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

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

data_si331a_a
_database_code_depnum_ccdc_archive 'CCDC 1060708'
_audit_update_record             
;
2015-04-21 deposited with the CCDC.
2015-05-20 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        'bicyclic [4]dendralene'
_chemical_name_common            ?
_chemical_melting_point          422-423
_chemical_formula_moiety         'C42 H88 Si10, C4 H10 O'
_chemical_formula_sum            'C46 H98 O Si10'
_chemical_formula_weight         948.14

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

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   P-1

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

_cell_length_a                   9.4329(13)
_cell_length_b                   11.2567(16)
_cell_length_c                   29.197(4)
_cell_angle_alpha                85.049(2)
_cell_angle_beta                 83.862(2)
_cell_angle_gamma                67.021(2)
_cell_volume                     2834.5(7)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    6883
_cell_measurement_theta_min      2.36
_cell_measurement_theta_max      28.07

_exptl_crystal_description       plate
_exptl_crystal_colour            pale-yellow
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.111
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1044
_exptl_absorpt_coefficient_mu    0.263
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.9254
_exptl_absorpt_correction_T_max  0.9742
_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_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            13273
_diffrn_reflns_av_R_equivalents  0.0201
_diffrn_reflns_av_sigmaI/netI    0.0510
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_theta_min         1.40
_diffrn_reflns_theta_max         25.00
_reflns_number_total             9746
_reflns_number_gt                7974
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'APEX2 (Bruker AXS, 2006)'
_computing_cell_refinement       'APEX2 (Bruker AXS, 2006)'
_computing_data_reduction        'SAINT (Bruker AXS, 2004)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'XSHEL (Bruker AXS,2002)'
_computing_publication_material  'XCIF (Bruker AXS, 2001)'

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0394P)²+2.3744P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         9746
_refine_ls_number_parameters     540
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0608
_refine_ls_R_factor_gt           0.0445
_refine_ls_wR_factor_ref         0.1036
_refine_ls_wR_factor_gt          0.0999
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_restrained_S_all      1.074
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Si1 Si 0.21350(8) 0.44706(7) 0.14344(2) 0.01343(16) Uani 1 1 d . . .
C1 C 0.1425(3) 0.3821(2) 0.19774(9) 0.0165(6) Uani 1 1 d . . .
H1 H 0.1057 0.3151 0.1965 0.020 Uiso 1 1 calc R . .
C2 C 0.1424(3) 0.4283(3) 0.23864(9) 0.0164(6) Uani 1 1 d . . .
H2 H 0.1017 0.3909 0.2645 0.020 Uiso 1 1 calc R . .
C3 C 0.1965(3) 0.5288(3) 0.24924(9) 0.0160(6) Uani 1 1 d . . .
C4 C 0.1496(3) 0.5719(3) 0.29246(9) 0.0175(6) Uani 1 1 d . . .
H3 H 0.0839 0.5339 0.3087 0.021 Uiso 1 1 calc R . .
C5 C 0.1757(3) 0.6631(2) 0.32012(8) 0.0150(5) Uani 1 1 d . . .
H4 H 0.0760 0.7255 0.3342 0.018 Uiso 1 1 calc R . .
C6 C 0.2910(3) 0.7293(2) 0.30595(9) 0.0174(6) Uani 1 1 d . . .
H5 H 0.2436 0.8218 0.3142 0.021 Uiso 1 1 calc R . .
C7 C 0.3732(3) 0.7183(3) 0.26011(9) 0.0186(6) Uani 1 1 d . . .
H6 H 0.4390 0.7649 0.2557 0.022 Uiso 1 1 calc R . .
C8 C 0.3739(3) 0.6556(2) 0.22316(9) 0.0165(6) Uani 1 1 d . . .
H7 H 0.4393 0.6678 0.1977 0.020 Uiso 1 1 calc R . .
C9 C 0.2944(3) 0.5713(2) 0.21358(9) 0.0144(5) Uani 1 1 d . . .
C10 C 0.3148(3) 0.5350(2) 0.16956(9) 0.0165(6) Uani 1 1 d . . .
H8 H 0.3887 0.5566 0.1497 0.020 Uiso 1 1 calc R . .
Si2 Si 0.33543(7) 0.62021(7) 0.36027(2) 0.01320(15) Uani 1 1 d . . .
C11 C 0.3238(3) 0.3185(2) 0.09952(8) 0.0147(5) Uani 1 1 d . . .
C12 C 0.2506(3) 0.3880(3) 0.05363(9) 0.0177(6) Uani 1 1 d . . .
H9 H 0.3064 0.4420 0.0393 0.021 Uiso 1 1 calc R . .
H10 H 0.2607 0.3226 0.0316 0.021 Uiso 1 1 calc R . .
C13 C 0.0786(3) 0.4733(2) 0.06415(9) 0.0165(6) Uani 1 1 d . . .
H11 H 0.0193 0.4180 0.0729 0.020 Uiso 1 1 calc R . .
H12 H 0.0369 0.5270 0.0363 0.020 Uiso 1 1 calc R . .
C14 C 0.0603(3) 0.5632(2) 0.10481(8) 0.0154(5) Uani 1 1 d . . .
Si3 Si 0.54257(8) 0.27223(7) 0.09744(3) 0.01811(17) Uani 1 1 d . . .
C15 C 0.6598(3) 0.1258(3) 0.06390(11) 0.0300(7) Uani 1 1 d . . .
H13 H 0.7691 0.1133 0.0618 0.045 Uiso 1 1 calc R . .
H14 H 0.6247 0.1381 0.0328 0.045 Uiso 1 1 calc R . .
H15 H 0.6470 0.0497 0.0796 0.045 Uiso 1 1 calc R . .
C16 C 0.6133(3) 0.2403(3) 0.15677(10) 0.0238(6) Uani 1 1 d . . .
H16 H 0.7264 0.2079 0.1543 0.036 Uiso 1 1 calc R . .
H17 H 0.5795 0.1757 0.1737 0.036 Uiso 1 1 calc R . .
H18 H 0.5709 0.3206 0.1732 0.036 Uiso 1 1 calc R . .
C17 C 0.6023(3) 0.4012(3) 0.06680(10) 0.0236(6) Uani 1 1 d . . .
H19 H 0.5633 0.4779 0.0853 0.035 Uiso 1 1 calc R . .
H20 H 0.5594 0.4239 0.0366 0.035 Uiso 1 1 calc R . .
H21 H 0.7152 0.3691 0.0625 0.035 Uiso 1 1 calc R . .
Si4 Si 0.28765(8) 0.16123(7) 0.10933(3) 0.01829(17) Uani 1 1 d . . .
C18 C 0.3510(3) 0.0630(3) 0.05613(10) 0.0266(6) Uani 1 1 d . . .
H22 H 0.4159 -0.0265 0.0647 0.040 Uiso 1 1 calc R . .
H23 H 0.4100 0.0996 0.0338 0.040 Uiso 1 1 calc R . .
H24 H 0.2598 0.0650 0.0423 0.040 Uiso 1 1 calc R . .
C19 C 0.3905(3) 0.0565(3) 0.15876(10) 0.0246(6) Uani 1 1 d . . .
H25 H 0.3610 0.1062 0.1866 0.037 Uiso 1 1 calc R . .
H26 H 0.5024 0.0274 0.1514 0.037 Uiso 1 1 calc R . .
H27 H 0.3618 -0.0186 0.1640 0.037 Uiso 1 1 calc R . .
C20 C 0.0795(3) 0.1810(3) 0.12014(10) 0.0248(6) Uani 1 1 d . . .
H28 H 0.0742 0.0966 0.1288 0.037 Uiso 1 1 calc R . .
H29 H 0.0262 0.2167 0.0920 0.037 Uiso 1 1 calc R . .
H30 H 0.0297 0.2397 0.1452 0.037 Uiso 1 1 calc R . .
Si5 Si -0.14290(8) 0.61808(7) 0.13519(3) 0.01808(17) Uani 1 1 d . . .
C21 C -0.2048(3) 0.4809(3) 0.15355(10) 0.0252(6) Uani 1 1 d . . .
H31 H -0.1444 0.4291 0.1787 0.038 Uiso 1 1 calc R . .
H32 H -0.1878 0.4266 0.1274 0.038 Uiso 1 1 calc R . .
H33 H -0.3148 0.5151 0.1642 0.038 Uiso 1 1 calc R . .
C22 C -0.1666(3) 0.7057(3) 0.18902(10) 0.0270(7) Uani 1 1 d . . .
H34 H -0.2488 0.6940 0.2101 0.040 Uiso 1 1 calc R . .
H35 H -0.1938 0.7979 0.1811 0.040 Uiso 1 1 calc R . .
H36 H -0.0695 0.6709 0.2040 0.040 Uiso 1 1 calc R . .
C23 C -0.2939(3) 0.7247(3) 0.09608(10) 0.0273(7) Uani 1 1 d . . .
H37 H -0.3966 0.7468 0.1123 0.041 Uiso 1 1 calc R . .
H38 H -0.2876 0.6788 0.0684 0.041 Uiso 1 1 calc R . .
H39 H -0.2760 0.8040 0.0872 0.041 Uiso 1 1 calc R . .
Si6 Si 0.09230(8) 0.71469(7) 0.07929(3) 0.01805(17) Uani 1 1 d . . .
C24 C 0.2945(3) 0.7041(3) 0.06292(10) 0.0257(7) Uani 1 1 d . . .
H40 H 0.2916 0.7810 0.0439 0.039 Uiso 1 1 calc R . .
H41 H 0.3517 0.6268 0.0454 0.039 Uiso 1 1 calc R . .
H42 H 0.3460 0.6989 0.0909 0.039 Uiso 1 1 calc R . .
C25 C 0.0125(4) 0.8531(3) 0.11825(11) 0.0331(7) Uani 1 1 d . . .
H43 H 0.0582 0.8262 0.1479 0.050 Uiso 1 1 calc R . .
H44 H -0.0999 0.8801 0.1232 0.050 Uiso 1 1 calc R . .
H45 H 0.0373 0.9255 0.1041 0.050 Uiso 1 1 calc R . .
C26 C -0.0015(3) 0.7685(3) 0.02319(10) 0.0300(7) Uani 1 1 d . . .
H46 H -0.1018 0.7604 0.0263 0.045 Uiso 1 1 calc R . .
H47 H 0.0650 0.7142 -0.0014 0.045 Uiso 1 1 calc R . .
H48 H -0.0163 0.8588 0.0155 0.045 Uiso 1 1 calc R . .
C27 C 0.5023(3) 0.4632(2) 0.37346(8) 0.0141(5) Uani 1 1 d . . .
C28 C 0.5468(3) 0.5005(3) 0.41922(9) 0.0157(5) Uani 1 1 d . . .
H49 H 0.6032 0.4207 0.4375 0.019 Uiso 1 1 calc R . .
H50 H 0.6167 0.5471 0.4112 0.019 Uiso 1 1 calc R . .
C29 C 0.4036(3) 0.5861(2) 0.44872(9) 0.0162(5) Uani 1 1 d . . .
H51 H 0.4367 0.6253 0.4725 0.019 Uiso 1 1 calc R . .
H52 H 0.3505 0.5319 0.4647 0.019 Uiso 1 1 calc R . .
C30 C 0.2873(3) 0.6967(2) 0.41830(8) 0.0132(5) Uani 1 1 d . . .
Si7 Si 0.67671(8) 0.43003(7) 0.32895(2) 0.01768(17) Uani 1 1 d . . .
C31 C 0.6480(3) 0.3617(3) 0.27627(9) 0.0265(6) Uani 1 1 d . . .
H53 H 0.5469 0.4158 0.2653 0.040 Uiso 1 1 calc R . .
H54 H 0.6527 0.2738 0.2837 0.040 Uiso 1 1 calc R . .
H55 H 0.7293 0.3598 0.2521 0.040 Uiso 1 1 calc R . .
C32 C 0.8618(3) 0.3178(3) 0.35360(10) 0.0294(7) Uani 1 1 d . . .
H56 H 0.8674 0.2289 0.3547 0.044 Uiso 1 1 calc R . .
H57 H 0.8642 0.3422 0.3848 0.044 Uiso 1 1 calc R . .
H58 H 0.9500 0.3241 0.3341 0.044 Uiso 1 1 calc R . .
C33 C 0.7157(3) 0.5804(3) 0.31354(10) 0.0255(6) Uani 1 1 d . . .
H59 H 0.7912 0.5660 0.2867 0.038 Uiso 1 1 calc R . .
H60 H 0.7570 0.6019 0.3397 0.038 Uiso 1 1 calc R . .
H61 H 0.6194 0.6520 0.3062 0.038 Uiso 1 1 calc R . .
Si8 Si 0.45635(8) 0.31190(7) 0.38622(3) 0.01793(17) Uani 1 1 d . . .
C34 C 0.6357(3) 0.1627(3) 0.38676(10) 0.0272(7) Uani 1 1 d . . .
H62 H 0.6092 0.0883 0.3972 0.041 Uiso 1 1 calc R . .
H63 H 0.7049 0.1715 0.4078 0.041 Uiso 1 1 calc R . .
H64 H 0.6875 0.1497 0.3556 0.041 Uiso 1 1 calc R . .
C35 C 0.3614(3) 0.3028(3) 0.44587(10) 0.0276(7) Uani 1 1 d . . .
H65 H 0.3457 0.2214 0.4506 0.041 Uiso 1 1 calc R . .
H66 H 0.2614 0.3756 0.4491 0.041 Uiso 1 1 calc R . .
H67 H 0.4278 0.3067 0.4688 0.041 Uiso 1 1 calc R . .
C36 C 0.3316(4) 0.2919(3) 0.34454(11) 0.0322(7) Uani 1 1 d . . .
H68 H 0.3676 0.3108 0.3131 0.048 Uiso 1 1 calc R . .
H69 H 0.2246 0.3515 0.3513 0.048 Uiso 1 1 calc R . .
H70 H 0.3371 0.2029 0.3473 0.048 Uiso 1 1 calc R . .
Si9 Si 0.33016(8) 0.84827(7) 0.41965(2) 0.01859(17) Uani 1 1 d . . .
C37 C 0.5422(3) 0.8116(3) 0.41134(11) 0.0327(7) Uani 1 1 d . . .
H71 H 0.5602 0.8905 0.4144 0.049 Uiso 1 1 calc R . .
H72 H 0.5820 0.7791 0.3805 0.049 Uiso 1 1 calc R . .
H73 H 0.5955 0.7460 0.4347 0.049 Uiso 1 1 calc R . .
C38 C 0.2679(3) 0.9198(3) 0.47777(10) 0.0261(6) Uani 1 1 d . . .
H74 H 0.3091 0.8522 0.5019 0.039 Uiso 1 1 calc R . .
H75 H 0.1548 0.9566 0.4821 0.039 Uiso 1 1 calc R . .
H76 H 0.3072 0.9878 0.4797 0.039 Uiso 1 1 calc R . .
C39 C 0.2344(4) 0.9816(3) 0.37610(10) 0.0339(8) Uani 1 1 d . . .
H77 H 0.2166 1.0652 0.3882 0.051 Uiso 1 1 calc R . .
H78 H 0.1355 0.9791 0.3700 0.051 Uiso 1 1 calc R . .
H79 H 0.3014 0.9698 0.3474 0.051 Uiso 1 1 calc R . .
Si10 Si 0.08126(8) 0.72566(7) 0.44230(2) 0.01674(16) Uani 1 1 d . . .
C40 C 0.0672(3) 0.7164(3) 0.50707(9) 0.0268(7) Uani 1 1 d . . .
H80 H 0.1013 0.7800 0.5180 0.040 Uiso 1 1 calc R . .
H81 H 0.1331 0.6296 0.5181 0.040 Uiso 1 1 calc R . .
H82 H -0.0401 0.7349 0.5188 0.040 Uiso 1 1 calc R . .
C41 C 0.0077(3) 0.6037(3) 0.42533(11) 0.0280(7) Uani 1 1 d . . .
H83 H -0.0538 0.5828 0.4516 0.042 Uiso 1 1 calc R . .
H84 H 0.0954 0.5251 0.4162 0.042 Uiso 1 1 calc R . .
H85 H -0.0567 0.6398 0.3994 0.042 Uiso 1 1 calc R . .
C42 C -0.0606(3) 0.8861(3) 0.42226(10) 0.0245(6) Uani 1 1 d . . .
H86 H -0.1653 0.8948 0.4340 0.037 Uiso 1 1 calc R . .
H87 H -0.0537 0.8927 0.3885 0.037 Uiso 1 1 calc R . .
H88 H -0.0371 0.9551 0.4338 0.037 Uiso 1 1 calc R . .
O1 O -0.1258(2) 0.9758(2) 0.29468(7) 0.0283(5) Uani 1 1 d . . .
C43 C -0.0460(4) 0.9753(3) 0.25042(10) 0.0344(8) Uani 1 1 d . . .
H89 H -0.1206 1.0086 0.2265 0.041 Uiso 1 1 calc R . .
H90 H 0.0249 0.8861 0.2433 0.041 Uiso 1 1 calc R . .
C44 C 0.0437(4) 1.0593(3) 0.25078(11) 0.0373(8) Uani 1 1 d . . .
H91 H -0.0275 1.1479 0.2568 0.056 Uiso 1 1 calc R . .
H92 H 0.1016 1.0582 0.2208 0.056 Uiso 1 1 calc R . .
H93 H 0.1159 1.0267 0.2750 0.056 Uiso 1 1 calc R . .
C45 C -0.2197(3) 0.9010(3) 0.29768(10) 0.0287(7) Uani 1 1 d . . .
H94 H -0.2410 0.8789 0.3305 0.034 Uiso 1 1 calc R . .
H95 H -0.1613 0.8192 0.2821 0.034 Uiso 1 1 calc R . .
C46 C -0.3716(4) 0.9701(3) 0.27617(12) 0.0373(8) Uani 1 1 d . . .
H96 H -0.4265 1.0544 0.2896 0.056 Uiso 1 1 calc R . .
H97 H -0.4349 0.9182 0.2822 0.056 Uiso 1 1 calc R . .
H98 H -0.3519 0.9824 0.2428 0.056 Uiso 1 1 calc R . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Si1 C1 1.858(2) . ?
Si1 C10 1.871(2) . ?
Si1 C11 1.919(3) . ?
Si1 C14 1.921(3) . ?
C1 C2 1.343(4) . ?
C2 C3 1.477(3) . ?
C3 C4 1.357(4) . ?
C3 C9 1.490(3) . ?
C4 C5 1.467(4) . ?
C5 C6 1.546(3) . ?
C5 Si2 1.894(2) . ?
C6 C7 1.463(4) . ?
C6 Si2 1.898(2) . ?
C7 C8 1.337(4) . ?
C8 C9 1.479(3) . ?
C9 C10 1.354(4) . ?
Si2 C27 1.894(3) . ?
Si2 C30 1.897(3) . ?
C11 C12 1.574(3) . ?
C11 Si3 1.917(2) . ?
C11 Si4 1.922(2) . ?
C12 C13 1.542(4) . ?
C13 C14 1.578(4) . ?
C14 Si5 1.910(3) . ?
C14 Si6 1.921(2) . ?
Si3 C15 1.877(3) . ?
Si3 C16 1.878(3) . ?
Si3 C17 1.879(2) . ?
Si4 C19 1.878(3) . ?
Si4 C20 1.882(3) . ?
Si4 C18 1.891(3) . ?
Si5 C21 1.874(3) . ?
Si5 C22 1.874(3) . ?
Si5 C23 1.884(3) . ?
Si6 C25 1.869(3) . ?
Si6 C24 1.876(3) . ?
Si6 C26 1.885(3) . ?
C27 C28 1.579(3) . ?
C27 Si8 1.914(2) . ?
C27 Si7 1.919(2) . ?
C28 C29 1.541(4) . ?
C29 C30 1.579(3) . ?
C30 Si10 1.905(2) . ?
C30 Si9 1.906(2) . ?
Si7 C31 1.867(3) . ?
Si7 C33 1.877(3) . ?
Si7 C32 1.885(3) . ?
Si8 C34 1.862(3) . ?
Si8 C36 1.864(3) . ?
Si8 C35 1.885(3) . ?
Si9 C37 1.871(3) . ?
Si9 C38 1.878(3) . ?
Si9 C39 1.882(3) . ?
Si10 C42 1.869(3) . ?
Si10 C40 1.878(3) . ?
Si10 C41 1.883(3) . ?
O1 C43 1.424(3) . ?
O1 C45 1.432(3) . ?
C43 C44 1.495(4) . ?
C45 C46 1.514(4) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 Si1 C10 98.13(11) . . ?
C1 Si1 C11 113.82(11) . . ?
C10 Si1 C11 120.20(11) . . ?
C1 Si1 C14 116.99(11) . . ?
C10 Si1 C14 110.55(11) . . ?
C11 Si1 C14 98.32(11) . . ?
C2 C1 Si1 121.11(17) . . ?
C1 C2 C3 129.3(2) . . ?
C4 C3 C2 113.7(2) . . ?
C4 C3 C9 127.0(2) . . ?
C2 C3 C9 119.4(2) . . ?
C3 C4 C5 135.4(2) . . ?
C4 C5 C6 125.1(2) . . ?
C4 C5 Si2 125.44(19) . . ?
C6 C5 Si2 66.06(13) . . ?
C7 C6 C5 122.2(2) . . ?
C7 C6 Si2 131.6(2) . . ?
C5 C6 Si2 65.81(12) . . ?
C8 C7 C6 132.6(2) . . ?
C7 C8 C9 133.5(2) . . ?
C10 C9 C8 115.6(2) . . ?
C10 C9 C3 121.2(2) . . ?
C8 C9 C3 123.2(2) . . ?
C9 C10 Si1 127.21(17) . . ?
C5 Si2 C27 132.08(12) . . ?
C5 Si2 C30 118.42(11) . . ?
C27 Si2 C30 101.30(11) . . ?
C5 Si2 C6 48.13(10) . . ?
C27 Si2 C6 131.82(12) . . ?
C30 Si2 C6 118.81(12) . . ?
C12 C11 Si3 113.74(15) . . ?
C12 C11 Si1 101.50(17) . . ?
Si3 C11 Si1 111.99(12) . . ?
C12 C11 Si4 107.46(16) . . ?
Si3 C11 Si4 107.28(13) . . ?
Si1 C11 Si4 114.89(12) . . ?
C13 C12 C11 109.9(2) . . ?
C12 C13 C14 109.80(19) . . ?
C13 C14 Si5 111.23(15) . . ?
C13 C14 Si1 100.52(16) . . ?
Si5 C14 Si1 112.19(12) . . ?
C13 C14 Si6 108.36(15) . . ?
Si5 C14 Si6 107.72(13) . . ?
Si1 C14 Si6 116.63(11) . . ?
C15 Si3 C16 107.02(14) . . ?
C15 Si3 C17 102.93(13) . . ?
C16 Si3 C17 108.35(12) . . ?
C15 Si3 C11 114.25(12) . . ?
C16 Si3 C11 111.78(11) . . ?
C17 Si3 C11 111.97(11) . . ?
C19 Si4 C20 106.41(12) . . ?
C19 Si4 C18 108.06(13) . . ?
C20 Si4 C18 101.72(13) . . ?
C19 Si4 C11 112.52(11) . . ?
C20 Si4 C11 115.89(12) . . ?
C18 Si4 C11 111.44(11) . . ?
C21 Si5 C22 105.10(13) . . ?
C21 Si5 C23 103.97(12) . . ?
C22 Si5 C23 108.02(14) . . ?
C21 Si5 C14 113.04(12) . . ?
C22 Si5 C14 114.00(11) . . ?
C23 Si5 C14 111.99(12) . . ?
C25 Si6 C24 102.78(13) . . ?
C25 Si6 C26 108.30(15) . . ?
C24 Si6 C26 102.78(12) . . ?
C25 Si6 C14 113.43(12) . . ?
C24 Si6 C14 119.14(12) . . ?
C26 Si6 C14 109.47(11) . . ?
C28 C27 Si2 98.75(16) . . ?
C28 C27 Si8 108.89(15) . . ?
Si2 C27 Si8 117.16(12) . . ?
C28 C27 Si7 107.43(14) . . ?
Si2 C27 Si7 113.00(12) . . ?
Si8 C27 Si7 110.51(13) . . ?
C29 C28 C27 112.02(19) . . ?
C28 C29 C30 111.5(2) . . ?
C29 C30 Si2 100.86(17) . . ?
C29 C30 Si10 109.11(15) . . ?
Si2 C30 Si10 112.00(12) . . ?
C29 C30 Si9 108.22(15) . . ?
Si2 C30 Si9 114.67(12) . . ?
Si10 C30 Si9 111.29(13) . . ?
C31 Si7 C33 110.74(13) . . ?
C31 Si7 C32 109.72(14) . . ?
C33 Si7 C32 102.22(13) . . ?
C31 Si7 C27 111.09(12) . . ?
C33 Si7 C27 110.90(12) . . ?
C32 Si7 C27 111.85(11) . . ?
C34 Si8 C36 107.70(14) . . ?
C34 Si8 C35 102.09(13) . . ?
C36 Si8 C35 107.26(14) . . ?
C34 Si8 C27 111.45(11) . . ?
C36 Si8 C27 113.84(11) . . ?
C35 Si8 C27 113.68(12) . . ?
C37 Si9 C38 104.76(14) . . ?
C37 Si9 C39 107.09(14) . . ?
C38 Si9 C39 106.44(14) . . ?
C37 Si9 C30 111.79(12) . . ?
C38 Si9 C30 110.65(11) . . ?
C39 Si9 C30 115.42(12) . . ?
C42 Si10 C40 108.57(14) . . ?
C42 Si10 C41 105.29(13) . . ?
C40 Si10 C41 105.69(13) . . ?
C42 Si10 C30 112.33(11) . . ?
C40 Si10 C30 110.53(11) . . ?
C41 Si10 C30 114.02(12) . . ?
C43 O1 C45 113.0(2) . . ?
O1 C43 C44 108.5(3) . . ?
O1 C45 C46 113.4(2) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C10 Si1 C1 C2 14.7(2) . . . . ?
C11 Si1 C1 C2 142.9(2) . . . . ?
C14 Si1 C1 C2 -103.4(2) . . . . ?
Si1 C1 C2 C3 -1.5(4) . . . . ?
C1 C2 C3 C4 166.5(3) . . . . ?
C1 C2 C3 C9 -14.1(4) . . . . ?
C2 C3 C4 C5 176.7(3) . . . . ?
C9 C3 C4 C5 -2.7(5) . . . . ?
C3 C4 C5 C6 -7.3(5) . . . . ?
C3 C4 C5 Si2 -91.1(4) . . . . ?
C4 C5 C6 C7 7.6(4) . . . . ?
Si2 C5 C6 C7 125.2(3) . . . . ?
C4 C5 C6 Si2 -117.6(3) . . . . ?
C5 C6 C7 C8 -1.2(5) . . . . ?
Si2 C6 C7 C8 83.8(4) . . . . ?
C6 C7 C8 C9 -0.8(5) . . . . ?
C7 C8 C9 C10 174.0(3) . . . . ?
C7 C8 C9 C3 -5.4(4) . . . . ?
C4 C3 C9 C10 -170.2(3) . . . . ?
C2 C3 C9 C10 10.4(4) . . . . ?
C4 C3 C9 C8 9.2(4) . . . . ?
C2 C3 C9 C8 -170.2(2) . . . . ?
C8 C9 C10 Si1 -171.77(18) . . . . ?
C3 C9 C10 Si1 7.7(4) . . . . ?
C1 Si1 C10 C9 -18.4(3) . . . . ?
C11 Si1 C10 C9 -142.1(2) . . . . ?
C14 Si1 C10 C9 104.5(2) . . . . ?
C4 C5 Si2 C27 3.8(3) . . . . ?
C6 C5 Si2 C27 -113.40(17) . . . . ?
C4 C5 Si2 C30 -138.3(2) . . . . ?
C6 C5 Si2 C30 104.53(16) . . . . ?
C4 C5 Si2 C6 117.2(3) . . . . ?
C7 C6 Si2 C5 -112.5(3) . . . . ?
C7 C6 Si2 C27 1.4(3) . . . . ?
C5 C6 Si2 C27 113.93(17) . . . . ?
C7 C6 Si2 C30 143.8(2) . . . . ?
C5 C6 Si2 C30 -103.68(16) . . . . ?
C1 Si1 C11 C12 134.42(14) . . . . ?
C10 Si1 C11 C12 -109.74(15) . . . . ?
C14 Si1 C11 C12 9.97(15) . . . . ?
C1 Si1 C11 Si3 -103.89(13) . . . . ?
C10 Si1 C11 Si3 11.94(17) . . . . ?
C14 Si1 C11 Si3 131.65(12) . . . . ?
C1 Si1 C11 Si4 18.83(17) . . . . ?
C10 Si1 C11 Si4 134.66(12) . . . . ?
C14 Si1 C11 Si4 -105.63(13) . . . . ?
Si3 C11 C12 C13 -154.71(16) . . . . ?
Si1 C11 C12 C13 -34.3(2) . . . . ?
Si4 C11 C12 C13 86.7(2) . . . . ?
C11 C12 C13 C14 50.7(2) . . . . ?
C12 C13 C14 Si5 -157.02(16) . . . . ?
C12 C13 C14 Si1 -38.06(19) . . . . ?
C12 C13 C14 Si6 84.8(2) . . . . ?
C1 Si1 C14 C13 -106.96(16) . . . . ?
C10 Si1 C14 C13 141.91(14) . . . . ?
C11 Si1 C14 C13 15.21(15) . . . . ?
C1 Si1 C14 Si5 11.30(18) . . . . ?
C10 Si1 C14 Si5 -99.83(13) . . . . ?
C11 Si1 C14 Si5 133.46(12) . . . . ?
C1 Si1 C14 Si6 136.20(14) . . . . ?
C10 Si1 C14 Si6 25.07(18) . . . . ?
C11 Si1 C14 Si6 -101.63(14) . . . . ?
C12 C11 Si3 C15 -76.7(2) . . . . ?
Si1 C11 Si3 C15 168.97(12) . . . . ?
Si4 C11 Si3 C15 42.02(16) . . . . ?
C12 C11 Si3 C16 161.62(18) . . . . ?
Si1 C11 Si3 C16 47.26(16) . . . . ?
Si4 C11 Si3 C16 -79.69(15) . . . . ?
C12 C11 Si3 C17 39.8(2) . . . . ?
Si1 C11 Si3 C17 -74.53(15) . . . . ?
Si4 C11 Si3 C17 158.53(13) . . . . ?
C12 C11 Si4 C19 172.58(17) . . . . ?
Si3 C11 Si4 C19 49.90(17) . . . . ?
Si1 C11 Si4 C19 -75.31(17) . . . . ?
C12 C11 Si4 C20 -64.7(2) . . . . ?
Si3 C11 Si4 C20 172.67(13) . . . . ?
Si1 C11 Si4 C20 47.45(18) . . . . ?
C12 C11 Si4 C18 51.0(2) . . . . ?
Si3 C11 Si4 C18 -71.67(15) . . . . ?
Si1 C11 Si4 C18 163.12(13) . . . . ?
C13 C14 Si5 C21 51.8(2) . . . . ?
Si1 C14 Si5 C21 -59.87(17) . . . . ?
Si6 C14 Si5 C21 170.46(12) . . . . ?
C13 C14 Si5 C22 171.79(17) . . . . ?
Si1 C14 Si5 C22 60.08(16) . . . . ?
Si6 C14 Si5 C22 -69.60(16) . . . . ?
C13 C14 Si5 C23 -65.2(2) . . . . ?
Si1 C14 Si5 C23 -176.91(13) . . . . ?
Si6 C14 Si5 C23 53.42(16) . . . . ?
C13 C14 Si6 C25 160.89(17) . . . . ?
Si5 C14 Si6 C25 40.45(17) . . . . ?
Si1 C14 Si6 C25 -86.69(18) . . . . ?
C13 C14 Si6 C24 -77.9(2) . . . . ?
Si5 C14 Si6 C24 161.62(13) . . . . ?
Si1 C14 Si6 C24 34.5(2) . . . . ?
C13 C14 Si6 C26 39.8(2) . . . . ?
Si5 C14 Si6 C26 -80.63(16) . . . . ?
Si1 C14 Si6 C26 152.24(15) . . . . ?
C5 Si2 C27 C28 -164.47(13) . . . . ?
C30 Si2 C27 C28 -17.93(14) . . . . ?
C6 Si2 C27 C28 129.03(15) . . . . ?
C5 Si2 C27 Si8 -47.9(2) . . . . ?
C30 Si2 C27 Si8 98.63(14) . . . . ?
C6 Si2 C27 Si8 -114.42(15) . . . . ?
C5 Si2 C27 Si7 82.29(16) . . . . ?
C30 Si2 C27 Si7 -131.16(12) . . . . ?
C6 Si2 C27 Si7 15.8(2) . . . . ?
Si2 C27 C28 C29 36.5(2) . . . . ?
Si8 C27 C28 C29 -86.2(2) . . . . ?
Si7 C27 C28 C29 154.05(16) . . . . ?
C27 C28 C29 C30 -44.6(2) . . . . ?
C28 C29 C30 Si2 26.1(2) . . . . ?
C28 C29 C30 Si10 144.15(17) . . . . ?
C28 C29 C30 Si9 -94.6(2) . . . . ?
C5 Si2 C30 C29 148.64(13) . . . . ?
C27 Si2 C30 C29 -3.64(15) . . . . ?
C6 Si2 C30 C29 -156.01(13) . . . . ?
C5 Si2 C30 Si10 32.72(16) . . . . ?
C27 Si2 C30 Si10 -119.56(12) . . . . ?
C6 Si2 C30 Si10 88.07(14) . . . . ?
C5 Si2 C30 Si9 -95.35(14) . . . . ?
C27 Si2 C30 Si9 112.38(13) . . . . ?
C6 Si2 C30 Si9 -39.99(17) . . . . ?
C28 C27 Si7 C31 171.71(16) . . . . ?
Si2 C27 Si7 C31 -80.45(16) . . . . ?
Si8 C27 Si7 C31 53.05(16) . . . . ?
C28 C27 Si7 C33 -64.67(19) . . . . ?
Si2 C27 Si7 C33 43.17(17) . . . . ?
Si8 C27 Si7 C33 176.66(12) . . . . ?
C28 C27 Si7 C32 48.7(2) . . . . ?
Si2 C27 Si7 C32 156.57(14) . . . . ?
Si8 C27 Si7 C32 -69.93(16) . . . . ?
C28 C27 Si8 C34 -80.53(19) . . . . ?
Si2 C27 Si8 C34 168.61(14) . . . . ?
Si7 C27 Si8 C34 37.25(17) . . . . ?
C28 C27 Si8 C36 157.42(18) . . . . ?
Si2 C27 Si8 C36 46.6(2) . . . . ?
Si7 C27 Si8 C36 -84.81(17) . . . . ?
C28 C27 Si8 C35 34.2(2) . . . . ?
Si2 C27 Si8 C35 -76.67(17) . . . . ?
Si7 C27 Si8 C35 151.97(13) . . . . ?
C29 C30 Si9 C37 45.0(2) . . . . ?
Si2 C30 Si9 C37 -66.72(17) . . . . ?
Si10 C30 Si9 C37 164.86(14) . . . . ?
C29 C30 Si9 C38 -71.39(19) . . . . ?
Si2 C30 Si9 C38 176.92(13) . . . . ?
Si10 C30 Si9 C38 48.50(16) . . . . ?
C29 C30 Si9 C39 167.68(17) . . . . ?
Si2 C30 Si9 C39 55.99(18) . . . . ?
Si10 C30 Si9 C39 -72.43(17) . . . . ?
C29 C30 Si10 C42 161.02(17) . . . . ?
Si2 C30 Si10 C42 -88.18(15) . . . . ?
Si9 C30 Si10 C42 41.66(17) . . . . ?
C29 C30 Si10 C40 39.6(2) . . . . ?
Si2 C30 Si10 C40 150.39(14) . . . . ?
Si9 C30 Si10 C40 -79.77(16) . . . . ?
C29 C30 Si10 C41 -79.30(19) . . . . ?
Si2 C30 Si10 C41 31.51(17) . . . . ?
Si9 C30 Si10 C41 161.34(13) . . . . ?
C45 O1 C43 C44 178.2(2) . . . . ?
C43 O1 C45 C46 -78.8(3) . . . . ?

_diffrn_measured_fraction_theta_max 0.974
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.974
_refine_diff_density_max         0.494
_refine_diff_density_min         -0.346
_refine_diff_density_rms         0.058
_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_si337a_a
_database_code_depnum_ccdc_archive 'CCDC 1060709'
_audit_update_record             
;
2015-04-21 deposited with the CCDC.
2015-05-20 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        'bicyclic heptafulvene'
_chemical_name_common            ?
_chemical_melting_point          402-403
_chemical_formula_moiety         'C31 H58 Si5'
_chemical_formula_sum            'C31 H58 Si5'
_chemical_formula_weight         571.22

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'

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   P-1

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

_cell_length_a                   9.5864(15)
_cell_length_b                   10.9534(17)
_cell_length_c                   18.638(3)
_cell_angle_alpha                105.877(2)
_cell_angle_beta                 92.815(2)
_cell_angle_gamma                110.499(2)
_cell_volume                     1740.3(5)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9953
_cell_measurement_theta_min      2.30
_cell_measurement_theta_max      27.78

_exptl_crystal_description       plate
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.090
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             628
_exptl_absorpt_coefficient_mu    0.223
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.9360
_exptl_absorpt_correction_T_max  0.9780
_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_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            16560
_diffrn_reflns_av_R_equivalents  0.0298
_diffrn_reflns_av_sigmaI/netI    0.0317
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         1.15
_diffrn_reflns_theta_max         25.00
_reflns_number_total             6099
_reflns_number_gt                5531
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'APEX2 (Bruker AXS, 2006)'
_computing_cell_refinement       'APEX2 (Bruker AXS, 2006)'
_computing_data_reduction        'SAINT (Bruker AXS, 2004)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'XSHEL (Bruker AXS,2002)'
_computing_publication_material  'XCIF (Bruker AXS, 2001)'

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0551P)²+0.7140P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         6099
_refine_ls_number_parameters     341
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0382
_refine_ls_R_factor_gt           0.0348
_refine_ls_wR_factor_ref         0.0980
_refine_ls_wR_factor_gt          0.0954
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_restrained_S_all      1.043
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Si1 Si 0.79377(4) 0.08325(4) 0.23454(2) 0.01384(11) Uani 1 1 d . . .
C1 C 0.91800(17) -0.00284(15) 0.25712(8) 0.0165(3) Uani 1 1 d . . .
H1 H 0.9849 -0.0195 0.2232 0.020 Uiso 1 1 calc R . .
C2 C 0.91788(16) -0.04288(14) 0.31923(8) 0.0160(3) Uani 1 1 d . . .
C3 C 0.82772(16) -0.01286(15) 0.37970(8) 0.0162(3) Uani 1 1 d . . .
C4 C 0.78310(16) 0.10755(14) 0.38982(8) 0.0157(3) Uani 1 1 d . . .
C5 C 0.76456(17) 0.15580(15) 0.33186(8) 0.0165(3) Uani 1 1 d . . .
H2 H 0.7346 0.2320 0.3419 0.020 Uiso 1 1 calc R . .
C6 C 0.78715(17) -0.10329(16) 0.41985(8) 0.0193(3) Uani 1 1 d . . .
H3 H 0.8275 -0.1728 0.4067 0.023 Uiso 1 1 calc R . .
C7 C 0.69513(18) -0.11407(16) 0.47832(9) 0.0210(3) Uani 1 1 d . . .
C8 C 0.66676(18) -0.00867(17) 0.52315(9) 0.0224(3) Uani 1 1 d . . .
H4 H 0.6031 -0.0291 0.5593 0.027 Uiso 1 1 calc R . .
C9 C 0.72184(18) 0.13100(17) 0.52250(9) 0.0218(3) Uani 1 1 d . . .
H5 H 0.7217 0.1961 0.5682 0.026 Uiso 1 1 calc R . .
C10 C 0.77376(17) 0.18470(15) 0.46752(8) 0.0189(3) Uani 1 1 d . . .
C11 C 1.00771(19) -0.12937(17) 0.32700(9) 0.0239(4) Uani 1 1 d . . .
H6 H 1.0805 -0.1227 0.2917 0.036 Uiso 1 1 calc R . .
H7 H 0.9391 -0.2252 0.3155 0.036 Uiso 1 1 calc R . .
H8 H 1.0617 -0.0962 0.3788 0.036 Uiso 1 1 calc R . .
C12 C 0.6384(2) -0.25296(17) 0.49222(10) 0.0280(4) Uani 1 1 d . . .
H9 H 0.5741 -0.2474 0.5327 0.034 Uiso 1 1 calc R . .
C13 C 0.5404(2) -0.36777(18) 0.42205(11) 0.0346(4) Uani 1 1 d . . .
H10 H 0.6003 -0.3755 0.3811 0.052 Uiso 1 1 calc R . .
H11 H 0.4545 -0.3470 0.4062 0.052 Uiso 1 1 calc R . .
H12 H 0.5034 -0.4546 0.4337 0.052 Uiso 1 1 calc R . .
C14 C 0.7698(2) -0.2858(2) 0.52106(12) 0.0391(5) Uani 1 1 d . . .
H13 H 0.8312 -0.2108 0.5660 0.059 Uiso 1 1 calc R . .
H14 H 0.8323 -0.2965 0.4815 0.059 Uiso 1 1 calc R . .
H15 H 0.7297 -0.3711 0.5340 0.059 Uiso 1 1 calc R . .
C15 C 0.8191(2) 0.33768(16) 0.48377(9) 0.0284(4) Uani 1 1 d . . .
H16 H 0.8299 0.3815 0.5382 0.043 Uiso 1 1 calc R . .
H17 H 0.7414 0.3555 0.4570 0.043 Uiso 1 1 calc R . .
H18 H 0.9155 0.3752 0.4665 0.043 Uiso 1 1 calc R . .
C16 C 0.61919(17) -0.04054(15) 0.16131(8) 0.0166(3) Uani 1 1 d . . .
C17 C 0.61413(18) 0.04957(16) 0.10890(8) 0.0199(3) Uani 1 1 d . . .
H19 H 0.5574 -0.0106 0.0582 0.024 Uiso 1 1 calc R . .
H20 H 0.5615 0.1110 0.1306 0.024 Uiso 1 1 calc R . .
C18 C 0.77514(18) 0.13550(16) 0.10172(8) 0.0200(3) Uani 1 1 d . . .
H21 H 0.7721 0.2015 0.0751 0.024 Uiso 1 1 calc R . .
H22 H 0.8215 0.0748 0.0718 0.024 Uiso 1 1 calc R . .
C19 C 0.87276(17) 0.21553(15) 0.18268(8) 0.0169(3) Uani 1 1 d . . .
Si2 Si 0.43913(5) -0.08595(4) 0.20468(2) 0.01930(12) Uani 1 1 d . . .
C20 C 0.2692(2) -0.19926(19) 0.13018(10) 0.0320(4) Uani 1 1 d . . .
H23 H 0.2665 -0.1571 0.0903 0.048 Uiso 1 1 calc R . .
H24 H 0.1774 -0.2106 0.1530 0.048 Uiso 1 1 calc R . .
H25 H 0.2752 -0.2891 0.1084 0.048 Uiso 1 1 calc R . .
C21 C 0.4394(2) -0.17198(18) 0.27897(10) 0.0276(4) Uani 1 1 d . . .
H26 H 0.3506 -0.1774 0.3038 0.041 Uiso 1 1 calc R . .
H27 H 0.5311 -0.1188 0.3166 0.041 Uiso 1 1 calc R . .
H28 H 0.4367 -0.2647 0.2554 0.041 Uiso 1 1 calc R . .
C22 C 0.39625(19) 0.06798(17) 0.25254(10) 0.0273(4) Uani 1 1 d . . .
H29 H 0.2970 0.0383 0.2683 0.041 Uiso 1 1 calc R . .
H30 H 0.3959 0.1200 0.2174 0.041 Uiso 1 1 calc R . .
H31 H 0.4734 0.1262 0.2970 0.041 Uiso 1 1 calc R . .
Si3 Si 0.63527(5) -0.20644(4) 0.10197(2) 0.02139(12) Uani 1 1 d . . .
C23 C 0.5827(2) -0.34223(18) 0.14895(12) 0.0366(5) Uani 1 1 d . . .
H32 H 0.6430 -0.3065 0.1995 0.055 Uiso 1 1 calc R . .
H33 H 0.6019 -0.4216 0.1188 0.055 Uiso 1 1 calc R . .
H34 H 0.4753 -0.3702 0.1533 0.055 Uiso 1 1 calc R . .
C24 C 0.8220(2) -0.20158(17) 0.07420(10) 0.0287(4) Uani 1 1 d . . .
H35 H 0.8077 -0.2877 0.0353 0.043 Uiso 1 1 calc R . .
H36 H 0.8905 -0.1897 0.1185 0.043 Uiso 1 1 calc R . .
H37 H 0.8652 -0.1248 0.0542 0.043 Uiso 1 1 calc R . .
C25 C 0.5118(3) -0.2712(2) 0.00701(11) 0.0463(5) Uani 1 1 d . . .
H38 H 0.4117 -0.2698 0.0141 0.069 Uiso 1 1 calc R . .
H39 H 0.5022 -0.3652 -0.0189 0.069 Uiso 1 1 calc R . .
H40 H 0.5573 -0.2122 -0.0235 0.069 Uiso 1 1 calc R . .
Si4 Si 1.08433(5) 0.25991(4) 0.18196(2) 0.02038(12) Uani 1 1 d . . .
C26 C 1.12726(19) 0.11800(17) 0.11683(9) 0.0251(4) Uani 1 1 d . . .
H41 H 1.2355 0.1499 0.1144 0.038 Uiso 1 1 calc R . .
H42 H 1.0702 0.0909 0.0662 0.038 Uiso 1 1 calc R . .
H43 H 1.0985 0.0391 0.1359 0.038 Uiso 1 1 calc R . .
C27 C 1.1915(2) 0.30557(18) 0.27867(10) 0.0297(4) Uani 1 1 d . . .
H44 H 1.1845 0.3893 0.3115 0.045 Uiso 1 1 calc R . .
H45 H 1.2977 0.3209 0.2752 0.045 Uiso 1 1 calc R . .
H46 H 1.1485 0.2304 0.2998 0.045 Uiso 1 1 calc R . .
C28 C 1.1785(2) 0.40706(18) 0.14536(12) 0.0346(4) Uani 1 1 d . . .
H47 H 1.2833 0.4169 0.1417 0.052 Uiso 1 1 calc R . .
H48 H 1.1767 0.4916 0.1800 0.052 Uiso 1 1 calc R . .
H49 H 1.1247 0.3895 0.0952 0.052 Uiso 1 1 calc R . .
Si5 Si 0.84410(5) 0.38457(4) 0.22005(2) 0.02067(12) Uani 1 1 d . . .
C29 C 0.6518(2) 0.37535(18) 0.24102(11) 0.0295(4) Uani 1 1 d . . .
H50 H 0.6511 0.4681 0.2575 0.044 Uiso 1 1 calc R . .
H51 H 0.6269 0.3331 0.2811 0.044 Uiso 1 1 calc R . .
H52 H 0.5769 0.3201 0.1953 0.044 Uiso 1 1 calc R . .
C30 C 0.9759(2) 0.49759(17) 0.31065(10) 0.0298(4) Uani 1 1 d . . .
H53 H 0.9758 0.4431 0.3445 0.045 Uiso 1 1 calc R . .
H54 H 0.9425 0.5716 0.3349 0.045 Uiso 1 1 calc R . .
H55 H 1.0782 0.5370 0.2997 0.045 Uiso 1 1 calc R . .
C31 C 0.8718(2) 0.47909(18) 0.14820(10) 0.0315(4) Uani 1 1 d . . .
H56 H 0.9625 0.4776 0.1265 0.047 Uiso 1 1 calc R . .
H57 H 0.8836 0.5743 0.1727 0.047 Uiso 1 1 calc R . .
H58 H 0.7839 0.4346 0.1080 0.047 Uiso 1 1 calc R . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Si1 C5 1.8486(16) . ?
Si1 C1 1.8545(15) . ?
Si1 C16 1.9173(15) . ?
Si1 C19 1.9176(15) . ?
C1 C2 1.345(2) . ?
C2 C3 1.489(2) . ?
C2 C11 1.515(2) . ?
C3 C6 1.363(2) . ?
C3 C4 1.492(2) . ?
C4 C5 1.355(2) . ?
C4 C10 1.488(2) . ?
C6 C7 1.439(2) . ?
C7 C8 1.349(2) . ?
C7 C12 1.525(2) . ?
C8 C9 1.437(2) . ?
C9 C10 1.349(2) . ?
C10 C15 1.512(2) . ?
C12 C13 1.525(2) . ?
C12 C14 1.537(3) . ?
C16 C17 1.5770(19) . ?
C16 Si2 1.9069(16) . ?
C16 Si3 1.9137(16) . ?
C17 C18 1.536(2) . ?
C18 C19 1.576(2) . ?
C19 Si5 1.9126(16) . ?
C19 Si4 1.9146(16) . ?
Si2 C22 1.8725(17) . ?
Si2 C21 1.8762(17) . ?
Si2 C20 1.8819(17) . ?
Si3 C23 1.8611(18) . ?
Si3 C24 1.8744(19) . ?
Si3 C25 1.8858(19) . ?
Si4 C28 1.8764(18) . ?
Si4 C27 1.8764(17) . ?
Si4 C26 1.8772(18) . ?
Si5 C29 1.8772(19) . ?
Si5 C30 1.8794(17) . ?
Si5 C31 1.8806(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 C1 97.83(7) . . ?
C5 Si1 C16 117.79(7) . . ?
C1 Si1 C16 112.45(7) . . ?
C5 Si1 C19 114.54(7) . . ?
C1 Si1 C19 116.75(7) . . ?
C16 Si1 C19 98.60(6) . . ?
C2 C1 Si1 123.13(12) . . ?
C1 C2 C3 123.62(13) . . ?
C1 C2 C11 118.83(14) . . ?
C3 C2 C11 117.48(13) . . ?
C6 C3 C2 116.02(14) . . ?
C6 C3 C4 125.04(14) . . ?
C2 C3 C4 118.87(12) . . ?
C5 C4 C10 119.20(13) . . ?
C5 C4 C3 122.02(13) . . ?
C10 C4 C3 118.49(12) . . ?
C4 C5 Si1 124.38(12) . . ?
C3 C6 C7 132.55(15) . . ?
C8 C7 C6 124.26(14) . . ?
C8 C7 C12 119.89(15) . . ?
C6 C7 C12 115.67(14) . . ?
C7 C8 C9 127.40(15) . . ?
C10 C9 C8 130.46(15) . . ?
C9 C10 C4 126.58(14) . . ?
C9 C10 C15 117.62(14) . . ?
C4 C10 C15 115.70(13) . . ?
C13 C12 C7 111.88(13) . . ?
C13 C12 C14 110.89(16) . . ?
C7 C12 C14 111.30(15) . . ?
C17 C16 Si2 110.25(10) . . ?
C17 C16 Si3 109.09(10) . . ?
Si2 C16 Si3 108.80(7) . . ?
C17 C16 Si1 100.56(9) . . ?
Si2 C16 Si1 112.75(8) . . ?
Si3 C16 Si1 115.06(8) . . ?
C18 C17 C16 110.01(12) . . ?
C17 C18 C19 109.82(12) . . ?
C18 C19 Si5 108.40(10) . . ?
C18 C19 Si4 112.91(11) . . ?
Si5 C19 Si4 107.32(7) . . ?
C18 C19 Si1 100.78(9) . . ?
Si5 C19 Si1 116.29(8) . . ?
Si4 C19 Si1 111.17(7) . . ?
C22 Si2 C21 104.38(8) . . ?
C22 Si2 C20 104.65(8) . . ?
C21 Si2 C20 107.65(8) . . ?
C22 Si2 C16 112.74(7) . . ?
C21 Si2 C16 115.29(7) . . ?
C20 Si2 C16 111.34(8) . . ?
C23 Si3 C24 103.37(8) . . ?
C23 Si3 C25 109.70(10) . . ?
C24 Si3 C25 101.80(9) . . ?
C23 Si3 C16 112.57(8) . . ?
C24 Si3 C16 119.16(7) . . ?
C25 Si3 C16 109.48(8) . . ?
C28 Si4 C27 106.17(9) . . ?
C28 Si4 C26 102.02(8) . . ?
C27 Si4 C26 108.16(8) . . ?
C28 Si4 C19 114.52(8) . . ?
C27 Si4 C19 112.18(8) . . ?
C26 Si4 C19 113.03(7) . . ?
C29 Si5 C30 104.91(9) . . ?
C29 Si5 C31 101.68(8) . . ?
C30 Si5 C31 109.52(8) . . ?
C29 Si5 C19 117.66(7) . . ?
C30 Si5 C19 111.36(7) . . ?
C31 Si5 C19 111.05(8) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C5 Si1 C1 C2 24.60(14) . . . . ?
C16 Si1 C1 C2 -99.87(13) . . . . ?
C19 Si1 C1 C2 147.21(12) . . . . ?
Si1 C1 C2 C3 -5.1(2) . . . . ?
Si1 C1 C2 C11 171.71(11) . . . . ?
C1 C2 C3 C6 152.91(14) . . . . ?
C11 C2 C3 C6 -23.95(19) . . . . ?
C1 C2 C3 C4 -24.5(2) . . . . ?
C11 C2 C3 C4 158.67(13) . . . . ?
C6 C3 C4 C5 -149.55(15) . . . . ?
C2 C3 C4 C5 27.6(2) . . . . ?
C6 C3 C4 C10 36.6(2) . . . . ?
C2 C3 C4 C10 -146.27(13) . . . . ?
C10 C4 C5 Si1 172.87(11) . . . . ?
C3 C4 C5 Si1 -0.9(2) . . . . ?
C1 Si1 C5 C4 -21.67(14) . . . . ?
C16 Si1 C5 C4 98.87(14) . . . . ?
C19 Si1 C5 C4 -145.89(13) . . . . ?
C2 C3 C6 C7 -175.94(15) . . . . ?
C4 C3 C6 C7 1.3(3) . . . . ?
C3 C6 C7 C8 -22.6(3) . . . . ?
C3 C6 C7 C12 162.17(16) . . . . ?
C6 C7 C8 C9 -0.8(3) . . . . ?
C12 C7 C8 C9 174.26(15) . . . . ?
C7 C8 C9 C10 22.0(3) . . . . ?
C8 C9 C10 C4 1.8(3) . . . . ?
C8 C9 C10 C15 177.89(16) . . . . ?
C5 C4 C10 C9 147.61(16) . . . . ?
C3 C4 C10 C9 -38.4(2) . . . . ?
C5 C4 C10 C15 -28.6(2) . . . . ?
C3 C4 C10 C15 145.43(14) . . . . ?
C8 C7 C12 C13 123.99(17) . . . . ?
C6 C7 C12 C13 -60.5(2) . . . . ?
C8 C7 C12 C14 -111.34(18) . . . . ?
C6 C7 C12 C14 64.16(19) . . . . ?
C5 Si1 C16 C17 110.82(10) . . . . ?
C1 Si1 C16 C17 -136.58(10) . . . . ?
C19 Si1 C16 C17 -12.86(11) . . . . ?
C5 Si1 C16 Si2 -6.57(10) . . . . ?
C1 Si1 C16 Si2 106.04(8) . . . . ?
C19 Si1 C16 Si2 -130.24(8) . . . . ?
C5 Si1 C16 Si3 -132.15(8) . . . . ?
C1 Si1 C16 Si3 -19.55(10) . . . . ?
C19 Si1 C16 Si3 104.17(8) . . . . ?
Si2 C16 C17 C18 155.83(11) . . . . ?
Si3 C16 C17 C18 -84.75(13) . . . . ?
Si1 C16 C17 C18 36.62(14) . . . . ?
C16 C17 C18 C19 -51.23(16) . . . . ?
C17 C18 C19 Si5 -86.39(12) . . . . ?
C17 C18 C19 Si4 154.85(10) . . . . ?
C17 C18 C19 Si1 36.19(13) . . . . ?
C5 Si1 C19 C18 -138.34(10) . . . . ?
C1 Si1 C19 C18 108.21(10) . . . . ?
C16 Si1 C19 C18 -12.37(11) . . . . ?
C5 Si1 C19 Si5 -21.45(11) . . . . ?
C1 Si1 C19 Si5 -134.89(8) . . . . ?
C16 Si1 C19 Si5 104.52(9) . . . . ?
C5 Si1 C19 Si4 101.74(9) . . . . ?
C1 Si1 C19 Si4 -11.71(10) . . . . ?
C16 Si1 C19 Si4 -132.29(8) . . . . ?
C17 C16 Si2 C22 -52.07(12) . . . . ?
Si3 C16 Si2 C22 -171.67(7) . . . . ?
Si1 C16 Si2 C22 59.43(10) . . . . ?
C17 C16 Si2 C21 -171.80(10) . . . . ?
Si3 C16 Si2 C21 68.60(9) . . . . ?
Si1 C16 Si2 C21 -60.30(10) . . . . ?
C17 C16 Si2 C20 65.20(12) . . . . ?
Si3 C16 Si2 C20 -54.40(10) . . . . ?
Si1 C16 Si2 C20 176.70(8) . . . . ?
C17 C16 Si3 C23 -162.11(11) . . . . ?
Si2 C16 Si3 C23 -41.79(10) . . . . ?
Si1 C16 Si3 C23 85.81(11) . . . . ?
C17 C16 Si3 C24 76.65(12) . . . . ?
Si2 C16 Si3 C24 -163.04(8) . . . . ?
Si1 C16 Si3 C24 -35.44(11) . . . . ?
C17 C16 Si3 C25 -39.81(14) . . . . ?
Si2 C16 Si3 C25 80.50(11) . . . . ?
Si1 C16 Si3 C25 -151.90(10) . . . . ?
C18 C19 Si4 C28 76.19(12) . . . . ?
Si5 C19 Si4 C28 -43.20(11) . . . . ?
Si1 C19 Si4 C28 -171.39(8) . . . . ?
C18 C19 Si4 C27 -162.71(10) . . . . ?
Si5 C19 Si4 C27 77.90(9) . . . . ?
Si1 C19 Si4 C27 -50.29(10) . . . . ?
C18 C19 Si4 C26 -40.09(12) . . . . ?
Si5 C19 Si4 C26 -159.48(7) . . . . ?
Si1 C19 Si4 C26 72.33(9) . . . . ?
C18 C19 Si5 C29 66.48(12) . . . . ?
Si4 C19 Si5 C29 -171.27(7) . . . . ?
Si1 C19 Si5 C29 -46.10(11) . . . . ?
C18 C19 Si5 C30 -172.39(11) . . . . ?
Si4 C19 Si5 C30 -50.14(10) . . . . ?
Si1 C19 Si5 C30 75.03(10) . . . . ?
C18 C19 Si5 C31 -50.04(12) . . . . ?
Si4 C19 Si5 C31 72.20(9) . . . . ?
Si1 C19 Si5 C31 -162.63(8) . . . . ?

_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max         0.458
_refine_diff_density_min         -0.335
_refine_diff_density_rms         0.050
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: hexane'
