# Electronic Supplementary Material (ESI) for Chemical Communications.
# 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_4586_a
_database_code_depnum_ccdc_archive 'CCDC 2174673'
loop_
_audit_author_name
_audit_author_address
'Bernd Morgenstern'
;Universitaet des Saarlandes
Germany
;
_audit_update_record             
;
2022-07-04 deposited with the CCDC.	2022-07-12 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C26 H47 Ge N3 Si'
_chemical_formula_sum            'C26 H47 Ge N3 Si'
_chemical_formula_weight         502.34

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ge Ge 0.1547 1.8001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      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                   10.5226(3)
_cell_length_b                   16.5510(5)
_cell_length_c                   16.5994(7)
_cell_angle_alpha                90
_cell_angle_beta                 104.6320(10)
_cell_angle_gamma                90
_cell_volume                     2797.19(17)
_cell_formula_units_Z            4
_cell_measurement_temperature    132(2)
_cell_measurement_reflns_used    9305
_cell_measurement_theta_min      2.42
_cell_measurement_theta_max      31.53

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.193
_exptl_crystal_F_000             1080
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.349
_exptl_crystal_size_mid          0.340
_exptl_crystal_size_min          0.276
_exptl_absorpt_coefficient_mu    1.155
_shelx_estimated_absorpt_T_min   0.689
_shelx_estimated_absorpt_T_max   0.741
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7061
_exptl_absorpt_correction_T_max  0.7462
_exptl_absorpt_process_details   
;
 SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D.,
 J. Appl. Cryst. 48 (2015) 3-10
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      132(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'sealed tube'
_diffrn_measurement_device_type  'Bruker X8 Apex, Nonius Kappa CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            57712
_diffrn_reflns_av_unetI/netI     0.0245
_diffrn_reflns_av_R_equivalents  0.0328
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         1.767
_diffrn_reflns_theta_max         31.583
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             9376
_reflns_number_gt                7758
_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       'APEX2 (Bruker, 2010)'
_computing_cell_refinement       'SAINT (Bruker, 2010)'
_computing_data_reduction        'SAINT (Bruker, 2010)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_computing_structure_refinement  
;
SHELXL-2018/3 (Sheldrick, 2018),                                              
SHELXLe Rev 1000 (Huebschle et al., 2011)
;
_computing_molecular_graphics    'DIAMOND, (Brandenburg, 2018)'
_computing_publication_material  'SHELXL-2018/3 (Sheldrick, 2018)'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0345P)²+1.4783P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         9376
_refine_ls_number_parameters     335
_refine_ls_number_restraints     133
_refine_ls_R_factor_all          0.0426
_refine_ls_R_factor_gt           0.0317
_refine_ls_wR_factor_ref         0.0816
_refine_ls_wR_factor_gt          0.0765
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_restrained_S_all      1.028
_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 0.67003(2) 0.22486(2) 0.36295(2) 0.01727(4) Uani 1 1 d . . . . .
Si1 Si 0.58288(4) 0.22406(3) 0.50539(3) 0.02791(9) Uani 1 1 d . . . . .
N1 N 0.58912(12) 0.40983(7) 0.30763(7) 0.0236(2) Uani 1 1 d . . . . .
C1 C 0.67778(13) 0.35033(8) 0.33294(8) 0.0188(2) Uani 1 1 d . . . . .
N2 N 0.78932(12) 0.37740(7) 0.31586(7) 0.0229(2) Uani 1 1 d . . . . .
C2 C 0.77029(18) 0.45338(9) 0.27902(9) 0.0329(3) Uani 1 1 d . . . . .
C3 C 0.64519(19) 0.47425(9) 0.27438(10) 0.0348(4) Uani 1 1 d . . . . .
N3 N 0.51354(12) 0.21191(7) 0.40151(8) 0.0236(2) Uani 1 1 d . . . . .
C4 C 0.8710(2) 0.49863(13) 0.24749(13) 0.0538(6) Uani 1 1 d . . . . .
H4A H 0.902007 0.464761 0.207919 0.081 Uiso 1 1 calc R U . . .
H4B H 0.945167 0.512609 0.294315 0.081 Uiso 1 1 calc R U . . .
H4C H 0.831780 0.548159 0.219576 0.081 Uiso 1 1 calc R U . . .
C5 C 0.5755(3) 0.55033(12) 0.23946(15) 0.0631(7) Uani 1 1 d . . . . .
H5A H 0.635645 0.585131 0.218752 0.095 Uiso 1 1 calc R U . . .
H5B H 0.545737 0.578729 0.283177 0.095 Uiso 1 1 calc R U . . .
H5C H 0.499526 0.536896 0.193609 0.095 Uiso 1 1 calc R U . . .
C6 C 0.45469(16) 0.40335(10) 0.31781(9) 0.0312(3) Uani 1 1 d . . . . .
H6 H 0.448067 0.349798 0.344341 0.037 Uiso 1 1 calc R U . . .
C9 C 0.91082(14) 0.32850(10) 0.33449(9) 0.0270(3) Uani 1 1 d . . . . .
H9 H 0.897749 0.283997 0.372350 0.032 Uiso 1 1 calc R U . . .
C8 C 0.3537(2) 0.40333(19) 0.23423(12) 0.0655(8) Uani 1 1 d . . . . .
H8A H 0.348758 0.457362 0.209479 0.098 Uiso 1 1 calc R U . . .
H8B H 0.267577 0.388464 0.242262 0.098 Uiso 1 1 calc R U . . .
H8C H 0.379599 0.364163 0.197060 0.098 Uiso 1 1 calc R U . . .
C7 C 0.4260(3) 0.46763(12) 0.37637(14) 0.0579(6) Uani 1 1 d . . . . .
H7A H 0.413992 0.520019 0.347934 0.087 Uiso 1 1 calc R U . . .
H7B H 0.499810 0.470972 0.425961 0.087 Uiso 1 1 calc R U . . .
H7C H 0.345880 0.453303 0.392922 0.087 Uiso 1 1 calc R U . . .
C10 C 0.92826(19) 0.28835(11) 0.25546(11) 0.0379(4) Uani 1 1 d . . . . .
H10A H 0.852059 0.254041 0.231820 0.057 Uiso 1 1 calc R U . . .
H10B H 1.008021 0.255210 0.268731 0.057 Uiso 1 1 calc R U . . .
H10C H 0.935926 0.329960 0.214945 0.057 Uiso 1 1 calc R U . . .
C11 C 1.03091(17) 0.37573(14) 0.38129(12) 0.0463(5) Uani 1 1 d . . . . .
H11A H 1.065602 0.407300 0.341662 0.069 Uiso 1 1 calc R U . . .
H11B H 1.098381 0.338053 0.411124 0.069 Uiso 1 1 calc R U . . .
H11C H 1.006096 0.412239 0.421231 0.069 Uiso 1 1 calc R U . . .
C12 C 0.75614(14) 0.23591(10) 0.49450(8) 0.0269(3) Uani 1 1 d . . . . .
C13 C 0.84770(16) 0.16586(11) 0.51256(9) 0.0340(4) Uani 1 1 d . . . . .
C14 C 0.97063(16) 0.19310(13) 0.54909(10) 0.0403(4) Uani 1 1 d . . . . .
C15 C 0.96733(16) 0.27919(13) 0.55904(9) 0.0391(4) Uani 1 1 d . . . . .
C16 C 0.84116(15) 0.30586(11) 0.52730(9) 0.0313(3) Uani 1 1 d . . . . .
C17 C 0.79691(17) 0.39161(12) 0.52928(11) 0.0390(4) Uani 1 1 d . . . . .
H17A H 0.865896 0.427967 0.520819 0.059 Uiso 1 1 calc R U . . .
H17B H 0.779190 0.402906 0.583368 0.059 Uiso 1 1 calc R U . . .
H17C H 0.716655 0.400097 0.484948 0.059 Uiso 1 1 calc R U . . .
C18 C 0.8116(2) 0.07993(11) 0.48940(12) 0.0449(5) Uani 1 1 d . . . . .
H18A H 0.723428 0.077995 0.451635 0.067 Uiso 1 1 calc R U . . .
H18B H 0.812593 0.048786 0.539775 0.067 Uiso 1 1 calc R U . . .
H18C H 0.875003 0.056768 0.461644 0.067 Uiso 1 1 calc R U . . .
C19 C 1.09337(19) 0.14270(17) 0.57615(14) 0.0594(7) Uani 1 1 d . . . . .
H19A H 1.071470 0.085639 0.564397 0.089 Uiso 1 1 calc R U . . .
H19B H 1.131215 0.149865 0.636019 0.089 Uiso 1 1 calc R U . . .
H19C H 1.157204 0.159834 0.545620 0.089 Uiso 1 1 calc R U . . .
C20 C 1.08518(18) 0.32900(17) 0.59907(12) 0.0579(6) Uani 1 1 d . . . . .
H20A H 1.157329 0.316024 0.573747 0.087 Uiso 1 1 calc R U . . .
H20B H 1.112049 0.317116 0.658812 0.087 Uiso 1 1 calc R U . . .
H20C H 1.063290 0.386468 0.590849 0.087 Uiso 1 1 calc R U . . .
C21 C 0.51780(17) 0.31230(13) 0.55331(11) 0.0414(4) Uani 1 1 d . . . . .
H21A H 0.514584 0.359973 0.517829 0.062 Uiso 1 1 calc R U . . .
H21B H 0.575553 0.323171 0.608523 0.062 Uiso 1 1 calc R U . . .
H21C H 0.429207 0.299920 0.558629 0.062 Uiso 1 1 calc R U . . .
C22 C 0.5598(2) 0.13841(17) 0.57391(17) 0.0781(10) Uani 1 1 d . . . . .
H22A H 0.466350 0.132864 0.571897 0.117 Uiso 1 1 calc R U . . .
H22B H 0.609383 0.149240 0.631292 0.117 Uiso 1 1 calc R U . . .
H22C H 0.591667 0.088264 0.554427 0.117 Uiso 1 1 calc R U . . .
C23A C 0.3810(6) 0.1795(4) 0.3452(5) 0.0233(10) Uani 0.497(15) 1 d D U P A 1
C24A C 0.3743(6) 0.0892(3) 0.3594(5) 0.0375(14) Uani 0.497(15) 1 d D U P A 1
H24A H 0.294877 0.067170 0.321568 0.056 Uiso 0.497(15) 1 calc R U P A 1
H24B H 0.371826 0.079098 0.417111 0.056 Uiso 0.497(15) 1 calc R U P A 1
H24C H 0.451892 0.063085 0.348519 0.056 Uiso 0.497(15) 1 calc R U P A 1
C25A C 0.3713(6) 0.1929(5) 0.2530(4) 0.0399(12) Uani 0.497(15) 1 d D U P A 1
H25A H 0.439106 0.161083 0.236542 0.060 Uiso 0.497(15) 1 calc R U P A 1
H25B H 0.384246 0.250371 0.243143 0.060 Uiso 0.497(15) 1 calc R U P A 1
H25C H 0.284413 0.176016 0.220170 0.060 Uiso 0.497(15) 1 calc R U P A 1
C26A C 0.2687(7) 0.2208(5) 0.3708(6) 0.0418(15) Uani 0.497(15) 1 d D U P A 1
H26A H 0.266541 0.278058 0.355596 0.063 Uiso 0.497(15) 1 calc R U P A 1
H26B H 0.281507 0.215807 0.431190 0.063 Uiso 0.497(15) 1 calc R U P A 1
H26C H 0.185568 0.195185 0.342279 0.063 Uiso 0.497(15) 1 calc R U P A 1
C23B C 0.4031(6) 0.1642(4) 0.3676(4) 0.0218(9) Uani 0.503(15) 1 d D U P A 2
C24B C 0.4174(7) 0.0745(3) 0.3930(5) 0.0334(12) Uani 0.503(15) 1 d D U P A 2
H24D H 0.339510 0.044683 0.362628 0.050 Uiso 0.503(15) 1 calc R U P A 2
H24E H 0.426173 0.069696 0.452973 0.050 Uiso 0.503(15) 1 calc R U P A 2
H24F H 0.495671 0.052014 0.379444 0.050 Uiso 0.503(15) 1 calc R U P A 2
C25B C 0.3785(5) 0.1677(4) 0.2735(4) 0.0336(11) Uani 0.503(15) 1 d D U P A 2
H25D H 0.457813 0.150592 0.257421 0.050 Uiso 0.503(15) 1 calc R U P A 2
H25E H 0.356208 0.223170 0.254346 0.050 Uiso 0.503(15) 1 calc R U P A 2
H25F H 0.305596 0.131644 0.247918 0.050 Uiso 0.503(15) 1 calc R U P A 2
C26B C 0.2847(7) 0.1983(5) 0.3942(5) 0.0403(14) Uani 0.503(15) 1 d D U P A 2
H26D H 0.273700 0.255578 0.378885 0.061 Uiso 0.503(15) 1 calc R U P A 2
H26E H 0.299139 0.192791 0.454597 0.061 Uiso 0.503(15) 1 calc R U P A 2
H26F H 0.205462 0.168495 0.366067 0.061 Uiso 0.503(15) 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
Ge1 N3 1.9236(11) . ?
Ge1 C1 2.1419(13) . ?
Ge1 C12 2.1502(14) . ?
Si1 N3 1.7060(13) . ?
Si1 C22 1.871(2) . ?
Si1 C21 1.8735(17) . ?
Si1 C12 1.8872(15) . ?
N1 C1 1.3487(16) . ?
N1 C3 1.398(2) . ?
N1 C6 1.470(2) . ?
C1 N2 1.3516(17) . ?
N2 C2 1.3905(19) . ?
N2 C9 1.4783(19) . ?
C2 C3 1.344(3) . ?
C2 C4 1.496(2) . ?
C3 C5 1.498(2) . ?
N3 C23B 1.400(6) . ?
N3 C23A 1.565(6) . ?
C6 C8 1.520(2) . ?
C6 C7 1.522(2) . ?
C9 C11 1.522(2) . ?
C9 C10 1.522(2) . ?
C12 C16 1.480(2) . ?
C12 C13 1.489(2) . ?
C13 C14 1.359(3) . ?
C13 C18 1.497(3) . ?
C14 C15 1.436(3) . ?
C14 C19 1.508(2) . ?
C15 C16 1.372(2) . ?
C15 C20 1.498(3) . ?
C16 C17 1.497(2) . ?
C23A C26A 1.515(7) . ?
C23A C24A 1.516(6) . ?
C23A C25A 1.525(6) . ?
C23B C25B 1.519(6) . ?
C23B C26B 1.530(7) . ?
C23B C24B 1.541(6) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N3 Ge1 C1 105.75(5) . . ?
N3 Ge1 C12 81.26(5) . . ?
C1 Ge1 C12 97.05(5) . . ?
N3 Si1 C22 115.92(12) . . ?
N3 Si1 C21 114.33(7) . . ?
C22 Si1 C21 102.42(11) . . ?
N3 Si1 C12 95.30(6) . . ?
C22 Si1 C12 114.44(8) . . ?
C21 Si1 C12 115.16(8) . . ?
C1 N1 C3 110.62(13) . . ?
C1 N1 C6 121.39(12) . . ?
C3 N1 C6 127.98(13) . . ?
N1 C1 N2 105.16(11) . . ?
N1 C1 Ge1 135.76(10) . . ?
N2 C1 Ge1 117.15(9) . . ?
C1 N2 C2 110.85(13) . . ?
C1 N2 C9 121.70(11) . . ?
C2 N2 C9 127.44(13) . . ?
C3 C2 N2 106.72(13) . . ?
C3 C2 C4 128.41(16) . . ?
N2 C2 C4 124.79(17) . . ?
C2 C3 N1 106.64(13) . . ?
C2 C3 C5 127.93(17) . . ?
N1 C3 C5 125.42(18) . . ?
C23B N3 Si1 124.9(3) . . ?
C23A N3 Si1 137.1(3) . . ?
C23B N3 Ge1 128.5(2) . . ?
C23A N3 Ge1 123.3(2) . . ?
Si1 N3 Ge1 98.03(6) . . ?
N1 C6 C8 111.49(13) . . ?
N1 C6 C7 111.96(16) . . ?
C8 C6 C7 112.19(16) . . ?
N2 C9 C11 112.85(14) . . ?
N2 C9 C10 110.17(13) . . ?
C11 C9 C10 113.50(13) . . ?
C16 C12 C13 103.58(13) . . ?
C16 C12 Si1 123.70(10) . . ?
C13 C12 Si1 119.43(12) . . ?
C16 C12 Ge1 120.04(10) . . ?
C13 C12 Ge1 102.91(10) . . ?
Si1 C12 Ge1 85.35(6) . . ?
C14 C13 C12 109.02(16) . . ?
C14 C13 C18 125.53(15) . . ?
C12 C13 C18 125.36(15) . . ?
C13 C14 C15 109.43(14) . . ?
C13 C14 C19 126.6(2) . . ?
C15 C14 C19 123.96(19) . . ?
C16 C15 C14 108.92(16) . . ?
C16 C15 C20 127.29(19) . . ?
C14 C15 C20 123.78(16) . . ?
C15 C16 C12 109.03(15) . . ?
C15 C16 C17 124.96(17) . . ?
C12 C16 C17 125.97(13) . . ?
C26A C23A C24A 109.4(5) . . ?
C26A C23A C25A 110.9(4) . . ?
C24A C23A C25A 107.8(4) . . ?
C26A C23A N3 108.6(4) . . ?
C24A C23A N3 108.4(3) . . ?
C25A C23A N3 111.9(4) . . ?
N3 C23B C25B 107.5(4) . . ?
N3 C23B C26B 109.3(5) . . ?
C25B C23B C26B 110.1(4) . . ?
N3 C23B C24B 114.8(3) . . ?
C25B C23B C24B 107.3(4) . . ?
C26B C23B C24B 107.9(4) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C3 N1 C1 N2 0.17(15) . . . . ?
C6 N1 C1 N2 -178.59(12) . . . . ?
C3 N1 C1 Ge1 -162.78(11) . . . . ?
C6 N1 C1 Ge1 18.5(2) . . . . ?
N1 C1 N2 C2 -0.68(15) . . . . ?
Ge1 C1 N2 C2 166.03(9) . . . . ?
N1 C1 N2 C9 -179.74(11) . . . . ?
Ge1 C1 N2 C9 -13.03(16) . . . . ?
C1 N2 C2 C3 0.95(16) . . . . ?
C9 N2 C2 C3 179.94(13) . . . . ?
C1 N2 C2 C4 -176.10(15) . . . . ?
C9 N2 C2 C4 2.9(2) . . . . ?
N2 C2 C3 N1 -0.79(16) . . . . ?
C4 C2 C3 N1 176.11(16) . . . . ?
N2 C2 C3 C5 -179.76(17) . . . . ?
C4 C2 C3 C5 -2.9(3) . . . . ?
C1 N1 C3 C2 0.41(17) . . . . ?
C6 N1 C3 C2 179.06(14) . . . . ?
C1 N1 C3 C5 179.41(17) . . . . ?
C6 N1 C3 C5 -1.9(3) . . . . ?
C22 Si1 N3 C23B 27.4(3) . . . . ?
C21 Si1 N3 C23B -91.4(3) . . . . ?
C12 Si1 N3 C23B 147.9(3) . . . . ?
C22 Si1 N3 C23A 42.6(4) . . . . ?
C21 Si1 N3 C23A -76.2(4) . . . . ?
C12 Si1 N3 C23A 163.1(4) . . . . ?
C22 Si1 N3 Ge1 -122.53(8) . . . . ?
C21 Si1 N3 Ge1 118.64(8) . . . . ?
C12 Si1 N3 Ge1 -2.07(7) . . . . ?
C1 N1 C6 C8 -117.17(18) . . . . ?
C3 N1 C6 C8 64.3(2) . . . . ?
C1 N1 C6 C7 116.22(15) . . . . ?
C3 N1 C6 C7 -62.31(19) . . . . ?
C1 N2 C9 C11 -130.80(14) . . . . ?
C2 N2 C9 C11 50.31(19) . . . . ?
C1 N2 C9 C10 101.19(15) . . . . ?
C2 N2 C9 C10 -77.70(18) . . . . ?
N3 Si1 C12 C16 125.17(12) . . . . ?
C22 Si1 C12 C16 -113.21(16) . . . . ?
C21 Si1 C12 C16 5.12(15) . . . . ?
N3 Si1 C12 C13 -100.38(12) . . . . ?
C22 Si1 C12 C13 21.25(18) . . . . ?
C21 Si1 C12 C13 139.57(13) . . . . ?
N3 Si1 C12 Ge1 1.84(6) . . . . ?
C22 Si1 C12 Ge1 123.46(12) . . . . ?
C21 Si1 C12 Ge1 -118.21(8) . . . . ?
C16 C12 C13 C14 -1.53(15) . . . . ?
Si1 C12 C13 C14 -143.87(11) . . . . ?
Ge1 C12 C13 C14 124.19(11) . . . . ?
C16 C12 C13 C18 -178.08(14) . . . . ?
Si1 C12 C13 C18 39.58(19) . . . . ?
Ge1 C12 C13 C18 -52.36(17) . . . . ?
C12 C13 C14 C15 1.47(17) . . . . ?
C18 C13 C14 C15 178.01(15) . . . . ?
C12 C13 C14 C19 -178.81(15) . . . . ?
C18 C13 C14 C19 -2.3(3) . . . . ?
C13 C14 C15 C16 -0.81(18) . . . . ?
C19 C14 C15 C16 179.46(15) . . . . ?
C13 C14 C15 C20 178.49(16) . . . . ?
C19 C14 C15 C20 -1.2(3) . . . . ?
C14 C15 C16 C12 -0.21(17) . . . . ?
C20 C15 C16 C12 -179.47(16) . . . . ?
C14 C15 C16 C17 177.38(15) . . . . ?
C20 C15 C16 C17 -1.9(3) . . . . ?
C13 C12 C16 C15 1.03(16) . . . . ?
Si1 C12 C16 C15 141.27(12) . . . . ?
Ge1 C12 C16 C15 -112.88(12) . . . . ?
C13 C12 C16 C17 -176.53(14) . . . . ?
Si1 C12 C16 C17 -36.3(2) . . . . ?
Ge1 C12 C16 C17 69.56(18) . . . . ?
Si1 N3 C23A C26A 51.1(5) . . . . ?
Ge1 N3 C23A C26A -146.6(3) . . . . ?
Si1 N3 C23A C24A -67.6(5) . . . . ?
Ge1 N3 C23A C24A 94.7(4) . . . . ?
Si1 N3 C23A C25A 173.8(3) . . . . ?
Ge1 N3 C23A C25A -23.9(5) . . . . ?
Si1 N3 C23B C25B -177.7(2) . . . . ?
Ge1 N3 C23B C25B -37.0(5) . . . . ?
Si1 N3 C23B C26B 62.9(4) . . . . ?
Ge1 N3 C23B C26B -156.4(3) . . . . ?
Si1 N3 C23B C24B -58.4(5) . . . . ?
Ge1 N3 C23B C24B 82.2(5) . . . . ?

_refine_diff_density_max         0.674
_refine_diff_density_min         -0.533
_refine_diff_density_rms         0.059



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

data_4786_a
_database_code_depnum_ccdc_archive 'CCDC 2174665'
loop_
_audit_author_name
_audit_author_address
'Bernd Morgenstern'
;Universitaet des Saarlandes
Germany
;
_audit_update_record             
;
2022-07-04 deposited with the CCDC.	2022-07-12 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C11 H19 N Si Sn'
_chemical_formula_sum            'C11 H19 N Si Sn'
_chemical_formula_weight         312.05

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Sn Sn -0.6537 1.4246 '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                   12.4653(5)
_cell_length_b                   9.4098(4)
_cell_length_c                   11.5289(5)
_cell_angle_alpha                90
_cell_angle_beta                 106.4120(10)
_cell_angle_gamma                90
_cell_volume                     1297.19(9)
_cell_formula_units_Z            4
_cell_measurement_temperature    133(2)
_cell_measurement_reflns_used    9977
_cell_measurement_theta_min      2.84
_cell_measurement_theta_max      27.88

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.598
_exptl_crystal_F_000             624
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.220
_exptl_crystal_size_mid          0.161
_exptl_crystal_size_min          0.080
_exptl_absorpt_coefficient_mu    2.028
_shelx_estimated_absorpt_T_min   0.664
_shelx_estimated_absorpt_T_max   0.855
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6690
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_process_details   
;
 SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D.,
 J. Appl. Cryst. 48 (2015) 3-10
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      133(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'INCOATEC I\^A?S microfocus sealed tube'
_diffrn_measurement_device_type  'Bruker AXS D8 Venture, Photon II'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            18869
_diffrn_reflns_av_unetI/netI     0.0269
_diffrn_reflns_av_R_equivalents  0.0406
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         2.755
_diffrn_reflns_theta_max         27.888
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             3099
_reflns_number_gt                2934
_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       'APEX 3 (Bruker, 2019)'
_computing_cell_refinement       'SAINT  (Bruker, 2019)'
_computing_data_reduction        'SAINT  (Bruker, 2019)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_computing_structure_refinement  
;
SHELXL-2018/3 (Sheldrick, 2018),                                              
SHELXLe Rev 1000 (Huebschle et al., 2011)
;
_computing_molecular_graphics    'DIAMOND, (Brandenburg, 2018)'
_computing_publication_material  'SHELXL-2018/3 (Sheldrick, 2018)'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0154P)²+0.5850P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         3099
_refine_ls_number_parameters     132
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0182
_refine_ls_R_factor_gt           0.0170
_refine_ls_wR_factor_ref         0.0433
_refine_ls_wR_factor_gt          0.0425
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_restrained_S_all      1.063
_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 0.41932(2) 0.44724(2) 0.82214(2) 0.01649(5) Uani 1 1 d . . . . .
C1 C 0.42762(13) 0.66657(16) 0.70332(14) 0.0183(3) Uani 1 1 d . . . . .
Si1 Si 0.27387(3) 0.64266(4) 0.63595(4) 0.01717(9) Uani 1 1 d . . . . .
N1 N 0.25508(10) 0.51509(14) 0.73595(12) 0.0164(2) Uani 1 1 d . . . . .
C4 C 0.59569(14) 0.72325(16) 0.84256(15) 0.0221(3) Uani 1 1 d . . . . .
H4 H 0.649120 0.761282 0.911373 0.026 Uiso 1 1 calc R U . . .
C3 C 0.61950(13) 0.64218(16) 0.74924(15) 0.0222(3) Uani 1 1 d . . . . .
H3 H 0.691733 0.615660 0.744700 0.027 Uiso 1 1 calc R U . . .
C2 C 0.51795(14) 0.60816(16) 0.66510(14) 0.0201(3) Uani 1 1 d . . . . .
H2 H 0.510110 0.554416 0.593428 0.024 Uiso 1 1 calc R U . . .
C8 C 0.15126(13) 0.44598(15) 0.74443(15) 0.0193(3) Uani 1 1 d . . . . .
C7 C 0.24739(16) 0.5829(2) 0.47553(16) 0.0284(4) Uani 1 1 d . . . . .
H7A H 0.291881 0.497721 0.472878 0.043 Uiso 1 1 calc R U . . .
H7B H 0.268617 0.658698 0.428045 0.043 Uiso 1 1 calc R U . . .
H7C H 0.167806 0.560954 0.441650 0.043 Uiso 1 1 calc R U . . .
C6 C 0.19655(16) 0.81415(18) 0.63111(17) 0.0285(4) Uani 1 1 d . . . . .
H6A H 0.200441 0.843881 0.713659 0.043 Uiso 1 1 calc R U . . .
H6B H 0.118161 0.801031 0.584780 0.043 Uiso 1 1 calc R U . . .
H6C H 0.230581 0.887284 0.592344 0.043 Uiso 1 1 calc R U . . .
C5 C 0.47901(13) 0.73737(16) 0.81521(14) 0.0194(3) Uani 1 1 d . . . . .
H5 H 0.440311 0.786166 0.863327 0.023 Uiso 1 1 calc R U . . .
C9 C 0.17593(14) 0.35898(19) 0.86135(15) 0.0256(3) Uani 1 1 d . . . . .
H9A H 0.208048 0.421103 0.930707 0.038 Uiso 1 1 calc R U . . .
H9B H 0.229179 0.283180 0.858960 0.038 Uiso 1 1 calc R U . . .
H9C H 0.106360 0.317022 0.869174 0.038 Uiso 1 1 calc R U . . .
C10 C 0.10316(14) 0.34782(19) 0.63612(16) 0.0268(3) Uani 1 1 d . . . . .
H10A H 0.033682 0.304756 0.643142 0.040 Uiso 1 1 calc R U . . .
H10B H 0.157399 0.272883 0.634817 0.040 Uiso 1 1 calc R U . . .
H10C H 0.087630 0.403067 0.561139 0.040 Uiso 1 1 calc R U . . .
C11 C 0.06410(15) 0.55923(19) 0.7495(2) 0.0318(4) Uani 1 1 d . . . . .
H11A H 0.096128 0.625183 0.816069 0.048 Uiso 1 1 calc R U . . .
H11B H -0.001972 0.513108 0.762676 0.048 Uiso 1 1 calc R U . . .
H11C H 0.042475 0.611726 0.672985 0.048 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Sn1 N1 2.1064(13) . ?
Sn1 C1 2.4954(15) . ?
Sn1 C5 2.8367(15) . ?
Sn1 C2 2.8879(15) . ?
C1 C2 1.430(2) . ?
C1 C5 1.432(2) . ?
C1 Si1 1.8671(16) . ?
Si1 N1 1.7256(13) . ?
Si1 C7 1.8710(18) . ?
Si1 C6 1.8723(17) . ?
N1 C8 1.4761(19) . ?
C4 C5 1.405(2) . ?
C4 C3 1.417(2) . ?
C3 C2 1.397(2) . ?
C8 C9 1.532(2) . ?
C8 C10 1.533(2) . ?
C8 C11 1.535(2) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Sn1 C1 71.09(5) . . ?
N1 Sn1 C5 85.57(5) . . ?
C1 Sn1 C5 30.31(5) . . ?
N1 Sn1 C2 94.27(5) . . ?
C1 Sn1 C2 29.68(5) . . ?
C5 Sn1 C2 46.86(4) . . ?
C2 C1 C5 105.40(13) . . ?
C2 C1 Si1 129.09(12) . . ?
C5 C1 Si1 125.18(12) . . ?
C2 C1 Sn1 90.55(9) . . ?
C5 C1 Sn1 88.15(9) . . ?
Si1 C1 Sn1 86.09(5) . . ?
N1 Si1 C1 97.07(6) . . ?
N1 Si1 C7 115.59(8) . . ?
C1 Si1 C7 108.73(8) . . ?
N1 Si1 C6 116.97(7) . . ?
C1 Si1 C6 111.58(8) . . ?
C7 Si1 C6 106.50(9) . . ?
C8 N1 Si1 129.63(10) . . ?
C8 N1 Sn1 126.06(10) . . ?
Si1 N1 Sn1 103.22(6) . . ?
C5 C4 C3 107.83(14) . . ?
C2 C3 C4 107.91(14) . . ?
C3 C2 C1 109.62(14) . . ?
C3 C2 Sn1 98.48(10) . . ?
C1 C2 Sn1 59.77(8) . . ?
N1 C8 C9 109.38(13) . . ?
N1 C8 C10 111.10(13) . . ?
C9 C8 C10 109.26(13) . . ?
N1 C8 C11 109.87(12) . . ?
C9 C8 C11 107.81(14) . . ?
C10 C8 C11 109.35(15) . . ?
C4 C5 C1 109.23(14) . . ?
C4 C5 Sn1 99.55(10) . . ?
C1 C5 Sn1 61.55(8) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C2 C1 Si1 N1 99.59(14) . . . . ?
C5 C1 Si1 N1 -72.90(14) . . . . ?
Sn1 C1 Si1 N1 12.06(6) . . . . ?
C2 C1 Si1 C7 -20.52(16) . . . . ?
C5 C1 Si1 C7 166.99(13) . . . . ?
Sn1 C1 Si1 C7 -108.05(7) . . . . ?
C2 C1 Si1 C6 -137.70(14) . . . . ?
C5 C1 Si1 C6 49.81(15) . . . . ?
Sn1 C1 Si1 C6 134.77(7) . . . . ?
C1 Si1 N1 C8 176.87(13) . . . . ?
C7 Si1 N1 C8 -68.41(15) . . . . ?
C6 Si1 N1 C8 58.26(16) . . . . ?
C1 Si1 N1 Sn1 -14.69(7) . . . . ?
C7 Si1 N1 Sn1 100.03(8) . . . . ?
C6 Si1 N1 Sn1 -133.31(8) . . . . ?
C5 C4 C3 C2 0.47(17) . . . . ?
C4 C3 C2 C1 -0.13(17) . . . . ?
C4 C3 C2 Sn1 -60.97(12) . . . . ?
C5 C1 C2 C3 -0.26(17) . . . . ?
Si1 C1 C2 C3 -173.89(11) . . . . ?
Sn1 C1 C2 C3 -88.49(12) . . . . ?
C5 C1 C2 Sn1 88.23(11) . . . . ?
Si1 C1 C2 Sn1 -85.41(12) . . . . ?
Si1 N1 C8 C9 -170.43(11) . . . . ?
Sn1 N1 C8 C9 23.54(17) . . . . ?
Si1 N1 C8 C10 68.86(17) . . . . ?
Sn1 N1 C8 C10 -97.17(14) . . . . ?
Si1 N1 C8 C11 -52.27(19) . . . . ?
Sn1 N1 C8 C11 141.69(13) . . . . ?
C3 C4 C5 C1 -0.64(17) . . . . ?
C3 C4 C5 Sn1 62.42(12) . . . . ?
C2 C1 C5 C4 0.55(17) . . . . ?
Si1 C1 C5 C4 174.51(11) . . . . ?
Sn1 C1 C5 C4 90.61(11) . . . . ?
C2 C1 C5 Sn1 -90.06(11) . . . . ?
Si1 C1 C5 Sn1 83.90(11) . . . . ?

_refine_diff_density_max         0.386
_refine_diff_density_min         -0.406
_refine_diff_density_rms         0.076



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

data_sh4900_a
_database_code_depnum_ccdc_archive 'CCDC 2174675'
loop_
_audit_author_name
_audit_author_address
'Bernd Morgenstern'
;Universitaet des Saarlandes
Germany
;
_audit_update_record             
;
2022-07-04 deposited with the CCDC.	2022-07-12 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C20 H27 Ge N O5 Si W'
_chemical_formula_sum            'C20 H27 Ge N O5 Si W'
_chemical_formula_weight         645.95

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'
Ge Ge 0.1547 1.8001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
W W -0.8490 6.8722 '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                   9.1997(4)
_cell_length_b                   26.2141(10)
_cell_length_c                   10.2037(4)
_cell_angle_alpha                90
_cell_angle_beta                 100.750(2)
_cell_angle_gamma                90
_cell_volume                     2417.56(17)
_cell_formula_units_Z            4
_cell_measurement_temperature    133(2)
_cell_measurement_reflns_used    9906
_cell_measurement_theta_min      2.38
_cell_measurement_theta_max      27.85

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.775
_exptl_crystal_F_000             1256
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.180
_exptl_crystal_size_min          0.030
_exptl_absorpt_coefficient_mu    6.075
_shelx_estimated_absorpt_T_min   0.376
_shelx_estimated_absorpt_T_max   0.839
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5176
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_process_details   
;
 SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D.,
 J. Appl. Cryst. 48 (2015) 3-10
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      133(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'INCOATEC I\^A?S microfocus sealed tube'
_diffrn_measurement_device_type  'Bruker AXS D8 Venture, Photon II'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            32787
_diffrn_reflns_av_unetI/netI     0.0263
_diffrn_reflns_av_R_equivalents  0.0382
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         2.175
_diffrn_reflns_theta_max         27.902
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             5770
_reflns_number_gt                4998
_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       'APEX 3 (Bruker, 2019)'
_computing_cell_refinement       'SAINT  (Bruker, 2019)'
_computing_data_reduction        'SAINT  (Bruker, 2019)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_computing_structure_refinement  
;
SHELXL-2018/3 (Sheldrick, 2018),                                              
SHELXLe Rev 1000 (Huebschle et al., 2011)
;
_computing_molecular_graphics    'DIAMOND, (Brandenburg, 2018)'
_computing_publication_material  'SHELXL-2018/3 (Sheldrick, 2018)'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0116P)²+2.4981P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         5770
_refine_ls_number_parameters     271
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0299
_refine_ls_R_factor_gt           0.0220
_refine_ls_wR_factor_ref         0.0453
_refine_ls_wR_factor_gt          0.0426
_refine_ls_goodness_of_fit_ref   1.078
_refine_ls_restrained_S_all      1.078
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_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
W1 W 0.58410(2) 0.30384(2) 0.41823(2) 0.02296(4) Uani 1 1 d . . . . .
Ge1 Ge 0.70092(3) 0.35822(2) 0.26120(3) 0.02372(7) Uani 1 1 d . . . . .
Si1 Si 0.84349(9) 0.41652(3) 0.10989(8) 0.03047(18) Uani 1 1 d . . . . .
O1 O 0.4477(3) 0.24254(10) 0.6321(3) 0.0493(6) Uani 1 1 d . . . . .
O2 O 0.8935(2) 0.30670(9) 0.6197(2) 0.0399(5) Uani 1 1 d . . . . .
O3 O 0.4781(3) 0.40458(9) 0.5463(3) 0.0475(6) Uani 1 1 d . . . . .
O4 O 0.2813(2) 0.29708(10) 0.2108(3) 0.0503(7) Uani 1 1 d . . . . .
O5 O 0.6911(3) 0.20165(10) 0.2970(3) 0.0572(8) Uani 1 1 d . . . . .
N1 N 0.7036(3) 0.36980(9) 0.0855(2) 0.0281(5) Uani 1 1 d . . . . .
C1 C 0.8447(3) 0.41699(10) 0.2951(3) 0.0261(6) Uani 1 1 d . . . . .
C2 C 0.7557(3) 0.45375(11) 0.3589(3) 0.0296(6) Uani 1 1 d . . . . .
C3 C 0.8198(3) 0.45796(11) 0.4906(3) 0.0306(6) Uani 1 1 d . . . . .
C4 C 0.9494(3) 0.42606(11) 0.5177(3) 0.0297(6) Uani 1 1 d . . . . .
C5 C 0.9671(3) 0.40189(11) 0.4038(3) 0.0273(6) Uani 1 1 d . . . . .
C6 C 1.0871(3) 0.36429(13) 0.3897(3) 0.0384(8) Uani 1 1 d . . . . .
H6A H 1.130186 0.350458 0.477626 0.058 Uiso 1 1 calc R U . . .
H6B H 1.164197 0.381542 0.351766 0.058 Uiso 1 1 calc R U . . .
H6C H 1.044910 0.336429 0.330643 0.058 Uiso 1 1 calc R U . . .
C7 C 1.0463(4) 0.42190(14) 0.6526(3) 0.0455(9) Uani 1 1 d . . . . .
H7A H 0.988502 0.408485 0.716496 0.068 Uiso 1 1 calc R U . . .
H7B H 1.084955 0.455694 0.681831 0.068 Uiso 1 1 calc R U . . .
H7C H 1.128922 0.398790 0.647876 0.068 Uiso 1 1 calc R U . . .
C8 C 0.7682(4) 0.49096(13) 0.5929(4) 0.0463(9) Uani 1 1 d . . . . .
H8A H 0.848656 0.513663 0.633612 0.070 Uiso 1 1 calc R U . . .
H8B H 0.738813 0.469385 0.661961 0.070 Uiso 1 1 calc R U . . .
H8C H 0.683324 0.511389 0.549974 0.070 Uiso 1 1 calc R U . . .
C9 C 0.6190(4) 0.48099(13) 0.2897(4) 0.0441(8) Uani 1 1 d . . . . .
H9A H 0.646644 0.514070 0.256879 0.066 Uiso 1 1 calc R U . . .
H9B H 0.551953 0.486312 0.352658 0.066 Uiso 1 1 calc R U . . .
H9C H 0.569282 0.460365 0.214437 0.066 Uiso 1 1 calc R U . . .
C10 C 0.7902(4) 0.47772(13) 0.0207(4) 0.0485(9) Uani 1 1 d . . . . .
H10A H 0.854967 0.505121 0.062901 0.073 Uiso 1 1 calc R U . . .
H10B H 0.687275 0.485876 0.025203 0.073 Uiso 1 1 calc R U . . .
H10C H 0.800331 0.474347 -0.072799 0.073 Uiso 1 1 calc R U . . .
C11 C 1.0215(4) 0.39528(14) 0.0649(3) 0.0429(8) Uani 1 1 d . . . . .
H11A H 1.041455 0.359881 0.093542 0.064 Uiso 1 1 calc R U . . .
H11B H 1.102038 0.417203 0.109379 0.064 Uiso 1 1 calc R U . . .
H11C H 1.014384 0.397598 -0.031983 0.064 Uiso 1 1 calc R U . . .
C12 C 0.6149(4) 0.34772(13) -0.0375(3) 0.0352(7) Uani 1 1 d . . . . .
C13 C 0.4796(4) 0.38112(16) -0.0817(4) 0.0614(12) Uani 1 1 d . . . . .
H13A H 0.418527 0.381077 -0.012632 0.092 Uiso 1 1 calc R U . . .
H13B H 0.421829 0.367753 -0.165106 0.092 Uiso 1 1 calc R U . . .
H13C H 0.511190 0.416063 -0.095956 0.092 Uiso 1 1 calc R U . . .
C14 C 0.5675(4) 0.29354(13) -0.0117(3) 0.0411(8) Uani 1 1 d . . . . .
H14A H 0.504524 0.294107 0.055861 0.062 Uiso 1 1 calc R U . . .
H14B H 0.655378 0.272676 0.020306 0.062 Uiso 1 1 calc R U . . .
H14C H 0.512222 0.278976 -0.094636 0.062 Uiso 1 1 calc R U . . .
C15 C 0.7106(5) 0.34600(18) -0.1452(3) 0.0584(11) Uani 1 1 d . . . . .
H15A H 0.797873 0.324720 -0.114478 0.088 Uiso 1 1 calc R U . . .
H15B H 0.742103 0.380644 -0.162796 0.088 Uiso 1 1 calc R U . . .
H15C H 0.653003 0.331535 -0.227300 0.088 Uiso 1 1 calc R U . . .
C16 C 0.4969(3) 0.26426(12) 0.5535(3) 0.0322(7) Uani 1 1 d . . . . .
C17 C 0.7834(3) 0.30675(11) 0.5470(3) 0.0274(6) Uani 1 1 d . . . . .
C18 C 0.5161(3) 0.36921(12) 0.4975(3) 0.0304(6) Uani 1 1 d . . . . .
C19 C 0.3893(3) 0.29993(11) 0.2851(3) 0.0318(7) Uani 1 1 d . . . . .
C20 C 0.6531(3) 0.23797(12) 0.3402(3) 0.0336(7) Uani 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
W1 C16 2.009(3) . ?
W1 C19 2.039(3) . ?
W1 C18 2.042(3) . ?
W1 C17 2.048(3) . ?
W1 C20 2.051(3) . ?
W1 Ge1 2.5293(3) . ?
Ge1 N1 1.823(2) . ?
Ge1 C1 2.018(3) . ?
Si1 N1 1.760(3) . ?
Si1 C10 1.864(3) . ?
Si1 C11 1.866(3) . ?
Si1 C1 1.888(3) . ?
O1 C16 1.144(4) . ?
O2 C17 1.139(3) . ?
O3 C18 1.138(4) . ?
O4 C19 1.135(4) . ?
O5 C20 1.131(4) . ?
N1 C12 1.481(4) . ?
C1 C5 1.479(4) . ?
C1 C2 1.491(4) . ?
C2 C3 1.367(4) . ?
C2 C9 1.503(4) . ?
C3 C4 1.440(4) . ?
C3 C8 1.500(4) . ?
C4 C5 1.359(4) . ?
C4 C7 1.499(4) . ?
C5 C6 1.507(4) . ?
C12 C13 1.520(5) . ?
C12 C14 1.523(4) . ?
C12 C15 1.532(5) . ?

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
C16 W1 C19 91.01(12) . . ?
C16 W1 C18 88.30(12) . . ?
C19 W1 C18 90.58(12) . . ?
C16 W1 C17 90.17(12) . . ?
C19 W1 C17 178.03(12) . . ?
C18 W1 C17 91.04(12) . . ?
C16 W1 C20 91.36(13) . . ?
C19 W1 C20 89.80(11) . . ?
C18 W1 C20 179.50(12) . . ?
C17 W1 C20 88.59(11) . . ?
C16 W1 Ge1 175.86(9) . . ?
C19 W1 Ge1 91.77(9) . . ?
C18 W1 Ge1 88.61(9) . . ?
C17 W1 Ge1 87.14(8) . . ?
C20 W1 Ge1 91.71(9) . . ?
N1 Ge1 C1 84.99(11) . . ?
N1 Ge1 W1 143.34(8) . . ?
C1 Ge1 W1 131.62(8) . . ?
N1 Si1 C10 114.27(15) . . ?
N1 Si1 C11 114.18(14) . . ?
C10 Si1 C11 107.43(17) . . ?
N1 Si1 C1 90.79(12) . . ?
C10 Si1 C1 115.78(15) . . ?
C11 Si1 C1 113.99(15) . . ?
C12 N1 Si1 131.6(2) . . ?
C12 N1 Ge1 131.4(2) . . ?
Si1 N1 Ge1 96.93(11) . . ?
C5 C1 C2 104.4(2) . . ?
C5 C1 Si1 127.7(2) . . ?
C2 C1 Si1 122.7(2) . . ?
C5 C1 Ge1 107.88(19) . . ?
C2 C1 Ge1 99.90(18) . . ?
Si1 C1 Ge1 86.68(12) . . ?
C3 C2 C1 108.0(3) . . ?
C3 C2 C9 126.4(3) . . ?
C1 C2 C9 125.6(3) . . ?
C2 C3 C4 109.4(3) . . ?
C2 C3 C8 126.6(3) . . ?
C4 C3 C8 124.0(3) . . ?
C5 C4 C3 109.5(3) . . ?
C5 C4 C7 127.3(3) . . ?
C3 C4 C7 123.2(3) . . ?
C4 C5 C1 108.7(3) . . ?
C4 C5 C6 126.4(3) . . ?
C1 C5 C6 124.9(3) . . ?
N1 C12 C13 108.5(3) . . ?
N1 C12 C14 110.4(3) . . ?
C13 C12 C14 110.1(3) . . ?
N1 C12 C15 108.7(3) . . ?
C13 C12 C15 110.6(3) . . ?
C14 C12 C15 108.5(3) . . ?
O1 C16 W1 178.6(3) . . ?
O2 C17 W1 177.7(3) . . ?
O3 C18 W1 177.3(3) . . ?
O4 C19 W1 179.1(3) . . ?
O5 C20 W1 179.9(4) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C10 Si1 N1 C12 53.7(3) . . . . ?
C11 Si1 N1 C12 -70.5(3) . . . . ?
C1 Si1 N1 C12 172.6(3) . . . . ?
C10 Si1 N1 Ge1 -125.31(16) . . . . ?
C11 Si1 N1 Ge1 110.45(15) . . . . ?
C1 Si1 N1 Ge1 -6.41(13) . . . . ?
C1 Ge1 N1 C12 -173.0(3) . . . . ?
W1 Ge1 N1 C12 4.3(4) . . . . ?
C1 Ge1 N1 Si1 6.02(12) . . . . ?
W1 Ge1 N1 Si1 -176.73(4) . . . . ?
N1 Si1 C1 C5 115.9(3) . . . . ?
C10 Si1 C1 C5 -126.6(3) . . . . ?
C11 Si1 C1 C5 -1.2(3) . . . . ?
N1 Si1 C1 C2 -93.9(2) . . . . ?
C10 Si1 C1 C2 23.7(3) . . . . ?
C11 Si1 C1 C2 149.1(2) . . . . ?
N1 Si1 C1 Ge1 5.75(11) . . . . ?
C10 Si1 C1 Ge1 123.34(15) . . . . ?
C11 Si1 C1 Ge1 -111.27(15) . . . . ?
C5 C1 C2 C3 -1.2(3) . . . . ?
Si1 C1 C2 C3 -157.2(2) . . . . ?
Ge1 C1 C2 C3 110.3(2) . . . . ?
C5 C1 C2 C9 179.1(3) . . . . ?
Si1 C1 C2 C9 23.0(4) . . . . ?
Ge1 C1 C2 C9 -69.4(3) . . . . ?
C1 C2 C3 C4 0.7(3) . . . . ?
C9 C2 C3 C4 -179.6(3) . . . . ?
C1 C2 C3 C8 179.6(3) . . . . ?
C9 C2 C3 C8 -0.7(5) . . . . ?
C2 C3 C4 C5 0.0(3) . . . . ?
C8 C3 C4 C5 -178.9(3) . . . . ?
C2 C3 C4 C7 179.7(3) . . . . ?
C8 C3 C4 C7 0.8(5) . . . . ?
C3 C4 C5 C1 -0.8(3) . . . . ?
C7 C4 C5 C1 179.5(3) . . . . ?
C3 C4 C5 C6 -178.6(3) . . . . ?
C7 C4 C5 C6 1.7(5) . . . . ?
C2 C1 C5 C4 1.2(3) . . . . ?
Si1 C1 C5 C4 155.7(2) . . . . ?
Ge1 C1 C5 C4 -104.4(2) . . . . ?
C2 C1 C5 C6 179.1(3) . . . . ?
Si1 C1 C5 C6 -26.5(4) . . . . ?
Ge1 C1 C5 C6 73.4(3) . . . . ?
Si1 N1 C12 C13 -87.3(3) . . . . ?
Ge1 N1 C12 C13 91.4(3) . . . . ?
Si1 N1 C12 C14 151.9(2) . . . . ?
Ge1 N1 C12 C14 -29.4(4) . . . . ?
Si1 N1 C12 C15 33.0(4) . . . . ?
Ge1 N1 C12 C15 -148.3(3) . . . . ?

_refine_diff_density_max         0.557
_refine_diff_density_min         -0.991
_refine_diff_density_rms         0.098



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

data_sh4573_a
_database_code_depnum_ccdc_archive 'CCDC 2174664'
loop_
_audit_author_name
_audit_author_address
'Bernd Morgenstern'
;Universitaet des Saarlandes
Germany
;
_audit_update_record             
;
2022-07-04 deposited with the CCDC.	2022-07-12 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C15 H27 N Pb Si'
_chemical_formula_sum            'C15 H27 N Pb Si'
_chemical_formula_weight         456.65

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -3.3944 10.1111 '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                   10.7347(2)
_cell_length_b                   18.9400(4)
_cell_length_c                   17.5783(4)
_cell_angle_alpha                90
_cell_angle_beta                 104.5410(10)
_cell_angle_gamma                90
_cell_volume                     3459.46(13)
_cell_formula_units_Z            8
_cell_measurement_temperature    133(2)
_cell_measurement_reflns_used    9987
_cell_measurement_theta_min      2.29
_cell_measurement_theta_max      27.88

_exptl_crystal_description       block
_exptl_crystal_colour            red
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.754
_exptl_crystal_F_000             1760
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.149
_exptl_crystal_size_mid          0.135
_exptl_crystal_size_min          0.100
_exptl_absorpt_coefficient_mu    9.809
_shelx_estimated_absorpt_T_min   0.323
_shelx_estimated_absorpt_T_max   0.440
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5699
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_process_details   
;
 SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D.,
 J. Appl. Cryst. 48 (2015) 3-10
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      133(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'INCOATEC I\^A?S microfocus sealed tube'
_diffrn_measurement_device_type  'Bruker AXS D8 Venture, Photon II'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            57554
_diffrn_reflns_av_unetI/netI     0.0202
_diffrn_reflns_av_R_equivalents  0.0350
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         2.151
_diffrn_reflns_theta_max         27.890
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             8246
_reflns_number_gt                7379
_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       'APEX 3 (Bruker Nano, Inc., 2019)'
_computing_cell_refinement       'SAINT V8.40A (Bruker Nano, Inc., 2019)'
_computing_data_reduction        'SAINT V8.40A (Bruker Nano, Inc., 2019)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_computing_structure_refinement  
;
SHELXL-2018/3 (Sheldrick, 2018),                                              
SHELXLe Rev 1000 (Huebschle et al., 2011)
;
_computing_molecular_graphics    'DIAMOND, (Brandenburg, 2018)'
_computing_publication_material  'SHELXL-2018/3 (Sheldrick, 2018)'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0106P)²+3.2959P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         8246
_refine_ls_number_parameters     344
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0218
_refine_ls_R_factor_gt           0.0169
_refine_ls_wR_factor_ref         0.0349
_refine_ls_wR_factor_gt          0.0336
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_restrained_S_all      1.026
_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
Pb1 Pb 0.57443(2) 0.14773(2) 0.38008(2) 0.01964(3) Uani 1 1 d . . . . .
Si1 Si 0.63693(7) 0.30002(3) 0.43751(4) 0.01966(13) Uani 1 1 d . . . . .
N1 N 0.7170(2) 0.22071(10) 0.45281(12) 0.0204(4) Uani 1 1 d . . . . .
C1 C 0.4913(2) 0.27105(12) 0.35997(14) 0.0181(5) Uani 1 1 d . . . . .
C2 C 0.4879(2) 0.25950(12) 0.27782(14) 0.0188(5) Uani 1 1 d . . . . .
C3 C 0.3641(3) 0.23590(13) 0.23910(15) 0.0230(5) Uani 1 1 d . . . . .
C4 C 0.2913(2) 0.22854(13) 0.29531(16) 0.0243(5) Uani 1 1 d . . . . .
C5 C 0.3664(2) 0.24881(12) 0.36895(15) 0.0210(5) Uani 1 1 d . . . . .
C6 C 0.3238(3) 0.24534(15) 0.44419(17) 0.0308(6) Uani 1 1 d . . . . .
H6A H 0.291307 0.291647 0.455031 0.046 Uiso 1 1 calc R U . . .
H6B H 0.396959 0.232063 0.487550 0.046 Uiso 1 1 calc R U . . .
H6C H 0.255375 0.210070 0.438966 0.046 Uiso 1 1 calc R U . . .
C7 C 0.1555(3) 0.20068(16) 0.2775(2) 0.0380(7) Uani 1 1 d . . . . .
H7A H 0.095471 0.238157 0.253543 0.057 Uiso 1 1 calc R U . . .
H7B H 0.135929 0.184973 0.326325 0.057 Uiso 1 1 calc R U . . .
H7C H 0.146915 0.160801 0.241016 0.057 Uiso 1 1 calc R U . . .
C8 C 0.3149(3) 0.22223(16) 0.15268(17) 0.0377(7) Uani 1 1 d . . . . .
H8A H 0.256776 0.260497 0.128648 0.057 Uiso 1 1 calc R U . . .
H8B H 0.268188 0.177279 0.144647 0.057 Uiso 1 1 calc R U . . .
H8C H 0.387465 0.219990 0.128304 0.057 Uiso 1 1 calc R U . . .
C9 C 0.5916(3) 0.28076(14) 0.23824(16) 0.0267(6) Uani 1 1 d . . . . .
H9A H 0.579413 0.255361 0.188331 0.040 Uiso 1 1 calc R U . . .
H9B H 0.676179 0.269030 0.272446 0.040 Uiso 1 1 calc R U . . .
H9C H 0.586736 0.331712 0.228209 0.040 Uiso 1 1 calc R U . . .
C10 C 0.5920(3) 0.33813(17) 0.52531(17) 0.0361(7) Uani 1 1 d . . . . .
H10A H 0.524466 0.373698 0.508061 0.054 Uiso 1 1 calc R U . . .
H10B H 0.667724 0.360183 0.560112 0.054 Uiso 1 1 calc R U . . .
H10C H 0.560159 0.300436 0.553685 0.054 Uiso 1 1 calc R U . . .
C11 C 0.7241(3) 0.37449(15) 0.40326(19) 0.0370(7) Uani 1 1 d . . . . .
H11A H 0.761179 0.357877 0.360928 0.055 Uiso 1 1 calc R U . . .
H11B H 0.792966 0.391501 0.447182 0.055 Uiso 1 1 calc R U . . .
H11C H 0.663593 0.413046 0.383745 0.055 Uiso 1 1 calc R U . . .
C12 C 0.8435(3) 0.20256(15) 0.50450(17) 0.0285(6) Uani 1 1 d . . . . .
C13 C 0.8568(3) 0.12260(17) 0.5056(2) 0.0511(9) Uani 1 1 d . . . . .
H13A H 0.788997 0.101579 0.526667 0.077 Uiso 1 1 calc R U . . .
H13B H 0.941200 0.109289 0.538832 0.077 Uiso 1 1 calc R U . . .
H13C H 0.848668 0.105403 0.451988 0.077 Uiso 1 1 calc R U . . .
C14 C 0.9503(3) 0.2324(2) 0.4710(3) 0.0657(12) Uani 1 1 d . . . . .
H14A H 0.938696 0.215849 0.416834 0.099 Uiso 1 1 calc R U . . .
H14B H 1.033890 0.216349 0.502995 0.099 Uiso 1 1 calc R U . . .
H14C H 0.946964 0.284057 0.471613 0.099 Uiso 1 1 calc R U . . .
C15 C 0.8544(4) 0.2274(3) 0.5871(2) 0.0851(18) Uani 1 1 d . . . . .
H15A H 0.851793 0.279106 0.588056 0.128 Uiso 1 1 calc R U . . .
H15B H 0.936000 0.210919 0.621285 0.128 Uiso 1 1 calc R U . . .
H15C H 0.782674 0.208370 0.605920 0.128 Uiso 1 1 calc R U . . .
Pb2 Pb 0.34297(2) 0.40296(2) 0.27494(2) 0.02395(3) Uani 1 1 d . . . . .
Si2 Si 0.17369(6) 0.53450(3) 0.23284(4) 0.01799(13) Uani 1 1 d . . . . .
N2 N 0.2023(2) 0.47511(11) 0.30904(13) 0.0235(5) Uani 1 1 d . . . . .
C16 C 0.3161(2) 0.51291(12) 0.19280(14) 0.0181(5) Uani 1 1 d . . . . .
C17 C 0.4487(2) 0.52155(12) 0.24044(15) 0.0185(5) Uani 1 1 d . . . . .
C18 C 0.5324(2) 0.49162(12) 0.19893(16) 0.0220(5) Uani 1 1 d . . . . .
C19 C 0.4588(3) 0.46246(12) 0.12840(16) 0.0230(5) Uani 1 1 d . . . . .
C20 C 0.3275(3) 0.47367(12) 0.12435(15) 0.0219(5) Uani 1 1 d . . . . .
C21 C 0.2199(3) 0.44839(15) 0.05725(17) 0.0321(6) Uani 1 1 d . . . . .
H21A H 0.235825 0.463998 0.007365 0.048 Uiso 1 1 calc R U . . .
H21B H 0.138098 0.468016 0.062611 0.048 Uiso 1 1 calc R U . . .
H21C H 0.215916 0.396714 0.058109 0.048 Uiso 1 1 calc R U . . .
C22 C 0.5108(3) 0.42348(15) 0.06849(18) 0.0347(7) Uani 1 1 d . . . . .
H22A H 0.446346 0.423533 0.017898 0.052 Uiso 1 1 calc R U . . .
H22B H 0.530595 0.374689 0.085938 0.052 Uiso 1 1 calc R U . . .
H22C H 0.589306 0.446802 0.062587 0.052 Uiso 1 1 calc R U . . .
C23 C 0.6766(3) 0.49425(15) 0.22281(19) 0.0325(6) Uani 1 1 d . . . . .
H23A H 0.711303 0.447703 0.215073 0.049 Uiso 1 1 calc R U . . .
H23B H 0.705394 0.507544 0.278346 0.049 Uiso 1 1 calc R U . . .
H23C H 0.707198 0.529227 0.190638 0.049 Uiso 1 1 calc R U . . .
C24 C 0.4894(3) 0.56260(13) 0.31597(16) 0.0252(5) Uani 1 1 d . . . . .
H24A H 0.494559 0.612907 0.304077 0.038 Uiso 1 1 calc R U . . .
H24B H 0.573850 0.545950 0.346013 0.038 Uiso 1 1 calc R U . . .
H24C H 0.426172 0.555676 0.346993 0.038 Uiso 1 1 calc R U . . .
C25 C 0.0139(3) 0.52112(15) 0.16065(17) 0.0314(6) Uani 1 1 d . . . . .
H25A H 0.009736 0.549976 0.113811 0.047 Uiso 1 1 calc R U . . .
H25B H -0.055275 0.535179 0.184821 0.047 Uiso 1 1 calc R U . . .
H25C H 0.003674 0.471214 0.145650 0.047 Uiso 1 1 calc R U . . .
C26 C 0.1767(3) 0.63038(13) 0.25962(16) 0.0245(5) Uani 1 1 d . . . . .
H26A H 0.166932 0.659150 0.212142 0.037 Uiso 1 1 calc R U . . .
H26B H 0.258832 0.641598 0.296799 0.037 Uiso 1 1 calc R U . . .
H26C H 0.105872 0.640538 0.283918 0.037 Uiso 1 1 calc R U . . .
C27 C 0.1335(3) 0.45912(15) 0.36917(19) 0.0333(7) Uani 1 1 d . . . . .
C28 C 0.0444(3) 0.51986(18) 0.3790(2) 0.0473(9) Uani 1 1 d . . . . .
H28A H -0.021880 0.526593 0.329855 0.071 Uiso 1 1 calc R U . . .
H28B H 0.094783 0.563314 0.392097 0.071 Uiso 1 1 calc R U . . .
H28C H 0.003323 0.508491 0.421389 0.071 Uiso 1 1 calc R U . . .
C29 C 0.0538(4) 0.39212(18) 0.3467(3) 0.0537(10) Uani 1 1 d . . . . .
H29A H -0.009624 0.399441 0.296472 0.081 Uiso 1 1 calc R U . . .
H29B H 0.009298 0.381029 0.387518 0.081 Uiso 1 1 calc R U . . .
H29C H 0.110679 0.352864 0.341614 0.081 Uiso 1 1 calc R U . . .
C30 C 0.2328(4) 0.4481(2) 0.4482(2) 0.0519(9) Uani 1 1 d . . . . .
H30A H 0.290812 0.409411 0.443274 0.078 Uiso 1 1 calc R U . . .
H30B H 0.188119 0.436471 0.488793 0.078 Uiso 1 1 calc R U . . .
H30C H 0.282741 0.491552 0.462833 0.078 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
Pb1 N1 2.215(2) . ?
Pb1 C1 2.494(2) . ?
Pb1 C2 2.781(2) . ?
Pb1 C5 2.910(2) . ?
Si1 N1 1.718(2) . ?
Si1 C11 1.873(3) . ?
Si1 C10 1.874(3) . ?
Si1 C1 1.880(2) . ?
N1 C12 1.473(3) . ?
C1 C5 1.451(3) . ?
C1 C2 1.452(3) . ?
C2 C3 1.405(4) . ?
C2 C9 1.508(3) . ?
C3 C4 1.413(4) . ?
C3 C8 1.500(4) . ?
C4 C5 1.396(4) . ?
C4 C7 1.507(4) . ?
C5 C6 1.506(4) . ?
C12 C15 1.503(5) . ?
C12 C13 1.521(4) . ?
C12 C14 1.522(5) . ?
Pb2 N2 2.228(2) . ?
Pb2 C16 2.509(2) . ?
Pb2 C17 2.654(2) . ?
Pb2 C20 2.934(3) . ?
Si2 N2 1.717(2) . ?
Si2 C26 1.874(2) . ?
Si2 C25 1.877(3) . ?
Si2 C16 1.881(2) . ?
N2 C27 1.465(3) . ?
C16 C20 1.445(3) . ?
C16 C17 1.468(3) . ?
C17 C18 1.411(3) . ?
C17 C24 1.506(3) . ?
C18 C19 1.405(4) . ?
C18 C23 1.499(3) . ?
C19 C20 1.409(4) . ?
C19 C22 1.504(3) . ?
C20 C21 1.507(4) . ?
C27 C29 1.526(4) . ?
C27 C28 1.533(4) . ?
C27 C30 1.538(5) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Pb1 C1 70.62(7) . . ?
N1 Pb1 C2 88.18(7) . . ?
C1 Pb1 C2 31.36(7) . . ?
N1 Pb1 C5 92.04(7) . . ?
C1 Pb1 C5 29.89(7) . . ?
C2 Pb1 C5 47.93(7) . . ?
N1 Si1 C11 115.98(13) . . ?
N1 Si1 C10 115.48(13) . . ?
C11 Si1 C10 103.14(15) . . ?
N1 Si1 C1 98.67(10) . . ?
C11 Si1 C1 112.22(12) . . ?
C10 Si1 C1 111.74(12) . . ?
C12 N1 Si1 130.42(17) . . ?
C12 N1 Pb1 127.38(16) . . ?
Si1 N1 Pb1 102.08(10) . . ?
C5 C1 C2 105.8(2) . . ?
C5 C1 Si1 128.97(19) . . ?
C2 C1 Si1 124.99(18) . . ?
C5 C1 Pb1 91.15(14) . . ?
C2 C1 Pb1 85.32(13) . . ?
Si1 C1 Pb1 88.15(9) . . ?
C3 C2 C1 108.3(2) . . ?
C3 C2 C9 125.4(2) . . ?
C1 C2 C9 125.6(2) . . ?
C3 C2 Pb1 101.10(15) . . ?
C1 C2 Pb1 63.33(12) . . ?
C9 C2 Pb1 109.64(15) . . ?
C2 C3 C4 108.4(2) . . ?
C2 C3 C8 126.5(3) . . ?
C4 C3 C8 125.1(3) . . ?
C5 C4 C3 109.2(2) . . ?
C5 C4 C7 126.3(3) . . ?
C3 C4 C7 124.4(3) . . ?
C4 C5 C1 108.3(2) . . ?
C4 C5 C6 124.8(2) . . ?
C1 C5 C6 126.9(2) . . ?
C4 C5 Pb1 97.84(15) . . ?
C1 C5 Pb1 58.95(12) . . ?
C6 C5 Pb1 108.03(16) . . ?
N1 C12 C15 111.1(2) . . ?
N1 C12 C13 108.0(2) . . ?
C15 C12 C13 108.4(3) . . ?
N1 C12 C14 110.0(2) . . ?
C15 C12 C14 112.0(3) . . ?
C13 C12 C14 107.3(3) . . ?
N2 Pb2 C16 70.00(8) . . ?
N2 Pb2 C17 84.26(7) . . ?
C16 Pb2 C17 32.88(7) . . ?
N2 Pb2 C20 94.25(7) . . ?
C16 Pb2 C20 29.50(7) . . ?
C17 Pb2 C20 48.56(7) . . ?
N2 Si2 C26 116.77(12) . . ?
N2 Si2 C25 113.12(12) . . ?
C26 Si2 C25 104.82(12) . . ?
N2 Si2 C16 98.44(10) . . ?
C26 Si2 C16 109.89(11) . . ?
C25 Si2 C16 114.10(12) . . ?
C27 N2 Si2 132.44(18) . . ?
C27 N2 Pb2 124.47(16) . . ?
Si2 N2 Pb2 101.09(10) . . ?
C20 C16 C17 105.1(2) . . ?
C20 C16 Si2 132.04(19) . . ?
C17 C16 Si2 121.65(18) . . ?
C20 C16 Pb2 91.76(14) . . ?
C17 C16 Pb2 79.00(13) . . ?
Si2 C16 Pb2 87.24(9) . . ?
C18 C17 C16 108.2(2) . . ?
C18 C17 C24 125.6(2) . . ?
C16 C17 C24 125.9(2) . . ?
C18 C17 Pb2 98.19(14) . . ?
C16 C17 Pb2 68.12(12) . . ?
C24 C17 Pb2 106.35(15) . . ?
C19 C18 C17 108.9(2) . . ?
C19 C18 C23 124.9(2) . . ?
C17 C18 C23 126.1(2) . . ?
C18 C19 C20 108.6(2) . . ?
C18 C19 C22 125.8(2) . . ?
C20 C19 C22 125.5(3) . . ?
C19 C20 C16 109.2(2) . . ?
C19 C20 C21 123.5(2) . . ?
C16 C20 C21 127.4(2) . . ?
C19 C20 Pb2 93.23(16) . . ?
C16 C20 Pb2 58.74(13) . . ?
C21 C20 Pb2 114.84(17) . . ?
N2 C27 C29 109.6(3) . . ?
N2 C27 C28 111.6(2) . . ?
C29 C27 C28 109.2(3) . . ?
N2 C27 C30 108.6(2) . . ?
C29 C27 C30 109.7(3) . . ?
C28 C27 C30 108.1(3) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C11 Si1 N1 C12 57.5(3) . . . . ?
C10 Si1 N1 C12 -63.3(3) . . . . ?
C1 Si1 N1 C12 177.5(2) . . . . ?
C11 Si1 N1 Pb1 -126.36(13) . . . . ?
C10 Si1 N1 Pb1 112.82(13) . . . . ?
C1 Si1 N1 Pb1 -6.37(12) . . . . ?
N1 Si1 C1 C5 95.5(2) . . . . ?
C11 Si1 C1 C5 -141.7(2) . . . . ?
C10 Si1 C1 C5 -26.4(3) . . . . ?
N1 Si1 C1 C2 -77.4(2) . . . . ?
C11 Si1 C1 C2 45.3(2) . . . . ?
C10 Si1 C1 C2 160.6(2) . . . . ?
N1 Si1 C1 Pb1 5.53(10) . . . . ?
C11 Si1 C1 Pb1 128.28(12) . . . . ?
C10 Si1 C1 Pb1 -116.42(12) . . . . ?
C5 C1 C2 C3 3.6(3) . . . . ?
Si1 C1 C2 C3 177.93(17) . . . . ?
Pb1 C1 C2 C3 93.49(17) . . . . ?
C5 C1 C2 C9 174.2(2) . . . . ?
Si1 C1 C2 C9 -11.5(3) . . . . ?
Pb1 C1 C2 C9 -95.9(2) . . . . ?
C5 C1 C2 Pb1 -89.88(16) . . . . ?
Si1 C1 C2 Pb1 84.44(16) . . . . ?
C1 C2 C3 C4 -3.1(3) . . . . ?
C9 C2 C3 C4 -173.8(2) . . . . ?
Pb1 C2 C3 C4 62.2(2) . . . . ?
C1 C2 C3 C8 175.5(2) . . . . ?
C9 C2 C3 C8 4.9(4) . . . . ?
Pb1 C2 C3 C8 -119.2(2) . . . . ?
C2 C3 C4 C5 1.4(3) . . . . ?
C8 C3 C4 C5 -177.3(2) . . . . ?
C2 C3 C4 C7 -176.7(2) . . . . ?
C8 C3 C4 C7 4.7(4) . . . . ?
C3 C4 C5 C1 0.9(3) . . . . ?
C7 C4 C5 C1 178.9(2) . . . . ?
C3 C4 C5 C6 -177.3(2) . . . . ?
C7 C4 C5 C6 0.7(4) . . . . ?
C3 C4 C5 Pb1 -58.9(2) . . . . ?
C7 C4 C5 Pb1 119.1(2) . . . . ?
C2 C1 C5 C4 -2.8(3) . . . . ?
Si1 C1 C5 C4 -176.77(18) . . . . ?
Pb1 C1 C5 C4 -88.22(18) . . . . ?
C2 C1 C5 C6 175.4(2) . . . . ?
Si1 C1 C5 C6 1.4(4) . . . . ?
Pb1 C1 C5 C6 90.0(2) . . . . ?
C2 C1 C5 Pb1 85.46(16) . . . . ?
Si1 C1 C5 Pb1 -88.55(19) . . . . ?
Si1 N1 C12 C15 51.7(4) . . . . ?
Pb1 N1 C12 C15 -123.6(3) . . . . ?
Si1 N1 C12 C13 170.4(2) . . . . ?
Pb1 N1 C12 C13 -4.9(3) . . . . ?
Si1 N1 C12 C14 -72.9(3) . . . . ?
Pb1 N1 C12 C14 111.9(3) . . . . ?
C26 Si2 N2 C27 62.4(3) . . . . ?
C25 Si2 N2 C27 -59.4(3) . . . . ?
C16 Si2 N2 C27 179.8(3) . . . . ?
C26 Si2 N2 Pb2 -133.69(11) . . . . ?
C25 Si2 N2 Pb2 104.51(12) . . . . ?
C16 Si2 N2 Pb2 -16.30(11) . . . . ?
N2 Si2 C16 C20 104.1(2) . . . . ?
C26 Si2 C16 C20 -133.4(2) . . . . ?
C25 Si2 C16 C20 -16.0(3) . . . . ?
N2 Si2 C16 C17 -61.1(2) . . . . ?
C26 Si2 C16 C17 61.4(2) . . . . ?
C25 Si2 C16 C17 178.80(19) . . . . ?
N2 Si2 C16 Pb2 14.17(10) . . . . ?
C26 Si2 C16 Pb2 136.71(10) . . . . ?
C25 Si2 C16 Pb2 -105.91(12) . . . . ?
C20 C16 C17 C18 2.8(3) . . . . ?
Si2 C16 C17 C18 171.48(16) . . . . ?
Pb2 C16 C17 C18 91.70(17) . . . . ?
C20 C16 C17 C24 176.3(2) . . . . ?
Si2 C16 C17 C24 -15.0(3) . . . . ?
Pb2 C16 C17 C24 -94.8(2) . . . . ?
C20 C16 C17 Pb2 -88.86(16) . . . . ?
Si2 C16 C17 Pb2 79.79(15) . . . . ?
C16 C17 C18 C19 -1.9(3) . . . . ?
C24 C17 C18 C19 -175.4(2) . . . . ?
Pb2 C17 C18 C19 67.71(19) . . . . ?
C16 C17 C18 C23 174.4(2) . . . . ?
C24 C17 C18 C23 0.9(4) . . . . ?
Pb2 C17 C18 C23 -116.0(2) . . . . ?
C17 C18 C19 C20 0.1(3) . . . . ?
C23 C18 C19 C20 -176.3(2) . . . . ?
C17 C18 C19 C22 -177.9(2) . . . . ?
C23 C18 C19 C22 5.8(4) . . . . ?
C18 C19 C20 C16 1.8(3) . . . . ?
C22 C19 C20 C16 179.8(2) . . . . ?
C18 C19 C20 C21 -179.0(2) . . . . ?
C22 C19 C20 C21 -1.0(4) . . . . ?
C18 C19 C20 Pb2 -56.19(19) . . . . ?
C22 C19 C20 Pb2 121.8(2) . . . . ?
C17 C16 C20 C19 -2.8(3) . . . . ?
Si2 C16 C20 C19 -169.76(19) . . . . ?
Pb2 C16 C20 C19 -81.89(19) . . . . ?
C17 C16 C20 C21 178.0(2) . . . . ?
Si2 C16 C20 C21 11.0(4) . . . . ?
Pb2 C16 C20 C21 98.9(3) . . . . ?
C17 C16 C20 Pb2 79.09(16) . . . . ?
Si2 C16 C20 Pb2 -87.9(2) . . . . ?
Si2 N2 C27 C29 101.4(3) . . . . ?
Pb2 N2 C27 C29 -59.3(3) . . . . ?
Si2 N2 C27 C28 -19.7(4) . . . . ?
Pb2 N2 C27 C28 179.6(2) . . . . ?
Si2 N2 C27 C30 -138.7(2) . . . . ?
Pb2 N2 C27 C30 60.6(3) . . . . ?

_refine_diff_density_max         0.628
_refine_diff_density_min         -0.584
_refine_diff_density_rms         0.086



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

data_sh4595_b
_database_code_depnum_ccdc_archive 'CCDC 2174674'
loop_
_audit_author_name
_audit_author_address
'Bernd Morgenstern'
;Universitaet des Saarlandes
Germany
;
_audit_update_record             
;
2022-07-04 deposited with the CCDC.	2022-07-12 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C26 H47 N3 Pb Si'
_chemical_formula_sum            'C26 H47 N3 Pb Si'
_chemical_formula_weight         636.94

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_H-M_alt        'P 21'
_space_group_name_Hall           'P 2yb'

_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'

_cell_length_a                   9.0843(2)
_cell_length_b                   15.3056(4)
_cell_length_c                   10.2605(3)
_cell_angle_alpha                90
_cell_angle_beta                 98.3690(10)
_cell_angle_gamma                90
_cell_volume                     1411.43(6)
_cell_formula_units_Z            2
_cell_measurement_temperature    133(2)
_cell_measurement_reflns_used    9686
_cell_measurement_theta_min      2.41
_cell_measurement_theta_max      31.50

_exptl_crystal_description       plate
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.499
_exptl_crystal_F_000             640
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.320
_exptl_crystal_size_mid          0.273
_exptl_crystal_size_min          0.096
_exptl_absorpt_coefficient_mu    6.036
_shelx_estimated_absorpt_T_min   0.248
_shelx_estimated_absorpt_T_max   0.595
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.4419
_exptl_absorpt_correction_T_max  0.7462
_exptl_absorpt_process_details   
;
 SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D.,
 J. Appl. Cryst. 48 (2015) 3-10
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      133(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'INCOATEC I\^A?S microfocus sealed tube'
_diffrn_measurement_device_type  'Bruker AXS D8 Venture, Photon II'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            39122
_diffrn_reflns_av_unetI/netI     0.0338
_diffrn_reflns_av_R_equivalents  0.0455
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         2.006
_diffrn_reflns_theta_max         26.728
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             5966
_reflns_number_gt                5703
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.923
_reflns_Friedel_fraction_max     0.996
_reflns_Friedel_fraction_full    0.996

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

_computing_data_collection       'APEX 3 (Bruker Nano, Inc., 2019)'
_computing_cell_refinement       'SAINT V8.40A (Bruker Nano, Inc., 2019)'
_computing_data_reduction        'SAINT V8.40A (Bruker Nano, Inc., 2019)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_computing_structure_refinement  
;
SHELXL-2018/3 (Sheldrick, 2018),                                              
SHELXLe Rev 1000 (Huebschle et al., 2011)
;
_computing_molecular_graphics    'DIAMOND, (Brandenburg, 2018)'
_computing_publication_material  'SHELXL-2018/3 (Sheldrick, 2018)'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     'w=1/[σ²(Fo²)] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Flack x determined using 2623 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.005(3)
_chemical_absolute_configuration ad
_refine_ls_number_reflns         5966
_refine_ls_number_parameters     295
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0147
_refine_ls_R_factor_gt           0.0134
_refine_ls_wR_factor_ref         0.0292
_refine_ls_wR_factor_gt          0.0290
_refine_ls_goodness_of_fit_ref   0.868
_refine_ls_restrained_S_all      0.868
_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
Pb1 Pb -0.06784(2) 0.55223(2) 0.40731(2) 0.01753(4) Uani 1 1 d . . . . .
C1 C 0.1660(4) 0.4902(2) 0.3606(4) 0.0194(7) Uani 1 1 d . . . . .
N1 N -0.0454(3) 0.41966(16) 0.4987(3) 0.0186(6) Uani 1 1 d . . . . .
Si1 Si 0.11718(10) 0.38767(6) 0.44641(10) 0.01776(18) Uani 1 1 d . . . . .
N2 N -0.2197(3) 0.57604(15) 0.0859(3) 0.0186(6) Uani 1 1 d . . . . .
C2 C 0.2696(3) 0.5540(4) 0.4335(3) 0.0270(6) Uani 1 1 d . . . . .
C3 C 0.3427(4) 0.5976(2) 0.3456(5) 0.0305(9) Uani 1 1 d . . . . .
N3 N -0.2988(3) 0.45003(16) 0.1354(3) 0.0176(6) Uani 1 1 d . . . . .
C4 C 0.2925(4) 0.5651(3) 0.2161(4) 0.0284(10) Uani 1 1 d . . . . .
C5 C 0.1892(4) 0.5006(2) 0.2237(4) 0.0221(7) Uani 1 1 d . . . . .
C9 C 0.2877(5) 0.5698(3) 0.5802(4) 0.0467(14) Uani 1 1 d . . . . .
H9A H 0.297711 0.632598 0.597703 0.070 Uiso 1 1 calc R U . . .
H9B H 0.377024 0.539524 0.622884 0.070 Uiso 1 1 calc R U . . .
H9C H 0.200318 0.547427 0.615276 0.070 Uiso 1 1 calc R U . . .
C8 C 0.4609(5) 0.6667(3) 0.3767(6) 0.0520(14) Uani 1 1 d . . . . .
H8A H 0.558082 0.642268 0.365788 0.078 Uiso 1 1 calc R U . . .
H8B H 0.463161 0.686477 0.467858 0.078 Uiso 1 1 calc R U . . .
H8C H 0.438396 0.716336 0.316773 0.078 Uiso 1 1 calc R U . . .
C7 C 0.3523(5) 0.5977(3) 0.0963(5) 0.0476(13) Uani 1 1 d . . . . .
H7A H 0.308236 0.564094 0.019093 0.071 Uiso 1 1 calc R U . . .
H7B H 0.460670 0.590842 0.108781 0.071 Uiso 1 1 calc R U . . .
H7C H 0.326964 0.659638 0.082700 0.071 Uiso 1 1 calc R U . . .
C6 C 0.1179(4) 0.4459(2) 0.1103(4) 0.0294(8) Uani 1 1 d . . . . .
H6A H 0.122907 0.476817 0.027391 0.044 Uiso 1 1 calc R U . . .
H6B H 0.013539 0.435106 0.119494 0.044 Uiso 1 1 calc R U . . .
H6C H 0.170551 0.390037 0.109871 0.044 Uiso 1 1 calc R U . . .
C26 C -0.4631(5) 0.4066(3) -0.0799(4) 0.0356(9) Uani 1 1 d . . . . .
H26A H -0.500835 0.436496 -0.162525 0.053 Uiso 1 1 calc R U . . .
H26B H -0.546503 0.391493 -0.033429 0.053 Uiso 1 1 calc R U . . .
H26C H -0.410817 0.353202 -0.099240 0.053 Uiso 1 1 calc R U . . .
C12 C -0.1190(4) 0.3910(2) 0.6076(4) 0.0228(7) Uani 1 1 d . . . . .
C11 C 0.2723(4) 0.3528(3) 0.5790(4) 0.0328(9) Uani 1 1 d . . . . .
H11A H 0.253850 0.293080 0.607004 0.049 Uiso 1 1 calc R U . . .
H11B H 0.276489 0.392401 0.654451 0.049 Uiso 1 1 calc R U . . .
H11C H 0.367235 0.354795 0.544237 0.049 Uiso 1 1 calc R U . . .
C10 C 0.0990(5) 0.2902(3) 0.3341(5) 0.0306(11) Uani 1 1 d . . . . .
H10A H 0.017704 0.300030 0.261689 0.046 Uiso 1 1 calc R U . . .
H10B H 0.077496 0.238200 0.383749 0.046 Uiso 1 1 calc R U . . .
H10C H 0.192228 0.281601 0.298357 0.046 Uiso 1 1 calc R U . . .
C13 C -0.1072(6) 0.2905(3) 0.6218(5) 0.0370(12) Uani 1 1 d . . . . .
H13A H -0.155803 0.262851 0.540708 0.055 Uiso 1 1 calc R U . . .
H13B H -0.156108 0.271677 0.696082 0.055 Uiso 1 1 calc R U . . .
H13C H -0.002114 0.273468 0.637667 0.055 Uiso 1 1 calc R U . . .
C16 C -0.2139(3) 0.5181(2) 0.1861(4) 0.0175(7) Uani 1 1 d . . . . .
C15 C -0.2833(4) 0.4164(3) 0.5845(4) 0.0315(9) Uani 1 1 d . . . . .
H15A H -0.332177 0.388670 0.503450 0.047 Uiso 1 1 calc R U . . .
H15B H -0.292351 0.480017 0.575978 0.047 Uiso 1 1 calc R U . . .
H15C H -0.330944 0.396767 0.659107 0.047 Uiso 1 1 calc R U . . .
C14 C -0.0477(5) 0.4328(3) 0.7372(4) 0.0359(9) Uani 1 1 d . . . . .
H14A H 0.058274 0.417785 0.753717 0.054 Uiso 1 1 calc R U . . .
H14B H -0.096876 0.410844 0.809555 0.054 Uiso 1 1 calc R U . . .
H14C H -0.058828 0.496394 0.731209 0.054 Uiso 1 1 calc R U . . .
C19 C -0.3242(4) 0.37351(19) 0.2168(4) 0.0185(7) Uani 1 1 d . . . . .
H19 H -0.252510 0.378140 0.300298 0.022 Uiso 1 1 calc R U . . .
C21 C -0.2916(4) 0.2875(2) 0.1517(4) 0.0290(8) Uani 1 1 d . . . . .
H21A H -0.277128 0.241232 0.218310 0.043 Uiso 1 1 calc R U . . .
H21B H -0.201153 0.293701 0.110746 0.043 Uiso 1 1 calc R U . . .
H21C H -0.375414 0.272392 0.084178 0.043 Uiso 1 1 calc R U . . .
C20 C -0.4803(4) 0.3746(2) 0.2551(4) 0.0269(8) Uani 1 1 d . . . . .
H20A H -0.490568 0.326250 0.315752 0.040 Uiso 1 1 calc R U . . .
H20B H -0.553939 0.368050 0.175838 0.040 Uiso 1 1 calc R U . . .
H20C H -0.496654 0.430144 0.298240 0.040 Uiso 1 1 calc R U . . .
C24 C -0.0286(5) 0.6747(3) 0.0138(6) 0.0436(12) Uani 1 1 d . . . . .
H24A H 0.026986 0.728542 0.038332 0.065 Uiso 1 1 calc R U . . .
H24B H -0.076718 0.678873 -0.077917 0.065 Uiso 1 1 calc R U . . .
H24C H 0.039802 0.624862 0.023229 0.065 Uiso 1 1 calc R U . . .
C23 C -0.2575(5) 0.7361(2) 0.0911(5) 0.0403(11) Uani 1 1 d . . . . .
H23A H -0.206280 0.791205 0.116366 0.060 Uiso 1 1 calc R U . . .
H23B H -0.331357 0.724582 0.149714 0.060 Uiso 1 1 calc R U . . .
H23C H -0.307479 0.740188 -0.000008 0.060 Uiso 1 1 calc R U . . .
C22 C -0.1451(4) 0.6622(2) 0.1023(4) 0.0263(8) Uani 1 1 d . . . . .
H22 H -0.091660 0.663902 0.194595 0.032 Uiso 1 1 calc R U . . .
C25 C -0.3433(4) 0.5936(2) -0.1548(4) 0.0293(8) Uani 1 1 d . . . . .
H25A H -0.392435 0.554037 -0.222616 0.044 Uiso 1 1 calc R U . . .
H25B H -0.250945 0.615645 -0.181565 0.044 Uiso 1 1 calc R U . . .
H25C H -0.409506 0.642782 -0.143708 0.044 Uiso 1 1 calc R U . . .
C18 C -0.3580(4) 0.4656(2) 0.0046(4) 0.0218(7) Uani 1 1 d . . . . .
C17 C -0.3082(3) 0.5453(4) -0.0270(3) 0.0202(7) Uani 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pb1 N1 2.232(3) . ?
Pb1 C1 2.437(3) . ?
Pb1 C16 2.512(3) . ?
C1 C5 1.460(5) . ?
C1 C2 1.481(5) . ?
C1 Si1 1.883(3) . ?
N1 C12 1.450(5) . ?
N1 Si1 1.715(3) . ?
Si1 C10 1.877(4) . ?
Si1 C11 1.888(4) . ?
N2 C16 1.353(4) . ?
N2 C17 1.392(4) . ?
N2 C22 1.481(4) . ?
C2 C3 1.369(6) . ?
C2 C9 1.510(5) . ?
C3 C4 1.430(6) . ?
C3 C8 1.508(5) . ?
N3 C16 1.355(4) . ?
N3 C18 1.391(4) . ?
N3 C19 1.476(4) . ?
C4 C5 1.372(5) . ?
C4 C7 1.500(6) . ?
C5 C6 1.502(5) . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C26 C18 1.496(5) . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C12 C15 1.527(5) . ?
C12 C14 1.531(5) . ?
C12 C13 1.547(5) . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C19 C21 1.524(4) . ?
C19 C20 1.526(5) . ?
C19 H19 1.0000 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C24 C22 1.504(6) . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C23 C22 1.516(5) . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C22 H22 1.0000 . ?
C25 C17 1.499(5) . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C18 C17 1.357(7) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Pb1 C1 72.51(10) . . ?
N1 Pb1 C16 101.23(10) . . ?
C1 Pb1 C16 95.87(11) . . ?
C5 C1 C2 104.1(3) . . ?
C5 C1 Si1 128.2(2) . . ?
C2 C1 Si1 119.3(3) . . ?
C5 C1 Pb1 113.5(2) . . ?
C2 C1 Pb1 98.7(2) . . ?
Si1 C1 Pb1 87.81(13) . . ?
C12 N1 Si1 132.0(2) . . ?
C12 N1 Pb1 125.0(2) . . ?
Si1 N1 Pb1 99.10(13) . . ?
N1 Si1 C10 114.58(18) . . ?
N1 Si1 C1 100.40(14) . . ?
C10 Si1 C1 112.38(19) . . ?
N1 Si1 C11 116.24(17) . . ?
C10 Si1 C11 102.0(2) . . ?
C1 Si1 C11 111.74(16) . . ?
C16 N2 C17 111.4(3) . . ?
C16 N2 C22 122.0(3) . . ?
C17 N2 C22 126.5(3) . . ?
C3 C2 C1 108.8(3) . . ?
C3 C2 C9 125.8(4) . . ?
C1 C2 C9 125.3(4) . . ?
C2 C3 C4 108.8(3) . . ?
C2 C3 C8 127.0(4) . . ?
C4 C3 C8 124.1(4) . . ?
C16 N3 C18 110.9(3) . . ?
C16 N3 C19 121.4(3) . . ?
C18 N3 C19 127.7(3) . . ?
C5 C4 C3 109.0(3) . . ?
C5 C4 C7 128.2(4) . . ?
C3 C4 C7 122.8(4) . . ?
C4 C5 C1 109.2(3) . . ?
C4 C5 C6 125.4(4) . . ?
C1 C5 C6 125.3(3) . . ?
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 . . ?
C3 C8 H8A 109.5 . . ?
C3 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C3 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C4 C7 H7A 109.5 . . ?
C4 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C4 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
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 . . ?
C18 C26 H26A 109.5 . . ?
C18 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
C18 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
N1 C12 C15 110.7(3) . . ?
N1 C12 C14 111.0(3) . . ?
C15 C12 C14 108.0(3) . . ?
N1 C12 C13 109.8(3) . . ?
C15 C12 C13 108.7(3) . . ?
C14 C12 C13 108.5(3) . . ?
Si1 C11 H11A 109.5 . . ?
Si1 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
Si1 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 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 . . ?
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 . . ?
N2 C16 N3 104.8(3) . . ?
N2 C16 Pb1 120.5(2) . . ?
N3 C16 Pb1 134.7(2) . . ?
C12 C15 H15A 109.5 . . ?
C12 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C12 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
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 . . ?
N3 C19 C21 112.4(3) . . ?
N3 C19 C20 111.4(3) . . ?
C21 C19 C20 111.7(3) . . ?
N3 C19 H19 107.0 . . ?
C21 C19 H19 107.0 . . ?
C20 C19 H19 107.0 . . ?
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 . . ?
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 . . ?
C22 C24 H24A 109.5 . . ?
C22 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C22 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C22 C23 H23A 109.5 . . ?
C22 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C22 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
N2 C22 C24 113.3(3) . . ?
N2 C22 C23 111.3(3) . . ?
C24 C22 C23 112.6(3) . . ?
N2 C22 H22 106.3 . . ?
C24 C22 H22 106.3 . . ?
C23 C22 H22 106.3 . . ?
C17 C25 H25A 109.5 . . ?
C17 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
C17 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C17 C18 N3 106.8(3) . . ?
C17 C18 C26 127.6(3) . . ?
N3 C18 C26 125.5(3) . . ?
C18 C17 N2 106.1(3) . . ?
C18 C17 C25 128.1(3) . . ?
N2 C17 C25 125.8(4) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C12 N1 Si1 C10 85.3(4) . . . . ?
Pb1 N1 Si1 C10 -116.8(2) . . . . ?
C12 N1 Si1 C1 -154.0(3) . . . . ?
Pb1 N1 Si1 C1 3.89(16) . . . . ?
C12 N1 Si1 C11 -33.3(4) . . . . ?
Pb1 N1 Si1 C11 124.58(16) . . . . ?
C5 C1 Si1 N1 -122.0(3) . . . . ?
C2 C1 Si1 N1 95.2(3) . . . . ?
Pb1 C1 Si1 N1 -3.52(14) . . . . ?
C5 C1 Si1 C10 0.2(4) . . . . ?
C2 C1 Si1 C10 -142.6(3) . . . . ?
Pb1 C1 Si1 C10 118.68(18) . . . . ?
C5 C1 Si1 C11 114.1(3) . . . . ?
C2 C1 Si1 C11 -28.6(3) . . . . ?
Pb1 C1 Si1 C11 -127.38(16) . . . . ?
C5 C1 C2 C3 1.0(4) . . . . ?
Si1 C1 C2 C3 151.6(3) . . . . ?
Pb1 C1 C2 C3 -116.0(3) . . . . ?
C5 C1 C2 C9 179.4(4) . . . . ?
Si1 C1 C2 C9 -30.0(6) . . . . ?
Pb1 C1 C2 C9 62.4(5) . . . . ?
C1 C2 C3 C4 -0.3(5) . . . . ?
C9 C2 C3 C4 -178.7(4) . . . . ?
C1 C2 C3 C8 -178.4(4) . . . . ?
C9 C2 C3 C8 3.2(7) . . . . ?
C2 C3 C4 C5 -0.6(4) . . . . ?
C8 C3 C4 C5 177.6(4) . . . . ?
C2 C3 C4 C7 -178.9(4) . . . . ?
C8 C3 C4 C7 -0.7(6) . . . . ?
C3 C4 C5 C1 1.2(4) . . . . ?
C7 C4 C5 C1 179.4(4) . . . . ?
C3 C4 C5 C6 -175.6(3) . . . . ?
C7 C4 C5 C6 2.6(6) . . . . ?
C2 C1 C5 C4 -1.3(4) . . . . ?
Si1 C1 C5 C4 -148.3(3) . . . . ?
Pb1 C1 C5 C4 104.9(3) . . . . ?
C2 C1 C5 C6 175.4(3) . . . . ?
Si1 C1 C5 C6 28.4(5) . . . . ?
Pb1 C1 C5 C6 -78.3(3) . . . . ?
Si1 N1 C12 C15 -160.4(3) . . . . ?
Pb1 N1 C12 C15 46.6(4) . . . . ?
Si1 N1 C12 C14 79.7(4) . . . . ?
Pb1 N1 C12 C14 -73.3(3) . . . . ?
Si1 N1 C12 C13 -40.4(4) . . . . ?
Pb1 N1 C12 C13 166.6(3) . . . . ?
C17 N2 C16 N3 0.4(4) . . . . ?
C22 N2 C16 N3 177.6(3) . . . . ?
C17 N2 C16 Pb1 -179.0(2) . . . . ?
C22 N2 C16 Pb1 -1.8(4) . . . . ?
C18 N3 C16 N2 -0.4(3) . . . . ?
C19 N3 C16 N2 -178.1(3) . . . . ?
C18 N3 C16 Pb1 178.9(2) . . . . ?
C19 N3 C16 Pb1 1.1(5) . . . . ?
C16 N3 C19 C21 -129.1(3) . . . . ?
C18 N3 C19 C21 53.5(4) . . . . ?
C16 N3 C19 C20 104.7(3) . . . . ?
C18 N3 C19 C20 -72.6(4) . . . . ?
C16 N2 C22 C24 119.2(4) . . . . ?
C17 N2 C22 C24 -64.1(5) . . . . ?
C16 N2 C22 C23 -112.7(4) . . . . ?
C17 N2 C22 C23 64.0(5) . . . . ?
C16 N3 C18 C17 0.2(4) . . . . ?
C19 N3 C18 C17 177.8(3) . . . . ?
C16 N3 C18 C26 -176.7(4) . . . . ?
C19 N3 C18 C26 0.9(5) . . . . ?
N3 C18 C17 N2 0.0(4) . . . . ?
C26 C18 C17 N2 176.8(4) . . . . ?
N3 C18 C17 C25 -178.1(3) . . . . ?
C26 C18 C17 C25 -1.3(7) . . . . ?
C16 N2 C17 C18 -0.3(4) . . . . ?
C22 N2 C17 C18 -177.3(3) . . . . ?
C16 N2 C17 C25 177.9(3) . . . . ?
C22 N2 C17 C25 0.9(6) . . . . ?

_refine_diff_density_max         0.356
_refine_diff_density_min         -0.661
_refine_diff_density_rms         0.059



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

data_sh4579_a
_database_code_depnum_ccdc_archive 'CCDC 2174672'
loop_
_audit_author_name
_audit_author_address
'Bernd Morgenstern'
;Universitaet des Saarlandes
Germany
;
_audit_update_record             
;
2022-07-04 deposited with the CCDC.	2022-07-12 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C26 H47 N3 Si Sn'
_chemical_formula_sum            'C26 H47 N3 Si Sn'
_chemical_formula_weight         548.44

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Sn Sn -0.6537 1.4246 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_H-M_alt        'P 21'
_space_group_name_Hall           'P 2yb'

_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'

_cell_length_a                   9.0621(2)
_cell_length_b                   15.2311(3)
_cell_length_c                   10.2462(2)
_cell_angle_alpha                90
_cell_angle_beta                 99.6810(10)
_cell_angle_gamma                90
_cell_volume                     1394.10(5)
_cell_formula_units_Z            2
_cell_measurement_temperature    132(2)
_cell_measurement_reflns_used    9211
_cell_measurement_theta_min      2.28
_cell_measurement_theta_max      29.61

_exptl_crystal_description       plate
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.307
_exptl_crystal_F_000             576
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.316
_exptl_crystal_size_mid          0.224
_exptl_crystal_size_min          0.114
_exptl_absorpt_coefficient_mu    0.977
_shelx_estimated_absorpt_T_min   0.748
_shelx_estimated_absorpt_T_max   0.897
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6976
_exptl_absorpt_correction_T_max  0.7459
_exptl_absorpt_process_details   
;
 SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D.,
 J. Appl. Cryst. 48 (2015) 3-10
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      132(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'sealed tube'
_diffrn_measurement_device_type  'Bruker X8 Apex, Nonius Kappa CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            22591
_diffrn_reflns_av_unetI/netI     0.0398
_diffrn_reflns_av_R_equivalents  0.0294
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         2.016
_diffrn_reflns_theta_max         29.633
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             7838
_reflns_number_gt                7326
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.922
_reflns_Friedel_fraction_max     0.989
_reflns_Friedel_fraction_full    0.999

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

_computing_data_collection       'APEX2 (Bruker, 2010)'
_computing_cell_refinement       'SAINT (Bruker, 2010)'
_computing_data_reduction        'SAINT (Bruker, 2010)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_computing_structure_refinement  
;
SHELXL-2018/3 (Sheldrick, 2018),                                              
SHELXLe Rev 1000 (Huebschle et al., 2011)
;
_computing_molecular_graphics    'DIAMOND, (Brandenburg, 2018)'
_computing_publication_material  'SHELXL-2018/3 (Sheldrick, 2018)'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0161P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Flack x determined using 3285 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.001(8)
_chemical_absolute_configuration ad
_refine_ls_number_reflns         7838
_refine_ls_number_parameters     295
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0266
_refine_ls_R_factor_gt           0.0226
_refine_ls_wR_factor_ref         0.0454
_refine_ls_wR_factor_gt          0.0437
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_restrained_S_all      1.014
_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 0.42434(2) 0.45931(2) 0.39948(2) 0.01528(4) Uani 1 1 d . . . . .
Si1 Si 0.61397(8) 0.61593(5) 0.44281(7) 0.01623(15) Uani 1 1 d . . . . .
N1 N 0.4501(3) 0.58427(14) 0.4919(2) 0.0156(5) Uani 1 1 d . . . . .
N2 N 0.2872(2) 0.43494(13) 0.0859(2) 0.0166(5) Uani 1 1 d . . . . .
N3 N 0.2029(2) 0.56046(15) 0.1332(2) 0.0156(5) Uani 1 1 d . . . . .
C1 C 0.6546(3) 0.51145(18) 0.3574(3) 0.0182(6) Uani 1 1 d . . . . .
C2 C 0.7595(3) 0.4471(2) 0.4331(3) 0.0228(7) Uani 1 1 d . . . . .
C3 C 0.8390(3) 0.4073(2) 0.3487(4) 0.0298(7) Uani 1 1 d . . . . .
C4 C 0.7917(3) 0.44141(18) 0.2183(3) 0.0280(8) Uani 1 1 d . . . . .
C5 C 0.6844(3) 0.5039(2) 0.2214(3) 0.0213(6) Uani 1 1 d . . . . .
C6 C 0.6167(4) 0.5607(2) 0.1077(3) 0.0292(7) Uani 1 1 d . . . . .
H6A H 0.619904 0.529868 0.024248 0.044 Uiso 1 1 calc R U . . .
H6B H 0.673435 0.615598 0.109515 0.044 Uiso 1 1 calc R U . . .
H6C H 0.512526 0.573822 0.114868 0.044 Uiso 1 1 calc R U . . .
C7 C 0.7720(4) 0.4289(2) 0.5784(3) 0.0396(9) Uani 1 1 d . . . . .
H7A H 0.677825 0.444709 0.607575 0.059 Uiso 1 1 calc R U . . .
H7B H 0.853826 0.463861 0.627510 0.059 Uiso 1 1 calc R U . . .
H7C H 0.792397 0.366405 0.595155 0.059 Uiso 1 1 calc R U . . .
C8 C 0.9582(4) 0.3379(2) 0.3829(5) 0.0505(11) Uani 1 1 d . . . . .
H8A H 0.933922 0.287021 0.324762 0.076 Uiso 1 1 calc R U . . .
H8B H 0.962840 0.319832 0.475282 0.076 Uiso 1 1 calc R U . . .
H8C H 1.055400 0.361909 0.370852 0.076 Uiso 1 1 calc R U . . .
C9 C 0.8589(4) 0.4124(3) 0.1001(4) 0.0486(11) Uani 1 1 d . . . . .
H9A H 0.812596 0.445304 0.021625 0.073 Uiso 1 1 calc R U . . .
H9B H 0.840632 0.349460 0.084944 0.073 Uiso 1 1 calc R U . . .
H9C H 0.966913 0.423454 0.116957 0.073 Uiso 1 1 calc R U . . .
C10 C 0.5967(4) 0.7143(2) 0.3322(4) 0.0280(9) Uani 1 1 d . . . . .
H10A H 0.689237 0.721747 0.295763 0.042 Uiso 1 1 calc R U . . .
H10B H 0.579341 0.766662 0.383134 0.042 Uiso 1 1 calc R U . . .
H10C H 0.512434 0.706158 0.259592 0.042 Uiso 1 1 calc R U . . .
C11 C 0.7723(3) 0.6490(2) 0.5768(3) 0.0291(7) Uani 1 1 d . . . . .
H11A H 0.867019 0.645627 0.542920 0.044 Uiso 1 1 calc R U . . .
H11B H 0.775977 0.609308 0.652585 0.044 Uiso 1 1 calc R U . . .
H11C H 0.756433 0.709299 0.604832 0.044 Uiso 1 1 calc R U . . .
C12 C 0.3803(3) 0.6126(2) 0.6036(3) 0.0207(6) Uani 1 1 d . . . . .
C13 C 0.4554(4) 0.5687(2) 0.7320(3) 0.0313(7) Uani 1 1 d . . . . .
H13A H 0.443038 0.504929 0.724012 0.047 Uiso 1 1 calc R U . . .
H13B H 0.409059 0.589951 0.805814 0.047 Uiso 1 1 calc R U . . .
H13C H 0.562316 0.583199 0.748353 0.047 Uiso 1 1 calc R U . . .
C14 C 0.3935(5) 0.7126(2) 0.6193(4) 0.0336(10) Uani 1 1 d . . . . .
H14A H 0.345288 0.740994 0.537372 0.050 Uiso 1 1 calc R U . . .
H14B H 0.499437 0.729174 0.637915 0.050 Uiso 1 1 calc R U . . .
H14C H 0.344216 0.731372 0.692741 0.050 Uiso 1 1 calc R U . . .
C15 C 0.2144(3) 0.5880(2) 0.5791(3) 0.0292(7) Uani 1 1 d . . . . .
H15A H 0.163642 0.618169 0.499571 0.044 Uiso 1 1 calc R U . . .
H15B H 0.169153 0.605801 0.655418 0.044 Uiso 1 1 calc R U . . .
H15C H 0.204025 0.524406 0.566635 0.044 Uiso 1 1 calc R U . . .
C16 C 0.2924(3) 0.49361(18) 0.1855(3) 0.0153(5) Uani 1 1 d . . . . .
C17 C 0.1945(3) 0.4639(3) -0.0284(2) 0.0189(5) Uani 1 1 d . . . . .
C18 C 0.1420(3) 0.54354(19) 0.0018(3) 0.0195(6) Uani 1 1 d . . . . .
C19 C 0.0343(4) 0.6018(2) -0.0849(3) 0.0326(8) Uani 1 1 d . . . . .
H19A H 0.085674 0.655613 -0.104625 0.049 Uiso 1 1 calc R U . . .
H19B H -0.048998 0.616919 -0.039212 0.049 Uiso 1 1 calc R U . . .
H19C H -0.004374 0.571146 -0.167672 0.049 Uiso 1 1 calc R U . . .
C20 C 0.1594(4) 0.4145(2) -0.1558(3) 0.0278(7) Uani 1 1 d . . . . .
H20A H 0.094371 0.450177 -0.221263 0.042 Uiso 1 1 calc R U . . .
H20B H 0.108343 0.359516 -0.141186 0.042 Uiso 1 1 calc R U . . .
H20C H 0.252567 0.401259 -0.188540 0.042 Uiso 1 1 calc R U . . .
C21 C 0.3640(3) 0.34915(19) 0.1038(3) 0.0232(6) Uani 1 1 d . . . . .
H21 H 0.425828 0.350283 0.194328 0.028 Uiso 1 1 calc R U . . .
C22 C 0.2535(4) 0.2749(2) 0.1042(4) 0.0359(8) Uani 1 1 d . . . . .
H22A H 0.191632 0.269880 0.016365 0.054 Uiso 1 1 calc R U . . .
H22B H 0.189325 0.286886 0.170137 0.054 Uiso 1 1 calc R U . . .
H22C H 0.307908 0.219850 0.126325 0.054 Uiso 1 1 calc R U . . .
C23 C 0.4723(4) 0.3343(2) 0.0085(4) 0.0362(8) Uani 1 1 d . . . . .
H23A H 0.416337 0.318869 -0.078853 0.054 Uiso 1 1 calc R U . . .
H23B H 0.540667 0.286275 0.041114 0.054 Uiso 1 1 calc R U . . .
H23C H 0.529915 0.387994 0.001525 0.054 Uiso 1 1 calc R U . . .
C24 C 0.1748(3) 0.63724(18) 0.2133(3) 0.0184(6) Uani 1 1 d . . . . .
H24 H 0.247365 0.633990 0.298234 0.022 Uiso 1 1 calc R U . . .
C25 C 0.2028(4) 0.72378(19) 0.1473(3) 0.0279(7) Uani 1 1 d . . . . .
H25A H 0.291702 0.718332 0.105074 0.042 Uiso 1 1 calc R U . . .
H25B H 0.218825 0.770395 0.214101 0.042 Uiso 1 1 calc R U . . .
H25C H 0.115841 0.738345 0.080196 0.042 Uiso 1 1 calc R U . . .
C26 C 0.0179(3) 0.6337(2) 0.2484(3) 0.0259(7) Uani 1 1 d . . . . .
H26A H -0.056431 0.638794 0.167399 0.039 Uiso 1 1 calc R U . . .
H26B H 0.005214 0.682240 0.308231 0.039 Uiso 1 1 calc R U . . .
H26C H 0.004220 0.577730 0.292000 0.039 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 N1 2.121(2) . ?
Sn1 C1 2.339(3) . ?
Sn1 C16 2.373(3) . ?
Si1 N1 1.715(2) . ?
Si1 C10 1.870(3) . ?
Si1 C11 1.880(3) . ?
Si1 C1 1.882(3) . ?
N1 C12 1.463(3) . ?
N2 C16 1.351(3) . ?
N2 C17 1.393(3) . ?
N2 C21 1.478(3) . ?
N3 C16 1.355(3) . ?
N3 C18 1.391(3) . ?
N3 C24 1.475(3) . ?
C1 C5 1.469(4) . ?
C1 C2 1.490(4) . ?
C2 C3 1.358(4) . ?
C2 C7 1.500(4) . ?
C3 C4 1.431(5) . ?
C3 C8 1.509(5) . ?
C4 C5 1.364(4) . ?
C4 C9 1.511(4) . ?
C5 C6 1.497(4) . ?
C12 C15 1.529(4) . ?
C12 C13 1.529(4) . ?
C12 C14 1.534(5) . ?
C17 C18 1.358(5) . ?
C17 C20 1.495(4) . ?
C18 C19 1.496(4) . ?
C21 C22 1.511(4) . ?
C21 C23 1.513(4) . ?
C24 C25 1.522(4) . ?
C24 C26 1.525(4) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Sn1 C1 75.10(9) . . ?
N1 Sn1 C16 102.44(9) . . ?
C1 Sn1 C16 94.68(9) . . ?
N1 Si1 C10 114.50(15) . . ?
N1 Si1 C11 116.95(13) . . ?
C10 Si1 C11 101.77(17) . . ?
N1 Si1 C1 98.34(12) . . ?
C10 Si1 C1 113.51(15) . . ?
C11 Si1 C1 112.41(14) . . ?
C12 N1 Si1 131.01(19) . . ?
C12 N1 Sn1 125.73(17) . . ?
Si1 N1 Sn1 99.05(10) . . ?
C16 N2 C17 111.4(3) . . ?
C16 N2 C21 122.4(2) . . ?
C17 N2 C21 126.1(3) . . ?
C16 N3 C18 110.9(2) . . ?
C16 N3 C24 121.6(2) . . ?
C18 N3 C24 127.4(2) . . ?
C5 C1 C2 103.8(2) . . ?
C5 C1 Si1 126.1(2) . . ?
C2 C1 Si1 118.2(2) . . ?
C5 C1 Sn1 117.43(18) . . ?
C2 C1 Sn1 101.08(18) . . ?
Si1 C1 Sn1 87.21(11) . . ?
C3 C2 C1 108.9(3) . . ?
C3 C2 C7 126.2(3) . . ?
C1 C2 C7 125.0(3) . . ?
C2 C3 C4 108.9(3) . . ?
C2 C3 C8 126.9(3) . . ?
C4 C3 C8 124.2(3) . . ?
C5 C4 C3 109.6(3) . . ?
C5 C4 C9 127.4(3) . . ?
C3 C4 C9 123.0(3) . . ?
C4 C5 C1 108.8(3) . . ?
C4 C5 C6 125.8(3) . . ?
C1 C5 C6 125.2(3) . . ?
N1 C12 C15 110.0(2) . . ?
N1 C12 C13 110.9(2) . . ?
C15 C12 C13 108.5(2) . . ?
N1 C12 C14 109.8(2) . . ?
C15 C12 C14 108.5(3) . . ?
C13 C12 C14 109.1(3) . . ?
N2 C16 N3 104.8(2) . . ?
N2 C16 Sn1 120.03(18) . . ?
N3 C16 Sn1 134.93(19) . . ?
C18 C17 N2 106.1(3) . . ?
C18 C17 C20 128.2(3) . . ?
N2 C17 C20 125.8(4) . . ?
C17 C18 N3 106.8(2) . . ?
C17 C18 C19 127.9(3) . . ?
N3 C18 C19 125.3(3) . . ?
N2 C21 C22 111.3(2) . . ?
N2 C21 C23 113.3(3) . . ?
C22 C21 C23 113.1(3) . . ?
N3 C24 C25 112.5(2) . . ?
N3 C24 C26 111.0(2) . . ?
C25 C24 C26 111.5(2) . . ?

_refine_diff_density_max         0.331
_refine_diff_density_min         -0.263
_refine_diff_density_rms         0.055



_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: THF/n-Hexane'
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
