# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2020

####################################################################### 
# 
# 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_tn08a_a
_database_code_depnum_ccdc_archive 'CCDC 2032837'
loop_
_audit_author_name
_audit_author_address
'Takumi Nukazawa'
;Tohoku University
Japan
;
_audit_update_record             
;
2020-09-19 deposited with the CCDC.	2020-10-27 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        1,3-dichlorobicyclo[1.1.0]tetrasilane
_chemical_name_common            ?
_chemical_melting_point          434
_chemical_formula_moiety         'C32 H80 Cl2 Si12'
_chemical_formula_sum            'C32 H80 Cl2 Si12'
_chemical_formula_weight         872.94

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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/n'
_space_group_name_Hall           '-P 2yn'

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

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

_cell_length_a                   11.4596(9)
_cell_length_b                   17.1621(13)
_cell_length_c                   13.4942(10)
_cell_angle_alpha                90
_cell_angle_beta                 112.624(2)
_cell_angle_gamma                90
_cell_volume                     2449.7(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    4070
_cell_measurement_theta_min      2.26
_cell_measurement_theta_max      25.31

_exptl_crystal_description       block
_exptl_crystal_colour            orange
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.183
_exptl_crystal_F_000             948
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.020
_exptl_crystal_size_mid          0.010
_exptl_crystal_size_min          0.010
_exptl_absorpt_coefficient_mu    0.449
_shelx_estimated_absorpt_T_min   0.991
_shelx_estimated_absorpt_T_max   0.996
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.5998
_exptl_absorpt_correction_T_max  0.7452
_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            29568
_diffrn_reflns_av_unetI/netI     0.0580
_diffrn_reflns_av_R_equivalents  0.0903
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         1.989
_diffrn_reflns_theta_max         25.536
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             4540
_reflns_number_gt                3540
_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)+(0.0723P)²+6.9954P] 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         4540
_refine_ls_number_parameters     220
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0896
_refine_ls_R_factor_gt           0.0661
_refine_ls_wR_factor_ref         0.1657
_refine_ls_wR_factor_gt          0.1531
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_restrained_S_all      1.079
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Si1 Si 0.48863(13) 0.44435(7) 0.43258(10) 0.0234(3) Uani 1 1 d . . . . .
Si2 Si 0.40574(10) 0.56841(6) 0.38175(9) 0.0128(3) Uani 1 1 d . . . . .
Si3 Si 0.10126(11) 0.52032(8) 0.26339(10) 0.0216(3) Uani 1 1 d . . . . .
Si4 Si 0.17804(12) 0.66349(7) 0.41333(11) 0.0217(3) Uani 1 1 d . . . . .
Si6 Si 0.48373(11) 0.57914(7) 0.17569(9) 0.0194(3) Uani 1 1 d . . . . .
Si5 Si 0.61524(11) 0.69153(7) 0.36979(10) 0.0193(3) Uani 1 1 d . . . . .
Cl1 Cl 0.47612(15) 0.35547(8) 0.32535(10) 0.0423(4) Uani 1 1 d . . . . .
C4 C 0.1897(5) 0.6116(3) 0.5401(4) 0.0337(12) Uani 1 1 d . . . . .
H10 H 0.2299 0.5607 0.5437 0.050 Uiso 1 1 calc R U . . .
H11 H 0.1048 0.6043 0.5398 0.050 Uiso 1 1 calc R U . . .
H12 H 0.2405 0.6429 0.6026 0.050 Uiso 1 1 calc R U . . .
C6 C 0.2691(5) 0.7564(3) 0.4570(4) 0.0312(12) Uani 1 1 d . . . . .
H16 H 0.2605 0.7876 0.3936 0.047 Uiso 1 1 calc R U . . .
H17 H 0.3585 0.7444 0.4974 0.047 Uiso 1 1 calc R U . . .
H18 H 0.2359 0.7859 0.5026 0.047 Uiso 1 1 calc R U . . .
C5 C 0.0104(5) 0.6975(3) 0.3403(5) 0.0349(13) Uani 1 1 d . . . . .
H13 H -0.0135 0.7322 0.3869 0.052 Uiso 1 1 calc R U . . .
H14 H -0.0463 0.6523 0.3206 0.052 Uiso 1 1 calc R U . . .
H15 H 0.0039 0.7256 0.2751 0.052 Uiso 1 1 calc R U . . .
C3 C -0.0213(5) 0.5559(4) 0.1336(4) 0.0405(14) Uani 1 1 d . . . . .
H7 H 0.0164 0.5608 0.0799 0.061 Uiso 1 1 calc R U . . .
H8 H -0.0529 0.6068 0.1449 0.061 Uiso 1 1 calc R U . . .
H9 H -0.0915 0.5187 0.1081 0.061 Uiso 1 1 calc R U . . .
C1 C 0.0136(4) 0.4919(3) 0.3496(4) 0.0279(11) Uani 1 1 d . . . . .
H1 H -0.0541 0.4553 0.3104 0.042 Uiso 1 1 calc R U . . .
H2 H -0.0231 0.5385 0.3683 0.042 Uiso 1 1 calc R U . . .
H3 H 0.0720 0.4671 0.4154 0.042 Uiso 1 1 calc R U . . .
C2 C 0.1556(5) 0.4236(3) 0.2322(5) 0.0392(14) Uani 1 1 d . . . . .
H4 H 0.2255 0.4042 0.2959 0.059 Uiso 1 1 calc R U . . .
H5 H 0.1843 0.4296 0.1730 0.059 Uiso 1 1 calc R U . . .
H6 H 0.0854 0.3864 0.2115 0.059 Uiso 1 1 calc R U . . .
C7 C 0.2296(4) 0.5990(2) 0.3214(3) 0.0152(9) Uani 1 1 d . . . . .
C8 C 0.2278(4) 0.6509(3) 0.2244(3) 0.0179(9) Uani 1 1 d . . . . .
H19 H 0.2092 0.6176 0.1602 0.021 Uiso 1 1 calc R U . . .
H20 H 0.1596 0.6902 0.2078 0.021 Uiso 1 1 calc R U . . .
C9 C 0.3544(4) 0.6924(3) 0.2500(3) 0.0180(9) Uani 1 1 d . . . . .
H21 H 0.3652 0.7335 0.3042 0.022 Uiso 1 1 calc R U . . .
H22 H 0.3552 0.7175 0.1842 0.022 Uiso 1 1 calc R U . . .
C10 C 0.4664(4) 0.6325(2) 0.2939(3) 0.0157(9) Uani 1 1 d . . . . .
C16 C 0.5912(5) 0.7621(3) 0.4656(4) 0.0291(11) Uani 1 1 d . . . . .
H38 H 0.5674 0.7337 0.5180 0.044 Uiso 1 1 calc R U . . .
H39 H 0.5237 0.7987 0.4259 0.044 Uiso 1 1 calc R U . . .
H40 H 0.6697 0.7909 0.5030 0.044 Uiso 1 1 calc R U . . .
C15 C 0.6625(5) 0.7532(3) 0.2764(4) 0.0329(12) Uani 1 1 d . . . . .
H35 H 0.5897 0.7839 0.2304 0.049 Uiso 1 1 calc R U . . .
H36 H 0.6913 0.7195 0.2317 0.049 Uiso 1 1 calc R U . . .
H37 H 0.7311 0.7883 0.3184 0.049 Uiso 1 1 calc R U . . .
C14 C 0.4607(5) 0.6481(3) 0.0613(4) 0.0303(11) Uani 1 1 d . . . . .
H32 H 0.5077 0.6963 0.0891 0.045 Uiso 1 1 calc R U . . .
H33 H 0.3706 0.6601 0.0247 0.045 Uiso 1 1 calc R U . . .
H34 H 0.4918 0.6237 0.0104 0.045 Uiso 1 1 calc R U . . .
C12 C 0.7549(5) 0.6310(3) 0.4524(4) 0.0327(12) Uani 1 1 d . . . . .
H26 H 0.8273 0.6651 0.4892 0.049 Uiso 1 1 calc R U . . .
H27 H 0.7761 0.5950 0.4055 0.049 Uiso 1 1 calc R U . . .
H28 H 0.7344 0.6013 0.5055 0.049 Uiso 1 1 calc R U . . .
C13 C 0.6404(5) 0.5314(3) 0.2110(4) 0.0356(13) Uani 1 1 d . . . . .
H29 H 0.6576 0.4979 0.2738 0.053 Uiso 1 1 calc R U . . .
H30 H 0.7063 0.5714 0.2275 0.053 Uiso 1 1 calc R U . . .
H31 H 0.6398 0.4999 0.1502 0.053 Uiso 1 1 calc R U . . .
C11 C 0.3634(5) 0.5013(3) 0.1128(4) 0.0352(12) Uani 1 1 d . . . . .
H23 H 0.3729 0.4818 0.0481 0.053 Uiso 1 1 calc R U . . .
H24 H 0.2784 0.5230 0.0935 0.053 Uiso 1 1 calc R U . . .
H25 H 0.3759 0.4585 0.1639 0.053 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 2.0690(18) . ?
Si1 Si2 2.3249(17) . ?
Si1 Si2 2.3361(17) 3_666 ?
Si1 Si1 2.581(2) 3_666 ?
Si2 C10 1.931(4) . ?
Si2 C7 1.936(4) . ?
Si2 Si1 2.3360(17) 3_666 ?
Si3 C1 1.871(5) . ?
Si3 C3 1.877(5) . ?
Si3 C2 1.877(5) . ?
Si3 C7 1.928(4) . ?
Si4 C6 1.873(5) . ?
Si4 C5 1.883(5) . ?
Si4 C4 1.887(5) . ?
Si4 C7 1.917(4) . ?
Si6 C13 1.861(5) . ?
Si6 C11 1.872(5) . ?
Si6 C14 1.881(5) . ?
Si6 C10 1.915(4) . ?
Si5 C16 1.868(5) . ?
Si5 C12 1.873(5) . ?
Si5 C15 1.878(5) . ?
Si5 C10 1.908(4) . ?
C4 H10 0.9800 . ?
C4 H11 0.9800 . ?
C4 H12 0.9800 . ?
C6 H16 0.9800 . ?
C6 H17 0.9800 . ?
C6 H18 0.9800 . ?
C5 H13 0.9800 . ?
C5 H14 0.9800 . ?
C5 H15 0.9800 . ?
C3 H7 0.9800 . ?
C3 H8 0.9800 . ?
C3 H9 0.9800 . ?
C1 H1 0.9800 . ?
C1 H2 0.9800 . ?
C1 H3 0.9800 . ?
C2 H4 0.9800 . ?
C2 H5 0.9800 . ?
C2 H6 0.9800 . ?
C7 C8 1.576(6) . ?
C8 C9 1.532(6) . ?
C8 H19 0.9900 . ?
C8 H20 0.9900 . ?
C9 C10 1.572(6) . ?
C9 H21 0.9900 . ?
C9 H22 0.9900 . ?
C16 H38 0.9800 . ?
C16 H39 0.9800 . ?
C16 H40 0.9800 . ?
C15 H35 0.9800 . ?
C15 H36 0.9800 . ?
C15 H37 0.9800 . ?
C14 H32 0.9800 . ?
C14 H33 0.9800 . ?
C14 H34 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 . ?
C11 H23 0.9800 . ?
C11 H24 0.9800 . ?
C11 H25 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
Cl1 Si1 Si2 123.94(7) . . ?
Cl1 Si1 Si2 123.29(7) . 3_666 ?
Si2 Si1 Si2 112.74(6) . 3_666 ?
Cl1 Si1 Si1 178.27(11) . 3_666 ?
Si2 Si1 Si1 56.58(5) . 3_666 ?
Si2 Si1 Si1 56.16(5) 3_666 3_666 ?
C10 Si2 C7 98.65(17) . . ?
C10 Si2 Si1 119.98(14) . . ?
C7 Si2 Si1 127.90(14) . . ?
C10 Si2 Si1 123.45(14) . 3_666 ?
C7 Si2 Si1 120.19(13) . 3_666 ?
Si1 Si2 Si1 67.26(6) . 3_666 ?
C1 Si3 C3 106.1(2) . . ?
C1 Si3 C2 102.3(2) . . ?
C3 Si3 C2 105.8(3) . . ?
C1 Si3 C7 116.0(2) . . ?
C3 Si3 C7 109.3(2) . . ?
C2 Si3 C7 116.4(2) . . ?
C6 Si4 C5 103.5(2) . . ?
C6 Si4 C4 106.3(2) . . ?
C5 Si4 C4 108.9(2) . . ?
C6 Si4 C7 114.9(2) . . ?
C5 Si4 C7 110.2(2) . . ?
C4 Si4 C7 112.5(2) . . ?
C13 Si6 C11 105.8(3) . . ?
C13 Si6 C14 107.7(2) . . ?
C11 Si6 C14 103.3(2) . . ?
C13 Si6 C10 113.3(2) . . ?
C11 Si6 C10 115.1(2) . . ?
C14 Si6 C10 110.9(2) . . ?
C16 Si5 C12 105.5(2) . . ?
C16 Si5 C15 104.9(2) . . ?
C12 Si5 C15 108.1(2) . . ?
C16 Si5 C10 112.1(2) . . ?
C12 Si5 C10 114.0(2) . . ?
C15 Si5 C10 111.6(2) . . ?
Si4 C4 H10 109.5 . . ?
Si4 C4 H11 109.5 . . ?
H10 C4 H11 109.5 . . ?
Si4 C4 H12 109.5 . . ?
H10 C4 H12 109.5 . . ?
H11 C4 H12 109.5 . . ?
Si4 C6 H16 109.5 . . ?
Si4 C6 H17 109.5 . . ?
H16 C6 H17 109.5 . . ?
Si4 C6 H18 109.5 . . ?
H16 C6 H18 109.5 . . ?
H17 C6 H18 109.5 . . ?
Si4 C5 H13 109.5 . . ?
Si4 C5 H14 109.5 . . ?
H13 C5 H14 109.5 . . ?
Si4 C5 H15 109.5 . . ?
H13 C5 H15 109.5 . . ?
H14 C5 H15 109.5 . . ?
Si3 C3 H7 109.5 . . ?
Si3 C3 H8 109.5 . . ?
H7 C3 H8 109.5 . . ?
Si3 C3 H9 109.5 . . ?
H7 C3 H9 109.5 . . ?
H8 C3 H9 109.5 . . ?
Si3 C1 H1 109.5 . . ?
Si3 C1 H2 109.5 . . ?
H1 C1 H2 109.5 . . ?
Si3 C1 H3 109.5 . . ?
H1 C1 H3 109.5 . . ?
H2 C1 H3 109.5 . . ?
Si3 C2 H4 109.5 . . ?
Si3 C2 H5 109.5 . . ?
H4 C2 H5 109.5 . . ?
Si3 C2 H6 109.5 . . ?
H4 C2 H6 109.5 . . ?
H5 C2 H6 109.5 . . ?
C8 C7 Si4 107.6(3) . . ?
C8 C7 Si3 107.1(3) . . ?
Si4 C7 Si3 106.88(19) . . ?
C8 C7 Si2 100.4(2) . . ?
Si4 C7 Si2 114.5(2) . . ?
Si3 C7 Si2 119.3(2) . . ?
C9 C8 C7 111.5(3) . . ?
C9 C8 H19 109.3 . . ?
C7 C8 H19 109.3 . . ?
C9 C8 H20 109.3 . . ?
C7 C8 H20 109.3 . . ?
H19 C8 H20 108.0 . . ?
C8 C9 C10 110.3(3) . . ?
C8 C9 H21 109.6 . . ?
C10 C9 H21 109.6 . . ?
C8 C9 H22 109.6 . . ?
C10 C9 H22 109.6 . . ?
H21 C9 H22 108.1 . . ?
C9 C10 Si5 106.6(3) . . ?
C9 C10 Si6 109.2(3) . . ?
Si5 C10 Si6 110.1(2) . . ?
C9 C10 Si2 99.8(2) . . ?
Si5 C10 Si2 115.6(2) . . ?
Si6 C10 Si2 114.6(2) . . ?
Si5 C16 H38 109.5 . . ?
Si5 C16 H39 109.5 . . ?
H38 C16 H39 109.5 . . ?
Si5 C16 H40 109.5 . . ?
H38 C16 H40 109.5 . . ?
H39 C16 H40 109.5 . . ?
Si5 C15 H35 109.5 . . ?
Si5 C15 H36 109.5 . . ?
H35 C15 H36 109.5 . . ?
Si5 C15 H37 109.5 . . ?
H35 C15 H37 109.5 . . ?
H36 C15 H37 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 . . ?
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 . . ?
Si6 C13 H29 109.5 . . ?
Si6 C13 H30 109.5 . . ?
H29 C13 H30 109.5 . . ?
Si6 C13 H31 109.5 . . ?
H29 C13 H31 109.5 . . ?
H30 C13 H31 109.5 . . ?
Si6 C11 H23 109.5 . . ?
Si6 C11 H24 109.5 . . ?
H23 C11 H24 109.5 . . ?
Si6 C11 H25 109.5 . . ?
H23 C11 H25 109.5 . . ?
H24 C11 H25 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 C7 C8 C9 88.5(4) . . . . ?
Si3 C7 C8 C9 -156.9(3) . . . . ?
Si2 C7 C8 C9 -31.6(4) . . . . ?
C7 C8 C9 C10 50.2(5) . . . . ?
C8 C9 C10 Si5 -159.5(3) . . . . ?
C8 C9 C10 Si6 81.5(4) . . . . ?
C8 C9 C10 Si2 -39.0(4) . . . . ?

_refine_diff_density_max         0.996
_refine_diff_density_min         -0.845
_refine_diff_density_rms         0.103


_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_tn49a_a
_database_code_depnum_ccdc_archive 'CCDC 2032838'
loop_
_audit_author_name
_audit_author_address
'Takumi Nukazawa'
;Tohoku University
Japan
;
_audit_update_record             
;
2020-09-19 deposited with the CCDC.	2020-10-27 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        (chloro)(chlorosilyl)cyclotrisilene-DMAP
_chemical_name_common            ?
_chemical_melting_point          353
_chemical_formula_moiety         'C39 H90 Cl2 N2 Si12, 2(C6 H6)'
_chemical_formula_sum            'C51 H102 Cl2 N2 Si12'
_chemical_formula_weight         1151.32

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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                   13.5086(3)
_cell_length_b                   15.0599(4)
_cell_length_c                   16.6833(4)
_cell_angle_alpha                89.3640(10)
_cell_angle_beta                 85.2090(10)
_cell_angle_gamma                76.7430(10)
_cell_volume                     3291.92(14)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9712
_cell_measurement_theta_min      2.27
_cell_measurement_theta_max      28.94

_exptl_crystal_description       plate
_exptl_crystal_colour            red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.162
_exptl_crystal_F_000             1248
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.010
_exptl_absorpt_coefficient_mu    0.350
_shelx_estimated_absorpt_T_min   0.966
_shelx_estimated_absorpt_T_max   0.997
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.7081
_exptl_absorpt_correction_T_max  0.7461
_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            49798
_diffrn_reflns_av_unetI/netI     0.0498
_diffrn_reflns_av_R_equivalents  0.0453
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         1.225
_diffrn_reflns_theta_max         27.500
_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             15123
_reflns_number_gt                11884
_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)+(0.0362P)²+1.1232P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         15123
_refine_ls_number_parameters     678
_refine_ls_number_restraints     12
_refine_ls_R_factor_all          0.0521
_refine_ls_R_factor_gt           0.0356
_refine_ls_wR_factor_ref         0.0887
_refine_ls_wR_factor_gt          0.0802
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_restrained_S_all      1.015
_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
C1 C 0.6984(2) 0.61387(18) 0.21187(17) 0.0441(7) Uani 1 1 d . . . . .
H1 H 0.6682 0.5628 0.2111 0.052(11) Uiso 0.740(6) 1 calc R . P A 1
H1A H 0.6961 0.5567 0.2357 0.7(4) Uiso 0.260(6) 1 calc R . P A 2
C2A C 0.7680(3) 0.6145(2) 0.2630(2) 0.0372(10) Uani 0.740(6) 1 d . . P A 1
H2A H 0.7826 0.5672 0.3014 0.045 Uiso 0.740(6) 1 calc R U P A 1
C3A C 0.8195(3) 0.6840(2) 0.2604(2) 0.0344(9) Uani 0.740(6) 1 d . . P A 1
H3A H 0.8715 0.6834 0.2956 0.041 Uiso 0.740(6) 1 calc R U P A 1
C4A C 0.7953(5) 0.7541(5) 0.2067(5) 0.0353(13) Uani 0.740(6) 1 d . . P A 1
H4A H 0.8312 0.8016 0.2039 0.042 Uiso 0.740(6) 1 calc R U P A 1
C5A C 0.7178(5) 0.7549(3) 0.1568(3) 0.0534(14) Uani 0.740(6) 1 d . . P A 1
H5A H 0.6991 0.8040 0.1207 0.064 Uiso 0.740(6) 1 calc R U P A 1
C6A C 0.6681(4) 0.6847(3) 0.1595(2) 0.0507(13) Uani 0.740(6) 1 d . . P A 1
H6A H 0.6143 0.6849 0.1262 0.061 Uiso 0.740(6) 1 calc R U P A 1
C2B C 0.7832(8) 0.6654(8) 0.2282(9) 0.045(3) Uani 0.260(6) 1 d . . P A 2
H2B H 0.8450 0.6369 0.2504 0.054 Uiso 0.260(6) 1 calc R U P A 2
C3B C 0.7591(11) 0.7562(16) 0.2073(15) 0.035(4) Uani 0.260(6) 1 d . U P A 2
H3B H 0.8054 0.7925 0.2184 0.042 Uiso 0.260(6) 1 calc R U P A 2
C4B C 0.6742(10) 0.7966(9) 0.1720(8) 0.040(3) Uani 0.260(6) 1 d . U P A 2
H4B H 0.6588 0.8605 0.1627 0.048 Uiso 0.260(6) 1 calc R U P A 2
C5B C 0.6092(8) 0.7425(7) 0.1494(5) 0.031(2) Uani 0.260(6) 1 d . . P A 2
H5B H 0.5493 0.7681 0.1234 0.037 Uiso 0.260(6) 1 calc R U P A 2
C6B C 0.6354(9) 0.6516(8) 0.1665(7) 0.039(3) Uani 0.260(6) 1 d . . P A 2
H6B H 0.6008 0.6134 0.1403 0.047 Uiso 0.260(6) 1 calc R U P A 2
C7 C 0.0606(2) 0.8017(2) 0.2811(2) 0.0566(8) Uani 1 1 d . . . . .
H7 H 0.0625 0.7387 0.2744 0.068 Uiso 1 1 calc R U . . .
C8 C 0.0723(2) 0.8349(3) 0.3547(2) 0.0647(10) Uani 1 1 d . . . . .
H8 H 0.0831 0.7947 0.3991 0.078 Uiso 1 1 calc R U . . .
C9 C 0.04602(18) 0.8602(2) 0.21651(16) 0.0445(7) Uani 1 1 d . . . . .
H9 H 0.0380 0.8375 0.1651 0.053 Uiso 1 1 calc R U . . .
C10 C 0.06857(19) 0.9255(3) 0.36480(17) 0.0584(9) Uani 1 1 d . . . . .
H10 H 0.0759 0.9484 0.4163 0.070 Uiso 1 1 calc R U . . .
C11 C 0.04315(17) 0.95106(18) 0.22661(15) 0.0373(6) Uani 1 1 d . . . . .
H11 H 0.0334 0.9911 0.1821 0.045 Uiso 1 1 calc R U . . .
C12 C 0.05417(17) 0.98391(19) 0.30016(16) 0.0428(6) Uani 1 1 d . . . . .
H12 H 0.0520 1.0469 0.3071 0.051 Uiso 1 1 calc R U . . .
Si1 Si 0.37761(4) 0.43293(3) 0.21235(3) 0.01301(10) Uani 1 1 d . . . . .
Cl1 Cl 0.36671(4) 0.46279(3) 0.08905(3) 0.01886(10) Uani 1 1 d . . . . .
Si2 Si 0.45768(4) 0.30598(3) 0.26911(3) 0.01255(10) Uani 1 1 d . . . . .
Si3 Si 0.60778(4) 0.19545(3) 0.22467(3) 0.01074(10) Uani 1 1 d . . . . .
Si4 Si 0.27617(4) 0.34075(3) 0.26744(3) 0.01140(10) Uani 1 1 d . . . . .
Cl2 Cl 0.54136(3) 0.08043(3) 0.21919(3) 0.01638(9) Uani 1 1 d . . . . .
Si5 Si 0.71435(4) 0.09033(3) 0.06095(3) 0.01566(11) Uani 1 1 d . . . . .
C13 C 0.59329(15) 0.07271(14) 0.02291(12) 0.0242(4) Uani 1 1 d . . . . .
H13 H 0.6010 0.0691 -0.0360 0.036 Uiso 1 1 calc R U . . .
H13A H 0.5367 0.1240 0.0402 0.036 Uiso 1 1 calc R U . . .
H13B H 0.5789 0.0158 0.0446 0.036 Uiso 1 1 calc R U . . .
C14 C 0.80305(16) 0.09638(14) -0.03127(12) 0.0243(4) Uani 1 1 d . . . . .
H14 H 0.8653 0.1118 -0.0153 0.036 Uiso 1 1 calc R U . . .
H14A H 0.7693 0.1433 -0.0674 0.036 Uiso 1 1 calc R U . . .
H14B H 0.8207 0.0372 -0.0591 0.036 Uiso 1 1 calc R U . . .
C15 C 0.78014(16) -0.01860(13) 0.10753(12) 0.0244(4) Uani 1 1 d . . . . .
H15 H 0.7423 -0.0279 0.1585 0.037 Uiso 1 1 calc R U . . .
H15A H 0.8496 -0.0153 0.1176 0.037 Uiso 1 1 calc R U . . .
H15B H 0.7830 -0.0697 0.0709 0.037 Uiso 1 1 calc R U . . .
C16 C 0.57251(14) 0.29943(13) -0.00839(11) 0.0193(4) Uani 1 1 d . . . . .
H16 H 0.5103 0.2920 0.0230 0.029 Uiso 1 1 calc R U . . .
H16A H 0.5961 0.2485 -0.0466 0.029 Uiso 1 1 calc R U . . .
H16B H 0.5580 0.3569 -0.0379 0.029 Uiso 1 1 calc R U . . .
C17 C 0.64081(15) 0.41205(12) 0.11692(11) 0.0177(4) Uani 1 1 d . . . . .
H17 H 0.6176 0.4618 0.0796 0.027 Uiso 1 1 calc R U . . .
H17A H 0.7012 0.4216 0.1412 0.027 Uiso 1 1 calc R U . . .
H17B H 0.5862 0.4110 0.1592 0.027 Uiso 1 1 calc R U . . .
Si6 Si 0.67392(4) 0.30106(3) 0.06099(3) 0.01368(11) Uani 1 1 d . . . . .
C18 C 0.79397(14) 0.31055(13) -0.00195(11) 0.0202(4) Uani 1 1 d . . . . .
H18 H 0.7896 0.3744 -0.0168 0.030 Uiso 1 1 calc R U . . .
H18A H 0.8014 0.2732 -0.0508 0.030 Uiso 1 1 calc R U . . .
H18B H 0.8532 0.2890 0.0291 0.030 Uiso 1 1 calc R U . . .
C19 C 0.69808(13) 0.19589(12) 0.12884(10) 0.0124(3) Uani 1 1 d . . . . .
C20 C 0.80235(13) 0.19218(12) 0.16622(11) 0.0151(4) Uani 1 1 d . . . . .
H20 H 0.8596 0.1635 0.1270 0.018 Uiso 1 1 calc R U . . .
H20A H 0.8087 0.2551 0.1771 0.018 Uiso 1 1 calc R U . . .
C21 C 0.80938(13) 0.13779(13) 0.24457(11) 0.0157(4) Uani 1 1 d . . . . .
H21 H 0.8682 0.1472 0.2723 0.019 Uiso 1 1 calc R U . . .
H21A H 0.8208 0.0719 0.2320 0.019 Uiso 1 1 calc R U . . .
C22 C 0.70896(13) 0.16858(12) 0.30161(10) 0.0120(3) Uani 1 1 d . . . . .
Si7 Si 0.71802(4) 0.27057(3) 0.36558(3) 0.01422(11) Uani 1 1 d . . . . .
C23 C 0.69759(15) 0.38261(13) 0.31304(12) 0.0215(4) Uani 1 1 d . . . . .
H23 H 0.6317 0.3949 0.2897 0.032 Uiso 1 1 calc R U . . .
H23A H 0.7523 0.3807 0.2702 0.032 Uiso 1 1 calc R U . . .
H23B H 0.6980 0.4310 0.3517 0.032 Uiso 1 1 calc R U . . .
C24 C 0.85023(15) 0.25669(15) 0.39955(12) 0.0245(4) Uani 1 1 d . . . . .
H24 H 0.8490 0.3015 0.4420 0.037 Uiso 1 1 calc R U . . .
H24A H 0.8970 0.2664 0.3539 0.037 Uiso 1 1 calc R U . . .
H24B H 0.8734 0.1950 0.4204 0.037 Uiso 1 1 calc R U . . .
C25 C 0.62436(15) 0.28922(14) 0.45652(11) 0.0214(4) Uani 1 1 d . . . . .
H25 H 0.6315 0.3427 0.4866 0.032 Uiso 1 1 calc R U . . .
H25A H 0.6377 0.2353 0.4909 0.032 Uiso 1 1 calc R U . . .
H25B H 0.5549 0.2994 0.4397 0.032 Uiso 1 1 calc R U . . .
Si8 Si 0.69752(4) 0.07114(3) 0.37414(3) 0.01468(11) Uani 1 1 d . . . . .
C26 C 0.78552(15) 0.06193(14) 0.45712(12) 0.0238(4) Uani 1 1 d . . . . .
H26 H 0.7675 0.1182 0.4894 0.036 Uiso 1 1 calc R U . . .
H26A H 0.8562 0.0527 0.4337 0.036 Uiso 1 1 calc R U . . .
H26B H 0.7787 0.0101 0.4914 0.036 Uiso 1 1 calc R U . . .
C27 C 0.56513(14) 0.08229(13) 0.42306(11) 0.0199(4) Uani 1 1 d . . . . .
H27 H 0.5319 0.0402 0.3971 0.030 Uiso 1 1 calc R U . . .
H27A H 0.5257 0.1450 0.4174 0.030 Uiso 1 1 calc R U . . .
H27B H 0.5685 0.0675 0.4803 0.030 Uiso 1 1 calc R U . . .
C28 C 0.73881(15) -0.04481(13) 0.32633(12) 0.0218(4) Uani 1 1 d . . . . .
H28 H 0.7339 -0.0914 0.3670 0.033 Uiso 1 1 calc R U . . .
H28A H 0.8096 -0.0541 0.3032 0.033 Uiso 1 1 calc R U . . .
H28B H 0.6945 -0.0496 0.2837 0.033 Uiso 1 1 calc R U . . .
C29 C 0.26140(15) 0.10204(13) 0.18296(12) 0.0223(4) Uani 1 1 d . . . . .
H29 H 0.2805 0.0538 0.1419 0.033 Uiso 1 1 calc R U . . .
H29A H 0.2089 0.0880 0.2220 0.033 Uiso 1 1 calc R U . . .
H29B H 0.3216 0.1058 0.2106 0.033 Uiso 1 1 calc R U . . .
C30 C 0.31597(15) 0.22736(14) 0.05954(12) 0.0234(4) Uani 1 1 d . . . . .
H30 H 0.3729 0.2380 0.0878 0.035 Uiso 1 1 calc R U . . .
H30A H 0.2917 0.2794 0.0249 0.035 Uiso 1 1 calc R U . . .
H30B H 0.3389 0.1718 0.0266 0.035 Uiso 1 1 calc R U . . .
Si9 Si 0.21034(4) 0.21363(3) 0.13417(3) 0.01556(11) Uani 1 1 d . . . . .
C31 C 0.09707(15) 0.19337(14) 0.08451(13) 0.0253(4) Uani 1 1 d . . . . .
H31 H 0.0694 0.2463 0.0518 0.038 Uiso 1 1 calc R U . . .
H31A H 0.0444 0.1843 0.1258 0.038 Uiso 1 1 calc R U . . .
H31B H 0.1184 0.1390 0.0500 0.038 Uiso 1 1 calc R U . . .
Si10 Si 0.09183(4) 0.41552(4) 0.15021(3) 0.01644(11) Uani 1 1 d . . . . .
C32 C -0.04721(14) 0.41238(14) 0.16023(13) 0.0244(4) Uani 1 1 d . . . . .
H32 H -0.0735 0.4209 0.2168 0.037 Uiso 1 1 calc R U . . .
H32A H -0.0549 0.3533 0.1409 0.037 Uiso 1 1 calc R U . . .
H32B H -0.0856 0.4613 0.1282 0.037 Uiso 1 1 calc R U . . .
C33 C 0.12928(16) 0.41941(14) 0.03952(12) 0.0243(4) Uani 1 1 d . . . . .
H33 H 0.0866 0.4735 0.0163 0.036 Uiso 1 1 calc R U . . .
H33A H 0.1197 0.3644 0.0133 0.036 Uiso 1 1 calc R U . . .
H33B H 0.2011 0.4224 0.0311 0.036 Uiso 1 1 calc R U . . .
C34 C 0.09179(15) 0.53223(13) 0.18838(13) 0.0240(4) Uani 1 1 d . . . . .
H34 H 0.1621 0.5366 0.1942 0.036 Uiso 1 1 calc R U . . .
H34A H 0.0521 0.5429 0.2407 0.036 Uiso 1 1 calc R U . . .
H34B H 0.0611 0.5782 0.1501 0.036 Uiso 1 1 calc R U . . .
C35 C 0.16884(13) 0.31373(12) 0.20693(11) 0.0139(4) Uani 1 1 d . . . . .
C36 C 0.09538(13) 0.29022(12) 0.27780(11) 0.0158(4) Uani 1 1 d . . . . .
H36 H 0.0263 0.2958 0.2596 0.019 Uiso 1 1 calc R U . . .
H36A H 0.1209 0.2267 0.2953 0.019 Uiso 1 1 calc R U . . .
C37 C 0.09047(13) 0.35620(12) 0.34801(11) 0.0154(4) Uani 1 1 d . . . . .
H37 H 0.0471 0.3403 0.3943 0.018 Uiso 1 1 calc R U . . .
H37A H 0.0604 0.4194 0.3317 0.018 Uiso 1 1 calc R U . . .
C38 C 0.20186(13) 0.34892(12) 0.37255(10) 0.0136(4) Uani 1 1 d . . . . .
C39 C 0.29472(15) 0.13196(13) 0.38059(12) 0.0207(4) Uani 1 1 d . . . . .
H39 H 0.3487 0.1411 0.3405 0.031 Uiso 1 1 calc R U . . .
H39A H 0.2415 0.1125 0.3535 0.031 Uiso 1 1 calc R U . . .
H39B H 0.3236 0.0849 0.4186 0.031 Uiso 1 1 calc R U . . .
C40 C 0.33350(14) 0.24887(14) 0.50977(11) 0.0209(4) Uani 1 1 d . . . . .
H40 H 0.3540 0.1899 0.5363 0.031 Uiso 1 1 calc R U . . .
H40A H 0.3029 0.2961 0.5502 0.031 Uiso 1 1 calc R U . . .
H40B H 0.3936 0.2644 0.4812 0.031 Uiso 1 1 calc R U . . .
C41 C 0.15179(16) 0.56323(13) 0.38738(12) 0.0251(4) Uani 1 1 d . . . . .
H41 H 0.1513 0.6134 0.4244 0.038 Uiso 1 1 calc R U . . .
H41A H 0.0818 0.5646 0.3749 0.038 Uiso 1 1 calc R U . . .
H41B H 0.1934 0.5699 0.3376 0.038 Uiso 1 1 calc R U . . .
C42 C 0.12115(15) 0.22082(15) 0.49627(12) 0.0250(5) Uani 1 1 d . . . . .
H42 H 0.1416 0.1725 0.5354 0.037 Uiso 1 1 calc R U . . .
H42A H 0.0762 0.2021 0.4599 0.037 Uiso 1 1 calc R U . . .
H42B H 0.0849 0.2770 0.5246 0.037 Uiso 1 1 calc R U . . .
C43 C 0.12828(16) 0.45254(15) 0.53404(12) 0.0270(5) Uani 1 1 d . . . . .
H43 H 0.1216 0.5109 0.5618 0.040 Uiso 1 1 calc R U . . .
H43A H 0.1618 0.4026 0.5676 0.040 Uiso 1 1 calc R U . . .
H43B H 0.0604 0.4445 0.5240 0.040 Uiso 1 1 calc R U . . .
Si11 Si 0.20704(4) 0.45179(4) 0.43554(3) 0.01756(11) Uani 1 1 d . . . . .
C44 C 0.33827(15) 0.45897(14) 0.46064(12) 0.0242(4) Uani 1 1 d . . . . .
H44 H 0.3896 0.4205 0.4231 0.036 Uiso 1 1 calc R U . . .
H44A H 0.3487 0.4378 0.5157 0.036 Uiso 1 1 calc R U . . .
H44B H 0.3448 0.5224 0.4562 0.036 Uiso 1 1 calc R U . . .
N1 N 0.38552(11) 0.55097(10) 0.24193(9) 0.0143(3) Uani 1 1 d . . . . .
C45 C 0.32888(14) 0.62741(12) 0.20965(11) 0.0172(4) Uani 1 1 d . . . . .
H45 H 0.2829 0.6203 0.1714 0.021 Uiso 1 1 calc R U . . .
C46 C 0.44776(14) 0.56387(12) 0.29836(11) 0.0168(4) Uani 1 1 d . . . . .
H46 H 0.4856 0.5118 0.3239 0.020 Uiso 1 1 calc R U . . .
C47 C 0.45882(14) 0.64763(12) 0.32031(11) 0.0184(4) Uani 1 1 d . . . . .
H47 H 0.5034 0.6527 0.3603 0.022 Uiso 1 1 calc R U . . .
C48 C 0.33444(14) 0.71313(12) 0.22902(11) 0.0177(4) Uani 1 1 d . . . . .
H48 H 0.2914 0.7640 0.2057 0.021 Uiso 1 1 calc R U . . .
C49 C 0.40405(14) 0.72737(12) 0.28384(11) 0.0173(4) Uani 1 1 d . . . . .
C50 C 0.35950(19) 0.89140(14) 0.26011(15) 0.0346(6) Uani 1 1 d . . . . .
H50 H 0.3803 0.8886 0.2023 0.052 Uiso 1 1 calc R U . . .
H50A H 0.3730 0.9465 0.2833 0.052 Uiso 1 1 calc R U . . .
H50B H 0.2864 0.8931 0.2685 0.052 Uiso 1 1 calc R U . . .
N2 N 0.41728(13) 0.81100(11) 0.29903(10) 0.0236(4) Uani 1 1 d . . . . .
C51 C 0.49982(17) 0.82277(14) 0.34635(13) 0.0297(5) Uani 1 1 d . . . . .
H51 H 0.4879 0.8019 0.4014 0.045 Uiso 1 1 calc R U . . .
H51A H 0.5018 0.8874 0.3474 0.045 Uiso 1 1 calc R U . . .
H51B H 0.5650 0.7869 0.3220 0.045 Uiso 1 1 calc R U . . .
Si12 Si 0.23800(4) 0.24163(4) 0.43636(3) 0.01593(11) Uani 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C6B 1.224(13) . ?
C1 C2A 1.323(5) . ?
C1 C6A 1.381(5) . ?
C1 C2B 1.566(12) . ?
C2A C3A 1.383(5) . ?
C3A C4A 1.376(8) . ?
C4A C5A 1.390(8) . ?
C5A C6A 1.375(6) . ?
C2B C3B 1.38(3) . ?
C3B C4B 1.35(2) . ?
C4B C5B 1.403(15) . ?
C5B C6B 1.367(15) . ?
C7 C8 1.365(5) . ?
C7 C9 1.383(4) . ?
C8 C10 1.366(5) . ?
C9 C11 1.372(4) . ?
C10 C12 1.382(4) . ?
C11 C12 1.360(4) . ?
Si1 N1 1.8789(15) . ?
Si1 Cl1 2.1107(6) . ?
Si1 Si2 2.2145(7) . ?
Si1 Si4 2.2986(7) . ?
Si2 Si3 2.3791(7) . ?
Si2 Si4 2.3893(7) . ?
Si3 C22 1.9254(18) . ?
Si3 C19 1.9292(18) . ?
Si3 Cl2 2.1317(6) . ?
Si4 C38 1.9370(18) . ?
Si4 C35 1.9522(18) . ?
Si5 C15 1.872(2) . ?
Si5 C13 1.877(2) . ?
Si5 C14 1.884(2) . ?
Si5 C19 1.9227(18) . ?
C16 Si6 1.8704(19) . ?
C17 Si6 1.8673(19) . ?
Si6 C18 1.8898(19) . ?
Si6 C19 1.9186(18) . ?
C19 C20 1.577(2) . ?
C20 C21 1.533(2) . ?
C21 C22 1.570(2) . ?
C22 Si7 1.9125(18) . ?
C22 Si8 1.9170(18) . ?
Si7 C23 1.8669(19) . ?
Si7 C25 1.8729(19) . ?
Si7 C24 1.8841(19) . ?
Si8 C28 1.872(2) . ?
Si8 C27 1.8746(19) . ?
Si8 C26 1.883(2) . ?
C29 Si9 1.869(2) . ?
C30 Si9 1.861(2) . ?
Si9 C31 1.885(2) . ?
Si9 C35 1.8973(19) . ?
Si10 C34 1.876(2) . ?
Si10 C33 1.877(2) . ?
Si10 C32 1.883(2) . ?
Si10 C35 1.9309(18) . ?
C35 C36 1.570(2) . ?
C36 C37 1.532(3) . ?
C37 C38 1.572(2) . ?
C38 Si11 1.8993(19) . ?
C38 Si12 1.9154(18) . ?
C39 Si12 1.875(2) . ?
C40 Si12 1.8727(19) . ?
C41 Si11 1.875(2) . ?
C42 Si12 1.883(2) . ?
C43 Si11 1.880(2) . ?
Si11 C44 1.882(2) . ?
N1 C46 1.357(2) . ?
N1 C45 1.361(2) . ?
C45 C48 1.354(3) . ?
C46 C47 1.361(3) . ?
C47 C49 1.418(3) . ?
C48 C49 1.417(3) . ?
C49 N2 1.342(2) . ?
C50 N2 1.460(3) . ?
N2 C51 1.462(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
C2A C1 C6A 122.5(3) . . ?
C6B C1 C2B 116.0(7) . . ?
C1 C2A C3A 119.8(3) . . ?
C4A C3A C2A 119.8(4) . . ?
C3A C4A C5A 119.4(5) . . ?
C6A C5A C4A 120.1(5) . . ?
C5A C6A C1 118.2(4) . . ?
C3B C2B C1 113.3(10) . . ?
C4B C3B C2B 124.2(15) . . ?
C3B C4B C5B 118.7(14) . . ?
C6B C5B C4B 117.3(11) . . ?
C1 C6B C5B 127.2(11) . . ?
C8 C7 C9 119.6(3) . . ?
C7 C8 C10 120.3(3) . . ?
C11 C9 C7 120.0(3) . . ?
C8 C10 C12 120.0(3) . . ?
C12 C11 C9 120.2(2) . . ?
C11 C12 C10 119.9(3) . . ?
N1 Si1 Cl1 94.96(5) . . ?
N1 Si1 Si2 124.56(5) . . ?
Cl1 Si1 Si2 128.97(3) . . ?
N1 Si1 Si4 130.26(5) . . ?
Cl1 Si1 Si4 116.27(3) . . ?
Si2 Si1 Si4 63.90(2) . . ?
Si1 Si2 Si3 131.10(3) . . ?
Si1 Si2 Si4 59.76(2) . . ?
Si3 Si2 Si4 142.33(3) . . ?
C22 Si3 C19 98.41(7) . . ?
C22 Si3 Cl2 107.48(6) . . ?
C19 Si3 Cl2 108.49(6) . . ?
C22 Si3 Si2 114.45(6) . . ?
C19 Si3 Si2 128.68(6) . . ?
Cl2 Si3 Si2 98.22(2) . . ?
C38 Si4 C35 96.82(8) . . ?
C38 Si4 Si1 128.87(6) . . ?
C35 Si4 Si1 119.78(6) . . ?
C38 Si4 Si2 114.79(6) . . ?
C35 Si4 Si2 141.08(6) . . ?
Si1 Si4 Si2 56.34(2) . . ?
C15 Si5 C13 108.15(10) . . ?
C15 Si5 C14 101.78(9) . . ?
C13 Si5 C14 105.81(9) . . ?
C15 Si5 C19 113.82(8) . . ?
C13 Si5 C19 114.93(8) . . ?
C14 Si5 C19 111.25(8) . . ?
C17 Si6 C16 108.64(9) . . ?
C17 Si6 C18 101.64(9) . . ?
C16 Si6 C18 108.16(9) . . ?
C17 Si6 C19 114.08(8) . . ?
C16 Si6 C19 112.34(8) . . ?
C18 Si6 C19 111.33(8) . . ?
C20 C19 Si6 106.85(11) . . ?
C20 C19 Si5 108.39(11) . . ?
Si6 C19 Si5 107.33(8) . . ?
C20 C19 Si3 101.07(11) . . ?
Si6 C19 Si3 118.48(9) . . ?
Si5 C19 Si3 113.98(9) . . ?
C21 C20 C19 111.38(14) . . ?
C20 C21 C22 110.87(14) . . ?
C21 C22 Si7 109.60(12) . . ?
C21 C22 Si8 108.64(11) . . ?
Si7 C22 Si8 107.05(8) . . ?
C21 C22 Si3 101.13(11) . . ?
Si7 C22 Si3 114.68(9) . . ?
Si8 C22 Si3 115.44(9) . . ?
C23 Si7 C25 105.44(9) . . ?
C23 Si7 C24 102.63(9) . . ?
C25 Si7 C24 108.47(9) . . ?
C23 Si7 C22 115.62(8) . . ?
C25 Si7 C22 112.83(8) . . ?
C24 Si7 C22 111.11(9) . . ?
C28 Si8 C27 107.65(9) . . ?
C28 Si8 C26 102.00(9) . . ?
C27 Si8 C26 107.16(9) . . ?
C28 Si8 C22 113.67(8) . . ?
C27 Si8 C22 113.12(8) . . ?
C26 Si8 C22 112.44(8) . . ?
C30 Si9 C29 104.04(9) . . ?
C30 Si9 C31 112.19(9) . . ?
C29 Si9 C31 103.37(9) . . ?
C30 Si9 C35 112.46(9) . . ?
C29 Si9 C35 114.21(8) . . ?
C31 Si9 C35 110.15(9) . . ?
C34 Si10 C33 104.44(10) . . ?
C34 Si10 C32 103.58(9) . . ?
C33 Si10 C32 106.34(9) . . ?
C34 Si10 C35 116.39(8) . . ?
C33 Si10 C35 115.55(9) . . ?
C32 Si10 C35 109.46(8) . . ?
C36 C35 Si9 110.02(12) . . ?
C36 C35 Si10 107.16(11) . . ?
Si9 C35 Si10 108.00(9) . . ?
C36 C35 Si4 100.13(11) . . ?
Si9 C35 Si4 115.54(9) . . ?
Si10 C35 Si4 115.40(9) . . ?
C37 C36 C35 109.01(14) . . ?
C36 C37 C38 108.49(14) . . ?
C37 C38 Si11 110.36(12) . . ?
C37 C38 Si12 107.79(11) . . ?
Si11 C38 Si12 108.49(9) . . ?
C37 C38 Si4 100.49(11) . . ?
Si11 C38 Si4 115.12(9) . . ?
Si12 C38 Si4 114.12(9) . . ?
C41 Si11 C43 105.11(9) . . ?
C41 Si11 C44 105.66(10) . . ?
C43 Si11 C44 106.59(10) . . ?
C41 Si11 C38 113.17(9) . . ?
C43 Si11 C38 110.26(9) . . ?
C44 Si11 C38 115.34(8) . . ?
C46 N1 C45 116.56(15) . . ?
C46 N1 Si1 120.91(12) . . ?
C45 N1 Si1 122.52(12) . . ?
C48 C45 N1 123.61(17) . . ?
N1 C46 C47 123.39(17) . . ?
C46 C47 C49 120.33(17) . . ?
C45 C48 C49 120.37(17) . . ?
N2 C49 C48 121.64(17) . . ?
N2 C49 C47 122.84(17) . . ?
C48 C49 C47 115.52(16) . . ?
C49 N2 C50 121.16(17) . . ?
C49 N2 C51 120.60(16) . . ?
C50 N2 C51 117.72(16) . . ?
C40 Si12 C39 103.94(9) . . ?
C40 Si12 C42 107.07(9) . . ?
C39 Si12 C42 104.89(9) . . ?
C40 Si12 C38 113.59(9) . . ?
C39 Si12 C38 116.65(8) . . ?
C42 Si12 C38 109.91(8) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C6A C1 C2A C3A -5.7(5) . . . . ?
C1 C2A C3A C4A 2.5(6) . . . . ?
C2A C3A C4A C5A 1.2(8) . . . . ?
C3A C4A C5A C6A -2.0(9) . . . . ?
C4A C5A C6A C1 -0.9(8) . . . . ?
C2A C1 C6A C5A 4.9(6) . . . . ?
C6B C1 C2B C3B 16.8(16) . . . . ?
C1 C2B C3B C4B -3(3) . . . . ?
C2B C3B C4B C5B -5(3) . . . . ?
C3B C4B C5B C6B 1.4(19) . . . . ?
C2B C1 C6B C5B -23.0(13) . . . . ?
C4B C5B C6B C1 14.4(16) . . . . ?
C9 C7 C8 C10 0.7(4) . . . . ?
C8 C7 C9 C11 -0.1(4) . . . . ?
C7 C8 C10 C12 -0.8(4) . . . . ?
C7 C9 C11 C12 -0.3(4) . . . . ?
C9 C11 C12 C10 0.2(4) . . . . ?
C8 C10 C12 C11 0.4(4) . . . . ?
Si6 C19 C20 C21 156.99(12) . . . . ?
Si5 C19 C20 C21 -87.63(15) . . . . ?
Si3 C19 C20 C21 32.46(16) . . . . ?
C19 C20 C21 C22 -47.56(19) . . . . ?
C20 C21 C22 Si7 -86.52(15) . . . . ?
C20 C21 C22 Si8 156.83(12) . . . . ?
C20 C21 C22 Si3 34.94(16) . . . . ?
C30 Si9 C35 C36 -169.14(12) . . . . ?
C29 Si9 C35 C36 -50.87(14) . . . . ?
C31 Si9 C35 C36 64.92(14) . . . . ?
C30 Si9 C35 Si10 74.21(11) . . . . ?
C29 Si9 C35 Si10 -167.52(9) . . . . ?
C31 Si9 C35 Si10 -51.73(11) . . . . ?
C30 Si9 C35 Si4 -56.72(12) . . . . ?
C29 Si9 C35 Si4 61.56(12) . . . . ?
C31 Si9 C35 Si4 177.34(10) . . . . ?
Si9 C35 C36 C37 161.87(12) . . . . ?
Si10 C35 C36 C37 -80.95(14) . . . . ?
Si4 C35 C36 C37 39.79(15) . . . . ?
C35 C36 C37 C38 -56.81(18) . . . . ?
C36 C37 C38 Si11 162.70(12) . . . . ?
C36 C37 C38 Si12 -78.98(15) . . . . ?
C36 C37 C38 Si4 40.74(15) . . . . ?
C37 C38 Si11 C41 -52.12(14) . . . . ?
Si12 C38 Si11 C41 -170.01(9) . . . . ?
Si4 C38 Si11 C41 60.74(12) . . . . ?
C37 C38 Si11 C43 65.28(14) . . . . ?
Si12 C38 Si11 C43 -52.61(11) . . . . ?
Si4 C38 Si11 C43 178.14(9) . . . . ?
C37 C38 Si11 C44 -173.95(12) . . . . ?
Si12 C38 Si11 C44 68.16(11) . . . . ?
Si4 C38 Si11 C44 -61.09(12) . . . . ?
Cl1 Si1 N1 C46 -141.69(13) . . . . ?
Si2 Si1 N1 C46 4.05(16) . . . . ?
Si4 Si1 N1 C46 87.34(15) . . . . ?
Cl1 Si1 N1 C45 39.45(14) . . . . ?
Si2 Si1 N1 C45 -174.81(12) . . . . ?
Si4 Si1 N1 C45 -91.52(15) . . . . ?
C46 N1 C45 C48 2.2(3) . . . . ?
Si1 N1 C45 C48 -178.89(15) . . . . ?
C45 N1 C46 C47 -3.1(3) . . . . ?
Si1 N1 C46 C47 177.94(15) . . . . ?
N1 C46 C47 C49 -0.1(3) . . . . ?
N1 C45 C48 C49 1.9(3) . . . . ?
C45 C48 C49 N2 174.37(19) . . . . ?
C45 C48 C49 C47 -5.0(3) . . . . ?
C46 C47 C49 N2 -175.24(19) . . . . ?
C46 C47 C49 C48 4.1(3) . . . . ?
C48 C49 N2 C50 0.6(3) . . . . ?
C47 C49 N2 C50 179.89(19) . . . . ?
C48 C49 N2 C51 -170.89(19) . . . . ?
C47 C49 N2 C51 8.4(3) . . . . ?

_refine_diff_density_max         0.448
_refine_diff_density_min         -0.330
_refine_diff_density_rms         0.060


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