# Supplementary Information (SI) for Organic & Biomolecular Chemistry.
# This journal is © The Royal Society of Chemistry 2024

####################################################################### 
# 
# 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_2a
_database_code_depnum_ccdc_archive 'CCDC 2367922'
loop_
_audit_author_name
_audit_author_address
'Wataru Setaka'
;Tokyo Metropolitan University
Japan
;
_audit_update_record             
;
2024-08-05 deposited with the CCDC.	2024-08-08 downloaded from the CCDC.
;

# start Validation Reply Form
_vrf_PLAT049_2a                  
;
PROBLEM: Calculated Density Less Than 1.0 gcm-3 .........     0.9776 Check 
RESPONSE: This is caused by some void spaces in the crystal.
;
# end Validation Reply Form

_audit_creation_method           SHELXL-2018/3
_chemical_name_systematic        tricycloalkane
_chemical_name_common            2a
_chemical_melting_point          '323-325 K'
_chemical_formula_moiety         'C64 H132 Si4'
_chemical_formula_sum            'C64 H132 Si4'
_chemical_formula_weight         1014.05

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.2541 0.3302 '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                   10.0201(10)
_cell_length_b                   13.7449(13)
_cell_length_c                   13.8357(13)
_cell_angle_alpha                114.915(6)
_cell_angle_beta                 92.110(5)
_cell_angle_gamma                92.923(5)
_cell_volume                     1722.4(3)
_cell_formula_units_Z            1
_cell_measurement_temperature    250(2)
_cell_measurement_reflns_used    4601
_cell_measurement_theta_min      5.7702
_cell_measurement_theta_max      68.4797

_exptl_crystal_description       prism
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    0.978
_exptl_crystal_F_000             572
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.240
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.120
_exptl_absorpt_coefficient_mu    1.029
_shelx_estimated_absorpt_T_min   0.790
_shelx_estimated_absorpt_T_max   0.886
_exptl_absorpt_correction_type   Multi-Scan
_exptl_absorpt_process_details   
;
Krause, L., Herbst-Irmer, R., Sheldrick, G. M., Stalke, D. (2015).
"Comparison of silver and molybdenum microfocus X-ray sources for
single-crystal structure determination"
J. Appl. Cryst. 48, 3-10.
doi:10.1107/S1600576714022985
;
_exptl_absorpt_correction_T_min  0.73
_exptl_absorpt_correction_T_max  0.95


_diffrn_ambient_temperature      250(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_source                   'sealed tube'
_diffrn_radiation_monochromator  'multilayered conforcal mirror'
_diffrn_measurement_device       ?
_diffrn_measurement_device_type  'Bruker D8 goniometer'
_diffrn_measurement_method       'omega scans'

_diffrn_detector_area_resol_mean 7.3910
_diffrn_reflns_number            32186
_diffrn_reflns_av_unetI/netI     0.0481
_diffrn_reflns_av_R_equivalents  0.0579
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         3.802
_diffrn_reflns_theta_max         73.085
_diffrn_reflns_theta_full        67.679
_diffrn_measured_fraction_theta_max 0.956
_diffrn_measured_fraction_theta_full 0.975
_diffrn_reflns_Laue_measured_fraction_max 0.956
_diffrn_reflns_Laue_measured_fraction_full 0.975
_diffrn_reflns_point_group_measured_fraction_max 0.956
_diffrn_reflns_point_group_measured_fraction_full 0.975
_reflns_number_total             6601
_reflns_number_gt                4906
_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 Instrument Service vV6.2.16'
_computing_cell_refinement       'SAINT V8.40B (Bruker AXS LLC, 2019)'
_computing_data_reduction        'SAINT V8.40B (Bruker AXS LLC, 2019)'
_computing_structure_solution    'Sir-2019 (IUCr, 2019)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 2020)'
_computing_publication_material  'WinGX (Farrugia, 2020)'


_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)+(0.0870P)²+1.1586P] 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         6601
_refine_ls_number_parameters     307
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1002
_refine_ls_R_factor_gt           0.0731
_refine_ls_wR_factor_ref         0.2109
_refine_ls_wR_factor_gt          0.1837
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_restrained_S_all      1.041
_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 0.25191(8) 0.40219(6) 0.28730(7) 0.0589(2) Uani 1 1 d . . . . .
Si2 Si 0.83338(8) -0.37803(6) 0.19950(7) 0.0632(3) Uani 1 1 d . . . . .
C1 C 0.4136(3) 0.3872(3) 0.3507(3) 0.0653(7) Uani 1 1 d . . . . .
H1A H 0.425799 0.444488 0.423394 0.078 Uiso 1 1 calc R U . . .
H1B H 0.407164 0.318361 0.356113 0.078 Uiso 1 1 calc R U . . .
C2 C 0.5368(3) 0.3917(3) 0.2908(3) 0.0794(10) Uani 1 1 d . . . . .
H2A H 0.514734 0.349425 0.214176 0.095 Uiso 1 1 calc R U . . .
H2B H 0.557463 0.466438 0.302433 0.095 Uiso 1 1 calc R U . . .
C3 C 0.6621(3) 0.3505(3) 0.3222(3) 0.0761(9) Uani 1 1 d . . . . .
H3A H 0.738776 0.368325 0.289218 0.091 Uiso 1 1 calc R U . . .
H3B H 0.679748 0.387166 0.399865 0.091 Uiso 1 1 calc R U . . .
C4 C 0.6492(3) 0.2306(3) 0.2886(3) 0.0728(8) Uani 1 1 d . . . . .
H4A H 0.617895 0.195086 0.213014 0.087 Uiso 1 1 calc R U . . .
H4B H 0.580536 0.214569 0.329487 0.087 Uiso 1 1 calc R U . . .
C5 C 0.7780(3) 0.1826(3) 0.3038(3) 0.0698(8) Uani 1 1 d . . . . .
H5A H 0.847589 0.199210 0.263975 0.084 Uiso 1 1 calc R U . . .
H5B H 0.808486 0.216191 0.379624 0.084 Uiso 1 1 calc R U . . .
C6 C 0.7601(3) 0.0630(3) 0.2669(3) 0.0707(8) Uani 1 1 d . . . . .
H6A H 0.723086 0.030961 0.192685 0.085 Uiso 1 1 calc R U . . .
H6B H 0.693625 0.047763 0.309836 0.085 Uiso 1 1 calc R U . . .
C7 C 0.8844(3) 0.0078(3) 0.2728(3) 0.0772(9) Uani 1 1 d . . . . .
H7A H 0.916390 0.032858 0.347766 0.093 Uiso 1 1 calc R U . . .
H7B H 0.954700 0.027854 0.235764 0.093 Uiso 1 1 calc R U . . .
C8 C 0.8594(3) -0.1146(3) 0.2228(3) 0.0724(8) Uani 1 1 d . . . . .
H8A H 0.789500 -0.133839 0.260733 0.087 Uiso 1 1 calc R U . . .
H8B H 0.825151 -0.138652 0.148515 0.087 Uiso 1 1 calc R U . . .
C9 C 0.9801(3) -0.1746(3) 0.2245(4) 0.0787(9) Uani 1 1 d . . . . .
H9A H 1.006033 -0.159496 0.298733 0.094 Uiso 1 1 calc R U . . .
H9B H 1.054622 -0.147470 0.196523 0.094 Uiso 1 1 calc R U . . .
C10 C 0.9581(3) -0.2965(3) 0.1595(3) 0.0766(9) Uani 1 1 d . . . . .
H10A H 1.045030 -0.326473 0.158091 0.092 Uiso 1 1 calc R U . . .
H10B H 0.932000 -0.309425 0.085864 0.092 Uiso 1 1 calc R U . . .
C11 C 0.6567(3) -0.3518(2) 0.1736(2) 0.0580(6) Uani 1 1 d . . . . .
H11A H 0.595484 -0.398867 0.191390 0.070 Uiso 1 1 calc R U . . .
H11B H 0.641665 -0.277275 0.221403 0.070 Uiso 1 1 calc R U . . .
C12 C 0.6221(3) -0.3695(2) 0.0592(2) 0.0635(7) Uani 1 1 d . . . . .
H12A H 0.624781 -0.446234 0.012645 0.076 Uiso 1 1 calc R U . . .
H12B H 0.691298 -0.330578 0.038117 0.076 Uiso 1 1 calc R U . . .
C13 C 0.4852(3) -0.3337(2) 0.0396(2) 0.0622(7) Uani 1 1 d . . . . .
H13A H 0.459973 -0.368525 -0.037187 0.075 Uiso 1 1 calc R U . . .
H13B H 0.418418 -0.358820 0.075533 0.075 Uiso 1 1 calc R U . . .
C14 C 0.4804(3) -0.2131(2) 0.0781(3) 0.0625(7) Uani 1 1 d . . . . .
H14A H 0.548724 -0.187361 0.043780 0.075 Uiso 1 1 calc R U . . .
H14B H 0.502460 -0.178157 0.155304 0.075 Uiso 1 1 calc R U . . .
C15 C 0.3452(3) -0.1801(2) 0.0547(3) 0.0614(7) Uani 1 1 d . . . . .
H15A H 0.317803 -0.223215 -0.020880 0.074 Uiso 1 1 calc R U . . .
H15B H 0.279448 -0.197738 0.096728 0.074 Uiso 1 1 calc R U . . .
C16 C 0.3402(3) -0.0624(2) 0.0783(3) 0.0658(7) Uani 1 1 d . . . . .
H16A H 0.405969 -0.043999 0.036858 0.079 Uiso 1 1 calc R U . . .
H16B H 0.365592 -0.018732 0.154188 0.079 Uiso 1 1 calc R U . . .
C17 C 0.2026(3) -0.0343(3) 0.0521(3) 0.0739(9) Uani 1 1 d . . . . .
H17A H 0.170060 -0.088195 -0.019012 0.089 Uiso 1 1 calc R U . . .
H17B H 0.141211 -0.039996 0.103230 0.089 Uiso 1 1 calc R U . . .
C18 C 0.1954(4) 0.0762(3) 0.0534(3) 0.0748(9) Uani 1 1 d . . . . .
H18A H 0.260528 0.083710 0.005353 0.090 Uiso 1 1 calc R U . . .
H18B H 0.106197 0.080487 0.024625 0.090 Uiso 1 1 calc R U . . .
C19 C 0.2220(4) 0.1698(3) 0.1618(3) 0.0752(9) Uani 1 1 d . . . . .
H19A H 0.311189 0.166162 0.191102 0.090 Uiso 1 1 calc R U . . .
H19B H 0.156450 0.163444 0.210080 0.090 Uiso 1 1 calc R U . . .
C20 C 0.2143(4) 0.2805(3) 0.1584(3) 0.0717(8) Uani 1 1 d . . . . .
H20A H 0.123905 0.283892 0.130854 0.086 Uiso 1 1 calc R U . . .
H20B H 0.276736 0.284294 0.107000 0.086 Uiso 1 1 calc R U . . .
C21 C 0.2703(3) 0.5227(2) 0.2572(3) 0.0640(7) Uani 1 1 d . . . . .
H21A H 0.346965 0.514797 0.213164 0.077 Uiso 1 1 calc R U . . .
H21B H 0.190320 0.522707 0.214275 0.077 Uiso 1 1 calc R U . . .
C22 C 0.2899(3) 0.6319(2) 0.3532(3) 0.0661(7) Uani 1 1 d . . . . .
H22A H 0.211371 0.642206 0.395651 0.079 Uiso 1 1 calc R U . . .
H22B H 0.367822 0.631692 0.398054 0.079 Uiso 1 1 calc R U . . .
C23 C 0.3105(3) 0.7262(2) 0.3241(3) 0.0658(7) Uani 1 1 d . . . . .
H23A H 0.398614 0.723822 0.295049 0.079 Uiso 1 1 calc R U . . .
H23B H 0.242997 0.717554 0.267386 0.079 Uiso 1 1 calc R U . . .
C24 C 0.3019(4) 0.8349(3) 0.4150(3) 0.0718(8) Uani 1 1 d . . . . .
H24A H 0.369018 0.843531 0.471902 0.086 Uiso 1 1 calc R U . . .
H24B H 0.213498 0.837597 0.443755 0.086 Uiso 1 1 calc R U . . .
C25 C 0.3234(3) 0.9285(3) 0.3848(3) 0.0701(8) Uani 1 1 d . . . . .
H25A H 0.416632 0.932876 0.366897 0.084 Uiso 1 1 calc R U . . .
H25B H 0.265943 0.914477 0.320781 0.084 Uiso 1 1 calc R U . . .
C26 C 0.2936(4) 1.0361(3) 0.4725(3) 0.0779(9) Uani 1 1 d . . . . .
H26A H 0.201533 1.030596 0.492235 0.094 Uiso 1 1 calc R U . . .
H26B H 0.353423 1.051075 0.535585 0.094 Uiso 1 1 calc R U . . .
C27 C 0.3098(4) 1.1298(3) 0.4423(3) 0.0810(10) Uani 1 1 d . . . . .
H27A H 0.245178 1.117726 0.382712 0.097 Uiso 1 1 calc R U . . .
H27B H 0.399826 1.132466 0.417706 0.097 Uiso 1 1 calc R U . . .
C28 C 0.2887(4) 1.2396(3) 0.5358(3) 0.0809(10) Uani 1 1 d . . . . .
H28A H 0.347398 1.248374 0.597613 0.097 Uiso 1 1 calc R U . . .
H28B H 0.315491 1.297248 0.514927 0.097 Uiso 1 1 calc R U . . .
C29 C 0.8511(4) -0.2512(3) 0.4324(3) 0.0845(10) Uani 1 1 d . . . . .
H29A H 0.909514 -0.242979 0.494106 0.101 Uiso 1 1 calc R U . . .
H29B H 0.878031 -0.192956 0.412341 0.101 Uiso 1 1 calc R U . . .
C30 C 0.8724(4) -0.3582(3) 0.3400(3) 0.0786(9) Uani 1 1 d . . . . .
H30A H 0.818964 -0.413998 0.350912 0.094 Uiso 1 1 calc R U . . .
H30B H 0.966596 -0.372109 0.345888 0.094 Uiso 1 1 calc R U . . .
C31 C 0.1142(3) 0.4159(3) 0.3786(3) 0.0810(10) Uani 1 1 d . . . . .
H31A H 0.134689 0.479198 0.445163 0.122 Uiso 1 1 calc R U . . .
H31B H 0.030687 0.422978 0.345135 0.122 Uiso 1 1 calc R U . . .
H31C H 0.105588 0.352580 0.392778 0.122 Uiso 1 1 calc R U . . .
C32 C 0.8597(4) -0.5230(3) 0.1125(4) 0.0911(11) Uani 1 1 d . . . . .
H32A H 0.840662 -0.537626 0.038158 0.137 Uiso 1 1 calc R U . . .
H32B H 0.951858 -0.536805 0.122947 0.137 Uiso 1 1 calc R U . . .
H32C H 0.800197 -0.569174 0.131410 0.137 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 C31 1.868(3) . ?
Si1 C20 1.869(3) . ?
Si1 C21 1.873(3) . ?
Si1 C1 1.875(3) . ?
Si2 C30 1.868(4) . ?
Si2 C11 1.877(3) . ?
Si2 C32 1.883(4) . ?
Si2 C10 1.885(3) . ?
C1 C2 1.525(4) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C2 C3 1.525(4) . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C3 C4 1.508(5) . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C4 C5 1.526(4) . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C5 C6 1.500(4) . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C6 C7 1.508(4) . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C7 C8 1.529(5) . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C8 C9 1.503(4) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C9 C10 1.532(5) . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C11 C12 1.521(4) . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C12 C13 1.533(4) . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C13 C14 1.516(4) . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C14 C15 1.517(4) . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C15 C16 1.514(4) . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C16 C17 1.523(4) . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C17 C18 1.516(4) . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C18 C19 1.513(5) . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C19 C20 1.548(4) . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C21 C22 1.525(5) . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C22 C23 1.517(4) . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C23 C24 1.503(5) . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C24 C25 1.520(4) . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C25 C26 1.519(5) . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C26 C27 1.516(4) . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C27 C28 1.550(5) . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C28 C29 1.480(5) 2_666 ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C29 C30 1.520(5) . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C31 H31A 0.9700 . ?
C31 H31B 0.9700 . ?
C31 H31C 0.9700 . ?
C32 H32A 0.9700 . ?
C32 H32B 0.9700 . ?
C32 H32C 0.9700 . ?

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
C31 Si1 C20 110.15(18) . . ?
C31 Si1 C21 110.61(15) . . ?
C20 Si1 C21 108.18(15) . . ?
C31 Si1 C1 109.84(16) . . ?
C20 Si1 C1 108.56(15) . . ?
C21 Si1 C1 109.47(14) . . ?
C30 Si2 C11 113.44(15) . . ?
C30 Si2 C32 106.13(18) . . ?
C11 Si2 C32 108.70(16) . . ?
C30 Si2 C10 110.91(18) . . ?
C11 Si2 C10 111.52(14) . . ?
C32 Si2 C10 105.68(18) . . ?
C2 C1 Si1 114.5(2) . . ?
C2 C1 H1A 108.6 . . ?
Si1 C1 H1A 108.6 . . ?
C2 C1 H1B 108.6 . . ?
Si1 C1 H1B 108.6 . . ?
H1A C1 H1B 107.6 . . ?
C3 C2 C1 115.3(3) . . ?
C3 C2 H2A 108.4 . . ?
C1 C2 H2A 108.4 . . ?
C3 C2 H2B 108.4 . . ?
C1 C2 H2B 108.4 . . ?
H2A C2 H2B 107.5 . . ?
C4 C3 C2 112.6(3) . . ?
C4 C3 H3A 109.1 . . ?
C2 C3 H3A 109.1 . . ?
C4 C3 H3B 109.1 . . ?
C2 C3 H3B 109.1 . . ?
H3A C3 H3B 107.8 . . ?
C3 C4 C5 114.8(3) . . ?
C3 C4 H4A 108.6 . . ?
C5 C4 H4A 108.6 . . ?
C3 C4 H4B 108.6 . . ?
C5 C4 H4B 108.6 . . ?
H4A C4 H4B 107.5 . . ?
C6 C5 C4 112.5(3) . . ?
C6 C5 H5A 109.1 . . ?
C4 C5 H5A 109.1 . . ?
C6 C5 H5B 109.1 . . ?
C4 C5 H5B 109.1 . . ?
H5A C5 H5B 107.8 . . ?
C5 C6 C7 116.1(3) . . ?
C5 C6 H6A 108.2 . . ?
C7 C6 H6A 108.2 . . ?
C5 C6 H6B 108.2 . . ?
C7 C6 H6B 108.2 . . ?
H6A C6 H6B 107.4 . . ?
C6 C7 C8 112.3(3) . . ?
C6 C7 H7A 109.1 . . ?
C8 C7 H7A 109.1 . . ?
C6 C7 H7B 109.1 . . ?
C8 C7 H7B 109.1 . . ?
H7A C7 H7B 107.9 . . ?
C9 C8 C7 114.9(3) . . ?
C9 C8 H8A 108.5 . . ?
C7 C8 H8A 108.5 . . ?
C9 C8 H8B 108.5 . . ?
C7 C8 H8B 108.5 . . ?
H8A C8 H8B 107.5 . . ?
C8 C9 C10 113.9(3) . . ?
C8 C9 H9A 108.8 . . ?
C10 C9 H9A 108.8 . . ?
C8 C9 H9B 108.8 . . ?
C10 C9 H9B 108.8 . . ?
H9A C9 H9B 107.7 . . ?
C9 C10 Si2 120.5(3) . . ?
C9 C10 H10A 107.2 . . ?
Si2 C10 H10A 107.2 . . ?
C9 C10 H10B 107.2 . . ?
Si2 C10 H10B 107.2 . . ?
H10A C10 H10B 106.8 . . ?
C12 C11 Si2 114.3(2) . . ?
C12 C11 H11A 108.7 . . ?
Si2 C11 H11A 108.7 . . ?
C12 C11 H11B 108.7 . . ?
Si2 C11 H11B 108.7 . . ?
H11A C11 H11B 107.6 . . ?
C11 C12 C13 115.2(2) . . ?
C11 C12 H12A 108.5 . . ?
C13 C12 H12A 108.5 . . ?
C11 C12 H12B 108.5 . . ?
C13 C12 H12B 108.5 . . ?
H12A C12 H12B 107.5 . . ?
C14 C13 C12 114.4(2) . . ?
C14 C13 H13A 108.7 . . ?
C12 C13 H13A 108.7 . . ?
C14 C13 H13B 108.7 . . ?
C12 C13 H13B 108.7 . . ?
H13A C13 H13B 107.6 . . ?
C13 C14 C15 113.3(2) . . ?
C13 C14 H14A 108.9 . . ?
C15 C14 H14A 108.9 . . ?
C13 C14 H14B 108.9 . . ?
C15 C14 H14B 108.9 . . ?
H14A C14 H14B 107.7 . . ?
C16 C15 C14 115.3(2) . . ?
C16 C15 H15A 108.4 . . ?
C14 C15 H15A 108.4 . . ?
C16 C15 H15B 108.4 . . ?
C14 C15 H15B 108.4 . . ?
H15A C15 H15B 107.5 . . ?
C15 C16 C17 113.0(3) . . ?
C15 C16 H16A 109.0 . . ?
C17 C16 H16A 109.0 . . ?
C15 C16 H16B 109.0 . . ?
C17 C16 H16B 109.0 . . ?
H16A C16 H16B 107.8 . . ?
C18 C17 C16 116.2(3) . . ?
C18 C17 H17A 108.2 . . ?
C16 C17 H17A 108.2 . . ?
C18 C17 H17B 108.2 . . ?
C16 C17 H17B 108.2 . . ?
H17A C17 H17B 107.4 . . ?
C19 C18 C17 115.3(3) . . ?
C19 C18 H18A 108.4 . . ?
C17 C18 H18A 108.4 . . ?
C19 C18 H18B 108.4 . . ?
C17 C18 H18B 108.4 . . ?
H18A C18 H18B 107.5 . . ?
C18 C19 C20 113.1(3) . . ?
C18 C19 H19A 109.0 . . ?
C20 C19 H19A 109.0 . . ?
C18 C19 H19B 109.0 . . ?
C20 C19 H19B 109.0 . . ?
H19A C19 H19B 107.8 . . ?
C19 C20 Si1 116.8(2) . . ?
C19 C20 H20A 108.1 . . ?
Si1 C20 H20A 108.1 . . ?
C19 C20 H20B 108.1 . . ?
Si1 C20 H20B 108.1 . . ?
H20A C20 H20B 107.3 . . ?
C22 C21 Si1 116.4(2) . . ?
C22 C21 H21A 108.2 . . ?
Si1 C21 H21A 108.2 . . ?
C22 C21 H21B 108.2 . . ?
Si1 C21 H21B 108.2 . . ?
H21A C21 H21B 107.3 . . ?
C23 C22 C21 114.1(3) . . ?
C23 C22 H22A 108.7 . . ?
C21 C22 H22A 108.7 . . ?
C23 C22 H22B 108.7 . . ?
C21 C22 H22B 108.7 . . ?
H22A C22 H22B 107.6 . . ?
C24 C23 C22 114.8(3) . . ?
C24 C23 H23A 108.6 . . ?
C22 C23 H23A 108.6 . . ?
C24 C23 H23B 108.6 . . ?
C22 C23 H23B 108.6 . . ?
H23A C23 H23B 107.5 . . ?
C23 C24 C25 114.2(3) . . ?
C23 C24 H24A 108.7 . . ?
C25 C24 H24A 108.7 . . ?
C23 C24 H24B 108.7 . . ?
C25 C24 H24B 108.7 . . ?
H24A C24 H24B 107.6 . . ?
C26 C25 C24 113.5(3) . . ?
C26 C25 H25A 108.9 . . ?
C24 C25 H25A 108.9 . . ?
C26 C25 H25B 108.9 . . ?
C24 C25 H25B 108.9 . . ?
H25A C25 H25B 107.7 . . ?
C27 C26 C25 114.2(3) . . ?
C27 C26 H26A 108.7 . . ?
C25 C26 H26A 108.7 . . ?
C27 C26 H26B 108.7 . . ?
C25 C26 H26B 108.7 . . ?
H26A C26 H26B 107.6 . . ?
C26 C27 C28 113.1(3) . . ?
C26 C27 H27A 109.0 . . ?
C28 C27 H27A 109.0 . . ?
C26 C27 H27B 109.0 . . ?
C28 C27 H27B 109.0 . . ?
H27A C27 H27B 107.8 . . ?
C29 C28 C27 113.6(3) 2_666 . ?
C29 C28 H28A 108.8 2_666 . ?
C27 C28 H28A 108.8 . . ?
C29 C28 H28B 108.8 2_666 . ?
C27 C28 H28B 108.8 . . ?
H28A C28 H28B 107.7 . . ?
C28 C29 C30 114.0(3) 2_666 . ?
C28 C29 H29A 108.8 2_666 . ?
C30 C29 H29A 108.8 . . ?
C28 C29 H29B 108.8 2_666 . ?
C30 C29 H29B 108.8 . . ?
H29A C29 H29B 107.7 . . ?
C29 C30 Si2 120.0(2) . . ?
C29 C30 H30A 107.3 . . ?
Si2 C30 H30A 107.3 . . ?
C29 C30 H30B 107.3 . . ?
Si2 C30 H30B 107.3 . . ?
H30A C30 H30B 106.9 . . ?
Si1 C31 H31A 109.5 . . ?
Si1 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
Si1 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
Si2 C32 H32A 109.5 . . ?
Si2 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
Si2 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 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
C31 Si1 C1 C2 -171.6(3) . . . . ?
C20 Si1 C1 C2 67.9(3) . . . . ?
C21 Si1 C1 C2 -50.0(3) . . . . ?
Si1 C1 C2 C3 -164.3(3) . . . . ?
C1 C2 C3 C4 68.7(4) . . . . ?
C2 C3 C4 C5 171.8(3) . . . . ?
C3 C4 C5 C6 -178.7(3) . . . . ?
C4 C5 C6 C7 176.4(3) . . . . ?
C5 C6 C7 C8 -174.0(3) . . . . ?
C6 C7 C8 C9 179.0(3) . . . . ?
C7 C8 C9 C10 -171.3(3) . . . . ?
C8 C9 C10 Si2 -64.5(4) . . . . ?
C30 Si2 C10 C9 -56.5(3) . . . . ?
C11 Si2 C10 C9 70.9(3) . . . . ?
C32 Si2 C10 C9 -171.1(3) . . . . ?
C30 Si2 C11 C12 -178.9(2) . . . . ?
C32 Si2 C11 C12 -61.1(3) . . . . ?
C10 Si2 C11 C12 55.0(3) . . . . ?
Si2 C11 C12 C13 -171.9(2) . . . . ?
C11 C12 C13 C14 76.5(3) . . . . ?
C12 C13 C14 C15 178.2(2) . . . . ?
C13 C14 C15 C16 -172.3(3) . . . . ?
C14 C15 C16 C17 179.3(3) . . . . ?
C15 C16 C17 C18 -168.8(3) . . . . ?
C16 C17 C18 C19 -67.0(4) . . . . ?
C17 C18 C19 C20 179.6(3) . . . . ?
C18 C19 C20 Si1 -177.7(3) . . . . ?
C31 Si1 C20 C19 -70.4(3) . . . . ?
C21 Si1 C20 C19 168.6(3) . . . . ?
C1 Si1 C20 C19 49.9(3) . . . . ?
C31 Si1 C21 C22 54.4(3) . . . . ?
C20 Si1 C21 C22 175.1(2) . . . . ?
C1 Si1 C21 C22 -66.8(3) . . . . ?
Si1 C21 C22 C23 177.4(2) . . . . ?
C21 C22 C23 C24 168.1(3) . . . . ?
C22 C23 C24 C25 179.7(3) . . . . ?
C23 C24 C25 C26 171.2(3) . . . . ?
C24 C25 C26 C27 -177.9(3) . . . . ?
C25 C26 C27 C28 -175.9(3) . . . . ?
C26 C27 C28 C29 -68.2(4) . . . 2_666 ?
C28 C29 C30 Si2 82.6(4) 2_666 . . . ?
C11 Si2 C30 C29 -56.1(3) . . . . ?
C32 Si2 C30 C29 -175.4(3) . . . . ?
C10 Si2 C30 C29 70.3(3) . . . . ?

_refine_diff_density_max         0.658
_refine_diff_density_min         -0.339
_refine_diff_density_rms         0.048


_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_chemical_compound_source        no
####################################################################### 
# 
# 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_trans3
_database_code_depnum_ccdc_archive 'CCDC 2369099'
loop_
_audit_author_name
_audit_author_address
'Wataru Setaka'
;Tokyo Metropolitan University
Japan
;
_audit_update_record             
;
2024-07-09 deposited with the CCDC.	2024-08-08 downloaded from the CCDC.
;


_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        trans-difluorodimethyldisilacyclodocosane
_chemical_name_common            trans-3
_chemical_melting_point          ?
_chemical_formula_moiety         'C22 H46 F2 Si2'
_chemical_formula_sum            'C22 H46 F2 Si2'
_chemical_formula_weight         404.77

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.2541 0.3302 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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                   5.8392(2)
_cell_length_b                   10.0661(3)
_cell_length_c                   11.6107(4)
_cell_angle_alpha                88.9020(10)
_cell_angle_beta                 75.5770(10)
_cell_angle_gamma                78.9050(10)
_cell_volume                     648.29(4)
_cell_formula_units_Z            1
_cell_measurement_temperature    300(2)
_cell_measurement_reflns_used    8476
_cell_measurement_theta_min      3.9330
_cell_measurement_theta_max      72.3058

_exptl_crystal_description       prism
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.037
_exptl_crystal_F_000             224
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.940
_exptl_crystal_size_mid          0.220
_exptl_crystal_size_min          0.150
_exptl_absorpt_coefficient_mu    1.380
_shelx_estimated_absorpt_T_min   0.357
_shelx_estimated_absorpt_T_max   0.820


_exptl_absorpt_correction_type   Multi-Scan
_exptl_absorpt_process_details   
;
Krause, L., Herbst-Irmer, R., Sheldrick, G. M., Stalke, D. (2015).
"Comparison of silver and molybdenum microfocus X-ray sources for
single-crystal structure determination"
J. Appl. Cryst. 48, 3-10.
doi:10.1107/S1600576714022985
;
_exptl_absorpt_correction_T_min  0.59
_exptl_absorpt_correction_T_max  0.82


_diffrn_ambient_temperature      300(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_source                   'sealed tube'
_diffrn_radiation_monochromator  'multilayered conforcal mirror'
_diffrn_measurement_device       ?
_diffrn_measurement_device_type  'Bruker D8 goniometer'
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean 7.3910
_diffrn_reflns_number            9532
_diffrn_reflns_av_unetI/netI     0.0269
_diffrn_reflns_av_R_equivalents  0.0301
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         3.933
_diffrn_reflns_theta_max         72.298
_diffrn_reflns_theta_full        67.679
_diffrn_measured_fraction_theta_max 0.958
_diffrn_measured_fraction_theta_full 0.966
_diffrn_reflns_Laue_measured_fraction_max 0.958
_diffrn_reflns_Laue_measured_fraction_full 0.966
_diffrn_reflns_point_group_measured_fraction_max 0.958
_diffrn_reflns_point_group_measured_fraction_full 0.966
_reflns_number_total             2462
_reflns_number_gt                2399
_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 Instrument Service vV6.2.16'
_computing_cell_refinement       'SAINT V8.40B (Bruker AXS LLC, 2019)'
_computing_data_reduction        'SAINT V8.40B (Bruker AXS LLC, 2019)'
_computing_structure_solution    'Sir-2019 (IUCr, 2019)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 2020)'
_computing_publication_material  'WinGX (Farrugia, 2020)'


_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)+(0.0716P)²+0.0901P] 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         2462
_refine_ls_number_parameters     118
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0433
_refine_ls_R_factor_gt           0.0429
_refine_ls_wR_factor_ref         0.1279
_refine_ls_wR_factor_gt          0.1275
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_restrained_S_all      1.075
_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 0.52490(6) 0.04491(4) 0.18981(3) 0.05495(19) Uani 1 1 d . . . . .
F1 F 0.31475(17) 0.00288(11) 0.13969(9) 0.0803(3) Uani 1 1 d . . . . .
C1 C 0.5842(3) 0.20589(15) 0.11987(13) 0.0609(4) Uani 1 1 d . . . . .
H1A H 0.645900 0.189688 0.034677 0.073 Uiso 1 1 calc R U . . .
H1B H 0.433176 0.270582 0.133195 0.073 Uiso 1 1 calc R U . . .
C2 C 0.7639(3) 0.26815(15) 0.16702(15) 0.0631(4) Uani 1 1 d . . . . .
H2A H 0.708862 0.277150 0.253023 0.076 Uiso 1 1 calc R U . . .
H2B H 0.918634 0.206472 0.147811 0.076 Uiso 1 1 calc R U . . .
C3 C 0.7986(3) 0.40642(18) 0.11742(17) 0.0761(5) Uani 1 1 d . . . . .
H3A H 0.926327 0.433667 0.145484 0.091 Uiso 1 1 calc R U . . .
H3B H 0.851417 0.397436 0.031358 0.091 Uiso 1 1 calc R U . . .
C4 C 0.5762(4) 0.51774(17) 0.15067(16) 0.0741(5) Uani 1 1 d . . . . .
H4A H 0.612436 0.598910 0.109632 0.089 Uiso 1 1 calc R U . . .
H4B H 0.448572 0.490660 0.122390 0.089 Uiso 1 1 calc R U . . .
C5 C 0.4841(3) 0.55190(18) 0.28260(16) 0.0750(5) Uani 1 1 d . . . . .
H5A H 0.607786 0.584197 0.310344 0.090 Uiso 1 1 calc R U . . .
H5B H 0.455276 0.470031 0.324453 0.090 Uiso 1 1 calc R U . . .
C6 C 0.2543(4) 0.65811(18) 0.31349(16) 0.0754(5) Uani 1 1 d . . . . .
H6A H 0.131779 0.626401 0.284340 0.091 Uiso 1 1 calc R U . . .
H6B H 0.284194 0.740350 0.272557 0.091 Uiso 1 1 calc R U . . .
C7 C -0.1580(4) 0.30857(19) 0.55432(16) 0.0790(5) Uani 1 1 d . . . . .
H7A H -0.279418 0.275048 0.525663 0.095 Uiso 1 1 calc R U . . .
H7B H -0.131975 0.391297 0.513303 0.095 Uiso 1 1 calc R U . . .
C8 C 0.0747(3) 0.20479(19) 0.52220(15) 0.0730(4) Uani 1 1 d . . . . .
H8A H 0.195689 0.237208 0.552071 0.088 Uiso 1 1 calc R U . . .
H8B H 0.048170 0.121137 0.561434 0.088 Uiso 1 1 calc R U . . .
C9 C 0.1701(3) 0.17551(19) 0.38976(15) 0.0748(5) Uani 1 1 d . . . . .
H9A H 0.197885 0.259327 0.351175 0.090 Uiso 1 1 calc R U . . .
H9B H 0.046834 0.145223 0.360127 0.090 Uiso 1 1 calc R U . . .
C10 C 0.4012(3) 0.07017(17) 0.35365(14) 0.0650(4) Uani 1 1 d . . . . .
H10A H 0.370784 -0.015574 0.387345 0.078 Uiso 1 1 calc R U . . .
H10B H 0.521815 0.097166 0.387543 0.078 Uiso 1 1 calc R U . . .
C11 C 0.7849(3) -0.09657(18) 0.15043(17) 0.0736(4) Uani 1 1 d . . . . .
H11A H 0.915505 -0.075854 0.178747 0.110 Uiso 1 1 calc R U . . .
H11B H 0.740133 -0.177501 0.186466 0.110 Uiso 1 1 calc R U . . .
H11C H 0.834728 -0.110116 0.065549 0.110 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 F1 1.6088(9) . ?
Si1 C11 1.8410(17) . ?
Si1 C1 1.8523(15) . ?
Si1 C10 1.8624(16) . ?
C1 C2 1.531(2) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C2 C3 1.526(2) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C3 C4 1.516(3) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C4 C5 1.514(2) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C5 C6 1.515(2) . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C6 C7 1.517(2) 2_566 ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C7 C8 1.514(3) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C8 C9 1.513(2) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C9 C10 1.518(2) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C11 H11A 0.9600 . ?
C11 H11B 0.9600 . ?
C11 H11C 0.9600 . ?

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
F1 Si1 C11 106.53(7) . . ?
F1 Si1 C1 106.82(7) . . ?
C11 Si1 C1 113.69(8) . . ?
F1 Si1 C10 105.97(7) . . ?
C11 Si1 C10 112.45(8) . . ?
C1 Si1 C10 110.82(7) . . ?
C2 C1 Si1 113.82(10) . . ?
C2 C1 H1A 108.8 . . ?
Si1 C1 H1A 108.8 . . ?
C2 C1 H1B 108.8 . . ?
Si1 C1 H1B 108.8 . . ?
H1A C1 H1B 107.7 . . ?
C3 C2 C1 114.25(14) . . ?
C3 C2 H2A 108.7 . . ?
C1 C2 H2A 108.7 . . ?
C3 C2 H2B 108.7 . . ?
C1 C2 H2B 108.7 . . ?
H2A C2 H2B 107.6 . . ?
C4 C3 C2 114.88(13) . . ?
C4 C3 H3A 108.5 . . ?
C2 C3 H3A 108.5 . . ?
C4 C3 H3B 108.5 . . ?
C2 C3 H3B 108.5 . . ?
H3A C3 H3B 107.5 . . ?
C5 C4 C3 114.76(15) . . ?
C5 C4 H4A 108.6 . . ?
C3 C4 H4A 108.6 . . ?
C5 C4 H4B 108.6 . . ?
C3 C4 H4B 108.6 . . ?
H4A C4 H4B 107.6 . . ?
C4 C5 C6 113.44(15) . . ?
C4 C5 H5A 108.9 . . ?
C6 C5 H5A 108.9 . . ?
C4 C5 H5B 108.9 . . ?
C6 C5 H5B 108.9 . . ?
H5A C5 H5B 107.7 . . ?
C5 C6 C7 113.91(16) . 2_566 ?
C5 C6 H6A 108.8 . . ?
C7 C6 H6A 108.8 2_566 . ?
C5 C6 H6B 108.8 . . ?
C7 C6 H6B 108.8 2_566 . ?
H6A C6 H6B 107.7 . . ?
C8 C7 C6 114.36(16) . 2_566 ?
C8 C7 H7A 108.7 . . ?
C6 C7 H7A 108.7 2_566 . ?
C8 C7 H7B 108.7 . . ?
C6 C7 H7B 108.7 2_566 . ?
H7A C7 H7B 107.6 . . ?
C9 C8 C7 113.39(15) . . ?
C9 C8 H8A 108.9 . . ?
C7 C8 H8A 108.9 . . ?
C9 C8 H8B 108.9 . . ?
C7 C8 H8B 108.9 . . ?
H8A C8 H8B 107.7 . . ?
C8 C9 C10 115.17(14) . . ?
C8 C9 H9A 108.5 . . ?
C10 C9 H9A 108.5 . . ?
C8 C9 H9B 108.5 . . ?
C10 C9 H9B 108.5 . . ?
H9A C9 H9B 107.5 . . ?
C9 C10 Si1 114.10(11) . . ?
C9 C10 H10A 108.7 . . ?
Si1 C10 H10A 108.7 . . ?
C9 C10 H10B 108.7 . . ?
Si1 C10 H10B 108.7 . . ?
H10A C10 H10B 107.6 . . ?
Si1 C11 H11A 109.5 . . ?
Si1 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
Si1 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 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
F1 Si1 C1 C2 174.41(10) . . . . ?
C11 Si1 C1 C2 -68.38(13) . . . . ?
C10 Si1 C1 C2 59.42(13) . . . . ?
Si1 C1 C2 C3 -175.29(11) . . . . ?
C1 C2 C3 C4 64.1(2) . . . . ?
C2 C3 C4 C5 63.2(2) . . . . ?
C3 C4 C5 C6 -176.91(15) . . . . ?
C4 C5 C6 C7 179.02(16) . . . 2_566 ?
C6 C7 C8 C9 -178.72(16) 2_566 . . . ?
C7 C8 C9 C10 -179.02(16) . . . . ?
C8 C9 C10 Si1 -176.09(13) . . . . ?
F1 Si1 C10 C9 -57.58(14) . . . . ?
C11 Si1 C10 C9 -173.58(13) . . . . ?
C1 Si1 C10 C9 57.94(15) . . . . ?

_refine_diff_density_max         0.279
_refine_diff_density_min         -0.182
_refine_diff_density_rms         0.030


_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: MeOH'
####################################################################### 
# 
# 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_2b
_database_code_depnum_ccdc_archive 'CCDC 2367923'
loop_
_audit_author_name
_audit_author_address
'Wataru Setaka'
;Tokyo Metropolitan University
Japan
;
_audit_update_record             
;
2024-08-05 deposited with the CCDC.	2024-08-08 downloaded from the CCDC.
;


# start Validation Reply Form
_vrf_PLAT049_2b                  
;
PROBLEM: Calculated Density Less Than 1.0 gcm-3 .........     0.9736 Check 
RESPONSE: This is caused by some void spaces in the crystal.
;
# end Validation Reply Form

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        tricycloalkane
_chemical_name_common            2b
_chemical_melting_point          '338-339 K'
_chemical_formula_moiety         'C80 H164 Si4'
_chemical_formula_sum            'C80 H164 Si4'
_chemical_formula_weight         1238.46



loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.2541 0.3302 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_H-M_alt        'P b c a'
_space_group_name_Hall           '-P 2ac 2ab'

_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, z+1/2'
'x+1/2, -y+1/2, -z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'-x-1/2, y-1/2, z'
'x, -y-1/2, z-1/2'

_cell_length_a                   14.9494(4)
_cell_length_b                   8.4932(2)
_cell_length_c                   66.5433(18)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     8448.9(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    200(2)
_cell_measurement_reflns_used    6552
_cell_measurement_theta_min      3.2409
_cell_measurement_theta_max      59.2622

_exptl_crystal_description       plate
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    0.974
_exptl_crystal_F_000             2800
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.160
_exptl_crystal_size_mid          0.140
_exptl_crystal_size_min          0.060
_exptl_absorpt_coefficient_mu    0.908
_shelx_estimated_absorpt_T_min   0.868
_shelx_estimated_absorpt_T_max   0.948
_exptl_absorpt_correction_type   Multi-Scan
_exptl_absorpt_process_details   
;
Krause, L., Herbst-Irmer, R., Sheldrick, G. M., Stalke, D. (2015).
"Comparison of silver and molybdenum microfocus X-ray sources for
single-crystal structure determination"
J. Appl. Cryst. 48, 3-10.
doi:10.1107/S1600576714022985
;
_exptl_absorpt_correction_T_min  0.85
_exptl_absorpt_correction_T_max  0.96


_diffrn_ambient_temperature      200(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_source                   'sealed tube'
_diffrn_radiation_monochromator  'multilayered conforcal mirror'
_diffrn_measurement_device       ?
_diffrn_measurement_device_type  'Bruker D8 goniometer'
_diffrn_measurement_method       'omega scans'

_diffrn_detector_area_resol_mean 7.3910
_diffrn_reflns_number            121616
_diffrn_reflns_av_unetI/netI     0.0649
_diffrn_reflns_av_R_equivalents  0.1447
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -81
_diffrn_reflns_limit_l_max       82
_diffrn_reflns_theta_min         2.656
_diffrn_reflns_theta_max         73.028
_diffrn_reflns_theta_full        67.679
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measured_fraction_theta_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_point_group_measured_fraction_full 0.996
_reflns_number_total             8371
_reflns_number_gt                5943
_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 Instrument Service vV6.2.16'
_computing_cell_refinement       'SAINT V8.40B (Bruker AXS LLC, 2019)'
_computing_data_reduction        'SAINT V8.40B (Bruker AXS LLC, 2019)'
_computing_structure_solution    'Sir-2019 (IUCr, 2019)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 2020)'
_computing_publication_material  'WinGX (Farrugia, 2020)'


_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)+(0.0754P)²+1.9372P] 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     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_extinction_coef       0.00056(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         8371
_refine_ls_number_parameters     380
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0938
_refine_ls_R_factor_gt           0.0672
_refine_ls_wR_factor_ref         0.1759
_refine_ls_wR_factor_gt          0.1598
_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 0.45472(4) 0.21723(8) 0.28696(2) 0.05218(18) Uani 1 1 d . . . . .
Si2 Si 0.39033(4) 0.13974(10) 0.45995(2) 0.0591(2) Uani 1 1 d . . . . .
C1 C 0.51672(17) 0.2742(3) 0.31035(4) 0.0566(6) Uani 1 1 d . . . . .
H1A H 0.554775 0.184391 0.314460 0.068 Uiso 1 1 calc R U . . .
H1B H 0.556975 0.363127 0.307077 0.068 Uiso 1 1 calc R U . . .
C2 C 0.45868(16) 0.3219(3) 0.32830(4) 0.0546(6) Uani 1 1 d . . . . .
H2A H 0.420199 0.411378 0.324268 0.066 Uiso 1 1 calc R U . . .
H2B H 0.418997 0.232742 0.331810 0.066 Uiso 1 1 calc R U . . .
C3 C 0.51119(17) 0.3686(4) 0.34672(4) 0.0620(6) Uani 1 1 d . . . . .
H3A H 0.551005 0.457394 0.343140 0.074 Uiso 1 1 calc R U . . .
H3B H 0.549654 0.278936 0.350696 0.074 Uiso 1 1 calc R U . . .
C4 C 0.45490(17) 0.4166(3) 0.36468(4) 0.0577(6) Uani 1 1 d . . . . .
H4A H 0.415333 0.504527 0.360644 0.069 Uiso 1 1 calc R U . . .
H4B H 0.416269 0.326832 0.368529 0.069 Uiso 1 1 calc R U . . .
C5 C 0.50843(18) 0.4668(4) 0.38281(4) 0.0645(7) Uani 1 1 d . . . . .
H5A H 0.545081 0.559482 0.379107 0.077 Uiso 1 1 calc R U . . .
H5B H 0.549951 0.380637 0.386458 0.077 Uiso 1 1 calc R U . . .
C6 C 0.45296(17) 0.5082(3) 0.40106(4) 0.0584(6) Uani 1 1 d . . . . .
H6A H 0.416491 0.415703 0.404915 0.070 Uiso 1 1 calc R U . . .
H6B H 0.411463 0.594736 0.397533 0.070 Uiso 1 1 calc R U . . .
C7 C 0.50925(18) 0.5582(4) 0.41889(4) 0.0662(7) Uani 1 1 d . . . . .
H7A H 0.544379 0.652220 0.415000 0.079 Uiso 1 1 calc R U . . .
H7B H 0.552226 0.472830 0.421949 0.079 Uiso 1 1 calc R U . . .
C8 C 0.4572(2) 0.5965(4) 0.43796(4) 0.0691(7) Uani 1 1 d . . . . .
H8A H 0.415465 0.684168 0.435082 0.083 Uiso 1 1 calc R U . . .
H8B H 0.499711 0.633137 0.448359 0.083 Uiso 1 1 calc R U . . .
C9 C 0.40360(17) 0.4571(3) 0.44639(4) 0.0625(6) Uani 1 1 d . . . . .
H9A H 0.367290 0.495270 0.457843 0.075 Uiso 1 1 calc R U . . .
H9B H 0.361657 0.420358 0.435880 0.075 Uiso 1 1 calc R U . . .
C10 C 0.45884(16) 0.3171(3) 0.45346(4) 0.0630(7) Uani 1 1 d . . . . .
H10A H 0.493825 0.348820 0.465424 0.076 Uiso 1 1 calc R U . . .
H10B H 0.501789 0.288311 0.442747 0.076 Uiso 1 1 calc R U . . .
C11 C 0.33146(17) 0.0647(4) 0.43704(4) 0.0672(7) Uani 1 1 d . . . . .
H11A H 0.301834 -0.035534 0.440716 0.081 Uiso 1 1 calc R U . . .
H11B H 0.283542 0.140686 0.433681 0.081 Uiso 1 1 calc R U . . .
C12 C 0.38540(17) 0.0352(4) 0.41796(4) 0.0615(6) Uani 1 1 d . . . . .
H12A H 0.414799 0.134599 0.413848 0.074 Uiso 1 1 calc R U . . .
H12B H 0.432921 -0.042639 0.420884 0.074 Uiso 1 1 calc R U . . .
C13 C 0.32855(18) -0.0250(4) 0.40063(4) 0.0678(7) Uani 1 1 d . . . . .
H13A H 0.299258 -0.124081 0.404888 0.081 Uiso 1 1 calc R U . . .
H13B H 0.280741 0.052847 0.397934 0.081 Uiso 1 1 calc R U . . .
C14 C 0.37832(17) -0.0555(4) 0.38131(4) 0.0630(7) Uani 1 1 d . . . . .
H14A H 0.424393 -0.136936 0.383785 0.076 Uiso 1 1 calc R U . . .
H14B H 0.409577 0.042252 0.377254 0.076 Uiso 1 1 calc R U . . .
C15 C 0.31921(18) -0.1092(4) 0.36408(4) 0.0665(7) Uani 1 1 d . . . . .
H15A H 0.287957 -0.206991 0.368099 0.080 Uiso 1 1 calc R U . . .
H15B H 0.273171 -0.027743 0.361560 0.080 Uiso 1 1 calc R U . . .
C16 C 0.36964(17) -0.1394(3) 0.34483(4) 0.0606(6) Uani 1 1 d . . . . .
H16A H 0.412865 -0.225862 0.347119 0.073 Uiso 1 1 calc R U . . .
H16B H 0.404222 -0.043852 0.341322 0.073 Uiso 1 1 calc R U . . .
C17 C 0.30993(18) -0.1827(3) 0.32716(4) 0.0643(7) Uani 1 1 d . . . . .
H17A H 0.270139 -0.092603 0.324137 0.077 Uiso 1 1 calc R U . . .
H17B H 0.271665 -0.272778 0.331074 0.077 Uiso 1 1 calc R U . . .
C18 C 0.36149(19) -0.2264(3) 0.30812(4) 0.0647(7) Uani 1 1 d . . . . .
H18A H 0.397473 -0.321757 0.310908 0.078 Uiso 1 1 calc R U . . .
H18B H 0.317860 -0.253624 0.297481 0.078 Uiso 1 1 calc R U . . .
C19 C 0.42376(16) -0.0983(3) 0.30007(4) 0.0549(6) Uani 1 1 d . . . . .
H19A H 0.466993 -0.070052 0.310746 0.066 Uiso 1 1 calc R U . . .
H19B H 0.458235 -0.142088 0.288660 0.066 Uiso 1 1 calc R U . . .
C20 C 0.37660(15) 0.0514(3) 0.29305(4) 0.0545(6) Uani 1 1 d . . . . .
H20A H 0.334879 0.086447 0.303710 0.065 Uiso 1 1 calc R U . . .
H20B H 0.340641 0.026692 0.280968 0.065 Uiso 1 1 calc R U . . .
C21 C 0.53469(18) 0.1516(3) 0.26699(4) 0.0610(6) Uani 1 1 d . . . . .
H21A H 0.569340 0.061550 0.272333 0.073 Uiso 1 1 calc R U . . .
H21B H 0.499288 0.112172 0.255465 0.073 Uiso 1 1 calc R U . . .
C22 C 0.60102(19) 0.2738(4) 0.25906(4) 0.0710(7) Uani 1 1 d . . . . .
H22A H 0.590356 0.287029 0.244471 0.085 Uiso 1 1 calc R U . . .
H22B H 0.587515 0.375872 0.265574 0.085 Uiso 1 1 calc R U . . .
C23 C 0.6978(2) 0.2394(4) 0.26207(4) 0.0763(8) Uani 1 1 d . . . . .
H23A H 0.733274 0.321784 0.255194 0.092 Uiso 1 1 calc R U . . .
H23B H 0.711894 0.137499 0.255592 0.092 Uiso 1 1 calc R U . . .
C24 C 0.27348(18) 0.7680(4) 0.71622(4) 0.0689(7) Uani 1 1 d . . . . .
H24A H 0.295484 0.672306 0.709313 0.083 Uiso 1 1 calc R U . . .
H24B H 0.302955 0.859741 0.709862 0.083 Uiso 1 1 calc R U . . .
C25 C 0.17343(19) 0.7810(4) 0.71270(5) 0.0712(7) Uani 1 1 d . . . . .
H25A H 0.144158 0.685193 0.718041 0.085 Uiso 1 1 calc R U . . .
H25B H 0.150350 0.872108 0.720392 0.085 Uiso 1 1 calc R U . . .
C26 C 0.14748(18) 0.8003(3) 0.69111(4) 0.0671(7) Uani 1 1 d . . . . .
H26A H 0.169821 0.903413 0.686309 0.080 Uiso 1 1 calc R U . . .
H26B H 0.081394 0.802286 0.690198 0.080 Uiso 1 1 calc R U . . .
C27 C 0.18254(19) 0.6726(3) 0.67724(4) 0.0673(7) Uani 1 1 d . . . . .
H27A H 0.248302 0.683764 0.676213 0.081 Uiso 1 1 calc R U . . .
H27B H 0.170097 0.568985 0.683455 0.081 Uiso 1 1 calc R U . . .
C28 C 0.14400(18) 0.6733(4) 0.65640(4) 0.0658(7) Uani 1 1 d . . . . .
H28A H 0.146629 0.781811 0.651015 0.079 Uiso 1 1 calc R U . . .
H28B H 0.080249 0.642251 0.657140 0.079 Uiso 1 1 calc R U . . .
C29 C 0.19173(19) 0.5642(4) 0.64202(4) 0.0725(8) Uani 1 1 d . . . . .
H29A H 0.253906 0.602157 0.640367 0.087 Uiso 1 1 calc R U . . .
H29B H 0.194776 0.458378 0.648227 0.087 Uiso 1 1 calc R U . . .
C30 C 0.15038(18) 0.5477(4) 0.62140(4) 0.0697(7) Uani 1 1 d . . . . .
H30A H 0.094502 0.485789 0.622573 0.084 Uiso 1 1 calc R U . . .
H30B H 0.134279 0.653612 0.616359 0.084 Uiso 1 1 calc R U . . .
C31 C 0.21086(19) 0.4690(4) 0.60633(4) 0.0755(8) Uani 1 1 d . . . . .
H31A H 0.230633 0.367064 0.612013 0.091 Uiso 1 1 calc R U . . .
H31B H 0.264777 0.535332 0.604620 0.091 Uiso 1 1 calc R U . . .
C32 C 0.17116(17) 0.4384(4) 0.58572(4) 0.0668(7) Uani 1 1 d . . . . .
H32A H 0.140019 0.534406 0.581009 0.080 Uiso 1 1 calc R U . . .
H32B H 0.126347 0.352918 0.586731 0.080 Uiso 1 1 calc R U . . .
C33 C 0.24211(18) 0.3923(4) 0.57046(4) 0.0682(7) Uani 1 1 d . . . . .
H33A H 0.285406 0.480064 0.569358 0.082 Uiso 1 1 calc R U . . .
H33B H 0.274976 0.300033 0.575769 0.082 Uiso 1 1 calc R U . . .
C34 C 0.20940(17) 0.3525(4) 0.54960(4) 0.0653(7) Uani 1 1 d . . . . .
H34A H 0.172136 0.440466 0.544562 0.078 Uiso 1 1 calc R U . . .
H34B H 0.171083 0.257643 0.550318 0.078 Uiso 1 1 calc R U . . .
C35 C 0.28444(17) 0.3227(4) 0.53487(4) 0.0643(7) Uani 1 1 d . . . . .
H35A H 0.322909 0.237804 0.540264 0.077 Uiso 1 1 calc R U . . .
H35B H 0.321434 0.419125 0.533907 0.077 Uiso 1 1 calc R U . . .
C36 C 0.25439(17) 0.2768(4) 0.51388(4) 0.0635(6) Uani 1 1 d . . . . .
H36A H 0.217707 0.180031 0.514791 0.076 Uiso 1 1 calc R U . . .
H36B H 0.215808 0.361508 0.508460 0.076 Uiso 1 1 calc R U . . .
C37 C 0.33060(17) 0.2480(4) 0.49927(4) 0.0653(7) Uani 1 1 d . . . . .
H37A H 0.371906 0.169655 0.505209 0.078 Uiso 1 1 calc R U . . .
H37B H 0.364320 0.347364 0.497501 0.078 Uiso 1 1 calc R U . . .
C38 C 0.30075(17) 0.1892(4) 0.47868(4) 0.0641(7) Uani 1 1 d . . . . .
H38A H 0.261709 0.270655 0.472645 0.077 Uiso 1 1 calc R U . . .
H38B H 0.263645 0.094005 0.480717 0.077 Uiso 1 1 calc R U . . .
C39 C 0.3891(2) 0.3891(4) 0.27781(5) 0.0727(8) Uani 1 1 d . . . . .
H39A H 0.347324 0.423074 0.288304 0.109 Uiso 1 1 calc R U . . .
H39B H 0.429865 0.475776 0.274546 0.109 Uiso 1 1 calc R U . . .
H39C H 0.355479 0.359068 0.265759 0.109 Uiso 1 1 calc R U . . .
C40 C 0.4652(2) -0.0179(4) 0.47010(5) 0.0761(8) Uani 1 1 d . . . . .
H40A H 0.429410 -0.110820 0.473509 0.114 Uiso 1 1 calc R U . . .
H40B H 0.509786 -0.046218 0.459932 0.114 Uiso 1 1 calc R U . . .
H40C H 0.495576 0.020804 0.482181 0.114 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 C39 1.862(3) . ?
Si1 C21 1.872(3) . ?
Si1 C20 1.874(3) . ?
Si1 C1 1.875(2) . ?
Si2 C40 1.871(3) . ?
Si2 C10 1.872(3) . ?
Si2 C11 1.873(3) . ?
Si2 C38 1.877(3) . ?
C1 C2 1.531(3) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 C3 1.508(3) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 C4 1.518(3) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 C5 1.509(3) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 C6 1.512(3) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C6 C7 1.515(3) . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C7 C8 1.524(4) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 C9 1.536(4) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C9 C10 1.522(4) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C11 C12 1.525(4) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 C13 1.521(4) . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C13 C14 1.508(4) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C14 C15 1.518(4) . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C15 C16 1.508(4) . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C16 C17 1.522(4) . ?
C16 H16A 0.9900 . ?
C16 H16B 0.9900 . ?
C17 C18 1.529(4) . ?
C17 H17A 0.9900 . ?
C17 H17B 0.9900 . ?
C18 C19 1.529(4) . ?
C18 H18A 0.9900 . ?
C18 H18B 0.9900 . ?
C19 C20 1.527(3) . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C21 C22 1.529(4) . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C22 C23 1.489(4) . ?
C22 H22A 0.9900 . ?
C22 H22B 0.9900 . ?
C23 C24 1.509(4) 5_666 ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C24 C25 1.518(4) . ?
C24 H24A 0.9900 . ?
C24 H24B 0.9900 . ?
C25 C26 1.497(4) . ?
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?
C26 C27 1.518(4) . ?
C26 H26A 0.9900 . ?
C26 H26B 0.9900 . ?
C27 C28 1.502(4) . ?
C27 H27A 0.9900 . ?
C27 H27B 0.9900 . ?
C28 C29 1.511(4) . ?
C28 H28A 0.9900 . ?
C28 H28B 0.9900 . ?
C29 C30 1.511(4) . ?
C29 H29A 0.9900 . ?
C29 H29B 0.9900 . ?
C30 C31 1.507(4) . ?
C30 H30A 0.9900 . ?
C30 H30B 0.9900 . ?
C31 C32 1.517(4) . ?
C31 H31A 0.9900 . ?
C31 H31B 0.9900 . ?
C32 C33 1.520(4) . ?
C32 H32A 0.9900 . ?
C32 H32B 0.9900 . ?
C33 C34 1.510(4) . ?
C33 H33A 0.9900 . ?
C33 H33B 0.9900 . ?
C34 C35 1.511(4) . ?
C34 H34A 0.9900 . ?
C34 H34B 0.9900 . ?
C35 C36 1.518(4) . ?
C35 H35A 0.9900 . ?
C35 H35B 0.9900 . ?
C36 C37 1.518(4) . ?
C36 H36A 0.9900 . ?
C36 H36B 0.9900 . ?
C37 C38 1.525(4) . ?
C37 H37A 0.9900 . ?
C37 H37B 0.9900 . ?
C38 H38A 0.9900 . ?
C38 H38B 0.9900 . ?
C39 H39A 0.9800 . ?
C39 H39B 0.9800 . ?
C39 H39C 0.9800 . ?
C40 H40A 0.9800 . ?
C40 H40B 0.9800 . ?
C40 H40C 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
C39 Si1 C21 109.75(13) . . ?
C39 Si1 C20 109.37(13) . . ?
C21 Si1 C20 109.14(12) . . ?
C39 Si1 C1 109.25(13) . . ?
C21 Si1 C1 110.51(12) . . ?
C20 Si1 C1 108.79(11) . . ?
C40 Si2 C10 109.38(14) . . ?
C40 Si2 C11 109.35(15) . . ?
C10 Si2 C11 110.07(13) . . ?
C40 Si2 C38 110.33(13) . . ?
C10 Si2 C38 111.31(13) . . ?
C11 Si2 C38 106.35(12) . . ?
C2 C1 Si1 115.83(17) . . ?
C2 C1 H1A 108.3 . . ?
Si1 C1 H1A 108.3 . . ?
C2 C1 H1B 108.3 . . ?
Si1 C1 H1B 108.3 . . ?
H1A C1 H1B 107.4 . . ?
C3 C2 C1 114.1(2) . . ?
C3 C2 H2A 108.7 . . ?
C1 C2 H2A 108.7 . . ?
C3 C2 H2B 108.7 . . ?
C1 C2 H2B 108.7 . . ?
H2A C2 H2B 107.6 . . ?
C2 C3 C4 115.0(2) . . ?
C2 C3 H3A 108.5 . . ?
C4 C3 H3A 108.5 . . ?
C2 C3 H3B 108.5 . . ?
C4 C3 H3B 108.5 . . ?
H3A C3 H3B 107.5 . . ?
C5 C4 C3 114.3(2) . . ?
C5 C4 H4A 108.7 . . ?
C3 C4 H4A 108.7 . . ?
C5 C4 H4B 108.7 . . ?
C3 C4 H4B 108.7 . . ?
H4A C4 H4B 107.6 . . ?
C4 C5 C6 114.6(2) . . ?
C4 C5 H5A 108.6 . . ?
C6 C5 H5A 108.6 . . ?
C4 C5 H5B 108.6 . . ?
C6 C5 H5B 108.6 . . ?
H5A C5 H5B 107.6 . . ?
C5 C6 C7 112.9(2) . . ?
C5 C6 H6A 109.0 . . ?
C7 C6 H6A 109.0 . . ?
C5 C6 H6B 109.0 . . ?
C7 C6 H6B 109.0 . . ?
H6A C6 H6B 107.8 . . ?
C6 C7 C8 115.3(2) . . ?
C6 C7 H7A 108.4 . . ?
C8 C7 H7A 108.4 . . ?
C6 C7 H7B 108.4 . . ?
C8 C7 H7B 108.4 . . ?
H7A C7 H7B 107.5 . . ?
C7 C8 C9 114.0(2) . . ?
C7 C8 H8A 108.8 . . ?
C9 C8 H8A 108.8 . . ?
C7 C8 H8B 108.8 . . ?
C9 C8 H8B 108.8 . . ?
H8A C8 H8B 107.7 . . ?
C10 C9 C8 115.6(2) . . ?
C10 C9 H9A 108.4 . . ?
C8 C9 H9A 108.4 . . ?
C10 C9 H9B 108.4 . . ?
C8 C9 H9B 108.4 . . ?
H9A C9 H9B 107.4 . . ?
C9 C10 Si2 113.77(18) . . ?
C9 C10 H10A 108.8 . . ?
Si2 C10 H10A 108.8 . . ?
C9 C10 H10B 108.8 . . ?
Si2 C10 H10B 108.8 . . ?
H10A C10 H10B 107.7 . . ?
C12 C11 Si2 119.04(18) . . ?
C12 C11 H11A 107.6 . . ?
Si2 C11 H11A 107.6 . . ?
C12 C11 H11B 107.6 . . ?
Si2 C11 H11B 107.6 . . ?
H11A C11 H11B 107.0 . . ?
C13 C12 C11 113.0(2) . . ?
C13 C12 H12A 109.0 . . ?
C11 C12 H12A 109.0 . . ?
C13 C12 H12B 109.0 . . ?
C11 C12 H12B 109.0 . . ?
H12A C12 H12B 107.8 . . ?
C14 C13 C12 115.4(2) . . ?
C14 C13 H13A 108.4 . . ?
C12 C13 H13A 108.4 . . ?
C14 C13 H13B 108.4 . . ?
C12 C13 H13B 108.4 . . ?
H13A C13 H13B 107.5 . . ?
C13 C14 C15 114.1(2) . . ?
C13 C14 H14A 108.7 . . ?
C15 C14 H14A 108.7 . . ?
C13 C14 H14B 108.7 . . ?
C15 C14 H14B 108.7 . . ?
H14A C14 H14B 107.6 . . ?
C16 C15 C14 113.7(2) . . ?
C16 C15 H15A 108.8 . . ?
C14 C15 H15A 108.8 . . ?
C16 C15 H15B 108.8 . . ?
C14 C15 H15B 108.8 . . ?
H15A C15 H15B 107.7 . . ?
C15 C16 C17 113.8(2) . . ?
C15 C16 H16A 108.8 . . ?
C17 C16 H16A 108.8 . . ?
C15 C16 H16B 108.8 . . ?
C17 C16 H16B 108.8 . . ?
H16A C16 H16B 107.7 . . ?
C16 C17 C18 113.8(2) . . ?
C16 C17 H17A 108.8 . . ?
C18 C17 H17A 108.8 . . ?
C16 C17 H17B 108.8 . . ?
C18 C17 H17B 108.8 . . ?
H17A C17 H17B 107.7 . . ?
C19 C18 C17 115.2(2) . . ?
C19 C18 H18A 108.5 . . ?
C17 C18 H18A 108.5 . . ?
C19 C18 H18B 108.5 . . ?
C17 C18 H18B 108.5 . . ?
H18A C18 H18B 107.5 . . ?
C20 C19 C18 114.7(2) . . ?
C20 C19 H19A 108.6 . . ?
C18 C19 H19A 108.6 . . ?
C20 C19 H19B 108.6 . . ?
C18 C19 H19B 108.6 . . ?
H19A C19 H19B 107.6 . . ?
C19 C20 Si1 113.85(16) . . ?
C19 C20 H20A 108.8 . . ?
Si1 C20 H20A 108.8 . . ?
C19 C20 H20B 108.8 . . ?
Si1 C20 H20B 108.8 . . ?
H20A C20 H20B 107.7 . . ?
C22 C21 Si1 117.2(2) . . ?
C22 C21 H21A 108.0 . . ?
Si1 C21 H21A 108.0 . . ?
C22 C21 H21B 108.0 . . ?
Si1 C21 H21B 108.0 . . ?
H21A C21 H21B 107.2 . . ?
C23 C22 C21 116.8(3) . . ?
C23 C22 H22A 108.1 . . ?
C21 C22 H22A 108.1 . . ?
C23 C22 H22B 108.1 . . ?
C21 C22 H22B 108.1 . . ?
H22A C22 H22B 107.3 . . ?
C22 C23 C24 114.4(3) . 5_666 ?
C22 C23 H23A 108.6 . . ?
C24 C23 H23A 108.6 5_666 . ?
C22 C23 H23B 108.6 . . ?
C24 C23 H23B 108.6 5_666 . ?
H23A C23 H23B 107.6 . . ?
C23 C24 C25 115.6(2) 5_666 . ?
C23 C24 H24A 108.4 5_666 . ?
C25 C24 H24A 108.4 . . ?
C23 C24 H24B 108.4 5_666 . ?
C25 C24 H24B 108.4 . . ?
H24A C24 H24B 107.4 . . ?
C26 C25 C24 114.3(2) . . ?
C26 C25 H25A 108.7 . . ?
C24 C25 H25A 108.7 . . ?
C26 C25 H25B 108.7 . . ?
C24 C25 H25B 108.7 . . ?
H25A C25 H25B 107.6 . . ?
C25 C26 C27 114.6(3) . . ?
C25 C26 H26A 108.6 . . ?
C27 C26 H26A 108.6 . . ?
C25 C26 H26B 108.6 . . ?
C27 C26 H26B 108.6 . . ?
H26A C26 H26B 107.6 . . ?
C28 C27 C26 115.2(2) . . ?
C28 C27 H27A 108.5 . . ?
C26 C27 H27A 108.5 . . ?
C28 C27 H27B 108.5 . . ?
C26 C27 H27B 108.5 . . ?
H27A C27 H27B 107.5 . . ?
C27 C28 C29 113.7(2) . . ?
C27 C28 H28A 108.8 . . ?
C29 C28 H28A 108.8 . . ?
C27 C28 H28B 108.8 . . ?
C29 C28 H28B 108.8 . . ?
H28A C28 H28B 107.7 . . ?
C30 C29 C28 116.0(2) . . ?
C30 C29 H29A 108.3 . . ?
C28 C29 H29A 108.3 . . ?
C30 C29 H29B 108.3 . . ?
C28 C29 H29B 108.3 . . ?
H29A C29 H29B 107.4 . . ?
C31 C30 C29 113.6(2) . . ?
C31 C30 H30A 108.8 . . ?
C29 C30 H30A 108.8 . . ?
C31 C30 H30B 108.8 . . ?
C29 C30 H30B 108.8 . . ?
H30A C30 H30B 107.7 . . ?
C30 C31 C32 116.3(2) . . ?
C30 C31 H31A 108.2 . . ?
C32 C31 H31A 108.2 . . ?
C30 C31 H31B 108.2 . . ?
C32 C31 H31B 108.2 . . ?
H31A C31 H31B 107.4 . . ?
C31 C32 C33 112.0(2) . . ?
C31 C32 H32A 109.2 . . ?
C33 C32 H32A 109.2 . . ?
C31 C32 H32B 109.2 . . ?
C33 C32 H32B 109.2 . . ?
H32A C32 H32B 107.9 . . ?
C34 C33 C32 116.5(2) . . ?
C34 C33 H33A 108.2 . . ?
C32 C33 H33A 108.2 . . ?
C34 C33 H33B 108.2 . . ?
C32 C33 H33B 108.2 . . ?
H33A C33 H33B 107.3 . . ?
C33 C34 C35 113.2(2) . . ?
C33 C34 H34A 108.9 . . ?
C35 C34 H34A 108.9 . . ?
C33 C34 H34B 108.9 . . ?
C35 C34 H34B 108.9 . . ?
H34A C34 H34B 107.8 . . ?
C34 C35 C36 114.8(2) . . ?
C34 C35 H35A 108.6 . . ?
C36 C35 H35A 108.6 . . ?
C34 C35 H35B 108.6 . . ?
C36 C35 H35B 108.6 . . ?
H35A C35 H35B 107.5 . . ?
C37 C36 C35 114.1(2) . . ?
C37 C36 H36A 108.7 . . ?
C35 C36 H36A 108.7 . . ?
C37 C36 H36B 108.7 . . ?
C35 C36 H36B 108.7 . . ?
H36A C36 H36B 107.6 . . ?
C36 C37 C38 114.1(2) . . ?
C36 C37 H37A 108.7 . . ?
C38 C37 H37A 108.7 . . ?
C36 C37 H37B 108.7 . . ?
C38 C37 H37B 108.7 . . ?
H37A C37 H37B 107.6 . . ?
C37 C38 Si2 117.45(18) . . ?
C37 C38 H38A 107.9 . . ?
Si2 C38 H38A 107.9 . . ?
C37 C38 H38B 107.9 . . ?
Si2 C38 H38B 107.9 . . ?
H38A C38 H38B 107.2 . . ?
Si1 C39 H39A 109.5 . . ?
Si1 C39 H39B 109.5 . . ?
H39A C39 H39B 109.5 . . ?
Si1 C39 H39C 109.5 . . ?
H39A C39 H39C 109.5 . . ?
H39B C39 H39C 109.5 . . ?
Si2 C40 H40A 109.5 . . ?
Si2 C40 H40B 109.5 . . ?
H40A C40 H40B 109.5 . . ?
Si2 C40 H40C 109.5 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 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
C39 Si1 C1 C2 62.3(2) . . . . ?
C21 Si1 C1 C2 -176.85(19) . . . . ?
C20 Si1 C1 C2 -57.0(2) . . . . ?
Si1 C1 C2 C3 -179.35(19) . . . . ?
C1 C2 C3 C4 179.9(2) . . . . ?
C2 C3 C4 C5 -178.5(2) . . . . ?
C3 C4 C5 C6 -177.5(2) . . . . ?
C4 C5 C6 C7 -179.9(2) . . . . ?
C5 C6 C7 C8 -178.2(2) . . . . ?
C6 C7 C8 C9 61.5(3) . . . . ?
C7 C8 C9 C10 63.9(3) . . . . ?
C8 C9 C10 Si2 -171.31(19) . . . . ?
C40 Si2 C10 C9 -176.0(2) . . . . ?
C11 Si2 C10 C9 63.9(2) . . . . ?
C38 Si2 C10 C9 -53.8(2) . . . . ?
C40 Si2 C11 C12 -69.1(3) . . . . ?
C10 Si2 C11 C12 51.0(3) . . . . ?
C38 Si2 C11 C12 171.7(2) . . . . ?
Si2 C11 C12 C13 -179.8(2) . . . . ?
C11 C12 C13 C14 179.7(3) . . . . ?
C12 C13 C14 C15 -177.7(3) . . . . ?
C13 C14 C15 C16 -180.0(3) . . . . ?
C14 C15 C16 C17 -176.2(2) . . . . ?
C15 C16 C17 C18 -175.3(2) . . . . ?
C16 C17 C18 C19 -58.7(3) . . . . ?
C17 C18 C19 C20 -64.1(3) . . . . ?
C18 C19 C20 Si1 171.22(18) . . . . ?
C39 Si1 C20 C19 178.04(19) . . . . ?
C21 Si1 C20 C19 58.0(2) . . . . ?
C1 Si1 C20 C19 -62.7(2) . . . . ?
C39 Si1 C21 C22 56.9(2) . . . . ?
C20 Si1 C21 C22 176.7(2) . . . . ?
C1 Si1 C21 C22 -63.7(2) . . . . ?
Si1 C21 C22 C23 118.4(3) . . . . ?
C21 C22 C23 C24 -63.7(4) . . . 5_666 ?
C23 C24 C25 C26 175.6(3) 5_666 . . . ?
C24 C25 C26 C27 55.5(4) . . . . ?
C25 C26 C27 C28 169.4(2) . . . . ?
C26 C27 C28 C29 169.8(3) . . . . ?
C27 C28 C29 C30 174.2(3) . . . . ?
C28 C29 C30 C31 166.7(3) . . . . ?
C29 C30 C31 C32 175.9(3) . . . . ?
C30 C31 C32 C33 167.6(3) . . . . ?
C31 C32 C33 C34 177.6(3) . . . . ?
C32 C33 C34 C35 174.7(3) . . . . ?
C33 C34 C35 C36 178.0(3) . . . . ?
C34 C35 C36 C37 179.8(3) . . . . ?
C35 C36 C37 C38 175.4(2) . . . . ?
C36 C37 C38 Si2 -176.8(2) . . . . ?
C40 Si2 C38 C37 59.3(3) . . . . ?
C10 Si2 C38 C37 -62.4(2) . . . . ?
C11 Si2 C38 C37 177.8(2) . . . . ?

_refine_diff_density_max         0.242
_refine_diff_density_min         -0.255
_refine_diff_density_rms         0.046


_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_chemical_compound_source        no
