# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2022

####################################################################### 
# 
# 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_fl180217sq
_database_code_depnum_ccdc_archive 'CCDC 2093200'
loop_
_audit_author_name
_audit_author_address
'Felicitas Lips'
;Westfaelische Wilhelms Universitaet Muenster
Germany
;
_audit_update_record             
;
2021-06-29 deposited with the CCDC.	2022-06-15 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C60 H104 Ge2.28 N4 Si7.72'
_chemical_formula_weight         1263.60

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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      tetragonal
_space_group_IT_number           114
_space_group_name_H-M_alt        'P -4 21 c'
_space_group_name_Hall           'P -4 2n'

_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'
'y, -x, -z'
'-y, x, -z'
'x+1/2, -y+1/2, -z+1/2'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, z'
'-y+1/2, -x+1/2, z+1/2'
'y+1/2, x+1/2, z+1/2'

_cell_length_a                   16.3651(5)
_cell_length_b                   16.3651(5)
_cell_length_c                   27.0314(9)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     7239.5(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9900
_cell_measurement_theta_min      2.32
_cell_measurement_theta_max      27.16

_exptl_crystal_description       rod
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.159
_exptl_crystal_F_000             2692
_exptl_transmission_factor_min   2.32
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.584
_exptl_crystal_size_mid          0.289
_exptl_crystal_size_min          0.176
_exptl_absorpt_coefficient_mu    1.106
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5839
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_process_details   SADABS
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            91036
_diffrn_reflns_av_unetI/netI     0.0213
_diffrn_reflns_av_R_equivalents  0.0372
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_theta_min         2.317
_diffrn_reflns_theta_max         27.169
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_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             8000
_reflns_number_gt                7813
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.832
_reflns_Friedel_fraction_max     0.999
_reflns_Friedel_fraction_full    1.000

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _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       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          
;
 Refined as a 2-component inversion twin.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0276P)²+0.9569P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.021(7)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         8000
_refine_ls_number_parameters     339
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0182
_refine_ls_R_factor_gt           0.0175
_refine_ls_wR_factor_ref         0.0493
_refine_ls_wR_factor_gt          0.0490
_refine_ls_goodness_of_fit_ref   1.080
_refine_ls_restrained_S_all      1.080
_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_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
Ge2 Ge 0.43895(2) 0.05935(2) 0.81841(2) 0.01453(5) Uani 1 1 d . . . . .
Ge1A Ge 0.5994(6) 0.0748(6) 0.8516(3) 0.0123(3) Uani 0.1374(18) 1 d . . P A 1
Si1B Si 0.5918(2) 0.0730(3) 0.84676(13) 0.0123(3) Uani 0.8626(18) 1 d . . P A 2
Si3 Si 0.48646(3) 0.07158(3) 0.90530(2) 0.01209(9) Uani 1 1 d . . . . .
Si4 Si 0.70138(3) 0.22924(3) 0.82671(2) 0.01856(10) Uani 1 1 d . . . . .
Si5 Si 0.49697(3) 0.18865(3) 0.99596(2) 0.01577(10) Uani 1 1 d . . . . .
N1 N 0.65394(9) 0.13632(9) 0.81044(6) 0.0158(3) Uani 1 1 d . . . . .
N2 N 0.44529(9) 0.14364(9) 0.94555(5) 0.0140(3) Uani 1 1 d . . . . .
C1 C 0.67543(11) 0.09831(10) 0.76363(6) 0.0157(3) Uani 1 1 d . . . . .
C2 C 0.74437(11) 0.04650(11) 0.76117(7) 0.0194(4) Uani 1 1 d . . . . .
C3 C 0.76273(13) 0.00951(13) 0.71597(7) 0.0272(4) Uani 1 1 d . . . . .
H3 H 0.8089 -0.0255 0.7138 0.033 Uiso 1 1 calc R U . . .
C4 C 0.71591(14) 0.02240(13) 0.67472(8) 0.0321(5) Uani 1 1 d . . . . .
H4 H 0.7295 -0.0037 0.6444 0.038 Uiso 1 1 calc R U . . .
C5 C 0.64888(13) 0.07354(13) 0.67731(7) 0.0267(4) Uani 1 1 d . . . . .
H5 H 0.6173 0.0829 0.6484 0.032 Uiso 1 1 calc R U . . .
C6 C 0.62654(12) 0.11169(12) 0.72135(7) 0.0192(4) Uani 1 1 d . . . . .
C7 C 0.79933(12) 0.02908(12) 0.80519(7) 0.0249(4) Uani 1 1 d . . . . .
H7 H 0.7784 0.0616 0.8338 0.030 Uiso 1 1 calc R U . . .
C8 C 0.79721(14) -0.06111(13) 0.82003(9) 0.0372(5) Uani 1 1 d . . . . .
H8A H 0.8333 -0.0699 0.8485 0.056 Uiso 1 1 calc R U . . .
H8B H 0.7412 -0.0765 0.8289 0.056 Uiso 1 1 calc R U . . .
H8C H 0.8157 -0.0947 0.7922 0.056 Uiso 1 1 calc R U . . .
C9 C 0.88727(14) 0.05574(17) 0.79556(10) 0.0454(6) Uani 1 1 d . . . . .
H9A H 0.9208 0.0436 0.8247 0.068 Uiso 1 1 calc R U . . .
H9B H 0.9088 0.0262 0.7669 0.068 Uiso 1 1 calc R U . . .
H9C H 0.8886 0.1146 0.7890 0.068 Uiso 1 1 calc R U . . .
C10 C 0.55212(12) 0.16681(13) 0.72138(7) 0.0239(4) Uani 1 1 d . . . . .
H10 H 0.5354 0.1753 0.7566 0.029 Uiso 1 1 calc R U . . .
C11 C 0.57070(16) 0.25050(15) 0.69923(10) 0.0405(6) Uani 1 1 d . . . . .
H11A H 0.5212 0.2842 0.6999 0.061 Uiso 1 1 calc R U . . .
H11B H 0.6138 0.2772 0.7186 0.061 Uiso 1 1 calc R U . . .
H11C H 0.5891 0.2439 0.6650 0.061 Uiso 1 1 calc R U . . .
C12 C 0.47963(13) 0.12862(17) 0.69407(8) 0.0374(5) Uani 1 1 d . . . . .
H12A H 0.4331 0.1663 0.6950 0.056 Uiso 1 1 calc R U . . .
H12B H 0.4949 0.1181 0.6596 0.056 Uiso 1 1 calc R U . . .
H12C H 0.4645 0.0771 0.7101 0.056 Uiso 1 1 calc R U . . .
C13 C 0.76833(13) 0.26328(13) 0.77498(9) 0.0297(5) Uani 1 1 d . . . . .
H13A H 0.7948 0.3149 0.7839 0.045 Uiso 1 1 calc R U . . .
H13B H 0.8101 0.2217 0.7687 0.045 Uiso 1 1 calc R U . . .
H13C H 0.7353 0.2712 0.7451 0.045 Uiso 1 1 calc R U . . .
C14 C 0.76555(13) 0.21628(14) 0.88305(8) 0.0316(5) Uani 1 1 d . . . . .
H14A H 0.7913 0.2685 0.8915 0.047 Uiso 1 1 calc R U . . .
H14B H 0.7312 0.1982 0.9107 0.047 Uiso 1 1 calc R U . . .
H14C H 0.8079 0.1753 0.8767 0.047 Uiso 1 1 calc R U . . .
C15 C 0.62251(13) 0.30864(12) 0.83884(8) 0.0267(4) Uani 1 1 d . . . . .
H15A H 0.6493 0.3601 0.8479 0.040 Uiso 1 1 calc R U . . .
H15B H 0.5895 0.3169 0.8090 0.040 Uiso 1 1 calc R U . . .
H15C H 0.5872 0.2908 0.8661 0.040 Uiso 1 1 calc R U . . .
C16 C 0.36074(11) 0.16851(11) 0.93762(6) 0.0160(3) Uani 1 1 d . . . . .
C17 C 0.29766(11) 0.12315(12) 0.96028(7) 0.0198(4) Uani 1 1 d . . . . .
C18 C 0.21777(12) 0.15182(13) 0.95588(8) 0.0270(4) Uani 1 1 d . . . . .
H18 H 0.1749 0.1229 0.9718 0.032 Uiso 1 1 calc R U . . .
C19 C 0.19936(12) 0.22109(14) 0.92902(8) 0.0294(4) Uani 1 1 d . . . . .
H19 H 0.1445 0.2396 0.9267 0.035 Uiso 1 1 calc R U . . .
C20 C 0.26104(13) 0.26307(13) 0.90562(8) 0.0252(4) Uani 1 1 d . . . . .
H20 H 0.2479 0.3098 0.8863 0.030 Uiso 1 1 calc R U . . .
C21 C 0.34287(11) 0.23850(11) 0.90961(7) 0.0193(4) Uani 1 1 d . . . . .
C22 C 0.31342(12) 0.04487(12) 0.98842(7) 0.0228(4) Uani 1 1 d . . . . .
H22 H 0.3732 0.0328 0.9859 0.027 Uiso 1 1 calc R U . . .
C23 C 0.29276(15) 0.05242(14) 1.04343(8) 0.0333(5) Uani 1 1 d . . . . .
H23A H 0.3039 0.0004 1.0600 0.050 Uiso 1 1 calc R U . . .
H23B H 0.3263 0.0955 1.0583 0.050 Uiso 1 1 calc R U . . .
H23C H 0.2348 0.0662 1.0472 0.050 Uiso 1 1 calc R U . . .
C24 C 0.26781(14) -0.02692(13) 0.96537(8) 0.0311(5) Uani 1 1 d . . . . .
H24A H 0.2792 -0.0767 0.9844 0.047 Uiso 1 1 calc R U . . .
H24B H 0.2090 -0.0159 0.9658 0.047 Uiso 1 1 calc R U . . .
H24C H 0.2860 -0.0344 0.9311 0.047 Uiso 1 1 calc R U . . .
C25 C 0.40779(12) 0.28811(12) 0.88318(7) 0.0226(4) Uani 1 1 d . . . . .
H25 H 0.4615 0.2601 0.8882 0.027 Uiso 1 1 calc R U . . .
C26 C 0.39159(13) 0.29235(13) 0.82749(7) 0.0279(4) Uani 1 1 d . . . . .
H26A H 0.4345 0.3247 0.8115 0.042 Uiso 1 1 calc R U . . .
H26B H 0.3915 0.2370 0.8137 0.042 Uiso 1 1 calc R U . . .
H26C H 0.3384 0.3180 0.8216 0.042 Uiso 1 1 calc R U . . .
C27 C 0.41514(15) 0.37462(13) 0.90382(8) 0.0342(5) Uani 1 1 d . . . . .
H27A H 0.4577 0.4043 0.8857 0.051 Uiso 1 1 calc R U . . .
H27B H 0.3628 0.4030 0.9001 0.051 Uiso 1 1 calc R U . . .
H27C H 0.4297 0.3720 0.9390 0.051 Uiso 1 1 calc R U . . .
C28 C 0.42609(12) 0.25747(12) 1.03038(7) 0.0245(4) Uani 1 1 d . . . . .
H28A H 0.4551 0.2823 1.0583 0.037 Uiso 1 1 calc R U . . .
H28B H 0.4064 0.3005 1.0082 0.037 Uiso 1 1 calc R U . . .
H28C H 0.3796 0.2258 1.0427 0.037 Uiso 1 1 calc R U . . .
C29 C 0.53467(14) 0.10878(13) 1.03913(8) 0.0289(4) Uani 1 1 d . . . . .
H29A H 0.5632 0.1348 1.0669 0.043 Uiso 1 1 calc R U . . .
H29B H 0.4883 0.0771 1.0517 0.043 Uiso 1 1 calc R U . . .
H29C H 0.5724 0.0724 1.0216 0.043 Uiso 1 1 calc R U . . .
C30 C 0.58665(13) 0.24827(14) 0.97436(8) 0.0302(5) Uani 1 1 d . . . . .
H30A H 0.6144 0.2727 1.0029 0.045 Uiso 1 1 calc R U . . .
H30B H 0.6245 0.2120 0.9569 0.045 Uiso 1 1 calc R U . . .
H30C H 0.5683 0.2916 0.9519 0.045 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
Ge2 Si1B 2.352(4) 6_655 ?
Ge2 Ge1A 2.453(10) 6_655 ?
Ge2 Si3 2.4823(5) . ?
Ge2 Si1B 2.626(3) . ?
Ge2 Ge1A 2.786(9) . ?
Ge2 Ge2 2.7868(4) 6_655 ?
Ge1A N1 1.747(10) . ?
Ge1A Si3 2.350(10) . ?
Ge1A Ge2 2.453(10) 6_655 ?
Si1B N1 1.753(4) . ?
Si1B Si3 2.341(4) . ?
Si1B Ge2 2.352(4) 6_655 ?
Si3 N2 1.7402(14) . ?
Si3 Si3 2.3843(9) 6_655 ?
Si4 N1 1.7631(16) . ?
Si4 C15 1.861(2) . ?
Si4 C13 1.862(2) . ?
Si4 C14 1.862(2) . ?
Si5 N2 1.7649(14) . ?
Si5 C30 1.857(2) . ?
Si5 C29 1.858(2) . ?
Si5 C28 1.8654(19) . ?
N1 C1 1.453(2) . ?
N2 C16 1.458(2) . ?
C1 C6 1.412(3) . ?
C1 C2 1.413(3) . ?
C2 C3 1.396(3) . ?
C2 C7 1.519(3) . ?
C3 C4 1.369(3) . ?
C3 H3 0.9500 . ?
C4 C5 1.382(3) . ?
C4 H4 0.9500 . ?
C5 C6 1.393(3) . ?
C5 H5 0.9500 . ?
C6 C10 1.516(3) . ?
C7 C9 1.526(3) . ?
C7 C8 1.530(3) . ?
C7 H7 1.0000 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 C11 1.525(3) . ?
C10 C12 1.531(3) . ?
C10 H10 1.0000 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 C21 1.404(3) . ?
C16 C17 1.411(3) . ?
C17 C18 1.394(3) . ?
C17 C22 1.512(3) . ?
C18 C19 1.380(3) . ?
C18 H18 0.9500 . ?
C19 C20 1.375(3) . ?
C19 H19 0.9500 . ?
C20 C21 1.402(3) . ?
C20 H20 0.9500 . ?
C21 C25 1.516(3) . ?
C22 C24 1.525(3) . ?
C22 C23 1.530(3) . ?
C22 H22 1.0000 . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C25 C27 1.526(3) . ?
C25 C26 1.530(3) . ?
C25 H25 1.0000 . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Si1B Ge2 Si3 80.38(9) 6_655 . ?
Ge1A Ge2 Si3 78.8(2) 6_655 . ?
Si1B Ge2 Si1B 100.78(14) 6_655 . ?
Si3 Ge2 Si1B 54.45(8) . . ?
Ge1A Ge2 Ge1A 101.8(3) 6_655 . ?
Si3 Ge2 Ge1A 52.6(2) . . ?
Si1B Ge2 Ge2 60.77(9) 6_655 6_655 ?
Ge1A Ge2 Ge2 63.9(2) 6_655 6_655 ?
Si3 Ge2 Ge2 80.306(11) . 6_655 ?
Si1B Ge2 Ge2 51.40(9) . 6_655 ?
Ge1A Ge2 Ge2 52.2(2) . 6_655 ?
N1 Ge1A Si3 144.0(6) . . ?
N1 Ge1A Ge2 114.4(5) . 6_655 ?
Si3 Ge1A Ge2 90.3(3) . 6_655 ?
N1 Ge1A Ge2 109.2(4) . . ?
Si3 Ge1A Ge2 57.0(2) . . ?
Ge2 Ge1A Ge2 63.9(2) 6_655 . ?
N1 Si1B Si3 144.3(2) . . ?
N1 Si1B Ge2 119.1(2) . 6_655 ?
Si3 Si1B Ge2 93.07(14) . 6_655 ?
N1 Si1B Ge2 116.06(17) . . ?
Si3 Si1B Ge2 59.64(9) . . ?
Ge2 Si1B Ge2 67.83(8) 6_655 . ?
N2 Si3 Si1B 134.53(11) . . ?
N2 Si3 Ge1A 132.5(3) . . ?
N2 Si3 Si3 137.55(5) . 6_655 ?
Si1B Si3 Si3 82.68(11) . 6_655 ?
Ge1A Si3 Si3 82.9(3) . 6_655 ?
N2 Si3 Ge2 121.67(5) . . ?
Si1B Si3 Ge2 65.91(7) . . ?
Ge1A Si3 Ge2 70.4(2) . . ?
Si3 Si3 Ge2 88.799(13) 6_655 . ?
N1 Si4 C15 109.93(8) . . ?
N1 Si4 C13 109.26(9) . . ?
C15 Si4 C13 109.36(10) . . ?
N1 Si4 C14 110.74(9) . . ?
C15 Si4 C14 109.06(10) . . ?
C13 Si4 C14 108.46(11) . . ?
N2 Si5 C30 110.81(8) . . ?
N2 Si5 C29 110.52(8) . . ?
C30 Si5 C29 107.75(11) . . ?
N2 Si5 C28 109.82(8) . . ?
C30 Si5 C28 109.33(10) . . ?
C29 Si5 C28 108.55(10) . . ?
C1 N1 Ge1A 115.6(3) . . ?
C1 N1 Si1B 112.02(17) . . ?
C1 N1 Si4 118.67(12) . . ?
Ge1A N1 Si4 124.3(3) . . ?
Si1B N1 Si4 128.74(15) . . ?
C16 N2 Si3 117.68(11) . . ?
C16 N2 Si5 116.85(11) . . ?
Si3 N2 Si5 125.46(8) . . ?
C6 C1 C2 120.49(16) . . ?
C6 C1 N1 120.09(16) . . ?
C2 C1 N1 119.40(16) . . ?
C3 C2 C1 118.24(18) . . ?
C3 C2 C7 118.47(17) . . ?
C1 C2 C7 123.29(16) . . ?
C4 C3 C2 121.7(2) . . ?
C4 C3 H3 119.2 . . ?
C2 C3 H3 119.2 . . ?
C3 C4 C5 119.75(18) . . ?
C3 C4 H4 120.1 . . ?
C5 C4 H4 120.1 . . ?
C4 C5 C6 121.55(19) . . ?
C4 C5 H5 119.2 . . ?
C6 C5 H5 119.2 . . ?
C5 C6 C1 118.26(17) . . ?
C5 C6 C10 118.56(18) . . ?
C1 C6 C10 123.17(17) . . ?
C2 C7 C9 111.79(17) . . ?
C2 C7 C8 111.91(17) . . ?
C9 C7 C8 109.99(18) . . ?
C2 C7 H7 107.6 . . ?
C9 C7 H7 107.6 . . ?
C8 C7 H7 107.6 . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C7 C9 H9A 109.5 . . ?
C7 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C7 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C6 C10 C11 111.96(17) . . ?
C6 C10 C12 112.31(18) . . ?
C11 C10 C12 109.37(18) . . ?
C6 C10 H10 107.7 . . ?
C11 C10 H10 107.7 . . ?
C12 C10 H10 107.7 . . ?
C10 C11 H11A 109.5 . . ?
C10 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C10 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C10 C12 H12A 109.5 . . ?
C10 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C10 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
Si4 C13 H13A 109.5 . . ?
Si4 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
Si4 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
Si4 C14 H14A 109.5 . . ?
Si4 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
Si4 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
Si4 C15 H15A 109.5 . . ?
Si4 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
Si4 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C21 C16 C17 120.72(16) . . ?
C21 C16 N2 120.31(16) . . ?
C17 C16 N2 118.91(15) . . ?
C18 C17 C16 118.15(18) . . ?
C18 C17 C22 119.21(17) . . ?
C16 C17 C22 122.64(16) . . ?
C19 C18 C17 121.76(19) . . ?
C19 C18 H18 119.1 . . ?
C17 C18 H18 119.1 . . ?
C20 C19 C18 119.49(18) . . ?
C20 C19 H19 120.3 . . ?
C18 C19 H19 120.3 . . ?
C19 C20 C21 121.50(19) . . ?
C19 C20 H20 119.3 . . ?
C21 C20 H20 119.3 . . ?
C20 C21 C16 118.32(18) . . ?
C20 C21 C25 118.65(17) . . ?
C16 C21 C25 123.03(16) . . ?
C17 C22 C24 111.33(16) . . ?
C17 C22 C23 112.51(16) . . ?
C24 C22 C23 110.56(17) . . ?
C17 C22 H22 107.4 . . ?
C24 C22 H22 107.4 . . ?
C23 C22 H22 107.4 . . ?
C22 C23 H23A 109.5 . . ?
C22 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C22 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C22 C24 H24A 109.5 . . ?
C22 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C22 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C21 C25 C27 112.31(17) . . ?
C21 C25 C26 111.50(16) . . ?
C27 C25 C26 109.34(17) . . ?
C21 C25 H25 107.8 . . ?
C27 C25 H25 107.8 . . ?
C26 C25 H25 107.8 . . ?
C25 C26 H26A 109.5 . . ?
C25 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
C25 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C25 C27 H27A 109.5 . . ?
C25 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
C25 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
Si5 C28 H28A 109.5 . . ?
Si5 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
Si5 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
Si5 C29 H29A 109.5 . . ?
Si5 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
Si5 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
Si5 C30 H30A 109.5 . . ?
Si5 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
Si5 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Si3 Ge1A N1 C1 -134.0(6) . . . . ?
Ge2 Ge1A N1 C1 -4.8(6) 6_655 . . . ?
Ge2 Ge1A N1 C1 -74.1(4) . . . . ?
Si3 Ge1A N1 Si4 59.9(8) . . . . ?
Ge2 Ge1A N1 Si4 -170.86(19) 6_655 . . . ?
Ge2 Ge1A N1 Si4 119.9(3) . . . . ?
Si3 Si1B N1 C1 -147.9(2) . . . . ?
Ge2 Si1B N1 C1 3.6(3) 6_655 . . . ?
Ge2 Si1B N1 C1 -74.4(2) . . . . ?
Si3 Si1B N1 Si4 41.0(4) . . . . ?
Ge2 Si1B N1 Si4 -167.53(10) 6_655 . . . ?
Ge2 Si1B N1 Si4 114.50(16) . . . . ?
C15 Si4 N1 C1 123.62(14) . . . . ?
C13 Si4 N1 C1 3.60(16) . . . . ?
C14 Si4 N1 C1 -115.80(14) . . . . ?
C15 Si4 N1 Ge1A -70.7(4) . . . . ?
C13 Si4 N1 Ge1A 169.3(4) . . . . ?
C14 Si4 N1 Ge1A 49.9(4) . . . . ?
C15 Si4 N1 Si1B -65.7(2) . . . . ?
C13 Si4 N1 Si1B 174.2(2) . . . . ?
C14 Si4 N1 Si1B 54.8(2) . . . . ?
Si1B Si3 N2 C16 115.44(16) . . . . ?
Ge1A Si3 N2 C16 120.9(3) . . . . ?
Si3 Si3 N2 C16 -100.40(13) 6_655 . . . ?
Ge2 Si3 N2 C16 29.23(14) . . . . ?
Si1B Si3 N2 Si5 -65.38(17) . . . . ?
Ge1A Si3 N2 Si5 -59.9(3) . . . . ?
Si3 Si3 N2 Si5 78.78(12) 6_655 . . . ?
Ge2 Si3 N2 Si5 -151.60(7) . . . . ?
C30 Si5 N2 C16 -118.40(14) . . . . ?
C29 Si5 N2 C16 122.23(14) . . . . ?
C28 Si5 N2 C16 2.49(15) . . . . ?
C30 Si5 N2 Si3 62.42(13) . . . . ?
C29 Si5 N2 Si3 -56.96(13) . . . . ?
C28 Si5 N2 Si3 -176.69(10) . . . . ?
Ge1A N1 C1 C6 97.3(4) . . . . ?
Si1B N1 C1 C6 92.0(2) . . . . ?
Si4 N1 C1 C6 -95.83(18) . . . . ?
Ge1A N1 C1 C2 -81.2(4) . . . . ?
Si1B N1 C1 C2 -86.5(2) . . . . ?
Si4 N1 C1 C2 85.66(18) . . . . ?
C6 C1 C2 C3 0.3(3) . . . . ?
N1 C1 C2 C3 178.78(16) . . . . ?
C6 C1 C2 C7 -179.70(17) . . . . ?
N1 C1 C2 C7 -1.2(3) . . . . ?
C1 C2 C3 C4 0.0(3) . . . . ?
C7 C2 C3 C4 180.00(18) . . . . ?
C2 C3 C4 C5 0.4(3) . . . . ?
C3 C4 C5 C6 -1.1(3) . . . . ?
C4 C5 C6 C1 1.4(3) . . . . ?
C4 C5 C6 C10 -179.85(19) . . . . ?
C2 C1 C6 C5 -1.0(3) . . . . ?
N1 C1 C6 C5 -179.44(16) . . . . ?
C2 C1 C6 C10 -179.66(17) . . . . ?
N1 C1 C6 C10 1.8(3) . . . . ?
C3 C2 C7 C9 60.2(2) . . . . ?
C1 C2 C7 C9 -119.8(2) . . . . ?
C3 C2 C7 C8 -63.7(2) . . . . ?
C1 C2 C7 C8 116.3(2) . . . . ?
C5 C6 C10 C11 -78.4(2) . . . . ?
C1 C6 C10 C11 100.3(2) . . . . ?
C5 C6 C10 C12 45.1(2) . . . . ?
C1 C6 C10 C12 -136.16(19) . . . . ?
Si3 N2 C16 C21 -94.64(17) . . . . ?
Si5 N2 C16 C21 86.11(17) . . . . ?
Si3 N2 C16 C17 88.04(17) . . . . ?
Si5 N2 C16 C17 -91.21(17) . . . . ?
C21 C16 C17 C18 -2.8(3) . . . . ?
N2 C16 C17 C18 174.52(16) . . . . ?
C21 C16 C17 C22 176.56(17) . . . . ?
N2 C16 C17 C22 -6.1(3) . . . . ?
C16 C17 C18 C19 2.0(3) . . . . ?
C22 C17 C18 C19 -177.41(19) . . . . ?
C17 C18 C19 C20 0.4(3) . . . . ?
C18 C19 C20 C21 -1.9(3) . . . . ?
C19 C20 C21 C16 1.1(3) . . . . ?
C19 C20 C21 C25 -179.47(19) . . . . ?
C17 C16 C21 C20 1.3(3) . . . . ?
N2 C16 C21 C20 -175.94(16) . . . . ?
C17 C16 C21 C25 -178.11(17) . . . . ?
N2 C16 C21 C25 4.6(3) . . . . ?
C18 C17 C22 C24 59.6(2) . . . . ?
C16 C17 C22 C24 -119.78(19) . . . . ?
C18 C17 C22 C23 -65.2(2) . . . . ?
C16 C17 C22 C23 115.5(2) . . . . ?
C20 C21 C25 C27 64.9(2) . . . . ?
C16 C21 C25 C27 -115.7(2) . . . . ?
C20 C21 C25 C26 -58.2(2) . . . . ?
C16 C21 C25 C26 121.19(19) . . . . ?

_refine_diff_density_max         0.179
_refine_diff_density_min         -0.396
_refine_diff_density_rms         0.038




####################################################################### 
# 
# 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_fl190118sq
_database_code_depnum_ccdc_archive 'CCDC 2093202'
loop_
_audit_author_name
_audit_author_address
'Felicitas Lips'
;Westfaelische Wilhelms Universitaet Muenster
Germany
;
_audit_update_record             
;
2021-06-29 deposited with the CCDC.	2022-06-15 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C60 H104 Ge3.89 N4 Si6.11'
_chemical_formula_weight         1335.47

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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      tetragonal
_space_group_IT_number           114
_space_group_name_H-M_alt        'P -4 21 c'
_space_group_name_Hall           'P -4 2n'

_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'
'y, -x, -z'
'-y, x, -z'
'x+1/2, -y+1/2, -z+1/2'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, z'
'-y+1/2, -x+1/2, z+1/2'
'y+1/2, x+1/2, z+1/2'

_cell_length_a                   16.3876(8)
_cell_length_b                   16.3876(8)
_cell_length_c                   27.0831(13)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     7273.3(8)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9219
_cell_measurement_theta_min      2.31
_cell_measurement_theta_max      27.11

_exptl_crystal_description       rod
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.220
_exptl_crystal_F_000             2808
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.388
_exptl_crystal_size_mid          0.201
_exptl_crystal_size_min          0.140
_exptl_absorpt_coefficient_mu    1.729
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5539
_exptl_absorpt_correction_T_max  0.7358
_exptl_absorpt_process_details   SADABS
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'Bruker APEX-II CCD'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            85997
_diffrn_reflns_av_unetI/netI     0.0288
_diffrn_reflns_av_R_equivalents  0.0536
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_theta_min         1.951
_diffrn_reflns_theta_max         27.135
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             8042
_reflns_number_gt                7658
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.833
_reflns_Friedel_fraction_max     1.000
_reflns_Friedel_fraction_full    1.000

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _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       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          
;
 Refined as a 2-component inversion twin.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0334P)²+1.8942P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.055(9)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         8042
_refine_ls_number_parameters     343
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0293
_refine_ls_R_factor_gt           0.0267
_refine_ls_wR_factor_ref         0.0641
_refine_ls_wR_factor_gt          0.0632
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_restrained_S_all      1.077
_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_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
Ge1A Ge -0.07422(17) 0.59839(13) 0.65063(8) 0.0146(2) Uani 0.755(3) 1 d . . P A
1
Si1B Si -0.0721(15) 0.5897(12) 0.6546(8) 0.0146(2) Uani 0.245(3) 1 d . . P A 2
Ge2 Ge 0.05910(2) 0.56048(2) 0.68367(2) 0.01842(9) Uani 1 1 d . . . . .
Ge3A Ge 0.0715(10) 0.5182(11) 0.5954(7) 0.0143(3) Uani 0.190(3) 1 d . . P A 1
Si3B Si 0.0726(6) 0.5164(7) 0.5957(4) 0.0143(3) Uani 0.810(3) 1 d . . P A 2
Si4 Si -0.23181(5) 0.70396(5) 0.67507(4) 0.0223(2) Uani 1 1 d . . . . .
Si5 Si 0.18888(5) 0.50348(5) 0.50451(3) 0.01820(18) Uani 1 1 d . . . . .
N1 N -0.13935(15) 0.65801(15) 0.69194(10) 0.0186(5) Uani 1 1 d . . . . .
N2 N 0.14482(15) 0.55701(15) 0.55421(9) 0.0172(5) Uani 1 1 d . . . . .
C1 C -0.09960(18) 0.67861(19) 0.73787(11) 0.0183(6) Uani 1 1 d . . . . .
C2 C -0.1112(2) 0.6286(2) 0.77998(12) 0.0227(7) Uani 1 1 d . . . . .
C3 C -0.0712(2) 0.6499(2) 0.82354(12) 0.0315(8) Uani 1 1 d . . . . .
H3 H -0.0791 0.6177 0.8523 0.038 Uiso 1 1 calc R U . . .
C4 C -0.0201(2) 0.7169(3) 0.82573(13) 0.0382(9) Uani 1 1 d . . . . .
H4 H 0.0071 0.7300 0.8557 0.046 Uiso 1 1 calc R U . . .
C5 C -0.0086(2) 0.7647(2) 0.78456(13) 0.0315(8) Uani 1 1 d . . . . .
H5 H 0.0267 0.8105 0.7865 0.038 Uiso 1 1 calc R U . . .
C6 C -0.04757(19) 0.7473(2) 0.74026(12) 0.0230(7) Uani 1 1 d . . . . .
C7 C -0.1661(2) 0.5544(2) 0.77972(13) 0.0284(8) Uani 1 1 d . . . . .
H7 H -0.1737 0.5373 0.7446 0.034 Uiso 1 1 calc R U . . .
C8 C -0.1293(3) 0.4823(2) 0.80763(15) 0.0458(11) Uani 1 1 d . . . . .
H8A H -0.1671 0.4360 0.8064 0.069 Uiso 1 1 calc R U . . .
H8B H -0.0774 0.4669 0.7923 0.069 Uiso 1 1 calc R U . . .
H8C H -0.1199 0.4979 0.8421 0.069 Uiso 1 1 calc R U . . .
C9 C -0.2504(2) 0.5741(3) 0.80086(17) 0.0448(10) Uani 1 1 d . . . . .
H9A H -0.2844 0.5250 0.8002 0.067 Uiso 1 1 calc R U . . .
H9B H -0.2446 0.5931 0.8350 0.067 Uiso 1 1 calc R U . . .
H9C H -0.2761 0.6169 0.7809 0.067 Uiso 1 1 calc R U . . .
C10 C -0.0322(2) 0.8032(2) 0.69635(14) 0.0306(8) Uani 1 1 d . . . . .
H10 H -0.0661 0.7828 0.6682 0.037 Uiso 1 1 calc R U . . .
C11 C -0.0581(3) 0.8904(2) 0.70695(19) 0.0574(13) Uani 1 1 d . . . . .
H11A H -0.0473 0.9245 0.6779 0.086 Uiso 1 1 calc R U . . .
H11B H -0.1166 0.8917 0.7145 0.086 Uiso 1 1 calc R U . . .
H11C H -0.0273 0.9114 0.7352 0.086 Uiso 1 1 calc R U . . .
C12 C 0.0569(2) 0.8011(3) 0.67992(17) 0.0432(10) Uani 1 1 d . . . . .
H12A H 0.0730 0.7446 0.6732 0.065 Uiso 1 1 calc R U . . .
H12B H 0.0634 0.8338 0.6499 0.065 Uiso 1 1 calc R U . . .
H12C H 0.0915 0.8235 0.7061 0.065 Uiso 1 1 calc R U . . .
C13 C -0.3095(2) 0.6237(2) 0.66245(14) 0.0300(8) Uani 1 1 d . . . . .
H13A H -0.3611 0.6495 0.6530 0.045 Uiso 1 1 calc R U . . .
H13B H -0.2904 0.5886 0.6355 0.045 Uiso 1 1 calc R U . . .
H13C H -0.3177 0.5907 0.6922 0.045 Uiso 1 1 calc R U . . .
C14 C -0.2673(2) 0.7712(2) 0.72614(16) 0.0353(9) Uani 1 1 d . . . . .
H14A H -0.3190 0.7969 0.7168 0.053 Uiso 1 1 calc R U . . .
H14B H -0.2752 0.7385 0.7561 0.053 Uiso 1 1 calc R U . . .
H14C H -0.2262 0.8134 0.7324 0.053 Uiso 1 1 calc R U . . .
C15 C -0.2192(3) 0.7670(2) 0.61810(16) 0.0375(9) Uani 1 1 d . . . . .
H15A H -0.2716 0.7920 0.6094 0.056 Uiso 1 1 calc R U . . .
H15B H -0.1787 0.8098 0.6241 0.056 Uiso 1 1 calc R U . . .
H15C H -0.2007 0.7321 0.5909 0.056 Uiso 1 1 calc R U . . .
C16 C 0.17019(19) 0.64104(18) 0.56220(12) 0.0181(6) Uani 1 1 d . . . . .
C17 C 0.1247(2) 0.70462(19) 0.54020(12) 0.0226(7) Uani 1 1 d . . . . .
C18 C 0.1538(2) 0.7842(2) 0.54497(14) 0.0311(8) Uani 1 1 d . . . . .
H18 H 0.1246 0.8274 0.5297 0.037 Uiso 1 1 calc R U . . .
C19 C 0.2233(2) 0.8019(2) 0.57116(14) 0.0329(8) Uani 1 1 d . . . . .
H19 H 0.2420 0.8566 0.5737 0.039 Uiso 1 1 calc R U . . .
C20 C 0.2658(2) 0.7396(2) 0.59378(14) 0.0294(8) Uani 1 1 d . . . . .
H20 H 0.3132 0.7522 0.6125 0.035 Uiso 1 1 calc R U . . .
C21 C 0.2408(2) 0.6583(2) 0.58985(12) 0.0218(7) Uani 1 1 d . . . . .
C22 C 0.0457(2) 0.6897(2) 0.51313(12) 0.0263(7) Uani 1 1 d . . . . .
H22 H 0.0328 0.6302 0.5163 0.032 Uiso 1 1 calc R U . . .
C23 C 0.0537(2) 0.7085(3) 0.45807(14) 0.0376(9) Uani 1 1 d . . . . .
H23A H 0.0015 0.6982 0.4416 0.056 Uiso 1 1 calc R U . . .
H23B H 0.0690 0.7659 0.4537 0.056 Uiso 1 1 calc R U . . .
H23C H 0.0959 0.6736 0.4436 0.056 Uiso 1 1 calc R U . . .
C24 C -0.0250(2) 0.7366(2) 0.53567(14) 0.0374(9) Uani 1 1 d . . . . .
H24A H -0.0750 0.7251 0.5170 0.056 Uiso 1 1 calc R U . . .
H24B H -0.0324 0.7197 0.5701 0.056 Uiso 1 1 calc R U . . .
H24C H -0.0134 0.7952 0.5344 0.056 Uiso 1 1 calc R U . . .
C25 C 0.2906(2) 0.5927(2) 0.61539(13) 0.0262(7) Uani 1 1 d . . . . .
H25 H 0.2627 0.5393 0.6097 0.031 Uiso 1 1 calc R U . . .
C26 C 0.3766(2) 0.5859(3) 0.59538(14) 0.0403(10) Uani 1 1 d . . . . .
H26A H 0.4059 0.5428 0.6131 0.060 Uiso 1 1 calc R U . . .
H26B H 0.3746 0.5725 0.5601 0.060 Uiso 1 1 calc R U . . .
H26C H 0.4051 0.6379 0.5999 0.060 Uiso 1 1 calc R U . . .
C27 C 0.2940(2) 0.6074(2) 0.67121(13) 0.0315(8) Uani 1 1 d . . . . .
H27A H 0.2384 0.6118 0.6842 0.047 Uiso 1 1 calc R U . . .
H27B H 0.3220 0.5616 0.6872 0.047 Uiso 1 1 calc R U . . .
H27C H 0.3237 0.6580 0.6779 0.047 Uiso 1 1 calc R U . . .
C28 C 0.2576(2) 0.5728(2) 0.46966(13) 0.0282(7) Uani 1 1 d . . . . .
H28A H 0.2821 0.5431 0.4420 0.042 Uiso 1 1 calc R U . . .
H28B H 0.2261 0.6192 0.4570 0.042 Uiso 1 1 calc R U . . .
H28C H 0.3007 0.5928 0.4916 0.042 Uiso 1 1 calc R U . . .
C29 C 0.1081(2) 0.4655(2) 0.46231(13) 0.0309(8) Uani 1 1 d . . . . .
H29A H 0.1333 0.4358 0.4348 0.046 Uiso 1 1 calc R U . . .
H29B H 0.0716 0.4288 0.4804 0.046 Uiso 1 1 calc R U . . .
H29C H 0.0768 0.5117 0.4494 0.046 Uiso 1 1 calc R U . . .
C30 C 0.2479(2) 0.4139(2) 0.52664(13) 0.0330(8) Uani 1 1 d . . . . .
H30A H 0.2717 0.3852 0.4983 0.049 Uiso 1 1 calc R U . . .
H30B H 0.2916 0.4323 0.5487 0.049 Uiso 1 1 calc R U . . .
H30C H 0.2116 0.3768 0.5446 0.049 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
Ge1A N1 1.829(4) . ?
Ge1A Ge3A 2.428(18) 6_565 ?
Ge1A Ge2 2.441(2) . ?
Ge1A Ge2 2.7641(18) 6_565 ?
Si1B N1 1.87(2) . ?
Si1B Ge2 2.34(2) . ?
Si1B Si3B 2.36(2) 6_565 ?
Si1B Ge2 2.592(19) 6_565 ?
Ge2 Ge3A 2.497(18) . ?
Ge2 Si3B 2.500(11) . ?
Ge2 Si1B 2.592(19) 6_565 ?
Ge2 Ge1A 2.7641(18) 6_565 ?
Ge2 Ge2 2.7715(7) 6_565 ?
Ge3A N2 1.759(18) . ?
Ge3A Ge3A 2.42(3) 6_565 ?
Ge3A Ge1A 2.428(18) 6_565 ?
Si3B N2 1.762(11) . ?
Si3B Si1B 2.36(2) 6_565 ?
Si3B Si3B 2.44(2) 6_565 ?
Si4 N1 1.753(3) . ?
Si4 C14 1.861(4) . ?
Si4 C13 1.862(4) . ?
Si4 C15 1.868(4) . ?
Si5 N2 1.762(3) . ?
Si5 C29 1.856(3) . ?
Si5 C28 1.857(3) . ?
Si5 C30 1.858(4) . ?
N1 C1 1.444(4) . ?
N2 C16 1.455(4) . ?
C1 C6 1.413(5) . ?
C1 C2 1.417(5) . ?
C2 C3 1.394(5) . ?
C2 C7 1.514(5) . ?
C3 C4 1.383(6) . ?
C3 H3 0.9500 . ?
C4 C5 1.375(5) . ?
C4 H4 0.9500 . ?
C5 C6 1.388(5) . ?
C5 H5 0.9500 . ?
C6 C10 1.523(5) . ?
C7 C8 1.526(5) . ?
C7 C9 1.529(5) . ?
C7 H7 1.0000 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 C11 1.519(5) . ?
C10 C12 1.527(5) . ?
C10 H10 1.0000 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 C21 1.407(4) . ?
C16 C17 1.413(4) . ?
C17 C18 1.394(5) . ?
C17 C22 1.508(5) . ?
C18 C19 1.374(5) . ?
C18 H18 0.9500 . ?
C19 C20 1.380(5) . ?
C19 H19 0.9500 . ?
C20 C21 1.398(5) . ?
C20 H20 0.9500 . ?
C21 C25 1.516(5) . ?
C22 C24 1.519(5) . ?
C22 C23 1.528(5) . ?
C22 H22 1.0000 . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C25 C26 1.515(5) . ?
C25 C27 1.532(5) . ?
C25 H25 1.0000 . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Ge1A Ge3A 143.9(4) . 6_565 ?
N1 Ge1A Ge2 115.72(14) . . ?
Ge3A Ge1A Ge2 90.5(4) 6_565 . ?
N1 Ge1A Ge2 110.94(12) . 6_565 ?
Ge3A Ge1A Ge2 57.1(4) 6_565 6_565 ?
Ge2 Ge1A Ge2 63.99(4) . 6_565 ?
N1 Si1B Ge2 118.8(11) . . ?
N1 Si1B Si3B 143.7(13) . 6_565 ?
Ge2 Si1B Si3B 94.6(8) . 6_565 ?
N1 Si1B Ge2 117.0(10) . 6_565 ?
Ge2 Si1B Ge2 68.2(5) . 6_565 ?
Si3B Si1B Ge2 60.4(6) 6_565 6_565 ?
Ge1A Ge2 Ge3A 78.0(4) . . ?
Si1B Ge2 Si3B 79.6(6) . . ?
Si1B Ge2 Si1B 99.6(8) . 6_565 ?
Si3B Ge2 Si1B 55.2(6) . 6_565 ?
Ge1A Ge2 Ge1A 101.61(9) . 6_565 ?
Ge3A Ge2 Ge1A 54.7(4) . 6_565 ?
Si1B Ge2 Ge2 60.2(5) . 6_565 ?
Ge1A Ge2 Ge2 63.68(5) . 6_565 ?
Ge3A Ge2 Ge2 81.9(4) . 6_565 ?
Si3B Ge2 Ge2 81.7(3) . 6_565 ?
Si1B Ge2 Ge2 51.6(5) 6_565 6_565 ?
Ge1A Ge2 Ge2 52.34(6) 6_565 6_565 ?
N2 Ge3A Ge3A 138.7(7) . 6_565 ?
N2 Ge3A Ge1A 131.5(9) . 6_565 ?
Ge3A Ge3A Ge1A 79.8(7) 6_565 6_565 ?
N2 Ge3A Ge2 124.2(9) . . ?
Ge3A Ge3A Ge2 89.4(5) 6_565 . ?
Ge1A Ge3A Ge2 68.3(5) 6_565 . ?
N2 Si3B Si1B 135.4(8) . 6_565 ?
N2 Si3B Si3B 137.6(4) . 6_565 ?
Si1B Si3B Si3B 80.5(7) 6_565 6_565 ?
N2 Si3B Ge2 123.9(5) . . ?
Si1B Si3B Ge2 64.4(5) 6_565 . ?
Si3B Si3B Ge2 88.7(3) 6_565 . ?
N1 Si4 C14 109.29(15) . . ?
N1 Si4 C13 109.58(15) . . ?
C14 Si4 C13 109.95(17) . . ?
N1 Si4 C15 110.92(16) . . ?
C14 Si4 C15 108.7(2) . . ?
C13 Si4 C15 108.34(18) . . ?
N2 Si5 C29 110.21(15) . . ?
N2 Si5 C28 109.39(14) . . ?
C29 Si5 C28 108.94(17) . . ?
N2 Si5 C30 111.14(14) . . ?
C29 Si5 C30 107.74(18) . . ?
C28 Si5 C30 109.39(17) . . ?
C1 N1 Si4 120.9(2) . . ?
C1 N1 Ge1A 112.9(2) . . ?
Si4 N1 Ge1A 125.07(17) . . ?
C1 N1 Si1B 109.9(7) . . ?
Si4 N1 Si1B 128.8(7) . . ?
C16 N2 Ge3A 116.3(6) . . ?
C16 N2 Si5 117.91(19) . . ?
Ge3A N2 Si5 125.8(6) . . ?
C16 N2 Si3B 117.1(4) . . ?
Si5 N2 Si3B 125.0(4) . . ?
C6 C1 C2 120.3(3) . . ?
C6 C1 N1 119.8(3) . . ?
C2 C1 N1 119.9(3) . . ?
C3 C2 C1 118.3(3) . . ?
C3 C2 C7 119.0(3) . . ?
C1 C2 C7 122.7(3) . . ?
C4 C3 C2 121.3(3) . . ?
C4 C3 H3 119.3 . . ?
C2 C3 H3 119.3 . . ?
C5 C4 C3 120.0(3) . . ?
C5 C4 H4 120.0 . . ?
C3 C4 H4 120.0 . . ?
C4 C5 C6 121.4(3) . . ?
C4 C5 H5 119.3 . . ?
C6 C5 H5 119.3 . . ?
C5 C6 C1 118.7(3) . . ?
C5 C6 C10 118.4(3) . . ?
C1 C6 C10 122.9(3) . . ?
C2 C7 C8 112.6(3) . . ?
C2 C7 C9 111.4(3) . . ?
C8 C7 C9 109.6(3) . . ?
C2 C7 H7 107.7 . . ?
C8 C7 H7 107.7 . . ?
C9 C7 H7 107.7 . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C7 C9 H9A 109.5 . . ?
C7 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C7 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C11 C10 C6 111.9(3) . . ?
C11 C10 C12 110.1(3) . . ?
C6 C10 C12 111.9(3) . . ?
C11 C10 H10 107.6 . . ?
C6 C10 H10 107.6 . . ?
C12 C10 H10 107.6 . . ?
C10 C11 H11A 109.5 . . ?
C10 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C10 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C10 C12 H12A 109.5 . . ?
C10 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C10 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
Si4 C13 H13A 109.5 . . ?
Si4 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
Si4 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
Si4 C14 H14A 109.5 . . ?
Si4 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
Si4 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
Si4 C15 H15A 109.5 . . ?
Si4 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
Si4 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C21 C16 C17 120.7(3) . . ?
C21 C16 N2 120.3(3) . . ?
C17 C16 N2 119.0(3) . . ?
C18 C17 C16 118.0(3) . . ?
C18 C17 C22 119.4(3) . . ?
C16 C17 C22 122.6(3) . . ?
C19 C18 C17 122.0(3) . . ?
C19 C18 H18 119.0 . . ?
C17 C18 H18 119.0 . . ?
C18 C19 C20 119.4(3) . . ?
C18 C19 H19 120.3 . . ?
C20 C19 H19 120.3 . . ?
C19 C20 C21 121.6(3) . . ?
C19 C20 H20 119.2 . . ?
C21 C20 H20 119.2 . . ?
C20 C21 C16 118.3(3) . . ?
C20 C21 C25 118.9(3) . . ?
C16 C21 C25 122.9(3) . . ?
C17 C22 C24 112.2(3) . . ?
C17 C22 C23 111.5(3) . . ?
C24 C22 C23 110.8(3) . . ?
C17 C22 H22 107.3 . . ?
C24 C22 H22 107.3 . . ?
C23 C22 H22 107.3 . . ?
C22 C23 H23A 109.5 . . ?
C22 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C22 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C22 C24 H24A 109.5 . . ?
C22 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C22 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C26 C25 C21 113.0(3) . . ?
C26 C25 C27 109.3(3) . . ?
C21 C25 C27 111.0(3) . . ?
C26 C25 H25 107.8 . . ?
C21 C25 H25 107.8 . . ?
C27 C25 H25 107.8 . . ?
C25 C26 H26A 109.5 . . ?
C25 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
C25 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C25 C27 H27A 109.5 . . ?
C25 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
C25 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
Si5 C28 H28A 109.5 . . ?
Si5 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
Si5 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
Si5 C29 H29A 109.5 . . ?
Si5 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
Si5 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
Si5 C30 H30A 109.5 . . ?
Si5 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
Si5 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?

_refine_diff_density_max         0.398
_refine_diff_density_min         -0.437
_refine_diff_density_rms         0.072




####################################################################### 
# 
# 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_fl180216sq
_database_code_depnum_ccdc_archive 'CCDC 2093201'
loop_
_audit_author_name
_audit_author_address
'Felicitas Lips'
;Westfaelische Wilhelms Universitaet Muenster
Germany
;
_audit_update_record             
;
2021-06-29 deposited with the CCDC.	2022-06-15 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C60 H104 Ge2.90 N4 Si7.10'
_chemical_formula_weight         1291.53

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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      tetragonal
_space_group_IT_number           114
_space_group_name_H-M_alt        'P -4 21 c'
_space_group_name_Hall           'P -4 2n'

_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'
'y, -x, -z'
'-y, x, -z'
'x+1/2, -y+1/2, -z+1/2'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, z'
'-y+1/2, -x+1/2, z+1/2'
'y+1/2, x+1/2, z+1/2'

_cell_length_a                   16.3758(5)
_cell_length_b                   16.3758(5)
_cell_length_c                   27.0498(9)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     7253.9(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9288
_cell_measurement_theta_min      2.32
_cell_measurement_theta_max      27.14

_exptl_crystal_description       rod
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.183
_exptl_crystal_F_000             2737
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.566
_exptl_crystal_size_mid          0.194
_exptl_crystal_size_min          0.170
_exptl_absorpt_coefficient_mu    1.348
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5883
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_process_details   SADABS
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            92304
_diffrn_reflns_av_unetI/netI     0.0231
_diffrn_reflns_av_R_equivalents  0.0401
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_theta_min         2.315
_diffrn_reflns_theta_max         27.193
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             8055
_reflns_number_gt                7822
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.832
_reflns_Friedel_fraction_max     0.999
_reflns_Friedel_fraction_full    1.000

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _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       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          
;
 Refined as a 2-component inversion twin.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0263P)²+1.0777P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.017(6)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         8055
_refine_ls_number_parameters     339
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0188
_refine_ls_R_factor_gt           0.0179
_refine_ls_wR_factor_ref         0.0479
_refine_ls_wR_factor_gt          0.0476
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_restrained_S_all      1.030
_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_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
Ge1A Ge 0.5746(2) 0.9010(2) 1.35045(12) 0.0134(3) Uani 0.452(2) 1 d . . P A 1
Si1B Si 0.5716(5) 0.9083(5) 1.3465(3) 0.0134(3) Uani 0.548(2) 1 d . . P A 2
Ge2 Ge 0.55935(2) 1.06067(2) 1.31756(2) 0.01661(6) Uani 1 1 d . . . . .
Si3 Si 0.57149(3) 1.01539(3) 1.40487(2) 0.01252(10) Uani 1 1 d . . . . .
Si4 Si 0.73053(3) 0.79742(3) 1.32587(2) 0.02098(12) Uani 1 1 d . . . . .
Si5 Si 0.68818(3) 1.00339(3) 1.49562(2) 0.01734(11) Uani 1 1 d . . . . .
N1 N 0.63776(10) 0.84411(10) 1.30935(6) 0.0183(3) Uani 1 1 d . . . . .
N2 N 0.64325(9) 1.05579(9) 1.44549(5) 0.0153(3) Uani 1 1 d . . . . .
C1 C 0.59881(12) 0.82308(12) 1.26292(7) 0.0177(4) Uani 1 1 d . . . . .
C2 C 0.54702(12) 0.75436(12) 1.26053(7) 0.0213(4) Uani 1 1 d . . . . .
C3 C 0.50917(14) 0.73626(14) 1.21569(8) 0.0298(5) Uani 1 1 d . . . . .
H3 H 0.4742 0.6901 1.2136 0.036 Uiso 1 1 calc R U . . .
C4 C 0.52140(15) 0.78376(16) 1.17453(8) 0.0350(6) Uani 1 1 d . . . . .
H4 H 0.4947 0.7706 1.1444 0.042 Uiso 1 1 calc R U . . .
C5 C 0.57249(14) 0.85069(14) 1.17702(8) 0.0287(5) Uani 1 1 d . . . . .
H5 H 0.5813 0.8826 1.1482 0.034 Uiso 1 1 calc R U . . .
C6 C 0.61148(13) 0.87257(13) 1.22086(8) 0.0210(4) Uani 1 1 d . . . . .
C7 C 0.53070(13) 0.69898(13) 1.30455(8) 0.0280(5) Uani 1 1 d . . . . .
H7 H 0.5639 0.7197 1.3329 0.034 Uiso 1 1 calc R U . . .
C8 C 0.5569(2) 0.61124(15) 1.29447(12) 0.0526(8) Uani 1 1 d . . . . .
H8A H 0.5454 0.5775 1.3236 0.079 Uiso 1 1 calc R U . . .
H8B H 0.5265 0.5899 1.2660 0.079 Uiso 1 1 calc R U . . .
H8C H 0.6155 0.6098 1.2873 0.079 Uiso 1 1 calc R U . . .
C9 C 0.44083(15) 0.70137(16) 1.32002(10) 0.0411(6) Uani 1 1 d . . . . .
H9A H 0.4324 0.6651 1.3484 0.062 Uiso 1 1 calc R U . . .
H9B H 0.4259 0.7573 1.3292 0.062 Uiso 1 1 calc R U . . .
H9C H 0.4066 0.6832 1.2924 0.062 Uiso 1 1 calc R U . . .
C10 C 0.66650(14) 0.94692(13) 1.22093(8) 0.0259(4) Uani 1 1 d . . . . .
H10 H 0.6746 0.9639 1.2561 0.031 Uiso 1 1 calc R U . . .
C11 C 0.75038(16) 0.92782(17) 1.19930(11) 0.0420(6) Uani 1 1 d . . . . .
H11A H 0.7842 0.9772 1.1999 0.063 Uiso 1 1 calc R U . . .
H11B H 0.7766 0.8849 1.2190 0.063 Uiso 1 1 calc R U . . .
H11C H 0.7442 0.9091 1.1651 0.063 Uiso 1 1 calc R U . . .
C12 C 0.6291(2) 1.01927(15) 1.19326(9) 0.0419(6) Uani 1 1 d . . . . .
H12A H 0.6668 1.0657 1.1943 0.063 Uiso 1 1 calc R U . . .
H12B H 0.6191 1.0039 1.1588 0.063 Uiso 1 1 calc R U . . .
H12C H 0.5773 1.0346 1.2089 0.063 Uiso 1 1 calc R U . . .
C13 C 0.71789(16) 0.73369(15) 1.38250(9) 0.0343(5) Uani 1 1 d . . . . .
H13A H 0.7702 0.7083 1.3910 0.051 Uiso 1 1 calc R U . . .
H13B H 0.6996 0.7682 1.4099 0.051 Uiso 1 1 calc R U . . .
H13C H 0.6772 0.6911 1.3763 0.051 Uiso 1 1 calc R U . . .
C14 C 0.76516(14) 0.73035(15) 1.27430(10) 0.0326(5) Uani 1 1 d . . . . .
H14A H 0.8169 0.7042 1.2834 0.049 Uiso 1 1 calc R U . . .
H14B H 0.7238 0.6883 1.2680 0.049 Uiso 1 1 calc R U . . .
H14C H 0.7730 0.7633 1.2444 0.049 Uiso 1 1 calc R U . . .
C15 C 0.80923(13) 0.87680(14) 1.33816(9) 0.0291(5) Uani 1 1 d . . . . .
H15A H 0.8607 0.8504 1.3473 0.044 Uiso 1 1 calc R U . . .
H15B H 0.8175 0.9098 1.3083 0.044 Uiso 1 1 calc R U . . .
H15C H 0.7909 0.9120 1.3653 0.044 Uiso 1 1 calc R U . . .
C16 C 0.66864(12) 1.14009(11) 1.43757(7) 0.0167(4) Uani 1 1 d . . . . .
C17 C 0.62346(13) 1.20341(12) 1.45979(7) 0.0213(4) Uani 1 1 d . . . . .
C18 C 0.65251(15) 1.28319(13) 1.45529(9) 0.0293(5) Uani 1 1 d . . . . .
H18 H 0.6235 1.3263 1.4708 0.035 Uiso 1 1 calc R U . . .
C19 C 0.72207(15) 1.30106(13) 1.42893(9) 0.0315(5) Uani 1 1 d . . . . .
H19 H 0.7410 1.3558 1.4267 0.038 Uiso 1 1 calc R U . . .
C20 C 0.76417(14) 1.23878(14) 1.40573(9) 0.0268(5) Uani 1 1 d . . . . .
H20 H 0.8112 1.2515 1.3867 0.032 Uiso 1 1 calc R U . . .
C21 C 0.73906(12) 1.15764(12) 1.40973(7) 0.0206(4) Uani 1 1 d . . . . .
C22 C 0.54477(13) 1.18827(13) 1.48770(8) 0.0247(4) Uani 1 1 d . . . . .
H22 H 0.5322 1.1287 1.4848 0.030 Uiso 1 1 calc R U . . .
C23 C 0.47354(14) 1.23466(15) 1.46484(9) 0.0336(5) Uani 1 1 d . . . . .
H23A H 0.4237 1.2235 1.4837 0.050 Uiso 1 1 calc R U . . .
H23B H 0.4851 1.2934 1.4655 0.050 Uiso 1 1 calc R U . . .
H23C H 0.4660 1.2169 1.4305 0.050 Uiso 1 1 calc R U . . .
C24 C 0.55242(15) 1.20779(17) 1.54271(8) 0.0365(5) Uani 1 1 d . . . . .
H24A H 0.5002 1.1971 1.5592 0.055 Uiso 1 1 calc R U . . .
H24B H 0.5949 1.1734 1.5574 0.055 Uiso 1 1 calc R U . . .
H24C H 0.5670 1.2654 1.5469 0.055 Uiso 1 1 calc R U . . .
C25 C 0.78875(13) 1.09216(13) 1.38364(8) 0.0243(4) Uani 1 1 d . . . . .
H25 H 0.7607 1.0386 1.3889 0.029 Uiso 1 1 calc R U . . .
C26 C 0.87513(15) 1.08484(16) 1.40419(9) 0.0366(6) Uani 1 1 d . . . . .
H26A H 0.9046 1.0420 1.3863 0.055 Uiso 1 1 calc R U . . .
H26B H 0.9037 1.1370 1.4001 0.055 Uiso 1 1 calc R U . . .
H26C H 0.8726 1.0708 1.4394 0.055 Uiso 1 1 calc R U . . .
C27 C 0.79272(15) 1.10782(15) 1.32797(8) 0.0299(5) Uani 1 1 d . . . . .
H27A H 0.8250 1.0648 1.3121 0.045 Uiso 1 1 calc R U . . .
H27B H 0.7373 1.1077 1.3143 0.045 Uiso 1 1 calc R U . . .
H27C H 0.8183 1.1610 1.3219 0.045 Uiso 1 1 calc R U . . .
C28 C 0.75700(13) 1.07372(14) 1.53027(8) 0.0268(5) Uani 1 1 d . . . . .
H28A H 0.7818 1.0444 1.5581 0.040 Uiso 1 1 calc R U . . .
H28B H 0.8000 1.0936 1.5082 0.040 Uiso 1 1 calc R U . . .
H28C H 0.7254 1.1201 1.5428 0.040 Uiso 1 1 calc R U . . .
C29 C 0.74760(16) 0.91384(14) 1.47375(8) 0.0333(5) Uani 1 1 d . . . . .
H29A H 0.7719 0.8858 1.5022 0.050 Uiso 1 1 calc R U . . .
H29B H 0.7113 0.8762 1.4561 0.050 Uiso 1 1 calc R U . . .
H29C H 0.7910 0.9322 1.4514 0.050 Uiso 1 1 calc R U . . .
C30 C 0.60817(14) 0.96540(16) 1.53851(8) 0.0320(5) Uani 1 1 d . . . . .
H30A H 0.6340 0.9365 1.5661 0.048 Uiso 1 1 calc R U . . .
H30B H 0.5766 1.0117 1.5513 0.048 Uiso 1 1 calc R U . . .
H30C H 0.5717 0.9280 1.5208 0.048 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
Ge1A N1 1.781(4) . ?
Ge1A Si3 2.383(4) . ?
Ge1A Ge2 2.449(3) 6_675 ?
Ge1A Ge2 2.773(3) . ?
Si1B N1 1.813(8) . ?
Si1B Ge2 2.338(8) 6_675 ?
Si1B Si3 2.360(8) . ?
Si1B Ge2 2.622(8) . ?
Ge2 Si1B 2.338(8) 6_675 ?
Ge2 Ge1A 2.449(3) 6_675 ?
Ge2 Si3 2.4832(5) . ?
Ge2 Ge2 2.7798(4) 6_675 ?
Si3 N2 1.7396(16) . ?
Si3 Si3 2.3950(10) 6_675 ?
Si4 N1 1.7585(18) . ?
Si4 C15 1.860(2) . ?
Si4 C14 1.864(3) . ?
Si4 C13 1.865(2) . ?
Si5 N2 1.7653(16) . ?
Si5 C29 1.857(2) . ?
Si5 C30 1.858(2) . ?
Si5 C28 1.864(2) . ?
N1 C1 1.450(2) . ?
N2 C16 1.458(2) . ?
C1 C2 1.411(3) . ?
C1 C6 1.412(3) . ?
C2 C3 1.394(3) . ?
C2 C7 1.520(3) . ?
C3 C4 1.373(3) . ?
C3 H3 0.9500 . ?
C4 C5 1.381(4) . ?
C4 H4 0.9500 . ?
C5 C6 1.394(3) . ?
C5 H5 0.9500 . ?
C6 C10 1.515(3) . ?
C7 C8 1.524(3) . ?
C7 C9 1.531(3) . ?
C7 H7 1.0000 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 C11 1.525(3) . ?
C10 C12 1.530(3) . ?
C10 H10 1.0000 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 C21 1.407(3) . ?
C16 C17 1.408(3) . ?
C17 C18 1.396(3) . ?
C17 C22 1.514(3) . ?
C18 C19 1.375(3) . ?
C18 H18 0.9500 . ?
C19 C20 1.382(3) . ?
C19 H19 0.9500 . ?
C20 C21 1.395(3) . ?
C20 H20 0.9500 . ?
C21 C25 1.520(3) . ?
C22 C23 1.523(3) . ?
C22 C24 1.527(3) . ?
C22 H22 1.0000 . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C25 C26 1.525(3) . ?
C25 C27 1.529(3) . ?
C25 H25 1.0000 . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Ge1A Si3 144.0(2) . . ?
N1 Ge1A Ge2 115.30(17) . 6_675 ?
Si3 Ge1A Ge2 90.21(11) . 6_675 ?
N1 Ge1A Ge2 110.19(16) . . ?
Si3 Ge1A Ge2 56.97(8) . . ?
Ge2 Ge1A Ge2 63.97(7) 6_675 . ?
N1 Si1B Ge2 119.3(4) . 6_675 ?
N1 Si1B Si3 143.3(4) . . ?
Ge2 Si1B Si3 93.5(3) 6_675 . ?
N1 Si1B Ge2 115.6(4) . . ?
Ge2 Si1B Ge2 67.90(19) 6_675 . ?
Si3 Si1B Ge2 59.51(19) . . ?
Si1B Ge2 Si3 79.7(2) 6_675 . ?
Ge1A Ge2 Si3 78.63(8) 6_675 . ?
Si1B Ge2 Si1B 100.2(3) 6_675 . ?
Si3 Ge2 Si1B 55.00(17) . . ?
Ge1A Ge2 Ge1A 101.88(12) 6_675 . ?
Si3 Ge2 Ge1A 53.57(7) . . ?
Si1B Ge2 Ge2 60.9(2) 6_675 6_675 ?
Ge1A Ge2 Ge2 63.70(9) 6_675 6_675 ?
Si3 Ge2 Ge2 80.937(13) . 6_675 ?
Si1B Ge2 Ge2 51.18(18) . 6_675 ?
Ge1A Ge2 Ge2 52.33(8) . 6_675 ?
N2 Si3 Si1B 134.8(2) . . ?
N2 Si3 Ge1A 132.43(10) . . ?
N2 Si3 Si3 137.77(5) . 6_675 ?
Si1B Si3 Si3 81.0(2) . 6_675 ?
Ge1A Si3 Si3 81.69(9) . 6_675 ?
N2 Si3 Ge2 122.77(6) . . ?
Si1B Si3 Ge2 65.50(18) . . ?
Ge1A Si3 Ge2 69.45(8) . . ?
Si3 Si3 Ge2 89.121(15) 6_675 . ?
N1 Si4 C15 109.88(9) . . ?
N1 Si4 C14 109.19(10) . . ?
C15 Si4 C14 109.55(11) . . ?
N1 Si4 C13 110.87(10) . . ?
C15 Si4 C13 108.73(11) . . ?
C14 Si4 C13 108.59(12) . . ?
N2 Si5 C29 110.96(9) . . ?
N2 Si5 C30 110.41(9) . . ?
C29 Si5 C30 107.71(12) . . ?
N2 Si5 C28 109.75(9) . . ?
C29 Si5 C28 109.34(11) . . ?
C30 Si5 C28 108.62(11) . . ?
C1 N1 Si4 119.79(13) . . ?
C1 N1 Ge1A 114.16(17) . . ?
Si4 N1 Ge1A 124.77(14) . . ?
C1 N1 Si1B 110.7(3) . . ?
Si4 N1 Si1B 128.9(3) . . ?
C16 N2 Si3 117.40(12) . . ?
C16 N2 Si5 117.02(12) . . ?
Si3 N2 Si5 125.58(9) . . ?
C2 C1 C6 120.61(18) . . ?
C2 C1 N1 119.58(17) . . ?
C6 C1 N1 119.80(17) . . ?
C3 C2 C1 118.5(2) . . ?
C3 C2 C7 118.45(19) . . ?
C1 C2 C7 123.07(18) . . ?
C4 C3 C2 121.4(2) . . ?
C4 C3 H3 119.3 . . ?
C2 C3 H3 119.3 . . ?
C3 C4 C5 119.9(2) . . ?
C3 C4 H4 120.0 . . ?
C5 C4 H4 120.0 . . ?
C4 C5 C6 121.5(2) . . ?
C4 C5 H5 119.2 . . ?
C6 C5 H5 119.2 . . ?
C5 C6 C1 118.09(19) . . ?
C5 C6 C10 118.70(19) . . ?
C1 C6 C10 123.21(18) . . ?
C2 C7 C8 111.9(2) . . ?
C2 C7 C9 111.58(19) . . ?
C8 C7 C9 110.1(2) . . ?
C2 C7 H7 107.7 . . ?
C8 C7 H7 107.7 . . ?
C9 C7 H7 107.7 . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C7 C9 H9A 109.5 . . ?
C7 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C7 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C6 C10 C11 111.74(19) . . ?
C6 C10 C12 112.6(2) . . ?
C11 C10 C12 109.4(2) . . ?
C6 C10 H10 107.6 . . ?
C11 C10 H10 107.6 . . ?
C12 C10 H10 107.6 . . ?
C10 C11 H11A 109.5 . . ?
C10 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C10 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C10 C12 H12A 109.5 . . ?
C10 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C10 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
Si4 C13 H13A 109.5 . . ?
Si4 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
Si4 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
Si4 C14 H14A 109.5 . . ?
Si4 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
Si4 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
Si4 C15 H15A 109.5 . . ?
Si4 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
Si4 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C21 C16 C17 120.57(18) . . ?
C21 C16 N2 120.39(17) . . ?
C17 C16 N2 119.00(17) . . ?
C18 C17 C16 118.2(2) . . ?
C18 C17 C22 119.14(19) . . ?
C16 C17 C22 122.64(17) . . ?
C19 C18 C17 121.8(2) . . ?
C19 C18 H18 119.1 . . ?
C17 C18 H18 119.1 . . ?
C18 C19 C20 119.4(2) . . ?
C18 C19 H19 120.3 . . ?
C20 C19 H19 120.3 . . ?
C19 C20 C21 121.4(2) . . ?
C19 C20 H20 119.3 . . ?
C21 C20 H20 119.3 . . ?
C20 C21 C16 118.52(19) . . ?
C20 C21 C25 118.57(19) . . ?
C16 C21 C25 122.90(18) . . ?
C17 C22 C23 111.59(18) . . ?
C17 C22 C24 112.45(18) . . ?
C23 C22 C24 110.73(18) . . ?
C17 C22 H22 107.3 . . ?
C23 C22 H22 107.3 . . ?
C24 C22 H22 107.3 . . ?
C22 C23 H23A 109.5 . . ?
C22 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C22 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C22 C24 H24A 109.5 . . ?
C22 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C22 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C21 C25 C26 112.52(19) . . ?
C21 C25 C27 111.21(18) . . ?
C26 C25 C27 109.43(18) . . ?
C21 C25 H25 107.8 . . ?
C26 C25 H25 107.8 . . ?
C27 C25 H25 107.8 . . ?
C25 C26 H26A 109.5 . . ?
C25 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
C25 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C25 C27 H27A 109.5 . . ?
C25 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
C25 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
Si5 C28 H28A 109.5 . . ?
Si5 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
Si5 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
Si5 C29 H29A 109.5 . . ?
Si5 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
Si5 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
Si5 C30 H30A 109.5 . . ?
Si5 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
Si5 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C15 Si4 N1 C1 124.00(15) . . . . ?
C14 Si4 N1 C1 3.83(18) . . . . ?
C13 Si4 N1 C1 -115.78(16) . . . . ?
C15 Si4 N1 Ge1A -69.7(2) . . . . ?
C14 Si4 N1 Ge1A 170.17(19) . . . . ?
C13 Si4 N1 Ge1A 50.6(2) . . . . ?
C15 Si4 N1 Si1B -65.5(4) . . . . ?
C14 Si4 N1 Si1B 174.3(4) . . . . ?
C13 Si4 N1 Si1B 54.7(4) . . . . ?
Si3 Ge1A N1 C1 -135.3(3) . . . . ?
Ge2 Ge1A N1 C1 -4.2(2) 6_675 . . . ?
Ge2 Ge1A N1 C1 -74.1(2) . . . . ?
Si3 Ge1A N1 Si4 57.7(3) . . . . ?
Ge2 Ge1A N1 Si4 -171.19(10) 6_675 . . . ?
Ge2 Ge1A N1 Si4 118.89(13) . . . . ?
Ge2 Si1B N1 C1 2.9(5) 6_675 . . . ?
Si3 Si1B N1 C1 -147.6(6) . . . . ?
Ge2 Si1B N1 C1 -75.0(4) . . . . ?
Ge2 Si1B N1 Si4 -168.23(19) 6_675 . . . ?
Si3 Si1B N1 Si4 41.2(8) . . . . ?
Ge2 Si1B N1 Si4 113.9(3) . . . . ?
Si1B Si3 N2 C16 116.5(3) . . . . ?
Ge1A Si3 N2 C16 120.97(17) . . . . ?
Si3 Si3 N2 C16 -103.33(14) 6_675 . . . ?
Ge2 Si3 N2 C16 29.67(16) . . . . ?
Si1B Si3 N2 Si5 -63.5(3) . . . . ?
Ge1A Si3 N2 Si5 -59.00(17) . . . . ?
Si3 Si3 N2 Si5 76.70(14) 6_675 . . . ?
Ge2 Si3 N2 Si5 -150.31(8) . . . . ?
C29 Si5 N2 C16 -117.90(15) . . . . ?
C30 Si5 N2 C16 122.76(15) . . . . ?
C28 Si5 N2 C16 3.06(16) . . . . ?
C29 Si5 N2 Si3 62.08(15) . . . . ?
C30 Si5 N2 Si3 -57.26(15) . . . . ?
C28 Si5 N2 Si3 -176.97(11) . . . . ?
Si4 N1 C1 C2 85.4(2) . . . . ?
Ge1A N1 C1 C2 -82.4(2) . . . . ?
Si1B N1 C1 C2 -86.7(3) . . . . ?
Si4 N1 C1 C6 -96.1(2) . . . . ?
Ge1A N1 C1 C6 96.1(2) . . . . ?
Si1B N1 C1 C6 91.8(3) . . . . ?
C6 C1 C2 C3 0.4(3) . . . . ?
N1 C1 C2 C3 178.88(18) . . . . ?
C6 C1 C2 C7 -179.75(19) . . . . ?
N1 C1 C2 C7 -1.3(3) . . . . ?
C1 C2 C3 C4 -0.1(3) . . . . ?
C7 C2 C3 C4 -179.9(2) . . . . ?
C2 C3 C4 C5 0.4(3) . . . . ?
C3 C4 C5 C6 -1.1(3) . . . . ?
C4 C5 C6 C1 1.4(3) . . . . ?
C4 C5 C6 C10 -179.8(2) . . . . ?
C2 C1 C6 C5 -1.0(3) . . . . ?
N1 C1 C6 C5 -179.52(18) . . . . ?
C2 C1 C6 C10 -179.76(19) . . . . ?
N1 C1 C6 C10 1.7(3) . . . . ?
C3 C2 C7 C8 59.9(3) . . . . ?
C1 C2 C7 C8 -119.9(2) . . . . ?
C3 C2 C7 C9 -63.9(3) . . . . ?
C1 C2 C7 C9 116.2(2) . . . . ?
C5 C6 C10 C11 -79.8(3) . . . . ?
C1 C6 C10 C11 98.9(2) . . . . ?
C5 C6 C10 C12 43.8(3) . . . . ?
C1 C6 C10 C12 -137.5(2) . . . . ?
Si3 N2 C16 C21 -94.53(19) . . . . ?
Si5 N2 C16 C21 85.45(19) . . . . ?
Si3 N2 C16 C17 87.90(19) . . . . ?
Si5 N2 C16 C17 -92.12(19) . . . . ?
C21 C16 C17 C18 -2.9(3) . . . . ?
N2 C16 C17 C18 174.71(18) . . . . ?
C21 C16 C17 C22 176.52(18) . . . . ?
N2 C16 C17 C22 -5.9(3) . . . . ?
C16 C17 C18 C19 1.7(3) . . . . ?
C22 C17 C18 C19 -177.7(2) . . . . ?
C17 C18 C19 C20 0.7(4) . . . . ?
C18 C19 C20 C21 -2.0(3) . . . . ?
C19 C20 C21 C16 0.8(3) . . . . ?
C19 C20 C21 C25 -179.4(2) . . . . ?
C17 C16 C21 C20 1.6(3) . . . . ?
N2 C16 C21 C20 -175.90(18) . . . . ?
C17 C16 C21 C25 -178.10(19) . . . . ?
N2 C16 C21 C25 4.4(3) . . . . ?
C18 C17 C22 C23 58.8(3) . . . . ?
C16 C17 C22 C23 -120.5(2) . . . . ?
C18 C17 C22 C24 -66.3(3) . . . . ?
C16 C17 C22 C24 114.3(2) . . . . ?
C20 C21 C25 C26 64.2(3) . . . . ?
C16 C21 C25 C26 -116.1(2) . . . . ?
C20 C21 C25 C27 -59.0(3) . . . . ?
C16 C21 C25 C27 120.7(2) . . . . ?

_refine_diff_density_max         0.199
_refine_diff_density_min         -0.367
_refine_diff_density_rms         0.038




