# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2019

####################################################################### 
# 
# 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_tk17a
_database_code_depnum_ccdc_archive 'CCDC 1908502'
loop_
_audit_author_name
_audit_author_address
'Tomoyuki Kosai'
;Tohoku University
Japan
;
_audit_update_record             
;
2019-04-08 deposited with the CCDC.	2019-05-09 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          548
_chemical_formula_moiety         'C32 H80 Si12'
_chemical_formula_sum            'C32 H80 Si12'
_chemical_formula_weight         802.04

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

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

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

_cell_length_a                   9.2308(5)
_cell_length_b                   11.5172(6)
_cell_length_c                   13.2387(6)
_cell_angle_alpha                64.9580(10)
_cell_angle_beta                 75.3080(10)
_cell_angle_gamma                66.7880(10)
_cell_volume                     1165.54(10)
_cell_formula_units_Z            1
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    4909
_cell_measurement_theta_min      2.41
_cell_measurement_theta_max      29.22

_exptl_crystal_description       plate
_exptl_crystal_colour            orange
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.143
_exptl_crystal_F_000             440
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.030
_exptl_crystal_size_min          0.010
_exptl_absorpt_coefficient_mu    0.355
_shelx_estimated_absorpt_T_min   0.965
_shelx_estimated_absorpt_T_max   0.996
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.6536
_exptl_absorpt_correction_T_max  0.7459
_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            15586
_diffrn_reflns_av_unetI/netI     0.0424
_diffrn_reflns_av_R_equivalents  0.0397
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         1.707
_diffrn_reflns_theta_max         26.498
_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             4847
_reflns_number_gt                3837
_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)+(0.0458P)²] 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         4847
_refine_ls_number_parameters     211
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0485
_refine_ls_R_factor_gt           0.0333
_refine_ls_wR_factor_ref         0.0832
_refine_ls_wR_factor_gt          0.0787
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_restrained_S_all      1.012
_refine_ls_shift/su_max          0.018
_refine_ls_shift/su_mean         0.003

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 0.62575(6) 0.52673(5) 0.46361(4) 0.01483(13) Uani 1 1 d . . . . .
Si2 Si 0.54108(6) 0.45101(5) 0.65117(4) 0.00989(12) Uani 1 1 d . . . . .
Si3 Si 0.51277(6) 0.71782(5) 0.69924(4) 0.01414(12) Uani 1 1 d . . . . .
Si4 Si 0.24495(6) 0.58664(5) 0.79949(4) 0.01368(12) Uani 1 1 d . . . . .
Si5 Si 0.88331(6) 0.26021(5) 0.72742(4) 0.01442(12) Uani 1 1 d . . . . .
Si6 Si 0.63324(6) 0.12427(5) 0.75551(4) 0.01471(12) Uani 1 1 d . . . . .
C1 C 0.4664(2) 0.55173(17) 0.74906(14) 0.0112(4) Uani 1 1 d . . . . .
C2 C 0.5593(2) 0.44528(18) 0.85357(14) 0.0126(4) Uani 1 1 d . . . . .
H1 H 0.6620 0.4586 0.8449 0.015 Uiso 1 1 calc R U . . .
H2 H 0.4972 0.4606 0.9224 0.015 Uiso 1 1 calc R U . . .
C3 C 0.5892(2) 0.29942(17) 0.86588(14) 0.0131(4) Uani 1 1 d . . . . .
H3 H 0.4882 0.2794 0.8905 0.016 Uiso 1 1 calc R U . . .
H4 H 0.6630 0.2352 0.9234 0.016 Uiso 1 1 calc R U . . .
C4 C 0.6621(2) 0.28147(17) 0.75043(14) 0.0113(4) Uani 1 1 d . . . . .
C5 C 0.6030(3) 0.7153(2) 0.81269(17) 0.0266(5) Uani 1 1 d . . . . .
H5 H 0.7042 0.6410 0.8256 0.040 Uiso 1 1 calc R U . . .
H6 H 0.5308 0.7017 0.8820 0.040 Uiso 1 1 calc R U . . .
H7 H 0.6210 0.8017 0.7897 0.040 Uiso 1 1 calc R U . . .
C6 C 0.3382(2) 0.87750(19) 0.66853(17) 0.0230(4) Uani 1 1 d . . . . .
H8 H 0.3719 0.9543 0.6543 0.035 Uiso 1 1 calc R U . . .
H9 H 0.2571 0.8692 0.7329 0.035 Uiso 1 1 calc R U . . .
H10 H 0.2943 0.8925 0.6023 0.035 Uiso 1 1 calc R U . . .
C7 C 0.6537(2) 0.7550(2) 0.56984(16) 0.0226(4) Uani 1 1 d . . . . .
H11 H 0.6101 0.7623 0.5064 0.034 Uiso 1 1 calc R U . . .
H12 H 0.7556 0.6816 0.5812 0.034 Uiso 1 1 calc R U . . .
H13 H 0.6692 0.8408 0.5542 0.034 Uiso 1 1 calc R U . . .
C8 C 0.1821(2) 0.4322(2) 0.86899(17) 0.0216(4) Uani 1 1 d . . . . .
H14 H 0.0672 0.4593 0.8895 0.032 Uiso 1 1 calc R U . . .
H15 H 0.2363 0.3722 0.9366 0.032 Uiso 1 1 calc R U . . .
H16 H 0.2098 0.3842 0.8172 0.032 Uiso 1 1 calc R U . . .
C9 C 0.1945(2) 0.6578(2) 0.91338(16) 0.0216(4) Uani 1 1 d . . . . .
H17 H 0.0793 0.6987 0.9252 0.032 Uiso 1 1 calc R U . . .
H18 H 0.2447 0.7271 0.8911 0.032 Uiso 1 1 calc R U . . .
H19 H 0.2334 0.5848 0.9831 0.032 Uiso 1 1 calc R U . . .
C10 C 0.1111(2) 0.7027(2) 0.68584(16) 0.0219(4) Uani 1 1 d . . . . .
H20 H 0.0957 0.6495 0.6504 0.033 Uiso 1 1 calc R U . . .
H21 H 0.1593 0.7694 0.6295 0.033 Uiso 1 1 calc R U . . .
H22 H 0.0085 0.7497 0.7182 0.033 Uiso 1 1 calc R U . . .
C11 C 0.9322(2) 0.4210(2) 0.67035(17) 0.0228(4) Uani 1 1 d . . . . .
H23 H 1.0470 0.3993 0.6655 0.034 Uiso 1 1 calc R U . . .
H24 H 0.8786 0.4721 0.7202 0.034 Uiso 1 1 calc R U . . .
H25 H 0.8965 0.4758 0.5955 0.034 Uiso 1 1 calc R U . . .
C12 C 0.9955(2) 0.1743(2) 0.62608(17) 0.0260(5) Uani 1 1 d . . . . .
H26 H 0.9500 0.2263 0.5543 0.039 Uiso 1 1 calc R U . . .
H27 H 0.9888 0.0827 0.6556 0.039 Uiso 1 1 calc R U . . .
H28 H 1.1068 0.1688 0.6150 0.039 Uiso 1 1 calc R U . . .
C13 C 0.9722(2) 0.1598(2) 0.86373(16) 0.0228(5) Uani 1 1 d . . . . .
H29 H 0.9422 0.0776 0.9021 0.034 Uiso 1 1 calc R U . . .
H30 H 0.9330 0.2147 0.9110 0.034 Uiso 1 1 calc R U . . .
H31 H 1.0879 0.1347 0.8495 0.034 Uiso 1 1 calc R U . . .
C14 C 0.6890(2) 0.0962(2) 0.61949(16) 0.0212(4) Uani 1 1 d . . . . .
H32 H 0.8026 0.0463 0.6121 0.032 Uiso 1 1 calc R U . . .
H33 H 0.6650 0.1839 0.5573 0.032 Uiso 1 1 calc R U . . .
H34 H 0.6286 0.0437 0.6179 0.032 Uiso 1 1 calc R U . . .
C15 C 0.7513(3) -0.0298(2) 0.86398(17) 0.0260(5) Uani 1 1 d . . . . .
H35 H 0.7207 -0.1077 0.8768 0.039 Uiso 1 1 calc R U . . .
H36 H 0.7303 -0.0138 0.9342 0.039 Uiso 1 1 calc R U . . .
H37 H 0.8644 -0.0484 0.8377 0.039 Uiso 1 1 calc R U . . .
C16 C 0.4216(2) 0.1298(2) 0.79774(17) 0.0233(4) Uani 1 1 d . . . . .
H38 H 0.4126 0.0453 0.8033 0.035 Uiso 1 1 calc R U . . .
H39 H 0.3552 0.2066 0.7414 0.035 Uiso 1 1 calc R U . . .
H40 H 0.3863 0.1404 0.8706 0.035 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 Si2 2.2928(7) . ?
Si1 Si2 2.3004(7) 2_666 ?
Si1 Si1 2.4873(10) 2_666 ?
Si2 C4 1.9082(17) . ?
Si2 C1 1.9208(18) . ?
Si2 Si1 2.3004(7) 2_666 ?
Si3 C7 1.870(2) . ?
Si3 C6 1.873(2) . ?
Si3 C5 1.878(2) . ?
Si3 C1 1.9266(18) . ?
Si4 C8 1.872(2) . ?
Si4 C10 1.8747(19) . ?
Si4 C9 1.8847(19) . ?
Si4 C1 1.9164(18) . ?
Si5 C12 1.861(2) . ?
Si5 C13 1.8716(19) . ?
Si5 C11 1.872(2) . ?
Si5 C4 1.9169(18) . ?
Si6 C14 1.8719(19) . ?
Si6 C15 1.873(2) . ?
Si6 C16 1.874(2) . ?
Si6 C4 1.9032(18) . ?
C1 C2 1.578(2) . ?
C2 C3 1.533(2) . ?
C2 H1 0.9900 . ?
C2 H2 0.9900 . ?
C3 C4 1.571(2) . ?
C3 H3 0.9900 . ?
C3 H4 0.9900 . ?
C5 H5 0.9800 . ?
C5 H6 0.9800 . ?
C5 H7 0.9800 . ?
C6 H8 0.9800 . ?
C6 H9 0.9800 . ?
C6 H10 0.9800 . ?
C7 H11 0.9800 . ?
C7 H12 0.9800 . ?
C7 H13 0.9800 . ?
C8 H14 0.9800 . ?
C8 H15 0.9800 . ?
C8 H16 0.9800 . ?
C9 H17 0.9800 . ?
C9 H18 0.9800 . ?
C9 H19 0.9800 . ?
C10 H20 0.9800 . ?
C10 H21 0.9800 . ?
C10 H22 0.9800 . ?
C11 H23 0.9800 . ?
C11 H24 0.9800 . ?
C11 H25 0.9800 . ?
C12 H26 0.9800 . ?
C12 H27 0.9800 . ?
C12 H28 0.9800 . ?
C13 H29 0.9800 . ?
C13 H30 0.9800 . ?
C13 H31 0.9800 . ?
C14 H32 0.9800 . ?
C14 H33 0.9800 . ?
C14 H34 0.9800 . ?
C15 H35 0.9800 . ?
C15 H36 0.9800 . ?
C15 H37 0.9800 . ?
C16 H38 0.9800 . ?
C16 H39 0.9800 . ?
C16 H40 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Si2 Si1 Si2 114.43(2) . 2_666 ?
Si2 Si1 Si1 57.36(2) . 2_666 ?
Si2 Si1 Si1 57.06(2) 2_666 2_666 ?
C4 Si2 C1 99.09(7) . . ?
C4 Si2 Si1 120.43(6) . . ?
C1 Si2 Si1 127.40(6) . . ?
C4 Si2 Si1 124.17(6) . 2_666 ?
C1 Si2 Si1 120.31(6) . 2_666 ?
Si1 Si2 Si1 65.57(2) . 2_666 ?
C7 Si3 C6 102.90(9) . . ?
C7 Si3 C5 105.68(10) . . ?
C6 Si3 C5 104.99(10) . . ?
C7 Si3 C1 117.25(8) . . ?
C6 Si3 C1 115.87(9) . . ?
C5 Si3 C1 109.04(8) . . ?
C8 Si4 C10 104.82(9) . . ?
C8 Si4 C9 103.26(9) . . ?
C10 Si4 C9 109.97(9) . . ?
C8 Si4 C1 114.80(8) . . ?
C10 Si4 C1 114.29(8) . . ?
C9 Si4 C1 109.08(9) . . ?
C12 Si5 C13 108.83(9) . . ?
C12 Si5 C11 104.26(10) . . ?
C13 Si5 C11 105.00(9) . . ?
C12 Si5 C4 112.43(9) . . ?
C13 Si5 C4 110.08(8) . . ?
C11 Si5 C4 115.73(8) . . ?
C14 Si6 C15 108.36(9) . . ?
C14 Si6 C16 105.38(9) . . ?
C15 Si6 C16 106.26(10) . . ?
C14 Si6 C4 114.82(8) . . ?
C15 Si6 C4 109.63(9) . . ?
C16 Si6 C4 111.95(9) . . ?
C2 C1 Si4 106.94(11) . . ?
C2 C1 Si2 100.49(11) . . ?
Si4 C1 Si2 113.31(9) . . ?
C2 C1 Si3 108.85(12) . . ?
Si4 C1 Si3 108.59(9) . . ?
Si2 C1 Si3 117.81(9) . . ?
C3 C2 C1 111.45(14) . . ?
C3 C2 H1 109.3 . . ?
C1 C2 H1 109.3 . . ?
C3 C2 H2 109.3 . . ?
C1 C2 H2 109.3 . . ?
H1 C2 H2 108.0 . . ?
C2 C3 C4 109.63(14) . . ?
C2 C3 H3 109.7 . . ?
C4 C3 H3 109.7 . . ?
C2 C3 H4 109.7 . . ?
C4 C3 H4 109.7 . . ?
H3 C3 H4 108.2 . . ?
C3 C4 Si6 107.78(11) . . ?
C3 C4 Si2 100.03(11) . . ?
Si6 C4 Si2 116.16(9) . . ?
C3 C4 Si5 109.43(12) . . ?
Si6 C4 Si5 110.38(9) . . ?
Si2 C4 Si5 112.33(9) . . ?
Si3 C5 H5 109.5 . . ?
Si3 C5 H6 109.5 . . ?
H5 C5 H6 109.5 . . ?
Si3 C5 H7 109.5 . . ?
H5 C5 H7 109.5 . . ?
H6 C5 H7 109.5 . . ?
Si3 C6 H8 109.5 . . ?
Si3 C6 H9 109.5 . . ?
H8 C6 H9 109.5 . . ?
Si3 C6 H10 109.5 . . ?
H8 C6 H10 109.5 . . ?
H9 C6 H10 109.5 . . ?
Si3 C7 H11 109.5 . . ?
Si3 C7 H12 109.5 . . ?
H11 C7 H12 109.5 . . ?
Si3 C7 H13 109.5 . . ?
H11 C7 H13 109.5 . . ?
H12 C7 H13 109.5 . . ?
Si4 C8 H14 109.5 . . ?
Si4 C8 H15 109.5 . . ?
H14 C8 H15 109.5 . . ?
Si4 C8 H16 109.5 . . ?
H14 C8 H16 109.5 . . ?
H15 C8 H16 109.5 . . ?
Si4 C9 H17 109.5 . . ?
Si4 C9 H18 109.5 . . ?
H17 C9 H18 109.5 . . ?
Si4 C9 H19 109.5 . . ?
H17 C9 H19 109.5 . . ?
H18 C9 H19 109.5 . . ?
Si4 C10 H20 109.5 . . ?
Si4 C10 H21 109.5 . . ?
H20 C10 H21 109.5 . . ?
Si4 C10 H22 109.5 . . ?
H20 C10 H22 109.5 . . ?
H21 C10 H22 109.5 . . ?
Si5 C11 H23 109.5 . . ?
Si5 C11 H24 109.5 . . ?
H23 C11 H24 109.5 . . ?
Si5 C11 H25 109.5 . . ?
H23 C11 H25 109.5 . . ?
H24 C11 H25 109.5 . . ?
Si5 C12 H26 109.5 . . ?
Si5 C12 H27 109.5 . . ?
H26 C12 H27 109.5 . . ?
Si5 C12 H28 109.5 . . ?
H26 C12 H28 109.5 . . ?
H27 C12 H28 109.5 . . ?
Si5 C13 H29 109.5 . . ?
Si5 C13 H30 109.5 . . ?
H29 C13 H30 109.5 . . ?
Si5 C13 H31 109.5 . . ?
H29 C13 H31 109.5 . . ?
H30 C13 H31 109.5 . . ?
Si6 C14 H32 109.5 . . ?
Si6 C14 H33 109.5 . . ?
H32 C14 H33 109.5 . . ?
Si6 C14 H34 109.5 . . ?
H32 C14 H34 109.5 . . ?
H33 C14 H34 109.5 . . ?
Si6 C15 H35 109.5 . . ?
Si6 C15 H36 109.5 . . ?
H35 C15 H36 109.5 . . ?
Si6 C15 H37 109.5 . . ?
H35 C15 H37 109.5 . . ?
H36 C15 H37 109.5 . . ?
Si6 C16 H38 109.5 . . ?
Si6 C16 H39 109.5 . . ?
H38 C16 H39 109.5 . . ?
Si6 C16 H40 109.5 . . ?
H38 C16 H40 109.5 . . ?
H39 C16 H40 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Si4 C1 C2 C3 87.93(15) . . . . ?
Si2 C1 C2 C3 -30.57(16) . . . . ?
Si3 C1 C2 C3 -154.94(12) . . . . ?
C1 C2 C3 C4 49.63(19) . . . . ?
C2 C3 C4 Si6 -161.39(12) . . . . ?
C2 C3 C4 Si2 -39.60(16) . . . . ?
C2 C3 C4 Si5 78.54(15) . . . . ?

_refine_diff_density_max         0.394
_refine_diff_density_min         -0.329
_refine_diff_density_rms         0.060

_shelxl_version_number           2014-3


_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: toluene'
_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_TK89a
_database_code_depnum_ccdc_archive 'CCDC 1908505'
loop_
_audit_author_name
_audit_author_address
'Tomoyuki Kosai'
;Tohoku University
Japan
;
_audit_update_record             
;
2019-05-07 deposited with the CCDC.	2019-05-09 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/1
_shelx_SHELXL_version_number     2018/1
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          436
_chemical_formula_moiety         ?
_chemical_formula_sum            'C36 H91 Cl2 O Si12'
_chemical_formula_weight         948.06

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'
Cl Cl 0.1484 0.1585 '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                   18.4326(8)
_cell_length_b                   12.7398(6)
_cell_length_c                   23.2524(10)
_cell_angle_alpha                90
_cell_angle_beta                 93.1569(12)
_cell_angle_gamma                90
_cell_volume                     5452.0(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9428
_cell_measurement_theta_min      2.37
_cell_measurement_theta_max      33.64

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.155
_exptl_crystal_F_000             2068
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.300
_exptl_crystal_size_min          0.300
_exptl_absorpt_coefficient_mu    0.409
_shelx_estimated_absorpt_T_min   0.887
_shelx_estimated_absorpt_T_max   0.887
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.6471
_exptl_absorpt_correction_T_max  0.7467
_exptl_absorpt_process_details   
;
SADABS Sheldrick 1996
;
_exptl_absorpt_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            34636
_diffrn_reflns_av_unetI/netI     0.0266
_diffrn_reflns_av_R_equivalents  0.0258
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_theta_min         1.106
_diffrn_reflns_theta_max         25.997
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             10706
_reflns_number_gt                9306
_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)+(0.0514P)²+6.5712P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         10706
_refine_ls_number_parameters     499
_refine_ls_number_restraints     18
_refine_ls_R_factor_all          0.0504
_refine_ls_R_factor_gt           0.0428
_refine_ls_wR_factor_ref         0.1130
_refine_ls_wR_factor_gt          0.1065
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_restrained_S_all      1.059
_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 0.66695(3) 0.49947(5) 0.33073(3) 0.02301(15) Uani 1 1 d . . . . .
Cl1 Cl 0.57953(3) 0.59198(5) 0.30278(3) 0.03963(17) Uani 1 1 d . . . . .
H1 H 0.6600(16) 0.487(2) 0.3945(13) 0.039(8) Uiso 1 1 d . . . . .
Si2 Si 0.78779(3) 0.56211(4) 0.34843(2) 0.01441(12) Uani 1 1 d . . . . .
Si3 Si 0.80108(3) 0.37345(4) 0.33717(2) 0.01554(13) Uani 1 1 d . . . . .
Si4 Si 0.67689(3) 0.31577(4) 0.31726(2) 0.01388(12) Uani 1 1 d . . . . .
Cl2 Cl 0.84136(3) 0.37629(5) 0.25568(3) 0.03106(14) Uani 1 1 d . . . . .
O1 O 0.85562(9) 0.29991(13) 0.37695(7) 0.0255(4) Uani 1 1 d . . . . .
C1 C 0.92364(14) 0.2520(2) 0.36939(13) 0.0383(6) Uani 1 1 d . . . . .
H2 H 0.939441 0.268138 0.330818 0.057 Uiso 1 1 calc R U . . .
H3 H 0.919081 0.175790 0.373714 0.057 Uiso 1 1 calc R U . . .
H4 H 0.959530 0.278817 0.398402 0.057 Uiso 1 1 calc R U . . .
C2 C 0.84454(12) 0.64989(18) 0.29887(10) 0.0213(5) Uani 1 1 d . . . . .
C3 C 0.84217(14) 0.75403(18) 0.33521(11) 0.0276(5) Uani 1 1 d . . . . .
H5 H 0.880332 0.802769 0.323194 0.033 Uiso 1 1 calc R U . . .
H6 H 0.794452 0.788673 0.328041 0.033 Uiso 1 1 calc R U . . .
C4 C 0.85422(13) 0.72966(19) 0.39917(11) 0.0271(5) Uani 1 1 d . . . . .
H7 H 0.849213 0.794919 0.421725 0.033 Uiso 1 1 calc R U . . .
H8 H 0.904132 0.702514 0.406926 0.033 Uiso 1 1 calc R U . . .
C5 C 0.79768(12) 0.64582(17) 0.41881(10) 0.0207(5) Uani 1 1 d . . . . .
Si5 Si 0.80626(4) 0.69133(6) 0.22368(3) 0.03184(17) Uani 1 1 d . . . . .
C6 C 0.85873(18) 0.8099(2) 0.20047(13) 0.0452(7) Uani 1 1 d . . . . .
H9 H 0.837213 0.836180 0.163770 0.068 Uiso 1 1 calc R U . . .
H10 H 0.909442 0.790130 0.195763 0.068 Uiso 1 1 calc R U . . .
H11 H 0.856759 0.864855 0.229820 0.068 Uiso 1 1 calc R U . . .
C7 C 0.70976(17) 0.7344(3) 0.22379(15) 0.0527(9) Uani 1 1 d . . . . .
H12 H 0.693964 0.760128 0.185389 0.079 Uiso 1 1 calc R U . . .
H13 H 0.705265 0.790869 0.252012 0.079 Uiso 1 1 calc R U . . .
H14 H 0.679263 0.675020 0.234012 0.079 Uiso 1 1 calc R U . . .
C8 C 0.81063(18) 0.5948(3) 0.16305(12) 0.0450(7) Uani 1 1 d . . . . .
H15 H 0.809631 0.523199 0.178438 0.067 Uiso 1 1 calc R U . . .
H16 H 0.855678 0.605441 0.143326 0.067 Uiso 1 1 calc R U . . .
H17 H 0.768858 0.605228 0.135727 0.067 Uiso 1 1 calc R U . . .
Si6 Si 0.94599(4) 0.61404(6) 0.29423(3) 0.02667(15) Uani 1 1 d . . . . .
C9 C 1.00448(15) 0.7342(2) 0.30542(14) 0.0426(7) Uani 1 1 d . . . . .
H18 H 0.998866 0.762040 0.344207 0.064 Uiso 1 1 calc R U . . .
H19 H 0.989578 0.787538 0.276812 0.064 Uiso 1 1 calc R U . . .
H20 H 1.055460 0.715455 0.301084 0.064 Uiso 1 1 calc R U . . .
C10 C 0.98215(14) 0.5203(2) 0.35061(13) 0.0379(6) Uani 1 1 d . . . . .
H21 H 0.949464 0.459870 0.352266 0.057 Uiso 1 1 calc R U . . .
H22 H 0.985414 0.555619 0.388114 0.057 Uiso 1 1 calc R U . . .
H23 H 1.030541 0.496371 0.341021 0.057 Uiso 1 1 calc R U . . .
C11 C 0.97362(16) 0.5599(3) 0.22358(13) 0.0425(7) Uani 1 1 d . . . . .
H24 H 1.026116 0.547041 0.225632 0.064 Uiso 1 1 calc R U . . .
H25 H 0.961333 0.610519 0.192838 0.064 Uiso 1 1 calc R U . . .
H26 H 0.947821 0.493837 0.215388 0.064 Uiso 1 1 calc R U . . .
Si7 Si 0.71331(4) 0.72515(6) 0.43823(3) 0.03174(17) Uani 1 1 d . . . . .
C12 C 0.67451(16) 0.8123(2) 0.37921(14) 0.0457(8) Uani 1 1 d . . . . .
H27 H 0.660555 0.769709 0.345295 0.068 Uiso 1 1 calc R U . . .
H28 H 0.711076 0.864020 0.369128 0.068 Uiso 1 1 calc R U . . .
H29 H 0.631642 0.848760 0.392378 0.068 Uiso 1 1 calc R U . . .
C13 C 0.73898(17) 0.8184(2) 0.49901(13) 0.0413(7) Uani 1 1 d . . . . .
H30 H 0.697403 0.863467 0.506365 0.062 Uiso 1 1 calc R U . . .
H31 H 0.779972 0.861990 0.488409 0.062 Uiso 1 1 calc R U . . .
H32 H 0.752894 0.778237 0.533829 0.062 Uiso 1 1 calc R U . . .
C14 C 0.63339(17) 0.6495(3) 0.46236(16) 0.0562(10) Uani 1 1 d . . . . .
H33 H 0.606467 0.692639 0.488814 0.084 Uiso 1 1 calc R U . . .
H34 H 0.650372 0.585360 0.482110 0.084 Uiso 1 1 calc R U . . .
H35 H 0.601500 0.630860 0.428800 0.084 Uiso 1 1 calc R U . . .
Si8 Si 0.83934(4) 0.58511(5) 0.48926(3) 0.02599(15) Uani 1 1 d . . . . .
C15 C 0.89575(15) 0.4647(2) 0.48163(11) 0.0341(6) Uani 1 1 d . . . . .
H36 H 0.909497 0.436395 0.519885 0.051 Uiso 1 1 calc R U . . .
H37 H 0.939667 0.482467 0.461793 0.051 Uiso 1 1 calc R U . . .
H38 H 0.867705 0.411963 0.459209 0.051 Uiso 1 1 calc R U . . .
C16 C 0.90378(17) 0.6817(2) 0.52623(12) 0.0399(7) Uani 1 1 d . . . . .
H39 H 0.920217 0.654222 0.564112 0.060 Uiso 1 1 calc R U . . .
H40 H 0.878841 0.748773 0.530991 0.060 Uiso 1 1 calc R U . . .
H41 H 0.945790 0.692168 0.502819 0.060 Uiso 1 1 calc R U . . .
C17 C 0.77268(18) 0.5489(2) 0.54408(12) 0.0429(7) Uani 1 1 d . . . . .
H42 H 0.737961 0.497514 0.527402 0.064 Uiso 1 1 calc R U . . .
H43 H 0.746524 0.611809 0.555515 0.064 Uiso 1 1 calc R U . . .
H44 H 0.798731 0.518326 0.577942 0.064 Uiso 1 1 calc R U . . .
C18 C 0.64902(12) 0.24020(18) 0.24748(9) 0.0202(4) Uani 1 1 d . . . . .
C19 C 0.58885(12) 0.16669(19) 0.27160(10) 0.0240(5) Uani 1 1 d . . . . .
H45 H 0.542533 0.205709 0.272986 0.029 Uiso 1 1 calc R U . . .
H46 H 0.580696 0.105530 0.245778 0.029 Uiso 1 1 calc R U . . .
C20 C 0.61314(13) 0.12922(18) 0.33180(10) 0.0232(5) Uani 1 1 d . . . . .
H47 H 0.657387 0.085544 0.330032 0.028 Uiso 1 1 calc R U . . .
H48 H 0.574499 0.085854 0.347800 0.028 Uiso 1 1 calc R U . . .
C21 C 0.62939(12) 0.22689(17) 0.37153(9) 0.0211(5) Uani 1 1 d . . . . .
Si9 Si 0.60238(4) 0.32110(6) 0.18691(3) 0.03604(19) Uani 1 1 d . . . . .
C22 C 0.6601(2) 0.4321(3) 0.16435(16) 0.0614(10) Uani 1 1 d . . . . .
H49 H 0.703839 0.404355 0.147649 0.092 Uiso 1 1 calc R U . . .
H50 H 0.674063 0.475513 0.197937 0.092 Uiso 1 1 calc R U . . .
H51 H 0.632731 0.474775 0.135582 0.092 Uiso 1 1 calc R U . . .
C23 C 0.51362(18) 0.3801(3) 0.20531(15) 0.0518(9) Uani 1 1 d . . . . .
H52 H 0.493515 0.420998 0.172491 0.078 Uiso 1 1 calc R U . . .
H53 H 0.521247 0.426105 0.238872 0.078 Uiso 1 1 calc R U . . .
H54 H 0.479598 0.324017 0.214217 0.078 Uiso 1 1 calc R U . . .
C24 C 0.57579(18) 0.2363(3) 0.12345(12) 0.0520(9) Uani 1 1 d . . . . .
H55 H 0.548947 0.278315 0.094101 0.078 Uiso 1 1 calc R U . . .
H56 H 0.544957 0.178680 0.135723 0.078 Uiso 1 1 calc R U . . .
H57 H 0.619556 0.207371 0.107306 0.078 Uiso 1 1 calc R U . . .
Si10 Si 0.72069(4) 0.15081(6) 0.21563(3) 0.03151(17) Uani 1 1 d . . . . .
C26 C 0.67641(19) 0.0269(3) 0.18774(16) 0.0539(9) Uani 1 1 d . . . . .
H58 H 0.711714 -0.014693 0.167428 0.081 Uiso 1 1 calc R U . . .
H59 H 0.635096 0.044464 0.161158 0.081 Uiso 1 1 calc R U . . .
H60 H 0.659306 -0.013938 0.220057 0.081 Uiso 1 1 calc R U . . .
Si11 Si 0.53931(4) 0.27661(6) 0.39913(4) 0.03589(19) Uani 1 1 d . . . . .
C28 C 0.5522(2) 0.3584(3) 0.46601(15) 0.0533(9) Uani 1 1 d . . . . .
H61 H 0.586295 0.415573 0.459261 0.080 Uiso 1 1 calc R U . . .
H62 H 0.571795 0.314460 0.497820 0.080 Uiso 1 1 calc R U . . .
H63 H 0.505414 0.387792 0.475897 0.080 Uiso 1 1 calc R U . . .
C29 C 0.47815(19) 0.1627(3) 0.41386(19) 0.0632(11) Uani 1 1 d . . . . .
H64 H 0.437246 0.187192 0.435483 0.095 Uiso 1 1 calc R U . . .
H65 H 0.505590 0.109615 0.436488 0.095 Uiso 1 1 calc R U . . .
H66 H 0.459742 0.131880 0.377293 0.095 Uiso 1 1 calc R U . . .
C30 C 0.48090(17) 0.3585(3) 0.34970(18) 0.0592(10) Uani 1 1 d . . . . .
H67 H 0.467905 0.318712 0.314552 0.089 Uiso 1 1 calc R U . . .
H68 H 0.507273 0.422175 0.339774 0.089 Uiso 1 1 calc R U . . .
H69 H 0.436613 0.377868 0.368619 0.089 Uiso 1 1 calc R U . . .
Si12 Si 0.68948(4) 0.18217(6) 0.43670(3) 0.03011(16) Uani 1 1 d . . . . .
C25 C 0.79523(16) 0.1037(2) 0.26714(14) 0.0414(7) Uani 1 1 d . . . . .
H70 H 0.831805 0.066516 0.245867 0.062 Uiso 1 1 calc R U . . .
H71 H 0.775070 0.056041 0.295229 0.062 Uiso 1 1 calc R U . . .
H72 H 0.817857 0.163923 0.287291 0.062 Uiso 1 1 calc R U . . .
C27 C 0.76747(18) 0.2075(3) 0.15310(12) 0.0508(9) Uani 1 1 d . . . . .
H73 H 0.787615 0.276435 0.163747 0.076 Uiso 1 1 calc R U . . .
H74 H 0.732415 0.215109 0.120119 0.076 Uiso 1 1 calc R U . . .
H75 H 0.806815 0.160574 0.142763 0.076 Uiso 1 1 calc R U . . .
C31 C 0.73004(19) 0.2950(2) 0.47851(12) 0.0443(7) Uani 1 1 d . . . . .
H76 H 0.773732 0.271456 0.500769 0.066 Uiso 1 1 calc R U . . .
H77 H 0.694676 0.321954 0.504788 0.066 Uiso 1 1 calc R U . . .
H78 H 0.743001 0.350712 0.451894 0.066 Uiso 1 1 calc R U . . .
C32 C 0.6382(2) 0.0987(3) 0.48737(14) 0.0522(8) Uani 1 1 d . . . . .
H79 H 0.671377 0.074546 0.518996 0.078 Uiso 1 1 calc R U . . .
H80 H 0.617398 0.037971 0.466541 0.078 Uiso 1 1 calc R U . . .
H81 H 0.599049 0.140213 0.502995 0.078 Uiso 1 1 calc R U . . .
C33 C 0.76530(16) 0.0951(2) 0.41690(13) 0.0401(7) Uani 1 1 d . . . . .
H82 H 0.794836 0.131242 0.389265 0.060 Uiso 1 1 calc R U . . .
H83 H 0.745359 0.030441 0.399477 0.060 Uiso 1 1 calc R U . . .
H84 H 0.795605 0.077630 0.451537 0.060 Uiso 1 1 calc R U . . .
C34 C 0.1110(3) 0.8786(5) 0.4302(2) 0.1065(19) Uani 1 1 d . U . . .
H99 H 0.118398 0.805429 0.418834 0.160 Uiso 0.385(17) 1 calc R U P A 1
H100 H 0.097971 0.920708 0.395894 0.160 Uiso 0.385(17) 1 calc R U P A 1
H101 H 0.155826 0.905992 0.449162 0.160 Uiso 0.385(17) 1 calc R U P A 1
H102 H 0.111141 0.854486 0.390162 0.160 Uiso 0.615(17) 1 calc R U P A 2
H103 H 0.153600 0.922889 0.438950 0.160 Uiso 0.615(17) 1 calc R U P A 2
H104 H 0.112438 0.817735 0.456024 0.160 Uiso 0.615(17) 1 calc R U P A 2
C35 C 0.0342(4) 0.9793(6) 0.4904(3) 0.125(2) Uani 1 1 d . . . . .
H91 H 0.048203 1.029287 0.460395 0.151 Uiso 0.385(17) 1 calc R U P A 1
H92 H 0.069258 0.991066 0.523611 0.151 Uiso 0.385(17) 1 calc R U P A 1
H93 H 0.070334 1.036368 0.496157 0.151 Uiso 0.615(17) 1 calc R U P A 2
H94 H 0.049214 0.923081 0.517976 0.151 Uiso 0.615(17) 1 calc R U P A 2
C36 C 0.0429(6) 0.9410(12) 0.4385(5) 0.114(5) Uani 0.615(17) 1 d . U P A 2
H95 H 0.041620 1.000288 0.410979 0.137 Uiso 0.615(17) 1 calc R U P A 2
H96 H 0.000614 0.895535 0.427988 0.137 Uiso 0.615(17) 1 calc R U P A 2
C37 C 0.0526(7) 0.8838(11) 0.4698(6) 0.070(5) Uani 0.385(17) 1 d . U P A 1
H97 H 0.008662 0.852933 0.450109 0.084 Uiso 0.385(17) 1 calc R U P A 1
H98 H 0.066245 0.838286 0.503127 0.084 Uiso 0.385(17) 1 calc R U P A 1


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Si1 Cl1 2.0719(9) . ?
Si1 Si4 2.3696(8) . ?
Si1 Si2 2.3804(8) . ?
Si2 C2 1.951(2) . ?
Si2 C5 1.953(2) . ?
Si2 Si3 2.4316(8) . ?
Si3 O1 1.6253(16) . ?
Si3 Cl2 2.0730(8) . ?
Si3 Si4 2.4244(8) . ?
Si4 C18 1.932(2) . ?
Si4 C21 1.940(2) . ?
O1 C1 1.414(3) . ?
C2 C3 1.575(3) . ?
C2 Si5 1.923(2) . ?
C2 Si6 1.934(2) . ?
C3 C4 1.524(3) . ?
C4 C5 1.577(3) . ?
C5 Si7 1.929(2) . ?
C5 Si8 1.932(2) . ?
Si5 C7 1.862(3) . ?
Si5 C8 1.876(3) . ?
Si5 C6 1.888(3) . ?
Si6 C10 1.869(3) . ?
Si6 C11 1.878(3) . ?
Si6 C9 1.882(3) . ?
Si7 C14 1.872(3) . ?
Si7 C12 1.876(3) . ?
Si7 C13 1.887(3) . ?
Si8 C15 1.867(3) . ?
Si8 C17 1.876(3) . ?
Si8 C16 1.884(3) . ?
C18 C19 1.578(3) . ?
C18 Si9 1.911(2) . ?
C18 Si10 1.923(2) . ?
C19 C20 1.523(3) . ?
C20 C21 1.569(3) . ?
C21 Si12 1.914(2) . ?
C21 Si11 1.920(2) . ?
Si9 C22 1.862(3) . ?
Si9 C23 1.871(4) . ?
Si9 C24 1.873(3) . ?
Si10 C25 1.871(3) . ?
Si10 C27 1.875(3) . ?
Si10 C26 1.877(3) . ?
Si11 C30 1.853(4) . ?
Si11 C28 1.876(3) . ?
Si11 C29 1.881(3) . ?
Si12 C33 1.862(3) . ?
Si12 C31 1.868(3) . ?
Si12 C32 1.880(3) . ?
C34 C37 1.455(13) . ?
C34 C36 1.507(11) . ?
C35 C36 1.320(11) . ?
C35 C37 1.358(14) . ?
C35 C35 1.458(11) 3_576 ?

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
Cl1 Si1 Si4 125.79(4) . . ?
Cl1 Si1 Si2 124.59(4) . . ?
Si4 Si1 Si2 105.99(3) . . ?
C2 Si2 C5 98.83(10) . . ?
C2 Si2 Si1 128.11(7) . . ?
C5 Si2 Si1 111.79(7) . . ?
C2 Si2 Si3 116.27(7) . . ?
C5 Si2 Si3 128.65(7) . . ?
Si1 Si2 Si3 75.46(3) . . ?
O1 Si3 Cl2 106.79(7) . . ?
O1 Si3 Si4 118.81(7) . . ?
Cl2 Si3 Si4 102.28(3) . . ?
O1 Si3 Si2 124.84(7) . . ?
Cl2 Si3 Si2 97.15(3) . . ?
Si4 Si3 Si2 102.73(3) . . ?
C18 Si4 C21 98.44(10) . . ?
C18 Si4 Si1 125.76(7) . . ?
C21 Si4 Si1 116.72(7) . . ?
C18 Si4 Si3 121.06(7) . . ?
C21 Si4 Si3 120.53(7) . . ?
Si1 Si4 Si3 75.79(3) . . ?
C1 O1 Si3 134.66(17) . . ?
C3 C2 Si5 103.71(15) . . ?
C3 C2 Si6 106.52(15) . . ?
Si5 C2 Si6 108.76(11) . . ?
C3 C2 Si2 97.72(15) . . ?
Si5 C2 Si2 120.84(12) . . ?
Si6 C2 Si2 116.69(12) . . ?
C4 C3 C2 110.20(19) . . ?
C3 C4 C5 110.94(19) . . ?
C4 C5 Si7 105.49(15) . . ?
C4 C5 Si8 106.16(15) . . ?
Si7 C5 Si8 107.41(11) . . ?
C4 C5 Si2 99.20(14) . . ?
Si7 C5 Si2 116.29(11) . . ?
Si8 C5 Si2 120.41(12) . . ?
C7 Si5 C8 105.96(16) . . ?
C7 Si5 C6 105.60(15) . . ?
C8 Si5 C6 105.41(14) . . ?
C7 Si5 C2 112.50(13) . . ?
C8 Si5 C2 118.32(12) . . ?
C6 Si5 C2 108.15(12) . . ?
C10 Si6 C11 106.00(15) . . ?
C10 Si6 C9 104.06(14) . . ?
C11 Si6 C9 103.82(14) . . ?
C10 Si6 C2 114.86(11) . . ?
C11 Si6 C2 116.44(12) . . ?
C9 Si6 C2 110.40(12) . . ?
C14 Si7 C12 104.44(17) . . ?
C14 Si7 C13 105.59(14) . . ?
C12 Si7 C13 104.18(14) . . ?
C14 Si7 C5 117.28(14) . . ?
C12 Si7 C5 114.75(12) . . ?
C13 Si7 C5 109.46(12) . . ?
C15 Si8 C17 104.55(14) . . ?
C15 Si8 C16 103.85(13) . . ?
C17 Si8 C16 105.70(14) . . ?
C15 Si8 C5 116.48(11) . . ?
C17 Si8 C5 115.46(13) . . ?
C16 Si8 C5 109.68(12) . . ?
C19 C18 Si9 106.59(15) . . ?
C19 C18 Si10 107.25(15) . . ?
Si9 C18 Si10 109.04(11) . . ?
C19 C18 Si4 99.03(14) . . ?
Si9 C18 Si4 115.99(12) . . ?
Si10 C18 Si4 117.53(11) . . ?
C20 C19 C18 109.62(18) . . ?
C19 C20 C21 109.25(18) . . ?
C20 C21 Si12 108.28(15) . . ?
C20 C21 Si11 108.54(15) . . ?
Si12 C21 Si11 107.88(11) . . ?
C20 C21 Si4 99.10(14) . . ?
Si12 C21 Si4 115.25(11) . . ?
Si11 C21 Si4 117.02(12) . . ?
C22 Si9 C23 106.25(18) . . ?
C22 Si9 C24 110.18(16) . . ?
C23 Si9 C24 102.58(15) . . ?
C22 Si9 C18 112.11(13) . . ?
C23 Si9 C18 114.30(13) . . ?
C24 Si9 C18 110.92(14) . . ?
C25 Si10 C27 105.48(15) . . ?
C25 Si10 C26 103.97(16) . . ?
C27 Si10 C26 105.42(15) . . ?
C25 Si10 C18 116.05(11) . . ?
C27 Si10 C18 115.18(14) . . ?
C26 Si10 C18 109.67(13) . . ?
C30 Si11 C28 104.17(18) . . ?
C30 Si11 C29 102.34(18) . . ?
C28 Si11 C29 109.12(16) . . ?
C30 Si11 C21 117.52(13) . . ?
C28 Si11 C21 112.79(13) . . ?
C29 Si11 C21 110.14(13) . . ?
C33 Si12 C31 107.63(15) . . ?
C33 Si12 C32 103.19(15) . . ?
C31 Si12 C32 108.03(14) . . ?
C33 Si12 C21 113.02(12) . . ?
C31 Si12 C21 112.37(12) . . ?
C32 Si12 C21 112.05(14) . . ?
C36 C35 C35 124.2(10) . 3_576 ?
C37 C35 C35 132.0(10) . 3_576 ?
C35 C36 C34 117.1(10) . . ?
C35 C37 C34 118.3(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
Cl2 Si3 O1 C1 8.4(2) . . . . ?
Si4 Si3 O1 C1 123.2(2) . . . . ?
Si2 Si3 O1 C1 -103.3(2) . . . . ?
Si5 C2 C3 C4 166.93(16) . . . . ?
Si6 C2 C3 C4 -78.4(2) . . . . ?
Si2 C2 C3 C4 42.5(2) . . . . ?
C2 C3 C4 C5 -55.2(3) . . . . ?
C3 C4 C5 Si7 -86.8(2) . . . . ?
C3 C4 C5 Si8 159.37(17) . . . . ?
C3 C4 C5 Si2 33.9(2) . . . . ?
Si9 C18 C19 C20 -160.01(16) . . . . ?
Si10 C18 C19 C20 83.32(19) . . . . ?
Si4 C18 C19 C20 -39.3(2) . . . . ?
C18 C19 C20 C21 56.8(2) . . . . ?
C19 C20 C21 Si12 -160.65(15) . . . . ?
C19 C20 C21 Si11 82.50(19) . . . . ?
C19 C20 C21 Si4 -40.1(2) . . . . ?
C35 C35 C36 C34 -165.8(10) 3_576 . . . ?
C35 C35 C37 C34 151.3(11) 3_576 . . . ?

_refine_diff_density_max         1.521
_refine_diff_density_min         -0.765
_refine_diff_density_rms         0.068


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

data_TK64a_a
_database_code_depnum_ccdc_archive 'CCDC 1908503'
loop_
_audit_author_name
_audit_author_address
'Tomoyuki Kosai'
;Tohoku University
Japan
;
_audit_update_record             
;
2019-04-08 deposited with the CCDC.	2019-05-09 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          443
_chemical_formula_moiety         'C32 H80 Cl40 Si12'
_chemical_formula_sum            'C32 H80 Cl4 Si12'
_chemical_formula_weight         943.84

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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

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

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

_cell_length_a                   10.6683(5)
_cell_length_b                   10.7582(5)
_cell_length_c                   12.9529(6)
_cell_angle_alpha                69.0200(10)
_cell_angle_beta                 84.5210(10)
_cell_angle_gamma                65.6520(10)
_cell_volume                     1262.24(10)
_cell_formula_units_Z            1
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    8117
_cell_measurement_theta_min      2.22
_cell_measurement_theta_max      33.13

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.242
_exptl_crystal_F_000             508
_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    0.543
_shelx_estimated_absorpt_T_min   0.948
_shelx_estimated_absorpt_T_max   0.948
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.6725
_exptl_absorpt_correction_T_max  0.7467
_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            18763
_diffrn_reflns_av_unetI/netI     0.0253
_diffrn_reflns_av_R_equivalents  0.0250
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         1.687
_diffrn_reflns_theta_max         27.497
_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             5793
_reflns_number_gt                5055
_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)+(0.0358P)²+1.0187P] 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         5793
_refine_ls_number_parameters     229
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0387
_refine_ls_R_factor_gt           0.0318
_refine_ls_wR_factor_ref         0.0816
_refine_ls_wR_factor_gt          0.0779
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_restrained_S_all      1.049
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_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 0.59936(5) 0.53473(5) 0.54138(4) 0.01165(10) Uani 1 1 d . . . . .
Si2 Si 0.53627(4) 0.59628(5) 0.34864(3) 0.00929(10) Uani 1 1 d . . . . .
Si3 Si 0.40652(5) 0.95797(5) 0.28809(4) 0.01729(11) Uani 1 1 d . . . . .
Si4 Si 0.27252(5) 0.83235(5) 0.16831(4) 0.01678(11) Uani 1 1 d . . . . .
Si5 Si 0.85945(5) 0.52501(6) 0.27273(4) 0.02058(12) Uani 1 1 d . . . . .
Si6 Si 0.71426(5) 0.35426(5) 0.22181(4) 0.01837(11) Uani 1 1 d . . . . .
Cl1 Cl 0.64729(5) 0.67282(5) 0.59173(4) 0.02279(11) Uani 1 1 d . . . . .
Cl2 Cl 0.78221(4) 0.35309(5) 0.55133(4) 0.02193(10) Uani 1 1 d . . . . .
C1 C 0.43784(17) 0.79457(17) 0.24593(13) 0.0126(3) Uani 1 1 d . . . . .
C2 C 0.55064(18) 0.79724(18) 0.15804(14) 0.0155(3) Uani 1 1 d . . . . .
H1 H 0.5084 0.8777 0.0874 0.019 Uiso 1 1 calc R U . . .
H2 H 0.6240 0.8138 0.1852 0.019 Uiso 1 1 calc R U . . .
C3 C 0.61198(18) 0.65300(19) 0.13937(14) 0.0160(3) Uani 1 1 d . . . . .
H3 H 0.6821 0.6539 0.0836 0.019 Uiso 1 1 calc R U . . .
H4 H 0.5389 0.6369 0.1113 0.019 Uiso 1 1 calc R U . . .
C4 C 0.68044(17) 0.52669(18) 0.25261(13) 0.0133(3) Uani 1 1 d . . . . .
C5 C 0.2995(3) 0.9650(2) 0.40871(18) 0.0338(5) Uani 1 1 d . . . . .
H5 H 0.3451 0.8766 0.4728 0.051 Uiso 1 1 calc R U . . .
H6 H 0.2091 0.9714 0.3913 0.051 Uiso 1 1 calc R U . . .
H7 H 0.2875 1.0507 0.4259 0.051 Uiso 1 1 calc R U . . .
C6 C 0.3281(2) 1.1327(2) 0.16673(17) 0.0259(4) Uani 1 1 d . . . . .
H8 H 0.2384 1.1437 0.1432 0.039 Uiso 1 1 calc R U . . .
H9 H 0.3892 1.1302 0.1053 0.039 Uiso 1 1 calc R U . . .
H10 H 0.3160 1.2152 0.1884 0.039 Uiso 1 1 calc R U . . .
C7 C 0.5690(2) 0.9639(2) 0.32427(17) 0.0277(4) Uani 1 1 d . . . . .
H11 H 0.5462 1.0464 0.3489 0.042 Uiso 1 1 calc R U . . .
H12 H 0.6236 0.9752 0.2590 0.042 Uiso 1 1 calc R U . . .
H13 H 0.6224 0.8730 0.3839 0.042 Uiso 1 1 calc R U . . .
C8 C 0.2767(2) 0.9339(2) 0.01618(16) 0.0277(4) Uani 1 1 d . . . . .
H14 H 0.3530 0.8714 -0.0151 0.042 Uiso 1 1 calc R U . . .
H15 H 0.2897 1.0222 0.0069 0.042 Uiso 1 1 calc R U . . .
H16 H 0.1895 0.9608 -0.0222 0.042 Uiso 1 1 calc R U . . .
C9 C 0.1058(2) 0.9485(2) 0.21152(19) 0.0295(5) Uani 1 1 d . . . . .
H17 H 0.0290 0.9629 0.1663 0.044 Uiso 1 1 calc R U . . .
H18 H 0.1061 1.0432 0.2010 0.044 Uiso 1 1 calc R U . . .
H19 H 0.0952 0.9001 0.2898 0.044 Uiso 1 1 calc R U . . .
C10 C 0.2489(2) 0.6690(2) 0.17012(17) 0.0255(4) Uani 1 1 d . . . . .
H20 H 0.2341 0.6152 0.2458 0.038 Uiso 1 1 calc R U . . .
H21 H 0.3315 0.6059 0.1445 0.038 Uiso 1 1 calc R U . . .
H22 H 0.1688 0.7002 0.1211 0.038 Uiso 1 1 calc R U . . .
C11 C 0.8693(2) 0.6325(2) 0.35572(18) 0.0291(4) Uani 1 1 d . . . . .
H23 H 0.8345 0.5999 0.4289 0.044 Uiso 1 1 calc R U . . .
H24 H 0.8131 0.7362 0.3173 0.044 Uiso 1 1 calc R U . . .
H25 H 0.9653 0.6174 0.3644 0.044 Uiso 1 1 calc R U . . .
C12 C 0.9180(2) 0.6100(3) 0.13363(18) 0.0319(5) Uani 1 1 d . . . . .
H26 H 0.8608 0.7150 0.1049 0.048 Uiso 1 1 calc R U . . .
H27 H 0.9092 0.5656 0.0821 0.048 Uiso 1 1 calc R U . . .
H28 H 1.0146 0.5936 0.1416 0.048 Uiso 1 1 calc R U . . .
C13 C 1.0020(2) 0.3397(2) 0.33404(18) 0.0307(5) Uani 1 1 d . . . . .
H29 H 1.0884 0.3496 0.3388 0.046 Uiso 1 1 calc R U . . .
H30 H 1.0123 0.2826 0.2870 0.046 Uiso 1 1 calc R U . . .
H31 H 0.9799 0.2901 0.4084 0.046 Uiso 1 1 calc R U . . .
C14 C 0.8304(2) 0.3460(2) 0.10350(16) 0.0264(4) Uani 1 1 d . . . . .
H32 H 0.9194 0.3391 0.1247 0.040 Uiso 1 1 calc R U . . .
H33 H 0.7878 0.4342 0.0386 0.040 Uiso 1 1 calc R U . . .
H34 H 0.8446 0.2602 0.0855 0.040 Uiso 1 1 calc R U . . .
C15 C 0.7950(3) 0.1785(2) 0.33931(17) 0.0351(5) Uani 1 1 d . . . . .
H35 H 0.7341 0.1268 0.3565 0.053 Uiso 1 1 calc R U . . .
H36 H 0.8093 0.1980 0.4046 0.053 Uiso 1 1 calc R U . . .
H37 H 0.8839 0.1182 0.3186 0.053 Uiso 1 1 calc R U . . .
C16 C 0.5568(2) 0.3558(2) 0.16797(18) 0.0290(4) Uani 1 1 d . . . . .
H38 H 0.5808 0.2651 0.1541 0.043 Uiso 1 1 calc R U . . .
H39 H 0.5204 0.4389 0.0988 0.043 Uiso 1 1 calc R U . . .
H40 H 0.4867 0.3641 0.2228 0.043 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 Cl1 2.0682(6) . ?
Si1 Cl2 2.0892(6) . ?
Si1 Si2 2.4277(6) . ?
Si1 Si2 2.4413(6) 2_666 ?
Si2 C1 1.9521(17) . ?
Si2 C4 1.9559(17) . ?
Si2 Si1 2.4413(6) 2_666 ?
Si3 C5 1.850(2) . ?
Si3 C7 1.870(2) . ?
Si3 C6 1.882(2) . ?
Si3 C1 1.9153(17) . ?
Si4 C10 1.867(2) . ?
Si4 C9 1.875(2) . ?
Si4 C8 1.887(2) . ?
Si4 C1 1.9343(18) . ?
Si5 C11 1.875(2) . ?
Si5 C13 1.875(2) . ?
Si5 C12 1.884(2) . ?
Si5 C4 1.9439(18) . ?
Si6 C15 1.866(2) . ?
Si6 C16 1.871(2) . ?
Si6 C14 1.880(2) . ?
Si6 C4 1.9186(17) . ?
C1 C2 1.578(2) . ?
C2 C3 1.515(2) . ?
C3 C4 1.578(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
Cl1 Si1 Cl2 107.49(3) . . ?
Cl1 Si1 Si2 121.17(3) . . ?
Cl2 Si1 Si2 96.23(2) . . ?
Cl1 Si1 Si2 122.06(3) . 2_666 ?
Cl2 Si1 Si2 97.51(2) . 2_666 ?
Si2 Si1 Si2 106.35(2) . 2_666 ?
C1 Si2 C4 98.20(7) . . ?
C1 Si2 Si1 124.37(5) . . ?
C4 Si2 Si1 118.83(5) . . ?
C1 Si2 Si1 118.10(5) . 2_666 ?
C4 Si2 Si1 125.35(5) . 2_666 ?
Si1 Si2 Si1 73.65(2) . 2_666 ?
C5 Si3 C7 106.16(11) . . ?
C5 Si3 C6 110.41(10) . . ?
C7 Si3 C6 102.53(9) . . ?
C5 Si3 C1 113.59(9) . . ?
C7 Si3 C1 113.34(9) . . ?
C6 Si3 C1 110.21(8) . . ?
C10 Si4 C9 105.50(10) . . ?
C10 Si4 C8 103.55(9) . . ?
C9 Si4 C8 105.08(10) . . ?
C10 Si4 C1 116.26(8) . . ?
C9 Si4 C1 115.88(9) . . ?
C8 Si4 C1 109.34(8) . . ?
C11 Si5 C13 105.30(10) . . ?
C11 Si5 C12 103.51(10) . . ?
C13 Si5 C12 104.97(10) . . ?
C11 Si5 C4 117.24(8) . . ?
C13 Si5 C4 115.31(9) . . ?
C12 Si5 C4 109.24(9) . . ?
C15 Si6 C16 107.39(11) . . ?
C15 Si6 C14 107.44(10) . . ?
C16 Si6 C14 102.60(10) . . ?
C15 Si6 C4 115.67(9) . . ?
C16 Si6 C4 113.47(8) . . ?
C14 Si6 C4 109.32(8) . . ?
C2 C1 Si3 103.73(11) . . ?
C2 C1 Si4 106.86(11) . . ?
Si3 C1 Si4 108.78(8) . . ?
C2 C1 Si2 98.14(10) . . ?
Si3 C1 Si2 120.31(9) . . ?
Si4 C1 Si2 116.64(8) . . ?
C3 C2 C1 109.23(13) . . ?
C2 C3 C4 108.92(14) . . ?
C3 C4 Si6 103.00(11) . . ?
C3 C4 Si5 106.59(11) . . ?
Si6 C4 Si5 106.82(8) . . ?
C3 C4 Si2 98.01(10) . . ?
Si6 C4 Si2 121.92(9) . . ?
Si5 C4 Si2 117.84(9) . . ?

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 165.53(12) . . . . ?
Si4 C1 C2 C3 -79.61(14) . . . . ?
Si2 C1 C2 C3 41.49(15) . . . . ?
C1 C2 C3 C4 -60.25(18) . . . . ?
C2 C3 C4 Si6 167.58(12) . . . . ?
C2 C3 C4 Si5 -80.17(14) . . . . ?
C2 C3 C4 Si2 42.10(15) . . . . ?

_refine_diff_density_max         0.672
_refine_diff_density_min         -0.333
_refine_diff_density_rms         0.062

_shelxl_version_number           2014-3


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

data_SNH93b_a
_database_code_depnum_ccdc_archive 'CCDC 1908569'
loop_
_audit_author_name
_audit_author_address
'Shunya Honda'
;Tohoku University
Japan
;
_audit_update_record             
;
2019-04-08 deposited with the CCDC.	2019-05-09 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          423
_chemical_formula_moiety         'C35 H92 O3 Si12'
_chemical_formula_sum            'C35 H92 O3 Si12'
_chemical_formula_weight         898.16

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                   11.3627(5)
_cell_length_b                   16.4034(8)
_cell_length_c                   17.0141(8)
_cell_angle_alpha                112.0530(10)
_cell_angle_beta                 94.2250(10)
_cell_angle_gamma                109.5290(10)
_cell_volume                     2697.1(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9822
_cell_measurement_theta_min      2.24
_cell_measurement_theta_max      33.98

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.106
_exptl_crystal_F_000             988
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.050
_exptl_absorpt_coefficient_mu    0.317
_shelx_estimated_absorpt_T_min   0.939
_shelx_estimated_absorpt_T_max   0.984
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.6888
_exptl_absorpt_correction_T_max  0.7468
_exptl_absorpt_process_details   'SADABS Sheldrick 1996'
_exptl_absorpt_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            40126
_diffrn_reflns_av_unetI/netI     0.0196
_diffrn_reflns_av_R_equivalents  0.0207
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         1.326
_diffrn_reflns_theta_max         27.499
_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             12401
_reflns_number_gt                11155
_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)+(0.0413P)²+1.1719P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         12401
_refine_ls_number_parameters     490
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0313
_refine_ls_R_factor_gt           0.0273
_refine_ls_wR_factor_ref         0.0785
_refine_ls_wR_factor_gt          0.0751
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_restrained_S_all      1.031
_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 0.35834(3) 0.70490(2) 0.29321(2) 0.01387(7) Uani 1 1 d . . . . .
Si2 Si 0.27886(3) 0.56094(2) 0.16344(2) 0.01575(7) Uani 1 1 d . . . . .
Si3 Si 0.37113(3) 0.45665(2) 0.18191(2) 0.01584(7) Uani 1 1 d . . . . .
Si4 Si 0.28533(3) 0.29947(2) 0.17667(2) 0.01234(7) Uani 1 1 d . . . . .
C1 C 0.27203(12) 0.79083(9) 0.31766(8) 0.0167(2) Uani 1 1 d . . . . .
C2 C 0.38957(13) 0.89066(9) 0.35845(9) 0.0200(3) Uani 1 1 d . . . . .
H82 H 0.4075 0.9135 0.3127 0.024 Uiso 1 1 calc R U . . .
H83 H 0.3669 0.9377 0.4043 0.024 Uiso 1 1 calc R U . . .
C3 C 0.51095(13) 0.88487(9) 0.39811(9) 0.0194(3) Uani 1 1 d . . . . .
H84 H 0.5032 0.8825 0.4549 0.023 Uiso 1 1 calc R U . . .
H85 H 0.5862 0.9433 0.4088 0.023 Uiso 1 1 calc R U . . .
C4 C 0.53354(12) 0.79419(8) 0.33678(8) 0.0155(2) Uani 1 1 d . . . . .
Si5 Si 0.16298(4) 0.78626(3) 0.22435(2) 0.02081(8) Uani 1 1 d . . . . .
C5 C 0.15064(16) 0.90548(11) 0.25539(11) 0.0320(3) Uani 1 1 d . . . . .
H1 H 0.2356 0.9546 0.2657 0.048 Uiso 1 1 calc R U . . .
H2 H 0.1180 0.9218 0.3085 0.048 Uiso 1 1 calc R U . . .
H3 H 0.0918 0.9021 0.2081 0.048 Uiso 1 1 calc R U . . .
C6 C -0.00386(14) 0.69283(11) 0.19262(11) 0.0298(3) Uani 1 1 d . . . . .
H4 H -0.0551 0.6953 0.1453 0.045 Uiso 1 1 calc R U . . .
H5 H -0.0432 0.7049 0.2430 0.045 Uiso 1 1 calc R U . . .
H6 H -0.0004 0.6295 0.1730 0.045 Uiso 1 1 calc R U . . .
C7 C 0.22024(16) 0.76318(12) 0.12055(10) 0.0300(3) Uani 1 1 d . . . . .
H7 H 0.2503 0.7111 0.1079 0.045 Uiso 1 1 calc R U . . .
H8 H 0.2908 0.8212 0.1268 0.045 Uiso 1 1 calc R U . . .
H9 H 0.1495 0.7452 0.0727 0.045 Uiso 1 1 calc R U . . .
Si6 Si 0.17824(4) 0.77319(3) 0.40281(2) 0.01954(8) Uani 1 1 d . . . . .
C8 C 0.08044(15) 0.84804(11) 0.43014(11) 0.0293(3) Uani 1 1 d . . . . .
H10 H 0.0146 0.8277 0.3784 0.044 Uiso 1 1 calc R U . . .
H11 H 0.1364 0.9154 0.4494 0.044 Uiso 1 1 calc R U . . .
H12 H 0.0392 0.8401 0.4769 0.044 Uiso 1 1 calc R U . . .
C9 C 0.28547(16) 0.81295(12) 0.51078(10) 0.0294(3) Uani 1 1 d . . . . .
H13 H 0.3438 0.8800 0.5315 0.044 Uiso 1 1 calc R U . . .
H14 H 0.3355 0.7733 0.5042 0.044 Uiso 1 1 calc R U . . .
H15 H 0.2331 0.8063 0.5530 0.044 Uiso 1 1 calc R U . . .
C10 C 0.06781(14) 0.64512(10) 0.36645(10) 0.0270(3) Uani 1 1 d . . . . .
H16 H -0.0209 0.6403 0.3634 0.041 Uiso 1 1 calc R U . . .
H17 H 0.0904 0.6217 0.4082 0.041 Uiso 1 1 calc R U . . .
H18 H 0.0762 0.6065 0.3088 0.041 Uiso 1 1 calc R U . . .
Si7 Si 0.62637(4) 0.82067(3) 0.25474(2) 0.01974(8) Uani 1 1 d . . . . .
C11 C 0.57401(15) 0.89200(12) 0.20694(11) 0.0314(3) Uani 1 1 d . . . . .
H19 H 0.5865 0.9539 0.2535 0.047 Uiso 1 1 calc R U . . .
H20 H 0.4831 0.8572 0.1773 0.047 Uiso 1 1 calc R U . . .
H21 H 0.6250 0.9023 0.1650 0.047 Uiso 1 1 calc R U . . .
C12 C 0.80051(14) 0.89955(11) 0.30526(11) 0.0289(3) Uani 1 1 d . . . . .
H22 H 0.8428 0.9139 0.2611 0.043 Uiso 1 1 calc R U . . .
H23 H 0.8416 0.8667 0.3282 0.043 Uiso 1 1 calc R U . . .
H24 H 0.8080 0.9592 0.3528 0.043 Uiso 1 1 calc R U . . .
C13 C 0.61546(16) 0.70671(11) 0.16435(10) 0.0307(3) Uani 1 1 d . . . . .
H25 H 0.5440 0.6858 0.1158 0.046 Uiso 1 1 calc R U . . .
H26 H 0.6010 0.6572 0.1857 0.046 Uiso 1 1 calc R U . . .
H27 H 0.6957 0.7178 0.1444 0.046 Uiso 1 1 calc R U . . .
Si8 Si 0.63619(3) 0.76624(2) 0.40989(2) 0.01669(7) Uani 1 1 d . . . . .
C14 C 0.76313(14) 0.87940(10) 0.49610(9) 0.0265(3) Uani 1 1 d . . . . .
H28 H 0.8124 0.8637 0.5339 0.040 Uiso 1 1 calc R U . . .
H29 H 0.7225 0.9201 0.5310 0.040 Uiso 1 1 calc R U . . .
H30 H 0.8207 0.9134 0.4684 0.040 Uiso 1 1 calc R U . . .
C15 C 0.71809(13) 0.68807(10) 0.34990(9) 0.0233(3) Uani 1 1 d . . . . .
H31 H 0.7709 0.6789 0.3915 0.035 Uiso 1 1 calc R U . . .
H32 H 0.7727 0.7185 0.3185 0.035 Uiso 1 1 calc R U . . .
H33 H 0.6535 0.6259 0.3083 0.035 Uiso 1 1 calc R U . . .
C16 C 0.54711(14) 0.70788(10) 0.47536(9) 0.0240(3) Uani 1 1 d . . . . .
H34 H 0.4751 0.6486 0.4362 0.036 Uiso 1 1 calc R U . . .
H35 H 0.5146 0.7512 0.5157 0.036 Uiso 1 1 calc R U . . .
H36 H 0.6050 0.6932 0.5085 0.036 Uiso 1 1 calc R U . . .
C17 C 0.17258(11) 0.26254(8) 0.24584(8) 0.0147(2) Uani 1 1 d . . . . .
C18 C 0.25466(12) 0.23151(9) 0.29907(8) 0.0188(2) Uani 1 1 d . . . . .
H86 H 0.3066 0.2872 0.3544 0.023 Uiso 1 1 calc R U . . .
H87 H 0.1966 0.1816 0.3135 0.023 Uiso 1 1 calc R U . . .
C19 C 0.34383(12) 0.19267(9) 0.24669(9) 0.0195(3) Uani 1 1 d . . . . .
H88 H 0.2926 0.1287 0.1990 0.023 Uiso 1 1 calc R U . . .
H89 H 0.4060 0.1858 0.2851 0.023 Uiso 1 1 calc R U . . .
C20 C 0.41848(12) 0.26236(9) 0.20713(8) 0.0153(2) Uani 1 1 d . . . . .
O1 O 0.30669(11) 0.57442(7) 0.07504(6) 0.0263(2) Uani 1 1 d . . . . .
C21 C 0.31027(17) 0.50719(11) -0.00597(9) 0.0309(3) Uani 1 1 d . . . . .
H37 H 0.3985 0.5115 -0.0056 0.046 Uiso 1 1 calc R U . . .
H38 H 0.2801 0.5210 -0.0531 0.046 Uiso 1 1 calc R U . . .
H39 H 0.2548 0.4426 -0.0151 0.046 Uiso 1 1 calc R U . . .
O2 O 0.12352(9) 0.52248(7) 0.15845(6) 0.0231(2) Uani 1 1 d . . . . .
C22 C 0.03147(15) 0.44031(11) 0.08657(10) 0.0319(3) Uani 1 1 d . . . . .
H40 H 0.0304 0.4525 0.0344 0.048 Uiso 1 1 calc R U . . .
H41 H -0.0537 0.4268 0.0996 0.048 Uiso 1 1 calc R U . . .
H42 H 0.0545 0.3853 0.0763 0.048 Uiso 1 1 calc R U . . .
O3 O 0.20715(9) 0.22797(6) 0.07413(6) 0.01760(18) Uani 1 1 d . . . . .
C23 C 0.19598(16) 0.24504(11) -0.00087(9) 0.0276(3) Uani 1 1 d . . . . .
H43 H 0.1077 0.2371 -0.0196 0.041 Uiso 1 1 calc R U . . .
H44 H 0.2179 0.1995 -0.0476 0.041 Uiso 1 1 calc R U . . .
H45 H 0.2546 0.3104 0.0126 0.041 Uiso 1 1 calc R U . . .
Si9 Si 0.46555(4) 0.19269(3) 0.10514(2) 0.01983(8) Uani 1 1 d . . . . .
C24 C 0.33393(15) 0.07544(10) 0.02999(10) 0.0290(3) Uani 1 1 d . . . . .
H46 H 0.3646 0.0434 -0.0204 0.043 Uiso 1 1 calc R U . . .
H47 H 0.2601 0.0867 0.0101 0.043 Uiso 1 1 calc R U . . .
H48 H 0.3083 0.0349 0.0610 0.043 Uiso 1 1 calc R U . . .
C25 C 0.51868(16) 0.26248(11) 0.03953(10) 0.0299(3) Uani 1 1 d . . . . .
H49 H 0.5993 0.3176 0.0726 0.045 Uiso 1 1 calc R U . . .
H50 H 0.4528 0.2849 0.0270 0.045 Uiso 1 1 calc R U . . .
H51 H 0.5318 0.2215 -0.0153 0.045 Uiso 1 1 calc R U . . .
C26 C 0.59844(15) 0.15650(12) 0.13041(11) 0.0344(4) Uani 1 1 d . . . . .
H52 H 0.6122 0.1153 0.0760 0.052 Uiso 1 1 calc R U . . .
H53 H 0.5753 0.1216 0.1665 0.052 Uiso 1 1 calc R U . . .
H54 H 0.6773 0.2137 0.1620 0.052 Uiso 1 1 calc R U . . .
Si10 Si 0.57270(3) 0.35766(3) 0.29119(2) 0.01712(8) Uani 1 1 d . . . . .
C27 C 0.55324(13) 0.45148(10) 0.38813(9) 0.0234(3) Uani 1 1 d . . . . .
H55 H 0.6376 0.4958 0.4266 0.035 Uiso 1 1 calc R U . . .
H56 H 0.4995 0.4210 0.4198 0.035 Uiso 1 1 calc R U . . .
H57 H 0.5124 0.4867 0.3687 0.035 Uiso 1 1 calc R U . . .
C28 C 0.69054(13) 0.42469(10) 0.24284(9) 0.0232(3) Uani 1 1 d . . . . .
H58 H 0.6481 0.4507 0.2119 0.035 Uiso 1 1 calc R U . . .
H59 H 0.7223 0.3812 0.2020 0.035 Uiso 1 1 calc R U . . .
H60 H 0.7626 0.4771 0.2894 0.035 Uiso 1 1 calc R U . . .
C29 C 0.65473(14) 0.30220(12) 0.34338(10) 0.0273(3) Uani 1 1 d . . . . .
H61 H 0.7424 0.3480 0.3746 0.041 Uiso 1 1 calc R U . . .
H62 H 0.6574 0.2446 0.2983 0.041 Uiso 1 1 calc R U . . .
H63 H 0.6072 0.2851 0.3845 0.041 Uiso 1 1 calc R U . . .
Si11 Si 0.01752(3) 0.15470(2) 0.17481(2) 0.01765(8) Uani 1 1 d . . . . .
C30 C -0.06773(13) 0.17328(10) 0.08837(9) 0.0224(3) Uani 1 1 d . . . . .
H64 H -0.0474 0.1422 0.0326 0.034 Uiso 1 1 calc R U . . .
H65 H -0.0398 0.2419 0.1043 0.034 Uiso 1 1 calc R U . . .
H66 H -0.1605 0.1454 0.0830 0.034 Uiso 1 1 calc R U . . .
C31 C 0.04248(14) 0.04089(10) 0.12183(10) 0.0263(3) Uani 1 1 d . . . . .
H67 H -0.0402 -0.0118 0.0888 0.039 Uiso 1 1 calc R U . . .
H68 H 0.0810 0.0276 0.1666 0.039 Uiso 1 1 calc R U . . .
H69 H 0.0998 0.0473 0.0823 0.039 Uiso 1 1 calc R U . . .
C32 C -0.09958(14) 0.12443(11) 0.24232(11) 0.0304(3) Uani 1 1 d . . . . .
H70 H -0.1757 0.0674 0.2047 0.046 Uiso 1 1 calc R U . . .
H71 H -0.1249 0.1782 0.2703 0.046 Uiso 1 1 calc R U . . .
H72 H -0.0591 0.1120 0.2871 0.046 Uiso 1 1 calc R U . . .
Si12 Si 0.12427(3) 0.35544(3) 0.32749(2) 0.01680(8) Uani 1 1 d . . . . .
C33 C -0.01333(13) 0.37249(10) 0.27780(10) 0.0259(3) Uani 1 1 d . . . . .
H73 H -0.0370 0.4178 0.3235 0.039 Uiso 1 1 calc R U . . .
H74 H -0.0868 0.3110 0.2490 0.039 Uiso 1 1 calc R U . . .
H75 H 0.0119 0.3975 0.2349 0.039 Uiso 1 1 calc R U . . .
C34 C 0.08527(16) 0.32416(12) 0.42065(10) 0.0319(3) Uani 1 1 d . . . . .
H76 H 0.1613 0.3233 0.4511 0.048 Uiso 1 1 calc R U . . .
H77 H 0.0153 0.2609 0.3982 0.048 Uiso 1 1 calc R U . . .
H78 H 0.0589 0.3719 0.4612 0.048 Uiso 1 1 calc R U . . .
C35 C 0.25396(13) 0.47780(9) 0.38232(9) 0.0217(3) Uani 1 1 d . . . . .
H79 H 0.2773 0.5023 0.3388 0.033 Uiso 1 1 calc R U . . .
H80 H 0.3292 0.4750 0.4115 0.033 Uiso 1 1 calc R U . . .
H81 H 0.2234 0.5204 0.4254 0.033 Uiso 1 1 calc R U . . .
H92 H 0.3312(15) 0.6594(11) 0.3491(10) 0.022(4) Uiso 1 1 d . . . . .
H91 H 0.4528(18) 0.5156(13) 0.2634(12) 0.038(5) Uiso 1 1 d . . . . .
H90 H 0.4540(18) 0.4494(13) 0.1257(12) 0.037(5) Uiso 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Si1 C1 1.9145(13) . ?
Si1 C4 1.9172(13) . ?
Si1 Si2 2.3732(5) . ?
Si2 O1 1.6385(10) . ?
Si2 O2 1.6473(10) . ?
Si2 Si3 2.3828(5) . ?
Si3 Si4 2.3959(5) . ?
Si4 O3 1.6574(9) . ?
Si4 C17 1.9057(12) . ?
Si4 C20 1.9146(12) . ?
C1 C2 1.5795(17) . ?
C1 Si5 1.9027(13) . ?
C1 Si6 1.9117(13) . ?
C2 C3 1.5378(19) . ?
C3 C4 1.5801(17) . ?
C4 Si7 1.9014(13) . ?
C4 Si8 1.9210(13) . ?
Si5 C7 1.8755(16) . ?
Si5 C6 1.8761(16) . ?
Si5 C5 1.8819(15) . ?
Si6 C10 1.8756(15) . ?
Si6 C8 1.8757(15) . ?
Si6 C9 1.8772(16) . ?
Si7 C11 1.8691(16) . ?
Si7 C12 1.8790(15) . ?
Si7 C13 1.8797(15) . ?
Si8 C16 1.8710(14) . ?
Si8 C15 1.8727(14) . ?
Si8 C14 1.8791(14) . ?
C17 C18 1.5775(17) . ?
C17 Si12 1.9066(13) . ?
C17 Si11 1.9212(12) . ?
C18 C19 1.5379(18) . ?
C19 C20 1.5788(17) . ?
C20 Si9 1.9130(13) . ?
C20 Si10 1.9185(13) . ?
O1 C21 1.4192(17) . ?
O2 C22 1.4274(17) . ?
O3 C23 1.4109(16) . ?
Si9 C26 1.8742(15) . ?
Si9 C25 1.8755(16) . ?
Si9 C24 1.8760(15) . ?
Si10 C27 1.8743(14) . ?
Si10 C28 1.8802(14) . ?
Si10 C29 1.8807(14) . ?
Si11 C31 1.8725(14) . ?
Si11 C30 1.8758(14) . ?
Si11 C32 1.8836(15) . ?
Si12 C35 1.8667(14) . ?
Si12 C33 1.8742(15) . ?
Si12 C34 1.8799(15) . ?

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 C4 100.45(5) . . ?
C1 Si1 Si2 120.48(4) . . ?
C4 Si1 Si2 125.39(4) . . ?
O1 Si2 O2 109.83(6) . . ?
O1 Si2 Si1 114.79(4) . . ?
O2 Si2 Si1 101.76(4) . . ?
O1 Si2 Si3 109.44(4) . . ?
O2 Si2 Si3 112.77(4) . . ?
Si1 Si2 Si3 108.161(18) . . ?
Si2 Si3 Si4 134.237(19) . . ?
O3 Si4 C17 105.67(5) . . ?
O3 Si4 C20 109.59(5) . . ?
C17 Si4 C20 99.61(5) . . ?
O3 Si4 Si3 105.16(4) . . ?
C17 Si4 Si3 124.70(4) . . ?
C20 Si4 Si3 111.52(4) . . ?
C2 C1 Si5 108.47(8) . . ?
C2 C1 Si6 111.01(8) . . ?
Si5 C1 Si6 109.74(6) . . ?
C2 C1 Si1 101.07(8) . . ?
Si5 C1 Si1 119.31(7) . . ?
Si6 C1 Si1 106.89(6) . . ?
C3 C2 C1 112.13(10) . . ?
C2 C3 C4 112.20(10) . . ?
C3 C4 Si7 110.79(8) . . ?
C3 C4 Si1 98.54(8) . . ?
Si7 C4 Si1 117.61(6) . . ?
C3 C4 Si8 106.93(8) . . ?
Si7 C4 Si8 108.06(6) . . ?
Si1 C4 Si8 114.11(6) . . ?
C7 Si5 C6 105.16(7) . . ?
C7 Si5 C5 104.42(7) . . ?
C6 Si5 C5 107.82(7) . . ?
C7 Si5 C1 115.30(6) . . ?
C6 Si5 C1 113.77(7) . . ?
C5 Si5 C1 109.71(6) . . ?
C10 Si6 C8 108.11(7) . . ?
C10 Si6 C9 107.87(7) . . ?
C8 Si6 C9 103.28(7) . . ?
C10 Si6 C1 111.94(6) . . ?
C8 Si6 C1 112.47(6) . . ?
C9 Si6 C1 112.68(6) . . ?
C11 Si7 C12 101.58(7) . . ?
C11 Si7 C13 109.21(8) . . ?
C12 Si7 C13 108.38(7) . . ?
C11 Si7 C4 113.86(6) . . ?
C12 Si7 C4 112.73(6) . . ?
C13 Si7 C4 110.63(6) . . ?
C16 Si8 C15 106.08(7) . . ?
C16 Si8 C14 102.68(7) . . ?
C15 Si8 C14 107.68(7) . . ?
C16 Si8 C4 114.63(6) . . ?
C15 Si8 C4 114.15(6) . . ?
C14 Si8 C4 110.78(6) . . ?
C18 C17 Si4 101.24(8) . . ?
C18 C17 Si12 107.60(8) . . ?
Si4 C17 Si12 119.30(6) . . ?
C18 C17 Si11 109.55(8) . . ?
Si4 C17 Si11 111.43(6) . . ?
Si12 C17 Si11 107.29(6) . . ?
C19 C18 C17 111.09(10) . . ?
C18 C19 C20 110.54(10) . . ?
C19 C20 Si9 109.86(8) . . ?
C19 C20 Si4 99.53(8) . . ?
Si9 C20 Si4 110.64(6) . . ?
C19 C20 Si10 108.81(8) . . ?
Si9 C20 Si10 108.11(6) . . ?
Si4 C20 Si10 119.40(6) . . ?
C21 O1 Si2 129.65(9) . . ?
C22 O2 Si2 123.17(10) . . ?
C23 O3 Si4 132.03(9) . . ?
C26 Si9 C25 107.12(8) . . ?
C26 Si9 C24 102.77(7) . . ?
C25 Si9 C24 107.18(7) . . ?
C26 Si9 C20 112.93(7) . . ?
C25 Si9 C20 112.38(6) . . ?
C24 Si9 C20 113.78(6) . . ?
C27 Si10 C28 105.64(7) . . ?
C27 Si10 C29 102.06(7) . . ?
C28 Si10 C29 108.07(7) . . ?
C27 Si10 C20 116.55(6) . . ?
C28 Si10 C20 112.88(6) . . ?
C29 Si10 C20 110.80(6) . . ?
C31 Si11 C30 108.46(7) . . ?
C31 Si11 C32 102.19(7) . . ?
C30 Si11 C32 107.20(7) . . ?
C31 Si11 C17 113.30(6) . . ?
C30 Si11 C17 113.48(6) . . ?
C32 Si11 C17 111.46(6) . . ?
C35 Si12 C33 104.59(6) . . ?
C35 Si12 C34 103.36(7) . . ?
C33 Si12 C34 109.77(7) . . ?
C35 Si12 C17 114.38(6) . . ?
C33 Si12 C17 113.44(6) . . ?
C34 Si12 C17 110.67(7) . . ?

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
Si5 C1 C2 C3 -150.76(9) . . . . ?
Si6 C1 C2 C3 88.59(11) . . . . ?
Si1 C1 C2 C3 -24.50(12) . . . . ?
C1 C2 C3 C4 44.36(14) . . . . ?
C2 C3 C4 Si7 86.43(11) . . . . ?
C2 C3 C4 Si1 -37.51(11) . . . . ?
C2 C3 C4 Si8 -156.03(9) . . . . ?
Si4 C17 C18 C19 -29.80(11) . . . . ?
Si12 C17 C18 C19 -155.70(9) . . . . ?
Si11 C17 C18 C19 87.97(11) . . . . ?
C17 C18 C19 C20 48.05(14) . . . . ?
C18 C19 C20 Si9 -154.26(9) . . . . ?
C18 C19 C20 Si4 -38.11(11) . . . . ?
C18 C19 C20 Si10 87.55(11) . . . . ?
O2 Si2 O1 C21 -87.82(14) . . . . ?
Si1 Si2 O1 C21 158.28(12) . . . . ?
Si3 Si2 O1 C21 36.47(14) . . . . ?
O1 Si2 O2 C22 52.65(12) . . . . ?
Si1 Si2 O2 C22 174.68(11) . . . . ?
Si3 Si2 O2 C22 -69.69(12) . . . . ?
C17 Si4 O3 C23 139.01(12) . . . . ?
C20 Si4 O3 C23 -114.50(13) . . . . ?
Si3 Si4 O3 C23 5.49(13) . . . . ?

_refine_diff_density_max         0.475
_refine_diff_density_min         -0.344
_refine_diff_density_rms         0.050


_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: hexane'
####################################################################### 
# 
# 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_TK87b_a
_database_code_depnum_ccdc_archive 'CCDC 1908504'
loop_
_audit_author_name
_audit_author_address
'Tomoyuki Kosai'
;Tohoku University
Japan
;
_audit_update_record             
;
2019-04-08 deposited with the CCDC.	2019-05-09 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          507
_chemical_formula_moiety         'C32 H80 Cl6 Si12'
_chemical_formula_sum            'C32 H80 Cl6 Si12'
_chemical_formula_weight         1014.74

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'
Cl Cl 0.1484 0.1585 '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                   11.7581(5)
_cell_length_b                   20.4191(9)
_cell_length_c                   23.6336(10)
_cell_angle_alpha                99.4190(10)
_cell_angle_beta                 104.2580(10)
_cell_angle_gamma                94.1290(10)
_cell_volume                     5387.7(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9095
_cell_measurement_theta_min      2.19
_cell_measurement_theta_max      34.09

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.251
_exptl_crystal_F_000             2168
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.100
_exptl_absorpt_coefficient_mu    0.609
_shelx_estimated_absorpt_T_min   0.888
_shelx_estimated_absorpt_T_max   0.942
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.6275
_exptl_absorpt_correction_T_max  0.7467
_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            81679
_diffrn_reflns_av_unetI/netI     0.0312
_diffrn_reflns_av_R_equivalents  0.0304
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_theta_min         1.018
_diffrn_reflns_theta_max         27.499
_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             24772
_reflns_number_gt                20660
_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)+(0.0460P)²+3.7061P] 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         24772
_refine_ls_number_parameters     949
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0430
_refine_ls_R_factor_gt           0.0330
_refine_ls_wR_factor_ref         0.0913
_refine_ls_wR_factor_gt          0.0861
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_restrained_S_all      1.023
_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 0.79919(5) 0.73345(3) 0.11928(2) 0.01337(10) Uani 1 1 d . . . . .
Si2 Si 0.89584(5) 0.71313(3) 0.21746(2) 0.01406(10) Uani 1 1 d . . . . .
Si3 Si 0.87334(5) 0.79397(3) 0.29925(2) 0.01333(10) Uani 1 1 d . . . . .
Si4 Si 0.83587(4) 0.76525(2) 0.38845(2) 0.01111(10) Uani 1 1 d . . . . .
Si5 Si 0.52159(5) 0.69896(3) 0.12326(2) 0.01923(12) Uani 1 1 d . . . . .
Si6 Si 0.58813(6) 0.81886(3) 0.06656(3) 0.02277(13) Uani 1 1 d . . . . .
Si7 Si 0.84684(5) 0.59179(3) 0.05354(2) 0.02229(13) Uani 1 1 d . . . . .
Si8 Si 0.97888(6) 0.72151(4) 0.03222(3) 0.03216(16) Uani 1 1 d . . . . .
Si9 Si 0.57300(5) 0.78308(3) 0.40720(2) 0.01718(11) Uani 1 1 d . . . . .
Si10 Si 0.75195(5) 0.91083(3) 0.43408(2) 0.01407(10) Uani 1 1 d . . . . .
Si11 Si 0.94803(5) 0.66311(3) 0.47295(2) 0.01546(11) Uani 1 1 d . . . . .
Si12 Si 1.11582(5) 0.77413(3) 0.45127(2) 0.01475(11) Uani 1 1 d . . . . .
Cl1 Cl 0.88516(5) 0.83192(2) 0.14471(2) 0.02257(11) Uani 1 1 d . . . . .
Cl2 Cl 0.88240(5) 0.61748(2) 0.23504(2) 0.02331(11) Uani 1 1 d . . . . .
Cl3 Cl 1.07391(4) 0.73004(3) 0.22217(2) 0.02274(11) Uani 1 1 d . . . . .
Cl4 Cl 0.72114(4) 0.83250(3) 0.26239(2) 0.02107(10) Uani 1 1 d . . . . .
Cl5 Cl 1.00816(4) 0.86875(2) 0.30848(2) 0.02113(10) Uani 1 1 d . . . . .
Cl6 Cl 0.74124(4) 0.67417(2) 0.33848(2) 0.01774(9) Uani 1 1 d . . . . .
C1 C 0.63455(17) 0.73460(10) 0.08552(8) 0.0157(4) Uani 1 1 d . . . . .
C2 C 0.61955(17) 0.68741(10) 0.02291(8) 0.0185(4) Uani 1 1 d . . . . .
H1 H 0.5999 0.6404 0.0261 0.022 Uiso 1 1 calc R U . . .
H2 H 0.5535 0.6997 -0.0069 0.022 Uiso 1 1 calc R U . . .
C3 C 0.73227(18) 0.69372(11) 0.00251(8) 0.0198(4) Uani 1 1 d . . . . .
H3 H 0.7432 0.7380 -0.0085 0.024 Uiso 1 1 calc R U . . .
H4 H 0.7254 0.6590 -0.0331 0.024 Uiso 1 1 calc R U . . .
C4 C 0.84285(17) 0.68540(10) 0.05332(8) 0.0180(4) Uani 1 1 d . . . . .
C5 C 0.4063(2) 0.63747(13) 0.06649(11) 0.0335(5) Uani 1 1 d . . . . .
H5 H 0.4420 0.5976 0.0538 0.050 Uiso 1 1 calc R U . . .
H6 H 0.3743 0.6579 0.0321 0.050 Uiso 1 1 calc R U . . .
H7 H 0.3425 0.6248 0.0839 0.050 Uiso 1 1 calc R U . . .
C6 C 0.44051(19) 0.76108(12) 0.16016(10) 0.0290(5) Uani 1 1 d . . . . .
H8 H 0.3793 0.7374 0.1734 0.044 Uiso 1 1 calc R U . . .
H9 H 0.4037 0.7884 0.1319 0.044 Uiso 1 1 calc R U . . .
H10 H 0.4961 0.7899 0.1945 0.044 Uiso 1 1 calc R U . . .
C7 C 0.5864(2) 0.65356(11) 0.18385(10) 0.0259(5) Uani 1 1 d . . . . .
H11 H 0.6476 0.6838 0.2147 0.039 Uiso 1 1 calc R U . . .
H12 H 0.6214 0.6151 0.1675 0.039 Uiso 1 1 calc R U . . .
H13 H 0.5241 0.6380 0.2012 0.039 Uiso 1 1 calc R U . . .
C8 C 0.4283(2) 0.80466(13) 0.02202(10) 0.0342(6) Uani 1 1 d . . . . .
H14 H 0.3994 0.8478 0.0174 0.051 Uiso 1 1 calc R U . . .
H15 H 0.3808 0.7810 0.0428 0.051 Uiso 1 1 calc R U . . .
H16 H 0.4217 0.7778 -0.0172 0.051 Uiso 1 1 calc R U . . .
C9 C 0.6640(3) 0.85398(13) 0.01546(12) 0.0396(6) Uani 1 1 d . . . . .
H17 H 0.6368 0.8972 0.0093 0.059 Uiso 1 1 calc R U . . .
H18 H 0.6453 0.8231 -0.0228 0.059 Uiso 1 1 calc R U . . .
H19 H 0.7496 0.8601 0.0330 0.059 Uiso 1 1 calc R U . . .
C10 C 0.6051(2) 0.88857(11) 0.13130(10) 0.0306(5) Uani 1 1 d . . . . .
H20 H 0.6890 0.9003 0.1520 0.046 Uiso 1 1 calc R U . . .
H21 H 0.5623 0.8743 0.1587 0.046 Uiso 1 1 calc R U . . .
H22 H 0.5728 0.9276 0.1171 0.046 Uiso 1 1 calc R U . . .
C11 C 0.7330(2) 0.55250(12) 0.08431(11) 0.0315(5) Uani 1 1 d . . . . .
H23 H 0.6542 0.5534 0.0584 0.047 Uiso 1 1 calc R U . . .
H24 H 0.7383 0.5774 0.1242 0.047 Uiso 1 1 calc R U . . .
H25 H 0.7466 0.5061 0.0865 0.047 Uiso 1 1 calc R U . . .
C12 C 0.9936(2) 0.57400(13) 0.09682(10) 0.0339(6) Uani 1 1 d . . . . .
H26 H 1.0140 0.6017 0.1367 0.051 Uiso 1 1 calc R U . . .
H27 H 1.0540 0.5844 0.0765 0.051 Uiso 1 1 calc R U . . .
H28 H 0.9896 0.5267 0.0999 0.051 Uiso 1 1 calc R U . . .
C13 C 0.8123(2) 0.54128(13) -0.02352(10) 0.0392(6) Uani 1 1 d . . . . .
H29 H 0.8309 0.4955 -0.0216 0.059 Uiso 1 1 calc R U . . .
H30 H 0.8598 0.5615 -0.0463 0.059 Uiso 1 1 calc R U . . .
H31 H 0.7282 0.5404 -0.0430 0.059 Uiso 1 1 calc R U . . .
C14 C 0.9591(3) 0.80372(17) 0.00815(13) 0.0517(8) Uani 1 1 d . . . . .
H32 H 0.9486 0.8365 0.0411 0.078 Uiso 1 1 calc R U . . .
H33 H 0.8893 0.7985 -0.0257 0.078 Uiso 1 1 calc R U . . .
H34 H 1.0291 0.8193 -0.0036 0.078 Uiso 1 1 calc R U . . .
C15 C 1.0044(3) 0.66540(19) -0.03406(12) 0.0557(9) Uani 1 1 d . . . . .
H35 H 1.0661 0.6878 -0.0479 0.084 Uiso 1 1 calc R U . . .
H36 H 0.9310 0.6556 -0.0660 0.084 Uiso 1 1 calc R U . . .
H37 H 1.0295 0.6236 -0.0227 0.084 Uiso 1 1 calc R U . . .
C16 C 1.1218(2) 0.73544(16) 0.09064(11) 0.0423(7) Uani 1 1 d . . . . .
H38 H 1.1864 0.7466 0.0732 0.063 Uiso 1 1 calc R U . . .
H39 H 1.1346 0.6947 0.1071 0.063 Uiso 1 1 calc R U . . .
H40 H 1.1195 0.7724 0.1224 0.063 Uiso 1 1 calc R U . . .
C17 C 0.73856(16) 0.81503(9) 0.42851(8) 0.0129(4) Uani 1 1 d . . . . .
C18 C 0.79276(17) 0.80075(10) 0.49291(8) 0.0145(4) Uani 1 1 d . . . . .
H41 H 0.7734 0.8349 0.5229 0.017 Uiso 1 1 calc R U . . .
H42 H 0.7579 0.7564 0.4962 0.017 Uiso 1 1 calc R U . . .
C19 C 0.92644(17) 0.80228(9) 0.50495(8) 0.0140(4) Uani 1 1 d . . . . .
H43 H 0.9592 0.7897 0.5439 0.017 Uiso 1 1 calc R U . . .
H44 H 0.9624 0.8480 0.5062 0.017 Uiso 1 1 calc R U . . .
C20 C 0.95653(16) 0.75165(9) 0.45408(8) 0.0121(3) Uani 1 1 d . . . . .
C21 C 0.49658(18) 0.77630(12) 0.32698(10) 0.0257(5) Uani 1 1 d . . . . .
H45 H 0.5296 0.7427 0.3030 0.039 Uiso 1 1 calc R U . . .
H46 H 0.5081 0.8197 0.3153 0.039 Uiso 1 1 calc R U . . .
H47 H 0.4119 0.7629 0.3205 0.039 Uiso 1 1 calc R U . . .
C22 C 0.4933(2) 0.83764(12) 0.45274(11) 0.0287(5) Uani 1 1 d . . . . .
H48 H 0.4095 0.8201 0.4419 0.043 Uiso 1 1 calc R U . . .
H49 H 0.5012 0.8833 0.4451 0.043 Uiso 1 1 calc R U . . .
H50 H 0.5277 0.8380 0.4950 0.043 Uiso 1 1 calc R U . . .
C23 C 0.54125(19) 0.69968(11) 0.42646(10) 0.0249(5) Uani 1 1 d . . . . .
H51 H 0.4557 0.6866 0.4151 0.037 Uiso 1 1 calc R U . . .
H52 H 0.5722 0.7023 0.4694 0.037 Uiso 1 1 calc R U . . .
H53 H 0.5792 0.6664 0.4050 0.037 Uiso 1 1 calc R U . . .
C24 C 0.63569(19) 0.94103(11) 0.37809(9) 0.0224(4) Uani 1 1 d . . . . .
H54 H 0.6449 0.9900 0.3860 0.034 Uiso 1 1 calc R U . . .
H55 H 0.5574 0.9243 0.3808 0.034 Uiso 1 1 calc R U . . .
H56 H 0.6439 0.9246 0.3381 0.034 Uiso 1 1 calc R U . . .
C25 C 0.89345(18) 0.95075(10) 0.42633(9) 0.0200(4) Uani 1 1 d . . . . .
H57 H 0.9041 0.9326 0.3872 0.030 Uiso 1 1 calc R U . . .
H58 H 0.9593 0.9415 0.4574 0.030 Uiso 1 1 calc R U . . .
H59 H 0.8914 0.9992 0.4303 0.030 Uiso 1 1 calc R U . . .
C26 C 0.7427(2) 0.95205(10) 0.50962(9) 0.0227(4) Uani 1 1 d . . . . .
H60 H 0.8154 0.9483 0.5393 0.034 Uiso 1 1 calc R U . . .
H61 H 0.6749 0.9300 0.5192 0.034 Uiso 1 1 calc R U . . .
H62 H 0.7331 0.9993 0.5098 0.034 Uiso 1 1 calc R U . . .
C27 C 0.79988(19) 0.61568(11) 0.46366(10) 0.0235(4) Uani 1 1 d . . . . .
H63 H 0.8105 0.5752 0.4807 0.035 Uiso 1 1 calc R U . . .
H64 H 0.7591 0.6032 0.4213 0.035 Uiso 1 1 calc R U . . .
H65 H 0.7526 0.6438 0.4841 0.035 Uiso 1 1 calc R U . . .
C28 C 1.0162(2) 0.66909(11) 0.55443(9) 0.0242(4) Uani 1 1 d . . . . .
H66 H 0.9612 0.6861 0.5768 0.036 Uiso 1 1 calc R U . . .
H67 H 1.0898 0.6996 0.5666 0.036 Uiso 1 1 calc R U . . .
H68 H 1.0332 0.6247 0.5624 0.036 Uiso 1 1 calc R U . . .
C29 C 1.02631(19) 0.60660(10) 0.42877(10) 0.0223(4) Uani 1 1 d . . . . .
H69 H 1.1104 0.6236 0.4394 0.034 Uiso 1 1 calc R U . . .
H70 H 0.9921 0.6051 0.3863 0.034 Uiso 1 1 calc R U . . .
H71 H 1.0175 0.5615 0.4375 0.034 Uiso 1 1 calc R U . . .
C30 C 1.23033(18) 0.75056(11) 0.51319(10) 0.0249(5) Uani 1 1 d . . . . .
H72 H 1.3094 0.7641 0.5094 0.037 Uiso 1 1 calc R U . . .
H73 H 1.2195 0.7021 0.5109 0.037 Uiso 1 1 calc R U . . .
H74 H 1.2217 0.7733 0.5515 0.037 Uiso 1 1 calc R U . . .
C31 C 1.15537(18) 0.86638(10) 0.46227(10) 0.0215(4) Uani 1 1 d . . . . .
H75 H 1.2370 0.8758 0.4602 0.032 Uiso 1 1 calc R U . . .
H76 H 1.1478 0.8876 0.5013 0.032 Uiso 1 1 calc R U . . .
H77 H 1.1020 0.8842 0.4311 0.032 Uiso 1 1 calc R U . . .
C32 C 1.14071(18) 0.73435(10) 0.37872(9) 0.0210(4) Uani 1 1 d . . . . .
H78 H 1.1596 0.7692 0.3574 0.032 Uiso 1 1 calc R U . . .
H79 H 1.0690 0.7057 0.3547 0.032 Uiso 1 1 calc R U . . .
H80 H 1.2066 0.7074 0.3862 0.032 Uiso 1 1 calc R U . . .
Si13 Si 0.58669(4) 0.61658(2) 0.73726(2) 0.01136(10) Uani 1 1 d . . . . .
Si14 Si 0.60307(5) 0.72741(3) 0.71378(2) 0.01598(11) Uani 1 1 d . . . . .
Si15 Si 0.79351(5) 0.77693(3) 0.71521(2) 0.01580(11) Uani 1 1 d . . . . .
Si16 Si 0.87785(4) 0.87964(2) 0.78389(2) 0.01132(10) Uani 1 1 d . . . . .
Si17 Si 0.67787(5) 0.54022(3) 0.62470(2) 0.01628(11) Uani 1 1 d . . . . .
Si18 Si 0.75748(5) 0.49839(3) 0.74781(2) 0.01614(11) Uani 1 1 d . . . . .
Si19 Si 0.30264(4) 0.59483(3) 0.68399(2) 0.01468(11) Uani 1 1 d . . . . .
Si20 Si 0.40659(5) 0.60573(3) 0.82087(2) 0.01644(11) Uani 1 1 d . . . . .
Si21 Si 1.08049(5) 0.90886(3) 0.71773(2) 0.01403(10) Uani 1 1 d . . . . .
Si22 Si 1.15717(5) 0.87633(3) 0.84645(2) 0.01789(11) Uani 1 1 d . . . . .
Si23 Si 0.67636(5) 0.97446(3) 0.72802(3) 0.01892(12) Uani 1 1 d . . . . .
Si24 Si 0.77303(5) 0.99111(3) 0.86423(3) 0.02620(14) Uani 1 1 d . . . . .
Cl7 Cl 0.70499(4) 0.65096(2) 0.82218(2) 0.01631(9) Uani 1 1 d . . . . .
Cl8 Cl 0.48963(5) 0.74569(3) 0.63723(3) 0.02871(12) Uani 1 1 d . . . . .
Cl9 Cl 0.55289(6) 0.78980(3) 0.77843(3) 0.03496(13) Uani 1 1 d . . . . .
Cl10 Cl 0.79108(5) 0.77180(3) 0.62699(2) 0.02909(12) Uani 1 1 d . . . . .
Cl11 Cl 0.90509(5) 0.70827(3) 0.73987(3) 0.03441(13) Uani 1 1 d . . . . .
Cl12 Cl 0.86364(4) 0.83220(3) 0.85505(2) 0.02031(10) Uani 1 1 d . . . . .
C33 C 0.63589(16) 0.53860(9) 0.69841(8) 0.0125(3) Uani 1 1 d . . . . .
C34 C 0.51885(16) 0.48875(9) 0.68509(8) 0.0139(4) Uani 1 1 d . . . . .
H81 H 0.4667 0.4917 0.6459 0.017 Uiso 1 1 calc R U . . .
H82 H 0.5391 0.4424 0.6833 0.017 Uiso 1 1 calc R U . . .
C35 C 0.45333(16) 0.50524(9) 0.73312(8) 0.0139(4) Uani 1 1 d . . . . .
H83 H 0.4984 0.4934 0.7706 0.017 Uiso 1 1 calc R U . . .
H84 H 0.3748 0.4784 0.7207 0.017 Uiso 1 1 calc R U . . .
C36 C 0.43741(16) 0.58175(9) 0.74406(8) 0.0126(4) Uani 1 1 d . . . . .
C37 C 0.6164(2) 0.60557(11) 0.58354(10) 0.0262(5) Uani 1 1 d . . . . .
H85 H 0.6483 0.6499 0.6075 0.039 Uiso 1 1 calc R U . . .
H86 H 0.5301 0.6002 0.5756 0.039 Uiso 1 1 calc R U . . .
H87 H 0.6386 0.6010 0.5458 0.039 Uiso 1 1 calc R U . . .
C38 C 0.8398(2) 0.55305(13) 0.63091(11) 0.0301(5) Uani 1 1 d . . . . .
H88 H 0.8524 0.5498 0.5911 0.045 Uiso 1 1 calc R U . . .
H89 H 0.8788 0.5187 0.6503 0.045 Uiso 1 1 calc R U . . .
H90 H 0.8731 0.5974 0.6546 0.045 Uiso 1 1 calc R U . . .
C39 C 0.6183(2) 0.45945(11) 0.57169(10) 0.0320(5) Uani 1 1 d . . . . .
H91 H 0.5318 0.4543 0.5618 0.048 Uiso 1 1 calc R U . . .
H92 H 0.6478 0.4222 0.5902 0.048 Uiso 1 1 calc R U . . .
H93 H 0.6442 0.4595 0.5353 0.048 Uiso 1 1 calc R U . . .
C40 C 0.90392(18) 0.55013(12) 0.77947(10) 0.0260(5) Uani 1 1 d . . . . .
H94 H 0.8980 0.5863 0.8111 0.039 Uiso 1 1 calc R U . . .
H95 H 0.9276 0.5692 0.7481 0.039 Uiso 1 1 calc R U . . .
H96 H 0.9630 0.5220 0.7959 0.039 Uiso 1 1 calc R U . . .
C41 C 0.7821(2) 0.41825(11) 0.70332(10) 0.0275(5) Uani 1 1 d . . . . .
H97 H 0.8380 0.3954 0.7290 0.041 Uiso 1 1 calc R U . . .
H98 H 0.8142 0.4281 0.6707 0.041 Uiso 1 1 calc R U . . .
H99 H 0.7068 0.3895 0.6870 0.041 Uiso 1 1 calc R U . . .
C42 C 0.71401(18) 0.46965(11) 0.81145(9) 0.0230(4) Uani 1 1 d . . . . .
H100 H 0.7803 0.4511 0.8351 0.035 Uiso 1 1 calc R U . . .
H101 H 0.6459 0.4352 0.7962 0.035 Uiso 1 1 calc R U . . .
H102 H 0.6930 0.5076 0.8365 0.035 Uiso 1 1 calc R U . . .
C43 C 0.32132(18) 0.58704(11) 0.60664(9) 0.0215(4) Uani 1 1 d . . . . .
H103 H 0.2476 0.5944 0.5796 0.032 Uiso 1 1 calc R U . . .
H104 H 0.3410 0.5422 0.5937 0.032 Uiso 1 1 calc R U . . .
H105 H 0.3852 0.6204 0.6063 0.032 Uiso 1 1 calc R U . . .
C44 C 0.25434(19) 0.67856(11) 0.70345(10) 0.0233(4) Uani 1 1 d . . . . .
H106 H 0.3188 0.7134 0.7068 0.035 Uiso 1 1 calc R U . . .
H107 H 0.2336 0.6822 0.7415 0.035 Uiso 1 1 calc R U . . .
H108 H 0.1853 0.6841 0.6723 0.035 Uiso 1 1 calc R U . . .
C45 C 0.17674(18) 0.52842(11) 0.67395(10) 0.0248(5) Uani 1 1 d . . . . .
H109 H 0.1586 0.5278 0.7122 0.037 Uiso 1 1 calc R U . . .
H110 H 0.1988 0.4848 0.6591 0.037 Uiso 1 1 calc R U . . .
H111 H 0.1070 0.5380 0.6453 0.037 Uiso 1 1 calc R U . . .
C46 C 0.4358(2) 0.69619(11) 0.85521(10) 0.0261(5) Uani 1 1 d . . . . .
H112 H 0.4063 0.7036 0.8908 0.039 Uiso 1 1 calc R U . . .
H113 H 0.3956 0.7223 0.8267 0.039 Uiso 1 1 calc R U . . .
H114 H 0.5211 0.7103 0.8663 0.039 Uiso 1 1 calc R U . . .
C47 C 0.24931(19) 0.58064(12) 0.82010(10) 0.0275(5) Uani 1 1 d . . . . .
H115 H 0.2403 0.5908 0.8606 0.041 Uiso 1 1 calc R U . . .
H116 H 0.2288 0.5326 0.8045 0.041 Uiso 1 1 calc R U . . .
H117 H 0.1968 0.6055 0.7947 0.041 Uiso 1 1 calc R U . . .
C48 C 0.49524(18) 0.56101(11) 0.87646(9) 0.0220(4) Uani 1 1 d . . . . .
H118 H 0.5796 0.5736 0.8814 0.033 Uiso 1 1 calc R U . . .
H119 H 0.4761 0.5126 0.8624 0.033 Uiso 1 1 calc R U . . .
H120 H 0.4764 0.5734 0.9147 0.033 Uiso 1 1 calc R U . . .
C49 C 1.03784(16) 0.91103(9) 0.79130(8) 0.0126(4) Uani 1 1 d . . . . .
C50 C 1.03540(16) 0.98659(10) 0.81811(9) 0.0175(4) Uani 1 1 d . . . . .
H121 H 1.0450 0.9919 0.8615 0.021 Uiso 1 1 calc R U . . .
H122 H 1.1022 1.0141 0.8116 0.021 Uiso 1 1 calc R U . . .
C51 C 0.91888(16) 1.01103(9) 0.78903(9) 0.0177(4) Uani 1 1 d . . . . .
H123 H 0.9168 1.0146 0.7475 0.021 Uiso 1 1 calc R U . . .
H124 H 0.9137 1.0560 0.8108 0.021 Uiso 1 1 calc R U . . .
C52 C 0.80941(16) 0.96110(9) 0.78950(8) 0.0147(4) Uani 1 1 d . . . . .
C53 C 0.96298(18) 0.92642(10) 0.65437(9) 0.0211(4) Uani 1 1 d . . . . .
H125 H 0.9903 0.9196 0.6181 0.032 Uiso 1 1 calc R U . . .
H126 H 0.9463 0.9728 0.6633 0.032 Uiso 1 1 calc R U . . .
H127 H 0.8909 0.8960 0.6485 0.032 Uiso 1 1 calc R U . . .
C54 C 1.1257(2) 0.82602(11) 0.69133(10) 0.0246(5) Uani 1 1 d . . . . .
H128 H 1.1442 0.8260 0.6531 0.037 Uiso 1 1 calc R U . . .
H129 H 1.0609 0.7908 0.6865 0.037 Uiso 1 1 calc R U . . .
H130 H 1.1957 0.8177 0.7205 0.037 Uiso 1 1 calc R U . . .
C55 C 1.20303(18) 0.97646(11) 0.72547(10) 0.0239(4) Uani 1 1 d . . . . .
H131 H 1.2671 0.9752 0.7607 0.036 Uiso 1 1 calc R U . . .
H132 H 1.1731 1.0201 0.7298 0.036 Uiso 1 1 calc R U . . .
H133 H 1.2330 0.9695 0.6900 0.036 Uiso 1 1 calc R U . . .
C56 C 1.1447(2) 0.78396(11) 0.83973(11) 0.0297(5) Uani 1 1 d . . . . .
H134 H 1.2124 0.7718 0.8679 0.045 Uiso 1 1 calc R U . . .
H135 H 1.1438 0.7632 0.7992 0.045 Uiso 1 1 calc R U . . .
H136 H 1.0714 0.7683 0.8486 0.045 Uiso 1 1 calc R U . . .
C57 C 1.31071(18) 0.90197(13) 0.84185(11) 0.0297(5) Uani 1 1 d . . . . .
H137 H 1.3682 0.8856 0.8724 0.045 Uiso 1 1 calc R U . . .
H138 H 1.3249 0.9508 0.8482 0.045 Uiso 1 1 calc R U . . .
H139 H 1.3192 0.8828 0.8025 0.045 Uiso 1 1 calc R U . . .
C58 C 1.1617(2) 0.91134(13) 0.92542(9) 0.0298(5) Uani 1 1 d . . . . .
H140 H 1.0841 0.9007 0.9323 0.045 Uiso 1 1 calc R U . . .
H141 H 1.1816 0.9600 0.9331 0.045 Uiso 1 1 calc R U . . .
H142 H 1.2215 0.8917 0.9522 0.045 Uiso 1 1 calc R U . . .
C59 C 0.6526(2) 0.91869(14) 0.65428(10) 0.0347(6) Uani 1 1 d . . . . .
H143 H 0.6400 0.8720 0.6586 0.052 Uiso 1 1 calc R U . . .
H144 H 0.7222 0.9253 0.6391 0.052 Uiso 1 1 calc R U . . .
H145 H 0.5830 0.9295 0.6264 0.052 Uiso 1 1 calc R U . . .
C60 C 0.52982(19) 0.96307(14) 0.74462(12) 0.0359(6) Uani 1 1 d . . . . .
H146 H 0.4686 0.9744 0.7125 0.054 Uiso 1 1 calc R U . . .
H147 H 0.5320 0.9924 0.7822 0.054 Uiso 1 1 calc R U . . .
H148 H 0.5120 0.9164 0.7479 0.054 Uiso 1 1 calc R U . . .
C61 C 0.6985(2) 1.06141(13) 0.71320(14) 0.0420(7) Uani 1 1 d . . . . .
H149 H 0.7580 1.0637 0.6907 0.063 Uiso 1 1 calc R U . . .
H150 H 0.7253 1.0931 0.7510 0.063 Uiso 1 1 calc R U . . .
H151 H 0.6237 1.0728 0.6901 0.063 Uiso 1 1 calc R U . . .
C62 C 0.6558(2) 0.93808(15) 0.88160(11) 0.0367(6) Uani 1 1 d . . . . .
H152 H 0.6856 0.8965 0.8910 0.055 Uiso 1 1 calc R U . . .
H153 H 0.5867 0.9277 0.8472 0.055 Uiso 1 1 calc R U . . .
H154 H 0.6332 0.9621 0.9158 0.055 Uiso 1 1 calc R U . . .
C63 C 0.7264(3) 1.07771(14) 0.86588(14) 0.0468(7) Uani 1 1 d . . . . .
H155 H 0.6523 1.0760 0.8353 0.070 Uiso 1 1 calc R U . . .
H156 H 0.7879 1.1074 0.8582 0.070 Uiso 1 1 calc R U . . .
H157 H 0.7148 1.0948 0.9051 0.070 Uiso 1 1 calc R U . . .
C64 C 0.9020(2) 1.00266(15) 0.93062(10) 0.0414(7) Uani 1 1 d . . . . .
H158 H 0.8763 1.0173 0.9666 0.062 Uiso 1 1 calc R U . . .
H159 H 0.9622 1.0365 0.9274 0.062 Uiso 1 1 calc R U . . .
H160 H 0.9353 0.9602 0.9328 0.062 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 1.903(2) . ?
Si1 C1 1.907(2) . ?
Si1 Cl1 2.1067(7) . ?
Si1 Si2 2.4356(7) . ?
Si2 Cl2 2.0652(7) . ?
Si2 Cl3 2.0698(7) . ?
Si2 Si3 2.4086(7) . ?
Si3 Cl4 2.0590(7) . ?
Si3 Cl5 2.0650(7) . ?
Si3 Si4 2.4098(7) . ?
Si4 C20 1.8998(18) . ?
Si4 C17 1.9038(19) . ?
Si4 Cl6 2.1042(7) . ?
Si5 C7 1.868(2) . ?
Si5 C6 1.871(2) . ?
Si5 C5 1.876(2) . ?
Si5 C1 1.936(2) . ?
Si6 C9 1.868(3) . ?
Si6 C10 1.872(2) . ?
Si6 C8 1.890(2) . ?
Si6 C1 1.930(2) . ?
Si7 C11 1.866(3) . ?
Si7 C12 1.870(2) . ?
Si7 C13 1.872(2) . ?
Si7 C4 1.916(2) . ?
Si8 C16 1.863(3) . ?
Si8 C14 1.871(3) . ?
Si8 C15 1.884(3) . ?
Si8 C4 1.922(2) . ?
Si9 C21 1.865(2) . ?
Si9 C23 1.869(2) . ?
Si9 C22 1.880(2) . ?
Si9 C17 1.9223(19) . ?
Si10 C25 1.863(2) . ?
Si10 C24 1.870(2) . ?
Si10 C26 1.877(2) . ?
Si10 C17 1.9313(19) . ?
Si11 C29 1.871(2) . ?
Si11 C28 1.874(2) . ?
Si11 C27 1.876(2) . ?
Si11 C20 1.9332(19) . ?
Si12 C31 1.867(2) . ?
Si12 C32 1.874(2) . ?
Si12 C30 1.881(2) . ?
Si12 C20 1.9158(19) . ?
C1 C2 1.590(3) . ?
C2 C3 1.522(3) . ?
C2 H1 0.9900 . ?
C2 H2 0.9900 . ?
C3 C4 1.578(3) . ?
C3 H3 0.9900 . ?
C3 H4 0.9900 . ?
C5 H5 0.9800 . ?
C5 H6 0.9800 . ?
C5 H7 0.9800 . ?
C6 H8 0.9800 . ?
C6 H9 0.9800 . ?
C6 H10 0.9800 . ?
C7 H11 0.9800 . ?
C7 H12 0.9800 . ?
C7 H13 0.9800 . ?
C8 H14 0.9800 . ?
C8 H15 0.9800 . ?
C8 H16 0.9800 . ?
C9 H17 0.9800 . ?
C9 H18 0.9800 . ?
C9 H19 0.9800 . ?
C10 H20 0.9800 . ?
C10 H21 0.9800 . ?
C10 H22 0.9800 . ?
C11 H23 0.9800 . ?
C11 H24 0.9800 . ?
C11 H25 0.9800 . ?
C12 H26 0.9800 . ?
C12 H27 0.9800 . ?
C12 H28 0.9800 . ?
C13 H29 0.9800 . ?
C13 H30 0.9800 . ?
C13 H31 0.9800 . ?
C14 H32 0.9800 . ?
C14 H33 0.9800 . ?
C14 H34 0.9800 . ?
C15 H35 0.9800 . ?
C15 H36 0.9800 . ?
C15 H37 0.9800 . ?
C16 H38 0.9800 . ?
C16 H39 0.9800 . ?
C16 H40 0.9800 . ?
C17 C18 1.582(2) . ?
C18 C19 1.524(3) . ?
C18 H41 0.9900 . ?
C18 H42 0.9900 . ?
C19 C20 1.580(2) . ?
C19 H43 0.9900 . ?
C19 H44 0.9900 . ?
C21 H45 0.9800 . ?
C21 H46 0.9800 . ?
C21 H47 0.9800 . ?
C22 H48 0.9800 . ?
C22 H49 0.9800 . ?
C22 H50 0.9800 . ?
C23 H51 0.9800 . ?
C23 H52 0.9800 . ?
C23 H53 0.9800 . ?
C24 H54 0.9800 . ?
C24 H55 0.9800 . ?
C24 H56 0.9800 . ?
C25 H57 0.9800 . ?
C25 H58 0.9800 . ?
C25 H59 0.9800 . ?
C26 H60 0.9800 . ?
C26 H61 0.9800 . ?
C26 H62 0.9800 . ?
C27 H63 0.9800 . ?
C27 H64 0.9800 . ?
C27 H65 0.9800 . ?
C28 H66 0.9800 . ?
C28 H67 0.9800 . ?
C28 H68 0.9800 . ?
C29 H69 0.9800 . ?
C29 H70 0.9800 . ?
C29 H71 0.9800 . ?
C30 H72 0.9800 . ?
C30 H73 0.9800 . ?
C30 H74 0.9800 . ?
C31 H75 0.9800 . ?
C31 H76 0.9800 . ?
C31 H77 0.9800 . ?
C32 H78 0.9800 . ?
C32 H79 0.9800 . ?
C32 H80 0.9800 . ?
Si13 C36 1.8997(19) . ?
Si13 C33 1.9050(19) . ?
Si13 Cl7 2.1162(7) . ?
Si13 Si14 2.4222(7) . ?
Si14 Cl9 2.0543(8) . ?
Si14 Cl8 2.0726(8) . ?
Si14 Si15 2.3797(8) . ?
Si15 Cl11 2.0450(8) . ?
Si15 Cl10 2.0635(7) . ?
Si15 Si16 2.4103(7) . ?
Si16 C52 1.8986(19) . ?
Si16 C49 1.8994(19) . ?
Si16 Cl12 2.1078(7) . ?
Si17 C37 1.862(2) . ?
Si17 C38 1.869(2) . ?
Si17 C39 1.872(2) . ?
Si17 C33 1.9287(19) . ?
Si18 C40 1.867(2) . ?
Si18 C42 1.869(2) . ?
Si18 C41 1.877(2) . ?
Si18 C33 1.9344(19) . ?
Si19 C44 1.862(2) . ?
Si19 C43 1.877(2) . ?
Si19 C45 1.876(2) . ?
Si19 C36 1.9170(19) . ?
Si20 C46 1.863(2) . ?
Si20 C48 1.871(2) . ?
Si20 C47 1.878(2) . ?
Si20 C36 1.9300(19) . ?
Si21 C54 1.865(2) . ?
Si21 C53 1.873(2) . ?
Si21 C55 1.875(2) . ?
Si21 C49 1.9193(19) . ?
Si22 C56 1.859(2) . ?
Si22 C58 1.873(2) . ?
Si22 C57 1.877(2) . ?
Si22 C49 1.9272(19) . ?
Si23 C59 1.865(3) . ?
Si23 C60 1.866(2) . ?
Si23 C61 1.877(2) . ?
Si23 C52 1.9248(19) . ?
Si24 C62 1.858(3) . ?
Si24 C64 1.863(3) . ?
Si24 C63 1.886(3) . ?
Si24 C52 1.932(2) . ?
C33 C34 1.584(2) . ?
C34 C35 1.529(3) . ?
C34 H81 0.9900 . ?
C34 H82 0.9900 . ?
C35 C36 1.574(2) . ?
C35 H83 0.9900 . ?
C35 H84 0.9900 . ?
C37 H85 0.9800 . ?
C37 H86 0.9800 . ?
C37 H87 0.9800 . ?
C38 H88 0.9800 . ?
C38 H89 0.9800 . ?
C38 H90 0.9800 . ?
C39 H91 0.9800 . ?
C39 H92 0.9800 . ?
C39 H93 0.9800 . ?
C40 H94 0.9800 . ?
C40 H95 0.9800 . ?
C40 H96 0.9800 . ?
C41 H97 0.9800 . ?
C41 H98 0.9800 . ?
C41 H99 0.9800 . ?
C42 H100 0.9800 . ?
C42 H101 0.9800 . ?
C42 H102 0.9800 . ?
C43 H103 0.9800 . ?
C43 H104 0.9800 . ?
C43 H105 0.9800 . ?
C44 H106 0.9800 . ?
C44 H107 0.9800 . ?
C44 H108 0.9800 . ?
C45 H109 0.9800 . ?
C45 H110 0.9800 . ?
C45 H111 0.9800 . ?
C46 H112 0.9800 . ?
C46 H113 0.9800 . ?
C46 H114 0.9800 . ?
C47 H115 0.9800 . ?
C47 H116 0.9800 . ?
C47 H117 0.9800 . ?
C48 H118 0.9800 . ?
C48 H119 0.9800 . ?
C48 H120 0.9800 . ?
C49 C50 1.574(3) . ?
C50 C51 1.532(3) . ?
C50 H121 0.9900 . ?
C50 H122 0.9900 . ?
C51 C52 1.587(3) . ?
C51 H123 0.9900 . ?
C51 H124 0.9900 . ?
C53 H125 0.9800 . ?
C53 H126 0.9800 . ?
C53 H127 0.9800 . ?
C54 H128 0.9800 . ?
C54 H129 0.9800 . ?
C54 H130 0.9800 . ?
C55 H131 0.9800 . ?
C55 H132 0.9800 . ?
C55 H133 0.9800 . ?
C56 H134 0.9800 . ?
C56 H135 0.9800 . ?
C56 H136 0.9800 . ?
C57 H137 0.9800 . ?
C57 H138 0.9800 . ?
C57 H139 0.9800 . ?
C58 H140 0.9800 . ?
C58 H141 0.9800 . ?
C58 H142 0.9800 . ?
C59 H143 0.9800 . ?
C59 H144 0.9800 . ?
C59 H145 0.9800 . ?
C60 H146 0.9800 . ?
C60 H147 0.9800 . ?
C60 H148 0.9800 . ?
C61 H149 0.9800 . ?
C61 H150 0.9800 . ?
C61 H151 0.9800 . ?
C62 H152 0.9800 . ?
C62 H153 0.9800 . ?
C62 H154 0.9800 . ?
C63 H155 0.9800 . ?
C63 H156 0.9800 . ?
C63 H157 0.9800 . ?
C64 H158 0.9800 . ?
C64 H159 0.9800 . ?
C64 H160 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C4 Si1 C1 100.72(8) . . ?
C4 Si1 Cl1 111.53(7) . . ?
C1 Si1 Cl1 109.87(6) . . ?
C4 Si1 Si2 117.23(6) . . ?
C1 Si1 Si2 127.92(6) . . ?
Cl1 Si1 Si2 88.82(3) . . ?
Cl2 Si2 Cl3 101.59(3) . . ?
Cl2 Si2 Si3 111.09(3) . . ?
Cl3 Si2 Si3 103.22(3) . . ?
Cl2 Si2 Si1 119.72(3) . . ?
Cl3 Si2 Si1 103.51(3) . . ?
Si3 Si2 Si1 114.91(3) . . ?
Cl4 Si3 Cl5 104.89(3) . . ?
Cl4 Si3 Si2 102.79(3) . . ?
Cl5 Si3 Si2 102.55(3) . . ?
Cl4 Si3 Si4 102.57(3) . . ?
Cl5 Si3 Si4 117.84(3) . . ?
Si2 Si3 Si4 123.79(3) . . ?
C20 Si4 C17 100.72(8) . . ?
C20 Si4 Cl6 111.58(6) . . ?
C17 Si4 Cl6 110.39(6) . . ?
C20 Si4 Si3 123.62(6) . . ?
C17 Si4 Si3 120.44(6) . . ?
Cl6 Si4 Si3 89.58(2) . . ?
C7 Si5 C6 102.87(11) . . ?
C7 Si5 C5 106.43(11) . . ?
C6 Si5 C5 106.54(11) . . ?
C7 Si5 C1 114.49(9) . . ?
C6 Si5 C1 116.33(10) . . ?
C5 Si5 C1 109.42(10) . . ?
C9 Si6 C10 105.36(12) . . ?
C9 Si6 C8 102.41(12) . . ?
C10 Si6 C8 108.51(11) . . ?
C9 Si6 C1 115.19(10) . . ?
C10 Si6 C1 116.06(9) . . ?
C8 Si6 C1 108.31(10) . . ?
C11 Si7 C12 106.73(12) . . ?
C11 Si7 C13 101.90(12) . . ?
C12 Si7 C13 108.84(11) . . ?
C11 Si7 C4 115.06(10) . . ?
C12 Si7 C4 111.71(11) . . ?
C13 Si7 C4 111.99(11) . . ?
C16 Si8 C14 105.57(14) . . ?
C16 Si8 C15 106.11(14) . . ?
C14 Si8 C15 104.49(15) . . ?
C16 Si8 C4 116.64(10) . . ?
C14 Si8 C4 112.39(12) . . ?
C15 Si8 C4 110.74(12) . . ?
C21 Si9 C23 106.64(10) . . ?
C21 Si9 C22 108.62(11) . . ?
C23 Si9 C22 101.84(10) . . ?
C21 Si9 C17 114.71(9) . . ?
C23 Si9 C17 113.50(9) . . ?
C22 Si9 C17 110.65(9) . . ?
C25 Si10 C24 104.07(10) . . ?
C25 Si10 C26 104.33(10) . . ?
C24 Si10 C26 107.22(10) . . ?
C25 Si10 C17 116.10(9) . . ?
C24 Si10 C17 114.69(9) . . ?
C26 Si10 C17 109.58(9) . . ?
C29 Si11 C28 110.04(10) . . ?
C29 Si11 C27 105.57(10) . . ?
C28 Si11 C27 101.25(10) . . ?
C29 Si11 C20 110.87(9) . . ?
C28 Si11 C20 109.06(9) . . ?
C27 Si11 C20 119.49(9) . . ?
C31 Si12 C32 108.52(10) . . ?
C31 Si12 C30 102.34(10) . . ?
C32 Si12 C30 108.40(10) . . ?
C31 Si12 C20 111.95(9) . . ?
C32 Si12 C20 111.31(9) . . ?
C30 Si12 C20 113.83(9) . . ?
C2 C1 Si1 99.59(12) . . ?
C2 C1 Si6 104.85(12) . . ?
Si1 C1 Si6 115.77(10) . . ?
C2 C1 Si5 108.30(13) . . ?
Si1 C1 Si5 119.35(10) . . ?
Si6 C1 Si5 107.48(9) . . ?
C3 C2 C1 110.97(16) . . ?
C3 C2 H1 109.4 . . ?
C1 C2 H1 109.4 . . ?
C3 C2 H2 109.4 . . ?
C1 C2 H2 109.4 . . ?
H1 C2 H2 108.0 . . ?
C2 C3 C4 110.73(16) . . ?
C2 C3 H3 109.5 . . ?
C4 C3 H3 109.5 . . ?
C2 C3 H4 109.5 . . ?
C4 C3 H4 109.5 . . ?
H3 C3 H4 108.1 . . ?
C3 C4 Si1 98.48(12) . . ?
C3 C4 Si7 107.94(13) . . ?
Si1 C4 Si7 114.21(10) . . ?
C3 C4 Si8 105.96(13) . . ?
Si1 C4 Si8 118.51(11) . . ?
Si7 C4 Si8 110.21(10) . . ?
Si5 C5 H5 109.5 . . ?
Si5 C5 H6 109.5 . . ?
H5 C5 H6 109.5 . . ?
Si5 C5 H7 109.5 . . ?
H5 C5 H7 109.5 . . ?
H6 C5 H7 109.5 . . ?
Si5 C6 H8 109.5 . . ?
Si5 C6 H9 109.5 . . ?
H8 C6 H9 109.5 . . ?
Si5 C6 H10 109.5 . . ?
H8 C6 H10 109.5 . . ?
H9 C6 H10 109.5 . . ?
Si5 C7 H11 109.5 . . ?
Si5 C7 H12 109.5 . . ?
H11 C7 H12 109.5 . . ?
Si5 C7 H13 109.5 . . ?
H11 C7 H13 109.5 . . ?
H12 C7 H13 109.5 . . ?
Si6 C8 H14 109.5 . . ?
Si6 C8 H15 109.5 . . ?
H14 C8 H15 109.5 . . ?
Si6 C8 H16 109.5 . . ?
H14 C8 H16 109.5 . . ?
H15 C8 H16 109.5 . . ?
Si6 C9 H17 109.5 . . ?
Si6 C9 H18 109.5 . . ?
H17 C9 H18 109.5 . . ?
Si6 C9 H19 109.5 . . ?
H17 C9 H19 109.5 . . ?
H18 C9 H19 109.5 . . ?
Si6 C10 H20 109.5 . . ?
Si6 C10 H21 109.5 . . ?
H20 C10 H21 109.5 . . ?
Si6 C10 H22 109.5 . . ?
H20 C10 H22 109.5 . . ?
H21 C10 H22 109.5 . . ?
Si7 C11 H23 109.5 . . ?
Si7 C11 H24 109.5 . . ?
H23 C11 H24 109.5 . . ?
Si7 C11 H25 109.5 . . ?
H23 C11 H25 109.5 . . ?
H24 C11 H25 109.5 . . ?
Si7 C12 H26 109.5 . . ?
Si7 C12 H27 109.5 . . ?
H26 C12 H27 109.5 . . ?
Si7 C12 H28 109.5 . . ?
H26 C12 H28 109.5 . . ?
H27 C12 H28 109.5 . . ?
Si7 C13 H29 109.5 . . ?
Si7 C13 H30 109.5 . . ?
H29 C13 H30 109.5 . . ?
Si7 C13 H31 109.5 . . ?
H29 C13 H31 109.5 . . ?
H30 C13 H31 109.5 . . ?
Si8 C14 H32 109.5 . . ?
Si8 C14 H33 109.5 . . ?
H32 C14 H33 109.5 . . ?
Si8 C14 H34 109.5 . . ?
H32 C14 H34 109.5 . . ?
H33 C14 H34 109.5 . . ?
Si8 C15 H35 109.5 . . ?
Si8 C15 H36 109.5 . . ?
H35 C15 H36 109.5 . . ?
Si8 C15 H37 109.5 . . ?
H35 C15 H37 109.5 . . ?
H36 C15 H37 109.5 . . ?
Si8 C16 H38 109.5 . . ?
Si8 C16 H39 109.5 . . ?
H38 C16 H39 109.5 . . ?
Si8 C16 H40 109.5 . . ?
H38 C16 H40 109.5 . . ?
H39 C16 H40 109.5 . . ?
C18 C17 Si4 97.96(11) . . ?
C18 C17 Si9 106.84(12) . . ?
Si4 C17 Si9 117.20(10) . . ?
C18 C17 Si10 107.46(12) . . ?
Si4 C17 Si10 118.56(10) . . ?
Si9 C17 Si10 107.39(9) . . ?
C19 C18 C17 110.12(15) . . ?
C19 C18 H41 109.6 . . ?
C17 C18 H41 109.6 . . ?
C19 C18 H42 109.6 . . ?
C17 C18 H42 109.6 . . ?
H41 C18 H42 108.1 . . ?
C18 C19 C20 109.23(15) . . ?
C18 C19 H43 109.8 . . ?
C20 C19 H43 109.8 . . ?
C18 C19 H44 109.8 . . ?
C20 C19 H44 109.8 . . ?
H43 C19 H44 108.3 . . ?
C19 C20 Si4 99.02(11) . . ?
C19 C20 Si12 110.01(12) . . ?
Si4 C20 Si12 116.17(9) . . ?
C19 C20 Si11 108.86(12) . . ?
Si4 C20 Si11 115.76(9) . . ?
Si12 C20 Si11 106.63(9) . . ?
Si9 C21 H45 109.5 . . ?
Si9 C21 H46 109.5 . . ?
H45 C21 H46 109.5 . . ?
Si9 C21 H47 109.5 . . ?
H45 C21 H47 109.5 . . ?
H46 C21 H47 109.5 . . ?
Si9 C22 H48 109.5 . . ?
Si9 C22 H49 109.5 . . ?
H48 C22 H49 109.5 . . ?
Si9 C22 H50 109.5 . . ?
H48 C22 H50 109.5 . . ?
H49 C22 H50 109.5 . . ?
Si9 C23 H51 109.5 . . ?
Si9 C23 H52 109.5 . . ?
H51 C23 H52 109.5 . . ?
Si9 C23 H53 109.5 . . ?
H51 C23 H53 109.5 . . ?
H52 C23 H53 109.5 . . ?
Si10 C24 H54 109.5 . . ?
Si10 C24 H55 109.5 . . ?
H54 C24 H55 109.5 . . ?
Si10 C24 H56 109.5 . . ?
H54 C24 H56 109.5 . . ?
H55 C24 H56 109.5 . . ?
Si10 C25 H57 109.5 . . ?
Si10 C25 H58 109.5 . . ?
H57 C25 H58 109.5 . . ?
Si10 C25 H59 109.5 . . ?
H57 C25 H59 109.5 . . ?
H58 C25 H59 109.5 . . ?
Si10 C26 H60 109.5 . . ?
Si10 C26 H61 109.5 . . ?
H60 C26 H61 109.5 . . ?
Si10 C26 H62 109.5 . . ?
H60 C26 H62 109.5 . . ?
H61 C26 H62 109.5 . . ?
Si11 C27 H63 109.5 . . ?
Si11 C27 H64 109.5 . . ?
H63 C27 H64 109.5 . . ?
Si11 C27 H65 109.5 . . ?
H63 C27 H65 109.5 . . ?
H64 C27 H65 109.5 . . ?
Si11 C28 H66 109.5 . . ?
Si11 C28 H67 109.5 . . ?
H66 C28 H67 109.5 . . ?
Si11 C28 H68 109.5 . . ?
H66 C28 H68 109.5 . . ?
H67 C28 H68 109.5 . . ?
Si11 C29 H69 109.5 . . ?
Si11 C29 H70 109.5 . . ?
H69 C29 H70 109.5 . . ?
Si11 C29 H71 109.5 . . ?
H69 C29 H71 109.5 . . ?
H70 C29 H71 109.5 . . ?
Si12 C30 H72 109.5 . . ?
Si12 C30 H73 109.5 . . ?
H72 C30 H73 109.5 . . ?
Si12 C30 H74 109.5 . . ?
H72 C30 H74 109.5 . . ?
H73 C30 H74 109.5 . . ?
Si12 C31 H75 109.5 . . ?
Si12 C31 H76 109.5 . . ?
H75 C31 H76 109.5 . . ?
Si12 C31 H77 109.5 . . ?
H75 C31 H77 109.5 . . ?
H76 C31 H77 109.5 . . ?
Si12 C32 H78 109.5 . . ?
Si12 C32 H79 109.5 . . ?
H78 C32 H79 109.5 . . ?
Si12 C32 H80 109.5 . . ?
H78 C32 H80 109.5 . . ?
H79 C32 H80 109.5 . . ?
C36 Si13 C33 100.94(8) . . ?
C36 Si13 Cl7 110.85(6) . . ?
C33 Si13 Cl7 109.84(6) . . ?
C36 Si13 Si14 117.32(6) . . ?
C33 Si13 Si14 126.38(6) . . ?
Cl7 Si13 Si14 90.88(3) . . ?
Cl9 Si14 Cl8 101.39(3) . . ?
Cl9 Si14 Si15 104.71(3) . . ?
Cl8 Si14 Si15 105.61(3) . . ?
Cl9 Si14 Si13 106.30(3) . . ?
Cl8 Si14 Si13 118.71(3) . . ?
Si15 Si14 Si13 117.99(3) . . ?
Cl11 Si15 Cl10 102.16(3) . . ?
Cl11 Si15 Si14 104.88(3) . . ?
Cl10 Si15 Si14 105.04(3) . . ?
Cl11 Si15 Si16 105.12(3) . . ?
Cl10 Si15 Si16 118.27(3) . . ?
Si14 Si15 Si16 119.25(3) . . ?
C52 Si16 C49 101.21(8) . . ?
C52 Si16 Cl12 110.29(6) . . ?
C49 Si16 Cl12 110.81(6) . . ?
C52 Si16 Si15 126.31(6) . . ?
C49 Si16 Si15 117.85(6) . . ?
Cl12 Si16 Si15 89.58(3) . . ?
C37 Si17 C38 104.07(11) . . ?
C37 Si17 C39 104.54(11) . . ?
C38 Si17 C39 106.67(12) . . ?
C37 Si17 C33 115.23(9) . . ?
C38 Si17 C33 115.50(9) . . ?
C39 Si17 C33 109.93(9) . . ?
C40 Si18 C42 106.57(10) . . ?
C40 Si18 C41 107.65(11) . . ?
C42 Si18 C41 102.42(10) . . ?
C40 Si18 C33 116.32(9) . . ?
C42 Si18 C33 113.97(9) . . ?
C41 Si18 C33 108.85(9) . . ?
C44 Si19 C43 107.11(10) . . ?
C44 Si19 C45 109.34(10) . . ?
C43 Si19 C45 102.08(10) . . ?
C44 Si19 C36 110.80(9) . . ?
C43 Si19 C36 116.20(9) . . ?
C45 Si19 C36 110.84(9) . . ?
C46 Si20 C48 106.21(10) . . ?
C46 Si20 C47 104.80(11) . . ?
C48 Si20 C47 104.10(10) . . ?
C46 Si20 C36 116.32(9) . . ?
C48 Si20 C36 111.39(9) . . ?
C47 Si20 C36 113.02(9) . . ?
C54 Si21 C53 106.34(10) . . ?
C54 Si21 C55 109.57(10) . . ?
C53 Si21 C55 102.30(10) . . ?
C54 Si21 C49 111.42(9) . . ?
C53 Si21 C49 115.76(9) . . ?
C55 Si21 C49 110.94(9) . . ?
C56 Si22 C58 106.24(11) . . ?
C56 Si22 C57 105.59(11) . . ?
C58 Si22 C57 103.22(11) . . ?
C56 Si22 C49 116.39(10) . . ?
C58 Si22 C49 111.67(9) . . ?
C57 Si22 C49 112.65(9) . . ?
C59 Si23 C60 103.10(12) . . ?
C59 Si23 C61 104.87(13) . . ?
C60 Si23 C61 107.87(12) . . ?
C59 Si23 C52 115.98(10) . . ?
C60 Si23 C52 115.24(10) . . ?
C61 Si23 C52 109.02(10) . . ?
C62 Si24 C64 105.39(13) . . ?
C62 Si24 C63 107.50(13) . . ?
C64 Si24 C63 103.07(13) . . ?
C62 Si24 C52 116.36(10) . . ?
C64 Si24 C52 114.40(10) . . ?
C63 Si24 C52 109.12(12) . . ?
C34 C33 Si13 99.48(11) . . ?
C34 C33 Si17 108.43(12) . . ?
Si13 C33 Si17 119.30(10) . . ?
C34 C33 Si18 105.47(12) . . ?
Si13 C33 Si18 115.70(9) . . ?
Si17 C33 Si18 107.12(9) . . ?
C35 C34 C33 111.01(15) . . ?
C35 C34 H81 109.4 . . ?
C33 C34 H81 109.4 . . ?
C35 C34 H82 109.4 . . ?
C33 C34 H82 109.4 . . ?
H81 C34 H82 108.0 . . ?
C34 C35 C36 110.72(15) . . ?
C34 C35 H83 109.5 . . ?
C36 C35 H83 109.5 . . ?
C34 C35 H84 109.5 . . ?
C36 C35 H84 109.5 . . ?
H83 C35 H84 108.1 . . ?
C35 C36 Si13 98.56(11) . . ?
C35 C36 Si19 107.68(12) . . ?
Si13 C36 Si19 115.94(10) . . ?
C35 C36 Si20 108.64(12) . . ?
Si13 C36 Si20 116.23(9) . . ?
Si19 C36 Si20 108.81(9) . . ?
Si17 C37 H85 109.5 . . ?
Si17 C37 H86 109.5 . . ?
H85 C37 H86 109.5 . . ?
Si17 C37 H87 109.5 . . ?
H85 C37 H87 109.5 . . ?
H86 C37 H87 109.5 . . ?
Si17 C38 H88 109.5 . . ?
Si17 C38 H89 109.5 . . ?
H88 C38 H89 109.5 . . ?
Si17 C38 H90 109.5 . . ?
H88 C38 H90 109.5 . . ?
H89 C38 H90 109.5 . . ?
Si17 C39 H91 109.5 . . ?
Si17 C39 H92 109.5 . . ?
H91 C39 H92 109.5 . . ?
Si17 C39 H93 109.5 . . ?
H91 C39 H93 109.5 . . ?
H92 C39 H93 109.5 . . ?
Si18 C40 H94 109.5 . . ?
Si18 C40 H95 109.5 . . ?
H94 C40 H95 109.5 . . ?
Si18 C40 H96 109.5 . . ?
H94 C40 H96 109.5 . . ?
H95 C40 H96 109.5 . . ?
Si18 C41 H97 109.5 . . ?
Si18 C41 H98 109.5 . . ?
H97 C41 H98 109.5 . . ?
Si18 C41 H99 109.5 . . ?
H97 C41 H99 109.5 . . ?
H98 C41 H99 109.5 . . ?
Si18 C42 H100 109.5 . . ?
Si18 C42 H101 109.5 . . ?
H100 C42 H101 109.5 . . ?
Si18 C42 H102 109.5 . . ?
H100 C42 H102 109.5 . . ?
H101 C42 H102 109.5 . . ?
Si19 C43 H103 109.5 . . ?
Si19 C43 H104 109.5 . . ?
H103 C43 H104 109.5 . . ?
Si19 C43 H105 109.5 . . ?
H103 C43 H105 109.5 . . ?
H104 C43 H105 109.5 . . ?
Si19 C44 H106 109.5 . . ?
Si19 C44 H107 109.5 . . ?
H106 C44 H107 109.5 . . ?
Si19 C44 H108 109.5 . . ?
H106 C44 H108 109.5 . . ?
H107 C44 H108 109.5 . . ?
Si19 C45 H109 109.5 . . ?
Si19 C45 H110 109.5 . . ?
H109 C45 H110 109.5 . . ?
Si19 C45 H111 109.5 . . ?
H109 C45 H111 109.5 . . ?
H110 C45 H111 109.5 . . ?
Si20 C46 H112 109.5 . . ?
Si20 C46 H113 109.5 . . ?
H112 C46 H113 109.5 . . ?
Si20 C46 H114 109.5 . . ?
H112 C46 H114 109.5 . . ?
H113 C46 H114 109.5 . . ?
Si20 C47 H115 109.5 . . ?
Si20 C47 H116 109.5 . . ?
H115 C47 H116 109.5 . . ?
Si20 C47 H117 109.5 . . ?
H115 C47 H117 109.5 . . ?
H116 C47 H117 109.5 . . ?
Si20 C48 H118 109.5 . . ?
Si20 C48 H119 109.5 . . ?
H118 C48 H119 109.5 . . ?
Si20 C48 H120 109.5 . . ?
H118 C48 H120 109.5 . . ?
H119 C48 H120 109.5 . . ?
C50 C49 Si16 98.37(12) . . ?
C50 C49 Si21 107.08(13) . . ?
Si16 C49 Si21 115.35(9) . . ?
C50 C49 Si22 107.85(12) . . ?
Si16 C49 Si22 117.04(10) . . ?
Si21 C49 Si22 109.81(9) . . ?
C51 C50 C49 110.85(15) . . ?
C51 C50 H121 109.5 . . ?
C49 C50 H121 109.5 . . ?
C51 C50 H122 109.5 . . ?
C49 C50 H122 109.5 . . ?
H121 C50 H122 108.1 . . ?
C50 C51 C52 110.80(16) . . ?
C50 C51 H123 109.5 . . ?
C52 C51 H123 109.5 . . ?
C50 C51 H124 109.5 . . ?
C52 C51 H124 109.5 . . ?
H123 C51 H124 108.1 . . ?
C51 C52 Si16 99.56(11) . . ?
C51 C52 Si23 107.73(13) . . ?
Si16 C52 Si23 120.89(10) . . ?
C51 C52 Si24 105.61(12) . . ?
Si16 C52 Si24 115.07(10) . . ?
Si23 C52 Si24 106.53(9) . . ?
Si21 C53 H125 109.5 . . ?
Si21 C53 H126 109.5 . . ?
H125 C53 H126 109.5 . . ?
Si21 C53 H127 109.5 . . ?
H125 C53 H127 109.5 . . ?
H126 C53 H127 109.5 . . ?
Si21 C54 H128 109.5 . . ?
Si21 C54 H129 109.5 . . ?
H128 C54 H129 109.5 . . ?
Si21 C54 H130 109.5 . . ?
H128 C54 H130 109.5 . . ?
H129 C54 H130 109.5 . . ?
Si21 C55 H131 109.5 . . ?
Si21 C55 H132 109.5 . . ?
H131 C55 H132 109.5 . . ?
Si21 C55 H133 109.5 . . ?
H131 C55 H133 109.5 . . ?
H132 C55 H133 109.5 . . ?
Si22 C56 H134 109.5 . . ?
Si22 C56 H135 109.5 . . ?
H134 C56 H135 109.5 . . ?
Si22 C56 H136 109.5 . . ?
H134 C56 H136 109.5 . . ?
H135 C56 H136 109.5 . . ?
Si22 C57 H137 109.5 . . ?
Si22 C57 H138 109.5 . . ?
H137 C57 H138 109.5 . . ?
Si22 C57 H139 109.5 . . ?
H137 C57 H139 109.5 . . ?
H138 C57 H139 109.5 . . ?
Si22 C58 H140 109.5 . . ?
Si22 C58 H141 109.5 . . ?
H140 C58 H141 109.5 . . ?
Si22 C58 H142 109.5 . . ?
H140 C58 H142 109.5 . . ?
H141 C58 H142 109.5 . . ?
Si23 C59 H143 109.5 . . ?
Si23 C59 H144 109.5 . . ?
H143 C59 H144 109.5 . . ?
Si23 C59 H145 109.5 . . ?
H143 C59 H145 109.5 . . ?
H144 C59 H145 109.5 . . ?
Si23 C60 H146 109.5 . . ?
Si23 C60 H147 109.5 . . ?
H146 C60 H147 109.5 . . ?
Si23 C60 H148 109.5 . . ?
H146 C60 H148 109.5 . . ?
H147 C60 H148 109.5 . . ?
Si23 C61 H149 109.5 . . ?
Si23 C61 H150 109.5 . . ?
H149 C61 H150 109.5 . . ?
Si23 C61 H151 109.5 . . ?
H149 C61 H151 109.5 . . ?
H150 C61 H151 109.5 . . ?
Si24 C62 H152 109.5 . . ?
Si24 C62 H153 109.5 . . ?
H152 C62 H153 109.5 . . ?
Si24 C62 H154 109.5 . . ?
H152 C62 H154 109.5 . . ?
H153 C62 H154 109.5 . . ?
Si24 C63 H155 109.5 . . ?
Si24 C63 H156 109.5 . . ?
H155 C63 H156 109.5 . . ?
Si24 C63 H157 109.5 . . ?
H155 C63 H157 109.5 . . ?
H156 C63 H157 109.5 . . ?
Si24 C64 H158 109.5 . . ?
Si24 C64 H159 109.5 . . ?
H158 C64 H159 109.5 . . ?
Si24 C64 H160 109.5 . . ?
H158 C64 H160 109.5 . . ?
H159 C64 H160 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Si1 C1 C2 C3 -31.19(18) . . . . ?
Si6 C1 C2 C3 88.88(16) . . . . ?
Si5 C1 C2 C3 -156.60(14) . . . . ?
C1 C2 C3 C4 50.4(2) . . . . ?
C2 C3 C4 Si1 -39.39(18) . . . . ?
C2 C3 C4 Si7 79.57(17) . . . . ?
C2 C3 C4 Si8 -162.38(14) . . . . ?
Si4 C17 C18 C19 39.34(16) . . . . ?
Si9 C17 C18 C19 160.98(12) . . . . ?
Si10 C17 C18 C19 -84.03(15) . . . . ?
C17 C18 C19 C20 -54.86(19) . . . . ?
C18 C19 C20 Si4 37.37(16) . . . . ?
C18 C19 C20 Si12 159.59(12) . . . . ?
C18 C19 C20 Si11 -83.91(15) . . . . ?
C17 Si4 C20 C19 -12.07(13) . . . . ?
Cl6 Si4 C20 C19 -129.21(10) . . . . ?
Si3 Si4 C20 C19 126.11(10) . . . . ?
C17 Si4 C20 Si12 -129.71(10) . . . . ?
Cl6 Si4 C20 Si12 113.15(8) . . . . ?
Si3 Si4 C20 Si12 8.46(13) . . . . ?
C17 Si4 C20 Si11 104.04(10) . . . . ?
Cl6 Si4 C20 Si11 -13.10(11) . . . . ?
Si3 Si4 C20 Si11 -117.78(8) . . . . ?
Si13 C33 C34 C35 -31.47(16) . . . . ?
Si17 C33 C34 C35 -156.83(12) . . . . ?
Si18 C33 C34 C35 88.70(15) . . . . ?
C33 C34 C35 C36 50.22(19) . . . . ?
C34 C35 C36 Si13 -38.74(16) . . . . ?
C34 C35 C36 Si19 82.07(15) . . . . ?
C34 C35 C36 Si20 -160.24(12) . . . . ?
C33 Si13 C36 C35 17.12(13) . . . . ?
Cl7 Si13 C36 C35 -99.21(11) . . . . ?
Si14 Si13 C36 C35 158.37(9) . . . . ?
C33 Si13 C36 Si19 -97.38(11) . . . . ?
Cl7 Si13 C36 Si19 146.29(8) . . . . ?
Si14 Si13 C36 Si19 43.87(11) . . . . ?
C33 Si13 C36 Si20 132.88(10) . . . . ?
Cl7 Si13 C36 Si20 16.55(11) . . . . ?
Si14 Si13 C36 Si20 -85.88(10) . . . . ?
C52 Si16 C49 C50 17.17(13) . . . . ?
Cl12 Si16 C49 C50 -99.80(11) . . . . ?
Si15 Si16 C49 C50 159.13(9) . . . . ?
C52 Si16 C49 Si21 -96.29(10) . . . . ?
Cl12 Si16 C49 Si21 146.74(7) . . . . ?
Si15 Si16 C49 Si21 45.67(11) . . . . ?
C52 Si16 C49 Si22 132.20(10) . . . . ?
Cl12 Si16 C49 Si22 15.23(11) . . . . ?
Si15 Si16 C49 Si22 -85.84(10) . . . . ?
Si16 C49 C50 C51 -38.75(17) . . . . ?
Si21 C49 C50 C51 81.11(17) . . . . ?
Si22 C49 C50 C51 -160.76(14) . . . . ?
C49 C50 C51 C52 50.1(2) . . . . ?
C50 C51 C52 Si16 -31.28(17) . . . . ?
C50 C51 C52 Si23 -158.18(13) . . . . ?
C50 C51 C52 Si24 88.27(16) . . . . ?
C49 Si16 C52 C51 6.93(13) . . . . ?
Cl12 Si16 C52 C51 124.28(11) . . . . ?
Si15 Si16 C52 C51 -130.53(10) . . . . ?
C49 Si16 C52 Si23 124.36(11) . . . . ?
Cl12 Si16 C52 Si23 -118.29(10) . . . . ?
Si15 Si16 C52 Si23 -13.10(15) . . . . ?
C49 Si16 C52 Si24 -105.41(10) . . . . ?
Cl12 Si16 C52 Si24 11.94(11) . . . . ?
Si15 Si16 C52 Si24 117.13(8) . . . . ?

_refine_diff_density_max         0.992
_refine_diff_density_min         -0.919
_refine_diff_density_rms         0.070

_shelxl_version_number           2014-3


_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: hexane'
_chemical_properties_physical    Moisture-sensitive
