# 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_shelx
_database_code_depnum_ccdc_archive 'CCDC 2153532'
loop_
_audit_author_name
_audit_author_address
'Hartmut Schubert'
;Universtity of Tuebingen
Germany
;
_audit_update_record             
;
2022-02-21 deposited with the CCDC.	2022-03-22 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/1
_shelx_SHELXL_version_number     2018/1
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C24 H52 Ge Si4'
_chemical_formula_sum            'C24 H52 Ge Si4'
_chemical_formula_weight         525.63

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'
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'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_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'

_cell_length_a                   10.8467(4)
_cell_length_b                   12.2159(4)
_cell_length_c                   13.8073(4)
_cell_angle_alpha                66.376(2)
_cell_angle_beta                 75.966(2)
_cell_angle_gamma                76.691(2)
_cell_volume                     1607.83(10)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    8860
_cell_measurement_theta_min      2.87
_cell_measurement_theta_max      26.69

_exptl_crystal_description       prism
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.086
_exptl_crystal_F_000             568
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.14
_exptl_absorpt_coefficient_mu    1.111
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6784
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_process_details   'SADABS V2012/1 (Bruker AXS Inc.)'
_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 8.333
_diffrn_reflns_number            27919
_diffrn_reflns_av_unetI/netI     0.0382
_diffrn_reflns_av_R_equivalents  0.0353
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         1.633
_diffrn_reflns_theta_max         27.156
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measured_fraction_theta_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_point_group_measured_fraction_full 0.991
_reflns_number_total             6995
_reflns_number_gt                5558
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_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       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXT 2014/4 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2018/1 (Sheldrick, 2018)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_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)+(0.0536P)²+0.3846P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         6995
_refine_ls_number_parameters     289
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0527
_refine_ls_R_factor_gt           0.0358
_refine_ls_wR_factor_ref         0.0981
_refine_ls_wR_factor_gt          0.0908
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_restrained_S_all      1.060
_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
Ge1 Ge 0.02551(2) 0.30263(2) 0.32580(2) 0.02719(9) Uani 1 1 d . . . . .
Si3 Si 0.17918(6) 0.27947(5) -0.01526(4) 0.01660(13) Uani 1 1 d . . . . .
Si2 Si 0.17904(6) 0.02071(5) 0.18612(5) 0.02061(14) Uani 1 1 d . . . . .
Si1 Si 0.29579(6) 0.50121(5) 0.36823(5) 0.02199(14) Uani 1 1 d . . . . .
Si4 Si 0.30942(7) 0.21949(5) 0.53256(5) 0.02313(15) Uani 1 1 d . . . . .
C1 C 0.4753(2) 0.23851(17) 0.18703(15) 0.0154(4) Uani 1 1 d . . . . .
C2 C 0.4293(2) 0.28098(17) 0.27077(15) 0.0162(4) Uani 1 1 d . . . . .
H2 H 0.488864 0.298030 0.301245 0.019 Uiso 1 1 calc R U . . .
C3 C 0.3848(2) 0.21211(18) 0.14638(15) 0.0162(4) Uani 1 1 d . . . . .
H3 H 0.414229 0.182299 0.089624 0.019 Uiso 1 1 calc R U . . .
C4 C 0.7038(2) 0.2478(2) 0.19698(17) 0.0230(5) Uani 1 1 d . . . . .
H4A H 0.678986 0.330977 0.195009 0.034 Uiso 1 1 calc R U . . .
H4B H 0.793560 0.236576 0.162452 0.034 Uiso 1 1 calc R U . . .
H4C H 0.694074 0.191485 0.271686 0.034 Uiso 1 1 calc R U . . .
C5 C 0.6174(2) 0.22352(19) 0.13730(16) 0.0187(4) Uani 1 1 d . . . . .
C6 C 0.2535(2) 0.22717(17) 0.18465(15) 0.0158(4) Uani 1 1 d . . . . .
C7 C 0.2980(2) 0.29940(17) 0.31158(15) 0.0165(4) Uani 1 1 d . . . . .
C8 C 0.0693(2) -0.0227(2) 0.1267(2) 0.0281(5) Uani 1 1 d . . . . .
H8A H 0.066616 -0.109722 0.161721 0.042 Uiso 1 1 calc R U . . .
H8B H 0.100850 -0.002733 0.049778 0.042 Uiso 1 1 calc R U . . .
H8C H -0.017353 0.021632 0.137555 0.042 Uiso 1 1 calc R U . . .
C9 C 0.2603(2) 0.34326(18) 0.40534(15) 0.0184(4) Uani 1 1 d . . . . .
H9 H 0.164274 0.352656 0.420003 0.022 Uiso 1 1 calc R U . . .
C10 C 0.1666(2) 0.19110(18) 0.13392(15) 0.0163(4) Uani 1 1 d . . . . .
H10 H 0.077404 0.219096 0.164856 0.020 Uiso 1 1 calc R U . . .
C11 C 0.2082(2) 0.27339(18) 0.26837(15) 0.0172(4) Uani 1 1 d . . . . .
C12 C 0.6609(2) 0.0939(2) 0.1390(2) 0.0298(5) Uani 1 1 d . . . . .
H12A H 0.645691 0.036495 0.213012 0.045 Uiso 1 1 calc R U . . .
H12B H 0.752732 0.083438 0.109632 0.045 Uiso 1 1 calc R U . . .
H12C H 0.611980 0.079186 0.095475 0.045 Uiso 1 1 calc R U . . .
C13 C 0.0253(2) 0.2875(2) -0.05788(18) 0.0263(5) Uani 1 1 d . . . . .
H13A H 0.029359 0.337135 -0.134328 0.040 Uiso 1 1 calc R U . . .
H13B H -0.046407 0.323742 -0.016181 0.040 Uiso 1 1 calc R U . . .
H13C H 0.012172 0.205878 -0.045465 0.040 Uiso 1 1 calc R U . . .
C14 C 0.6335(2) 0.3132(2) 0.02057(17) 0.0319(6) Uani 1 1 d . . . . .
H14A H 0.579877 0.297640 -0.018967 0.048 Uiso 1 1 calc R U . . .
H14B H 0.723756 0.303286 -0.013183 0.048 Uiso 1 1 calc R U . . .
H14C H 0.607015 0.395984 0.019468 0.048 Uiso 1 1 calc R U . . .
C15 C 0.3128(2) 0.2148(2) -0.10042(18) 0.0308(6) Uani 1 1 d . . . . .
H15A H 0.297603 0.135311 -0.092259 0.046 Uiso 1 1 calc R U . . .
H15B H 0.394527 0.206501 -0.077900 0.046 Uiso 1 1 calc R U . . .
H15C H 0.316160 0.268832 -0.175718 0.046 Uiso 1 1 calc R U . . .
C16 C 0.4670(3) 0.5233(2) 0.3094(2) 0.0336(6) Uani 1 1 d . . . . .
H16A H 0.488772 0.514462 0.239479 0.050 Uiso 1 1 calc R U . . .
H16B H 0.523527 0.462644 0.357536 0.050 Uiso 1 1 calc R U . . .
H16C H 0.478353 0.604330 0.300361 0.050 Uiso 1 1 calc R U . . .
C17 C 0.4716(3) 0.2246(2) 0.5523(2) 0.0359(6) Uani 1 1 d . . . . .
H17A H 0.471321 0.301131 0.559844 0.054 Uiso 1 1 calc R U . . .
H17B H 0.535467 0.218292 0.490290 0.054 Uiso 1 1 calc R U . . .
H17C H 0.493372 0.157124 0.617311 0.054 Uiso 1 1 calc R U . . .
C18 C 0.1850(3) 0.2359(2) 0.64864(17) 0.0351(6) Uani 1 1 d . . . . .
H18A H 0.206272 0.170888 0.715140 0.053 Uiso 1 1 calc R U . . .
H18B H 0.100509 0.231060 0.638227 0.053 Uiso 1 1 calc R U . . .
H18C H 0.183329 0.314213 0.653244 0.053 Uiso 1 1 calc R U . . .
C19 C 0.3099(3) 0.0694(2) 0.52581(19) 0.0367(6) Uani 1 1 d . . . . .
H19A H 0.369234 0.062138 0.461933 0.055 Uiso 1 1 calc R U . . .
H19B H 0.223100 0.062648 0.521895 0.055 Uiso 1 1 calc R U . . .
H19C H 0.337727 0.004679 0.590058 0.055 Uiso 1 1 calc R U . . .
C20 C 0.1935(3) 0.6056(2) 0.2671(2) 0.0366(6) Uani 1 1 d . . . . .
H20A H 0.102689 0.602306 0.299085 0.055 Uiso 1 1 calc R U . . .
H20B H 0.212968 0.581054 0.204947 0.055 Uiso 1 1 calc R U . . .
H20C H 0.211200 0.688271 0.244172 0.055 Uiso 1 1 calc R U . . .
C21 C 0.3460(2) -0.0567(2) 0.1552(2) 0.0323(6) Uani 1 1 d . . . . .
H21A H 0.345022 -0.143525 0.177632 0.048 Uiso 1 1 calc R U . . .
H21B H 0.402824 -0.043981 0.193926 0.048 Uiso 1 1 calc R U . . .
H21C H 0.377475 -0.023203 0.077923 0.048 Uiso 1 1 calc R U . . .
C22 C 0.2026(3) 0.4360(2) -0.0422(2) 0.0382(7) Uani 1 1 d . . . . .
H22A H 0.287540 0.434410 -0.028367 0.057 Uiso 1 1 calc R U . . .
H22B H 0.136098 0.469547 0.004914 0.057 Uiso 1 1 calc R U . . .
H22C H 0.196329 0.486397 -0.117188 0.057 Uiso 1 1 calc R U . . .
C23 C 0.2499(3) 0.5447(2) 0.4892(2) 0.0376(6) Uani 1 1 d . . . . .
H23A H 0.258197 0.629837 0.467861 0.056 Uiso 1 1 calc R U . . .
H23B H 0.306763 0.494171 0.541187 0.056 Uiso 1 1 calc R U . . .
H23C H 0.160735 0.532943 0.521986 0.056 Uiso 1 1 calc R U . . .
C24 C 0.1287(3) -0.0352(3) 0.3352(2) 0.0456(7) Uani 1 1 d . . . . .
H24A H 0.039358 -0.000186 0.353032 0.068 Uiso 1 1 calc R U . . .
H24B H 0.184358 -0.011119 0.367184 0.068 Uiso 1 1 calc R U . . .
H24C H 0.136052 -0.123477 0.363499 0.068 Uiso 1 1 calc R U . . .
H1 H 0.001(3) 0.236(3) 0.444(2) 0.058(9) Uiso 1 1 d . . . . .
H100 H -0.056(3) 0.267(3) 0.285(3) 0.078(11) Uiso 1 1 d . . . . .
H101 H -0.026(3) 0.439(3) 0.306(3) 0.072(10) Uiso 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ge1 C11 1.955(2) . ?
Ge1 H1 1.49(3) . ?
Ge1 H100 1.38(4) . ?
Ge1 H101 1.56(3) . ?
Si3 C22 1.862(2) . ?
Si3 C15 1.870(2) . ?
Si3 C13 1.870(2) . ?
Si3 C10 1.891(2) . ?
Si2 C8 1.866(2) . ?
Si2 C24 1.871(3) . ?
Si2 C21 1.876(3) . ?
Si2 C10 1.894(2) . ?
Si1 C20 1.865(2) . ?
Si1 C16 1.872(3) . ?
Si1 C23 1.873(2) . ?
Si1 C9 1.894(2) . ?
Si4 C17 1.863(3) . ?
Si4 C19 1.872(3) . ?
Si4 C18 1.874(2) . ?
Si4 C9 1.900(2) . ?
C1 C2 1.392(3) . ?
C1 C3 1.393(3) . ?
C1 C5 1.529(3) . ?
C2 C7 1.400(3) . ?
C2 H2 0.9500 . ?
C3 C6 1.390(3) . ?
C3 H3 0.9500 . ?
C4 C5 1.531(3) . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C5 C12 1.537(3) . ?
C5 C14 1.538(3) . ?
C6 C11 1.420(3) . ?
C6 C10 1.527(3) . ?
C7 C11 1.407(3) . ?
C7 C9 1.526(3) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 H9 1.0000 . ?
C10 H10 1.0000 . ?
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 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 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
C11 Ge1 H1 110.4(12) . . ?
C11 Ge1 H100 115.6(14) . . ?
H1 Ge1 H100 105.7(19) . . ?
C11 Ge1 H101 113.1(13) . . ?
H1 Ge1 H101 106.7(16) . . ?
H100 Ge1 H101 104.7(19) . . ?
C22 Si3 C15 108.42(13) . . ?
C22 Si3 C13 108.37(11) . . ?
C15 Si3 C13 107.64(11) . . ?
C22 Si3 C10 108.35(11) . . ?
C15 Si3 C10 114.79(10) . . ?
C13 Si3 C10 109.11(10) . . ?
C8 Si2 C24 108.72(13) . . ?
C8 Si2 C21 108.36(11) . . ?
C24 Si2 C21 108.10(13) . . ?
C8 Si2 C10 109.88(10) . . ?
C24 Si2 C10 108.58(11) . . ?
C21 Si2 C10 113.11(10) . . ?
C20 Si1 C16 108.05(12) . . ?
C20 Si1 C23 108.51(12) . . ?
C16 Si1 C23 108.00(13) . . ?
C20 Si1 C9 107.04(11) . . ?
C16 Si1 C9 115.21(10) . . ?
C23 Si1 C9 109.85(11) . . ?
C17 Si4 C19 108.66(13) . . ?
C17 Si4 C18 110.18(12) . . ?
C19 Si4 C18 108.39(12) . . ?
C17 Si4 C9 112.97(11) . . ?
C19 Si4 C9 108.71(10) . . ?
C18 Si4 C9 107.83(10) . . ?
C2 C1 C3 116.99(19) . . ?
C2 C1 C5 123.20(19) . . ?
C3 C1 C5 119.78(18) . . ?
C1 C2 C7 122.14(19) . . ?
C1 C2 H2 118.9 . . ?
C7 C2 H2 118.9 . . ?
C6 C3 C1 123.34(18) . . ?
C6 C3 H3 118.3 . . ?
C1 C3 H3 118.3 . . ?
C5 C4 H4A 109.5 . . ?
C5 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
C5 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
C1 C5 C4 112.61(17) . . ?
C1 C5 C12 109.49(18) . . ?
C4 C5 C12 108.27(17) . . ?
C1 C5 C14 108.39(17) . . ?
C4 C5 C14 108.62(18) . . ?
C12 C5 C14 109.43(19) . . ?
C3 C6 C11 118.78(19) . . ?
C3 C6 C10 117.22(17) . . ?
C11 C6 C10 123.99(18) . . ?
C2 C7 C11 119.81(18) . . ?
C2 C7 C9 117.00(18) . . ?
C11 C7 C9 123.15(19) . . ?
Si2 C8 H8A 109.5 . . ?
Si2 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
Si2 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C7 C9 Si1 113.26(14) . . ?
C7 C9 Si4 111.02(13) . . ?
Si1 C9 Si4 118.97(11) . . ?
C7 C9 H9 103.9 . . ?
Si1 C9 H9 103.9 . . ?
Si4 C9 H9 103.9 . . ?
C6 C10 Si3 112.37(14) . . ?
C6 C10 Si2 110.08(13) . . ?
Si3 C10 Si2 119.41(10) . . ?
C6 C10 H10 104.5 . . ?
Si3 C10 H10 104.5 . . ?
Si2 C10 H10 104.5 . . ?
C7 C11 C6 118.90(19) . . ?
C7 C11 Ge1 118.68(15) . . ?
C6 C11 Ge1 122.41(16) . . ?
C5 C12 H12A 109.5 . . ?
C5 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C5 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
Si3 C13 H13A 109.5 . . ?
Si3 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
Si3 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C5 C14 H14A 109.5 . . ?
C5 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C5 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
Si3 C15 H15A 109.5 . . ?
Si3 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
Si3 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
Si1 C16 H16A 109.5 . . ?
Si1 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
Si1 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
Si4 C17 H17A 109.5 . . ?
Si4 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
Si4 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
Si4 C18 H18A 109.5 . . ?
Si4 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
Si4 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
Si4 C19 H19A 109.5 . . ?
Si4 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
Si4 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
Si1 C20 H20A 109.5 . . ?
Si1 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
Si1 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
Si2 C21 H21A 109.5 . . ?
Si2 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
Si2 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
Si3 C22 H22A 109.5 . . ?
Si3 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
Si3 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
Si1 C23 H23A 109.5 . . ?
Si1 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
Si1 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
Si2 C24 H24A 109.5 . . ?
Si2 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
Si2 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?

_refine_diff_density_max         0.642
_refine_diff_density_min         -0.744
_refine_diff_density_rms         0.095



####################################################################### 
# 
# 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_shelx_CCDC1
_database_code_depnum_ccdc_archive 'CCDC 2153533'
loop_
_audit_author_name
_audit_author_address
'Hartmut Schubert'
;Universtity of Tuebingen
Germany
;
_audit_update_record             
;
2022-02-21 deposited with the CCDC.	2022-03-22 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C49 H68 Ge N2'
_chemical_formula_weight         757.66

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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ge Ge 0.1547 1.8001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_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'

_cell_length_a                   12.3798(4)
_cell_length_b                   13.1930(4)
_cell_length_c                   14.5014(5)
_cell_angle_alpha                76.764(2)
_cell_angle_beta                 74.374(2)
_cell_angle_gamma                86.728(2)
_cell_volume                     2220.31(13)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9711
_cell_measurement_theta_min      2.33
_cell_measurement_theta_max      27.96

_exptl_crystal_description       prism
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.133
_exptl_crystal_F_000             816
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.440
_exptl_crystal_size_mid          0.331
_exptl_crystal_size_min          0.188
_exptl_absorpt_coefficient_mu    0.723
_shelx_estimated_absorpt_T_min   0.742
_shelx_estimated_absorpt_T_max   0.876
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6618
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_process_details   'SADABS V2012/1 (Bruker AXS Inc.)'


_exptl_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            61443
_diffrn_reflns_av_unetI/netI     0.0212
_diffrn_reflns_av_R_equivalents  0.0263
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         1.923
_diffrn_reflns_theta_max         27.979
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measured_fraction_theta_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_point_group_measured_fraction_full 0.996
_reflns_number_total             10590
_reflns_number_gt                9383
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_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       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_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)+(0.0267P)²+1.2161P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         10590
_refine_ls_number_parameters     489
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0361
_refine_ls_R_factor_gt           0.0288
_refine_ls_wR_factor_ref         0.0704
_refine_ls_wR_factor_gt          0.0667
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_restrained_S_all      1.037
_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
Ge1 Ge 0.40656(2) 0.59926(2) 0.14718(2) 0.01747(4) Uani 1 1 d . . . . .
N1 N 0.37169(9) 0.39522(9) 0.09520(8) 0.0188(2) Uani 1 1 d . . . . .
N2 N 0.47700(9) 0.36773(9) 0.19302(8) 0.0203(2) Uani 1 1 d . . . . .
C1 C 0.32490(10) 0.60481(9) 0.28708(8) 0.0128(2) Uani 1 1 d . . . . .
C2 C 0.21766(10) 0.56024(9) 0.33434(9) 0.0134(2) Uani 1 1 d . . . . .
C6 C 0.36466(10) 0.67374(9) 0.33262(9) 0.0135(2) Uani 1 1 d . . . . .
C37 C 0.41207(11) 0.44143(10) 0.15342(9) 0.0181(2) Uani 1 1 d . . . . .
C33 C 0.09853(10) 0.55273(10) 0.21990(9) 0.0155(2) Uani 1 1 d . . . . .
C5 C 0.30419(11) 0.68977(10) 0.42456(9) 0.0161(2) Uani 1 1 d . . . . .
H5 H 0.3338 0.7343 0.4548 0.019 Uiso 1 1 calc R U . . .
C23 C 0.14621(10) 0.38993(10) 0.31954(9) 0.0152(2) Uani 1 1 d . . . . .
C15 C 0.65054(10) 0.87777(9) 0.18475(9) 0.0156(2) Uani 1 1 d . . . . .
C22 C 0.15630(10) 0.49915(9) 0.28822(9) 0.0139(2) Uani 1 1 d . . . . .
C34 C 0.10779(11) 0.67083(10) 0.18404(9) 0.0171(2) Uani 1 1 d . . . . .
H34 H 0.1800 0.6925 0.1925 0.021 Uiso 1 1 calc R U . . .
C3 C 0.15805(10) 0.57861(10) 0.42572(9) 0.0164(2) Uani 1 1 d . . . . .
H3 H 0.0863 0.5474 0.4567 0.020 Uiso 1 1 calc R U . . .
C10 C 0.54516(11) 0.90208(9) 0.16945(9) 0.0158(2) Uani 1 1 d . . . . .
H10 H 0.5359 0.9656 0.1257 0.019 Uiso 1 1 calc R U . . .
C32 C 0.02929(11) 0.49625(10) 0.18790(10) 0.0197(3) Uani 1 1 d . . . . .
H32 H -0.0108 0.5326 0.1430 0.024 Uiso 1 1 calc R U . . .
C8 C 0.57262(10) 0.71467(9) 0.29502(9) 0.0149(2) Uani 1 1 d . . . . .
C9 C 0.66239(10) 0.78321(10) 0.24809(9) 0.0163(2) Uani 1 1 d . . . . .
H9 H 0.7338 0.7651 0.2595 0.020 Uiso 1 1 calc R U . . .
C27 C 0.07663(11) 0.33727(10) 0.28504(10) 0.0191(3) Uani 1 1 d . . . . .
H27 H 0.0696 0.2638 0.3070 0.023 Uiso 1 1 calc R U . . .
C24 C 0.21005(10) 0.32843(10) 0.39055(9) 0.0163(2) Uani 1 1 d . . . . .
H24 H 0.2771 0.3705 0.3850 0.020 Uiso 1 1 calc R U . . .
C11 C 0.45223(10) 0.83662(9) 0.21609(9) 0.0147(2) Uani 1 1 d . . . . .
C4 C 0.20137(11) 0.64125(10) 0.47197(9) 0.0177(2) Uani 1 1 d . . . . .
H4 H 0.1613 0.6508 0.5352 0.021 Uiso 1 1 calc R U . . .
C7 C 0.46619(10) 0.74189(9) 0.27959(9) 0.0138(2) Uani 1 1 d . . . . .
C16 C 0.74941(11) 0.95153(10) 0.13339(10) 0.0190(3) Uani 1 1 d . . . . .
H16 H 0.7203 1.0160 0.0965 0.023 Uiso 1 1 calc R U . . .
C40 C 0.41056(11) 0.29384(10) 0.09842(10) 0.0207(3) Uani 1 1 d . . . . .
C19 C 0.58966(11) 0.61250(10) 0.36337(9) 0.0175(2) Uani 1 1 d . . . . .
H19 H 0.5274 0.5645 0.3692 0.021 Uiso 1 1 calc R U . . .
C26 C 0.25164(12) 0.22320(10) 0.36677(10) 0.0217(3) Uani 1 1 d . . . . .
H26A H 0.1884 0.1744 0.3874 0.033 Uiso 1 1 calc R U . . .
H26B H 0.3082 0.1954 0.4019 0.033 Uiso 1 1 calc R U . . .
H26C H 0.2849 0.2326 0.2959 0.033 Uiso 1 1 calc R U . . .
C28 C 0.01693(11) 0.38887(10) 0.21936(10) 0.0208(3) Uani 1 1 d . . . . .
C25 C 0.13804(11) 0.31026(11) 0.49706(9) 0.0208(3) Uani 1 1 d . . . . .
H25A H 0.1244 0.3769 0.5171 0.031 Uiso 1 1 calc R U . . .
H25B H 0.1774 0.2635 0.5400 0.031 Uiso 1 1 calc R U . . .
H25C H 0.0663 0.2787 0.5022 0.031 Uiso 1 1 calc R U . . .
C12 C 0.33799(10) 0.87237(10) 0.20034(9) 0.0172(2) Uani 1 1 d . . . . .
H12 H 0.2842 0.8131 0.2331 0.021 Uiso 1 1 calc R U . . .
C41 C 0.47810(12) 0.27688(10) 0.15976(10) 0.0224(3) Uani 1 1 d . . . . .
C20 C 0.58139(13) 0.62838(11) 0.46659(10) 0.0255(3) Uani 1 1 d . . . . .
H20A H 0.6360 0.6813 0.4624 0.038 Uiso 1 1 calc R U . . .
H20B H 0.5974 0.5626 0.5081 0.038 Uiso 1 1 calc R U . . .
H20C H 0.5056 0.6514 0.4952 0.038 Uiso 1 1 calc R U . . .
C39 C 0.29756(12) 0.44523(12) 0.03531(10) 0.0251(3) Uani 1 1 d . . . . .
H39A H 0.2226 0.4139 0.0631 0.038 Uiso 1 1 calc R U . . .
H39B H 0.3273 0.4355 -0.0319 0.038 Uiso 1 1 calc R U . . .
H39C H 0.2930 0.5198 0.0345 0.038 Uiso 1 1 calc R U . . .
C29 C -0.05739(13) 0.32845(11) 0.18241(11) 0.0274(3) Uani 1 1 d . . . . .
H29 H -0.0860 0.3785 0.1313 0.033 Uiso 1 1 calc R U . . .
C18 C 0.80246(13) 0.98390(11) 0.20622(11) 0.0276(3) Uani 1 1 d . . . . .
H18A H 0.7461 1.0185 0.2503 0.041 Uiso 1 1 calc R U . . .
H18B H 0.8650 1.0319 0.1702 0.041 Uiso 1 1 calc R U . . .
H18C H 0.8302 0.9220 0.2448 0.041 Uiso 1 1 calc R U . . .
C13 C 0.33923(12) 0.90125(11) 0.09169(10) 0.0229(3) Uani 1 1 d . . . . .
H13A H 0.3906 0.9600 0.0578 0.034 Uiso 1 1 calc R U . . .
H13B H 0.2635 0.9208 0.0856 0.034 Uiso 1 1 calc R U . . .
H13C H 0.3644 0.8414 0.0621 0.034 Uiso 1 1 calc R U . . .
C17 C 0.83751(12) 0.90463(11) 0.05847(11) 0.0255(3) Uani 1 1 d . . . . .
H17A H 0.8677 0.8410 0.0925 0.038 Uiso 1 1 calc R U . . .
H17B H 0.8984 0.9550 0.0245 0.038 Uiso 1 1 calc R U . . .
H17C H 0.8028 0.8878 0.0105 0.038 Uiso 1 1 calc R U . . .
C43 C 0.37518(13) 0.22420(11) 0.04419(11) 0.0273(3) Uani 1 1 d . . . . .
H43A H 0.4173 0.1589 0.0513 0.041 Uiso 1 1 calc R U . . .
H43B H 0.3902 0.2586 -0.0255 0.041 Uiso 1 1 calc R U . . .
H43C H 0.2947 0.2093 0.0711 0.041 Uiso 1 1 calc R U . . .
C21 C 0.70024(12) 0.55907(11) 0.32466(11) 0.0252(3) Uani 1 1 d . . . . .
H21A H 0.7080 0.5555 0.2564 0.038 Uiso 1 1 calc R U . . .
H21B H 0.7005 0.4885 0.3650 0.038 Uiso 1 1 calc R U . . .
H21C H 0.7630 0.5991 0.3278 0.038 Uiso 1 1 calc R U . . .
C36 C 0.01328(14) 0.72512(12) 0.24639(12) 0.0313(3) Uani 1 1 d . . . . .
H36A H -0.0590 0.7048 0.2405 0.047 Uiso 1 1 calc R U . . .
H36B H 0.0229 0.8007 0.2235 0.047 Uiso 1 1 calc R U . . .
H36C H 0.0153 0.7047 0.3153 0.047 Uiso 1 1 calc R U . . .
C38 C 0.53473(14) 0.37908(12) 0.26529(12) 0.0303(3) Uani 1 1 d . . . . .
H38A H 0.5109 0.4437 0.2872 0.045 Uiso 1 1 calc R U . . .
H38B H 0.6159 0.3814 0.2356 0.045 Uiso 1 1 calc R U . . .
H38C H 0.5163 0.3197 0.3217 0.045 Uiso 1 1 calc R U . . .
C46 C 0.50598(14) 0.06197(12) 0.56389(11) 0.0315(3) Uani 1 1 d . . . . .
H46 H 0.5103 0.1045 0.6076 0.038 Uiso 1 1 calc R U . . .
C14 C 0.29530(12) 0.96356(11) 0.24942(11) 0.0256(3) Uani 1 1 d . . . . .
H14A H 0.2878 0.9414 0.3201 0.038 Uiso 1 1 calc R U . . .
H14B H 0.2221 0.9859 0.2383 0.038 Uiso 1 1 calc R U . . .
H14C H 0.3487 1.0216 0.2212 0.038 Uiso 1 1 calc R U . . .
C30 C 0.00807(14) 0.24384(13) 0.13462(12) 0.0321(3) Uani 1 1 d . . . . .
H30A H 0.0719 0.2754 0.0810 0.048 Uiso 1 1 calc R U . . .
H30B H -0.0411 0.2091 0.1085 0.048 Uiso 1 1 calc R U . . .
H30C H 0.0354 0.1927 0.1837 0.048 Uiso 1 1 calc R U . . .
C35 C 0.11129(14) 0.70789(11) 0.07546(10) 0.0288(3) Uani 1 1 d . . . . .
H35A H 0.1726 0.6730 0.0361 0.043 Uiso 1 1 calc R U . . .
H35B H 0.1235 0.7834 0.0554 0.043 Uiso 1 1 calc R U . . .
H35C H 0.0399 0.6910 0.0652 0.043 Uiso 1 1 calc R U . . .
C45 C 0.40569(14) 0.05054(12) 0.54310(11) 0.0308(3) Uani 1 1 d . . . . .
H45 H 0.3406 0.0851 0.5727 0.037 Uiso 1 1 calc R U . . .
C42 C 0.54500(14) 0.18435(12) 0.19087(13) 0.0343(4) Uani 1 1 d . . . . .
H42A H 0.5369 0.1300 0.1570 0.051 Uiso 1 1 calc R U . . .
H42B H 0.5179 0.1579 0.2620 0.051 Uiso 1 1 calc R U . . .
H42C H 0.6242 0.2042 0.1741 0.051 Uiso 1 1 calc R U . . .
C44 C 0.39948(14) -0.01107(13) 0.47931(12) 0.0336(3) Uani 1 1 d . . . . .
H44 H 0.3302 -0.0185 0.4650 0.040 Uiso 1 1 calc R U . . .
C48 C 0.07748(15) 0.92115(14) 0.50120(15) 0.0442(4) Uani 1 1 d . . . . .
H48 H 0.1308 0.8665 0.5019 0.053 Uiso 1 1 calc R U . . .
C31 C -0.15889(13) 0.28092(13) 0.26524(14) 0.0358(4) Uani 1 1 d . . . . .
H31A H -0.1331 0.2319 0.3166 0.054 Uiso 1 1 calc R U . . .
H31B H -0.2062 0.2441 0.2391 0.054 Uiso 1 1 calc R U . . .
H31C H -0.2023 0.3364 0.2930 0.054 Uiso 1 1 calc R U . . .
C47 C 0.01921(16) 0.94105(14) 0.43032(14) 0.0437(4) Uani 1 1 d . . . . .
H47 H 0.0327 0.9003 0.3822 0.052 Uiso 1 1 calc R U . . .
C49 C 0.05885(16) 0.97984(15) 0.57072(14) 0.0441(4) Uani 1 1 d . . . . .
H49 H 0.0994 0.9662 0.6193 0.053 Uiso 1 1 calc R U . . .
H500 H 0.5230(14) 0.5946(13) 0.1627(13) 0.034(5) Uiso 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ge1 C1 2.0244(12) . ?
Ge1 C37 2.0613(13) . ?
Ge1 H500 1.513(17) . ?
N1 C37 1.3535(17) . ?
N1 C40 1.3903(17) . ?
N1 C39 1.4594(17) . ?
N2 C37 1.3510(17) . ?
N2 C41 1.3888(17) . ?
N2 C38 1.4558(18) . ?
C1 C2 1.4115(16) . ?
C1 C6 1.4165(17) . ?
C2 C3 1.3997(17) . ?
C2 C22 1.5047(17) . ?
C6 C5 1.3986(17) . ?
C6 C7 1.5071(16) . ?
C33 C32 1.3967(18) . ?
C33 C22 1.4129(16) . ?
C33 C34 1.5259(17) . ?
C5 C4 1.3866(18) . ?
C5 H5 0.9500 . ?
C23 C27 1.3910(18) . ?
C23 C22 1.4101(17) . ?
C23 C24 1.5250(16) . ?
C15 C10 1.3891(17) . ?
C15 C9 1.3959(17) . ?
C15 C16 1.5208(17) . ?
C34 C36 1.5266(19) . ?
C34 C35 1.5276(18) . ?
C34 H34 1.0000 . ?
C3 C4 1.3852(18) . ?
C3 H3 0.9500 . ?
C10 C11 1.3977(17) . ?
C10 H10 0.9500 . ?
C32 C28 1.3892(18) . ?
C32 H32 0.9500 . ?
C8 C9 1.3934(17) . ?
C8 C7 1.4082(17) . ?
C8 C19 1.5205(16) . ?
C9 H9 0.9500 . ?
C27 C28 1.3934(18) . ?
C27 H27 0.9500 . ?
C24 C25 1.5334(18) . ?
C24 C26 1.5342(18) . ?
C24 H24 1.0000 . ?
C11 C7 1.4049(16) . ?
C11 C12 1.5242(17) . ?
C4 H4 0.9500 . ?
C16 C18 1.5301(19) . ?
C16 C17 1.5313(19) . ?
C16 H16 1.0000 . ?
C40 C41 1.352(2) . ?
C40 C43 1.4889(19) . ?
C19 C21 1.5307(19) . ?
C19 C20 1.5341(19) . ?
C19 H19 1.0000 . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C28 C29 1.5212(18) . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C12 C13 1.5299(18) . ?
C12 C14 1.5330(19) . ?
C12 H12 1.0000 . ?
C41 C42 1.488(2) . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C39 H39A 0.9800 . ?
C39 H39B 0.9800 . ?
C39 H39C 0.9800 . ?
C29 C30 1.527(2) . ?
C29 C31 1.532(2) . ?
C29 H29 1.0000 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C43 H43A 0.9800 . ?
C43 H43B 0.9800 . ?
C43 H43C 0.9800 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?
C38 H38A 0.9800 . ?
C38 H38B 0.9800 . ?
C38 H38C 0.9800 . ?
C46 C45 1.378(2) . ?
C46 C44 1.386(2) 2_656 ?
C46 H46 0.9500 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
C35 H35A 0.9800 . ?
C35 H35B 0.9800 . ?
C35 H35C 0.9800 . ?
C45 C44 1.383(2) . ?
C45 H45 0.9500 . ?
C42 H42A 0.9800 . ?
C42 H42B 0.9800 . ?
C42 H42C 0.9800 . ?
C44 C46 1.386(2) 2_656 ?
C44 H44 0.9500 . ?
C48 C49 1.371(3) . ?
C48 C47 1.378(3) . ?
C48 H48 0.9500 . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
C47 C49 1.382(3) 2_576 ?
C47 H47 0.9500 . ?
C49 C47 1.382(3) 2_576 ?
C49 H49 0.9500 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 Ge1 C37 102.04(5) . . ?
C1 Ge1 H500 95.5(7) . . ?
C37 Ge1 H500 89.9(7) . . ?
C37 N1 C40 111.62(11) . . ?
C37 N1 C39 124.62(11) . . ?
C40 N1 C39 123.76(11) . . ?
C37 N2 C41 111.62(11) . . ?
C37 N2 C38 124.77(11) . . ?
C41 N2 C38 123.54(12) . . ?
C2 C1 C6 117.16(11) . . ?
C2 C1 Ge1 122.70(9) . . ?
C6 C1 Ge1 118.79(8) . . ?
C3 C2 C1 120.45(11) . . ?
C3 C2 C22 115.82(11) . . ?
C1 C2 C22 123.53(11) . . ?
C5 C6 C1 121.14(11) . . ?
C5 C6 C7 116.97(11) . . ?
C1 C6 C7 121.53(10) . . ?
N2 C37 N1 104.12(11) . . ?
N2 C37 Ge1 129.42(10) . . ?
N1 C37 Ge1 124.45(9) . . ?
C32 C33 C22 118.91(11) . . ?
C32 C33 C34 120.15(11) . . ?
C22 C33 C34 120.91(11) . . ?
C4 C5 C6 120.64(12) . . ?
C4 C5 H5 119.7 . . ?
C6 C5 H5 119.7 . . ?
C27 C23 C22 119.36(11) . . ?
C27 C23 C24 119.36(11) . . ?
C22 C23 C24 121.28(11) . . ?
C10 C15 C9 117.67(11) . . ?
C10 C15 C16 120.91(11) . . ?
C9 C15 C16 121.42(11) . . ?
C23 C22 C33 119.44(11) . . ?
C23 C22 C2 120.82(10) . . ?
C33 C22 C2 119.43(11) . . ?
C33 C34 C36 111.17(11) . . ?
C33 C34 C35 113.19(11) . . ?
C36 C34 C35 110.20(11) . . ?
C33 C34 H34 107.3 . . ?
C36 C34 H34 107.3 . . ?
C35 C34 H34 107.3 . . ?
C4 C3 C2 121.47(12) . . ?
C4 C3 H3 119.3 . . ?
C2 C3 H3 119.3 . . ?
C15 C10 C11 122.45(11) . . ?
C15 C10 H10 118.8 . . ?
C11 C10 H10 118.8 . . ?
C28 C32 C33 122.32(11) . . ?
C28 C32 H32 118.8 . . ?
C33 C32 H32 118.8 . . ?
C9 C8 C7 119.30(11) . . ?
C9 C8 C19 120.03(11) . . ?
C7 C8 C19 120.67(11) . . ?
C8 C9 C15 121.94(11) . . ?
C8 C9 H9 119.0 . . ?
C15 C9 H9 119.0 . . ?
C23 C27 C28 122.10(12) . . ?
C23 C27 H27 118.9 . . ?
C28 C27 H27 118.9 . . ?
C23 C24 C25 111.29(10) . . ?
C23 C24 C26 112.57(10) . . ?
C25 C24 C26 109.11(10) . . ?
C23 C24 H24 107.9 . . ?
C25 C24 H24 107.9 . . ?
C26 C24 H24 107.9 . . ?
C10 C11 C7 118.84(11) . . ?
C10 C11 C12 119.07(11) . . ?
C7 C11 C12 122.02(11) . . ?
C3 C4 C5 118.92(12) . . ?
C3 C4 H4 120.5 . . ?
C5 C4 H4 120.5 . . ?
C11 C7 C8 119.78(11) . . ?
C11 C7 C6 118.48(10) . . ?
C8 C7 C6 121.69(10) . . ?
C15 C16 C18 112.16(11) . . ?
C15 C16 C17 111.30(11) . . ?
C18 C16 C17 110.74(12) . . ?
C15 C16 H16 107.5 . . ?
C18 C16 H16 107.5 . . ?
C17 C16 H16 107.5 . . ?
C41 C40 N1 106.19(12) . . ?
C41 C40 C43 131.25(13) . . ?
N1 C40 C43 122.53(13) . . ?
C8 C19 C21 113.17(11) . . ?
C8 C19 C20 110.93(11) . . ?
C21 C19 C20 110.14(11) . . ?
C8 C19 H19 107.4 . . ?
C21 C19 H19 107.4 . . ?
C20 C19 H19 107.4 . . ?
C24 C26 H26A 109.5 . . ?
C24 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
C24 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C32 C28 C27 117.83(12) . . ?
C32 C28 C29 121.58(12) . . ?
C27 C28 C29 120.58(12) . . ?
C24 C25 H25A 109.5 . . ?
C24 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
C24 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C11 C12 C13 112.62(11) . . ?
C11 C12 C14 110.45(11) . . ?
C13 C12 C14 110.63(11) . . ?
C11 C12 H12 107.6 . . ?
C13 C12 H12 107.6 . . ?
C14 C12 H12 107.6 . . ?
C40 C41 N2 106.44(12) . . ?
C40 C41 C42 131.25(13) . . ?
N2 C41 C42 122.31(13) . . ?
C19 C20 H20A 109.5 . . ?
C19 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C19 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
N1 C39 H39A 109.5 . . ?
N1 C39 H39B 109.5 . . ?
H39A C39 H39B 109.5 . . ?
N1 C39 H39C 109.5 . . ?
H39A C39 H39C 109.5 . . ?
H39B C39 H39C 109.5 . . ?
C28 C29 C30 111.61(12) . . ?
C28 C29 C31 111.23(13) . . ?
C30 C29 C31 110.27(12) . . ?
C28 C29 H29 107.9 . . ?
C30 C29 H29 107.9 . . ?
C31 C29 H29 107.9 . . ?
C16 C18 H18A 109.5 . . ?
C16 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C16 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C12 C13 H13A 109.5 . . ?
C12 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C12 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C16 C17 H17A 109.5 . . ?
C16 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C16 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C40 C43 H43A 109.5 . . ?
C40 C43 H43B 109.5 . . ?
H43A C43 H43B 109.5 . . ?
C40 C43 H43C 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?
C19 C21 H21A 109.5 . . ?
C19 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C19 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C34 C36 H36A 109.5 . . ?
C34 C36 H36B 109.5 . . ?
H36A C36 H36B 109.5 . . ?
C34 C36 H36C 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
N2 C38 H38A 109.5 . . ?
N2 C38 H38B 109.5 . . ?
H38A C38 H38B 109.5 . . ?
N2 C38 H38C 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
C45 C46 C44 119.59(14) . 2_656 ?
C45 C46 H46 120.2 . . ?
C44 C46 H46 120.2 2_656 . ?
C12 C14 H14A 109.5 . . ?
C12 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C12 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C29 C30 H30A 109.5 . . ?
C29 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
C29 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C34 C35 H35A 109.5 . . ?
C34 C35 H35B 109.5 . . ?
H35A C35 H35B 109.5 . . ?
C34 C35 H35C 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
C46 C45 C44 120.21(15) . . ?
C46 C45 H45 119.9 . . ?
C44 C45 H45 119.9 . . ?
C41 C42 H42A 109.5 . . ?
C41 C42 H42B 109.5 . . ?
H42A C42 H42B 109.5 . . ?
C41 C42 H42C 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
C45 C44 C46 120.20(15) . 2_656 ?
C45 C44 H44 119.9 . . ?
C46 C44 H44 119.9 2_656 . ?
C49 C48 C47 120.36(17) . . ?
C49 C48 H48 119.8 . . ?
C47 C48 H48 119.8 . . ?
C29 C31 H31A 109.5 . . ?
C29 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
C29 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C48 C47 C49 120.03(18) . 2_576 ?
C48 C47 H47 120.0 . . ?
C49 C47 H47 120.0 2_576 . ?
C48 C49 C47 119.60(19) . 2_576 ?
C48 C49 H49 120.2 . . ?
C47 C49 H49 120.2 2_576 . ?

_refine_diff_density_max         0.462
_refine_diff_density_min         -0.440
_refine_diff_density_rms         0.047

_shelxl_version_number           2014-3



####################################################################### 
# 
# 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_MA55_0m_a
_database_code_depnum_ccdc_archive 'CCDC 2153535'
loop_
_audit_author_name
_audit_author_address
'Hartmut Schubert'
;Universtity of Tuebingen
Germany
;
_audit_update_record             
;
2022-02-21 deposited with the CCDC.	2022-03-22 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/1
_shelx_SHELXL_version_number     2018/1
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C48 H102 Si8 Sn2, C6 H6'
_chemical_formula_sum            'C54 H108 Si8 Sn2'
_chemical_formula_weight         1219.54

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'
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'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_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'

_cell_length_a                   9.1345(2)
_cell_length_b                   12.1875(3)
_cell_length_c                   17.1264(3)
_cell_angle_alpha                108.1370(10)
_cell_angle_beta                 95.7350(10)
_cell_angle_gamma                104.1100(10)
_cell_volume                     1724.96(7)
_cell_formula_units_Z            1
_cell_measurement_temperature    170(2)
_cell_measurement_reflns_used    9871
_cell_measurement_theta_min      2.91
_cell_measurement_theta_max      28.09

_exptl_crystal_description       prism
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.174
_exptl_crystal_F_000             644
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.18
_exptl_absorpt_coefficient_mu    0.892
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6932
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_process_details   'SADABS V2012/1 (Bruker AXS Inc.)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      170(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            35182
_diffrn_reflns_av_unetI/netI     0.0178
_diffrn_reflns_av_R_equivalents  0.0215
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         2.912
_diffrn_reflns_theta_max         28.152
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             8352
_reflns_number_gt                7782
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_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       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXT 2014/4 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2018/1 (Sheldrick, 2018)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_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)+(0.0305P)²+0.8288P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         8352
_refine_ls_number_parameters     312
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0243
_refine_ls_R_factor_gt           0.0219
_refine_ls_wR_factor_ref         0.0600
_refine_ls_wR_factor_gt          0.0583
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_restrained_S_all      1.065
_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
Sn1 Sn 0.59967(2) 0.52637(2) 0.07409(2) 0.02115(4) Uani 1 1 d . . . . .
Si3 Si 0.11584(5) 0.41750(4) 0.13794(3) 0.02736(9) Uani 1 1 d . . . . .
Si4 Si 0.35618(5) 0.28813(4) 0.20188(3) 0.02769(10) Uani 1 1 d . . . . .
Si1 Si 0.62125(6) 0.92836(4) 0.19019(3) 0.02896(10) Uani 1 1 d . . . . .
Si2 Si 0.91996(6) 0.88002(5) 0.27871(4) 0.04146(13) Uani 1 1 d . . . . .
C1 C 0.42302(16) 0.53714(12) 0.21978(9) 0.0186(3) Uani 1 1 d . . . . .
C2 C 0.53278(16) 0.60952(12) 0.18985(8) 0.0179(3) Uani 1 1 d . . . . .
C3 C 0.40487(17) 0.58175(14) 0.30280(9) 0.0222(3) Uani 1 1 d . . . . .
H3 H 0.331636 0.532343 0.322671 0.027 Uiso 1 1 calc R U . . .
C4 C 0.49059(18) 0.69630(14) 0.35746(9) 0.0223(3) Uani 1 1 d . . . . .
C5 C 0.32072(16) 0.41234(13) 0.16472(9) 0.0209(3) Uani 1 1 d . . . . .
H5 H 0.357501 0.397488 0.110345 0.025 Uiso 1 1 calc R U . . .
C6 C 0.1269(2) 0.55490(17) 0.10945(12) 0.0349(4) Uani 1 1 d . . . . .
H6A H 0.022810 0.557164 0.091409 0.052 Uiso 1 1 calc R U . . .
H6B H 0.184084 0.552500 0.063763 0.052 Uiso 1 1 calc R U . . .
H6C H 0.179766 0.627144 0.158240 0.052 Uiso 1 1 calc R U . . .
C7 C 0.4737(2) 0.73990(16) 0.44928(9) 0.0297(3) Uani 1 1 d . . . . .
C8 C 0.61091(16) 0.72963(13) 0.24201(9) 0.0204(3) Uani 1 1 d . . . . .
C9 C 0.58790(18) 0.76926(14) 0.32466(9) 0.0241(3) Uani 1 1 d . . . . .
H9 H 0.641395 0.849715 0.359776 0.029 Uiso 1 1 calc R U . . .
C10 C 0.0052(2) 0.27850(19) 0.04767(14) 0.0479(5) Uani 1 1 d . . . . .
H10A H -0.092981 0.288164 0.026791 0.072 Uiso 1 1 calc R U . . .
H10B H -0.014084 0.208649 0.066086 0.072 Uiso 1 1 calc R U . . .
H10C H 0.064894 0.265897 0.002856 0.072 Uiso 1 1 calc R U . . .
C11 C 0.0077(2) 0.4285(2) 0.22568(14) 0.0492(5) Uani 1 1 d . . . . .
H11A H 0.066427 0.497889 0.274998 0.074 Uiso 1 1 calc R U . . .
H11B H -0.007792 0.354518 0.239190 0.074 Uiso 1 1 calc R U . . .
H11C H -0.092433 0.438789 0.208876 0.074 Uiso 1 1 calc R U . . .
C12 C 0.71929(18) 0.81865(13) 0.21338(10) 0.0251(3) Uani 1 1 d . . . . .
H12 H 0.732127 0.768646 0.157326 0.030 Uiso 1 1 calc R U . . .
C13 C 0.4530(3) 0.83969(19) 0.10285(13) 0.0465(5) Uani 1 1 d . . . . .
H13A H 0.400033 0.894471 0.089673 0.070 Uiso 1 1 calc R U . . .
H13B H 0.381924 0.780851 0.119792 0.070 Uiso 1 1 calc R U . . .
H13C H 0.488870 0.797251 0.053274 0.070 Uiso 1 1 calc R U . . .
C14 C 0.2413(3) 0.25853(19) 0.28158(14) 0.0464(5) Uani 1 1 d . . . . .
H14A H 0.269975 0.196878 0.300045 0.070 Uiso 1 1 calc R U . . .
H14B H 0.131536 0.230029 0.256724 0.070 Uiso 1 1 calc R U . . .
H14C H 0.262328 0.333188 0.329703 0.070 Uiso 1 1 calc R U . . .
C15 C 0.5484(3) 1.01239(19) 0.28153(13) 0.0452(5) Uani 1 1 d . . . . .
H15A H 0.635287 1.062831 0.327340 0.068 Uiso 1 1 calc R U . . .
H15B H 0.478756 0.954851 0.300137 0.068 Uiso 1 1 calc R U . . .
H15C H 0.493011 1.063619 0.265096 0.068 Uiso 1 1 calc R U . . .
C16 C 0.7552(3) 1.03912(19) 0.15590(15) 0.0510(5) Uani 1 1 d . . . . .
H16A H 0.699672 1.089615 0.138573 0.076 Uiso 1 1 calc R U . . .
H16B H 0.795755 0.995563 0.108709 0.076 Uiso 1 1 calc R U . . .
H16C H 0.840514 1.090214 0.202447 0.076 Uiso 1 1 calc R U . . .
C17 C 0.3066(3) 0.14594(18) 0.10938(14) 0.0534(6) Uani 1 1 d . . . . .
H17A H 0.324923 0.080804 0.127403 0.080 Uiso 1 1 calc R U . . .
H17B H 0.370861 0.157958 0.068493 0.080 Uiso 1 1 calc R U . . .
H17C H 0.198020 0.124391 0.083680 0.080 Uiso 1 1 calc R U . . .
C18 C 0.5636(2) 0.3317(2) 0.25017(18) 0.0541(6) Uani 1 1 d . . . . .
H18A H 0.589790 0.407904 0.297428 0.081 Uiso 1 1 calc R U . . .
H18B H 0.626721 0.341495 0.208405 0.081 Uiso 1 1 calc R U . . .
H18C H 0.583321 0.268457 0.270055 0.081 Uiso 1 1 calc R U . . .
C19 C 1.0602(3) 0.9076(2) 0.20932(19) 0.0623(7) Uani 1 1 d . . . . .
H19A H 1.165036 0.938787 0.242184 0.094 Uiso 1 1 calc R U . . .
H19B H 1.039014 0.966722 0.185378 0.094 Uiso 1 1 calc R U . . .
H19C H 1.049816 0.831762 0.164091 0.094 Uiso 1 1 calc R U . . .
C20 C 0.4625(5) 0.6381(3) 0.48490(15) 0.0870(11) Uani 1 1 d . . . . .
H20A H 0.549039 0.604774 0.474437 0.130 Uiso 1 1 calc R U . . .
H20B H 0.365641 0.574332 0.457742 0.130 Uiso 1 1 calc R U . . .
H20C H 0.465754 0.669870 0.545318 0.130 Uiso 1 1 calc R U . . .
C21 C 0.9039(4) 0.5153(3) 0.44002(18) 0.0760(9) Uani 1 1 d . . . . .
H21 H 0.837412 0.525635 0.398284 0.091 Uiso 1 1 calc R U . . .
C22 C 1.0307(4) 0.3906(3) 0.48582(19) 0.0732(8) Uani 1 1 d . . . . .
H22 H 1.051935 0.315432 0.476027 0.088 Uiso 1 1 calc R U . . .
C23 C 0.9342(4) 0.4067(3) 0.42596(16) 0.0738(9) Uani 1 1 d . . . . .
H23 H 0.888245 0.342110 0.374633 0.089 Uiso 1 1 calc R U . . .
C24 C 0.3282(3) 0.7773(3) 0.45462(15) 0.0791(10) Uani 1 1 d . . . . .
H24A H 0.312098 0.798857 0.512541 0.119 Uiso 1 1 calc R U . . .
H24B H 0.240720 0.710188 0.418231 0.119 Uiso 1 1 calc R U . . .
H24C H 0.337334 0.847069 0.436572 0.119 Uiso 1 1 calc R U . . .
C25 C 0.6110(3) 0.8436(3) 0.50367(13) 0.0738(9) Uani 1 1 d . . . . .
H25A H 0.599755 0.864172 0.562381 0.111 Uiso 1 1 calc R U . . .
H25B H 0.616543 0.913909 0.486572 0.111 Uiso 1 1 calc R U . . .
H25C H 0.705311 0.819782 0.497226 0.111 Uiso 1 1 calc R U . . .
C26 C 0.9493(3) 1.0247(2) 0.36862(16) 0.0655(7) Uani 1 1 d . . . . .
H26A H 0.878498 1.010530 0.406228 0.098 Uiso 1 1 calc R U . . .
H26B H 0.929084 1.086223 0.347017 0.098 Uiso 1 1 calc R U . . .
H26C H 1.055497 1.052509 0.399407 0.098 Uiso 1 1 calc R U . . .
C27 C 0.9594(3) 0.7632(3) 0.3200(2) 0.0853(11) Uani 1 1 d . . . . .
H27A H 0.934112 0.685706 0.273904 0.128 Uiso 1 1 calc R U . . .
H27B H 0.896273 0.754897 0.361997 0.128 Uiso 1 1 calc R U . . .
H27C H 1.068388 0.787523 0.345633 0.128 Uiso 1 1 calc R U . . .
H500 H 0.772(3) 0.607(2) 0.0674(14) 0.047(6) Uiso 1 1 d . . . . .
H501 H 0.630(3) 0.397(2) 0.0726(16) 0.059(7) Uiso 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Sn1 C2 2.1504(14) . ?
Sn1 Sn1 2.7674(2) 2_665 ?
Sn1 H500 1.68(2) . ?
Sn1 H501 1.66(3) . ?
Si3 C11 1.868(2) . ?
Si3 C6 1.8677(19) . ?
Si3 C10 1.872(2) . ?
Si3 C5 1.9028(15) . ?
Si4 C17 1.866(2) . ?
Si4 C18 1.865(2) . ?
Si4 C14 1.871(2) . ?
Si4 C5 1.8971(16) . ?
Si1 C15 1.866(2) . ?
Si1 C13 1.868(2) . ?
Si1 C16 1.870(2) . ?
Si1 C12 1.8951(17) . ?
Si2 C27 1.866(3) . ?
Si2 C19 1.873(3) . ?
Si2 C26 1.884(3) . ?
Si2 C12 1.8899(17) . ?
C1 C3 1.398(2) . ?
C1 C2 1.414(2) . ?
C1 C5 1.5212(19) . ?
C2 C8 1.4140(19) . ?
C3 C4 1.395(2) . ?
C3 H3 0.9500 . ?
C4 C9 1.386(2) . ?
C4 C7 1.532(2) . ?
C5 H5 1.0000 . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C7 C24 1.508(3) . ?
C7 C25 1.516(3) . ?
C7 C20 1.531(3) . ?
C8 C9 1.402(2) . ?
C8 C12 1.517(2) . ?
C9 H9 0.9500 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 H12 1.0000 . ?
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 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 C22 1.376(4) 2_766 ?
C21 C23 1.371(5) . ?
C21 H21 0.9500 . ?
C22 C23 1.377(5) . ?
C22 H22 0.9500 . ?
C23 H23 0.9500 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 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
C2 Sn1 Sn1 118.21(4) . 2_665 ?
C2 Sn1 H500 111.5(8) . . ?
Sn1 Sn1 H500 107.4(8) 2_665 . ?
C2 Sn1 H501 109.7(9) . . ?
Sn1 Sn1 H501 106.1(9) 2_665 . ?
H500 Sn1 H501 102.7(12) . . ?
C11 Si3 C6 107.27(10) . . ?
C11 Si3 C10 107.83(11) . . ?
C6 Si3 C10 110.35(10) . . ?
C11 Si3 C5 114.44(8) . . ?
C6 Si3 C5 107.42(7) . . ?
C10 Si3 C5 109.49(9) . . ?
C17 Si4 C18 109.87(12) . . ?
C17 Si4 C14 108.20(11) . . ?
C18 Si4 C14 107.54(11) . . ?
C17 Si4 C5 108.36(9) . . ?
C18 Si4 C5 108.65(8) . . ?
C14 Si4 C5 114.17(8) . . ?
C15 Si1 C13 107.91(11) . . ?
C15 Si1 C16 109.03(10) . . ?
C13 Si1 C16 108.51(11) . . ?
C15 Si1 C12 112.85(9) . . ?
C13 Si1 C12 107.84(8) . . ?
C16 Si1 C12 110.57(10) . . ?
C27 Si2 C19 108.18(15) . . ?
C27 Si2 C26 109.40(16) . . ?
C19 Si2 C26 108.86(12) . . ?
C27 Si2 C12 108.48(11) . . ?
C19 Si2 C12 108.44(11) . . ?
C26 Si2 C12 113.35(10) . . ?
C3 C1 C2 119.30(13) . . ?
C3 C1 C5 118.07(13) . . ?
C2 C1 C5 122.63(12) . . ?
C1 C2 C8 119.12(12) . . ?
C1 C2 Sn1 118.78(10) . . ?
C8 C2 Sn1 121.49(10) . . ?
C4 C3 C1 122.26(14) . . ?
C4 C3 H3 118.9 . . ?
C1 C3 H3 118.9 . . ?
C9 C4 C3 117.24(13) . . ?
C9 C4 C7 121.84(14) . . ?
C3 C4 C7 120.90(14) . . ?
C1 C5 Si4 112.88(10) . . ?
C1 C5 Si3 109.96(10) . . ?
Si4 C5 Si3 119.61(8) . . ?
C1 C5 H5 104.2 . . ?
Si4 C5 H5 104.2 . . ?
Si3 C5 H5 104.2 . . ?
Si3 C6 H6A 109.5 . . ?
Si3 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
Si3 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C24 C7 C25 110.2(2) . . ?
C24 C7 C4 109.00(15) . . ?
C25 C7 C4 112.07(15) . . ?
C24 C7 C20 108.5(2) . . ?
C25 C7 C20 106.6(2) . . ?
C4 C7 C20 110.30(15) . . ?
C9 C8 C2 118.68(13) . . ?
C9 C8 C12 117.86(13) . . ?
C2 C8 C12 123.46(13) . . ?
C4 C9 C8 122.94(14) . . ?
C4 C9 H9 118.5 . . ?
C8 C9 H9 118.5 . . ?
Si3 C10 H10A 109.5 . . ?
Si3 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
Si3 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
Si3 C11 H11A 109.5 . . ?
Si3 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
Si3 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C8 C12 Si2 113.16(11) . . ?
C8 C12 Si1 110.49(11) . . ?
Si2 C12 Si1 118.71(8) . . ?
C8 C12 H12 104.3 . . ?
Si2 C12 H12 104.3 . . ?
Si1 C12 H12 104.3 . . ?
Si1 C13 H13A 109.5 . . ?
Si1 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
Si1 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 . . ?
Si1 C15 H15A 109.5 . . ?
Si1 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
Si1 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
Si1 C16 H16A 109.5 . . ?
Si1 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
Si1 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
Si4 C17 H17A 109.5 . . ?
Si4 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
Si4 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
Si4 C18 H18A 109.5 . . ?
Si4 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
Si4 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
Si2 C19 H19A 109.5 . . ?
Si2 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
Si2 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C7 C20 H20A 109.5 . . ?
C7 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C7 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C22 C21 C23 120.4(3) 2_766 . ?
C22 C21 H21 119.8 2_766 . ?
C23 C21 H21 119.8 . . ?
C21 C22 C23 119.2(3) 2_766 . ?
C21 C22 H22 120.4 2_766 . ?
C23 C22 H22 120.4 . . ?
C21 C23 C22 120.4(3) . . ?
C21 C23 H23 119.8 . . ?
C22 C23 H23 119.8 . . ?
C7 C24 H24A 109.5 . . ?
C7 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C7 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C7 C25 H25A 109.5 . . ?
C7 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
C7 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
Si2 C26 H26A 109.5 . . ?
Si2 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
Si2 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
Si2 C27 H27A 109.5 . . ?
Si2 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
Si2 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?

_refine_diff_density_max         0.717
_refine_diff_density_min         -0.536
_refine_diff_density_rms         0.059



####################################################################### 
# 
# 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_ma46_0m_a
_database_code_depnum_ccdc_archive 'CCDC 2153536'
loop_
_audit_author_name
_audit_author_address
'Hartmut Schubert'
;Universtity of Tuebingen
Germany
;
_audit_update_record             
;
2022-02-21 deposited with the CCDC.	2022-03-22 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/1
_shelx_SHELXL_version_number     2018/1
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C40 H82 Ge K O7 Si4'
_chemical_formula_weight         899.10

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'
Ge Ge 0.1547 1.8001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 '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'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

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

_cell_length_a                   15.8808(5)
_cell_length_b                   14.7774(5)
_cell_length_c                   23.6977(8)
_cell_angle_alpha                90
_cell_angle_beta                 107.598(2)
_cell_angle_gamma                90
_cell_volume                     5301.0(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    117(2)
_cell_measurement_reflns_used    9709
_cell_measurement_theta_min      2.27
_cell_measurement_theta_max      27.39

_exptl_crystal_description       prism
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.127
_exptl_crystal_F_000             1940
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.16
_exptl_absorpt_coefficient_mu    0.785
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6921
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_process_details   'SADABS V2012/1 (Bruker AXS Inc.)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      117(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            131244
_diffrn_reflns_av_unetI/netI     0.0180
_diffrn_reflns_av_R_equivalents  0.0234
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_theta_min         1.803
_diffrn_reflns_theta_max         27.490
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.970
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.970
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.970
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             11810
_reflns_number_gt                9870
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_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       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXT 2014/4 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2018/1 (Sheldrick, 2018)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_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)+(0.0408P)²+2.3135P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         11810
_refine_ls_number_parameters     549
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0420
_refine_ls_R_factor_gt           0.0300
_refine_ls_wR_factor_ref         0.0816
_refine_ls_wR_factor_gt          0.0747
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_restrained_S_all      1.055
_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
Ge1 Ge 0.30060(2) 0.35416(2) 0.40718(2) 0.02266(5) Uani 1 1 d . . . . .
K1 K 0.26347(2) 0.55270(2) 0.33416(2) 0.02424(8) Uani 1 1 d . . . . .
Si2 Si 0.02964(3) 0.29397(3) 0.41327(2) 0.02422(10) Uani 1 1 d . . . . .
Si4 Si 0.31076(3) 0.14477(3) 0.27131(2) 0.02440(10) Uani 1 1 d . . . . .
Si1 Si 0.17550(3) 0.27341(3) 0.54412(2) 0.02487(10) Uani 1 1 d . . . . .
Si3 Si 0.47131(3) 0.11864(3) 0.39530(2) 0.02343(9) Uani 1 1 d . . . . .
C00D C 0.25887(9) 0.22497(9) 0.41051(6) 0.0179(3) Uani 1 1 d . . . . .
C1 C 0.48273(12) 0.12455(12) 0.47592(7) 0.0320(4) Uani 1 1 d . . . . .
H1A H 0.543714 0.110279 0.498924 0.048 Uiso 1 1 calc R U . . .
H1B H 0.442562 0.080791 0.485311 0.048 Uiso 1 1 calc R U . . .
H1C H 0.467907 0.185672 0.485864 0.048 Uiso 1 1 calc R U . . .
C2 C 0.36029(9) 0.16620(10) 0.35270(6) 0.0199(3) Uani 1 1 d . . . . .
H2 H 0.370173 0.233110 0.355023 0.024 Uiso 1 1 calc R U . . .
C800 C 0.19260(9) 0.20434(10) 0.43687(6) 0.0192(3) Uani 1 1 d . . . . .
C4 C 0.48844(12) -0.00150(12) 0.37508(8) 0.0330(4) Uani 1 1 d . . . . .
H4A H 0.480371 -0.005344 0.332486 0.049 Uiso 1 1 calc R U . . .
H4B H 0.445457 -0.040872 0.385180 0.049 Uiso 1 1 calc R U . . .
H4C H 0.548406 -0.020914 0.397040 0.049 Uiso 1 1 calc R U . . .
C5 C 0.29290(9) 0.15175(10) 0.38578(6) 0.0189(3) Uani 1 1 d . . . . .
C6 C 0.16854(10) 0.11450(10) 0.44307(7) 0.0231(3) Uani 1 1 d . . . . .
H6 H 0.124108 0.102711 0.461409 0.028 Uiso 1 1 calc R U . . .
C7 C 0.14686(10) 0.27869(10) 0.46118(6) 0.0203(3) Uani 1 1 d . . . . .
H7 H 0.176825 0.335183 0.454098 0.024 Uiso 1 1 calc R U . . .
C8 C 0.20785(10) 0.04205(10) 0.42315(7) 0.0245(3) Uani 1 1 d . . . . .
C9 C 0.09196(13) 0.20884(13) 0.56956(8) 0.0365(4) Uani 1 1 d . . . . .
H9A H 0.110167 0.207624 0.612924 0.055 Uiso 1 1 calc R U . . .
H9B H 0.087860 0.146775 0.554389 0.055 Uiso 1 1 calc R U . . .
H9C H 0.034217 0.238371 0.554651 0.055 Uiso 1 1 calc R U . . .
C10 C 0.26796(10) 0.06273(10) 0.39297(7) 0.0231(3) Uani 1 1 d . . . . .
H10 H 0.292989 0.014783 0.376651 0.028 Uiso 1 1 calc R U . . .
C12 C 0.12538(13) 0.48543(12) 0.18889(8) 0.0393(4) Uani 1 1 d . . . . .
H12A H 0.077181 0.491920 0.151185 0.047 Uiso 1 1 calc R U . . .
H12B H 0.121719 0.424077 0.204762 0.047 Uiso 1 1 calc R U . . .
C13 C 0.21899(11) 0.22780(12) 0.24262(8) 0.0336(4) Uani 1 1 d . . . . .
H13A H 0.187827 0.214303 0.201045 0.050 Uiso 1 1 calc R U . . .
H13B H 0.243357 0.289180 0.245794 0.050 Uiso 1 1 calc R U . . .
H13C H 0.177668 0.223469 0.265962 0.050 Uiso 1 1 calc R U . . .
C14 C 0.55923(11) 0.19074(14) 0.37982(9) 0.0383(4) Uani 1 1 d . . . . .
H14A H 0.554696 0.186626 0.337731 0.057 Uiso 1 1 calc R U . . .
H14B H 0.617553 0.169398 0.403692 0.057 Uiso 1 1 calc R U . . .
H14C H 0.551317 0.253803 0.389972 0.057 Uiso 1 1 calc R U . . .
C15 C 0.18099(14) 0.39196(12) 0.57353(8) 0.0378(4) Uani 1 1 d . . . . .
H15A H 0.193051 0.390138 0.616592 0.057 Uiso 1 1 calc R U . . .
H15B H 0.124467 0.422490 0.555430 0.057 Uiso 1 1 calc R U . . .
H15C H 0.228316 0.425140 0.563933 0.057 Uiso 1 1 calc R U . . .
C16 C 0.21262(13) 0.49761(13) 0.17820(8) 0.0387(4) Uani 1 1 d . . . . .
H16A H 0.217241 0.456106 0.146471 0.046 Uiso 1 1 calc R U . . .
H16B H 0.218258 0.560483 0.165372 0.046 Uiso 1 1 calc R U . . .
C17 C 0.28544(12) 0.21829(13) 0.57575(8) 0.0389(4) Uani 1 1 d . . . . .
H17A H 0.301930 0.219616 0.619077 0.058 Uiso 1 1 calc R U . . .
H17B H 0.329857 0.250932 0.562599 0.058 Uiso 1 1 calc R U . . .
H17C H 0.282269 0.155370 0.562199 0.058 Uiso 1 1 calc R U . . .
C18 C -0.04462(11) 0.19533(13) 0.41306(8) 0.0355(4) Uani 1 1 d . . . . .
H18A H -0.105428 0.210955 0.390407 0.053 Uiso 1 1 calc R U . . .
H18B H -0.042060 0.180458 0.453846 0.053 Uiso 1 1 calc R U . . .
H18C H -0.025223 0.143007 0.394812 0.053 Uiso 1 1 calc R U . . .
C19 C 0.18851(12) -0.05646(11) 0.43631(10) 0.0388(4) Uani 1 1 d . . . . .
C20 C 0.03088(12) 0.60901(14) 0.28950(9) 0.0422(5) Uani 1 1 d . . . . .
H20A H 0.045653 0.671082 0.279933 0.051 Uiso 1 1 calc R U . . .
H20B H -0.028861 0.610057 0.294390 0.051 Uiso 1 1 calc R U . . .
C21 C 0.39546(13) 0.16289(14) 0.23183(8) 0.0406(5) Uani 1 1 d . . . . .
H21A H 0.367999 0.154395 0.189194 0.061 Uiso 1 1 calc R U . . .
H21B H 0.443632 0.119231 0.246297 0.061 Uiso 1 1 calc R U . . .
H21C H 0.419006 0.224503 0.239373 0.061 Uiso 1 1 calc R U . . .
C22 C 0.03229(12) 0.54595(13) 0.24062(9) 0.0409(4) Uani 1 1 d . . . . .
H22A H 0.022011 0.483184 0.251577 0.049 Uiso 1 1 calc R U . . .
H22B H -0.015290 0.562214 0.204173 0.049 Uiso 1 1 calc R U . . .
C23 C 0.50200(12) 0.51673(14) 0.37743(9) 0.0416(5) Uani 1 1 d . . . . .
H23A H 0.561782 0.516279 0.372596 0.050 Uiso 1 1 calc R U . . .
H23B H 0.491720 0.457299 0.393468 0.050 Uiso 1 1 calc R U . . .
C24 C 0.08951(14) 0.62956(14) 0.39294(10) 0.0461(5) Uani 1 1 d . . . . .
H24A H 0.032544 0.618016 0.400606 0.055 Uiso 1 1 calc R U . . .
H24B H 0.093441 0.695050 0.385283 0.055 Uiso 1 1 calc R U . . .
C25 C 0.31914(14) 0.61427(14) 0.48803(8) 0.0435(5) Uani 1 1 d . . . . .
H25A H 0.321512 0.549030 0.497895 0.052 Uiso 1 1 calc R U . . .
H25B H 0.313947 0.648899 0.522583 0.052 Uiso 1 1 calc R U . . .
C26 C -0.01974(13) 0.39609(14) 0.43777(10) 0.0480(5) Uani 1 1 d . . . . .
H26A H -0.079364 0.406155 0.410850 0.072 Uiso 1 1 calc R U . . .
H26B H 0.017081 0.449115 0.437273 0.072 Uiso 1 1 calc R U . . .
H26C H -0.022800 0.386447 0.478023 0.072 Uiso 1 1 calc R U . . .
C27 C 0.26392(17) 0.02838(13) 0.25287(9) 0.0519(6) Uani 1 1 d . . . . .
H27A H 0.244203 0.020361 0.209804 0.078 Uiso 1 1 calc R U . . .
H27B H 0.213626 0.020495 0.268253 0.078 Uiso 1 1 calc R U . . .
H27C H 0.309408 -0.016640 0.270903 0.078 Uiso 1 1 calc R U . . .
C28 C 0.36636(13) 0.47949(14) 0.22369(9) 0.0411(4) Uani 1 1 d . . . . .
H28A H 0.378465 0.539664 0.209488 0.049 Uiso 1 1 calc R U . . .
H28B H 0.369383 0.433742 0.193845 0.049 Uiso 1 1 calc R U . . .
C29 C 0.49576(12) 0.59036(14) 0.41923(9) 0.0435(5) Uani 1 1 d . . . . .
H29A H 0.543820 0.584148 0.457033 0.052 Uiso 1 1 calc R U . . .
H29B H 0.501280 0.650248 0.401951 0.052 Uiso 1 1 calc R U . . .
C30 C 0.03221(13) 0.31302(15) 0.33588(8) 0.0432(5) Uani 1 1 d . . . . .
H30A H -0.026908 0.329974 0.310769 0.065 Uiso 1 1 calc R U . . .
H30B H 0.050958 0.257328 0.320685 0.065 Uiso 1 1 calc R U . . .
H30C H 0.073923 0.361755 0.335577 0.065 Uiso 1 1 calc R U . . .
C31 C 0.40131(14) 0.64154(13) 0.47395(9) 0.0430(5) Uani 1 1 d . . . . .
H31A H 0.396233 0.704943 0.459816 0.052 Uiso 1 1 calc R U . . .
H31B H 0.453019 0.637057 0.509852 0.052 Uiso 1 1 calc R U . . .
C32 C 0.16451(14) 0.60204(15) 0.44570(9) 0.0457(5) Uani 1 1 d . . . . .
H32A H 0.156920 0.629195 0.482041 0.055 Uiso 1 1 calc R U . . .
H32B H 0.165487 0.535390 0.450073 0.055 Uiso 1 1 calc R U . . .
C33 C 0.43343(13) 0.45860(13) 0.28161(9) 0.0415(4) Uani 1 1 d . . . . .
H33A H 0.417034 0.402192 0.298249 0.050 Uiso 1 1 calc R U . . .
H33B H 0.492047 0.449625 0.275833 0.050 Uiso 1 1 calc R U . . .
O7 O 0.25886(19) 0.72960(16) 0.29917(11) 0.0394(6) Uani 0.729(5) 1 d . . P A 1
C301 C 0.3754(2) 0.7733(3) 0.2647(2) 0.0579(13) Uani 0.729(5) 1 d . . P A 1
H30D H 0.411106 0.827954 0.263863 0.069 Uiso 0.729(5) 1 calc R U P A 1
H30E H 0.411717 0.718886 0.264631 0.069 Uiso 0.729(5) 1 calc R U P A 1
C300 C 0.3421(2) 0.77405(19) 0.31843(15) 0.0452(9) Uani 0.729(5) 1 d . . P A 1
H30F H 0.383285 0.741174 0.351936 0.054 Uiso 0.729(5) 1 calc R U P A 1
H30G H 0.335393 0.836830 0.331015 0.054 Uiso 0.729(5) 1 calc R U P A 1
C302 C 0.2917(3) 0.7723(3) 0.21275(17) 0.0491(9) Uani 0.729(5) 1 d . . P A 1
H30H H 0.285342 0.829130 0.189706 0.059 Uiso 0.729(5) 1 calc R U P A 1
H30I H 0.291471 0.720492 0.186207 0.059 Uiso 0.729(5) 1 calc R U P A 1
O100 O 0.2913(5) 0.7141(5) 0.2835(4) 0.0466(18) Uani 0.271(5) 1 d . . P A 2
C400 C 0.3725(7) 0.7636(6) 0.2918(5) 0.0368(4) Uani 0.271(5) 1 d . . P A 2
H40A H 0.423290 0.721383 0.301368 0.044 Uiso 0.271(5) 1 calc R U P A 2
H40B H 0.381384 0.807025 0.324894 0.044 Uiso 0.271(5) 1 calc R U P A 2
C401 C 0.3662(5) 0.8132(5) 0.2355(4) 0.0368(4) Uani 0.271(5) 1 d . . P A 2
H40C H 0.410183 0.790073 0.217120 0.044 Uiso 0.271(5) 1 calc R U P A 2
H40D H 0.375797 0.878877 0.242923 0.044 Uiso 0.271(5) 1 calc R U P A 2
C402 C 0.2716(7) 0.7943(8) 0.1958(5) 0.0452(9) Uani 0.271(5) 1 d . . P A 2
H40E H 0.271099 0.745768 0.166892 0.054 Uiso 0.271(5) 1 calc R U P A 2
H40F H 0.244661 0.849468 0.174063 0.054 Uiso 0.271(5) 1 calc R U P A 2
C303 C 0.22019(12) 0.76328(12) 0.24092(8) 0.0368(4) Uani 1 1 d . . . . .
H30J H 0.192350 0.822833 0.242333 0.044 Uiso 1 1 calc R U . A 1
H30K H 0.174220 0.721018 0.217883 0.044 Uiso 1 1 calc R U . A 1
C200 C 0.0961(2) -0.0773(2) 0.4218(2) 0.0359(9) Uani 0.541(4) 1 d . . P B 2
H20C H 0.073796 -0.131546 0.401128 0.043 Uiso 0.541(4) 1 calc R U P B 2
H20D H 0.057338 -0.036942 0.432872 0.043 Uiso 0.541(4) 1 calc R U P B 2
C202 C 0.2426(2) -0.1260(2) 0.4163(2) 0.0359(9) Uani 0.541(4) 1 d . . P B 2
H20E H 0.235367 -0.185116 0.432954 0.054 Uiso 0.541(4) 1 calc R U P B 2
H20F H 0.305031 -0.108487 0.429838 0.054 Uiso 0.541(4) 1 calc R U P B 2
H20G H 0.222632 -0.129651 0.372945 0.054 Uiso 0.541(4) 1 calc R U P B 2
C201 C 0.2281(3) -0.0659(2) 0.51144(15) 0.0429(10) Uani 0.541(4) 1 d . . P B 2
H20H H 0.216390 -0.126956 0.523334 0.064 Uiso 0.541(4) 1 calc R U P B 2
H20I H 0.198803 -0.021380 0.529772 0.064 Uiso 0.541(4) 1 calc R U P B 2
H20J H 0.291940 -0.054733 0.524387 0.064 Uiso 0.541(4) 1 calc R U P B 2
C101 C 0.2663(3) -0.1055(3) 0.4607(2) 0.0409(12) Uani 0.459(4) 1 d . . P B 1
H10A H 0.271571 -0.144277 0.493550 0.049 Uiso 0.459(4) 1 calc R U P B 1
H10B H 0.313883 -0.099938 0.444449 0.049 Uiso 0.459(4) 1 calc R U P B 1
C102 C 0.1414(3) -0.1031(2) 0.36700(19) 0.0388(11) Uani 0.459(4) 1 d . . P B 1
H10C H 0.136979 -0.168860 0.370650 0.058 Uiso 0.459(4) 1 calc R U P B 1
H10D H 0.178278 -0.089265 0.341587 0.058 Uiso 0.459(4) 1 calc R U P B 1
H10E H 0.082277 -0.077613 0.349470 0.058 Uiso 0.459(4) 1 calc R U P B 1
C100 C 0.1152(3) -0.0660(3) 0.4623(3) 0.0402(11) Uani 0.459(4) 1 d . . P B 1
H10F H 0.095427 -0.129141 0.459091 0.060 Uiso 0.459(4) 1 calc R U P B 1
H10G H 0.066025 -0.026988 0.440885 0.060 Uiso 0.459(4) 1 calc R U P B 1
H10H H 0.135631 -0.048239 0.504058 0.060 Uiso 0.459(4) 1 calc R U P B 1
O4 O 0.28095(8) 0.47882(8) 0.23132(5) 0.0327(3) Uani 1 1 d . . . . .
O3 O 0.11584(8) 0.55184(8) 0.23017(5) 0.0320(3) Uani 1 1 d . . . . .
O1 O 0.24488(9) 0.63221(8) 0.43766(5) 0.0358(3) Uani 1 1 d . . . . .
O5 O 0.43723(8) 0.53191(8) 0.32142(6) 0.0343(3) Uani 1 1 d . . . . .
O2 O 0.09383(8) 0.57899(8) 0.34292(5) 0.0341(3) Uani 1 1 d . . . . .
O6 O 0.41225(8) 0.58264(9) 0.42924(5) 0.0373(3) Uani 1 1 d . . . . .
H20 H 0.3092(14) 0.3782(15) 0.4718(9) 0.053(6) Uiso 1 1 d . . . . .
H8 H 0.3944(15) 0.3337(15) 0.4191(10) 0.055(6) Uiso 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ge1 C00D 2.0301(14) . ?
Ge1 K1 3.3666(4) . ?
Ge1 H20 1.54(2) . ?
Ge1 H8 1.46(2) . ?
K1 O7 2.737(2) . ?
K1 O4 2.7600(12) . ?
K1 O6 2.7633(12) . ?
K1 O100 2.765(6) . ?
K1 O2 2.7910(12) . ?
K1 O1 2.8146(13) . ?
K1 O3 2.8417(12) . ?
K1 O5 2.8816(12) . ?
K1 C32 3.535(2) . ?
Si2 C30 1.8682(19) . ?
Si2 C26 1.8721(19) . ?
Si2 C18 1.8740(18) . ?
Si2 C7 1.8781(15) . ?
Si4 C13 1.8688(17) . ?
Si4 C27 1.872(2) . ?
Si4 C21 1.8754(19) . ?
Si4 C2 1.8766(15) . ?
Si1 C17 1.8661(19) . ?
Si1 C9 1.8755(18) . ?
Si1 C15 1.8778(18) . ?
Si1 C7 1.8802(15) . ?
Si3 C1 1.8657(17) . ?
Si3 C14 1.8785(17) . ?
Si3 C4 1.8800(18) . ?
Si3 C2 1.8830(15) . ?
C00D C800 1.410(2) . ?
C00D C5 1.413(2) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C2 C5 1.5209(19) . ?
C2 H2 1.0000 . ?
C800 C6 1.401(2) . ?
C800 C7 1.523(2) . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C5 C10 1.399(2) . ?
C6 C8 1.392(2) . ?
C6 H6 0.9500 . ?
C7 H7 1.0000 . ?
C8 C10 1.389(2) . ?
C8 C19 1.539(2) . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 H10 0.9500 . ?
C12 O3 1.426(2) . ?
C12 C16 1.493(3) . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
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 O4 1.419(2) . ?
C16 H16A 0.9900 . ?
C16 H16B 0.9900 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 C101 1.397(4) . ?
C19 C200 1.435(4) . ?
C19 C100 1.479(4) . ?
C19 C202 1.505(4) . ?
C19 C201 1.705(4) . ?
C19 C102 1.729(4) . ?
C20 O2 1.426(2) . ?
C20 C22 1.492(3) . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 O3 1.424(2) . ?
C22 H22A 0.9900 . ?
C22 H22B 0.9900 . ?
C23 O5 1.430(2) . ?
C23 C29 1.495(3) . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C24 O2 1.420(2) . ?
C24 C32 1.499(3) . ?
C24 H24A 0.9900 . ?
C24 H24B 0.9900 . ?
C25 O1 1.426(2) . ?
C25 C31 1.497(3) . ?
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?
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 O4 1.421(2) . ?
C28 C33 1.493(3) . ?
C28 H28A 0.9900 . ?
C28 H28B 0.9900 . ?
C29 O6 1.421(2) . ?
C29 H29A 0.9900 . ?
C29 H29B 0.9900 . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
C31 O6 1.422(2) . ?
C31 H31A 0.9900 . ?
C31 H31B 0.9900 . ?
C32 O1 1.418(2) . ?
C32 H32A 0.9900 . ?
C32 H32B 0.9900 . ?
C33 O5 1.426(2) . ?
C33 H33A 0.9900 . ?
C33 H33B 0.9900 . ?
O7 C303 1.420(3) . ?
O7 C300 1.422(4) . ?
C301 C302 1.515(5) . ?
C301 C300 1.519(5) . ?
C301 H30D 0.9900 . ?
C301 H30E 0.9900 . ?
C300 H30F 0.9900 . ?
C300 H30G 0.9900 . ?
C302 C303 1.488(4) . ?
C302 H30H 0.9900 . ?
C302 H30I 0.9900 . ?
O100 C400 1.444(12) . ?
O100 C303 1.461(7) . ?
C400 C401 1.498(11) . ?
C400 H40A 0.9900 . ?
C400 H40B 0.9900 . ?
C401 C402 1.538(13) . ?
C401 H40C 0.9900 . ?
C401 H40D 0.9900 . ?
C402 C303 1.596(13) . ?
C402 H40E 0.9900 . ?
C402 H40F 0.9900 . ?
C303 H30J 0.9900 . ?
C303 H30K 0.9900 . ?
C200 H20C 0.9500 . ?
C200 H20D 0.9500 . ?
C202 H20E 0.9800 . ?
C202 H20F 0.9800 . ?
C202 H20G 0.9800 . ?
C201 H20H 0.9800 . ?
C201 H20I 0.9800 . ?
C201 H20J 0.9800 . ?
C101 H10A 0.9500 . ?
C101 H10B 0.9500 . ?
C102 H10C 0.9800 . ?
C102 H10D 0.9800 . ?
C102 H10E 0.9800 . ?
C100 H10F 0.9800 . ?
C100 H10G 0.9800 . ?
C100 H10H 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
C00D Ge1 K1 146.20(4) . . ?
C00D Ge1 H20 96.3(8) . . ?
K1 Ge1 H20 105.0(8) . . ?
C00D Ge1 H8 97.1(9) . . ?
K1 Ge1 H8 106.8(9) . . ?
H20 Ge1 H8 94.4(12) . . ?
O7 K1 O4 96.37(7) . . ?
O7 K1 O6 91.83(6) . . ?
O4 K1 O6 119.59(4) . . ?
O4 K1 O100 83.4(2) . . ?
O6 K1 O100 90.36(15) . . ?
O7 K1 O2 87.23(7) . . ?
O4 K1 O2 118.54(4) . . ?
O6 K1 O2 121.57(4) . . ?
O100 K1 O2 101.37(17) . . ?
O7 K1 O1 82.24(6) . . ?
O4 K1 O1 178.60(4) . . ?
O6 K1 O1 60.77(4) . . ?
O100 K1 O1 95.2(2) . . ?
O2 K1 O1 61.26(4) . . ?
O7 K1 O3 78.59(6) . . ?
O4 K1 O3 60.62(4) . . ?
O6 K1 O3 170.28(4) . . ?
O100 K1 O3 79.97(15) . . ?
O2 K1 O3 60.22(4) . . ?
O1 K1 O3 118.76(4) . . ?
O7 K1 O5 90.51(7) . . ?
O4 K1 O5 60.67(4) . . ?
O6 K1 O5 59.51(4) . . ?
O100 K1 O5 76.26(17) . . ?
O2 K1 O5 177.51(4) . . ?
O1 K1 O5 119.46(4) . . ?
O3 K1 O5 118.28(4) . . ?
O7 K1 Ge1 166.57(5) . . ?
O4 K1 Ge1 93.46(3) . . ?
O6 K1 Ge1 75.33(3) . . ?
O100 K1 Ge1 161.56(15) . . ?
O2 K1 Ge1 96.09(3) . . ?
O1 K1 Ge1 87.94(3) . . ?
O3 K1 Ge1 114.34(3) . . ?
O5 K1 Ge1 86.36(3) . . ?
O7 K1 C32 93.00(8) . . ?
O4 K1 C32 158.10(4) . . ?
O6 K1 C32 79.70(5) . . ?
O100 K1 C32 108.2(2) . . ?
O2 K1 C32 42.14(4) . . ?
O1 K1 C32 22.32(4) . . ?
O3 K1 C32 102.27(4) . . ?
O5 K1 C32 139.15(4) . . ?
Ge1 K1 C32 81.01(4) . . ?
C30 Si2 C26 108.57(11) . . ?
C30 Si2 C18 108.37(9) . . ?
C26 Si2 C18 107.79(9) . . ?
C30 Si2 C7 107.44(8) . . ?
C26 Si2 C7 109.94(8) . . ?
C18 Si2 C7 114.59(8) . . ?
C13 Si4 C27 107.89(10) . . ?
C13 Si4 C21 108.83(8) . . ?
C27 Si4 C21 108.00(11) . . ?
C13 Si4 C2 107.55(7) . . ?
C27 Si4 C2 114.10(8) . . ?
C21 Si4 C2 110.34(8) . . ?
C17 Si1 C9 108.40(9) . . ?
C17 Si1 C15 108.98(9) . . ?
C9 Si1 C15 108.26(9) . . ?
C17 Si1 C7 109.83(8) . . ?
C9 Si1 C7 112.71(7) . . ?
C15 Si1 C7 108.59(7) . . ?
C1 Si3 C14 109.00(8) . . ?
C1 Si3 C4 109.17(8) . . ?
C14 Si3 C4 108.21(9) . . ?
C1 Si3 C2 108.48(7) . . ?
C14 Si3 C2 108.32(8) . . ?
C4 Si3 C2 113.57(7) . . ?
C800 C00D C5 116.63(13) . . ?
C800 C00D Ge1 121.12(10) . . ?
C5 C00D Ge1 122.24(10) . . ?
Si3 C1 H1A 109.5 . . ?
Si3 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
Si3 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
C5 C2 Si4 111.38(10) . . ?
C5 C2 Si3 111.22(10) . . ?
Si4 C2 Si3 121.45(8) . . ?
C5 C2 H2 103.5 . . ?
Si4 C2 H2 103.5 . . ?
Si3 C2 H2 103.5 . . ?
C6 C800 C00D 121.00(13) . . ?
C6 C800 C7 117.86(13) . . ?
C00D C800 C7 121.11(13) . . ?
Si3 C4 H4A 109.5 . . ?
Si3 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
Si3 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
C10 C5 C00D 120.76(13) . . ?
C10 C5 C2 117.65(13) . . ?
C00D C5 C2 121.55(13) . . ?
C8 C6 C800 121.92(14) . . ?
C8 C6 H6 119.0 . . ?
C800 C6 H6 119.0 . . ?
C800 C7 Si2 110.91(10) . . ?
C800 C7 Si1 111.92(10) . . ?
Si2 C7 Si1 121.28(8) . . ?
C800 C7 H7 103.5 . . ?
Si2 C7 H7 103.5 . . ?
Si1 C7 H7 103.5 . . ?
C10 C8 C6 117.00(14) . . ?
C10 C8 C19 121.51(14) . . ?
C6 C8 C19 121.43(14) . . ?
Si1 C9 H9A 109.5 . . ?
Si1 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
Si1 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C8 C10 C5 122.24(14) . . ?
C8 C10 H10 118.9 . . ?
C5 C10 H10 118.9 . . ?
O3 C12 C16 109.28(14) . . ?
O3 C12 H12A 109.8 . . ?
C16 C12 H12A 109.8 . . ?
O3 C12 H12B 109.8 . . ?
C16 C12 H12B 109.8 . . ?
H12A C12 H12B 108.3 . . ?
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 . . ?
Si3 C14 H14A 109.5 . . ?
Si3 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
Si3 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
Si1 C15 H15A 109.5 . . ?
Si1 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
Si1 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
O4 C16 C12 109.02(15) . . ?
O4 C16 H16A 109.9 . . ?
C12 C16 H16A 109.9 . . ?
O4 C16 H16B 109.9 . . ?
C12 C16 H16B 109.9 . . ?
H16A C16 H16B 108.3 . . ?
Si1 C17 H17A 109.5 . . ?
Si1 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
Si1 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
Si2 C18 H18A 109.5 . . ?
Si2 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
Si2 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C101 C19 C100 119.1(3) . . ?
C200 C19 C202 114.7(3) . . ?
C101 C19 C8 111.6(2) . . ?
C200 C19 C8 114.00(19) . . ?
C100 C19 C8 113.9(2) . . ?
C202 C19 C8 114.45(18) . . ?
C200 C19 C201 105.1(3) . . ?
C202 C19 C201 102.0(2) . . ?
C8 C19 C201 104.81(17) . . ?
C101 C19 C102 105.1(3) . . ?
C100 C19 C102 100.9(3) . . ?
C8 C19 C102 103.89(18) . . ?
O2 C20 C22 108.89(15) . . ?
O2 C20 H20A 109.9 . . ?
C22 C20 H20A 109.9 . . ?
O2 C20 H20B 109.9 . . ?
C22 C20 H20B 109.9 . . ?
H20A C20 H20B 108.3 . . ?
Si4 C21 H21A 109.5 . . ?
Si4 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
Si4 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
O3 C22 C20 109.29(15) . . ?
O3 C22 H22A 109.8 . . ?
C20 C22 H22A 109.8 . . ?
O3 C22 H22B 109.8 . . ?
C20 C22 H22B 109.8 . . ?
H22A C22 H22B 108.3 . . ?
O5 C23 C29 109.13(15) . . ?
O5 C23 H23A 109.9 . . ?
C29 C23 H23A 109.9 . . ?
O5 C23 H23B 109.9 . . ?
C29 C23 H23B 109.9 . . ?
H23A C23 H23B 108.3 . . ?
O2 C24 C32 109.06(16) . . ?
O2 C24 H24A 109.9 . . ?
C32 C24 H24A 109.9 . . ?
O2 C24 H24B 109.9 . . ?
C32 C24 H24B 109.9 . . ?
H24A C24 H24B 108.3 . . ?
O1 C25 C31 108.63(16) . . ?
O1 C25 H25A 110.0 . . ?
C31 C25 H25A 110.0 . . ?
O1 C25 H25B 110.0 . . ?
C31 C25 H25B 110.0 . . ?
H25A C25 H25B 108.3 . . ?
Si2 C26 H26A 109.5 . . ?
Si2 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
Si2 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
Si4 C27 H27A 109.5 . . ?
Si4 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
Si4 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
O4 C28 C33 108.94(15) . . ?
O4 C28 H28A 109.9 . . ?
C33 C28 H28A 109.9 . . ?
O4 C28 H28B 109.9 . . ?
C33 C28 H28B 109.9 . . ?
H28A C28 H28B 108.3 . . ?
O6 C29 C23 107.73(15) . . ?
O6 C29 H29A 110.2 . . ?
C23 C29 H29A 110.2 . . ?
O6 C29 H29B 110.2 . . ?
C23 C29 H29B 110.2 . . ?
H29A C29 H29B 108.5 . . ?
Si2 C30 H30A 109.5 . . ?
Si2 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
Si2 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
O6 C31 C25 108.20(15) . . ?
O6 C31 H31A 110.1 . . ?
C25 C31 H31A 110.1 . . ?
O6 C31 H31B 110.1 . . ?
C25 C31 H31B 110.1 . . ?
H31A C31 H31B 108.4 . . ?
O1 C32 C24 108.85(17) . . ?
O1 C32 K1 48.92(8) . . ?
C24 C32 K1 81.55(11) . . ?
O1 C32 H32A 109.9 . . ?
C24 C32 H32A 109.9 . . ?
K1 C32 H32A 158.8 . . ?
O1 C32 H32B 109.9 . . ?
C24 C32 H32B 109.9 . . ?
K1 C32 H32B 82.9 . . ?
H32A C32 H32B 108.3 . . ?
O5 C33 C28 109.08(15) . . ?
O5 C33 H33A 109.9 . . ?
C28 C33 H33A 109.9 . . ?
O5 C33 H33B 109.9 . . ?
C28 C33 H33B 109.9 . . ?
H33A C33 H33B 108.3 . . ?
C303 O7 C300 103.7(2) . . ?
C303 O7 K1 126.38(15) . . ?
C300 O7 K1 114.01(18) . . ?
C302 C301 C300 103.8(3) . . ?
C302 C301 H30D 111.0 . . ?
C300 C301 H30D 111.0 . . ?
C302 C301 H30E 111.0 . . ?
C300 C301 H30E 111.0 . . ?
H30D C301 H30E 109.0 . . ?
O7 C300 C301 104.7(2) . . ?
O7 C300 H30F 110.8 . . ?
C301 C300 H30F 110.8 . . ?
O7 C300 H30G 110.8 . . ?
C301 C300 H30G 110.8 . . ?
H30F C300 H30G 108.9 . . ?
C303 C302 C301 103.7(3) . . ?
C303 C302 H30H 111.0 . . ?
C301 C302 H30H 111.0 . . ?
C303 C302 H30I 111.0 . . ?
C301 C302 H30I 111.0 . . ?
H30H C302 H30I 109.0 . . ?
C400 O100 C303 108.3(5) . . ?
C400 O100 K1 129.2(5) . . ?
C303 O100 K1 122.5(4) . . ?
O100 C400 C401 108.1(7) . . ?
O100 C400 H40A 110.1 . . ?
C401 C400 H40A 110.1 . . ?
O100 C400 H40B 110.1 . . ?
C401 C400 H40B 110.1 . . ?
H40A C400 H40B 108.4 . . ?
C400 C401 C402 104.3(7) . . ?
C400 C401 H40C 110.9 . . ?
C402 C401 H40C 110.9 . . ?
C400 C401 H40D 110.9 . . ?
C402 C401 H40D 110.9 . . ?
H40C C401 H40D 108.9 . . ?
C401 C402 C303 104.2(7) . . ?
C401 C402 H40E 110.9 . . ?
C303 C402 H40E 110.9 . . ?
C401 C402 H40F 110.9 . . ?
C303 C402 H40F 110.9 . . ?
H40E C402 H40F 108.9 . . ?
O7 C303 C302 107.6(2) . . ?
O100 C303 C402 99.2(5) . . ?
O7 C303 H30J 110.2 . . ?
C302 C303 H30J 110.2 . . ?
O7 C303 H30K 110.2 . . ?
C302 C303 H30K 110.2 . . ?
H30J C303 H30K 108.5 . . ?
C19 C200 H20C 120.0 . . ?
C19 C200 H20D 120.0 . . ?
H20C C200 H20D 120.0 . . ?
C19 C202 H20E 109.5 . . ?
C19 C202 H20F 109.5 . . ?
H20E C202 H20F 109.5 . . ?
C19 C202 H20G 109.5 . . ?
H20E C202 H20G 109.5 . . ?
H20F C202 H20G 109.5 . . ?
C19 C201 H20H 109.5 . . ?
C19 C201 H20I 109.5 . . ?
H20H C201 H20I 109.5 . . ?
C19 C201 H20J 109.5 . . ?
H20H C201 H20J 109.5 . . ?
H20I C201 H20J 109.5 . . ?
C19 C101 H10A 120.0 . . ?
C19 C101 H10B 120.0 . . ?
H10A C101 H10B 120.0 . . ?
C19 C102 H10C 109.5 . . ?
C19 C102 H10D 109.5 . . ?
H10C C102 H10D 109.5 . . ?
C19 C102 H10E 109.5 . . ?
H10C C102 H10E 109.5 . . ?
H10D C102 H10E 109.5 . . ?
C19 C100 H10F 109.5 . . ?
C19 C100 H10G 109.5 . . ?
H10F C100 H10G 109.5 . . ?
C19 C100 H10H 109.5 . . ?
H10F C100 H10H 109.5 . . ?
H10G C100 H10H 109.5 . . ?
C16 O4 C28 112.90(14) . . ?
C16 O4 K1 116.86(10) . . ?
C28 O4 K1 117.65(10) . . ?
C22 O3 C12 112.04(13) . . ?
C22 O3 K1 114.67(10) . . ?
C12 O3 K1 111.53(10) . . ?
C32 O1 C25 112.29(15) . . ?
C32 O1 K1 108.76(10) . . ?
C25 O1 K1 111.94(11) . . ?
C33 O5 C23 111.70(14) . . ?
C33 O5 K1 107.46(10) . . ?
C23 O5 K1 111.25(10) . . ?
C24 O2 C20 112.29(14) . . ?
C24 O2 K1 115.25(11) . . ?
C20 O2 K1 114.25(10) . . ?
C29 O6 C31 113.94(14) . . ?
C29 O6 K1 119.21(11) . . ?
C31 O6 K1 116.02(11) . . ?

_refine_diff_density_max         0.496
_refine_diff_density_min         -0.331
_refine_diff_density_rms         0.053



####################################################################### 
# 
# 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_MA50_0m_a
_database_code_depnum_ccdc_archive 'CCDC 2153538'
loop_
_audit_author_name
_audit_author_address
'Hartmut Schubert'
;Universtity of Tuebingen
Germany
;
_audit_update_record             
;
2022-02-21 deposited with the CCDC.	2022-03-22 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/1
_shelx_SHELXL_version_number     2018/1
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C16 Al F36 O4, C32 H67 O2 Si4 Sn'
_chemical_formula_sum            'C48 H67 Al F36 O6 Si4 Sn'
_chemical_formula_weight         1682.07

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Al Al 0.0645 0.0514 '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'
P P 0.1023 0.0942 '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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 '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'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_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'

_cell_length_a                   12.5225(4)
_cell_length_b                   16.1355(5)
_cell_length_c                   18.0799(5)
_cell_angle_alpha                103.153(2)
_cell_angle_beta                 100.644(2)
_cell_angle_gamma                93.328(2)
_cell_volume                     3476.95(19)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9981
_cell_measurement_theta_min      2.81
_cell_measurement_theta_max      23.96

_exptl_crystal_description       prism
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.607
_exptl_crystal_F_000             1692
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.15
_exptl_absorpt_coefficient_mu    0.588
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6928
_exptl_absorpt_correction_T_max  0.7451
_exptl_absorpt_process_details   'SADABS V2012/1 (Bruker AXS Inc.)'
_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            59241
_diffrn_reflns_av_unetI/netI     0.0392
_diffrn_reflns_av_R_equivalents  0.0424
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         1.664
_diffrn_reflns_theta_max         24.640
_diffrn_reflns_theta_full        24.640
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measured_fraction_theta_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_point_group_measured_fraction_full 0.994
_reflns_number_total             11672
_reflns_number_gt                9319
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_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       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXT 2014/4 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2018/1 (Sheldrick, 2018)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_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)+(0.0664P)²+13.1303P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         11672
_refine_ls_number_parameters     888
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0739
_refine_ls_R_factor_gt           0.0546
_refine_ls_wR_factor_ref         0.1469
_refine_ls_wR_factor_gt          0.1339
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_restrained_S_all      1.032
_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
Sn1 Sn 0.51743(3) 0.31309(2) 0.21385(2) 0.02349(11) Uani 1 1 d D . . . .
Si1 Si 0.74094(12) 0.47395(9) 0.43184(8) 0.0336(3) Uani 1 1 d . . . . .
Al1 Al 0.19190(12) 0.22476(8) 0.81742(8) 0.0221(3) Uani 1 1 d . . . . .
Si3 Si 0.23879(12) 0.17300(10) 0.30776(8) 0.0323(3) Uani 1 1 d . . . . .
O4 O 0.1778(3) 0.1864(2) 0.71871(18) 0.0273(7) Uani 1 1 d . . . . .
Si4 Si 0.39699(13) 0.04759(9) 0.22669(8) 0.0330(3) Uani 1 1 d . . . . .
F32 F 0.2511(3) 0.0335(2) 0.6939(2) 0.0562(10) Uani 1 1 d . . . . .
F13 F 0.0911(3) 0.2160(2) 0.9924(2) 0.0567(10) Uani 1 1 d . . . . .
O5 O 0.3499(3) 0.3622(2) 0.22649(19) 0.0323(8) Uani 1 1 d . . . . .
O1 O 0.3116(3) 0.2928(2) 0.85128(19) 0.0304(8) Uani 1 1 d . . . . .
F6 F -0.0342(3) 0.1396(2) 0.7070(2) 0.0501(9) Uani 1 1 d . . . . .
O3 O 0.0874(3) 0.2817(2) 0.8447(2) 0.0328(8) Uani 1 1 d . . . . .
F34 F 0.2032(3) 0.4574(2) 0.8905(3) 0.0659(11) Uani 1 1 d . . . . .
F5 F -0.0548(3) 0.0617(2) 0.5920(2) 0.0553(9) Uani 1 1 d . . . . .
F19 F 0.2632(3) 0.1359(2) 1.05646(18) 0.0538(9) Uani 1 1 d . . . . .
F2 F 0.0934(4) 0.1113(3) 0.51664(18) 0.0672(12) Uani 1 1 d . . . . .
Si2 Si 0.86262(12) 0.30856(10) 0.36233(9) 0.0360(4) Uani 1 1 d . . . . .
O6 O 0.6715(3) 0.2903(2) 0.1610(2) 0.0336(8) Uani 1 1 d . . . . .
F17 F 0.1939(4) -0.0234(2) 0.9610(2) 0.0663(12) Uani 1 1 d . . . . .
O2 O 0.1899(3) 0.1370(2) 0.85774(18) 0.0285(8) Uani 1 1 d . . . . .
F21 F 0.2467(4) -0.0158(2) 0.8556(2) 0.0645(11) Uani 1 1 d . . . . .
F31 F 0.1322(4) -0.0180(2) 0.5893(2) 0.0732(12) Uani 1 1 d . . . . .
F7 F 0.1064(4) 0.3726(3) 0.7420(2) 0.0655(12) Uani 1 1 d . . . . .
F20 F 0.3033(3) 0.2271(2) 0.99370(18) 0.0523(9) Uani 1 1 d . . . . .
F14 F -0.0086(3) 0.1260(3) 0.8915(3) 0.0712(12) Uani 1 1 d . . . . .
F15 F 0.0463(4) 0.0858(3) 0.9967(3) 0.0744(12) Uani 1 1 d . . . . .
F3 F 0.1803(4) 0.2288(2) 0.58795(19) 0.0683(12) Uani 1 1 d . . . . .
F35 F 0.0691(4) 0.4941(2) 0.9457(3) 0.0795(14) Uani 1 1 d . . . . .
F28 F 0.5156(3) 0.3784(3) 0.7702(2) 0.0704(12) Uani 1 1 d . . . . .
F26 F 0.5788(3) 0.3958(3) 0.9249(2) 0.0700(12) Uani 1 1 d . . . . .
F24 F 0.5750(3) 0.2387(3) 0.8244(3) 0.0797(14) Uani 1 1 d . . . . .
F12 F -0.0495(4) 0.3400(3) 0.9533(3) 0.0840(15) Uani 1 1 d . . . . .
F16 F 0.0745(4) -0.0249(2) 0.8563(2) 0.0747(13) Uani 1 1 d . . . . .
F25 F 0.4443(4) 0.3770(3) 0.9799(2) 0.0811(14) Uani 1 1 d . . . . .
F27 F 0.4352(4) 0.4602(2) 0.9023(3) 0.0804(14) Uani 1 1 d . . . . .
F18 F 0.3674(3) 0.1027(3) 0.9724(2) 0.0645(11) Uani 1 1 d . . . . .
F9 F 0.0112(4) 0.4709(2) 0.7887(3) 0.0718(13) Uani 1 1 d . . . . .
F36 F 0.1652(4) 0.3967(2) 0.9773(2) 0.0784(14) Uani 1 1 d . . . . .
F33 F 0.0754(4) 0.0109(2) 0.7055(2) 0.0755(14) Uani 1 1 d . . . . .
F29 F 0.3436(4) 0.3862(3) 0.7538(3) 0.0819(14) Uani 1 1 d . . . . .
F30 F 0.4045(4) 0.2668(3) 0.7099(2) 0.0887(16) Uani 1 1 d . . . . .
F8 F -0.0652(4) 0.3444(3) 0.7283(3) 0.0852(14) Uani 1 1 d . . . . .
F23 F 0.5083(4) 0.2241(3) 0.9219(3) 0.0859(15) Uani 1 1 d . . . . .
F22 F 0.4227(3) 0.1613(2) 0.8083(3) 0.0803(14) Uani 1 1 d . . . . .
F4 F -0.0182(5) 0.2058(3) 0.6133(3) 0.113(2) Uani 1 1 d . . . . .
F11 F -0.1281(4) 0.4081(3) 0.8728(3) 0.0867(16) Uani 1 1 d . . . . .
F10 F -0.1236(3) 0.2713(3) 0.8370(3) 0.0828(14) Uani 1 1 d . . . . .
C42 C 0.6418(4) 0.3027(3) 0.3749(3) 0.0215(10) Uani 1 1 d . . . . .
C43 C 0.3715(4) 0.1625(3) 0.2710(3) 0.0238(10) Uani 1 1 d . . . . .
H43 H 0.364355 0.192176 0.227700 0.029 Uiso 1 1 calc R U . . .
C44 C 0.4713(4) 0.2077(3) 0.3295(3) 0.0229(10) Uani 1 1 d . . . . .
C45 C 0.5477(4) 0.2680(3) 0.3169(3) 0.0196(9) Uani 1 1 d . . . . .
C46 C 0.4900(4) 0.1865(3) 0.4015(3) 0.0268(11) Uani 1 1 d . . . . .
H46 H 0.438402 0.146475 0.410735 0.032 Uiso 1 1 calc R U . . .
F1 F 0.2708(4) 0.1111(4) 0.5880(3) 0.140(3) Uani 1 1 d . . . . .
C48 C 0.1791(5) 0.1077(3) 0.9202(3) 0.0331(12) Uani 1 1 d . . . . .
C49 C 0.6001(5) 0.1952(4) 0.5373(3) 0.0417(14) Uani 1 1 d . . . . .
C50 C 0.5798(4) 0.2210(3) 0.4596(3) 0.0275(11) Uani 1 1 d . . . . .
C51 C 0.2735(6) -0.0147(4) 0.1595(3) 0.0493(16) Uani 1 1 d . . . . .
H51A H 0.247220 0.015855 0.119681 0.074 Uiso 1 1 calc R U . . .
H51B H 0.216317 -0.021580 0.188606 0.074 Uiso 1 1 calc R U . . .
H51C H 0.291852 -0.071101 0.134582 0.074 Uiso 1 1 calc R U . . .
C52 C 0.1267(4) 0.1280(3) 0.6546(3) 0.0286(11) Uani 1 1 d . . . . .
C53 C 0.4427(6) -0.0122(4) 0.3025(3) 0.0499(16) Uani 1 1 d . . . . .
H53A H 0.450625 -0.071471 0.277246 0.075 Uiso 1 1 calc R U . . .
H53B H 0.388313 -0.011846 0.335151 0.075 Uiso 1 1 calc R U . . .
H53C H 0.513103 0.015289 0.334668 0.075 Uiso 1 1 calc R U . . .
C54 C 0.2500(5) 0.2760(4) 0.3815(4) 0.0497(16) Uani 1 1 d . . . . .
H54A H 0.180787 0.282308 0.399073 0.075 Uiso 1 1 calc R U . . .
H54B H 0.266501 0.323508 0.358525 0.075 Uiso 1 1 calc R U . . .
H54C H 0.308740 0.276560 0.425796 0.075 Uiso 1 1 calc R U . . .
C55 C 0.7326(4) 0.3635(3) 0.3650(3) 0.0247(10) Uani 1 1 d . . . . .
H55 H 0.708898 0.371890 0.311558 0.030 Uiso 1 1 calc R U . . .
C56 C 0.4160(5) 0.3104(3) 0.8459(3) 0.0338(12) Uani 1 1 d . . . . .
C57 C 0.2721(5) 0.3585(4) 0.1550(3) 0.0438(14) Uani 1 1 d . . . . .
H57A H 0.240527 0.298898 0.129804 0.053 Uiso 1 1 calc R U . . .
H57B H 0.307804 0.381580 0.118318 0.053 Uiso 1 1 calc R U . . .
C58 C 0.5068(5) 0.0536(4) 0.1713(4) 0.0480(15) Uani 1 1 d . . . . .
H58A H 0.519316 -0.004332 0.145610 0.072 Uiso 1 1 calc R U . . .
H58B H 0.574261 0.082494 0.206778 0.072 Uiso 1 1 calc R U . . .
H58C H 0.484904 0.085901 0.132096 0.072 Uiso 1 1 calc R U . . .
C59 C 0.0436(5) 0.3576(3) 0.8538(3) 0.0403(14) Uani 1 1 d . . . . .
C60 C 0.6547(4) 0.2780(3) 0.4443(3) 0.0246(10) Uani 1 1 d . . . . .
H60 H 0.717894 0.301234 0.483207 0.030 Uiso 1 1 calc R U . . .
C61 C 0.1205(7) 0.4275(4) 0.9190(4) 0.0569(19) Uani 1 1 d . . . . .
C62 C 0.3470(5) 0.4460(4) 0.2796(3) 0.0431(14) Uani 1 1 d . . . . .
H62A H 0.350651 0.440007 0.333261 0.052 Uiso 1 1 calc R U . . .
H62B H 0.409055 0.486779 0.279268 0.052 Uiso 1 1 calc R U . . .
C63 C 0.1279(5) 0.1741(4) 0.2237(3) 0.0467(15) Uani 1 1 d . . . . .
H63A H 0.123107 0.121037 0.183467 0.070 Uiso 1 1 calc R U . . .
H63B H 0.144123 0.223169 0.202664 0.070 Uiso 1 1 calc R U . . .
H63C H 0.058185 0.178635 0.240837 0.070 Uiso 1 1 calc R U . . .
C64 C 0.0763(6) 0.1353(4) 0.9522(4) 0.0528(17) Uani 1 1 d . . . . .
C65 C 0.7704(7) 0.2286(4) 0.0690(5) 0.078(3) Uani 1 1 d . . . . .
H65A H 0.835027 0.207483 0.096571 0.094 Uiso 1 1 calc R U . . .
H65B H 0.757574 0.199384 0.013257 0.094 Uiso 1 1 calc R U . . .
C66 C 0.2006(5) 0.0858(4) 0.3529(4) 0.0495(16) Uani 1 1 d . . . . .
H66A H 0.258476 0.084837 0.397222 0.074 Uiso 1 1 calc R U . . .
H66B H 0.191162 0.030685 0.314592 0.074 Uiso 1 1 calc R U . . .
H66C H 0.132006 0.095808 0.370585 0.074 Uiso 1 1 calc R U . . .
C67 C 0.4702(6) 0.3871(4) 0.9152(4) 0.0565(18) Uani 1 1 d . . . . .
C68 C 0.1746(7) 0.0092(4) 0.8990(4) 0.0561(18) Uani 1 1 d . . . . .
C69 C 0.7928(9) 0.4778(4) 0.5351(4) 0.092(3) Uani 1 1 d . . . . .
H69A H 0.862258 0.452581 0.540832 0.139 Uiso 1 1 calc R U . . .
H69B H 0.739517 0.445363 0.554069 0.139 Uiso 1 1 calc R U . . .
H69C H 0.803989 0.537398 0.565332 0.139 Uiso 1 1 calc R U . . .
C70 C 0.6734(6) 0.2113(4) 0.1013(4) 0.0519(16) Uani 1 1 d . . . . .
H70A H 0.605950 0.200079 0.060510 0.062 Uiso 1 1 calc R U . . .
H70B H 0.680557 0.161505 0.124542 0.062 Uiso 1 1 calc R U . . .
C71 C 0.1852(6) 0.4129(5) 0.1795(4) 0.071(2) Uani 1 1 d . . . . .
H71A H 0.154570 0.441774 0.138674 0.086 Uiso 1 1 calc R U . . .
H71B H 0.125248 0.377997 0.190574 0.086 Uiso 1 1 calc R U . . .
C72 C 0.4820(6) 0.2330(4) 0.8498(5) 0.0587(18) Uani 1 1 d . . . . .
C73 C 0.2806(5) 0.1439(4) 0.9883(3) 0.0461(15) Uani 1 1 d . . . . .
C74 C 0.9517(6) 0.3638(5) 0.3137(6) 0.086(3) Uani 1 1 d . . . . .
H74A H 0.909863 0.368807 0.263720 0.129 Uiso 1 1 calc R U . . .
H74B H 1.013495 0.330786 0.305023 0.129 Uiso 1 1 calc R U . . .
H74C H 0.979094 0.420993 0.346454 0.129 Uiso 1 1 calc R U . . .
C75 C 0.4210(6) 0.3372(5) 0.7689(4) 0.0572(18) Uani 1 1 d . . . . .
C76 C 0.2426(7) 0.4754(6) 0.2498(5) 0.089(3) Uani 1 1 d . . . . .
H76A H 0.197019 0.482496 0.289631 0.107 Uiso 1 1 calc R U . . .
H76B H 0.255989 0.531589 0.237886 0.107 Uiso 1 1 calc R U . . .
C77 C 0.7198(6) 0.3611(4) 0.1352(4) 0.0541(18) Uani 1 1 d . . . . .
H77A H 0.765295 0.403528 0.180001 0.065 Uiso 1 1 calc R U . . .
H77B H 0.661929 0.390176 0.109266 0.065 Uiso 1 1 calc R U . . .
C78 C 0.4967(5) 0.1516(5) 0.5515(4) 0.0577(19) Uani 1 1 d . . . . .
H78A H 0.437140 0.187984 0.545760 0.087 Uiso 1 1 calc R U . . .
H78B H 0.510382 0.142596 0.604068 0.087 Uiso 1 1 calc R U . . .
H78C H 0.476129 0.096306 0.513675 0.087 Uiso 1 1 calc R U . . .
C79 C 0.6872(7) 0.1331(7) 0.5360(5) 0.097(3) Uani 1 1 d . . . . .
H79A H 0.660747 0.081569 0.494296 0.145 Uiso 1 1 calc R U . . .
H79B H 0.702947 0.117463 0.585877 0.145 Uiso 1 1 calc R U . . .
H79C H 0.753996 0.160400 0.526923 0.145 Uiso 1 1 calc R U . . .
C80 C 0.7888(7) 0.3217(4) 0.0795(5) 0.075(2) Uani 1 1 d . . . . .
H80A H 0.767000 0.337082 0.029270 0.090 Uiso 1 1 calc R U . . .
H80B H 0.866897 0.342099 0.100777 0.090 Uiso 1 1 calc R U . . .
C81 C 0.0256(7) 0.3875(5) 0.7776(4) 0.060(2) Uani 1 1 d . . . . .
C82 C 0.8265(6) 0.1979(4) 0.3038(5) 0.072(2) Uani 1 1 d . . . . .
H82A H 0.789059 0.198411 0.251275 0.109 Uiso 1 1 calc R U . . .
H82B H 0.778147 0.167156 0.327699 0.109 Uiso 1 1 calc R U . . .
H82C H 0.893111 0.169319 0.301157 0.109 Uiso 1 1 calc R U . . .
C83 C 0.6358(8) 0.2743(6) 0.6046(4) 0.090(3) Uani 1 1 d . . . . .
H83A H 0.708406 0.299136 0.602942 0.135 Uiso 1 1 calc R U . . .
H83B H 0.638649 0.257910 0.653854 0.135 Uiso 1 1 calc R U . . .
H83C H 0.583403 0.316586 0.600227 0.135 Uiso 1 1 calc R U . . .
C84 C 0.6037(6) 0.5131(5) 0.4210(5) 0.089(3) Uani 1 1 d . . . . .
H84A H 0.552925 0.474710 0.436206 0.133 Uiso 1 1 calc R U . . .
H84B H 0.577282 0.514310 0.366772 0.133 Uiso 1 1 calc R U . . .
H84C H 0.608544 0.570911 0.454248 0.133 Uiso 1 1 calc R U . . .
C85 C 0.1509(8) 0.0367(5) 0.6589(5) 0.100(4) Uani 1 1 d . . . . .
C86 C -0.0678(7) 0.3434(5) 0.8770(5) 0.067(2) Uani 1 1 d . . . . .
C87 C -0.0004(6) 0.1277(6) 0.6435(5) 0.084(3) Uani 1 1 d . . . . .
C88 C 0.8308(7) 0.5494(4) 0.4009(5) 0.082(3) Uani 1 1 d . . . . .
H88A H 0.831237 0.607455 0.432547 0.123 Uiso 1 1 calc R U . . .
H88B H 0.803469 0.547916 0.346158 0.123 Uiso 1 1 calc R U . . .
H88C H 0.905312 0.532552 0.407613 0.123 Uiso 1 1 calc R U . . .
C89 C 0.1549(10) 0.1519(6) 0.5840(4) 0.116(5) Uani 1 1 d . . . . .
C90 C 0.9391(7) 0.3042(10) 0.4580(5) 0.145(6) Uani 1 1 d . . . . .
H90A H 1.004350 0.274686 0.451886 0.217 Uiso 1 1 calc R U . . .
H90B H 0.892839 0.273039 0.483045 0.217 Uiso 1 1 calc R U . . .
H90C H 0.961048 0.362483 0.490140 0.217 Uiso 1 1 calc R U . . .
H6 H 0.562(4) 0.4205(15) 0.215(3) 0.029(13) Uiso 1 1 d D . . . .
H10 H 0.452(4) 0.242(3) 0.1224(16) 0.028(13) Uiso 1 1 d D . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Sn1 C45 2.129(4) . ?
Sn1 O5 2.317(3) . ?
Sn1 O6 2.318(3) . ?
Sn1 H6 1.784(19) . ?
Sn1 H10 1.804(19) . ?
Si1 C69 1.846(6) . ?
Si1 C88 1.856(7) . ?
Si1 C84 1.857(8) . ?
Si1 C55 1.897(5) . ?
Al1 O4 1.723(3) . ?
Al1 O3 1.724(4) . ?
Al1 O1 1.730(4) . ?
Al1 O2 1.734(3) . ?
Si3 C54 1.859(6) . ?
Si3 C66 1.861(6) . ?
Si3 C63 1.863(6) . ?
Si3 C43 1.903(5) . ?
O4 C52 1.341(6) . ?
Si4 C58 1.856(6) . ?
Si4 C51 1.857(6) . ?
Si4 C53 1.875(6) . ?
Si4 C43 1.915(5) . ?
F32 C85 1.306(9) . ?
F13 C64 1.322(8) . ?
O5 C57 1.455(6) . ?
O5 C62 1.476(6) . ?
O1 C56 1.346(6) . ?
F6 C87 1.273(8) . ?
O3 C59 1.358(6) . ?
F34 C61 1.351(8) . ?
F5 C87 1.303(8) . ?
F19 C73 1.323(7) . ?
F2 C89 1.318(8) . ?
Si2 C90 1.834(8) . ?
Si2 C82 1.838(7) . ?
Si2 C74 1.849(7) . ?
Si2 C55 1.902(5) . ?
O6 C77 1.467(6) . ?
O6 C70 1.476(7) . ?
F17 C68 1.333(7) . ?
O2 C48 1.346(6) . ?
F21 C68 1.324(8) . ?
F31 C85 1.334(8) . ?
F7 C81 1.301(7) . ?
F20 C73 1.334(7) . ?
F14 C64 1.354(8) . ?
F15 C64 1.340(7) . ?
F3 C89 1.246(9) . ?
F35 C61 1.328(7) . ?
F28 C75 1.318(7) . ?
F26 C67 1.333(8) . ?
F24 C72 1.334(8) . ?
F12 C86 1.370(9) . ?
F16 C68 1.357(8) . ?
F25 C67 1.312(8) . ?
F27 C67 1.336(8) . ?
F18 C73 1.349(7) . ?
F9 C81 1.342(7) . ?
F36 C61 1.313(8) . ?
F33 C85 1.477(13) . ?
F29 C75 1.315(9) . ?
F30 C75 1.346(8) . ?
F8 C81 1.350(9) . ?
F23 C72 1.327(9) . ?
F22 C72 1.325(8) . ?
F4 C87 1.495(11) . ?
F11 C86 1.332(7) . ?
F10 C86 1.304(9) . ?
C42 C60 1.386(6) . ?
C42 C45 1.414(6) . ?
C42 C55 1.520(6) . ?
C43 C44 1.506(6) . ?
C43 H43 1.0000 . ?
C44 C46 1.402(7) . ?
C44 C45 1.410(6) . ?
C46 C50 1.379(7) . ?
C46 H46 0.9500 . ?
F1 C89 1.624(15) . ?
C48 C68 1.542(8) . ?
C48 C64 1.553(9) . ?
C48 C73 1.575(8) . ?
C49 C79 1.523(10) . ?
C49 C83 1.528(10) . ?
C49 C78 1.529(8) . ?
C49 C50 1.536(7) . ?
C50 C60 1.382(7) . ?
C51 H51A 0.9800 . ?
C51 H51B 0.9800 . ?
C51 H51C 0.9800 . ?
C52 C89 1.509(9) . ?
C52 C85 1.538(9) . ?
C52 C87 1.567(9) . ?
C53 H53A 0.9800 . ?
C53 H53B 0.9800 . ?
C53 H53C 0.9800 . ?
C54 H54A 0.9800 . ?
C54 H54B 0.9800 . ?
C54 H54C 0.9800 . ?
C55 H55 1.0000 . ?
C56 C72 1.544(8) . ?
C56 C75 1.561(8) . ?
C56 C67 1.564(8) . ?
C57 C71 1.504(9) . ?
C57 H57A 0.9900 . ?
C57 H57B 0.9900 . ?
C58 H58A 0.9800 . ?
C58 H58B 0.9800 . ?
C58 H58C 0.9800 . ?
C59 C81 1.544(8) . ?
C59 C86 1.548(9) . ?
C59 C61 1.561(9) . ?
C60 H60 0.9500 . ?
C62 C76 1.468(9) . ?
C62 H62A 0.9900 . ?
C62 H62B 0.9900 . ?
C63 H63A 0.9800 . ?
C63 H63B 0.9800 . ?
C63 H63C 0.9800 . ?
C65 C80 1.468(9) . ?
C65 C70 1.480(9) . ?
C65 H65A 0.9900 . ?
C65 H65B 0.9900 . ?
C66 H66A 0.9800 . ?
C66 H66B 0.9800 . ?
C66 H66C 0.9800 . ?
C69 H69A 0.9800 . ?
C69 H69B 0.9800 . ?
C69 H69C 0.9800 . ?
C70 H70A 0.9900 . ?
C70 H70B 0.9900 . ?
C71 C76 1.465(10) . ?
C71 H71A 0.9900 . ?
C71 H71B 0.9900 . ?
C74 H74A 0.9800 . ?
C74 H74B 0.9800 . ?
C74 H74C 0.9800 . ?
C76 H76A 0.9900 . ?
C76 H76B 0.9900 . ?
C77 C80 1.503(9) . ?
C77 H77A 0.9900 . ?
C77 H77B 0.9900 . ?
C78 H78A 0.9800 . ?
C78 H78B 0.9800 . ?
C78 H78C 0.9800 . ?
C79 H79A 0.9800 . ?
C79 H79B 0.9800 . ?
C79 H79C 0.9800 . ?
C80 H80A 0.9900 . ?
C80 H80B 0.9900 . ?
C82 H82A 0.9800 . ?
C82 H82B 0.9800 . ?
C82 H82C 0.9800 . ?
C83 H83A 0.9800 . ?
C83 H83B 0.9800 . ?
C83 H83C 0.9800 . ?
C84 H84A 0.9800 . ?
C84 H84B 0.9800 . ?
C84 H84C 0.9800 . ?
C88 H88A 0.9800 . ?
C88 H88B 0.9800 . ?
C88 H88C 0.9800 . ?
C90 H90A 0.9800 . ?
C90 H90B 0.9800 . ?
C90 H90C 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
C45 Sn1 O5 97.50(14) . . ?
C45 Sn1 O6 105.19(15) . . ?
O5 Sn1 O6 157.15(12) . . ?
C45 Sn1 H6 121.0(15) . . ?
O5 Sn1 H6 85.9(16) . . ?
O6 Sn1 H6 80.2(15) . . ?
C45 Sn1 H10 120.6(15) . . ?
O5 Sn1 H10 88.7(15) . . ?
O6 Sn1 H10 82.1(15) . . ?
H6 Sn1 H10 118(2) . . ?
C69 Si1 C88 109.1(4) . . ?
C69 Si1 C84 108.9(5) . . ?
C88 Si1 C84 106.5(4) . . ?
C69 Si1 C55 113.8(3) . . ?
C88 Si1 C55 108.9(3) . . ?
C84 Si1 C55 109.5(3) . . ?
O4 Al1 O3 114.40(18) . . ?
O4 Al1 O1 108.09(17) . . ?
O3 Al1 O1 107.31(18) . . ?
O4 Al1 O2 107.39(17) . . ?
O3 Al1 O2 106.14(18) . . ?
O1 Al1 O2 113.67(17) . . ?
C54 Si3 C66 107.6(3) . . ?
C54 Si3 C63 108.6(3) . . ?
C66 Si3 C63 109.0(3) . . ?
C54 Si3 C43 109.5(2) . . ?
C66 Si3 C43 114.3(3) . . ?
C63 Si3 C43 107.7(2) . . ?
C52 O4 Al1 147.0(3) . . ?
C58 Si4 C51 108.6(3) . . ?
C58 Si4 C53 108.4(3) . . ?
C51 Si4 C53 107.9(3) . . ?
C58 Si4 C43 107.4(2) . . ?
C51 Si4 C43 112.1(3) . . ?
C53 Si4 C43 112.3(2) . . ?
C57 O5 C62 107.2(4) . . ?
C57 O5 Sn1 116.7(3) . . ?
C62 O5 Sn1 119.1(3) . . ?
C56 O1 Al1 147.6(3) . . ?
C59 O3 Al1 147.0(3) . . ?
C90 Si2 C82 107.7(6) . . ?
C90 Si2 C74 109.4(5) . . ?
C82 Si2 C74 107.5(4) . . ?
C90 Si2 C55 114.2(3) . . ?
C82 Si2 C55 108.8(3) . . ?
C74 Si2 C55 109.1(3) . . ?
C77 O6 C70 106.8(4) . . ?
C77 O6 Sn1 117.3(3) . . ?
C70 O6 Sn1 120.0(3) . . ?
C48 O2 Al1 146.7(3) . . ?
C60 C42 C45 118.5(4) . . ?
C60 C42 C55 117.4(4) . . ?
C45 C42 C55 124.1(4) . . ?
C44 C43 Si3 114.1(3) . . ?
C44 C43 Si4 109.8(3) . . ?
Si3 C43 Si4 114.9(2) . . ?
C44 C43 H43 105.7 . . ?
Si3 C43 H43 105.7 . . ?
Si4 C43 H43 105.7 . . ?
C46 C44 C45 117.9(4) . . ?
C46 C44 C43 116.9(4) . . ?
C45 C44 C43 125.2(4) . . ?
C44 C45 C42 120.0(4) . . ?
C44 C45 Sn1 120.3(3) . . ?
C42 C45 Sn1 119.6(3) . . ?
C50 C46 C44 123.1(4) . . ?
C50 C46 H46 118.5 . . ?
C44 C46 H46 118.5 . . ?
O2 C48 C68 109.1(4) . . ?
O2 C48 C64 113.0(4) . . ?
C68 C48 C64 109.8(5) . . ?
O2 C48 C73 110.2(4) . . ?
C68 C48 C73 108.1(5) . . ?
C64 C48 C73 106.6(5) . . ?
C79 C49 C83 111.0(7) . . ?
C79 C49 C78 108.7(6) . . ?
C83 C49 C78 106.4(6) . . ?
C79 C49 C50 108.4(5) . . ?
C83 C49 C50 110.4(5) . . ?
C78 C49 C50 111.9(5) . . ?
C46 C50 C60 117.4(4) . . ?
C46 C50 C49 122.2(4) . . ?
C60 C50 C49 120.4(4) . . ?
Si4 C51 H51A 109.5 . . ?
Si4 C51 H51B 109.5 . . ?
H51A C51 H51B 109.5 . . ?
Si4 C51 H51C 109.5 . . ?
H51A C51 H51C 109.5 . . ?
H51B C51 H51C 109.5 . . ?
O4 C52 C89 109.5(4) . . ?
O4 C52 C85 111.8(5) . . ?
C89 C52 C85 113.0(7) . . ?
O4 C52 C87 111.2(4) . . ?
C89 C52 C87 105.2(7) . . ?
C85 C52 C87 105.9(6) . . ?
Si4 C53 H53A 109.5 . . ?
Si4 C53 H53B 109.5 . . ?
H53A C53 H53B 109.5 . . ?
Si4 C53 H53C 109.5 . . ?
H53A C53 H53C 109.5 . . ?
H53B C53 H53C 109.5 . . ?
Si3 C54 H54A 109.5 . . ?
Si3 C54 H54B 109.5 . . ?
H54A C54 H54B 109.5 . . ?
Si3 C54 H54C 109.5 . . ?
H54A C54 H54C 109.5 . . ?
H54B C54 H54C 109.5 . . ?
C42 C55 Si1 112.0(3) . . ?
C42 C55 Si2 110.1(3) . . ?
Si1 C55 Si2 118.7(2) . . ?
C42 C55 H55 104.9 . . ?
Si1 C55 H55 104.9 . . ?
Si2 C55 H55 104.9 . . ?
O1 C56 C72 111.7(4) . . ?
O1 C56 C75 110.7(5) . . ?
C72 C56 C75 109.2(5) . . ?
O1 C56 C67 108.5(5) . . ?
C72 C56 C67 108.6(5) . . ?
C75 C56 C67 108.1(5) . . ?
O5 C57 C71 105.0(5) . . ?
O5 C57 H57A 110.7 . . ?
C71 C57 H57A 110.7 . . ?
O5 C57 H57B 110.7 . . ?
C71 C57 H57B 110.7 . . ?
H57A C57 H57B 108.8 . . ?
Si4 C58 H58A 109.5 . . ?
Si4 C58 H58B 109.5 . . ?
H58A C58 H58B 109.5 . . ?
Si4 C58 H58C 109.5 . . ?
H58A C58 H58C 109.5 . . ?
H58B C58 H58C 109.5 . . ?
O3 C59 C81 111.0(4) . . ?
O3 C59 C86 107.2(5) . . ?
C81 C59 C86 109.4(6) . . ?
O3 C59 C61 110.3(5) . . ?
C81 C59 C61 109.2(5) . . ?
C86 C59 C61 109.8(5) . . ?
C50 C60 C42 123.1(4) . . ?
C50 C60 H60 118.4 . . ?
C42 C60 H60 118.4 . . ?
F36 C61 F35 109.0(5) . . ?
F36 C61 F34 106.7(6) . . ?
F35 C61 F34 106.9(5) . . ?
F36 C61 C59 111.9(5) . . ?
F35 C61 C59 112.3(6) . . ?
F34 C61 C59 109.6(5) . . ?
C76 C62 O5 105.1(5) . . ?
C76 C62 H62A 110.7 . . ?
O5 C62 H62A 110.7 . . ?
C76 C62 H62B 110.7 . . ?
O5 C62 H62B 110.7 . . ?
H62A C62 H62B 108.8 . . ?
Si3 C63 H63A 109.5 . . ?
Si3 C63 H63B 109.5 . . ?
H63A C63 H63B 109.5 . . ?
Si3 C63 H63C 109.5 . . ?
H63A C63 H63C 109.5 . . ?
H63B C63 H63C 109.5 . . ?
F13 C64 F15 108.9(5) . . ?
F13 C64 F14 108.7(5) . . ?
F15 C64 F14 106.3(5) . . ?
F13 C64 C48 111.7(5) . . ?
F15 C64 C48 112.6(5) . . ?
F14 C64 C48 108.5(5) . . ?
C80 C65 C70 107.3(6) . . ?
C80 C65 H65A 110.2 . . ?
C70 C65 H65A 110.2 . . ?
C80 C65 H65B 110.2 . . ?
C70 C65 H65B 110.2 . . ?
H65A C65 H65B 108.5 . . ?
Si3 C66 H66A 109.5 . . ?
Si3 C66 H66B 109.5 . . ?
H66A C66 H66B 109.5 . . ?
Si3 C66 H66C 109.5 . . ?
H66A C66 H66C 109.5 . . ?
H66B C66 H66C 109.5 . . ?
F25 C67 F26 108.6(6) . . ?
F25 C67 F27 108.2(6) . . ?
F26 C67 F27 107.3(5) . . ?
F25 C67 C56 110.5(5) . . ?
F26 C67 C56 112.1(5) . . ?
F27 C67 C56 110.0(5) . . ?
F21 C68 F17 108.5(6) . . ?
F21 C68 F16 107.0(5) . . ?
F17 C68 F16 108.3(5) . . ?
F21 C68 C48 110.4(5) . . ?
F17 C68 C48 112.9(5) . . ?
F16 C68 C48 109.5(5) . . ?
Si1 C69 H69A 109.5 . . ?
Si1 C69 H69B 109.5 . . ?
H69A C69 H69B 109.5 . . ?
Si1 C69 H69C 109.5 . . ?
H69A C69 H69C 109.5 . . ?
H69B C69 H69C 109.5 . . ?
O6 C70 C65 104.2(5) . . ?
O6 C70 H70A 110.9 . . ?
C65 C70 H70A 110.9 . . ?
O6 C70 H70B 110.9 . . ?
C65 C70 H70B 110.9 . . ?
H70A C70 H70B 108.9 . . ?
C76 C71 C57 104.0(6) . . ?
C76 C71 H71A 111.0 . . ?
C57 C71 H71A 111.0 . . ?
C76 C71 H71B 111.0 . . ?
C57 C71 H71B 111.0 . . ?
H71A C71 H71B 109.0 . . ?
F22 C72 F23 106.4(6) . . ?
F22 C72 F24 108.1(6) . . ?
F23 C72 F24 106.9(6) . . ?
F22 C72 C56 110.3(6) . . ?
F23 C72 C56 111.3(6) . . ?
F24 C72 C56 113.4(6) . . ?
F19 C73 F20 107.5(5) . . ?
F19 C73 F18 109.2(5) . . ?
F20 C73 F18 109.0(5) . . ?
F19 C73 C48 113.0(5) . . ?
F20 C73 C48 108.9(5) . . ?
F18 C73 C48 109.1(5) . . ?
Si2 C74 H74A 109.5 . . ?
Si2 C74 H74B 109.5 . . ?
H74A C74 H74B 109.5 . . ?
Si2 C74 H74C 109.5 . . ?
H74A C74 H74C 109.5 . . ?
H74B C74 H74C 109.5 . . ?
F29 C75 F28 108.4(6) . . ?
F29 C75 F30 107.8(6) . . ?
F28 C75 F30 107.6(6) . . ?
F29 C75 C56 110.4(5) . . ?
F28 C75 C56 113.2(5) . . ?
F30 C75 C56 109.2(6) . . ?
C71 C76 C62 109.7(6) . . ?
C71 C76 H76A 109.7 . . ?
C62 C76 H76A 109.7 . . ?
C71 C76 H76B 109.7 . . ?
C62 C76 H76B 109.7 . . ?
H76A C76 H76B 108.2 . . ?
O6 C77 C80 106.1(5) . . ?
O6 C77 H77A 110.5 . . ?
C80 C77 H77A 110.5 . . ?
O6 C77 H77B 110.5 . . ?
C80 C77 H77B 110.5 . . ?
H77A C77 H77B 108.7 . . ?
C49 C78 H78A 109.5 . . ?
C49 C78 H78B 109.5 . . ?
H78A C78 H78B 109.5 . . ?
C49 C78 H78C 109.5 . . ?
H78A C78 H78C 109.5 . . ?
H78B C78 H78C 109.5 . . ?
C49 C79 H79A 109.5 . . ?
C49 C79 H79B 109.5 . . ?
H79A C79 H79B 109.5 . . ?
C49 C79 H79C 109.5 . . ?
H79A C79 H79C 109.5 . . ?
H79B C79 H79C 109.5 . . ?
C65 C80 C77 106.6(5) . . ?
C65 C80 H80A 110.4 . . ?
C77 C80 H80A 110.4 . . ?
C65 C80 H80B 110.4 . . ?
C77 C80 H80B 110.4 . . ?
H80A C80 H80B 108.6 . . ?
F7 C81 F9 109.0(6) . . ?
F7 C81 F8 106.7(6) . . ?
F9 C81 F8 106.4(6) . . ?
F7 C81 C59 111.5(5) . . ?
F9 C81 C59 112.6(6) . . ?
F8 C81 C59 110.3(6) . . ?
Si2 C82 H82A 109.5 . . ?
Si2 C82 H82B 109.5 . . ?
H82A C82 H82B 109.5 . . ?
Si2 C82 H82C 109.5 . . ?
H82A C82 H82C 109.5 . . ?
H82B C82 H82C 109.5 . . ?
C49 C83 H83A 109.5 . . ?
C49 C83 H83B 109.5 . . ?
H83A C83 H83B 109.5 . . ?
C49 C83 H83C 109.5 . . ?
H83A C83 H83C 109.5 . . ?
H83B C83 H83C 109.5 . . ?
Si1 C84 H84A 109.5 . . ?
Si1 C84 H84B 109.5 . . ?
H84A C84 H84B 109.5 . . ?
Si1 C84 H84C 109.5 . . ?
H84A C84 H84C 109.5 . . ?
H84B C84 H84C 109.5 . . ?
F32 C85 F31 108.3(7) . . ?
F32 C85 F33 108.7(7) . . ?
F31 C85 F33 109.5(8) . . ?
F32 C85 C52 112.7(7) . . ?
F31 C85 C52 112.8(7) . . ?
F33 C85 C52 104.7(6) . . ?
F10 C86 F11 110.1(7) . . ?
F10 C86 F12 106.8(6) . . ?
F11 C86 F12 105.3(6) . . ?
F10 C86 C59 112.6(6) . . ?
F11 C86 C59 112.6(5) . . ?
F12 C86 C59 108.9(7) . . ?
F6 C87 F5 111.7(6) . . ?
F6 C87 F4 107.1(7) . . ?
F5 C87 F4 108.5(7) . . ?
F6 C87 C52 113.4(6) . . ?
F5 C87 C52 114.0(7) . . ?
F4 C87 C52 101.4(6) . . ?
Si1 C88 H88A 109.5 . . ?
Si1 C88 H88B 109.5 . . ?
H88A C88 H88B 109.5 . . ?
Si1 C88 H88C 109.5 . . ?
H88A C88 H88C 109.5 . . ?
H88B C88 H88C 109.5 . . ?
F3 C89 F2 112.9(8) . . ?
F3 C89 C52 118.3(7) . . ?
F2 C89 C52 116.1(6) . . ?
F3 C89 F1 103.6(8) . . ?
F2 C89 F1 105.8(8) . . ?
C52 C89 F1 96.8(7) . . ?
Si2 C90 H90A 109.5 . . ?
Si2 C90 H90B 109.5 . . ?
H90A C90 H90B 109.5 . . ?
Si2 C90 H90C 109.5 . . ?
H90A C90 H90C 109.5 . . ?
H90B C90 H90C 109.5 . . ?

_refine_diff_density_max         1.707
_refine_diff_density_min         -1.020
_refine_diff_density_rms         0.099



####################################################################### 
# 
# 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_MA103_0m_neu_a
_database_code_depnum_ccdc_archive 'CCDC 2153540'
loop_
_audit_author_name
_audit_author_address
'Hartmut Schubert'
;Universtity of Tuebingen
Germany
;
_audit_update_record             
;
2022-02-21 deposited with the CCDC.	2022-03-22 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/1
_shelx_SHELXL_version_number     2018/1
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         '2 (C32 H65 Br2 Li O2 Pb Si4), C5 H12'
_chemical_formula_sum            'C69 H142 Br4 Li2 O4 Pb2 Si8'
_chemical_formula_weight         2008.43

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'
Li Li -0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 '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'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -3.3944 10.1111 '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'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_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'

_cell_length_a                   9.40780(10)
_cell_length_b                   12.5125(2)
_cell_length_c                   20.8396(3)
_cell_angle_alpha                89.4300(10)
_cell_angle_beta                 88.5550(10)
_cell_angle_gamma                72.1210(10)
_cell_volume                     2333.92(6)
_cell_formula_units_Z            1
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9933
_cell_measurement_theta_min      2.97
_cell_measurement_theta_max      29.95

_exptl_crystal_description       prism
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.429
_exptl_crystal_F_000             1010
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.312
_exptl_crystal_size_mid          0.267
_exptl_crystal_size_min          0.178
_exptl_absorpt_coefficient_mu    5.454
_shelx_estimated_absorpt_T_min   0.281
_shelx_estimated_absorpt_T_max   0.444
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5708
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_process_details   'SADABS V2012/1 (Bruker AXS Inc.)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'sealed tube'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean 8.333
_diffrn_reflns_number            80930
_diffrn_reflns_av_unetI/netI     0.0339
_diffrn_reflns_av_R_equivalents  0.0432
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_theta_min         2.561
_diffrn_reflns_theta_max         30.541
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             14169
_reflns_number_gt                12528
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_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       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXT 2014/4 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2018/1 (Sheldrick, 2018)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_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)+(0.0403P)²+5.9304P] 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_number_reflns         14169
_refine_ls_number_parameters     445
_refine_ls_number_restraints     68
_refine_ls_R_factor_all          0.0445
_refine_ls_R_factor_gt           0.0365
_refine_ls_wR_factor_ref         0.0912
_refine_ls_wR_factor_gt          0.0879
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_restrained_S_all      1.048
_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
Si1 Si 0.56547(11) 1.03185(8) 0.23893(5) 0.0276(2) Uani 1 1 d . . . . .
O1 O 0.3552(3) 0.7674(3) 0.48680(17) 0.0498(9) Uani 1 1 d . . . . .
C1 C 0.6732(3) 0.7151(3) 0.23807(15) 0.0182(6) Uani 1 1 d . . . . .
Si2 Si 0.28717(11) 0.93778(10) 0.27634(5) 0.0308(2) Uani 1 1 d . . . . .
O2 O 0.6521(3) 0.6779(3) 0.55100(14) 0.0380(6) Uani 1 1 d . . . . .
C2 C 0.5603(3) 0.8116(3) 0.21755(15) 0.0177(6) Uani 1 1 d . . . . .
Si3 Si 0.76396(12) 0.39011(9) 0.21391(5) 0.0306(2) Uani 1 1 d . . . . .
C3 C 0.5059(3) 0.8147(3) 0.15532(16) 0.0215(6) Uani 1 1 d . . . . .
H3 H 0.431463 0.880448 0.141458 0.026 Uiso 1 1 calc R U . . .
Si4 Si 1.02776(11) 0.49718(10) 0.17316(5) 0.0318(2) Uani 1 1 d . . . . .
C4 C 0.5570(3) 0.7247(3) 0.11314(15) 0.0221(6) Uani 1 1 d . . . . .
C5 C 0.6659(4) 0.6295(3) 0.13503(16) 0.0229(6) Uani 1 1 d . . . . .
H5 H 0.701505 0.566639 0.107295 0.027 Uiso 1 1 calc R U . . .
C6 C 0.7246(3) 0.6233(3) 0.19629(15) 0.0193(6) Uani 1 1 d . . . . .
C7 C 0.4935(3) 0.9122(3) 0.26071(15) 0.0194(6) Uani 1 1 d . . . . .
H7 H 0.538724 0.886556 0.303271 0.023 Uiso 1 1 calc R U . . .
C8 C 0.8416(4) 0.5133(3) 0.21496(16) 0.0226(6) Uani 1 1 d . . . . .
H8 H 0.859888 0.523024 0.261287 0.027 Uiso 1 1 calc R U . . .
C9 C 0.4868(4) 0.7280(4) 0.04667(17) 0.0316(8) Uani 1 1 d . . . . .
C10 C 0.4257(7) 0.8469(5) 0.0213(2) 0.0624(17) Uani 1 1 d . . . . .
H10A H 0.507396 0.879753 0.015887 0.094 Uiso 1 1 calc R U . . .
H10B H 0.350889 0.892132 0.051878 0.094 Uiso 1 1 calc R U . . .
H10C H 0.379331 0.845833 -0.020132 0.094 Uiso 1 1 calc R U . . .
C11 C 0.3557(7) 0.6794(8) 0.0548(3) 0.078(2) Uani 1 1 d . . . . .
H11A H 0.306319 0.682827 0.013614 0.117 Uiso 1 1 calc R U . . .
H11B H 0.283977 0.723205 0.086824 0.117 Uiso 1 1 calc R U . . .
H11C H 0.393473 0.601032 0.069003 0.117 Uiso 1 1 calc R U . . .
C12 C 0.5976(6) 0.6592(5) -0.0024(2) 0.0642(18) Uani 1 1 d . . . . .
H12A H 0.550362 0.666156 -0.044270 0.096 Uiso 1 1 calc R U . . .
H12B H 0.629834 0.580218 0.010876 0.096 Uiso 1 1 calc R U . . .
H12C H 0.684561 0.686667 -0.005673 0.096 Uiso 1 1 calc R U . . .
C13 C 0.7739(5) 0.9793(4) 0.2433(3) 0.0477(12) Uani 1 1 d . . . . .
H13A H 0.813208 0.915931 0.213859 0.071 Uiso 1 1 calc R U . . .
H13B H 0.802389 0.954679 0.287248 0.071 Uiso 1 1 calc R U . . .
H13C H 0.815387 1.039730 0.231172 0.071 Uiso 1 1 calc R U . . .
C14 C 0.4955(5) 1.1484(4) 0.2978(2) 0.0414(10) Uani 1 1 d . . . . .
H14A H 0.554452 1.200543 0.293148 0.062 Uiso 1 1 calc R U . . .
H14B H 0.505008 1.117553 0.341473 0.062 Uiso 1 1 calc R U . . .
H14C H 0.390325 1.188439 0.289828 0.062 Uiso 1 1 calc R U . . .
C15 C 0.5159(6) 1.0882(4) 0.1565(2) 0.0444(11) Uani 1 1 d . . . . .
H15A H 0.562126 1.029590 0.124848 0.067 Uiso 1 1 calc R U . . .
H15B H 0.552527 1.152701 0.148951 0.067 Uiso 1 1 calc R U . . .
H15C H 0.407158 1.111815 0.152349 0.067 Uiso 1 1 calc R U . . .
C16 C 0.2222(6) 1.0299(5) 0.3475(3) 0.0599(15) Uani 1 1 d . . . . .
H16A H 0.225697 1.105688 0.337269 0.090 Uiso 1 1 calc R U . . .
H16B H 0.287311 0.999596 0.383610 0.090 Uiso 1 1 calc R U . . .
H16C H 0.119454 1.032960 0.359078 0.090 Uiso 1 1 calc R U . . .
C17 C 0.2607(7) 0.7988(5) 0.2945(4) 0.085(3) Uani 1 1 d . . . . .
H17A H 0.290250 0.750102 0.256845 0.127 Uiso 1 1 calc R U . . .
H17B H 0.155350 0.809332 0.305513 0.127 Uiso 1 1 calc R U . . .
H17C H 0.322486 0.763956 0.330840 0.127 Uiso 1 1 calc R U . . .
Li17 Li 0.5628(8) 0.7209(7) 0.4696(3) 0.0379(16) Uani 1 1 d . . . . .
C18 C 0.1687(8) 1.0081(8) 0.2082(4) 0.100(2) Uani 1 1 d . . . . .
H18A H 0.200615 1.071588 0.192933 0.150 Uiso 1 1 calc R U . . .
H18B H 0.063901 1.035228 0.222765 0.150 Uiso 1 1 calc R U . . .
H18C H 0.179327 0.954259 0.173205 0.150 Uiso 1 1 calc R U . . .
C19 C 0.5577(5) 0.4422(4) 0.2294(2) 0.0423(10) Uani 1 1 d . . . . .
H19A H 0.509316 0.488215 0.193017 0.063 Uiso 1 1 calc R U . . .
H19B H 0.536273 0.487495 0.268558 0.063 Uiso 1 1 calc R U . . .
H19C H 0.519217 0.378063 0.234609 0.063 Uiso 1 1 calc R U . . .
C20 C 0.8528(5) 0.2912(4) 0.2798(2) 0.0419(10) Uani 1 1 d . . . . .
H20A H 0.814816 0.226481 0.279917 0.063 Uiso 1 1 calc R U . . .
H20B H 0.828720 0.329862 0.321167 0.063 Uiso 1 1 calc R U . . .
H20C H 0.961416 0.265356 0.272772 0.063 Uiso 1 1 calc R U . . .
C21 C 0.8025(7) 0.3105(4) 0.1363(2) 0.0520(13) Uani 1 1 d . . . . .
H21A H 0.755067 0.360392 0.101193 0.078 Uiso 1 1 calc R U . . .
H21B H 0.761981 0.247113 0.139102 0.078 Uiso 1 1 calc R U . . .
H21C H 0.910602 0.282262 0.128007 0.078 Uiso 1 1 calc R U . . .
C22 C 1.1664(5) 0.3603(4) 0.1955(3) 0.0510(13) Uani 1 1 d . . . . .
H22A H 1.139250 0.298611 0.175865 0.076 Uiso 1 1 calc R U . . .
H22B H 1.166289 0.351625 0.242299 0.076 Uiso 1 1 calc R U . . .
H22C H 1.266204 0.358827 0.180081 0.076 Uiso 1 1 calc R U . . .
C23 C 1.0988(5) 0.6129(4) 0.1998(2) 0.0437(10) Uani 1 1 d . . . . .
H23A H 1.196605 0.604403 0.179386 0.066 Uiso 1 1 calc R U . . .
H23B H 1.108535 0.609773 0.246582 0.066 Uiso 1 1 calc R U . . .
H23C H 1.028584 0.685409 0.187553 0.066 Uiso 1 1 calc R U . . .
C24 C 1.0166(6) 0.5043(6) 0.0840(3) 0.0703(13) Uani 1 1 d . . . . .
H24A H 1.116803 0.491713 0.065150 0.106 Uiso 1 1 calc R U . . .
H24B H 0.951846 0.578465 0.071213 0.106 Uiso 1 1 calc R U . . .
H24C H 0.975194 0.446358 0.068888 0.106 Uiso 1 1 calc R U . . .
C100_1 C -0.119(3) 0.8410(17) 0.0410(12) 0.088(7) Uani 0.5 1 d D U P A -1
H10A_1 H -0.186217 0.854884 0.004741 0.131 Uiso 0.5 1 calc R U P A -1
H10B_1 H -0.170996 0.826976 0.079833 0.131 Uiso 0.5 1 calc R U P A -1
H10C_1 H -0.031787 0.775399 0.031809 0.131 Uiso 0.5 1 calc R U P A -1
C101_1 C -0.0670(11) 0.9422(10) 0.0511(5) 0.055(2) Uani 0.5 1 d D U P A -1
H10D_1 H -0.152800 1.004988 0.066990 0.066 Uiso 0.5 1 calc R U P A -1
H10E_1 H 0.009378 0.924483 0.084706 0.066 Uiso 0.5 1 calc R U P A -1
C102_1 C -0.0023(15) 0.9798(8) -0.0086(5) 0.042(2) Uani 0.5 1 d D U P A -1
H10F_1 H 0.086636 0.918142 -0.022993 0.050 Uiso 0.5 1 calc R U P A -1
H10G_1 H -0.076761 0.992817 -0.042876 0.050 Uiso 0.5 1 calc R U P A -1
C103_1 C 0.0426(11) 1.0845(8) -0.0012(5) 0.051(2) Uani 0.5 1 d D U P A -1
H10H_1 H 0.118886 1.071219 0.032327 0.061 Uiso 0.5 1 calc R U P A -1
H10I_1 H -0.045684 1.146101 0.013888 0.061 Uiso 0.5 1 calc R U P A -1
C104_1 C 0.105(2) 1.1218(16) -0.0624(9) 0.075(5) Uani 0.5 1 d D U P A -1
H10J_1 H 0.033884 1.128201 -0.096998 0.112 Uiso 0.5 1 calc R U P A -1
H10K_1 H 0.200238 1.066355 -0.074170 0.112 Uiso 0.5 1 calc R U P A -1
H10L_1 H 0.119705 1.194841 -0.055417 0.112 Uiso 0.5 1 calc R U P A -1
C25 C 0.2396(8) 0.7186(6) 0.4815(4) 0.0704(17) Uani 1 1 d . . . . .
H25A H 0.269744 0.640739 0.498241 0.085 Uiso 1 1 calc R U . . .
H25B H 0.208743 0.718478 0.436402 0.085 Uiso 1 1 calc R U . . .
C26 C 0.1110(8) 0.7990(9) 0.5245(5) 0.114(3) Uani 1 1 d . . . . .
H26A H 0.027083 0.841326 0.497538 0.137 Uiso 1 1 calc R U . . .
H26B H 0.073059 0.754732 0.556488 0.137 Uiso 1 1 calc R U . . .
C27 C 0.1732(8) 0.8744(8) 0.5561(4) 0.100(2) Uani 1 1 d D . . . .
H27A H 0.101561 0.951245 0.556446 0.120 Uiso 1 1 calc R U . . .
H27B H 0.196225 0.850200 0.601071 0.120 Uiso 1 1 calc R U . . .
C28 C 0.3065(7) 0.8728(7) 0.5214(4) 0.096(3) Uani 1 1 d D . . . .
H28A H 0.384356 0.877900 0.551306 0.116 Uiso 1 1 calc R U . . .
H28B H 0.286587 0.936879 0.491135 0.116 Uiso 1 1 calc R U . . .
C29 C 0.6072(6) 0.5959(4) 0.5887(2) 0.0479(11) Uani 1 1 d . . . . .
H29A H 0.582189 0.541671 0.560223 0.057 Uiso 1 1 calc R U . . .
H29B H 0.518041 0.633353 0.615689 0.057 Uiso 1 1 calc R U . . .
C30 C 0.7345(9) 0.5368(5) 0.6297(3) 0.0709(18) Uani 1 1 d . . . . .
H30A H 0.725442 0.572361 0.672484 0.085 Uiso 1 1 calc R U . . .
H30B H 0.742403 0.456526 0.635109 0.085 Uiso 1 1 calc R U . . .
C31 C 0.8589(6) 0.5505(6) 0.5934(3) 0.0703(13) Uani 1 1 d . . . . .
H31A H 0.894274 0.489684 0.561294 0.084 Uiso 1 1 calc R U . . .
H31B H 0.942186 0.547494 0.622134 0.084 Uiso 1 1 calc R U . . .
C32 C 0.8070(6) 0.6641(5) 0.5598(3) 0.0530(12) Uani 1 1 d . . . . .
H32A H 0.820803 0.724397 0.587059 0.064 Uiso 1 1 calc R U . . .
H32B H 0.860627 0.662897 0.518248 0.064 Uiso 1 1 calc R U . . .
Pb1 Pb 0.81453(2) 0.69978(2) 0.32937(2) 0.02126(4) Uani 0.9688(4) 1 d . U P B 1
Br1 Br 0.67800(5) 0.55689(3) 0.39480(2) 0.03160(9) Uani 0.9688(4) 1 d . U P B 1
Br2 Br 0.66483(5) 0.86795(3) 0.42026(2) 0.03590(9) Uani 0.9688(4) 1 d . . P B 1
Pb2 Pb 0.8010(4) 0.6415(4) 0.30545(18) 0.02126(4) Uani 0.0312(4) 1 d D U P B 2
Br3 Br 0.579(3) 0.5837(17) 0.3777(6) 0.059(5) Uani 0.0312(4) 1 d . U P B 2
Br4 Br 0.6307(16) 0.8062(10) 0.4011(5) 0.03590(9) Uani 0.0312(4) 1 d D . P B 2


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Si1 C14 1.863(4) . ?
Si1 C15 1.866(5) . ?
Si1 C7 1.871(3) . ?
Si1 C13 1.872(4) . ?
O1 C25 1.409(7) . ?
O1 C28 1.450(7) . ?
O1 Li17 1.884(8) . ?
C1 C6 1.403(4) . ?
C1 C2 1.413(4) . ?
C1 Pb2 1.909(5) . ?
C1 Pb1 2.321(3) . ?
Si2 C16 1.859(5) . ?
Si2 C17 1.865(6) . ?
Si2 C18 1.867(10) . ?
Si2 C7 1.888(3) . ?
O2 C32 1.430(6) . ?
O2 C29 1.443(5) . ?
O2 Li17 1.911(8) . ?
C2 C3 1.402(4) . ?
C2 C7 1.515(4) . ?
Si3 C19 1.868(5) . ?
Si3 C20 1.872(4) . ?
Si3 C21 1.877(5) . ?
Si3 C8 1.898(4) . ?
C3 C4 1.392(5) . ?
C3 H3 0.9500 . ?
Si4 C24 1.862(6) . ?
Si4 C23 1.866(5) . ?
Si4 C22 1.869(5) . ?
Si4 C8 1.891(4) . ?
C4 C5 1.393(5) . ?
C4 C9 1.544(5) . ?
C5 C6 1.396(4) . ?
C5 H5 0.9500 . ?
C6 C8 1.529(4) . ?
C7 H7 1.0000 . ?
C8 H8 1.0000 . ?
C9 C12 1.513(6) . ?
C9 C10 1.516(7) . ?
C9 C11 1.539(7) . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
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 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
Li17 Br4 1.982(15) . ?
Li17 Br2 2.522(8) . ?
Li17 Br1 2.535(8) . ?
Li17 Br3 2.555(17) . ?
Li17 C28 2.772(9) . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C100_1 C101_1 1.507(13) . ?
C100_1 H10A_1 0.9800 . ?
C100_1 H10B_1 0.9800 . ?
C100_1 H10C_1 0.9800 . ?
C101_1 C102_1 1.506(12) . ?
C101_1 H10D_1 0.9900 . ?
C101_1 H10E_1 0.9900 . ?
C102_1 C103_1 1.505(11) . ?
C102_1 H10F_1 0.9900 . ?
C102_1 H10G_1 0.9900 . ?
C103_1 C104_1 1.517(13) . ?
C103_1 H10H_1 0.9900 . ?
C103_1 H10I_1 0.9900 . ?
C104_1 H10J_1 0.9800 . ?
C104_1 H10K_1 0.9800 . ?
C104_1 H10L_1 0.9800 . ?
C25 C26 1.580(11) . ?
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?
C26 C27 1.428(12) . ?
C26 H26A 0.9900 . ?
C26 H26B 0.9900 . ?
C27 C28 1.427(5) . ?
C27 H27A 0.9900 . ?
C27 H27B 0.9900 . ?
C28 H28A 0.9900 . ?
C28 H28B 0.9900 . ?
C29 C30 1.485(9) . ?
C29 H29A 0.9900 . ?
C29 H29B 0.9900 . ?
C30 C31 1.431(9) . ?
C30 H30A 0.9900 . ?
C30 H30B 0.9900 . ?
C31 C32 1.523(9) . ?
C31 H31A 0.9900 . ?
C31 H31B 0.9900 . ?
C32 H32A 0.9900 . ?
C32 H32B 0.9900 . ?
Pb1 Br1 2.8246(4) . ?
Pb1 Br2 2.8502(4) . ?
Pb2 Br3 2.812(17) . ?
Pb2 Br4 2.946(11) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C14 Si1 C15 108.9(2) . . ?
C14 Si1 C7 110.52(18) . . ?
C15 Si1 C7 113.64(19) . . ?
C14 Si1 C13 107.9(2) . . ?
C15 Si1 C13 108.2(2) . . ?
C7 Si1 C13 107.45(18) . . ?
C25 O1 C28 112.0(4) . . ?
C25 O1 Li17 135.5(4) . . ?
C28 O1 Li17 111.9(4) . . ?
C6 C1 C2 119.0(3) . . ?
C6 C1 Pb2 93.5(2) . . ?
C2 C1 Pb2 147.5(3) . . ?
C6 C1 Pb1 113.9(2) . . ?
C2 C1 Pb1 126.3(2) . . ?
C16 Si2 C17 108.3(3) . . ?
C16 Si2 C18 106.6(3) . . ?
C17 Si2 C18 110.8(4) . . ?
C16 Si2 C7 110.4(2) . . ?
C17 Si2 C7 107.1(2) . . ?
C18 Si2 C7 113.5(3) . . ?
C32 O2 C29 110.0(4) . . ?
C32 O2 Li17 121.0(4) . . ?
C29 O2 Li17 118.4(4) . . ?
C3 C2 C1 119.2(3) . . ?
C3 C2 C7 118.4(3) . . ?
C1 C2 C7 122.4(3) . . ?
C19 Si3 C20 109.0(2) . . ?
C19 Si3 C21 109.0(2) . . ?
C20 Si3 C21 108.1(2) . . ?
C19 Si3 C8 109.24(18) . . ?
C20 Si3 C8 108.10(18) . . ?
C21 Si3 C8 113.4(2) . . ?
C4 C3 C2 122.3(3) . . ?
C4 C3 H3 118.8 . . ?
C2 C3 H3 118.8 . . ?
C24 Si4 C23 107.8(3) . . ?
C24 Si4 C22 108.3(3) . . ?
C23 Si4 C22 108.4(2) . . ?
C24 Si4 C8 113.3(2) . . ?
C23 Si4 C8 108.62(17) . . ?
C22 Si4 C8 110.3(2) . . ?
C3 C4 C5 117.4(3) . . ?
C3 C4 C9 120.8(3) . . ?
C5 C4 C9 121.7(3) . . ?
C4 C5 C6 122.3(3) . . ?
C4 C5 H5 118.9 . . ?
C6 C5 H5 118.9 . . ?
C5 C6 C1 119.8(3) . . ?
C5 C6 C8 117.2(3) . . ?
C1 C6 C8 123.0(3) . . ?
C2 C7 Si1 111.8(2) . . ?
C2 C7 Si2 111.8(2) . . ?
Si1 C7 Si2 120.20(17) . . ?
C2 C7 H7 103.6 . . ?
Si1 C7 H7 103.6 . . ?
Si2 C7 H7 103.6 . . ?
C6 C8 Si4 111.6(2) . . ?
C6 C8 Si3 111.9(2) . . ?
Si4 C8 Si3 118.32(18) . . ?
C6 C8 H8 104.5 . . ?
Si4 C8 H8 104.5 . . ?
Si3 C8 H8 104.5 . . ?
C12 C9 C10 108.4(4) . . ?
C12 C9 C11 109.1(5) . . ?
C10 C9 C11 108.0(5) . . ?
C12 C9 C4 111.9(3) . . ?
C10 C9 C4 111.9(4) . . ?
C11 C9 C4 107.4(3) . . ?
C9 C10 H10A 109.5 . . ?
C9 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C9 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C9 C11 H11A 109.5 . . ?
C9 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C9 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C9 C12 H12A 109.5 . . ?
C9 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C9 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
Si1 C13 H13A 109.5 . . ?
Si1 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
Si1 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
Si1 C14 H14A 109.5 . . ?
Si1 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
Si1 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
Si1 C15 H15A 109.5 . . ?
Si1 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
Si1 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
Si2 C16 H16A 109.5 . . ?
Si2 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
Si2 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
Si2 C17 H17A 109.5 . . ?
Si2 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
Si2 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
O1 Li17 O2 105.2(4) . . ?
O1 Li17 Br4 115.3(6) . . ?
O2 Li17 Br4 126.8(6) . . ?
O1 Li17 Br2 115.5(4) . . ?
O2 Li17 Br2 108.8(3) . . ?
O1 Li17 Br1 119.8(4) . . ?
O2 Li17 Br1 106.2(3) . . ?
Br2 Li17 Br1 100.8(2) . . ?
O1 Li17 Br3 100.1(7) . . ?
O2 Li17 Br3 123.8(7) . . ?
Br4 Li17 Br3 82.3(5) . . ?
O1 Li17 C28 29.0(2) . . ?
O2 Li17 C28 94.1(3) . . ?
Br4 Li17 C28 104.6(5) . . ?
Br2 Li17 C28 95.3(3) . . ?
Br1 Li17 C28 148.2(3) . . ?
Br3 Li17 C28 127.1(7) . . ?
Si2 C18 H18A 109.5 . . ?
Si2 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
Si2 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
Si3 C19 H19A 109.5 . . ?
Si3 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
Si3 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
Si3 C20 H20A 109.5 . . ?
Si3 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
Si3 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
Si3 C21 H21A 109.5 . . ?
Si3 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
Si3 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
Si4 C22 H22A 109.5 . . ?
Si4 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
Si4 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
Si4 C23 H23A 109.5 . . ?
Si4 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
Si4 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
Si4 C24 H24A 109.5 . . ?
Si4 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
Si4 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C101_1 C100_1 H10A_1 109.5 . . ?
C101_1 C100_1 H10B_1 109.5 . . ?
H10A_1 C100_1 H10B_1 109.5 . . ?
C101_1 C100_1 H10C_1 109.5 . . ?
H10A_1 C100_1 H10C_1 109.5 . . ?
H10B_1 C100_1 H10C_1 109.5 . . ?
C102_1 C101_1 C100_1 113.6(12) . . ?
C102_1 C101_1 H10D_1 108.8 . . ?
C100_1 C101_1 H10D_1 108.8 . . ?
C102_1 C101_1 H10E_1 108.8 . . ?
C100_1 C101_1 H10E_1 108.8 . . ?
H10D_1 C101_1 H10E_1 107.7 . . ?
C103_1 C102_1 C101_1 115.0(8) . . ?
C103_1 C102_1 H10F_1 108.5 . . ?
C101_1 C102_1 H10F_1 108.5 . . ?
C103_1 C102_1 H10G_1 108.5 . . ?
C101_1 C102_1 H10G_1 108.5 . . ?
H10F_1 C102_1 H10G_1 107.5 . . ?
C102_1 C103_1 C104_1 113.9(11) . . ?
C102_1 C103_1 H10H_1 108.8 . . ?
C104_1 C103_1 H10H_1 108.8 . . ?
C102_1 C103_1 H10I_1 108.8 . . ?
C104_1 C103_1 H10I_1 108.8 . . ?
H10H_1 C103_1 H10I_1 107.7 . . ?
C103_1 C104_1 H10J_1 109.5 . . ?
C103_1 C104_1 H10K_1 109.5 . . ?
H10J_1 C104_1 H10K_1 109.5 . . ?
C103_1 C104_1 H10L_1 109.5 . . ?
H10J_1 C104_1 H10L_1 109.5 . . ?
H10K_1 C104_1 H10L_1 109.5 . . ?
O1 C25 C26 102.1(5) . . ?
O1 C25 H25A 111.4 . . ?
C26 C25 H25A 111.4 . . ?
O1 C25 H25B 111.4 . . ?
C26 C25 H25B 111.4 . . ?
H25A C25 H25B 109.2 . . ?
C27 C26 C25 107.3(5) . . ?
C27 C26 H26A 110.2 . . ?
C25 C26 H26A 110.2 . . ?
C27 C26 H26B 110.2 . . ?
C25 C26 H26B 110.2 . . ?
H26A C26 H26B 108.5 . . ?
C28 C27 C26 107.2(7) . . ?
C28 C27 H27A 110.3 . . ?
C26 C27 H27A 110.3 . . ?
C28 C27 H27B 110.3 . . ?
C26 C27 H27B 110.3 . . ?
H27A C27 H27B 108.5 . . ?
C27 C28 O1 106.6(6) . . ?
C27 C28 Li17 140.1(6) . . ?
O1 C28 Li17 39.1(3) . . ?
C27 C28 H28A 110.4 . . ?
O1 C28 H28A 110.4 . . ?
Li17 C28 H28A 77.4 . . ?
C27 C28 H28B 110.4 . . ?
O1 C28 H28B 110.4 . . ?
Li17 C28 H28B 103.1 . . ?
H28A C28 H28B 108.6 . . ?
O2 C29 C30 107.4(5) . . ?
O2 C29 H29A 110.2 . . ?
C30 C29 H29A 110.2 . . ?
O2 C29 H29B 110.2 . . ?
C30 C29 H29B 110.2 . . ?
H29A C29 H29B 108.5 . . ?
C31 C30 C29 101.8(5) . . ?
C31 C30 H30A 111.4 . . ?
C29 C30 H30A 111.4 . . ?
C31 C30 H30B 111.4 . . ?
C29 C30 H30B 111.4 . . ?
H30A C30 H30B 109.3 . . ?
C30 C31 C32 107.7(5) . . ?
C30 C31 H31A 110.2 . . ?
C32 C31 H31A 110.2 . . ?
C30 C31 H31B 110.2 . . ?
C32 C31 H31B 110.2 . . ?
H31A C31 H31B 108.5 . . ?
O2 C32 C31 101.9(4) . . ?
O2 C32 H32A 111.4 . . ?
C31 C32 H32A 111.4 . . ?
O2 C32 H32B 111.4 . . ?
C31 C32 H32B 111.4 . . ?
H32A C32 H32B 109.3 . . ?
C1 Pb1 Br1 94.57(8) . . ?
C1 Pb1 Br2 110.37(8) . . ?
Br1 Pb1 Br2 86.740(13) . . ?
Li17 Br1 Pb1 86.37(17) . . ?
Li17 Br2 Pb1 86.07(17) . . ?
C1 Pb2 Br3 95.8(5) . . ?
C1 Pb2 Br4 92.1(3) . . ?
Br3 Pb2 Br4 63.1(5) . . ?
Li17 Br3 Pb2 96.3(6) . . ?
Li17 Br4 Pb2 107.0(5) . . ?

_refine_diff_density_max         2.728
_refine_diff_density_min         -2.238
_refine_diff_density_rms         0.129



####################################################################### 
# 
# 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_ma27_0m_a
_database_code_depnum_ccdc_archive 'CCDC 2153539'
loop_
_audit_author_name
_audit_author_address
'Hartmut Schubert'
;Universtity of Tuebingen
Germany
;
_audit_update_record             
;
2022-02-21 deposited with the CCDC.	2022-03-22 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/1
_shelx_SHELXL_version_number     2018/1
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C35 H72 Br2 Li O2 Si4 Sn'
_chemical_formula_weight         922.73

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'
Li Li -0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 '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'
Br Br -0.2901 2.4595 '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'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_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'

_cell_length_a                   9.4333(3)
_cell_length_b                   12.6264(4)
_cell_length_c                   20.6027(6)
_cell_angle_alpha                89.2150(10)
_cell_angle_beta                 89.8210(10)
_cell_angle_gamma                71.5940(10)
_cell_volume                     2328.20(13)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9772
_cell_measurement_theta_min      2.37
_cell_measurement_theta_max      27.25

_exptl_crystal_description       prism
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.316
_exptl_crystal_F_000             954
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.17
_exptl_absorpt_coefficient_mu    2.394
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6413
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_process_details   'SADABS V2008/1 (Bruker AXS)'
_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            62977
_diffrn_reflns_av_unetI/netI     0.0182
_diffrn_reflns_av_R_equivalents  0.0215
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_theta_min         2.966
_diffrn_reflns_theta_max         27.266
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             10379
_reflns_number_gt                9250
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_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       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXT 2014/4 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2018/1 (Sheldrick, 2018)'
_computing_molecular_graphics    ?
_computing_publication_material  Platon,Wingx,Shelxle,DSR
_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)+(0.0378P)²+4.1710P] 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_number_reflns         10379
_refine_ls_number_parameters     438
_refine_ls_number_restraints     184
_refine_ls_R_factor_all          0.0359
_refine_ls_R_factor_gt           0.0298
_refine_ls_wR_factor_ref         0.0792
_refine_ls_wR_factor_gt          0.0761
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_restrained_S_all      1.021
_refine_ls_shift/su_max          0.007
_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
C1 C 0.4957(3) 0.80726(19) 0.84318(11) 0.0154(4) Uani 1 1 d . . . . .
H1 H 0.421957 0.872946 0.857685 0.018 Uiso 1 1 calc R U . . .
C2 C 0.5432(3) 0.71594(19) 0.88561(11) 0.0141(4) Uani 1 1 d . . . . .
C3 C 0.5517(2) 0.80652(18) 0.78041(11) 0.0128(4) Uani 1 1 d . . . . .
C4 C 0.6523(3) 0.62131(19) 0.86248(11) 0.0144(4) Uani 1 1 d . . . . .
H4 H 0.686133 0.557294 0.890003 0.017 Uiso 1 1 calc R U . . .
C5 C 0.4701(3) 0.7172(2) 0.95215(11) 0.0168(5) Uani 1 1 d . . . . .
C6 C 0.4182(3) 0.8344(2) 0.98103(13) 0.0268(6) Uani 1 1 d . . . . .
H6A H 0.503240 0.862943 0.983865 0.040 Uiso 1 1 calc R U . . .
H6B H 0.377380 0.830996 1.024526 0.040 Uiso 1 1 calc R U . . .
H6C H 0.340834 0.884170 0.953166 0.040 Uiso 1 1 calc R U . . .
C7 C 0.9784(3) 0.9473(2) 1.00426(14) 0.0264(6) Uani 1 1 d . . . . .
H7A H 0.906791 0.957661 1.040667 0.032 Uiso 1 1 calc R U . . .
H7B H 1.068710 0.884752 1.016151 0.032 Uiso 1 1 calc R U . . .
C8 C 0.4880(4) 1.1464(2) 0.70341(15) 0.0311(6) Uani 1 1 d . . . . .
H8A H 0.544135 1.198893 0.709634 0.047 Uiso 1 1 calc R U . . .
H8B H 0.381503 1.184612 0.710780 0.047 Uiso 1 1 calc R U . . .
H8C H 0.502759 1.118238 0.658984 0.047 Uiso 1 1 calc R U . . .
C9 C 0.4855(2) 0.90955(18) 0.73806(11) 0.0136(4) Uani 1 1 d . . . . .
H9 H 0.531841 0.887141 0.694580 0.016 Uiso 1 1 calc R U . . .
C10 C 0.8400(4) 0.2920(2) 0.71317(14) 0.0304(6) Uani 1 1 d . . . . .
H10A H 0.805515 0.226456 0.713961 0.046 Uiso 1 1 calc R U . . .
H10B H 0.948843 0.267997 0.718298 0.046 Uiso 1 1 calc R U . . .
H10C H 0.812456 0.331951 0.671659 0.046 Uiso 1 1 calc R U . . .
C11 C 0.6646(2) 0.71084(18) 0.75789(11) 0.0122(4) Uani 1 1 d . . . . .
C12 C 0.9992(3) 0.4814(3) 0.91496(14) 0.0333(7) Uani 1 1 d . . . . .
H12A H 0.963321 0.419396 0.928055 0.050 Uiso 1 1 calc R U . . .
H12B H 0.928701 0.551831 0.929886 0.050 Uiso 1 1 calc R U . . .
H12C H 1.097504 0.470748 0.934347 0.050 Uiso 1 1 calc R U . . .
C13 C 0.7134(2) 0.61722(18) 0.80047(11) 0.0134(4) Uani 1 1 d . . . . .
C14 C 0.5768(3) 0.6395(2) 1.00103(13) 0.0281(6) Uani 1 1 d . . . . .
H14A H 0.602848 0.562306 0.986213 0.042 Uiso 1 1 calc R U . . .
H14B H 0.528171 0.645740 1.043535 0.042 Uiso 1 1 calc R U . . .
H14C H 0.667777 0.660806 1.004611 0.042 Uiso 1 1 calc R U . . .
C15 C 1.0877(3) 0.6022(2) 0.80199(15) 0.0305(6) Uani 1 1 d . . . . .
H15A H 1.182908 0.591747 0.824222 0.046 Uiso 1 1 calc R U . . .
H15B H 1.015565 0.673437 0.814890 0.046 Uiso 1 1 calc R U . . .
H15C H 1.102955 0.602761 0.754934 0.046 Uiso 1 1 calc R U . . .
C16 C 0.8299(3) 0.50788(18) 0.78120(11) 0.0148(4) Uani 1 1 d . . . . .
H16 H 0.851907 0.519088 0.734563 0.018 Uiso 1 1 calc R U . . .
C17 C 0.5012(4) 1.0785(2) 0.84631(14) 0.0313(6) Uani 1 1 d . . . . .
H17A H 0.533725 1.143620 0.854290 0.047 Uiso 1 1 calc R U . . .
H17B H 0.548713 1.019259 0.877875 0.047 Uiso 1 1 calc R U . . .
H17C H 0.392373 1.099634 0.850779 0.047 Uiso 1 1 calc R U . . .
C18 C 0.3324(3) 0.6779(3) 0.94271(14) 0.0286(6) Uani 1 1 d . . . . .
H18A H 0.263539 0.727830 0.911717 0.043 Uiso 1 1 calc R U . . .
H18B H 0.281775 0.679189 0.984436 0.043 Uiso 1 1 calc R U . . .
H18C H 0.364532 0.601701 0.925983 0.043 Uiso 1 1 calc R U . . .
C19 C 0.5446(3) 0.4409(3) 0.76810(16) 0.0322(6) Uani 1 1 d . . . . .
H19A H 0.505702 0.378183 0.762950 0.048 Uiso 1 1 calc R U . . .
H19B H 0.522953 0.488122 0.728890 0.048 Uiso 1 1 calc R U . . .
H19C H 0.496996 0.485034 0.805599 0.048 Uiso 1 1 calc R U . . .
C20 C 1.1524(3) 0.3506(3) 0.79839(17) 0.0380(7) Uani 1 1 d . . . . .
H20A H 1.251337 0.344441 0.815781 0.057 Uiso 1 1 calc R U . . .
H20B H 1.156801 0.348766 0.750877 0.057 Uiso 1 1 calc R U . . .
H20C H 1.121357 0.288109 0.814744 0.057 Uiso 1 1 calc R U . . .
C21 C 0.9087(3) 0.9159(3) 0.94411(16) 0.0349(7) Uani 1 1 d . . . . .
H21A H 0.818919 0.978593 0.931904 0.042 Uiso 1 1 calc R U . . .
H21B H 0.980712 0.904513 0.907782 0.042 Uiso 1 1 calc R U . . .
C22 C 0.7868(4) 0.3016(2) 0.85840(15) 0.0346(7) Uani 1 1 d . . . . .
H22A H 0.742200 0.349597 0.894954 0.052 Uiso 1 1 calc R U . . .
H22B H 0.894737 0.269452 0.865247 0.052 Uiso 1 1 calc R U . . .
H22C H 0.742226 0.241489 0.855299 0.052 Uiso 1 1 calc R U . . .
C23 C 0.6027(4) 0.6001(3) 0.41227(16) 0.0384(7) Uani 1 1 d . . . . .
H23A H 0.515465 0.636732 0.384221 0.046 Uiso 1 1 calc R U . . .
H23B H 0.575278 0.548565 0.442808 0.046 Uiso 1 1 calc R U . . .
C24 C 0.2207(4) 1.0269(4) 0.64945(19) 0.0549(11) Uani 1 1 d . . . . .
H24A H 0.121670 1.026211 0.635669 0.082 Uiso 1 1 calc R U . . .
H24B H 0.292829 0.998155 0.614510 0.082 Uiso 1 1 calc R U . . .
H24C H 0.216763 1.103450 0.659301 0.082 Uiso 1 1 calc R U . . .
C25 C 0.8040(4) 0.6639(3) 0.43822(18) 0.0426(8) Uani 1 1 d . . . . .
H25A H 0.853818 0.667601 0.479957 0.051 Uiso 1 1 calc R U . . .
H25B H 0.821162 0.719744 0.407621 0.051 Uiso 1 1 calc R U . . .
C26 C 0.1570(3) 1.0097(4) 0.79131(18) 0.0480(9) Uani 1 1 d . . . . .
H26A H 0.052067 1.029228 0.778107 0.072 Uiso 1 1 calc R U . . .
H26B H 0.180339 1.077744 0.801963 0.072 Uiso 1 1 calc R U . . .
H26C H 0.174378 0.960105 0.829513 0.072 Uiso 1 1 calc R U . . .
C27 C 0.7338(5) 0.5377(4) 0.3719(2) 0.0606(8) Uani 1 1 d . . . . .
H27A H 0.739496 0.458503 0.367361 0.073 Uiso 1 1 calc R U . . .
H27B H 0.730130 0.572248 0.328294 0.073 Uiso 1 1 calc R U . . .
C28 C 0.7650(3) 0.9749(3) 0.75811(18) 0.0370(7) Uani 1 1 d . . . . .
H28A H 0.796335 0.956550 0.713141 0.055 Uiso 1 1 calc R U . . .
H28B H 0.802862 0.907917 0.785600 0.055 Uiso 1 1 calc R U . . .
H28C H 0.805076 1.032837 0.773430 0.055 Uiso 1 1 calc R U . . .
C29 C 0.2499(4) 0.8004(3) 0.7088(2) 0.0579(11) Uani 1 1 d . . . . .
H29A H 0.268617 0.755853 0.749022 0.087 Uiso 1 1 calc R U . . .
H29B H 0.318804 0.760362 0.675035 0.087 Uiso 1 1 calc R U . . .
H29C H 0.146741 0.813018 0.694616 0.087 Uiso 1 1 calc R U . . .
C31 C 0.8646(4) 0.8111(3) 0.9535(2) 0.0559(11) Uani 1 1 d . . . . .
H31A H 0.953779 0.747736 0.963378 0.084 Uiso 1 1 calc R U . . .
H31B H 0.818002 0.796245 0.913647 0.084 Uiso 1 1 calc R U . . .
H31C H 0.793558 0.821528 0.989481 0.084 Uiso 1 1 calc R U . . .
C33 C 0.8605(4) 0.5486(4) 0.4106(2) 0.0583(8) Uani 1 1 d . . . . .
H33A H 0.948931 0.540472 0.382796 0.070 Uiso 1 1 calc R U . . .
H33B H 0.887862 0.491439 0.445724 0.070 Uiso 1 1 calc R U . . .
Li1 Li 0.5537(5) 0.7282(4) 0.5290(2) 0.0308(10) Uani 1 1 d . . . . .
O2 O 0.6470(2) 0.68253(18) 0.44747(10) 0.0309(4) Uani 1 1 d . . . . .
Si1 Si 0.27954(8) 0.93703(6) 0.72332(3) 0.02006(14) Uani 1 1 d . . . . .
Si2 Si 0.55607(8) 1.02701(5) 0.76225(3) 0.01873(14) Uani 1 1 d . . . . .
Si3 Si 0.75062(8) 0.38666(6) 0.78117(3) 0.02055(14) Uani 1 1 d . . . . .
Si4 Si 1.01429(8) 0.48552(6) 0.82475(4) 0.02117(15) Uani 1 1 d . . . . .
Br1 Br 0.66544(3) 0.56469(2) 0.60612(2) 0.02927(7) Uani 1 1 d . . . . .
Br2 Br 0.66491(4) 0.86267(2) 0.58063(2) 0.03144(7) Uani 1 1 d . . . . .
Sn1 Sn 0.80225(2) 0.69507(2) 0.66831(2) 0.01658(5) Uani 1 1 d . . . . .
O1_1 O 0.3442(8) 0.7786(10) 0.5160(7) 0.0346(19) Uani 0.712(5) 1 d D U P A 1
C1_1 C 0.2298(8) 0.7252(6) 0.5137(4) 0.0490(18) Uani 0.712(5) 1 d D U P A 1
H1A_1 H 0.193881 0.715262 0.557808 0.059 Uiso 0.712(5) 1 calc R U P A 1
H1AB_1 H 0.267736 0.651411 0.492824 0.059 Uiso 0.712(5) 1 calc R U P A 1
C2_1 C 0.1050(6) 0.8058(5) 0.4729(3) 0.0583(8) Uani 0.712(5) 1 d D U P A 1
H2A_1 H 0.062630 0.764840 0.441797 0.070 Uiso 0.712(5) 1 calc R U P A 1
H2AB_1 H 0.023854 0.851660 0.500919 0.070 Uiso 0.712(5) 1 calc R U P A 1
C3_1 C 0.1830(7) 0.8772(5) 0.4380(3) 0.0606(8) Uani 0.712(5) 1 d D U P A 1
H3A_1 H 0.227801 0.842065 0.396935 0.073 Uiso 0.712(5) 1 calc R U P A 1
H3AB_1 H 0.112232 0.952145 0.428010 0.073 Uiso 0.712(5) 1 calc R U P A 1
C4_1 C 0.2949(7) 0.8845(5) 0.4815(3) 0.0531(15) Uani 0.712(5) 1 d D U P A 1
H4A_1 H 0.253980 0.946470 0.512101 0.064 Uiso 0.712(5) 1 calc R U P A 1
H4AB_1 H 0.379059 0.897638 0.457501 0.064 Uiso 0.712(5) 1 calc R U P A 1
O1_2 O 0.355(2) 0.762(3) 0.5078(19) 0.045(6) Uani 0.288(5) 1 d D U P A 2
C1_2 C 0.2505(18) 0.7137(17) 0.5360(11) 0.059(5) Uani 0.288(5) 1 d D U P A 2
H1A_2 H 0.262318 0.706735 0.583779 0.071 Uiso 0.288(5) 1 calc R U P A 2
H1AB_2 H 0.263544 0.638905 0.517973 0.071 Uiso 0.288(5) 1 calc R U P A 2
C2_2 C 0.0997(15) 0.7946(11) 0.5177(8) 0.0606(8) Uani 0.288(5) 1 d D U P A 2
H2A_2 H 0.041407 0.823217 0.557335 0.073 Uiso 0.288(5) 1 calc R U P A 2
H2AB_2 H 0.043299 0.756313 0.491494 0.073 Uiso 0.288(5) 1 calc R U P A 2
C3_2 C 0.1228(13) 0.8907(12) 0.4788(7) 0.0583(8) Uani 0.288(5) 1 d D U P A 2
H3A_2 H 0.058151 0.908095 0.439784 0.070 Uiso 0.288(5) 1 calc R U P A 2
H3AB_2 H 0.102255 0.958610 0.505417 0.070 Uiso 0.288(5) 1 calc R U P A 2
C4_2 C 0.2856(13) 0.8463(12) 0.4605(7) 0.0426(8) Uani 0.288(5) 1 d D U P A 2
H4A_2 H 0.296900 0.814078 0.416547 0.051 Uiso 0.288(5) 1 calc R U P A 2
H4AB_2 H 0.331390 0.906893 0.460913 0.051 Uiso 0.288(5) 1 calc R U P A 2


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C2 1.394(3) . ?
C1 C3 1.394(3) . ?
C1 H1 0.9500 . ?
C2 C4 1.396(3) . ?
C2 C5 1.531(3) . ?
C3 C11 1.417(3) . ?
C3 C9 1.518(3) . ?
C4 C13 1.395(3) . ?
C4 H4 0.9500 . ?
C5 C14 1.531(3) . ?
C5 C6 1.532(3) . ?
C5 C18 1.543(4) . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C7 C7 1.518(5) 2_777 ?
C7 C21 1.519(4) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 Si2 1.870(3) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 Si2 1.881(2) . ?
C9 Si1 1.887(2) . ?
C9 H9 1.0000 . ?
C10 Si3 1.872(3) . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 C13 1.417(3) . ?
C11 Sn1 2.228(2) . ?
C12 Si4 1.865(3) . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 C16 1.525(3) . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 Si4 1.869(3) . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 Si4 1.898(2) . ?
C16 Si3 1.904(2) . ?
C16 H16 1.0000 . ?
C17 Si2 1.872(3) . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 Si3 1.864(3) . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C20 Si4 1.874(3) . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 C31 1.517(5) . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C22 Si3 1.878(3) . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 O2 1.442(4) . ?
C23 C27 1.496(6) . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C24 Si1 1.863(3) . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C25 O2 1.437(4) . ?
C25 C33 1.502(5) . ?
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?
C26 Si1 1.870(3) . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C27 C33 1.481(6) . ?
C27 H27A 0.9900 . ?
C27 H27B 0.9900 . ?
C28 Si2 1.872(3) . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C29 Si1 1.861(3) . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
C33 H33A 0.9900 . ?
C33 H33B 0.9900 . ?
Li1 O1_2 1.836(19) . ?
Li1 O1_1 1.895(8) . ?
Li1 O2 1.905(5) . ?
Li1 Br2 2.509(5) . ?
Li1 Br1 2.538(5) . ?
Li1 C4_1 2.781(7) . ?
Br1 Sn1 2.7253(3) . ?
Br2 Sn1 2.7566(3) . ?
O1_1 C1_1 1.442(9) . ?
O1_1 C4_1 1.447(7) . ?
C1_1 C2_1 1.534(8) . ?
C1_1 H1A_1 0.9900 . ?
C1_1 H1AB_1 0.9900 . ?
C2_1 C3_1 1.506(8) . ?
C2_1 H2A_1 0.9900 . ?
C2_1 H2AB_1 0.9900 . ?
C3_1 C4_1 1.413(8) . ?
C3_1 H3A_1 0.9900 . ?
C3_1 H3AB_1 0.9900 . ?
C4_1 H4A_1 0.9900 . ?
C4_1 H4AB_1 0.9900 . ?
O1_2 C4_2 1.430(13) . ?
O1_2 C1_2 1.436(14) . ?
C1_2 C2_2 1.512(13) . ?
C1_2 H1A_2 0.9900 . ?
C1_2 H1AB_2 0.9900 . ?
C2_2 C3_2 1.517(13) . ?
C2_2 H2A_2 0.9900 . ?
C2_2 H2AB_2 0.9900 . ?
C3_2 C4_2 1.508(12) . ?
C3_2 H3A_2 0.9900 . ?
C3_2 H3AB_2 0.9900 . ?
C4_2 H4A_2 0.9900 . ?
C4_2 H4AB_2 0.9900 . ?

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 C1 C3 122.9(2) . . ?
C2 C1 H1 118.5 . . ?
C3 C1 H1 118.5 . . ?
C1 C2 C4 116.7(2) . . ?
C1 C2 C5 121.1(2) . . ?
C4 C2 C5 122.0(2) . . ?
C1 C3 C11 119.9(2) . . ?
C1 C3 C9 117.7(2) . . ?
C11 C3 C9 122.4(2) . . ?
C13 C4 C2 122.5(2) . . ?
C13 C4 H4 118.8 . . ?
C2 C4 H4 118.8 . . ?
C2 C5 C14 111.8(2) . . ?
C2 C5 C6 111.9(2) . . ?
C14 C5 C6 107.6(2) . . ?
C2 C5 C18 107.5(2) . . ?
C14 C5 C18 109.3(2) . . ?
C6 C5 C18 108.6(2) . . ?
C5 C6 H6A 109.5 . . ?
C5 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
C5 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C7 C7 C21 113.7(3) 2_777 . ?
C7 C7 H7A 108.8 2_777 . ?
C21 C7 H7A 108.8 . . ?
C7 C7 H7B 108.8 2_777 . ?
C21 C7 H7B 108.8 . . ?
H7A C7 H7B 107.7 . . ?
Si2 C8 H8A 109.5 . . ?
Si2 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
Si2 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C3 C9 Si2 111.55(15) . . ?
C3 C9 Si1 111.71(15) . . ?
Si2 C9 Si1 120.00(12) . . ?
C3 C9 H9 103.9 . . ?
Si2 C9 H9 103.9 . . ?
Si1 C9 H9 103.9 . . ?
Si3 C10 H10A 109.5 . . ?
Si3 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
Si3 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C3 C11 C13 117.7(2) . . ?
C3 C11 Sn1 127.94(16) . . ?
C13 C11 Sn1 113.72(15) . . ?
Si4 C12 H12A 109.5 . . ?
Si4 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
Si4 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C4 C13 C11 120.3(2) . . ?
C4 C13 C16 116.9(2) . . ?
C11 C13 C16 122.8(2) . . ?
C5 C14 H14A 109.5 . . ?
C5 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C5 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 . . ?
C13 C16 Si4 111.78(16) . . ?
C13 C16 Si3 112.18(16) . . ?
Si4 C16 Si3 117.42(12) . . ?
C13 C16 H16 104.7 . . ?
Si4 C16 H16 104.7 . . ?
Si3 C16 H16 104.7 . . ?
Si2 C17 H17A 109.5 . . ?
Si2 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
Si2 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C5 C18 H18A 109.5 . . ?
C5 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C5 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
Si3 C19 H19A 109.5 . . ?
Si3 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
Si3 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
Si4 C20 H20A 109.5 . . ?
Si4 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
Si4 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C31 C21 C7 113.2(3) . . ?
C31 C21 H21A 108.9 . . ?
C7 C21 H21A 108.9 . . ?
C31 C21 H21B 108.9 . . ?
C7 C21 H21B 108.9 . . ?
H21A C21 H21B 107.8 . . ?
Si3 C22 H22A 109.5 . . ?
Si3 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
Si3 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
O2 C23 C27 106.7(3) . . ?
O2 C23 H23A 110.4 . . ?
C27 C23 H23A 110.4 . . ?
O2 C23 H23B 110.4 . . ?
C27 C23 H23B 110.4 . . ?
H23A C23 H23B 108.6 . . ?
Si1 C24 H24A 109.5 . . ?
Si1 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
Si1 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
O2 C25 C33 104.0(3) . . ?
O2 C25 H25A 111.0 . . ?
C33 C25 H25A 111.0 . . ?
O2 C25 H25B 111.0 . . ?
C33 C25 H25B 111.0 . . ?
H25A C25 H25B 109.0 . . ?
Si1 C26 H26A 109.5 . . ?
Si1 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
Si1 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C33 C27 C23 101.8(3) . . ?
C33 C27 H27A 111.4 . . ?
C23 C27 H27A 111.4 . . ?
C33 C27 H27B 111.4 . . ?
C23 C27 H27B 111.4 . . ?
H27A C27 H27B 109.3 . . ?
Si2 C28 H28A 109.5 . . ?
Si2 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
Si2 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
Si1 C29 H29A 109.5 . . ?
Si1 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
Si1 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C21 C31 H31A 109.5 . . ?
C21 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
C21 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C27 C33 C25 104.6(3) . . ?
C27 C33 H33A 110.8 . . ?
C25 C33 H33A 110.8 . . ?
C27 C33 H33B 110.8 . . ?
C25 C33 H33B 110.8 . . ?
H33A C33 H33B 108.9 . . ?
O1_2 Li1 O2 101.5(14) . . ?
O1_1 Li1 O2 108.1(5) . . ?
O1_2 Li1 Br2 123.9(14) . . ?
O1_1 Li1 Br2 116.7(5) . . ?
O2 Li1 Br2 109.7(2) . . ?
O1_2 Li1 Br1 117.9(6) . . ?
O1_1 Li1 Br1 118.7(3) . . ?
O2 Li1 Br1 105.4(2) . . ?
Br2 Li1 Br1 97.36(17) . . ?
O1_1 Li1 C4_1 28.8(3) . . ?
O2 Li1 C4_1 97.3(2) . . ?
Br2 Li1 C4_1 97.5(2) . . ?
Br1 Li1 C4_1 146.7(2) . . ?
C25 O2 C23 109.4(2) . . ?
C25 O2 Li1 121.3(2) . . ?
C23 O2 Li1 117.5(2) . . ?
C29 Si1 C24 108.7(2) . . ?
C29 Si1 C26 109.6(2) . . ?
C24 Si1 C26 107.02(19) . . ?
C29 Si1 C9 107.75(14) . . ?
C24 Si1 C9 109.52(13) . . ?
C26 Si1 C9 114.17(13) . . ?
C8 Si2 C17 109.03(14) . . ?
C8 Si2 C28 107.98(15) . . ?
C17 Si2 C28 108.11(15) . . ?
C8 Si2 C9 109.99(12) . . ?
C17 Si2 C9 113.78(12) . . ?
C28 Si2 C9 107.76(12) . . ?
C19 Si3 C10 109.51(14) . . ?
C19 Si3 C22 108.06(15) . . ?
C10 Si3 C22 107.82(14) . . ?
C19 Si3 C16 109.56(12) . . ?
C10 Si3 C16 108.10(12) . . ?
C22 Si3 C16 113.73(13) . . ?
C12 Si4 C15 108.10(15) . . ?
C12 Si4 C20 108.10(15) . . ?
C15 Si4 C20 108.69(15) . . ?
C12 Si4 C16 113.65(12) . . ?
C15 Si4 C16 108.64(11) . . ?
C20 Si4 C16 109.55(13) . . ?
Li1 Br1 Sn1 87.62(12) . . ?
Li1 Br2 Sn1 87.52(11) . . ?
C11 Sn1 Br1 94.44(6) . . ?
C11 Sn1 Br2 110.30(6) . . ?
Br1 Sn1 Br2 87.481(10) . . ?
C1_1 O1_1 C4_1 110.0(5) . . ?
C1_1 O1_1 Li1 134.8(7) . . ?
C4_1 O1_1 Li1 112.0(5) . . ?
O1_1 C1_1 C2_1 104.1(5) . . ?
O1_1 C1_1 H1A_1 110.9 . . ?
C2_1 C1_1 H1A_1 110.9 . . ?
O1_1 C1_1 H1AB_1 110.9 . . ?
C2_1 C1_1 H1AB_1 110.9 . . ?
H1A_1 C1_1 H1AB_1 109.0 . . ?
C3_1 C2_1 C1_1 103.4(5) . . ?
C3_1 C2_1 H2A_1 111.1 . . ?
C1_1 C2_1 H2A_1 111.1 . . ?
C3_1 C2_1 H2AB_1 111.1 . . ?
C1_1 C2_1 H2AB_1 111.1 . . ?
H2A_1 C2_1 H2AB_1 109.0 . . ?
C4_1 C3_1 C2_1 104.9(5) . . ?
C4_1 C3_1 H3A_1 110.8 . . ?
C2_1 C3_1 H3A_1 110.8 . . ?
C4_1 C3_1 H3AB_1 110.8 . . ?
C2_1 C3_1 H3AB_1 110.8 . . ?
H3A_1 C3_1 H3AB_1 108.8 . . ?
C3_1 C4_1 O1_1 105.9(7) . . ?
C3_1 C4_1 Li1 132.9(5) . . ?
O1_1 C4_1 Li1 39.2(3) . . ?
C3_1 C4_1 H4A_1 110.6 . . ?
O1_1 C4_1 H4A_1 110.6 . . ?
Li1 C4_1 H4A_1 111.9 . . ?
C3_1 C4_1 H4AB_1 110.6 . . ?
O1_1 C4_1 H4AB_1 110.6 . . ?
Li1 C4_1 H4AB_1 73.7 . . ?
H4A_1 C4_1 H4AB_1 108.7 . . ?
C4_2 O1_2 C1_2 111.5(13) . . ?
C4_2 O1_2 Li1 122.0(13) . . ?
C1_2 O1_2 Li1 126.5(12) . . ?
O1_2 C1_2 C2_2 104.0(12) . . ?
O1_2 C1_2 H1A_2 111.0 . . ?
C2_2 C1_2 H1A_2 111.0 . . ?
O1_2 C1_2 H1AB_2 111.0 . . ?
C2_2 C1_2 H1AB_2 111.0 . . ?
H1A_2 C1_2 H1AB_2 109.0 . . ?
C1_2 C2_2 C3_2 109.0(10) . . ?
C1_2 C2_2 H2A_2 109.9 . . ?
C3_2 C2_2 H2A_2 109.9 . . ?
C1_2 C2_2 H2AB_2 109.9 . . ?
C3_2 C2_2 H2AB_2 109.9 . . ?
H2A_2 C2_2 H2AB_2 108.3 . . ?
C4_2 C3_2 C2_2 102.7(9) . . ?
C4_2 C3_2 H3A_2 111.2 . . ?
C2_2 C3_2 H3A_2 111.2 . . ?
C4_2 C3_2 H3AB_2 111.2 . . ?
C2_2 C3_2 H3AB_2 111.2 . . ?
H3A_2 C3_2 H3AB_2 109.1 . . ?
O1_2 C4_2 C3_2 106.4(13) . . ?
O1_2 C4_2 H4A_2 110.4 . . ?
C3_2 C4_2 H4A_2 110.4 . . ?
O1_2 C4_2 H4AB_2 110.4 . . ?
C3_2 C4_2 H4AB_2 110.4 . . ?
H4A_2 C4_2 H4AB_2 108.6 . . ?

_refine_diff_density_max         1.219
_refine_diff_density_min         -1.381
_refine_diff_density_rms         0.083



####################################################################### 
# 
# 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_shelx_CCDC2
_database_code_depnum_ccdc_archive 'CCDC 2153561'
loop_
_audit_author_name
_audit_author_address
'Hartmut Schubert'
;Universtity of Tuebingen
Germany
;
_audit_update_record             
;
2022-02-21 deposited with the CCDC.	2022-03-22 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/1
_shelx_SHELXL_version_number     2018/1
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C24 H52 Si4 Sn'
_chemical_formula_weight         571.73

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'
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'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

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

_cell_length_a                   16.6242(4)
_cell_length_b                   9.1360(2)
_cell_length_c                   21.6779(5)
_cell_angle_alpha                90
_cell_angle_beta                 101.7770(10)
_cell_angle_gamma                90
_cell_volume                     3223.10(13)
_cell_formula_units_Z            4
_cell_measurement_temperature    130(2)
_cell_measurement_reflns_used    9842
_cell_measurement_theta_min      2.50
_cell_measurement_theta_max      27.05

_exptl_crystal_description       prism
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.178
_exptl_crystal_F_000             1208
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.19
_exptl_absorpt_coefficient_mu    0.950
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6442
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_process_details   'SADABS V2012/1 (Bruker AXS Inc.)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      130(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            53525
_diffrn_reflns_av_unetI/netI     0.0336
_diffrn_reflns_av_R_equivalents  0.0364
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_theta_min         2.819
_diffrn_reflns_theta_max         27.366
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             7226
_reflns_number_gt                5996
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_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       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXT 2014/4 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2018/1 (Sheldrick, 2018)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_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)+(0.0226P)²+5.6562P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         7226
_refine_ls_number_parameters     279
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0529
_refine_ls_R_factor_gt           0.0402
_refine_ls_wR_factor_ref         0.0849
_refine_ls_wR_factor_gt          0.0816
_refine_ls_goodness_of_fit_ref   1.122
_refine_ls_restrained_S_all      1.122
_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 0.62569(2) 0.40225(3) 0.69347(2) 0.03026(8) Uani 1 1 d . . . . .
HN1A H 0.5818(6) 0.288(2) 0.6377(9) 0.045 Uiso 1 1 calc R U . . .
HN1B H 0.6950(11) 0.314(2) 0.7456(7) 0.045 Uiso 1 1 calc R U . . .
HN1C H 0.6708(10) 0.5356(16) 0.6618(9) 0.045 Uiso 1 1 calc R U . . .
Si1 Si 0.37356(5) 0.55612(9) 0.58385(4) 0.02306(18) Uani 1 1 d . . . . .
Si4 Si 0.66212(5) 0.45405(10) 0.90832(4) 0.02631(19) Uani 1 1 d . . . . .
Si2 Si 0.50266(5) 0.82469(9) 0.62592(4) 0.02612(19) Uani 1 1 d . . . . .
Si3 Si 0.53661(5) 0.18000(9) 0.86000(4) 0.02660(19) Uani 1 1 d . . . . .
C1 C 0.41562(17) 0.6517(3) 0.73494(13) 0.0188(6) Uani 1 1 d . . . . .
H1 H 0.376931 0.718257 0.711853 0.023 Uiso 1 1 calc R U . . .
C2 C 0.34600(17) 0.6842(3) 0.82973(13) 0.0208(6) Uani 1 1 d . . . . .
C3 C 0.41159(17) 0.6200(3) 0.79702(12) 0.0180(6) Uani 1 1 d . . . . .
C4 C 0.53397(16) 0.4928(3) 0.73928(12) 0.0180(6) Uani 1 1 d . . . . .
C5 C 0.38835(19) 0.7727(3) 0.88746(14) 0.0278(7) Uani 1 1 d . . . . .
H5A H 0.422869 0.707425 0.917687 0.042 Uiso 1 1 calc R U . . .
H5B H 0.346634 0.818004 0.907352 0.042 Uiso 1 1 calc R U . . .
H5C H 0.422585 0.849077 0.874215 0.042 Uiso 1 1 calc R U . . .
C6 C 0.46983(17) 0.5223(3) 0.82945(13) 0.0193(6) Uani 1 1 d . . . . .
H6 H 0.467774 0.497689 0.871675 0.023 Uiso 1 1 calc R U . . .
C7 C 0.47055(17) 0.6286(3) 0.63637(12) 0.0193(6) Uani 1 1 d . . . . .
H7 H 0.515353 0.568982 0.624251 0.023 Uiso 1 1 calc R U . . .
C8 C 0.59018(17) 0.3542(3) 0.84314(13) 0.0217(6) Uani 1 1 d . . . . .
H8 H 0.626850 0.321170 0.814573 0.026 Uiso 1 1 calc R U . . .
C9 C 0.29703(19) 0.5592(3) 0.85174(16) 0.0315(7) Uani 1 1 d . . . . .
H9A H 0.269979 0.501654 0.815220 0.047 Uiso 1 1 calc R U . . .
H9B H 0.255454 0.600072 0.873035 0.047 Uiso 1 1 calc R U . . .
H9C H 0.334384 0.496108 0.881038 0.047 Uiso 1 1 calc R U . . .
C10 C 0.27511(19) 0.6321(4) 0.59935(16) 0.0351(8) Uani 1 1 d . . . . .
H10A H 0.277260 0.739252 0.598815 0.053 Uiso 1 1 calc R U . . .
H10B H 0.267292 0.598732 0.640691 0.053 Uiso 1 1 calc R U . . .
H10C H 0.229204 0.598034 0.566669 0.053 Uiso 1 1 calc R U . . .
C11 C 0.53089(17) 0.4592(3) 0.80245(13) 0.0193(6) Uani 1 1 d . . . . .
C12 C 0.2863(2) 0.7852(4) 0.78621(15) 0.0323(8) Uani 1 1 d . . . . .
H12A H 0.316971 0.865111 0.771570 0.048 Uiso 1 1 calc R U . . .
H12B H 0.246536 0.825844 0.809330 0.048 Uiso 1 1 calc R U . . .
H12C H 0.257070 0.729295 0.749892 0.048 Uiso 1 1 calc R U . . .
C13 C 0.47473(17) 0.5889(3) 0.70516(12) 0.0182(6) Uani 1 1 d . . . . .
C14 C 0.3746(2) 0.3539(3) 0.59645(16) 0.0336(8) Uani 1 1 d . . . . .
H14A H 0.321833 0.312357 0.575306 0.050 Uiso 1 1 calc R U . . .
H14B H 0.383734 0.333032 0.641690 0.050 Uiso 1 1 calc R U . . .
H14C H 0.418949 0.310026 0.578960 0.050 Uiso 1 1 calc R U . . .
C15 C 0.5459(2) 0.8354(4) 0.55292(17) 0.0426(9) Uani 1 1 d . . . . .
H15A H 0.501960 0.818621 0.515938 0.064 Uiso 1 1 calc R U . . .
H15B H 0.588550 0.760681 0.554549 0.064 Uiso 1 1 calc R U . . .
H15C H 0.569796 0.932591 0.549993 0.064 Uiso 1 1 calc R U . . .
C16 C 0.6100(2) 0.5591(4) 0.96262(16) 0.0384(8) Uani 1 1 d . . . . .
H16A H 0.651313 0.598501 0.997472 0.058 Uiso 1 1 calc R U . . .
H16B H 0.572718 0.494125 0.979382 0.058 Uiso 1 1 calc R U . . .
H16C H 0.578588 0.639812 0.939549 0.058 Uiso 1 1 calc R U . . .
C17 C 0.4860(2) 0.1933(4) 0.92923(16) 0.0399(9) Uani 1 1 d . . . . .
H17A H 0.461507 0.098635 0.936077 0.060 Uiso 1 1 calc R U . . .
H17B H 0.442959 0.268265 0.921121 0.060 Uiso 1 1 calc R U . . .
H17C H 0.526964 0.219984 0.966808 0.060 Uiso 1 1 calc R U . . .
C18 C 0.4148(2) 0.9561(4) 0.61813(18) 0.0399(9) Uani 1 1 d . . . . .
H18A H 0.435046 1.056208 0.615504 0.060 Uiso 1 1 calc R U . . .
H18B H 0.389365 0.947415 0.654953 0.060 Uiso 1 1 calc R U . . .
H18C H 0.374061 0.933529 0.579869 0.060 Uiso 1 1 calc R U . . .
C19 C 0.4571(2) 0.1372(4) 0.78821(17) 0.0417(9) Uani 1 1 d . . . . .
H19A H 0.482145 0.139958 0.751029 0.063 Uiso 1 1 calc R U . . .
H19B H 0.412874 0.209796 0.783536 0.063 Uiso 1 1 calc R U . . .
H19C H 0.434574 0.039433 0.792364 0.063 Uiso 1 1 calc R U . . .
C20 C 0.3754(2) 0.5934(4) 0.49931(15) 0.0400(8) Uani 1 1 d . . . . .
H20A H 0.330040 0.541236 0.472241 0.060 Uiso 1 1 calc R U . . .
H20B H 0.427755 0.559839 0.490200 0.060 Uiso 1 1 calc R U . . .
H20C H 0.369445 0.698822 0.491213 0.060 Uiso 1 1 calc R U . . .
C21 C 0.6123(2) 0.0259(4) 0.8741(2) 0.0492(10) Uani 1 1 d . . . . .
H21A H 0.649123 0.038757 0.915234 0.074 Uiso 1 1 calc R U . . .
H21B H 0.644534 0.025507 0.840985 0.074 Uiso 1 1 calc R U . . .
H21C H 0.582846 -0.067150 0.873523 0.074 Uiso 1 1 calc R U . . .
C22 C 0.7321(2) 0.3182(4) 0.95696(17) 0.0434(9) Uani 1 1 d . . . . .
H22A H 0.774540 0.370269 0.987010 0.065 Uiso 1 1 calc R U . . .
H22B H 0.758141 0.257384 0.929353 0.065 Uiso 1 1 calc R U . . .
H22C H 0.700265 0.255991 0.979974 0.065 Uiso 1 1 calc R U . . .
C23 C 0.5842(2) 0.8763(4) 0.69543(18) 0.0416(9) Uani 1 1 d . . . . .
H23A H 0.599662 0.978949 0.691646 0.062 Uiso 1 1 calc R U . . .
H23B H 0.632463 0.813814 0.696904 0.062 Uiso 1 1 calc R U . . .
H23C H 0.563213 0.863273 0.734154 0.062 Uiso 1 1 calc R U . . .
C24 C 0.7236(2) 0.5853(4) 0.87086(18) 0.0450(9) Uani 1 1 d . . . . .
H24A H 0.686618 0.655535 0.845125 0.068 Uiso 1 1 calc R U . . .
H24B H 0.754296 0.531490 0.844082 0.068 Uiso 1 1 calc R U . . .
H24C H 0.762083 0.637821 0.903675 0.068 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 C4 2.148(3) . ?
Sn1 HN1A 1.65(2) . ?
Sn1 HN1B 1.65(2) . ?
Sn1 HN1C 1.65(2) . ?
Si1 C14 1.868(3) . ?
Si1 C10 1.870(3) . ?
Si1 C20 1.870(3) . ?
Si1 C7 1.893(3) . ?
Si4 C16 1.864(3) . ?
Si4 C24 1.865(4) . ?
Si4 C22 1.872(3) . ?
Si4 C8 1.889(3) . ?
Si2 C15 1.869(3) . ?
Si2 C23 1.870(4) . ?
Si2 C18 1.871(3) . ?
Si2 C7 1.896(3) . ?
Si3 C19 1.866(4) . ?
Si3 C17 1.868(3) . ?
Si3 C21 1.871(4) . ?
Si3 C8 1.895(3) . ?
C1 C3 1.391(4) . ?
C1 C13 1.404(4) . ?
C1 H1 0.9500 . ?
C2 C12 1.531(4) . ?
C2 C3 1.533(4) . ?
C2 C9 1.534(4) . ?
C2 C5 1.535(4) . ?
C3 C6 1.397(4) . ?
C4 C13 1.411(4) . ?
C4 C11 1.414(4) . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C6 C11 1.395(4) . ?
C6 H6 0.9500 . ?
C7 C13 1.522(4) . ?
C7 H7 1.0000 . ?
C8 C11 1.522(4) . ?
C8 H8 1.0000 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 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 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 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
C4 Sn1 HN1A 109.5 . . ?
C4 Sn1 HN1B 109.5 . . ?
HN1A Sn1 HN1B 109.5 . . ?
C4 Sn1 HN1C 109.5 . . ?
HN1A Sn1 HN1C 109.5 . . ?
HN1B Sn1 HN1C 109.5 . . ?
C14 Si1 C10 108.88(16) . . ?
C14 Si1 C20 108.79(16) . . ?
C10 Si1 C20 107.37(16) . . ?
C14 Si1 C7 106.04(14) . . ?
C10 Si1 C7 115.55(14) . . ?
C20 Si1 C7 110.06(15) . . ?
C16 Si4 C24 108.09(18) . . ?
C16 Si4 C22 107.52(17) . . ?
C24 Si4 C22 109.80(18) . . ?
C16 Si4 C8 114.59(14) . . ?
C24 Si4 C8 107.70(15) . . ?
C22 Si4 C8 109.09(16) . . ?
C15 Si2 C23 109.16(18) . . ?
C15 Si2 C18 108.52(16) . . ?
C23 Si2 C18 109.56(17) . . ?
C15 Si2 C7 108.47(15) . . ?
C23 Si2 C7 108.52(15) . . ?
C18 Si2 C7 112.55(14) . . ?
C19 Si3 C17 108.98(18) . . ?
C19 Si3 C21 108.48(18) . . ?
C17 Si3 C21 108.40(18) . . ?
C19 Si3 C8 107.20(14) . . ?
C17 Si3 C8 114.00(14) . . ?
C21 Si3 C8 109.66(16) . . ?
C3 C1 C13 122.4(3) . . ?
C3 C1 H1 118.8 . . ?
C13 C1 H1 118.8 . . ?
C12 C2 C3 112.2(2) . . ?
C12 C2 C9 108.8(3) . . ?
C3 C2 C9 109.4(2) . . ?
C12 C2 C5 108.5(2) . . ?
C3 C2 C5 109.1(2) . . ?
C9 C2 C5 108.8(2) . . ?
C1 C3 C6 117.0(2) . . ?
C1 C3 C2 123.2(2) . . ?
C6 C3 C2 119.8(2) . . ?
C13 C4 C11 118.9(2) . . ?
C13 C4 Sn1 118.85(19) . . ?
C11 C4 Sn1 122.26(19) . . ?
C2 C5 H5A 109.5 . . ?
C2 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
C2 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
C11 C6 C3 122.8(2) . . ?
C11 C6 H6 118.6 . . ?
C3 C6 H6 118.6 . . ?
C13 C7 Si1 111.64(19) . . ?
C13 C7 Si2 112.58(19) . . ?
Si1 C7 Si2 118.98(14) . . ?
C13 C7 H7 103.9 . . ?
Si1 C7 H7 103.9 . . ?
Si2 C7 H7 103.9 . . ?
C11 C8 Si4 111.4(2) . . ?
C11 C8 Si3 111.5(2) . . ?
Si4 C8 Si3 120.79(15) . . ?
C11 C8 H8 103.6 . . ?
Si4 C8 H8 103.7 . . ?
Si3 C8 H8 103.6 . . ?
C2 C9 H9A 109.5 . . ?
C2 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C2 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
Si1 C10 H10A 109.5 . . ?
Si1 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
Si1 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C6 C11 C4 119.3(2) . . ?
C6 C11 C8 117.3(2) . . ?
C4 C11 C8 123.4(2) . . ?
C2 C12 H12A 109.5 . . ?
C2 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C2 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C1 C13 C4 119.5(2) . . ?
C1 C13 C7 117.2(2) . . ?
C4 C13 C7 123.3(2) . . ?
Si1 C14 H14A 109.5 . . ?
Si1 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
Si1 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
Si2 C15 H15A 109.5 . . ?
Si2 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
Si2 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
Si4 C16 H16A 109.5 . . ?
Si4 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
Si4 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
Si3 C17 H17A 109.5 . . ?
Si3 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
Si3 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
Si2 C18 H18A 109.5 . . ?
Si2 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
Si2 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
Si3 C19 H19A 109.5 . . ?
Si3 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
Si3 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
Si1 C20 H20A 109.5 . . ?
Si1 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
Si1 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
Si3 C21 H21A 109.5 . . ?
Si3 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
Si3 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
Si4 C22 H22A 109.5 . . ?
Si4 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
Si4 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
Si2 C23 H23A 109.5 . . ?
Si2 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
Si2 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
Si4 C24 H24A 109.5 . . ?
Si4 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
Si4 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?

_refine_diff_density_max         0.881
_refine_diff_density_min         -0.812
_refine_diff_density_rms         0.079



####################################################################### 
# 
# 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_shelx_CCDC3
_database_code_depnum_ccdc_archive 'CCDC 2153537'
loop_
_audit_author_name
_audit_author_address
'Hartmut Schubert'
;Universtity of Tuebingen
Germany
;
_audit_update_record             
;
2022-02-21 deposited with the CCDC.	2022-03-22 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/1
_shelx_SHELXL_version_number     2018/1
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C36 H75 K O6 Si4 Sn'
_chemical_formula_weight         874.13

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'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
K K 0.2009 0.2494 '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'
O O 0.0106 0.0060 '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'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_H-M_alt        'P n a 21'
_space_group_name_Hall           'P 2c -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'
'-x, -y, z+1/2'
'x+1/2, -y+1/2, z'
'-x+1/2, y+1/2, z+1/2'

_cell_length_a                   25.4342(3)
_cell_length_b                   9.56500(10)
_cell_length_c                   19.6290(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     4775.31(10)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9944
_cell_measurement_theta_min      2.37
_cell_measurement_theta_max      29.53

_exptl_crystal_description       prism
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.216
_exptl_crystal_F_000             1856
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.16
_exptl_absorpt_coefficient_mu    0.759
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7145
_exptl_absorpt_correction_T_max  0.7459
_exptl_absorpt_process_details   'SADABS V2012/1 (Bruker AXS Inc.)'
_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            72216
_diffrn_reflns_av_unetI/netI     0.0399
_diffrn_reflns_av_R_equivalents  0.0489
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_theta_min         1.601
_diffrn_reflns_theta_max         29.611
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.957
_diffrn_reflns_point_group_measured_fraction_full 0.982
_reflns_number_total             12871
_reflns_number_gt                11511
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.869
_reflns_Friedel_fraction_max     0.915
_reflns_Friedel_fraction_full    0.964

_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       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXT 2014/4 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2018/1 (Sheldrick, 2018)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_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)+(0.0224P)²+0.3483P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Flack x determined using 4779 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.004(6)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         12871
_refine_ls_number_parameters     455
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0348
_refine_ls_R_factor_gt           0.0266
_refine_ls_wR_factor_ref         0.0533
_refine_ls_wR_factor_gt          0.0505
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_restrained_S_all      1.018
_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 0.35035(2) 0.70371(2) 0.70707(2) 0.01592(4) Uani 1 1 d . . . . .
K1 K 0.56620(2) 0.54591(6) 0.31240(3) 0.01762(12) Uani 1 1 d . . . . .
Si2 Si 0.18673(3) 0.55351(8) 0.64558(4) 0.01551(15) Uani 1 1 d . . . . .
Si4 Si 0.47488(3) 0.65042(8) 0.53541(4) 0.01584(15) Uani 1 1 d . . . . .
Si3 Si 0.38750(3) 0.89519(8) 0.50396(4) 0.01756(16) Uani 1 1 d . . . . .
Si1 Si 0.25817(3) 0.28006(8) 0.68068(4) 0.02093(17) Uani 1 1 d . . . . .
O5 O 0.46733(8) 0.4001(2) 0.30251(10) 0.0250(5) Uani 1 1 d . . . . .
O2 O 0.63195(8) 0.7426(2) 0.38089(11) 0.0220(4) Uani 1 1 d . . . . .
O4 O 0.48420(8) 0.6567(2) 0.23460(11) 0.0267(5) Uani 1 1 d . . . . .
O3 O 0.54828(8) 0.8480(2) 0.30094(10) 0.0247(5) Uani 1 1 d . . . . .
O1 O 0.62358(8) 0.4724(2) 0.43602(10) 0.0213(4) Uani 1 1 d . . . . .
O6 O 0.55067(9) 0.2840(2) 0.37924(10) 0.0235(4) Uani 1 1 d . . . . .
C7 C 0.52577(13) 0.7672(3) 0.57551(18) 0.0264(7) Uani 1 1 d . . . . .
H7A H 0.529737 0.852136 0.548095 0.040 Uiso 1 1 calc R U . . .
H7B H 0.559477 0.717738 0.577641 0.040 Uiso 1 1 calc R U . . .
H7C H 0.514581 0.792404 0.621675 0.040 Uiso 1 1 calc R U . . .
C8 C 0.24116(11) 0.4367(3) 0.38847(15) 0.0219(6) Uani 1 1 d . . . . .
H8A H 0.238207 0.538228 0.383138 0.033 Uiso 1 1 calc R U . . .
H8B H 0.216773 0.405027 0.423914 0.033 Uiso 1 1 calc R U . . .
H8C H 0.232453 0.390863 0.345259 0.033 Uiso 1 1 calc R U . . .
C9 C 0.29803(11) 0.3986(3) 0.40913(13) 0.0158(5) Uani 1 1 d . . . . .
C10 C 0.19568(13) 0.7452(3) 0.63153(18) 0.0277(7) Uani 1 1 d . . . . .
H10A H 0.218505 0.760220 0.591986 0.042 Uiso 1 1 calc R U . . .
H10B H 0.211827 0.787118 0.671988 0.042 Uiso 1 1 calc R U . . .
H10C H 0.161391 0.788716 0.623249 0.042 Uiso 1 1 calc R U . . .
C11 C 0.33447(13) 0.4442(3) 0.35146(15) 0.0262(7) Uani 1 1 d . . . . .
H11A H 0.332982 0.546117 0.346577 0.039 Uiso 1 1 calc R U . . .
H11B H 0.323249 0.400110 0.308815 0.039 Uiso 1 1 calc R U . . .
H11C H 0.370584 0.415750 0.361984 0.039 Uiso 1 1 calc R U . . .
C12 C 0.31109(11) 0.4691(3) 0.47742(14) 0.0128(5) Uani 1 1 d . . . . .
C13 C 0.44563(13) 0.4305(4) 0.23731(16) 0.0332(8) Uani 1 1 d . . . . .
H13A H 0.412310 0.378441 0.231162 0.040 Uiso 1 1 calc R U . . .
H13B H 0.470387 0.400813 0.201176 0.040 Uiso 1 1 calc R U . . .
C14 C 0.14670(13) 0.5284(4) 0.72447(15) 0.0302(8) Uani 1 1 d . . . . .
H14A H 0.165560 0.567607 0.763586 0.045 Uiso 1 1 calc R U . . .
H14B H 0.140715 0.428333 0.731890 0.045 Uiso 1 1 calc R U . . .
H14C H 0.112829 0.576072 0.719298 0.045 Uiso 1 1 calc R U . . .
C15 C 0.53000(14) 0.8733(3) 0.23372(16) 0.0299(7) Uani 1 1 d . . . . .
H15A H 0.555143 0.834682 0.200117 0.036 Uiso 1 1 calc R U . . .
H15B H 0.526624 0.975048 0.225674 0.036 Uiso 1 1 calc R U . . .
C16 C 0.47621(12) 0.4734(3) 0.57590(15) 0.0232(6) Uani 1 1 d . . . . .
H16A H 0.463003 0.480020 0.622694 0.035 Uiso 1 1 calc R U . . .
H16B H 0.512384 0.438120 0.576478 0.035 Uiso 1 1 calc R U . . .
H16C H 0.453939 0.409270 0.549752 0.035 Uiso 1 1 calc R U . . .
C17 C 0.43560(13) 0.5837(4) 0.23187(17) 0.0356(8) Uani 1 1 d . . . . .
H17A H 0.417485 0.604540 0.188395 0.043 Uiso 1 1 calc R U . . .
H17B H 0.412648 0.614468 0.269747 0.043 Uiso 1 1 calc R U . . .
C18 C 0.67171(12) 0.5483(3) 0.43557(17) 0.0258(7) Uani 1 1 d . . . . .
H18A H 0.691140 0.529831 0.392797 0.031 Uiso 1 1 calc R U . . .
H18B H 0.694011 0.519010 0.474373 0.031 Uiso 1 1 calc R U . . .
C19 C 0.14758(12) 0.4811(3) 0.57266(15) 0.0240(6) Uani 1 1 d . . . . .
H19A H 0.112942 0.525937 0.571496 0.036 Uiso 1 1 calc R U . . .
H19B H 0.143238 0.380021 0.578589 0.036 Uiso 1 1 calc R U . . .
H19C H 0.166094 0.499511 0.529807 0.036 Uiso 1 1 calc R U . . .
C20 C 0.47439(14) 0.2531(4) 0.31173(19) 0.0319(8) Uani 1 1 d . . . . .
H20A H 0.497362 0.215461 0.275388 0.038 Uiso 1 1 calc R U . . .
H20B H 0.440006 0.204897 0.309104 0.038 Uiso 1 1 calc R U . . .
C21 C 0.28009(10) 0.4448(3) 0.53441(13) 0.0134(5) Uani 1 1 d . . . . .
H21 H 0.250787 0.383828 0.530112 0.016 Uiso 1 1 calc R U . . .
C22 C 0.25318(10) 0.4703(3) 0.65633(13) 0.0133(5) Uani 1 1 d . . . . .
H22 H 0.268687 0.520546 0.696233 0.016 Uiso 1 1 calc R U . . .
C23 C 0.42785(14) 1.0462(3) 0.53441(17) 0.0296(7) Uani 1 1 d . . . . .
H23A H 0.414333 1.132941 0.514399 0.044 Uiso 1 1 calc R U . . .
H23B H 0.464529 1.032863 0.520590 0.044 Uiso 1 1 calc R U . . .
H23C H 0.425818 1.051996 0.584182 0.044 Uiso 1 1 calc R U . . .
C24 C 0.49507(12) 0.6267(3) 0.44451(15) 0.0243(6) Uani 1 1 d . . . . .
H24A H 0.494884 0.717515 0.421371 0.036 Uiso 1 1 calc R U . . .
H24B H 0.530538 0.586830 0.442757 0.036 Uiso 1 1 calc R U . . .
H24C H 0.470380 0.563415 0.421768 0.036 Uiso 1 1 calc R U . . .
C25 C 0.39408(14) 0.8869(3) 0.40878(15) 0.0293(7) Uani 1 1 d . . . . .
H25A H 0.372313 0.810499 0.391115 0.044 Uiso 1 1 calc R U . . .
H25B H 0.430930 0.870227 0.396682 0.044 Uiso 1 1 calc R U . . .
H25C H 0.382422 0.975572 0.388867 0.044 Uiso 1 1 calc R U . . .
C26 C 0.59413(13) 0.9276(3) 0.31683(16) 0.0268(7) Uani 1 1 d . . . . .
H26A H 0.585559 1.028573 0.317369 0.032 Uiso 1 1 calc R U . . .
H26B H 0.621632 0.911426 0.282016 0.032 Uiso 1 1 calc R U . . .
C27 C 0.40872(10) 0.7314(3) 0.55010(13) 0.0136(5) Uani 1 1 d . . . . .
H27 H 0.410048 0.761029 0.598927 0.016 Uiso 1 1 calc R U . . .
C28 C 0.29002(10) 0.5061(3) 0.59802(13) 0.0120(5) Uani 1 1 d . . . . .
C29 C 0.30144(15) 0.2394(3) 0.41669(17) 0.0326(8) Uani 1 1 d . . . . .
H29A H 0.291618 0.194873 0.373557 0.049 Uiso 1 1 calc R U . . .
H29B H 0.277396 0.208544 0.452696 0.049 Uiso 1 1 calc R U . . .
H29C H 0.337498 0.212853 0.428658 0.049 Uiso 1 1 calc R U . . .
C30 C 0.35332(11) 0.5612(3) 0.48555(14) 0.0141(5) Uani 1 1 d . . . . .
H30 H 0.375238 0.581193 0.447590 0.017 Uiso 1 1 calc R U . . .
C31 C 0.33371(10) 0.5960(3) 0.60680(13) 0.0120(5) Uani 1 1 d . . . . .
C32 C 0.47768(14) 0.8038(4) 0.22623(16) 0.0334(8) Uani 1 1 d . . . . .
H32A H 0.453013 0.840176 0.260997 0.040 Uiso 1 1 calc R U . . .
H32B H 0.462895 0.824009 0.180623 0.040 Uiso 1 1 calc R U . . .
C33 C 0.61357(12) 0.8827(3) 0.38549(16) 0.0238(6) Uani 1 1 d . . . . .
H33A H 0.642447 0.944833 0.400550 0.029 Uiso 1 1 calc R U . . .
H33B H 0.584747 0.888719 0.419256 0.029 Uiso 1 1 calc R U . . .
C34 C 0.65890(12) 0.7004(3) 0.44112(17) 0.0264(7) Uani 1 1 d . . . . .
H34A H 0.636462 0.717114 0.481511 0.032 Uiso 1 1 calc R U . . .
H34B H 0.691631 0.755348 0.446422 0.032 Uiso 1 1 calc R U . . .
C35 C 0.36412(10) 0.6249(3) 0.54848(13) 0.0126(5) Uani 1 1 d . . . . .
C36 C 0.21103(14) 0.1619(3) 0.6347(2) 0.0349(8) Uani 1 1 d . . . . .
H36A H 0.218878 0.064320 0.646098 0.052 Uiso 1 1 calc R U . . .
H36B H 0.214665 0.175568 0.585447 0.052 Uiso 1 1 calc R U . . .
H36C H 0.174974 0.184061 0.648573 0.052 Uiso 1 1 calc R U . . .
C37 C 0.49894(14) 0.2282(3) 0.38000(18) 0.0307(7) Uani 1 1 d . . . . .
H37A H 0.477862 0.274157 0.415991 0.037 Uiso 1 1 calc R U . . .
H37B H 0.500157 0.126655 0.389727 0.037 Uiso 1 1 calc R U . . .
C38 C 0.31676(13) 0.9245(3) 0.52556(19) 0.0329(8) Uani 1 1 d . . . . .
H38A H 0.311824 0.914963 0.574854 0.049 Uiso 1 1 calc R U . . .
H38B H 0.295051 0.855140 0.501882 0.049 Uiso 1 1 calc R U . . .
H38C H 0.306323 1.018617 0.511254 0.049 Uiso 1 1 calc R U . . .
C39 C 0.32647(14) 0.2190(3) 0.66233(19) 0.0340(8) Uani 1 1 d . . . . .
H39A H 0.351569 0.275107 0.688528 0.051 Uiso 1 1 calc R U . . .
H39B H 0.333783 0.229320 0.613575 0.051 Uiso 1 1 calc R U . . .
H39C H 0.329879 0.120426 0.675265 0.051 Uiso 1 1 calc R U . . .
C40 C 0.63113(13) 0.3254(3) 0.43555(16) 0.0263(7) Uani 1 1 d . . . . .
H40A H 0.653399 0.297069 0.474550 0.032 Uiso 1 1 calc R U . . .
H40B H 0.648917 0.296553 0.392938 0.032 Uiso 1 1 calc R U . . .
C41 C 0.57838(14) 0.2570(3) 0.44051(16) 0.0271(7) Uani 1 1 d . . . . .
H41A H 0.582549 0.155010 0.447087 0.032 Uiso 1 1 calc R U . . .
H41B H 0.558702 0.295189 0.479855 0.032 Uiso 1 1 calc R U . . .
C42 C 0.24546(18) 0.2631(4) 0.77414(19) 0.0459(10) Uani 1 1 d . . . . .
H42A H 0.209909 0.296573 0.784419 0.069 Uiso 1 1 calc R U . . .
H42B H 0.271175 0.319160 0.799379 0.069 Uiso 1 1 calc R U . . .
H42C H 0.248624 0.164845 0.787599 0.069 Uiso 1 1 calc R U . . .
H400 H 0.4181(13) 0.667(3) 0.704(2) 0.039(9) Uiso 1 1 d . . . . .
H401 H 0.3384(15) 0.562(4) 0.764(2) 0.052(12) Uiso 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Sn1 C31 2.262(3) . ?
Sn1 K1 3.8053(6) 2_665 ?
Sn1 H400 1.76(3) . ?
Sn1 H401 1.78(4) . ?
K1 O4 2.794(2) . ?
K1 O2 2.854(2) . ?
K1 O6 2.855(2) . ?
K1 O5 2.882(2) . ?
K1 O1 2.918(2) . ?
K1 O3 2.934(2) . ?
Si2 C10 1.868(3) . ?
Si2 C14 1.869(3) . ?
Si2 C19 1.876(3) . ?
Si2 C22 1.880(3) . ?
Si4 C24 1.871(3) . ?
Si4 C16 1.871(3) . ?
Si4 C27 1.875(3) . ?
Si4 C7 1.882(3) . ?
Si3 C38 1.869(3) . ?
Si3 C23 1.870(3) . ?
Si3 C25 1.877(3) . ?
Si3 C27 1.888(3) . ?
Si1 C39 1.868(4) . ?
Si1 C42 1.870(4) . ?
Si1 C36 1.879(3) . ?
Si1 C22 1.886(3) . ?
O5 C13 1.424(4) . ?
O5 C20 1.429(4) . ?
O2 C33 1.422(3) . ?
O2 C34 1.425(4) . ?
O4 C17 1.420(4) . ?
O4 C32 1.427(4) . ?
O3 C15 1.420(4) . ?
O3 C26 1.427(4) . ?
O1 C40 1.419(3) . ?
O1 C18 1.423(4) . ?
O6 C41 1.418(4) . ?
O6 C37 1.420(4) . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 C9 1.546(4) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 C11 1.527(4) . ?
C9 C29 1.533(4) . ?
C9 C12 1.537(4) . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 C21 1.388(4) . ?
C12 C30 1.398(4) . ?
C13 C17 1.492(5) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 C32 1.494(5) . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 H17A 0.9900 . ?
C17 H17B 0.9900 . ?
C18 C34 1.495(4) . ?
C18 H18A 0.9900 . ?
C18 H18B 0.9900 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C20 C37 1.497(5) . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C21 C28 1.402(4) . ?
C21 H21 0.9500 . ?
C22 C28 1.518(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 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C26 C33 1.499(4) . ?
C26 H26A 0.9900 . ?
C26 H26B 0.9900 . ?
C27 C35 1.525(3) . ?
C27 H27 1.0000 . ?
C28 C31 1.416(4) . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
C30 C35 1.404(4) . ?
C30 H30 0.9500 . ?
C31 C35 1.409(4) . ?
C32 H32A 0.9900 . ?
C32 H32B 0.9900 . ?
C33 H33A 0.9900 . ?
C33 H33B 0.9900 . ?
C34 H34A 0.9900 . ?
C34 H34B 0.9900 . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?
C37 H37A 0.9900 . ?
C37 H37B 0.9900 . ?
C38 H38A 0.9800 . ?
C38 H38B 0.9800 . ?
C38 H38C 0.9800 . ?
C39 H39A 0.9800 . ?
C39 H39B 0.9800 . ?
C39 H39C 0.9800 . ?
C40 C41 1.496(5) . ?
C40 H40A 0.9900 . ?
C40 H40B 0.9900 . ?
C41 H41A 0.9900 . ?
C41 H41B 0.9900 . ?
C42 H42A 0.9800 . ?
C42 H42B 0.9800 . ?
C42 H42C 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
C31 Sn1 K1 106.94(6) . 2_665 ?
C31 Sn1 H400 93.8(13) . . ?
K1 Sn1 H400 49.0(12) 2_665 . ?
C31 Sn1 H401 99.4(13) . . ?
K1 Sn1 H401 43.8(12) 2_665 . ?
H400 Sn1 H401 91.9(17) . . ?
O4 K1 O2 116.43(7) . . ?
O4 K1 O6 118.73(7) . . ?
O2 K1 O6 116.29(6) . . ?
O4 K1 O5 59.69(6) . . ?
O2 K1 O5 149.55(6) . . ?
O6 K1 O5 59.05(6) . . ?
O4 K1 O1 156.85(6) . . ?
O2 K1 O1 58.26(6) . . ?
O6 K1 O1 58.37(6) . . ?
O5 K1 O1 112.08(6) . . ?
O4 K1 O3 57.90(6) . . ?
O2 K1 O3 58.53(6) . . ?
O6 K1 O3 151.38(6) . . ?
O5 K1 O3 109.63(6) . . ?
O1 K1 O3 112.26(6) . . ?
O4 K1 Sn1 110.94(5) . 2_664 ?
O2 K1 Sn1 110.04(4) . 2_664 ?
O6 K1 Sn1 77.08(4) . 2_664 ?
O5 K1 Sn1 98.42(4) . 2_664 ?
O1 K1 Sn1 91.24(4) . 2_664 ?
O3 K1 Sn1 131.52(4) . 2_664 ?
C10 Si2 C14 108.35(15) . . ?
C10 Si2 C19 108.32(15) . . ?
C14 Si2 C19 107.19(14) . . ?
C10 Si2 C22 108.82(13) . . ?
C14 Si2 C22 110.02(14) . . ?
C19 Si2 C22 113.99(13) . . ?
C24 Si4 C16 106.90(14) . . ?
C24 Si4 C27 116.31(13) . . ?
C16 Si4 C27 108.96(13) . . ?
C24 Si4 C7 106.38(15) . . ?
C16 Si4 C7 110.30(14) . . ?
C27 Si4 C7 107.92(14) . . ?
C38 Si3 C23 109.87(16) . . ?
C38 Si3 C25 108.53(16) . . ?
C23 Si3 C25 107.57(15) . . ?
C38 Si3 C27 106.90(13) . . ?
C23 Si3 C27 109.31(13) . . ?
C25 Si3 C27 114.63(13) . . ?
C39 Si1 C42 108.84(19) . . ?
C39 Si1 C36 108.21(17) . . ?
C42 Si1 C36 108.00(18) . . ?
C39 Si1 C22 108.39(14) . . ?
C42 Si1 C22 108.70(16) . . ?
C36 Si1 C22 114.58(13) . . ?
C13 O5 C20 111.3(2) . . ?
C13 O5 K1 107.46(17) . . ?
C20 O5 K1 110.98(17) . . ?
C33 O2 C34 111.9(2) . . ?
C33 O2 K1 117.28(17) . . ?
C34 O2 K1 119.08(16) . . ?
C17 O4 C32 112.3(2) . . ?
C17 O4 K1 118.94(18) . . ?
C32 O4 K1 121.59(18) . . ?
C15 O3 C26 112.3(2) . . ?
C15 O3 K1 106.85(17) . . ?
C26 O3 K1 112.45(16) . . ?
C40 O1 C18 112.9(2) . . ?
C40 O1 K1 107.52(17) . . ?
C18 O1 K1 107.59(16) . . ?
C41 O6 C37 112.5(2) . . ?
C41 O6 K1 118.74(16) . . ?
C37 O6 K1 117.58(18) . . ?
Si4 C7 H7A 109.5 . . ?
Si4 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
Si4 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C9 C8 H8A 109.5 . . ?
C9 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C9 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C11 C9 C29 108.8(2) . . ?
C11 C9 C12 112.9(2) . . ?
C29 C9 C12 109.8(2) . . ?
C11 C9 C8 107.8(2) . . ?
C29 C9 C8 108.2(2) . . ?
C12 C9 C8 109.1(2) . . ?
Si2 C10 H10A 109.5 . . ?
Si2 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
Si2 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C9 C11 H11A 109.5 . . ?
C9 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C9 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C21 C12 C30 116.7(2) . . ?
C21 C12 C9 120.4(2) . . ?
C30 C12 C9 122.8(2) . . ?
O5 C13 C17 109.3(3) . . ?
O5 C13 H13A 109.8 . . ?
C17 C13 H13A 109.8 . . ?
O5 C13 H13B 109.8 . . ?
C17 C13 H13B 109.8 . . ?
H13A C13 H13B 108.3 . . ?
Si2 C14 H14A 109.5 . . ?
Si2 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
Si2 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
O3 C15 C32 107.9(3) . . ?
O3 C15 H15A 110.1 . . ?
C32 C15 H15A 110.1 . . ?
O3 C15 H15B 110.1 . . ?
C32 C15 H15B 110.1 . . ?
H15A C15 H15B 108.4 . . ?
Si4 C16 H16A 109.5 . . ?
Si4 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
Si4 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
O4 C17 C13 109.4(3) . . ?
O4 C17 H17A 109.8 . . ?
C13 C17 H17A 109.8 . . ?
O4 C17 H17B 109.8 . . ?
C13 C17 H17B 109.8 . . ?
H17A C17 H17B 108.3 . . ?
O1 C18 C34 108.0(2) . . ?
O1 C18 H18A 110.1 . . ?
C34 C18 H18A 110.1 . . ?
O1 C18 H18B 110.1 . . ?
C34 C18 H18B 110.1 . . ?
H18A C18 H18B 108.4 . . ?
Si2 C19 H19A 109.5 . . ?
Si2 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
Si2 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
O5 C20 C37 108.8(3) . . ?
O5 C20 H20A 109.9 . . ?
C37 C20 H20A 109.9 . . ?
O5 C20 H20B 109.9 . . ?
C37 C20 H20B 109.9 . . ?
H20A C20 H20B 108.3 . . ?
C12 C21 C28 123.0(2) . . ?
C12 C21 H21 118.5 . . ?
C28 C21 H21 118.5 . . ?
C28 C22 Si2 112.01(17) . . ?
C28 C22 Si1 111.53(17) . . ?
Si2 C22 Si1 119.83(14) . . ?
C28 C22 H22 103.8 . . ?
Si2 C22 H22 103.8 . . ?
Si1 C22 H22 103.8 . . ?
Si3 C23 H23A 109.5 . . ?
Si3 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
Si3 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
Si4 C24 H24A 109.5 . . ?
Si4 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
Si4 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
Si3 C25 H25A 109.5 . . ?
Si3 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
Si3 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
O3 C26 C33 108.2(2) . . ?
O3 C26 H26A 110.1 . . ?
C33 C26 H26A 110.0 . . ?
O3 C26 H26B 110.0 . . ?
C33 C26 H26B 110.0 . . ?
H26A C26 H26B 108.4 . . ?
C35 C27 Si4 112.85(17) . . ?
C35 C27 Si3 109.36(17) . . ?
Si4 C27 Si3 121.71(14) . . ?
C35 C27 H27 103.6 . . ?
Si4 C27 H27 103.6 . . ?
Si3 C27 H27 103.6 . . ?
C21 C28 C31 120.3(2) . . ?
C21 C28 C22 117.8(2) . . ?
C31 C28 C22 122.0(2) . . ?
C9 C29 H29A 109.5 . . ?
C9 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
C9 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C12 C30 C35 121.6(2) . . ?
C12 C30 H30 119.2 . . ?
C35 C30 H30 119.2 . . ?
C35 C31 C28 116.8(2) . . ?
C35 C31 Sn1 120.98(18) . . ?
C28 C31 Sn1 121.99(18) . . ?
O4 C32 C15 108.9(2) . . ?
O4 C32 H32A 109.9 . . ?
C15 C32 H32A 109.9 . . ?
O4 C32 H32B 109.9 . . ?
C15 C32 H32B 109.9 . . ?
H32A C32 H32B 108.3 . . ?
O2 C33 C26 108.8(2) . . ?
O2 C33 H33A 109.9 . . ?
C26 C33 H33A 109.9 . . ?
O2 C33 H33B 109.9 . . ?
C26 C33 H33B 109.9 . . ?
H33A C33 H33B 108.3 . . ?
O2 C34 C18 108.7(3) . . ?
O2 C34 H34A 110.0 . . ?
C18 C34 H34A 110.0 . . ?
O2 C34 H34B 110.0 . . ?
C18 C34 H34B 110.0 . . ?
H34A C34 H34B 108.3 . . ?
C30 C35 C31 121.5(2) . . ?
C30 C35 C27 117.0(2) . . ?
C31 C35 C27 121.5(2) . . ?
Si1 C36 H36A 109.5 . . ?
Si1 C36 H36B 109.5 . . ?
H36A C36 H36B 109.5 . . ?
Si1 C36 H36C 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
O6 C37 C20 108.5(3) . . ?
O6 C37 H37A 110.0 . . ?
C20 C37 H37A 110.0 . . ?
O6 C37 H37B 110.0 . . ?
C20 C37 H37B 110.0 . . ?
H37A C37 H37B 108.4 . . ?
Si3 C38 H38A 109.5 . . ?
Si3 C38 H38B 109.5 . . ?
H38A C38 H38B 109.5 . . ?
Si3 C38 H38C 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
Si1 C39 H39A 109.5 . . ?
Si1 C39 H39B 109.5 . . ?
H39A C39 H39B 109.5 . . ?
Si1 C39 H39C 109.5 . . ?
H39A C39 H39C 109.5 . . ?
H39B C39 H39C 109.5 . . ?
O1 C40 C41 108.1(3) . . ?
O1 C40 H40A 110.1 . . ?
C41 C40 H40A 110.1 . . ?
O1 C40 H40B 110.1 . . ?
C41 C40 H40B 110.1 . . ?
H40A C40 H40B 108.4 . . ?
O6 C41 C40 108.1(2) . . ?
O6 C41 H41A 110.1 . . ?
C40 C41 H41A 110.1 . . ?
O6 C41 H41B 110.1 . . ?
C40 C41 H41B 110.1 . . ?
H41A C41 H41B 108.4 . . ?
Si1 C42 H42A 109.5 . . ?
Si1 C42 H42B 109.5 . . ?
H42A C42 H42B 109.5 . . ?
Si1 C42 H42C 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?

_refine_diff_density_max         0.430
_refine_diff_density_min         -0.247
_refine_diff_density_rms         0.058


