# Electronic Supplementary Material (ESI) for Chemical Science.
# This journal is © The Royal Society of Chemistry 2015

####################################################################### 
# 
# 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_LGe2C2H4
_database_code_depnum_ccdc_archive 'CCDC 1422725'
_audit_update_record             
;
2015-09-07 deposited with the CCDC.
2015-09-22 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C91.50 H111.50 Ge2 N2 Si2'
_chemical_formula_weight         1440.69

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'

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   P-1

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   10.806(2)
_cell_length_b                   18.897(4)
_cell_length_c                   21.557(4)
_cell_angle_alpha                108.61(3)
_cell_angle_beta                 90.43(3)
_cell_angle_gamma                103.93(3)
_cell_volume                     4032.0(14)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       plate
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.01
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.187
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1533
_exptl_absorpt_coefficient_mu    0.820
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9224
_exptl_absorpt_correction_T_max  0.9918
_exptl_absorpt_process_details   XDS

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71080
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_source         'Australian Synchrotron'
_diffrn_radiation_monochromator  ?
_diffrn_measurement_device_type  'ADSC Quantum 210r'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            52997
_diffrn_reflns_av_R_equivalents  0.0750
_diffrn_reflns_av_sigmaI/netI    0.0570
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         2.92
_diffrn_reflns_theta_max         25.25
_reflns_number_total             13668
_reflns_number_gt                10373
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Blu-Ice (McPhillips, 2002)'
_computing_cell_refinement       'XDS (Kabsch, 1993)'
_computing_data_reduction        'XDS (Kabsch, 1993)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    X-Seed
_computing_publication_material  CifTAB

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
 One half of a molecule of hexane of crystallisation was refined in the 
 asymmetric unit with its carbon atoms set as isotropic, and its carbon
 and hydrogen atoms set at 50% occupancy. 
 The low value (93.7%) for completeness of data to theta = 25.25 deg. arises 
 from hardware constraints associated with the diffractometer used at the 
 Australian Synchrotron and is common for triclinic data sets on that instrument. 
 Its minimum crystal to detector distance is 72 mm and its
 goniometer only rotates about the phi axis.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0934P)²+5.9756P] 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         13668
_refine_ls_number_parameters     894
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.0828
_refine_ls_R_factor_gt           0.0609
_refine_ls_wR_factor_ref         0.1722
_refine_ls_wR_factor_gt          0.1581
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_restrained_S_all      1.030
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ge1 Ge 0.22225(5) 0.62739(3) 0.25613(2) 0.03514(14) Uani 1 1 d . . .
Ge2 Ge 0.18546(5) 0.42578(2) 0.27132(2) 0.03297(14) Uani 1 1 d . . .
Si1 Si 0.20938(11) 0.79814(6) 0.27278(5) 0.0247(2) Uani 1 1 d . . .
Si2 Si 0.09922(11) 0.24755(6) 0.25013(5) 0.0261(2) Uani 1 1 d . . .
N1 N 0.2907(3) 0.73479(18) 0.29076(14) 0.0227(7) Uani 1 1 d . . .
N2 N 0.2041(3) 0.32541(18) 0.23334(14) 0.0242(7) Uani 1 1 d . . .
C1 C 0.4060(4) 0.7630(2) 0.33535(18) 0.0220(8) Uani 1 1 d . . .
C2 C 0.3998(4) 0.7758(2) 0.40316(18) 0.0218(8) Uani 1 1 d . . .
C3 C 0.5124(4) 0.8032(2) 0.44476(18) 0.0235(8) Uani 1 1 d . . .
H3 H 0.5066 0.8131 0.4906 0.028 Uiso 1 1 calc R . .
C4 C 0.6327(4) 0.8165(2) 0.42201(18) 0.0246(8) Uani 1 1 d . . .
C5 C 0.6380(4) 0.8033(2) 0.35478(19) 0.0240(8) Uani 1 1 d . . .
H5 H 0.7193 0.8130 0.3382 0.029 Uiso 1 1 calc R . .
C6 C 0.5277(4) 0.7763(2) 0.31094(17) 0.0216(8) Uani 1 1 d . . .
C7 C 0.7544(4) 0.8395(2) 0.46775(19) 0.0273(8) Uani 1 1 d . . .
H7 H 0.8287 0.8581 0.4445 0.033 Uiso 1 1 calc R . .
C8 C 0.7718(5) 0.7674(3) 0.4816(3) 0.0409(11) Uani 1 1 d . . .
H8A H 0.7056 0.7520 0.5090 0.061 Uiso 1 1 calc R . .
H8B H 0.8566 0.7791 0.5047 0.061 Uiso 1 1 calc R . .
H8C H 0.7643 0.7251 0.4400 0.061 Uiso 1 1 calc R . .
C9 C 0.7559(5) 0.9032(3) 0.5333(2) 0.0425(12) Uani 1 1 d . . .
H9A H 0.7454 0.9495 0.5248 0.064 Uiso 1 1 calc R . .
H9B H 0.8376 0.9155 0.5593 0.064 Uiso 1 1 calc R . .
H9C H 0.6855 0.8853 0.5575 0.064 Uiso 1 1 calc R . .
C10 C 0.2730(4) 0.7585(2) 0.43255(18) 0.0253(8) Uani 1 1 d . . .
H10 H 0.2055 0.7498 0.3970 0.030 Uiso 1 1 calc R . .
C11 C 0.2467(4) 0.6825(2) 0.44807(18) 0.0278(9) Uani 1 1 d . . .
C12 C 0.3396(4) 0.6575(3) 0.4737(2) 0.0347(10) Uani 1 1 d . . .
H12 H 0.4255 0.6882 0.4821 0.042 Uiso 1 1 calc R . .
C13 C 0.3098(5) 0.5882(3) 0.4875(2) 0.0408(11) Uani 1 1 d . . .
H13 H 0.3753 0.5724 0.5051 0.049 Uiso 1 1 calc R . .
C14 C 0.1868(5) 0.5429(3) 0.4758(2) 0.0412(11) Uani 1 1 d . . .
H14 H 0.1664 0.4962 0.4858 0.049 Uiso 1 1 calc R . .
C15 C 0.0926(5) 0.5655(3) 0.4494(2) 0.0429(12) Uani 1 1 d . . .
H15 H 0.0074 0.5338 0.4406 0.052 Uiso 1 1 calc R . .
C16 C 0.1217(4) 0.6343(3) 0.4356(2) 0.0362(10) Uani 1 1 d . . .
H16 H 0.0557 0.6490 0.4173 0.043 Uiso 1 1 calc R . .
C17 C 0.2531(4) 0.8264(2) 0.49029(18) 0.0250(8) Uani 1 1 d . . .
C18 C 0.1525(4) 0.8145(3) 0.5299(2) 0.0333(9) Uani 1 1 d . . .
H18 H 0.1034 0.7635 0.5240 0.040 Uiso 1 1 calc R . .
C19 C 0.1241(5) 0.8765(3) 0.5775(2) 0.0427(11) Uani 1 1 d . . .
H19 H 0.0541 0.8674 0.6028 0.051 Uiso 1 1 calc R . .
C20 C 0.1965(5) 0.9514(3) 0.5887(2) 0.0381(11) Uani 1 1 d . . .
H20 H 0.1763 0.9937 0.6211 0.046 Uiso 1 1 calc R . .
C21 C 0.2985(5) 0.9634(3) 0.5519(2) 0.0380(10) Uani 1 1 d . . .
H21 H 0.3506 1.0143 0.5600 0.046 Uiso 1 1 calc R . .
C22 C 0.3258(4) 0.9019(3) 0.5030(2) 0.0329(9) Uani 1 1 d . . .
H22 H 0.3956 0.9117 0.4778 0.040 Uiso 1 1 calc R . .
C23 C 0.5421(4) 0.7572(2) 0.23715(17) 0.0229(8) Uani 1 1 d . . .
H23 H 0.4617 0.7616 0.2171 0.027 Uiso 1 1 calc R . .
C24 C 0.6521(4) 0.8133(2) 0.21967(18) 0.0285(9) Uani 1 1 d . . .
C25 C 0.6774(4) 0.8930(2) 0.25215(19) 0.0306(9) Uani 1 1 d . . .
H25 H 0.6282 0.9121 0.2870 0.037 Uiso 1 1 calc R . .
C26 C 0.7729(5) 0.9444(3) 0.2344(2) 0.0424(12) Uani 1 1 d . . .
H26 H 0.7873 0.9983 0.2564 0.051 Uiso 1 1 calc R . .
C27 C 0.8477(6) 0.9174(3) 0.1846(2) 0.0497(14) Uani 1 1 d . . .
H27 H 0.9138 0.9528 0.1728 0.060 Uiso 1 1 calc R . .
C28 C 0.8253(6) 0.8388(3) 0.1523(2) 0.0481(13) Uani 1 1 d . . .
H28 H 0.8762 0.8199 0.1182 0.058 Uiso 1 1 calc R . .
C29 C 0.7285(5) 0.7877(3) 0.1698(2) 0.0381(11) Uani 1 1 d . . .
H29 H 0.7138 0.7338 0.1472 0.046 Uiso 1 1 calc R . .
C30 C 0.5468(4) 0.6739(2) 0.20607(19) 0.0271(8) Uani 1 1 d . . .
C31 C 0.4719(5) 0.6283(3) 0.1473(2) 0.0362(10) Uani 1 1 d . . .
H31 H 0.4163 0.6494 0.1285 0.043 Uiso 1 1 calc R . .
C32 C 0.4773(5) 0.5522(3) 0.1159(2) 0.0433(12) Uani 1 1 d . . .
H32 H 0.4259 0.5220 0.0759 0.052 Uiso 1 1 calc R . .
C33 C 0.5567(5) 0.5214(3) 0.1427(3) 0.0485(13) Uani 1 1 d . . .
H33 H 0.5604 0.4696 0.1213 0.058 Uiso 1 1 calc R . .
C34 C 0.6325(5) 0.5652(3) 0.2013(2) 0.0438(12) Uani 1 1 d . . .
H34 H 0.6873 0.5435 0.2200 0.053 Uiso 1 1 calc R . .
C35 C 0.6271(4) 0.6415(2) 0.2323(2) 0.0337(9) Uani 1 1 d . . .
H35 H 0.6794 0.6716 0.2720 0.040 Uiso 1 1 calc R . .
C36 C 0.0985(4) 0.8275(3) 0.3391(2) 0.0342(10) Uani 1 1 d . . .
H36 H 0.1536 0.8507 0.3817 0.041 Uiso 1 1 calc R . .
C37 C -0.0056(5) 0.7589(3) 0.3460(3) 0.0453(12) Uani 1 1 d . . .
H37A H -0.0261 0.7706 0.3918 0.068 Uiso 1 1 calc R . .
H37B H 0.0262 0.7123 0.3330 0.068 Uiso 1 1 calc R . .
H37C H -0.0828 0.7502 0.3175 0.068 Uiso 1 1 calc R . .
C38 C 0.0366(5) 0.8908(3) 0.3326(2) 0.0455(12) Uani 1 1 d . . .
H38A H -0.0165 0.8715 0.2907 0.068 Uiso 1 1 calc R . .
H38B H 0.1038 0.9367 0.3342 0.068 Uiso 1 1 calc R . .
H38C H -0.0169 0.9042 0.3689 0.068 Uiso 1 1 calc R . .
C39 C 0.1144(5) 0.7523(3) 0.1900(2) 0.0396(11) Uani 1 1 d . . .
H39 H 0.0894 0.7969 0.1827 0.048 Uiso 1 1 calc R . .
C40 C -0.0125(6) 0.6941(3) 0.1815(3) 0.0574(14) Uani 1 1 d . . .
H40A H -0.0534 0.6812 0.1372 0.086 Uiso 1 1 calc R . .
H40B H -0.0678 0.7159 0.2141 0.086 Uiso 1 1 calc R . .
H40C H 0.0010 0.6473 0.1877 0.086 Uiso 1 1 calc R . .
C41 C 0.1964(5) 0.7282(3) 0.1332(2) 0.0419(11) Uani 1 1 d . . .
H41A H 0.2228 0.6825 0.1343 0.063 Uiso 1 1 calc R . .
H41B H 0.2725 0.7706 0.1376 0.063 Uiso 1 1 calc R . .
H41C H 0.1464 0.7161 0.0913 0.063 Uiso 1 1 calc R . .
C42 C 0.3325(5) 0.8872(2) 0.2707(2) 0.0349(10) Uani 1 1 d . . .
H42 H 0.4057 0.8688 0.2490 0.042 Uiso 1 1 calc R . .
C43 C 0.3876(5) 0.9436(3) 0.3402(2) 0.0407(11) Uani 1 1 d . . .
H43A H 0.4541 0.9871 0.3364 0.061 Uiso 1 1 calc R . .
H43B H 0.4246 0.9165 0.3644 0.061 Uiso 1 1 calc R . .
H43C H 0.3188 0.9628 0.3638 0.061 Uiso 1 1 calc R . .
C44 C 0.2877(5) 0.9315(3) 0.2296(2) 0.0450(12) Uani 1 1 d . . .
H44A H 0.2140 0.9496 0.2482 0.067 Uiso 1 1 calc R . .
H44B H 0.2629 0.8971 0.1841 0.067 Uiso 1 1 calc R . .
H44C H 0.3576 0.9758 0.2303 0.067 Uiso 1 1 calc R . .
C45 C 0.3047(4) 0.3182(2) 0.18982(18) 0.0229(8) Uani 1 1 d . . .
C46 C 0.2821(4) 0.3102(2) 0.12251(18) 0.0256(8) Uani 1 1 d . . .
C47 C 0.3835(4) 0.3071(2) 0.08278(19) 0.0309(9) Uani 1 1 d . . .
H47 H 0.3671 0.3009 0.0377 0.037 Uiso 1 1 calc R . .
C48 C 0.5063(4) 0.3127(2) 0.1057(2) 0.0326(9) Uani 1 1 d . . .
C49 C 0.5262(4) 0.3196(3) 0.1708(2) 0.0339(10) Uani 1 1 d . . .
H49 H 0.6096 0.3226 0.1876 0.041 Uiso 1 1 calc R . .
C50 C 0.4295(4) 0.3226(2) 0.21306(18) 0.0264(8) Uani 1 1 d . . .
C51 C 0.6165(5) 0.3087(3) 0.0606(2) 0.0482(12) Uani 1 1 d . . .
H51 H 0.6339 0.2568 0.0514 0.058 Uiso 1 1 calc R . .
C52 C 0.5897(8) 0.3180(5) -0.0020(3) 0.089(2) Uani 1 1 d . . .
H52A H 0.5246 0.2726 -0.0293 0.134 Uiso 1 1 calc R . .
H52B H 0.6683 0.3235 -0.0243 0.134 Uiso 1 1 calc R . .
H52C H 0.5581 0.3643 0.0055 0.134 Uiso 1 1 calc R . .
C53 C 0.7414(6) 0.3706(4) 0.0938(3) 0.0575(15) Uani 1 1 d . . .
H53A H 0.8085 0.3666 0.0635 0.086 Uiso 1 1 calc R . .
H53B H 0.7689 0.3624 0.1339 0.086 Uiso 1 1 calc R . .
H53C H 0.7261 0.4221 0.1052 0.086 Uiso 1 1 calc R . .
C54 C 0.1520(4) 0.3059(2) 0.09200(18) 0.0261(8) Uani 1 1 d . . .
H54 H 0.0964 0.3156 0.1291 0.031 Uiso 1 1 calc R . .
C55 C 0.1564(4) 0.3697(2) 0.06232(19) 0.0284(9) Uani 1 1 d . . .
C56 C 0.1118(5) 0.4334(3) 0.0961(2) 0.0380(10) Uani 1 1 d . . .
H56 H 0.0796 0.4368 0.1376 0.046 Uiso 1 1 calc R . .
C57 C 0.1139(5) 0.4926(3) 0.0700(3) 0.0504(14) Uani 1 1 d . . .
H57 H 0.0825 0.5354 0.0937 0.060 Uiso 1 1 calc R . .
C58 C 0.1601(6) 0.4893(3) 0.0112(3) 0.0536(14) Uani 1 1 d . . .
H58 H 0.1630 0.5301 -0.0058 0.064 Uiso 1 1 calc R . .
C59 C 0.2034(5) 0.4258(3) -0.0239(2) 0.0478(13) Uani 1 1 d . . .
H59 H 0.2352 0.4229 -0.0654 0.057 Uiso 1 1 calc R . .
C60 C 0.2004(5) 0.3664(3) 0.0014(2) 0.0376(10) Uani 1 1 d . . .
H60 H 0.2288 0.3228 -0.0234 0.045 Uiso 1 1 calc R . .
C61 C 0.0839(4) 0.2273(2) 0.04269(19) 0.0295(9) Uani 1 1 d . . .
C62 C -0.0382(5) 0.2179(3) 0.0154(2) 0.0408(11) Uani 1 1 d . . .
H62 H -0.0741 0.2610 0.0262 0.049 Uiso 1 1 calc R . .
C63 C -0.1091(6) 0.1476(3) -0.0268(3) 0.0527(13) Uani 1 1 d . . .
H63 H -0.1926 0.1426 -0.0447 0.063 Uiso 1 1 calc R . .
C64 C -0.0573(6) 0.0844(3) -0.0430(3) 0.0550(15) Uani 1 1 d . . .
H64 H -0.1057 0.0356 -0.0716 0.066 Uiso 1 1 calc R . .
C65 C 0.0625(6) 0.0923(3) -0.0178(2) 0.0492(13) Uani 1 1 d . . .
H65 H 0.0975 0.0487 -0.0291 0.059 Uiso 1 1 calc R . .
C66 C 0.1358(5) 0.1636(3) 0.0247(2) 0.0380(11) Uani 1 1 d . . .
H66 H 0.2203 0.1685 0.0411 0.046 Uiso 1 1 calc R . .
C67 C 0.4660(4) 0.3316(2) 0.28481(19) 0.0284(9) Uani 1 1 d . . .
H67 H 0.3868 0.3333 0.3083 0.034 Uiso 1 1 calc R . .
C68 C 0.5121(4) 0.2635(2) 0.2921(2) 0.0308(9) Uani 1 1 d . . .
C69 C 0.5178(4) 0.1984(3) 0.2404(2) 0.0357(10) Uani 1 1 d . . .
H69 H 0.4957 0.1952 0.1967 0.043 Uiso 1 1 calc R . .
C70 C 0.5556(5) 0.1373(3) 0.2515(2) 0.0407(11) Uani 1 1 d . . .
H70 H 0.5573 0.0927 0.2154 0.049 Uiso 1 1 calc R . .
C71 C 0.5906(5) 0.1413(3) 0.3148(3) 0.0444(12) Uani 1 1 d . . .
H71 H 0.6169 0.1002 0.3225 0.053 Uiso 1 1 calc R . .
C72 C 0.5864(5) 0.2064(3) 0.3662(3) 0.0516(13) Uani 1 1 d . . .
H72 H 0.6117 0.2103 0.4097 0.062 Uiso 1 1 calc R . .
C73 C 0.5459(5) 0.2662(3) 0.3557(2) 0.0449(12) Uani 1 1 d . . .
H73 H 0.5411 0.3096 0.3922 0.054 Uiso 1 1 calc R . .
C74 C 0.5650(4) 0.4085(3) 0.3189(2) 0.0339(10) Uani 1 1 d . . .
C75 C 0.6963(5) 0.4178(3) 0.3110(2) 0.0427(11) Uani 1 1 d . . .
H75 H 0.7253 0.3747 0.2856 0.051 Uiso 1 1 calc R . .
C76 C 0.7846(5) 0.4886(3) 0.3395(3) 0.0530(14) Uani 1 1 d . . .
H76 H 0.8724 0.4945 0.3318 0.064 Uiso 1 1 calc R . .
C77 C 0.7434(6) 0.5506(3) 0.3792(3) 0.0597(16) Uani 1 1 d . . .
H77 H 0.8030 0.5991 0.3997 0.072 Uiso 1 1 calc R . .
C78 C 0.6157(5) 0.5416(3) 0.3889(3) 0.0582(15) Uani 1 1 d . . .
H78 H 0.5876 0.5841 0.4162 0.070 Uiso 1 1 calc R . .
C79 C 0.5272(5) 0.4711(3) 0.3591(2) 0.0411(11) Uani 1 1 d . . .
H79 H 0.4395 0.4660 0.3666 0.049 Uiso 1 1 calc R . .
C80 C -0.0454(4) 0.2033(2) 0.1874(2) 0.0348(10) Uani 1 1 d . . .
H80 H -0.0112 0.1874 0.1435 0.042 Uiso 1 1 calc R . .
C81 C -0.1294(5) 0.2572(3) 0.1836(2) 0.0414(11) Uani 1 1 d . . .
H81A H -0.1841 0.2347 0.1420 0.062 Uiso 1 1 calc R . .
H81B H -0.0746 0.3077 0.1859 0.062 Uiso 1 1 calc R . .
H81C H -0.1831 0.2636 0.2204 0.062 Uiso 1 1 calc R . .
C82 C -0.1311(5) 0.1289(3) 0.1949(3) 0.0589(15) Uani 1 1 d . . .
H82A H -0.1602 0.1405 0.2391 0.088 Uiso 1 1 calc R . .
H82B H -0.0820 0.0901 0.1881 0.088 Uiso 1 1 calc R . .
H82C H -0.2054 0.1089 0.1622 0.088 Uiso 1 1 calc R . .
C83 C 0.1887(4) 0.1714(2) 0.2458(2) 0.0303(9) Uani 1 1 d . . .
H83 H 0.2782 0.2005 0.2648 0.036 Uiso 1 1 calc R . .
C84 C 0.2001(5) 0.1219(2) 0.1751(2) 0.0360(10) Uani 1 1 d . . .
H84A H 0.2475 0.0840 0.1761 0.054 Uiso 1 1 calc R . .
H84B H 0.2457 0.1553 0.1515 0.054 Uiso 1 1 calc R . .
H84C H 0.1143 0.0948 0.1528 0.054 Uiso 1 1 calc R . .
C85 C 0.1407(6) 0.1184(3) 0.2871(3) 0.0516(14) Uani 1 1 d . . .
H85A H 0.0516 0.0895 0.2717 0.077 Uiso 1 1 calc R . .
H85B H 0.1458 0.1499 0.3334 0.077 Uiso 1 1 calc R . .
H85C H 0.1941 0.0821 0.2822 0.077 Uiso 1 1 calc R . .
C86 C 0.0489(5) 0.2795(3) 0.3371(2) 0.0431(11) Uani 1 1 d . . .
H86 H 0.0086 0.2295 0.3440 0.052 Uiso 1 1 calc R . .
C87 C -0.0531(6) 0.3232(3) 0.3539(3) 0.0560(14) Uani 1 1 d . . .
H87A H -0.0667 0.3338 0.4005 0.084 Uiso 1 1 calc R . .
H87B H -0.1332 0.2921 0.3270 0.084 Uiso 1 1 calc R . .
H87C H -0.0256 0.3721 0.3450 0.084 Uiso 1 1 calc R . .
C88 C 0.1633(6) 0.3150(3) 0.3892(2) 0.0527(14) Uani 1 1 d . . .
H88A H 0.2081 0.3660 0.3875 0.079 Uiso 1 1 calc R . .
H88B H 0.2219 0.2814 0.3806 0.079 Uiso 1 1 calc R . .
H88C H 0.1331 0.3205 0.4328 0.079 Uiso 1 1 calc R . .
C89 C 0.3368(4) 0.5813(2) 0.2935(2) 0.0307(9) Uani 1 1 d . . .
H89A H 0.4265 0.6122 0.2977 0.037 Uiso 1 1 calc R . .
H89B H 0.3135 0.5814 0.3379 0.037 Uiso 1 1 calc R . .
C90 C 0.3246(4) 0.4970(2) 0.2480(2) 0.0321(9) Uani 1 1 d . . .
H90A H 0.4060 0.4829 0.2523 0.039 Uiso 1 1 calc R . .
H90B H 0.3080 0.4932 0.2016 0.039 Uiso 1 1 calc R . .
C91 C -0.498(2) 0.0067(14) -0.0324(6) 0.133(7) Uiso 0.50 1 d PD . .
H91A H -0.5326 -0.0431 -0.0680 0.160 Uiso 0.50 1 calc PR . .
H91B H -0.4081 0.0275 -0.0395 0.160 Uiso 0.50 1 calc PR . .
C93 C -0.5464(17) 0.0810(10) -0.0968(8) 0.096(5) Uiso 0.50 1 d PD . .
H93A H -0.4585 0.1131 -0.0918 0.144 Uiso 0.50 1 calc PR . .
H93B H -0.6063 0.1091 -0.1052 0.144 Uiso 0.50 1 calc PR . .
H93C H -0.5558 0.0331 -0.1338 0.144 Uiso 0.50 1 calc PR . .
C92 C -0.574(3) 0.0621(16) -0.0352(11) 0.168(10) Uiso 0.50 1 d PD . .
H92A H -0.6670 0.0384 -0.0362 0.202 Uiso 0.50 1 calc PR . .
H92B H -0.5494 0.1096 0.0037 0.202 Uiso 0.50 1 calc PR . .


_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 N1 1.877(3) . ?
Ge1 C89 1.973(4) . ?
Ge2 N2 1.872(3) . ?
Ge2 C90 1.948(5) . ?
Si1 N1 1.776(3) . ?
Si1 C39 1.884(4) . ?
Si1 C42 1.891(5) . ?
Si1 C36 1.905(5) . ?
Si2 N2 1.767(3) . ?
Si2 C80 1.894(5) . ?
Si2 C83 1.898(4) . ?
Si2 C86 1.905(5) . ?
N1 C1 1.448(5) . ?
N2 C45 1.445(5) . ?
C1 C2 1.408(5) . ?
C1 C6 1.416(6) . ?
C2 C3 1.391(5) . ?
C2 C10 1.522(5) . ?
C3 C4 1.388(6) . ?
C4 C5 1.394(5) . ?
C4 C7 1.524(5) . ?
C5 C6 1.399(5) . ?
C6 C23 1.533(5) . ?
C7 C9 1.533(6) . ?
C7 C8 1.537(6) . ?
C10 C17 1.536(5) . ?
C10 C11 1.539(6) . ?
C11 C12 1.386(6) . ?
C11 C16 1.404(6) . ?
C12 C13 1.399(6) . ?
C13 C14 1.369(7) . ?
C14 C15 1.377(7) . ?
C15 C16 1.389(7) . ?
C17 C22 1.391(6) . ?
C17 C18 1.407(6) . ?
C18 C19 1.389(6) . ?
C19 C20 1.386(7) . ?
C20 C21 1.380(7) . ?
C21 C22 1.392(6) . ?
C23 C30 1.515(5) . ?
C23 C24 1.528(6) . ?
C24 C29 1.396(6) . ?
C24 C25 1.399(6) . ?
C25 C26 1.384(6) . ?
C26 C27 1.388(7) . ?
C27 C28 1.384(7) . ?
C28 C29 1.385(7) . ?
C30 C35 1.385(6) . ?
C30 C31 1.397(6) . ?
C31 C32 1.396(6) . ?
C32 C33 1.363(8) . ?
C33 C34 1.394(7) . ?
C34 C35 1.398(6) . ?
C36 C38 1.545(6) . ?
C36 C37 1.546(7) . ?
C39 C40 1.506(8) . ?
C39 C41 1.532(6) . ?
C42 C44 1.543(6) . ?
C42 C43 1.548(6) . ?
C45 C50 1.409(6) . ?
C45 C46 1.423(5) . ?
C46 C47 1.397(6) . ?
C46 C54 1.521(6) . ?
C47 C48 1.381(6) . ?
C48 C49 1.378(6) . ?
C48 C51 1.543(7) . ?
C49 C50 1.391(6) . ?
C50 C67 1.538(5) . ?
C51 C52 1.451(8) . ?
C51 C53 1.547(8) . ?
C54 C55 1.526(5) . ?
C54 C61 1.527(5) . ?
C55 C60 1.387(6) . ?
C55 C56 1.392(6) . ?
C56 C57 1.399(7) . ?
C57 C58 1.354(8) . ?
C58 C59 1.388(8) . ?
C59 C60 1.390(6) . ?
C61 C62 1.388(6) . ?
C61 C66 1.394(6) . ?
C62 C63 1.382(7) . ?
C63 C64 1.385(8) . ?
C64 C65 1.355(8) . ?
C65 C66 1.404(7) . ?
C67 C74 1.533(6) . ?
C67 C68 1.539(5) . ?
C68 C69 1.385(6) . ?
C68 C73 1.399(6) . ?
C69 C70 1.400(6) . ?
C70 C71 1.386(7) . ?
C71 C72 1.378(8) . ?
C72 C73 1.385(7) . ?
C74 C79 1.381(6) . ?
C74 C75 1.404(7) . ?
C75 C76 1.389(7) . ?
C76 C77 1.386(8) . ?
C77 C78 1.374(8) . ?
C78 C79 1.390(7) . ?
C80 C81 1.538(6) . ?
C80 C82 1.543(7) . ?
C83 C84 1.536(6) . ?
C83 C85 1.545(6) . ?
C86 C87 1.510(7) . ?
C86 C88 1.529(8) . ?
C89 C90 1.554(6) . ?
C91 C91 1.495(8) 2_455 ?
C91 C92 1.496(8) . ?
C93 C92 1.495(8) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Ge1 C89 106.08(16) . . ?
N2 Ge2 C90 108.55(16) . . ?
N1 Si1 C39 111.58(18) . . ?
N1 Si1 C42 108.49(18) . . ?
C39 Si1 C42 107.7(2) . . ?
N1 Si1 C36 109.96(17) . . ?
C39 Si1 C36 109.7(2) . . ?
C42 Si1 C36 109.3(2) . . ?
N2 Si2 C80 110.71(18) . . ?
N2 Si2 C83 108.39(18) . . ?
C80 Si2 C83 108.9(2) . . ?
N2 Si2 C86 110.99(19) . . ?
C80 Si2 C86 111.0(2) . . ?
C83 Si2 C86 106.6(2) . . ?
C1 N1 Si1 122.1(2) . . ?
C1 N1 Ge1 117.5(2) . . ?
Si1 N1 Ge1 120.24(17) . . ?
C45 N2 Si2 124.8(2) . . ?
C45 N2 Ge2 115.3(2) . . ?
Si2 N2 Ge2 119.87(18) . . ?
C2 C1 C6 118.8(3) . . ?
C2 C1 N1 121.0(4) . . ?
C6 C1 N1 120.2(3) . . ?
C3 C2 C1 119.6(4) . . ?
C3 C2 C10 118.4(3) . . ?
C1 C2 C10 121.9(3) . . ?
C4 C3 C2 122.6(3) . . ?
C3 C4 C5 117.4(4) . . ?
C3 C4 C7 121.5(3) . . ?
C5 C4 C7 121.0(4) . . ?
C4 C5 C6 122.2(4) . . ?
C5 C6 C1 119.3(3) . . ?
C5 C6 C23 118.9(4) . . ?
C1 C6 C23 121.7(3) . . ?
C4 C7 C9 114.4(3) . . ?
C4 C7 C8 108.5(3) . . ?
C9 C7 C8 109.0(4) . . ?
C2 C10 C17 114.1(3) . . ?
C2 C10 C11 112.7(3) . . ?
C17 C10 C11 112.8(3) . . ?
C12 C11 C16 116.9(4) . . ?
C12 C11 C10 124.0(4) . . ?
C16 C11 C10 119.1(4) . . ?
C11 C12 C13 121.6(4) . . ?
C14 C13 C12 120.3(5) . . ?
C13 C14 C15 119.6(4) . . ?
C14 C15 C16 120.4(5) . . ?
C15 C16 C11 121.3(4) . . ?
C22 C17 C18 117.2(4) . . ?
C22 C17 C10 122.5(4) . . ?
C18 C17 C10 120.1(4) . . ?
C19 C18 C17 120.9(4) . . ?
C20 C19 C18 121.0(4) . . ?
C21 C20 C19 118.6(4) . . ?
C20 C21 C22 120.8(4) . . ?
C17 C22 C21 121.4(4) . . ?
C30 C23 C24 112.2(3) . . ?
C30 C23 C6 111.0(3) . . ?
C24 C23 C6 114.6(3) . . ?
C29 C24 C25 117.5(4) . . ?
C29 C24 C23 121.7(4) . . ?
C25 C24 C23 120.8(3) . . ?
C26 C25 C24 121.1(4) . . ?
C25 C26 C27 120.3(4) . . ?
C28 C27 C26 119.6(4) . . ?
C27 C28 C29 119.8(4) . . ?
C28 C29 C24 121.7(4) . . ?
C35 C30 C31 118.1(4) . . ?
C35 C30 C23 122.3(4) . . ?
C31 C30 C23 119.5(4) . . ?
C32 C31 C30 121.3(4) . . ?
C33 C32 C31 119.7(4) . . ?
C32 C33 C34 120.5(4) . . ?
C33 C34 C35 119.4(5) . . ?
C30 C35 C34 121.0(4) . . ?
C38 C36 C37 110.0(4) . . ?
C38 C36 Si1 113.7(3) . . ?
C37 C36 Si1 113.9(3) . . ?
C40 C39 C41 112.3(4) . . ?
C40 C39 Si1 120.3(4) . . ?
C41 C39 Si1 113.4(3) . . ?
C44 C42 C43 109.8(4) . . ?
C44 C42 Si1 114.9(3) . . ?
C43 C42 Si1 112.7(3) . . ?
C50 C45 C46 117.9(4) . . ?
C50 C45 N2 121.4(3) . . ?
C46 C45 N2 120.7(3) . . ?
C47 C46 C45 119.0(4) . . ?
C47 C46 C54 118.3(3) . . ?
C45 C46 C54 122.7(4) . . ?
C48 C47 C46 123.3(4) . . ?
C49 C48 C47 116.9(4) . . ?
C49 C48 C51 120.8(4) . . ?
C47 C48 C51 122.3(4) . . ?
C48 C49 C50 122.8(4) . . ?
C49 C50 C45 120.1(4) . . ?
C49 C50 C67 117.2(4) . . ?
C45 C50 C67 122.7(4) . . ?
C52 C51 C48 114.5(5) . . ?
C52 C51 C53 106.8(5) . . ?
C48 C51 C53 112.1(4) . . ?
C46 C54 C55 112.7(3) . . ?
C46 C54 C61 115.0(3) . . ?
C55 C54 C61 110.4(3) . . ?
C60 C55 C56 117.6(4) . . ?
C60 C55 C54 122.7(4) . . ?
C56 C55 C54 119.7(4) . . ?
C55 C56 C57 121.0(5) . . ?
C58 C57 C56 120.6(5) . . ?
C57 C58 C59 119.6(5) . . ?
C58 C59 C60 120.2(5) . . ?
C55 C60 C59 121.1(5) . . ?
C62 C61 C66 117.8(4) . . ?
C62 C61 C54 118.3(4) . . ?
C66 C61 C54 123.8(4) . . ?
C63 C62 C61 122.0(5) . . ?
C62 C63 C64 119.4(5) . . ?
C65 C64 C63 119.8(5) . . ?
C64 C65 C66 121.2(5) . . ?
C61 C66 C65 119.7(5) . . ?
C74 C67 C50 111.2(3) . . ?
C74 C67 C68 110.8(3) . . ?
C50 C67 C68 113.4(3) . . ?
C69 C68 C73 117.7(4) . . ?
C69 C68 C67 124.8(4) . . ?
C73 C68 C67 117.5(4) . . ?
C68 C69 C70 121.2(4) . . ?
C71 C70 C69 120.4(5) . . ?
C72 C71 C70 118.6(4) . . ?
C71 C72 C73 121.3(5) . . ?
C72 C73 C68 120.8(5) . . ?
C79 C74 C75 117.6(4) . . ?
C79 C74 C67 120.4(4) . . ?
C75 C74 C67 121.9(4) . . ?
C76 C75 C74 121.6(4) . . ?
C77 C76 C75 119.3(5) . . ?
C78 C77 C76 119.6(5) . . ?
C77 C78 C79 120.9(5) . . ?
C74 C79 C78 120.9(5) . . ?
C81 C80 C82 109.0(4) . . ?
C81 C80 Si2 116.2(3) . . ?
C82 C80 Si2 112.5(4) . . ?
C84 C83 C85 109.7(4) . . ?
C84 C83 Si2 113.2(3) . . ?
C85 C83 Si2 115.9(3) . . ?
C87 C86 C88 111.3(4) . . ?
C87 C86 Si2 121.4(4) . . ?
C88 C86 Si2 112.5(3) . . ?
C90 C89 Ge1 109.5(3) . . ?
C89 C90 Ge2 110.3(3) . . ?
C91 C91 C92 112(2) 2_455 . ?
C93 C92 C91 106.7(14) . . ?

_diffrn_measured_fraction_theta_max 0.937
_diffrn_reflns_theta_full        25.25
_diffrn_measured_fraction_theta_full 0.937
_refine_diff_density_max         1.189
_refine_diff_density_min         -0.832
_refine_diff_density_rms         0.084
####################################################################### 
# 
# 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_LPhC2H4GeO2
_database_code_depnum_ccdc_archive 'CCDC 1422726'
_audit_update_record             
;
2015-09-07 deposited with the CCDC.
2015-09-22 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C104 H122 Ge2 N2 O2 Si2'
_chemical_formula_weight         1633.40

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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   P2(1)/n

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

_cell_length_a                   13.373(3)
_cell_length_b                   21.643(4)
_cell_length_c                   15.884(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 102.62(3)
_cell_angle_gamma                90.00
_cell_volume                     4486.3(16)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.209
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1736
_exptl_absorpt_coefficient_mu    0.747
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.923
_exptl_absorpt_correction_T_max  0.961
_exptl_absorpt_process_details   XDS

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71080
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_source         'Australian Synchrotron'
_diffrn_radiation_monochromator  ?
_diffrn_measurement_device_type  'ADSC Quantum 210r'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            59686
_diffrn_reflns_av_R_equivalents  0.0947
_diffrn_reflns_av_sigmaI/netI    0.0452
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         2.93
_diffrn_reflns_theta_max         25.50
_reflns_number_total             8072
_reflns_number_gt                5590
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Blu-Ice (McPhillips, 2002)'
_computing_cell_refinement       'XDS (Kabsch, 1993)'
_computing_data_reduction        'XDS (Kabsch, 1993)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    X-Seed
_computing_publication_material  CifTAB

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger.
 The carbon atoms of the SiPri3 group were found to be disordered over two 
 sites. This disorder was modelled, and the carbon atoms of the minor 
 occupied disorded set, refined isotropically.
 The low value (96.7%) for completeness of data to theta = 25.5 deg. arises 
 from hardware constraints associated with the diffractometer used at the 
 Australian Synchrotron.Its minimum crystal to detector distance is 72 mm 
 and its goniometer only rotates about the phi axis.
  
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0622P)²+8.5051P] 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     SHELXL
_refine_ls_extinction_coef       0.0159(11)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         8072
_refine_ls_number_parameters     548
_refine_ls_number_restraints     69
_refine_ls_R_factor_all          0.1042
_refine_ls_R_factor_gt           0.0699
_refine_ls_wR_factor_ref         0.1796
_refine_ls_wR_factor_gt          0.1581
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_restrained_S_all      1.095
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ge1 Ge 0.47842(4) 0.03409(3) 0.92975(3) 0.0546(2) Uani 1 1 d . . .
Si1 Si 0.22588(10) 0.02649(7) 0.87159(9) 0.0606(4) Uani 1 1 d D . .
O1 O 0.5017(3) -0.04646(17) 0.9554(2) 0.0627(10) Uani 1 1 d . . .
N1 N 0.3500(3) 0.05387(19) 0.8647(2) 0.0545(10) Uani 1 1 d . A .
C1 C 0.3598(4) 0.0993(2) 0.7984(3) 0.0556(13) Uani 1 1 d . . .
C2 C 0.3595(4) 0.1626(3) 0.8159(3) 0.0623(14) Uani 1 1 d . A .
C3 C 0.3779(5) 0.2045(3) 0.7541(4) 0.0824(19) Uani 1 1 d . . .
H3 H 0.3770 0.2475 0.7661 0.099 Uiso 1 1 calc R A .
C4 C 0.3971(6) 0.1855(3) 0.6767(4) 0.093(2) Uani 1 1 d . A .
C5 C 0.3950(6) 0.1234(3) 0.6595(4) 0.085(2) Uani 1 1 d . . .
H5 H 0.4069 0.1100 0.6056 0.102 Uiso 1 1 calc R A .
C6 C 0.3759(4) 0.0791(3) 0.7180(3) 0.0645(14) Uani 1 1 d . A .
C7 C 0.4254(9) 0.2324(4) 0.6131(6) 0.131(3) Uani 1 1 d U . .
H7 H 0.3740 0.2632 0.6242 0.157 Uiso 1 1 calc R A .
C8 C 0.5088(7) 0.2707(4) 0.6495(5) 0.121(3) Uani 1 1 d . A .
H8A H 0.5700 0.2453 0.6694 0.182 Uiso 1 1 calc R . .
H8B H 0.4931 0.2934 0.6985 0.182 Uiso 1 1 calc R . .
H8C H 0.5212 0.3001 0.6060 0.182 Uiso 1 1 calc R . .
C9 C 0.3762(7) 0.2253(5) 0.5286(6) 0.131(3) Uani 1 1 d U A .
H9A H 0.3944 0.2595 0.4944 0.196 Uiso 1 1 calc R . .
H9B H 0.3019 0.2251 0.5241 0.196 Uiso 1 1 calc R . .
H9C H 0.3969 0.1860 0.5067 0.196 Uiso 1 1 calc R . .
C10 C 0.3413(4) 0.1891(3) 0.9010(3) 0.0652(14) Uani 1 1 d . . .
H10 H 0.3336 0.1528 0.9379 0.078 Uiso 1 1 calc R A .
C11 C 0.4326(4) 0.2265(3) 0.9519(4) 0.0690(15) Uani 1 1 d . A .
C12 C 0.4952(5) 0.2018(3) 1.0246(4) 0.096(2) Uani 1 1 d . . .
H12 H 0.4833 0.1610 1.0422 0.115 Uiso 1 1 calc R A .
C13 C 0.5768(6) 0.2368(4) 1.0728(5) 0.106(2) Uani 1 1 d U A .
H13 H 0.6174 0.2202 1.1245 0.128 Uiso 1 1 calc R . .
C14 C 0.5971(7) 0.2925(5) 1.0468(7) 0.115(3) Uani 1 1 d U . .
H14 H 0.6556 0.3143 1.0773 0.138 Uiso 1 1 calc R A .
C15 C 0.5361(8) 0.3184(4) 0.9780(7) 0.122(3) Uani 1 1 d . A .
H15 H 0.5486 0.3594 0.9619 0.147 Uiso 1 1 calc R . .
C16 C 0.4533(5) 0.2848(3) 0.9294(5) 0.089(2) Uani 1 1 d . . .
H16 H 0.4110 0.3033 0.8800 0.107 Uiso 1 1 calc R A .
C17 C 0.2436(5) 0.2273(3) 0.8931(4) 0.0773(17) Uani 1 1 d . A .
C18 C 0.2186(5) 0.2472(4) 0.9674(5) 0.102(2) Uani 1 1 d . . .
H18 H 0.2623 0.2371 1.0213 0.122 Uiso 1 1 calc R A .
C19 C 0.1294(7) 0.2824(5) 0.9662(7) 0.133(4) Uani 1 1 d . A .
H19 H 0.1133 0.2964 1.0183 0.160 Uiso 1 1 calc R . .
C20 C 0.0658(7) 0.2959(4) 0.8871(7) 0.119(3) Uani 1 1 d U . .
H20 H 0.0051 0.3192 0.8850 0.143 Uiso 1 1 calc R A .
C21 C 0.0888(6) 0.2765(4) 0.8143(6) 0.105(2) Uani 1 1 d U A .
H21 H 0.0442 0.2863 0.7608 0.126 Uiso 1 1 calc R . .
C22 C 0.1767(5) 0.2423(3) 0.8149(5) 0.088(2) Uani 1 1 d . . .
H22 H 0.1916 0.2290 0.7620 0.106 Uiso 1 1 calc R A .
C23 C 0.3741(4) 0.0110(3) 0.6924(3) 0.0652(14) Uani 1 1 d . . .
H23 H 0.3562 -0.0121 0.7417 0.078 Uiso 1 1 calc R A .
C24 C 0.2908(4) -0.0062(3) 0.6128(3) 0.0673(15) Uani 1 1 d . A .
C25 C 0.2230(5) 0.0349(3) 0.5649(4) 0.091(2) Uani 1 1 d . . .
H25 H 0.2275 0.0776 0.5794 0.109 Uiso 1 1 calc R A .
C26 C 0.1476(6) 0.0146(4) 0.4954(4) 0.100(2) Uani 1 1 d . A .
H26 H 0.1019 0.0439 0.4629 0.120 Uiso 1 1 calc R . .
C27 C 0.1380(5) -0.0445(4) 0.4734(4) 0.094(2) Uani 1 1 d . . .
H27 H 0.0860 -0.0576 0.4260 0.113 Uiso 1 1 calc R A .
C28 C 0.2044(6) -0.0862(3) 0.5200(4) 0.098(2) Uani 1 1 d . A .
H28 H 0.1987 -0.1288 0.5051 0.118 Uiso 1 1 calc R . .
C29 C 0.2794(5) -0.0668(3) 0.5885(4) 0.0849(19) Uani 1 1 d . . .
H29 H 0.3249 -0.0966 0.6200 0.102 Uiso 1 1 calc R A .
C30 C 0.4782(5) -0.0147(3) 0.6835(3) 0.0694(16) Uani 1 1 d . A .
C31 C 0.5249(5) 0.0028(3) 0.6176(4) 0.0833(19) Uani 1 1 d . . .
H31 H 0.4918 0.0321 0.5762 0.100 Uiso 1 1 calc R A .
C32 C 0.6180(6) -0.0211(4) 0.6104(4) 0.095(2) Uani 1 1 d . A .
H32 H 0.6488 -0.0078 0.5650 0.114 Uiso 1 1 calc R . .
C33 C 0.6664(6) -0.0641(4) 0.6689(5) 0.094(2) Uani 1 1 d . . .
H33 H 0.7309 -0.0805 0.6644 0.112 Uiso 1 1 calc R A .
C34 C 0.6204(6) -0.0832(3) 0.7345(4) 0.087(2) Uani 1 1 d . A .
H34 H 0.6532 -0.1133 0.7748 0.105 Uiso 1 1 calc R . .
C35 C 0.5271(5) -0.0588(3) 0.7417(4) 0.0758(17) Uani 1 1 d . . .
H35 H 0.4962 -0.0724 0.7869 0.091 Uiso 1 1 calc R A .
C36 C 0.1744(5) 0.0814(4) 0.9467(5) 0.065(2) Uani 0.654(5) 1 d PD A 1
H36 H 0.1834 0.1237 0.9242 0.078 Uiso 0.654(5) 1 calc PR A 1
C36A C 0.2300(10) 0.0045(7) 0.9874(6) 0.070(4) Uiso 0.346(5) 1 d PD A 2
H36A H 0.2966 -0.0173 1.0085 0.084 Uiso 0.346(5) 1 calc PR A 2
C37 C 0.2354(9) 0.0822(8) 1.0403(5) 0.065(3) Uani 0.654(5) 1 d PD A 1
H37A H 0.2129 0.1171 1.0709 0.097 Uiso 0.654(5) 1 calc PR A 1
H37B H 0.3085 0.0864 1.0412 0.097 Uiso 0.654(5) 1 calc PR A 1
H37C H 0.2237 0.0435 1.0688 0.097 Uiso 0.654(5) 1 calc PR A 1
C38 C 0.0593(6) 0.0764(5) 0.9448(7) 0.081(3) Uani 0.654(5) 1 d PD A 1
H38A H 0.0446 0.0357 0.9665 0.122 Uiso 0.654(5) 1 calc PR A 1
H38B H 0.0202 0.0815 0.8854 0.122 Uiso 0.654(5) 1 calc PR A 1
H38C H 0.0398 0.1087 0.9813 0.122 Uiso 0.654(5) 1 calc PR A 1
C39 C 0.2442(5) -0.0539(4) 0.9153(5) 0.063(2) Uani 0.654(5) 1 d PD A 1
H39 H 0.3080 -0.0526 0.9619 0.075 Uiso 0.654(5) 1 calc PR A 1
C40 C 0.2661(11) -0.0993(5) 0.8482(8) 0.070(4) Uani 0.654(5) 1 d PD A 1
H40A H 0.2649 -0.1416 0.8701 0.105 Uiso 0.654(5) 1 calc PR A 1
H40B H 0.3338 -0.0906 0.8366 0.105 Uiso 0.654(5) 1 calc PR A 1
H40C H 0.2137 -0.0950 0.7947 0.105 Uiso 0.654(5) 1 calc PR A 1
C41 C 0.1590(5) -0.0753(4) 0.9592(5) 0.066(2) Uani 0.654(5) 1 d PD A 1
H41A H 0.0930 -0.0739 0.9176 0.099 Uiso 0.654(5) 1 calc PR A 1
H41B H 0.1566 -0.0480 1.0080 0.099 Uiso 0.654(5) 1 calc PR A 1
H41C H 0.1728 -0.1177 0.9801 0.099 Uiso 0.654(5) 1 calc PR A 1
C41A C 0.0865(8) -0.0697(8) 0.7747(12) 0.078(5) Uiso 0.346(5) 1 d PD A 2
H41D H 0.0845 -0.1057 0.7370 0.117 Uiso 0.346(5) 1 calc PR A 2
H41E H 0.0400 -0.0378 0.7447 0.117 Uiso 0.346(5) 1 calc PR A 2
H41F H 0.0651 -0.0820 0.8275 0.117 Uiso 0.346(5) 1 calc PR A 2
C42 C 0.1370(5) 0.0288(4) 0.7628(5) 0.066(2) Uani 0.654(5) 1 d PD A 1
H42 H 0.1761 0.0109 0.7216 0.079 Uiso 0.654(5) 1 calc PR A 1
C43 C 0.1016(15) 0.0927(6) 0.7278(7) 0.072(7) Uani 0.654(5) 1 d PD A 1
H43A H 0.0575 0.0886 0.6700 0.109 Uiso 0.654(5) 1 calc PR A 1
H43B H 0.1615 0.1180 0.7246 0.109 Uiso 0.654(5) 1 calc PR A 1
H43C H 0.0632 0.1125 0.7663 0.109 Uiso 0.654(5) 1 calc PR A 1
C44 C 0.0412(6) -0.0118(4) 0.7556(7) 0.082(3) Uani 0.654(5) 1 d PD A 1
H44A H -0.0061 0.0079 0.7865 0.123 Uiso 0.654(5) 1 calc PR A 1
H44B H 0.0613 -0.0524 0.7809 0.123 Uiso 0.654(5) 1 calc PR A 1
H44C H 0.0074 -0.0168 0.6947 0.123 Uiso 0.654(5) 1 calc PR A 1
C44A C 0.0228(10) 0.0770(10) 0.8547(13) 0.088(6) Uiso 0.346(5) 1 d PD A 2
H44D H -0.0250 0.1100 0.8302 0.132 Uiso 0.346(5) 1 calc PR A 2
H44E H 0.0349 0.0782 0.9178 0.132 Uiso 0.346(5) 1 calc PR A 2
H44F H -0.0065 0.0369 0.8339 0.132 Uiso 0.346(5) 1 calc PR A 2
C45 C 0.5872(5) 0.0632(3) 0.8715(4) 0.090(2) Uani 1 1 d . . .
H45A H 0.6482 0.0366 0.8908 0.108 Uiso 1 1 calc R . .
H45B H 0.5628 0.0567 0.8087 0.108 Uiso 1 1 calc R . .
C46 C 0.6191(6) 0.1260(3) 0.8850(4) 0.098(2) Uani 1 1 d . . .
H46A H 0.6536 0.1318 0.9462 0.117 Uiso 1 1 calc R . .
H46B H 0.5581 0.1531 0.8725 0.117 Uiso 1 1 calc R . .
C47 C 0.6954(4) 0.1456(3) 0.8253(4) 0.0663(15) Uani 1 1 d . . .
C48 C 0.7308(6) 0.1122(4) 0.7694(6) 0.105(2) Uani 1 1 d . . .
H48 H 0.7089 0.0704 0.7614 0.126 Uiso 1 1 calc R . .
C49 C 0.7945(8) 0.1328(5) 0.7238(6) 0.136(3) Uani 1 1 d U . .
H49 H 0.8207 0.1052 0.6873 0.163 Uiso 1 1 calc R . .
C50 C 0.8225(7) 0.1907(5) 0.7279(6) 0.126(3) Uani 1 1 d U . .
H50 H 0.8654 0.2051 0.6917 0.151 Uiso 1 1 calc R . .
C51 C 0.7916(7) 0.2311(4) 0.7831(7) 0.124(3) Uani 1 1 d U . .
H51 H 0.8135 0.2730 0.7871 0.148 Uiso 1 1 calc R . .
C52 C 0.7231(4) 0.2069(2) 0.8357(3) 0.102(2) Uani 1 1 d . . .
H52 H 0.6987 0.2326 0.8755 0.122 Uiso 1 1 calc R . .
C38A C 0.1471(4) -0.0384(2) 1.0052(3) 0.082(5) Uiso 0.346(5) 1 d PRD A 2
H38D H 0.1414 -0.0337 1.0653 0.123 Uiso 0.346(5) 1 calc PR A 2
H38E H 0.1651 -0.0813 0.9950 0.123 Uiso 0.346(5) 1 calc PR A 2
H38F H 0.0815 -0.0280 0.9667 0.123 Uiso 0.346(5) 1 calc PR A 2
C39A C 0.1953(4) -0.0441(2) 0.7979(3) 0.068(4) Uiso 0.346(5) 1 d PRD A 2
H39A H 0.2110 -0.0311 0.7418 0.081 Uiso 0.346(5) 1 calc PR A 2
C42A C 0.1244(4) 0.0863(2) 0.8269(3) 0.067(4) Uiso 0.346(5) 1 d PRD A 2
H42A H 0.1523 0.1260 0.8547 0.080 Uiso 0.346(5) 1 calc PR A 2
C37A C 0.232(3) 0.0611(11) 1.0446(18) 0.097(14) Uiso 0.346(5) 1 d PD A 2
H37D H 0.1765 0.0892 1.0186 0.145 Uiso 0.346(5) 1 calc PR A 2
H37E H 0.2980 0.0823 1.0505 0.145 Uiso 0.346(5) 1 calc PR A 2
H37F H 0.2232 0.0482 1.1017 0.145 Uiso 0.346(5) 1 calc PR A 2
C43A C 0.110(4) 0.0981(17) 0.7306(8) 0.086(17) Uiso 0.346(5) 1 d PD A 2
H43D H 0.0813 0.0611 0.6986 0.129 Uiso 0.346(5) 1 calc PR A 2
H43E H 0.1758 0.1082 0.7170 0.129 Uiso 0.346(5) 1 calc PR A 2
H43F H 0.0623 0.1328 0.7140 0.129 Uiso 0.346(5) 1 calc PR A 2
C40A C 0.261(3) -0.1014(13) 0.825(2) 0.089(11) Uiso 0.346(5) 1 d PD A 2
H40D H 0.2506 -0.1161 0.8810 0.133 Uiso 0.346(5) 1 calc PR A 2
H40E H 0.3335 -0.0909 0.8303 0.133 Uiso 0.346(5) 1 calc PR A 2
H40F H 0.2414 -0.1339 0.7818 0.133 Uiso 0.346(5) 1 calc PR 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 O1 1.802(4) . ?
Ge1 O1 1.805(3) 3_657 ?
Ge1 N1 1.851(4) . ?
Ge1 C45 1.989(8) . ?
Ge1 Ge1 2.6323(11) 3_657 ?
Si1 N1 1.788(4) . ?
Si1 C39 1.870(8) . ?
Si1 C42 1.872(7) . ?
Si1 C36A 1.889(8) . ?
Si1 C42A 1.897(5) . ?
Si1 C39A 1.914(5) . ?
Si1 C36 1.916(9) . ?
O1 Ge1 1.805(3) 3_657 ?
N1 C1 1.467(6) . ?
C1 C2 1.398(7) . ?
C1 C6 1.411(7) . ?
C2 C3 1.398(7) . ?
C2 C10 1.536(8) . ?
C3 C4 1.373(9) . ?
C4 C5 1.371(9) . ?
C4 C7 1.536(9) . ?
C5 C6 1.396(7) . ?
C6 C23 1.527(8) . ?
C7 C9 1.369(11) . ?
C7 C8 1.409(11) . ?
C10 C17 1.527(8) . ?
C10 C11 1.539(7) . ?
C11 C16 1.356(9) . ?
C11 C12 1.378(8) . ?
C12 C13 1.409(10) . ?
C13 C14 1.322(12) . ?
C14 C15 1.337(12) . ?
C15 C16 1.406(10) . ?
C17 C18 1.364(10) . ?
C17 C22 1.401(8) . ?
C18 C19 1.412(10) . ?
C19 C20 1.385(12) . ?
C20 C21 1.328(12) . ?
C21 C22 1.387(10) . ?
C23 C30 1.535(8) . ?
C23 C24 1.537(7) . ?
C24 C29 1.368(8) . ?
C24 C25 1.375(8) . ?
C25 C26 1.394(8) . ?
C26 C27 1.325(10) . ?
C27 C28 1.365(10) . ?
C28 C29 1.374(8) . ?
C30 C31 1.385(9) . ?
C30 C35 1.389(8) . ?
C31 C32 1.374(10) . ?
C32 C33 1.374(10) . ?
C33 C34 1.384(10) . ?
C34 C35 1.383(9) . ?
C36 C37 1.532(7) . ?
C36 C38 1.536(7) . ?
C36A C38A 1.519(8) . ?
C36A C37A 1.522(8) . ?
C39 C40 1.526(8) . ?
C39 C41 1.532(7) . ?
C41A C39A 1.525(8) . ?
C42 C43 1.527(8) . ?
C42 C44 1.536(7) . ?
C44A C42A 1.531(8) . ?
C45 C46 1.426(9) . ?
C46 C47 1.594(9) . ?
C47 C48 1.311(9) . ?
C47 C52 1.379(8) . ?
C48 C49 1.311(11) . ?
C49 C50 1.306(12) . ?
C50 C51 1.363(12) . ?
C51 C52 1.466(11) . ?
C39A C40A 1.526(8) . ?
C42A C43A 1.521(8) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Ge1 O1 86.27(17) . 3_657 ?
O1 Ge1 N1 116.34(16) . . ?
O1 Ge1 N1 116.34(17) 3_657 . ?
O1 Ge1 C45 107.7(2) . . ?
O1 Ge1 C45 117.5(2) 3_657 . ?
N1 Ge1 C45 110.5(2) . . ?
O1 Ge1 Ge1 43.18(11) . 3_657 ?
O1 Ge1 Ge1 43.09(12) 3_657 3_657 ?
N1 Ge1 Ge1 127.44(13) . 3_657 ?
C45 Ge1 Ge1 121.63(18) . 3_657 ?
N1 Si1 C39 106.5(3) . . ?
N1 Si1 C42 110.2(3) . . ?
C39 Si1 C42 111.9(3) . . ?
N1 Si1 C36A 108.3(4) . . ?
C39 Si1 C36A 55.3(5) . . ?
C42 Si1 C36A 141.5(4) . . ?
N1 Si1 C42A 110.4(2) . . ?
C39 Si1 C42A 143.0(3) . . ?
C42 Si1 C42A 51.6(3) . . ?
C36A Si1 C42A 113.7(6) . . ?
N1 Si1 C39A 107.7(2) . . ?
C39 Si1 C39A 58.5(3) . . ?
C42 Si1 C39A 56.5(3) . . ?
C36A Si1 C39A 110.6(5) . . ?
C42A Si1 C39A 106.0(2) . . ?
N1 Si1 C36 107.3(3) . . ?
C39 Si1 C36 112.4(3) . . ?
C42 Si1 C36 108.5(4) . . ?
C36A Si1 C36 59.2(6) . . ?
C42A Si1 C36 59.0(3) . . ?
C39A Si1 C36 144.9(3) . . ?
Ge1 O1 Ge1 93.73(17) . 3_657 ?
C1 N1 Si1 119.7(3) . . ?
C1 N1 Ge1 109.8(3) . . ?
Si1 N1 Ge1 130.5(2) . . ?
C2 C1 C6 119.5(5) . . ?
C2 C1 N1 120.6(5) . . ?
C6 C1 N1 119.8(5) . . ?
C1 C2 C3 119.2(5) . . ?
C1 C2 C10 123.4(5) . . ?
C3 C2 C10 117.4(5) . . ?
C4 C3 C2 122.0(6) . . ?
C5 C4 C3 118.2(6) . . ?
C5 C4 C7 120.9(7) . . ?
C3 C4 C7 120.8(7) . . ?
C4 C5 C6 122.6(6) . . ?
C5 C6 C1 118.4(5) . . ?
C5 C6 C23 118.7(5) . . ?
C1 C6 C23 122.9(4) . . ?
C9 C7 C8 129.6(8) . . ?
C9 C7 C4 115.8(7) . . ?
C8 C7 C4 113.9(7) . . ?
C17 C10 C2 115.3(5) . . ?
C17 C10 C11 109.0(5) . . ?
C2 C10 C11 113.5(5) . . ?
C16 C11 C12 117.4(6) . . ?
C16 C11 C10 122.4(6) . . ?
C12 C11 C10 120.2(6) . . ?
C11 C12 C13 120.2(8) . . ?
C14 C13 C12 120.5(8) . . ?
C13 C14 C15 120.5(9) . . ?
C14 C15 C16 120.0(9) . . ?
C11 C16 C15 121.2(8) . . ?
C18 C17 C22 117.6(7) . . ?
C18 C17 C10 117.8(6) . . ?
C22 C17 C10 124.6(6) . . ?
C17 C18 C19 121.6(8) . . ?
C20 C19 C18 118.4(9) . . ?
C21 C20 C19 120.7(9) . . ?
C20 C21 C22 121.3(8) . . ?
C21 C22 C17 120.4(8) . . ?
C6 C23 C30 114.4(5) . . ?
C6 C23 C24 114.7(5) . . ?
C30 C23 C24 110.2(5) . . ?
C29 C24 C25 116.4(5) . . ?
C29 C24 C23 118.7(5) . . ?
C25 C24 C23 124.8(6) . . ?
C24 C25 C26 120.7(7) . . ?
C27 C26 C25 121.7(7) . . ?
C26 C27 C28 118.7(6) . . ?
C27 C28 C29 120.3(7) . . ?
C24 C29 C28 122.2(6) . . ?
C31 C30 C35 117.8(6) . . ?
C31 C30 C23 122.6(5) . . ?
C35 C30 C23 119.5(6) . . ?
C32 C31 C30 121.8(6) . . ?
C33 C32 C31 120.0(7) . . ?
C32 C33 C34 119.4(7) . . ?
C35 C34 C33 120.4(7) . . ?
C34 C35 C30 120.7(7) . . ?
C37 C36 C38 109.8(8) . . ?
C37 C36 Si1 115.1(7) . . ?
C38 C36 Si1 116.0(6) . . ?
C38A C36A C37A 107.5(17) . . ?
C38A C36A Si1 117.9(6) . . ?
C37A C36A Si1 111.8(15) . . ?
C40 C39 C41 113.5(9) . . ?
C40 C39 Si1 111.7(6) . . ?
C41 C39 Si1 113.6(6) . . ?
C43 C42 C44 107.7(10) . . ?
C43 C42 Si1 116.3(6) . . ?
C44 C42 Si1 113.9(6) . . ?
C46 C45 Ge1 117.2(6) . . ?
C45 C46 C47 112.0(6) . . ?
C48 C47 C52 119.0(6) . . ?
C48 C47 C46 128.9(7) . . ?
C52 C47 C46 112.1(6) . . ?
C49 C48 C47 124.2(9) . . ?
C50 C49 C48 120.8(10) . . ?
C49 C50 C51 121.6(9) . . ?
C50 C51 C52 116.9(7) . . ?
C47 C52 C51 117.4(6) . . ?
C41A C39A C40A 104(2) . . ?
C41A C39A Si1 120.2(8) . . ?
C40A C39A Si1 116.2(15) . . ?
C43A C42A C44A 113(2) . . ?
C43A C42A Si1 114.6(15) . . ?
C44A C42A Si1 114.2(9) . . ?

_diffrn_measured_fraction_theta_max 0.967
_diffrn_reflns_theta_full        25.50
_diffrn_measured_fraction_theta_full 0.967
_refine_diff_density_max         0.994
_refine_diff_density_min         -0.737
_refine_diff_density_rms         0.065
####################################################################### 
# 
# 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_compound5
_database_code_depnum_ccdc_archive 'CCDC 1422727'
_audit_update_record             
;
2015-09-07 deposited with the CCDC.
2015-09-22 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C46 H57 Ge N Si'
_chemical_formula_weight         724.61

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'

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   P-1

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   10.783(2)
_cell_length_b                   11.465(2)
_cell_length_c                   16.298(3)
_cell_angle_alpha                97.01(3)
_cell_angle_beta                 91.76(3)
_cell_angle_gamma                92.77(3)
_cell_volume                     1996.1(7)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.01
_exptl_crystal_size_mid          0.01
_exptl_crystal_size_min          0.01
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.206
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             772
_exptl_absorpt_coefficient_mu    0.829
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.985
_exptl_absorpt_correction_T_max  0.990
_exptl_absorpt_process_details   XDS

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71080
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_source         'Australian Synchrotron'
_diffrn_radiation_monochromator  ?
_diffrn_measurement_device_type  'ADSC Quantum 210r'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            25550
_diffrn_reflns_av_R_equivalents  0.0495
_diffrn_reflns_av_sigmaI/netI    0.0392
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         3.08
_diffrn_reflns_theta_max         25.20
_reflns_number_total             6617
_reflns_number_gt                5669
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Blu-Ice (McPhillips, 2002)'
_computing_cell_refinement       'XDS (Kabsch, 1993)'
_computing_data_reduction        'XDS (Kabsch, 1993)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    X-Seed
_computing_publication_material  CifTAB

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger.
 The germanium atom was found to be disordered over two sites in an approx
 92:8 ratio. The ADP for the minor site was refined isotropically. Although
 an ethyl ligand, the atoms of which have ca. 8% occupancy, is likely attached
 to the minor occupancy Ge center, it proved difficult to locate these partially
 occupied atoms from difference maps. Accordingly, the C and H atoms of the 
 ethyl ligand bonded to the major occupancy Ge atom were refined at full 
 occupancy.  
 The low value (92.o%) for completeness of data to theta = 25.2 deg. arises 
 from hardware constraints associated with the diffractometer used at the 
 Australian Synchrotron and is common for triclinic data sets on that instrument. 
 Its minimum crystal to detector distance is 72 mm and its
 goniometer only rotates about the phi axis.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0394P)²+1.9227P] 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     SHELXL
_refine_ls_extinction_coef       0.0194(14)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         6617
_refine_ls_number_parameters     457
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0496
_refine_ls_R_factor_gt           0.0405
_refine_ls_wR_factor_ref         0.0996
_refine_ls_wR_factor_gt          0.0955
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_restrained_S_all      1.049
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ge1 Ge 0.94740(3) 0.79841(3) 0.637559(18) 0.02768(13) Uani 0.9205(17) 1 d P A 1
Ge1A Ge 0.9665(4) 0.7755(5) 0.6997(3) 0.054(2) Uiso 0.0795(17) 1 d PD A 2
Si1 Si 0.66314(6) 0.82929(6) 0.61874(4) 0.01951(17) Uani 1 1 d . A .
N1 N 0.78904(17) 0.78914(18) 0.68129(12) 0.0194(4) Uani 1 1 d D . .
C1 C 0.7726(2) 0.7563(2) 0.76315(14) 0.0184(5) Uani 1 1 d . A .
C2 C 0.7466(2) 0.6385(2) 0.77686(14) 0.0192(5) Uani 1 1 d . . .
C3 C 0.7365(2) 0.6111(2) 0.85730(15) 0.0214(5) Uani 1 1 d . A .
H3 H 0.7181 0.5333 0.8653 0.026 Uiso 1 1 calc R . .
C4 C 0.7528(2) 0.6954(2) 0.92601(15) 0.0230(5) Uani 1 1 d . . .
C5 C 0.7767(2) 0.8109(2) 0.91215(15) 0.0228(5) Uani 1 1 d . A .
H5 H 0.7866 0.8688 0.9574 0.027 Uiso 1 1 calc R . .
C6 C 0.7866(2) 0.8437(2) 0.83272(14) 0.0191(5) Uani 1 1 d . . .
C7 C 0.7566(3) 0.6603(3) 1.01308(16) 0.0355(7) Uani 1 1 d . A .
H7 H 0.7543 0.7316 1.0527 0.043 Uiso 1 1 calc R . .
C8 C 0.6500(3) 0.5770(3) 1.02880(19) 0.0402(7) Uani 1 1 d . . .
H8A H 0.5729 0.6131 1.0204 0.060 Uiso 1 1 calc R A .
H8B H 0.6568 0.5589 1.0847 0.060 Uiso 1 1 calc R . .
H8C H 0.6524 0.5058 0.9913 0.060 Uiso 1 1 calc R . .
C9 C 0.8813(3) 0.6020(4) 1.0269(2) 0.0557(10) Uani 1 1 d . . .
H9A H 0.8864 0.5339 0.9869 0.084 Uiso 1 1 calc R A .
H9B H 0.8854 0.5791 1.0816 0.084 Uiso 1 1 calc R . .
H9C H 0.9492 0.6572 1.0208 0.084 Uiso 1 1 calc R . .
C10 C 0.8223(2) 0.9718(2) 0.82378(14) 0.0190(5) Uani 1 1 d . A .
H10 H 0.7931 0.9847 0.7682 0.023 Uiso 1 1 calc R . .
C11 C 0.7584(2) 1.0604(2) 0.88464(14) 0.0214(5) Uani 1 1 d . . .
C12 C 0.6353(2) 1.0408(2) 0.90516(15) 0.0245(5) Uani 1 1 d . A .
H12 H 0.5919 0.9715 0.8829 0.029 Uiso 1 1 calc R . .
C13 C 0.5759(2) 1.1225(2) 0.95803(16) 0.0289(6) Uani 1 1 d . . .
H13 H 0.4935 1.1078 0.9705 0.035 Uiso 1 1 calc R A .
C14 C 0.6394(3) 1.2264(3) 0.99241(18) 0.0338(6) Uani 1 1 d . A .
H14 H 0.6004 1.2809 1.0286 0.041 Uiso 1 1 calc R . .
C15 C 0.7608(3) 1.2475(3) 0.97216(19) 0.0359(7) Uani 1 1 d . . .
H15 H 0.8038 1.3169 0.9946 0.043 Uiso 1 1 calc R A .
C16 C 0.8199(2) 1.1660(2) 0.91845(17) 0.0285(6) Uani 1 1 d . A .
H16 H 0.9016 1.1821 0.9049 0.034 Uiso 1 1 calc R . .
C17 C 0.9634(2) 0.9931(2) 0.82661(15) 0.0202(5) Uani 1 1 d . . .
C18 C 1.0396(2) 0.9537(2) 0.88742(15) 0.0222(5) Uani 1 1 d . A .
H18 H 1.0043 0.9123 0.9273 0.027 Uiso 1 1 calc R . .
C19 C 1.1673(2) 0.9758(2) 0.88888(15) 0.0250(5) Uani 1 1 d . . .
H19 H 1.2169 0.9494 0.9298 0.030 Uiso 1 1 calc R A .
C20 C 1.2212(2) 1.0365(2) 0.83002(16) 0.0270(6) Uani 1 1 d . A .
H20 H 1.3070 1.0506 0.8309 0.032 Uiso 1 1 calc R . .
C21 C 1.1470(2) 1.0765(2) 0.76949(17) 0.0293(6) Uani 1 1 d . . .
H21 H 1.1829 1.1173 0.7296 0.035 Uiso 1 1 calc R A .
C22 C 1.0190(2) 1.0554(2) 0.76851(16) 0.0259(5) Uani 1 1 d . A .
H22 H 0.9697 1.0835 0.7282 0.031 Uiso 1 1 calc R . .
C23 C 0.7329(2) 0.5368(2) 0.70672(14) 0.0203(5) Uani 1 1 d . A .
H23 H 0.7098 0.5702 0.6562 0.024 Uiso 1 1 calc R . .
C24 C 0.6262(2) 0.4488(2) 0.72274(14) 0.0206(5) Uani 1 1 d . . .
C25 C 0.5041(2) 0.4828(2) 0.71723(15) 0.0248(5) Uani 1 1 d . A .
H25 H 0.4886 0.5567 0.7025 0.030 Uiso 1 1 calc R . .
C26 C 0.4056(2) 0.4081(3) 0.73328(16) 0.0296(6) Uani 1 1 d . . .
H26 H 0.3247 0.4317 0.7285 0.036 Uiso 1 1 calc R A .
C27 C 0.4268(3) 0.2989(3) 0.75626(17) 0.0328(6) Uani 1 1 d . A .
H27 H 0.3607 0.2490 0.7678 0.039 Uiso 1 1 calc R . .
C28 C 0.5467(3) 0.2644(3) 0.76199(18) 0.0348(6) Uani 1 1 d . . .
H28 H 0.5616 0.1908 0.7774 0.042 Uiso 1 1 calc R A .
C29 C 0.6458(2) 0.3383(2) 0.74499(17) 0.0289(6) Uani 1 1 d . A .
H29 H 0.7263 0.3132 0.7486 0.035 Uiso 1 1 calc R . .
C30 C 0.8520(2) 0.4721(2) 0.68994(15) 0.0236(5) Uani 1 1 d . . .
C31 C 0.9382(3) 0.4545(3) 0.75187(17) 0.0333(6) Uani 1 1 d . A .
H31 H 0.9298 0.4907 0.8055 0.040 Uiso 1 1 calc R . .
C32 C 1.0374(3) 0.3827(3) 0.7341(2) 0.0404(7) Uani 1 1 d . . .
H32 H 1.0932 0.3700 0.7764 0.048 Uiso 1 1 calc R A .
C33 C 1.0535(3) 0.3309(3) 0.6553(2) 0.0416(7) Uani 1 1 d . A .
H33 H 1.1205 0.2842 0.6439 0.050 Uiso 1 1 calc R . .
C34 C 0.9703(3) 0.3483(3) 0.59317(19) 0.0392(7) Uani 1 1 d . . .
H34 H 0.9809 0.3135 0.5395 0.047 Uiso 1 1 calc R A .
C35 C 0.8700(3) 0.4180(3) 0.61033(17) 0.0323(6) Uani 1 1 d . A .
H35 H 0.8138 0.4287 0.5678 0.039 Uiso 1 1 calc R . .
C36 C 0.7082(2) 0.9452(2) 0.54924(15) 0.0254(5) Uani 1 1 d . . .
H36 H 0.6281 0.9693 0.5289 0.030 Uiso 1 1 calc R A .
C37 C 0.7777(3) 0.9106(3) 0.47004(16) 0.0323(6) Uani 1 1 d . A .
H37A H 0.7932 0.9788 0.4424 0.048 Uiso 1 1 calc R . .
H37B H 0.7282 0.8524 0.4342 0.048 Uiso 1 1 calc R . .
H37C H 0.8553 0.8789 0.4839 0.048 Uiso 1 1 calc R . .
C38 C 0.7691(3) 1.0591(3) 0.59517(17) 0.0328(6) Uani 1 1 d . A .
H38A H 0.8552 1.0481 0.6071 0.049 Uiso 1 1 calc R . .
H38B H 0.7279 1.0792 0.6460 0.049 Uiso 1 1 calc R . .
H38C H 0.7623 1.1215 0.5612 0.049 Uiso 1 1 calc R . .
C39 C 0.5893(2) 0.6952(2) 0.55154(15) 0.0255(5) Uani 1 1 d . . .
H39 H 0.5573 0.6422 0.5897 0.031 Uiso 1 1 calc R A .
C40 C 0.4769(3) 0.7219(3) 0.49766(17) 0.0346(7) Uani 1 1 d . A .
H40A H 0.5021 0.7788 0.4620 0.052 Uiso 1 1 calc R . .
H40B H 0.4131 0.7529 0.5326 0.052 Uiso 1 1 calc R . .
H40C H 0.4454 0.6509 0.4648 0.052 Uiso 1 1 calc R . .
C41 C 0.6811(3) 0.6246(3) 0.49693(16) 0.0322(6) Uani 1 1 d . A .
H41A H 0.6459 0.5465 0.4802 0.048 Uiso 1 1 calc R . .
H41B H 0.7577 0.6205 0.5278 0.048 Uiso 1 1 calc R . .
H41C H 0.6968 0.6630 0.4488 0.048 Uiso 1 1 calc R . .
C42 C 0.5437(2) 0.8976(2) 0.69103(14) 0.0214(5) Uani 1 1 d . . .
H42 H 0.5908 0.9495 0.7345 0.026 Uiso 1 1 calc R A .
C43 C 0.4680(2) 0.8093(2) 0.73496(16) 0.0277(6) Uani 1 1 d . A .
H43A H 0.4149 0.8507 0.7734 0.042 Uiso 1 1 calc R . .
H43B H 0.5232 0.7642 0.7642 0.042 Uiso 1 1 calc R . .
H43C H 0.4182 0.7574 0.6949 0.042 Uiso 1 1 calc R . .
C44 C 0.4543(2) 0.9759(2) 0.64995(16) 0.0290(6) Uani 1 1 d . A .
H44A H 0.4091 0.9299 0.6045 0.043 Uiso 1 1 calc R . .
H44B H 0.5010 1.0394 0.6299 0.043 Uiso 1 1 calc R . .
H44C H 0.3970 1.0074 0.6898 0.043 Uiso 1 1 calc R . .
C45 C 1.0598(2) 0.7331(3) 0.71763(18) 0.0325(6) Uani 1 1 d . A 1
H45A H 1.1067 0.7965 0.7518 0.039 Uiso 1 1 calc R A 1
H45B H 1.0117 0.6881 0.7534 0.039 Uiso 1 1 calc R A 1
C46 C 1.1480(3) 0.6538(3) 0.6679(2) 0.0444(8) Uani 1 1 d . A 1
H46A H 1.1014 0.5871 0.6388 0.067 Uiso 1 1 calc R A 1
H46B H 1.2087 0.6274 0.7047 0.067 Uiso 1 1 calc R A 1
H46C H 1.1891 0.6972 0.6289 0.067 Uiso 1 1 calc R A 1


_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 N1 1.874(2) . ?
Ge1 C45 1.990(3) . ?
Ge1A N1 1.944(5) . ?
Si1 N1 1.784(2) . ?
Si1 C39 1.901(3) . ?
Si1 C36 1.903(3) . ?
Si1 C42 1.904(3) . ?
N1 C1 1.443(3) . ?
C1 C2 1.412(4) . ?
C1 C6 1.417(3) . ?
C2 C3 1.391(3) . ?
C2 C23 1.529(3) . ?
C3 C4 1.388(3) . ?
C4 C5 1.384(4) . ?
C4 C7 1.521(4) . ?
C5 C6 1.397(3) . ?
C6 C10 1.525(3) . ?
C7 C8 1.507(4) . ?
C7 C9 1.552(5) . ?
C10 C17 1.527(3) . ?
C10 C11 1.535(3) . ?
C11 C12 1.394(4) . ?
C11 C16 1.395(4) . ?
C12 C13 1.387(4) . ?
C13 C14 1.392(4) . ?
C14 C15 1.377(4) . ?
C15 C16 1.392(4) . ?
C17 C22 1.387(4) . ?
C17 C18 1.399(3) . ?
C18 C19 1.387(4) . ?
C19 C20 1.379(4) . ?
C20 C21 1.386(4) . ?
C21 C22 1.390(4) . ?
C23 C30 1.530(3) . ?
C23 C24 1.542(3) . ?
C24 C29 1.384(4) . ?
C24 C25 1.394(4) . ?
C25 C26 1.383(4) . ?
C26 C27 1.377(4) . ?
C27 C28 1.373(4) . ?
C28 C29 1.387(4) . ?
C30 C31 1.391(4) . ?
C30 C35 1.392(4) . ?
C31 C32 1.396(4) . ?
C32 C33 1.367(4) . ?
C33 C34 1.372(5) . ?
C34 C35 1.390(4) . ?
C36 C38 1.532(4) . ?
C36 C37 1.533(4) . ?
C39 C40 1.539(3) . ?
C39 C41 1.543(4) . ?
C42 C43 1.529(4) . ?
C42 C44 1.541(3) . ?
C45 C46 1.530(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 Ge1 C45 105.41(11) . . ?
N1 Si1 C39 110.83(11) . . ?
N1 Si1 C36 113.99(11) . . ?
C39 Si1 C36 108.50(12) . . ?
N1 Si1 C42 107.61(10) . . ?
C39 Si1 C42 109.75(11) . . ?
C36 Si1 C42 106.01(11) . . ?
C1 N1 Si1 122.52(15) . . ?
C1 N1 Ge1 120.83(15) . . ?
Si1 N1 Ge1 116.59(11) . . ?
C1 N1 Ge1A 87.7(2) . . ?
Si1 N1 Ge1A 149.6(2) . . ?
Ge1 N1 Ge1A 33.18(16) . . ?
C2 C1 C6 118.3(2) . . ?
C2 C1 N1 122.1(2) . . ?
C6 C1 N1 119.6(2) . . ?
C3 C2 C1 119.7(2) . . ?
C3 C2 C23 117.4(2) . . ?
C1 C2 C23 122.8(2) . . ?
C4 C3 C2 122.5(2) . . ?
C5 C4 C3 117.5(2) . . ?
C5 C4 C7 121.2(2) . . ?
C3 C4 C7 121.0(2) . . ?
C4 C5 C6 122.4(2) . . ?
C5 C6 C1 119.5(2) . . ?
C5 C6 C10 118.7(2) . . ?
C1 C6 C10 121.7(2) . . ?
C8 C7 C4 113.3(2) . . ?
C8 C7 C9 109.5(3) . . ?
C4 C7 C9 108.2(3) . . ?
C6 C10 C17 110.84(19) . . ?
C6 C10 C11 113.6(2) . . ?
C17 C10 C11 112.58(19) . . ?
C12 C11 C16 117.6(2) . . ?
C12 C11 C10 121.2(2) . . ?
C16 C11 C10 121.1(2) . . ?
C13 C12 C11 121.4(2) . . ?
C12 C13 C14 120.2(3) . . ?
C15 C14 C13 119.1(3) . . ?
C14 C15 C16 120.7(3) . . ?
C15 C16 C11 121.0(3) . . ?
C22 C17 C18 118.2(2) . . ?
C22 C17 C10 119.8(2) . . ?
C18 C17 C10 122.1(2) . . ?
C19 C18 C17 120.7(2) . . ?
C20 C19 C18 120.4(2) . . ?
C19 C20 C21 119.7(2) . . ?
C20 C21 C22 119.9(3) . . ?
C17 C22 C21 121.2(2) . . ?
C2 C23 C30 114.15(19) . . ?
C2 C23 C24 110.70(19) . . ?
C30 C23 C24 110.1(2) . . ?
C29 C24 C25 118.0(2) . . ?
C29 C24 C23 123.1(2) . . ?
C25 C24 C23 118.9(2) . . ?
C26 C25 C24 121.0(2) . . ?
C27 C26 C25 120.4(3) . . ?
C28 C27 C26 119.2(3) . . ?
C27 C28 C29 120.7(3) . . ?
C24 C29 C28 120.7(3) . . ?
C31 C30 C35 117.7(2) . . ?
C31 C30 C23 123.3(2) . . ?
C35 C30 C23 118.7(2) . . ?
C30 C31 C32 120.5(3) . . ?
C33 C32 C31 120.7(3) . . ?
C32 C33 C34 119.6(3) . . ?
C33 C34 C35 120.1(3) . . ?
C34 C35 C30 121.3(3) . . ?
C38 C36 C37 109.3(2) . . ?
C38 C36 Si1 114.41(17) . . ?
C37 C36 Si1 120.03(19) . . ?
C40 C39 C41 109.4(2) . . ?
C40 C39 Si1 114.00(19) . . ?
C41 C39 Si1 114.32(18) . . ?
C43 C42 C44 109.1(2) . . ?
C43 C42 Si1 114.44(17) . . ?
C44 C42 Si1 113.97(17) . . ?
C46 C45 Ge1 107.7(2) . . ?

_diffrn_measured_fraction_theta_max 0.920
_diffrn_reflns_theta_full        25.20
_diffrn_measured_fraction_theta_full 0.920
_refine_diff_density_max         0.583
_refine_diff_density_min         -0.776
_refine_diff_density_rms         0.058
####################################################################### 
# 
# 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_compound6
_database_code_depnum_ccdc_archive 'CCDC 1422728'
_audit_update_record             
;
2015-09-07 deposited with the CCDC.
2015-09-22 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C52 H61 Ge N Si'
_chemical_formula_weight         800.70

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'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   P2(1)/n

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

_cell_length_a                   11.5430(4)
_cell_length_b                   23.7164(9)
_cell_length_c                   16.3022(6)
_cell_angle_alpha                90.00
_cell_angle_beta                 97.9790(10)
_cell_angle_gamma                90.00
_cell_volume                     4419.7(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    123(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.203
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1704
_exptl_absorpt_coefficient_mu    0.755
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.801
_exptl_absorpt_correction_T_max  0.860
_exptl_absorpt_process_details   'SCALE3 ABSPACK'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      123(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Oxford Gemini Ultra'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            38192
_diffrn_reflns_av_R_equivalents  0.0570
_diffrn_reflns_av_sigmaI/netI    0.0809
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         3.47
_diffrn_reflns_theta_max         30.00
_reflns_number_total             12845
_reflns_number_gt                8300
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       CrysalisPro
_computing_cell_refinement       CrysalisPro
_computing_data_reduction        CrysalisPro
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    X-Seed
_computing_publication_material  CifTAB

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0407P)²+0.8215P] 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         12845
_refine_ls_number_parameters     504
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0919
_refine_ls_R_factor_gt           0.0477
_refine_ls_wR_factor_ref         0.1088
_refine_ls_wR_factor_gt          0.0942
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_restrained_S_all      1.018
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ge1 Ge 0.44815(2) 0.209613(9) 0.156416(14) 0.02195(7) Uani 1 1 d . . .
Si1 Si 0.51463(5) 0.33714(2) 0.18888(3) 0.01507(12) Uani 1 1 d . . .
N1 N 0.44691(13) 0.28405(7) 0.11940(10) 0.0141(3) Uani 1 1 d . . .
C42 C 0.40646(17) 0.36216(9) 0.25870(13) 0.0192(4) Uani 1 1 d . . .
H42 H 0.3319 0.3703 0.2216 0.023 Uiso 1 1 calc R . .
C43 C 0.4381(2) 0.41647(10) 0.30902(14) 0.0289(5) Uani 1 1 d . . .
H43A H 0.3770 0.4246 0.3435 0.043 Uiso 1 1 calc R . .
H43B H 0.4443 0.4480 0.2710 0.043 Uiso 1 1 calc R . .
H43C H 0.5131 0.4113 0.3445 0.043 Uiso 1 1 calc R . .
C44 C 0.37882(19) 0.31423(10) 0.31649(13) 0.0249(5) Uani 1 1 d . . .
H44A H 0.4487 0.3056 0.3559 0.037 Uiso 1 1 calc R . .
H44B H 0.3549 0.2806 0.2836 0.037 Uiso 1 1 calc R . .
H44C H 0.3153 0.3259 0.3469 0.037 Uiso 1 1 calc R . .
C36 C 0.56252(16) 0.39765(8) 0.12575(12) 0.0182(4) Uani 1 1 d . . .
H36 H 0.6011 0.3804 0.0806 0.022 Uiso 1 1 calc R . .
C38 C 0.65387(18) 0.43684(9) 0.17446(14) 0.0266(5) Uani 1 1 d . . .
H38A H 0.6786 0.4654 0.1370 0.040 Uiso 1 1 calc R . .
H38B H 0.7218 0.4146 0.1984 0.040 Uiso 1 1 calc R . .
H38C H 0.6193 0.4555 0.2189 0.040 Uiso 1 1 calc R . .
C37 C 0.46090(18) 0.43387(9) 0.08297(14) 0.0250(5) Uani 1 1 d . . .
H37A H 0.4172 0.4499 0.1249 0.038 Uiso 1 1 calc R . .
H37B H 0.4086 0.4103 0.0447 0.038 Uiso 1 1 calc R . .
H37C H 0.4922 0.4645 0.0521 0.038 Uiso 1 1 calc R . .
C39 C 0.64332(17) 0.30202(9) 0.25446(13) 0.0223(5) Uani 1 1 d . . .
H39 H 0.6130 0.2653 0.2729 0.027 Uiso 1 1 calc R . .
C40 C 0.69518(18) 0.33296(10) 0.33407(13) 0.0286(5) Uani 1 1 d . . .
H40A H 0.7561 0.3095 0.3652 0.043 Uiso 1 1 calc R . .
H40B H 0.6332 0.3402 0.3682 0.043 Uiso 1 1 calc R . .
H40C H 0.7293 0.3688 0.3196 0.043 Uiso 1 1 calc R . .
C41 C 0.74244(19) 0.28684(11) 0.20467(15) 0.0353(6) Uani 1 1 d . . .
H41A H 0.7745 0.3214 0.1837 0.053 Uiso 1 1 calc R . .
H41B H 0.7118 0.2626 0.1580 0.053 Uiso 1 1 calc R . .
H41C H 0.8043 0.2669 0.2405 0.053 Uiso 1 1 calc R . .
C1 C 0.38682(16) 0.29930(8) 0.03851(12) 0.0135(4) Uani 1 1 d . . .
C6 C 0.44726(16) 0.30354(8) -0.03068(12) 0.0150(4) Uani 1 1 d . . .
C5 C 0.38766(16) 0.32243(8) -0.10632(12) 0.0166(4) Uani 1 1 d . . .
H5 H 0.4296 0.3257 -0.1523 0.020 Uiso 1 1 calc R . .
C4 C 0.26961(16) 0.33656(8) -0.11691(12) 0.0163(4) Uani 1 1 d . . .
C7 C 0.20499(17) 0.36082(9) -0.19680(13) 0.0211(4) Uani 1 1 d . . .
H7 H 0.1412 0.3337 -0.2176 0.025 Uiso 1 1 calc R . .
C9 C 0.2803(2) 0.36839(11) -0.26532(13) 0.0330(6) Uani 1 1 d . . .
H9A H 0.3422 0.3959 -0.2478 0.050 Uiso 1 1 calc R . .
H9B H 0.2318 0.3820 -0.3155 0.050 Uiso 1 1 calc R . .
H9C H 0.3156 0.3322 -0.2769 0.050 Uiso 1 1 calc R . .
C8 C 0.1470(2) 0.41689(10) -0.18086(15) 0.0319(5) Uani 1 1 d . . .
H8A H 0.0965 0.4118 -0.1378 0.048 Uiso 1 1 calc R . .
H8B H 0.0999 0.4299 -0.2320 0.048 Uiso 1 1 calc R . .
H8C H 0.2074 0.4449 -0.1625 0.048 Uiso 1 1 calc R . .
C3 C 0.21054(16) 0.32872(8) -0.04938(12) 0.0165(4) Uani 1 1 d . . .
H3 H 0.1288 0.3359 -0.0561 0.020 Uiso 1 1 calc R . .
C2 C 0.26471(16) 0.31086(8) 0.02759(12) 0.0144(4) Uani 1 1 d . . .
C10 C 0.19044(16) 0.30574(8) 0.09796(12) 0.0152(4) Uani 1 1 d . . .
H10 H 0.2449 0.3110 0.1507 0.018 Uiso 1 1 calc R . .
C17 C 0.09993(16) 0.35348(9) 0.09441(12) 0.0174(4) Uani 1 1 d . . .
C18 C -0.01994(17) 0.34433(9) 0.08288(14) 0.0236(5) Uani 1 1 d . . .
H18 H -0.0491 0.3068 0.0798 0.028 Uiso 1 1 calc R . .
C19 C -0.09785(19) 0.38929(10) 0.07582(14) 0.0284(5) Uani 1 1 d . . .
H19 H -0.1796 0.3821 0.0669 0.034 Uiso 1 1 calc R . .
C20 C -0.0584(2) 0.44385(10) 0.08154(15) 0.0319(6) Uani 1 1 d . . .
H20 H -0.1121 0.4744 0.0771 0.038 Uiso 1 1 calc R . .
C21 C 0.0606(2) 0.45365(10) 0.09385(16) 0.0349(6) Uani 1 1 d . . .
H21 H 0.0893 0.4912 0.0981 0.042 Uiso 1 1 calc R . .
C22 C 0.13822(18) 0.40907(9) 0.10004(15) 0.0279(5) Uani 1 1 d . . .
H22 H 0.2198 0.4166 0.1084 0.033 Uiso 1 1 calc R . .
C11 C 0.13489(16) 0.24777(9) 0.10330(12) 0.0168(4) Uani 1 1 d . . .
C12 C 0.13807(18) 0.22196(9) 0.17987(13) 0.0219(5) Uani 1 1 d . . .
H12 H 0.1765 0.2403 0.2279 0.026 Uiso 1 1 calc R . .
C13 C 0.0861(2) 0.16965(10) 0.18772(14) 0.0292(5) Uani 1 1 d . . .
H13 H 0.0901 0.1523 0.2406 0.035 Uiso 1 1 calc R . .
C14 C 0.0288(2) 0.14305(10) 0.11868(14) 0.0305(5) Uani 1 1 d . . .
H14 H -0.0071 0.1074 0.1238 0.037 Uiso 1 1 calc R . .
C15 C 0.02386(19) 0.16850(9) 0.04163(14) 0.0265(5) Uani 1 1 d . . .
H15 H -0.0162 0.1504 -0.0060 0.032 Uiso 1 1 calc R . .
C16 C 0.07700(17) 0.22012(9) 0.03386(13) 0.0214(5) Uani 1 1 d . . .
H16 H 0.0741 0.2369 -0.0193 0.026 Uiso 1 1 calc R . .
C23 C 0.57624(16) 0.28670(9) -0.02609(12) 0.0173(4) Uani 1 1 d . . .
H23 H 0.6095 0.2877 0.0339 0.021 Uiso 1 1 calc R . .
C24 C 0.58889(17) 0.22580(9) -0.05473(13) 0.0186(4) Uani 1 1 d . . .
C25 C 0.54036(17) 0.20788(9) -0.13340(14) 0.0229(5) Uani 1 1 d . . .
H25 H 0.4949 0.2334 -0.1695 0.027 Uiso 1 1 calc R . .
C26 C 0.55741(19) 0.15315(10) -0.16001(16) 0.0317(6) Uani 1 1 d . . .
H26 H 0.5241 0.1417 -0.2140 0.038 Uiso 1 1 calc R . .
C27 C 0.6227(2) 0.11534(10) -0.10802(17) 0.0355(6) Uani 1 1 d . . .
H27 H 0.6341 0.0779 -0.1261 0.043 Uiso 1 1 calc R . .
C28 C 0.6709(2) 0.13216(10) -0.03017(17) 0.0364(6) Uani 1 1 d . . .
H28 H 0.7156 0.1063 0.0058 0.044 Uiso 1 1 calc R . .
C29 C 0.6545(2) 0.18708(10) -0.00360(14) 0.0295(5) Uani 1 1 d . . .
H29 H 0.6887 0.1983 0.0503 0.035 Uiso 1 1 calc R . .
C30 C 0.65173(16) 0.32670(9) -0.07052(12) 0.0177(4) Uani 1 1 d . . .
C31 C 0.75528(17) 0.30702(9) -0.09551(13) 0.0216(5) Uani 1 1 d . . .
H31 H 0.7768 0.2687 -0.0860 0.026 Uiso 1 1 calc R . .
C32 C 0.82748(18) 0.34205(10) -0.13378(14) 0.0276(5) Uani 1 1 d . . .
H32 H 0.8969 0.3274 -0.1508 0.033 Uiso 1 1 calc R . .
C33 C 0.79930(19) 0.39805(10) -0.14734(14) 0.0292(5) Uani 1 1 d . . .
H33 H 0.8482 0.4219 -0.1743 0.035 Uiso 1 1 calc R . .
C34 C 0.69862(19) 0.41904(10) -0.12111(14) 0.0271(5) Uani 1 1 d . . .
H34 H 0.6794 0.4578 -0.1290 0.033 Uiso 1 1 calc R . .
C35 C 0.62568(17) 0.38388(9) -0.08341(13) 0.0214(4) Uani 1 1 d . . .
H35 H 0.5568 0.3989 -0.0660 0.026 Uiso 1 1 calc R . .
C45 C 0.37173(18) 0.16422(8) 0.06122(13) 0.0211(4) Uani 1 1 d . . .
H45A H 0.2875 0.1736 0.0495 0.025 Uiso 1 1 calc R . .
H45B H 0.4084 0.1723 0.0111 0.025 Uiso 1 1 calc R . .
C46 C 0.3875(3) 0.10184(10) 0.08505(17) 0.0525(8) Uani 1 1 d . . .
H46A H 0.4719 0.0925 0.0910 0.063 Uiso 1 1 calc R . .
H46B H 0.3611 0.0961 0.1397 0.063 Uiso 1 1 calc R . .
C47 C 0.3221(2) 0.06173(9) 0.02386(14) 0.0303(5) Uani 1 1 d . . .
C48 C 0.2183(3) 0.03743(12) 0.0370(2) 0.0604(9) Uani 1 1 d . . .
H48 H 0.1878 0.0451 0.0871 0.073 Uiso 1 1 calc R . .
C49 C 0.1575(3) 0.00225(13) -0.0209(3) 0.0706(12) Uani 1 1 d . . .
H49 H 0.0867 -0.0147 -0.0098 0.085 Uiso 1 1 calc R . .
C50 C 0.1979(3) -0.00820(11) -0.0930(2) 0.0559(9) Uani 1 1 d . . .
H50 H 0.1538 -0.0312 -0.1338 0.067 Uiso 1 1 calc R . .
C51 C 0.3007(3) 0.01390(12) -0.10743(18) 0.0535(8) Uani 1 1 d . . .
H51 H 0.3303 0.0056 -0.1576 0.064 Uiso 1 1 calc R . .
C52 C 0.3633(2) 0.04888(11) -0.04890(17) 0.0425(7) Uani 1 1 d . . .
H52 H 0.4359 0.0642 -0.0594 0.051 Uiso 1 1 calc R . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ge1 N1 1.8651(16) . ?
Ge1 C45 1.991(2) . ?
Si1 N1 1.7982(16) . ?
Si1 C36 1.893(2) . ?
Si1 C42 1.898(2) . ?
Si1 C39 1.898(2) . ?
N1 C1 1.448(2) . ?
C42 C44 1.538(3) . ?
C42 C43 1.543(3) . ?
C36 C37 1.540(3) . ?
C36 C38 1.541(3) . ?
C39 C41 1.535(3) . ?
C39 C40 1.538(3) . ?
C1 C6 1.410(3) . ?
C1 C2 1.423(3) . ?
C6 C5 1.400(3) . ?
C6 C23 1.533(3) . ?
C5 C4 1.391(3) . ?
C4 C3 1.386(3) . ?
C4 C7 1.521(3) . ?
C7 C9 1.518(3) . ?
C7 C8 1.527(3) . ?
C3 C2 1.388(3) . ?
C2 C10 1.529(3) . ?
C10 C11 1.524(3) . ?
C10 C17 1.536(3) . ?
C17 C18 1.387(3) . ?
C17 C22 1.389(3) . ?
C18 C19 1.389(3) . ?
C19 C20 1.371(3) . ?
C20 C21 1.380(3) . ?
C21 C22 1.380(3) . ?
C11 C12 1.386(3) . ?
C11 C16 1.396(3) . ?
C12 C13 1.392(3) . ?
C13 C14 1.377(3) . ?
C14 C15 1.388(3) . ?
C15 C16 1.383(3) . ?
C23 C24 1.531(3) . ?
C23 C30 1.536(3) . ?
C24 C29 1.392(3) . ?
C24 C25 1.393(3) . ?
C25 C26 1.391(3) . ?
C26 C27 1.383(3) . ?
C27 C28 1.372(4) . ?
C28 C29 1.394(3) . ?
C30 C31 1.396(3) . ?
C30 C35 1.399(3) . ?
C31 C32 1.385(3) . ?
C32 C33 1.378(3) . ?
C33 C34 1.385(3) . ?
C34 C35 1.388(3) . ?
C45 C46 1.534(3) . ?
C46 C47 1.504(3) . ?
C47 C52 1.372(3) . ?
C47 C48 1.373(4) . ?
C48 C49 1.376(4) . ?
C49 C50 1.347(5) . ?
C50 C51 1.348(4) . ?
C51 C52 1.389(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 Ge1 C45 106.08(8) . . ?
N1 Si1 C36 108.83(8) . . ?
N1 Si1 C42 109.39(8) . . ?
C36 Si1 C42 110.80(9) . . ?
N1 Si1 C39 106.58(9) . . ?
C36 Si1 C39 111.98(9) . . ?
C42 Si1 C39 109.15(9) . . ?
C1 N1 Si1 120.67(12) . . ?
C1 N1 Ge1 120.81(12) . . ?
Si1 N1 Ge1 118.41(8) . . ?
C44 C42 C43 110.19(17) . . ?
C44 C42 Si1 110.24(14) . . ?
C43 C42 Si1 116.93(14) . . ?
C37 C36 C38 108.70(17) . . ?
C37 C36 Si1 114.05(13) . . ?
C38 C36 Si1 114.07(14) . . ?
C41 C39 C40 109.07(17) . . ?
C41 C39 Si1 112.81(15) . . ?
C40 C39 Si1 116.64(15) . . ?
C6 C1 C2 118.54(17) . . ?
C6 C1 N1 121.25(16) . . ?
C2 C1 N1 120.20(16) . . ?
C5 C6 C1 119.37(17) . . ?
C5 C6 C23 118.79(17) . . ?
C1 C6 C23 121.83(17) . . ?
C4 C5 C6 122.67(18) . . ?
C3 C4 C5 116.80(18) . . ?
C3 C4 C7 119.61(17) . . ?
C5 C4 C7 123.57(18) . . ?
C9 C7 C4 114.32(17) . . ?
C9 C7 C8 109.36(18) . . ?
C4 C7 C8 110.98(17) . . ?
C4 C3 C2 123.33(18) . . ?
C3 C2 C1 119.08(17) . . ?
C3 C2 C10 118.24(16) . . ?
C1 C2 C10 122.66(16) . . ?
C11 C10 C2 113.48(16) . . ?
C11 C10 C17 112.19(15) . . ?
C2 C10 C17 111.24(16) . . ?
C18 C17 C22 117.35(19) . . ?
C18 C17 C10 123.37(18) . . ?
C22 C17 C10 119.24(17) . . ?
C17 C18 C19 120.9(2) . . ?
C20 C19 C18 120.9(2) . . ?
C19 C20 C21 118.9(2) . . ?
C22 C21 C20 120.3(2) . . ?
C21 C22 C17 121.6(2) . . ?
C12 C11 C16 118.20(19) . . ?
C12 C11 C10 119.40(18) . . ?
C16 C11 C10 122.36(18) . . ?
C11 C12 C13 121.2(2) . . ?
C14 C13 C12 119.8(2) . . ?
C13 C14 C15 119.7(2) . . ?
C16 C15 C14 120.3(2) . . ?
C15 C16 C11 120.7(2) . . ?
C24 C23 C6 111.34(16) . . ?
C24 C23 C30 110.76(16) . . ?
C6 C23 C30 115.26(16) . . ?
C29 C24 C25 117.8(2) . . ?
C29 C24 C23 120.46(19) . . ?
C25 C24 C23 121.70(18) . . ?
C26 C25 C24 121.0(2) . . ?
C27 C26 C25 120.2(2) . . ?
C28 C27 C26 119.6(2) . . ?
C27 C28 C29 120.3(2) . . ?
C24 C29 C28 121.1(2) . . ?
C31 C30 C35 117.09(19) . . ?
C31 C30 C23 119.74(18) . . ?
C35 C30 C23 123.06(17) . . ?
C32 C31 C30 121.6(2) . . ?
C33 C32 C31 120.5(2) . . ?
C32 C33 C34 119.1(2) . . ?
C33 C34 C35 120.5(2) . . ?
C34 C35 C30 121.22(19) . . ?
C46 C45 Ge1 107.45(15) . . ?
C47 C46 C45 114.3(2) . . ?
C52 C47 C48 117.1(2) . . ?
C52 C47 C46 120.8(2) . . ?
C48 C47 C46 122.1(3) . . ?
C47 C48 C49 121.4(3) . . ?
C50 C49 C48 120.3(3) . . ?
C49 C50 C51 120.0(3) . . ?
C50 C51 C52 119.9(3) . . ?
C47 C52 C51 121.1(3) . . ?

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        30.00
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         0.509
_refine_diff_density_min         -0.474
_refine_diff_density_rms         0.073
####################################################################### 
# 
# 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_compound8
_database_code_depnum_ccdc_archive 'CCDC 1422729'
_audit_update_record             
;
2015-09-07 deposited with the CCDC.
2015-09-22 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C49 H61 Ge N Si'
_chemical_formula_weight         764.67

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'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   P2(1)/c

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

_cell_length_a                   10.319(2)
_cell_length_b                   18.286(4)
_cell_length_c                   22.437(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 91.27(3)
_cell_angle_gamma                90.00
_cell_volume                     4232.7(15)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.05
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.200
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1632
_exptl_absorpt_coefficient_mu    0.785
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.882
_exptl_absorpt_correction_T_max  0.958
_exptl_absorpt_process_details   XDS

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71080
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_source         'Australian Synchrotron'
_diffrn_radiation_monochromator  ?
_diffrn_measurement_device_type  'ADSC Quantum 210r'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            22341
_diffrn_reflns_av_R_equivalents  0.1448
_diffrn_reflns_av_sigmaI/netI    0.1195
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         2.98
_diffrn_reflns_theta_max         26.00
_reflns_number_total             8201
_reflns_number_gt                6142
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Blu-Ice (McPhillips, 2002)'
_computing_cell_refinement       'XDS (Kabsch, 1993)'
_computing_data_reduction        'XDS (Kabsch, 1993)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    X-Seed
_computing_publication_material  CifTAB

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.1009P)²+1.3928P] 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         8201
_refine_ls_number_parameters     477
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0838
_refine_ls_R_factor_gt           0.0678
_refine_ls_wR_factor_ref         0.1968
_refine_ls_wR_factor_gt          0.1839
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_restrained_S_all      1.030
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ge1 Ge 0.50266(4) 0.276686(19) 0.604106(17) 0.03805(17) Uani 1 1 d . . .
Si1 Si 0.17815(9) 0.30147(5) 0.60266(4) 0.0346(2) Uani 1 1 d . . .
C45 C 0.5204(4) 0.37678(19) 0.56940(17) 0.0414(8) Uani 1 1 d . . .
H45 H 0.4368 0.3960 0.5523 0.050 Uiso 1 1 calc R . .
C49 C 0.6269(4) 0.3745(2) 0.52410(18) 0.0509(10) Uani 1 1 d . . .
H49A H 0.5913 0.3616 0.4841 0.061 Uiso 1 1 calc R . .
H49B H 0.6939 0.3382 0.5357 0.061 Uiso 1 1 calc R . .
C47 C 0.6815(5) 0.4725(3) 0.5888(3) 0.0784(16) Uani 1 1 d . . .
H47A H 0.6609 0.5251 0.5927 0.094 Uiso 1 1 calc R . .
H47B H 0.7674 0.4634 0.6079 0.094 Uiso 1 1 calc R . .
C46 C 0.5786(4) 0.4266(2) 0.61854(19) 0.0508(10) Uani 1 1 d . . .
H46A H 0.5107 0.4583 0.6353 0.061 Uiso 1 1 calc R . .
H46B H 0.6177 0.3969 0.6512 0.061 Uiso 1 1 calc R . .
C42 C 0.2120(4) 0.39814(19) 0.62907(18) 0.0455(9) Uani 1 1 d . . .
H42 H 0.2895 0.4145 0.6067 0.055 Uiso 1 1 calc R . .
N1 N 0.3265(3) 0.25131(14) 0.61056(12) 0.0336(6) Uani 1 1 d . . .
C5 C 0.3169(3) 0.04668(17) 0.59399(14) 0.0325(7) Uani 1 1 d . . .
H5 H 0.3114 0.0119 0.5626 0.039 Uiso 1 1 calc R . .
C4 C 0.3224(3) 0.02186(17) 0.65211(15) 0.0346(7) Uani 1 1 d . . .
C6 C 0.3193(3) 0.12127(16) 0.57965(14) 0.0312(7) Uani 1 1 d . . .
C1 C 0.3225(3) 0.17400(16) 0.62581(14) 0.0309(7) Uani 1 1 d . . .
C2 C 0.3341(3) 0.14915(17) 0.68520(14) 0.0331(7) Uani 1 1 d . . .
C3 C 0.3342(3) 0.07406(17) 0.69685(14) 0.0356(7) Uani 1 1 d . . .
H3 H 0.3426 0.0581 0.7370 0.043 Uiso 1 1 calc R . .
C12 C 0.2276(4) 0.27354(19) 0.81120(17) 0.0447(9) Uani 1 1 d . . .
H12 H 0.2945 0.3091 0.8096 0.054 Uiso 1 1 calc R . .
C11 C 0.2368(4) 0.20982(19) 0.77787(15) 0.0380(8) Uani 1 1 d . . .
C7 C 0.3216(4) -0.05960(17) 0.66672(15) 0.0395(8) Uani 1 1 d . . .
H7 H 0.3215 -0.0873 0.6283 0.047 Uiso 1 1 calc R . .
C37 C 0.2172(4) 0.3433(2) 0.48114(17) 0.0454(9) Uani 1 1 d . . .
H37A H 0.1916 0.3353 0.4393 0.068 Uiso 1 1 calc R . .
H37B H 0.3050 0.3245 0.4883 0.068 Uiso 1 1 calc R . .
H37C H 0.2153 0.3958 0.4899 0.068 Uiso 1 1 calc R . .
C10 C 0.3549(3) 0.19993(18) 0.73868(14) 0.0346(7) Uani 1 1 d . . .
H10 H 0.3755 0.2493 0.7222 0.042 Uiso 1 1 calc R . .
C36 C 0.1220(3) 0.3030(2) 0.52186(17) 0.0416(8) Uani 1 1 d . . .
H36 H 0.1223 0.2509 0.5085 0.050 Uiso 1 1 calc R . .
C24 C 0.4738(3) 0.15500(16) 0.49866(14) 0.0307(7) Uani 1 1 d . . .
C31 C 0.3178(4) 0.05959(18) 0.42363(15) 0.0390(8) Uani 1 1 d . . .
H31 H 0.4089 0.0638 0.4193 0.047 Uiso 1 1 calc R . .
C43 C 0.2521(4) 0.4027(2) 0.6946(2) 0.0538(10) Uani 1 1 d . . .
H43A H 0.2744 0.4533 0.7047 0.081 Uiso 1 1 calc R . .
H43B H 0.3276 0.3712 0.7021 0.081 Uiso 1 1 calc R . .
H43C H 0.1802 0.3864 0.7191 0.081 Uiso 1 1 calc R . .
C16 C 0.1405(4) 0.1572(2) 0.78354(16) 0.0431(8) Uani 1 1 d . . .
H16 H 0.1466 0.1127 0.7620 0.052 Uiso 1 1 calc R . .
C25 C 0.5748(3) 0.11679(19) 0.52700(15) 0.0389(8) Uani 1 1 d . . .
H25 H 0.5558 0.0833 0.5580 0.047 Uiso 1 1 calc R . .
C28 C 0.6327(4) 0.21338(19) 0.43692(19) 0.0469(10) Uani 1 1 d . . .
H28 H 0.6519 0.2463 0.4056 0.056 Uiso 1 1 calc R . .
C30 C 0.2579(3) 0.09483(16) 0.47089(14) 0.0318(7) Uani 1 1 d . . .
C39 C 0.0527(4) 0.25481(19) 0.64992(17) 0.0401(8) Uani 1 1 d . . .
H39 H 0.1005 0.2402 0.6873 0.048 Uiso 1 1 calc R . .
C15 C 0.0375(4) 0.1685(2) 0.81953(17) 0.0500(9) Uani 1 1 d . . .
H15 H -0.0268 0.1317 0.8231 0.060 Uiso 1 1 calc R . .
C18 C 0.4620(4) 0.1370(2) 0.82815(17) 0.0484(9) Uani 1 1 d . . .
H18 H 0.3784 0.1274 0.8432 0.058 Uiso 1 1 calc R . .
C29 C 0.5057(4) 0.20355(19) 0.45346(16) 0.0418(8) Uani 1 1 d . . .
H29 H 0.4389 0.2304 0.4336 0.050 Uiso 1 1 calc R . .
C17 C 0.4735(4) 0.17601(19) 0.77525(15) 0.0389(8) Uani 1 1 d . . .
C40 C -0.0025(4) 0.1840(2) 0.62450(19) 0.0465(9) Uani 1 1 d . . .
H40A H -0.0602 0.1617 0.6535 0.070 Uiso 1 1 calc R . .
H40B H 0.0686 0.1502 0.6161 0.070 Uiso 1 1 calc R . .
H40C H -0.0513 0.1944 0.5875 0.070 Uiso 1 1 calc R . .
C9 C 0.4409(4) -0.0829(2) 0.70348(18) 0.0468(9) Uani 1 1 d . . .
H9A H 0.4404 -0.0585 0.7423 0.070 Uiso 1 1 calc R . .
H9B H 0.5194 -0.0692 0.6824 0.070 Uiso 1 1 calc R . .
H9C H 0.4394 -0.1360 0.7093 0.070 Uiso 1 1 calc R . .
C14 C 0.0262(4) 0.2334(3) 0.85091(19) 0.0555(11) Uani 1 1 d . . .
H14 H -0.0468 0.2417 0.8751 0.067 Uiso 1 1 calc R . .
C23 C 0.3329(3) 0.14438(17) 0.51454(14) 0.0331(7) Uani 1 1 d . . .
H23 H 0.2916 0.1937 0.5111 0.040 Uiso 1 1 calc R . .
C8 C 0.1995(4) -0.0806(2) 0.7000(2) 0.0607(12) Uani 1 1 d . . .
H8A H 0.1994 -0.1334 0.7073 0.091 Uiso 1 1 calc R . .
H8B H 0.1227 -0.0673 0.6759 0.091 Uiso 1 1 calc R . .
H8C H 0.1981 -0.0545 0.7381 0.091 Uiso 1 1 calc R . .
C38 C -0.0171(4) 0.3305(2) 0.5103(2) 0.0532(10) Uani 1 1 d . . .
H38A H -0.0236 0.3817 0.5229 0.080 Uiso 1 1 calc R . .
H38B H -0.0776 0.3007 0.5330 0.080 Uiso 1 1 calc R . .
H38C H -0.0387 0.3268 0.4677 0.080 Uiso 1 1 calc R . .
C35 C 0.1247(3) 0.08590(18) 0.47647(15) 0.0368(8) Uani 1 1 d . . .
H35 H 0.0822 0.1089 0.5086 0.044 Uiso 1 1 calc R . .
C13 C 0.1212(4) 0.2856(2) 0.84686(18) 0.0542(11) Uani 1 1 d . . .
H13 H 0.1142 0.3301 0.8684 0.065 Uiso 1 1 calc R . .
C41 C -0.0592(4) 0.3039(2) 0.6708(2) 0.0518(10) Uani 1 1 d . . .
H41A H -0.1093 0.3214 0.6360 0.078 Uiso 1 1 calc R . .
H41B H -0.0235 0.3458 0.6929 0.078 Uiso 1 1 calc R . .
H41C H -0.1158 0.2757 0.6967 0.078 Uiso 1 1 calc R . .
C44 C 0.1055(4) 0.4548(2) 0.6143(2) 0.0613(12) Uani 1 1 d . . .
H44A H 0.0236 0.4389 0.6313 0.092 Uiso 1 1 calc R . .
H44B H 0.0950 0.4593 0.5709 0.092 Uiso 1 1 calc R . .
H44C H 0.1304 0.5023 0.6313 0.092 Uiso 1 1 calc R . .
C21 C 0.7055(5) 0.1675(3) 0.7874(2) 0.0780(16) Uani 1 1 d . . .
H21 H 0.7895 0.1786 0.7735 0.094 Uiso 1 1 calc R . .
C48 C 0.6835(4) 0.4512(2) 0.5241(2) 0.0558(11) Uani 1 1 d . . .
H48A H 0.7730 0.4512 0.5091 0.067 Uiso 1 1 calc R . .
H48B H 0.6295 0.4848 0.4994 0.067 Uiso 1 1 calc R . .
C27 C 0.7321(4) 0.1757(2) 0.46564(18) 0.0460(9) Uani 1 1 d . . .
H27 H 0.8196 0.1831 0.4547 0.055 Uiso 1 1 calc R . .
C22 C 0.5951(4) 0.1915(3) 0.75567(19) 0.0605(12) Uani 1 1 d . . .
H22 H 0.6047 0.2188 0.7201 0.073 Uiso 1 1 calc R . .
C34 C 0.0527(4) 0.04413(19) 0.43605(16) 0.0407(8) Uani 1 1 d . . .
H34 H -0.0381 0.0386 0.4407 0.049 Uiso 1 1 calc R . .
C32 C 0.2448(4) 0.01824(19) 0.38274(16) 0.0437(9) Uani 1 1 d . . .
H32 H 0.2864 -0.0047 0.3503 0.052 Uiso 1 1 calc R . .
C26 C 0.7022(4) 0.1269(2) 0.51055(17) 0.0434(8) Uani 1 1 d . . .
H26 H 0.7696 0.1002 0.5302 0.052 Uiso 1 1 calc R . .
C33 C 0.1137(4) 0.01052(19) 0.38900(16) 0.0435(9) Uani 1 1 d . . .
H33 H 0.0648 -0.0178 0.3611 0.052 Uiso 1 1 calc R . .
C19 C 0.5716(4) 0.1119(2) 0.85933(18) 0.0528(10) Uani 1 1 d . . .
H19 H 0.5622 0.0839 0.8947 0.063 Uiso 1 1 calc R . .
C20 C 0.6917(5) 0.1274(3) 0.8392(2) 0.0632(12) Uani 1 1 d . . .
H20 H 0.7663 0.1107 0.8607 0.076 Uiso 1 1 calc R . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ge1 N1 1.885(3) . ?
Ge1 C45 1.999(3) . ?
Si1 N1 1.790(3) . ?
Si1 C36 1.891(4) . ?
Si1 C42 1.894(4) . ?
Si1 C39 1.895(4) . ?
C45 C49 1.514(5) . ?
C45 C46 1.542(5) . ?
C49 C48 1.520(5) . ?
C47 C48 1.503(7) . ?
C47 C46 1.520(6) . ?
C42 C43 1.520(6) . ?
C42 C44 1.541(5) . ?
N1 C1 1.455(4) . ?
C5 C4 1.381(4) . ?
C5 C6 1.402(4) . ?
C4 C3 1.389(4) . ?
C4 C7 1.525(4) . ?
C6 C1 1.415(4) . ?
C6 C23 1.530(4) . ?
C1 C2 1.411(4) . ?
C2 C3 1.398(4) . ?
C2 C10 1.528(4) . ?
C12 C11 1.389(5) . ?
C12 C13 1.391(6) . ?
C11 C16 1.391(5) . ?
C11 C10 1.530(5) . ?
C7 C9 1.527(5) . ?
C7 C8 1.527(5) . ?
C37 C36 1.543(5) . ?
C10 C17 1.522(5) . ?
C36 C38 1.537(5) . ?
C24 C29 1.393(5) . ?
C24 C25 1.396(5) . ?
C24 C23 1.517(5) . ?
C31 C32 1.397(5) . ?
C31 C30 1.397(5) . ?
C16 C15 1.365(5) . ?
C25 C26 1.387(5) . ?
C28 C29 1.381(5) . ?
C28 C27 1.384(6) . ?
C30 C35 1.392(5) . ?
C30 C23 1.532(4) . ?
C39 C40 1.521(5) . ?
C39 C41 1.543(5) . ?
C15 C14 1.387(6) . ?
C18 C17 1.392(5) . ?
C18 C19 1.394(6) . ?
C17 C22 1.368(5) . ?
C14 C13 1.373(6) . ?
C35 C34 1.389(5) . ?
C21 C20 1.384(7) . ?
C21 C22 1.401(6) . ?
C27 C26 1.385(5) . ?
C34 C33 1.385(5) . ?
C32 C33 1.371(5) . ?
C19 C20 1.358(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
N1 Ge1 C45 110.63(14) . . ?
N1 Si1 C36 110.23(15) . . ?
N1 Si1 C42 107.21(15) . . ?
C36 Si1 C42 109.65(17) . . ?
N1 Si1 C39 107.90(15) . . ?
C36 Si1 C39 110.16(17) . . ?
C42 Si1 C39 111.63(17) . . ?
C49 C45 C46 102.7(3) . . ?
C49 C45 Ge1 108.1(2) . . ?
C46 C45 Ge1 107.5(3) . . ?
C45 C49 C48 105.0(3) . . ?
C48 C47 C46 107.8(4) . . ?
C47 C46 C45 106.1(3) . . ?
C43 C42 C44 110.4(3) . . ?
C43 C42 Si1 113.4(3) . . ?
C44 C42 Si1 115.8(3) . . ?
C1 N1 Si1 119.5(2) . . ?
C1 N1 Ge1 106.8(2) . . ?
Si1 N1 Ge1 133.66(15) . . ?
C4 C5 C6 122.4(3) . . ?
C5 C4 C3 117.2(3) . . ?
C5 C4 C7 121.6(3) . . ?
C3 C4 C7 121.1(3) . . ?
C5 C6 C1 119.7(3) . . ?
C5 C6 C23 119.4(3) . . ?
C1 C6 C23 120.6(3) . . ?
C2 C1 C6 118.2(3) . . ?
C2 C1 N1 122.2(3) . . ?
C6 C1 N1 119.4(3) . . ?
C3 C2 C1 119.5(3) . . ?
C3 C2 C10 116.8(3) . . ?
C1 C2 C10 123.6(3) . . ?
C4 C3 C2 122.7(3) . . ?
C11 C12 C13 120.5(4) . . ?
C12 C11 C16 118.3(3) . . ?
C12 C11 C10 118.3(3) . . ?
C16 C11 C10 123.4(3) . . ?
C4 C7 C9 112.3(3) . . ?
C4 C7 C8 111.0(3) . . ?
C9 C7 C8 109.2(3) . . ?
C17 C10 C2 110.2(3) . . ?
C17 C10 C11 111.4(3) . . ?
C2 C10 C11 115.0(3) . . ?
C38 C36 C37 110.4(3) . . ?
C38 C36 Si1 115.6(3) . . ?
C37 C36 Si1 112.9(3) . . ?
C29 C24 C25 117.7(3) . . ?
C29 C24 C23 119.7(3) . . ?
C25 C24 C23 122.6(3) . . ?
C32 C31 C30 120.4(3) . . ?
C15 C16 C11 121.1(4) . . ?
C26 C25 C24 121.0(3) . . ?
C29 C28 C27 120.5(3) . . ?
C35 C30 C31 118.0(3) . . ?
C35 C30 C23 119.8(3) . . ?
C31 C30 C23 122.1(3) . . ?
C40 C39 C41 109.5(3) . . ?
C40 C39 Si1 115.4(2) . . ?
C41 C39 Si1 115.7(3) . . ?
C16 C15 C14 120.4(4) . . ?
C17 C18 C19 120.9(4) . . ?
C28 C29 C24 121.3(4) . . ?
C22 C17 C18 118.4(4) . . ?
C22 C17 C10 120.0(3) . . ?
C18 C17 C10 121.6(3) . . ?
C13 C14 C15 119.6(4) . . ?
C24 C23 C6 111.6(3) . . ?
C24 C23 C30 113.5(3) . . ?
C6 C23 C30 113.0(3) . . ?
C34 C35 C30 121.4(3) . . ?
C14 C13 C12 120.1(4) . . ?
C20 C21 C22 119.7(4) . . ?
C47 C48 C49 103.0(3) . . ?
C28 C27 C26 119.0(4) . . ?
C17 C22 C21 120.9(4) . . ?
C33 C34 C35 119.7(3) . . ?
C33 C32 C31 120.5(3) . . ?
C27 C26 C25 120.5(4) . . ?
C32 C33 C34 119.9(3) . . ?
C20 C19 C18 120.1(4) . . ?
C19 C20 C21 120.1(4) . . ?

_diffrn_measured_fraction_theta_max 0.986
_diffrn_reflns_theta_full        26.00
_diffrn_measured_fraction_theta_full 0.986
_refine_diff_density_max         0.534
_refine_diff_density_min         -2.079
_refine_diff_density_rms         0.077
####################################################################### 
# 
# 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_compound9
_database_code_depnum_ccdc_archive 'CCDC 1422730'
_audit_update_record             
;
2015-09-07 deposited with the CCDC.
2015-09-22 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C50 H63 Ge N Si'
_chemical_formula_weight         778.69

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'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   P2(1)

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

_cell_length_a                   10.2741(5)
_cell_length_b                   14.6818(7)
_cell_length_c                   14.6417(7)
_cell_angle_alpha                90.00
_cell_angle_beta                 102.077(3)
_cell_angle_gamma                90.00
_cell_volume                     2159.71(18)
_cell_formula_units_Z            2
_cell_measurement_temperature    123(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.25
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.197
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             832
_exptl_absorpt_coefficient_mu    0.771
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.761
_exptl_absorpt_correction_T_max  0.828
_exptl_absorpt_process_details   'SCALE3 ABSPACK'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      123(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Oxford Gemini Ultra'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            34220
_diffrn_reflns_av_R_equivalents  0.0585
_diffrn_reflns_av_sigmaI/netI    0.0607
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         3.04
_diffrn_reflns_theta_max         26.00
_reflns_number_total             8466
_reflns_number_gt                7107
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       CrysalisPro
_computing_cell_refinement       CrysalisPro
_computing_data_reduction        CrysalisPro
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    X-Seed
_computing_publication_material  CifTAB

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0456P)²+0.8199P] 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 H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.393(9)
_refine_ls_number_reflns         8466
_refine_ls_number_parameters     487
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0588
_refine_ls_R_factor_gt           0.0426
_refine_ls_wR_factor_ref         0.0965
_refine_ls_wR_factor_gt          0.0897
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_restrained_S_all      1.016
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ge1 Ge 0.62502(3) 0.75018(2) 0.82369(2) 0.02207(9) Uani 1 1 d . . .
Si1 Si 0.30708(7) 0.75200(8) 0.85768(5) 0.01912(17) Uani 1 1 d . . .
N1 N 0.4358(2) 0.7436(2) 0.79349(15) 0.0172(5) Uani 1 1 d . . .
C1 C 0.3994(3) 0.7292(2) 0.6940(2) 0.0180(8) Uani 1 1 d . . .
C2 C 0.3847(3) 0.6400(2) 0.6593(2) 0.0165(7) Uani 1 1 d . . .
C3 C 0.3469(3) 0.6280(2) 0.5614(2) 0.0182(7) Uani 1 1 d . . .
H3 H 0.3339 0.5678 0.5374 0.022 Uiso 1 1 calc R . .
C4 C 0.3279(3) 0.6994(2) 0.4994(2) 0.0185(8) Uani 1 1 d . . .
C5 C 0.3474(3) 0.7874(2) 0.5358(2) 0.0185(8) Uani 1 1 d . . .
H5 H 0.3349 0.8377 0.4940 0.022 Uiso 1 1 calc R . .
C6 C 0.3847(3) 0.8039(2) 0.6320(2) 0.0174(7) Uani 1 1 d . . .
C7 C 0.2887(3) 0.6827(2) 0.3957(2) 0.0219(7) Uani 1 1 d . . .
H7 H 0.3019 0.6164 0.3849 0.026 Uiso 1 1 calc R . .
C8 C 0.3736(3) 0.7358(3) 0.3404(2) 0.0317(9) Uani 1 1 d . . .
H8A H 0.4679 0.7227 0.3653 0.047 Uiso 1 1 calc R . .
H8B H 0.3573 0.8011 0.3457 0.047 Uiso 1 1 calc R . .
H8C H 0.3501 0.7176 0.2746 0.047 Uiso 1 1 calc R . .
C9 C 0.1421(3) 0.7041(3) 0.3591(3) 0.0352(9) Uani 1 1 d . . .
H9A H 0.1265 0.7692 0.3672 0.053 Uiso 1 1 calc R . .
H9B H 0.0880 0.6684 0.3937 0.053 Uiso 1 1 calc R . .
H9C H 0.1175 0.6886 0.2926 0.053 Uiso 1 1 calc R . .
C10 C 0.4130(3) 0.5585(2) 0.7223(2) 0.0204(7) Uani 1 1 d . . .
H10 H 0.3970 0.5780 0.7845 0.025 Uiso 1 1 calc R . .
C11 C 0.3245(3) 0.4753(2) 0.6930(2) 0.0230(7) Uani 1 1 d . . .
C12 C 0.3767(4) 0.3874(2) 0.7083(3) 0.0338(9) Uani 1 1 d . . .
H12 H 0.4689 0.3792 0.7339 0.041 Uiso 1 1 calc R . .
C13 C 0.2948(4) 0.3121(3) 0.6863(3) 0.0391(10) Uani 1 1 d . . .
H13 H 0.3315 0.2527 0.6972 0.047 Uiso 1 1 calc R . .
C14 C 0.1624(4) 0.3221(3) 0.6494(3) 0.0395(10) Uani 1 1 d . . .
H14 H 0.1071 0.2701 0.6338 0.047 Uiso 1 1 calc R . .
C15 C 0.1093(4) 0.4091(2) 0.6348(3) 0.0300(8) Uani 1 1 d . . .
H15 H 0.0168 0.4165 0.6101 0.036 Uiso 1 1 calc R . .
C16 C 0.1888(3) 0.4845(2) 0.6556(2) 0.0244(8) Uani 1 1 d . . .
H16 H 0.1510 0.5435 0.6444 0.029 Uiso 1 1 calc R . .
C17 C 0.5597(3) 0.5332(2) 0.7376(2) 0.0201(7) Uani 1 1 d . . .
C18 C 0.6349(4) 0.5180(3) 0.8263(3) 0.0318(9) Uani 1 1 d . . .
H18 H 0.5953 0.5254 0.8789 0.038 Uiso 1 1 calc R . .
C19 C 0.7667(4) 0.4922(3) 0.8395(3) 0.0379(10) Uani 1 1 d . . .
H19 H 0.8168 0.4827 0.9010 0.045 Uiso 1 1 calc R . .
C20 C 0.8263(4) 0.4800(3) 0.7651(3) 0.0326(9) Uani 1 1 d . . .
H20 H 0.9166 0.4611 0.7747 0.039 Uiso 1 1 calc R . .
C21 C 0.7550(4) 0.4951(3) 0.6779(3) 0.0329(9) Uani 1 1 d . . .
H21 H 0.7962 0.4873 0.6261 0.039 Uiso 1 1 calc R . .
C22 C 0.6221(4) 0.5218(3) 0.6628(3) 0.0305(9) Uani 1 1 d . . .
H22 H 0.5737 0.5324 0.6010 0.037 Uiso 1 1 calc R . .
C23 C 0.4184(3) 0.9001(2) 0.6662(2) 0.0172(7) Uani 1 1 d . . .
H23 H 0.4041 0.9024 0.7316 0.021 Uiso 1 1 calc R . .
C24 C 0.3265(3) 0.9720(2) 0.6118(2) 0.0195(7) Uani 1 1 d . . .
C25 C 0.1892(3) 0.9617(2) 0.5995(2) 0.0257(8) Uani 1 1 d . . .
H25 H 0.1542 0.9079 0.6212 0.031 Uiso 1 1 calc R . .
C26 C 0.1022(3) 1.0292(2) 0.5556(3) 0.0287(8) Uani 1 1 d . . .
H26 H 0.0088 1.0214 0.5484 0.034 Uiso 1 1 calc R . .
C27 C 0.1518(4) 1.1068(2) 0.5227(2) 0.0286(8) Uani 1 1 d . . .
H27 H 0.0928 1.1526 0.4925 0.034 Uiso 1 1 calc R . .
C28 C 0.2866(4) 1.1178(2) 0.5339(2) 0.0293(8) Uani 1 1 d . . .
H28 H 0.3211 1.1713 0.5112 0.035 Uiso 1 1 calc R . .
C29 C 0.3730(3) 1.0513(2) 0.5781(2) 0.0228(8) Uani 1 1 d . . .
H29 H 0.4662 1.0601 0.5855 0.027 Uiso 1 1 calc R . .
C30 C 0.5658(3) 0.9202(2) 0.6725(2) 0.0206(7) Uani 1 1 d . . .
C31 C 0.6363(4) 0.9686(2) 0.7475(3) 0.0272(8) Uani 1 1 d . . .
H31 H 0.5918 0.9906 0.7938 0.033 Uiso 1 1 calc R . .
C32 C 0.7725(4) 0.9856(3) 0.7566(3) 0.0352(10) Uani 1 1 d . . .
H32 H 0.8198 1.0186 0.8090 0.042 Uiso 1 1 calc R . .
C33 C 0.8371(4) 0.9551(3) 0.6906(3) 0.0394(10) Uani 1 1 d . . .
H33 H 0.9297 0.9663 0.6971 0.047 Uiso 1 1 calc R . .
C34 C 0.7687(4) 0.9080(3) 0.6142(3) 0.0380(10) Uani 1 1 d . . .
H34 H 0.8142 0.8870 0.5680 0.046 Uiso 1 1 calc R . .
C35 C 0.6340(3) 0.8910(2) 0.6043(3) 0.0296(8) Uani 1 1 d . . .
H35 H 0.5873 0.8594 0.5508 0.035 Uiso 1 1 calc R . .
C36 C 0.3696(4) 0.6948(3) 0.9739(3) 0.0390(10) Uani 1 1 d . . .
H36 H 0.4679 0.7054 0.9888 0.047 Uiso 1 1 calc R . .
C37 C 0.3528(5) 0.5926(3) 0.9744(3) 0.0539(13) Uani 1 1 d . . .
H37A H 0.2578 0.5776 0.9636 0.081 Uiso 1 1 calc R . .
H37B H 0.3982 0.5682 1.0350 0.081 Uiso 1 1 calc R . .
H37C H 0.3914 0.5656 0.9249 0.081 Uiso 1 1 calc R . .
C38 C 0.3181(6) 0.7344(4) 1.0578(3) 0.0798(19) Uani 1 1 d . . .
H38A H 0.3650 0.7053 1.1156 0.120 Uiso 1 1 calc R . .
H38B H 0.2224 0.7227 1.0492 0.120 Uiso 1 1 calc R . .
H38C H 0.3343 0.8002 1.0616 0.120 Uiso 1 1 calc R . .
C39 C 0.2647(4) 0.8775(3) 0.8669(3) 0.0361(10) Uani 1 1 d . . .
H39 H 0.2495 0.9010 0.8014 0.043 Uiso 1 1 calc R . .
C40 C 0.3841(4) 0.9318(3) 0.9202(3) 0.0425(11) Uani 1 1 d . . .
H40A H 0.3991 0.9169 0.9869 0.064 Uiso 1 1 calc R . .
H40B H 0.3660 0.9971 0.9116 0.064 Uiso 1 1 calc R . .
H40C H 0.4635 0.9161 0.8963 0.064 Uiso 1 1 calc R . .
C41 C 0.1375(4) 0.9012(3) 0.9004(3) 0.0473(11) Uani 1 1 d . . .
H41A H 0.1270 0.9676 0.9012 0.071 Uiso 1 1 calc R . .
H41B H 0.1432 0.8771 0.9635 0.071 Uiso 1 1 calc R . .
H41C H 0.0607 0.8743 0.8580 0.071 Uiso 1 1 calc R . .
C42 C 0.1504(3) 0.6914(2) 0.7954(2) 0.0228(7) Uani 1 1 d . . .
H42 H 0.1786 0.6287 0.7811 0.027 Uiso 1 1 calc R . .
C43 C 0.0493(4) 0.6789(3) 0.8588(3) 0.0369(10) Uani 1 1 d . . .
H43A H -0.0198 0.6358 0.8297 0.055 Uiso 1 1 calc R . .
H43B H 0.0083 0.7378 0.8673 0.055 Uiso 1 1 calc R . .
H43C H 0.0951 0.6554 0.9197 0.055 Uiso 1 1 calc R . .
C44 C 0.0781(3) 0.7315(2) 0.7027(2) 0.0274(9) Uani 1 1 d . . .
H44A H 0.0518 0.7944 0.7124 0.041 Uiso 1 1 calc R . .
H44B H -0.0014 0.6952 0.6779 0.041 Uiso 1 1 calc R . .
H44C H 0.1374 0.7309 0.6583 0.041 Uiso 1 1 calc R . .
C45 C 0.6818(3) 0.7793(2) 0.9619(2) 0.0283(9) Uani 1 1 d . . .
H45 H 0.6037 0.7959 0.9893 0.034 Uiso 1 1 calc R . .
C46 C 0.7510(4) 0.6937(3) 1.0075(3) 0.0383(10) Uani 1 1 d . . .
H46A H 0.8150 0.6721 0.9703 0.046 Uiso 1 1 calc R . .
H46B H 0.6837 0.6453 1.0067 0.046 Uiso 1 1 calc R . .
C47 C 0.8252(5) 0.7098(3) 1.1087(3) 0.0474(11) Uani 1 1 d . . .
H47A H 0.7602 0.7237 1.1480 0.057 Uiso 1 1 calc R . .
H47B H 0.8738 0.6538 1.1332 0.057 Uiso 1 1 calc R . .
C48 C 0.9234(4) 0.7885(3) 1.1141(3) 0.0445(11) Uani 1 1 d . . .
H48A H 0.9658 0.8004 1.1802 0.053 Uiso 1 1 calc R . .
H48B H 0.9942 0.7719 1.0805 0.053 Uiso 1 1 calc R . .
C49 C 0.8530(4) 0.8736(3) 1.0712(3) 0.0406(10) Uani 1 1 d . . .
H49A H 0.9189 0.9231 1.0729 0.049 Uiso 1 1 calc R . .
H49B H 0.7880 0.8933 1.1084 0.049 Uiso 1 1 calc R . .
C50 C 0.7810(4) 0.8574(3) 0.9706(3) 0.0321(9) Uani 1 1 d . . .
H50A H 0.7333 0.9137 0.9458 0.039 Uiso 1 1 calc R . .
H50B H 0.8472 0.8438 0.9322 0.039 Uiso 1 1 calc R . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ge1 N1 1.904(2) . ?
Ge1 C45 2.031(4) . ?
Si1 N1 1.780(2) . ?
Si1 C36 1.886(4) . ?
Si1 C42 1.898(3) . ?
Si1 C39 1.905(4) . ?
N1 C1 1.441(4) . ?
C1 C2 1.401(4) . ?
C1 C6 1.412(4) . ?
C2 C3 1.416(4) . ?
C2 C10 1.502(5) . ?
C3 C4 1.374(5) . ?
C4 C5 1.396(4) . ?
C4 C7 1.507(5) . ?
C5 C6 1.402(5) . ?
C6 C23 1.514(4) . ?
C7 C9 1.522(5) . ?
C7 C8 1.523(5) . ?
C10 C17 1.522(5) . ?
C10 C11 1.529(5) . ?
C11 C16 1.394(5) . ?
C11 C12 1.397(5) . ?
C12 C13 1.386(5) . ?
C13 C14 1.363(5) . ?
C14 C15 1.388(5) . ?
C15 C16 1.372(5) . ?
C17 C18 1.383(5) . ?
C17 C22 1.389(5) . ?
C18 C19 1.381(5) . ?
C19 C20 1.367(5) . ?
C20 C21 1.350(5) . ?
C21 C22 1.394(5) . ?
C23 C24 1.525(5) . ?
C23 C30 1.527(4) . ?
C24 C29 1.387(5) . ?
C24 C25 1.393(5) . ?
C25 C26 1.398(5) . ?
C26 C27 1.376(5) . ?
C27 C28 1.370(5) . ?
C28 C29 1.385(5) . ?
C30 C31 1.379(5) . ?
C30 C35 1.401(5) . ?
C31 C32 1.401(5) . ?
C32 C33 1.358(6) . ?
C33 C34 1.377(6) . ?
C34 C35 1.384(5) . ?
C36 C37 1.511(6) . ?
C36 C38 1.548(6) . ?
C39 C41 1.529(5) . ?
C39 C40 1.533(5) . ?
C42 C44 1.523(5) . ?
C42 C43 1.542(5) . ?
C45 C50 1.521(5) . ?
C45 C46 1.527(5) . ?
C46 C47 1.536(5) . ?
C47 C48 1.525(6) . ?
C48 C49 1.513(6) . ?
C49 C50 1.522(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 Ge1 C45 107.99(12) . . ?
N1 Si1 C36 107.17(15) . . ?
N1 Si1 C42 111.30(14) . . ?
C36 Si1 C42 108.62(17) . . ?
N1 Si1 C39 108.10(17) . . ?
C36 Si1 C39 114.0(2) . . ?
C42 Si1 C39 107.71(16) . . ?
C1 N1 Si1 118.62(18) . . ?
C1 N1 Ge1 106.20(17) . . ?
Si1 N1 Ge1 135.18(13) . . ?
C2 C1 C6 120.2(3) . . ?
C2 C1 N1 119.3(3) . . ?
C6 C1 N1 120.4(3) . . ?
C1 C2 C3 118.0(3) . . ?
C1 C2 C10 122.0(3) . . ?
C3 C2 C10 120.0(3) . . ?
C4 C3 C2 123.0(3) . . ?
C3 C4 C5 117.7(3) . . ?
C3 C4 C7 120.8(3) . . ?
C5 C4 C7 121.5(3) . . ?
C4 C5 C6 122.0(3) . . ?
C5 C6 C1 118.9(3) . . ?
C5 C6 C23 119.2(3) . . ?
C1 C6 C23 121.7(3) . . ?
C4 C7 C9 111.0(3) . . ?
C4 C7 C8 113.0(3) . . ?
C9 C7 C8 110.0(3) . . ?
C2 C10 C17 110.0(3) . . ?
C2 C10 C11 115.9(3) . . ?
C17 C10 C11 111.0(3) . . ?
C16 C11 C12 118.1(3) . . ?
C16 C11 C10 121.3(3) . . ?
C12 C11 C10 120.5(3) . . ?
C13 C12 C11 120.4(3) . . ?
C14 C13 C12 120.9(4) . . ?
C13 C14 C15 119.2(3) . . ?
C16 C15 C14 120.8(3) . . ?
C15 C16 C11 120.6(3) . . ?
C18 C17 C22 117.5(3) . . ?
C18 C17 C10 121.2(3) . . ?
C22 C17 C10 121.3(3) . . ?
C19 C18 C17 121.0(4) . . ?
C20 C19 C18 120.9(4) . . ?
C21 C20 C19 119.1(4) . . ?
C20 C21 C22 121.0(4) . . ?
C17 C22 C21 120.5(4) . . ?
C6 C23 C24 113.6(3) . . ?
C6 C23 C30 110.8(3) . . ?
C24 C23 C30 113.3(3) . . ?
C29 C24 C25 117.4(3) . . ?
C29 C24 C23 123.0(3) . . ?
C25 C24 C23 119.4(3) . . ?
C24 C25 C26 121.0(3) . . ?
C27 C26 C25 120.0(3) . . ?
C28 C27 C26 119.7(3) . . ?
C27 C28 C29 120.4(3) . . ?
C28 C29 C24 121.5(3) . . ?
C31 C30 C35 117.9(3) . . ?
C31 C30 C23 119.8(3) . . ?
C35 C30 C23 122.4(3) . . ?
C30 C31 C32 121.0(4) . . ?
C33 C32 C31 120.0(4) . . ?
C32 C33 C34 120.1(4) . . ?
C33 C34 C35 120.3(4) . . ?
C34 C35 C30 120.6(4) . . ?
C37 C36 C38 108.1(3) . . ?
C37 C36 Si1 115.4(3) . . ?
C38 C36 Si1 116.1(3) . . ?
C41 C39 C40 111.4(3) . . ?
C41 C39 Si1 117.8(3) . . ?
C40 C39 Si1 111.6(3) . . ?
C44 C42 C43 108.5(3) . . ?
C44 C42 Si1 116.9(2) . . ?
C43 C42 Si1 112.1(2) . . ?
C50 C45 C46 110.0(3) . . ?
C50 C45 Ge1 106.9(2) . . ?
C46 C45 Ge1 105.8(2) . . ?
C45 C46 C47 112.8(3) . . ?
C48 C47 C46 110.9(3) . . ?
C49 C48 C47 110.5(3) . . ?
C48 C49 C50 111.5(3) . . ?
C45 C50 C49 112.3(3) . . ?

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        26.00
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         0.589
_refine_diff_density_min         -0.379
_refine_diff_density_rms         0.059
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_compound10
_database_code_depnum_ccdc_archive 'CCDC 1422731'
_audit_update_record             
;
2015-09-07 deposited with the CCDC.
2015-09-22 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C52 H67 Ge N Si'
_chemical_formula_weight         806.75

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'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   P2(1)/n

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

_cell_length_a                   9.942(2)
_cell_length_b                   15.413(3)
_cell_length_c                   28.793(6)
_cell_angle_alpha                90.00
_cell_angle_beta                 97.18(3)
_cell_angle_gamma                90.00
_cell_volume                     4377.6(15)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.05
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.224
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1728
_exptl_absorpt_coefficient_mu    0.763
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9251
_exptl_absorpt_correction_T_max  0.960
_exptl_absorpt_process_details   XDS

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71080
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_source         'Australian Synchrotron'
_diffrn_radiation_monochromator  ?
_diffrn_measurement_device_type  'ADSC Quantum 210r'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            69020
_diffrn_reflns_av_R_equivalents  0.0799
_diffrn_reflns_av_sigmaI/netI    0.0446
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_theta_min         2.96
_diffrn_reflns_theta_max         27.00
_reflns_number_total             9523
_reflns_number_gt                7948
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Blu-Ice (McPhillips, 2002)'
_computing_cell_refinement       'XDS (Kabsch, 1993)'
_computing_data_reduction        'XDS (Kabsch, 1993)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    X-Seed
_computing_publication_material  CifTAB

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger.
 The carbon atoms of the cycloctyl ligand were found to be disorded over 
 two sites. This disorder was modelled, and the carbon atoms of the minor
 set refined isotropically. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0829P)²+3.4502P] 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         9523
_refine_ls_number_parameters     537
_refine_ls_number_restraints     35
_refine_ls_R_factor_all          0.0599
_refine_ls_R_factor_gt           0.0501
_refine_ls_wR_factor_ref         0.1476
_refine_ls_wR_factor_gt          0.1404
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_restrained_S_all      1.095
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ge1 Ge 0.94782(3) 0.776528(18) 0.836071(9) 0.02977(10) Uani 1 1 d D . .
Si1 Si 0.60499(7) 0.77174(4) 0.81911(2) 0.02605(16) Uani 1 1 d . . .
N1 N 0.7686(2) 0.77649(12) 0.85237(7) 0.0246(4) Uani 1 1 d . A .
C1 C 0.7808(2) 0.77534(15) 0.90339(8) 0.0237(5) Uani 1 1 d . . .
C2 C 0.7845(2) 0.85324(15) 0.92939(8) 0.0239(5) Uani 1 1 d . A .
C3 C 0.7993(2) 0.84953(15) 0.97834(8) 0.0251(5) Uani 1 1 d . . .
H3 H 0.8008 0.9023 0.9955 0.030 Uiso 1 1 calc R A .
C4 C 0.8119(3) 0.77180(15) 1.00291(8) 0.0259(5) Uani 1 1 d . A .
C5 C 0.8106(3) 0.69506(16) 0.97672(8) 0.0273(5) Uani 1 1 d . . .
H5 H 0.8192 0.6410 0.9927 0.033 Uiso 1 1 calc R A .
C6 C 0.7972(3) 0.69556(15) 0.92799(8) 0.0253(5) Uani 1 1 d . A .
C7 C 0.7821(3) 0.94204(15) 0.90558(8) 0.0248(5) Uani 1 1 d . . .
H7 H 0.7234 0.9360 0.8749 0.030 Uiso 1 1 calc R A .
C8 C 0.7178(3) 1.01278(15) 0.93302(8) 0.0270(5) Uani 1 1 d . A .
C9 C 0.5798(3) 1.01261(19) 0.93484(10) 0.0384(6) Uani 1 1 d . . .
H9 H 0.5260 0.9679 0.9192 0.046 Uiso 1 1 calc R A .
C10 C 0.5173(3) 1.0764(2) 0.95897(11) 0.0421(7) Uani 1 1 d . A .
H10 H 0.4219 1.0751 0.9594 0.050 Uiso 1 1 calc R . .
C11 C 0.5938(3) 1.14126(17) 0.98219(9) 0.0364(6) Uani 1 1 d . . .
H11 H 0.5516 1.1850 0.9986 0.044 Uiso 1 1 calc R A .
C12 C 0.7315(3) 1.14201(18) 0.98144(10) 0.0383(6) Uani 1 1 d . A .
H12 H 0.7849 1.1860 0.9978 0.046 Uiso 1 1 calc R . .
C13 C 0.7941(3) 1.07858(17) 0.95674(9) 0.0346(6) Uani 1 1 d . . .
H13 H 0.8894 1.0804 0.9561 0.042 Uiso 1 1 calc R A .
C14 C 0.9228(3) 0.96882(15) 0.89438(8) 0.0274(5) Uani 1 1 d . A .
C15 C 1.0414(3) 0.94284(16) 0.92178(9) 0.0319(5) Uani 1 1 d . . .
H15 H 1.0365 0.9049 0.9475 0.038 Uiso 1 1 calc R A .
C16 C 1.1670(3) 0.97209(18) 0.91172(10) 0.0365(6) Uani 1 1 d . A .
H16 H 1.2472 0.9546 0.9308 0.044 Uiso 1 1 calc R . .
C17 C 1.1755(3) 1.02648(18) 0.87408(10) 0.0375(6) Uani 1 1 d . . .
H17 H 1.2615 1.0458 0.8671 0.045 Uiso 1 1 calc R A .
C18 C 1.0591(3) 1.05268(19) 0.84659(9) 0.0404(6) Uani 1 1 d . A .
H18 H 1.0650 1.0899 0.8206 0.048 Uiso 1 1 calc R . .
C19 C 0.9333(3) 1.02462(18) 0.85680(9) 0.0356(6) Uani 1 1 d . . .
H19 H 0.8534 1.0436 0.8380 0.043 Uiso 1 1 calc R A .
C20 C 0.8080(3) 0.60979(15) 0.90213(8) 0.0275(5) Uani 1 1 d . . .
H20 H 0.7554 0.6175 0.8705 0.033 Uiso 1 1 calc R A .
C21 C 0.7411(3) 0.53443(16) 0.92520(9) 0.0305(5) Uani 1 1 d . A .
C22 C 0.8130(3) 0.46226(18) 0.94278(11) 0.0417(7) Uani 1 1 d . . .
H22 H 0.9081 0.4594 0.9420 0.050 Uiso 1 1 calc R A .
C23 C 0.7457(4) 0.3935(2) 0.96172(12) 0.0475(7) Uani 1 1 d . A .
H23 H 0.7959 0.3440 0.9734 0.057 Uiso 1 1 calc R . .
C24 C 0.6101(4) 0.3962(2) 0.96371(11) 0.0480(7) Uani 1 1 d . . .
H24 H 0.5655 0.3487 0.9762 0.058 Uiso 1 1 calc R A .
C25 C 0.5375(3) 0.4690(2) 0.94731(12) 0.0469(7) Uani 1 1 d . A .
H25 H 0.4429 0.4723 0.9491 0.056 Uiso 1 1 calc R . .
C26 C 0.6031(3) 0.53702(19) 0.92825(11) 0.0409(6) Uani 1 1 d . . .
H26 H 0.5525 0.5866 0.9170 0.049 Uiso 1 1 calc R A .
C27 C 0.9530(3) 0.58923(16) 0.89395(9) 0.0310(5) Uani 1 1 d . A .
C28 C 0.9757(3) 0.5399(2) 0.85516(10) 0.0403(6) Uani 1 1 d . . .
H28 H 0.9004 0.5213 0.8339 0.048 Uiso 1 1 calc R A .
C29 C 1.1057(3) 0.5171(2) 0.84677(11) 0.0468(7) Uani 1 1 d . A .
H29 H 1.1185 0.4845 0.8196 0.056 Uiso 1 1 calc R . .
C30 C 1.2150(3) 0.5414(2) 0.87739(11) 0.0464(7) Uani 1 1 d . . .
H30 H 1.3039 0.5258 0.8717 0.056 Uiso 1 1 calc R A .
C31 C 1.1958(3) 0.5886(3) 0.91653(12) 0.0506(8) Uani 1 1 d . A .
H31 H 1.2715 0.6044 0.9383 0.061 Uiso 1 1 calc R . .
C32 C 1.0654(3) 0.6133(2) 0.92447(11) 0.0437(7) Uani 1 1 d . . .
H32 H 1.0537 0.6472 0.9512 0.052 Uiso 1 1 calc R A .
C33 C 0.8315(3) 0.77056(16) 1.05606(8) 0.0308(5) Uani 1 1 d . . .
H33 H 0.8274 0.8320 1.0669 0.037 Uiso 1 1 calc R A .
C34 C 0.9687(3) 0.7347(2) 1.07571(10) 0.0419(7) Uani 1 1 d . A .
H34A H 0.9755 0.6740 1.0661 0.063 Uiso 1 1 calc R . .
H34B H 0.9791 0.7381 1.1100 0.063 Uiso 1 1 calc R . .
H34C H 1.0403 0.7688 1.0638 0.063 Uiso 1 1 calc R . .
C35 C 0.7204(4) 0.7210(3) 1.07610(11) 0.0531(9) Uani 1 1 d . A .
H35A H 0.7224 0.6601 1.0664 0.080 Uiso 1 1 calc R . .
H35B H 0.6322 0.7463 1.0645 0.080 Uiso 1 1 calc R . .
H35C H 0.7348 0.7245 1.1103 0.080 Uiso 1 1 calc R . .
C36 C 0.4730(3) 0.8172(2) 0.85448(10) 0.0384(6) Uani 1 1 d . A .
H36 H 0.5111 0.8730 0.8681 0.046 Uiso 1 1 calc R . .
C37 C 0.3396(3) 0.8411(2) 0.82387(12) 0.0480(8) Uani 1 1 d . . .
H37A H 0.2960 0.7882 0.8104 0.072 Uiso 1 1 calc R A .
H37B H 0.3592 0.8799 0.7986 0.072 Uiso 1 1 calc R . .
H37C H 0.2788 0.8704 0.8431 0.072 Uiso 1 1 calc R . .
C38 C 0.4414(3) 0.7625(2) 0.89569(11) 0.0430(7) Uani 1 1 d . . .
H38A H 0.3729 0.7919 0.9117 0.065 Uiso 1 1 calc R A .
H38B H 0.5242 0.7545 0.9176 0.065 Uiso 1 1 calc R . .
H38C H 0.4069 0.7058 0.8844 0.065 Uiso 1 1 calc R . .
C39 C 0.5603(3) 0.65363(18) 0.80281(9) 0.0334(6) Uani 1 1 d . A .
H39 H 0.5747 0.6204 0.8328 0.040 Uiso 1 1 calc R . .
C40 C 0.6576(3) 0.61411(18) 0.77159(10) 0.0380(6) Uani 1 1 d . . .
H40A H 0.6384 0.5521 0.7674 0.057 Uiso 1 1 calc R A .
H40B H 0.7512 0.6219 0.7863 0.057 Uiso 1 1 calc R . .
H40C H 0.6459 0.6430 0.7410 0.057 Uiso 1 1 calc R . .
C41 C 0.4127(3) 0.6363(2) 0.78217(11) 0.0407(6) Uani 1 1 d . . .
H41A H 0.3898 0.6721 0.7542 0.061 Uiso 1 1 calc R A .
H41B H 0.3523 0.6508 0.8054 0.061 Uiso 1 1 calc R . .
H41C H 0.4020 0.5749 0.7737 0.061 Uiso 1 1 calc R . .
C42 C 0.6119(3) 0.8399(2) 0.76469(10) 0.0401(6) Uani 1 1 d . A .
H42 H 0.7024 0.8271 0.7545 0.048 Uiso 1 1 calc R . .
C43 C 0.5087(4) 0.8183(2) 0.72195(11) 0.0527(8) Uani 1 1 d . . .
H43A H 0.4168 0.8295 0.7294 0.079 Uiso 1 1 calc R A .
H43B H 0.5172 0.7570 0.7137 0.079 Uiso 1 1 calc R . .
H43C H 0.5263 0.8547 0.6954 0.079 Uiso 1 1 calc R . .
C44 C 0.6137(4) 0.9375(2) 0.77456(11) 0.0505(8) Uani 1 1 d . . .
H44A H 0.6205 0.9693 0.7455 0.076 Uiso 1 1 calc R A .
H44B H 0.6918 0.9515 0.7976 0.076 Uiso 1 1 calc R . .
H44C H 0.5299 0.9540 0.7870 0.076 Uiso 1 1 calc R . .
C45 C 0.9422(9) 0.7666(4) 0.76470(17) 0.052(3) Uani 0.793(8) 1 d PD A 1
H45 H 0.8481 0.7517 0.7505 0.062 Uiso 0.793(8) 1 calc PR A 1
C46 C 0.9798(10) 0.8539(4) 0.74776(19) 0.069(3) Uani 0.793(8) 1 d PD A 1
H46A H 0.9149 0.8962 0.7581 0.082 Uiso 0.793(8) 1 calc PR A 1
H46B H 1.0702 0.8685 0.7644 0.082 Uiso 0.793(8) 1 calc PR A 1
C47 C 0.9854(8) 0.8690(3) 0.69718(15) 0.083(2) Uani 0.793(8) 1 d PD A 1
H47A H 1.0734 0.8467 0.6896 0.100 Uiso 0.793(8) 1 calc PR A 1
H47B H 0.9854 0.9325 0.6920 0.100 Uiso 0.793(8) 1 calc PR A 1
C48 C 0.8755(9) 0.8305(4) 0.66237(18) 0.096(3) Uani 0.793(8) 1 d PD A 1
H48A H 0.7891 0.8360 0.6759 0.116 Uiso 0.793(8) 1 calc PR A 1
H48B H 0.8675 0.8676 0.6341 0.116 Uiso 0.793(8) 1 calc PR A 1
C48A C 0.9579(19) 0.8316(9) 0.6619(4) 0.055(5) Uiso 0.207(8) 1 d PD A 2
H48C H 1.0580 0.8275 0.6672 0.065 Uiso 0.207(8) 1 calc PR A 2
H48D H 0.9323 0.8641 0.6325 0.065 Uiso 0.207(8) 1 calc PR A 2
C49 C 0.8851(7) 0.7423(3) 0.6471(3) 0.077(3) Uani 0.793(8) 1 d PD A 1
H49A H 0.7902 0.7254 0.6363 0.092 Uiso 0.793(8) 1 calc PR A 1
H49B H 0.9303 0.7465 0.6184 0.092 Uiso 0.793(8) 1 calc PR A 1
C49A C 0.898(2) 0.7404(9) 0.6570(7) 0.12(2) Uiso 0.207(8) 1 d PD A 2
H49C H 0.8257 0.7343 0.6777 0.138 Uiso 0.207(8) 1 calc PR A 2
H49D H 0.8563 0.7308 0.6243 0.138 Uiso 0.207(8) 1 calc PR A 2
C50 C 0.9431(9) 0.6674(4) 0.67057(19) 0.092(2) Uani 0.793(8) 1 d PD A 1
H50A H 0.9697 0.6281 0.6461 0.111 Uiso 0.793(8) 1 calc PR A 1
H50B H 0.8694 0.6380 0.6846 0.111 Uiso 0.793(8) 1 calc PR A 1
C50A C 1.0078(18) 0.6734(10) 0.6702(5) 0.049(5) Uiso 0.207(8) 1 d PD A 2
H50C H 0.9959 0.6246 0.6477 0.059 Uiso 0.207(8) 1 calc PR A 2
H50D H 1.0975 0.7000 0.6681 0.059 Uiso 0.207(8) 1 calc PR A 2
C51 C 1.0605(6) 0.6725(4) 0.70762(15) 0.0678(16) Uani 0.793(8) 1 d PD A 1
H51A H 1.1235 0.7167 0.6979 0.081 Uiso 0.793(8) 1 calc PR A 1
H51B H 1.1083 0.6160 0.7083 0.081 Uiso 0.793(8) 1 calc PR A 1
C51A C 1.0042(18) 0.6392(7) 0.7190(5) 0.055(5) Uiso 0.207(8) 1 d PD A 2
H51C H 0.9105 0.6205 0.7222 0.066 Uiso 0.207(8) 1 calc PR A 2
H51D H 1.0631 0.5873 0.7234 0.066 Uiso 0.207(8) 1 calc PR A 2
C52 C 1.0369(4) 0.6930(3) 0.75650(12) 0.0417(12) Uani 0.793(8) 1 d PD A 1
H52A H 1.1260 0.7059 0.7746 0.050 Uiso 0.793(8) 1 calc PR A 1
H52B H 1.0018 0.6399 0.7701 0.050 Uiso 0.793(8) 1 calc PR A 1
C46A C 0.9769(13) 0.8568(7) 0.7496(3) 0.006(3) Uiso 0.207(8) 1 d PD A 2
H46C H 0.9537 0.9008 0.7723 0.007 Uiso 0.207(8) 1 calc PR A 2
H46D H 1.0764 0.8582 0.7493 0.007 Uiso 0.207(8) 1 calc PR A 2
C45A C 0.9355(14) 0.7664(6) 0.7658(2) 0.003(4) Uiso 0.207(8) 1 d PDU A 2
H45A H 0.8439 0.7477 0.7508 0.003 Uiso 0.207(8) 1 calc PR A 2
C52A C 1.049(2) 0.7029(10) 0.7571(6) 0.15(2) Uiso 0.207(8) 1 d PDU A 2
H52C H 1.1274 0.7361 0.7485 0.179 Uiso 0.207(8) 1 calc PR A 2
H52D H 1.0790 0.6709 0.7864 0.179 Uiso 0.207(8) 1 calc PR A 2
C47A C 0.9084(16) 0.8797(8) 0.7019(4) 0.051(5) Uiso 0.207(8) 1 d PD A 2
H47C H 0.9204 0.9426 0.6969 0.061 Uiso 0.207(8) 1 calc PR A 2
H47D H 0.8101 0.8688 0.7011 0.061 Uiso 0.207(8) 1 calc PR 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 N1 1.898(2) . ?
Ge1 C45A 2.018(7) . ?
Ge1 C45 2.054(5) . ?
Si1 N1 1.783(2) . ?
Si1 C36 1.893(3) . ?
Si1 C42 1.895(3) . ?
Si1 C39 1.918(3) . ?
N1 C1 1.459(3) . ?
C1 C2 1.413(3) . ?
C1 C6 1.418(3) . ?
C2 C3 1.400(3) . ?
C2 C7 1.530(3) . ?
C3 C4 1.389(3) . ?
C4 C5 1.402(3) . ?
C4 C33 1.519(3) . ?
C5 C6 1.393(3) . ?
C6 C20 1.527(3) . ?
C7 C14 1.531(3) . ?
C7 C8 1.532(3) . ?
C8 C9 1.380(4) . ?
C8 C13 1.393(4) . ?
C9 C10 1.394(4) . ?
C10 C11 1.378(4) . ?
C11 C12 1.372(4) . ?
C12 C13 1.400(4) . ?
C14 C15 1.393(4) . ?
C14 C19 1.396(3) . ?
C15 C16 1.391(4) . ?
C16 C17 1.381(4) . ?
C17 C18 1.378(4) . ?
C18 C19 1.390(4) . ?
C20 C27 1.523(4) . ?
C20 C21 1.530(3) . ?
C21 C22 1.383(4) . ?
C21 C26 1.386(4) . ?
C22 C23 1.400(4) . ?
C23 C24 1.357(5) . ?
C24 C25 1.385(5) . ?
C25 C26 1.384(4) . ?
C27 C32 1.383(4) . ?
C27 C28 1.393(4) . ?
C28 C29 1.390(4) . ?
C29 C30 1.363(5) . ?
C30 C31 1.374(5) . ?
C31 C32 1.397(4) . ?
C33 C34 1.514(4) . ?
C33 C35 1.515(4) . ?
C36 C38 1.520(4) . ?
C36 C37 1.543(4) . ?
C39 C40 1.528(4) . ?
C39 C41 1.536(4) . ?
C42 C44 1.529(4) . ?
C42 C43 1.537(4) . ?
C45 C46 1.494(6) . ?
C45 C52 1.511(6) . ?
C46 C47 1.483(6) . ?
C47 C48 1.509(6) . ?
C48 C49 1.436(6) . ?
C48A C47A 1.504(8) . ?
C48A C49A 1.527(9) . ?
C49 C50 1.423(6) . ?
C49A C50A 1.519(8) . ?
C50 C51 1.482(6) . ?
C50A C51A 1.506(8) . ?
C51 C52 1.490(4) . ?
C51A C52A 1.497(8) . ?
C46A C47A 1.497(8) . ?
C46A C45A 1.541(7) . ?
C45A C52A 1.537(8) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Ge1 C45A 107.9(4) . . ?
N1 Ge1 C45 109.8(3) . . ?
C45A Ge1 C45 1.9(6) . . ?
N1 Si1 C36 110.05(11) . . ?
N1 Si1 C42 107.25(12) . . ?
C36 Si1 C42 109.78(14) . . ?
N1 Si1 C39 109.77(11) . . ?
C36 Si1 C39 109.16(13) . . ?
C42 Si1 C39 110.81(13) . . ?
C1 N1 Si1 119.72(16) . . ?
C1 N1 Ge1 106.64(15) . . ?
Si1 N1 Ge1 133.53(12) . . ?
C2 C1 C6 118.6(2) . . ?
C2 C1 N1 121.1(2) . . ?
C6 C1 N1 120.2(2) . . ?
C3 C2 C1 119.4(2) . . ?
C3 C2 C7 118.8(2) . . ?
C1 C2 C7 121.7(2) . . ?
C4 C3 C2 122.6(2) . . ?
C3 C4 C5 117.4(2) . . ?
C3 C4 C33 121.1(2) . . ?
C5 C4 C33 121.5(2) . . ?
C6 C5 C4 122.0(2) . . ?
C5 C6 C1 119.9(2) . . ?
C5 C6 C20 118.9(2) . . ?
C1 C6 C20 121.2(2) . . ?
C2 C7 C14 111.84(19) . . ?
C2 C7 C8 112.93(19) . . ?
C14 C7 C8 111.6(2) . . ?
C9 C8 C13 117.8(2) . . ?
C9 C8 C7 119.9(2) . . ?
C13 C8 C7 122.3(2) . . ?
C8 C9 C10 121.6(3) . . ?
C11 C10 C9 120.0(3) . . ?
C12 C11 C10 119.3(2) . . ?
C11 C12 C13 120.7(3) . . ?
C8 C13 C12 120.5(3) . . ?
C15 C14 C19 118.4(2) . . ?
C15 C14 C7 122.3(2) . . ?
C19 C14 C7 119.2(2) . . ?
C16 C15 C14 120.5(2) . . ?
C17 C16 C15 120.3(3) . . ?
C18 C17 C16 119.9(3) . . ?
C17 C18 C19 120.1(3) . . ?
C18 C19 C14 120.8(3) . . ?
C27 C20 C6 112.4(2) . . ?
C27 C20 C21 112.3(2) . . ?
C6 C20 C21 112.6(2) . . ?
C22 C21 C26 118.0(3) . . ?
C22 C21 C20 122.5(3) . . ?
C26 C21 C20 119.5(2) . . ?
C21 C22 C23 120.1(3) . . ?
C24 C23 C22 121.2(3) . . ?
C23 C24 C25 119.3(3) . . ?
C26 C25 C24 119.8(3) . . ?
C25 C26 C21 121.5(3) . . ?
C32 C27 C28 117.2(3) . . ?
C32 C27 C20 123.5(2) . . ?
C28 C27 C20 119.3(2) . . ?
C29 C28 C27 121.6(3) . . ?
C30 C29 C28 120.1(3) . . ?
C29 C30 C31 119.7(3) . . ?
C30 C31 C32 120.3(3) . . ?
C27 C32 C31 121.0(3) . . ?
C34 C33 C35 109.8(2) . . ?
C34 C33 C4 112.2(2) . . ?
C35 C33 C4 112.5(2) . . ?
C38 C36 C37 109.3(3) . . ?
C38 C36 Si1 116.0(2) . . ?
C37 C36 Si1 112.6(2) . . ?
C40 C39 C41 110.3(2) . . ?
C40 C39 Si1 112.21(19) . . ?
C41 C39 Si1 116.1(2) . . ?
C44 C42 C43 110.7(3) . . ?
C44 C42 Si1 113.1(2) . . ?
C43 C42 Si1 116.9(2) . . ?
C46 C45 C52 116.0(5) . . ?
C46 C45 Ge1 106.4(4) . . ?
C52 C45 Ge1 105.8(3) . . ?
C47 C46 C45 120.3(4) . . ?
C46 C47 C48 118.5(6) . . ?
C49 C48 C47 120.4(5) . . ?
C47A C48A C49A 111.3(8) . . ?
C50 C49 C48 131.4(6) . . ?
C50A C49A C48A 109.9(8) . . ?
C49 C50 C51 122.4(5) . . ?
C51A C50A C49A 111.8(8) . . ?
C50 C51 C52 119.2(5) . . ?
C52A C51A C50A 114.5(8) . . ?
C51 C52 C45 118.8(3) . . ?
C47A C46A C45A 112.5(7) . . ?
C52A C45A C46A 107.3(7) . . ?
C52A C45A Ge1 105.0(9) . . ?
C46A C45A Ge1 104.4(6) . . ?
C51A C52A C45A 112.4(9) . . ?
C46A C47A C48A 115.6(8) . . ?

_diffrn_measured_fraction_theta_max 0.995
_diffrn_reflns_theta_full        27.00
_diffrn_measured_fraction_theta_full 0.995
_refine_diff_density_max         0.596
_refine_diff_density_min         -0.793
_refine_diff_density_rms         0.074
####################################################################### 
# 
# 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_compound11
_database_code_depnum_ccdc_archive 'CCDC 1422732'
_audit_update_record             
;
2015-09-07 deposited with the CCDC.
2015-09-22 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C46 H57 N Si Sn'
_chemical_formula_weight         770.71

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'

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   P-1

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   10.673(2)
_cell_length_b                   12.534(3)
_cell_length_c                   15.493(3)
_cell_angle_alpha                82.27(3)
_cell_angle_beta                 85.09(3)
_cell_angle_gamma                73.63(3)
_cell_volume                     1968.0(7)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       block
_exptl_crystal_colour            yellow-orange
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.04
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.301
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             808
_exptl_absorpt_coefficient_mu    0.712
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.961
_exptl_absorpt_correction_T_max  0.970
_exptl_absorpt_process_details   XDS

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71080
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_source         'Australian Synchrotron'
_diffrn_radiation_monochromator  ?
_diffrn_measurement_device_type  'ADSC Quantum 210r'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            22483
_diffrn_reflns_av_R_equivalents  0.0623
_diffrn_reflns_av_sigmaI/netI    0.0554
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         3.20
_diffrn_reflns_theta_max         25.20
_reflns_number_total             6158
_reflns_number_gt                5779
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Blu-Ice (McPhillips, 2002)'
_computing_cell_refinement       'XDS (Kabsch, 1993)'
_computing_data_reduction        'XDS (Kabsch, 1993)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    X-Seed
_computing_publication_material  CifTAB

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
 The tin atom was found to be disordered over two sites in an approx
 93:7 ratio. The ADP for the minor site was refined isotropically. Although
 an ethyl ligand, the atoms of which have ca. 7% occupancy, is likely attached
 to the minor occupancy Sn center, it proved difficult to locate these partially
 occupied atoms from difference maps. Accordingly, the C and H atoms of the 
 ethyl ligand bonded to the major occupancy Sn atom were refined at full 
 occupancy.
 The low value (87.0%) for completeness of data to theta = 25.2 deg. arises 
 from hardware constraints associated with the diffractometer used at the 
 Australian Synchrotron and is common for triclinic data sets on that instrument. 
 Its minimum crystal to detector distance is 72 mm and its
 goniometer only rotates about the phi axis.

;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0547P)²+1.6330P] 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         6158
_refine_ls_number_parameters     456
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0415
_refine_ls_R_factor_gt           0.0396
_refine_ls_wR_factor_ref         0.1052
_refine_ls_wR_factor_gt          0.1038
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_restrained_S_all      1.075
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Sn1 Sn 0.587220(19) 0.581611(17) 0.715482(15) 0.02434(11) Uani 0.9298(18) 1 d P
A 1
Si1 Si 0.90794(7) 0.55467(6) 0.73664(5) 0.01727(18) Uani 1 1 d . A .
N1 N 0.7470(2) 0.64488(18) 0.73282(15) 0.0180(5) Uani 1 1 d D . .
C1 C 0.7166(2) 0.7644(2) 0.72986(18) 0.0167(5) Uani 1 1 d . A .
C2 C 0.6937(2) 0.8197(2) 0.80570(18) 0.0179(5) Uani 1 1 d . . .
C3 C 0.6617(3) 0.9370(2) 0.79789(19) 0.0204(5) Uani 1 1 d . A .
H3 H 0.6510 0.9727 0.8494 0.024 Uiso 1 1 calc R . .
C4 C 0.6449(3) 1.0032(2) 0.71800(19) 0.0206(6) Uani 1 1 d . . .
C5 C 0.6662(3) 0.9480(2) 0.64429(18) 0.0199(6) Uani 1 1 d . A .
H5 H 0.6561 0.9917 0.5889 0.024 Uiso 1 1 calc R . .
C6 C 0.7017(2) 0.8317(2) 0.64697(18) 0.0180(5) Uani 1 1 d . . .
C7 C 0.6093(3) 1.1303(2) 0.7114(2) 0.0262(6) Uani 1 1 d . A .
H7 H 0.5837 1.1599 0.6503 0.031 Uiso 1 1 calc R . .
C8 C 0.7264(3) 1.1695(3) 0.7271(3) 0.0373(8) Uani 1 1 d . . .
H8A H 0.7536 1.1423 0.7867 0.056 Uiso 1 1 calc R A .
H8B H 0.7028 1.2515 0.7190 0.056 Uiso 1 1 calc R . .
H8C H 0.7985 1.1401 0.6856 0.056 Uiso 1 1 calc R . .
C9 C 0.4929(3) 1.1785(2) 0.7723(2) 0.0287(6) Uani 1 1 d . . .
H9A H 0.5170 1.1556 0.8330 0.043 Uiso 1 1 calc R A .
H9B H 0.4192 1.1504 0.7619 0.043 Uiso 1 1 calc R . .
H9C H 0.4676 1.2604 0.7610 0.043 Uiso 1 1 calc R . .
C10 C 0.7039(3) 0.7577(2) 0.89803(18) 0.0180(5) Uani 1 1 d . A .
H10 H 0.7523 0.6780 0.8919 0.022 Uiso 1 1 calc R . .
C11 C 0.7871(3) 0.8018(2) 0.95392(18) 0.0186(5) Uani 1 1 d . . .
C12 C 0.9093(3) 0.8120(3) 0.9200(2) 0.0276(6) Uani 1 1 d . A .
H12 H 0.9380 0.7940 0.8627 0.033 Uiso 1 1 calc R . .
C13 C 0.9898(3) 0.8482(3) 0.9689(2) 0.0326(7) Uani 1 1 d . . .
H13 H 1.0725 0.8547 0.9446 0.039 Uiso 1 1 calc R A .
C14 C 0.9502(3) 0.8745(2) 1.0521(2) 0.0296(7) Uani 1 1 d . A .
H14 H 1.0053 0.8988 1.0856 0.035 Uiso 1 1 calc R . .
C15 C 0.8294(3) 0.8650(2) 1.0865(2) 0.0272(6) Uani 1 1 d . . .
H15 H 0.8010 0.8834 1.1438 0.033 Uiso 1 1 calc R A .
C16 C 0.7491(3) 0.8287(2) 1.03753(19) 0.0231(6) Uani 1 1 d . A .
H16 H 0.6665 0.8223 1.0622 0.028 Uiso 1 1 calc R . .
C17 C 0.5732(3) 0.7556(2) 0.94570(18) 0.0193(5) Uani 1 1 d . . .
C18 C 0.5667(3) 0.6596(2) 1.0013(2) 0.0238(6) Uani 1 1 d . A .
H18 H 0.6410 0.5963 1.0049 0.029 Uiso 1 1 calc R . .
C19 C 0.4533(3) 0.6547(3) 1.0517(2) 0.0294(7) Uani 1 1 d . . .
H19 H 0.4507 0.5886 1.0889 0.035 Uiso 1 1 calc R A .
C20 C 0.3445(3) 0.7466(3) 1.0472(2) 0.0291(7) Uani 1 1 d . A .
H20 H 0.2667 0.7434 1.0810 0.035 Uiso 1 1 calc R . .
C21 C 0.3496(3) 0.8430(3) 0.9935(2) 0.0278(6) Uani 1 1 d . . .
H21 H 0.2755 0.9065 0.9911 0.033 Uiso 1 1 calc R A .
C22 C 0.4632(3) 0.8475(2) 0.9426(2) 0.0239(6) Uani 1 1 d . A .
H22 H 0.4654 0.9139 0.9056 0.029 Uiso 1 1 calc R . .
C23 C 0.7183(3) 0.7793(2) 0.56251(19) 0.0197(5) Uani 1 1 d . A .
H23 H 0.7857 0.7056 0.5721 0.024 Uiso 1 1 calc R . .
C24 C 0.5942(3) 0.7541(2) 0.54071(18) 0.0219(6) Uani 1 1 d . . .
C25 C 0.4705(3) 0.8227(3) 0.5609(2) 0.0337(7) Uani 1 1 d . A .
H25 H 0.4624 0.8848 0.5920 0.040 Uiso 1 1 calc R . .
C26 C 0.3575(4) 0.8009(5) 0.5358(3) 0.0559(13) Uani 1 1 d . . .
H26 H 0.2742 0.8492 0.5497 0.067 Uiso 1 1 calc R A .
C27 C 0.3648(5) 0.7132(4) 0.4925(3) 0.0543(12) Uani 1 1 d . A .
H27 H 0.2875 0.6989 0.4766 0.065 Uiso 1 1 calc R . .
C28 C 0.4860(7) 0.6444(3) 0.4715(3) 0.0702(19) Uani 1 1 d . . .
H28 H 0.4919 0.5820 0.4412 0.084 Uiso 1 1 calc R A .
C29 C 0.6002(4) 0.6648(3) 0.4941(3) 0.0458(10) Uani 1 1 d . A .
H29 H 0.6828 0.6174 0.4777 0.055 Uiso 1 1 calc R . .
C30 C 0.7718(3) 0.8484(2) 0.48543(19) 0.0207(6) Uani 1 1 d . . .
C31 C 0.7039(3) 0.8915(2) 0.4099(2) 0.0246(6) Uani 1 1 d . A .
H31 H 0.6216 0.8784 0.4045 0.029 Uiso 1 1 calc R . .
C32 C 0.7561(3) 0.9542(3) 0.3419(2) 0.0315(7) Uani 1 1 d . . .
H32 H 0.7084 0.9839 0.2910 0.038 Uiso 1 1 calc R A .
C33 C 0.8758(4) 0.9731(3) 0.3481(2) 0.0329(7) Uani 1 1 d . A .
H33 H 0.9108 1.0156 0.3018 0.039 Uiso 1 1 calc R . .
C34 C 0.9446(3) 0.9297(3) 0.4226(2) 0.0297(7) Uani 1 1 d . . .
H34 H 1.0278 0.9416 0.4271 0.036 Uiso 1 1 calc R A .
C35 C 0.8925(3) 0.8686(2) 0.4911(2) 0.0250(6) Uani 1 1 d . A .
H35 H 0.9399 0.8404 0.5423 0.030 Uiso 1 1 calc R . .
C36 C 0.9573(3) 0.5165(2) 0.85453(19) 0.0206(5) Uani 1 1 d . . .
H36 H 0.9355 0.5884 0.8811 0.025 Uiso 1 1 calc R A .
C37 C 1.1031(3) 0.4589(3) 0.8694(2) 0.0297(7) Uani 1 1 d . A .
H37A H 1.1140 0.4306 0.9312 0.045 Uiso 1 1 calc R . .
H37B H 1.1540 0.5130 0.8523 0.045 Uiso 1 1 calc R . .
H37C H 1.1339 0.3964 0.8340 0.045 Uiso 1 1 calc R . .
C38 C 0.8723(3) 0.4460(3) 0.9053(2) 0.0275(6) Uani 1 1 d . A .
H38A H 0.9001 0.3701 0.8880 0.041 Uiso 1 1 calc R . .
H38B H 0.7804 0.4804 0.8923 0.041 Uiso 1 1 calc R . .
H38C H 0.8823 0.4425 0.9680 0.041 Uiso 1 1 calc R . .
C39 C 1.0266(3) 0.6227(2) 0.66680(19) 0.0228(6) Uani 1 1 d . . .
H39 H 0.9863 0.6509 0.6093 0.027 Uiso 1 1 calc R A .
C40 C 1.1607(3) 0.5402(3) 0.6473(2) 0.0328(7) Uani 1 1 d . A .
H40A H 1.2157 0.5801 0.6098 0.049 Uiso 1 1 calc R . .
H40B H 1.1482 0.4800 0.6176 0.049 Uiso 1 1 calc R . .
H40C H 1.2033 0.5083 0.7021 0.049 Uiso 1 1 calc R . .
C41 C 1.0481(3) 0.7242(2) 0.7017(2) 0.0257(6) Uani 1 1 d . A .
H41A H 1.0898 0.7006 0.7577 0.039 Uiso 1 1 calc R . .
H41B H 0.9637 0.7795 0.7099 0.039 Uiso 1 1 calc R . .
H41C H 1.1046 0.7576 0.6599 0.039 Uiso 1 1 calc R . .
C42 C 0.9038(3) 0.4209(2) 0.6921(2) 0.0248(6) Uani 1 1 d . . .
H42 H 0.8230 0.4025 0.7194 0.030 Uiso 1 1 calc R A .
C43 C 0.8883(3) 0.4366(3) 0.5940(2) 0.0333(7) Uani 1 1 d . A .
H43A H 0.9643 0.4567 0.5638 0.050 Uiso 1 1 calc R . .
H43B H 0.8088 0.4965 0.5797 0.050 Uiso 1 1 calc R . .
H43C H 0.8816 0.3667 0.5755 0.050 Uiso 1 1 calc R . .
C44 C 1.0175(4) 0.3163(3) 0.7154(2) 0.0345(7) Uani 1 1 d . A .
H44A H 1.0065 0.2534 0.6882 0.052 Uiso 1 1 calc R . .
H44B H 1.0177 0.2973 0.7788 0.052 Uiso 1 1 calc R . .
H44C H 1.1005 0.3314 0.6938 0.052 Uiso 1 1 calc R . .
C45 C 0.4214(3) 0.7129(3) 0.7596(2) 0.0322(7) Uani 1 1 d . . .
H45A H 0.4520 0.7720 0.7805 0.039 Uiso 1 1 calc R A 1
H45B H 0.3626 0.7473 0.7114 0.039 Uiso 1 1 calc R A 1
C46 C 0.3499(3) 0.6565(3) 0.8340(2) 0.0388(8) Uani 1 1 d . A .
H46A H 0.3307 0.5918 0.8145 0.058 Uiso 1 1 calc R . .
H46B H 0.2680 0.7100 0.8509 0.058 Uiso 1 1 calc R . .
H46C H 0.4053 0.6316 0.8842 0.058 Uiso 1 1 calc R . .
Sn1A Sn 0.5567(4) 0.6394(4) 0.7581(4) 0.060(2) Uiso 0.0702(18) 1 d PD 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
Sn1 N1 2.123(2) . ?
Sn1 C45 2.182(3) . ?
Si1 N1 1.771(2) . ?
Si1 C39 1.905(3) . ?
Si1 C36 1.905(3) . ?
Si1 C42 1.909(3) . ?
N1 C1 1.436(3) . ?
N1 Sn1A 2.055(5) . ?
C1 C2 1.413(4) . ?
C1 C6 1.433(4) . ?
C2 C3 1.403(4) . ?
C2 C10 1.531(4) . ?
C3 C4 1.389(4) . ?
C4 C5 1.383(5) . ?
C4 C7 1.521(4) . ?
C5 C6 1.396(4) . ?
C6 C23 1.516(4) . ?
C7 C8 1.514(5) . ?
C7 C9 1.526(4) . ?
C10 C17 1.527(4) . ?
C10 C11 1.544(4) . ?
C11 C16 1.381(4) . ?
C11 C12 1.398(4) . ?
C12 C13 1.393(5) . ?
C13 C14 1.376(5) . ?
C14 C15 1.383(5) . ?
C15 C16 1.394(4) . ?
C17 C22 1.393(4) . ?
C17 C18 1.398(4) . ?
C18 C19 1.394(4) . ?
C19 C20 1.385(5) . ?
C20 C21 1.384(5) . ?
C21 C22 1.399(4) . ?
C23 C24 1.520(4) . ?
C23 C30 1.545(4) . ?
C24 C25 1.394(5) . ?
C24 C29 1.395(5) . ?
C25 C26 1.405(5) . ?
C26 C27 1.344(8) . ?
C27 C28 1.378(9) . ?
C28 C29 1.395(7) . ?
C30 C35 1.393(4) . ?
C30 C31 1.393(4) . ?
C31 C32 1.400(4) . ?
C32 C33 1.377(5) . ?
C33 C34 1.386(5) . ?
C34 C35 1.393(4) . ?
C36 C38 1.538(4) . ?
C36 C37 1.542(4) . ?
C39 C41 1.528(4) . ?
C39 C40 1.545(4) . ?
C42 C43 1.524(4) . ?
C42 C44 1.540(4) . ?
C45 C46 1.531(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 Sn1 C45 101.74(11) . . ?
N1 Si1 C39 110.37(11) . . ?
N1 Si1 C36 109.81(12) . . ?
C39 Si1 C36 111.55(13) . . ?
N1 Si1 C42 106.71(13) . . ?
C39 Si1 C42 110.17(14) . . ?
C36 Si1 C42 108.08(13) . . ?
C1 N1 Si1 123.83(17) . . ?
C1 N1 Sn1A 94.6(2) . . ?
Si1 N1 Sn1A 139.99(19) . . ?
C1 N1 Sn1 115.33(16) . . ?
Si1 N1 Sn1 120.39(12) . . ?
Sn1A N1 Sn1 28.00(17) . . ?
C2 C1 C6 118.0(2) . . ?
C2 C1 N1 122.8(2) . . ?
C6 C1 N1 119.1(2) . . ?
C3 C2 C1 119.7(2) . . ?
C3 C2 C10 117.2(3) . . ?
C1 C2 C10 123.1(2) . . ?
C4 C3 C2 122.8(3) . . ?
C5 C4 C3 116.9(3) . . ?
C5 C4 C7 121.3(3) . . ?
C3 C4 C7 121.7(3) . . ?
C4 C5 C6 123.4(3) . . ?
C5 C6 C1 119.1(3) . . ?
C5 C6 C23 119.4(2) . . ?
C1 C6 C23 121.5(2) . . ?
C8 C7 C4 110.8(3) . . ?
C8 C7 C9 111.0(3) . . ?
C4 C7 C9 112.5(2) . . ?
C17 C10 C2 114.9(2) . . ?
C17 C10 C11 110.7(2) . . ?
C2 C10 C11 111.3(2) . . ?
C16 C11 C12 117.7(3) . . ?
C16 C11 C10 123.4(2) . . ?
C12 C11 C10 118.9(3) . . ?
C13 C12 C11 121.1(3) . . ?
C14 C13 C12 120.3(3) . . ?
C13 C14 C15 119.2(3) . . ?
C14 C15 C16 120.3(3) . . ?
C11 C16 C15 121.3(3) . . ?
C22 C17 C18 118.1(3) . . ?
C22 C17 C10 123.5(2) . . ?
C18 C17 C10 118.2(2) . . ?
C19 C18 C17 121.3(3) . . ?
C20 C19 C18 119.8(3) . . ?
C21 C20 C19 119.7(3) . . ?
C20 C21 C22 120.4(3) . . ?
C17 C22 C21 120.6(3) . . ?
C6 C23 C24 112.3(2) . . ?
C6 C23 C30 112.7(2) . . ?
C24 C23 C30 111.8(2) . . ?
C25 C24 C29 117.2(3) . . ?
C25 C24 C23 121.9(3) . . ?
C29 C24 C23 120.8(3) . . ?
C24 C25 C26 120.7(4) . . ?
C27 C26 C25 121.4(4) . . ?
C26 C27 C28 118.9(4) . . ?
C27 C28 C29 121.1(4) . . ?
C28 C29 C24 120.6(4) . . ?
C35 C30 C31 118.4(3) . . ?
C35 C30 C23 119.1(3) . . ?
C31 C30 C23 122.5(3) . . ?
C30 C31 C32 120.4(3) . . ?
C33 C32 C31 120.6(3) . . ?
C32 C33 C34 119.4(3) . . ?
C33 C34 C35 120.3(3) . . ?
C30 C35 C34 120.8(3) . . ?
C38 C36 C37 110.0(2) . . ?
C38 C36 Si1 109.9(2) . . ?
C37 C36 Si1 116.9(2) . . ?
C41 C39 C40 109.1(2) . . ?
C41 C39 Si1 114.7(2) . . ?
C40 C39 Si1 113.7(2) . . ?
C43 C42 C44 109.0(3) . . ?
C43 C42 Si1 113.1(2) . . ?
C44 C42 Si1 116.4(2) . . ?
C46 C45 Sn1 106.4(2) . . ?

_diffrn_measured_fraction_theta_max 0.870
_diffrn_reflns_theta_full        25.20
_diffrn_measured_fraction_theta_full 0.870
_refine_diff_density_max         0.810
_refine_diff_density_min         -0.717
_refine_diff_density_rms         0.082
####################################################################### 
# 
# 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_compound13
_database_code_depnum_ccdc_archive 'CCDC 1422733'
_audit_update_record             
;
2015-09-07 deposited with the CCDC.
2015-09-22 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C52 H68 N Si Sn'
_chemical_formula_weight         853.85

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'

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   P-1

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   10.2591(9)
_cell_length_b                   13.6505(10)
_cell_length_c                   17.3164(15)
_cell_angle_alpha                99.111(7)
_cell_angle_beta                 105.293(8)
_cell_angle_gamma                95.189(7)
_cell_volume                     2287.3(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    123(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.05
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.240
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             902
_exptl_absorpt_coefficient_mu    0.619
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.742
_exptl_absorpt_correction_T_max  0.967
_exptl_absorpt_process_details   'SCALE3 ABSPACK'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      123(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Oxford Gemini Ultra'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            17097
_diffrn_reflns_av_R_equivalents  0.0927
_diffrn_reflns_av_sigmaI/netI    0.1692
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         3.05
_diffrn_reflns_theta_max         26.00
_reflns_number_total             8971
_reflns_number_gt                5584
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       CrysalisPro
_computing_cell_refinement       CrysalisPro
_computing_data_reduction        CrysalisPro
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    X-Seed
_computing_publication_material  CifTAB

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger.
 A half molecule of hexane, sitting on a crystallographic centre of inversion,
 was refined in the asymmetric unit with its carbon atoms set as anisotropic. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0191P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         8971
_refine_ls_number_parameters     505
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1164
_refine_ls_R_factor_gt           0.0668
_refine_ls_wR_factor_ref         0.1259
_refine_ls_wR_factor_gt          0.1044
_refine_ls_goodness_of_fit_ref   0.963
_refine_ls_restrained_S_all      0.963
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Sn1 Sn 0.82725(4) 0.87366(3) 0.73178(2) 0.02877(13) Uani 1 1 d . . .
Si1 Si 0.50814(16) 0.94839(9) 0.74034(8) 0.0194(3) Uani 1 1 d . . .
N1 N 0.6167(4) 0.8579(3) 0.7263(2) 0.0165(9) Uani 1 1 d . . .
C3 C 0.4149(5) 0.6087(3) 0.6188(3) 0.0164(11) Uani 1 1 d . . .
H3 H 0.3671 0.5760 0.5647 0.020 Uiso 1 1 calc R . .
C1 C 0.5561(5) 0.7544(3) 0.7107(3) 0.0164(11) Uani 1 1 d . . .
C2 C 0.4892(5) 0.7032(3) 0.6301(3) 0.0178(12) Uani 1 1 d . . .
C44 C 0.5608(6) 1.0331(4) 0.6090(3) 0.0303(14) Uani 1 1 d . . .
H44A H 0.4661 1.0103 0.5762 0.045 Uiso 1 1 calc R . .
H44B H 0.6163 0.9795 0.6016 0.045 Uiso 1 1 calc R . .
H44C H 0.5966 1.0922 0.5914 0.045 Uiso 1 1 calc R . .
C10 C 0.5085(5) 0.7451(4) 0.5567(3) 0.0201(12) Uani 1 1 d . . .
H10 H 0.5070 0.8189 0.5700 0.024 Uiso 1 1 calc R . .
C23 C 0.6555(5) 0.7467(3) 0.8596(3) 0.0195(12) Uani 1 1 d . . .
H23 H 0.6484 0.8200 0.8688 0.023 Uiso 1 1 calc R . .
C17 C 0.3932(6) 0.7055(3) 0.4781(3) 0.0186(12) Uani 1 1 d . . .
C4 C 0.4072(5) 0.5603(3) 0.6818(3) 0.0189(12) Uani 1 1 d . . .
C16 C 0.7180(6) 0.6539(4) 0.5705(3) 0.0238(13) Uani 1 1 d . . .
H16 H 0.6756 0.6061 0.5938 0.029 Uiso 1 1 calc R . .
C11 C 0.6498(6) 0.7319(4) 0.5460(3) 0.0217(12) Uani 1 1 d . . .
C6 C 0.5604(5) 0.7026(3) 0.7745(3) 0.0163(11) Uani 1 1 d . . .
C24 C 0.6119(6) 0.7067(3) 0.9278(3) 0.0208(12) Uani 1 1 d . . .
C7 C 0.3085(6) 0.4651(3) 0.6665(3) 0.0247(13) Uani 1 1 d . . .
H7 H 0.3073 0.4262 0.6122 0.030 Uiso 1 1 calc R . .
C36 C 0.5178(6) 0.9861(3) 0.8531(3) 0.0219(12) Uani 1 1 d . . .
H36 H 0.4985 0.9217 0.8713 0.026 Uiso 1 1 calc R . .
C38 C 0.4084(6) 1.0489(4) 0.8706(3) 0.0346(15) Uani 1 1 d . . .
H38A H 0.4078 1.0519 0.9274 0.052 Uiso 1 1 calc R . .
H38B H 0.3187 1.0179 0.8342 0.052 Uiso 1 1 calc R . .
H38C H 0.4288 1.1168 0.8612 0.052 Uiso 1 1 calc R . .
C42 C 0.5659(6) 1.0605(3) 0.6997(3) 0.0253(13) Uani 1 1 d . . .
H42 H 0.6648 1.0802 0.7297 0.030 Uiso 1 1 calc R . .
C5 C 0.4870(5) 0.6080(3) 0.7602(3) 0.0195(12) Uani 1 1 d . . .
H5 H 0.4908 0.5744 0.8046 0.023 Uiso 1 1 calc R . .
C39 C 0.3266(5) 0.8898(3) 0.6832(3) 0.0224(12) Uani 1 1 d . . .
H39 H 0.3346 0.8438 0.6341 0.027 Uiso 1 1 calc R . .
C12 C 0.7129(6) 0.7988(4) 0.5098(3) 0.0281(14) Uani 1 1 d . . .
H12 H 0.6668 0.8512 0.4905 0.034 Uiso 1 1 calc R . .
C30 C 0.8040(6) 0.7386(4) 0.8621(3) 0.0210(12) Uani 1 1 d . . .
C40 C 0.2274(6) 0.9603(4) 0.6489(3) 0.0382(15) Uani 1 1 d . . .
H40A H 0.1370 0.9219 0.6218 0.057 Uiso 1 1 calc R . .
H40B H 0.2606 0.9922 0.6095 0.057 Uiso 1 1 calc R . .
H40C H 0.2211 1.0120 0.6936 0.057 Uiso 1 1 calc R . .
C22 C 0.2721(6) 0.7453(4) 0.4638(3) 0.0247(13) Uani 1 1 d . . .
H22 H 0.2610 0.7986 0.5030 0.030 Uiso 1 1 calc R . .
C41 C 0.2573(6) 0.8213(4) 0.7287(3) 0.0291(13) Uani 1 1 d . . .
H41A H 0.2449 0.8618 0.7776 0.044 Uiso 1 1 calc R . .
H41B H 0.3150 0.7702 0.7445 0.044 Uiso 1 1 calc R . .
H41C H 0.1682 0.7885 0.6927 0.044 Uiso 1 1 calc R . .
C45 C 0.8970(6) 1.0295(4) 0.7888(3) 0.0306(14) Uani 1 1 d . . .
H45 H 0.8244 1.0599 0.8093 0.037 Uiso 1 1 calc R . .
C20 C 0.1808(6) 0.6327(4) 0.3355(3) 0.0295(14) Uani 1 1 d . . .
H20 H 0.1088 0.6079 0.2870 0.035 Uiso 1 1 calc R . .
C18 C 0.4081(6) 0.6283(4) 0.4191(3) 0.0264(13) Uani 1 1 d . . .
H18 H 0.4908 0.6001 0.4269 0.032 Uiso 1 1 calc R . .
C19 C 0.3013(7) 0.5931(4) 0.3493(3) 0.0354(15) Uani 1 1 d . . .
H19 H 0.3117 0.5400 0.3097 0.042 Uiso 1 1 calc R . .
C13 C 0.8423(7) 0.7898(4) 0.5016(3) 0.0398(16) Uani 1 1 d . . .
H13 H 0.8850 0.8372 0.4781 0.048 Uiso 1 1 calc R . .
C21 C 0.1666(6) 0.7092(4) 0.3935(3) 0.0308(14) Uani 1 1 d . . .
H21 H 0.0838 0.7373 0.3852 0.037 Uiso 1 1 calc R . .
C27 C 0.5228(7) 0.6364(4) 1.0499(3) 0.0357(16) Uani 1 1 d . . .
H27 H 0.4932 0.6123 1.0919 0.043 Uiso 1 1 calc R . .
C35 C 0.9091(7) 0.8101(4) 0.9122(3) 0.0341(15) Uani 1 1 d . . .
H35 H 0.8884 0.8642 0.9467 0.041 Uiso 1 1 calc R . .
C15 C 0.8469(6) 0.6443(4) 0.5616(3) 0.0355(15) Uani 1 1 d . . .
H15 H 0.8919 0.5906 0.5792 0.043 Uiso 1 1 calc R . .
C26 C 0.4432(6) 0.6934(4) 1.0021(3) 0.0307(14) Uani 1 1 d . . .
H26 H 0.3589 0.7087 1.0105 0.037 Uiso 1 1 calc R . .
C43 C 0.4990(6) 1.1552(4) 0.7151(3) 0.0371(15) Uani 1 1 d . . .
H43A H 0.5399 1.2087 0.6936 0.056 Uiso 1 1 calc R . .
H43B H 0.5135 1.1767 0.7738 0.056 Uiso 1 1 calc R . .
H43C H 0.4009 1.1405 0.6876 0.056 Uiso 1 1 calc R . .
C9 C 0.3491(7) 0.3973(4) 0.7279(3) 0.0453(19) Uani 1 1 d . . .
H9A H 0.4411 0.3812 0.7300 0.068 Uiso 1 1 calc R . .
H9B H 0.2844 0.3353 0.7113 0.068 Uiso 1 1 calc R . .
H9C H 0.3481 0.4315 0.7818 0.068 Uiso 1 1 calc R . .
C37 C 0.6582(6) 1.0333(4) 0.9079(3) 0.0313(14) Uani 1 1 d . . .
H37A H 0.6805 1.0998 0.8963 0.047 Uiso 1 1 calc R . .
H37B H 0.7262 0.9909 0.8976 0.047 Uiso 1 1 calc R . .
H37C H 0.6583 1.0397 0.9651 0.047 Uiso 1 1 calc R . .
C31 C 0.8403(6) 0.6591(4) 0.8146(3) 0.0292(13) Uani 1 1 d . . .
H31 H 0.7711 0.6080 0.7801 0.035 Uiso 1 1 calc R . .
C25 C 0.4903(6) 0.7277(4) 0.9415(3) 0.0263(13) Uani 1 1 d . . .
H25 H 0.4366 0.7669 0.9085 0.032 Uiso 1 1 calc R . .
C14 C 0.9099(6) 0.7121(4) 0.5275(3) 0.0344(14) Uani 1 1 d . . .
H14 H 0.9985 0.7059 0.5217 0.041 Uiso 1 1 calc R . .
C29 C 0.6871(6) 0.6495(4) 0.9765(3) 0.0316(14) Uani 1 1 d . . .
H29 H 0.7713 0.6335 0.9683 0.038 Uiso 1 1 calc R . .
C32 C 0.9746(7) 0.6535(4) 0.8167(3) 0.0368(15) Uani 1 1 d . . .
H32 H 0.9967 0.5986 0.7837 0.044 Uiso 1 1 calc R . .
C46 C 1.0336(7) 1.0478(5) 0.8575(4) 0.0552(19) Uani 1 1 d . . .
H46A H 1.0162 1.0367 0.9092 0.066 Uiso 1 1 calc R . .
H46B H 1.0946 1.0001 0.8434 0.066 Uiso 1 1 calc R . .
C28 C 0.6425(7) 0.6148(4) 1.0370(3) 0.0390(16) Uani 1 1 d . . .
H28 H 0.6963 0.5755 1.0700 0.047 Uiso 1 1 calc R . .
C33 C 1.0768(7) 0.7261(5) 0.8659(4) 0.0429(17) Uani 1 1 d . . .
H33 H 1.1692 0.7221 0.8671 0.051 Uiso 1 1 calc R . .
C8 C 0.1658(7) 0.4902(4) 0.6588(4) 0.0532(19) Uani 1 1 d . . .
H8A H 0.1620 0.5280 0.7111 0.080 Uiso 1 1 calc R . .
H8B H 0.1013 0.4282 0.6439 0.080 Uiso 1 1 calc R . .
H8C H 0.1415 0.5308 0.6166 0.080 Uiso 1 1 calc R . .
C34 C 1.0433(7) 0.8046(4) 0.9133(4) 0.0435(17) Uani 1 1 d . . .
H34 H 1.1131 0.8557 0.9472 0.052 Uiso 1 1 calc R . .
C49 C 0.9450(8) 1.0933(5) 0.7306(4) 0.061(2) Uani 1 1 d . . .
H49A H 0.9710 1.0485 0.6881 0.074 Uiso 1 1 calc R . .
H49B H 0.8686 1.1265 0.7033 0.074 Uiso 1 1 calc R . .
C48 C 1.0617(8) 1.1695(5) 0.7763(4) 0.057(2) Uani 1 1 d . . .
H48A H 1.0370 1.2376 0.7742 0.068 Uiso 1 1 calc R . .
H48B H 1.1398 1.1619 0.7534 0.068 Uiso 1 1 calc R . .
C47 C 1.0991(8) 1.1508(5) 0.8675(4) 0.069(2) Uani 1 1 d . . .
H47A H 1.1991 1.1568 0.8913 0.083 Uiso 1 1 calc R . .
H47B H 1.0615 1.1984 0.9025 0.083 Uiso 1 1 calc R . .
C51 C 0.0770(7) 0.5948(4) 0.1033(3) 0.0361(16) Uani 1 1 d . . .
H51A H 0.1005 0.5441 0.1378 0.043 Uiso 1 1 calc R . .
H51B H -0.0089 0.6173 0.1104 0.043 Uiso 1 1 calc R . .
C50 C 0.1895(6) 0.6835(4) 0.1325(3) 0.0380(16) Uani 1 1 d . . .
H50A H 0.2763 0.6610 0.1293 0.057 Uiso 1 1 calc R . .
H50B H 0.1968 0.7133 0.1891 0.057 Uiso 1 1 calc R . .
H50C H 0.1680 0.7336 0.0980 0.057 Uiso 1 1 calc R . .
C52 C 0.0534(6) 0.5463(3) 0.0151(3) 0.0312(14) Uani 1 1 d . . .
H52A H 0.1410 0.5277 0.0076 0.037 Uiso 1 1 calc R . .
H52B H 0.0254 0.5964 -0.0193 0.037 Uiso 1 1 calc R . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Sn1 N1 2.127(4) . ?
Sn1 C45 2.168(5) . ?
Si1 N1 1.767(4) . ?
Si1 C42 1.894(5) . ?
Si1 C39 1.896(6) . ?
Si1 C36 1.912(4) . ?
N1 C1 1.445(5) . ?
C3 C4 1.378(6) . ?
C3 C2 1.394(6) . ?
C1 C6 1.397(6) . ?
C1 C2 1.416(6) . ?
C2 C10 1.526(6) . ?
C44 C42 1.542(6) . ?
C10 C17 1.531(7) . ?
C10 C11 1.532(7) . ?
C23 C24 1.527(6) . ?
C23 C30 1.527(7) . ?
C23 C6 1.529(6) . ?
C17 C22 1.379(7) . ?
C17 C18 1.395(6) . ?
C4 C5 1.405(7) . ?
C4 C7 1.516(6) . ?
C16 C15 1.386(7) . ?
C16 C11 1.388(7) . ?
C11 C12 1.390(6) . ?
C6 C5 1.385(6) . ?
C24 C29 1.376(7) . ?
C24 C25 1.377(7) . ?
C7 C8 1.511(8) . ?
C7 C9 1.519(6) . ?
C36 C37 1.519(7) . ?
C36 C38 1.536(7) . ?
C42 C43 1.536(7) . ?
C39 C40 1.534(7) . ?
C39 C41 1.553(6) . ?
C12 C13 1.386(8) . ?
C30 C35 1.384(7) . ?
C30 C31 1.394(7) . ?
C22 C21 1.384(7) . ?
C45 C46 1.550(9) . ?
C45 C49 1.574(7) . ?
C20 C19 1.373(8) . ?
C20 C21 1.375(7) . ?
C18 C19 1.384(7) . ?
C13 C14 1.387(8) . ?
C27 C28 1.354(8) . ?
C27 C26 1.386(7) . ?
C35 C34 1.381(8) . ?
C15 C14 1.375(7) . ?
C26 C25 1.390(6) . ?
C31 C32 1.379(8) . ?
C29 C28 1.380(7) . ?
C32 C33 1.372(8) . ?
C46 C47 1.466(8) . ?
C33 C34 1.369(8) . ?
C49 C48 1.467(9) . ?
C48 C47 1.592(8) . ?
C51 C52 1.511(7) . ?
C51 C50 1.516(7) . ?
C52 C52 1.521(10) 2_565 ?

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 C45 102.78(18) . . ?
N1 Si1 C42 107.1(2) . . ?
N1 Si1 C39 107.8(2) . . ?
C42 Si1 C39 112.4(2) . . ?
N1 Si1 C36 110.9(2) . . ?
C42 Si1 C36 110.6(2) . . ?
C39 Si1 C36 108.0(2) . . ?
C1 N1 Si1 116.2(3) . . ?
C1 N1 Sn1 112.6(3) . . ?
Si1 N1 Sn1 131.17(19) . . ?
C4 C3 C2 123.5(4) . . ?
C6 C1 C2 118.2(4) . . ?
C6 C1 N1 121.1(4) . . ?
C2 C1 N1 120.7(4) . . ?
C3 C2 C1 118.7(4) . . ?
C3 C2 C10 120.0(4) . . ?
C1 C2 C10 121.1(4) . . ?
C2 C10 C17 114.0(4) . . ?
C2 C10 C11 110.6(4) . . ?
C17 C10 C11 112.7(4) . . ?
C24 C23 C30 113.8(4) . . ?
C24 C23 C6 113.5(4) . . ?
C30 C23 C6 110.8(4) . . ?
C22 C17 C18 118.3(5) . . ?
C22 C17 C10 120.8(4) . . ?
C18 C17 C10 120.8(5) . . ?
C3 C4 C5 116.5(4) . . ?
C3 C4 C7 120.6(4) . . ?
C5 C4 C7 122.8(4) . . ?
C15 C16 C11 121.2(5) . . ?
C16 C11 C12 118.0(5) . . ?
C16 C11 C10 122.2(4) . . ?
C12 C11 C10 119.9(5) . . ?
C5 C6 C1 120.6(4) . . ?
C5 C6 C23 119.5(4) . . ?
C1 C6 C23 119.8(4) . . ?
C29 C24 C25 117.5(4) . . ?
C29 C24 C23 123.6(5) . . ?
C25 C24 C23 118.9(5) . . ?
C8 C7 C4 109.9(4) . . ?
C8 C7 C9 111.9(4) . . ?
C4 C7 C9 114.6(5) . . ?
C37 C36 C38 110.5(4) . . ?
C37 C36 Si1 114.7(3) . . ?
C38 C36 Si1 115.1(3) . . ?
C43 C42 C44 110.4(4) . . ?
C43 C42 Si1 117.0(4) . . ?
C44 C42 Si1 112.2(3) . . ?
C6 C5 C4 121.8(4) . . ?
C40 C39 C41 109.0(5) . . ?
C40 C39 Si1 117.0(3) . . ?
C41 C39 Si1 114.9(3) . . ?
C13 C12 C11 120.8(5) . . ?
C35 C30 C31 116.9(5) . . ?
C35 C30 C23 121.2(5) . . ?
C31 C30 C23 121.9(5) . . ?
C17 C22 C21 121.3(5) . . ?
C46 C45 C49 97.5(5) . . ?
C46 C45 Sn1 114.5(4) . . ?
C49 C45 Sn1 112.8(3) . . ?
C19 C20 C21 118.5(5) . . ?
C19 C18 C17 119.5(5) . . ?
C20 C19 C18 121.9(5) . . ?
C12 C13 C14 120.5(5) . . ?
C20 C21 C22 120.4(6) . . ?
C28 C27 C26 120.2(5) . . ?
C34 C35 C30 121.5(6) . . ?
C14 C15 C16 120.4(5) . . ?
C27 C26 C25 118.2(5) . . ?
C32 C31 C30 121.2(5) . . ?
C24 C25 C26 122.3(5) . . ?
C15 C14 C13 119.1(6) . . ?
C24 C29 C28 121.2(6) . . ?
C33 C32 C31 120.8(6) . . ?
C47 C46 C45 109.5(5) . . ?
C27 C28 C29 120.6(5) . . ?
C34 C33 C32 118.9(6) . . ?
C33 C34 C35 120.6(6) . . ?
C48 C49 C45 111.1(5) . . ?
C49 C48 C47 105.6(5) . . ?
C46 C47 C48 102.4(6) . . ?
C52 C51 C50 113.5(4) . . ?
C51 C52 C52 115.0(5) . 2_565 ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        26.00
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         1.098
_refine_diff_density_min         -1.005
_refine_diff_density_rms         0.112
####################################################################### 
# 
# 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_compound14
_database_code_depnum_ccdc_archive 'CCDC 1422734'
_audit_update_record             
;
2015-09-07 deposited with the CCDC.
2015-09-22 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C53 H61 Ge N Si'
_chemical_formula_weight         812.71

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

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   P2(1)/n

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

_cell_length_a                   10.0813(17)
_cell_length_b                   15.796(3)
_cell_length_c                   28.096(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 96.916(13)
_cell_angle_gamma                90.00
_cell_volume                     4441.7(13)
_cell_formula_units_Z            4
_cell_measurement_temperature    123(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.215
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1728
_exptl_absorpt_coefficient_mu    0.753
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.861
_exptl_absorpt_correction_T_max  0.891
_exptl_absorpt_process_details   'SCALE3 ABSPACK'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      123(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Oxford Gemini Ultra'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            21378
_diffrn_reflns_av_R_equivalents  0.1932
_diffrn_reflns_av_sigmaI/netI    0.3249
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         2.92
_diffrn_reflns_theta_max         25.50
_reflns_number_total             8251
_reflns_number_gt                2654
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       CrysalisPro
_computing_cell_refinement       CrysalisPro
_computing_data_reduction        CrysalisPro
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    X-Seed
_computing_publication_material  CifTAB

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger.
 The carbon atoms of the SiPri3 substituent were found to be disordered over
 two sites. This disorder was modelled and the carbon atoms of the minor disordered
 set refined isotropically.
 The high r-factors for the structure are due to weak reflection data above theta
 angles of 23 deg.  
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0938P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         8251
_refine_ls_number_parameters     551
_refine_ls_number_restraints     18
_refine_ls_R_factor_all          0.2768
_refine_ls_R_factor_gt           0.0925
_refine_ls_wR_factor_ref         0.2723
_refine_ls_wR_factor_gt          0.1923
_refine_ls_goodness_of_fit_ref   0.914
_refine_ls_restrained_S_all      0.920
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ge1 Ge 0.96730(8) 0.80583(7) 0.83251(3) 0.0512(4) Uani 1 1 d . . .
Si1 Si 0.6256(2) 0.79624(16) 0.81221(7) 0.0424(7) Uani 1 1 d D . .
N1 N 0.7900(5) 0.7989(4) 0.8468(2) 0.0364(17) Uani 1 1 d . A .
C1 C 0.7956(7) 0.7909(5) 0.8995(3) 0.039(2) Uani 1 1 d . . .
C16 C 1.1801(8) 0.9770(6) 0.9151(3) 0.051(2) Uani 1 1 d . A .
H16 H 1.2577 0.9571 0.9344 0.062 Uiso 1 1 calc R . .
C6 C 0.7943(7) 0.8656(5) 0.9283(3) 0.0329(19) Uani 1 1 d . A .
C20 C 0.8269(7) 0.6290(5) 0.8936(3) 0.040(2) Uani 1 1 d . . .
H20 H 0.7831 0.6397 0.8603 0.048 Uiso 1 1 calc R A .
C7 C 0.7988(7) 0.9535(5) 0.9063(3) 0.038(2) Uani 1 1 d . . .
H7 H 0.7419 0.9509 0.8746 0.046 Uiso 1 1 calc R A .
C2 C 0.8061(7) 0.7096(5) 0.9221(3) 0.043(2) Uani 1 1 d . A .
C19 C 0.9533(9) 1.0357(5) 0.8594(3) 0.045(2) Uani 1 1 d . . .
H19 H 0.8760 1.0570 0.8405 0.054 Uiso 1 1 calc R A .
C8 C 0.7374(7) 1.0222(5) 0.9356(3) 0.036(2) Uani 1 1 d . A .
C14 C 0.9391(7) 0.9775(5) 0.8956(3) 0.038(2) Uani 1 1 d . A .
C3 C 0.8134(7) 0.7055(5) 0.9721(3) 0.038(2) Uani 1 1 d . . .
H3 H 0.8219 0.6517 0.9873 0.046 Uiso 1 1 calc R A .
C4 C 0.8086(7) 0.7773(5) 1.0004(3) 0.034(2) Uani 1 1 d . A .
C35 C 0.6973(9) 0.7222(6) 1.0702(3) 0.066(3) Uani 1 1 d . A .
H35A H 0.6923 0.6651 1.0565 0.099 Uiso 1 1 calc R . .
H35B H 0.6157 0.7535 1.0587 0.099 Uiso 1 1 calc R . .
H35C H 0.7062 0.7186 1.1052 0.099 Uiso 1 1 calc R . .
C27 C 0.9750(7) 0.6118(5) 0.8890(3) 0.044(2) Uani 1 1 d . A .
C18 C 1.0785(9) 1.0631(6) 0.8503(3) 0.059(3) Uani 1 1 d . A .
H18 H 1.0869 1.1015 0.8249 0.071 Uiso 1 1 calc R . .
C15 C 1.0532(8) 0.9485(5) 0.9236(3) 0.045(2) Uani 1 1 d . . .
H15 H 1.0451 0.9091 0.9486 0.054 Uiso 1 1 calc R A .
C17 C 1.1914(8) 1.0342(6) 0.8786(3) 0.052(2) Uani 1 1 d . . .
H17 H 1.2772 1.0538 0.8728 0.062 Uiso 1 1 calc R A .
C5 C 0.8013(7) 0.8552(5) 0.9781(3) 0.038(2) Uani 1 1 d . . .
H5 H 0.8009 0.9044 0.9976 0.045 Uiso 1 1 calc R A .
C9 C 0.6008(8) 1.0169(6) 0.9416(3) 0.047(2) Uani 1 1 d . . .
H9 H 0.5495 0.9694 0.9295 0.056 Uiso 1 1 calc R A .
C33 C 0.8182(8) 0.7684(5) 1.0548(3) 0.047(2) Uani 1 1 d . . .
H33 H 0.8195 0.8267 1.0687 0.057 Uiso 1 1 calc R A .
C45 C 0.9702(8) 0.8271(7) 0.7628(3) 0.057(3) Uani 1 1 d . . .
C32 C 1.0085(9) 0.5760(6) 0.8482(3) 0.060(3) Uani 1 1 d . . .
H32 H 0.9406 0.5666 0.8222 0.072 Uiso 1 1 calc R A .
C13 C 0.8118(8) 1.0902(5) 0.9552(3) 0.040(2) Uani 1 1 d . . .
H13 H 0.9042 1.0940 0.9519 0.048 Uiso 1 1 calc R A .
C12 C 0.7496(9) 1.1537(6) 0.9801(3) 0.052(2) Uani 1 1 d . A .
H12 H 0.8009 1.1999 0.9939 0.062 Uiso 1 1 calc R . .
C39 C 0.5760(7) 0.6814(4) 0.7976(3) 0.049(3) Uani 0.836(7) 1 d PD A 1
H39 H 0.5904 0.6502 0.8288 0.059 Uiso 0.836(7) 1 calc PR A 1
C40 C 0.6682(13) 0.6391(9) 0.7651(5) 0.054(4) Uani 0.836(7) 1 d PD A 1
H40A H 0.6464 0.5788 0.7619 0.081 Uiso 0.836(7) 1 calc PR A 1
H40B H 0.7614 0.6457 0.7793 0.081 Uiso 0.836(7) 1 calc PR A 1
H40C H 0.6558 0.6659 0.7334 0.081 Uiso 0.836(7) 1 calc PR A 1
C28 C 1.0737(8) 0.6226(6) 0.9275(3) 0.074(3) Uani 1 1 d . . .
H28 H 1.0524 0.6453 0.9570 0.088 Uiso 1 1 calc R A .
C42 C 0.6470(9) 0.8493(6) 0.7536(2) 0.054(3) Uani 0.836(7) 1 d PD A 1
H42 H 0.7317 0.8259 0.7437 0.065 Uiso 0.836(7) 1 calc PR A 1
C10 C 0.5413(8) 1.0818(6) 0.9652(3) 0.052(2) Uani 1 1 d . A .
H10 H 0.4484 1.0792 0.9680 0.062 Uiso 1 1 calc R . .
C34 C 0.9454(8) 0.7246(6) 1.0754(3) 0.062(3) Uani 1 1 d . A .
H34A H 0.9591 0.7330 1.1102 0.093 Uiso 1 1 calc R . .
H34B H 1.0211 0.7485 1.0611 0.093 Uiso 1 1 calc R . .
H34C H 0.9385 0.6639 1.0683 0.093 Uiso 1 1 calc R . .
C41 C 0.4273(7) 0.6672(8) 0.7780(4) 0.055(3) Uani 0.836(7) 1 d PD A 1
H41A H 0.4048 0.7014 0.7490 0.082 Uiso 0.836(7) 1 calc PR A 1
H41B H 0.3706 0.6842 0.8023 0.082 Uiso 0.836(7) 1 calc PR A 1
H41C H 0.4126 0.6072 0.7702 0.082 Uiso 0.836(7) 1 calc PR A 1
C11 C 0.6149(9) 1.1493(6) 0.9845(3) 0.053(2) Uani 1 1 d . . .
H11 H 0.5733 1.1927 1.0008 0.063 Uiso 1 1 calc R A .
C43 C 0.6716(13) 0.9451(6) 0.7611(4) 0.054(3) Uani 0.836(7) 1 d PD A 1
H43A H 0.6941 0.9704 0.7312 0.081 Uiso 0.836(7) 1 calc PR A 1
H43B H 0.7457 0.9538 0.7865 0.081 Uiso 0.836(7) 1 calc PR A 1
H43C H 0.5907 0.9719 0.7702 0.081 Uiso 0.836(7) 1 calc PR A 1
C36 C 0.4947(7) 0.8464(6) 0.8452(3) 0.044(3) Uani 0.836(7) 1 d PD A 1
H36 H 0.5359 0.8997 0.8594 0.053 Uiso 0.836(7) 1 calc PR A 1
C44 C 0.5395(10) 0.8348(8) 0.7109(3) 0.062(4) Uani 0.836(7) 1 d PD A 1
H44A H 0.4546 0.8590 0.7180 0.093 Uiso 0.836(7) 1 calc PR A 1
H44B H 0.5286 0.7739 0.7050 0.093 Uiso 0.836(7) 1 calc PR A 1
H44C H 0.5668 0.8622 0.6823 0.093 Uiso 0.836(7) 1 calc PR A 1
C21 C 0.7534(8) 0.5524(6) 0.9122(3) 0.043(2) Uani 1 1 d . A .
C30 C 1.2397(10) 0.5660(8) 0.8808(4) 0.089(4) Uani 1 1 d . . .
H30 H 1.3299 0.5520 0.8777 0.107 Uiso 1 1 calc R A .
C22 C 0.8108(10) 0.4737(7) 0.9135(4) 0.079(3) Uani 1 1 d . . .
H22 H 0.8976 0.4673 0.9040 0.095 Uiso 1 1 calc R A .
C37 C 0.4545(14) 0.7954(8) 0.8876(3) 0.044(3) Uani 0.836(7) 1 d PD A 1
H37A H 0.3852 0.8262 0.9022 0.067 Uiso 0.836(7) 1 calc PR A 1
H37B H 0.5327 0.7874 0.9115 0.067 Uiso 0.836(7) 1 calc PR A 1
H37C H 0.4197 0.7402 0.8762 0.067 Uiso 0.836(7) 1 calc PR A 1
C29 C 1.2034(9) 0.5997(8) 0.9222(4) 0.097(5) Uani 1 1 d . A .
H29 H 1.2706 0.6078 0.9485 0.116 Uiso 1 1 calc R . .
C26 C 0.6238(8) 0.5583(6) 0.9248(3) 0.053(2) Uani 1 1 d . . .
H26 H 0.5808 0.6119 0.9233 0.064 Uiso 1 1 calc R A .
C38 C 0.3688(8) 0.8744(7) 0.8124(4) 0.056(3) Uani 0.836(7) 1 d PD A 1
H38A H 0.3225 0.8243 0.7980 0.084 Uiso 0.836(7) 1 calc PR A 1
H38B H 0.3946 0.9113 0.7871 0.084 Uiso 0.836(7) 1 calc PR A 1
H38C H 0.3090 0.9052 0.8314 0.084 Uiso 0.836(7) 1 calc PR A 1
C31 C 1.1369(10) 0.5533(7) 0.8433(3) 0.076(3) Uani 1 1 d . A .
H31 H 1.1567 0.5285 0.8142 0.091 Uiso 1 1 calc R . .
C25 C 0.5573(9) 0.4902(6) 0.9391(3) 0.058(3) Uani 1 1 d . A .
H25 H 0.4698 0.4963 0.9479 0.070 Uiso 1 1 calc R . .
C24 C 0.6176(11) 0.4128(7) 0.9406(4) 0.080(3) Uani 1 1 d . . .
H24 H 0.5712 0.3646 0.9503 0.096 Uiso 1 1 calc R A .
C23 C 0.7453(12) 0.4039(8) 0.9283(4) 0.097(4) Uani 1 1 d . A .
H23 H 0.7875 0.3501 0.9299 0.116 Uiso 1 1 calc R . .
C53 C 1.0658(9) 0.6915(8) 0.7416(4) 0.074(3) Uani 1 1 d . . .
H53 H 1.1209 0.6933 0.7715 0.088 Uiso 1 1 calc R . .
C46 C 1.0005(10) 0.9049(8) 0.7476(4) 0.080(3) Uani 1 1 d . . .
H46 H 0.9989 0.9487 0.7707 0.096 Uiso 1 1 calc R . .
C48 C 0.9776(10) 0.7554(7) 0.7294(3) 0.066(3) Uani 1 1 d . . .
C49 C 0.8939(10) 0.7481(8) 0.6853(3) 0.084(4) Uani 1 1 d . . .
H49 H 0.8303 0.7912 0.6760 0.100 Uiso 1 1 calc R . .
C47 C 1.0363(12) 0.9330(7) 0.6995(4) 0.099(4) Uani 1 1 d . . .
H47A H 1.1141 0.9706 0.7041 0.148 Uiso 1 1 calc R . .
H47B H 0.9605 0.9633 0.6821 0.148 Uiso 1 1 calc R . .
H47C H 1.0575 0.8834 0.6809 0.148 Uiso 1 1 calc R . .
C50 C 0.9037(10) 0.6798(7) 0.6560(3) 0.069(3) Uani 1 1 d . . .
H50 H 0.8475 0.6785 0.6263 0.083 Uiso 1 1 calc R . .
C52 C 1.0762(10) 0.6235(8) 0.7108(4) 0.090(4) Uani 1 1 d . . .
H52 H 1.1444 0.5831 0.7199 0.108 Uiso 1 1 calc R . .
C51 C 0.9936(8) 0.6095(6) 0.6671(2) 0.092(4) Uani 1 1 d . . .
H51 H 0.9970 0.5605 0.6477 0.110 Uiso 1 1 calc R . .
C39A C 0.6424(8) 0.7492(6) 0.7542(2) 0.031(12) Uiso 0.164(7) 1 d PRD A 2
H39A H 0.7216 0.7811 0.7454 0.037 Uiso 0.164(7) 1 calc PR A 2
C36A C 0.5136(8) 0.7293(6) 0.8438(2) 0.017(10) Uiso 0.164(7) 1 d PRD A 2
H36A H 0.5649 0.6763 0.8525 0.021 Uiso 0.164(7) 1 calc PR A 2
C42A C 0.557(3) 0.9079(9) 0.8068(14) 0.030(11) Uiso 0.164(7) 1 d PD A 2
H42A H 0.5622 0.9297 0.8404 0.036 Uiso 0.164(7) 1 calc PR A 2
C43A C 0.636(6) 0.971(3) 0.780(2) 0.047(19) Uiso 0.164(7) 1 d PD A 2
H43D H 0.5763 1.0166 0.7669 0.070 Uiso 0.164(7) 1 calc PR A 2
H43E H 0.6727 0.9419 0.7537 0.070 Uiso 0.164(7) 1 calc PR A 2
H43F H 0.7088 0.9948 0.8020 0.070 Uiso 0.164(7) 1 calc PR A 2
C37A C 0.472(8) 0.763(4) 0.8908(13) 0.04(2) Uiso 0.164(7) 1 d PD A 2
H37D H 0.4379 0.8211 0.8859 0.059 Uiso 0.164(7) 1 calc PR A 2
H37E H 0.5500 0.7637 0.9154 0.059 Uiso 0.164(7) 1 calc PR A 2
H37F H 0.4026 0.7270 0.9013 0.059 Uiso 0.164(7) 1 calc PR A 2
C40A C 0.695(5) 0.6586(14) 0.754(2) 0.016(14) Uiso 0.164(7) 1 d PD A 2
H40D H 0.6378 0.6212 0.7700 0.024 Uiso 0.164(7) 1 calc PR A 2
H40E H 0.7865 0.6566 0.7701 0.024 Uiso 0.164(7) 1 calc PR A 2
H40F H 0.6952 0.6398 0.7203 0.024 Uiso 0.164(7) 1 calc PR A 2
C38A C 0.377(4) 0.700(5) 0.820(3) 0.11(3) Uiso 0.164(7) 1 d PD A 2
H38D H 0.3403 0.6577 0.8398 0.169 Uiso 0.164(7) 1 calc PR A 2
H38E H 0.3870 0.6755 0.7883 0.169 Uiso 0.164(7) 1 calc PR A 2
H38F H 0.3163 0.7488 0.8155 0.169 Uiso 0.164(7) 1 calc PR A 2
C41A C 0.542(4) 0.766(3) 0.7098(13) 0.032(12) Uiso 0.164(7) 1 d PD A 2
H41D H 0.5483 0.8257 0.7003 0.048 Uiso 0.164(7) 1 calc PR A 2
H41E H 0.4516 0.7542 0.7173 0.048 Uiso 0.164(7) 1 calc PR A 2
H41F H 0.5627 0.7297 0.6835 0.048 Uiso 0.164(7) 1 calc PR A 2
C44A C 0.415(3) 0.928(3) 0.7838(18) 0.040(13) Uiso 0.164(7) 1 d PD A 2
H44D H 0.4155 0.9807 0.7655 0.060 Uiso 0.164(7) 1 calc PR A 2
H44E H 0.3560 0.9342 0.8089 0.060 Uiso 0.164(7) 1 calc PR A 2
H44F H 0.3823 0.8817 0.7622 0.060 Uiso 0.164(7) 1 calc PR 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 N1 1.881(6) . ?
Ge1 C45 1.991(10) . ?
Si1 N1 1.818(5) . ?
Si1 C39A 1.818(6) . ?
Si1 C36A 1.849(7) . ?
Si1 C36 1.878(6) . ?
Si1 C42 1.883(6) . ?
Si1 C42A 1.894(8) . ?
Si1 C39 1.913(6) . ?
N1 C1 1.483(9) . ?
C1 C2 1.430(11) . ?
C1 C6 1.432(10) . ?
C16 C17 1.382(11) . ?
C16 C15 1.403(11) . ?
C6 C5 1.404(9) . ?
C6 C7 1.523(11) . ?
C20 C2 1.531(11) . ?
C20 C27 1.538(10) . ?
C20 C21 1.542(11) . ?
C7 C14 1.528(10) . ?
C7 C8 1.536(11) . ?
C2 C3 1.401(10) . ?
C19 C18 1.386(11) . ?
C19 C14 1.392(10) . ?
C8 C13 1.385(10) . ?
C8 C9 1.409(10) . ?
C14 C15 1.390(10) . ?
C3 C4 1.388(10) . ?
C4 C5 1.378(10) . ?
C4 C33 1.526(10) . ?
C35 C33 1.528(11) . ?
C27 C32 1.358(11) . ?
C27 C28 1.389(10) . ?
C18 C17 1.384(11) . ?
C9 C10 1.396(11) . ?
C33 C34 1.509(11) . ?
C45 C46 1.348(13) . ?
C45 C48 1.480(13) . ?
C32 C31 1.366(11) . ?
C13 C12 1.413(11) . ?
C12 C11 1.381(11) . ?
C39 C40 1.532(7) . ?
C39 C41 1.550(7) . ?
C28 C29 1.382(12) . ?
C42 C44 1.535(7) . ?
C42 C43 1.543(7) . ?
C10 C11 1.372(11) . ?
C36 C37 1.532(7) . ?
C36 C38 1.541(7) . ?
C21 C22 1.369(11) . ?
C21 C26 1.398(11) . ?
C30 C29 1.368(13) . ?
C30 C31 1.401(12) . ?
C22 C23 1.375(14) . ?
C26 C25 1.352(11) . ?
C25 C24 1.364(13) . ?
C24 C23 1.380(13) . ?
C53 C48 1.362(13) . ?
C53 C52 1.389(13) . ?
C46 C47 1.507(13) . ?
C48 C49 1.416(11) . ?
C49 C50 1.369(13) . ?
C50 C51 1.443(13) . ?
C52 C51 1.417(12) . ?
C39A C40A 1.529(8) . ?
C39A C41A 1.529(8) . ?
C36A C38A 1.529(8) . ?
C36A C37A 1.530(8) . ?
C42A C43A 1.529(8) . ?
C42A C44A 1.531(8) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Ge1 C45 110.3(3) . . ?
N1 Si1 C39A 108.1(4) . . ?
N1 Si1 C36A 109.1(4) . . ?
C39A Si1 C36A 109.0(4) . . ?
N1 Si1 C36 112.1(3) . . ?
C39A Si1 C36 139.7(4) . . ?
C36A Si1 C36 59.9(4) . . ?
N1 Si1 C42 105.3(3) . . ?
C39A Si1 C42 50.6(4) . . ?
C36A Si1 C42 144.6(4) . . ?
C36 Si1 C42 113.9(4) . . ?
N1 Si1 C42A 108.8(10) . . ?
C39A Si1 C42A 112.4(13) . . ?
C36A Si1 C42A 109.4(11) . . ?
C36 Si1 C42A 51.3(12) . . ?
C42 Si1 C42A 66.1(13) . . ?
N1 Si1 C39 109.5(3) . . ?
C39A Si1 C39 58.0(4) . . ?
C36A Si1 C39 53.3(4) . . ?
C36 Si1 C39 109.0(4) . . ?
C42 Si1 C39 106.8(4) . . ?
C42A Si1 C39 141.4(10) . . ?
C1 N1 Si1 117.0(4) . . ?
C1 N1 Ge1 107.2(4) . . ?
Si1 N1 Ge1 135.8(3) . . ?
C2 C1 C6 119.8(7) . . ?
C2 C1 N1 120.7(7) . . ?
C6 C1 N1 119.5(7) . . ?
C17 C16 C15 119.6(8) . . ?
C5 C6 C1 117.6(7) . . ?
C5 C6 C7 120.8(6) . . ?
C1 C6 C7 121.3(7) . . ?
C2 C20 C27 112.7(6) . . ?
C2 C20 C21 111.9(7) . . ?
C27 C20 C21 113.6(7) . . ?
C6 C7 C14 112.3(6) . . ?
C6 C7 C8 113.0(6) . . ?
C14 C7 C8 111.9(6) . . ?
C3 C2 C1 118.5(7) . . ?
C3 C2 C20 119.5(7) . . ?
C1 C2 C20 121.6(7) . . ?
C18 C19 C14 121.0(7) . . ?
C13 C8 C9 119.2(7) . . ?
C13 C8 C7 121.7(7) . . ?
C9 C8 C7 119.0(7) . . ?
C15 C14 C19 118.7(8) . . ?
C15 C14 C7 122.0(7) . . ?
C19 C14 C7 119.1(7) . . ?
C4 C3 C2 122.4(7) . . ?
C5 C4 C3 118.3(7) . . ?
C5 C4 C33 122.0(7) . . ?
C3 C4 C33 119.7(7) . . ?
C32 C27 C28 118.8(8) . . ?
C32 C27 C20 119.1(7) . . ?
C28 C27 C20 121.6(8) . . ?
C17 C18 C19 119.8(8) . . ?
C14 C15 C16 120.5(8) . . ?
C16 C17 C18 120.3(8) . . ?
C4 C5 C6 123.5(7) . . ?
C10 C9 C8 119.7(8) . . ?
C34 C33 C4 112.1(7) . . ?
C34 C33 C35 110.0(7) . . ?
C4 C33 C35 111.8(6) . . ?
C46 C45 C48 117.8(10) . . ?
C46 C45 Ge1 119.8(8) . . ?
C48 C45 Ge1 120.2(8) . . ?
C27 C32 C31 121.9(8) . . ?
C8 C13 C12 119.8(7) . . ?
C11 C12 C13 120.5(8) . . ?
C40 C39 C41 110.8(9) . . ?
C40 C39 Si1 112.3(7) . . ?
C41 C39 Si1 115.5(6) . . ?
C29 C28 C27 118.8(9) . . ?
C44 C42 C43 109.9(8) . . ?
C44 C42 Si1 118.2(7) . . ?
C43 C42 Si1 110.6(6) . . ?
C11 C10 C9 121.0(8) . . ?
C10 C11 C12 119.7(9) . . ?
C37 C36 C38 109.8(9) . . ?
C37 C36 Si1 115.5(6) . . ?
C38 C36 Si1 113.8(6) . . ?
C22 C21 C26 117.3(9) . . ?
C22 C21 C20 120.1(8) . . ?
C26 C21 C20 122.4(8) . . ?
C29 C30 C31 116.5(9) . . ?
C21 C22 C23 121.3(10) . . ?
C30 C29 C28 123.2(8) . . ?
C25 C26 C21 122.3(8) . . ?
C32 C31 C30 120.8(9) . . ?
C26 C25 C24 119.2(9) . . ?
C25 C24 C23 120.5(10) . . ?
C22 C23 C24 119.4(11) . . ?
C48 C53 C52 120.9(10) . . ?
C45 C46 C47 129.9(11) . . ?
C53 C48 C49 117.5(10) . . ?
C53 C48 C45 119.3(8) . . ?
C49 C48 C45 123.1(10) . . ?
C50 C49 C48 120.7(10) . . ?
C49 C50 C51 124.5(8) . . ?
C53 C52 C51 125.4(10) . . ?
C52 C51 C50 110.8(8) . . ?
C40A C39A C41A 111(3) . . ?
C40A C39A Si1 118(2) . . ?
C41A C39A Si1 122(2) . . ?
C38A C36A C37A 99(5) . . ?
C38A C36A Si1 122(3) . . ?
C37A C36A Si1 117(3) . . ?
C43A C42A C44A 100(4) . . ?
C43A C42A Si1 116(3) . . ?
C44A C42A Si1 123(3) . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        25.50
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         1.021
_refine_diff_density_min         -1.186
_refine_diff_density_rms         0.098
####################################################################### 
# 
# 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_compound15
_database_code_depnum_ccdc_archive 'CCDC 1422735'
_audit_update_record             
;
2015-09-07 deposited with the CCDC.
2015-09-22 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C53 H61 N Si Sn'
_chemical_formula_weight         858.81

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'
Sn Sn -0.6537 1.4246 '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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   P2(1)/n

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

_cell_length_a                   10.1088(10)
_cell_length_b                   15.7379(15)
_cell_length_c                   28.106(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 96.853(8)
_cell_angle_gamma                90.00
_cell_volume                     4439.5(7)
_cell_formula_units_Z            4
_cell_measurement_temperature    123(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       block
_exptl_crystal_colour            yellow-orange
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.285
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1800
_exptl_absorpt_coefficient_mu    0.639
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.908
_exptl_absorpt_correction_T_max  0.933
_exptl_absorpt_process_details   'SCALE3 ABSPACK'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      123(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Oxford Gemini Ultra'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            21635
_diffrn_reflns_av_R_equivalents  0.0598
_diffrn_reflns_av_sigmaI/netI    0.0819
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_theta_min         2.92
_diffrn_reflns_theta_max         25.50
_reflns_number_total             8243
_reflns_number_gt                5733
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       CrysalisPro
_computing_cell_refinement       CrysalisPro
_computing_data_reduction        CrysalisPro
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    X-Seed
_computing_publication_material  CifTAB

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
 The high r-factors for the structure are due to weak reflection data above theta
 angles of 23 deg.
 The highest residual electron density peak (2.39 e-/ang3) in the final difference
 map was located close (ca. 1 ang.) from Sn(1).
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0605P)²+32.7059P] 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         8243
_refine_ls_number_parameters     514
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.1223
_refine_ls_R_factor_gt           0.0813
_refine_ls_wR_factor_ref         0.1985
_refine_ls_wR_factor_gt          0.1748
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_restrained_S_all      1.077
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Sn1 Sn 0.98588(5) 0.80789(4) 0.834460(17) 0.03064(18) Uani 1 1 d . . .
Si1 Si 0.62763(17) 0.79665(13) 0.81346(6) 0.0243(4) Uani 1 1 d . . .
N1 N 0.7851(5) 0.7999(4) 0.84904(17) 0.0211(12) Uani 1 1 d . . .
C20 C 0.7986(6) 0.9532(4) 0.9077(2) 0.0209(14) Uani 1 1 d . . .
H20 H 0.7420 0.9507 0.8760 0.025 Uiso 1 1 calc R . .
C23 C 1.1769(7) 0.9762(5) 0.9181(3) 0.0360(18) Uani 1 1 d . . .
H23 H 1.2528 0.9575 0.9387 0.043 Uiso 1 1 calc R . .
C21 C 0.9380(7) 0.9768(5) 0.8971(2) 0.0258(16) Uani 1 1 d . . .
C43 C 0.4548(7) 0.7934(5) 0.8879(2) 0.0355(19) Uani 1 1 d . . .
H43A H 0.3835 0.8227 0.9021 0.053 Uiso 1 1 calc R . .
H43B H 0.5317 0.7858 0.9122 0.053 Uiso 1 1 calc R . .
H43C H 0.4229 0.7377 0.8759 0.053 Uiso 1 1 calc R . .
C5 C 0.8100(6) 0.7064(5) 0.9726(2) 0.0264(16) Uani 1 1 d . . .
H5 H 0.8172 0.6520 0.9874 0.032 Uiso 1 1 calc R . .
C22 C 1.0516(7) 0.9506(5) 0.9268(3) 0.0291(16) Uani 1 1 d . . .
H22 H 1.0423 0.9146 0.9533 0.035 Uiso 1 1 calc R . .
C6 C 0.8029(6) 0.7109(4) 0.9229(2) 0.0227(15) Uani 1 1 d . . .
C27 C 0.7393(7) 1.0229(4) 0.9366(2) 0.0232(15) Uani 1 1 d . . .
C7 C 0.8224(7) 0.6298(4) 0.8953(2) 0.0259(15) Uani 1 1 d . . .
H7 H 0.7792 0.6402 0.8619 0.031 Uiso 1 1 calc R . .
C39 C 0.5751(8) 0.6802(6) 0.7993(3) 0.045(2) Uani 1 1 d . . .
H39 H 0.5907 0.6476 0.8300 0.054 Uiso 1 1 calc R . .
C4 C 0.8071(7) 0.7776(4) 1.0016(2) 0.0251(15) Uani 1 1 d . . .
C37 C 0.6721(10) 0.9476(5) 0.7634(3) 0.059(3) Uani 1 1 d D . .
H37A H 0.6871 0.9748 0.7332 0.088 Uiso 1 1 calc R . .
H37B H 0.7498 0.9570 0.7873 0.088 Uiso 1 1 calc R . .
H37C H 0.5929 0.9723 0.7751 0.088 Uiso 1 1 calc R . .
C33 C 0.8167(8) 0.7688(5) 1.0559(2) 0.0315(17) Uani 1 1 d . . .
H33 H 0.8182 0.8274 1.0697 0.038 Uiso 1 1 calc R . .
C3 C 0.8004(6) 0.8563(4) 0.9793(2) 0.0242(15) Uani 1 1 d . . .
H3 H 0.8005 0.9060 0.9985 0.029 Uiso 1 1 calc R . .
C24 C 1.1931(8) 1.0289(5) 0.8798(3) 0.0386(19) Uani 1 1 d . . .
H24 H 1.2797 1.0466 0.8741 0.046 Uiso 1 1 calc R . .
C40 C 0.6720(8) 0.6427(6) 0.7647(3) 0.052(3) Uani 1 1 d . . .
H40A H 0.6606 0.5809 0.7625 0.078 Uiso 1 1 calc R . .
H40B H 0.7643 0.6560 0.7773 0.078 Uiso 1 1 calc R . .
H40C H 0.6515 0.6679 0.7328 0.078 Uiso 1 1 calc R . .
C25 C 1.0827(8) 1.0555(5) 0.8501(3) 0.040(2) Uani 1 1 d . . .
H25 H 1.0931 1.0909 0.8234 0.048 Uiso 1 1 calc R . .
C42 C 0.4971(8) 0.8478(6) 0.8452(3) 0.046(2) Uani 1 1 d . . .
H42 H 0.5383 0.9009 0.8600 0.056 Uiso 1 1 calc R . .
C41 C 0.4266(9) 0.6678(6) 0.7792(4) 0.056(3) Uani 1 1 d . . .
H41A H 0.4069 0.7004 0.7495 0.085 Uiso 1 1 calc R . .
H41B H 0.3697 0.6877 0.8028 0.085 Uiso 1 1 calc R . .
H41C H 0.4093 0.6074 0.7726 0.085 Uiso 1 1 calc R . .
C36 C 0.6509(9) 0.8508(5) 0.7553(3) 0.053(2) Uani 1 1 d D . .
H36 H 0.7378 0.8291 0.7466 0.064 Uiso 1 1 calc R . .
C44 C 0.3736(8) 0.8771(6) 0.8104(3) 0.053(2) Uani 1 1 d . . .
H44A H 0.3310 0.8274 0.7940 0.080 Uiso 1 1 calc R . .
H44B H 0.4024 0.9164 0.7866 0.080 Uiso 1 1 calc R . .
H44C H 0.3099 0.9058 0.8286 0.080 Uiso 1 1 calc R . .
C35 C 0.6958(8) 0.7227(6) 1.0716(3) 0.046(2) Uani 1 1 d . . .
H35A H 0.6141 0.7519 1.0583 0.069 Uiso 1 1 calc R . .
H35B H 0.7020 0.7227 1.1067 0.069 Uiso 1 1 calc R . .
H35C H 0.6940 0.6640 1.0599 0.069 Uiso 1 1 calc R . .
C32 C 0.6047(7) 1.0211(5) 0.9434(3) 0.0309(17) Uani 1 1 d . . .
H32 H 0.5522 0.9740 0.9313 0.037 Uiso 1 1 calc R . .
C29 C 0.7549(8) 1.1563(5) 0.9791(3) 0.0330(17) Uani 1 1 d . . .
H29 H 0.8079 1.2024 0.9922 0.040 Uiso 1 1 calc R . .
C19 C 1.0077(8) 0.5826(6) 0.8477(3) 0.042(2) Uani 1 1 d . . .
H19 H 0.9433 0.5770 0.8204 0.051 Uiso 1 1 calc R . .
C28 C 0.8124(7) 1.0929(5) 0.9550(2) 0.0292(16) Uani 1 1 d . . .
H28 H 0.9041 1.0969 0.9508 0.035 Uiso 1 1 calc R . .
C9 C 0.6230(7) 0.5589(5) 0.9260(3) 0.0332(17) Uani 1 1 d . . .
H9 H 0.5801 0.6127 0.9245 0.040 Uiso 1 1 calc R . .
C26 C 0.9579(8) 1.0310(5) 0.8589(3) 0.0347(18) Uani 1 1 d . . .
H26 H 0.8826 1.0512 0.8386 0.042 Uiso 1 1 calc R . .
C8 C 0.7526(7) 0.5519(5) 0.9132(3) 0.0286(16) Uani 1 1 d . . .
C48 C 0.9833(7) 0.7599(5) 0.7246(3) 0.0355(18) Uani 1 1 d . . .
C31 C 0.5453(7) 1.0844(5) 0.9667(3) 0.0323(17) Uani 1 1 d . . .
H31 H 0.4535 1.0810 0.9707 0.039 Uiso 1 1 calc R . .
C10 C 0.5573(8) 0.4890(5) 0.9406(3) 0.040(2) Uani 1 1 d . . .
H10 H 0.4707 0.4955 0.9501 0.048 Uiso 1 1 calc R . .
C53 C 1.0732(9) 0.6946(7) 0.7369(3) 0.058(3) Uani 1 1 d . . .
H53 H 1.1316 0.6993 0.7659 0.069 Uiso 1 1 calc R . .
C30 C 0.6218(8) 1.1540(5) 0.9846(3) 0.0366(19) Uani 1 1 d . . .
H30 H 0.5821 1.1990 1.0004 0.044 Uiso 1 1 calc R . .
C14 C 0.9676(7) 0.6124(5) 0.8910(3) 0.0288(16) Uani 1 1 d . . .
C45 C 0.9816(8) 0.8336(6) 0.7563(3) 0.042(2) Uani 1 1 d . . .
C34 C 0.9435(8) 0.7245(6) 1.0768(3) 0.043(2) Uani 1 1 d . . .
H34A H 0.9423 0.6655 1.0656 0.065 Uiso 1 1 calc R . .
H34B H 0.9496 0.7254 1.1119 0.065 Uiso 1 1 calc R . .
H34C H 1.0206 0.7540 1.0665 0.065 Uiso 1 1 calc R . .
C49 C 0.8956(8) 0.7485(6) 0.6823(3) 0.044(2) Uani 1 1 d . . .
H49 H 0.8314 0.7912 0.6726 0.053 Uiso 1 1 calc R . .
C15 C 1.0669(8) 0.6234(6) 0.9292(3) 0.044(2) Uani 1 1 d . . .
H15 H 1.0444 0.6446 0.9589 0.053 Uiso 1 1 calc R . .
C12 C 0.7422(9) 0.4028(5) 0.9285(3) 0.049(2) Uani 1 1 d . . .
H12 H 0.7844 0.3488 0.9292 0.059 Uiso 1 1 calc R . .
C18 C 1.1361(8) 0.5618(6) 0.8441(3) 0.048(2) Uani 1 1 d . . .
H18 H 1.1594 0.5384 0.8151 0.058 Uiso 1 1 calc R . .
C38 C 0.5465(9) 0.8290(9) 0.7112(3) 0.080(4) Uani 1 1 d . . .
H38A H 0.4589 0.8512 0.7166 0.119 Uiso 1 1 calc R . .
H38B H 0.5411 0.7672 0.7070 0.119 Uiso 1 1 calc R . .
H38C H 0.5741 0.8550 0.6822 0.119 Uiso 1 1 calc R . .
C13 C 0.8085(8) 0.4726(5) 0.9142(3) 0.043(2) Uani 1 1 d . . .
H13 H 0.8951 0.4658 0.9048 0.052 Uiso 1 1 calc R . .
C16 C 1.1971(9) 0.6040(8) 0.9245(3) 0.065(3) Uani 1 1 d . . .
H16 H 1.2636 0.6113 0.9511 0.079 Uiso 1 1 calc R . .
C50 C 0.9011(9) 0.6772(7) 0.6548(3) 0.055(3) Uani 1 1 d . . .
H50 H 0.8404 0.6712 0.6265 0.066 Uiso 1 1 calc R . .
C11 C 0.6150(9) 0.4093(6) 0.9418(3) 0.047(2) Uani 1 1 d . . .
H11 H 0.5692 0.3607 0.9515 0.057 Uiso 1 1 calc R . .
C17 C 1.2328(9) 0.5741(7) 0.8820(3) 0.062(3) Uani 1 1 d . . .
H17 H 1.3234 0.5621 0.8789 0.075 Uiso 1 1 calc R . .
C51 C 0.9932(10) 0.6134(7) 0.6673(4) 0.063(3) Uani 1 1 d . . .
H51 H 0.9960 0.5641 0.6479 0.076 Uiso 1 1 calc R . .
C52 C 1.0817(10) 0.6231(7) 0.7091(4) 0.066(3) Uani 1 1 d . . .
H52 H 1.1471 0.5809 0.7182 0.080 Uiso 1 1 calc R . .
C1 C 0.7917(6) 0.7922(4) 0.9003(2) 0.0226(15) Uani 1 1 d . . .
C2 C 0.7933(6) 0.8653(4) 0.9296(2) 0.0216(14) Uani 1 1 d . . .
C47 C 1.0337(11) 0.9377(7) 0.6921(3) 0.070(3) Uani 1 1 d . . .
H47A H 1.1169 0.9702 0.6948 0.105 Uiso 1 1 calc R . .
H47B H 0.9606 0.9729 0.6769 0.105 Uiso 1 1 calc R . .
H47C H 1.0427 0.8868 0.6727 0.105 Uiso 1 1 calc R . .
C46 C 1.0041(9) 0.9117(6) 0.7417(3) 0.049(2) Uani 1 1 d . . .
H46 H 1.0014 0.9559 0.7646 0.058 Uiso 1 1 calc R . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Sn1 N1 2.122(5) . ?
Sn1 C45 2.229(8) . ?
Si1 N1 1.777(5) . ?
Si1 C42 1.862(8) . ?
Si1 C36 1.883(9) . ?
Si1 C39 1.937(9) . ?
N1 C1 1.440(8) . ?
C20 C2 1.518(9) . ?
C20 C21 1.520(9) . ?
C20 C27 1.530(9) . ?
C23 C22 1.378(10) . ?
C23 C24 1.384(11) . ?
C21 C22 1.399(9) . ?
C21 C26 1.405(10) . ?
C43 C42 1.574(12) . ?
C5 C4 1.388(10) . ?
C5 C6 1.392(9) . ?
C6 C1 1.426(9) . ?
C6 C7 1.519(9) . ?
C27 C28 1.392(10) . ?
C27 C32 1.396(10) . ?
C7 C14 1.512(10) . ?
C7 C8 1.529(10) . ?
C39 C41 1.552(11) . ?
C39 C40 1.574(11) . ?
C4 C3 1.386(10) . ?
C4 C33 1.525(9) . ?
C37 C36 1.552(7) . ?
C33 C34 1.514(11) . ?
C33 C35 1.531(11) . ?
C3 C2 1.398(9) . ?
C24 C25 1.378(11) . ?
C25 C26 1.370(11) . ?
C42 C44 1.561(11) . ?
C36 C38 1.568(11) . ?
C32 C31 1.370(10) . ?
C29 C30 1.373(11) . ?
C29 C28 1.374(10) . ?
C19 C18 1.354(11) . ?
C19 C14 1.408(10) . ?
C9 C10 1.373(11) . ?
C9 C8 1.404(10) . ?
C8 C13 1.368(11) . ?
C48 C53 1.390(12) . ?
C48 C49 1.407(11) . ?
C48 C45 1.462(12) . ?
C31 C30 1.399(11) . ?
C10 C11 1.382(12) . ?
C53 C52 1.379(13) . ?
C14 C15 1.392(10) . ?
C45 C46 1.324(12) . ?
C49 C50 1.367(13) . ?
C15 C16 1.374(12) . ?
C12 C13 1.372(12) . ?
C12 C11 1.385(12) . ?
C18 C17 1.371(12) . ?
C16 C17 1.370(13) . ?
C50 C51 1.385(14) . ?
C51 C52 1.397(13) . ?
C1 C2 1.413(9) . ?
C47 C46 1.515(12) . ?

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 C45 107.1(2) . . ?
N1 Si1 C42 110.9(3) . . ?
N1 Si1 C36 106.2(3) . . ?
C42 Si1 C36 112.9(4) . . ?
N1 Si1 C39 110.4(3) . . ?
C42 Si1 C39 108.4(4) . . ?
C36 Si1 C39 108.0(4) . . ?
C1 N1 Si1 119.5(4) . . ?
C1 N1 Sn1 105.5(4) . . ?
Si1 N1 Sn1 134.9(3) . . ?
C2 C20 C21 112.3(5) . . ?
C2 C20 C27 113.8(5) . . ?
C21 C20 C27 111.1(5) . . ?
C22 C23 C24 120.6(7) . . ?
C22 C21 C26 116.9(7) . . ?
C22 C21 C20 121.7(6) . . ?
C26 C21 C20 121.2(6) . . ?
C4 C5 C6 123.1(6) . . ?
C23 C22 C21 121.0(7) . . ?
C5 C6 C1 118.9(6) . . ?
C5 C6 C7 118.4(6) . . ?
C1 C6 C7 122.3(6) . . ?
C28 C27 C32 116.6(7) . . ?
C28 C27 C20 122.7(6) . . ?
C32 C27 C20 120.5(6) . . ?
C14 C7 C6 112.3(6) . . ?
C14 C7 C8 111.8(6) . . ?
C6 C7 C8 114.3(6) . . ?
C41 C39 C40 112.0(7) . . ?
C41 C39 Si1 115.1(6) . . ?
C40 C39 Si1 107.8(6) . . ?
C3 C4 C5 117.4(6) . . ?
C3 C4 C33 121.8(6) . . ?
C5 C4 C33 120.7(6) . . ?
C34 C33 C4 112.4(6) . . ?
C34 C33 C35 109.7(6) . . ?
C4 C33 C35 112.0(6) . . ?
C4 C3 C2 122.4(6) . . ?
C25 C24 C23 119.4(7) . . ?
C26 C25 C24 120.2(7) . . ?
C44 C42 C43 111.6(7) . . ?
C44 C42 Si1 112.7(6) . . ?
C43 C42 Si1 113.7(6) . . ?
C37 C36 C38 113.6(8) . . ?
C37 C36 Si1 110.2(6) . . ?
C38 C36 Si1 116.5(7) . . ?
C31 C32 C27 122.7(7) . . ?
C30 C29 C28 120.9(7) . . ?
C18 C19 C14 121.5(7) . . ?
C29 C28 C27 121.4(7) . . ?
C10 C9 C8 120.9(7) . . ?
C25 C26 C21 121.9(7) . . ?
C13 C8 C9 117.5(7) . . ?
C13 C8 C7 122.1(7) . . ?
C9 C8 C7 120.2(6) . . ?
C53 C48 C49 116.4(8) . . ?
C53 C48 C45 119.3(7) . . ?
C49 C48 C45 124.3(8) . . ?
C32 C31 C30 119.1(7) . . ?
C9 C10 C11 121.1(8) . . ?
C52 C53 C48 123.1(8) . . ?
C29 C30 C31 119.2(7) . . ?
C15 C14 C19 117.0(7) . . ?
C15 C14 C7 122.2(7) . . ?
C19 C14 C7 120.8(6) . . ?
C46 C45 C48 122.1(8) . . ?
C46 C45 Sn1 119.3(6) . . ?
C48 C45 Sn1 117.2(6) . . ?
C50 C49 C48 121.2(8) . . ?
C16 C15 C14 120.5(8) . . ?
C13 C12 C11 121.5(8) . . ?
C19 C18 C17 120.6(8) . . ?
C8 C13 C12 121.4(8) . . ?
C17 C16 C15 121.1(8) . . ?
C49 C50 C51 121.6(8) . . ?
C10 C11 C12 117.6(8) . . ?
C16 C17 C18 119.2(8) . . ?
C50 C51 C52 118.5(9) . . ?
C53 C52 C51 119.3(9) . . ?
C2 C1 C6 118.5(6) . . ?
C2 C1 N1 120.6(6) . . ?
C6 C1 N1 120.8(6) . . ?
C3 C2 C1 119.7(6) . . ?
C3 C2 C20 119.8(6) . . ?
C1 C2 C20 120.4(6) . . ?
C45 C46 C47 126.6(9) . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        25.50
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         2.395
_refine_diff_density_min         -0.856
_refine_diff_density_rms         0.134
####################################################################### 
# 
# 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_compound16
_database_code_depnum_ccdc_archive 'CCDC 1422736'
_audit_update_record             
;
2015-09-07 deposited with the CCDC.
2015-09-22 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C52 H65 Ge N Si'
_chemical_formula_weight         804.73

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   P2(1)/n

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

_cell_length_a                   10.0030(6)
_cell_length_b                   15.4017(12)
_cell_length_c                   28.920(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 97.698(2)
_cell_angle_gamma                90.00
_cell_volume                     4415.4(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.211
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1720
_exptl_absorpt_coefficient_mu    0.756
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.830
_exptl_absorpt_correction_T_max  0.926
_exptl_absorpt_process_details   XDS

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71080
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_source         'Australian Synchrotron'
_diffrn_radiation_monochromator  ?
_diffrn_measurement_device_type  'ADSC Quantum 210r'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            38995
_diffrn_reflns_av_R_equivalents  0.0512
_diffrn_reflns_av_sigmaI/netI    0.0556
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_theta_min         2.96
_diffrn_reflns_theta_max         25.10
_reflns_number_total             7515
_reflns_number_gt                5392
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Blu-Ice (McPhillips, 2002)'
_computing_cell_refinement       'XDS (Kabsch, 1993)'
_computing_data_reduction        'XDS (Kabsch, 1993)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    X-Seed
_computing_publication_material  CifTAB

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
 The low value (95.7%) for completeness of data to theta = 25.1 deg. arises 
 from hardware constraints associated with the diffractometer used at the 
 Australian Synchrotron. 
 Its minimum crystal to detector distance is 72 mm and its
 goniometer only rotates about the phi axis.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0507P)²+3.3469P] 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         7515
_refine_ls_number_parameters     504
_refine_ls_number_restraints     12
_refine_ls_R_factor_all          0.0746
_refine_ls_R_factor_gt           0.0452
_refine_ls_wR_factor_ref         0.1155
_refine_ls_wR_factor_gt          0.1035
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_restrained_S_all      1.067
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ge1 Ge 0.55489(3) 0.27962(2) 0.163942(11) 0.02431(12) Uani 1 1 d . . .
Si1 Si 0.89536(8) 0.27460(5) 0.18174(3) 0.0196(2) Uani 1 1 d . . .
N1 N 0.7320(2) 0.27954(14) 0.14795(8) 0.0185(5) Uani 1 1 d . . .
C1 C 0.7196(3) 0.27796(18) 0.09709(10) 0.0179(6) Uani 1 1 d . . .
C2 C 0.7162(3) 0.35568(18) 0.07076(10) 0.0183(7) Uani 1 1 d . . .
C3 C 0.7011(3) 0.35099(19) 0.02226(10) 0.0201(7) Uani 1 1 d . . .
H3 H 0.6998 0.4036 0.0051 0.024 Uiso 1 1 calc R . .
C4 C 0.6877(3) 0.27315(18) -0.00237(10) 0.0205(7) Uani 1 1 d . . .
C5 C 0.6891(3) 0.19770(18) 0.02419(10) 0.0214(7) Uani 1 1 d . . .
H5 H 0.6804 0.1434 0.0085 0.026 Uiso 1 1 calc R . .
C6 C 0.7026(3) 0.19831(18) 0.07260(10) 0.0185(7) Uani 1 1 d . . .
C7 C 0.6687(3) 0.27127(19) -0.05533(10) 0.0252(7) Uani 1 1 d . . .
H7 H 0.6722 0.3327 -0.0664 0.030 Uiso 1 1 calc R . .
C8 C 0.7799(4) 0.2219(3) -0.07455(12) 0.0490(10) Uani 1 1 d . . .
H8A H 0.7800 0.1614 -0.0640 0.073 Uiso 1 1 calc R . .
H8B H 0.8671 0.2486 -0.0634 0.073 Uiso 1 1 calc R . .
H8C H 0.7645 0.2235 -0.1087 0.073 Uiso 1 1 calc R . .
C9 C 0.5329(3) 0.2346(2) -0.07537(11) 0.0366(9) Uani 1 1 d . . .
H9A H 0.5215 0.2396 -0.1095 0.055 Uiso 1 1 calc R . .
H9B H 0.4612 0.2670 -0.0630 0.055 Uiso 1 1 calc R . .
H9C H 0.5281 0.1733 -0.0666 0.055 Uiso 1 1 calc R . .
C10 C 0.6906(3) 0.11261(18) 0.09853(10) 0.0209(7) Uani 1 1 d . . .
H10 H 0.7428 0.1205 0.1302 0.025 Uiso 1 1 calc R . .
C11 C 0.7571(3) 0.03625(18) 0.07591(10) 0.0224(7) Uani 1 1 d . . .
C12 C 0.8938(3) 0.0387(2) 0.07277(12) 0.0347(8) Uani 1 1 d . . .
H12 H 0.9443 0.0887 0.0836 0.042 Uiso 1 1 calc R . .
C13 C 0.9589(3) -0.0296(2) 0.05428(12) 0.0399(9) Uani 1 1 d . . .
H13 H 1.0529 -0.0263 0.0525 0.048 Uiso 1 1 calc R . .
C14 C 0.8876(4) -0.1023(2) 0.03841(12) 0.0382(9) Uani 1 1 d . . .
H14 H 0.9321 -0.1498 0.0261 0.046 Uiso 1 1 calc R . .
C15 C 0.7521(4) -0.1057(2) 0.04056(12) 0.0421(9) Uani 1 1 d . . .
H15 H 0.7020 -0.1556 0.0293 0.050 Uiso 1 1 calc R . .
C16 C 0.6870(3) -0.0368(2) 0.05906(12) 0.0351(8) Uani 1 1 d . . .
H16 H 0.5927 -0.0400 0.0601 0.042 Uiso 1 1 calc R . .
C17 C 0.5465(3) 0.09252(18) 0.10621(10) 0.0222(7) Uani 1 1 d . . .
C18 C 0.4351(3) 0.1163(2) 0.07498(12) 0.0392(9) Uani 1 1 d . . .
H18 H 0.4475 0.1487 0.0479 0.047 Uiso 1 1 calc R . .
C19 C 0.3061(3) 0.0935(3) 0.08261(13) 0.0461(10) Uani 1 1 d . . .
H19 H 0.2312 0.1097 0.0606 0.055 Uiso 1 1 calc R . .
C20 C 0.2852(3) 0.0477(2) 0.12154(12) 0.0379(9) Uani 1 1 d . . .
H20 H 0.1962 0.0333 0.1269 0.045 Uiso 1 1 calc R . .
C21 C 0.3930(3) 0.0231(2) 0.15263(12) 0.0402(9) Uani 1 1 d . . .
H21 H 0.3796 -0.0091 0.1796 0.048 Uiso 1 1 calc R . .
C22 C 0.5221(3) 0.0452(2) 0.14483(12) 0.0363(8) Uani 1 1 d . . .
H22 H 0.5964 0.0273 0.1667 0.044 Uiso 1 1 calc R . .
C23 C 0.7178(3) 0.44498(18) 0.09445(10) 0.0188(7) Uani 1 1 d . . .
H23 H 0.7770 0.4394 0.1250 0.023 Uiso 1 1 calc R . .
C24 C 0.5784(3) 0.47127(18) 0.10548(10) 0.0196(7) Uani 1 1 d . . .
C25 C 0.4601(3) 0.44560(19) 0.07787(11) 0.0259(7) Uani 1 1 d . . .
H25 H 0.4651 0.4084 0.0520 0.031 Uiso 1 1 calc R . .
C26 C 0.3352(3) 0.47351(19) 0.08763(11) 0.0282(8) Uani 1 1 d . . .
H26 H 0.2556 0.4559 0.0682 0.034 Uiso 1 1 calc R . .
C27 C 0.3260(3) 0.5270(2) 0.12561(11) 0.0302(8) Uani 1 1 d . . .
H27 H 0.2404 0.5458 0.1325 0.036 Uiso 1 1 calc R . .
C28 C 0.4415(3) 0.5526(2) 0.15318(11) 0.0328(8) Uani 1 1 d . . .
H28 H 0.4357 0.5888 0.1794 0.039 Uiso 1 1 calc R . .
C29 C 0.5663(3) 0.5260(2) 0.14305(11) 0.0287(8) Uani 1 1 d . . .
H29 H 0.6455 0.5454 0.1621 0.034 Uiso 1 1 calc R . .
C30 C 0.7806(3) 0.51543(18) 0.06682(10) 0.0203(7) Uani 1 1 d . . .
C31 C 0.7043(3) 0.58101(19) 0.04279(10) 0.0272(7) Uani 1 1 d . . .
H31 H 0.6096 0.5830 0.0435 0.033 Uiso 1 1 calc R . .
C32 C 0.7654(3) 0.6438(2) 0.01775(11) 0.0297(8) Uani 1 1 d . . .
H32 H 0.7118 0.6876 0.0013 0.036 Uiso 1 1 calc R . .
C33 C 0.9023(3) 0.6426(2) 0.01677(11) 0.0296(8) Uani 1 1 d . . .
H33 H 0.9436 0.6858 0.0000 0.035 Uiso 1 1 calc R . .
C34 C 0.9788(3) 0.5784(2) 0.04030(12) 0.0346(8) Uani 1 1 d . . .
H34 H 1.0736 0.5771 0.0398 0.042 Uiso 1 1 calc R . .
C35 C 0.9182(3) 0.5155(2) 0.06478(11) 0.0307(8) Uani 1 1 d . . .
H35 H 0.9725 0.4713 0.0806 0.037 Uiso 1 1 calc R . .
C36 C 0.8884(3) 0.3430(2) 0.23589(11) 0.0325(8) Uani 1 1 d . . .
H36 H 0.7989 0.3296 0.2461 0.039 Uiso 1 1 calc R . .
C37 C 0.9934(4) 0.3220(2) 0.27851(11) 0.0415(9) Uani 1 1 d . . .
H37A H 1.0841 0.3343 0.2710 0.062 Uiso 1 1 calc R . .
H37B H 0.9869 0.2604 0.2866 0.062 Uiso 1 1 calc R . .
H37C H 0.9758 0.3578 0.3051 0.062 Uiso 1 1 calc R . .
C38 C 0.8855(4) 0.4410(2) 0.22593(12) 0.0427(9) Uani 1 1 d . . .
H38A H 0.8735 0.4728 0.2545 0.064 Uiso 1 1 calc R . .
H38B H 0.8105 0.4543 0.2016 0.064 Uiso 1 1 calc R . .
H38C H 0.9707 0.4586 0.2154 0.064 Uiso 1 1 calc R . .
C39 C 1.0263(3) 0.3208(2) 0.14691(11) 0.0300(8) Uani 1 1 d . . .
H39 H 0.9876 0.3763 0.1331 0.036 Uiso 1 1 calc R . .
C40 C 1.1592(3) 0.3456(2) 0.17779(12) 0.0411(9) Uani 1 1 d . . .
H40A H 1.1993 0.2937 0.1936 0.062 Uiso 1 1 calc R . .
H40B H 1.1403 0.3884 0.2011 0.062 Uiso 1 1 calc R . .
H40C H 1.2223 0.3705 0.1582 0.062 Uiso 1 1 calc R . .
C41 C 1.0578(3) 0.2654(2) 0.10588(12) 0.0360(9) Uani 1 1 d . . .
H41A H 1.1268 0.2943 0.0903 0.054 Uiso 1 1 calc R . .
H41B H 0.9757 0.2578 0.0837 0.054 Uiso 1 1 calc R . .
H41C H 1.0913 0.2084 0.1173 0.054 Uiso 1 1 calc R . .
C42 C 0.9402(3) 0.1565(2) 0.19787(11) 0.0265(7) Uani 1 1 d . . .
H42 H 0.9248 0.1236 0.1678 0.032 Uiso 1 1 calc R . .
C43 C 0.8441(3) 0.1160(2) 0.22900(11) 0.0301(8) Uani 1 1 d . . .
H43A H 0.8639 0.0539 0.2330 0.045 Uiso 1 1 calc R . .
H43B H 0.7507 0.1235 0.2143 0.045 Uiso 1 1 calc R . .
H43C H 0.8563 0.1446 0.2595 0.045 Uiso 1 1 calc R . .
C44 C 1.0870(3) 0.1385(2) 0.21805(11) 0.0326(8) Uani 1 1 d . . .
H44A H 1.1103 0.1724 0.2467 0.049 Uiso 1 1 calc R . .
H44B H 1.1465 0.1552 0.1952 0.049 Uiso 1 1 calc R . .
H44C H 1.0982 0.0765 0.2252 0.049 Uiso 1 1 calc R . .
C45 C 0.5653(3) 0.2653(2) 0.23425(11) 0.0317(8) Uani 1 1 d . . .
H45 H 0.6584 0.2483 0.2483 0.038 Uiso 1 1 calc R . .
C46 C 0.4636(3) 0.1946(2) 0.24222(12) 0.0405(9) Uani 1 1 d . . .
H46A H 0.3750 0.2123 0.2255 0.049 Uiso 1 1 calc R . .
H46B H 0.4906 0.1410 0.2269 0.049 Uiso 1 1 calc R . .
C47 C 0.4437(5) 0.1721(4) 0.28884(16) 0.0892(18) Uani 1 1 d . . .
H47A H 0.3987 0.1147 0.2871 0.107 Uiso 1 1 calc R . .
H47B H 0.3781 0.2143 0.2985 0.107 Uiso 1 1 calc R . .
C48 C 0.5571(5) 0.1671(3) 0.32776(15) 0.0735(14) Uani 1 1 d . . .
H48A H 0.5356 0.1200 0.3489 0.088 Uiso 1 1 calc R . .
H48B H 0.6384 0.1486 0.3142 0.088 Uiso 1 1 calc R . .
C49 C 0.5945(5) 0.2448(3) 0.35691(15) 0.0624(12) Uani 1 1 d . . .
H49A H 0.6630 0.2267 0.3830 0.075 Uiso 1 1 calc R . .
H49B H 0.5136 0.2631 0.3707 0.075 Uiso 1 1 calc R . .
C50 C 0.6482(6) 0.3233(4) 0.33485(17) 0.0986(18) Uani 1 1 d U . .
H50A H 0.6823 0.3645 0.3599 0.118 Uiso 1 1 calc R . .
H50B H 0.7260 0.3051 0.3193 0.118 Uiso 1 1 calc R . .
C51 C 0.5510(7) 0.3703(3) 0.30006(17) 0.1006(18) Uani 1 1 d U . .
H51 H 0.5023 0.4172 0.3111 0.121 Uiso 1 1 calc R . .
C52 C 0.5261(4) 0.3512(2) 0.25335(13) 0.0461(10) Uani 1 1 d . . .
H52 H 0.4830 0.3934 0.2325 0.055 Uiso 1 1 calc R . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ge1 N1 1.890(2) . ?
Ge1 C45 2.034(3) . ?
Si1 N1 1.790(2) . ?
Si1 C39 1.895(3) . ?
Si1 C36 1.896(3) . ?
Si1 C42 1.915(3) . ?
N1 C1 1.459(4) . ?
C1 C6 1.415(4) . ?
C1 C2 1.417(4) . ?
C2 C3 1.392(4) . ?
C2 C23 1.536(4) . ?
C3 C4 1.392(4) . ?
C4 C5 1.392(4) . ?
C4 C7 1.518(4) . ?
C5 C6 1.388(4) . ?
C6 C10 1.531(4) . ?
C7 C8 1.513(4) . ?
C7 C9 1.513(4) . ?
C10 C17 1.520(4) . ?
C10 C11 1.540(4) . ?
C11 C16 1.379(4) . ?
C11 C12 1.383(4) . ?
C12 C13 1.383(4) . ?
C13 C14 1.373(5) . ?
C14 C15 1.367(5) . ?
C15 C16 1.390(5) . ?
C17 C22 1.382(4) . ?
C17 C18 1.386(4) . ?
C18 C19 1.383(4) . ?
C19 C20 1.368(5) . ?
C20 C21 1.362(5) . ?
C21 C22 1.383(4) . ?
C23 C24 1.527(4) . ?
C23 C30 1.531(4) . ?
C24 C29 1.393(4) . ?
C24 C25 1.393(4) . ?
C25 C26 1.385(4) . ?
C26 C27 1.386(4) . ?
C27 C28 1.370(4) . ?
C28 C29 1.382(4) . ?
C30 C35 1.385(4) . ?
C30 C31 1.394(4) . ?
C31 C32 1.397(4) . ?
C32 C33 1.373(4) . ?
C33 C34 1.374(4) . ?
C34 C35 1.386(4) . ?
C36 C38 1.537(5) . ?
C36 C37 1.543(4) . ?
C39 C41 1.529(5) . ?
C39 C40 1.547(4) . ?
C42 C44 1.532(4) . ?
C42 C43 1.535(4) . ?
C45 C52 1.506(5) . ?
C45 C46 1.528(5) . ?
C46 C47 1.431(5) . ?
C47 C48 1.489(6) . ?
C48 C49 1.483(6) . ?
C49 C50 1.499(6) . ?
C50 C51 1.490(7) . ?
C51 C52 1.372(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
N1 Ge1 C45 108.70(11) . . ?
N1 Si1 C39 109.84(13) . . ?
N1 Si1 C36 107.19(13) . . ?
C39 Si1 C36 109.58(14) . . ?
N1 Si1 C42 109.88(12) . . ?
C39 Si1 C42 109.27(14) . . ?
C36 Si1 C42 111.05(14) . . ?
C1 N1 Si1 119.86(17) . . ?
C1 N1 Ge1 106.89(16) . . ?
Si1 N1 Ge1 133.12(13) . . ?
C6 C1 C2 118.1(3) . . ?
C6 C1 N1 120.5(2) . . ?
C2 C1 N1 121.4(2) . . ?
C3 C2 C1 119.3(3) . . ?
C3 C2 C23 119.3(2) . . ?
C1 C2 C23 121.3(2) . . ?
C2 C3 C4 123.4(3) . . ?
C3 C4 C5 116.3(3) . . ?
C3 C4 C7 121.6(3) . . ?
C5 C4 C7 122.1(3) . . ?
C6 C5 C4 122.9(3) . . ?
C5 C6 C1 120.0(3) . . ?
C5 C6 C10 119.0(2) . . ?
C1 C6 C10 120.9(2) . . ?
C8 C7 C9 109.7(3) . . ?
C8 C7 C4 112.4(3) . . ?
C9 C7 C4 112.2(2) . . ?
C17 C10 C6 112.7(2) . . ?
C17 C10 C11 112.3(2) . . ?
C6 C10 C11 112.6(2) . . ?
C16 C11 C12 117.4(3) . . ?
C16 C11 C10 123.0(3) . . ?
C12 C11 C10 119.6(3) . . ?
C11 C12 C13 121.7(3) . . ?
C14 C13 C12 120.0(3) . . ?
C15 C14 C13 119.4(3) . . ?
C14 C15 C16 120.4(3) . . ?
C11 C16 C15 121.1(3) . . ?
C22 C17 C18 116.9(3) . . ?
C22 C17 C10 119.9(3) . . ?
C18 C17 C10 123.1(3) . . ?
C19 C18 C17 120.9(3) . . ?
C20 C19 C18 120.7(3) . . ?
C21 C20 C19 119.5(3) . . ?
C20 C21 C22 119.9(3) . . ?
C21 C22 C17 122.1(3) . . ?
C24 C23 C30 111.8(2) . . ?
C24 C23 C2 112.0(2) . . ?
C30 C23 C2 112.5(2) . . ?
C29 C24 C25 117.6(3) . . ?
C29 C24 C23 120.0(3) . . ?
C25 C24 C23 122.3(3) . . ?
C26 C25 C24 121.0(3) . . ?
C27 C26 C25 120.2(3) . . ?
C28 C27 C26 119.4(3) . . ?
C27 C28 C29 120.4(3) . . ?
C28 C29 C24 121.3(3) . . ?
C35 C30 C31 117.3(3) . . ?
C35 C30 C23 120.2(3) . . ?
C31 C30 C23 122.5(3) . . ?
C30 C31 C32 120.7(3) . . ?
C33 C32 C31 120.6(3) . . ?
C34 C33 C32 119.4(3) . . ?
C33 C34 C35 120.2(3) . . ?
C30 C35 C34 121.9(3) . . ?
C38 C36 C37 110.4(3) . . ?
C38 C36 Si1 113.1(2) . . ?
C37 C36 Si1 116.6(2) . . ?
C41 C39 C40 109.6(3) . . ?
C41 C39 Si1 115.6(2) . . ?
C40 C39 Si1 112.8(2) . . ?
C44 C42 C43 110.3(2) . . ?
C44 C42 Si1 116.5(2) . . ?
C43 C42 Si1 112.6(2) . . ?
C52 C45 C46 111.1(3) . . ?
C52 C45 Ge1 106.9(2) . . ?
C46 C45 Ge1 106.4(2) . . ?
C47 C46 C45 119.6(3) . . ?
C46 C47 C48 122.5(4) . . ?
C49 C48 C47 119.8(4) . . ?
C48 C49 C50 119.1(4) . . ?
C51 C50 C49 116.1(5) . . ?
C52 C51 C50 125.2(5) . . ?
C51 C52 C45 121.8(4) . . ?

_diffrn_measured_fraction_theta_max 0.957
_diffrn_reflns_theta_full        25.10
_diffrn_measured_fraction_theta_full 0.957
_refine_diff_density_max         0.686
_refine_diff_density_min         -0.437
_refine_diff_density_rms         0.063
####################################################################### 
# 
# 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_compound17
_database_code_depnum_ccdc_archive 'CCDC 1422737'
_audit_update_record             
;
2015-09-07 deposited with the CCDC.
2015-09-22 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C49 H63 Ge N Si'
_chemical_formula_weight         766.68

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'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   P2(1)/n

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

_cell_length_a                   11.3740(4)
_cell_length_b                   23.3065(8)
_cell_length_c                   16.3439(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 97.891(2)
_cell_angle_gamma                90.00
_cell_volume                     4291.5(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    123(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.25
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.187
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1640
_exptl_absorpt_coefficient_mu    0.775
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.798
_exptl_absorpt_correction_T_max  0.821
_exptl_absorpt_process_details   'SCALE3 ABSPACK'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      123(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Oxford Gemini Ultra'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            88866
_diffrn_reflns_av_R_equivalents  0.0835
_diffrn_reflns_av_sigmaI/netI    0.0489
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         2.92
_diffrn_reflns_theta_max         26.00
_reflns_number_total             8398
_reflns_number_gt                6416
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       CrysalisPro
_computing_cell_refinement       CrysalisPro
_computing_data_reduction        CrysalisPro
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    X-Seed
_computing_publication_material  CifTAB

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0383P)²+5.9394P] 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         8398
_refine_ls_number_parameters     479
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0698
_refine_ls_R_factor_gt           0.0457
_refine_ls_wR_factor_ref         0.1093
_refine_ls_wR_factor_gt          0.0989
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_restrained_S_all      1.029
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ge1 Ge 0.40560(3) 0.205974(12) 0.106590(18) 0.02448(10) Uani 1 1 d . . .
Si1 Si 0.47331(6) 0.33433(3) 0.14891(4) 0.01495(16) Uani 1 1 d . . .
N1 N 0.40042(19) 0.28351(9) 0.07653(13) 0.0154(5) Uani 1 1 d . . .
C1 C 0.3372(2) 0.30134(10) -0.00141(15) 0.0143(5) Uani 1 1 d . . .
C2 C 0.3970(2) 0.30668(10) -0.07158(15) 0.0148(5) Uani 1 1 d . . .
C3 C 0.3349(2) 0.32650(11) -0.14576(15) 0.0160(5) Uani 1 1 d . . .
H3 H 0.3757 0.3294 -0.1926 0.019 Uiso 1 1 calc R . .
C4 C 0.2167(2) 0.34211(11) -0.15408(15) 0.0158(5) Uani 1 1 d . . .
C5 C 0.1583(2) 0.33426(11) -0.08533(15) 0.0161(5) Uani 1 1 d . . .
H5 H 0.0762 0.3431 -0.0901 0.019 Uiso 1 1 calc R . .
C6 C 0.2148(2) 0.31408(11) -0.01041(15) 0.0148(5) Uani 1 1 d . . .
C7 C 0.1498(2) 0.36920(12) -0.23168(16) 0.0193(6) Uani 1 1 d . . .
H7 H 0.0780 0.3451 -0.2491 0.023 Uiso 1 1 calc R . .
C8 C 0.2200(3) 0.37201(14) -0.30399(17) 0.0306(7) Uani 1 1 d . . .
H8A H 0.2883 0.3976 -0.2902 0.046 Uiso 1 1 calc R . .
H8B H 0.1692 0.3868 -0.3527 0.046 Uiso 1 1 calc R . .
H8C H 0.2480 0.3335 -0.3158 0.046 Uiso 1 1 calc R . .
C9 C 0.1067(3) 0.42901(14) -0.2133(2) 0.0379(8) Uani 1 1 d . . .
H9A H 0.1751 0.4541 -0.1976 0.057 Uiso 1 1 calc R . .
H9B H 0.0589 0.4270 -0.1679 0.057 Uiso 1 1 calc R . .
H9C H 0.0582 0.4444 -0.2627 0.057 Uiso 1 1 calc R . .
C10 C 0.5280(2) 0.29075(11) -0.06787(15) 0.0157(5) Uani 1 1 d . . .
H10 H 0.5625 0.2924 -0.0082 0.019 Uiso 1 1 calc R . .
C11 C 0.6017(2) 0.33258(11) -0.11326(15) 0.0166(5) Uani 1 1 d . . .
C12 C 0.7070(2) 0.31396(12) -0.13911(17) 0.0209(6) Uani 1 1 d . . .
H12 H 0.7312 0.2752 -0.1296 0.025 Uiso 1 1 calc R . .
C13 C 0.7772(3) 0.35056(13) -0.17842(18) 0.0280(7) Uani 1 1 d . . .
H13 H 0.8484 0.3367 -0.1958 0.034 Uiso 1 1 calc R . .
C14 C 0.7441(3) 0.40699(13) -0.19239(19) 0.0305(7) Uani 1 1 d . . .
H14 H 0.7912 0.4321 -0.2201 0.037 Uiso 1 1 calc R . .
C15 C 0.6409(3) 0.42649(12) -0.16548(18) 0.0273(7) Uani 1 1 d . . .
H15 H 0.6180 0.4654 -0.1742 0.033 Uiso 1 1 calc R . .
C16 C 0.5710(2) 0.39006(11) -0.12614(16) 0.0206(6) Uani 1 1 d . . .
H16 H 0.5010 0.4044 -0.1076 0.025 Uiso 1 1 calc R . .
C17 C 0.5432(2) 0.22869(11) -0.09567(16) 0.0182(6) Uani 1 1 d . . .
C18 C 0.6107(3) 0.18994(12) -0.04444(18) 0.0248(6) Uani 1 1 d . . .
H18 H 0.6472 0.2021 0.0085 0.030 Uiso 1 1 calc R . .
C19 C 0.6256(3) 0.13381(13) -0.0693(2) 0.0337(7) Uani 1 1 d . . .
H19 H 0.6713 0.1077 -0.0332 0.040 Uiso 1 1 calc R . .
C20 C 0.5740(3) 0.11588(13) -0.1463(2) 0.0334(8) Uani 1 1 d . . .
H20 H 0.5834 0.0774 -0.1633 0.040 Uiso 1 1 calc R . .
C21 C 0.5085(3) 0.15403(13) -0.19888(19) 0.0287(7) Uani 1 1 d . . .
H21 H 0.4740 0.1419 -0.2523 0.034 Uiso 1 1 calc R . .
C22 C 0.4929(2) 0.21017(12) -0.17370(17) 0.0216(6) Uani 1 1 d . . .
H22 H 0.4476 0.2362 -0.2101 0.026 Uiso 1 1 calc R . .
C23 C 0.1414(2) 0.30753(11) 0.06108(15) 0.0157(5) Uani 1 1 d . . .
H23 H 0.1984 0.3111 0.1131 0.019 Uiso 1 1 calc R . .
C24 C 0.0521(2) 0.35671(11) 0.06211(15) 0.0175(6) Uani 1 1 d . . .
C25 C 0.0930(3) 0.41086(12) 0.08856(17) 0.0230(6) Uani 1 1 d . . .
H25 H 0.1752 0.4162 0.1071 0.028 Uiso 1 1 calc R . .
C26 C 0.0171(3) 0.45685(12) 0.08843(19) 0.0296(7) Uani 1 1 d . . .
H26 H 0.0471 0.4932 0.1075 0.036 Uiso 1 1 calc R . .
C27 C -0.1029(3) 0.45049(13) 0.06069(18) 0.0279(7) Uani 1 1 d . . .
H27 H -0.1555 0.4822 0.0604 0.033 Uiso 1 1 calc R . .
C28 C -0.1442(3) 0.39763(13) 0.03370(18) 0.0282(7) Uani 1 1 d . . .
H28 H -0.2260 0.3929 0.0135 0.034 Uiso 1 1 calc R . .
C29 C -0.0683(2) 0.35084(12) 0.03535(17) 0.0244(6) Uani 1 1 d . . .
H29 H -0.0993 0.3143 0.0179 0.029 Uiso 1 1 calc R . .
C30 C 0.0822(2) 0.24911(11) 0.06456(16) 0.0163(5) Uani 1 1 d . . .
C31 C 0.0229(2) 0.22204(12) -0.00537(17) 0.0220(6) Uani 1 1 d . . .
H31 H 0.0226 0.2391 -0.0582 0.026 Uiso 1 1 calc R . .
C32 C -0.0356(3) 0.17056(12) 0.00140(17) 0.0252(6) Uani 1 1 d . . .
H32 H -0.0764 0.1529 -0.0466 0.030 Uiso 1 1 calc R . .
C33 C -0.0349(3) 0.14474(12) 0.07748(18) 0.0272(7) Uani 1 1 d . . .
H33 H -0.0752 0.1094 0.0819 0.033 Uiso 1 1 calc R . .
C34 C 0.0246(3) 0.17056(12) 0.14713(17) 0.0259(7) Uani 1 1 d . . .
H34 H 0.0261 0.1528 0.1996 0.031 Uiso 1 1 calc R . .
C35 C 0.0821(2) 0.22231(12) 0.14065(16) 0.0202(6) Uani 1 1 d . . .
H35 H 0.1222 0.2399 0.1890 0.024 Uiso 1 1 calc R . .
C36 C 0.5151(2) 0.39964(11) 0.09026(16) 0.0170(6) Uani 1 1 d . . .
H36 H 0.5543 0.3851 0.0431 0.020 Uiso 1 1 calc R . .
C37 C 0.6056(2) 0.43921(12) 0.14167(17) 0.0227(6) Uani 1 1 d . . .
H37A H 0.6249 0.4715 0.1075 0.034 Uiso 1 1 calc R . .
H37B H 0.6780 0.4175 0.1608 0.034 Uiso 1 1 calc R . .
H37C H 0.5714 0.4538 0.1895 0.034 Uiso 1 1 calc R . .
C38 C 0.4077(2) 0.43544(11) 0.05249(17) 0.0207(6) Uani 1 1 d . . .
H38A H 0.3634 0.4484 0.0964 0.031 Uiso 1 1 calc R . .
H38B H 0.3560 0.4119 0.0129 0.031 Uiso 1 1 calc R . .
H38C H 0.4353 0.4688 0.0240 0.031 Uiso 1 1 calc R . .
C39 C 0.3685(2) 0.35524(11) 0.22516(16) 0.0187(6) Uani 1 1 d . . .
H39 H 0.2918 0.3653 0.1907 0.022 Uiso 1 1 calc R . .
C40 C 0.4016(3) 0.40801(12) 0.28050(17) 0.0249(6) Uani 1 1 d . . .
H40A H 0.3419 0.4135 0.3177 0.037 Uiso 1 1 calc R . .
H40B H 0.4043 0.4422 0.2458 0.037 Uiso 1 1 calc R . .
H40C H 0.4796 0.4019 0.3131 0.037 Uiso 1 1 calc R . .
C41 C 0.3407(3) 0.30369(11) 0.27777(16) 0.0217(6) Uani 1 1 d . . .
H41A H 0.4120 0.2930 0.3154 0.033 Uiso 1 1 calc R . .
H41B H 0.3152 0.2712 0.2416 0.033 Uiso 1 1 calc R . .
H41C H 0.2772 0.3140 0.3099 0.033 Uiso 1 1 calc R . .
C42 C 0.6092(2) 0.29762(12) 0.20644(17) 0.0230(6) Uani 1 1 d . . .
H42 H 0.5835 0.2579 0.2186 0.028 Uiso 1 1 calc R . .
C43 C 0.7103(3) 0.29068(14) 0.15419(19) 0.0330(7) Uani 1 1 d . . .
H43A H 0.7413 0.3286 0.1423 0.050 Uiso 1 1 calc R . .
H43B H 0.6804 0.2714 0.1022 0.050 Uiso 1 1 calc R . .
H43C H 0.7740 0.2677 0.1846 0.050 Uiso 1 1 calc R . .
C44 C 0.6586(3) 0.32395(13) 0.28982(17) 0.0277(7) Uani 1 1 d . . .
H44A H 0.7234 0.3000 0.3168 0.042 Uiso 1 1 calc R . .
H44B H 0.5954 0.3261 0.3249 0.042 Uiso 1 1 calc R . .
H44C H 0.6885 0.3626 0.2812 0.042 Uiso 1 1 calc R . .
C45 C 0.3188(3) 0.16445(12) 0.01051(17) 0.0233(6) Uani 1 1 d . . .
H45A H 0.2464 0.1858 -0.0123 0.028 Uiso 1 1 calc R . .
H45B H 0.3697 0.1599 -0.0335 0.028 Uiso 1 1 calc R . .
C46 C 0.2859(3) 0.10555(14) 0.0430(2) 0.0435(9) Uani 1 1 d . . .
H46A H 0.3599 0.0861 0.0674 0.052 Uiso 1 1 calc R . .
H46B H 0.2372 0.1118 0.0880 0.052 Uiso 1 1 calc R . .
C47 C 0.2187(4) 0.06562(16) -0.0200(3) 0.0558(11) Uani 1 1 d . . .
H47 H 0.1509 0.0868 -0.0519 0.067 Uiso 1 1 calc R . .
C48 C 0.1701(5) 0.01453(18) 0.0262(4) 0.0909(18) Uani 1 1 d . . .
H48A H 0.1300 -0.0127 -0.0141 0.136 Uiso 1 1 calc R . .
H48B H 0.1136 0.0288 0.0616 0.136 Uiso 1 1 calc R . .
H48C H 0.2360 -0.0048 0.0602 0.136 Uiso 1 1 calc R . .
C49 C 0.2982(5) 0.0439(2) -0.0776(3) 0.0813(15) Uani 1 1 d . . .
H49A H 0.3334 0.0764 -0.1036 0.122 Uiso 1 1 calc R . .
H49B H 0.2525 0.0203 -0.1203 0.122 Uiso 1 1 calc R . .
H49C H 0.3613 0.0207 -0.0470 0.122 Uiso 1 1 calc R . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ge1 N1 1.872(2) . ?
Ge1 C45 1.988(3) . ?
Si1 N1 1.794(2) . ?
Si1 C36 1.894(3) . ?
Si1 C42 1.899(3) . ?
Si1 C39 1.902(3) . ?
N1 C1 1.435(3) . ?
C1 C6 1.412(4) . ?
C1 C2 1.417(3) . ?
C2 C3 1.396(3) . ?
C2 C10 1.529(3) . ?
C3 C4 1.381(4) . ?
C3 H3 0.9500 . ?
C4 C5 1.393(3) . ?
C4 C7 1.524(4) . ?
C5 C6 1.384(4) . ?
C5 H5 0.9500 . ?
C6 C23 1.534(3) . ?
C7 C8 1.516(4) . ?
C7 C9 1.521(4) . ?
C7 H7 1.0000 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 C17 1.533(4) . ?
C10 C11 1.541(4) . ?
C10 H10 1.0000 . ?
C11 C12 1.393(4) . ?
C11 C16 1.393(4) . ?
C12 C13 1.386(4) . ?
C12 H12 0.9500 . ?
C13 C14 1.379(4) . ?
C13 H13 0.9500 . ?
C14 C15 1.385(4) . ?
C14 H14 0.9500 . ?
C15 C16 1.382(4) . ?
C15 H15 0.9500 . ?
C16 H16 0.9500 . ?
C17 C18 1.389(4) . ?
C17 C22 1.393(4) . ?
C18 C19 1.387(4) . ?
C18 H18 0.9500 . ?
C19 C20 1.380(5) . ?
C19 H19 0.9500 . ?
C20 C21 1.381(4) . ?
C20 H20 0.9500 . ?
C21 C22 1.390(4) . ?
C21 H21 0.9500 . ?
C22 H22 0.9500 . ?
C23 C30 1.523(4) . ?
C23 C24 1.533(4) . ?
C23 H23 1.0000 . ?
C24 C29 1.385(4) . ?
C24 C25 1.393(4) . ?
C25 C26 1.377(4) . ?
C25 H25 0.9500 . ?
C26 C27 1.386(4) . ?
C26 H26 0.9500 . ?
C27 C28 1.369(4) . ?
C27 H27 0.9500 . ?
C28 C29 1.389(4) . ?
C28 H28 0.9500 . ?
C29 H29 0.9500 . ?
C30 C35 1.392(4) . ?
C30 C31 1.396(4) . ?
C31 C32 1.383(4) . ?
C31 H31 0.9500 . ?
C32 C33 1.381(4) . ?
C32 H32 0.9500 . ?
C33 C34 1.380(4) . ?
C33 H33 0.9500 . ?
C34 C35 1.383(4) . ?
C34 H34 0.9500 . ?
C35 H35 0.9500 . ?
C36 C38 1.537(4) . ?
C36 C37 1.542(4) . ?
C36 H36 1.0000 . ?
C37 H37A 0.9800 . ?
C37 H37B 0.9800 . ?
C37 H37C 0.9800 . ?
C38 H38A 0.9800 . ?
C38 H38B 0.9800 . ?
C38 H38C 0.9800 . ?
C39 C41 1.535(4) . ?
C39 C40 1.542(4) . ?
C39 H39 1.0000 . ?
C40 H40A 0.9800 . ?
C40 H40B 0.9800 . ?
C40 H40C 0.9800 . ?
C41 H41A 0.9800 . ?
C41 H41B 0.9800 . ?
C41 H41C 0.9800 . ?
C42 C44 1.529(4) . ?
C42 C43 1.532(4) . ?
C42 H42 1.0000 . ?
C43 H43A 0.9800 . ?
C43 H43B 0.9800 . ?
C43 H43C 0.9800 . ?
C44 H44A 0.9800 . ?
C44 H44B 0.9800 . ?
C44 H44C 0.9800 . ?
C45 C46 1.537(4) . ?
C45 H45A 0.9900 . ?
C45 H45B 0.9900 . ?
C46 C47 1.515(5) . ?
C46 H46A 0.9900 . ?
C46 H46B 0.9900 . ?
C47 C49 1.480(6) . ?
C47 C48 1.552(6) . ?
C47 H47 1.0000 . ?
C48 H48A 0.9800 . ?
C48 H48B 0.9800 . ?
C48 H48C 0.9800 . ?
C49 H49A 0.9800 . ?
C49 H49B 0.9800 . ?
C49 H49C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Ge1 C45 105.57(10) . . ?
N1 Si1 C36 108.79(11) . . ?
N1 Si1 C42 107.46(11) . . ?
C36 Si1 C42 111.64(12) . . ?
N1 Si1 C39 109.06(11) . . ?
C36 Si1 C39 110.44(12) . . ?
C42 Si1 C39 109.37(12) . . ?
C1 N1 Si1 121.58(16) . . ?
C1 N1 Ge1 120.42(16) . . ?
Si1 N1 Ge1 117.98(11) . . ?
C6 C1 C2 118.3(2) . . ?
C6 C1 N1 121.3(2) . . ?
C2 C1 N1 120.4(2) . . ?
C3 C2 C1 119.3(2) . . ?
C3 C2 C10 119.3(2) . . ?
C1 C2 C10 121.4(2) . . ?
C4 C3 C2 122.9(2) . . ?
C4 C3 H3 118.6 . . ?
C2 C3 H3 118.6 . . ?
C3 C4 C5 116.8(2) . . ?
C3 C4 C7 124.0(2) . . ?
C5 C4 C7 119.1(2) . . ?
C6 C5 C4 122.9(2) . . ?
C6 C5 H5 118.5 . . ?
C4 C5 H5 118.5 . . ?
C5 C6 C1 119.6(2) . . ?
C5 C6 C23 118.2(2) . . ?
C1 C6 C23 122.1(2) . . ?
C8 C7 C9 109.4(2) . . ?
C8 C7 C4 114.2(2) . . ?
C9 C7 C4 110.7(2) . . ?
C8 C7 H7 107.4 . . ?
C9 C7 H7 107.4 . . ?
C4 C7 H7 107.4 . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C7 C9 H9A 109.5 . . ?
C7 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C7 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C2 C10 C17 111.5(2) . . ?
C2 C10 C11 114.7(2) . . ?
C17 C10 C11 111.3(2) . . ?
C2 C10 H10 106.2 . . ?
C17 C10 H10 106.2 . . ?
C11 C10 H10 106.2 . . ?
C12 C11 C16 117.5(2) . . ?
C12 C11 C10 119.7(2) . . ?
C16 C11 C10 122.7(2) . . ?
C13 C12 C11 121.6(3) . . ?
C13 C12 H12 119.2 . . ?
C11 C12 H12 119.2 . . ?
C14 C13 C12 120.1(3) . . ?
C14 C13 H13 119.9 . . ?
C12 C13 H13 119.9 . . ?
C13 C14 C15 119.0(3) . . ?
C13 C14 H14 120.5 . . ?
C15 C14 H14 120.5 . . ?
C16 C15 C14 120.9(3) . . ?
C16 C15 H15 119.6 . . ?
C14 C15 H15 119.6 . . ?
C15 C16 C11 120.8(3) . . ?
C15 C16 H16 119.6 . . ?
C11 C16 H16 119.6 . . ?
C18 C17 C22 118.3(3) . . ?
C18 C17 C10 120.7(2) . . ?
C22 C17 C10 121.0(2) . . ?
C19 C18 C17 121.1(3) . . ?
C19 C18 H18 119.4 . . ?
C17 C18 H18 119.4 . . ?
C20 C19 C18 119.9(3) . . ?
C20 C19 H19 120.0 . . ?
C18 C19 H19 120.0 . . ?
C19 C20 C21 119.9(3) . . ?
C19 C20 H20 120.1 . . ?
C21 C20 H20 120.1 . . ?
C20 C21 C22 120.1(3) . . ?
C20 C21 H21 119.9 . . ?
C22 C21 H21 119.9 . . ?
C21 C22 C17 120.7(3) . . ?
C21 C22 H22 119.7 . . ?
C17 C22 H22 119.7 . . ?
C30 C23 C24 111.8(2) . . ?
C30 C23 C6 114.0(2) . . ?
C24 C23 C6 111.4(2) . . ?
C30 C23 H23 106.4 . . ?
C24 C23 H23 106.4 . . ?
C6 C23 H23 106.4 . . ?
C29 C24 C25 117.5(3) . . ?
C29 C24 C23 123.4(2) . . ?
C25 C24 C23 119.1(2) . . ?
C26 C25 C24 121.5(3) . . ?
C26 C25 H25 119.3 . . ?
C24 C25 H25 119.3 . . ?
C25 C26 C27 120.5(3) . . ?
C25 C26 H26 119.8 . . ?
C27 C26 H26 119.8 . . ?
C28 C27 C26 118.7(3) . . ?
C28 C27 H27 120.6 . . ?
C26 C27 H27 120.6 . . ?
C27 C28 C29 121.0(3) . . ?
C27 C28 H28 119.5 . . ?
C29 C28 H28 119.5 . . ?
C24 C29 C28 120.9(3) . . ?
C24 C29 H29 119.6 . . ?
C28 C29 H29 119.6 . . ?
C35 C30 C31 118.0(2) . . ?
C35 C30 C23 119.3(2) . . ?
C31 C30 C23 122.7(2) . . ?
C32 C31 C30 120.7(2) . . ?
C32 C31 H31 119.7 . . ?
C30 C31 H31 119.7 . . ?
C33 C32 C31 120.5(3) . . ?
C33 C32 H32 119.8 . . ?
C31 C32 H32 119.8 . . ?
C34 C33 C32 119.6(3) . . ?
C34 C33 H33 120.2 . . ?
C32 C33 H33 120.2 . . ?
C33 C34 C35 120.0(3) . . ?
C33 C34 H34 120.0 . . ?
C35 C34 H34 120.0 . . ?
C34 C35 C30 121.2(3) . . ?
C34 C35 H35 119.4 . . ?
C30 C35 H35 119.4 . . ?
C38 C36 C37 109.2(2) . . ?
C38 C36 Si1 113.48(18) . . ?
C37 C36 Si1 113.58(18) . . ?
C38 C36 H36 106.7 . . ?
C37 C36 H36 106.7 . . ?
Si1 C36 H36 106.7 . . ?
C36 C37 H37A 109.5 . . ?
C36 C37 H37B 109.5 . . ?
H37A C37 H37B 109.5 . . ?
C36 C37 H37C 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
C36 C38 H38A 109.5 . . ?
C36 C38 H38B 109.5 . . ?
H38A C38 H38B 109.5 . . ?
C36 C38 H38C 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
C41 C39 C40 110.4(2) . . ?
C41 C39 Si1 111.24(18) . . ?
C40 C39 Si1 117.66(19) . . ?
C41 C39 H39 105.5 . . ?
C40 C39 H39 105.5 . . ?
Si1 C39 H39 105.5 . . ?
C39 C40 H40A 109.5 . . ?
C39 C40 H40B 109.5 . . ?
H40A C40 H40B 109.5 . . ?
C39 C40 H40C 109.5 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?
C39 C41 H41A 109.5 . . ?
C39 C41 H41B 109.5 . . ?
H41A C41 H41B 109.5 . . ?
C39 C41 H41C 109.5 . . ?
H41A C41 H41C 109.5 . . ?
H41B C41 H41C 109.5 . . ?
C44 C42 C43 109.1(2) . . ?
C44 C42 Si1 115.8(2) . . ?
C43 C42 Si1 113.19(19) . . ?
C44 C42 H42 106.0 . . ?
C43 C42 H42 106.0 . . ?
Si1 C42 H42 106.0 . . ?
C42 C43 H43A 109.5 . . ?
C42 C43 H43B 109.5 . . ?
H43A C43 H43B 109.5 . . ?
C42 C43 H43C 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?
C42 C44 H44A 109.5 . . ?
C42 C44 H44B 109.5 . . ?
H44A C44 H44B 109.5 . . ?
C42 C44 H44C 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
C46 C45 Ge1 106.25(19) . . ?
C46 C45 H45A 110.5 . . ?
Ge1 C45 H45A 110.5 . . ?
C46 C45 H45B 110.5 . . ?
Ge1 C45 H45B 110.5 . . ?
H45A C45 H45B 108.7 . . ?
C47 C46 C45 115.9(3) . . ?
C47 C46 H46A 108.3 . . ?
C45 C46 H46A 108.3 . . ?
C47 C46 H46B 108.3 . . ?
C45 C46 H46B 108.3 . . ?
H46A C46 H46B 107.4 . . ?
C49 C47 C46 110.3(4) . . ?
C49 C47 C48 109.7(4) . . ?
C46 C47 C48 108.7(4) . . ?
C49 C47 H47 109.4 . . ?
C46 C47 H47 109.4 . . ?
C48 C47 H47 109.4 . . ?
C47 C48 H48A 109.5 . . ?
C47 C48 H48B 109.5 . . ?
H48A C48 H48B 109.5 . . ?
C47 C48 H48C 109.5 . . ?
H48A C48 H48C 109.5 . . ?
H48B C48 H48C 109.5 . . ?
C47 C49 H49A 109.5 . . ?
C47 C49 H49B 109.5 . . ?
H49A C49 H49B 109.5 . . ?
C47 C49 H49C 109.5 . . ?
H49A C49 H49C 109.5 . . ?
H49B C49 H49C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C36 Si1 N1 C1 -26.7(2) . . . . ?
C42 Si1 N1 C1 -147.73(19) . . . . ?
C39 Si1 N1 C1 93.8(2) . . . . ?
C36 Si1 N1 Ge1 154.83(12) . . . . ?
C42 Si1 N1 Ge1 33.81(16) . . . . ?
C39 Si1 N1 Ge1 -84.65(14) . . . . ?
C45 Ge1 N1 C1 2.6(2) . . . . ?
C45 Ge1 N1 Si1 -178.97(13) . . . . ?
Si1 N1 C1 C6 -91.4(3) . . . . ?
Ge1 N1 C1 C6 87.1(3) . . . . ?
Si1 N1 C1 C2 88.5(3) . . . . ?
Ge1 N1 C1 C2 -93.1(2) . . . . ?
C6 C1 C2 C3 2.7(4) . . . . ?
N1 C1 C2 C3 -177.2(2) . . . . ?
C6 C1 C2 C10 -176.9(2) . . . . ?
N1 C1 C2 C10 3.3(4) . . . . ?
C1 C2 C3 C4 0.9(4) . . . . ?
C10 C2 C3 C4 -179.6(2) . . . . ?
C2 C3 C4 C5 -3.5(4) . . . . ?
C2 C3 C4 C7 173.9(2) . . . . ?
C3 C4 C5 C6 2.6(4) . . . . ?
C7 C4 C5 C6 -174.9(2) . . . . ?
C4 C5 C6 C1 0.9(4) . . . . ?
C4 C5 C6 C23 179.6(2) . . . . ?
C2 C1 C6 C5 -3.5(4) . . . . ?
N1 C1 C6 C5 176.4(2) . . . . ?
C2 C1 C6 C23 177.8(2) . . . . ?
N1 C1 C6 C23 -2.3(4) . . . . ?
C3 C4 C7 C8 6.4(4) . . . . ?
C5 C4 C7 C8 -176.3(2) . . . . ?
C3 C4 C7 C9 -117.7(3) . . . . ?
C5 C4 C7 C9 59.7(3) . . . . ?
C3 C2 C10 C17 -85.7(3) . . . . ?
C1 C2 C10 C17 93.8(3) . . . . ?
C3 C2 C10 C11 42.0(3) . . . . ?
C1 C2 C10 C11 -138.5(2) . . . . ?
C2 C10 C11 C12 -157.8(2) . . . . ?
C17 C10 C11 C12 -30.0(3) . . . . ?
C2 C10 C11 C16 25.8(3) . . . . ?
C17 C10 C11 C16 153.6(2) . . . . ?
C16 C11 C12 C13 -1.9(4) . . . . ?
C10 C11 C12 C13 -178.5(2) . . . . ?
C11 C12 C13 C14 0.4(4) . . . . ?
C12 C13 C14 C15 1.0(4) . . . . ?
C13 C14 C15 C16 -0.9(4) . . . . ?
C14 C15 C16 C11 -0.7(4) . . . . ?
C12 C11 C16 C15 2.0(4) . . . . ?
C10 C11 C16 C15 178.5(2) . . . . ?
C2 C10 C17 C18 -124.2(3) . . . . ?
C11 C10 C17 C18 106.3(3) . . . . ?
C2 C10 C17 C22 57.8(3) . . . . ?
C11 C10 C17 C22 -71.7(3) . . . . ?
C22 C17 C18 C19 -1.5(4) . . . . ?
C10 C17 C18 C19 -179.5(3) . . . . ?
C17 C18 C19 C20 0.7(5) . . . . ?
C18 C19 C20 C21 0.6(5) . . . . ?
C19 C20 C21 C22 -1.1(5) . . . . ?
C20 C21 C22 C17 0.2(4) . . . . ?
C18 C17 C22 C21 1.0(4) . . . . ?
C10 C17 C22 C21 179.1(2) . . . . ?
C5 C6 C23 C30 89.3(3) . . . . ?
C1 C6 C23 C30 -91.9(3) . . . . ?
C5 C6 C23 C24 -38.3(3) . . . . ?
C1 C6 C23 C24 140.4(2) . . . . ?
C30 C23 C24 C29 -25.0(3) . . . . ?
C6 C23 C24 C29 103.9(3) . . . . ?
C30 C23 C24 C25 157.2(2) . . . . ?
C6 C23 C24 C25 -73.9(3) . . . . ?
C29 C24 C25 C26 0.2(4) . . . . ?
C23 C24 C25 C26 178.1(3) . . . . ?
C24 C25 C26 C27 -0.8(5) . . . . ?
C25 C26 C27 C28 0.1(5) . . . . ?
C26 C27 C28 C29 1.2(5) . . . . ?
C25 C24 C29 C28 1.2(4) . . . . ?
C23 C24 C29 C28 -176.6(2) . . . . ?
C27 C28 C29 C24 -1.9(5) . . . . ?
C24 C23 C30 C35 -94.4(3) . . . . ?
C6 C23 C30 C35 138.2(2) . . . . ?
C24 C23 C30 C31 82.6(3) . . . . ?
C6 C23 C30 C31 -44.8(3) . . . . ?
C35 C30 C31 C32 0.9(4) . . . . ?
C23 C30 C31 C32 -176.1(2) . . . . ?
C30 C31 C32 C33 -0.8(4) . . . . ?
C31 C32 C33 C34 -0.1(4) . . . . ?
C32 C33 C34 C35 0.7(4) . . . . ?
C33 C34 C35 C30 -0.6(4) . . . . ?
C31 C30 C35 C34 -0.2(4) . . . . ?
C23 C30 C35 C34 176.9(2) . . . . ?
N1 Si1 C36 C38 69.5(2) . . . . ?
C42 Si1 C36 C38 -172.12(18) . . . . ?
C39 Si1 C36 C38 -50.2(2) . . . . ?
N1 Si1 C36 C37 -165.08(18) . . . . ?
C42 Si1 C36 C37 -46.7(2) . . . . ?
C39 Si1 C36 C37 75.3(2) . . . . ?
N1 Si1 C39 C41 64.6(2) . . . . ?
C36 Si1 C39 C41 -175.87(18) . . . . ?
C42 Si1 C39 C41 -52.6(2) . . . . ?
N1 Si1 C39 C40 -166.69(19) . . . . ?
C36 Si1 C39 C40 -47.2(2) . . . . ?
C42 Si1 C39 C40 76.1(2) . . . . ?
N1 Si1 C42 C44 -159.0(2) . . . . ?
C36 Si1 C42 C44 81.8(2) . . . . ?
C39 Si1 C42 C44 -40.7(2) . . . . ?
N1 Si1 C42 C43 74.0(2) . . . . ?
C36 Si1 C42 C43 -45.2(2) . . . . ?
C39 Si1 C42 C43 -167.7(2) . . . . ?
N1 Ge1 C45 C46 -161.7(2) . . . . ?
Ge1 C45 C46 C47 -179.7(3) . . . . ?
C45 C46 C47 C49 71.7(5) . . . . ?
C45 C46 C47 C48 -168.1(3) . . . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        26.00
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.853
_refine_diff_density_min         -0.433
_refine_diff_density_rms         0.067
####################################################################### 
# 
# 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_compound20
_database_code_depnum_ccdc_archive 'CCDC 1422738'
_audit_update_record             
;
2015-09-07 deposited with the CCDC.
2015-09-22 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C49 H62 Cl Ge N Si'
_chemical_formula_weight         801.13

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ge Ge 0.1547 1.8001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   P-1

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   10.731(2)
_cell_length_b                   14.446(3)
_cell_length_c                   15.647(3)
_cell_angle_alpha                77.83(3)
_cell_angle_beta                 78.54(3)
_cell_angle_gamma                69.06(3)
_cell_volume                     2194.1(8)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.04
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.02
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.213
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             852
_exptl_absorpt_coefficient_mu    0.819
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.961
_exptl_absorpt_correction_T_max  0.980
_exptl_absorpt_process_details   XDS

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71090
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_source         'Australian Synchrotron'
_diffrn_radiation_monochromator  ?
_diffrn_measurement_device_type  'ADSC Quantum 210r'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            14376
_diffrn_reflns_av_R_equivalents  0.0826
_diffrn_reflns_av_sigmaI/netI    0.1061
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         1.34
_diffrn_reflns_theta_max         25.20
_reflns_number_total             7198
_reflns_number_gt                5978
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Blu-Ice (McPhillips, 2002)'
_computing_cell_refinement       'XDS (Kabsch, 1993)'
_computing_data_reduction        'XDS (Kabsch, 1993)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    X-Seed
_computing_publication_material  CifTAB

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger.
 The ADP of hydrogen H(1), which was located from difference maps, and bonded 
 to the Ge atom was refined isotropically.
 The low value (91.0%) for completeness of data to theta = 25.2 deg. arises 
 from hardware constraints associated with the diffractometer used at the 
 Australian Synchrotron and is common for triclinic data sets on that instrument. 
 Its minimum crystal to detector distance is 72 mm and its
 goniometer only rotates about the phi axis.
 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0927P)²+1.0731P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         7198
_refine_ls_number_parameters     490
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0741
_refine_ls_R_factor_gt           0.0635
_refine_ls_wR_factor_ref         0.1805
_refine_ls_wR_factor_gt          0.1721
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_restrained_S_all      1.044
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ge1 Ge 0.95725(4) 0.88882(3) 0.74681(3) 0.03423(17) Uani 1 1 d D . .
Cl1 Cl 0.92178(11) 0.96072(8) 0.61189(7) 0.0496(3) Uani 1 1 d . . .
Si1 Si 1.25458(10) 0.89299(7) 0.75583(6) 0.0301(2) Uani 1 1 d . . .
N1 N 1.1409(3) 0.8288(2) 0.75417(18) 0.0281(6) Uani 1 1 d . . .
C1 C 1.1841(3) 0.7212(3) 0.7592(2) 0.0267(7) Uani 1 1 d . . .
C2 C 1.2239(3) 0.6755(3) 0.6823(2) 0.0279(7) Uani 1 1 d . . .
C3 C 1.2687(4) 0.5714(3) 0.6899(2) 0.0325(8) Uani 1 1 d . . .
H3 H 1.2916 0.5418 0.6377 0.039 Uiso 1 1 calc R . .
C4 C 1.2813(4) 0.5088(3) 0.7707(2) 0.0344(8) Uani 1 1 d . . .
C5 C 1.2364(4) 0.5542(3) 0.8459(2) 0.0334(8) Uani 1 1 d . . .
H5 H 1.2414 0.5132 0.9020 0.040 Uiso 1 1 calc R . .
C6 C 1.1843(3) 0.6579(3) 0.8421(2) 0.0275(7) Uani 1 1 d . . .
C7 C 1.2200(4) 0.7341(3) 0.5879(2) 0.0304(7) Uani 1 1 d . . .
H7 H 1.1658 0.8056 0.5931 0.036 Uiso 1 1 calc R . .
C8 C 1.3393(5) 0.3949(3) 0.7747(3) 0.0454(10) Uani 1 1 d . . .
H8 H 1.3606 0.3647 0.8359 0.054 Uiso 1 1 calc R . .
C9 C 1.2373(5) 0.3554(4) 0.7564(3) 0.0571(12) Uani 1 1 d . . .
H9A H 1.1570 0.3723 0.8004 0.086 Uiso 1 1 calc R . .
H9B H 1.2757 0.2824 0.7596 0.086 Uiso 1 1 calc R . .
H9C H 1.2126 0.3857 0.6973 0.086 Uiso 1 1 calc R . .
C10 C 1.4702(5) 0.3639(3) 0.7109(3) 0.0467(10) Uani 1 1 d . . .
H10A H 1.5053 0.2907 0.7155 0.070 Uiso 1 1 calc R . .
H10B H 1.5367 0.3877 0.7259 0.070 Uiso 1 1 calc R . .
H10C H 1.4521 0.3936 0.6504 0.070 Uiso 1 1 calc R . .
C11 C 1.1198(4) 0.7004(3) 0.9274(2) 0.0300(7) Uani 1 1 d . . .
H11 H 1.1268 0.7692 0.9176 0.036 Uiso 1 1 calc R . .
C12 C 1.1454(4) 0.6968(3) 0.5353(2) 0.0350(8) Uani 1 1 d . . .
C13 C 1.0161(5) 0.6940(4) 0.5725(3) 0.0541(11) Uani 1 1 d . . .
H13 H 0.9776 0.7151 0.6282 0.065 Uiso 1 1 calc R . .
C14 C 0.9447(6) 0.6605(5) 0.5279(4) 0.0666(14) Uani 1 1 d . . .
H14 H 0.8573 0.6586 0.5534 0.080 Uiso 1 1 calc R . .
C15 C 0.9998(6) 0.6298(4) 0.4470(4) 0.0649(14) Uani 1 1 d . . .
H15 H 0.9511 0.6061 0.4171 0.078 Uiso 1 1 calc R . .
C16 C 1.1256(6) 0.6335(5) 0.4098(4) 0.0709(15) Uani 1 1 d . . .
H16 H 1.1632 0.6134 0.3536 0.085 Uiso 1 1 calc R . .
C17 C 1.1984(5) 0.6669(4) 0.4545(3) 0.0541(11) Uani 1 1 d . . .
H17 H 1.2854 0.6689 0.4285 0.065 Uiso 1 1 calc R . .
C18 C 1.3584(4) 0.7328(3) 0.5393(2) 0.0319(8) Uani 1 1 d . . .
C19 C 1.3665(4) 0.8153(3) 0.4755(2) 0.0364(8) Uani 1 1 d . . .
H19 H 1.2863 0.8674 0.4608 0.044 Uiso 1 1 calc R . .
C20 C 1.4907(5) 0.8218(3) 0.4334(3) 0.0442(10) Uani 1 1 d . . .
H20 H 1.4947 0.8792 0.3917 0.053 Uiso 1 1 calc R . .
C21 C 1.6081(4) 0.7456(3) 0.4516(3) 0.0447(10) Uani 1 1 d . . .
H21 H 1.6929 0.7511 0.4238 0.054 Uiso 1 1 calc R . .
H1 H 0.898(5) 0.807(3) 0.748(3) 0.059(14) Uiso 1 1 d D . .
C22 C 1.6012(4) 0.6609(3) 0.5108(3) 0.0408(9) Uani 1 1 d . . .
H22 H 1.6814 0.6068 0.5218 0.049 Uiso 1 1 calc R . .
C23 C 1.4778(4) 0.6546(3) 0.5541(2) 0.0347(8) Uani 1 1 d . . .
H23 H 1.4745 0.5960 0.5945 0.042 Uiso 1 1 calc R . .
C24 C 0.9682(4) 0.7143(3) 0.9471(2) 0.0310(7) Uani 1 1 d . . .
C25 C 0.9125(4) 0.6532(3) 0.9200(3) 0.0421(9) Uani 1 1 d . . .
H25 H 0.9687 0.6017 0.8869 0.050 Uiso 1 1 calc R . .
C26 C 0.7747(5) 0.6671(4) 0.9410(3) 0.0486(10) Uani 1 1 d . . .
H26 H 0.7382 0.6247 0.9225 0.058 Uiso 1 1 calc R . .
C27 C 0.6913(4) 0.7422(4) 0.9886(3) 0.0480(11) Uani 1 1 d . . .
H27 H 0.5974 0.7526 1.0017 0.058 Uiso 1 1 calc R . .
C28 C 0.7463(4) 0.8024(3) 1.0172(3) 0.0472(10) Uani 1 1 d . . .
H28 H 0.6901 0.8531 1.0510 0.057 Uiso 1 1 calc R . .
C29 C 0.8834(4) 0.7884(3) 0.9962(3) 0.0400(9) Uani 1 1 d . . .
H29 H 0.9197 0.8302 1.0157 0.048 Uiso 1 1 calc R . .
C30 C 1.1933(4) 0.6422(3) 1.0068(2) 0.0332(8) Uani 1 1 d . . .
C31 C 1.1280(5) 0.6041(3) 1.0855(3) 0.0473(10) Uani 1 1 d . . .
H31 H 1.0353 0.6120 1.0899 0.057 Uiso 1 1 calc R . .
C32 C 1.1970(6) 0.5546(4) 1.1577(3) 0.0583(12) Uani 1 1 d . . .
H32 H 1.1509 0.5295 1.2107 0.070 Uiso 1 1 calc R . .
C33 C 1.3306(5) 0.5422(3) 1.1526(3) 0.0552(12) Uani 1 1 d . . .
H33 H 1.3775 0.5080 1.2017 0.066 Uiso 1 1 calc R . .
C34 C 1.3979(5) 0.5800(3) 1.0747(3) 0.0482(10) Uani 1 1 d . . .
H34 H 1.4903 0.5727 1.0709 0.058 Uiso 1 1 calc R . .
C35 C 1.3293(4) 0.6281(3) 1.0031(3) 0.0423(9) Uani 1 1 d . . .
H35 H 1.3763 0.6521 0.9500 0.051 Uiso 1 1 calc R . .
C36 C 1.4280(4) 0.8239(3) 0.7010(2) 0.0338(8) Uani 1 1 d . . .
H36 H 1.4131 0.8060 0.6464 0.041 Uiso 1 1 calc R . .
C37 C 1.5008(4) 0.7242(3) 0.7556(3) 0.0437(9) Uani 1 1 d . . .
H37A H 1.5825 0.6878 0.7197 0.065 Uiso 1 1 calc R . .
H37B H 1.4412 0.6836 0.7743 0.065 Uiso 1 1 calc R . .
H37C H 1.5253 0.7376 0.8078 0.065 Uiso 1 1 calc R . .
C38 C 1.5226(4) 0.8865(4) 0.6700(3) 0.0471(10) Uani 1 1 d . . .
H38A H 1.5444 0.9034 0.7214 0.071 Uiso 1 1 calc R . .
H38B H 1.4781 0.9483 0.6321 0.071 Uiso 1 1 calc R . .
H38C H 1.6056 0.8477 0.6367 0.071 Uiso 1 1 calc R . .
C39 C 1.1779(4) 1.0232(3) 0.6943(2) 0.0368(8) Uani 1 1 d . . .
H39 H 1.0783 1.0383 0.7094 0.044 Uiso 1 1 calc R . .
C40 C 1.2060(5) 1.0290(3) 0.5932(3) 0.0474(10) Uani 1 1 d . . .
H40A H 1.1512 1.0946 0.5657 0.071 Uiso 1 1 calc R . .
H40B H 1.1832 0.9761 0.5763 0.071 Uiso 1 1 calc R . .
H40C H 1.3016 1.0200 0.5734 0.071 Uiso 1 1 calc R . .
C41 C 1.2063(5) 1.1099(3) 0.7204(3) 0.0443(9) Uani 1 1 d . . .
H41A H 1.3018 1.1026 0.7030 0.066 Uiso 1 1 calc R . .
H41B H 1.1839 1.1084 0.7844 0.066 Uiso 1 1 calc R . .
H41C H 1.1512 1.1739 0.6904 0.066 Uiso 1 1 calc R . .
C42 C 1.2675(4) 0.8969(3) 0.8743(2) 0.0346(8) Uani 1 1 d . . .
H42 H 1.2908 0.8259 0.9049 0.042 Uiso 1 1 calc R . .
C43 C 1.1350(4) 0.9550(3) 0.9251(2) 0.0363(8) Uani 1 1 d . . .
H43A H 1.1423 0.9403 0.9883 0.054 Uiso 1 1 calc R . .
H43B H 1.0619 0.9349 0.9146 0.054 Uiso 1 1 calc R . .
H43C H 1.1159 1.0271 0.9049 0.054 Uiso 1 1 calc R . .
C44 C 1.3810(4) 0.9341(3) 0.8844(3) 0.0445(9) Uani 1 1 d . . .
H44A H 1.3708 0.9998 0.8478 0.067 Uiso 1 1 calc R . .
H44B H 1.4684 0.8862 0.8653 0.067 Uiso 1 1 calc R . .
H44C H 1.3759 0.9400 0.9463 0.067 Uiso 1 1 calc R . .
C45 C 0.8392(4) 0.9908(3) 0.8179(3) 0.0361(8) Uani 1 1 d . . .
H45 H 0.8571 0.9659 0.8804 0.043 Uiso 1 1 calc R . .
C46 C 0.8350(4) 1.0999(3) 0.7960(3) 0.0443(9) Uani 1 1 d . . .
H46A H 0.8364 1.1239 0.7318 0.053 Uiso 1 1 calc R . .
H46B H 0.9122 1.1080 0.8157 0.053 Uiso 1 1 calc R . .
C47 C 0.7010(5) 1.1567(4) 0.8476(3) 0.0531(11) Uani 1 1 d . . .
H47A H 0.6645 1.2265 0.8176 0.064 Uiso 1 1 calc R . .
H47B H 0.7132 1.1582 0.9083 0.064 Uiso 1 1 calc R . .
C48 C 0.6061(5) 1.0972(4) 0.8490(4) 0.0555(12) Uani 1 1 d . . .
H48A H 0.5625 1.0827 0.9099 0.067 Uiso 1 1 calc R . .
H48B H 0.5350 1.1365 0.8114 0.067 Uiso 1 1 calc R . .
C49 C 0.6909(4) 0.9999(3) 0.8142(3) 0.0479(10) Uani 1 1 d . . .
H49A H 0.6767 1.0029 0.7530 0.057 Uiso 1 1 calc R . .
H49B H 0.6683 0.9422 0.8518 0.057 Uiso 1 1 calc R . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ge1 N1 1.864(3) . ?
Ge1 C45 1.952(4) . ?
Ge1 Cl1 2.1891(12) . ?
Ge1 H1 1.526(19) . ?
Si1 N1 1.784(3) . ?
Si1 C39 1.894(4) . ?
Si1 C36 1.896(4) . ?
Si1 C42 1.901(4) . ?
N1 C1 1.443(4) . ?
C1 C2 1.413(5) . ?
C1 C6 1.421(5) . ?
C2 C3 1.392(5) . ?
C2 C7 1.540(5) . ?
C3 C4 1.390(5) . ?
C3 H3 0.9500 . ?
C4 C5 1.386(5) . ?
C4 C8 1.528(5) . ?
C5 C6 1.391(5) . ?
C5 H5 0.9500 . ?
C6 C11 1.521(5) . ?
C7 C18 1.524(5) . ?
C7 C12 1.538(5) . ?
C7 H7 1.0000 . ?
C8 C9 1.499(7) . ?
C8 C10 1.533(7) . ?
C8 H8 1.0000 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 C30 1.532(5) . ?
C11 C24 1.541(5) . ?
C11 H11 1.0000 . ?
C12 C17 1.370(6) . ?
C12 C13 1.405(6) . ?
C13 C14 1.389(6) . ?
C13 H13 0.9500 . ?
C14 C15 1.379(8) . ?
C14 H14 0.9500 . ?
C15 C16 1.375(8) . ?
C15 H15 0.9500 . ?
C16 C17 1.400(7) . ?
C16 H16 0.9500 . ?
C17 H17 0.9500 . ?
C18 C23 1.394(5) . ?
C18 C19 1.401(5) . ?
C19 C20 1.390(6) . ?
C19 H19 0.9500 . ?
C20 C21 1.378(6) . ?
C20 H20 0.9500 . ?
C21 C22 1.387(6) . ?
C21 H21 0.9500 . ?
C22 C23 1.388(6) . ?
C22 H22 0.9500 . ?
C23 H23 0.9500 . ?
C24 C29 1.393(5) . ?
C24 C25 1.398(6) . ?
C25 C26 1.399(6) . ?
C25 H25 0.9500 . ?
C26 C27 1.384(7) . ?
C26 H26 0.9500 . ?
C27 C28 1.393(7) . ?
C27 H27 0.9500 . ?
C28 C29 1.392(6) . ?
C28 H28 0.9500 . ?
C29 H29 0.9500 . ?
C30 C35 1.390(6) . ?
C30 C31 1.400(6) . ?
C31 C32 1.396(6) . ?
C31 H31 0.9500 . ?
C32 C33 1.368(7) . ?
C32 H32 0.9500 . ?
C33 C34 1.400(7) . ?
C33 H33 0.9500 . ?
C34 C35 1.383(6) . ?
C34 H34 0.9500 . ?
C35 H35 0.9500 . ?
C36 C38 1.536(5) . ?
C36 C37 1.535(6) . ?
C36 H36 1.0000 . ?
C37 H37A 0.9800 . ?
C37 H37B 0.9800 . ?
C37 H37C 0.9800 . ?
C38 H38A 0.9800 . ?
C38 H38B 0.9800 . ?
C38 H38C 0.9800 . ?
C39 C41 1.537(5) . ?
C39 C40 1.541(6) . ?
C39 H39 1.0000 . ?
C40 H40A 0.9800 . ?
C40 H40B 0.9800 . ?
C40 H40C 0.9800 . ?
C41 H41A 0.9800 . ?
C41 H41B 0.9800 . ?
C41 H41C 0.9800 . ?
C42 C43 1.528(5) . ?
C42 C44 1.541(5) . ?
C42 H42 1.0000 . ?
C43 H43A 0.9800 . ?
C43 H43B 0.9800 . ?
C43 H43C 0.9800 . ?
C44 H44A 0.9800 . ?
C44 H44B 0.9800 . ?
C44 H44C 0.9800 . ?
C45 C46 1.527(5) . ?
C45 C49 1.560(6) . ?
C45 H45 1.0000 . ?
C46 C47 1.539(7) . ?
C46 H46A 0.9900 . ?
C46 H46B 0.9900 . ?
C47 C48 1.545(7) . ?
C47 H47A 0.9900 . ?
C47 H47B 0.9900 . ?
C48 C49 1.520(7) . ?
C48 H48A 0.9900 . ?
C48 H48B 0.9900 . ?
C49 H49A 0.9900 . ?
C49 H49B 0.9900 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Ge1 C45 122.92(14) . . ?
N1 Ge1 Cl1 111.09(10) . . ?
C45 Ge1 Cl1 103.14(12) . . ?
N1 Ge1 H1 108.3(19) . . ?
C45 Ge1 H1 113(2) . . ?
Cl1 Ge1 H1 95.2(18) . . ?
N1 Si1 C39 104.55(16) . . ?
N1 Si1 C36 109.57(15) . . ?
C39 Si1 C36 112.81(18) . . ?
N1 Si1 C42 109.89(15) . . ?
C39 Si1 C42 111.52(17) . . ?
C36 Si1 C42 108.44(17) . . ?
C1 N1 Si1 122.1(2) . . ?
C1 N1 Ge1 112.3(2) . . ?
Si1 N1 Ge1 125.58(16) . . ?
C2 C1 C6 117.7(3) . . ?
C2 C1 N1 121.4(3) . . ?
C6 C1 N1 120.8(3) . . ?
C3 C2 C1 119.6(3) . . ?
C3 C2 C7 116.4(3) . . ?
C1 C2 C7 123.9(3) . . ?
C4 C3 C2 122.8(3) . . ?
C4 C3 H3 118.6 . . ?
C2 C3 H3 118.6 . . ?
C5 C4 C3 117.1(3) . . ?
C5 C4 C8 122.5(3) . . ?
C3 C4 C8 120.5(3) . . ?
C4 C5 C6 122.4(3) . . ?
C4 C5 H5 118.8 . . ?
C6 C5 H5 118.8 . . ?
C5 C6 C1 120.0(3) . . ?
C5 C6 C11 118.5(3) . . ?
C1 C6 C11 121.4(3) . . ?
C18 C7 C12 111.7(3) . . ?
C18 C7 C2 113.5(3) . . ?
C12 C7 C2 110.3(3) . . ?
C18 C7 H7 107.0 . . ?
C12 C7 H7 107.0 . . ?
C2 C7 H7 107.0 . . ?
C9 C8 C4 110.4(4) . . ?
C9 C8 C10 111.0(4) . . ?
C4 C8 C10 111.5(3) . . ?
C9 C8 H8 108.0 . . ?
C4 C8 H8 108.0 . . ?
C10 C8 H8 108.0 . . ?
C8 C9 H9A 109.5 . . ?
C8 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C8 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C8 C10 H10A 109.5 . . ?
C8 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C8 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C6 C11 C30 113.8(3) . . ?
C6 C11 C24 111.9(3) . . ?
C30 C11 C24 111.8(3) . . ?
C6 C11 H11 106.2 . . ?
C30 C11 H11 106.2 . . ?
C24 C11 H11 106.2 . . ?
C17 C12 C13 118.9(4) . . ?
C17 C12 C7 123.3(4) . . ?
C13 C12 C7 117.7(3) . . ?
C14 C13 C12 120.1(5) . . ?
C14 C13 H13 120.0 . . ?
C12 C13 H13 120.0 . . ?
C15 C14 C13 120.4(5) . . ?
C15 C14 H14 119.8 . . ?
C13 C14 H14 119.8 . . ?
C14 C15 C16 119.8(4) . . ?
C14 C15 H15 120.1 . . ?
C16 C15 H15 120.1 . . ?
C15 C16 C17 120.1(5) . . ?
C15 C16 H16 120.0 . . ?
C17 C16 H16 120.0 . . ?
C12 C17 C16 120.7(5) . . ?
C12 C17 H17 119.6 . . ?
C16 C17 H17 119.6 . . ?
C23 C18 C19 117.8(4) . . ?
C23 C18 C7 124.2(3) . . ?
C19 C18 C7 118.0(3) . . ?
C20 C19 C18 120.7(4) . . ?
C20 C19 H19 119.7 . . ?
C18 C19 H19 119.7 . . ?
C21 C20 C19 120.7(4) . . ?
C21 C20 H20 119.7 . . ?
C19 C20 H20 119.7 . . ?
C20 C21 C22 119.3(4) . . ?
C20 C21 H21 120.4 . . ?
C22 C21 H21 120.4 . . ?
C21 C22 C23 120.4(4) . . ?
C21 C22 H22 119.8 . . ?
C23 C22 H22 119.8 . . ?
C22 C23 C18 121.0(4) . . ?
C22 C23 H23 119.5 . . ?
C18 C23 H23 119.5 . . ?
C29 C24 C25 118.3(4) . . ?
C29 C24 C11 119.0(3) . . ?
C25 C24 C11 122.6(3) . . ?
C24 C25 C26 120.7(4) . . ?
C24 C25 H25 119.7 . . ?
C26 C25 H25 119.7 . . ?
C27 C26 C25 120.3(4) . . ?
C27 C26 H26 119.8 . . ?
C25 C26 H26 119.8 . . ?
C26 C27 C28 119.4(4) . . ?
C26 C27 H27 120.3 . . ?
C28 C27 H27 120.3 . . ?
C27 C28 C29 120.2(4) . . ?
C27 C28 H28 119.9 . . ?
C29 C28 H28 119.9 . . ?
C24 C29 C28 121.1(4) . . ?
C24 C29 H29 119.5 . . ?
C28 C29 H29 119.5 . . ?
C35 C30 C31 117.5(4) . . ?
C35 C30 C11 119.9(3) . . ?
C31 C30 C11 122.5(4) . . ?
C32 C31 C30 121.0(4) . . ?
C32 C31 H31 119.5 . . ?
C30 C31 H31 119.5 . . ?
C33 C32 C31 120.4(4) . . ?
C33 C32 H32 119.8 . . ?
C31 C32 H32 119.8 . . ?
C32 C33 C34 119.6(4) . . ?
C32 C33 H33 120.2 . . ?
C34 C33 H33 120.2 . . ?
C35 C34 C33 119.7(4) . . ?
C35 C34 H34 120.1 . . ?
C33 C34 H34 120.1 . . ?
C34 C35 C30 121.8(4) . . ?
C34 C35 H35 119.1 . . ?
C30 C35 H35 119.1 . . ?
C38 C36 C37 109.5(3) . . ?
C38 C36 Si1 114.9(3) . . ?
C37 C36 Si1 114.0(3) . . ?
C38 C36 H36 105.9 . . ?
C37 C36 H36 105.9 . . ?
Si1 C36 H36 105.9 . . ?
C36 C37 H37A 109.5 . . ?
C36 C37 H37B 109.5 . . ?
H37A C37 H37B 109.5 . . ?
C36 C37 H37C 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
C36 C38 H38A 109.5 . . ?
C36 C38 H38B 109.5 . . ?
H38A C38 H38B 109.5 . . ?
C36 C38 H38C 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
C41 C39 C40 109.4(3) . . ?
C41 C39 Si1 117.2(3) . . ?
C40 C39 Si1 113.5(3) . . ?
C41 C39 H39 105.2 . . ?
C40 C39 H39 105.2 . . ?
Si1 C39 H39 105.2 . . ?
C39 C40 H40A 109.5 . . ?
C39 C40 H40B 109.5 . . ?
H40A C40 H40B 109.5 . . ?
C39 C40 H40C 109.5 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?
C39 C41 H41A 109.5 . . ?
C39 C41 H41B 109.5 . . ?
H41A C41 H41B 109.5 . . ?
C39 C41 H41C 109.5 . . ?
H41A C41 H41C 109.5 . . ?
H41B C41 H41C 109.5 . . ?
C43 C42 C44 109.8(3) . . ?
C43 C42 Si1 113.8(3) . . ?
C44 C42 Si1 114.3(3) . . ?
C43 C42 H42 106.1 . . ?
C44 C42 H42 106.1 . . ?
Si1 C42 H42 106.1 . . ?
C42 C43 H43A 109.5 . . ?
C42 C43 H43B 109.5 . . ?
H43A C43 H43B 109.5 . . ?
C42 C43 H43C 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?
C42 C44 H44A 109.5 . . ?
C42 C44 H44B 109.5 . . ?
H44A C44 H44B 109.5 . . ?
C42 C44 H44C 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
C46 C45 C49 102.6(3) . . ?
C46 C45 Ge1 122.5(3) . . ?
C49 C45 Ge1 107.7(3) . . ?
C46 C45 H45 107.8 . . ?
C49 C45 H45 107.8 . . ?
Ge1 C45 H45 107.8 . . ?
C45 C46 C47 103.8(4) . . ?
C45 C46 H46A 111.0 . . ?
C47 C46 H46A 111.0 . . ?
C45 C46 H46B 111.0 . . ?
C47 C46 H46B 111.0 . . ?
H46A C46 H46B 109.0 . . ?
C46 C47 C48 104.8(4) . . ?
C46 C47 H47A 110.8 . . ?
C48 C47 H47A 110.8 . . ?
C46 C47 H47B 110.8 . . ?
C48 C47 H47B 110.8 . . ?
H47A C47 H47B 108.9 . . ?
C49 C48 C47 107.5(4) . . ?
C49 C48 H48A 110.2 . . ?
C47 C48 H48A 110.2 . . ?
C49 C48 H48B 110.2 . . ?
C47 C48 H48B 110.2 . . ?
H48A C48 H48B 108.5 . . ?
C48 C49 C45 104.6(4) . . ?
C48 C49 H49A 110.8 . . ?
C45 C49 H49A 110.8 . . ?
C48 C49 H49B 110.8 . . ?
C45 C49 H49B 110.8 . . ?
H49A C49 H49B 108.9 . . ?

_diffrn_measured_fraction_theta_max 0.910
_diffrn_reflns_theta_full        25.20
_diffrn_measured_fraction_theta_full 0.910
_refine_diff_density_max         1.180
_refine_diff_density_min         -1.021
_refine_diff_density_rms         0.079
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_compound22
_database_code_depnum_ccdc_archive 'CCDC 1422739'
_audit_update_record             
;
2015-09-07 deposited with the CCDC.
2015-09-22 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C48 H63 Ge N O Si'
_chemical_formula_weight         770.67

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   P-1

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   10.3990(4)
_cell_length_b                   14.2109(5)
_cell_length_c                   15.4524(5)
_cell_angle_alpha                90.4830(10)
_cell_angle_beta                 101.0260(10)
_cell_angle_gamma                105.1180(10)
_cell_volume                     2159.71(13)
_cell_formula_units_Z            2
_cell_measurement_temperature    123(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.25
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.185
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             824
_exptl_absorpt_coefficient_mu    0.772
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.800
_exptl_absorpt_correction_T_max  0.828
_exptl_absorpt_process_details   'SCALE3 ABSPACK'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      123(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Oxford Gemini Ultra'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            33814
_diffrn_reflns_av_R_equivalents  0.0361
_diffrn_reflns_av_sigmaI/netI    0.0407
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         2.93
_diffrn_reflns_theta_max         26.00
_reflns_number_total             8452
_reflns_number_gt                6806
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       CrysalisPro
_computing_cell_refinement       CrysalisPro
_computing_data_reduction        CrysalisPro
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    X-Seed
_computing_publication_material  CifTAB

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger.
 The oxygen and/or carbon atoms of the ethoxy and ethyl groups were found
 to be disordered over two sites. This disorder was modelled, and the 
 carbon and oxygen atoms of the minor disordered set (ca. 20% occupied)
 refined isotropically.
 The ADP and positional parameters of hydrogen H(1), which was located 
 from difference maps, and bonded to the Ge atom was refined isotropically. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0488P)²+2.0792P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         8452
_refine_ls_number_parameters     511
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.0617
_refine_ls_R_factor_gt           0.0440
_refine_ls_wR_factor_ref         0.1127
_refine_ls_wR_factor_gt          0.1047
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_restrained_S_all      1.048
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ge1 Ge 0.60821(4) 0.17420(3) 0.26009(8) 0.01971(16) Uani 0.808(3) 1 d P A 1
Si1 Si 0.28934(7) 0.06606(5) 0.23615(4) 0.01806(16) Uani 1 1 d . A .
N1 N 0.4269(2) 0.17299(14) 0.25121(13) 0.0174(4) Uani 1 1 d . . .
C4 C 0.3349(2) 0.44965(17) 0.24882(15) 0.0168(5) Uani 1 1 d . . .
C6 C 0.3791(2) 0.31537(17) 0.17157(15) 0.0164(5) Uani 1 1 d . . .
C2 C 0.3939(2) 0.31569(17) 0.33038(15) 0.0165(5) Uani 1 1 d . . .
C1 C 0.4000(2) 0.26835(16) 0.25128(15) 0.0152(5) Uani 1 1 d . A .
C7 C 0.2971(3) 0.54608(18) 0.24713(17) 0.0237(6) Uani 1 1 d . . .
H7 H 0.3069 0.5702 0.3097 0.028 Uiso 1 1 calc R . .
C25 C 0.1598(3) 0.28414(17) 0.00762(17) 0.0216(5) Uani 1 1 d . A .
H25 H 0.1358 0.2865 0.0637 0.026 Uiso 1 1 calc R . .
C24 C 0.2903(3) 0.27998(17) 0.00299(16) 0.0204(5) Uani 1 1 d . . .
C39 C 0.1358(3) 0.09009(18) 0.16076(17) 0.0241(6) Uani 1 1 d . . .
H39 H 0.1698 0.1252 0.1104 0.029 Uiso 1 1 calc R A .
C10 C 0.4293(2) 0.27576(17) 0.42058(15) 0.0190(5) Uani 1 1 d . A .
H10 H 0.4189 0.2044 0.4099 0.023 Uiso 1 1 calc R . .
C23 C 0.3976(2) 0.27369(17) 0.08477(15) 0.0183(5) Uani 1 1 d . A .
H23 H 0.3885 0.2025 0.0921 0.022 Uiso 1 1 calc R . .
C5 C 0.3467(2) 0.40412(17) 0.17215(16) 0.0183(5) Uani 1 1 d . A .
H5 H 0.3320 0.4347 0.1181 0.022 Uiso 1 1 calc R . .
C27 C 0.0953(3) 0.2792(2) -0.15020(18) 0.0330(7) Uani 1 1 d . A .
H27 H 0.0300 0.2804 -0.2021 0.040 Uiso 1 1 calc R . .
C3 C 0.3590(2) 0.40423(17) 0.32686(15) 0.0170(5) Uani 1 1 d . A .
H3 H 0.3516 0.4345 0.3801 0.020 Uiso 1 1 calc R . .
C12 C 0.6486(3) 0.2616(2) 0.51359(18) 0.0277(6) Uani 1 1 d . A .
H12 H 0.6056 0.1941 0.5155 0.033 Uiso 1 1 calc R . .
C40 C 0.0663(3) 0.1564(2) 0.20286(18) 0.0277(6) Uani 1 1 d . A .
H40A H -0.0086 0.1678 0.1588 0.042 Uiso 1 1 calc R . .
H40B H 0.1326 0.2189 0.2239 0.042 Uiso 1 1 calc R . .
H40C H 0.0307 0.1248 0.2527 0.042 Uiso 1 1 calc R . .
C16 C 0.6429(3) 0.41932(18) 0.46532(16) 0.0222(5) Uani 1 1 d . A .
H16 H 0.5955 0.4614 0.4340 0.027 Uiso 1 1 calc R . .
C36 C 0.2450(3) 0.02747(19) 0.34641(17) 0.0246(6) Uani 1 1 d . . .
H36 H 0.2390 0.0880 0.3770 0.029 Uiso 1 1 calc R A .
C11 C 0.5773(2) 0.32087(17) 0.46646(15) 0.0184(5) Uani 1 1 d . . .
C31 C 0.6161(3) 0.25590(19) 0.04690(17) 0.0265(6) Uani 1 1 d . A .
H31 H 0.5753 0.1875 0.0395 0.032 Uiso 1 1 calc R . .
C26 C 0.0641(3) 0.28498(18) -0.06802(17) 0.0251(6) Uani 1 1 d . . .
H26 H -0.0237 0.2896 -0.0631 0.030 Uiso 1 1 calc R A .
C34 C 0.7345(3) 0.4539(2) 0.06433(18) 0.0302(6) Uani 1 1 d . . .
H34 H 0.7746 0.5224 0.0696 0.036 Uiso 1 1 calc R . .
C35 C 0.6023(3) 0.41732(18) 0.07699(17) 0.0241(6) Uani 1 1 d . A .
H35 H 0.5529 0.4611 0.0908 0.029 Uiso 1 1 calc R . .
C41 C 0.0270(3) -0.0034(2) 0.12007(19) 0.0349(7) Uani 1 1 d . A .
H41A H -0.0104 -0.0401 0.1671 0.052 Uiso 1 1 calc R . .
H41B H 0.0683 -0.0438 0.0882 0.052 Uiso 1 1 calc R . .
H41C H -0.0460 0.0142 0.0789 0.052 Uiso 1 1 calc R . .
C13 C 0.7821(3) 0.2994(2) 0.55796(19) 0.0320(6) Uani 1 1 d . . .
H13 H 0.8293 0.2578 0.5903 0.038 Uiso 1 1 calc R A .
C30 C 0.5417(2) 0.31740(17) 0.06968(15) 0.0196(5) Uani 1 1 d . . .
C15 C 0.7765(3) 0.4570(2) 0.50918(17) 0.0259(6) Uani 1 1 d . . .
H15 H 0.8199 0.5245 0.5074 0.031 Uiso 1 1 calc R A .
C42 C 0.3510(3) -0.02990(18) 0.18328(18) 0.0259(6) Uani 1 1 d . . .
H42 H 0.4462 -0.0230 0.2157 0.031 Uiso 1 1 calc R A .
C38 C 0.1073(3) -0.0477(2) 0.34332(19) 0.0344(7) Uani 1 1 d . A .
H38A H 0.1057 -0.1084 0.3120 0.052 Uiso 1 1 calc R . .
H38B H 0.0339 -0.0215 0.3123 0.052 Uiso 1 1 calc R . .
H38C H 0.0945 -0.0610 0.4037 0.052 Uiso 1 1 calc R . .
O1 O 0.6467(3) 0.09766(17) 0.34866(15) 0.0328(7) Uani 0.808(3) 1 d P A 1
C32 C 0.7484(3) 0.2923(2) 0.03477(18) 0.0319(6) Uani 1 1 d . . .
H32 H 0.7978 0.2489 0.0201 0.038 Uiso 1 1 calc R A .
C37 C 0.3584(3) -0.0058(2) 0.40657(18) 0.0321(6) Uani 1 1 d . A .
H37A H 0.3364 -0.0162 0.4653 0.048 Uiso 1 1 calc R . .
H37B H 0.4447 0.0445 0.4116 0.048 Uiso 1 1 calc R . .
H37C H 0.3665 -0.0669 0.3812 0.048 Uiso 1 1 calc R . .
C44 C 0.3593(3) -0.0133(2) 0.08594(19) 0.0354(7) Uani 1 1 d . A .
H44A H 0.4000 -0.0611 0.0637 0.053 Uiso 1 1 calc R . .
H44B H 0.4156 0.0528 0.0814 0.053 Uiso 1 1 calc R . .
H44C H 0.2677 -0.0211 0.0508 0.053 Uiso 1 1 calc R . .
C33 C 0.8081(3) 0.3916(2) 0.04414(18) 0.0317(6) Uani 1 1 d . A .
H33 H 0.8991 0.4169 0.0368 0.038 Uiso 1 1 calc R . .
C8 C 0.3923(3) 0.62331(19) 0.20361(19) 0.0326(7) Uani 1 1 d . . .
H8A H 0.4869 0.6275 0.2311 0.049 Uiso 1 1 calc R . .
H8B H 0.3741 0.6868 0.2114 0.049 Uiso 1 1 calc R . .
H8C H 0.3770 0.6051 0.1404 0.049 Uiso 1 1 calc R . .
C29 C 0.3200(3) 0.2734(2) -0.08048(18) 0.0367(7) Uani 1 1 d . A .
H29 H 0.4083 0.2699 -0.0857 0.044 Uiso 1 1 calc R . .
C28 C 0.2238(3) 0.2717(3) -0.15572(19) 0.0452(9) Uani 1 1 d . . .
H28 H 0.2458 0.2654 -0.2120 0.054 Uiso 1 1 calc R A .
C43 C 0.2723(3) -0.13572(19) 0.1911(2) 0.0397(7) Uani 1 1 d . A .
H43A H 0.1759 -0.1449 0.1648 0.059 Uiso 1 1 calc R . .
H43B H 0.2816 -0.1501 0.2535 0.059 Uiso 1 1 calc R . .
H43C H 0.3088 -0.1799 0.1599 0.059 Uiso 1 1 calc R . .
C14 C 0.8466(3) 0.3969(2) 0.55539(18) 0.0292(6) Uani 1 1 d . A .
H14 H 0.9384 0.4226 0.5851 0.035 Uiso 1 1 calc R . .
C45 C 0.7432(4) 0.0462(3) 0.3449(3) 0.0501(12) Uani 0.808(3) 1 d P A 1
H45A H 0.8234 0.0728 0.3927 0.060 Uiso 0.808(3) 1 calc PR A 1
H45B H 0.7733 0.0563 0.2878 0.060 Uiso 0.808(3) 1 calc PR A 1
C46 C 0.6904(5) -0.0606(3) 0.3538(3) 0.0575(13) Uani 0.808(3) 1 d P A 1
H46A H 0.6516 -0.0710 0.4071 0.086 Uiso 0.808(3) 1 calc PR A 1
H46B H 0.7649 -0.0917 0.3583 0.086 Uiso 0.808(3) 1 calc PR A 1
H46C H 0.6199 -0.0893 0.3019 0.086 Uiso 0.808(3) 1 calc PR A 1
C9 C 0.1502(3) 0.5328(2) 0.2013(2) 0.0409(8) Uani 1 1 d . . .
H9A H 0.1374 0.5084 0.1399 0.061 Uiso 1 1 calc R . .
H9B H 0.1279 0.5956 0.2025 0.061 Uiso 1 1 calc R . .
H9C H 0.0903 0.4858 0.2320 0.061 Uiso 1 1 calc R . .
C17 C 0.3307(3) 0.28457(19) 0.48137(16) 0.0237(6) Uani 1 1 d . . .
C18 C 0.1919(3) 0.2494(2) 0.45277(18) 0.0272(6) Uani 1 1 d . A .
H18 H 0.1574 0.2240 0.3934 0.033 Uiso 1 1 calc R . .
C22 C 0.3741(3) 0.3321(2) 0.56544(19) 0.0344(7) Uani 1 1 d . A .
H22 H 0.4684 0.3615 0.5863 0.041 Uiso 1 1 calc R . .
C19 C 0.1016(3) 0.2497(2) 0.50727(18) 0.0302(6) Uani 1 1 d . . .
H19 H 0.0076 0.2190 0.4868 0.036 Uiso 1 1 calc R A .
C21 C 0.2832(3) 0.3377(2) 0.6195(2) 0.0404(7) Uani 1 1 d . . .
H21 H 0.3156 0.3714 0.6760 0.048 Uiso 1 1 calc R A .
C20 C 0.1459(3) 0.2942(3) 0.5911(2) 0.0423(8) Uani 1 1 d . A .
H20 H 0.0835 0.2949 0.6286 0.051 Uiso 1 1 calc R . .
O1A O 0.6462(10) 0.0970(7) 0.2119(7) 0.023(2) Uiso 0.192(3) 1 d P A 2
C45A C 0.7090(14) 0.0235(10) 0.2450(9) 0.026(3) Uiso 0.192(3) 1 d P A 2
H45C H 0.6668 -0.0072 0.2937 0.031 Uiso 0.192(3) 1 calc PR A 2
H45D H 0.8067 0.0536 0.2692 0.031 Uiso 0.192(3) 1 calc PR A 2
C46A C 0.6944(19) -0.0535(13) 0.1740(12) 0.049(5) Uiso 0.192(3) 1 d P A 2
H46D H 0.5979 -0.0809 0.1478 0.074 Uiso 0.192(3) 1 calc PR A 2
H46E H 0.7327 -0.1055 0.1996 0.074 Uiso 0.192(3) 1 calc PR A 2
H46F H 0.7430 -0.0243 0.1282 0.074 Uiso 0.192(3) 1 calc PR A 2
Ge1A Ge 0.6073(2) 0.17478(18) 0.2900(2) 0.0208(7) Uiso 0.192(3) 1 d PD A 2
C47 C 0.7270(4) 0.3050(3) 0.2804(4) 0.0237(14) Uani 0.808(3) 1 d P A 1
H47A H 0.7173 0.3391 0.2249 0.028 Uiso 0.808(3) 1 calc PR A 1
H47B H 0.6982 0.3409 0.3251 0.028 Uiso 0.808(3) 1 calc PR A 1
C48 C 0.8744(5) 0.3076(4) 0.3117(5) 0.075(2) Uani 0.808(3) 1 d P A 1
H48A H 0.8852 0.2752 0.3674 0.113 Uiso 0.808(3) 1 calc PR A 1
H48B H 0.9295 0.3757 0.3211 0.113 Uiso 0.808(3) 1 calc PR A 1
H48C H 0.9045 0.2738 0.2671 0.113 Uiso 0.808(3) 1 calc PR A 1
C48A C 0.8621(11) 0.3013(12) 0.2790(12) 0.019(4) Uiso 0.192(3) 1 d PD A 2
H48D H 0.9006 0.2543 0.3139 0.028 Uiso 0.192(3) 1 calc PR A 2
H48E H 0.9252 0.3666 0.2918 0.028 Uiso 0.192(3) 1 calc PR A 2
H48F H 0.8475 0.2826 0.2160 0.028 Uiso 0.192(3) 1 calc PR A 2
C47A C 0.7334(13) 0.3020(6) 0.3019(15) 0.011(5) Uiso 0.192(3) 1 d PD A 2
H47C H 0.6920 0.3460 0.2634 0.013 Uiso 0.192(3) 1 calc PR A 2
H47D H 0.7504 0.3286 0.3637 0.013 Uiso 0.192(3) 1 calc PR A 2
H1 H 0.622(3) 0.118(3) 0.183(2) 0.042(11) Uiso 1 1 d . B 1


_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 O1 1.805(2) . ?
Ge1 N1 1.860(2) . ?
Ge1 C47 1.930(3) . ?
Si1 N1 1.772(2) . ?
Si1 C42 1.891(3) . ?
Si1 C36 1.897(3) . ?
Si1 C39 1.898(3) . ?
N1 C1 1.453(3) . ?
N1 Ge1A 1.851(3) . ?
C4 C3 1.384(3) . ?
C4 C5 1.386(3) . ?
C4 C7 1.520(3) . ?
C6 C5 1.388(3) . ?
C6 C1 1.414(3) . ?
C6 C23 1.527(3) . ?
C2 C3 1.396(3) . ?
C2 C1 1.410(3) . ?
C2 C10 1.525(3) . ?
C7 C9 1.518(4) . ?
C7 C8 1.529(4) . ?
C25 C26 1.385(4) . ?
C25 C24 1.388(4) . ?
C24 C29 1.391(4) . ?
C24 C23 1.538(3) . ?
C39 C40 1.535(4) . ?
C39 C41 1.539(4) . ?
C10 C11 1.530(3) . ?
C10 C17 1.544(3) . ?
C23 C30 1.528(3) . ?
C27 C26 1.376(4) . ?
C27 C28 1.387(4) . ?
C12 C11 1.386(3) . ?
C12 C13 1.388(4) . ?
C16 C15 1.386(4) . ?
C16 C11 1.389(3) . ?
C36 C37 1.535(4) . ?
C36 C38 1.540(4) . ?
C31 C32 1.387(4) . ?
C31 C30 1.392(4) . ?
C34 C33 1.381(4) . ?
C34 C35 1.389(4) . ?
C35 C30 1.389(3) . ?
C13 C14 1.378(4) . ?
C15 C14 1.381(4) . ?
C42 C43 1.531(4) . ?
C42 C44 1.540(4) . ?
O1 C45 1.396(4) . ?
C32 C33 1.380(4) . ?
C29 C28 1.377(4) . ?
C45 C46 1.491(6) . ?
C17 C18 1.381(4) . ?
C17 C22 1.396(4) . ?
C18 C19 1.377(4) . ?
C22 C21 1.393(4) . ?
C19 C20 1.377(4) . ?
C21 C20 1.381(4) . ?
O1A C45A 1.420(17) . ?
O1A Ge1A 1.800(10) . ?
C45A C46A 1.50(2) . ?
Ge1A C47A 1.920(5) . ?
C47 C48 1.507(6) . ?
C48A C47A 1.450(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
O1 Ge1 N1 106.50(11) . . ?
O1 Ge1 C47 112.0(2) . . ?
N1 Ge1 C47 111.86(14) . . ?
N1 Si1 C42 105.29(11) . . ?
N1 Si1 C36 110.44(11) . . ?
C42 Si1 C36 110.84(12) . . ?
N1 Si1 C39 109.56(10) . . ?
C42 Si1 C39 110.89(12) . . ?
C36 Si1 C39 109.73(12) . . ?
C1 N1 Si1 119.68(15) . . ?
C1 N1 Ge1A 114.73(16) . . ?
Si1 N1 Ge1A 124.40(13) . . ?
C1 N1 Ge1 115.47(14) . . ?
Si1 N1 Ge1 124.72(11) . . ?
Ge1A N1 Ge1 14.35(9) . . ?
C3 C4 C5 117.6(2) . . ?
C3 C4 C7 121.3(2) . . ?
C5 C4 C7 121.1(2) . . ?
C5 C6 C1 119.6(2) . . ?
C5 C6 C23 118.5(2) . . ?
C1 C6 C23 121.8(2) . . ?
C3 C2 C1 119.2(2) . . ?
C3 C2 C10 118.4(2) . . ?
C1 C2 C10 122.4(2) . . ?
C2 C1 C6 118.7(2) . . ?
C2 C1 N1 120.9(2) . . ?
C6 C1 N1 120.4(2) . . ?
C9 C7 C4 111.2(2) . . ?
C9 C7 C8 110.6(2) . . ?
C4 C7 C8 111.5(2) . . ?
C26 C25 C24 121.2(2) . . ?
C25 C24 C29 117.6(2) . . ?
C25 C24 C23 123.1(2) . . ?
C29 C24 C23 119.1(2) . . ?
C40 C39 C41 108.5(2) . . ?
C40 C39 Si1 114.73(18) . . ?
C41 C39 Si1 113.76(18) . . ?
C2 C10 C11 112.50(19) . . ?
C2 C10 C17 112.6(2) . . ?
C11 C10 C17 111.18(19) . . ?
C6 C23 C30 110.92(19) . . ?
C6 C23 C24 115.3(2) . . ?
C30 C23 C24 111.39(19) . . ?
C4 C5 C6 122.3(2) . . ?
C26 C27 C28 118.7(3) . . ?
C4 C3 C2 122.5(2) . . ?
C11 C12 C13 120.9(2) . . ?
C15 C16 C11 121.0(2) . . ?
C37 C36 C38 109.9(2) . . ?
C37 C36 Si1 112.63(18) . . ?
C38 C36 Si1 116.62(18) . . ?
C12 C11 C16 118.1(2) . . ?
C12 C11 C10 118.7(2) . . ?
C16 C11 C10 123.2(2) . . ?
C32 C31 C30 121.5(3) . . ?
C27 C26 C25 120.6(3) . . ?
C33 C34 C35 120.6(3) . . ?
C34 C35 C30 120.6(2) . . ?
C14 C13 C12 120.4(2) . . ?
C35 C30 C31 117.9(2) . . ?
C35 C30 C23 122.5(2) . . ?
C31 C30 C23 119.6(2) . . ?
C14 C15 C16 120.3(3) . . ?
C43 C42 C44 109.3(2) . . ?
C43 C42 Si1 115.3(2) . . ?
C44 C42 Si1 112.99(18) . . ?
C45 O1 Ge1 119.2(2) . . ?
C33 C32 C31 119.8(3) . . ?
C32 C33 C34 119.5(3) . . ?
C28 C29 C24 121.2(3) . . ?
C29 C28 C27 120.7(3) . . ?
C13 C14 C15 119.3(3) . . ?
O1 C45 C46 112.9(3) . . ?
C18 C17 C22 116.0(2) . . ?
C18 C17 C10 120.9(2) . . ?
C22 C17 C10 123.0(2) . . ?
C19 C18 C17 122.4(3) . . ?
C21 C22 C17 121.9(3) . . ?
C18 C19 C20 120.7(3) . . ?
C20 C21 C22 120.1(3) . . ?
C19 C20 C21 118.5(3) . . ?
C45A O1A Ge1A 118.1(9) . . ?
O1A C45A C46A 111.2(12) . . ?
O1A Ge1A N1 106.4(4) . . ?
O1A Ge1A C47A 110.2(6) . . ?
N1 Ge1A C47A 114.9(6) . . ?
C48 C47 Ge1 113.2(3) . . ?
C48A C47A Ge1A 113.1(5) . . ?

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        26.00
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         1.182
_refine_diff_density_min         -0.342
_refine_diff_density_rms         0.061
####################################################################### 
# 
# 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_compound23
_database_code_depnum_ccdc_archive 'CCDC 1422740'
_audit_update_record             
;
2015-09-07 deposited with the CCDC.
2015-09-22 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C53 H70 N2 O Si Sn'
_chemical_formula_weight         897.89

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

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   P-1

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   14.604(3)
_cell_length_b                   15.840(3)
_cell_length_c                   20.773(4)
_cell_angle_alpha                88.61(3)
_cell_angle_beta                 82.84(3)
_cell_angle_gamma                84.99(3)
_cell_volume                     4749.2(17)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.03
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.256
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1896
_exptl_absorpt_coefficient_mu    0.602
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.961
_exptl_absorpt_correction_T_max  0.979
_exptl_absorpt_process_details   XDS

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71090
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_source         'Australian Synchrotron'
_diffrn_radiation_monochromator  ?
_diffrn_measurement_device_type  'ADSC Quantum 210r'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            72300
_diffrn_reflns_av_R_equivalents  0.0450
_diffrn_reflns_av_sigmaI/netI    0.0361
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         2.91
_diffrn_reflns_theta_max         26.00
_reflns_number_total             18572
_reflns_number_gt                16933
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Blu-Ice (McPhillips, 2002)'
_computing_cell_refinement       'XDS (Kabsch, 1993)'
_computing_data_reduction        'XDS (Kabsch, 1993)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    X-Seed
_computing_publication_material  CifTAB

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger.
 Two crystalographically independent molecules were refined in the asymmetric
 unit. There are no significant geometrical differences between them. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0320P)²+5.9728P] 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         18572
_refine_ls_number_parameters     1069
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0377
_refine_ls_R_factor_gt           0.0340
_refine_ls_wR_factor_ref         0.0877
_refine_ls_wR_factor_gt          0.0857
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_restrained_S_all      1.054
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Sn1 Sn 0.836778(10) 0.782391(10) 0.174091(7) 0.01995(5) Uani 1 1 d . . .
Si1 Si 0.86401(4) 0.77210(4) 0.34247(3) 0.01693(12) Uani 1 1 d . . .
O1 O 0.97510(11) 0.78836(11) 0.17710(7) 0.0232(3) Uani 1 1 d . . .
N1 N 0.79794(12) 0.77590(11) 0.27618(9) 0.0171(4) Uani 1 1 d . . .
C1 C 0.69859(15) 0.77791(13) 0.29051(10) 0.0167(4) Uani 1 1 d . . .
Sn2 Sn 0.846496(10) 0.750592(10) -0.327380(7) 0.01927(5) Uani 1 1 d . . .
Si2 Si 0.88007(4) 0.74593(4) -0.15971(3) 0.01556(11) Uani 1 1 d . . .
O2 O 0.98470(11) 0.72138(11) -0.32618(7) 0.0232(3) Uani 1 1 d . . .
N2 N 1.02085(13) 0.79084(12) 0.11040(9) 0.0199(4) Uani 1 1 d . . .
C2 C 0.65259(15) 0.70191(13) 0.29691(10) 0.0179(4) Uani 1 1 d . . .
N3 N 0.81257(12) 0.75415(11) -0.22522(8) 0.0157(3) Uani 1 1 d . . .
C3 C 0.55729(15) 0.70549(14) 0.31523(10) 0.0187(4) Uani 1 1 d . . .
H3 H 0.5280 0.6541 0.3192 0.022 Uiso 1 1 calc R . .
N4 N 1.02743(13) 0.71312(12) -0.39337(9) 0.0203(4) Uani 1 1 d . . .
C4 C 0.50331(15) 0.78152(14) 0.32797(10) 0.0188(4) Uani 1 1 d . . .
C5 C 0.54769(15) 0.85588(13) 0.31772(10) 0.0188(4) Uani 1 1 d . . .
H5 H 0.5118 0.9087 0.3239 0.023 Uiso 1 1 calc R . .
C6 C 0.64255(15) 0.85577(13) 0.29882(10) 0.0174(4) Uani 1 1 d . . .
C7 C 0.70581(15) 0.61607(13) 0.28111(11) 0.0183(4) Uani 1 1 d . . .
H7 H 0.7683 0.6186 0.2956 0.022 Uiso 1 1 calc R . .
C8 C 0.40341(16) 0.78411(15) 0.35796(12) 0.0246(5) Uani 1 1 d . . .
H8 H 0.3735 0.8417 0.3490 0.030 Uiso 1 1 calc R . .
C9 C 0.34650(18) 0.7193(2) 0.33210(14) 0.0393(7) Uani 1 1 d . . .
H9A H 0.3718 0.6620 0.3427 0.059 Uiso 1 1 calc R . .
H9B H 0.3490 0.7261 0.2849 0.059 Uiso 1 1 calc R . .
H9C H 0.2820 0.7282 0.3521 0.059 Uiso 1 1 calc R . .
C10 C 0.4011(2) 0.7742(2) 0.43116(13) 0.0421(7) Uani 1 1 d . . .
H10A H 0.4268 0.7170 0.4417 0.063 Uiso 1 1 calc R . .
H10B H 0.3370 0.7830 0.4518 0.063 Uiso 1 1 calc R . .
H10C H 0.4381 0.8161 0.4471 0.063 Uiso 1 1 calc R . .
C11 C 0.68483(15) 0.94022(13) 0.28427(10) 0.0178(4) Uani 1 1 d . . .
H11 H 0.7500 0.9313 0.2948 0.021 Uiso 1 1 calc R . .
C12 C 0.72243(16) 0.60147(14) 0.20793(11) 0.0215(4) Uani 1 1 d . . .
C13 C 0.79940(17) 0.54938(15) 0.18188(12) 0.0264(5) Uani 1 1 d . . .
H13 H 0.8420 0.5254 0.2097 0.032 Uiso 1 1 calc R . .
C14 C 0.81492(18) 0.53191(17) 0.11579(13) 0.0322(6) Uani 1 1 d . . .
H14 H 0.8678 0.4963 0.0990 0.039 Uiso 1 1 calc R . .
C15 C 0.75351(19) 0.56638(18) 0.07465(13) 0.0350(6) Uani 1 1 d . . .
H15 H 0.7636 0.5540 0.0297 0.042 Uiso 1 1 calc R . .
C16 C 0.6773(2) 0.6190(2) 0.09961(13) 0.0389(6) Uani 1 1 d . . .
H16 H 0.6353 0.6435 0.0716 0.047 Uiso 1 1 calc R . .
C17 C 0.66207(18) 0.63602(17) 0.16573(12) 0.0309(5) Uani 1 1 d . . .
H17 H 0.6093 0.6720 0.1823 0.037 Uiso 1 1 calc R . .
C18 C 0.66211(15) 0.54140(13) 0.31855(11) 0.0207(4) Uani 1 1 d . . .
C19 C 0.6412(2) 0.47012(17) 0.28735(14) 0.0367(6) Uani 1 1 d . . .
H19 H 0.6501 0.4681 0.2413 0.044 Uiso 1 1 calc R . .
C20 C 0.6073(2) 0.40146(19) 0.32328(16) 0.0487(8) Uani 1 1 d . . .
H20 H 0.5942 0.3528 0.3014 0.058 Uiso 1 1 calc R . .
C21 C 0.5926(2) 0.40333(17) 0.38981(15) 0.0393(7) Uani 1 1 d . . .
H21 H 0.5703 0.3560 0.4138 0.047 Uiso 1 1 calc R . .
C22 C 0.61051(17) 0.47502(16) 0.42173(13) 0.0292(5) Uani 1 1 d . . .
H22 H 0.5993 0.4775 0.4677 0.035 Uiso 1 1 calc R . .
C23 C 0.64493(16) 0.54302(15) 0.38609(12) 0.0246(5) Uani 1 1 d . . .
H23 H 0.6571 0.5918 0.4082 0.029 Uiso 1 1 calc R . .
C24 C 0.69158(15) 0.96290(13) 0.21215(11) 0.0188(4) Uani 1 1 d . . .
C25 C 0.75989(16) 1.01493(14) 0.18574(11) 0.0218(5) Uani 1 1 d . . .
H25 H 0.8003 1.0354 0.2131 0.026 Uiso 1 1 calc R . .
C26 C 0.76966(16) 1.03705(15) 0.12038(11) 0.0244(5) Uani 1 1 d . . .
H26 H 0.8165 1.0724 0.1034 0.029 Uiso 1 1 calc R . .
C27 C 0.71122(16) 1.00774(15) 0.07986(11) 0.0243(5) Uani 1 1 d . . .
H27 H 0.7185 1.0221 0.0349 0.029 Uiso 1 1 calc R . .
C28 C 0.64211(17) 0.95738(15) 0.10529(11) 0.0251(5) Uani 1 1 d . . .
H28 H 0.6014 0.9377 0.0778 0.030 Uiso 1 1 calc R . .
C29 C 0.63197(16) 0.93541(14) 0.17116(11) 0.0223(5) Uani 1 1 d . . .
H29 H 0.5840 0.9014 0.1882 0.027 Uiso 1 1 calc R . .
C30 C 0.63747(15) 1.01242(13) 0.32759(11) 0.0196(4) Uani 1 1 d . . .
C31 C 0.63157(18) 1.00306(15) 0.39494(12) 0.0268(5) Uani 1 1 d . . .
H31 H 0.6553 0.9514 0.4132 0.032 Uiso 1 1 calc R . .
C32 C 0.5916(2) 1.06802(17) 0.43567(12) 0.0336(6) Uani 1 1 d . . .
H32 H 0.5887 1.0605 0.4814 0.040 Uiso 1 1 calc R . .
C33 C 0.55601(19) 1.14389(16) 0.40992(13) 0.0323(6) Uani 1 1 d . . .
H33 H 0.5286 1.1883 0.4378 0.039 Uiso 1 1 calc R . .
C34 C 0.56082(18) 1.15410(15) 0.34339(12) 0.0280(5) Uani 1 1 d . . .
H34 H 0.5366 1.2058 0.3254 0.034 Uiso 1 1 calc R . .
C35 C 0.60110(16) 1.08876(14) 0.30226(11) 0.0228(5) Uani 1 1 d . . .
H35 H 0.6037 1.0965 0.2566 0.027 Uiso 1 1 calc R . .
C36 C 0.80037(16) 0.71366(15) 0.41336(11) 0.0222(5) Uani 1 1 d . . .
H36 H 0.7746 0.6652 0.3938 0.027 Uiso 1 1 calc R . .
C37 C 0.86396(17) 0.67337(15) 0.46187(12) 0.0270(5) Uani 1 1 d . . .
H37A H 0.8913 0.7181 0.4829 0.040 Uiso 1 1 calc R . .
H37B H 0.9134 0.6358 0.4387 0.040 Uiso 1 1 calc R . .
H37C H 0.8276 0.6406 0.4948 0.040 Uiso 1 1 calc R . .
C38 C 0.71670(17) 0.76492(16) 0.45032(12) 0.0277(5) Uani 1 1 d . . .
H38A H 0.6861 0.7289 0.4840 0.042 Uiso 1 1 calc R . .
H38B H 0.6729 0.7847 0.4200 0.042 Uiso 1 1 calc R . .
H38C H 0.7378 0.8138 0.4705 0.042 Uiso 1 1 calc R . .
C39 C 0.88088(17) 0.88354(14) 0.36885(11) 0.0228(5) Uani 1 1 d . . .
H39 H 0.8181 0.9151 0.3746 0.027 Uiso 1 1 calc R . .
C40 C 0.93961(19) 0.93047(15) 0.31482(12) 0.0288(5) Uani 1 1 d . . .
H40A H 0.9362 0.9908 0.3251 0.043 Uiso 1 1 calc R . .
H40B H 0.9158 0.9238 0.2733 0.043 Uiso 1 1 calc R . .
H40C H 1.0042 0.9066 0.3117 0.043 Uiso 1 1 calc R . .
C41 C 0.92051(19) 0.88810(15) 0.43390(12) 0.0279(5) Uani 1 1 d . . .
H41A H 0.9822 0.8575 0.4305 0.042 Uiso 1 1 calc R . .
H41B H 0.8795 0.8622 0.4683 0.042 Uiso 1 1 calc R . .
H41C H 0.9251 0.9475 0.4442 0.042 Uiso 1 1 calc R . .
C42 C 0.98032(15) 0.71649(14) 0.31210(11) 0.0207(4) Uani 1 1 d . . .
H42 H 1.0007 0.7458 0.2702 0.025 Uiso 1 1 calc R . .
C43 C 0.97225(17) 0.62426(15) 0.29397(12) 0.0276(5) Uani 1 1 d . . .
H43A H 1.0324 0.5997 0.2734 0.041 Uiso 1 1 calc R . .
H43B H 0.9261 0.6227 0.2637 0.041 Uiso 1 1 calc R . .
H43C H 0.9531 0.5915 0.3332 0.041 Uiso 1 1 calc R . .
C44 C 1.06041(17) 0.72066(17) 0.35327(12) 0.0283(5) Uani 1 1 d . . .
H44A H 1.0437 0.6951 0.3961 0.042 Uiso 1 1 calc R . .
H44B H 1.0722 0.7800 0.3583 0.042 Uiso 1 1 calc R . .
H44C H 1.1163 0.6895 0.3316 0.042 Uiso 1 1 calc R . .
C45 C 1.08525(17) 0.71277(15) 0.10014(12) 0.0262(5) Uani 1 1 d . . .
C46 C 1.13675(18) 0.71947(16) 0.03111(12) 0.0303(5) Uani 1 1 d . . .
H46A H 1.1844 0.6711 0.0242 0.036 Uiso 1 1 calc R . .
H46B H 1.0922 0.7150 -0.0006 0.036 Uiso 1 1 calc R . .
C47 C 1.18325(17) 0.80153(17) 0.01795(12) 0.0303(5) Uani 1 1 d . . .
H47A H 1.2330 0.8039 0.0460 0.036 Uiso 1 1 calc R . .
H47B H 1.2115 0.8038 -0.0279 0.036 Uiso 1 1 calc R . .
C48 C 1.11173(17) 0.87627(16) 0.03162(11) 0.0260(5) Uani 1 1 d . . .
H48A H 1.0659 0.8764 0.0003 0.031 Uiso 1 1 calc R . .
H48B H 1.1428 0.9294 0.0250 0.031 Uiso 1 1 calc R . .
C49 C 1.06076(15) 0.87430(14) 0.10079(11) 0.0214(5) Uani 1 1 d . . .
C50 C 1.0243(2) 0.63894(16) 0.10183(14) 0.0377(6) Uani 1 1 d . . .
H50A H 0.9987 0.6275 0.1467 0.057 Uiso 1 1 calc R . .
H50B H 1.0616 0.5884 0.0841 0.057 Uiso 1 1 calc R . .
H50C H 0.9736 0.6536 0.0757 0.057 Uiso 1 1 calc R . .
C51 C 1.15469(19) 0.69509(18) 0.15005(13) 0.0341(6) Uani 1 1 d . . .
H51A H 1.2046 0.7328 0.1412 0.051 Uiso 1 1 calc R . .
H51B H 1.1808 0.6360 0.1468 0.051 Uiso 1 1 calc R . .
H51C H 1.1227 0.7052 0.1939 0.051 Uiso 1 1 calc R . .
C52 C 0.97887(17) 0.94141(15) 0.10375(12) 0.0257(5) Uani 1 1 d . . .
H52A H 0.9330 0.9237 0.0773 0.039 Uiso 1 1 calc R . .
H52B H 1.0005 0.9955 0.0870 0.039 Uiso 1 1 calc R . .
H52C H 0.9505 0.9481 0.1488 0.039 Uiso 1 1 calc R . .
C53 C 1.12441(17) 0.89612(17) 0.15095(12) 0.0287(5) Uani 1 1 d . . .
H53A H 1.0942 0.8853 0.1948 0.043 Uiso 1 1 calc R . .
H53B H 1.1363 0.9560 0.1463 0.043 Uiso 1 1 calc R . .
H53C H 1.1832 0.8608 0.1436 0.043 Uiso 1 1 calc R . .
C54 C 0.71310(14) 0.76282(13) -0.20973(10) 0.0154(4) Uani 1 1 d . . .
C55 C 0.66169(15) 0.69039(13) -0.20169(10) 0.0160(4) Uani 1 1 d . . .
C56 C 0.56699(15) 0.69908(13) -0.18134(10) 0.0178(4) Uani 1 1 d . . .
H56 H 0.5341 0.6497 -0.1759 0.021 Uiso 1 1 calc R . .
C57 C 0.51898(15) 0.77789(14) -0.16869(11) 0.0193(4) Uani 1 1 d . . .
C58 C 0.56829(15) 0.84925(13) -0.18136(11) 0.0189(4) Uani 1 1 d . . .
H58 H 0.5359 0.9037 -0.1757 0.023 Uiso 1 1 calc R . .
C59 C 0.66295(15) 0.84384(13) -0.20193(10) 0.0177(4) Uani 1 1 d . . .
C60 C 0.70724(14) 0.60145(13) -0.21661(10) 0.0161(4) Uani 1 1 d . . .
H60 H 0.7730 0.6013 -0.2078 0.019 Uiso 1 1 calc R . .
C61 C 0.42114(16) 0.78501(16) -0.13445(12) 0.0258(5) Uani 1 1 d . . .
H61 H 0.3967 0.8459 -0.1358 0.031 Uiso 1 1 calc R . .
C62 C 0.35470(17) 0.73326(17) -0.16443(14) 0.0328(6) Uani 1 1 d . . .
H62A H 0.3508 0.7524 -0.2093 0.049 Uiso 1 1 calc R . .
H62B H 0.2932 0.7409 -0.1394 0.049 Uiso 1 1 calc R . .
H62C H 0.3773 0.6732 -0.1639 0.049 Uiso 1 1 calc R . .
C63 C 0.4264(2) 0.7596(3) -0.06341(15) 0.0640(12) Uani 1 1 d . . .
H63A H 0.4501 0.6999 -0.0608 0.096 Uiso 1 1 calc R . .
H63B H 0.3645 0.7675 -0.0390 0.096 Uiso 1 1 calc R . .
H63C H 0.4681 0.7950 -0.0450 0.096 Uiso 1 1 calc R . .
C64 C 0.71150(15) 0.92531(13) -0.21714(11) 0.0186(4) Uani 1 1 d . . .
H64 H 0.7748 0.9145 -0.2035 0.022 Uiso 1 1 calc R . .
C65 C 0.71006(15) 0.57941(13) -0.28803(10) 0.0186(4) Uani 1 1 d . . .
C66 C 0.77316(16) 0.51367(14) -0.31366(11) 0.0226(5) Uani 1 1 d . . .
H66 H 0.8149 0.4858 -0.2869 0.027 Uiso 1 1 calc R . .
C67 C 0.77604(17) 0.48832(16) -0.37739(12) 0.0279(5) Uani 1 1 d . . .
H67 H 0.8195 0.4435 -0.3938 0.033 Uiso 1 1 calc R . .
C68 C 0.71570(18) 0.52833(18) -0.41698(12) 0.0309(6) Uani 1 1 d . . .
H68 H 0.7173 0.5109 -0.4606 0.037 Uiso 1 1 calc R . .
C69 C 0.6531(2) 0.5938(2) -0.39272(13) 0.0388(7) Uani 1 1 d . . .
H69 H 0.6116 0.6214 -0.4198 0.047 Uiso 1 1 calc R . .
C70 C 0.65065(18) 0.61935(17) -0.32877(12) 0.0311(6) Uani 1 1 d . . .
H70 H 0.6077 0.6648 -0.3128 0.037 Uiso 1 1 calc R . .
C71 C 0.66299(15) 0.53334(13) -0.17151(11) 0.0188(4) Uani 1 1 d . . .
C72 C 0.66322(17) 0.53871(15) -0.10460(12) 0.0263(5) Uani 1 1 d . . .
H72 H 0.6902 0.5846 -0.0877 0.032 Uiso 1 1 calc R . .
C73 C 0.6249(2) 0.47846(18) -0.06215(13) 0.0355(6) Uani 1 1 d . . .
H73 H 0.6261 0.4833 -0.0168 0.043 Uiso 1 1 calc R . .
C74 C 0.5850(2) 0.41144(18) -0.08586(15) 0.0411(7) Uani 1 1 d . . .
H74 H 0.5594 0.3697 -0.0571 0.049 Uiso 1 1 calc R . .
C75 C 0.5829(2) 0.40600(18) -0.15181(15) 0.0416(7) Uani 1 1 d . . .
H75 H 0.5549 0.3605 -0.1683 0.050 Uiso 1 1 calc R . .
C76 C 0.62105(18) 0.46624(16) -0.19461(13) 0.0306(6) Uani 1 1 d . . .
H76 H 0.6185 0.4616 -0.2399 0.037 Uiso 1 1 calc R . .
C77 C 0.72501(16) 0.94500(13) -0.28989(11) 0.0205(4) Uani 1 1 d . . .
C78 C 0.80230(17) 0.98530(15) -0.31730(12) 0.0273(5) Uani 1 1 d . . .
H78 H 0.8472 0.9983 -0.2906 0.033 Uiso 1 1 calc R . .
C79 C 0.81474(19) 1.00671(17) -0.38302(13) 0.0335(6) Uani 1 1 d . . .
H79 H 0.8678 1.0340 -0.4008 0.040 Uiso 1 1 calc R . .
C80 C 0.7494(2) 0.98808(18) -0.42257(13) 0.0345(6) Uani 1 1 d . . .
H80 H 0.7576 1.0026 -0.4674 0.041 Uiso 1 1 calc R . .
C81 C 0.6724(2) 0.94828(17) -0.39637(12) 0.0325(6) Uani 1 1 d . . .
H81 H 0.6276 0.9356 -0.4233 0.039 Uiso 1 1 calc R . .
C82 C 0.66019(17) 0.92666(15) -0.33041(12) 0.0255(5) Uani 1 1 d . . .
H82 H 0.6071 0.8992 -0.3130 0.031 Uiso 1 1 calc R . .
C83 C 0.66365(15) 1.00195(13) -0.17791(11) 0.0192(4) Uani 1 1 d . . .
C84 C 0.63966(18) 1.07851(15) -0.20814(12) 0.0269(5) Uani 1 1 d . . .
H84 H 0.6507 1.0837 -0.2541 0.032 Uiso 1 1 calc R . .
C85 C 0.5992(2) 1.14826(15) -0.17120(13) 0.0336(6) Uani 1 1 d . . .
H85 H 0.5832 1.2003 -0.1925 0.040 Uiso 1 1 calc R . .
C86 C 0.58246(18) 1.14229(15) -0.10469(13) 0.0299(5) Uani 1 1 d . . .
H86 H 0.5554 1.1898 -0.0800 0.036 Uiso 1 1 calc R . .
C87 C 0.60559(17) 1.06583(15) -0.07411(12) 0.0261(5) Uani 1 1 d . . .
H87 H 0.5942 1.0609 -0.0282 0.031 Uiso 1 1 calc R . .
C88 C 0.64537(16) 0.99656(14) -0.11045(11) 0.0223(5) Uani 1 1 d . . .
H88 H 0.6604 0.9445 -0.0889 0.027 Uiso 1 1 calc R . .
C89 C 0.81490(15) 0.80935(14) -0.08891(11) 0.0195(4) Uani 1 1 d . . .
H89 H 0.7867 0.8621 -0.1087 0.023 Uiso 1 1 calc R . .
C90 C 0.73334(16) 0.76670(15) -0.05116(11) 0.0229(5) Uani 1 1 d . . .
H90A H 0.7568 0.7145 -0.0302 0.034 Uiso 1 1 calc R . .
H90B H 0.6903 0.7530 -0.0812 0.034 Uiso 1 1 calc R . .
H90C H 0.7010 0.8054 -0.0181 0.034 Uiso 1 1 calc R . .
C91 C 0.87675(17) 0.83968(15) -0.04049(11) 0.0246(5) Uani 1 1 d . . .
H91A H 0.8385 0.8742 -0.0071 0.037 Uiso 1 1 calc R . .
H91B H 0.9237 0.8736 -0.0637 0.037 Uiso 1 1 calc R . .
H91C H 0.9073 0.7904 -0.0200 0.037 Uiso 1 1 calc R . .
C92 C 0.90202(15) 0.63067(13) -0.13337(10) 0.0190(4) Uani 1 1 d . . .
H92 H 0.8404 0.6066 -0.1275 0.023 Uiso 1 1 calc R . .
C93 C 0.94219(17) 0.61663(14) -0.06839(11) 0.0237(5) Uani 1 1 d . . .
H93A H 0.9486 0.5558 -0.0582 0.036 Uiso 1 1 calc R . .
H93B H 0.9004 0.6460 -0.0339 0.036 Uiso 1 1 calc R . .
H93C H 1.0031 0.6391 -0.0718 0.036 Uiso 1 1 calc R . .
C94 C 0.96226(17) 0.57962(14) -0.18773(11) 0.0242(5) Uani 1 1 d . . .
H94A H 1.0256 0.5967 -0.1919 0.036 Uiso 1 1 calc R . .
H94B H 0.9366 0.5907 -0.2288 0.036 Uiso 1 1 calc R . .
H94C H 0.9628 0.5190 -0.1770 0.036 Uiso 1 1 calc R . .
C95 C 0.99484(15) 0.78771(14) -0.19122(11) 0.0195(4) Uani 1 1 d . . .
H95 H 1.0165 0.7564 -0.2323 0.023 Uiso 1 1 calc R . .
C96 C 1.07507(16) 0.77279(16) -0.14951(12) 0.0267(5) Uani 1 1 d . . .
H96A H 1.1298 0.7979 -0.1714 0.040 Uiso 1 1 calc R . .
H96B H 1.0896 0.7118 -0.1434 0.040 Uiso 1 1 calc R . .
H96C H 1.0568 0.7992 -0.1071 0.040 Uiso 1 1 calc R . .
C97 C 0.98374(17) 0.88129(15) -0.21166(12) 0.0255(5) Uani 1 1 d . . .
H97A H 0.9598 0.9156 -0.1737 0.038 Uiso 1 1 calc R . .
H97B H 0.9403 0.8887 -0.2441 0.038 Uiso 1 1 calc R . .
H97C H 1.0440 0.8994 -0.2303 0.038 Uiso 1 1 calc R . .
C98 C 1.09194(16) 0.78153(15) -0.40676(11) 0.0241(5) Uani 1 1 d . . .
C99 C 1.14057(18) 0.76797(15) -0.47631(12) 0.0278(5) Uani 1 1 d . . .
H99A H 1.0943 0.7792 -0.5071 0.033 Uiso 1 1 calc R . .
H99B H 1.1875 0.8095 -0.4857 0.033 Uiso 1 1 calc R . .
C100 C 1.18761(18) 0.67922(16) -0.48743(12) 0.0294(5) Uani 1 1 d . . .
H10D H 1.2377 0.6687 -0.4595 0.035 Uiso 1 1 calc R . .
H10E H 1.2154 0.6734 -0.5332 0.035 Uiso 1 1 calc R . .
C101 C 1.11577(18) 0.61516(15) -0.47131(11) 0.0264(5) Uani 1 1 d . . .
H10F H 1.1467 0.5572 -0.4771 0.032 Uiso 1 1 calc R . .
H10G H 1.0692 0.6232 -0.5022 0.032 Uiso 1 1 calc R . .
C102 C 1.06610(16) 0.62320(14) -0.40171(11) 0.0217(5) Uani 1 1 d . . .
C103 C 1.16296(18) 0.78722(18) -0.35835(13) 0.0319(6) Uani 1 1 d . . .
H10H H 1.1319 0.7826 -0.3139 0.048 Uiso 1 1 calc R . .
H10I H 1.1902 0.8417 -0.3642 0.048 Uiso 1 1 calc R . .
H10J H 1.2119 0.7409 -0.3661 0.048 Uiso 1 1 calc R . .
C104 C 1.0310(2) 0.86502(16) -0.40609(13) 0.0328(6) Uani 1 1 d . . .
H10K H 0.9804 0.8596 -0.4322 0.049 Uiso 1 1 calc R . .
H10L H 1.0683 0.9104 -0.4243 0.049 Uiso 1 1 calc R . .
H10M H 1.0052 0.8786 -0.3614 0.049 Uiso 1 1 calc R . .
C105 C 1.13084(17) 0.59005(16) -0.35192(12) 0.0290(5) Uani 1 1 d . . .
H10N H 1.1902 0.6151 -0.3613 0.044 Uiso 1 1 calc R . .
H10O H 1.1413 0.5282 -0.3546 0.044 Uiso 1 1 calc R . .
H10P H 1.1023 0.6057 -0.3082 0.044 Uiso 1 1 calc R . .
C106 C 0.98358(17) 0.56969(15) -0.39647(12) 0.0265(5) Uani 1 1 d . . .
H10Q H 0.9567 0.5657 -0.3510 0.040 Uiso 1 1 calc R . .
H10R H 1.0042 0.5127 -0.4127 0.040 Uiso 1 1 calc R . .
H10S H 0.9369 0.5962 -0.4223 0.040 Uiso 1 1 calc R . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Sn1 O1 2.0393(16) . ?
Sn1 N1 2.1282(18) . ?
Si1 N1 1.7742(19) . ?
Si1 C42 1.886(2) . ?
Si1 C36 1.906(2) . ?
Si1 C39 1.906(2) . ?
O1 N2 1.463(2) . ?
N1 C1 1.442(3) . ?
C1 C6 1.421(3) . ?
C1 C2 1.425(3) . ?
Sn2 O2 2.0340(16) . ?
Sn2 N3 2.1192(18) . ?
Si2 N3 1.7732(19) . ?
Si2 C95 1.891(2) . ?
Si2 C92 1.905(2) . ?
Si2 C89 1.906(2) . ?
O2 N4 1.460(2) . ?
N2 C45 1.490(3) . ?
N2 C49 1.490(3) . ?
C2 C3 1.393(3) . ?
C2 C7 1.528(3) . ?
N3 C54 1.443(3) . ?
C3 C4 1.393(3) . ?
C3 H3 0.9500 . ?
N4 C102 1.491(3) . ?
N4 C98 1.496(3) . ?
C4 C5 1.393(3) . ?
C4 C8 1.511(3) . ?
C5 C6 1.392(3) . ?
C5 H5 0.9500 . ?
C6 C11 1.530(3) . ?
C7 C12 1.529(3) . ?
C7 C18 1.541(3) . ?
C7 H7 1.0000 . ?
C8 C10 1.521(4) . ?
C8 C9 1.523(4) . ?
C8 H8 1.0000 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 C24 1.525(3) . ?
C11 C30 1.534(3) . ?
C11 H11 1.0000 . ?
C12 C17 1.389(3) . ?
C12 C13 1.395(3) . ?
C13 C14 1.394(3) . ?
C13 H13 0.9500 . ?
C14 C15 1.384(4) . ?
C14 H14 0.9500 . ?
C15 C16 1.384(4) . ?
C15 H15 0.9500 . ?
C16 C17 1.393(4) . ?
C16 H16 0.9500 . ?
C17 H17 0.9500 . ?
C18 C19 1.390(3) . ?
C18 C23 1.395(3) . ?
C19 C20 1.396(4) . ?
C19 H19 0.9500 . ?
C20 C21 1.372(4) . ?
C20 H20 0.9500 . ?
C21 C22 1.389(4) . ?
C21 H21 0.9500 . ?
C22 C23 1.387(3) . ?
C22 H22 0.9500 . ?
C23 H23 0.9500 . ?
C24 C29 1.393(3) . ?
C24 C25 1.400(3) . ?
C25 C26 1.387(3) . ?
C25 H25 0.9500 . ?
C26 C27 1.386(3) . ?
C26 H26 0.9500 . ?
C27 C28 1.386(3) . ?
C27 H27 0.9500 . ?
C28 C29 1.397(3) . ?
C28 H28 0.9500 . ?
C29 H29 0.9500 . ?
C30 C31 1.396(3) . ?
C30 C35 1.396(3) . ?
C31 C32 1.389(3) . ?
C31 H31 0.9500 . ?
C32 C33 1.389(4) . ?
C32 H32 0.9500 . ?
C33 C34 1.381(4) . ?
C33 H33 0.9500 . ?
C34 C35 1.400(3) . ?
C34 H34 0.9500 . ?
C35 H35 0.9500 . ?
C36 C38 1.538(3) . ?
C36 C37 1.544(3) . ?
C36 H36 1.0000 . ?
C37 H37A 0.9800 . ?
C37 H37B 0.9800 . ?
C37 H37C 0.9800 . ?
C38 H38A 0.9800 . ?
C38 H38B 0.9800 . ?
C38 H38C 0.9800 . ?
C39 C41 1.541(3) . ?
C39 C40 1.542(3) . ?
C39 H39 1.0000 . ?
C40 H40A 0.9800 . ?
C40 H40B 0.9800 . ?
C40 H40C 0.9800 . ?
C41 H41A 0.9800 . ?
C41 H41B 0.9800 . ?
C41 H41C 0.9800 . ?
C42 C43 1.535(3) . ?
C42 C44 1.539(3) . ?
C42 H42 1.0000 . ?
C43 H43A 0.9800 . ?
C43 H43B 0.9800 . ?
C43 H43C 0.9800 . ?
C44 H44A 0.9800 . ?
C44 H44B 0.9800 . ?
C44 H44C 0.9800 . ?
C45 C50 1.527(4) . ?
C45 C46 1.540(3) . ?
C45 C51 1.543(4) . ?
C46 C47 1.522(4) . ?
C46 H46A 0.9900 . ?
C46 H46B 0.9900 . ?
C47 C48 1.516(3) . ?
C47 H47A 0.9900 . ?
C47 H47B 0.9900 . ?
C48 C49 1.535(3) . ?
C48 H48A 0.9900 . ?
C48 H48B 0.9900 . ?
C49 C52 1.525(3) . ?
C49 C53 1.544(3) . ?
C50 H50A 0.9800 . ?
C50 H50B 0.9800 . ?
C50 H50C 0.9800 . ?
C51 H51A 0.9800 . ?
C51 H51B 0.9800 . ?
C51 H51C 0.9800 . ?
C52 H52A 0.9800 . ?
C52 H52B 0.9800 . ?
C52 H52C 0.9800 . ?
C53 H53A 0.9800 . ?
C53 H53B 0.9800 . ?
C53 H53C 0.9800 . ?
C54 C55 1.421(3) . ?
C54 C59 1.423(3) . ?
C55 C56 1.391(3) . ?
C55 C60 1.526(3) . ?
C56 C57 1.391(3) . ?
C56 H56 0.9500 . ?
C57 C58 1.395(3) . ?
C57 C61 1.511(3) . ?
C58 C59 1.391(3) . ?
C58 H58 0.9500 . ?
C59 C64 1.534(3) . ?
C60 C65 1.527(3) . ?
C60 C71 1.543(3) . ?
C60 H60 1.0000 . ?
C61 C62 1.522(3) . ?
C61 C63 1.530(4) . ?
C61 H61 1.0000 . ?
C62 H62A 0.9800 . ?
C62 H62B 0.9800 . ?
C62 H62C 0.9800 . ?
C63 H63A 0.9800 . ?
C63 H63B 0.9800 . ?
C63 H63C 0.9800 . ?
C64 C77 1.528(3) . ?
C64 C83 1.544(3) . ?
C64 H64 1.0000 . ?
C65 C70 1.389(3) . ?
C65 C66 1.398(3) . ?
C66 C67 1.387(3) . ?
C66 H66 0.9500 . ?
C67 C68 1.383(4) . ?
C67 H67 0.9500 . ?
C68 C69 1.381(4) . ?
C68 H68 0.9500 . ?
C69 C70 1.394(4) . ?
C69 H69 0.9500 . ?
C70 H70 0.9500 . ?
C71 C72 1.395(3) . ?
C71 C76 1.395(3) . ?
C72 C73 1.390(4) . ?
C72 H72 0.9500 . ?
C73 C74 1.383(4) . ?
C73 H73 0.9500 . ?
C74 C75 1.379(4) . ?
C74 H74 0.9500 . ?
C75 C76 1.393(4) . ?
C75 H75 0.9500 . ?
C76 H76 0.9500 . ?
C77 C82 1.396(3) . ?
C77 C78 1.398(3) . ?
C78 C79 1.392(4) . ?
C78 H78 0.9500 . ?
C79 C80 1.388(4) . ?
C79 H79 0.9500 . ?
C80 C81 1.383(4) . ?
C80 H80 0.9500 . ?
C81 C82 1.398(4) . ?
C81 H81 0.9500 . ?
C82 H82 0.9500 . ?
C83 C84 1.390(3) . ?
C83 C88 1.395(3) . ?
C84 C85 1.404(3) . ?
C84 H84 0.9500 . ?
C85 C86 1.375(4) . ?
C85 H85 0.9500 . ?
C86 C87 1.389(4) . ?
C86 H86 0.9500 . ?
C87 C88 1.389(3) . ?
C87 H87 0.9500 . ?
C88 H88 0.9500 . ?
C89 C90 1.540(3) . ?
C89 C91 1.544(3) . ?
C89 H89 1.0000 . ?
C90 H90A 0.9800 . ?
C90 H90B 0.9800 . ?
C90 H90C 0.9800 . ?
C91 H91A 0.9800 . ?
C91 H91B 0.9800 . ?
C91 H91C 0.9800 . ?
C92 C94 1.541(3) . ?
C92 C93 1.541(3) . ?
C92 H92 1.0000 . ?
C93 H93A 0.9800 . ?
C93 H93B 0.9800 . ?
C93 H93C 0.9800 . ?
C94 H94A 0.9800 . ?
C94 H94B 0.9800 . ?
C94 H94C 0.9800 . ?
C95 C97 1.532(3) . ?
C95 C96 1.541(3) . ?
C95 H95 1.0000 . ?
C96 H96A 0.9800 . ?
C96 H96B 0.9800 . ?
C96 H96C 0.9800 . ?
C97 H97A 0.9800 . ?
C97 H97B 0.9800 . ?
C97 H97C 0.9800 . ?
C98 C104 1.528(3) . ?
C98 C99 1.540(3) . ?
C98 C103 1.541(3) . ?
C99 C100 1.520(3) . ?
C99 H99A 0.9900 . ?
C99 H99B 0.9900 . ?
C100 C101 1.525(3) . ?
C100 H10D 0.9900 . ?
C100 H10E 0.9900 . ?
C101 C102 1.538(3) . ?
C101 H10F 0.9900 . ?
C101 H10G 0.9900 . ?
C102 C106 1.524(3) . ?
C102 C105 1.539(3) . ?
C103 H10H 0.9800 . ?
C103 H10I 0.9800 . ?
C103 H10J 0.9800 . ?
C104 H10K 0.9800 . ?
C104 H10L 0.9800 . ?
C104 H10M 0.9800 . ?
C105 H10N 0.9800 . ?
C105 H10O 0.9800 . ?
C105 H10P 0.9800 . ?
C106 H10Q 0.9800 . ?
C106 H10R 0.9800 . ?
C106 H10S 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Sn1 N1 96.76(7) . . ?
N1 Si1 C42 106.09(10) . . ?
N1 Si1 C36 108.95(10) . . ?
C42 Si1 C36 112.76(10) . . ?
N1 Si1 C39 110.78(10) . . ?
C42 Si1 C39 109.18(11) . . ?
C36 Si1 C39 109.07(10) . . ?
N2 O1 Sn1 108.21(12) . . ?
C1 N1 Si1 117.83(14) . . ?
C1 N1 Sn1 110.17(13) . . ?
Si1 N1 Sn1 131.96(10) . . ?
C6 C1 C2 117.26(19) . . ?
C6 C1 N1 121.38(19) . . ?
C2 C1 N1 121.36(19) . . ?
O2 Sn2 N3 95.79(7) . . ?
N3 Si2 C95 106.30(9) . . ?
N3 Si2 C92 110.76(9) . . ?
C95 Si2 C92 108.65(10) . . ?
N3 Si2 C89 108.59(9) . . ?
C95 Si2 C89 113.00(10) . . ?
C92 Si2 C89 109.51(10) . . ?
N4 O2 Sn2 107.71(12) . . ?
O1 N2 C45 107.84(16) . . ?
O1 N2 C49 106.94(16) . . ?
C45 N2 C49 117.89(18) . . ?
C3 C2 C1 120.07(19) . . ?
C3 C2 C7 119.06(19) . . ?
C1 C2 C7 120.81(19) . . ?
C54 N3 Si2 117.63(14) . . ?
C54 N3 Sn2 109.10(13) . . ?
Si2 N3 Sn2 133.25(10) . . ?
C4 C3 C2 122.6(2) . . ?
C4 C3 H3 118.7 . . ?
C2 C3 H3 118.7 . . ?
O2 N4 C102 106.91(16) . . ?
O2 N4 C98 107.61(16) . . ?
C102 N4 C98 118.42(18) . . ?
C5 C4 C3 117.1(2) . . ?
C5 C4 C8 120.6(2) . . ?
C3 C4 C8 122.1(2) . . ?
C6 C5 C4 122.5(2) . . ?
C6 C5 H5 118.7 . . ?
C4 C5 H5 118.7 . . ?
C5 C6 C1 120.25(19) . . ?
C5 C6 C11 119.19(19) . . ?
C1 C6 C11 120.51(19) . . ?
C2 C7 C12 111.40(18) . . ?
C2 C7 C18 113.47(18) . . ?
C12 C7 C18 112.24(18) . . ?
C2 C7 H7 106.4 . . ?
C12 C7 H7 106.4 . . ?
C18 C7 H7 106.4 . . ?
C4 C8 C10 108.5(2) . . ?
C4 C8 C9 115.2(2) . . ?
C10 C8 C9 110.3(2) . . ?
C4 C8 H8 107.5 . . ?
C10 C8 H8 107.5 . . ?
C9 C8 H8 107.5 . . ?
C8 C9 H9A 109.5 . . ?
C8 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C8 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C8 C10 H10A 109.5 . . ?
C8 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C8 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C24 C11 C6 111.48(18) . . ?
C24 C11 C30 112.91(18) . . ?
C6 C11 C30 113.30(18) . . ?
C24 C11 H11 106.2 . . ?
C6 C11 H11 106.2 . . ?
C30 C11 H11 106.2 . . ?
C17 C12 C13 117.8(2) . . ?
C17 C12 C7 122.7(2) . . ?
C13 C12 C7 119.5(2) . . ?
C14 C13 C12 121.2(2) . . ?
C14 C13 H13 119.4 . . ?
C12 C13 H13 119.4 . . ?
C15 C14 C13 120.1(2) . . ?
C15 C14 H14 119.9 . . ?
C13 C14 H14 119.9 . . ?
C16 C15 C14 119.4(2) . . ?
C16 C15 H15 120.3 . . ?
C14 C15 H15 120.3 . . ?
C15 C16 C17 120.2(3) . . ?
C15 C16 H16 119.9 . . ?
C17 C16 H16 119.9 . . ?
C12 C17 C16 121.3(2) . . ?
C12 C17 H17 119.3 . . ?
C16 C17 H17 119.3 . . ?
C19 C18 C23 118.0(2) . . ?
C19 C18 C7 122.1(2) . . ?
C23 C18 C7 119.9(2) . . ?
C18 C19 C20 120.4(3) . . ?
C18 C19 H19 119.8 . . ?
C20 C19 H19 119.8 . . ?
C21 C20 C19 120.9(3) . . ?
C21 C20 H20 119.5 . . ?
C19 C20 H20 119.5 . . ?
C20 C21 C22 119.5(2) . . ?
C20 C21 H21 120.2 . . ?
C22 C21 H21 120.2 . . ?
C23 C22 C21 119.6(3) . . ?
C23 C22 H22 120.2 . . ?
C21 C22 H22 120.2 . . ?
C22 C23 C18 121.6(2) . . ?
C22 C23 H23 119.2 . . ?
C18 C23 H23 119.2 . . ?
C29 C24 C25 118.1(2) . . ?
C29 C24 C11 123.2(2) . . ?
C25 C24 C11 118.7(2) . . ?
C26 C25 C24 121.2(2) . . ?
C26 C25 H25 119.4 . . ?
C24 C25 H25 119.4 . . ?
C27 C26 C25 120.1(2) . . ?
C27 C26 H26 119.9 . . ?
C25 C26 H26 119.9 . . ?
C26 C27 C28 119.6(2) . . ?
C26 C27 H27 120.2 . . ?
C28 C27 H27 120.2 . . ?
C27 C28 C29 120.3(2) . . ?
C27 C28 H28 119.8 . . ?
C29 C28 H28 119.8 . . ?
C24 C29 C28 120.7(2) . . ?
C24 C29 H29 119.7 . . ?
C28 C29 H29 119.7 . . ?
C31 C30 C35 118.0(2) . . ?
C31 C30 C11 119.5(2) . . ?
C35 C30 C11 122.4(2) . . ?
C32 C31 C30 121.1(2) . . ?
C32 C31 H31 119.4 . . ?
C30 C31 H31 119.4 . . ?
C31 C32 C33 120.3(2) . . ?
C31 C32 H32 119.8 . . ?
C33 C32 H32 119.8 . . ?
C34 C33 C32 119.3(2) . . ?
C34 C33 H33 120.3 . . ?
C32 C33 H33 120.3 . . ?
C33 C34 C35 120.4(2) . . ?
C33 C34 H34 119.8 . . ?
C35 C34 H34 119.8 . . ?
C30 C35 C34 120.7(2) . . ?
C30 C35 H35 119.6 . . ?
C34 C35 H35 119.6 . . ?
C38 C36 C37 109.74(19) . . ?
C38 C36 Si1 115.16(16) . . ?
C37 C36 Si1 113.99(16) . . ?
C38 C36 H36 105.7 . . ?
C37 C36 H36 105.7 . . ?
Si1 C36 H36 105.7 . . ?
C36 C37 H37A 109.5 . . ?
C36 C37 H37B 109.5 . . ?
H37A C37 H37B 109.5 . . ?
C36 C37 H37C 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
C36 C38 H38A 109.5 . . ?
C36 C38 H38B 109.5 . . ?
H38A C38 H38B 109.5 . . ?
C36 C38 H38C 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
C41 C39 C40 110.6(2) . . ?
C41 C39 Si1 115.01(16) . . ?
C40 C39 Si1 110.77(16) . . ?
C41 C39 H39 106.6 . . ?
C40 C39 H39 106.6 . . ?
Si1 C39 H39 106.6 . . ?
C39 C40 H40A 109.5 . . ?
C39 C40 H40B 109.5 . . ?
H40A C40 H40B 109.5 . . ?
C39 C40 H40C 109.5 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?
C39 C41 H41A 109.5 . . ?
C39 C41 H41B 109.5 . . ?
H41A C41 H41B 109.5 . . ?
C39 C41 H41C 109.5 . . ?
H41A C41 H41C 109.5 . . ?
H41B C41 H41C 109.5 . . ?
C43 C42 C44 109.91(19) . . ?
C43 C42 Si1 111.82(16) . . ?
C44 C42 Si1 118.35(16) . . ?
C43 C42 H42 105.2 . . ?
C44 C42 H42 105.2 . . ?
Si1 C42 H42 105.2 . . ?
C42 C43 H43A 109.5 . . ?
C42 C43 H43B 109.5 . . ?
H43A C43 H43B 109.5 . . ?
C42 C43 H43C 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?
C42 C44 H44A 109.5 . . ?
C42 C44 H44B 109.5 . . ?
H44A C44 H44B 109.5 . . ?
C42 C44 H44C 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
N2 C45 C50 106.2(2) . . ?
N2 C45 C46 106.82(19) . . ?
C50 C45 C46 108.0(2) . . ?
N2 C45 C51 116.1(2) . . ?
C50 C45 C51 108.8(2) . . ?
C46 C45 C51 110.6(2) . . ?
C47 C46 C45 113.6(2) . . ?
C47 C46 H46A 108.8 . . ?
C45 C46 H46A 108.8 . . ?
C47 C46 H46B 108.8 . . ?
C45 C46 H46B 108.8 . . ?
H46A C46 H46B 107.7 . . ?
C48 C47 C46 109.3(2) . . ?
C48 C47 H47A 109.8 . . ?
C46 C47 H47A 109.8 . . ?
C48 C47 H47B 109.8 . . ?
C46 C47 H47B 109.8 . . ?
H47A C47 H47B 108.3 . . ?
C47 C48 C49 112.8(2) . . ?
C47 C48 H48A 109.0 . . ?
C49 C48 H48A 109.0 . . ?
C47 C48 H48B 109.0 . . ?
C49 C48 H48B 109.0 . . ?
H48A C48 H48B 107.8 . . ?
N2 C49 C52 106.43(18) . . ?
N2 C49 C48 107.30(18) . . ?
C52 C49 C48 107.31(19) . . ?
N2 C49 C53 115.77(19) . . ?
C52 C49 C53 108.59(19) . . ?
C48 C49 C53 111.03(19) . . ?
C45 C50 H50A 109.5 . . ?
C45 C50 H50B 109.5 . . ?
H50A C50 H50B 109.5 . . ?
C45 C50 H50C 109.5 . . ?
H50A C50 H50C 109.5 . . ?
H50B C50 H50C 109.5 . . ?
C45 C51 H51A 109.5 . . ?
C45 C51 H51B 109.5 . . ?
H51A C51 H51B 109.5 . . ?
C45 C51 H51C 109.5 . . ?
H51A C51 H51C 109.5 . . ?
H51B C51 H51C 109.5 . . ?
C49 C52 H52A 109.5 . . ?
C49 C52 H52B 109.5 . . ?
H52A C52 H52B 109.5 . . ?
C49 C52 H52C 109.5 . . ?
H52A C52 H52C 109.5 . . ?
H52B C52 H52C 109.5 . . ?
C49 C53 H53A 109.5 . . ?
C49 C53 H53B 109.5 . . ?
H53A C53 H53B 109.5 . . ?
C49 C53 H53C 109.5 . . ?
H53A C53 H53C 109.5 . . ?
H53B C53 H53C 109.5 . . ?
C55 C54 C59 117.57(19) . . ?
C55 C54 N3 120.95(18) . . ?
C59 C54 N3 121.47(18) . . ?
C56 C55 C54 120.44(19) . . ?
C56 C55 C60 117.92(18) . . ?
C54 C55 C60 121.62(18) . . ?
C55 C56 C57 122.0(2) . . ?
C55 C56 H56 119.0 . . ?
C57 C56 H56 119.0 . . ?
C56 C57 C58 117.4(2) . . ?
C56 C57 C61 120.9(2) . . ?
C58 C57 C61 121.2(2) . . ?
C59 C58 C57 122.67(19) . . ?
C59 C58 H58 118.7 . . ?
C57 C58 H58 118.7 . . ?
C58 C59 C54 119.6(2) . . ?
C58 C59 C64 119.49(19) . . ?
C54 C59 C64 120.90(19) . . ?
C55 C60 C65 112.25(18) . . ?
C55 C60 C71 112.34(17) . . ?
C65 C60 C71 111.64(17) . . ?
C55 C60 H60 106.7 . . ?
C65 C60 H60 106.7 . . ?
C71 C60 H60 106.7 . . ?
C57 C61 C62 114.47(19) . . ?
C57 C61 C63 107.3(2) . . ?
C62 C61 C63 111.2(3) . . ?
C57 C61 H61 107.9 . . ?
C62 C61 H61 107.9 . . ?
C63 C61 H61 107.9 . . ?
C61 C62 H62A 109.5 . . ?
C61 C62 H62B 109.5 . . ?
H62A C62 H62B 109.5 . . ?
C61 C62 H62C 109.5 . . ?
H62A C62 H62C 109.5 . . ?
H62B C62 H62C 109.5 . . ?
C61 C63 H63A 109.5 . . ?
C61 C63 H63B 109.5 . . ?
H63A C63 H63B 109.5 . . ?
C61 C63 H63C 109.5 . . ?
H63A C63 H63C 109.5 . . ?
H63B C63 H63C 109.5 . . ?
C77 C64 C59 111.80(18) . . ?
C77 C64 C83 111.79(18) . . ?
C59 C64 C83 113.02(18) . . ?
C77 C64 H64 106.6 . . ?
C59 C64 H64 106.6 . . ?
C83 C64 H64 106.6 . . ?
C70 C65 C66 117.8(2) . . ?
C70 C65 C60 123.41(19) . . ?
C66 C65 C60 118.8(2) . . ?
C67 C66 C65 121.4(2) . . ?
C67 C66 H66 119.3 . . ?
C65 C66 H66 119.3 . . ?
C68 C67 C66 120.0(2) . . ?
C68 C67 H67 120.0 . . ?
C66 C67 H67 120.0 . . ?
C69 C68 C67 119.6(2) . . ?
C69 C68 H68 120.2 . . ?
C67 C68 H68 120.2 . . ?
C68 C69 C70 120.3(2) . . ?
C68 C69 H69 119.8 . . ?
C70 C69 H69 119.8 . . ?
C65 C70 C69 121.0(2) . . ?
C65 C70 H70 119.5 . . ?
C69 C70 H70 119.5 . . ?
C72 C71 C76 117.8(2) . . ?
C72 C71 C60 119.41(19) . . ?
C76 C71 C60 122.8(2) . . ?
C73 C72 C71 121.4(2) . . ?
C73 C72 H72 119.3 . . ?
C71 C72 H72 119.3 . . ?
C74 C73 C72 120.1(3) . . ?
C74 C73 H73 120.0 . . ?
C72 C73 H73 120.0 . . ?
C75 C74 C73 119.2(2) . . ?
C75 C74 H74 120.4 . . ?
C73 C74 H74 120.4 . . ?
C74 C75 C76 121.0(3) . . ?
C74 C75 H75 119.5 . . ?
C76 C75 H75 119.5 . . ?
C75 C76 C71 120.5(2) . . ?
C75 C76 H76 119.8 . . ?
C71 C76 H76 119.8 . . ?
C82 C77 C78 118.0(2) . . ?
C82 C77 C64 121.9(2) . . ?
C78 C77 C64 120.1(2) . . ?
C79 C78 C77 121.3(2) . . ?
C79 C78 H78 119.3 . . ?
C77 C78 H78 119.3 . . ?
C80 C79 C78 119.8(2) . . ?
C80 C79 H79 120.1 . . ?
C78 C79 H79 120.1 . . ?
C81 C80 C79 119.7(2) . . ?
C81 C80 H80 120.1 . . ?
C79 C80 H80 120.1 . . ?
C80 C81 C82 120.3(2) . . ?
C80 C81 H81 119.8 . . ?
C82 C81 H81 119.8 . . ?
C77 C82 C81 120.7(2) . . ?
C77 C82 H82 119.6 . . ?
C81 C82 H82 119.6 . . ?
C84 C83 C88 118.1(2) . . ?
C84 C83 C64 121.4(2) . . ?
C88 C83 C64 120.46(19) . . ?
C83 C84 C85 120.4(2) . . ?
C83 C84 H84 119.8 . . ?
C85 C84 H84 119.8 . . ?
C86 C85 C84 120.9(2) . . ?
C86 C85 H85 119.6 . . ?
C84 C85 H85 119.6 . . ?
C85 C86 C87 119.1(2) . . ?
C85 C86 H86 120.4 . . ?
C87 C86 H86 120.4 . . ?
C88 C87 C86 120.2(2) . . ?
C88 C87 H87 119.9 . . ?
C86 C87 H87 119.9 . . ?
C87 C88 C83 121.3(2) . . ?
C87 C88 H88 119.4 . . ?
C83 C88 H88 119.4 . . ?
C90 C89 C91 109.23(18) . . ?
C90 C89 Si2 115.06(15) . . ?
C91 C89 Si2 114.69(15) . . ?
C90 C89 H89 105.6 . . ?
C91 C89 H89 105.6 . . ?
Si2 C89 H89 105.6 . . ?
C89 C90 H90A 109.5 . . ?
C89 C90 H90B 109.5 . . ?
H90A C90 H90B 109.5 . . ?
C89 C90 H90C 109.5 . . ?
H90A C90 H90C 109.5 . . ?
H90B C90 H90C 109.5 . . ?
C89 C91 H91A 109.5 . . ?
C89 C91 H91B 109.5 . . ?
H91A C91 H91B 109.5 . . ?
C89 C91 H91C 109.5 . . ?
H91A C91 H91C 109.5 . . ?
H91B C91 H91C 109.5 . . ?
C94 C92 C93 110.76(18) . . ?
C94 C92 Si2 110.58(15) . . ?
C93 C92 Si2 115.51(15) . . ?
C94 C92 H92 106.5 . . ?
C93 C92 H92 106.5 . . ?
Si2 C92 H92 106.5 . . ?
C92 C93 H93A 109.5 . . ?
C92 C93 H93B 109.5 . . ?
H93A C93 H93B 109.5 . . ?
C92 C93 H93C 109.5 . . ?
H93A C93 H93C 109.5 . . ?
H93B C93 H93C 109.5 . . ?
C92 C94 H94A 109.5 . . ?
C92 C94 H94B 109.5 . . ?
H94A C94 H94B 109.5 . . ?
C92 C94 H94C 109.5 . . ?
H94A C94 H94C 109.5 . . ?
H94B C94 H94C 109.5 . . ?
C97 C95 C96 109.78(19) . . ?
C97 C95 Si2 112.08(16) . . ?
C96 C95 Si2 118.19(16) . . ?
C97 C95 H95 105.2 . . ?
C96 C95 H95 105.2 . . ?
Si2 C95 H95 105.2 . . ?
C95 C96 H96A 109.5 . . ?
C95 C96 H96B 109.5 . . ?
H96A C96 H96B 109.5 . . ?
C95 C96 H96C 109.5 . . ?
H96A C96 H96C 109.5 . . ?
H96B C96 H96C 109.5 . . ?
C95 C97 H97A 109.5 . . ?
C95 C97 H97B 109.5 . . ?
H97A C97 H97B 109.5 . . ?
C95 C97 H97C 109.5 . . ?
H97A C97 H97C 109.5 . . ?
H97B C97 H97C 109.5 . . ?
N4 C98 C104 106.23(19) . . ?
N4 C98 C99 106.57(18) . . ?
C104 C98 C99 107.9(2) . . ?
N4 C98 C103 115.9(2) . . ?
C104 C98 C103 108.7(2) . . ?
C99 C98 C103 111.1(2) . . ?
C100 C99 C98 113.4(2) . . ?
C100 C99 H99A 108.9 . . ?
C98 C99 H99A 108.9 . . ?
C100 C99 H99B 108.9 . . ?
C98 C99 H99B 108.9 . . ?
H99A C99 H99B 107.7 . . ?
C99 C100 C101 108.9(2) . . ?
C99 C100 H10D 109.9 . . ?
C101 C100 H10D 109.9 . . ?
C99 C100 H10E 109.9 . . ?
C101 C100 H10E 109.9 . . ?
H10D C100 H10E 108.3 . . ?
C100 C101 C102 113.0(2) . . ?
C100 C101 H10F 109.0 . . ?
C102 C101 H10F 109.0 . . ?
C100 C101 H10G 109.0 . . ?
C102 C101 H10G 109.0 . . ?
H10F C101 H10G 107.8 . . ?
N4 C102 C106 106.60(18) . . ?
N4 C102 C101 107.20(18) . . ?
C106 C102 C101 107.56(19) . . ?
N4 C102 C105 115.21(19) . . ?
C106 C102 C105 108.94(19) . . ?
C101 C102 C105 110.99(19) . . ?
C98 C103 H10H 109.5 . . ?
C98 C103 H10I 109.5 . . ?
H10H C103 H10I 109.5 . . ?
C98 C103 H10J 109.5 . . ?
H10H C103 H10J 109.5 . . ?
H10I C103 H10J 109.5 . . ?
C98 C104 H10K 109.5 . . ?
C98 C104 H10L 109.5 . . ?
H10K C104 H10L 109.5 . . ?
C98 C104 H10M 109.5 . . ?
H10K C104 H10M 109.5 . . ?
H10L C104 H10M 109.5 . . ?
C102 C105 H10N 109.5 . . ?
C102 C105 H10O 109.5 . . ?
H10N C105 H10O 109.5 . . ?
C102 C105 H10P 109.5 . . ?
H10N C105 H10P 109.5 . . ?
H10O C105 H10P 109.5 . . ?
C102 C106 H10Q 109.5 . . ?
C102 C106 H10R 109.5 . . ?
H10Q C106 H10R 109.5 . . ?
C102 C106 H10S 109.5 . . ?
H10Q C106 H10S 109.5 . . ?
H10R C106 H10S 109.5 . . ?

_diffrn_measured_fraction_theta_max 0.994
_diffrn_reflns_theta_full        26.00
_diffrn_measured_fraction_theta_full 0.994
_refine_diff_density_max         0.958
_refine_diff_density_min         -0.862
_refine_diff_density_rms         0.070
####################################################################### 
# 
# 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_compound25
_database_code_depnum_ccdc_archive 'CCDC 1422741'
_audit_update_record             
;
2015-09-07 deposited with the CCDC.
2015-09-22 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C112 H154 Ge2 N2 O2 Si2'
_chemical_formula_weight         1761.73

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.2541 0.3302 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ge Ge -1.0885 0.8855 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   P2(1)/n

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

_cell_length_a                   15.0392(3)
_cell_length_b                   12.4994(2)
_cell_length_c                   26.2128(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 93.127(2)
_cell_angle_gamma                90.00
_cell_volume                     4920.17(15)
_cell_formula_units_Z            2
_cell_measurement_temperature    123(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.189
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1896
_exptl_absorpt_coefficient_mu    1.359
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.681
_exptl_absorpt_correction_T_max  0.769
_exptl_absorpt_process_details   'SCALE3 ABSPACK'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      123(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         'Enhance (Cu) X-ray Source'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Oxford Gemini Ultra'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            37623
_diffrn_reflns_av_R_equivalents  0.0297
_diffrn_reflns_av_sigmaI/netI    0.0226
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_theta_min         6.64
_diffrn_reflns_theta_max         66.94
_reflns_number_total             8723
_reflns_number_gt                7914
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       CrysalisPro
_computing_cell_refinement       CrysalisPro
_computing_data_reduction        CrysalisPro
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    X-Seed
_computing_publication_material  CifTAB

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger.
 A molecule of hexane of crystallisation, which is disordered over two sites,
 was refined in the asymmetric unit with the carbon atoms of both disordered
 sets, set as isotropic. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0518P)²+4.8993P] 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         8723
_refine_ls_number_parameters     548
_refine_ls_number_restraints     18
_refine_ls_R_factor_all          0.0439
_refine_ls_R_factor_gt           0.0391
_refine_ls_wR_factor_ref         0.1043
_refine_ls_wR_factor_gt          0.1000
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_restrained_S_all      1.105
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ge1 Ge 0.577915(15) -0.012024(19) 0.026432(9) 0.01816(9) Uani 1 1 d . . .
Si1 Si 0.59319(4) 0.21646(4) 0.09518(2) 0.01939(13) Uani 1 1 d . . .
O1 O 0.53877(9) 0.04631(12) -0.03425(5) 0.0215(3) Uani 1 1 d . . .
N1 N 0.62542(11) 0.08525(14) 0.07557(6) 0.0179(4) Uani 1 1 d . . .
C1 C 0.70475(14) 0.03995(16) 0.10193(8) 0.0178(4) Uani 1 1 d . . .
C2 C 0.78951(14) 0.05559(16) 0.08170(7) 0.0182(4) Uani 1 1 d . . .
C3 C 0.86328(14) 0.00289(17) 0.10388(8) 0.0205(4) Uani 1 1 d . . .
H3 H 0.9200 0.0158 0.0908 0.025 Uiso 1 1 calc R . .
C4 C 0.85717(14) -0.06812(17) 0.14452(8) 0.0204(4) Uani 1 1 d . . .
C5 C 0.77460(14) -0.08010(17) 0.16480(8) 0.0204(4) Uani 1 1 d . . .
H5 H 0.7695 -0.1269 0.1930 0.024 Uiso 1 1 calc R . .
C6 C 0.69827(14) -0.02630(16) 0.14557(8) 0.0180(4) Uani 1 1 d . . .
C7 C 0.93903(14) -0.12649(18) 0.16649(8) 0.0247(5) Uani 1 1 d . . .
H7 H 0.9186 -0.1837 0.1898 0.030 Uiso 1 1 calc R . .
C8 C 0.99934(16) -0.0503(2) 0.19811(9) 0.0317(5) Uani 1 1 d . . .
H8A H 1.0153 0.0106 0.1769 0.048 Uiso 1 1 calc R . .
H8B H 1.0536 -0.0882 0.2102 0.048 Uiso 1 1 calc R . .
H8C H 0.9679 -0.0246 0.2275 0.048 Uiso 1 1 calc R . .
C9 C 0.99115(16) -0.1803(2) 0.12486(10) 0.0313(5) Uani 1 1 d . . .
H9A H 0.9504 -0.2236 0.1029 0.047 Uiso 1 1 calc R . .
H9B H 1.0375 -0.2264 0.1408 0.047 Uiso 1 1 calc R . .
H9C H 1.0189 -0.1254 0.1043 0.047 Uiso 1 1 calc R . .
C10 C 0.61121(14) -0.03885(17) 0.17306(8) 0.0198(4) Uani 1 1 d . . .
H10 H 0.5658 0.0049 0.1531 0.024 Uiso 1 1 calc R . .
C11 C 0.57251(14) -0.15182(18) 0.17523(8) 0.0218(4) Uani 1 1 d . . .
C12 C 0.49324(16) -0.1751(2) 0.14720(9) 0.0294(5) Uani 1 1 d . . .
H12 H 0.4649 -0.1212 0.1266 0.035 Uiso 1 1 calc R . .
C13 C 0.45552(18) -0.2763(2) 0.14922(10) 0.0376(6) Uani 1 1 d . . .
H13 H 0.4015 -0.2910 0.1300 0.045 Uiso 1 1 calc R . .
C14 C 0.49586(19) -0.3555(2) 0.17887(12) 0.0438(7) Uani 1 1 d . . .
H14 H 0.4711 -0.4254 0.1792 0.053 Uiso 1 1 calc R . .
C15 C 0.57290(18) -0.3322(2) 0.20813(12) 0.0423(7) Uani 1 1 d . . .
H15 H 0.6004 -0.3859 0.2292 0.051 Uiso 1 1 calc R . .
C16 C 0.61017(15) -0.23076(19) 0.20682(9) 0.0294(5) Uani 1 1 d . . .
H16 H 0.6621 -0.2151 0.2278 0.035 Uiso 1 1 calc R . .
C17 C 0.61547(15) 0.00728(17) 0.22755(8) 0.0215(4) Uani 1 1 d . . .
C18 C 0.53721(16) 0.00598(19) 0.25415(9) 0.0291(5) Uani 1 1 d . . .
H18 H 0.4843 -0.0229 0.2381 0.035 Uiso 1 1 calc R . .
C19 C 0.53530(18) 0.0459(2) 0.30339(10) 0.0343(6) Uani 1 1 d . . .
H19 H 0.4813 0.0447 0.3206 0.041 Uiso 1 1 calc R . .
C20 C 0.61177(18) 0.08740(19) 0.32752(9) 0.0319(5) Uani 1 1 d . . .
H20 H 0.6110 0.1133 0.3616 0.038 Uiso 1 1 calc R . .
C21 C 0.68897(17) 0.09091(18) 0.30175(9) 0.0284(5) Uani 1 1 d . . .
H21 H 0.7413 0.1209 0.3179 0.034 Uiso 1 1 calc R . .
C22 C 0.69102(15) 0.05098(18) 0.25230(8) 0.0241(5) Uani 1 1 d . . .
H22 H 0.7450 0.0536 0.2352 0.029 Uiso 1 1 calc R . .
C23 C 0.80332(14) 0.12641(17) 0.03488(8) 0.0198(4) Uani 1 1 d . . .
H23 H 0.7480 0.1703 0.0298 0.024 Uiso 1 1 calc R . .
C24 C 0.88052(14) 0.20702(17) 0.04296(8) 0.0221(4) Uani 1 1 d . . .
C25 C 0.91174(15) 0.24119(19) 0.09132(9) 0.0262(5) Uani 1 1 d . . .
H25 H 0.8882 0.2098 0.1207 0.031 Uiso 1 1 calc R . .
C26 C 0.97637(16) 0.3200(2) 0.09741(10) 0.0337(5) Uani 1 1 d . . .
H26 H 0.9961 0.3425 0.1307 0.040 Uiso 1 1 calc R . .
C27 C 1.01214(18) 0.3659(2) 0.05501(11) 0.0403(6) Uani 1 1 d . . .
H27 H 1.0564 0.4199 0.0591 0.048 Uiso 1 1 calc R . .
C28 C 0.98285(19) 0.3325(2) 0.00696(11) 0.0405(6) Uani 1 1 d . . .
H28 H 1.0074 0.3633 -0.0223 0.049 Uiso 1 1 calc R . .
C29 C 0.91767(16) 0.2541(2) 0.00080(9) 0.0307(5) Uani 1 1 d . . .
H29 H 0.8981 0.2322 -0.0326 0.037 Uiso 1 1 calc R . .
C30 C 0.81224(14) 0.06442(18) -0.01501(8) 0.0225(4) Uani 1 1 d . . .
C31 C 0.75756(15) 0.09141(19) -0.05780(8) 0.0266(5) Uani 1 1 d . . .
H31 H 0.7128 0.1444 -0.0548 0.032 Uiso 1 1 calc R . .
C32 C 0.76724(17) 0.0423(2) -0.10477(9) 0.0335(6) Uani 1 1 d . . .
H32 H 0.7295 0.0621 -0.1335 0.040 Uiso 1 1 calc R . .
C33 C 0.83169(17) -0.0354(2) -0.10977(9) 0.0343(6) Uani 1 1 d . . .
H33 H 0.8381 -0.0695 -0.1417 0.041 Uiso 1 1 calc R . .
C34 C 0.88699(16) -0.0630(2) -0.06760(10) 0.0325(5) Uani 1 1 d . . .
H34 H 0.9316 -0.1160 -0.0708 0.039 Uiso 1 1 calc R . .
C35 C 0.87752(15) -0.01346(18) -0.02075(9) 0.0260(5) Uani 1 1 d . . .
H35 H 0.9159 -0.0328 0.0077 0.031 Uiso 1 1 calc R . .
C36 C 0.51976(15) 0.20731(18) 0.15158(8) 0.0256(5) Uani 1 1 d . . .
H36 H 0.5554 0.1641 0.1775 0.031 Uiso 1 1 calc R . .
C37 C 0.50083(19) 0.3133(2) 0.17931(10) 0.0360(6) Uani 1 1 d . . .
H37A H 0.4615 0.3581 0.1573 0.054 Uiso 1 1 calc R . .
H37B H 0.5570 0.3512 0.1871 0.054 Uiso 1 1 calc R . .
H37C H 0.4720 0.2979 0.2111 0.054 Uiso 1 1 calc R . .
C38 C 0.43274(16) 0.1451(2) 0.14292(9) 0.0303(5) Uani 1 1 d . . .
H38A H 0.4136 0.1183 0.1757 0.045 Uiso 1 1 calc R . .
H38B H 0.4421 0.0846 0.1200 0.045 Uiso 1 1 calc R . .
H38C H 0.3868 0.1923 0.1275 0.045 Uiso 1 1 calc R . .
C39 C 0.53699(15) 0.28411(18) 0.03778(8) 0.0236(5) Uani 1 1 d . . .
H39 H 0.4927 0.2312 0.0231 0.028 Uiso 1 1 calc R . .
C40 C 0.59906(16) 0.3089(2) -0.00530(9) 0.0304(5) Uani 1 1 d . . .
H40A H 0.5669 0.3516 -0.0317 0.046 Uiso 1 1 calc R . .
H40B H 0.6191 0.2418 -0.0202 0.046 Uiso 1 1 calc R . .
H40C H 0.6508 0.3493 0.0086 0.046 Uiso 1 1 calc R . .
C41 C 0.48253(16) 0.38398(19) 0.05092(9) 0.0303(5) Uani 1 1 d . . .
H41A H 0.5216 0.4362 0.0688 0.045 Uiso 1 1 calc R . .
H41B H 0.4348 0.3633 0.0730 0.045 Uiso 1 1 calc R . .
H41C H 0.4565 0.4159 0.0194 0.045 Uiso 1 1 calc R . .
C42 C 0.69700(15) 0.29399(17) 0.11740(8) 0.0244(5) Uani 1 1 d . . .
H42 H 0.7439 0.2725 0.0938 0.029 Uiso 1 1 calc R . .
C43 C 0.68888(18) 0.41675(19) 0.11236(10) 0.0343(6) Uani 1 1 d . . .
H43A H 0.6459 0.4433 0.1361 0.051 Uiso 1 1 calc R . .
H43B H 0.6685 0.4352 0.0773 0.051 Uiso 1 1 calc R . .
H43C H 0.7471 0.4497 0.1204 0.051 Uiso 1 1 calc R . .
C44 C 0.73574(17) 0.2676(2) 0.17154(9) 0.0301(5) Uani 1 1 d . . .
H44A H 0.7882 0.3123 0.1795 0.045 Uiso 1 1 calc R . .
H44B H 0.7530 0.1920 0.1732 0.045 Uiso 1 1 calc R . .
H44C H 0.6907 0.2815 0.1964 0.045 Uiso 1 1 calc R . .
C45 C 0.66444(14) -0.13368(17) 0.02508(8) 0.0229(5) Uani 1 1 d . . .
H45 H 0.7217 -0.1040 0.0403 0.028 Uiso 1 1 calc R . .
C46 C 0.68727(15) -0.17665(19) -0.02724(9) 0.0262(5) Uani 1 1 d . . .
H46A H 0.7045 -0.1166 -0.0493 0.031 Uiso 1 1 calc R . .
H46B H 0.6343 -0.2119 -0.0438 0.031 Uiso 1 1 calc R . .
C47 C 0.76412(17) -0.2572(2) -0.02142(11) 0.0356(6) Uani 1 1 d . . .
H47A H 0.7756 -0.2870 -0.0554 0.043 Uiso 1 1 calc R . .
H47B H 0.8186 -0.2193 -0.0085 0.043 Uiso 1 1 calc R . .
C48 C 0.74532(17) -0.3489(2) 0.01479(10) 0.0342(6) Uani 1 1 d . . .
H48A H 0.6965 -0.3938 -0.0004 0.041 Uiso 1 1 calc R . .
H48B H 0.7990 -0.3943 0.0198 0.041 Uiso 1 1 calc R . .
C49 C 0.71933(17) -0.3056(2) 0.06599(10) 0.0330(5) Uani 1 1 d . . .
H49A H 0.7713 -0.2692 0.0831 0.040 Uiso 1 1 calc R . .
H49B H 0.7024 -0.3659 0.0880 0.040 Uiso 1 1 calc R . .
C50 C 0.64157(16) -0.22669(18) 0.06018(8) 0.0258(5) Uani 1 1 d . . .
H50A H 0.6280 -0.1985 0.0942 0.031 Uiso 1 1 calc R . .
H50B H 0.5880 -0.2642 0.0457 0.031 Uiso 1 1 calc R . .
C51 C 0.2648(8) 0.0713(10) 0.4018(3) 0.075(3) Uiso 0.413(6) 1 d PD A 1
H51A H 0.2125 0.0344 0.4140 0.113 Uiso 0.413(6) 1 calc PR A 1
H51B H 0.2621 0.1473 0.4109 0.113 Uiso 0.413(6) 1 calc PR A 1
H51C H 0.3190 0.0395 0.4178 0.113 Uiso 0.413(6) 1 calc PR A 1
C51A C 0.2899(5) 0.1016(5) 0.3949(3) 0.0643(19) Uiso 0.587(6) 1 d PD A 2
H51D H 0.3506 0.0794 0.4055 0.096 Uiso 0.587(6) 1 calc PR A 2
H51E H 0.2591 0.1257 0.4248 0.096 Uiso 0.587(6) 1 calc PR A 2
H51F H 0.2922 0.1604 0.3703 0.096 Uiso 0.587(6) 1 calc PR A 2
C52 C 0.2660(6) 0.0595(6) 0.3413(3) 0.061(2) Uiso 0.413(6) 1 d PD A 1
H52A H 0.2048 0.0658 0.3257 0.073 Uiso 0.413(6) 1 calc PR A 1
H52B H 0.3029 0.1168 0.3271 0.073 Uiso 0.413(6) 1 calc PR A 1
C52A C 0.2387(5) 0.0054(5) 0.3697(3) 0.074(2) Uiso 0.587(6) 1 d PD A 2
H52C H 0.2228 -0.0447 0.3970 0.089 Uiso 0.587(6) 1 calc PR A 2
H52D H 0.1825 0.0324 0.3530 0.089 Uiso 0.587(6) 1 calc PR A 2
C53 C 0.3042(9) -0.0484(11) 0.3292(6) 0.197(12) Uiso 0.413(6) 1 d PD A 1
H53A H 0.3507 -0.0367 0.3045 0.236 Uiso 0.413(6) 1 calc PR A 1
H53B H 0.3347 -0.0757 0.3610 0.236 Uiso 0.413(6) 1 calc PR A 1
C53A C 0.2852(4) -0.0529(4) 0.33273(18) 0.0424(13) Uiso 0.587(6) 1 d PD A 2
H53C H 0.3024 -0.1201 0.3507 0.051 Uiso 0.587(6) 1 calc PR A 2
H53D H 0.3414 -0.0124 0.3302 0.051 Uiso 0.587(6) 1 calc PR A 2
C54 C 0.2460(6) -0.1342(6) 0.3087(3) 0.069(3) Uiso 0.413(6) 1 d PD A 1
H54A H 0.1856 -0.1042 0.3019 0.083 Uiso 0.413(6) 1 calc PR A 1
H54B H 0.2417 -0.1896 0.3354 0.083 Uiso 0.413(6) 1 calc PR A 1
C54A C 0.2631(6) -0.0884(6) 0.2790(3) 0.101(3) Uiso 0.587(6) 1 d PD A 2
H54C H 0.2856 -0.0359 0.2545 0.121 Uiso 0.587(6) 1 calc PR A 2
H54D H 0.1979 -0.0951 0.2728 0.121 Uiso 0.587(6) 1 calc PR A 2
C55 C 0.2740(6) -0.1886(8) 0.2600(3) 0.074(3) Uiso 0.413(6) 1 d PD A 1
H55C H 0.2892 -0.1347 0.2342 0.089 Uiso 0.413(6) 1 calc PR A 1
H55D H 0.2255 -0.2345 0.2453 0.089 Uiso 0.413(6) 1 calc PR A 1
C55A C 0.3095(8) -0.2001(8) 0.2724(4) 0.133(4) Uiso 0.587(6) 1 d PD A 2
H55A H 0.3652 -0.1886 0.2547 0.160 Uiso 0.587(6) 1 calc PR A 2
H55B H 0.3261 -0.2289 0.3068 0.160 Uiso 0.587(6) 1 calc PR A 2
C56 C 0.3560(5) -0.2563(7) 0.2761(3) 0.063(2) Uiso 0.413(6) 1 d PD A 1
H56A H 0.4069 -0.2328 0.2572 0.094 Uiso 0.413(6) 1 calc PR A 1
H56B H 0.3435 -0.3318 0.2687 0.094 Uiso 0.413(6) 1 calc PR A 1
H56C H 0.3699 -0.2474 0.3129 0.094 Uiso 0.413(6) 1 calc PR A 1
C56A C 0.2564(10) -0.2808(8) 0.2441(6) 0.177(6) Uiso 0.587(6) 1 d PD A 2
H56D H 0.2610 -0.2696 0.2074 0.266 Uiso 0.587(6) 1 calc PR A 2
H56E H 0.1940 -0.2747 0.2527 0.266 Uiso 0.587(6) 1 calc PR A 2
H56F H 0.2787 -0.3523 0.2534 0.266 Uiso 0.587(6) 1 calc PR 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 O1 1.8182(14) . ?
Ge1 O1 1.8288(14) 3_655 ?
Ge1 N1 1.8834(17) . ?
Ge1 C45 2.003(2) . ?
Si1 N1 1.7933(18) . ?
Si1 C39 1.885(2) . ?
Si1 C36 1.896(2) . ?
Si1 C42 1.902(2) . ?
O1 Ge1 1.8288(14) 3_655 ?
N1 C1 1.460(3) . ?
C1 C6 1.420(3) . ?
C1 C2 1.421(3) . ?
C2 C3 1.390(3) . ?
C2 C23 1.536(3) . ?
C3 C4 1.393(3) . ?
C4 C5 1.385(3) . ?
C4 C7 1.517(3) . ?
C5 C6 1.400(3) . ?
C6 C10 1.537(3) . ?
C7 C8 1.528(3) . ?
C7 C9 1.533(3) . ?
C10 C11 1.529(3) . ?
C10 C17 1.538(3) . ?
C11 C16 1.389(3) . ?
C11 C12 1.396(3) . ?
C12 C13 1.388(4) . ?
C13 C14 1.379(4) . ?
C14 C15 1.385(4) . ?
C15 C16 1.387(4) . ?
C17 C22 1.389(3) . ?
C17 C18 1.400(3) . ?
C18 C19 1.386(4) . ?
C19 C20 1.383(4) . ?
C20 C21 1.375(4) . ?
C21 C22 1.391(3) . ?
C23 C30 1.532(3) . ?
C23 C24 1.543(3) . ?
C24 C25 1.394(3) . ?
C24 C29 1.395(3) . ?
C25 C26 1.387(3) . ?
C26 C27 1.386(4) . ?
C27 C28 1.376(4) . ?
C28 C29 1.389(3) . ?
C30 C31 1.396(3) . ?
C30 C35 1.397(3) . ?
C31 C32 1.391(3) . ?
C32 C33 1.383(4) . ?
C33 C34 1.390(4) . ?
C34 C35 1.389(3) . ?
C36 C38 1.529(3) . ?
C36 C37 1.545(3) . ?
C39 C40 1.536(3) . ?
C39 C41 1.542(3) . ?
C42 C44 1.540(3) . ?
C42 C43 1.544(3) . ?
C45 C46 1.529(3) . ?
C45 C50 1.533(3) . ?
C46 C47 1.534(3) . ?
C47 C48 1.525(4) . ?
C48 C49 1.518(4) . ?
C49 C50 1.531(3) . ?
C51 C52 1.595(7) . ?
C51A C52A 1.556(6) . ?
C52 C53 1.505(8) . ?
C52A C53A 1.425(6) . ?
C53 C54 1.468(8) . ?
C53A C54A 1.496(6) . ?
C54 C55 1.526(7) . ?
C54A C55A 1.573(7) . ?
C55 C56 1.535(8) . ?
C55A C56A 1.463(8) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Ge1 O1 85.70(6) . 3_655 ?
O1 Ge1 N1 115.59(7) . . ?
O1 Ge1 N1 113.90(7) 3_655 . ?
O1 Ge1 C45 117.94(8) . . ?
O1 Ge1 C45 116.90(8) 3_655 . ?
N1 Ge1 C45 106.24(8) . . ?
N1 Si1 C39 107.32(9) . . ?
N1 Si1 C36 110.26(9) . . ?
C39 Si1 C36 113.23(10) . . ?
N1 Si1 C42 108.89(9) . . ?
C39 Si1 C42 109.92(10) . . ?
C36 Si1 C42 107.17(10) . . ?
Ge1 O1 Ge1 94.30(6) . 3_655 ?
C1 N1 Si1 116.46(13) . . ?
C1 N1 Ge1 110.06(13) . . ?
Si1 N1 Ge1 133.48(10) . . ?
C6 C1 C2 118.91(18) . . ?
C6 C1 N1 121.15(18) . . ?
C2 C1 N1 119.78(18) . . ?
C3 C2 C1 119.39(19) . . ?
C3 C2 C23 117.87(18) . . ?
C1 C2 C23 122.72(18) . . ?
C2 C3 C4 122.5(2) . . ?
C5 C4 C3 117.40(19) . . ?
C5 C4 C7 121.87(19) . . ?
C3 C4 C7 120.70(19) . . ?
C4 C5 C6 122.98(19) . . ?
C5 C6 C1 118.63(19) . . ?
C5 C6 C10 119.00(18) . . ?
C1 C6 C10 122.35(18) . . ?
C4 C7 C8 110.59(19) . . ?
C4 C7 C9 112.12(18) . . ?
C8 C7 C9 110.37(19) . . ?
C11 C10 C6 116.58(18) . . ?
C11 C10 C17 107.94(17) . . ?
C6 C10 C17 113.82(17) . . ?
C16 C11 C12 118.3(2) . . ?
C16 C11 C10 122.31(19) . . ?
C12 C11 C10 119.2(2) . . ?
C13 C12 C11 120.6(2) . . ?
C14 C13 C12 120.5(2) . . ?
C13 C14 C15 119.4(2) . . ?
C14 C15 C16 120.4(2) . . ?
C15 C16 C11 120.8(2) . . ?
C22 C17 C18 117.4(2) . . ?
C22 C17 C10 124.9(2) . . ?
C18 C17 C10 117.7(2) . . ?
C19 C18 C17 121.4(2) . . ?
C20 C19 C18 120.1(2) . . ?
C21 C20 C19 119.4(2) . . ?
C20 C21 C22 120.6(2) . . ?
C17 C22 C21 121.1(2) . . ?
C30 C23 C2 114.35(17) . . ?
C30 C23 C24 110.30(17) . . ?
C2 C23 C24 113.58(17) . . ?
C25 C24 C29 117.5(2) . . ?
C25 C24 C23 122.56(19) . . ?
C29 C24 C23 119.8(2) . . ?
C26 C25 C24 121.4(2) . . ?
C27 C26 C25 120.1(2) . . ?
C28 C27 C26 119.3(2) . . ?
C27 C28 C29 120.6(2) . . ?
C28 C29 C24 121.1(2) . . ?
C31 C30 C35 118.0(2) . . ?
C31 C30 C23 119.2(2) . . ?
C35 C30 C23 122.63(19) . . ?
C32 C31 C30 121.3(2) . . ?
C33 C32 C31 120.1(2) . . ?
C32 C33 C34 119.4(2) . . ?
C35 C34 C33 120.4(2) . . ?
C34 C35 C30 120.8(2) . . ?
C38 C36 C37 109.1(2) . . ?
C38 C36 Si1 116.44(16) . . ?
C37 C36 Si1 116.43(17) . . ?
C40 C39 C41 110.62(19) . . ?
C40 C39 Si1 114.42(16) . . ?
C41 C39 Si1 113.90(16) . . ?
C44 C42 C43 108.43(19) . . ?
C44 C42 Si1 115.84(16) . . ?
C43 C42 Si1 114.86(16) . . ?
C46 C45 C50 109.91(18) . . ?
C46 C45 Ge1 117.41(15) . . ?
C50 C45 Ge1 113.44(15) . . ?
C45 C46 C47 110.25(19) . . ?
C48 C47 C46 113.0(2) . . ?
C49 C48 C47 110.3(2) . . ?
C48 C49 C50 111.97(19) . . ?
C49 C50 C45 110.66(19) . . ?
C53 C52 C51 108.5(7) . . ?
C53A C52A C51A 115.8(5) . . ?
C54 C53 C52 120.3(9) . . ?
C52A C53A C54A 134.3(6) . . ?
C53 C54 C55 116.5(7) . . ?
C53A C54A C55A 106.8(6) . . ?
C54 C55 C56 105.6(6) . . ?
C56A C55A C54A 115.8(8) . . ?

_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full        66.94
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max         0.662
_refine_diff_density_min         -0.579
_refine_diff_density_rms         0.056
####################################################################### 
# 
# 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_compound26
_database_code_depnum_ccdc_archive 'CCDC 1422742'
_audit_update_record             
;
2015-09-07 deposited with the CCDC.
2015-09-22 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C112 H158 N2 O2 Si2 Sn2'
_chemical_formula_weight         1857.96

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Sn Sn -0.6537 1.4246 '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'
O O 0.0106 0.0060 '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'
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'

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   P-1

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   15.4827(8)
_cell_length_b                   16.4448(9)
_cell_length_c                   23.7823(11)
_cell_angle_alpha                72.311(4)
_cell_angle_beta                 88.259(4)
_cell_angle_gamma                62.908(5)
_cell_volume                     5094.1(5)
_cell_formula_units_Z            2
_cell_measurement_temperature    123(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.211
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1976
_exptl_absorpt_coefficient_mu    0.563
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.843
_exptl_absorpt_correction_T_max  0.917
_exptl_absorpt_process_details   'SCALE3 ABSPACK'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      123(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Oxford Gemini Ultra'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            46935
_diffrn_reflns_av_R_equivalents  0.0474
_diffrn_reflns_av_sigmaI/netI    0.0616
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_theta_min         2.91
_diffrn_reflns_theta_max         25.50
_reflns_number_total             18919
_reflns_number_gt                14498
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       CrysalisPro
_computing_cell_refinement       CrysalisPro
_computing_data_reduction        CrysalisPro
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    X-Seed
_computing_publication_material  CifTAB

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger.
 Two crystalographically independent molecules were refined in the asymmetric
 unit. There are no significant geometrical differences between them.
 Two molecules of hexane of crystallisation were refined in the asymmetric
 unit with their carbon atoms set as isotropic.
  
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0562P)²+9.4645P] 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         18919
_refine_ls_number_parameters     1047
_refine_ls_number_restraints     9
_refine_ls_R_factor_all          0.0726
_refine_ls_R_factor_gt           0.0495
_refine_ls_wR_factor_ref         0.1342
_refine_ls_wR_factor_gt          0.1182
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_restrained_S_all      1.054
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Sn1 Sn 0.108661(17) 0.443951(19) 0.003599(11) 0.01943(8) Uani 1 1 d . . .
Sn2 Sn 0.396012(18) 0.54587(2) 0.473314(12) 0.02204(8) Uani 1 1 d . . .
Si2 Si 0.29539(8) 0.73200(8) 0.53375(5) 0.0240(2) Uani 1 1 d . . .
O2 O 0.48043(18) 0.4479(2) 0.54910(12) 0.0257(6) Uani 1 1 d . . .
N2 N 0.2891(2) 0.6704(2) 0.48559(14) 0.0222(7) Uani 1 1 d . . .
Si1 Si 0.13137(7) 0.44637(8) -0.14238(5) 0.0199(2) Uani 1 1 d . . .
O1 O 0.00670(17) 0.58205(19) -0.01610(12) 0.0213(6) Uani 1 1 d . . .
N1 N 0.1789(2) 0.4095(2) -0.06698(14) 0.0196(7) Uani 1 1 d . . .
C1 C 0.2839(3) 0.3505(3) -0.04917(16) 0.0190(8) Uani 1 1 d . . .
C51 C 0.1990(3) 0.7048(3) 0.44865(17) 0.0225(9) Uani 1 1 d . . .
C2 C 0.3445(3) 0.3948(3) -0.05102(16) 0.0197(8) Uani 1 1 d . . .
C30 C 0.2584(3) 0.1427(3) 0.03860(18) 0.0236(9) Uani 1 1 d . . .
C11 C 0.2961(3) 0.5396(3) -0.01542(17) 0.0204(8) Uani 1 1 d . . .
C23 C 0.2642(3) 0.1973(3) -0.02535(18) 0.0221(8) Uani 1 1 d . . .
H23 H 0.1960 0.2501 -0.0412 0.026 Uiso 1 1 calc R . .
C3 C 0.4450(3) 0.3361(3) -0.03506(17) 0.0219(8) Uani 1 1 d . . .
H3 H 0.4858 0.3660 -0.0384 0.026 Uiso 1 1 calc R . .
C54 C 0.0224(3) 0.7704(3) 0.37611(19) 0.0327(10) Uani 1 1 d . . .
C24 C 0.2878(3) 0.1324(3) -0.06390(18) 0.0238(9) Uani 1 1 d . . .
C10 C 0.3027(3) 0.5038(3) -0.06824(17) 0.0213(8) Uani 1 1 d . . .
H10 H 0.2336 0.5314 -0.0862 0.026 Uiso 1 1 calc R . .
C52 C 0.1781(3) 0.7704(3) 0.39034(18) 0.0243(9) Uani 1 1 d . . .
C53 C 0.0912(3) 0.8006(3) 0.35557(19) 0.0293(10) Uani 1 1 d . . .
H53 H 0.0787 0.8437 0.3161 0.035 Uiso 1 1 calc R . .
C6 C 0.3266(3) 0.2486(3) -0.02870(16) 0.0207(8) Uani 1 1 d . . .
C4 C 0.4881(3) 0.2366(3) -0.01471(17) 0.0210(8) Uani 1 1 d . . .
C42 C 0.0055(3) 0.4558(3) -0.13999(18) 0.0281(9) Uani 1 1 d . . .
H42 H -0.0254 0.4919 -0.1117 0.034 Uiso 1 1 calc R . .
C5 C 0.4274(3) 0.1935(3) -0.01088(17) 0.0213(8) Uani 1 1 d . . .
H5 H 0.4553 0.1251 0.0042 0.026 Uiso 1 1 calc R . .
C7 C 0.5986(3) 0.1747(3) 0.00018(18) 0.0242(9) Uani 1 1 d . . .
H7 H 0.6129 0.1066 0.0220 0.029 Uiso 1 1 calc R . .
C39 C 0.2116(3) 0.3509(3) -0.17651(18) 0.0263(9) Uani 1 1 d . . .
H39 H 0.2251 0.2875 -0.1464 0.032 Uiso 1 1 calc R . .
C12 C 0.2078(3) 0.6132(3) -0.00994(19) 0.0262(9) Uani 1 1 d . . .
H12 H 0.1522 0.6375 -0.0379 0.031 Uiso 1 1 calc R . .
C55 C 0.0443(3) 0.7051(3) 0.43299(19) 0.0303(10) Uani 1 1 d . . .
H55 H -0.0014 0.6829 0.4478 0.036 Uiso 1 1 calc R . .
C29 C 0.2184(3) 0.1039(3) -0.07303(19) 0.0292(10) Uani 1 1 d . . .
H29 H 0.1626 0.1206 -0.0525 0.035 Uiso 1 1 calc R . .
C25 C 0.3695(3) 0.1047(3) -0.09389(19) 0.0287(9) Uani 1 1 d . . .
H25 H 0.4182 0.1226 -0.0885 0.034 Uiso 1 1 calc R . .
C16 C 0.3761(3) 0.5057(3) 0.02599(18) 0.0263(9) Uani 1 1 d . . .
H16 H 0.4374 0.4558 0.0229 0.032 Uiso 1 1 calc R . .
C31 C 0.3348(3) 0.0545(3) 0.07182(19) 0.0289(9) Uani 1 1 d . . .
H31 H 0.3931 0.0260 0.0549 0.035 Uiso 1 1 calc R . .
C22 C 0.3982(3) 0.5002(3) -0.15787(18) 0.0266(9) Uani 1 1 d . . .
H22 H 0.4041 0.4384 -0.1536 0.032 Uiso 1 1 calc R . .
C13 C 0.1990(3) 0.6519(3) 0.0355(2) 0.0326(10) Uani 1 1 d . . .
H13 H 0.1380 0.7024 0.0384 0.039 Uiso 1 1 calc R . .
C81 C 0.2766(3) 0.4211(3) 0.5663(2) 0.0335(10) Uani 1 1 d . . .
H81 H 0.3109 0.4378 0.5894 0.040 Uiso 1 1 calc R . .
C68 C 0.2556(4) 0.9680(4) 0.3246(2) 0.0460(13) Uani 1 1 d . . .
H68 H 0.3225 0.9288 0.3221 0.055 Uiso 1 1 calc R . .
C21 C 0.4355(3) 0.5431(3) -0.20477(19) 0.0315(10) Uani 1 1 d . . .
H21 H 0.4668 0.5105 -0.2321 0.038 Uiso 1 1 calc R . .
C79 C 0.0398(3) 0.5526(4) 0.60395(18) 0.0320(10) Uani 1 1 d . . .
H79 H 0.0818 0.4864 0.6090 0.038 Uiso 1 1 calc R . .
C34 C 0.1658(4) 0.1342(4) 0.1218(2) 0.0388(12) Uani 1 1 d . . .
H34 H 0.1075 0.1616 0.1389 0.047 Uiso 1 1 calc R . .
C85 C 0.1417(3) 0.4659(4) 0.49704(19) 0.0325(10) Uani 1 1 d . . .
H85 H 0.0828 0.5137 0.4718 0.039 Uiso 1 1 calc R . .
C96 C 0.3446(3) 0.5252(3) 0.35317(18) 0.0269(9) Uani 1 1 d . . .
H96A H 0.4132 0.4818 0.3500 0.032 Uiso 1 1 calc R . .
H96B H 0.3351 0.5922 0.3381 0.032 Uiso 1 1 calc R . .
C26 C 0.3812(3) 0.0517(3) -0.1315(2) 0.0338(10) Uani 1 1 d . . .
H26 H 0.4380 0.0330 -0.1512 0.041 Uiso 1 1 calc R . .
C95 C 0.3298(3) 0.5020(3) 0.41857(17) 0.0247(9) Uani 1 1 d . . .
H95A H 0.3552 0.4312 0.4359 0.030 Uiso 1 1 calc R . .
H95B H 0.2586 0.5325 0.4209 0.030 Uiso 1 1 calc R . .
C78 C -0.0397(3) 0.5781(4) 0.6358(2) 0.0361(11) Uani 1 1 d . . .
H78 H -0.0518 0.5290 0.6622 0.043 Uiso 1 1 calc R . .
C61 C 0.3004(3) 0.7793(3) 0.31567(19) 0.0276(9) Uani 1 1 d . . .
C67 C 0.1972(3) 0.9245(3) 0.34543(18) 0.0311(10) Uani 1 1 d . . .
C80 C 0.1902(3) 0.4927(3) 0.53046(18) 0.0275(9) Uani 1 1 d . . .
C75 C -0.0039(3) 0.7193(4) 0.5592(2) 0.0374(11) Uani 1 1 d . . .
H75 H 0.0082 0.7687 0.5331 0.045 Uiso 1 1 calc R . .
C36 C 0.1255(3) 0.5675(3) -0.18568(17) 0.0253(9) Uani 1 1 d . . .
H36 H 0.1911 0.5610 -0.1755 0.030 Uiso 1 1 calc R . .
C14 C 0.2794(3) 0.6170(3) 0.07663(19) 0.0303(10) Uani 1 1 d . . .
H14 H 0.2738 0.6431 0.1079 0.036 Uiso 1 1 calc R . .
C35 C 0.1722(3) 0.1822(3) 0.0644(2) 0.0300(10) Uani 1 1 d . . .
H35 H 0.1184 0.2419 0.0422 0.036 Uiso 1 1 calc R . .
C38 C 0.1096(3) 0.5971(3) -0.25356(19) 0.0332(10) Uani 1 1 d . . .
H38A H 0.0458 0.6049 -0.2662 0.050 Uiso 1 1 calc R . .
H38B H 0.1613 0.5470 -0.2668 0.050 Uiso 1 1 calc R . .
H38C H 0.1114 0.6584 -0.2712 0.050 Uiso 1 1 calc R . .
C17 C 0.3521(3) 0.5464(3) -0.11684(18) 0.0229(9) Uani 1 1 d . . .
C97 C 0.2760(3) 0.5154(3) 0.31206(18) 0.0290(10) Uani 1 1 d . . .
C9 C 0.6454(3) 0.1765(3) -0.0575(2) 0.0321(10) Uani 1 1 d . . .
H9A H 0.6163 0.1552 -0.0824 0.048 Uiso 1 1 calc R . .
H9B H 0.7159 0.1330 -0.0480 0.048 Uiso 1 1 calc R . .
H9C H 0.6339 0.2424 -0.0790 0.048 Uiso 1 1 calc R . .
C60 C 0.2461(3) 0.8136(3) 0.36518(18) 0.0268(9) Uani 1 1 d . . .
H60 H 0.2977 0.7902 0.3989 0.032 Uiso 1 1 calc R . .
C41 C 0.1616(3) 0.3559(4) -0.2331(2) 0.0357(11) Uani 1 1 d . . .
H41A H 0.1453 0.4175 -0.2642 0.054 Uiso 1 1 calc R . .
H41B H 0.1016 0.3508 -0.2244 0.054 Uiso 1 1 calc R . .
H41C H 0.2059 0.3024 -0.2468 0.054 Uiso 1 1 calc R . .
C33 C 0.2428(4) 0.0467(4) 0.1547(2) 0.0408(12) Uani 1 1 d . . .
H33 H 0.2378 0.0141 0.1942 0.049 Uiso 1 1 calc R . .
C74 C 0.0585(3) 0.6234(3) 0.56461(18) 0.0295(10) Uani 1 1 d . . .
C19 C 0.3837(3) 0.6789(3) -0.1716(2) 0.0360(11) Uani 1 1 d . . .
H19 H 0.3790 0.7402 -0.1759 0.043 Uiso 1 1 calc R . .
C37 C 0.0507(3) 0.6502(3) -0.1645(2) 0.0315(10) Uani 1 1 d . . .
H37A H 0.0591 0.7080 -0.1818 0.047 Uiso 1 1 calc R . .
H37B H 0.0614 0.6305 -0.1210 0.047 Uiso 1 1 calc R . .
H37C H -0.0158 0.6647 -0.1772 0.047 Uiso 1 1 calc R . .
C8 C 0.6433(3) 0.2072(3) 0.0393(2) 0.0324(10) Uani 1 1 d . . .
H8A H 0.6330 0.2727 0.0178 0.049 Uiso 1 1 calc R . .
H8B H 0.7137 0.1630 0.0494 0.049 Uiso 1 1 calc R . .
H8C H 0.6123 0.2068 0.0758 0.049 Uiso 1 1 calc R . .
C18 C 0.3458(3) 0.6355(3) -0.12394(19) 0.0288(9) Uani 1 1 d . . .
H18 H 0.3154 0.6680 -0.0964 0.035 Uiso 1 1 calc R . .
C72 C 0.1000(4) 0.9854(4) 0.3485(2) 0.0442(12) Uani 1 1 d . . .
H72 H 0.0580 0.9582 0.3630 0.053 Uiso 1 1 calc R . .
C66 C 0.2536(3) 0.8105(3) 0.25812(19) 0.0304(10) Uani 1 1 d . . .
H66 H 0.1849 0.8514 0.2497 0.036 Uiso 1 1 calc R . .
C65 C 0.3060(3) 0.7825(3) 0.2132(2) 0.0348(10) Uani 1 1 d . . .
H65 H 0.2733 0.8046 0.1742 0.042 Uiso 1 1 calc R . .
C32 C 0.3268(4) 0.0076(3) 0.1294(2) 0.0362(11) Uani 1 1 d . . .
H32 H 0.3800 -0.0524 0.1517 0.043 Uiso 1 1 calc R . .
C47 C 0.3518(3) 0.2631(3) 0.16330(18) 0.0268(9) Uani 1 1 d . . .
C62 C 0.4010(3) 0.7193(3) 0.3264(2) 0.0320(10) Uani 1 1 d . . .
H62 H 0.4343 0.6972 0.3651 0.038 Uiso 1 1 calc R . .
C46 C 0.3017(3) 0.3045(3) 0.09822(18) 0.0288(9) Uani 1 1 d . . .
H46A H 0.3439 0.3243 0.0715 0.035 Uiso 1 1 calc R . .
H46B H 0.2977 0.2521 0.0880 0.035 Uiso 1 1 calc R . .
C73 C 0.1490(3) 0.5961(3) 0.53122(18) 0.0277(9) Uani 1 1 d . . .
H73 H 0.2003 0.5971 0.5551 0.033 Uiso 1 1 calc R . .
C45 C 0.2004(3) 0.3894(3) 0.08572(18) 0.0278(9) Uani 1 1 d . . .
H45A H 0.2078 0.4439 0.0902 0.033 Uiso 1 1 calc R . .
H45B H 0.1636 0.3724 0.1180 0.033 Uiso 1 1 calc R . .
C56 C 0.1312(3) 0.6703(3) 0.46984(17) 0.0246(9) Uani 1 1 d . . .
C40 C 0.3121(3) 0.3443(3) -0.18862(19) 0.0285(9) Uani 1 1 d . . .
H40A H 0.3480 0.2921 -0.2053 0.043 Uiso 1 1 calc R . .
H40B H 0.3491 0.3308 -0.1513 0.043 Uiso 1 1 calc R . .
H40C H 0.3035 0.4056 -0.2170 0.043 Uiso 1 1 calc R . .
C20 C 0.4277(3) 0.6323(3) -0.21185(19) 0.0329(11) Uani 1 1 d . . .
H20 H 0.4525 0.6618 -0.2443 0.039 Uiso 1 1 calc R . .
C15 C 0.3680(3) 0.5437(3) 0.07186(19) 0.0303(10) Uani 1 1 d . . .
H15 H 0.4233 0.5193 0.1000 0.036 Uiso 1 1 calc R . .
C84 C 0.1786(3) 0.3705(4) 0.5002(2) 0.0371(11) Uani 1 1 d . . .
H84 H 0.1442 0.3530 0.4778 0.045 Uiso 1 1 calc R . .
C27 C 0.3112(3) 0.0259(3) -0.1405(2) 0.0376(11) Uani 1 1 d . . .
H27 H 0.3191 -0.0098 -0.1668 0.045 Uiso 1 1 calc R . .
C43 C -0.0628(3) 0.5150(4) -0.19882(19) 0.0336(11) Uani 1 1 d . . .
H43A H -0.0352 0.4842 -0.2290 0.050 Uiso 1 1 calc R . .
H43B H -0.0698 0.5805 -0.2120 0.050 Uiso 1 1 calc R . .
H43C H -0.1271 0.5182 -0.1930 0.050 Uiso 1 1 calc R . .
C44 C 0.0058(3) 0.3584(4) -0.1139(2) 0.0357(11) Uani 1 1 d . . .
H44A H -0.0614 0.3680 -0.1176 0.054 Uiso 1 1 calc R . .
H44B H 0.0330 0.3298 -0.0718 0.054 Uiso 1 1 calc R . .
H44C H 0.0458 0.3150 -0.1356 0.054 Uiso 1 1 calc R . .
C88 C 0.3401(3) 0.5782(3) 0.6427(2) 0.0352(11) Uani 1 1 d . . .
H88A H 0.3994 0.5780 0.6562 0.053 Uiso 1 1 calc R . .
H88B H 0.3557 0.5402 0.6157 0.053 Uiso 1 1 calc R . .
H88C H 0.3146 0.5498 0.6772 0.053 Uiso 1 1 calc R . .
C86 C 0.2618(3) 0.6837(4) 0.6097(2) 0.0378(11) Uani 1 1 d . . .
H86 H 0.2002 0.6808 0.6021 0.045 Uiso 1 1 calc R . .
C28 C 0.2290(3) 0.0523(3) -0.1111(2) 0.0369(11) Uani 1 1 d . . .
H28 H 0.1802 0.0348 -0.1172 0.044 Uiso 1 1 calc R . .
C99 C 0.2841(3) 0.4150(3) 0.3323(2) 0.0353(11) Uani 1 1 d . . .
H99A H 0.2410 0.4118 0.3046 0.053 Uiso 1 1 calc R . .
H99B H 0.2647 0.4012 0.3723 0.053 Uiso 1 1 calc R . .
H99C H 0.3518 0.3672 0.3329 0.053 Uiso 1 1 calc R . .
C92 C 0.4259(3) 0.7104(4) 0.5407(2) 0.0372(11) Uani 1 1 d . . .
H92 H 0.4687 0.6398 0.5482 0.045 Uiso 1 1 calc R . .
C63 C 0.4536(3) 0.6911(4) 0.2812(2) 0.0382(11) Uani 1 1 d . . .
H63 H 0.5223 0.6504 0.2894 0.046 Uiso 1 1 calc R . .
C100 C 0.3050(4) 0.5366(4) 0.2493(2) 0.0405(12) Uani 1 1 d . . .
H10A H 0.3724 0.4885 0.2496 0.061 Uiso 1 1 calc R . .
H10B H 0.3002 0.6012 0.2361 0.061 Uiso 1 1 calc R . .
H10C H 0.2609 0.5338 0.2221 0.061 Uiso 1 1 calc R . .
C77 C -0.1010(3) 0.6729(4) 0.62979(19) 0.0376(12) Uani 1 1 d . . .
H77 H -0.1549 0.6895 0.6520 0.045 Uiso 1 1 calc R . .
C91 C 0.1003(3) 0.8893(4) 0.4993(2) 0.0461(13) Uani 1 1 d . . .
H91A H 0.0864 0.8738 0.5406 0.069 Uiso 1 1 calc R . .
H91B H 0.0871 0.8509 0.4798 0.069 Uiso 1 1 calc R . .
H91C H 0.0586 0.9582 0.4781 0.069 Uiso 1 1 calc R . .
C83 C 0.2647(4) 0.3007(4) 0.5357(2) 0.0409(12) Uani 1 1 d . . .
H83 H 0.2902 0.2353 0.5374 0.049 Uiso 1 1 calc R . .
C64 C 0.4071(3) 0.7217(3) 0.2250(2) 0.0375(11) Uani 1 1 d . . .
H64 H 0.4431 0.7018 0.1944 0.045 Uiso 1 1 calc R . .
C76 C -0.0835(3) 0.7446(4) 0.5909(2) 0.0394(11) Uani 1 1 d . . .
H76 H -0.1258 0.8106 0.5861 0.047 Uiso 1 1 calc R . .
C89 C 0.2090(3) 0.8659(4) 0.4984(2) 0.0407(12) Uani 1 1 d . . .
H89 H 0.2191 0.8823 0.4555 0.049 Uiso 1 1 calc R . .
C82 C 0.3135(4) 0.3261(4) 0.5687(2) 0.0417(12) Uani 1 1 d . . .
H82 H 0.3729 0.2781 0.5934 0.050 Uiso 1 1 calc R . .
C94 C 0.4546(4) 0.7342(4) 0.5932(2) 0.0467(13) Uani 1 1 d . . .
H94A H 0.5231 0.7208 0.5938 0.070 Uiso 1 1 calc R . .
H94B H 0.4461 0.6942 0.6307 0.070 Uiso 1 1 calc R . .
H94C H 0.4127 0.8026 0.5883 0.070 Uiso 1 1 calc R . .
C98 C 0.1701(3) 0.5904(4) 0.3098(2) 0.0420(12) Uani 1 1 d . . .
H98A H 0.1653 0.6550 0.2973 0.063 Uiso 1 1 calc R . .
H98B H 0.1491 0.5766 0.3493 0.063 Uiso 1 1 calc R . .
H98C H 0.1280 0.5876 0.2813 0.063 Uiso 1 1 calc R . .
C93 C 0.4508(3) 0.7639(4) 0.4823(2) 0.0404(12) Uani 1 1 d . . .
H93A H 0.4034 0.8328 0.4697 0.061 Uiso 1 1 calc R . .
H93B H 0.4480 0.7369 0.4513 0.061 Uiso 1 1 calc R . .
H93C H 0.5167 0.7561 0.4889 0.061 Uiso 1 1 calc R . .
C87 C 0.2393(4) 0.7474(4) 0.6498(2) 0.0447(12) Uani 1 1 d . . .
H87A H 0.2258 0.7153 0.6884 0.067 Uiso 1 1 calc R . .
H87B H 0.1820 0.8101 0.6308 0.067 Uiso 1 1 calc R . .
H87C H 0.2957 0.7573 0.6556 0.067 Uiso 1 1 calc R . .
C69 C 0.2188(5) 1.0672(5) 0.3073(2) 0.0611(17) Uani 1 1 d . . .
H69 H 0.2606 1.0951 0.2939 0.073 Uiso 1 1 calc R . .
C70 C 0.1215(5) 1.1257(4) 0.3094(2) 0.0564(16) Uani 1 1 d . . .
H70 H 0.0954 1.1940 0.2960 0.068 Uiso 1 1 calc R . .
C57 C -0.0753(3) 0.8122(4) 0.3392(2) 0.0459(13) Uani 1 1 d . . .
H57 H -0.0683 0.8444 0.2976 0.055 Uiso 1 1 calc R . .
C49 C 0.2954(4) 0.2254(4) 0.2069(2) 0.0512(14) Uani 1 1 d . . .
H49A H 0.2801 0.1825 0.1931 0.077 Uiso 1 1 calc R . .
H49B H 0.2346 0.2797 0.2100 0.077 Uiso 1 1 calc R . .
H49C H 0.3350 0.1894 0.2460 0.077 Uiso 1 1 calc R . .
C90 C 0.2285(5) 0.9342(4) 0.5227(3) 0.0572(15) Uani 1 1 d . . .
H90A H 0.1829 1.0015 0.5002 0.086 Uiso 1 1 calc R . .
H90B H 0.2958 0.9230 0.5183 0.086 Uiso 1 1 calc R . .
H90C H 0.2192 0.9214 0.5648 0.086 Uiso 1 1 calc R . .
C71 C 0.0632(5) 1.0845(4) 0.3310(3) 0.0594(16) Uani 1 1 d . . .
H71 H -0.0033 1.1241 0.3340 0.071 Uiso 1 1 calc R . .
C50 C 0.3639(4) 0.3384(4) 0.1815(2) 0.0395(12) Uani 1 1 d . . .
H50A H 0.3992 0.3090 0.2218 0.059 Uiso 1 1 calc R . .
H50B H 0.2994 0.3916 0.1808 0.059 Uiso 1 1 calc R . .
H50C H 0.4011 0.3632 0.1537 0.059 Uiso 1 1 calc R . .
C48 C 0.4522(4) 0.1801(4) 0.1658(3) 0.0606(16) Uani 1 1 d . . .
H48A H 0.4877 0.1537 0.2059 0.091 Uiso 1 1 calc R . .
H48B H 0.4889 0.2035 0.1368 0.091 Uiso 1 1 calc R . .
H48C H 0.4449 0.1293 0.1564 0.091 Uiso 1 1 calc R . .
C59 C -0.1535(4) 0.8915(5) 0.3600(3) 0.0681(18) Uani 1 1 d . . .
H59A H -0.2147 0.9233 0.3332 0.102 Uiso 1 1 calc R . .
H59B H -0.1318 0.9391 0.3597 0.102 Uiso 1 1 calc R . .
H59C H -0.1641 0.8630 0.4005 0.102 Uiso 1 1 calc R . .
C58 C -0.1034(5) 0.7416(6) 0.3364(3) 0.080(2) Uani 1 1 d . . .
H58A H -0.0522 0.6941 0.3212 0.120 Uiso 1 1 calc R . .
H58B H -0.1649 0.7735 0.3098 0.120 Uiso 1 1 calc R . .
H58C H -0.1125 0.7088 0.3763 0.120 Uiso 1 1 calc R . .
C103 C 0.0311(4) -0.0392(4) -0.1514(3) 0.0577(15) Uiso 1 1 d . . .
H10D H 0.0402 0.0190 -0.1675 0.069 Uiso 1 1 calc R . .
H10E H -0.0290 -0.0270 -0.1736 0.069 Uiso 1 1 calc R . .
C104 C 0.0168(5) -0.0539(5) -0.0872(3) 0.0639(16) Uiso 1 1 d . . .
H10F H 0.0748 -0.0606 -0.0658 0.077 Uiso 1 1 calc R . .
H10G H 0.0140 -0.1154 -0.0703 0.077 Uiso 1 1 calc R . .
C102 C 0.1183(5) -0.1249(5) -0.1620(3) 0.0681(17) Uiso 1 1 d . . .
H10H H 0.1779 -0.1389 -0.1384 0.082 Uiso 1 1 calc R . .
H10I H 0.1078 -0.1824 -0.1474 0.082 Uiso 1 1 calc R . .
C101 C 0.1353(7) -0.1090(7) -0.2259(4) 0.109(3) Uiso 1 1 d . . .
H10J H 0.0791 -0.1007 -0.2492 0.164 Uiso 1 1 calc R . .
H10K H 0.1944 -0.1650 -0.2290 0.164 Uiso 1 1 calc R . .
H10L H 0.1437 -0.0509 -0.2412 0.164 Uiso 1 1 calc R . .
C105 C -0.0737(5) 0.0256(5) -0.0752(3) 0.078(2) Uiso 1 1 d . . .
H10M H -0.1321 0.0331 -0.0966 0.093 Uiso 1 1 calc R . .
H10N H -0.0792 0.0066 -0.0321 0.093 Uiso 1 1 calc R . .
C106 C -0.0728(6) 0.1214(6) -0.0942(4) 0.095(2) Uiso 1 1 d . . .
H10O H -0.0161 0.1150 -0.0724 0.142 Uiso 1 1 calc R . .
H10P H -0.1330 0.1700 -0.0856 0.142 Uiso 1 1 calc R . .
H10Q H -0.0687 0.1413 -0.1370 0.142 Uiso 1 1 calc R . .
C110 C 0.4726(10) 0.9669(11) 0.6275(7) 0.238(8) Uiso 1 1 d D . .
H11A H 0.4011 0.9999 0.6156 0.285 Uiso 1 1 calc R . .
H11B H 0.4910 0.9032 0.6579 0.285 Uiso 1 1 calc R . .
C108 C 0.4200(7) 1.0771(7) 0.6885(5) 0.127(3) Uiso 1 1 d D . .
H10R H 0.3597 1.1262 0.6610 0.153 Uiso 1 1 calc R . .
H10S H 0.4048 1.0291 0.7174 0.153 Uiso 1 1 calc R . .
C109 C 0.5000(7) 1.0269(8) 0.6534(5) 0.149(4) Uiso 1 1 d D . .
H10T H 0.5087 1.0759 0.6208 0.178 Uiso 1 1 calc R . .
H10U H 0.5627 0.9848 0.6799 0.178 Uiso 1 1 calc R . .
C107 C 0.4550(8) 1.1248(8) 0.7209(5) 0.139(4) Uiso 1 1 d D . .
H10V H 0.5095 1.0751 0.7516 0.208 Uiso 1 1 calc R . .
H10W H 0.4013 1.1635 0.7395 0.208 Uiso 1 1 calc R . .
H10$ H 0.4768 1.1667 0.6925 0.208 Uiso 1 1 calc R . .
C112 C 0.6265(10) 0.8680(12) 0.5908(8) 0.234(8) Uiso 1 1 d D . .
H11C H 0.6278 0.8199 0.6277 0.351 Uiso 1 1 calc R . .
H11D H 0.6739 0.8895 0.5969 0.351 Uiso 1 1 calc R . .
H11E H 0.6435 0.8391 0.5590 0.351 Uiso 1 1 calc R . .
C111 C 0.5258(12) 0.9530(11) 0.5736(5) 0.294(11) Uiso 1 1 d D . .
H11F H 0.4871 0.9433 0.5463 0.353 Uiso 1 1 calc R . .
H11G H 0.5309 1.0122 0.5521 0.353 Uiso 1 1 calc R . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Sn1 O1 2.001(3) . ?
Sn1 O1 2.012(2) 2_565 ?
Sn1 N1 2.056(3) . ?
Sn1 C45 2.140(4) . ?
Sn1 Sn1 2.9905(5) 2_565 ?
Sn2 O2 2.003(3) . ?
Sn2 O2 2.010(3) 2_666 ?
Sn2 N2 2.065(3) . ?
Sn2 C95 2.143(4) . ?
Sn2 Sn2 2.9859(5) 2_666 ?
Si2 N2 1.775(3) . ?
Si2 C92 1.889(4) . ?
Si2 C89 1.898(5) . ?
Si2 C86 1.900(5) . ?
O2 Sn2 2.010(3) 2_666 ?
N2 C51 1.446(5) . ?
Si1 N1 1.771(3) . ?
Si1 C42 1.884(4) . ?
Si1 C39 1.898(4) . ?
Si1 C36 1.905(4) . ?
O1 Sn1 2.012(2) 2_565 ?
N1 C1 1.456(5) . ?
C1 C6 1.413(6) . ?
C1 C2 1.419(5) . ?
C51 C52 1.412(6) . ?
C51 C56 1.419(5) . ?
C2 C3 1.394(5) . ?
C2 C10 1.520(6) . ?
C30 C31 1.388(6) . ?
C30 C35 1.408(6) . ?
C30 C23 1.537(5) . ?
C11 C16 1.388(6) . ?
C11 C12 1.390(6) . ?
C11 C10 1.524(5) . ?
C23 C24 1.528(6) . ?
C23 C6 1.533(5) . ?
C3 C4 1.378(6) . ?
C54 C55 1.382(6) . ?
C54 C53 1.387(6) . ?
C54 C57 1.517(6) . ?
C24 C25 1.391(6) . ?
C24 C29 1.397(6) . ?
C10 C17 1.535(5) . ?
C52 C53 1.396(6) . ?
C52 C60 1.534(5) . ?
C6 C5 1.398(5) . ?
C4 C5 1.399(5) . ?
C4 C7 1.524(5) . ?
C42 C44 1.530(6) . ?
C42 C43 1.532(6) . ?
C7 C8 1.519(6) . ?
C7 C9 1.530(6) . ?
C39 C40 1.535(5) . ?
C39 C41 1.535(6) . ?
C12 C13 1.386(6) . ?
C55 C56 1.404(6) . ?
C29 C28 1.378(6) . ?
C25 C26 1.383(6) . ?
C16 C15 1.389(6) . ?
C31 C32 1.386(6) . ?
C22 C21 1.390(6) . ?
C22 C17 1.398(6) . ?
C13 C14 1.384(6) . ?
C81 C82 1.380(7) . ?
C81 C80 1.388(6) . ?
C68 C69 1.384(8) . ?
C68 C67 1.386(6) . ?
C21 C20 1.372(7) . ?
C79 C78 1.391(6) . ?
C79 C74 1.393(6) . ?
C34 C35 1.381(6) . ?
C34 C33 1.384(7) . ?
C85 C84 1.380(7) . ?
C85 C80 1.393(6) . ?
C96 C95 1.522(5) . ?
C96 C97 1.558(6) . ?
C26 C27 1.374(7) . ?
C78 C77 1.370(7) . ?
C61 C62 1.391(6) . ?
C61 C66 1.399(6) . ?
C61 C60 1.525(6) . ?
C67 C72 1.393(7) . ?
C67 C60 1.537(6) . ?
C80 C73 1.527(6) . ?
C75 C76 1.389(6) . ?
C75 C74 1.391(7) . ?
C36 C38 1.530(6) . ?
C36 C37 1.547(6) . ?
C14 C15 1.383(6) . ?
C17 C18 1.380(6) . ?
C97 C99 1.518(6) . ?
C97 C100 1.528(6) . ?
C97 C98 1.528(6) . ?
C33 C32 1.376(7) . ?
C74 C73 1.540(6) . ?
C19 C20 1.378(7) . ?
C19 C18 1.410(6) . ?
C72 C71 1.381(7) . ?
C66 C65 1.385(6) . ?
C65 C64 1.399(6) . ?
C47 C49 1.506(6) . ?
C47 C50 1.516(6) . ?
C47 C48 1.519(7) . ?
C47 C46 1.554(6) . ?
C62 C63 1.392(6) . ?
C46 C45 1.509(6) . ?
C73 C56 1.527(6) . ?
C84 C83 1.376(7) . ?
C27 C28 1.388(7) . ?
C88 C86 1.552(7) . ?
C86 C87 1.545(7) . ?
C92 C93 1.544(6) . ?
C92 C94 1.548(7) . ?
C63 C64 1.371(7) . ?
C77 C76 1.389(7) . ?
C91 C89 1.547(7) . ?
C83 C82 1.374(7) . ?
C89 C90 1.550(7) . ?
C69 C70 1.379(9) . ?
C70 C71 1.363(8) . ?
C57 C58 1.433(9) . ?
C57 C59 1.525(8) . ?
C103 C104 1.497(8) . ?
C103 C102 1.529(9) . ?
C104 C105 1.513(9) . ?
C102 C101 1.496(10) . ?
C105 C106 1.507(10) . ?
C110 C109 1.516(7) . ?
C110 C111 1.521(7) . ?
C108 C107 1.511(7) . ?
C108 C109 1.529(7) . ?
C112 C111 1.504(8) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Sn1 O1 83.63(11) . 2_565 ?
O1 Sn1 N1 114.38(12) . . ?
O1 Sn1 N1 113.98(11) 2_565 . ?
O1 Sn1 C45 113.68(14) . . ?
O1 Sn1 C45 111.08(14) 2_565 . ?
N1 Sn1 C45 115.91(14) . . ?
O1 Sn1 Sn1 41.96(7) . 2_565 ?
O1 Sn1 Sn1 41.67(7) 2_565 2_565 ?
N1 Sn1 Sn1 123.34(8) . 2_565 ?
C45 Sn1 Sn1 120.70(11) . 2_565 ?
O2 Sn2 O2 83.84(11) . 2_666 ?
O2 Sn2 N2 112.81(12) . . ?
O2 Sn2 N2 113.94(12) 2_666 . ?
O2 Sn2 C95 118.77(14) . . ?
O2 Sn2 C95 117.68(13) 2_666 . ?
N2 Sn2 C95 108.31(14) . . ?
O2 Sn2 Sn2 42.00(7) . 2_666 ?
O2 Sn2 Sn2 41.84(7) 2_666 2_666 ?
N2 Sn2 Sn2 122.22(9) . 2_666 ?
C95 Sn2 Sn2 129.46(11) . 2_666 ?
N2 Si2 C92 106.30(18) . . ?
N2 Si2 C89 108.6(2) . . ?
C92 Si2 C89 110.2(2) . . ?
N2 Si2 C86 110.89(19) . . ?
C92 Si2 C86 110.3(2) . . ?
C89 Si2 C86 110.4(2) . . ?
Sn2 O2 Sn2 96.16(11) . 2_666 ?
C51 N2 Si2 120.8(3) . . ?
C51 N2 Sn2 109.9(2) . . ?
Si2 N2 Sn2 129.28(17) . . ?
N1 Si1 C42 105.04(16) . . ?
N1 Si1 C39 109.37(17) . . ?
C42 Si1 C39 110.35(19) . . ?
N1 Si1 C36 110.50(17) . . ?
C42 Si1 C36 111.26(19) . . ?
C39 Si1 C36 110.19(18) . . ?
Sn1 O1 Sn1 96.37(11) . 2_565 ?
C1 N1 Si1 119.3(2) . . ?
C1 N1 Sn1 110.7(2) . . ?
Si1 N1 Sn1 129.88(16) . . ?
C6 C1 C2 119.1(3) . . ?
C6 C1 N1 120.5(3) . . ?
C2 C1 N1 120.3(3) . . ?
C52 C51 C56 118.6(3) . . ?
C52 C51 N2 121.0(3) . . ?
C56 C51 N2 120.3(3) . . ?
C3 C2 C1 118.7(4) . . ?
C3 C2 C10 119.4(3) . . ?
C1 C2 C10 121.9(3) . . ?
C31 C30 C35 118.4(4) . . ?
C31 C30 C23 122.3(4) . . ?
C35 C30 C23 119.3(4) . . ?
C16 C11 C12 118.0(4) . . ?
C16 C11 C10 122.9(3) . . ?
C12 C11 C10 119.0(3) . . ?
C24 C23 C6 116.4(3) . . ?
C24 C23 C30 109.9(3) . . ?
C6 C23 C30 113.4(3) . . ?
C4 C3 C2 123.1(3) . . ?
C55 C54 C53 117.2(4) . . ?
C55 C54 C57 121.5(4) . . ?
C53 C54 C57 121.2(4) . . ?
C25 C24 C29 117.3(4) . . ?
C25 C24 C23 125.2(3) . . ?
C29 C24 C23 117.3(4) . . ?
C2 C10 C11 113.8(3) . . ?
C2 C10 C17 114.0(3) . . ?
C11 C10 C17 111.3(3) . . ?
C53 C52 C51 119.4(4) . . ?
C53 C52 C60 118.9(4) . . ?
C51 C52 C60 121.6(3) . . ?
C54 C53 C52 122.9(4) . . ?
C5 C6 C1 119.5(3) . . ?
C5 C6 C23 119.3(3) . . ?
C1 C6 C23 121.2(3) . . ?
C3 C4 C5 117.8(3) . . ?
C3 C4 C7 121.6(3) . . ?
C5 C4 C7 120.5(4) . . ?
C44 C42 C43 110.4(4) . . ?
C44 C42 Si1 113.9(3) . . ?
C43 C42 Si1 115.1(3) . . ?
C6 C5 C4 121.6(4) . . ?
C8 C7 C4 112.6(3) . . ?
C8 C7 C9 110.0(3) . . ?
C4 C7 C9 109.4(3) . . ?
C40 C39 C41 108.6(3) . . ?
C40 C39 Si1 116.0(3) . . ?
C41 C39 Si1 114.2(3) . . ?
C13 C12 C11 121.4(4) . . ?
C54 C55 C56 122.8(4) . . ?
C28 C29 C24 121.7(4) . . ?
C26 C25 C24 121.2(4) . . ?
C11 C16 C15 121.0(4) . . ?
C32 C31 C30 120.6(4) . . ?
C21 C22 C17 121.0(4) . . ?
C14 C13 C12 119.9(4) . . ?
C82 C81 C80 121.0(4) . . ?
C69 C68 C67 121.5(5) . . ?
C20 C21 C22 120.6(4) . . ?
C78 C79 C74 120.5(5) . . ?
C35 C34 C33 121.0(4) . . ?
C84 C85 C80 120.5(4) . . ?
C95 C96 C97 115.5(3) . . ?
C27 C26 C25 120.4(4) . . ?
C96 C95 Sn2 117.2(3) . . ?
C77 C78 C79 121.0(4) . . ?
C62 C61 C66 118.1(4) . . ?
C62 C61 C60 119.6(4) . . ?
C66 C61 C60 122.2(4) . . ?
C68 C67 C72 116.7(5) . . ?
C68 C67 C60 117.4(4) . . ?
C72 C67 C60 125.8(4) . . ?
C81 C80 C85 118.1(4) . . ?
C81 C80 C73 119.5(4) . . ?
C85 C80 C73 122.3(4) . . ?
C76 C75 C74 121.5(4) . . ?
C38 C36 C37 110.1(3) . . ?
C38 C36 Si1 116.4(3) . . ?
C37 C36 Si1 112.0(3) . . ?
C15 C14 C13 119.5(4) . . ?
C34 C35 C30 120.1(4) . . ?
C18 C17 C22 118.0(4) . . ?
C18 C17 C10 120.6(4) . . ?
C22 C17 C10 121.3(4) . . ?
C99 C97 C100 109.0(4) . . ?
C99 C97 C98 109.7(4) . . ?
C100 C97 C98 108.1(4) . . ?
C99 C97 C96 112.4(4) . . ?
C100 C97 C96 107.8(3) . . ?
C98 C97 C96 109.8(4) . . ?
C61 C60 C52 115.0(4) . . ?
C61 C60 C67 109.3(3) . . ?
C52 C60 C67 114.4(3) . . ?
C32 C33 C34 119.0(4) . . ?
C75 C74 C79 117.9(4) . . ?
C75 C74 C73 120.9(4) . . ?
C79 C74 C73 121.1(4) . . ?
C20 C19 C18 119.9(4) . . ?
C17 C18 C19 120.9(4) . . ?
C71 C72 C67 121.7(5) . . ?
C65 C66 C61 120.9(4) . . ?
C66 C65 C64 120.2(4) . . ?
C33 C32 C31 121.0(5) . . ?
C49 C47 C50 108.5(4) . . ?
C49 C47 C48 108.9(4) . . ?
C50 C47 C48 109.0(4) . . ?
C49 C47 C46 112.1(3) . . ?
C50 C47 C46 111.5(4) . . ?
C48 C47 C46 106.9(4) . . ?
C61 C62 C63 121.0(4) . . ?
C45 C46 C47 115.5(3) . . ?
C56 C73 C80 113.7(3) . . ?
C56 C73 C74 112.8(3) . . ?
C80 C73 C74 111.3(3) . . ?
C46 C45 Sn1 122.0(3) . . ?
C55 C56 C51 119.0(4) . . ?
C55 C56 C73 118.3(3) . . ?
C51 C56 C73 122.7(4) . . ?
C21 C20 C19 119.7(4) . . ?
C14 C15 C16 120.2(4) . . ?
C83 C84 C85 120.6(5) . . ?
C26 C27 C28 119.7(4) . . ?
C87 C86 C88 111.1(4) . . ?
C87 C86 Si2 115.4(4) . . ?
C88 C86 Si2 110.9(3) . . ?
C29 C28 C27 119.6(4) . . ?
C93 C92 C94 109.7(4) . . ?
C93 C92 Si2 112.1(3) . . ?
C94 C92 Si2 114.6(3) . . ?
C64 C63 C62 120.6(4) . . ?
C78 C77 C76 119.4(4) . . ?
C82 C83 C84 119.5(5) . . ?
C63 C64 C65 119.3(4) . . ?
C77 C76 C75 119.7(5) . . ?
C91 C89 C90 110.2(4) . . ?
C91 C89 Si2 112.4(3) . . ?
C90 C89 Si2 115.6(4) . . ?
C83 C82 C81 120.3(5) . . ?
C70 C69 C68 120.3(5) . . ?
C71 C70 C69 119.2(5) . . ?
C58 C57 C54 114.3(5) . . ?
C58 C57 C59 112.7(5) . . ?
C54 C57 C59 109.8(4) . . ?
C70 C71 C72 120.5(6) . . ?
C104 C103 C102 113.8(5) . . ?
C103 C104 C105 115.4(6) . . ?
C101 C102 C103 114.0(6) . . ?
C106 C105 C104 112.9(6) . . ?
C109 C110 C111 109.4(7) . . ?
C107 C108 C109 109.2(6) . . ?
C110 C109 C108 110.1(6) . . ?
C112 C111 C110 112.1(8) . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        25.50
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         1.437
_refine_diff_density_min         -0.880
_refine_diff_density_rms         0.098
