           'C 2y'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   17.4066(7)
_cell_length_b                   8.7580(4)
_cell_length_c                   13.1177(6)
_cell_angle_alpha                90
_cell_angle_beta                 128.6390(10)
_cell_angle_gamma                90
_cell_volume                     1562.00(12)
_cell_formula_units_Z            2
_cell_measurement_temperature    133(2)
_cell_measurement_reflns_used    9941
_cell_measurement_theta_min      2.77
_cell_measurement_theta_max      31.45

_exptl_crystal_description       plate
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.529
_exptl_crystal_F_000             728
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.156
_exptl_crystal_size_mid          0.117
_exptl_crystal_size_min          0.051
_exptl_absorpt_coefficient_mu    3.830
_shelx_estimated_absorpt_T_min   0.586
_shelx_estimated_absorpt_T_max   0.829
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6487
_exptl_absorpt_correction_T_max  0.7462
_exptl_absorpt_process_details   
;
 SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D.,
 J. Appl. Cryst. 48 (2015) 3-10
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      133(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'INCOATEC I\^A?S microfocus sealed tube'
_diffrn_measurement_device_type  'Bruker AXS D8 Venture, Photon II'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            21387
_diffrn_reflns_av_unetI/netI     0.0351
_diffrn_reflns_av_R_equivalents  0.0322
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         1.988
_diffrn_reflns_theta_max         31.522
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             5215
_reflns_number_gt                4972
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.886
_reflns_Friedel_fraction_max     0.995
_reflns_Friedel_fraction_full    0.995

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'APEX 3 (Bruker Nano, Inc., 2019)'
_computing_cell_refinement       'SAINT V8.40A (Bruker Nano, Inc., 2019)'
_computing_data_reduction        'SAINT V8.40A (Bruker Nano, Inc., 2019)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_computing_structure_refinement  
;
SHELXL-2019/1 (Sheldrick, 2019),                                              
SHELXLe Rev 1000 (Huebschle et al., 2011)
;
_computing_molecular_graphics    'Diamond, (Brandenburg, K. 2018)'
_computing_publication_material  'SHELXL-2019/1 (Sheldrick, 2019)'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0171P)²] 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_abs_structure_details 
;
 Flack x determined using 2209 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.019(6)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         5215
_refine_ls_number_parameters     169
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0237
_refine_ls_R_factor_gt           0.0213
_refine_ls_wR_factor_ref         0.0443
_refine_ls_wR_factor_gt          0.0434
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_restrained_S_all      1.019
_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ge1 Ge 0.54107(2) 0.45200(3) 0.40208(2) 0.01678(6) Uani 1 1 d . . . . .
Ge2 Ge 0.26856(2) 0.35336(3) 0.19703(2) 0.02069(6) Uani 1 1 d . . . . .
C1 C 0.36592(16) 0.4836(3) 0.2113(2) 0.0191(5) Uani 1 1 d . . . . .
C2 C 0.42742(16) 0.4514(3) 0.1751(2) 0.0208(4) Uani 1 1 d . . . . .
C3 C 0.48883(18) 0.5808(3) 0.2094(2) 0.0220(5) Uani 1 1 d . . . . .
C4 C 0.46444(17) 0.6927(3) 0.2632(3) 0.0213(5) Uani 1 1 d . . . . .
C5 C 0.38880(16) 0.6343(3) 0.2628(2) 0.0193(5) Uani 1 1 d . . . . .
C6 C 0.4223(2) 0.3140(3) 0.1031(3) 0.0304(6) Uani 1 1 d . . . . .
H6A H 0.365500 0.323123 0.010418 0.046 Uiso 1 1 calc R U . . .
H6B H 0.415469 0.221903 0.139194 0.046 Uiso 1 1 calc R U . . .
H6C H 0.482657 0.307159 0.112438 0.046 Uiso 1 1 calc R U . . .
C7 C 0.5617(2) 0.6027(4) 0.1851(3) 0.0322(6) Uani 1 1 d . . . . .
H7A H 0.573255 0.504869 0.160340 0.048 Uiso 1 1 calc R U . . .
H7B H 0.623824 0.640847 0.264644 0.048 Uiso 1 1 calc R U . . .
H7C H 0.535719 0.676615 0.114351 0.048 Uiso 1 1 calc R U . . .
C8 C 0.51043(18) 0.8488(3) 0.3086(3) 0.0287(5) Uani 1 1 d . . . . .
H8A H 0.483616 0.914645 0.232760 0.043 Uiso 1 1 calc R U . . .
H8B H 0.581835 0.840146 0.359373 0.043 Uiso 1 1 calc R U . . .
H8C H 0.495761 0.893278 0.363329 0.043 Uiso 1 1 calc R U . . .
C9 C 0.34269(19) 0.7196(3) 0.3114(3) 0.0262(5) Uani 1 1 d . . . . .
H9A H 0.297716 0.797225 0.247257 0.039 Uiso 1 1 calc R U . . .
H9B H 0.394196 0.769210 0.394530 0.039 Uiso 1 1 calc R U . . .
H9C H 0.306038 0.648205 0.324226 0.039 Uiso 1 1 calc R U . . .
C10 C 0.30205(16) 0.3191(3) 0.3662(2) 0.0195(5) Uani 1 1 d . . . . .
C11 C 0.36573(19) 0.2045(3) 0.4560(3) 0.0229(5) Uani 1 1 d . . . . .
H11 H 0.399623 0.131797 0.443424 0.027 Uiso 1 1 calc R U . . .
C12 C 0.3709(2) 0.2153(3) 0.5674(3) 0.0283(6) Uani 1 1 d . . . . .
H12 H 0.408954 0.152220 0.642721 0.034 Uiso 1 1 calc R U . . .
C13 C 0.30948(19) 0.3367(4) 0.5469(3) 0.0290(6) Uani 1 1 d . . . . .
H13 H 0.298225 0.370023 0.605528 0.035 Uiso 1 1 calc R U . . .
C14 C 0.26798(18) 0.3994(3) 0.4238(3) 0.0254(5) Uani 1 1 d . . . . .
H14 H 0.223672 0.483259 0.385405 0.030 Uiso 1 1 calc R U . . .
C15 C 0.14143(18) 0.4562(5) 0.0852(3) 0.0431(8) Uani 1 1 d . . . . .
H15A H 0.126205 0.481548 0.001525 0.065 Uiso 1 1 calc R U . . .
H15B H 0.143890 0.550106 0.127768 0.065 Uiso 1 1 calc R U . . .
H15C H 0.090322 0.388630 0.070037 0.065 Uiso 1 1 calc R U . . .
C16 C 0.2555(2) 0.1532(4) 0.1227(3) 0.0362(7) Uani 1 1 d . . . . .
H16A H 0.203294 0.095575 0.113628 0.054 Uiso 1 1 calc R U . . .
H16B H 0.317809 0.097658 0.180337 0.054 Uiso 1 1 calc R U . . .
H16C H 0.238884 0.165787 0.036696 0.054 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ge1 C2 2.329(2) . ?
Ge1 C3 2.370(3) . ?
Ge1 C12 2.457(3) 2_656 ?
Ge1 C13 2.462(2) 2_656 ?
Ge1 C1 2.471(2) . ?
Ge2 C10 1.933(3) . ?
Ge2 C16 1.949(3) . ?
Ge2 C15 1.951(3) . ?
Ge2 C1 1.952(2) . ?
C1 C5 1.421(3) . ?
C1 C2 1.444(3) . ?
C2 C3 1.424(4) . ?
C2 C6 1.498(4) . ?
C3 C4 1.418(4) . ?
C3 C7 1.502(4) . ?
C4 C5 1.410(3) . ?
C4 C8 1.507(4) . ?
C5 C9 1.499(4) . ?
C10 C14 1.407(4) . ?
C10 C11 1.412(3) . ?
C11 C12 1.410(4) . ?
C12 C13 1.410(4) . ?
C13 C14 1.405(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
C2 Ge1 C3 35.27(9) . . ?
C2 Ge1 C12 98.73(10) . 2_656 ?
C3 Ge1 C12 111.10(9) . 2_656 ?
C2 Ge1 C13 104.86(9) . 2_656 ?
C3 Ge1 C13 96.99(9) . 2_656 ?
C12 Ge1 C13 33.31(10) 2_656 2_656 ?
C2 Ge1 C1 34.86(8) . . ?
C3 Ge1 C1 57.15(8) . . ?
C12 Ge1 C1 120.59(9) 2_656 . ?
C13 Ge1 C1 138.36(9) 2_656 . ?
C10 Ge2 C16 106.98(12) . . ?
C10 Ge2 C15 108.81(12) . . ?
C16 Ge2 C15 108.41(16) . . ?
C10 Ge2 C1 111.04(9) . . ?
C16 Ge2 C1 113.35(11) . . ?
C15 Ge2 C1 108.15(12) . . ?
C5 C1 C2 107.0(2) . . ?
C5 C1 Ge2 123.83(18) . . ?
C2 C1 Ge2 129.19(18) . . ?
C5 C1 Ge1 79.65(13) . . ?
C2 C1 Ge1 67.17(12) . . ?
Ge2 C1 Ge1 118.68(11) . . ?
C3 C2 C1 107.8(2) . . ?
C3 C2 C6 125.1(2) . . ?
C1 C2 C6 126.9(2) . . ?
C3 C2 Ge1 73.94(14) . . ?
C1 C2 Ge1 77.97(13) . . ?
C6 C2 Ge1 118.47(18) . . ?
C4 C3 C2 108.0(2) . . ?
C4 C3 C7 124.9(2) . . ?
C2 C3 C7 127.0(2) . . ?
C4 C3 Ge1 80.41(15) . . ?
C2 C3 Ge1 70.79(13) . . ?
C7 C3 Ge1 118.37(18) . . ?
C5 C4 C3 108.4(2) . . ?
C5 C4 C8 126.5(2) . . ?
C3 C4 C8 125.0(2) . . ?
C4 C5 C1 108.8(2) . . ?
C4 C5 C9 124.4(2) . . ?
C1 C5 C9 126.8(2) . . ?
C14 C10 C11 106.4(2) . . ?
C14 C10 Ge2 127.81(19) . . ?
C11 C10 Ge2 125.83(19) . . ?
C12 C11 C10 109.0(2) . . ?
C13 C12 C11 107.6(2) . . ?
C13 C12 Ge1 73.52(15) . 2_656 ?
C11 C12 Ge1 81.68(15) . 2_656 ?
C14 C13 C12 107.4(2) . . ?
C14 C13 Ge1 81.37(15) . 2_656 ?
C12 C13 Ge1 73.17(14) . 2_656 ?
C13 C14 C10 109.6(2) . . ?

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
C5 C1 C2 C3 2.0(3) . . . . ?
Ge2 C1 C2 C3 -177.76(18) . . . . ?
Ge1 C1 C2 C3 -68.57(16) . . . . ?
C5 C1 C2 C6 -172.7(2) . . . . ?
Ge2 C1 C2 C6 7.5(4) . . . . ?
Ge1 C1 C2 C6 116.7(3) . . . . ?
C5 C1 C2 Ge1 70.58(17) . . . . ?
Ge2 C1 C2 Ge1 -109.19(18) . . . . ?
C1 C2 C3 C4 -1.3(3) . . . . ?
C6 C2 C3 C4 173.5(2) . . . . ?
Ge1 C2 C3 C4 -72.65(18) . . . . ?
C1 C2 C3 C7 -177.1(3) . . . . ?
C6 C2 C3 C7 -2.3(4) . . . . ?
Ge1 C2 C3 C7 111.6(3) . . . . ?
C1 C2 C3 Ge1 71.33(16) . . . . ?
C6 C2 C3 Ge1 -113.8(2) . . . . ?
C2 C3 C4 C5 0.1(3) . . . . ?
C7 C3 C4 C5 176.0(2) . . . . ?
Ge1 C3 C4 C5 -65.97(18) . . . . ?
C2 C3 C4 C8 -178.2(2) . . . . ?
C7 C3 C4 C8 -2.3(4) . . . . ?
Ge1 C3 C4 C8 115.7(2) . . . . ?
C3 C4 C5 C1 1.2(3) . . . . ?
C8 C4 C5 C1 179.5(2) . . . . ?
C3 C4 C5 C9 -179.6(2) . . . . ?
C8 C4 C5 C9 -1.3(4) . . . . ?
C2 C1 C5 C4 -2.0(3) . . . . ?
Ge2 C1 C5 C4 177.83(17) . . . . ?
Ge1 C1 C5 C4 60.12(17) . . . . ?
C2 C1 C5 C9 178.9(2) . . . . ?
Ge2 C1 C5 C9 -1.4(3) . . . . ?
Ge1 C1 C5 C9 -119.1(2) . . . . ?
C14 C10 C11 C12 -0.3(3) . . . . ?
Ge2 C10 C11 C12 -179.53(17) . . . . ?
C10 C11 C12 C13 0.5(3) . . . . ?
C10 C11 C12 Ge1 -69.22(18) . . . 2_656 ?
C11 C12 C13 C14 -0.4(3) . . . . ?
Ge1 C12 C13 C14 74.99(18) 2_656 . . . ?
C11 C12 C13 Ge1 -75.39(18) . . . 2_656 ?
C12 C13 C14 C10 0.2(3) . . . . ?
Ge1 C13 C14 C10 69.44(19) 2_656 . . . ?
C11 C10 C14 C13 0.1(3) . . . . ?
Ge2 C10 C14 C13 179.26(17) . . . . ?

_refine_diff_density_max         0.317
_refine_diff_density_min         -0.279
_refine_diff_density_rms         0.059


_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: hexane / tetrahydrofurane'
_chemical_properties_physical    Air-sensitive,Moisture-sensitive,Hygroscopic
####################################################################### 
# 
# 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_4472_a
_database_code_depnum_ccdc_archive 'CCDC 2288212'
loop_
_audit_author_name
_audit_author_address
'Bernd Morgenstern'
;Universitaet des Saarlandes
Germany
;
_audit_update_record             
;
2023-09-14 deposited with the CCDC.	2023-10-20 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2019/1
_shelx_SHELXL_version_number     2019/1
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         '2(C16 H22 Ge Si)'
_chemical_formula_sum            'C32 H44 Ge2 Si2'
_chemical_formula_weight         630.03

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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           5
_space_group_name_H-M_alt        'C 2'
_space_group_name_Hall           'C 2y'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   17.5006(7)
_cell_length_b                   8.6628(3)
_cell_length_c                   13.3527(6)
_cell_angle_alpha                90
_cell_angle_beta                 130.200(2)
_cell_angle_gamma                90
_cell_volume                     1546.17(11)
_cell_formula_units_Z            2
_cell_measurement_temperature    133(2)
_cell_measurement_reflns_used    9935
_cell_measurement_theta_min      2.81
_cell_measurement_theta_max      32.04

_exptl_crystal_description       cuboid
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.353
_exptl_crystal_F_000             656
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.306
_exptl_crystal_size_mid          0.163
_exptl_crystal_size_min          0.128
_exptl_absorpt_coefficient_mu    2.041
_shelx_estimated_absorpt_T_min   0.574
_shelx_estimated_absorpt_T_max   0.780
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6492
_exptl_absorpt_correction_T_max  0.7463
_exptl_absorpt_process_details   
;
 SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D.,
 J. Appl. Cryst. 48 (2015) 3-10
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      133(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'INCOATEC I\^A?S microfocus sealed tube'
_diffrn_measurement_device_type  'Bruker AXS D8 Venture, Photon II'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            36114
_diffrn_reflns_av_unetI/netI     0.0273
_diffrn_reflns_av_R_equivalents  0.0249
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         1.997
_diffrn_reflns_theta_max         32.052
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_point_group_measured_fraction_full 0.994
_reflns_number_total             5375
_reflns_number_gt                5284
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.885
_reflns_Friedel_fraction_max     0.992
_reflns_Friedel_fraction_full    0.990

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'APEX 3 (Bruker Nano, Inc., 2019)'
_computing_cell_refinement       'SAINT V8.40A (Bruker Nano, Inc., 2019)'
_computing_data_reduction        'SAINT V8.40A (Bruker Nano, Inc., 2019)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_computing_structure_refinement  
;
SHELXL-2019/1 (Sheldrick, 2019)                                              
SHELXLe Rev 1000 (Huebschle et al., 2011)
;
_computing_molecular_graphics    'Diamond, (Brandenburg, K. 2018)'
_computing_publication_material  'SHELXL-2019/1 (Sheldrick, 2019)'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0127P)²+0.1612P] 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_abs_structure_details 
;
 Flack x determined using 2428 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.0102(18)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         5375
_refine_ls_number_parameters     169
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0143
_refine_ls_R_factor_gt           0.0139
_refine_ls_wR_factor_ref         0.0372
_refine_ls_wR_factor_gt          0.0371
_refine_ls_goodness_of_fit_ref   1.081
_refine_ls_restrained_S_all      1.081
_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ge1 Ge 0.54001(2) 0.55258(2) 0.40454(2) 0.01561(4) Uani 1 1 d . . . . .
C1 C 0.36081(9) 0.52445(14) 0.21167(12) 0.0177(2) Uani 1 1 d . . . . .
Si1 Si 0.26632(3) 0.64890(4) 0.19757(3) 0.01903(7) Uani 1 1 d . . . . .
C2 C 0.42152(9) 0.5579(2) 0.17646(11) 0.0197(2) Uani 1 1 d . . . . .
C5 C 0.38542(9) 0.37042(15) 0.26291(12) 0.0178(2) Uani 1 1 d . . . . .
C4 C 0.46042(10) 0.31185(16) 0.26233(13) 0.0197(2) Uani 1 1 d . . . . .
C3 C 0.48317(10) 0.42720(16) 0.20902(13) 0.0206(2) Uani 1 1 d . . . . .
C6 C 0.34133(11) 0.28114(17) 0.31115(15) 0.0234(3) Uani 1 1 d . . . . .
H6A H 0.310747 0.352825 0.333102 0.035 Uiso 1 1 calc R U . . .
H6B H 0.394175 0.222172 0.389381 0.035 Uiso 1 1 calc R U . . .
H6C H 0.290247 0.210107 0.242479 0.035 Uiso 1 1 calc R U . . .
C9 C 0.41610(13) 0.69776(19) 0.10530(15) 0.0290(3) Uani 1 1 d . . . . .
H9A H 0.474394 0.699668 0.110128 0.043 Uiso 1 1 calc R U . . .
H9B H 0.415551 0.791248 0.146165 0.043 Uiso 1 1 calc R U . . .
H9C H 0.354815 0.693489 0.013267 0.043 Uiso 1 1 calc R U . . .
C8 C 0.55505(13) 0.4067(2) 0.18427(16) 0.0304(3) Uani 1 1 d . . . . .
H8A H 0.524436 0.341122 0.107016 0.046 Uiso 1 1 calc R U . . .
H8B H 0.616509 0.357886 0.260739 0.046 Uiso 1 1 calc R U . . .
H8C H 0.571075 0.507705 0.168935 0.046 Uiso 1 1 calc R U . . .
C7 C 0.50735(12) 0.15522(18) 0.30665(15) 0.0271(3) Uani 1 1 d . . . . .
H7A H 0.485504 0.094018 0.230447 0.041 Uiso 1 1 calc R U . . .
H7B H 0.486936 0.103428 0.351345 0.041 Uiso 1 1 calc R U . . .
H7C H 0.580343 0.165627 0.367179 0.041 Uiso 1 1 calc R U . . .
C10 C 0.29959(9) 0.68260(15) 0.35930(13) 0.0179(2) Uani 1 1 d . . . . .
C11 C 0.26475(10) 0.60120(18) 0.41456(15) 0.0236(3) Uani 1 1 d . . . . .
H11 H 0.220308 0.515670 0.375143 0.028 Uiso 1 1 calc R U . . .
C12 C 0.30584(11) 0.6660(2) 0.53705(15) 0.0275(3) Uani 1 1 d . . . . .
H12 H 0.294114 0.632390 0.593840 0.033 Uiso 1 1 calc R U . . .
C13 C 0.36771(12) 0.79008(18) 0.55966(15) 0.0265(3) Uani 1 1 d . . . . .
H13 H 0.405334 0.855167 0.634623 0.032 Uiso 1 1 calc R U . . .
C14 C 0.36343(11) 0.79979(15) 0.45028(14) 0.0213(2) Uani 1 1 d . . . . .
H14 H 0.397959 0.873363 0.439643 0.026 Uiso 1 1 calc R U . . .
C15 C 0.25197(14) 0.8430(2) 0.12606(17) 0.0325(3) Uani 1 1 d . . . . .
H15A H 0.231458 0.830415 0.038719 0.049 Uiso 1 1 calc R U . . .
H15B H 0.315930 0.898120 0.182872 0.049 Uiso 1 1 calc R U . . .
H15C H 0.200993 0.902191 0.119088 0.049 Uiso 1 1 calc R U . . .
C16 C 0.14259(10) 0.5485(3) 0.08790(15) 0.0378(4) Uani 1 1 d . . . . .
H16A H 0.124558 0.528611 0.002680 0.057 Uiso 1 1 calc R U . . .
H16B H 0.091428 0.613846 0.075681 0.057 Uiso 1 1 calc R U . . .
H16C H 0.146944 0.450367 0.127850 0.057 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ge1 C2 2.3291(11) . ?
Ge1 C3 2.3733(13) . ?
Ge1 C13 2.4644(15) 2_656 ?
Ge1 C1 2.4700(12) . ?
Ge1 C12 2.4769(14) 2_656 ?
C1 C5 1.4331(18) . ?
C1 C2 1.4418(18) . ?
C1 Si1 1.8788(13) . ?
Si1 C10 1.8614(14) . ?
Si1 C15 1.8686(17) . ?
Si1 C16 1.8699(17) . ?
C2 C3 1.424(2) . ?
C2 C9 1.505(2) . ?
C5 C4 1.4119(19) . ?
C5 C6 1.500(2) . ?
C4 C3 1.425(2) . ?
C4 C7 1.496(2) . ?
C3 C8 1.503(2) . ?
C10 C11 1.412(2) . ?
C10 C14 1.4151(19) . ?
C11 C12 1.410(2) . ?
C12 C13 1.413(2) . ?
C13 C14 1.416(2) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2 Ge1 C3 35.25(5) . . ?
C2 Ge1 C13 98.98(6) . 2_656 ?
C3 Ge1 C13 110.63(5) . 2_656 ?
C2 Ge1 C1 34.81(4) . . ?
C3 Ge1 C1 57.27(4) . . ?
C13 Ge1 C1 121.11(5) 2_656 . ?
C2 Ge1 C12 105.87(5) . 2_656 ?
C3 Ge1 C12 97.23(5) . 2_656 ?
C13 Ge1 C12 33.24(6) 2_656 2_656 ?
C1 Ge1 C12 139.40(5) . 2_656 ?
C5 C1 C2 106.55(12) . . ?
C5 C1 Si1 123.78(10) . . ?
C2 C1 Si1 129.67(10) . . ?
C5 C1 Ge1 78.81(7) . . ?
C2 C1 Ge1 67.24(6) . . ?
Si1 C1 Ge1 119.40(6) . . ?
C10 Si1 C15 106.86(7) . . ?
C10 Si1 C16 108.57(7) . . ?
C15 Si1 C16 108.22(10) . . ?
C10 Si1 C1 112.19(6) . . ?
C15 Si1 C1 112.76(7) . . ?
C16 Si1 C1 108.11(7) . . ?
C3 C2 C1 108.26(13) . . ?
C3 C2 C9 124.02(12) . . ?
C1 C2 C9 127.46(13) . . ?
C3 C2 Ge1 74.07(7) . . ?
C1 C2 Ge1 77.95(7) . . ?
C9 C2 Ge1 118.79(11) . . ?
C4 C5 C1 109.03(12) . . ?
C4 C5 C6 123.70(12) . . ?
C1 C5 C6 127.27(12) . . ?
C5 C4 C3 108.13(12) . . ?
C5 C4 C7 126.77(14) . . ?
C3 C4 C7 125.08(13) . . ?
C2 C3 C4 108.01(12) . . ?
C2 C3 C8 127.10(14) . . ?
C4 C3 C8 124.77(13) . . ?
C2 C3 Ge1 70.68(7) . . ?
C4 C3 Ge1 79.94(8) . . ?
C8 C3 Ge1 118.67(10) . . ?
C11 C10 C14 106.11(12) . . ?
C11 C10 Si1 127.64(11) . . ?
C14 C10 Si1 126.22(11) . . ?
C12 C11 C10 109.78(13) . . ?
C11 C12 C13 107.29(13) . . ?
C11 C12 Ge1 81.02(8) . 2_656 ?
C13 C12 Ge1 72.89(8) . 2_656 ?
C12 C13 C14 107.56(13) . . ?
C12 C13 Ge1 73.86(8) . 2_656 ?
C14 C13 Ge1 80.87(8) . 2_656 ?
C10 C14 C13 109.26(13) . . ?

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
C5 C1 Si1 C10 59.52(12) . . . . ?
C2 C1 Si1 C10 -120.46(12) . . . . ?
Ge1 C1 Si1 C10 -36.75(9) . . . . ?
C5 C1 Si1 C15 -179.77(11) . . . . ?
C2 C1 Si1 C15 0.25(14) . . . . ?
Ge1 C1 Si1 C15 83.97(9) . . . . ?
C5 C1 Si1 C16 -60.18(13) . . . . ?
C2 C1 Si1 C16 119.85(13) . . . . ?
Ge1 C1 Si1 C16 -156.44(9) . . . . ?
C5 C1 C2 C3 -1.34(14) . . . . ?
Si1 C1 C2 C3 178.64(9) . . . . ?
Ge1 C1 C2 C3 68.53(8) . . . . ?
C5 C1 C2 C9 172.95(13) . . . . ?
Si1 C1 C2 C9 -7.1(2) . . . . ?
Ge1 C1 C2 C9 -117.17(15) . . . . ?
C5 C1 C2 Ge1 -69.87(9) . . . . ?
Si1 C1 C2 Ge1 110.11(10) . . . . ?
C2 C1 C5 C4 1.33(14) . . . . ?
Si1 C1 C5 C4 -178.65(9) . . . . ?
Ge1 C1 C5 C4 -60.63(9) . . . . ?
C2 C1 C5 C6 -178.95(12) . . . . ?
Si1 C1 C5 C6 1.07(18) . . . . ?
Ge1 C1 C5 C6 119.09(13) . . . . ?
C1 C5 C4 C3 -0.82(15) . . . . ?
C6 C5 C4 C3 179.45(12) . . . . ?
C1 C5 C4 C7 -179.57(13) . . . . ?
C6 C5 C4 C7 0.7(2) . . . . ?
C1 C2 C3 C4 0.86(14) . . . . ?
C9 C2 C3 C4 -173.68(13) . . . . ?
Ge1 C2 C3 C4 72.02(9) . . . . ?
C1 C2 C3 C8 176.98(13) . . . . ?
C9 C2 C3 C8 2.4(2) . . . . ?
Ge1 C2 C3 C8 -111.86(14) . . . . ?
C1 C2 C3 Ge1 -71.16(8) . . . . ?
C9 C2 C3 Ge1 114.30(14) . . . . ?
C5 C4 C3 C2 -0.03(15) . . . . ?
C7 C4 C3 C2 178.75(13) . . . . ?
C5 C4 C3 C8 -176.26(13) . . . . ?
C7 C4 C3 C8 2.5(2) . . . . ?
C5 C4 C3 Ge1 65.70(9) . . . . ?
C7 C4 C3 Ge1 -115.51(13) . . . . ?
C15 Si1 C10 C11 139.73(13) . . . . ?
C16 Si1 C10 C11 23.21(15) . . . . ?
C1 Si1 C10 C11 -96.21(12) . . . . ?
C15 Si1 C10 C14 -38.18(13) . . . . ?
C16 Si1 C10 C14 -154.70(13) . . . . ?
C1 Si1 C10 C14 85.88(12) . . . . ?
C14 C10 C11 C12 -0.01(15) . . . . ?
Si1 C10 C11 C12 -178.26(10) . . . . ?
C10 C11 C12 C13 -0.07(17) . . . . ?
C10 C11 C12 Ge1 -68.91(10) . . . 2_656 ?
C11 C12 C13 C14 0.13(17) . . . . ?
Ge1 C12 C13 C14 74.65(10) 2_656 . . . ?
C11 C12 C13 Ge1 -74.52(10) . . . 2_656 ?
C11 C10 C14 C13 0.09(15) . . . . ?
Si1 C10 C14 C13 178.37(10) . . . . ?
C12 C13 C14 C10 -0.14(16) . . . . ?
Ge1 C13 C14 C10 69.61(10) 2_656 . . . ?

_refine_diff_density_max         0.279
_refine_diff_density_min         -0.209
_refine_diff_density_rms         0.043


_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: hexane / tetrahydrofurane'
_chemical_properties_physical    Air-sensitive,Moisture-sensitive,Hygroscopic
