# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2017

####################################################################### 
# 
# 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_si344c
_database_code_depnum_ccdc_archive 'CCDC 1558534'
_audit_update_record             
;
2017-06-26 deposited with the CCDC.
2017-08-11 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014
_chemical_name_systematic        disilenylanthracene
_chemical_name_common            ?
_chemical_melting_point          461
_chemical_formula_moiety         'C39 H60 Si6, C4 H10 O2'
_chemical_formula_sum            'C43 H70 O2 Si6'
_chemical_formula_weight         787.53

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

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

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

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   11.4296(11)
_cell_length_b                   13.7384(13)
_cell_length_c                   15.2495(15)
_cell_angle_alpha                77.0900(10)
_cell_angle_beta                 82.3360(10)
_cell_angle_gamma                79.2250(10)
_cell_volume                     2282.4(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9950
_cell_measurement_theta_min      2.27
_cell_measurement_theta_max      27.95

_exptl_crystal_description       block
_exptl_crystal_colour            red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.146
_exptl_crystal_F_000             856
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.100
_exptl_absorpt_coefficient_mu    0.216
_shelx_estimated_absorpt_T_min   0.958
_shelx_estimated_absorpt_T_max   0.979
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.6545
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_process_details   'SADABS Sheldrick 1996'

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'Bruker TXS fine-focus rotating anode'
_diffrn_radiation_monochromator  'Bruker Helios multilayer confocal mirror'
_diffrn_measurement_device_type  'Bruker APEXII CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean 8.333
_diffrn_reflns_number            22849
_diffrn_reflns_av_unetI/netI     0.0157
_diffrn_reflns_av_R_equivalents  0.0137
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         1.376
_diffrn_reflns_theta_max         25.499
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             8479
_reflns_number_gt                7716
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

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

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0390P)²+1.5898P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         8479
_refine_ls_number_parameters     477
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0354
_refine_ls_R_factor_gt           0.0316
_refine_ls_wR_factor_ref         0.0843
_refine_ls_wR_factor_gt          0.0808
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_restrained_S_all      1.023
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Si1 Si 0.27424(3) 0.29933(3) 0.18536(2) 0.01340(9) Uani 1 1 d . . . . .
Si2 Si 0.15890(4) 0.19110(3) 0.25364(3) 0.01765(10) Uani 1 1 d . . . . .
C1 C 0.32970(12) 0.40075(11) 0.22935(9) 0.0141(3) Uani 1 1 d . . . . .
C2 C 0.39658(13) 0.45488(11) 0.13977(9) 0.0163(3) Uani 1 1 d . . . . .
H1 H 0.3393 0.5096 0.1069 0.020 Uiso 1 1 calc R U . . .
H2 H 0.4604 0.4861 0.1553 0.020 Uiso 1 1 calc R U . . .
C3 C 0.45210(13) 0.38024(11) 0.07824(10) 0.0158(3) Uani 1 1 d . . . . .
H3 H 0.5239 0.3368 0.1038 0.019 Uiso 1 1 calc R U . . .
H4 H 0.4776 0.4185 0.0178 0.019 Uiso 1 1 calc R U . . .
C4 C 0.36081(12) 0.31176(10) 0.06837(9) 0.0133(3) Uani 1 1 d . . . . .
Si3 Si 0.20330(4) 0.49892(3) 0.26730(3) 0.01727(10) Uani 1 1 d . . . . .
Si4 Si 0.43785(4) 0.34963(3) 0.32029(3) 0.01855(10) Uani 1 1 d . . . . .
Si5 Si 0.26397(4) 0.37509(3) -0.02778(3) 0.01680(10) Uani 1 1 d . . . . .
Si6 Si 0.45243(4) 0.18759(3) 0.04606(3) 0.01611(9) Uani 1 1 d . . . . .
C5 C 0.08052(15) 0.53289(13) 0.19009(11) 0.0267(4) Uani 1 1 d . . . . .
H5 H 0.0696 0.4723 0.1702 0.040 Uiso 1 1 calc R U . . .
H6 H 0.1019 0.5840 0.1373 0.040 Uiso 1 1 calc R U . . .
H7 H 0.0059 0.5600 0.2224 0.040 Uiso 1 1 calc R U . . .
C6 C 0.25613(17) 0.62321(12) 0.25602(12) 0.0302(4) Uani 1 1 d . . . . .
H8 H 0.1893 0.6732 0.2737 0.045 Uiso 1 1 calc R U . . .
H9 H 0.2865 0.6469 0.1931 0.045 Uiso 1 1 calc R U . . .
H10 H 0.3201 0.6143 0.2953 0.045 Uiso 1 1 calc R U . . .
C7 C 0.14121(14) 0.45840(12) 0.38707(10) 0.0220(3) Uani 1 1 d . . . . .
H11 H 0.0700 0.5067 0.4007 0.033 Uiso 1 1 calc R U . . .
H12 H 0.2016 0.4563 0.4277 0.033 Uiso 1 1 calc R U . . .
H13 H 0.1195 0.3910 0.3956 0.033 Uiso 1 1 calc R U . . .
C8 C 0.38447(17) 0.24653(15) 0.40880(12) 0.0363(4) Uani 1 1 d . . . . .
H14 H 0.3896 0.1862 0.3833 0.054 Uiso 1 1 calc R U . . .
H15 H 0.3012 0.2685 0.4306 0.054 Uiso 1 1 calc R U . . .
H16 H 0.4344 0.2304 0.4592 0.054 Uiso 1 1 calc R U . . .
C9 C 0.46362(15) 0.45180(14) 0.37603(12) 0.0299(4) Uani 1 1 d . . . . .
H17 H 0.3873 0.4820 0.4041 0.045 Uiso 1 1 calc R U . . .
H18 H 0.4980 0.5041 0.3306 0.045 Uiso 1 1 calc R U . . .
H19 H 0.5190 0.4226 0.4225 0.045 Uiso 1 1 calc R U . . .
C10 C 0.59259(15) 0.30074(14) 0.27432(12) 0.0298(4) Uani 1 1 d . . . . .
H20 H 0.6461 0.2836 0.3226 0.045 Uiso 1 1 calc R U . . .
H21 H 0.6214 0.3529 0.2255 0.045 Uiso 1 1 calc R U . . .
H22 H 0.5913 0.2402 0.2508 0.045 Uiso 1 1 calc R U . . .
C11 C 0.23017(15) 0.51641(12) -0.04295(11) 0.0252(3) Uani 1 1 d . . . . .
H23 H 0.1858 0.5447 -0.0961 0.038 Uiso 1 1 calc R U . . .
H24 H 0.3052 0.5436 -0.0514 0.038 Uiso 1 1 calc R U . . .
H25 H 0.1818 0.5348 0.0108 0.038 Uiso 1 1 calc R U . . .
C12 C 0.11905(15) 0.32661(13) -0.01032(11) 0.0262(4) Uani 1 1 d . . . . .
H26 H 0.0622 0.3632 0.0299 0.039 Uiso 1 1 calc R U . . .
H27 H 0.1320 0.2542 0.0170 0.039 Uiso 1 1 calc R U . . .
H28 H 0.0867 0.3369 -0.0686 0.039 Uiso 1 1 calc R U . . .
C13 C 0.34016(16) 0.35637(13) -0.14135(10) 0.0284(4) Uani 1 1 d . . . . .
H29 H 0.3549 0.2841 -0.1428 0.043 Uiso 1 1 calc R U . . .
H30 H 0.4164 0.3819 -0.1518 0.043 Uiso 1 1 calc R U . . .
H31 H 0.2888 0.3934 -0.1886 0.043 Uiso 1 1 calc R U . . .
C14 C 0.35684(14) 0.10779(12) 0.01249(11) 0.0216(3) Uani 1 1 d . . . . .
H32 H 0.4022 0.0397 0.0127 0.032 Uiso 1 1 calc R U . . .
H33 H 0.3331 0.1385 -0.0483 0.032 Uiso 1 1 calc R U . . .
H34 H 0.2852 0.1034 0.0555 0.032 Uiso 1 1 calc R U . . .
C15 C 0.57888(15) 0.21048(13) -0.04481(11) 0.0263(4) Uani 1 1 d . . . . .
H35 H 0.6365 0.1478 -0.0438 0.040 Uiso 1 1 calc R U . . .
H36 H 0.6188 0.2633 -0.0339 0.040 Uiso 1 1 calc R U . . .
H37 H 0.5471 0.2323 -0.1039 0.040 Uiso 1 1 calc R U . . .
C16 C 0.53324(14) 0.11459(12) 0.14580(11) 0.0225(3) Uani 1 1 d . . . . .
H38 H 0.4805 0.1188 0.2015 0.034 Uiso 1 1 calc R U . . .
H39 H 0.6051 0.1433 0.1474 0.034 Uiso 1 1 calc R U . . .
H40 H 0.5563 0.0436 0.1406 0.034 Uiso 1 1 calc R U . . .
C17 C 0.10561(13) 0.09506(11) 0.20188(9) 0.0155(3) Uani 1 1 d . . . . .
C18 C 0.17198(13) -0.00232(11) 0.20091(10) 0.0179(3) Uani 1 1 d . . . . .
C19 C 0.12340(15) -0.07384(12) 0.17094(10) 0.0220(3) Uani 1 1 d . . . . .
H41 H 0.1693 -0.1391 0.1713 0.026 Uiso 1 1 calc R U . . .
C20 C 0.01051(15) -0.05267(13) 0.14080(10) 0.0244(3) Uani 1 1 d . . . . .
C21 C -0.05435(14) 0.04326(13) 0.14095(10) 0.0228(3) Uani 1 1 d . . . . .
H42 H -0.1316 0.0594 0.1199 0.027 Uiso 1 1 calc R U . . .
C22 C -0.01028(13) 0.11673(12) 0.17079(10) 0.0188(3) Uani 1 1 d . . . . .
C23 C -0.09053(14) 0.21710(13) 0.17028(11) 0.0254(3) Uani 1 1 d . . . . .
H43 H -0.1519 0.2256 0.1288 0.038 Uiso 1 1 calc R U . . .
H44 H -0.0429 0.2718 0.1504 0.038 Uiso 1 1 calc R U . . .
H45 H -0.1291 0.2192 0.2314 0.038 Uiso 1 1 calc R U . . .
C24 C 0.29669(14) -0.03601(12) 0.23060(11) 0.0238(3) Uani 1 1 d . . . . .
H46 H 0.2929 -0.0797 0.2909 0.036 Uiso 1 1 calc R U . . .
H47 H 0.3315 0.0234 0.2324 0.036 Uiso 1 1 calc R U . . .
H48 H 0.3465 -0.0737 0.1877 0.036 Uiso 1 1 calc R U . . .
C25 C -0.03974(18) -0.13094(15) 0.10791(13) 0.0369(4) Uani 1 1 d . . . . .
H49 H 0.0222 -0.1904 0.1054 0.055 Uiso 1 1 calc R U . . .
H50 H -0.0658 -0.1022 0.0475 0.055 Uiso 1 1 calc R U . . .
H51 H -0.1081 -0.1509 0.1496 0.055 Uiso 1 1 calc R U . . .
C26 C 0.08279(14) 0.18897(12) 0.37257(10) 0.0203(3) Uani 1 1 d . . . . .
C27 C 0.12375(15) 0.10867(12) 0.44304(10) 0.0238(3) Uani 1 1 d . . . . .
C28 C 0.23076(17) 0.03901(12) 0.43221(11) 0.0290(4) Uani 1 1 d . . . . .
H52 H 0.2782 0.0471 0.3758 0.035 Uiso 1 1 calc R U . . .
C29 C 0.2675(2) -0.03905(14) 0.50028(12) 0.0382(5) Uani 1 1 d . . . . .
H53 H 0.3393 -0.0847 0.4909 0.046 Uiso 1 1 calc R U . . .
C30 C 0.1976(2) -0.05218(15) 0.58596(12) 0.0433(5) Uani 1 1 d . . . . .
H54 H 0.2226 -0.1072 0.6332 0.052 Uiso 1 1 calc R U . . .
C31 C 0.0973(2) 0.01264(16) 0.60000(12) 0.0399(5) Uani 1 1 d . . . . .
H55 H 0.0524 0.0031 0.6575 0.048 Uiso 1 1 calc R U . . .
C32 C 0.05648(17) 0.09521(14) 0.53104(11) 0.0316(4) Uani 1 1 d . . . . .
C33 C -0.04560(16) 0.16516(17) 0.54618(12) 0.0379(5) Uani 1 1 d . . . . .
H56 H -0.0902 0.1557 0.6038 0.045 Uiso 1 1 calc R U . . .
C34 C -0.08391(15) 0.24726(16) 0.48066(12) 0.0326(4) Uani 1 1 d . . . . .
C35 C -0.18492(17) 0.3230(2) 0.49855(15) 0.0468(6) Uani 1 1 d . . . . .
H57 H -0.2267 0.3154 0.5572 0.056 Uiso 1 1 calc R U . . .
C36 C -0.22170(17) 0.4037(2) 0.43497(16) 0.0489(6) Uani 1 1 d . . . . .
H58 H -0.2875 0.4530 0.4492 0.059 Uiso 1 1 calc R U . . .
C37 C -0.16251(16) 0.41511(17) 0.34707(15) 0.0399(5) Uani 1 1 d . . . . .
H59 H -0.1895 0.4715 0.3016 0.048 Uiso 1 1 calc R U . . .
C38 C -0.06616(15) 0.34520(13) 0.32687(12) 0.0287(4) Uani 1 1 d . . . . .
H60 H -0.0280 0.3545 0.2670 0.034 Uiso 1 1 calc R U . . .
C39 C -0.02099(14) 0.25958(13) 0.39146(11) 0.0253(4) Uani 1 1 d . . . . .
C40 C 0.4960(2) 0.73073(19) 0.36698(16) 0.0542(6) Uani 1 1 d . . . . .
H61 H 0.4737 0.7345 0.3063 0.081 Uiso 1 1 calc R U . . .
H62 H 0.4345 0.7039 0.4123 0.081 Uiso 1 1 calc R U . . .
H63 H 0.5730 0.6860 0.3753 0.081 Uiso 1 1 calc R U . . .
O1 O 0.50601(12) 0.82865(12) 0.37720(9) 0.0445(3) Uani 1 1 d . . . . .
C41 C 0.5933(2) 0.87149(16) 0.31367(14) 0.0469(5) Uani 1 1 d . . . . .
H64 H 0.5740 0.9461 0.3057 0.056 Uiso 1 1 calc R U . . .
H65 H 0.5882 0.8542 0.2548 0.056 Uiso 1 1 calc R U . . .
C42 C 0.71939(19) 0.83842(16) 0.33792(14) 0.0412(5) Uani 1 1 d . . . . .
H66 H 0.7717 0.8835 0.2983 0.049 Uiso 1 1 calc R U . . .
H67 H 0.7232 0.8432 0.4013 0.049 Uiso 1 1 calc R U . . .
O2 O 0.75971(12) 0.73813(12) 0.32769(11) 0.0466(4) Uani 1 1 d . . . . .
C43 C 0.87323(19) 0.69903(19) 0.35941(17) 0.0530(6) Uani 1 1 d . . . . .
H68 H 0.9333 0.7366 0.3218 0.079 Uiso 1 1 calc R U . . .
H69 H 0.8943 0.6273 0.3562 0.079 Uiso 1 1 calc R U . . .
H70 H 0.8709 0.7061 0.4222 0.079 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Si1 C4 1.9098(14) . ?
Si1 C1 1.9117(14) . ?
Si1 Si2 2.1697(6) . ?
Si2 C26 1.9005(15) . ?
Si2 C17 1.9049(15) . ?
C1 C2 1.5758(19) . ?
C1 Si3 1.9075(15) . ?
C1 Si4 1.9084(14) . ?
C2 C3 1.537(2) . ?
C3 C4 1.5712(19) . ?
C4 Si6 1.9023(14) . ?
C4 Si5 1.9064(14) . ?
Si3 C7 1.8700(15) . ?
Si3 C5 1.8772(17) . ?
Si3 C6 1.8805(17) . ?
Si4 C8 1.8572(18) . ?
Si4 C10 1.8724(17) . ?
Si4 C9 1.8799(17) . ?
Si5 C12 1.8637(16) . ?
Si5 C11 1.8749(16) . ?
Si5 C13 1.8807(16) . ?
Si6 C14 1.8724(16) . ?
Si6 C16 1.8759(16) . ?
Si6 C15 1.8838(16) . ?
C17 C18 1.411(2) . ?
C17 C22 1.423(2) . ?
C18 C19 1.398(2) . ?
C18 C24 1.511(2) . ?
C19 C20 1.385(2) . ?
C20 C21 1.386(2) . ?
C20 C25 1.512(2) . ?
C21 C22 1.391(2) . ?
C22 C23 1.506(2) . ?
C26 C27 1.415(2) . ?
C26 C39 1.426(2) . ?
C27 C28 1.421(3) . ?
C27 C32 1.447(2) . ?
C28 C29 1.362(3) . ?
C29 C30 1.431(3) . ?
C30 C31 1.339(3) . ?
C31 C32 1.418(3) . ?
C32 C33 1.395(3) . ?
C33 C34 1.375(3) . ?
C34 C39 1.442(2) . ?
C34 C35 1.443(3) . ?
C35 C36 1.342(3) . ?
C36 C37 1.408(3) . ?
C37 C38 1.370(2) . ?
C38 C39 1.418(3) . ?
C40 O1 1.415(3) . ?
O1 C41 1.409(3) . ?
C41 C42 1.498(3) . ?
C42 O2 1.405(2) . ?
O2 C43 1.413(3) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C4 Si1 C1 100.18(6) . . ?
C4 Si1 Si2 129.75(5) . . ?
C1 Si1 Si2 129.84(5) . . ?
C26 Si2 C17 109.86(6) . . ?
C26 Si2 Si1 123.54(5) . . ?
C17 Si2 Si1 126.30(5) . . ?
C2 C1 Si3 107.29(9) . . ?
C2 C1 Si4 110.22(9) . . ?
Si3 C1 Si4 110.48(7) . . ?
C2 C1 Si1 100.15(9) . . ?
Si3 C1 Si1 113.21(7) . . ?
Si4 C1 Si1 114.76(7) . . ?
C3 C2 C1 111.60(11) . . ?
C2 C3 C4 111.42(11) . . ?
C3 C4 Si6 106.86(9) . . ?
C3 C4 Si5 111.29(9) . . ?
Si6 C4 Si5 110.72(7) . . ?
C3 C4 Si1 100.25(9) . . ?
Si6 C4 Si1 113.39(7) . . ?
Si5 C4 Si1 113.68(7) . . ?
C7 Si3 C5 110.40(7) . . ?
C7 Si3 C6 108.25(7) . . ?
C5 Si3 C6 102.65(8) . . ?
C7 Si3 C1 112.67(7) . . ?
C5 Si3 C1 111.62(7) . . ?
C6 Si3 C1 110.75(7) . . ?
C8 Si4 C10 107.93(9) . . ?
C8 Si4 C9 108.72(9) . . ?
C10 Si4 C9 102.56(8) . . ?
C8 Si4 C1 111.94(7) . . ?
C10 Si4 C1 113.27(7) . . ?
C9 Si4 C1 111.91(7) . . ?
C12 Si5 C11 108.01(8) . . ?
C12 Si5 C13 108.38(8) . . ?
C11 Si5 C13 102.72(8) . . ?
C12 Si5 C4 111.23(7) . . ?
C11 Si5 C4 113.41(7) . . ?
C13 Si5 C4 112.63(7) . . ?
C14 Si6 C16 110.24(7) . . ?
C14 Si6 C15 109.34(7) . . ?
C16 Si6 C15 102.50(8) . . ?
C14 Si6 C4 111.24(7) . . ?
C16 Si6 C4 112.00(7) . . ?
C15 Si6 C4 111.17(7) . . ?
C18 C17 C22 117.49(13) . . ?
C18 C17 Si2 122.43(11) . . ?
C22 C17 Si2 119.78(11) . . ?
C19 C18 C17 120.26(14) . . ?
C19 C18 C24 116.12(14) . . ?
C17 C18 C24 123.62(13) . . ?
C20 C19 C18 122.17(15) . . ?
C19 C20 C21 117.62(14) . . ?
C19 C20 C25 121.24(16) . . ?
C21 C20 C25 121.14(16) . . ?
C20 C21 C22 122.34(15) . . ?
C21 C22 C17 120.11(14) . . ?
C21 C22 C23 117.44(14) . . ?
C17 C22 C23 122.45(13) . . ?
C27 C26 C39 118.94(14) . . ?
C27 C26 Si2 118.55(12) . . ?
C39 C26 Si2 122.22(12) . . ?
C26 C27 C28 122.86(14) . . ?
C26 C27 C32 120.11(16) . . ?
C28 C27 C32 117.02(16) . . ?
C29 C28 C27 122.03(17) . . ?
C28 C29 C30 119.8(2) . . ?
C31 C30 C29 120.40(18) . . ?
C30 C31 C32 121.49(18) . . ?
C33 C32 C31 121.79(17) . . ?
C33 C32 C27 118.96(17) . . ?
C31 C32 C27 119.23(18) . . ?
C34 C33 C32 122.30(16) . . ?
C33 C34 C39 119.50(17) . . ?
C33 C34 C35 122.01(17) . . ?
C39 C34 C35 118.48(19) . . ?
C36 C35 C34 122.11(18) . . ?
C35 C36 C37 119.79(18) . . ?
C38 C37 C36 120.2(2) . . ?
C37 C38 C39 122.83(18) . . ?
C38 C39 C26 123.40(15) . . ?
C38 C39 C34 116.55(16) . . ?
C26 C39 C34 120.02(17) . . ?
C41 O1 C40 112.18(17) . . ?
O1 C41 C42 115.11(16) . . ?
O2 C42 C41 109.91(16) . . ?
C42 O2 C43 112.34(16) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Si3 C1 C2 C3 -150.74(10) . . . . ?
Si4 C1 C2 C3 88.92(12) . . . . ?
Si1 C1 C2 C3 -32.38(13) . . . . ?
C1 C2 C3 C4 46.80(16) . . . . ?
C2 C3 C4 Si6 -151.80(10) . . . . ?
C2 C3 C4 Si5 87.21(12) . . . . ?
C2 C3 C4 Si1 -33.35(13) . . . . ?
C22 C17 C18 C19 -0.5(2) . . . . ?
Si2 C17 C18 C19 173.16(11) . . . . ?
C22 C17 C18 C24 179.15(13) . . . . ?
Si2 C17 C18 C24 -7.2(2) . . . . ?
C17 C18 C19 C20 0.5(2) . . . . ?
C24 C18 C19 C20 -179.23(14) . . . . ?
C18 C19 C20 C21 0.1(2) . . . . ?
C18 C19 C20 C25 179.45(15) . . . . ?
C19 C20 C21 C22 -0.6(2) . . . . ?
C25 C20 C21 C22 -179.97(15) . . . . ?
C20 C21 C22 C17 0.6(2) . . . . ?
C20 C21 C22 C23 -178.24(14) . . . . ?
C18 C17 C22 C21 0.0(2) . . . . ?
Si2 C17 C22 C21 -173.83(11) . . . . ?
C18 C17 C22 C23 178.77(13) . . . . ?
Si2 C17 C22 C23 4.92(19) . . . . ?
C39 C26 C27 C28 -175.49(14) . . . . ?
Si2 C26 C27 C28 10.5(2) . . . . ?
C39 C26 C27 C32 4.0(2) . . . . ?
Si2 C26 C27 C32 -170.01(11) . . . . ?
C26 C27 C28 C29 -178.63(16) . . . . ?
C32 C27 C28 C29 1.9(2) . . . . ?
C27 C28 C29 C30 -0.4(3) . . . . ?
C28 C29 C30 C31 -0.9(3) . . . . ?
C29 C30 C31 C32 0.5(3) . . . . ?
C30 C31 C32 C33 -177.61(17) . . . . ?
C30 C31 C32 C27 1.1(3) . . . . ?
C26 C27 C32 C33 -3.0(2) . . . . ?
C28 C27 C32 C33 176.49(15) . . . . ?
C26 C27 C32 C31 178.28(14) . . . . ?
C28 C27 C32 C31 -2.2(2) . . . . ?
C31 C32 C33 C34 177.94(16) . . . . ?
C27 C32 C33 C34 -0.8(2) . . . . ?
C32 C33 C34 C39 3.4(2) . . . . ?
C32 C33 C34 C35 -175.80(16) . . . . ?
C33 C34 C35 C36 179.30(18) . . . . ?
C39 C34 C35 C36 0.1(3) . . . . ?
C34 C35 C36 C37 1.4(3) . . . . ?
C35 C36 C37 C38 -1.3(3) . . . . ?
C36 C37 C38 C39 -0.2(3) . . . . ?
C37 C38 C39 C26 -176.76(15) . . . . ?
C37 C38 C39 C34 1.7(2) . . . . ?
C27 C26 C39 C38 177.02(14) . . . . ?
Si2 C26 C39 C38 -9.2(2) . . . . ?
C27 C26 C39 C34 -1.4(2) . . . . ?
Si2 C26 C39 C34 172.38(11) . . . . ?
C33 C34 C39 C38 179.23(15) . . . . ?
C35 C34 C39 C38 -1.6(2) . . . . ?
C33 C34 C39 C26 -2.3(2) . . . . ?
C35 C34 C39 C26 176.91(15) . . . . ?
C40 O1 C41 C42 -82.1(2) . . . . ?
O1 C41 C42 O2 72.9(2) . . . . ?
C41 C42 O2 C43 -173.25(18) . . . . ?

_refine_diff_density_max         0.496
_refine_diff_density_min         -0.281
_refine_diff_density_rms         0.046

_shelxl_version_number           2014-3



_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: 1,2-dimethoxyethane'
_chemical_properties_physical    
', Air-sensitive,Moisture-sensitive,Oxygen-sensitive'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_si361a
_database_code_depnum_ccdc_archive 'CCDC 1558535'
_audit_update_record             
;
2017-06-26 deposited with the CCDC.
2017-08-11 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014
_chemical_name_systematic        disilenylacridine
_chemical_name_common            ?
_chemical_melting_point          461
_chemical_formula_moiety         'C38 H59 N Si6'
_chemical_formula_sum            'C38 H59 N Si6'
_chemical_formula_weight         698.40

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'

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

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

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

_cell_length_a                   12.2262(11)
_cell_length_b                   16.6001(16)
_cell_length_c                   20.3560(19)
_cell_angle_alpha                90
_cell_angle_beta                 103.6680(10)
_cell_angle_gamma                90
_cell_volume                     4014.4(6)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9854
_cell_measurement_theta_min      2.40
_cell_measurement_theta_max      27.88

_exptl_crystal_description       block
_exptl_crystal_colour            blue
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.156
_exptl_crystal_F_000             1512
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.100
_exptl_absorpt_coefficient_mu    0.234
_shelx_estimated_absorpt_T_min   0.977
_shelx_estimated_absorpt_T_max   0.977
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.7036
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_process_details   'SADABS Sheldrick 1996'

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'Bruker TXS fine-focus rotating anode'
_diffrn_radiation_monochromator  'Bruker Helios multilayer confocal mirror'
_diffrn_measurement_device_type  'Bruker APEXII CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean 8.333
_diffrn_reflns_number            21223
_diffrn_reflns_av_unetI/netI     0.0143
_diffrn_reflns_av_R_equivalents  0.0120
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         1.601
_diffrn_reflns_theta_max         26.495
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measured_fraction_theta_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_point_group_measured_fraction_full 0.996
_reflns_number_total             8265
_reflns_number_gt                7524
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

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

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0400P)²+1.9792P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         8265
_refine_ls_number_parameters     421
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0318
_refine_ls_R_factor_gt           0.0285
_refine_ls_wR_factor_ref         0.0806
_refine_ls_wR_factor_gt          0.0776
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_restrained_S_all      1.032
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Si1 Si 0.25311(3) 0.23598(2) 0.76499(2) 0.01686(8) Uani 1 1 d . . . . .
Si2 Si 0.23628(3) 0.24316(2) 0.65676(2) 0.02146(9) Uani 1 1 d . . . . .
C1 C 0.36226(10) 0.28402(7) 0.83702(6) 0.0181(2) Uani 1 1 d . . . . .
C2 C 0.31304(11) 0.25337(8) 0.89785(6) 0.0206(3) Uani 1 1 d . . . . .
H1 H 0.3730 0.2541 0.9401 0.025 Uiso 1 1 calc R U . . .
H2 H 0.2520 0.2898 0.9038 0.025 Uiso 1 1 calc R U . . .
C3 C 0.26697(11) 0.16736(8) 0.88383(6) 0.0208(3) Uani 1 1 d . . . . .
H3 H 0.2307 0.1502 0.9202 0.025 Uiso 1 1 calc R U . . .
H4 H 0.3296 0.1298 0.8832 0.025 Uiso 1 1 calc R U . . .
C4 C 0.17818(10) 0.16458(7) 0.81329(6) 0.0171(2) Uani 1 1 d . . . . .
C5 C 0.33625(10) 0.30663(8) 0.61994(6) 0.0181(2) Uani 1 1 d . . . . .
C6 C 0.44757(10) 0.28108(8) 0.62344(6) 0.0185(2) Uani 1 1 d . . . . .
C7 C 0.49043(11) 0.20422(8) 0.64903(7) 0.0220(3) Uani 1 1 d . . . . .
H5 H 0.4417 0.1673 0.6637 0.026 Uiso 1 1 calc R U . . .
C8 C 0.59893(12) 0.18265(9) 0.65297(7) 0.0263(3) Uani 1 1 d . . . . .
H6 H 0.6249 0.1309 0.6697 0.032 Uiso 1 1 calc R U . . .
C9 C 0.67382(12) 0.23711(10) 0.63216(7) 0.0291(3) Uani 1 1 d . . . . .
H7 H 0.7501 0.2221 0.6361 0.035 Uiso 1 1 calc R U . . .
C10 C 0.63709(11) 0.31034(9) 0.60675(7) 0.0278(3) Uani 1 1 d . . . . .
H8 H 0.6883 0.3463 0.5935 0.033 Uiso 1 1 calc R U . . .
C11 C 0.52270(11) 0.33429(8) 0.59954(6) 0.0213(3) Uani 1 1 d . . . . .
C12 C 0.30304(11) 0.38163(8) 0.58851(6) 0.0188(2) Uani 1 1 d . . . . .
C13 C 0.19356(11) 0.41497(9) 0.58177(7) 0.0253(3) Uani 1 1 d . . . . .
H9 H 0.1388 0.3853 0.5979 0.030 Uiso 1 1 calc R U . . .
C14 C 0.16543(12) 0.48838(9) 0.55270(7) 0.0281(3) Uani 1 1 d . . . . .
H10 H 0.0921 0.5094 0.5495 0.034 Uiso 1 1 calc R U . . .
C15 C 0.24465(13) 0.53357(9) 0.52726(7) 0.0282(3) Uani 1 1 d . . . . .
H11 H 0.2241 0.5845 0.5068 0.034 Uiso 1 1 calc R U . . .
C16 C 0.35011(12) 0.50424(9) 0.53200(7) 0.0263(3) Uani 1 1 d . . . . .
H12 H 0.4022 0.5345 0.5141 0.032 Uiso 1 1 calc R U . . .
C17 C 0.38338(11) 0.42851(8) 0.56360(6) 0.0208(3) Uani 1 1 d . . . . .
C18 C 0.11396(10) 0.20369(7) 0.59008(6) 0.0165(2) Uani 1 1 d . . . . .
C19 C 0.13479(10) 0.14342(7) 0.54514(6) 0.0179(2) Uani 1 1 d . . . . .
C20 C 0.04580(11) 0.10970(8) 0.49760(6) 0.0200(3) Uani 1 1 d . . . . .
H13 H 0.0610 0.0692 0.4680 0.024 Uiso 1 1 calc R U . . .
C21 C -0.06505(11) 0.13383(8) 0.49243(6) 0.0201(3) Uani 1 1 d . . . . .
C22 C -0.08473(10) 0.19408(8) 0.53537(6) 0.0195(3) Uani 1 1 d . . . . .
H14 H -0.1598 0.2117 0.5319 0.023 Uiso 1 1 calc R U . . .
C23 C 0.00229(10) 0.22970(8) 0.58352(6) 0.0181(2) Uani 1 1 d . . . . .
C24 C 0.25255(11) 0.11317(8) 0.54852(7) 0.0230(3) Uani 1 1 d . . . . .
H15 H 0.2503 0.0727 0.5131 0.035 Uiso 1 1 calc R U . . .
H16 H 0.2834 0.0889 0.5929 0.035 Uiso 1 1 calc R U . . .
H17 H 0.3004 0.1583 0.5417 0.035 Uiso 1 1 calc R U . . .
C25 C -0.16076(12) 0.09726(9) 0.44063(7) 0.0283(3) Uani 1 1 d . . . . .
H18 H -0.2289 0.0971 0.4581 0.043 Uiso 1 1 calc R U . . .
H19 H -0.1415 0.0418 0.4312 0.043 Uiso 1 1 calc R U . . .
H20 H -0.1742 0.1290 0.3989 0.043 Uiso 1 1 calc R U . . .
C26 C -0.03017(11) 0.29701(9) 0.62486(7) 0.0277(3) Uani 1 1 d . . . . .
H21 H -0.0646 0.3409 0.5948 0.042 Uiso 1 1 calc R U . . .
H22 H 0.0371 0.3171 0.6569 0.042 Uiso 1 1 calc R U . . .
H23 H -0.0841 0.2769 0.6497 0.042 Uiso 1 1 calc R U . . .
Si3 Si 0.51391(3) 0.24506(2) 0.84853(2) 0.02086(9) Uani 1 1 d . . . . .
C27 C 0.58651(13) 0.24363(9) 0.94070(7) 0.0303(3) Uani 1 1 d . . . . .
H24 H 0.5529 0.2018 0.9637 0.045 Uiso 1 1 calc R U . . .
H25 H 0.5778 0.2962 0.9608 0.045 Uiso 1 1 calc R U . . .
H26 H 0.6667 0.2322 0.9458 0.045 Uiso 1 1 calc R U . . .
C28 C 0.60101(12) 0.30831(9) 0.80378(7) 0.0276(3) Uani 1 1 d . . . . .
H27 H 0.6764 0.2848 0.8104 0.041 Uiso 1 1 calc R U . . .
H28 H 0.6071 0.3631 0.8222 0.041 Uiso 1 1 calc R U . . .
H29 H 0.5651 0.3100 0.7554 0.041 Uiso 1 1 calc R U . . .
C29 C 0.52781(12) 0.13918(8) 0.82054(7) 0.0271(3) Uani 1 1 d . . . . .
H30 H 0.6070 0.1278 0.8219 0.041 Uiso 1 1 calc R U . . .
H31 H 0.4825 0.1322 0.7743 0.041 Uiso 1 1 calc R U . . .
H32 H 0.5012 0.1020 0.8508 0.041 Uiso 1 1 calc R U . . .
Si4 Si 0.36343(3) 0.39927(2) 0.83602(2) 0.02089(9) Uani 1 1 d . . . . .
C30 C 0.39088(14) 0.44412(9) 0.75719(7) 0.0300(3) Uani 1 1 d . . . . .
H33 H 0.3238 0.4380 0.7201 0.045 Uiso 1 1 calc R U . . .
H34 H 0.4546 0.4164 0.7456 0.045 Uiso 1 1 calc R U . . .
H35 H 0.4086 0.5015 0.7646 0.045 Uiso 1 1 calc R U . . .
C31 C 0.46948(13) 0.43891(9) 0.91157(8) 0.0316(3) Uani 1 1 d . . . . .
H36 H 0.4640 0.4978 0.9129 0.047 Uiso 1 1 calc R U . . .
H37 H 0.5454 0.4236 0.9082 0.047 Uiso 1 1 calc R U . . .
H38 H 0.4544 0.4160 0.9529 0.047 Uiso 1 1 calc R U . . .
C32 C 0.22691(13) 0.44520(9) 0.84319(9) 0.0327(3) Uani 1 1 d . . . . .
H39 H 0.2353 0.5038 0.8471 0.049 Uiso 1 1 calc R U . . .
H40 H 0.2058 0.4239 0.8834 0.049 Uiso 1 1 calc R U . . .
H41 H 0.1682 0.4319 0.8028 0.049 Uiso 1 1 calc R U . . .
Si5 Si 0.16616(3) 0.05612(2) 0.78092(2) 0.02056(9) Uani 1 1 d . . . . .
C33 C 0.30410(14) 0.00725(9) 0.78125(11) 0.0422(4) Uani 1 1 d . . . . .
H42 H 0.2912 -0.0485 0.7654 0.063 Uiso 1 1 calc R U . . .
H43 H 0.3518 0.0076 0.8273 0.063 Uiso 1 1 calc R U . . .
H44 H 0.3416 0.0370 0.7512 0.063 Uiso 1 1 calc R U . . .
C34 C 0.08083(14) 0.04332(9) 0.69254(7) 0.0313(3) Uani 1 1 d . . . . .
H45 H 0.1250 0.0608 0.6607 0.047 Uiso 1 1 calc R U . . .
H46 H 0.0123 0.0759 0.6860 0.047 Uiso 1 1 calc R U . . .
H47 H 0.0604 -0.0135 0.6845 0.047 Uiso 1 1 calc R U . . .
C35 C 0.10505(14) -0.00800(9) 0.83908(7) 0.0318(3) Uani 1 1 d . . . . .
H48 H 0.0276 0.0091 0.8369 0.048 Uiso 1 1 calc R U . . .
H49 H 0.1503 -0.0021 0.8855 0.048 Uiso 1 1 calc R U . . .
H50 H 0.1053 -0.0645 0.8252 0.048 Uiso 1 1 calc R U . . .
Si6 Si 0.03394(3) 0.19930(2) 0.82503(2) 0.02042(9) Uani 1 1 d . . . . .
C36 C 0.00537(12) 0.30982(8) 0.81359(7) 0.0274(3) Uani 1 1 d . . . . .
H51 H -0.0753 0.3198 0.8080 0.041 Uiso 1 1 calc R U . . .
H52 H 0.0288 0.3286 0.7734 0.041 Uiso 1 1 calc R U . . .
H53 H 0.0477 0.3389 0.8534 0.041 Uiso 1 1 calc R U . . .
C37 C 0.02083(14) 0.17527(9) 0.91285(8) 0.0319(3) Uani 1 1 d . . . . .
H54 H 0.0725 0.2094 0.9453 0.048 Uiso 1 1 calc R U . . .
H55 H 0.0398 0.1185 0.9228 0.048 Uiso 1 1 calc R U . . .
H56 H -0.0566 0.1853 0.9163 0.048 Uiso 1 1 calc R U . . .
C38 C -0.08861(13) 0.15040(10) 0.76505(9) 0.0389(4) Uani 1 1 d . . . . .
H57 H -0.0853 0.0920 0.7721 0.058 Uiso 1 1 calc R U . . .
H58 H -0.0854 0.1624 0.7184 0.058 Uiso 1 1 calc R U . . .
H59 H -0.1591 0.1713 0.7734 0.058 Uiso 1 1 calc R U . . .
N1 N 0.49079(9) 0.40558(7) 0.57029(6) 0.0240(2) Uani 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Si1 C4 1.9070(12) . ?
Si1 C1 1.9084(13) . ?
Si1 Si2 2.1669(5) . ?
Si2 C18 1.8838(13) . ?
Si2 C5 1.8970(13) . ?
C1 C2 1.5833(17) . ?
C1 Si4 1.9134(13) . ?
C1 Si3 1.9249(13) . ?
C2 C3 1.5366(18) . ?
C3 C4 1.5829(17) . ?
C4 Si5 1.9109(13) . ?
C4 Si6 1.9231(13) . ?
C5 C6 1.4112(18) . ?
C5 C12 1.4149(18) . ?
C6 C7 1.4300(19) . ?
C6 C11 1.4394(17) . ?
C7 C8 1.3580(19) . ?
C8 C9 1.421(2) . ?
C9 C10 1.355(2) . ?
C10 C11 1.4277(19) . ?
C11 N1 1.3408(18) . ?
C12 C13 1.4248(19) . ?
C12 C17 1.4362(17) . ?
C13 C14 1.363(2) . ?
C14 C15 1.416(2) . ?
C15 C16 1.360(2) . ?
C16 C17 1.4269(19) . ?
C17 N1 1.3429(17) . ?
C18 C23 1.4079(17) . ?
C18 C19 1.4188(17) . ?
C19 C20 1.3913(18) . ?
C19 C24 1.5110(17) . ?
C20 C21 1.3931(18) . ?
C21 C22 1.3862(18) . ?
C21 C25 1.5056(18) . ?
C22 C23 1.3962(18) . ?
C23 C26 1.5074(18) . ?
Si3 C29 1.8678(15) . ?
Si3 C27 1.8767(15) . ?
Si3 C28 1.8773(15) . ?
Si4 C30 1.8699(15) . ?
Si4 C32 1.8718(16) . ?
Si4 C31 1.8807(15) . ?
Si5 C34 1.8663(15) . ?
Si5 C33 1.8700(16) . ?
Si5 C35 1.8737(14) . ?
Si6 C36 1.8717(15) . ?
Si6 C37 1.8751(15) . ?
Si6 C38 1.8788(16) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C4 Si1 C1 101.39(5) . . ?
C4 Si1 Si2 128.07(4) . . ?
C1 Si1 Si2 129.74(4) . . ?
C18 Si2 C5 112.60(5) . . ?
C18 Si2 Si1 125.58(4) . . ?
C5 Si2 Si1 121.13(4) . . ?
C2 C1 Si1 98.08(8) . . ?
C2 C1 Si4 109.56(8) . . ?
Si1 C1 Si4 114.54(6) . . ?
C2 C1 Si3 109.27(8) . . ?
Si1 C1 Si3 115.58(6) . . ?
Si4 C1 Si3 109.14(6) . . ?
C3 C2 C1 110.10(10) . . ?
C2 C3 C4 109.77(10) . . ?
C3 C4 Si1 98.03(8) . . ?
C3 C4 Si5 108.70(8) . . ?
Si1 C4 Si5 114.52(6) . . ?
C3 C4 Si6 109.33(8) . . ?
Si1 C4 Si6 116.36(6) . . ?
Si5 C4 Si6 109.10(6) . . ?
C6 C5 C12 117.23(11) . . ?
C6 C5 Si2 121.13(10) . . ?
C12 C5 Si2 121.64(9) . . ?
C5 C6 C7 123.54(11) . . ?
C5 C6 C11 118.92(12) . . ?
C7 C6 C11 117.54(12) . . ?
C8 C7 C6 121.71(12) . . ?
C7 C8 C9 120.26(13) . . ?
C10 C9 C8 120.38(13) . . ?
C9 C10 C11 121.14(13) . . ?
N1 C11 C10 117.82(12) . . ?
N1 C11 C6 123.35(12) . . ?
C10 C11 C6 118.83(12) . . ?
C5 C12 C13 123.23(12) . . ?
C5 C12 C17 119.30(12) . . ?
C13 C12 C17 117.44(12) . . ?
C14 C13 C12 121.61(13) . . ?
C13 C14 C15 120.54(13) . . ?
C16 C15 C14 120.21(13) . . ?
C15 C16 C17 120.78(13) . . ?
N1 C17 C16 117.59(12) . . ?
N1 C17 C12 122.99(12) . . ?
C16 C17 C12 119.39(12) . . ?
C23 C18 C19 118.21(11) . . ?
C23 C18 Si2 123.28(9) . . ?
C19 C18 Si2 118.49(9) . . ?
C20 C19 C18 120.14(11) . . ?
C20 C19 C24 118.56(11) . . ?
C18 C19 C24 121.28(11) . . ?
C19 C20 C21 121.59(12) . . ?
C22 C21 C20 118.07(12) . . ?
C22 C21 C25 120.70(12) . . ?
C20 C21 C25 121.22(12) . . ?
C21 C22 C23 122.08(12) . . ?
C22 C23 C18 119.86(12) . . ?
C22 C23 C26 116.64(11) . . ?
C18 C23 C26 123.48(11) . . ?
C29 Si3 C27 103.73(7) . . ?
C29 Si3 C28 105.98(7) . . ?
C27 Si3 C28 107.68(7) . . ?
C29 Si3 C1 115.69(6) . . ?
C27 Si3 C1 109.90(6) . . ?
C28 Si3 C1 113.17(6) . . ?
C30 Si4 C32 104.41(7) . . ?
C30 Si4 C31 109.49(7) . . ?
C32 Si4 C31 104.41(7) . . ?
C30 Si4 C1 114.24(6) . . ?
C32 Si4 C1 113.42(6) . . ?
C31 Si4 C1 110.28(6) . . ?
C34 Si5 C33 104.61(8) . . ?
C34 Si5 C35 109.20(7) . . ?
C33 Si5 C35 104.20(8) . . ?
C34 Si5 C4 114.81(6) . . ?
C33 Si5 C4 114.31(7) . . ?
C35 Si5 C4 109.09(6) . . ?
C36 Si6 C37 105.76(7) . . ?
C36 Si6 C38 104.23(7) . . ?
C37 Si6 C38 107.03(8) . . ?
C36 Si6 C4 115.34(6) . . ?
C37 Si6 C4 110.01(6) . . ?
C38 Si6 C4 113.81(6) . . ?
C11 N1 C17 118.05(11) . . ?

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
Si1 C1 C2 C3 37.42(11) . . . . ?
Si4 C1 C2 C3 157.13(9) . . . . ?
Si3 C1 C2 C3 -83.35(11) . . . . ?
C1 C2 C3 C4 -54.71(13) . . . . ?
C2 C3 C4 Si1 38.57(11) . . . . ?
C2 C3 C4 Si5 157.92(9) . . . . ?
C2 C3 C4 Si6 -83.08(11) . . . . ?
C18 Si2 C5 C6 -114.30(10) . . . . ?
Si1 Si2 C5 C6 74.66(11) . . . . ?
C18 Si2 C5 C12 66.32(11) . . . . ?
Si1 Si2 C5 C12 -104.72(10) . . . . ?
C12 C5 C6 C7 -175.11(12) . . . . ?
Si2 C5 C6 C7 5.48(17) . . . . ?
C12 C5 C6 C11 4.25(17) . . . . ?
Si2 C5 C6 C11 -175.16(9) . . . . ?
C5 C6 C7 C8 -178.47(13) . . . . ?
C11 C6 C7 C8 2.16(19) . . . . ?
C6 C7 C8 C9 0.7(2) . . . . ?
C7 C8 C9 C10 -1.5(2) . . . . ?
C8 C9 C10 C11 -0.7(2) . . . . ?
C9 C10 C11 N1 -176.07(13) . . . . ?
C9 C10 C11 C6 3.6(2) . . . . ?
C5 C6 C11 N1 -3.99(19) . . . . ?
C7 C6 C11 N1 175.41(12) . . . . ?
C5 C6 C11 C10 176.37(12) . . . . ?
C7 C6 C11 C10 -4.23(18) . . . . ?
C6 C5 C12 C13 -179.67(12) . . . . ?
Si2 C5 C12 C13 -0.26(17) . . . . ?
C6 C5 C12 C17 -1.58(17) . . . . ?
Si2 C5 C12 C17 177.83(9) . . . . ?
C5 C12 C13 C14 178.30(13) . . . . ?
C17 C12 C13 C14 0.2(2) . . . . ?
C12 C13 C14 C15 0.9(2) . . . . ?
C13 C14 C15 C16 -0.4(2) . . . . ?
C14 C15 C16 C17 -1.1(2) . . . . ?
C15 C16 C17 N1 -175.93(13) . . . . ?
C15 C16 C17 C12 2.2(2) . . . . ?
C5 C12 C17 N1 -1.86(19) . . . . ?
C13 C12 C17 N1 176.34(12) . . . . ?
C5 C12 C17 C16 -179.88(12) . . . . ?
C13 C12 C17 C16 -1.68(18) . . . . ?
C5 Si2 C18 C23 -111.45(11) . . . . ?
Si1 Si2 C18 C23 59.12(12) . . . . ?
C5 Si2 C18 C19 70.03(11) . . . . ?
Si1 Si2 C18 C19 -119.40(9) . . . . ?
C23 C18 C19 C20 -2.06(17) . . . . ?
Si2 C18 C19 C20 176.54(9) . . . . ?
C23 C18 C19 C24 179.26(11) . . . . ?
Si2 C18 C19 C24 -2.15(16) . . . . ?
C18 C19 C20 C21 0.26(19) . . . . ?
C24 C19 C20 C21 178.98(12) . . . . ?
C19 C20 C21 C22 1.25(19) . . . . ?
C19 C20 C21 C25 179.73(12) . . . . ?
C20 C21 C22 C23 -0.94(19) . . . . ?
C25 C21 C22 C23 -179.43(12) . . . . ?
C21 C22 C23 C18 -0.88(19) . . . . ?
C21 C22 C23 C26 177.39(12) . . . . ?
C19 C18 C23 C22 2.35(17) . . . . ?
Si2 C18 C23 C22 -176.17(9) . . . . ?
C19 C18 C23 C26 -175.79(12) . . . . ?
Si2 C18 C23 C26 5.68(18) . . . . ?
C10 C11 N1 C17 -179.77(12) . . . . ?
C6 C11 N1 C17 0.58(19) . . . . ?
C16 C17 N1 C11 -179.59(12) . . . . ?
C12 C17 N1 C11 2.36(19) . . . . ?

_refine_diff_density_max         0.356
_refine_diff_density_min         -0.278
_refine_diff_density_rms         0.043

_shelxl_version_number           2014-3



_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: hexane/THF (5:1)'
_chemical_properties_physical    
', Air-sensitive,Moisture-sensitive,Oxygen-sensitive'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_NA15d
_database_code_depnum_ccdc_archive 'CCDC 1558533'
_audit_update_record             
;
2017-06-26 deposited with the CCDC.
2017-08-11 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014
_chemical_name_systematic        Bis(disilenyl)bithiophene
_chemical_name_common            ?
_chemical_melting_point          510
_chemical_formula_moiety         'C58 H106 S2 Si12, 4(C5 H10 O)'
_chemical_formula_sum            'C78 H146 O4 S2 Si12'
_chemical_formula_weight         1549.14

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 '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'

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

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

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

_cell_length_a                   16.030(3)
_cell_length_b                   30.312(6)
_cell_length_c                   9.521(2)
_cell_angle_alpha                90
_cell_angle_beta                 93.418(3)
_cell_angle_gamma                90
_cell_volume                     4617.9(17)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9970
_cell_measurement_theta_min      2.25
_cell_measurement_theta_max      27.43

_exptl_crystal_description       plate
_exptl_crystal_colour            orange
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.114
_exptl_crystal_F_000             1692
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.020
_exptl_absorpt_coefficient_mu    0.256
_shelx_estimated_absorpt_T_min   0.927
_shelx_estimated_absorpt_T_max   0.995
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.4925
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_process_details   'SADABS Sheldrick 1996'

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'Bruker TXS fine-focus rotating anode'
_diffrn_radiation_monochromator  'Bruker Helios multilayer confocal mirror'
_diffrn_measurement_device_type  'Bruker APEXII CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean 8.333
_diffrn_reflns_number            40728
_diffrn_reflns_av_unetI/netI     0.0800
_diffrn_reflns_av_R_equivalents  0.0975
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_theta_min         1.273
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measured_fraction_theta_full 0.969
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_Laue_measured_fraction_full 0.969
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_point_group_measured_fraction_full 0.969
_reflns_number_total             8100
_reflns_number_gt                5368
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

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

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1011P)²+3.6667P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         8100
_refine_ls_number_parameters     460
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1175
_refine_ls_R_factor_gt           0.0728
_refine_ls_wR_factor_ref         0.1991
_refine_ls_wR_factor_gt          0.1803
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_restrained_S_all      1.079
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Si1 Si 0.26450(6) 0.41385(3) 0.59027(12) 0.0207(3) Uani 1 1 d . . . . .
Si2 Si 0.1337(5) 0.4071(2) 0.6355(13) 0.0288(19) Uani 0.82(4) 1 d . . P A 1
Si3 Si 0.1530(15) 0.3989(5) 0.692(4) 0.018(5) Uani 0.18(4) 1 d . . P A 2
Si4 Si 0.28597(7) 0.51379(4) 0.48488(13) 0.0262(3) Uani 1 1 d . . . . .
Si5 Si 0.35285(7) 0.48506(4) 0.78897(12) 0.0278(3) Uani 1 1 d . . . . .
Si6 Si 0.27700(8) 0.34793(4) 0.33151(13) 0.0321(3) Uani 1 1 d . . . . .
Si7 Si 0.39409(7) 0.33432(4) 0.60540(14) 0.0311(3) Uani 1 1 d . . . . .
S1 S 0.08862(7) 0.45061(4) 0.92975(13) 0.0370(3) Uani 1 1 d . . . . .
C1 C 0.0824(3) 0.44732(14) 0.7498(5) 0.0373(12) Uani 1 1 d . . . . .
C2 C 0.0216(3) 0.47624(15) 0.7067(8) 0.0602(18) Uani 1 1 d . . . . .
H1 H 0.0057 0.4790 0.6093 0.072 Uiso 1 1 calc R U . . .
C3 C -0.0160(3) 0.50091(15) 0.8006(5) 0.0381(11) Uani 1 1 d . . . . .
H2 H -0.0573 0.5226 0.7772 0.046 Uiso 1 1 calc R U . . .
C4 C 0.0130(2) 0.49078(13) 0.9353(5) 0.0279(10) Uani 1 1 d . . . . .
C5 C 0.3286(2) 0.46639(12) 0.5982(4) 0.0188(8) Uani 1 1 d . . . . .
C6 C 0.4118(2) 0.44920(12) 0.5363(4) 0.0220(9) Uani 1 1 d . . . . .
H3 H 0.4392 0.4739 0.4888 0.026 Uiso 1 1 calc R U . . .
H4 H 0.4504 0.4388 0.6144 0.026 Uiso 1 1 calc R U . . .
C7 C 0.3952(2) 0.41128(12) 0.4306(4) 0.0225(9) Uani 1 1 d . . . . .
H5 H 0.4487 0.3968 0.4117 0.027 Uiso 1 1 calc R U . . .
H6 H 0.3709 0.4234 0.3407 0.027 Uiso 1 1 calc R U . . .
C8 C 0.3340(2) 0.37631(12) 0.4879(4) 0.0223(9) Uani 1 1 d . . . . .
C9 C 0.2866(3) 0.50186(16) 0.2920(5) 0.0447(12) Uani 1 1 d . . . . .
H7 H 0.2487 0.4772 0.2683 0.067 Uiso 1 1 calc R U . . .
H8 H 0.3434 0.4940 0.2682 0.067 Uiso 1 1 calc R U . . .
H9 H 0.2681 0.5281 0.2385 0.067 Uiso 1 1 calc R U . . .
C10 C 0.3543(3) 0.56369(14) 0.5095(5) 0.0371(11) Uani 1 1 d . . . . .
H10 H 0.3345 0.5868 0.4439 0.056 Uiso 1 1 calc R U . . .
H11 H 0.4120 0.5559 0.4913 0.056 Uiso 1 1 calc R U . . .
H12 H 0.3522 0.5744 0.6063 0.056 Uiso 1 1 calc R U . . .
C11 C 0.1771(3) 0.52937(15) 0.5177(6) 0.0432(13) Uani 1 1 d . . . . .
H13 H 0.1744 0.5392 0.6154 0.065 Uiso 1 1 calc R U . . .
H14 H 0.1404 0.5038 0.5009 0.065 Uiso 1 1 calc R U . . .
H15 H 0.1590 0.5534 0.4541 0.065 Uiso 1 1 calc R U . . .
C12 C 0.4597(3) 0.51102(17) 0.8045(5) 0.0409(12) Uani 1 1 d . . . . .
H16 H 0.4630 0.5343 0.7337 0.061 Uiso 1 1 calc R U . . .
H17 H 0.5021 0.4885 0.7892 0.061 Uiso 1 1 calc R U . . .
H18 H 0.4697 0.5237 0.8986 0.061 Uiso 1 1 calc R U . . .
C13 C 0.2765(3) 0.52587(15) 0.8530(5) 0.0443(13) Uani 1 1 d . . . . .
H19 H 0.2196 0.5143 0.8372 0.066 Uiso 1 1 calc R U . . .
H20 H 0.2814 0.5537 0.8017 0.066 Uiso 1 1 calc R U . . .
H21 H 0.2884 0.5311 0.9538 0.066 Uiso 1 1 calc R U . . .
C14 C 0.3547(3) 0.43823(16) 0.9183(5) 0.0394(12) Uani 1 1 d . . . . .
H22 H 0.3735 0.4491 1.0118 0.059 Uiso 1 1 calc R U . . .
H23 H 0.3932 0.4153 0.8889 0.059 Uiso 1 1 calc R U . . .
H24 H 0.2984 0.4258 0.9216 0.059 Uiso 1 1 calc R U . . .
C15 C 0.2158(3) 0.29870(15) 0.3853(6) 0.0455(13) Uani 1 1 d . . . . .
H25 H 0.1896 0.2845 0.3014 0.068 Uiso 1 1 calc R U . . .
H26 H 0.1725 0.3081 0.4473 0.068 Uiso 1 1 calc R U . . .
H27 H 0.2534 0.2777 0.4354 0.068 Uiso 1 1 calc R U . . .
C16 C 0.3515(3) 0.33082(18) 0.1962(5) 0.0488(13) Uani 1 1 d . . . . .
H28 H 0.3895 0.3082 0.2362 0.073 Uiso 1 1 calc R U . . .
H29 H 0.3839 0.3565 0.1686 0.073 Uiso 1 1 calc R U . . .
H30 H 0.3199 0.3189 0.1135 0.073 Uiso 1 1 calc R U . . .
C17 C 0.2043(3) 0.38666(18) 0.2317(5) 0.0466(13) Uani 1 1 d . . . . .
H31 H 0.2368 0.4079 0.1798 0.070 Uiso 1 1 calc R U . . .
H32 H 0.1705 0.4025 0.2977 0.070 Uiso 1 1 calc R U . . .
H33 H 0.1676 0.3699 0.1654 0.070 Uiso 1 1 calc R U . . .
C18 C 0.4385(3) 0.28818(16) 0.5024(6) 0.0536(15) Uani 1 1 d . . . . .
H34 H 0.4707 0.2684 0.5664 0.080 Uiso 1 1 calc R U . . .
H35 H 0.4752 0.3003 0.4332 0.080 Uiso 1 1 calc R U . . .
H36 H 0.3929 0.2717 0.4535 0.080 Uiso 1 1 calc R U . . .
C19 C 0.4898(3) 0.35799(16) 0.7013(6) 0.0494(13) Uani 1 1 d . . . . .
H37 H 0.4733 0.3818 0.7636 0.074 Uiso 1 1 calc R U . . .
H38 H 0.5274 0.3697 0.6330 0.074 Uiso 1 1 calc R U . . .
H39 H 0.5185 0.3348 0.7572 0.074 Uiso 1 1 calc R U . . .
C20 C 0.3271(3) 0.31011(16) 0.7395(6) 0.0504(14) Uani 1 1 d . . . . .
H40 H 0.2749 0.2993 0.6929 0.076 Uiso 1 1 calc R U . . .
H41 H 0.3145 0.3328 0.8085 0.076 Uiso 1 1 calc R U . . .
H42 H 0.3567 0.2856 0.7874 0.076 Uiso 1 1 calc R U . . .
C21 C 0.0766(2) 0.35251(13) 0.6341(5) 0.0280(10) Uani 1 1 d . . . . .
C22 C 0.0214(3) 0.34425(14) 0.5176(5) 0.0315(10) Uani 1 1 d . . . . .
C23 C -0.0196(3) 0.30365(15) 0.5058(5) 0.0364(11) Uani 1 1 d . . . . .
H43 H -0.0559 0.2981 0.4252 0.044 Uiso 1 1 calc R U . . .
C24 C -0.0092(3) 0.27157(14) 0.6066(5) 0.0384(12) Uani 1 1 d . . . . .
C25 C 0.0423(3) 0.28047(14) 0.7247(5) 0.0340(11) Uani 1 1 d . . . . .
H44 H 0.0494 0.2587 0.7961 0.041 Uiso 1 1 calc R U . . .
C26 C 0.0841(3) 0.32066(14) 0.7420(5) 0.0304(10) Uani 1 1 d . . . . .
C27 C 0.0014(3) 0.37798(18) 0.4030(6) 0.0515(14) Uani 1 1 d . . . . .
H45 H 0.0317 0.3705 0.3197 0.077 Uiso 1 1 calc R U . . .
H46 H 0.0185 0.4073 0.4368 0.077 Uiso 1 1 calc R U . . .
H47 H -0.0588 0.3779 0.3783 0.077 Uiso 1 1 calc R U . . .
C28 C -0.0537(4) 0.22773(17) 0.5899(6) 0.0630(17) Uani 1 1 d . . . . .
H48 H -0.1097 0.2302 0.6249 0.095 Uiso 1 1 calc R U . . .
H49 H -0.0220 0.2051 0.6437 0.095 Uiso 1 1 calc R U . . .
H50 H -0.0582 0.2195 0.4902 0.095 Uiso 1 1 calc R U . . .
C29 C 0.1317(3) 0.32936(18) 0.8805(5) 0.0450(13) Uani 1 1 d . . . . .
H51 H 0.0956 0.3450 0.9436 0.067 Uiso 1 1 calc R U . . .
H52 H 0.1809 0.3475 0.8647 0.067 Uiso 1 1 calc R U . . .
H53 H 0.1497 0.3013 0.9234 0.067 Uiso 1 1 calc R U . . .
O1 O 0.2059(3) 0.66236(16) 0.0655(6) 0.0919(15) Uani 1 1 d . . . . .
C30 C 0.2170(8) 0.6717(4) 0.2172(10) 0.164(5) Uani 1 1 d . . . . .
H54 H 0.2773 0.6719 0.2464 0.197 Uiso 1 1 calc R U . . .
H55 H 0.1939 0.7012 0.2369 0.197 Uiso 1 1 calc R U . . .
C31 C 0.1775(5) 0.6406(3) 0.2917(8) 0.087(2) Uani 1 1 d . . . . .
H56 H 0.1429 0.6547 0.3621 0.104 Uiso 1 1 calc R U . . .
H57 H 0.2185 0.6208 0.3413 0.104 Uiso 1 1 calc R U . . .
C32 C 0.1230(4) 0.6152(3) 0.1843(7) 0.080(2) Uani 1 1 d . . . . .
H58 H 0.1139 0.5845 0.2155 0.096 Uiso 1 1 calc R U . . .
H59 H 0.0682 0.6297 0.1654 0.096 Uiso 1 1 calc R U . . .
C33 C 0.1723(5) 0.6165(2) 0.0632(8) 0.092(2) Uani 1 1 d . . . . .
H60 H 0.2188 0.5945 0.0722 0.111 Uiso 1 1 calc R U . . .
C34 C 0.1238(4) 0.6108(2) -0.0677(8) 0.080(2) Uani 1 1 d . . . . .
H61 H 0.1147 0.5793 -0.0853 0.120 Uiso 1 1 calc R U . . .
H62 H 0.1540 0.6236 -0.1445 0.120 Uiso 1 1 calc R U . . .
H63 H 0.0698 0.6257 -0.0625 0.120 Uiso 1 1 calc R U . . .
O2 O 0.3501(7) 0.6451(3) 0.7774(10) 0.219(5) Uani 1 1 d . . . . .
C35 C 0.4029(5) 0.6425(2) 0.9043(9) 0.091(2) Uani 1 1 d . . . . .
H64 H 0.4579 0.6295 0.8859 0.109 Uiso 1 1 calc R U . . .
H65 H 0.3766 0.6245 0.9763 0.109 Uiso 1 1 calc R U . . .
C36 C 0.4114(5) 0.6879(3) 0.9483(9) 0.103(3) Uani 1 1 d . . . . .
H66 H 0.4707 0.6954 0.9719 0.123 Uiso 1 1 calc R U . . .
H67 H 0.3787 0.6937 1.0313 0.123 Uiso 1 1 calc R U . . .
C37 C 0.3765(7) 0.7145(3) 0.8192(10) 0.129(4) Uani 1 1 d . . . . .
H68 H 0.3536 0.7433 0.8480 0.155 Uiso 1 1 calc R U . . .
H69 H 0.4201 0.7197 0.7517 0.155 Uiso 1 1 calc R U . . .
C38 C 0.3110(8) 0.6860(4) 0.7592(13) 0.143(4) Uani 1 1 d . . . . .
H70 H 0.2610 0.6876 0.8169 0.172 Uiso 1 1 calc R U . . .
C39 C 0.2869(8) 0.6937(4) 0.6148(11) 0.176(6) Uani 1 1 d . . . . .
H71 H 0.3358 0.6907 0.5584 0.265 Uiso 1 1 calc R U . . .
H72 H 0.2639 0.7236 0.6036 0.265 Uiso 1 1 calc R U . . .
H73 H 0.2443 0.6721 0.5829 0.265 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Si1 C5 1.894(4) . ?
Si1 C8 1.902(4) . ?
Si1 Si3 2.133(12) . ?
Si1 Si2 2.176(4) . ?
Si2 C1 1.860(5) . ?
Si2 C21 1.889(5) . ?
Si3 C21 1.924(18) . ?
Si3 C1 1.953(15) . ?
Si4 C11 1.852(4) . ?
Si4 C9 1.872(5) . ?
Si4 C10 1.874(4) . ?
Si4 C5 1.899(4) . ?
Si5 C13 1.868(5) . ?
Si5 C14 1.878(5) . ?
Si5 C12 1.883(4) . ?
Si5 C5 1.920(4) . ?
Si6 C17 1.873(5) . ?
Si6 C15 1.874(5) . ?
Si6 C16 1.881(5) . ?
Si6 C8 1.905(4) . ?
Si7 C20 1.867(5) . ?
Si7 C18 1.873(5) . ?
Si7 C19 1.880(5) . ?
Si7 C8 1.916(4) . ?
S1 C1 1.713(5) . ?
S1 C4 1.721(4) . ?
C1 C2 1.355(7) . ?
C2 C3 1.337(7) . ?
C3 C4 1.372(6) . ?
C4 C4 1.436(8) 3_567 ?
C5 C6 1.578(5) . ?
C6 C7 1.541(5) . ?
C7 C8 1.564(5) . ?
C21 C22 1.400(6) . ?
C21 C26 1.410(6) . ?
C22 C23 1.397(6) . ?
C22 C27 1.515(6) . ?
C23 C24 1.370(7) . ?
C24 C25 1.381(7) . ?
C24 C28 1.512(6) . ?
C25 C26 1.396(6) . ?
C26 C29 1.507(6) . ?
O1 C30 1.472(10) . ?
O1 C33 1.490(9) . ?
C30 C31 1.359(10) . ?
C31 C32 1.516(10) . ?
C32 C33 1.437(9) . ?
C33 C34 1.439(10) . ?
O2 C38 1.397(12) . ?
O2 C35 1.435(10) . ?
C35 C36 1.443(10) . ?
C36 C37 1.548(11) . ?
C37 C38 1.450(12) . ?
C38 C39 1.425(13) . ?

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
C5 Si1 C8 100.98(16) . . ?
C5 Si1 Si3 128.9(3) . . ?
C8 Si1 Si3 129.7(3) . . ?
C5 Si1 Si2 126.76(18) . . ?
C8 Si1 Si2 130.25(14) . . ?
C1 Si2 C21 110.3(2) . . ?
C1 Si2 Si1 121.3(2) . . ?
C21 Si2 Si1 123.6(4) . . ?
C21 Si3 C1 105.1(11) . . ?
C21 Si3 Si1 124.1(11) . . ?
C1 Si3 Si1 118.9(8) . . ?
C11 Si4 C9 106.0(2) . . ?
C11 Si4 C10 108.8(2) . . ?
C9 Si4 C10 104.0(2) . . ?
C11 Si4 C5 114.06(19) . . ?
C9 Si4 C5 112.84(19) . . ?
C10 Si4 C5 110.60(19) . . ?
C13 Si5 C14 105.8(2) . . ?
C13 Si5 C12 108.0(2) . . ?
C14 Si5 C12 106.6(2) . . ?
C13 Si5 C5 113.8(2) . . ?
C14 Si5 C5 113.06(19) . . ?
C12 Si5 C5 109.24(18) . . ?
C17 Si6 C15 108.5(2) . . ?
C17 Si6 C16 103.1(2) . . ?
C15 Si6 C16 109.3(2) . . ?
C17 Si6 C8 111.6(2) . . ?
C15 Si6 C8 112.4(2) . . ?
C16 Si6 C8 111.4(2) . . ?
C20 Si7 C18 108.5(2) . . ?
C20 Si7 C19 107.7(3) . . ?
C18 Si7 C19 102.4(2) . . ?
C20 Si7 C8 111.77(19) . . ?
C18 Si7 C8 112.6(2) . . ?
C19 Si7 C8 113.39(19) . . ?
C1 S1 C4 94.2(2) . . ?
C2 C1 S1 105.3(4) . . ?
C2 C1 Si2 125.6(7) . . ?
S1 C1 Si2 128.5(6) . . ?
C2 C1 Si3 145.0(14) . . ?
S1 C1 Si3 108.9(14) . . ?
C3 C2 C1 120.2(6) . . ?
C2 C3 C4 111.1(5) . . ?
C3 C4 C4 127.9(5) . 3_567 ?
C3 C4 S1 109.2(3) . . ?
C4 C4 S1 122.9(5) 3_567 . ?
C6 C5 Si1 100.1(2) . . ?
C6 C5 Si4 108.7(2) . . ?
Si1 C5 Si4 116.0(2) . . ?
C6 C5 Si5 108.8(3) . . ?
Si1 C5 Si5 111.37(19) . . ?
Si4 C5 Si5 111.11(18) . . ?
C7 C6 C5 111.9(3) . . ?
C6 C7 C8 111.4(3) . . ?
C7 C8 Si1 99.9(2) . . ?
C7 C8 Si6 108.3(3) . . ?
Si1 C8 Si6 113.7(2) . . ?
C7 C8 Si7 110.5(3) . . ?
Si1 C8 Si7 112.8(2) . . ?
Si6 C8 Si7 110.93(19) . . ?
C22 C21 C26 118.5(4) . . ?
C22 C21 Si2 116.4(6) . . ?
C26 C21 Si2 125.0(6) . . ?
C22 C21 Si3 136.1(14) . . ?
C26 C21 Si3 105.4(14) . . ?
C23 C22 C21 119.6(4) . . ?
C23 C22 C27 117.3(4) . . ?
C21 C22 C27 123.1(4) . . ?
C24 C23 C22 122.2(4) . . ?
C23 C24 C25 118.3(4) . . ?
C23 C24 C28 120.9(5) . . ?
C25 C24 C28 120.8(5) . . ?
C24 C25 C26 121.8(4) . . ?
C25 C26 C21 119.5(4) . . ?
C25 C26 C29 118.1(4) . . ?
C21 C26 C29 122.3(4) . . ?
C30 O1 C33 102.5(6) . . ?
C31 C30 O1 110.2(8) . . ?
C30 C31 C32 105.6(7) . . ?
C33 C32 C31 101.8(6) . . ?
C32 C33 C34 113.4(7) . . ?
C32 C33 O1 103.3(5) . . ?
C34 C33 O1 107.6(6) . . ?
C38 O2 C35 113.0(7) . . ?
O2 C35 C36 103.4(7) . . ?
C35 C36 C37 104.1(7) . . ?
C38 C37 C36 102.8(8) . . ?
O2 C38 C39 111.0(11) . . ?
O2 C38 C37 99.9(9) . . ?
C39 C38 C37 115.6(10) . . ?

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
C4 S1 C1 C2 -1.5(3) . . . . ?
C4 S1 C1 Si2 -172.4(3) . . . . ?
C4 S1 C1 Si3 -174.0(4) . . . . ?
C21 Si2 C1 C2 -91.7(8) . . . . ?
Si1 Si2 C1 C2 112.0(8) . . . . ?
C21 Si2 C1 S1 77.5(8) . . . . ?
Si1 Si2 C1 S1 -78.8(8) . . . . ?
C21 Si2 C1 Si3 82.0(15) . . . . ?
Si1 Si2 C1 Si3 -74.3(12) . . . . ?
S1 C1 C2 C3 2.7(5) . . . . ?
Si2 C1 C2 C3 173.9(4) . . . . ?
Si3 C1 C2 C3 170.3(7) . . . . ?
C1 C2 C3 C4 -2.6(6) . . . . ?
C2 C3 C4 C4 -178.6(5) . . . 3_567 ?
C2 C3 C4 S1 1.2(5) . . . . ?
C1 S1 C4 C3 0.2(3) . . . . ?
C1 S1 C4 C4 180.0(5) . . . 3_567 ?
C8 Si1 C5 C6 -8.2(3) . . . . ?
Si3 Si1 C5 C6 164.7(16) . . . . ?
Si2 Si1 C5 C6 -173.3(5) . . . . ?
C8 Si1 C5 Si4 108.5(2) . . . . ?
Si3 Si1 C5 Si4 -78.6(16) . . . . ?
Si2 Si1 C5 Si4 -56.6(5) . . . . ?
C8 Si1 C5 Si5 -123.1(2) . . . . ?
Si3 Si1 C5 Si5 49.8(16) . . . . ?
Si2 Si1 C5 Si5 71.7(5) . . . . ?
C11 Si4 C5 C6 166.8(3) . . . . ?
C9 Si4 C5 C6 45.8(3) . . . . ?
C10 Si4 C5 C6 -70.2(3) . . . . ?
C11 Si4 C5 Si1 55.0(3) . . . . ?
C9 Si4 C5 Si1 -66.0(3) . . . . ?
C10 Si4 C5 Si1 178.0(2) . . . . ?
C11 Si4 C5 Si5 -73.5(3) . . . . ?
C9 Si4 C5 Si5 165.5(2) . . . . ?
C10 Si4 C5 Si5 49.5(2) . . . . ?
Si1 C5 C6 C7 30.0(4) . . . . ?
Si4 C5 C6 C7 -92.1(3) . . . . ?
Si5 C5 C6 C7 146.8(3) . . . . ?
C5 C6 C7 C8 -45.6(4) . . . . ?
C6 C7 C8 Si1 34.0(3) . . . . ?
C6 C7 C8 Si6 153.2(3) . . . . ?
C6 C7 C8 Si7 -85.1(3) . . . . ?
C1 Si2 C21 C22 100.0(7) . . . . ?
Si1 Si2 C21 C22 -104.4(8) . . . . ?
C1 Si2 C21 C26 -78.4(8) . . . . ?
Si1 Si2 C21 C26 77.3(8) . . . . ?
C1 Si2 C21 Si3 -85.6(11) . . . . ?
Si1 Si2 C21 Si3 70.1(15) . . . . ?
C26 C21 C22 C23 -5.0(6) . . . . ?
Si2 C21 C22 C23 176.6(3) . . . . ?
Si3 C21 C22 C23 173.9(6) . . . . ?
C26 C21 C22 C27 173.4(4) . . . . ?
Si2 C21 C22 C27 -5.0(5) . . . . ?
Si3 C21 C22 C27 -7.7(8) . . . . ?
C21 C22 C23 C24 1.5(6) . . . . ?
C27 C22 C23 C24 -176.9(4) . . . . ?
C22 C23 C24 C25 1.5(7) . . . . ?
C22 C23 C24 C28 -179.3(4) . . . . ?
C23 C24 C25 C26 -0.9(6) . . . . ?
C28 C24 C25 C26 179.8(4) . . . . ?
C24 C25 C26 C21 -2.5(6) . . . . ?
C24 C25 C26 C29 173.7(4) . . . . ?
C22 C21 C26 C25 5.4(6) . . . . ?
Si2 C21 C26 C25 -176.3(3) . . . . ?
Si3 C21 C26 C25 -173.7(4) . . . . ?
C22 C21 C26 C29 -170.7(4) . . . . ?
Si2 C21 C26 C29 7.6(6) . . . . ?
Si3 C21 C26 C29 10.1(6) . . . . ?
C33 O1 C30 C31 -12.8(12) . . . . ?
O1 C30 C31 C32 -12.0(12) . . . . ?
C30 C31 C32 C33 33.1(10) . . . . ?
C31 C32 C33 C34 -156.5(6) . . . . ?
C31 C32 C33 O1 -40.4(7) . . . . ?
C30 O1 C33 C32 33.6(9) . . . . ?
C30 O1 C33 C34 153.7(8) . . . . ?
C38 O2 C35 C36 -13.9(13) . . . . ?
O2 C35 C36 C37 -12.4(10) . . . . ?
C35 C36 C37 C38 33.3(11) . . . . ?
C35 O2 C38 C39 157.5(10) . . . . ?
C35 O2 C38 C37 35.0(13) . . . . ?
C36 C37 C38 O2 -39.7(11) . . . . ?
C36 C37 C38 C39 -158.9(11) . . . . ?

_refine_diff_density_max         1.178
_refine_diff_density_min         -0.776
_refine_diff_density_rms         0.088

_shelxl_version_number           2014-3



_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: 2-methyltetrahydrofuran'
_chemical_properties_physical    
', Air-sensitive,Moisture-sensitive,Oxygen-sensitive'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_TK59a_a
_database_code_depnum_ccdc_archive 'CCDC 1558536'
_audit_update_record             
;
2017-06-26 deposited with the CCDC.
2017-08-11 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014
_chemical_name_systematic        disilenylmesitylene
_chemical_name_common            ?
_chemical_melting_point          444
_chemical_formula_moiety         'C34 H62 Si6'
_chemical_formula_sum            'C34 H62 Si6'
_chemical_formula_weight         639.37

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

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

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

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

_cell_length_a                   11.3903(3)
_cell_length_b                   17.1318(4)
_cell_length_c                   19.8809(5)
_cell_angle_alpha                90
_cell_angle_beta                 90.9660(10)
_cell_angle_gamma                90
_cell_volume                     3878.93(17)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    5735
_cell_measurement_theta_min      2.37
_cell_measurement_theta_max      28.11

_exptl_crystal_description       block
_exptl_crystal_colour            orange
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.095
_exptl_crystal_F_000             1400
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.050
_exptl_absorpt_coefficient_mu    0.236
_shelx_estimated_absorpt_T_min   0.954
_shelx_estimated_absorpt_T_max   0.988
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.6619
_exptl_absorpt_correction_T_max  0.7466
_exptl_absorpt_process_details   'SADABS Sheldrick 1996'

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'Bruker TXS fine-focus rotating anode'
_diffrn_radiation_monochromator  'Bruker Helios multilayer confocal mirror'
_diffrn_measurement_device_type  'Bruker APEXII CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean 8.333
_diffrn_reflns_number            28627
_diffrn_reflns_av_unetI/netI     0.0491
_diffrn_reflns_av_R_equivalents  0.0462
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       14
_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         1.569
_diffrn_reflns_theta_max         27.494
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             8901
_reflns_number_gt                6796
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

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

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0463P)²+1.3162P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         8901
_refine_ls_number_parameters     379
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0593
_refine_ls_R_factor_gt           0.0386
_refine_ls_wR_factor_ref         0.1006
_refine_ls_wR_factor_gt          0.0904
_refine_ls_goodness_of_fit_ref   1.010
_refine_ls_restrained_S_all      1.010
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Si1 Si 0.70151(4) 0.26186(3) 0.28910(2) 0.01282(11) Uani 1 1 d . . . . .
Si2 Si 0.67359(5) 0.25148(3) 0.39642(3) 0.02143(13) Uani 1 1 d . . . . .
Si3 Si 0.98160(4) 0.24489(3) 0.26116(3) 0.01740(12) Uani 1 1 d . . . . .
Si4 Si 0.80946(4) 0.10944(3) 0.22344(3) 0.01659(12) Uani 1 1 d . . . . .
Si5 Si 0.63335(4) 0.42856(3) 0.23157(3) 0.01573(11) Uani 1 1 d . . . . .
Si6 Si 0.44980(4) 0.29542(3) 0.21418(3) 0.01435(11) Uani 1 1 d . . . . .
C1 C 0.82418(14) 0.21951(10) 0.23559(9) 0.0136(3) Uani 1 1 d . . . . .
C2 C 0.80049(15) 0.26460(10) 0.16736(9) 0.0151(4) Uani 1 1 d . . . . .
H1 H 0.8487 0.3127 0.1671 0.018 Uiso 1 1 calc R U . . .
H2 H 0.8257 0.2314 0.1295 0.018 Uiso 1 1 calc R U . . .
C3 C 0.67093(15) 0.28681(10) 0.15644(9) 0.0142(3) Uani 1 1 d . . . . .
H3 H 0.6267 0.2404 0.1405 0.017 Uiso 1 1 calc R U . . .
H4 H 0.6650 0.3273 0.1210 0.017 Uiso 1 1 calc R U . . .
C4 C 0.61368(14) 0.31850(10) 0.22259(8) 0.0119(3) Uani 1 1 d . . . . .
C5 C 1.08020(16) 0.23600(13) 0.18652(10) 0.0258(4) Uani 1 1 d . . . . .
H5 H 1.0375 0.2526 0.1458 0.039 Uiso 1 1 calc R U . . .
H6 H 1.1050 0.1816 0.1815 0.039 Uiso 1 1 calc R U . . .
H7 H 1.1495 0.2692 0.1934 0.039 Uiso 1 1 calc R U . . .
C6 C 1.04574(17) 0.18048(12) 0.32834(10) 0.0253(4) Uani 1 1 d . . . . .
H8 H 1.1203 0.2026 0.3446 0.038 Uiso 1 1 calc R U . . .
H9 H 1.0594 0.1283 0.3099 0.038 Uiso 1 1 calc R U . . .
H10 H 0.9910 0.1768 0.3657 0.038 Uiso 1 1 calc R U . . .
C7 C 0.99914(17) 0.34936(11) 0.28756(10) 0.0239(4) Uani 1 1 d . . . . .
H11 H 0.9313 0.3652 0.3140 0.036 Uiso 1 1 calc R U . . .
H12 H 1.0043 0.3825 0.2475 0.036 Uiso 1 1 calc R U . . .
H13 H 1.0710 0.3550 0.3149 0.036 Uiso 1 1 calc R U . . .
C8 C 0.93022(18) 0.06969(12) 0.16995(12) 0.0319(5) Uani 1 1 d . . . . .
H14 H 0.9114 0.0160 0.1567 0.048 Uiso 1 1 calc R U . . .
H15 H 1.0044 0.0703 0.1957 0.048 Uiso 1 1 calc R U . . .
H16 H 0.9378 0.1021 0.1296 0.048 Uiso 1 1 calc R U . . .
C9 C 0.81152(19) 0.05537(11) 0.30500(10) 0.0276(5) Uani 1 1 d . . . . .
H17 H 0.7471 0.0738 0.3329 0.041 Uiso 1 1 calc R U . . .
H18 H 0.8866 0.0645 0.3285 0.041 Uiso 1 1 calc R U . . .
H19 H 0.8020 -0.0006 0.2963 0.041 Uiso 1 1 calc R U . . .
C10 C 0.67074(17) 0.08044(11) 0.17890(10) 0.0224(4) Uani 1 1 d . . . . .
H20 H 0.6768 0.0261 0.1640 0.034 Uiso 1 1 calc R U . . .
H21 H 0.6579 0.1143 0.1397 0.034 Uiso 1 1 calc R U . . .
H22 H 0.6047 0.0857 0.2095 0.034 Uiso 1 1 calc R U . . .
C11 C 0.77965(17) 0.46536(11) 0.20444(12) 0.0285(5) Uani 1 1 d . . . . .
H23 H 0.7793 0.5226 0.2044 0.043 Uiso 1 1 calc R U . . .
H24 H 0.7956 0.4463 0.1590 0.043 Uiso 1 1 calc R U . . .
H25 H 0.8408 0.4465 0.2357 0.043 Uiso 1 1 calc R U . . .
C12 C 0.52943(18) 0.48416(11) 0.17531(10) 0.0235(4) Uani 1 1 d . . . . .
H26 H 0.4485 0.4740 0.1888 0.035 Uiso 1 1 calc R U . . .
H27 H 0.5395 0.4674 0.1286 0.035 Uiso 1 1 calc R U . . .
H28 H 0.5460 0.5401 0.1791 0.035 Uiso 1 1 calc R U . . .
C13 C 0.61420(19) 0.46218(11) 0.32006(10) 0.0252(4) Uani 1 1 d . . . . .
H29 H 0.6035 0.5189 0.3206 0.038 Uiso 1 1 calc R U . . .
H30 H 0.6840 0.4484 0.3470 0.038 Uiso 1 1 calc R U . . .
H31 H 0.5450 0.4369 0.3390 0.038 Uiso 1 1 calc R U . . .
C14 C 0.42066(16) 0.18821(10) 0.21892(10) 0.0201(4) Uani 1 1 d . . . . .
H32 H 0.4666 0.1656 0.2562 0.030 Uiso 1 1 calc R U . . .
H33 H 0.4432 0.1634 0.1766 0.030 Uiso 1 1 calc R U . . .
H34 H 0.3369 0.1794 0.2264 0.030 Uiso 1 1 calc R U . . .
C15 C 0.36119(16) 0.34693(11) 0.27928(10) 0.0209(4) Uani 1 1 d . . . . .
H35 H 0.2803 0.3275 0.2776 0.031 Uiso 1 1 calc R U . . .
H36 H 0.3615 0.4032 0.2703 0.031 Uiso 1 1 calc R U . . .
H37 H 0.3955 0.3370 0.3240 0.031 Uiso 1 1 calc R U . . .
C16 C 0.39125(16) 0.32250(12) 0.12822(10) 0.0225(4) Uani 1 1 d . . . . .
H38 H 0.4460 0.3045 0.0940 0.034 Uiso 1 1 calc R U . . .
H39 H 0.3827 0.3793 0.1252 0.034 Uiso 1 1 calc R U . . .
H40 H 0.3146 0.2977 0.1207 0.034 Uiso 1 1 calc R U . . .
C17 C 0.78283(16) 0.20103(11) 0.45480(9) 0.0200(4) Uani 1 1 d . . . . .
C18 C 0.89299(16) 0.23311(12) 0.47322(9) 0.0222(4) Uani 1 1 d . . . . .
C19 C 0.97200(17) 0.19003(13) 0.51289(10) 0.0268(5) Uani 1 1 d . . . . .
H41 H 1.0462 0.2123 0.5240 0.032 Uiso 1 1 calc R U . . .
C20 C 0.94630(19) 0.11661(13) 0.53642(10) 0.0294(5) Uani 1 1 d . . . . .
C21 C 0.83583(19) 0.08621(12) 0.52071(10) 0.0285(5) Uani 1 1 d . . . . .
H42 H 0.8155 0.0362 0.5375 0.034 Uiso 1 1 calc R U . . .
C22 C 0.75435(18) 0.12662(12) 0.48137(10) 0.0231(4) Uani 1 1 d . . . . .
C23 C 0.93357(17) 0.31300(13) 0.45255(11) 0.0265(4) Uani 1 1 d . . . . .
H43 H 0.9380 0.3470 0.4922 0.040 Uiso 1 1 calc R U . . .
H44 H 0.8778 0.3350 0.4196 0.040 Uiso 1 1 calc R U . . .
H45 H 1.0113 0.3091 0.4324 0.040 Uiso 1 1 calc R U . . .
C24 C 1.0334(2) 0.07080(15) 0.57900(11) 0.0403(6) Uani 1 1 d . . . . .
H46 H 1.1133 0.0882 0.5692 0.060 Uiso 1 1 calc R U . . .
H47 H 1.0259 0.0151 0.5686 0.060 Uiso 1 1 calc R U . . .
H48 H 1.0175 0.0794 0.6267 0.060 Uiso 1 1 calc R U . . .
C25 C 0.63614(19) 0.08939(12) 0.46881(11) 0.0295(5) Uani 1 1 d . . . . .
H49 H 0.6364 0.0364 0.4873 0.044 Uiso 1 1 calc R U . . .
H50 H 0.6198 0.0872 0.4203 0.044 Uiso 1 1 calc R U . . .
H51 H 0.5753 0.1204 0.4907 0.044 Uiso 1 1 calc R U . . .
C26 C 0.53987(15) 0.29033(11) 0.44137(9) 0.0170(4) Uani 1 1 d . . . . .
C27 C 0.55309(16) 0.35649(11) 0.48389(9) 0.0174(4) Uani 1 1 d . . . . .
C28 C 0.45696(16) 0.38720(11) 0.51696(9) 0.0193(4) Uani 1 1 d . . . . .
H52 H 0.4677 0.4316 0.5451 0.023 Uiso 1 1 calc R U . . .
C29 C 0.34531(16) 0.35473(11) 0.51000(10) 0.0200(4) Uani 1 1 d . . . . .
C30 C 0.33318(16) 0.28931(11) 0.47008(10) 0.0197(4) Uani 1 1 d . . . . .
H53 H 0.2580 0.2657 0.4657 0.024 Uiso 1 1 calc R U . . .
C31 C 0.42687(16) 0.25642(11) 0.43591(9) 0.0181(4) Uani 1 1 d . . . . .
C32 C 0.67141(16) 0.39418(12) 0.49554(10) 0.0227(4) Uani 1 1 d . . . . .
H54 H 0.6616 0.4428 0.5207 0.034 Uiso 1 1 calc R U . . .
H55 H 0.7071 0.4056 0.4521 0.034 Uiso 1 1 calc R U . . .
H56 H 0.7223 0.3586 0.5213 0.034 Uiso 1 1 calc R U . . .
C33 C 0.24161(17) 0.38919(13) 0.54578(11) 0.0289(5) Uani 1 1 d . . . . .
H57 H 0.2064 0.4306 0.5180 0.043 Uiso 1 1 calc R U . . .
H58 H 0.2679 0.4111 0.5890 0.043 Uiso 1 1 calc R U . . .
H59 H 0.1832 0.3483 0.5535 0.043 Uiso 1 1 calc R U . . .
C34 C 0.40066(17) 0.18420(12) 0.39509(10) 0.0253(4) Uani 1 1 d . . . . .
H60 H 0.3755 0.1422 0.4250 0.038 Uiso 1 1 calc R U . . .
H61 H 0.4715 0.1680 0.3715 0.038 Uiso 1 1 calc R U . . .
H62 H 0.3379 0.1955 0.3622 0.038 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Si1 C4 1.9095(17) . ?
Si1 C1 1.9133(17) . ?
Si1 Si2 2.1697(7) . ?
Si2 C17 1.8958(19) . ?
Si2 C26 1.8992(18) . ?
Si3 C6 1.871(2) . ?
Si3 C7 1.875(2) . ?
Si3 C5 1.8823(19) . ?
Si3 C1 1.9059(18) . ?
Si4 C10 1.866(2) . ?
Si4 C9 1.867(2) . ?
Si4 C8 1.880(2) . ?
Si4 C1 1.9080(18) . ?
Si5 C13 1.867(2) . ?
Si5 C11 1.870(2) . ?
Si5 C12 1.8748(19) . ?
Si5 C4 1.9068(17) . ?
Si6 C14 1.8690(18) . ?
Si6 C15 1.8753(19) . ?
Si6 C16 1.882(2) . ?
Si6 C4 1.9126(17) . ?
C1 C2 1.580(2) . ?
C2 C3 1.536(2) . ?
C3 C4 1.574(2) . ?
C17 C18 1.413(3) . ?
C17 C22 1.420(3) . ?
C18 C19 1.397(3) . ?
C18 C23 1.504(3) . ?
C19 C20 1.375(3) . ?
C20 C21 1.392(3) . ?
C20 C24 1.513(3) . ?
C21 C22 1.388(3) . ?
C22 C25 1.507(3) . ?
C26 C31 1.415(3) . ?
C26 C27 1.420(3) . ?
C27 C28 1.390(2) . ?
C27 C32 1.509(3) . ?
C28 C29 1.393(3) . ?
C29 C30 1.379(3) . ?
C29 C33 1.509(3) . ?
C30 C31 1.394(2) . ?
C31 C34 1.507(3) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C4 Si1 C1 100.76(7) . . ?
C4 Si1 Si2 129.70(6) . . ?
C1 Si1 Si2 129.51(6) . . ?
C17 Si2 C26 113.27(8) . . ?
C17 Si2 Si1 122.26(6) . . ?
C26 Si2 Si1 124.47(6) . . ?
C6 Si3 C7 108.95(9) . . ?
C6 Si3 C5 106.50(9) . . ?
C7 Si3 C5 103.64(9) . . ?
C6 Si3 C1 114.21(9) . . ?
C7 Si3 C1 112.82(8) . . ?
C5 Si3 C1 110.02(9) . . ?
C10 Si4 C9 106.15(9) . . ?
C10 Si4 C8 104.88(10) . . ?
C9 Si4 C8 108.23(10) . . ?
C10 Si4 C1 113.28(8) . . ?
C9 Si4 C1 112.37(9) . . ?
C8 Si4 C1 111.47(9) . . ?
C13 Si5 C11 106.66(10) . . ?
C13 Si5 C12 108.82(9) . . ?
C11 Si5 C12 102.32(9) . . ?
C13 Si5 C4 112.20(8) . . ?
C11 Si5 C4 114.23(8) . . ?
C12 Si5 C4 112.00(8) . . ?
C14 Si6 C15 109.24(9) . . ?
C14 Si6 C16 103.15(9) . . ?
C15 Si6 C16 108.91(9) . . ?
C14 Si6 C4 111.88(8) . . ?
C15 Si6 C4 112.22(8) . . ?
C16 Si6 C4 111.03(8) . . ?
C2 C1 Si3 105.29(11) . . ?
C2 C1 Si4 111.17(12) . . ?
Si3 C1 Si4 109.85(8) . . ?
C2 C1 Si1 100.15(11) . . ?
Si3 C1 Si1 117.24(9) . . ?
Si4 C1 Si1 112.44(9) . . ?
C3 C2 C1 113.09(14) . . ?
C2 C3 C4 112.20(14) . . ?
C3 C4 Si5 111.69(11) . . ?
C3 C4 Si1 100.59(10) . . ?
Si5 C4 Si1 112.23(9) . . ?
C3 C4 Si6 105.84(11) . . ?
Si5 C4 Si6 109.00(8) . . ?
Si1 C4 Si6 117.04(9) . . ?
C18 C17 C22 117.42(17) . . ?
C18 C17 Si2 123.53(15) . . ?
C22 C17 Si2 119.05(15) . . ?
C19 C18 C17 120.11(19) . . ?
C19 C18 C23 115.91(18) . . ?
C17 C18 C23 123.98(18) . . ?
C20 C19 C18 122.4(2) . . ?
C19 C20 C21 117.55(19) . . ?
C19 C20 C24 121.6(2) . . ?
C21 C20 C24 120.9(2) . . ?
C22 C21 C20 122.2(2) . . ?
C21 C22 C17 120.17(19) . . ?
C21 C22 C25 117.99(19) . . ?
C17 C22 C25 121.84(18) . . ?
C31 C26 C27 117.42(16) . . ?
C31 C26 Si2 123.77(14) . . ?
C27 C26 Si2 118.81(13) . . ?
C28 C27 C26 120.47(17) . . ?
C28 C27 C32 118.30(17) . . ?
C26 C27 C32 121.21(16) . . ?
C27 C28 C29 121.81(17) . . ?
C30 C29 C28 117.66(17) . . ?
C30 C29 C33 121.17(17) . . ?
C28 C29 C33 121.16(18) . . ?
C29 C30 C31 122.62(17) . . ?
C30 C31 C26 119.98(17) . . ?
C30 C31 C34 116.63(17) . . ?
C26 C31 C34 123.38(16) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Si3 C1 C2 C3 -150.88(12) . . . . ?
Si4 C1 C2 C3 90.21(15) . . . . ?
Si1 C1 C2 C3 -28.81(16) . . . . ?
C1 C2 C3 C4 42.34(19) . . . . ?
C2 C3 C4 Si5 88.74(15) . . . . ?
C2 C3 C4 Si1 -30.50(15) . . . . ?
C2 C3 C4 Si6 -152.77(12) . . . . ?
C26 Si2 C17 C18 -108.20(16) . . . . ?
Si1 Si2 C17 C18 72.16(17) . . . . ?
C26 Si2 C17 C22 72.44(16) . . . . ?
Si1 Si2 C17 C22 -107.20(14) . . . . ?
C22 C17 C18 C19 3.7(3) . . . . ?
Si2 C17 C18 C19 -175.69(14) . . . . ?
C22 C17 C18 C23 -176.49(17) . . . . ?
Si2 C17 C18 C23 4.1(3) . . . . ?
C17 C18 C19 C20 -1.2(3) . . . . ?
C23 C18 C19 C20 178.98(18) . . . . ?
C18 C19 C20 C21 -1.5(3) . . . . ?
C18 C19 C20 C24 179.65(18) . . . . ?
C19 C20 C21 C22 1.6(3) . . . . ?
C24 C20 C21 C22 -179.53(18) . . . . ?
C20 C21 C22 C17 0.9(3) . . . . ?
C20 C21 C22 C25 -178.46(18) . . . . ?
C18 C17 C22 C21 -3.6(3) . . . . ?
Si2 C17 C22 C21 175.84(14) . . . . ?
C18 C17 C22 C25 175.81(17) . . . . ?
Si2 C17 C22 C25 -4.8(2) . . . . ?
C17 Si2 C26 C31 -107.30(17) . . . . ?
Si1 Si2 C26 C31 72.33(17) . . . . ?
C17 Si2 C26 C27 71.69(17) . . . . ?
Si1 Si2 C26 C27 -108.68(14) . . . . ?
C31 C26 C27 C28 -1.8(3) . . . . ?
Si2 C26 C27 C28 179.18(14) . . . . ?
C31 C26 C27 C32 176.97(17) . . . . ?
Si2 C26 C27 C32 -2.1(2) . . . . ?
C26 C27 C28 C29 0.2(3) . . . . ?
C32 C27 C28 C29 -178.60(18) . . . . ?
C27 C28 C29 C30 1.5(3) . . . . ?
C27 C28 C29 C33 -179.47(18) . . . . ?
C28 C29 C30 C31 -1.5(3) . . . . ?
C33 C29 C30 C31 179.43(18) . . . . ?
C29 C30 C31 C26 -0.1(3) . . . . ?
C29 C30 C31 C34 179.04(18) . . . . ?
C27 C26 C31 C30 1.7(3) . . . . ?
Si2 C26 C31 C30 -179.27(14) . . . . ?
C27 C26 C31 C34 -177.35(18) . . . . ?
Si2 C26 C31 C34 1.7(3) . . . . ?

_refine_diff_density_max         0.415
_refine_diff_density_min         -0.323
_refine_diff_density_rms         0.058

_shelxl_version_number           2014-3



_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: diethyl ether'
####################################################################### 
# 
# 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_si366b
_database_code_depnum_ccdc_archive 'CCDC 1558531'
_audit_update_record             
;
2017-06-26 deposited with the CCDC.
2017-08-11 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014
_chemical_name_systematic        disilenylthiophene
_chemical_name_common            ?
_chemical_melting_point          390
_chemical_formula_moiety         'C29 H54 S Si6'
_chemical_formula_sum            'C29 H54 S Si6'
_chemical_formula_weight         603.32

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

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

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

_cell_length_a                   13.9334(13)
_cell_length_b                   16.8620(16)
_cell_length_c                   14.7774(14)
_cell_angle_alpha                90
_cell_angle_beta                 90.0935(10)
_cell_angle_gamma                90
_cell_volume                     3471.9(6)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9917
_cell_measurement_theta_min      2.34
_cell_measurement_theta_max      27.79

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.154
_exptl_crystal_F_000             1312
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.100
_exptl_absorpt_coefficient_mu    0.318
_shelx_estimated_absorpt_T_min   0.911
_shelx_estimated_absorpt_T_max   0.969
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.6173
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_process_details   'SADABS Sheldrick 1996'

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'Bruker TXS fine-focus rotating anode'
_diffrn_radiation_monochromator  'Bruker Helios multilayer confocal mirror'
_diffrn_measurement_device_type  'Bruker APEXII CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean 8.333
_diffrn_reflns_number            17762
_diffrn_reflns_av_unetI/netI     0.0250
_diffrn_reflns_av_R_equivalents  0.0222
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         1.832
_diffrn_reflns_theta_max         25.999
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             6781
_reflns_number_gt                6241
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

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

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0412P)²+2.3712P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         6781
_refine_ls_number_parameters     340
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0332
_refine_ls_R_factor_gt           0.0304
_refine_ls_wR_factor_ref         0.0839
_refine_ls_wR_factor_gt          0.0811
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_restrained_S_all      1.018
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Si1 Si 0.30048(3) 0.11418(2) 0.19384(2) 0.01221(9) Uani 1 1 d . . . . .
Si2 Si 0.18265(3) 0.15751(3) 0.27749(3) 0.01610(10) Uani 1 1 d . . . . .
Si3 Si 0.33198(3) 0.20668(3) -0.00139(3) 0.01605(10) Uani 1 1 d . . . . .
Si4 Si 0.21068(3) 0.04906(2) 0.01352(3) 0.01426(10) Uani 1 1 d . . . . .
Si5 Si 0.48633(3) 0.17962(3) 0.29564(3) 0.01614(10) Uani 1 1 d . . . . .
Si6 Si 0.44537(3) -0.00424(3) 0.29158(3) 0.01892(10) Uani 1 1 d . . . . .
S1 S -0.03877(3) 0.12124(3) 0.26199(4) 0.03170(12) Uani 1 1 d . . . . .
C1 C 0.06184(10) 0.17242(9) 0.22617(10) 0.0154(3) Uani 1 1 d . . . . .
C2 C 0.03396(11) 0.22734(10) 0.16297(10) 0.0222(3) Uani 1 1 d . . . . .
H1 H 0.0779 0.2625 0.1346 0.027 Uiso 1 1 calc R U . . .
C3 C -0.06580(11) 0.22750(11) 0.14321(11) 0.0250(4) Uani 1 1 d . . . . .
H2 H -0.0951 0.2619 0.1004 0.030 Uiso 1 1 calc R U . . .
C4 C -0.11405(12) 0.17325(11) 0.19213(13) 0.0282(4) Uani 1 1 d . . . . .
H3 H -0.1814 0.1649 0.1884 0.034 Uiso 1 1 calc R U . . .
C5 C 0.31190(10) 0.11118(9) 0.06571(9) 0.0135(3) Uani 1 1 d . . . . .
C6 C 0.40748(10) 0.06122(10) 0.06015(10) 0.0186(3) Uani 1 1 d . . . . .
H4 H 0.3923 0.0042 0.0670 0.022 Uiso 1 1 calc R U . . .
H5 H 0.4373 0.0689 0.0000 0.022 Uiso 1 1 calc R U . . .
C7 C 0.47898(10) 0.08649(10) 0.13465(10) 0.0198(3) Uani 1 1 d . . . . .
H6 H 0.5080 0.1381 0.1180 0.024 Uiso 1 1 calc R U . . .
H7 H 0.5312 0.0468 0.1386 0.024 Uiso 1 1 calc R U . . .
C8 C 0.42892(10) 0.09434(9) 0.23024(9) 0.0143(3) Uani 1 1 d . . . . .
C9 C 0.24522(12) 0.28685(10) 0.02836(11) 0.0254(4) Uani 1 1 d . . . . .
H8 H 0.2483 0.2972 0.0936 0.038 Uiso 1 1 calc R U . . .
H9 H 0.1801 0.2702 0.0120 0.038 Uiso 1 1 calc R U . . .
H10 H 0.2617 0.3353 -0.0048 0.038 Uiso 1 1 calc R U . . .
C10 C 0.32402(12) 0.18561(11) -0.12590(10) 0.0249(4) Uani 1 1 d . . . . .
H11 H 0.2611 0.1626 -0.1399 0.037 Uiso 1 1 calc R U . . .
H12 H 0.3746 0.1481 -0.1430 0.037 Uiso 1 1 calc R U . . .
H13 H 0.3322 0.2351 -0.1598 0.037 Uiso 1 1 calc R U . . .
C11 C 0.45558(13) 0.24977(13) 0.00831(12) 0.0326(4) Uani 1 1 d . . . . .
H14 H 0.4602 0.2972 -0.0298 0.049 Uiso 1 1 calc R U . . .
H15 H 0.5029 0.2105 -0.0117 0.049 Uiso 1 1 calc R U . . .
H16 H 0.4683 0.2641 0.0715 0.049 Uiso 1 1 calc R U . . .
C12 C 0.25896(12) -0.00995(10) -0.08408(11) 0.0226(3) Uani 1 1 d . . . . .
H17 H 0.3030 -0.0507 -0.0614 0.034 Uiso 1 1 calc R U . . .
H18 H 0.2934 0.0254 -0.1255 0.034 Uiso 1 1 calc R U . . .
H19 H 0.2057 -0.0354 -0.1163 0.034 Uiso 1 1 calc R U . . .
C13 C 0.10576(11) 0.10838(10) -0.02812(11) 0.0236(3) Uani 1 1 d . . . . .
H20 H 0.0610 0.0734 -0.0602 0.035 Uiso 1 1 calc R U . . .
H21 H 0.1284 0.1498 -0.0694 0.035 Uiso 1 1 calc R U . . .
H22 H 0.0731 0.1329 0.0234 0.035 Uiso 1 1 calc R U . . .
C14 C 0.15926(12) -0.02616(10) 0.09313(11) 0.0229(3) Uani 1 1 d . . . . .
H23 H 0.1200 0.0007 0.1388 0.034 Uiso 1 1 calc R U . . .
H24 H 0.2116 -0.0549 0.1230 0.034 Uiso 1 1 calc R U . . .
H25 H 0.1193 -0.0637 0.0592 0.034 Uiso 1 1 calc R U . . .
C15 C 0.44053(12) 0.28037(10) 0.26339(12) 0.0255(4) Uani 1 1 d . . . . .
H26 H 0.3702 0.2801 0.2641 0.038 Uiso 1 1 calc R U . . .
H27 H 0.4632 0.2938 0.2025 0.038 Uiso 1 1 calc R U . . .
H28 H 0.4643 0.3198 0.3067 0.038 Uiso 1 1 calc R U . . .
C16 C 0.61904(11) 0.18084(11) 0.27260(12) 0.0281(4) Uani 1 1 d . . . . .
H29 H 0.6489 0.2246 0.3060 0.042 Uiso 1 1 calc R U . . .
H30 H 0.6300 0.1881 0.2076 0.042 Uiso 1 1 calc R U . . .
H31 H 0.6474 0.1305 0.2921 0.042 Uiso 1 1 calc R U . . .
C17 C 0.46924(12) 0.17052(10) 0.42074(10) 0.0233(3) Uani 1 1 d . . . . .
H32 H 0.4906 0.2194 0.4504 0.035 Uiso 1 1 calc R U . . .
H33 H 0.5070 0.1257 0.4435 0.035 Uiso 1 1 calc R U . . .
H34 H 0.4012 0.1617 0.4339 0.035 Uiso 1 1 calc R U . . .
C18 C 0.57483(12) -0.02151(11) 0.32058(11) 0.0272(4) Uani 1 1 d . . . . .
H35 H 0.5946 0.0156 0.3681 0.041 Uiso 1 1 calc R U . . .
H36 H 0.6144 -0.0132 0.2666 0.041 Uiso 1 1 calc R U . . .
H37 H 0.5832 -0.0760 0.3422 0.041 Uiso 1 1 calc R U . . .
C19 C 0.41020(17) -0.08827(11) 0.21570(16) 0.0440(5) Uani 1 1 d . . . . .
H38 H 0.4228 -0.1387 0.2464 0.066 Uiso 1 1 calc R U . . .
H39 H 0.4477 -0.0857 0.1597 0.066 Uiso 1 1 calc R U . . .
H40 H 0.3417 -0.0843 0.2012 0.066 Uiso 1 1 calc R U . . .
C20 C 0.37587(13) -0.01394(12) 0.39886(13) 0.0326(4) Uani 1 1 d . . . . .
H41 H 0.3115 0.0083 0.3903 0.049 Uiso 1 1 calc R U . . .
H42 H 0.4090 0.0148 0.4473 0.049 Uiso 1 1 calc R U . . .
H43 H 0.3706 -0.0701 0.4152 0.049 Uiso 1 1 calc R U . . .
C21 C 0.17430(10) 0.12985(9) 0.40112(9) 0.0146(3) Uani 1 1 d . . . . .
C22 C 0.19862(10) 0.18698(9) 0.46747(10) 0.0153(3) Uani 1 1 d . . . . .
C23 C 0.19477(10) 0.16709(9) 0.55905(10) 0.0172(3) Uani 1 1 d . . . . .
H44 H 0.2133 0.2055 0.6028 0.021 Uiso 1 1 calc R U . . .
C24 C 0.16472(10) 0.09293(10) 0.58800(10) 0.0187(3) Uani 1 1 d . . . . .
C25 C 0.13824(11) 0.03756(10) 0.52290(10) 0.0186(3) Uani 1 1 d . . . . .
H45 H 0.1165 -0.0132 0.5418 0.022 Uiso 1 1 calc R U . . .
C26 C 0.14272(10) 0.05438(9) 0.43047(10) 0.0164(3) Uani 1 1 d . . . . .
C27 C 0.22769(12) 0.27068(9) 0.44316(11) 0.0213(3) Uani 1 1 d . . . . .
H46 H 0.2311 0.3029 0.4982 0.032 Uiso 1 1 calc R U . . .
H47 H 0.1801 0.2935 0.4017 0.032 Uiso 1 1 calc R U . . .
H48 H 0.2907 0.2699 0.4138 0.032 Uiso 1 1 calc R U . . .
C28 C 0.16122(12) 0.07299(11) 0.68760(10) 0.0264(4) Uani 1 1 d . . . . .
H49 H 0.0951 0.0780 0.7094 0.040 Uiso 1 1 calc R U . . .
H50 H 0.2028 0.1095 0.7212 0.040 Uiso 1 1 calc R U . . .
H51 H 0.1835 0.0184 0.6968 0.040 Uiso 1 1 calc R U . . .
C29 C 0.11523(12) -0.01134(10) 0.36580(11) 0.0216(3) Uani 1 1 d . . . . .
H52 H 0.1400 -0.0620 0.3885 0.032 Uiso 1 1 calc R U . . .
H53 H 0.1427 -0.0005 0.3061 0.032 Uiso 1 1 calc R U . . .
H54 H 0.0452 -0.0141 0.3609 0.032 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Si1 C8 1.8976(14) . ?
Si1 C5 1.9011(14) . ?
Si1 Si2 2.1826(6) . ?
Si2 C1 1.8621(15) . ?
Si2 C21 1.8893(15) . ?
Si3 C9 1.8665(17) . ?
Si3 C11 1.8745(17) . ?
Si3 C10 1.8770(16) . ?
Si3 C5 1.9120(15) . ?
Si4 C14 1.8733(17) . ?
Si4 C13 1.8743(16) . ?
Si4 C12 1.8778(16) . ?
Si4 C5 1.9176(15) . ?
Si5 C17 1.8706(16) . ?
Si5 C15 1.8760(18) . ?
Si5 C16 1.8809(16) . ?
Si5 C8 1.9077(15) . ?
Si6 C20 1.8662(18) . ?
Si6 C19 1.872(2) . ?
Si6 C18 1.8760(17) . ?
Si6 C8 1.9071(16) . ?
S1 C4 1.7121(18) . ?
S1 C1 1.7300(15) . ?
C1 C2 1.371(2) . ?
C2 C3 1.420(2) . ?
C3 C4 1.347(3) . ?
C5 C6 1.5781(19) . ?
C6 C7 1.544(2) . ?
C7 C8 1.5820(19) . ?
C21 C22 1.415(2) . ?
C21 C26 1.415(2) . ?
C22 C23 1.395(2) . ?
C22 C27 1.512(2) . ?
C23 C24 1.387(2) . ?
C24 C25 1.390(2) . ?
C24 C28 1.511(2) . ?
C25 C26 1.396(2) . ?
C26 C29 1.512(2) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C8 Si1 C5 101.37(6) . . ?
C8 Si1 Si2 127.48(5) . . ?
C5 Si1 Si2 129.58(5) . . ?
C1 Si2 C21 111.72(6) . . ?
C1 Si2 Si1 119.66(5) . . ?
C21 Si2 Si1 120.83(5) . . ?
C9 Si3 C11 107.25(9) . . ?
C9 Si3 C10 109.31(8) . . ?
C11 Si3 C10 101.61(8) . . ?
C9 Si3 C5 113.11(7) . . ?
C11 Si3 C5 114.97(8) . . ?
C10 Si3 C5 109.90(7) . . ?
C14 Si4 C13 105.58(8) . . ?
C14 Si4 C12 105.15(8) . . ?
C13 Si4 C12 108.11(7) . . ?
C14 Si4 C5 113.52(7) . . ?
C13 Si4 C5 114.41(7) . . ?
C12 Si4 C5 109.53(7) . . ?
C17 Si5 C15 106.35(8) . . ?
C17 Si5 C16 107.85(8) . . ?
C15 Si5 C16 106.15(8) . . ?
C17 Si5 C8 112.64(7) . . ?
C15 Si5 C8 114.32(7) . . ?
C16 Si5 C8 109.15(7) . . ?
C20 Si6 C19 107.87(11) . . ?
C20 Si6 C18 107.00(8) . . ?
C19 Si6 C18 105.67(9) . . ?
C20 Si6 C8 114.71(7) . . ?
C19 Si6 C8 110.12(8) . . ?
C18 Si6 C8 111.02(7) . . ?
C4 S1 C1 93.20(8) . . ?
C2 C1 S1 108.45(11) . . ?
C2 C1 Si2 128.58(12) . . ?
S1 C1 Si2 122.71(9) . . ?
C1 C2 C3 114.69(15) . . ?
C4 C3 C2 112.19(15) . . ?
C3 C4 S1 111.46(12) . . ?
C6 C5 Si1 97.94(9) . . ?
C6 C5 Si3 107.36(10) . . ?
Si1 C5 Si3 120.44(8) . . ?
C6 C5 Si4 107.92(10) . . ?
Si1 C5 Si4 110.64(7) . . ?
Si3 C5 Si4 111.08(7) . . ?
C7 C6 C5 111.06(12) . . ?
C6 C7 C8 112.02(12) . . ?
C7 C8 Si1 100.29(9) . . ?
C7 C8 Si6 107.38(10) . . ?
Si1 C8 Si6 113.64(7) . . ?
C7 C8 Si5 109.29(10) . . ?
Si1 C8 Si5 113.90(8) . . ?
Si6 C8 Si5 111.49(7) . . ?
C22 C21 C26 118.29(13) . . ?
C22 C21 Si2 119.13(11) . . ?
C26 C21 Si2 122.56(11) . . ?
C23 C22 C21 119.92(14) . . ?
C23 C22 C27 117.74(13) . . ?
C21 C22 C27 122.33(13) . . ?
C24 C23 C22 121.87(14) . . ?
C23 C24 C25 118.18(14) . . ?
C23 C24 C28 120.77(14) . . ?
C25 C24 C28 121.05(15) . . ?
C24 C25 C26 121.88(15) . . ?
C25 C26 C21 119.81(14) . . ?
C25 C26 C29 117.23(14) . . ?
C21 C26 C29 122.95(13) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C4 S1 C1 C2 0.39(13) . . . . ?
C4 S1 C1 Si2 175.09(10) . . . . ?
C21 Si2 C1 C2 142.60(14) . . . . ?
Si1 Si2 C1 C2 -67.88(16) . . . . ?
C21 Si2 C1 S1 -30.96(12) . . . . ?
Si1 Si2 C1 S1 118.56(8) . . . . ?
S1 C1 C2 C3 -0.66(18) . . . . ?
Si2 C1 C2 C3 -174.95(12) . . . . ?
C1 C2 C3 C4 0.7(2) . . . . ?
C2 C3 C4 S1 -0.34(19) . . . . ?
C1 S1 C4 C3 -0.03(14) . . . . ?
Si1 C5 C6 C7 -39.58(14) . . . . ?
Si3 C5 C6 C7 85.84(13) . . . . ?
Si4 C5 C6 C7 -154.36(11) . . . . ?
C5 C6 C7 C8 46.16(18) . . . . ?
C6 C7 C8 Si1 -24.83(15) . . . . ?
C6 C7 C8 Si6 94.11(13) . . . . ?
C6 C7 C8 Si5 -144.82(11) . . . . ?
C5 Si1 C8 C7 0.56(11) . . . . ?
Si2 Si1 C8 C7 -166.16(8) . . . . ?
C5 Si1 C8 Si6 -113.70(8) . . . . ?
Si2 Si1 C8 Si6 79.58(9) . . . . ?
C5 Si1 C8 Si5 117.15(8) . . . . ?
Si2 Si1 C8 Si5 -49.57(10) . . . . ?
C1 Si2 C21 C22 -106.12(12) . . . . ?
Si1 Si2 C21 C22 104.76(11) . . . . ?
C1 Si2 C21 C26 72.59(13) . . . . ?
Si1 Si2 C21 C26 -76.52(13) . . . . ?
C26 C21 C22 C23 2.5(2) . . . . ?
Si2 C21 C22 C23 -178.69(11) . . . . ?
C26 C21 C22 C27 -176.45(13) . . . . ?
Si2 C21 C22 C27 2.31(19) . . . . ?
C21 C22 C23 C24 -2.0(2) . . . . ?
C27 C22 C23 C24 177.03(14) . . . . ?
C22 C23 C24 C25 0.2(2) . . . . ?
C22 C23 C24 C28 -179.99(14) . . . . ?
C23 C24 C25 C26 1.1(2) . . . . ?
C28 C24 C25 C26 -178.77(14) . . . . ?
C24 C25 C26 C21 -0.5(2) . . . . ?
C24 C25 C26 C29 178.03(14) . . . . ?
C22 C21 C26 C25 -1.3(2) . . . . ?
Si2 C21 C26 C25 179.93(11) . . . . ?
C22 C21 C26 C29 -179.74(13) . . . . ?
Si2 C21 C26 C29 1.5(2) . . . . ?

_refine_diff_density_max         0.488
_refine_diff_density_min         -0.500
_refine_diff_density_rms         0.051

_shelxl_version_number           2014-3



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

data_si371a
_database_code_depnum_ccdc_archive 'CCDC 1558532'
_audit_update_record             
;
2017-06-26 deposited with the CCDC.
2017-08-11 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014
_chemical_name_systematic        bis(disilenyl)thiophene
_chemical_name_common            ?
_chemical_melting_point          472
_chemical_formula_moiety         'C54 H104 S Si12'
_chemical_formula_sum            'C54 H104 S Si12'
_chemical_formula_weight         1122.51

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

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

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   11.8362(12)
_cell_length_b                   17.6788(17)
_cell_length_c                   18.7605(18)
_cell_angle_alpha                84.1110(10)
_cell_angle_beta                 81.8700(10)
_cell_angle_gamma                89.7240(10)
_cell_volume                     3865.5(7)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9841
_cell_measurement_theta_min      2.38
_cell_measurement_theta_max      28.57

_exptl_crystal_description       plate
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    0.964
_exptl_crystal_F_000             1224
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.040
_exptl_absorpt_coefficient_mu    0.255
_shelx_estimated_absorpt_T_min   0.963
_shelx_estimated_absorpt_T_max   0.990
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.6850
_exptl_absorpt_correction_T_max  0.7458
_exptl_absorpt_process_details   'SADABS Sheldrick 1996'

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'Bruker TXS fine-focus rotating anode'
_diffrn_radiation_monochromator  'Bruker Helios multilayer confocal mirror'
_diffrn_measurement_device_type  'Bruker APEXII CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean 8.333
_diffrn_reflns_number            41666
_diffrn_reflns_av_unetI/netI     0.0224
_diffrn_reflns_av_R_equivalents  0.0177
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         1.514
_diffrn_reflns_theta_max         26.500
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measured_fraction_theta_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_point_group_measured_fraction_full 0.996
_reflns_number_total             15902
_reflns_number_gt                13622
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

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

_refine_special_details          ', SQUEEZE'
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0507P)²+0.6345P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         15902
_refine_ls_number_parameters     635
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0355
_refine_ls_R_factor_gt           0.0296
_refine_ls_wR_factor_ref         0.0844
_refine_ls_wR_factor_gt          0.0817
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_restrained_S_all      1.044
_refine_ls_shift/su_max          0.010
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Si1 Si 0.03458(3) 0.26092(2) 0.60714(2) 0.01392(7) Uani 1 1 d . . . . .
Si2 Si 0.14432(3) 0.26469(2) 0.50288(2) 0.01670(8) Uani 1 1 d . . . . .
Si3 Si -0.01153(3) 0.23926(2) 0.12548(2) 0.01621(8) Uani 1 1 d . . . . .
Si4 Si -0.09804(3) 0.24601(2) 0.23537(2) 0.02207(9) Uani 1 1 d . . . . .
Si5 Si 0.21996(3) 0.25179(2) 0.71383(2) 0.01686(8) Uani 1 1 d . . . . .
Si6 Si 0.05745(3) 0.39318(2) 0.70683(2) 0.01742(8) Uani 1 1 d . . . . .
Si7 Si -0.07684(3) 0.09172(2) 0.65222(2) 0.01729(8) Uani 1 1 d . . . . .
Si8 Si -0.21590(3) 0.22581(2) 0.58301(2) 0.02058(8) Uani 1 1 d . . . . .
Si9 Si -0.14306(3) 0.14482(2) 0.03082(2) 0.02377(9) Uani 1 1 d . . . . .
Si10 Si -0.18429(3) 0.32186(2) 0.02411(2) 0.02646(9) Uani 1 1 d . . . . .
Si11 Si 0.24186(3) 0.18169(2) 0.08333(2) 0.01973(8) Uani 1 1 d . . . . .
Si12 Si 0.20492(3) 0.34644(2) 0.13078(2) 0.02264(9) Uani 1 1 d . . . . .
S1 S 0.00349(3) 0.29463(2) 0.36886(2) 0.01959(7) Uani 1 1 d . . . . .
C1 C 0.08064(11) 0.23649(7) 0.42398(7) 0.0171(3) Uani 1 1 d . . . . .
C2 C 0.09347(11) 0.16682(7) 0.39705(7) 0.0185(3) Uani 1 1 d . . . . .
H1 H 0.1337 0.1261 0.4187 0.022 Uiso 1 1 calc R U . . .
C9 C 0.25991(12) 0.15764(8) 0.67933(8) 0.0228(3) Uani 1 1 d . . . . .
H2 H 0.2372 0.1564 0.6312 0.034 Uiso 1 1 calc R U . . .
H3 H 0.2207 0.1165 0.7126 0.034 Uiso 1 1 calc R U . . .
H4 H 0.3426 0.1509 0.6763 0.034 Uiso 1 1 calc R U . . .
C28 C 0.53903(15) 0.49901(10) 0.39956(11) 0.0455(5) Uani 1 1 d . . . . .
H5 H 0.5597 0.5008 0.3469 0.068 Uiso 1 1 calc R U . . .
H6 H 0.6054 0.4837 0.4232 0.068 Uiso 1 1 calc R U . . .
H7 H 0.5142 0.5494 0.4124 0.068 Uiso 1 1 calc R U . . .
C33 C -0.48578(12) 0.18218(9) 0.30891(7) 0.0257(3) Uani 1 1 d . . . . .
C38 C -0.29718(15) 0.35799(9) 0.28105(10) 0.0395(4) Uani 1 1 d . . . . .
H8 H -0.3632 0.3906 0.2752 0.059 Uiso 1 1 calc R U . . .
H9 H -0.2365 0.3709 0.2404 0.059 Uiso 1 1 calc R U . . .
H10 H -0.2693 0.3659 0.3265 0.059 Uiso 1 1 calc R U . . .
C43 C -0.06987(14) 0.06278(9) 0.07635(8) 0.0326(3) Uani 1 1 d . . . . .
H11 H -0.0677 0.0710 0.1270 0.049 Uiso 1 1 calc R U . . .
H12 H 0.0082 0.0589 0.0515 0.049 Uiso 1 1 calc R U . . .
H13 H -0.1119 0.0156 0.0743 0.049 Uiso 1 1 calc R U . . .
C44 C -0.12869(15) 0.12687(10) -0.06708(8) 0.0361(4) Uani 1 1 d . . . . .
H14 H -0.1637 0.0776 -0.0710 0.054 Uiso 1 1 calc R U . . .
H15 H -0.0477 0.1264 -0.0872 0.054 Uiso 1 1 calc R U . . .
H16 H -0.1672 0.1672 -0.0940 0.054 Uiso 1 1 calc R U . . .
C45 C -0.29614(13) 0.13516(11) 0.07091(9) 0.0393(4) Uani 1 1 d . . . . .
H17 H -0.3410 0.1728 0.0452 0.059 Uiso 1 1 calc R U . . .
H18 H -0.3043 0.1437 0.1222 0.059 Uiso 1 1 calc R U . . .
H19 H -0.3237 0.0839 0.0664 0.059 Uiso 1 1 calc R U . . .
C46 C -0.24036(17) 0.31543(14) -0.06393(9) 0.0554(6) Uani 1 1 d . . . . .
H20 H -0.2889 0.2700 -0.0599 0.083 Uiso 1 1 calc R U . . .
H21 H -0.1763 0.3122 -0.1027 0.083 Uiso 1 1 calc R U . . .
H22 H -0.2852 0.3608 -0.0751 0.083 Uiso 1 1 calc R U . . .
C47 C -0.31033(14) 0.32270(10) 0.09569(9) 0.0379(4) Uani 1 1 d . . . . .
H23 H -0.2855 0.3134 0.1434 0.057 Uiso 1 1 calc R U . . .
H24 H -0.3645 0.2828 0.0898 0.057 Uiso 1 1 calc R U . . .
H25 H -0.3473 0.3723 0.0915 0.057 Uiso 1 1 calc R U . . .
C48 C -0.11578(17) 0.41758(10) 0.01610(13) 0.0563(6) Uani 1 1 d . . . . .
H26 H -0.1706 0.4566 0.0033 0.084 Uiso 1 1 calc R U . . .
H27 H -0.0492 0.4202 -0.0217 0.084 Uiso 1 1 calc R U . . .
H28 H -0.0914 0.4263 0.0624 0.084 Uiso 1 1 calc R U . . .
C49 C 0.23374(14) 0.12499(9) 0.00495(8) 0.0321(3) Uani 1 1 d . . . . .
H29 H 0.2886 0.0834 0.0061 0.048 Uiso 1 1 calc R U . . .
H30 H 0.2518 0.1580 -0.0405 0.048 Uiso 1 1 calc R U . . .
H31 H 0.1565 0.1040 0.0082 0.048 Uiso 1 1 calc R U . . .
C3 C 0.04145(11) 0.16136(8) 0.33438(7) 0.0200(3) Uani 1 1 d . . . . .
H32 H 0.0432 0.1165 0.3105 0.024 Uiso 1 1 calc R U . . .
C4 C -0.01174(11) 0.22645(8) 0.31111(7) 0.0191(3) Uani 1 1 d . . . . .
C5 C 0.07320(10) 0.28723(7) 0.69614(7) 0.0150(2) Uani 1 1 d . . . . .
C6 C -0.02219(11) 0.24269(7) 0.75172(7) 0.0173(3) Uani 1 1 d . . . . .
H33 H 0.0083 0.1932 0.7697 0.021 Uiso 1 1 calc R U . . .
H34 H -0.0429 0.2722 0.7937 0.021 Uiso 1 1 calc R U . . .
C7 C -0.12962(11) 0.22878(7) 0.71729(7) 0.0185(3) Uani 1 1 d . . . . .
H35 H -0.1728 0.2767 0.7123 0.022 Uiso 1 1 calc R U . . .
H36 H -0.1793 0.1907 0.7492 0.022 Uiso 1 1 calc R U . . .
C8 C -0.09697(10) 0.19934(7) 0.64029(7) 0.0157(2) Uani 1 1 d . . . . .
C10 C 0.33519(11) 0.32091(8) 0.67227(8) 0.0233(3) Uani 1 1 d . . . . .
H37 H 0.3256 0.3680 0.6958 0.035 Uiso 1 1 calc R U . . .
H38 H 0.3308 0.3321 0.6205 0.035 Uiso 1 1 calc R U . . .
H39 H 0.4097 0.2990 0.6787 0.035 Uiso 1 1 calc R U . . .
C11 C 0.22401(13) 0.23549(9) 0.81374(7) 0.0283(3) Uani 1 1 d . . . . .
H40 H 0.3009 0.2201 0.8224 0.042 Uiso 1 1 calc R U . . .
H41 H 0.1692 0.1953 0.8352 0.042 Uiso 1 1 calc R U . . .
H42 H 0.2041 0.2826 0.8358 0.042 Uiso 1 1 calc R U . . .
C12 C 0.11024(13) 0.41793(8) 0.79144(8) 0.0279(3) Uani 1 1 d . . . . .
H43 H 0.1927 0.4094 0.7875 0.042 Uiso 1 1 calc R U . . .
H44 H 0.0712 0.3858 0.8333 0.042 Uiso 1 1 calc R U . . .
H45 H 0.0944 0.4715 0.7977 0.042 Uiso 1 1 calc R U . . .
C13 C 0.13204(13) 0.45626(8) 0.62858(8) 0.0268(3) Uani 1 1 d . . . . .
H46 H 0.0924 0.4538 0.5864 0.040 Uiso 1 1 calc R U . . .
H47 H 0.2109 0.4394 0.6171 0.040 Uiso 1 1 calc R U . . .
H48 H 0.1320 0.5087 0.6411 0.040 Uiso 1 1 calc R U . . .
C14 C -0.09655(12) 0.42077(8) 0.71820(8) 0.0228(3) Uani 1 1 d . . . . .
H49 H -0.1025 0.4755 0.7221 0.034 Uiso 1 1 calc R U . . .
H50 H -0.1369 0.3928 0.7622 0.034 Uiso 1 1 calc R U . . .
H51 H -0.1308 0.4084 0.6762 0.034 Uiso 1 1 calc R U . . .
C15 C 0.02157(13) 0.05701(8) 0.57604(8) 0.0252(3) Uani 1 1 d . . . . .
H52 H 0.0287 0.0017 0.5845 0.038 Uiso 1 1 calc R U . . .
H53 H 0.0968 0.0809 0.5731 0.038 Uiso 1 1 calc R U . . .
H54 H -0.0091 0.0702 0.5305 0.038 Uiso 1 1 calc R U . . .
C16 C -0.21617(13) 0.03900(9) 0.66185(9) 0.0310(3) Uani 1 1 d . . . . .
H55 H -0.2490 0.0479 0.6166 0.047 Uiso 1 1 calc R U . . .
H56 H -0.2690 0.0571 0.7015 0.047 Uiso 1 1 calc R U . . .
H57 H -0.2034 -0.0155 0.6725 0.047 Uiso 1 1 calc R U . . .
C17 C -0.02350(13) 0.05734(8) 0.73917(7) 0.0235(3) Uani 1 1 d . . . . .
H58 H -0.0193 0.0017 0.7436 0.035 Uiso 1 1 calc R U . . .
H59 H -0.0759 0.0734 0.7800 0.035 Uiso 1 1 calc R U . . .
H60 H 0.0526 0.0789 0.7394 0.035 Uiso 1 1 calc R U . . .
C18 C -0.21026(12) 0.17300(8) 0.50120(8) 0.0252(3) Uani 1 1 d . . . . .
H61 H -0.2268 0.1190 0.5163 0.038 Uiso 1 1 calc R U . . .
H62 H -0.1340 0.1786 0.4730 0.038 Uiso 1 1 calc R U . . .
H63 H -0.2671 0.1937 0.4714 0.038 Uiso 1 1 calc R U . . .
C19 C -0.21168(14) 0.32975(8) 0.55031(9) 0.0330(4) Uani 1 1 d . . . . .
H64 H -0.2799 0.3429 0.5278 0.050 Uiso 1 1 calc R U . . .
H65 H -0.1434 0.3411 0.5147 0.050 Uiso 1 1 calc R U . . .
H66 H -0.2095 0.3596 0.5914 0.050 Uiso 1 1 calc R U . . .
C20 C -0.35860(12) 0.20918(10) 0.64028(9) 0.0347(4) Uani 1 1 d . . . . .
H67 H -0.4188 0.2286 0.6126 0.052 Uiso 1 1 calc R U . . .
H68 H -0.3611 0.2357 0.6838 0.052 Uiso 1 1 calc R U . . .
H69 H -0.3705 0.1545 0.6543 0.052 Uiso 1 1 calc R U . . .
C21 C 0.26215(11) 0.33705(7) 0.47305(7) 0.0173(3) Uani 1 1 d . . . . .
C22 C 0.37724(11) 0.31449(8) 0.47233(7) 0.0207(3) Uani 1 1 d . . . . .
C23 C 0.46463(12) 0.36753(9) 0.44877(8) 0.0271(3) Uani 1 1 d . . . . .
H70 H 0.5415 0.3521 0.4494 0.033 Uiso 1 1 calc R U . . .
C24 C 0.44305(13) 0.44214(9) 0.42444(8) 0.0298(3) Uani 1 1 d . . . . .
C25 C 0.33057(13) 0.46370(8) 0.42409(8) 0.0281(3) Uani 1 1 d . . . . .
H71 H 0.3146 0.5147 0.4076 0.034 Uiso 1 1 calc R U . . .
C26 C 0.24006(12) 0.41296(8) 0.44713(7) 0.0218(3) Uani 1 1 d . . . . .
C27 C 0.40949(12) 0.23455(8) 0.49679(8) 0.0266(3) Uani 1 1 d . . . . .
H72 H 0.4836 0.2225 0.4701 0.040 Uiso 1 1 calc R U . . .
H73 H 0.3514 0.1990 0.4874 0.040 Uiso 1 1 calc R U . . .
H74 H 0.4144 0.2301 0.5488 0.040 Uiso 1 1 calc R U . . .
C29 C 0.12124(13) 0.44147(8) 0.44170(8) 0.0275(3) Uani 1 1 d . . . . .
H75 H 0.1164 0.4947 0.4519 0.041 Uiso 1 1 calc R U . . .
H76 H 0.0664 0.4108 0.4769 0.041 Uiso 1 1 calc R U . . .
H77 H 0.1035 0.4375 0.3927 0.041 Uiso 1 1 calc R U . . .
C30 C -0.25165(11) 0.21837(8) 0.26689(7) 0.0203(3) Uani 1 1 d . . . . .
C31 C -0.29021(12) 0.14194(8) 0.27697(7) 0.0232(3) Uani 1 1 d . . . . .
C32 C -0.40565(13) 0.12564(9) 0.29684(8) 0.0268(3) Uani 1 1 d . . . . .
H78 H -0.4306 0.0741 0.3024 0.032 Uiso 1 1 calc R U . . .
C34 C -0.44732(12) 0.25655(9) 0.30248(8) 0.0276(3) Uani 1 1 d . . . . .
H79 H -0.5009 0.2957 0.3119 0.033 Uiso 1 1 calc R U . . .
C35 C -0.33185(12) 0.27603(8) 0.28259(7) 0.0243(3) Uani 1 1 d . . . . .
C36 C -0.20891(14) 0.07641(9) 0.26989(9) 0.0351(4) Uani 1 1 d . . . . .
H80 H -0.1880 0.0588 0.3175 0.053 Uiso 1 1 calc R U . . .
H81 H -0.1401 0.0931 0.2366 0.053 Uiso 1 1 calc R U . . .
H82 H -0.2458 0.0347 0.2510 0.053 Uiso 1 1 calc R U . . .
C37 C -0.61057(13) 0.16154(11) 0.32908(9) 0.0366(4) Uani 1 1 d . . . . .
H83 H -0.6385 0.1408 0.2883 0.055 Uiso 1 1 calc R U . . .
H84 H -0.6540 0.2071 0.3408 0.055 Uiso 1 1 calc R U . . .
H85 H -0.6203 0.1234 0.3713 0.055 Uiso 1 1 calc R U . . .
C39 C -0.07930(11) 0.24205(8) 0.03939(7) 0.0192(3) Uani 1 1 d . . . . .
C40 C 0.02996(11) 0.25644(8) -0.01952(7) 0.0213(3) Uani 1 1 d . . . . .
H86 H 0.0603 0.2069 -0.0334 0.026 Uiso 1 1 calc R U . . .
H87 H 0.0078 0.2855 -0.0633 0.026 Uiso 1 1 calc R U . . .
C41 C 0.12380(11) 0.30029(8) 0.00768(7) 0.0206(3) Uani 1 1 d . . . . .
H88 H 0.1027 0.3545 0.0078 0.025 Uiso 1 1 calc R U . . .
H89 H 0.1961 0.2972 -0.0255 0.025 Uiso 1 1 calc R U . . .
C42 C 0.14171(11) 0.26683(7) 0.08657(7) 0.0173(3) Uani 1 1 d . . . . .
C50 C 0.21205(13) 0.11617(9) 0.16831(8) 0.0291(3) Uani 1 1 d . . . . .
H90 H 0.2705 0.0767 0.1685 0.044 Uiso 1 1 calc R U . . .
H91 H 0.1368 0.0924 0.1710 0.044 Uiso 1 1 calc R U . . .
H92 H 0.2132 0.1450 0.2101 0.044 Uiso 1 1 calc R U . . .
C51 C 0.39658(13) 0.20963(10) 0.06934(10) 0.0368(4) Uani 1 1 d . . . . .
H93 H 0.4125 0.2379 0.1091 0.055 Uiso 1 1 calc R U . . .
H94 H 0.4146 0.2417 0.0234 0.055 Uiso 1 1 calc R U . . .
H95 H 0.4435 0.1638 0.0682 0.055 Uiso 1 1 calc R U . . .
C52 C 0.32285(14) 0.39582(9) 0.06495(9) 0.0335(4) Uani 1 1 d . . . . .
H96 H 0.2935 0.4139 0.0200 0.050 Uiso 1 1 calc R U . . .
H97 H 0.3852 0.3601 0.0545 0.050 Uiso 1 1 calc R U . . .
H98 H 0.3513 0.4392 0.0861 0.050 Uiso 1 1 calc R U . . .
C53 C 0.26120(14) 0.31283(9) 0.21652(8) 0.0318(3) Uani 1 1 d . . . . .
H99 H 0.2849 0.3567 0.2389 0.048 Uiso 1 1 calc R U . . .
H100 H 0.3269 0.2798 0.2058 0.048 Uiso 1 1 calc R U . . .
H101 H 0.2014 0.2843 0.2498 0.048 Uiso 1 1 calc R U . . .
C54 C 0.09968(14) 0.42262(9) 0.15226(9) 0.0345(4) Uani 1 1 d . . . . .
H102 H 0.0397 0.4024 0.1909 0.052 Uiso 1 1 calc R U . . .
H103 H 0.0655 0.4401 0.1089 0.052 Uiso 1 1 calc R U . . .
H104 H 0.1385 0.4653 0.1682 0.052 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Si1 C5 1.8948(13) . ?
Si1 C8 1.8973(13) . ?
Si1 Si2 2.1846(5) . ?
Si2 C1 1.8652(13) . ?
Si2 C21 1.8825(13) . ?
Si3 C39 1.8984(13) . ?
Si3 C42 1.9030(13) . ?
Si3 Si4 2.1829(5) . ?
Si4 C4 1.8676(13) . ?
Si4 C30 1.8814(14) . ?
Si5 C10 1.8658(14) . ?
Si5 C11 1.8743(14) . ?
Si5 C9 1.8815(14) . ?
Si5 C5 1.9053(13) . ?
Si6 C13 1.8669(14) . ?
Si6 C14 1.8731(14) . ?
Si6 C12 1.8780(14) . ?
Si6 C5 1.9096(13) . ?
Si7 C15 1.8651(14) . ?
Si7 C16 1.8753(15) . ?
Si7 C17 1.8744(14) . ?
Si7 C8 1.9105(13) . ?
Si8 C18 1.8698(15) . ?
Si8 C19 1.8753(16) . ?
Si8 C20 1.8763(16) . ?
Si8 C8 1.9166(13) . ?
Si9 C45 1.8625(16) . ?
Si9 C43 1.8779(17) . ?
Si9 C44 1.8799(15) . ?
Si9 C39 1.9114(14) . ?
Si10 C47 1.8618(16) . ?
Si10 C48 1.863(2) . ?
Si10 C46 1.8790(18) . ?
Si10 C39 1.9021(14) . ?
Si11 C50 1.8637(15) . ?
Si11 C49 1.8762(15) . ?
Si11 C51 1.8742(16) . ?
Si11 C42 1.9119(13) . ?
Si12 C54 1.8657(16) . ?
Si12 C53 1.8675(16) . ?
Si12 C52 1.8811(16) . ?
Si12 C42 1.9115(14) . ?
S1 C4 1.7276(13) . ?
S1 C1 1.7319(13) . ?
C1 C2 1.3781(18) . ?
C2 C3 1.4140(18) . ?
C28 C24 1.511(2) . ?
C33 C34 1.381(2) . ?
C33 C32 1.388(2) . ?
C33 C37 1.509(2) . ?
C38 C35 1.504(2) . ?
C3 C4 1.3706(19) . ?
C5 C6 1.5777(17) . ?
C6 C7 1.5370(18) . ?
C7 C8 1.5816(17) . ?
C21 C26 1.4158(19) . ?
C21 C22 1.4162(19) . ?
C22 C23 1.3927(19) . ?
C22 C27 1.505(2) . ?
C23 C24 1.386(2) . ?
C24 C25 1.384(2) . ?
C25 C26 1.3920(19) . ?
C26 C29 1.505(2) . ?
C30 C35 1.4141(19) . ?
C30 C31 1.414(2) . ?
C31 C32 1.388(2) . ?
C31 C36 1.507(2) . ?
C34 C35 1.400(2) . ?
C39 C40 1.5812(18) . ?
C40 C41 1.5312(19) . ?
C41 C42 1.5791(17) . ?

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
C5 Si1 C8 100.73(5) . . ?
C5 Si1 Si2 127.84(4) . . ?
C8 Si1 Si2 127.99(4) . . ?
C1 Si2 C21 111.14(6) . . ?
C1 Si2 Si1 117.89(4) . . ?
C21 Si2 Si1 123.18(4) . . ?
C39 Si3 C42 100.68(6) . . ?
C39 Si3 Si4 127.32(4) . . ?
C42 Si3 Si4 128.34(4) . . ?
C4 Si4 C30 110.31(6) . . ?
C4 Si4 Si3 117.47(5) . . ?
C30 Si4 Si3 124.26(4) . . ?
C10 Si5 C11 108.95(7) . . ?
C10 Si5 C9 106.84(6) . . ?
C11 Si5 C9 104.65(7) . . ?
C10 Si5 C5 111.71(6) . . ?
C11 Si5 C5 109.91(6) . . ?
C9 Si5 C5 114.42(6) . . ?
C13 Si6 C14 107.14(7) . . ?
C13 Si6 C12 108.30(7) . . ?
C14 Si6 C12 104.67(7) . . ?
C13 Si6 C5 113.85(6) . . ?
C14 Si6 C5 110.85(6) . . ?
C12 Si6 C5 111.54(6) . . ?
C15 Si7 C16 108.66(7) . . ?
C15 Si7 C17 108.35(7) . . ?
C16 Si7 C17 101.65(7) . . ?
C15 Si7 C8 112.57(6) . . ?
C16 Si7 C8 111.83(6) . . ?
C17 Si7 C8 113.15(6) . . ?
C18 Si8 C19 106.86(7) . . ?
C18 Si8 C20 109.30(7) . . ?
C19 Si8 C20 105.22(8) . . ?
C18 Si8 C8 113.86(6) . . ?
C19 Si8 C8 111.53(6) . . ?
C20 Si8 C8 109.68(7) . . ?
C45 Si9 C43 105.27(8) . . ?
C45 Si9 C44 108.94(8) . . ?
C43 Si9 C44 105.15(8) . . ?
C45 Si9 C39 112.92(7) . . ?
C43 Si9 C39 114.04(6) . . ?
C44 Si9 C39 110.08(7) . . ?
C47 Si10 C48 106.41(9) . . ?
C47 Si10 C46 107.03(9) . . ?
C48 Si10 C46 105.72(11) . . ?
C47 Si10 C39 115.02(7) . . ?
C48 Si10 C39 112.23(7) . . ?
C46 Si10 C39 109.88(7) . . ?
C50 Si11 C49 108.07(7) . . ?
C50 Si11 C51 108.52(8) . . ?
C49 Si11 C51 101.80(8) . . ?
C50 Si11 C42 110.63(6) . . ?
C49 Si11 C42 114.14(6) . . ?
C51 Si11 C42 113.18(7) . . ?
C54 Si12 C53 107.05(8) . . ?
C54 Si12 C52 104.76(7) . . ?
C53 Si12 C52 109.21(7) . . ?
C54 Si12 C42 112.48(7) . . ?
C53 Si12 C42 113.59(6) . . ?
C52 Si12 C42 109.33(7) . . ?
C4 S1 C1 94.41(6) . . ?
C2 C1 S1 108.46(9) . . ?
C2 C1 Si2 125.33(10) . . ?
S1 C1 Si2 126.10(8) . . ?
C1 C2 C3 114.09(12) . . ?
C34 C33 C32 118.01(13) . . ?
C34 C33 C37 121.95(14) . . ?
C32 C33 C37 120.04(14) . . ?
C4 C3 C2 114.21(12) . . ?
C3 C4 S1 108.83(10) . . ?
C3 C4 Si4 130.45(10) . . ?
S1 C4 Si4 120.60(8) . . ?
C6 C5 Si1 100.99(8) . . ?
C6 C5 Si5 109.74(8) . . ?
Si1 C5 Si5 112.81(6) . . ?
C6 C5 Si6 108.18(8) . . ?
Si1 C5 Si6 113.18(6) . . ?
Si5 C5 Si6 111.33(6) . . ?
C7 C6 C5 111.88(10) . . ?
C6 C7 C8 110.91(10) . . ?
C7 C8 Si1 98.66(8) . . ?
C7 C8 Si7 109.09(8) . . ?
Si1 C8 Si7 117.57(6) . . ?
C7 C8 Si8 108.98(8) . . ?
Si1 C8 Si8 110.62(6) . . ?
Si7 C8 Si8 111.01(6) . . ?
C26 C21 C22 118.30(12) . . ?
C26 C21 Si2 122.08(10) . . ?
C22 C21 Si2 119.51(10) . . ?
C23 C22 C21 119.62(13) . . ?
C23 C22 C27 118.10(13) . . ?
C21 C22 C27 122.28(12) . . ?
C24 C23 C22 122.10(14) . . ?
C23 C24 C25 118.14(13) . . ?
C23 C24 C28 121.31(15) . . ?
C25 C24 C28 120.54(15) . . ?
C24 C25 C26 122.06(14) . . ?
C25 C26 C21 119.74(13) . . ?
C25 C26 C29 117.74(13) . . ?
C21 C26 C29 122.51(12) . . ?
C35 C30 C31 118.37(12) . . ?
C35 C30 Si4 118.94(10) . . ?
C31 C30 Si4 122.69(10) . . ?
C32 C31 C30 119.79(13) . . ?
C32 C31 C36 118.20(13) . . ?
C30 C31 C36 121.96(13) . . ?
C31 C32 C33 122.14(14) . . ?
C33 C34 C35 122.09(13) . . ?
C34 C35 C30 119.43(13) . . ?
C34 C35 C38 118.26(13) . . ?
C30 C35 C38 122.28(13) . . ?
C40 C39 Si3 100.39(8) . . ?
C40 C39 Si10 108.41(9) . . ?
Si3 C39 Si10 116.38(7) . . ?
C40 C39 Si9 108.68(9) . . ?
Si3 C39 Si9 110.35(7) . . ?
Si10 C39 Si9 111.80(7) . . ?
C41 C40 C39 112.37(11) . . ?
C40 C41 C42 110.94(10) . . ?
C41 C42 Si3 99.83(8) . . ?
C41 C42 Si11 110.72(9) . . ?
Si3 C42 Si11 113.01(7) . . ?
C41 C42 Si12 107.30(9) . . ?
Si3 C42 Si12 114.75(7) . . ?
Si11 C42 Si12 110.56(6) . . ?

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
C4 S1 C1 C2 0.28(10) . . . . ?
C4 S1 C1 Si2 176.54(9) . . . . ?
C21 Si2 C1 C2 109.36(12) . . . . ?
Si1 Si2 C1 C2 -100.35(11) . . . . ?
C21 Si2 C1 S1 -66.29(10) . . . . ?
Si1 Si2 C1 S1 84.00(9) . . . . ?
S1 C1 C2 C3 -0.48(14) . . . . ?
Si2 C1 C2 C3 -176.78(9) . . . . ?
C1 C2 C3 C4 0.50(17) . . . . ?
C2 C3 C4 S1 -0.26(15) . . . . ?
C2 C3 C4 Si4 -176.21(10) . . . . ?
C1 S1 C4 C3 -0.01(10) . . . . ?
C1 S1 C4 Si4 176.40(8) . . . . ?
C30 Si4 C4 C3 86.46(14) . . . . ?
Si3 Si4 C4 C3 -63.88(14) . . . . ?
C30 Si4 C4 S1 -89.08(9) . . . . ?
Si3 Si4 C4 S1 120.58(7) . . . . ?
C8 Si1 C5 C6 1.33(9) . . . . ?
Si2 Si1 C5 C6 -158.82(6) . . . . ?
C8 Si1 C5 Si5 118.39(7) . . . . ?
Si2 Si1 C5 Si5 -41.76(8) . . . . ?
C8 Si1 C5 Si6 -114.08(7) . . . . ?
Si2 Si1 C5 Si6 85.78(7) . . . . ?
Si1 C5 C6 C7 -25.27(11) . . . . ?
Si5 C5 C6 C7 -144.56(9) . . . . ?
Si6 C5 C6 C7 93.80(10) . . . . ?
C5 C6 C7 C8 45.55(14) . . . . ?
C6 C7 C8 Si1 -38.83(11) . . . . ?
C6 C7 C8 Si7 84.41(11) . . . . ?
C6 C7 C8 Si8 -154.24(9) . . . . ?
C5 Si1 C8 C7 20.76(9) . . . . ?
Si2 Si1 C8 C7 -179.14(6) . . . . ?
C5 Si1 C8 Si7 -96.17(7) . . . . ?
Si2 Si1 C8 Si7 63.94(8) . . . . ?
C5 Si1 C8 Si8 134.89(6) . . . . ?
Si2 Si1 C8 Si8 -65.00(8) . . . . ?
C1 Si2 C21 C26 71.07(12) . . . . ?
Si1 Si2 C21 C26 -77.37(11) . . . . ?
C1 Si2 C21 C22 -105.22(11) . . . . ?
Si1 Si2 C21 C22 106.34(10) . . . . ?
C26 C21 C22 C23 2.16(19) . . . . ?
Si2 C21 C22 C23 178.59(10) . . . . ?
C26 C21 C22 C27 -178.26(12) . . . . ?
Si2 C21 C22 C27 -1.84(17) . . . . ?
C21 C22 C23 C24 -1.2(2) . . . . ?
C27 C22 C23 C24 179.18(13) . . . . ?
C22 C23 C24 C25 0.2(2) . . . . ?
C22 C23 C24 C28 179.58(14) . . . . ?
C23 C24 C25 C26 -0.1(2) . . . . ?
C28 C24 C25 C26 -179.52(14) . . . . ?
C24 C25 C26 C21 1.1(2) . . . . ?
C24 C25 C26 C29 -177.58(14) . . . . ?
C22 C21 C26 C25 -2.10(19) . . . . ?
Si2 C21 C26 C25 -178.43(10) . . . . ?
C22 C21 C26 C29 176.52(12) . . . . ?
Si2 C21 C26 C29 0.18(18) . . . . ?
C4 Si4 C30 C35 102.35(11) . . . . ?
Si3 Si4 C30 C35 -109.74(10) . . . . ?
C4 Si4 C30 C31 -76.38(12) . . . . ?
Si3 Si4 C30 C31 71.54(12) . . . . ?
C35 C30 C31 C32 4.5(2) . . . . ?
Si4 C30 C31 C32 -176.78(10) . . . . ?
C35 C30 C31 C36 -172.86(13) . . . . ?
Si4 C30 C31 C36 5.87(19) . . . . ?
C30 C31 C32 C33 -1.4(2) . . . . ?
C36 C31 C32 C33 176.04(14) . . . . ?
C34 C33 C32 C31 -1.7(2) . . . . ?
C37 C33 C32 C31 178.87(14) . . . . ?
C32 C33 C34 C35 1.7(2) . . . . ?
C37 C33 C34 C35 -178.90(14) . . . . ?
C33 C34 C35 C30 1.4(2) . . . . ?
C33 C34 C35 C38 -176.63(14) . . . . ?
C31 C30 C35 C34 -4.5(2) . . . . ?
Si4 C30 C35 C34 176.72(11) . . . . ?
C31 C30 C35 C38 173.50(14) . . . . ?
Si4 C30 C35 C38 -5.28(19) . . . . ?
C42 Si3 C39 C40 6.22(9) . . . . ?
Si4 Si3 C39 C40 165.85(6) . . . . ?
C42 Si3 C39 Si10 -110.48(8) . . . . ?
Si4 Si3 C39 Si10 49.15(9) . . . . ?
C42 Si3 C39 Si9 120.76(7) . . . . ?
Si4 Si3 C39 Si9 -79.61(7) . . . . ?
Si3 C39 C40 C41 -28.83(12) . . . . ?
Si10 C39 C40 C41 93.67(11) . . . . ?
Si9 C39 C40 C41 -144.62(9) . . . . ?
C39 C40 C41 C42 45.49(15) . . . . ?
C40 C41 C42 Si3 -35.22(12) . . . . ?
C40 C41 C42 Si11 84.11(11) . . . . ?
C40 C41 C42 Si12 -155.15(9) . . . . ?

_refine_diff_density_max         0.501
_refine_diff_density_min         -0.344
_refine_diff_density_rms         0.044

_shelxl_version_number           2014-3


# SQUEEZE RESULTS (APPEND TO CIF)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.500 0.000 0.500 148 41 ' '
2 0.500 0.075 1.000 628 159 ' '
_platon_squeeze_details          
;
;

_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: tetrahydrofuran'
_chemical_properties_physical    
', Air-sensitive,Moisture-sensitive,Oxygen-sensitive'
