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

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

data_shelx
_audit_block_doi                 10.5517/ccdc.csd.cc1p5z0v
_database_code_depnum_ccdc_archive 'CCDC 1554867'
_audit_update_record             
;
2017-09-13 deposited with the CCDC.
2017-09-14 downloaded from the CCDC.
;



# start Validation Reply Form
_vrf_SHFSU01_I                   
;
PROBLEM: The absolute value of parameter shift to su ratio > 0.20
RESPONSE: Due to many restraints
;
_vrf_PLAT026_I                   
;
PROBLEM: Ratio Observed / Unique Reflections (too) Low ..         16 %     
RESPONSE: Due to high collection temperature, reflections at high resolution cannot be collected.
;
_vrf_PLAT080_I                   
;
PROBLEM: Maximum Shift/Error ............................       1.27 Why ? 
RESPONSE: This parameter was oscillated during the refinements due to many restraints.
;
_vrf_PLAT084_I                   
;
PROBLEM: High wR2 Value (i.e. > 0.25) ...................       0.49 Report
RESPONSE: Due to high collection temperature, reflections at high resolution cannot be collected.
;
_vrf_PLAT410_I                   
;
PROBLEM: Short Intra H...H Contact   H15A   ..  H17A    .       1.73 Ang.  
RESPONSE: Due to many restraints
;
# end Validation Reply Form



_audit_creation_method           SHELXL-2013
_chemical_name_systematic        C18BiPhcage
_chemical_name_common            C18BiPhcage
_chemical_melting_point          '274-276 deg.C'
_chemical_formula_moiety         'C66 H116 Si2'
_chemical_formula_sum            'C66 H116 Si2'
_chemical_formula_weight         965.76

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

_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_H-M_alt        'C c'
_space_group_name_Hall           'C -2yc'

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

_cell_length_a                   36.88(3)
_cell_length_b                   11.065(8)
_cell_length_c                   19.195(13)
_cell_angle_alpha                90
_cell_angle_beta                 121.141(8)
_cell_angle_gamma                90
_cell_volume                     6703(8)
_cell_formula_units_Z            4
_cell_measurement_temperature    320(2)
_cell_measurement_reflns_used    1014
_cell_measurement_theta_min      2.48
_cell_measurement_theta_max      14.99

_exptl_crystal_description       plate
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    0.957
_exptl_crystal_F_000             2160
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.400
_exptl_crystal_size_min          0.300
_exptl_absorpt_coefficient_mu    0.087
_shelx_estimated_absorpt_T_min   0.966
_shelx_estimated_absorpt_T_max   0.974
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5112
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_process_details   'SADABS (bruker)'

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      320(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker SMART CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean 8.333
_diffrn_reflns_number            18001
_diffrn_reflns_av_unetI/netI     0.1024
_diffrn_reflns_av_R_equivalents  0.0545
_diffrn_reflns_limit_h_min       -48
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         1.950
_diffrn_reflns_theta_max         27.980
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.909
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.909
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.581
_diffrn_reflns_point_group_measured_fraction_full 0.658
_reflns_number_total             9394
_reflns_number_gt                1467
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.279
_reflns_Friedel_fraction_max     0.254
_reflns_Friedel_fraction_full    0.317

_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, 1997)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX (Farrugia, 1999)'

_refine_special_details          
;
  The structure was refined in Cc, because the molecule has no center of symmetry due to
   unsymmetrical structure in alkyl chains.
  The structure was refined by applying many restraints because of the poor quality of the reflection data, 
   these restraints are required for the correct analysis.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.2000P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Flack x determined using 363 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.3(2)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         9394
_refine_ls_number_parameters     613
_refine_ls_number_restraints     577
_refine_ls_R_factor_all          0.3692
_refine_ls_R_factor_gt           0.1291
_refine_ls_wR_factor_ref         0.4925
_refine_ls_wR_factor_gt          0.3138
_refine_ls_goodness_of_fit_ref   0.954
_refine_ls_restrained_S_all      1.025
_refine_ls_shift/su_max          1.267
_refine_ls_shift/su_mean         0.269

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
Si01 Si 0.46705(17) 0.4937(5) 0.6721(3) 0.227(2) Uani 1 1 d D U . . .
Si02 Si 0.13179(17) 0.4969(5) 0.2095(3) 0.231(3) Uani 1 1 d D . . . .
C01 C 0.4098(4) 0.4872(10) 0.5973(9) 0.201(7) Uani 1 1 d D U . . .
C02 C 0.3771(6) 0.523(2) 0.6007(10) 0.312(14) Uani 1 1 d D U . . .
H02 H 0.3831 0.5437 0.6524 0.375 Uiso 1 1 calc R U . . .
C03 C 0.3385(6) 0.533(2) 0.5450(13) 0.312(15) Uani 1 1 d D U . . .
H03 H 0.3216 0.5861 0.5534 0.374 Uiso 1 1 calc R U . . .
C04 C 0.3213(5) 0.4731(11) 0.4764(11) 0.176(5) Uani 1 1 d D U . . .
C05 C 0.3498(5) 0.433(2) 0.4600(14) 0.367(15) Uani 1 1 d D U . . .
H05 H 0.3420 0.4069 0.4081 0.441 Uiso 1 1 calc R U . . .
C06 C 0.3919(5) 0.432(2) 0.5228(12) 0.339(15) Uani 1 1 d D U . . .
H06 H 0.4104 0.3889 0.5129 0.407 Uiso 1 1 calc R U . . .
C07 C 0.2761(5) 0.4765(13) 0.4101(10) 0.190(5) Uani 1 1 d D U . . .
C08 C 0.2444(5) 0.4169(18) 0.4123(11) 0.377(16) Uani 1 1 d D U . . .
H08 H 0.2522 0.3716 0.4588 0.452 Uiso 1 1 calc R U . . .
C09 C 0.2025(5) 0.417(2) 0.3534(12) 0.318(13) Uani 1 1 d D U . . .
H09 H 0.1835 0.3726 0.3614 0.382 Uiso 1 1 calc R U . . .
C10 C 0.1882(5) 0.4791(15) 0.2845(8) 0.215(7) Uani 1 1 d D U . . .
C11 C 0.2189(6) 0.544(2) 0.2802(14) 0.387(18) Uani 1 1 d D U . . .
H11 H 0.2107 0.6052 0.2415 0.465 Uiso 1 1 calc R U . . .
C12 C 0.2626(6) 0.521(2) 0.3333(12) 0.362(16) Uani 1 1 d D U . . .
H12 H 0.2819 0.5346 0.3167 0.434 Uiso 1 1 calc R U . . .
C13 C 0.4915(6) 0.3355(18) 0.6836(15) 0.339(11) Uani 1 1 d D U . . .
H13A H 0.4840 0.3045 0.6305 0.407 Uiso 1 1 calc R U . . .
H13B H 0.5221 0.3406 0.7168 0.407 Uiso 1 1 calc R U . . .
C14 C 0.4761(9) 0.256(2) 0.7207(18) 0.369(14) Uani 1 1 d D U . . .
H14A H 0.4454 0.2510 0.6902 0.443 Uiso 1 1 calc R U . . .
H14B H 0.4861 0.2783 0.7767 0.443 Uiso 1 1 calc R U . . .
C15 C 0.4979(7) 0.136(2) 0.7141(16) 0.350(11) Uani 1 1 d D U . . .
H15A H 0.4932 0.1255 0.6598 0.421 Uiso 1 1 calc R U . . .
H15B H 0.5281 0.1355 0.7533 0.421 Uiso 1 1 calc R U . . .
C16 C 0.4759(9) 0.040(2) 0.7331(17) 0.373(12) Uani 1 1 d D U . . .
H16A H 0.4695 0.0651 0.7740 0.447 Uiso 1 1 calc R U . . .
H16B H 0.4911 -0.0361 0.7484 0.447 Uiso 1 1 calc R U . . .
C17 C 0.4373(10) 0.038(3) 0.648(2) 0.477(18) Uani 1 1 d D U . . .
H17A H 0.4455 0.0480 0.6083 0.572 Uiso 1 1 calc R U . . .
H17B H 0.4182 0.1031 0.6419 0.572 Uiso 1 1 calc R U . . .
C18 C 0.4170(9) -0.075(2) 0.638(2) 0.443(14) Uani 1 1 d D U . . .
H18A H 0.4260 -0.1138 0.6897 0.531 Uiso 1 1 calc R U . . .
H18B H 0.4226 -0.1294 0.6046 0.531 Uiso 1 1 calc R U . . .
C19 C 0.3703(9) -0.040(4) 0.594(2) 0.521(19) Uani 1 1 d D U . . .
H19A H 0.3577 -0.0594 0.6267 0.626 Uiso 1 1 calc R U . . .
H19B H 0.3662 0.0452 0.5805 0.626 Uiso 1 1 calc R U . . .
C20 C 0.3526(12) -0.120(4) 0.519(3) 0.60(2) Uani 1 1 d D U . . .
H20A H 0.3425 -0.1977 0.5247 0.719 Uiso 1 1 calc R U . . .
H20B H 0.3715 -0.1283 0.4981 0.719 Uiso 1 1 calc R U . . .
C21 C 0.3158(16) -0.021(4) 0.471(3) 0.67(3) Uani 1 1 d D U . . .
H21A H 0.3017 0.0021 0.4997 0.800 Uiso 1 1 calc R U . . .
H21B H 0.3249 0.0491 0.4540 0.800 Uiso 1 1 calc R U . . .
C22 C 0.2898(12) -0.114(4) 0.400(3) 0.63(2) Uani 1 1 d D U . . .
H22A H 0.2795 -0.1837 0.4156 0.753 Uiso 1 1 calc R U . . .
H22B H 0.3029 -0.1364 0.3696 0.753 Uiso 1 1 calc R U . . .
C23 C 0.2573(11) -0.004(3) 0.363(3) 0.60(2) Uani 1 1 d D U . . .
H23A H 0.2489 0.0278 0.4000 0.721 Uiso 1 1 calc R U . . .
H23B H 0.2663 0.0598 0.3412 0.721 Uiso 1 1 calc R U . . .
C24 C 0.2249(10) -0.090(3) 0.299(3) 0.510(19) Uani 1 1 d D U . . .
H24A H 0.2270 -0.1709 0.3202 0.612 Uiso 1 1 calc R U . . .
H24B H 0.2270 -0.0928 0.2509 0.612 Uiso 1 1 calc R U . . .
C25 C 0.1849(10) -0.025(3) 0.284(2) 0.50(2) Uani 1 1 d D U . . .
H25A H 0.1674 -0.0773 0.2948 0.601 Uiso 1 1 calc R U . . .
H25B H 0.1917 0.0474 0.3167 0.601 Uiso 1 1 calc R U . . .
C26 C 0.1627(10) 0.007(3) 0.193(2) 0.480(17) Uani 1 1 d D U . . .
H26A H 0.1620 -0.0596 0.1588 0.576 Uiso 1 1 calc R U . . .
H26B H 0.1730 0.0801 0.1813 0.576 Uiso 1 1 calc R U . . .
C27 C 0.1193(9) 0.024(3) 0.193(2) 0.470(17) Uani 1 1 d D U . . .
H27A H 0.1011 -0.0466 0.1701 0.564 Uiso 1 1 calc R U . . .
H27B H 0.1247 0.0393 0.2468 0.564 Uiso 1 1 calc R U . . .
C28 C 0.1012(8) 0.128(2) 0.140(2) 0.430(15) Uani 1 1 d D U . . .
H28A H 0.0726 0.1347 0.1298 0.517 Uiso 1 1 calc R U . . .
H28B H 0.0982 0.1049 0.0887 0.517 Uiso 1 1 calc R U . . .
C29 C 0.1184(8) 0.262(2) 0.1552(18) 0.374(14) Uani 1 1 d D U . . .
H29A H 0.1486 0.2572 0.1942 0.449 Uiso 1 1 calc R U . . .
H29B H 0.1152 0.2898 0.1045 0.449 Uiso 1 1 calc R U . . .
C30 C 0.1018(7) 0.355(2) 0.1833(15) 0.327(12) Uani 1 1 d D U . . .
H30A H 0.1016 0.3263 0.2308 0.393 Uiso 1 1 calc R U . . .
H30B H 0.0727 0.3716 0.1411 0.393 Uiso 1 1 calc R U . . .
C31 C 0.4713(6) 0.575(2) 0.7630(10) 0.308(11) Uani 1 1 d D U . . .
H31A H 0.4551 0.6489 0.7442 0.370 Uiso 1 1 calc R U . . .
H31B H 0.4586 0.5244 0.7860 0.370 Uiso 1 1 calc R U . . .
C32 C 0.5139(5) 0.604(2) 0.8264(10) 0.331(11) Uani 1 1 d D U . . .
H32A H 0.5238 0.6674 0.8052 0.397 Uiso 1 1 calc R U . . .
H32B H 0.5312 0.5334 0.8340 0.397 Uiso 1 1 calc R U . . .
C33 C 0.5244(8) 0.644(3) 0.9093(13) 0.427(15) Uani 1 1 d D U . . .
H33A H 0.5391 0.5780 0.9471 0.512 Uiso 1 1 calc R U . . .
H33B H 0.5438 0.7113 0.9258 0.512 Uiso 1 1 calc R U . . .
C34 C 0.4879(10) 0.680(3) 0.9170(18) 0.419(14) Uani 1 1 d D U . . .
H34A H 0.4929 0.6669 0.9713 0.503 Uiso 1 1 calc R U . . .
H34B H 0.4616 0.6413 0.8769 0.503 Uiso 1 1 calc R U . . .
C35 C 0.4899(9) 0.813(3) 0.898(2) 0.452(14) Uani 1 1 d D U . . .
H35A H 0.4743 0.8285 0.8403 0.542 Uiso 1 1 calc R U . . .
H35B H 0.5189 0.8402 0.9217 0.542 Uiso 1 1 calc R U . . .
C36 C 0.4683(10) 0.873(3) 0.9409(18) 0.485(16) Uani 1 1 d D U . . .
H36A H 0.4867 0.8697 0.9997 0.582 Uiso 1 1 calc R U . . .
H36B H 0.4616 0.9571 0.9246 0.582 Uiso 1 1 calc R U . . .
C37 C 0.4282(10) 0.801(3) 0.914(2) 0.466(14) Uani 1 1 d D U . . .
H37A H 0.4329 0.7172 0.9059 0.559 Uiso 1 1 calc R U . . .
H37B H 0.4204 0.8051 0.9546 0.559 Uiso 1 1 calc R U . . .
C38 C 0.3934(10) 0.853(3) 0.835(2) 0.451(14) Uani 1 1 d D U . . .
H38A H 0.4022 0.8608 0.7956 0.541 Uiso 1 1 calc R U . . .
H38B H 0.3845 0.9311 0.8435 0.541 Uiso 1 1 calc R U . . .
C39 C 0.3575(11) 0.758(3) 0.807(2) 0.480(15) Uani 1 1 d D U . . .
H39A H 0.3661 0.6805 0.7967 0.575 Uiso 1 1 calc R U . . .
H39B H 0.3492 0.7483 0.8469 0.575 Uiso 1 1 calc R U . . .
C40 C 0.3220(11) 0.814(4) 0.729(3) 0.53(2) Uani 1 1 d D U . . .
H40A H 0.3307 0.8288 0.6898 0.641 Uiso 1 1 calc R U . . .
H40B H 0.3116 0.8880 0.7391 0.641 Uiso 1 1 calc R U . . .
C41 C 0.2878(12) 0.709(3) 0.699(3) 0.54(2) Uani 1 1 d D U . . .
H41A H 0.2981 0.6336 0.6899 0.646 Uiso 1 1 calc R U . . .
H41B H 0.2778 0.6958 0.7364 0.646 Uiso 1 1 calc R U . . .
C42 C 0.2547(11) 0.769(3) 0.620(2) 0.472(15) Uani 1 1 d D U . . .
H42A H 0.2485 0.8490 0.6317 0.567 Uiso 1 1 calc R U . . .
H42B H 0.2654 0.7760 0.5839 0.567 Uiso 1 1 calc R U . . .
C43 C 0.2150(12) 0.694(4) 0.581(2) 0.492(16) Uani 1 1 d D U . . .
H43A H 0.2210 0.6130 0.5700 0.590 Uiso 1 1 calc R U . . .
H43B H 0.2038 0.6875 0.6169 0.590 Uiso 1 1 calc R U . . .
C44 C 0.1859(11) 0.750(3) 0.509(2) 0.469(15) Uani 1 1 d D U . . .
H44A H 0.2003 0.7786 0.4819 0.562 Uiso 1 1 calc R U . . .
H44B H 0.1744 0.8203 0.5217 0.562 Uiso 1 1 calc R U . . .
C45 C 0.1499(14) 0.668(3) 0.452(2) 0.519(16) Uani 1 1 d D U . . .
H45A H 0.1368 0.6373 0.4815 0.622 Uiso 1 1 calc R U . . .
H45B H 0.1619 0.5994 0.4398 0.622 Uiso 1 1 calc R U . . .
C46 C 0.1144(11) 0.721(3) 0.371(2) 0.495(15) Uani 1 1 d D U . . .
H46A H 0.1125 0.8080 0.3750 0.594 Uiso 1 1 calc R U . . .
H46B H 0.0872 0.6855 0.3555 0.594 Uiso 1 1 calc R U . . .
C47 C 0.1276(10) 0.688(2) 0.3065(19) 0.442(14) Uani 1 1 d D U . . .
H47A H 0.1208 0.7549 0.2688 0.530 Uiso 1 1 calc R U . . .
H47B H 0.1579 0.6739 0.3342 0.530 Uiso 1 1 calc R U . . .
C48 C 0.1041(7) 0.577(3) 0.2608(16) 0.368(12) Uani 1 1 d D U . . .
H48A H 0.0754 0.5987 0.2192 0.442 Uiso 1 1 calc R U . . .
H48B H 0.1025 0.5210 0.2980 0.442 Uiso 1 1 calc R U . . .
C49 C 0.4905(8) 0.562(3) 0.6330(16) 0.368(12) Uani 1 1 d D U . . .
C50 C 0.4882(10) 0.683(3) 0.5975(16) 0.437(15) Uani 1 1 d D U . . .
H50A H 0.5141 0.7295 0.6257 0.525 Uiso 1 1 calc R U . . .
H50B H 0.4637 0.7303 0.5864 0.525 Uiso 1 1 calc R U . . .
C51 C 0.4825(10) 0.608(3) 0.5226(18) 0.446(13) Uani 1 1 d D U . . .
H51A H 0.5079 0.5636 0.5350 0.535 Uiso 1 1 calc R U . . .
H51B H 0.4583 0.5541 0.5001 0.535 Uiso 1 1 calc R U . . .
C52 C 0.4748(9) 0.721(3) 0.4675(18) 0.476(14) Uani 1 1 d D U . . .
H52A H 0.4917 0.7895 0.4992 0.571 Uiso 1 1 calc R U . . .
H52B H 0.4809 0.7034 0.4251 0.571 Uiso 1 1 calc R U . . .
C53 C 0.4286(9) 0.743(3) 0.4329(19) 0.453(15) Uani 1 1 d D U . . .
H53A H 0.4219 0.8287 0.4272 0.544 Uiso 1 1 calc R U . . .
H53B H 0.4185 0.7052 0.4652 0.544 Uiso 1 1 calc R U . . .
C54 C 0.4111(9) 0.681(3) 0.3506(19) 0.427(13) Uani 1 1 d D U . . .
H54A H 0.4104 0.5940 0.3536 0.512 Uiso 1 1 calc R U . . .
H54B H 0.4253 0.7061 0.3221 0.512 Uiso 1 1 calc R U . . .
C55 C 0.3675(11) 0.740(4) 0.317(2) 0.502(18) Uani 1 1 d D U . . .
H55A H 0.3572 0.7294 0.3537 0.602 Uiso 1 1 calc R U . . .
H55B H 0.3686 0.8261 0.3075 0.602 Uiso 1 1 calc R U . . .
C56 C 0.3407(11) 0.675(3) 0.239(2) 0.476(17) Uani 1 1 d D U . . .
H56A H 0.3190 0.6266 0.2402 0.571 Uiso 1 1 calc R U . . .
H56B H 0.3572 0.6249 0.2244 0.571 Uiso 1 1 calc R U . . .
C57 C 0.3216(10) 0.792(3) 0.182(2) 0.471(17) Uani 1 1 d D U . . .
H57A H 0.3289 0.8654 0.2141 0.566 Uiso 1 1 calc R U . . .
H57B H 0.3311 0.7974 0.1438 0.566 Uiso 1 1 calc R U . . .
C58 C 0.2745(9) 0.765(3) 0.1400(17) 0.430(15) Uani 1 1 d D U . . .
H58A H 0.2640 0.7843 0.1758 0.516 Uiso 1 1 calc R U . . .
H58B H 0.2693 0.6799 0.1261 0.516 Uiso 1 1 calc R U . . .
C59 C 0.2514(9) 0.844(3) 0.0614(18) 0.441(16) Uani 1 1 d D U . . .
H59A H 0.2496 0.9275 0.0740 0.529 Uiso 1 1 calc R U . . .
H59B H 0.2652 0.8387 0.0302 0.529 Uiso 1 1 calc R U . . .
C60 C 0.2070(10) 0.783(3) 0.016(2) 0.54(2) Uani 1 1 d D U . . .
H60A H 0.2032 0.7387 -0.0311 0.643 Uiso 1 1 calc R U . . .
H60B H 0.2043 0.7265 0.0516 0.643 Uiso 1 1 calc R U . . .
C61 C 0.1749(10) 0.878(3) -0.010(2) 0.480(16) Uani 1 1 d D U . . .
H61A H 0.1790 0.9356 -0.0435 0.576 Uiso 1 1 calc R U . . .
H61B H 0.1789 0.9203 0.0375 0.576 Uiso 1 1 calc R U . . .
C62 C 0.1287(9) 0.830(2) -0.0592(14) 0.453(14) Uani 1 1 d D U . . .
H62A H 0.1126 0.9031 -0.0665 0.544 Uiso 1 1 calc R U . . .
H62B H 0.1253 0.8150 -0.1121 0.544 Uiso 1 1 calc R U . . .
C63 C 0.1000(10) 0.734(4) -0.0563(17) 0.501(17) Uani 1 1 d D U . . .
H63A H 0.0718 0.7406 -0.1041 0.601 Uiso 1 1 calc R U . . .
H63B H 0.1109 0.6541 -0.0565 0.601 Uiso 1 1 calc R U . . .
C64 C 0.0977(10) 0.749(2) 0.0187(19) 0.473(15) Uani 1 1 d D U . . .
H64A H 0.0770 0.8090 0.0119 0.567 Uiso 1 1 calc R U . . .
H64B H 0.1250 0.7680 0.0661 0.567 Uiso 1 1 calc R U . . .
C65 C 0.0824(6) 0.612(2) 0.0223(16) 0.398(13) Uani 1 1 d D U . . .
H65A H 0.0566 0.6106 0.0239 0.478 Uiso 1 1 calc R U . . .
H65B H 0.0790 0.5621 -0.0224 0.478 Uiso 1 1 calc R U . . .
C66 C 0.1227(7) 0.574(2) 0.1066(13) 0.320(10) Uani 1 1 d D U . . .
H66A H 0.1390 0.6479 0.1257 0.384 Uiso 1 1 calc R U . . .
H66B H 0.1384 0.5219 0.0908 0.384 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
Si01 C49 1.60(3) . ?
Si01 C01 1.839(13) . ?
Si01 C31 1.894(17) . ?
Si01 C13 1.928(17) . ?
Si02 C30 1.83(2) . ?
Si02 C10 1.829(18) . ?
Si02 C48 1.958(16) . ?
Si02 C66 2.01(2) . ?
C01 C02 1.300(15) . ?
C01 C06 1.368(15) . ?
C02 C03 1.27(2) . ?
C02 H02 0.9300 . ?
C03 C04 1.309(18) . ?
C03 H03 0.9300 . ?
C04 C05 1.319(16) . ?
C04 C07 1.485(15) . ?
C05 C06 1.389(16) . ?
C05 H05 0.9300 . ?
C06 H06 0.9300 . ?
C07 C08 1.362(15) . ?
C07 C12 1.377(16) . ?
C08 C09 1.365(15) . ?
C08 H08 0.9300 . ?
C09 C10 1.335(15) . ?
C09 H09 0.9300 . ?
C10 C11 1.380(16) . ?
C11 C12 1.417(18) . ?
C11 H11 0.9300 . ?
C12 H12 0.9300 . ?
C13 C14 1.420(19) . ?
C13 H13A 0.9700 . ?
C13 H13B 0.9700 . ?
C14 C15 1.60(2) . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C15 C16 1.489(19) . ?
C15 H15A 0.9700 . ?
C15 H15B 0.9700 . ?
C16 C17 1.51(2) . ?
C16 H16A 0.9700 . ?
C16 H16B 0.9700 . ?
C17 C18 1.42(2) . ?
C17 H17A 0.9700 . ?
C17 H17B 0.9700 . ?
C18 C19 1.53(2) . ?
C18 H18A 0.9700 . ?
C18 H18B 0.9700 . ?
C19 C20 1.53(2) . ?
C19 H19A 0.9700 . ?
C19 H19B 0.9700 . ?
C20 C21 1.61(2) . ?
C20 H20A 0.9700 . ?
C20 H20B 0.9700 . ?
C21 C22 1.57(2) . ?
C21 H21A 0.9700 . ?
C21 H21B 0.9700 . ?
C22 C23 1.59(2) . ?
C22 H22A 0.9700 . ?
C22 H22B 0.9700 . ?
C23 C24 1.52(2) . ?
C23 H23A 0.9700 . ?
C23 H23B 0.9700 . ?
C24 C25 1.53(2) . ?
C24 H24A 0.9700 . ?
C24 H24B 0.9700 . ?
C25 C26 1.54(2) . ?
C25 H25A 0.9700 . ?
C25 H25B 0.9700 . ?
C26 C27 1.61(2) . ?
C26 H26A 0.9700 . ?
C26 H26B 0.9700 . ?
C27 C28 1.45(2) . ?
C27 H27A 0.9700 . ?
C27 H27B 0.9700 . ?
C28 C29 1.57(2) . ?
C28 H28A 0.9700 . ?
C28 H28B 0.9700 . ?
C29 C30 1.443(18) . ?
C29 H29A 0.9700 . ?
C29 H29B 0.9700 . ?
C30 H30A 0.9700 . ?
C30 H30B 0.9700 . ?
C31 C32 1.441(16) . ?
C31 H31A 0.9700 . ?
C31 H31B 0.9700 . ?
C32 C33 1.496(18) . ?
C32 H32A 0.9700 . ?
C32 H32B 0.9700 . ?
C33 C34 1.48(2) . ?
C33 H33A 0.9700 . ?
C33 H33B 0.9700 . ?
C34 C35 1.53(2) . ?
C34 H34A 0.9700 . ?
C34 H34B 0.9700 . ?
C35 C36 1.56(2) . ?
C35 H35A 0.9700 . ?
C35 H35B 0.9700 . ?
C36 C37 1.51(2) . ?
C36 H36A 0.9700 . ?
C36 H36B 0.9700 . ?
C37 C38 1.50(2) . ?
C37 H37A 0.9700 . ?
C37 H37B 0.9700 . ?
C38 C39 1.55(2) . ?
C38 H38A 0.9700 . ?
C38 H38B 0.9700 . ?
C39 C40 1.52(2) . ?
C39 H39A 0.9700 . ?
C39 H39B 0.9700 . ?
C40 C41 1.58(2) . ?
C40 H40A 0.9700 . ?
C40 H40B 0.9700 . ?
C41 C42 1.52(2) . ?
C41 H41A 0.9700 . ?
C41 H41B 0.9700 . ?
C42 C43 1.50(2) . ?
C42 H42A 0.9700 . ?
C42 H42B 0.9700 . ?
C43 C44 1.38(4) . ?
C43 H43A 0.9700 . ?
C43 H43B 0.9700 . ?
C44 C45 1.51(2) . ?
C44 H44A 0.9700 . ?
C44 H44B 0.9700 . ?
C45 C46 1.54(2) . ?
C45 H45A 0.9700 . ?
C45 H45B 0.9700 . ?
C46 C47 1.59(2) . ?
C46 H46A 0.9700 . ?
C46 H46B 0.9700 . ?
C47 C48 1.502(19) . ?
C47 H47A 0.9700 . ?
C47 H47B 0.9700 . ?
C48 H48A 0.9700 . ?
C48 H48B 0.9700 . ?
C49 C50 1.48(2) . ?
C49 C51 2.05(3) . ?
C50 C51 1.57(2) . ?
C50 H50A 0.9700 . ?
C50 H50B 0.9700 . ?
C51 C52 1.57(2) . ?
C51 H51A 0.9700 . ?
C51 H51B 0.9700 . ?
C52 C53 1.49(2) . ?
C52 H52A 0.9700 . ?
C52 H52B 0.9700 . ?
C53 C54 1.52(2) . ?
C53 H53A 0.9700 . ?
C53 H53B 0.9700 . ?
C54 C55 1.53(2) . ?
C54 H54A 0.9700 . ?
C54 H54B 0.9700 . ?
C55 C56 1.48(2) . ?
C55 H55A 0.9700 . ?
C55 H55B 0.9700 . ?
C56 C57 1.60(2) . ?
C56 H56A 0.9700 . ?
C56 H56B 0.9700 . ?
C57 C58 1.52(2) . ?
C57 H57A 0.9700 . ?
C57 H57B 0.9700 . ?
C58 C59 1.56(2) . ?
C58 H58A 0.9700 . ?
C58 H58B 0.9700 . ?
C59 C60 1.55(2) . ?
C59 H59A 0.9700 . ?
C59 H59B 0.9700 . ?
C60 C61 1.46(2) . ?
C60 H60A 0.9700 . ?
C60 H60B 0.9700 . ?
C61 C62 1.55(2) . ?
C61 H61A 0.9700 . ?
C61 H61B 0.9700 . ?
C62 C63 1.52(2) . ?
C62 H62A 0.9700 . ?
C62 H62B 0.9700 . ?
C63 C64 1.49(2) . ?
C63 H63A 0.9700 . ?
C63 H63B 0.9700 . ?
C64 C65 1.631(19) . ?
C64 H64A 0.9700 . ?
C64 H64B 0.9700 . ?
C65 C66 1.586(18) . ?
C65 H65A 0.9700 . ?
C65 H65B 0.9700 . ?
C66 H66A 0.9700 . ?
C66 H66B 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
C49 Si01 C01 109.5(10) . . ?
C49 Si01 C31 113.6(15) . . ?
C01 Si01 C31 104.7(8) . . ?
C49 Si01 C13 98.6(14) . . ?
C01 Si01 C13 109.5(7) . . ?
C31 Si01 C13 120.9(11) . . ?
C30 Si02 C10 113.8(9) . . ?
C30 Si02 C48 97.3(12) . . ?
C10 Si02 C48 109.3(9) . . ?
C30 Si02 C66 108.7(11) . . ?
C10 Si02 C66 111.3(9) . . ?
C48 Si02 C66 115.9(12) . . ?
C02 C01 C06 103.1(14) . . ?
C02 C01 Si01 131.9(14) . . ?
C06 C01 Si01 124.8(12) . . ?
C03 C02 C01 130.7(17) . . ?
C03 C02 H02 114.7 . . ?
C01 C02 H02 114.6 . . ?
C02 C03 C04 123.4(18) . . ?
C02 C03 H03 118.2 . . ?
C04 C03 H03 118.4 . . ?
C03 C04 C05 112.2(17) . . ?
C03 C04 C07 126.6(15) . . ?
C05 C04 C07 118.9(15) . . ?
C04 C05 C06 117.8(18) . . ?
C04 C05 H05 121.0 . . ?
C06 C05 H05 121.1 . . ?
C01 C06 C05 128.5(15) . . ?
C01 C06 H06 115.8 . . ?
C05 C06 H06 115.7 . . ?
C08 C07 C12 111.4(17) . . ?
C08 C07 C04 124.1(13) . . ?
C12 C07 C04 123.4(15) . . ?
C07 C08 C09 126.7(17) . . ?
C07 C08 H08 116.6 . . ?
C09 C08 H08 116.7 . . ?
C10 C09 C08 121.1(18) . . ?
C10 C09 H09 119.4 . . ?
C08 C09 H09 119.5 . . ?
C09 C10 C11 114.5(16) . . ?
C09 C10 Si02 122.7(15) . . ?
C11 C10 Si02 122.1(14) . . ?
C10 C11 C12 121.5(16) . . ?
C10 C11 H11 119.0 . . ?
C12 C11 H11 119.5 . . ?
C07 C12 C11 118.9(18) . . ?
C07 C12 H12 120.7 . . ?
C11 C12 H12 120.4 . . ?
C14 C13 Si01 109.5(17) . . ?
C14 C13 H13A 109.8 . . ?
Si01 C13 H13A 109.3 . . ?
C14 C13 H13B 110.2 . . ?
Si01 C13 H13B 109.8 . . ?
H13A C13 H13B 108.2 . . ?
C13 C14 C15 97.3(19) . . ?
C13 C14 H14A 112.5 . . ?
C15 C14 H14A 112.1 . . ?
C13 C14 H14B 112.0 . . ?
C15 C14 H14B 112.8 . . ?
H14A C14 H14B 109.7 . . ?
C16 C15 C14 102(2) . . ?
C16 C15 H15A 111.1 . . ?
C14 C15 H15A 112.3 . . ?
C16 C15 H15B 110.5 . . ?
C14 C15 H15B 111.3 . . ?
H15A C15 H15B 109.3 . . ?
C15 C16 C17 94(2) . . ?
C15 C16 H16A 111.8 . . ?
C17 C16 H16A 112.4 . . ?
C15 C16 H16B 114.2 . . ?
C17 C16 H16B 113.1 . . ?
H16A C16 H16B 110.2 . . ?
C16 C17 C18 108(2) . . ?
C16 C17 H17A 110.1 . . ?
C18 C17 H17A 110.1 . . ?
C16 C17 H17B 110.6 . . ?
C18 C17 H17B 110.0 . . ?
H17A C17 H17B 108.5 . . ?
C17 C18 C19 102(2) . . ?
C17 C18 H18A 111.3 . . ?
C19 C18 H18A 110.1 . . ?
C17 C18 H18B 111.6 . . ?
C19 C18 H18B 112.1 . . ?
H18A C18 H18B 109.4 . . ?
C20 C19 C18 100(2) . . ?
C20 C19 H19A 113.0 . . ?
C18 C19 H19A 113.1 . . ?
C20 C19 H19B 110.3 . . ?
C18 C19 H19B 110.6 . . ?
H19A C19 H19B 109.4 . . ?
C19 C20 C21 88(2) . . ?
C19 C20 H20A 112.4 . . ?
C21 C20 H20A 110.6 . . ?
C19 C20 H20B 114.7 . . ?
C21 C20 H20B 117.9 . . ?
H20A C20 H20B 111.1 . . ?
C22 C21 C20 91(2) . . ?
C22 C21 H21A 116.9 . . ?
C20 C21 H21A 117.2 . . ?
C22 C21 H21B 109.9 . . ?
C20 C21 H21B 109.7 . . ?
H21A C21 H21B 110.9 . . ?
C21 C22 C23 83(2) . . ?
C21 C22 H22A 111.2 . . ?
C23 C22 H22A 112.0 . . ?
C21 C22 H22B 118.4 . . ?
C23 C22 H22B 117.6 . . ?
H22A C22 H22B 112.0 . . ?
C24 C23 C22 89(2) . . ?
C24 C23 H23A 116.2 . . ?
C22 C23 H23A 116.1 . . ?
C24 C23 H23B 111.9 . . ?
C22 C23 H23B 110.8 . . ?
H23A C23 H23B 111.1 . . ?
C23 C24 C25 98(2) . . ?
C23 C24 H24A 111.3 . . ?
C25 C24 H24A 112.1 . . ?
C23 C24 H24B 114.4 . . ?
C25 C24 H24B 110.9 . . ?
H24A C24 H24B 109.7 . . ?
C26 C25 C24 103(3) . . ?
C26 C25 H25A 112.5 . . ?
C24 C25 H25A 111.5 . . ?
C26 C25 H25B 110.2 . . ?
C24 C25 H25B 110.4 . . ?
H25A C25 H25B 109.3 . . ?
C25 C26 C27 88(2) . . ?
C25 C26 H26A 112.6 . . ?
C27 C26 H26A 114.2 . . ?
C25 C26 H26B 115.0 . . ?
C27 C26 H26B 113.9 . . ?
H26A C26 H26B 111.0 . . ?
C28 C27 C26 101(3) . . ?
C28 C27 H27A 111.2 . . ?
C26 C27 H27A 111.3 . . ?
C28 C27 H27B 111.2 . . ?
C26 C27 H27B 112.3 . . ?
H27A C27 H27B 109.4 . . ?
C27 C28 C29 129(3) . . ?
C27 C28 H28A 105.9 . . ?
C29 C28 H28A 105.7 . . ?
C27 C28 H28B 104.6 . . ?
C29 C28 H28B 104.4 . . ?
H28A C28 H28B 105.9 . . ?
C30 C29 C28 122(3) . . ?
C30 C29 H29A 106.3 . . ?
C28 C29 H29A 106.8 . . ?
C30 C29 H29B 106.9 . . ?
C28 C29 H29B 107.1 . . ?
H29A C29 H29B 106.5 . . ?
C29 C30 Si02 113.9(18) . . ?
C29 C30 H30A 109.1 . . ?
Si02 C30 H30A 109.0 . . ?
C29 C30 H30B 108.5 . . ?
Si02 C30 H30B 108.5 . . ?
H30A C30 H30B 107.6 . . ?
C32 C31 Si01 114.8(15) . . ?
C32 C31 H31A 107.4 . . ?
Si01 C31 H31A 108.2 . . ?
C32 C31 H31B 109.5 . . ?
Si01 C31 H31B 109.1 . . ?
H31A C31 H31B 107.5 . . ?
C31 C32 C33 122.2(16) . . ?
C31 C32 H32A 107.9 . . ?
C33 C32 H32A 107.0 . . ?
C31 C32 H32B 106.0 . . ?
C33 C32 H32B 106.2 . . ?
H32A C32 H32B 106.7 . . ?
C34 C33 C32 116(2) . . ?
C34 C33 H33A 107.8 . . ?
C32 C33 H33A 108.8 . . ?
C34 C33 H33B 108.4 . . ?
C32 C33 H33B 108.2 . . ?
H33A C33 H33B 107.4 . . ?
C33 C34 C35 95(2) . . ?
C33 C34 H34A 113.2 . . ?
C35 C34 H34A 113.3 . . ?
C33 C34 H34B 112.7 . . ?
C35 C34 H34B 112.1 . . ?
H34A C34 H34B 110.2 . . ?
C34 C35 C36 101(2) . . ?
C34 C35 H35A 112.1 . . ?
C36 C35 H35A 112.1 . . ?
C34 C35 H35B 110.8 . . ?
C36 C35 H35B 111.4 . . ?
H35A C35 H35B 109.3 . . ?
C37 C36 C35 105(2) . . ?
C37 C36 H36A 111.6 . . ?
C35 C36 H36A 111.1 . . ?
C37 C36 H36B 110.1 . . ?
C35 C36 H36B 109.9 . . ?
H36A C36 H36B 108.7 . . ?
C38 C37 C36 109(2) . . ?
C38 C37 H37A 110.2 . . ?
C36 C37 H37A 109.9 . . ?
C38 C37 H37B 110.5 . . ?
C36 C37 H37B 108.9 . . ?
H37A C37 H37B 108.3 . . ?
C37 C38 C39 103(2) . . ?
C37 C38 H38A 111.7 . . ?
C39 C38 H38A 111.1 . . ?
C37 C38 H38B 111.0 . . ?
C39 C38 H38B 110.8 . . ?
H38A C38 H38B 108.9 . . ?
C40 C39 C38 103(2) . . ?
C40 C39 H39A 112.1 . . ?
C38 C39 H39A 111.3 . . ?
C40 C39 H39B 110.0 . . ?
C38 C39 H39B 111.6 . . ?
H39A C39 H39B 109.2 . . ?
C39 C40 C41 100(2) . . ?
C39 C40 H40A 110.3 . . ?
C41 C40 H40A 111.3 . . ?
C39 C40 H40B 112.4 . . ?
C41 C40 H40B 112.8 . . ?
H40A C40 H40B 109.4 . . ?
C42 C41 C40 97(2) . . ?
C42 C41 H41A 113.8 . . ?
C40 C41 H41A 113.3 . . ?
C42 C41 H41B 111.0 . . ?
C40 C41 H41B 111.7 . . ?
H41A C41 H41B 109.7 . . ?
C43 C42 C41 110(2) . . ?
C43 C42 H42A 111.6 . . ?
C41 C42 H42A 111.3 . . ?
C43 C42 H42B 107.5 . . ?
C41 C42 H42B 108.4 . . ?
H42A C42 H42B 108.2 . . ?
C44 C43 C42 108(3) . . ?
C44 C43 H43A 111.3 . . ?
C42 C43 H43A 112.3 . . ?
C44 C43 H43B 108.6 . . ?
C42 C43 H43B 108.2 . . ?
H43A C43 H43B 108.6 . . ?
C43 C44 C45 113(3) . . ?
C43 C44 H44A 107.5 . . ?
C45 C44 H44A 108.7 . . ?
C43 C44 H44B 110.5 . . ?
C45 C44 H44B 109.3 . . ?
H44A C44 H44B 107.9 . . ?
C44 C45 C46 118(3) . . ?
C44 C45 H45A 107.5 . . ?
C46 C45 H45A 107.9 . . ?
C44 C45 H45B 108.1 . . ?
C46 C45 H45B 107.7 . . ?
H45A C45 H45B 107.2 . . ?
C45 C46 C47 105(2) . . ?
C45 C46 H46A 110.6 . . ?
C47 C46 H46A 110.3 . . ?
C45 C46 H46B 111.0 . . ?
C47 C46 H46B 110.9 . . ?
H46A C46 H46B 108.9 . . ?
C48 C47 C46 109(2) . . ?
C48 C47 H47A 109.7 . . ?
C46 C47 H47A 110.6 . . ?
C48 C47 H47B 109.8 . . ?
C46 C47 H47B 109.4 . . ?
H47A C47 H47B 108.3 . . ?
C47 C48 Si02 111.7(17) . . ?
C47 C48 H48A 109.3 . . ?
Si02 C48 H48A 109.3 . . ?
C47 C48 H48B 109.0 . . ?
Si02 C48 H48B 109.4 . . ?
H48A C48 H48B 108.0 . . ?
C50 C49 Si01 137(3) . . ?
C50 C49 C51 50.0(12) . . ?
Si01 C49 C51 141.2(18) . . ?
C49 C50 C51 84.0(19) . . ?
C49 C50 H50A 113.3 . . ?
C51 C50 H50A 113.7 . . ?
C49 C50 H50B 116.2 . . ?
C51 C50 H50B 115.4 . . ?
H50A C50 H50B 111.7 . . ?
C52 C51 C50 95(2) . . ?
C52 C51 C49 141(2) . . ?
C50 C51 C49 46.0(10) . . ?
C52 C51 H51A 112.7 . . ?
C50 C51 H51A 113.5 . . ?
C49 C51 H51A 91.3 . . ?
C52 C51 H51B 112.8 . . ?
C50 C51 H51B 111.8 . . ?
C49 C51 H51B 84.6 . . ?
H51A C51 H51B 110.1 . . ?
C53 C52 C51 101(2) . . ?
C53 C52 H52A 111.0 . . ?
C51 C52 H52A 111.9 . . ?
C53 C52 H52B 111.3 . . ?
C51 C52 H52B 111.5 . . ?
H52A C52 H52B 109.5 . . ?
C52 C53 C54 99(2) . . ?
C52 C53 H53A 112.9 . . ?
C54 C53 H53A 112.7 . . ?
C52 C53 H53B 110.8 . . ?
C54 C53 H53B 111.2 . . ?
H53A C53 H53B 109.6 . . ?
C53 C54 C55 92.1(19) . . ?
C53 C54 H54A 114.0 . . ?
C55 C54 H54A 113.2 . . ?
C53 C54 H54B 112.7 . . ?
C55 C54 H54B 113.3 . . ?
H54A C54 H54B 110.5 . . ?
C56 C55 C54 103(2) . . ?
C56 C55 H55A 111.4 . . ?
C54 C55 H55A 111.3 . . ?
C56 C55 H55B 110.7 . . ?
C54 C55 H55B 111.2 . . ?
H55A C55 H55B 109.1 . . ?
C55 C56 C57 97(2) . . ?
C55 C56 H56A 112.1 . . ?
C57 C56 H56A 111.8 . . ?
C55 C56 H56B 112.4 . . ?
C57 C56 H56B 113.2 . . ?
H56A C56 H56B 110.0 . . ?
C58 C57 C56 101(2) . . ?
C58 C57 H57A 112.6 . . ?
C56 C57 H57A 111.9 . . ?
C58 C57 H57B 111.2 . . ?
C56 C57 H57B 110.8 . . ?
H57A C57 H57B 109.4 . . ?
C57 C58 C59 108(2) . . ?
C57 C58 H58A 109.5 . . ?
C59 C58 H58A 110.3 . . ?
C57 C58 H58B 111.1 . . ?
C59 C58 H58B 109.4 . . ?
H58A C58 H58B 108.4 . . ?
C60 C59 C58 101(2) . . ?
C60 C59 H59A 111.0 . . ?
C58 C59 H59A 111.1 . . ?
C60 C59 H59B 112.2 . . ?
C58 C59 H59B 111.7 . . ?
H59A C59 H59B 109.5 . . ?
C61 C60 C59 108(2) . . ?
C61 C60 H60A 108.9 . . ?
C59 C60 H60A 109.5 . . ?
C61 C60 H60B 111.9 . . ?
C59 C60 H60B 109.9 . . ?
H60A C60 H60B 108.4 . . ?
C60 C61 C62 114(2) . . ?
C60 C61 H61A 110.5 . . ?
C62 C61 H61A 110.1 . . ?
C60 C61 H61B 107.5 . . ?
C62 C61 H61B 107.2 . . ?
H61A C61 H61B 107.6 . . ?
C63 C62 C61 141(2) . . ?
C63 C62 H62A 101.9 . . ?
C61 C62 H62A 102.2 . . ?
C63 C62 H62B 101.8 . . ?
C61 C62 H62B 100.5 . . ?
H62A C62 H62B 104.8 . . ?
C64 C63 C62 110(2) . . ?
C64 C63 H63A 109.2 . . ?
C62 C63 H63A 110.2 . . ?
C64 C63 H63B 109.7 . . ?
C62 C63 H63B 109.4 . . ?
H63A C63 H63B 108.2 . . ?
C63 C64 C65 97(2) . . ?
C63 C64 H64A 112.5 . . ?
C65 C64 H64A 113.2 . . ?
C63 C64 H64B 111.7 . . ?
C65 C64 H64B 111.7 . . ?
H64A C64 H64B 109.9 . . ?
C66 C65 C64 97.3(16) . . ?
C66 C65 H65A 111.3 . . ?
C64 C65 H65A 111.4 . . ?
C66 C65 H65B 113.7 . . ?
C64 C65 H65B 112.7 . . ?
H65A C65 H65B 109.9 . . ?
C65 C66 Si02 135.0(17) . . ?
C65 C66 H66A 104.2 . . ?
Si02 C66 H66A 104.0 . . ?
C65 C66 H66B 102.3 . . ?
Si02 C66 H66B 103.1 . . ?
H66A C66 H66B 105.4 . . ?

_refine_diff_density_max         0.305
_refine_diff_density_min         -0.148
_refine_diff_density_rms         0.058

_shelxl_version_number           2013-4


_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: tetrahydrofuram/methanol=4:1'
_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_shelx_CCDC1
_audit_block_doi                 10.5517/ccdc.csd.cc1p5yyr
_database_code_depnum_ccdc_archive 'CCDC 1554865'
_audit_update_record             
;
2017-06-08 deposited with the CCDC.
2017-09-14 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT410_shelx               
;
PROBLEM: Short Intra H...H Contact   H31A   ..  H33A    .       1.82 Ang.
RESPONSE: Due to disordered position
;


_audit_creation_method           SHELXL-2013
_chemical_name_systematic        C18satBiphCage
_chemical_name_common            C18satBiphCage
_chemical_melting_point          "'274-276 deg.C'"
_chemical_formula_moiety         'C66 H116 Si2'
_chemical_formula_sum            'C66 H116 Si2'
_chemical_formula_weight         965.76

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

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'

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

_cell_length_a                   35.097(3)
_cell_length_b                   11.4728(10)
_cell_length_c                   16.9361(14)
_cell_angle_alpha                90
_cell_angle_beta                 110.8090(10)
_cell_angle_gamma                90
_cell_volume                     6374.6(9)
_cell_formula_units_Z            4
_cell_measurement_temperature    200(2)
_cell_measurement_reflns_used    3969
_cell_measurement_theta_min      2.48
_cell_measurement_theta_max      25.75

_exptl_crystal_description       prism
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.006
_exptl_crystal_F_000             2160
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.400
_exptl_crystal_size_min          0.050
_exptl_absorpt_coefficient_mu    0.091
_shelx_estimated_absorpt_T_min   0.964
_shelx_estimated_absorpt_T_max   0.995
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.902
_exptl_absorpt_correction_T_max  0.995
_exptl_absorpt_process_details   'SADABS Bruker'

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      200(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean 8.333
_diffrn_reflns_number            17101
_diffrn_reflns_av_unetI/netI     0.0337
_diffrn_reflns_av_R_equivalents  0.0242
_diffrn_reflns_limit_h_min       -40
_diffrn_reflns_limit_h_max       46
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         1.241
_diffrn_reflns_theta_max         27.932
_diffrn_reflns_theta_full        25.000
_diffrn_measured_fraction_theta_max 0.917
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.917
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.917
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             7008
_reflns_number_gt                4602
_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, 1997)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX (Farrugia, 1999)'

_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)+(0.1516P)²+5.6586P] 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         7008
_refine_ls_number_parameters     317
_refine_ls_number_restraints     67
_refine_ls_R_factor_all          0.1177
_refine_ls_R_factor_gt           0.0837
_refine_ls_wR_factor_ref         0.2783
_refine_ls_wR_factor_gt          0.2458
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_restrained_S_all      1.092
_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
Si01 Si 0.33658(2) 0.52809(7) 0.07844(4) 0.0445(3) Uani 1 1 d . . . . .
C01 C 0.39359(7) 0.5471(2) 0.12509(16) 0.0451(6) Uani 1 1 d . . . . .
C02 C 0.41161(8) 0.6459(2) 0.16925(17) 0.0481(6) Uani 1 1 d . . . . .
H02 H 0.3951 0.7123 0.1670 0.058 Uiso 1 1 calc R U . . .
C03 C 0.45306(8) 0.6521(2) 0.21690(17) 0.0472(6) Uani 1 1 d . . . . .
H03 H 0.4642 0.7221 0.2460 0.057 Uiso 1 1 calc R U . . .
C04 C 0.47818(7) 0.5576(2) 0.22234(17) 0.0471(6) Uani 1 1 d . . . . .
C05 C 0.46084(9) 0.4603(3) 0.1755(3) 0.0797(12) Uani 1 1 d . . . . .
H05 H 0.4776 0.3948 0.1767 0.096 Uiso 1 1 calc R U . . .
C06 C 0.41974(9) 0.4551(3) 0.1267(2) 0.0753(11) Uani 1 1 d . . . . .
H06 H 0.4092 0.3876 0.0938 0.090 Uiso 1 1 calc R U . . .
C07 C 0.32417(8) 0.4087(3) -0.00212(18) 0.0532(7) Uani 1 1 d . . . . .
H07A H 0.3392 0.4230 -0.0408 0.064 Uiso 1 1 calc R U . . .
H07B H 0.3340 0.3339 0.0271 0.064 Uiso 1 1 calc R U . . .
C08 C 0.27861(8) 0.3972(3) -0.0547(2) 0.0604(8) Uani 1 1 d . . . . .
H08A H 0.2631 0.4000 -0.0160 0.072 Uiso 1 1 calc R U . . .
H08B H 0.2702 0.4653 -0.0929 0.072 Uiso 1 1 calc R U . . .
C09 C 0.26702(10) 0.2869(3) -0.1072(2) 0.0708(9) Uani 1 1 d . . . . .
H09A H 0.2752 0.2188 -0.0690 0.085 Uiso 1 1 calc R U . . .
H09B H 0.2370 0.2846 -0.1349 0.085 Uiso 1 1 calc R U . . .
C10 C 0.28574(11) 0.2757(4) -0.1735(2) 0.0750(10) Uani 1 1 d . . . . .
H10A H 0.3157 0.2832 -0.1466 0.090 Uiso 1 1 calc R U . . .
H10B H 0.2760 0.3404 -0.2144 0.090 Uiso 1 1 calc R U . . .
C11 C 0.27566(10) 0.1584(3) -0.2219(2) 0.0708(10) Uani 1 1 d . . . . .
H11A H 0.2841 0.0937 -0.1806 0.085 Uiso 1 1 calc R U . . .
H11B H 0.2458 0.1529 -0.2513 0.085 Uiso 1 1 calc R U . . .
C12 C 0.29610(11) 0.1435(4) -0.2854(2) 0.0773(10) Uani 1 1 d . . . . .
H12A H 0.2853 0.2037 -0.3297 0.093 Uiso 1 1 calc R U . . .
H12B H 0.2881 0.0666 -0.3129 0.093 Uiso 1 1 calc R U . . .
C13 C 0.34224(11) 0.1512(4) -0.2523(2) 0.0757(10) Uani 1 1 d . . . . .
H13A H 0.3519 0.1398 -0.3000 0.091 Uiso 1 1 calc R U . . .
H13B H 0.3505 0.2304 -0.2294 0.091 Uiso 1 1 calc R U . . .
C14 C 0.36222(14) 0.0654(4) -0.1863(3) 0.0984(13) Uani 1 1 d . . . . .
H14A H 0.3532 -0.0136 -0.2086 0.118 Uiso 1 1 calc R U . . .
H14B H 0.3533 0.0787 -0.1378 0.118 Uiso 1 1 calc R U . . .
C15 C 0.40836(14) 0.0702(5) -0.1556(3) 0.1060(15) Uani 1 1 d . . . . .
H15A H 0.4194 0.0027 -0.1180 0.127 Uiso 1 1 calc R U . . .
H15B H 0.4171 0.0621 -0.2048 0.127 Uiso 1 1 calc R U . . .
C16 C 0.42678(12) 0.1797(4) -0.1088(3) 0.0905(13) Uani 1 1 d . . . . .
H16A H 0.4145 0.1958 -0.0657 0.109 Uiso 1 1 calc R U . . .
H16B H 0.4201 0.2458 -0.1490 0.109 Uiso 1 1 calc R U . . .
C17 C 0.47287(13) 0.1721(5) -0.0658(3) 0.0997(14) Uani 1 1 d . . . . .
H17A H 0.4792 0.1067 -0.0251 0.120 Uiso 1 1 calc R U . . .
H17B H 0.4848 0.1529 -0.1092 0.120 Uiso 1 1 calc R U . . .
C18 C 0.49305(12) 0.2775(5) -0.0209(3) 0.1018(15) Uani 1 1 d . . . . .
H18A H 0.4780 0.3059 0.0150 0.122 Uiso 1 1 calc R U . . .
H18B H 0.4917 0.3391 -0.0627 0.122 Uiso 1 1 calc R U . . .
C19 C 0.53716(13) 0.2575(5) 0.0339(3) 0.1061(16) Uani 1 1 d . . . . .
H19A H 0.5382 0.1944 0.0745 0.127 Uiso 1 1 calc R U . . .
H19B H 0.5519 0.2295 -0.0026 0.127 Uiso 1 1 calc R U . . .
C20 C 0.55943(12) 0.3601(5) 0.0824(3) 0.0973(14) Uani 1 1 d . . . . .
H20A H 0.5416 0.4018 0.1071 0.117 Uiso 1 1 calc R U . . .
H20B H 0.5659 0.4143 0.0434 0.117 Uiso 1 1 calc R U . . .
C21 C 0.59913(11) 0.3251(4) 0.1534(2) 0.0823(11) Uani 1 1 d . . . . .
H21A H 0.5923 0.2714 0.1922 0.099 Uiso 1 1 calc R U . . .
H21B H 0.6163 0.2814 0.1281 0.099 Uiso 1 1 calc R U . . .
C22 C 0.62340(10) 0.4224(4) 0.2035(2) 0.0791(11) Uani 1 1 d . . . . .
H22A H 0.6057 0.4699 0.2251 0.095 Uiso 1 1 calc R U . . .
H22B H 0.6322 0.4726 0.1656 0.095 Uiso 1 1 calc R U . . .
C23 C 0.66057(9) 0.3861(3) 0.2772(2) 0.0650(8) Uani 1 1 d . . . . .
H23A H 0.6800 0.3475 0.2552 0.078 Uiso 1 1 calc R U . . .
H23B H 0.6523 0.3282 0.3113 0.078 Uiso 1 1 calc R U . . .
C24 C 0.31752(8) 0.4875(3) 0.16520(19) 0.0579(7) Uani 1 1 d . . . . .
H24A H 0.3195 0.5571 0.2010 0.069 Uiso 1 1 calc R U . . .
H24B H 0.2883 0.4673 0.1392 0.069 Uiso 1 1 calc R U . . .
C25 C 0.31146(8) 0.6675(3) 0.03016(17) 0.0496(6) Uani 1 1 d . . . . .
H25A H 0.2816 0.6574 0.0125 0.060 Uiso 1 1 calc R U . . .
H25B H 0.3195 0.7289 0.0741 0.060 Uiso 1 1 calc R U . . .
C26 C 0.32135(10) 0.7102(3) -0.04596(19) 0.0619(8) Uani 1 1 d . . . . .
H26A H 0.3513 0.7130 -0.0301 0.074 Uiso 1 1 calc R U . . .
H26B H 0.3107 0.6527 -0.0922 0.074 Uiso 1 1 calc R U . . .
C27 C 0.30401(10) 0.8294(3) -0.0790(2) 0.0703(9) Uani 1 1 d . . . . .
H27A H 0.3113 0.8484 -0.1288 0.084 Uiso 1 1 calc R U . . .
H27B H 0.2739 0.8255 -0.0980 0.084 Uiso 1 1 calc R U . . .
C28 C 0.31870(12) 0.9266(3) -0.0153(2) 0.0774(10) Uani 1 1 d . . . . .
H28A H 0.3077 0.9140 0.0304 0.093 Uiso 1 1 calc R U . . .
H28B H 0.3076 1.0013 -0.0432 0.093 Uiso 1 1 calc R U . . .
C29 C 0.36480(13) 0.9362(4) 0.0235(2) 0.0899(12) Uani 1 1 d D . . . .
H29A H 0.3752 0.8648 0.0571 0.108 Uiso 1 1 calc R U . . .
H29B H 0.3757 0.9369 -0.0230 0.108 Uiso 1 1 calc R U . . .
C30 C 0.3817(2) 1.0372(5) 0.0779(3) 0.141(3) Uani 1 1 d . . . . .
H30A H 0.3689 1.0426 0.1213 0.169 Uiso 1 1 calc R U . . .
H30B H 0.3748 1.1091 0.0433 0.169 Uiso 1 1 calc R U . . .
C31 C 0.4283(2) 1.0295(7) 0.1218(4) 0.188(4) Uani 1 1 d D U . . .
H31A H 0.4340 0.9560 0.1546 0.226 Uiso 1 1 calc R U . . .
H31B H 0.4398 1.0200 0.0766 0.226 Uiso 1 1 calc R U . . .
C32 C 0.4512(3) 1.1160(8) 0.1756(5) 0.227(4) Uani 1 1 d D U . . .
H32A H 0.4425 1.1314 0.2242 0.273 Uiso 0.16(3) 1 calc R U P A 1
H32B H 0.4524 1.1895 0.1460 0.273 Uiso 0.16(3) 1 calc R U P A 1
H32C H 0.4384 1.1308 0.2182 0.273 Uiso 0.84(3) 1 calc R U P A 2
H32D H 0.4478 1.1881 0.1416 0.273 Uiso 0.84(3) 1 calc R U P A 2
C33 C 0.4940(5) 1.037(3) 0.2012(6) 0.242(13) Uani 0.16(3) 1 d D U P A 1
H33A H 0.4888 0.9572 0.1773 0.290 Uiso 0.16(3) 1 calc R U P A 1
H33B H 0.5149 1.0752 0.1834 0.290 Uiso 0.16(3) 1 calc R U P A 1
C133 C 0.4945(4) 1.1011(17) 0.2212(6) 0.268(8) Uani 0.84(3) 1 d D U P A 2
H13C H 0.5023 1.0263 0.2021 0.322 Uiso 0.84(3) 1 calc R U P A 2
H13D H 0.5085 1.1633 0.2015 0.322 Uiso 0.84(3) 1 calc R U P A 2


_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
Si01 C25 1.869(3) . ?
Si01 C07 1.872(3) . ?
Si01 C24 1.877(3) . ?
Si01 C01 1.885(3) . ?
C01 C02 1.381(4) . ?
C01 C06 1.392(4) . ?
C02 C03 1.393(3) . ?
C02 H02 0.9500 . ?
C03 C04 1.379(4) . ?
C03 H03 0.9500 . ?
C04 C05 1.380(4) . ?
C04 C04 1.485(5) 2_655 ?
C05 C06 1.386(4) . ?
C05 H05 0.9500 . ?
C06 H06 0.9500 . ?
C07 C08 1.535(4) . ?
C07 H07A 0.9900 . ?
C07 H07B 0.9900 . ?
C08 C09 1.517(5) . ?
C08 H08A 0.9900 . ?
C08 H08B 0.9900 . ?
C09 C10 1.494(5) . ?
C09 H09A 0.9900 . ?
C09 H09B 0.9900 . ?
C10 C11 1.550(5) . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C11 C12 1.500(5) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 C13 1.516(5) . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C13 C14 1.467(6) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C14 C15 1.516(6) . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C15 C16 1.503(6) . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C16 C17 1.522(5) . ?
C16 H16A 0.9900 . ?
C16 H16B 0.9900 . ?
C17 C18 1.470(7) . ?
C17 H17A 0.9900 . ?
C17 H17B 0.9900 . ?
C18 C19 1.513(5) . ?
C18 H18A 0.9900 . ?
C18 H18B 0.9900 . ?
C19 C20 1.488(6) . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C20 C21 1.536(5) . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C21 C22 1.475(5) . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C22 C23 1.509(4) . ?
C22 H22A 0.9900 . ?
C22 H22B 0.9900 . ?
C23 C24 1.537(4) 2_655 ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C24 C23 1.537(4) 2_655 ?
C24 H24A 0.9900 . ?
C24 H24B 0.9900 . ?
C25 C26 1.530(4) . ?
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?
C26 C27 1.520(5) . ?
C26 H26A 0.9900 . ?
C26 H26B 0.9900 . ?
C27 C28 1.509(5) . ?
C27 H27A 0.9900 . ?
C27 H27B 0.9900 . ?
C28 C29 1.519(5) . ?
C28 H28A 0.9900 . ?
C28 H28B 0.9900 . ?
C29 C30 1.467(6) . ?
C29 H29A 0.9900 . ?
C29 H29B 0.9900 . ?
C30 C31 1.541(9) . ?
C30 H30A 0.9900 . ?
C30 H30B 0.9900 . ?
C31 C32 1.393(8) . ?
C31 H31A 0.9900 . ?
C31 H31B 0.9900 . ?
C32 C133 1.451(13) . ?
C32 C33 1.677(17) . ?
C32 H32A 0.9900 . ?
C32 H32B 0.9900 . ?
C32 H32C 0.9900 . ?
C32 H32D 0.9900 . ?
C33 C33 1.55(2) 2_655 ?
C33 H33A 0.9900 . ?
C33 H33B 0.9900 . ?
C133 C133 0.91(2) 2_655 ?
C133 H13C 0.9900 . ?
C133 H13D 0.9900 . ?

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
C25 Si01 C07 110.85(13) . . ?
C25 Si01 C24 108.13(13) . . ?
C07 Si01 C24 109.49(15) . . ?
C25 Si01 C01 110.46(13) . . ?
C07 Si01 C01 109.13(12) . . ?
C24 Si01 C01 108.74(12) . . ?
C02 C01 C06 116.1(2) . . ?
C02 C01 Si01 122.38(19) . . ?
C06 C01 Si01 121.0(2) . . ?
C01 C02 C03 122.6(2) . . ?
C01 C02 H02 118.7 . . ?
C03 C02 H02 118.7 . . ?
C04 C03 C02 120.7(2) . . ?
C04 C03 H03 119.7 . . ?
C02 C03 H03 119.7 . . ?
C03 C04 C05 117.2(2) . . ?
C03 C04 C04 122.25(18) . 2_655 ?
C05 C04 C04 120.54(18) . 2_655 ?
C04 C05 C06 122.0(3) . . ?
C04 C05 H05 119.0 . . ?
C06 C05 H05 119.0 . . ?
C05 C06 C01 121.2(3) . . ?
C05 C06 H06 119.4 . . ?
C01 C06 H06 119.4 . . ?
C08 C07 Si01 114.2(2) . . ?
C08 C07 H07A 108.7 . . ?
Si01 C07 H07A 108.7 . . ?
C08 C07 H07B 108.7 . . ?
Si01 C07 H07B 108.7 . . ?
H07A C07 H07B 107.6 . . ?
C09 C08 C07 114.8(3) . . ?
C09 C08 H08A 108.6 . . ?
C07 C08 H08A 108.6 . . ?
C09 C08 H08B 108.6 . . ?
C07 C08 H08B 108.6 . . ?
H08A C08 H08B 107.5 . . ?
C10 C09 C08 114.5(3) . . ?
C10 C09 H09A 108.6 . . ?
C08 C09 H09A 108.6 . . ?
C10 C09 H09B 108.6 . . ?
C08 C09 H09B 108.6 . . ?
H09A C09 H09B 107.6 . . ?
C09 C10 C11 113.2(3) . . ?
C09 C10 H10A 108.9 . . ?
C11 C10 H10A 108.9 . . ?
C09 C10 H10B 108.9 . . ?
C11 C10 H10B 108.9 . . ?
H10A C10 H10B 107.8 . . ?
C12 C11 C10 113.6(3) . . ?
C12 C11 H11A 108.8 . . ?
C10 C11 H11A 108.8 . . ?
C12 C11 H11B 108.8 . . ?
C10 C11 H11B 108.8 . . ?
H11A C11 H11B 107.7 . . ?
C11 C12 C13 116.6(3) . . ?
C11 C12 H12A 108.1 . . ?
C13 C12 H12A 108.1 . . ?
C11 C12 H12B 108.1 . . ?
C13 C12 H12B 108.1 . . ?
H12A C12 H12B 107.3 . . ?
C14 C13 C12 113.7(3) . . ?
C14 C13 H13A 108.8 . . ?
C12 C13 H13A 108.8 . . ?
C14 C13 H13B 108.8 . . ?
C12 C13 H13B 108.8 . . ?
H13A C13 H13B 107.7 . . ?
C13 C14 C15 113.6(4) . . ?
C13 C14 H14A 108.8 . . ?
C15 C14 H14A 108.8 . . ?
C13 C14 H14B 108.8 . . ?
C15 C14 H14B 108.8 . . ?
H14A C14 H14B 107.7 . . ?
C16 C15 C14 114.8(4) . . ?
C16 C15 H15A 108.6 . . ?
C14 C15 H15A 108.6 . . ?
C16 C15 H15B 108.6 . . ?
C14 C15 H15B 108.6 . . ?
H15A C15 H15B 107.6 . . ?
C15 C16 C17 112.9(4) . . ?
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 115.8(4) . . ?
C18 C17 H17A 108.3 . . ?
C16 C17 H17A 108.3 . . ?
C18 C17 H17B 108.3 . . ?
C16 C17 H17B 108.3 . . ?
H17A C17 H17B 107.4 . . ?
C17 C18 C19 113.1(4) . . ?
C17 C18 H18A 109.0 . . ?
C19 C18 H18A 109.0 . . ?
C17 C18 H18B 109.0 . . ?
C19 C18 H18B 109.0 . . ?
H18A C18 H18B 107.8 . . ?
C20 C19 C18 116.2(5) . . ?
C20 C19 H19A 108.2 . . ?
C18 C19 H19A 108.2 . . ?
C20 C19 H19B 108.2 . . ?
C18 C19 H19B 108.2 . . ?
H19A C19 H19B 107.4 . . ?
C19 C20 C21 112.2(4) . . ?
C19 C20 H20A 109.2 . . ?
C21 C20 H20A 109.2 . . ?
C19 C20 H20B 109.2 . . ?
C21 C20 H20B 109.2 . . ?
H20A C20 H20B 107.9 . . ?
C22 C21 C20 115.5(4) . . ?
C22 C21 H21A 108.4 . . ?
C20 C21 H21A 108.4 . . ?
C22 C21 H21B 108.4 . . ?
C20 C21 H21B 108.4 . . ?
H21A C21 H21B 107.5 . . ?
C21 C22 C23 114.8(4) . . ?
C21 C22 H22A 108.6 . . ?
C23 C22 H22A 108.6 . . ?
C21 C22 H22B 108.6 . . ?
C23 C22 H22B 108.6 . . ?
H22A C22 H22B 107.5 . . ?
C22 C23 C24 114.1(3) . 2_655 ?
C22 C23 H23A 108.7 . . ?
C24 C23 H23A 108.7 2_655 . ?
C22 C23 H23B 108.7 . . ?
C24 C23 H23B 108.7 2_655 . ?
H23A C23 H23B 107.6 . . ?
C23 C24 Si01 116.6(2) 2_655 . ?
C23 C24 H24A 108.1 2_655 . ?
Si01 C24 H24A 108.1 . . ?
C23 C24 H24B 108.1 2_655 . ?
Si01 C24 H24B 108.1 . . ?
H24A C24 H24B 107.3 . . ?
C26 C25 Si01 115.5(2) . . ?
C26 C25 H25A 108.4 . . ?
Si01 C25 H25A 108.4 . . ?
C26 C25 H25B 108.4 . . ?
Si01 C25 H25B 108.4 . . ?
H25A C25 H25B 107.5 . . ?
C27 C26 C25 114.6(3) . . ?
C27 C26 H26A 108.6 . . ?
C25 C26 H26A 108.6 . . ?
C27 C26 H26B 108.6 . . ?
C25 C26 H26B 108.6 . . ?
H26A C26 H26B 107.6 . . ?
C28 C27 C26 114.3(3) . . ?
C28 C27 H27A 108.7 . . ?
C26 C27 H27A 108.7 . . ?
C28 C27 H27B 108.7 . . ?
C26 C27 H27B 108.7 . . ?
H27A C27 H27B 107.6 . . ?
C27 C28 C29 113.8(3) . . ?
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 117.3(5) . . ?
C30 C29 H29A 108.0 . . ?
C28 C29 H29A 108.0 . . ?
C30 C29 H29B 108.0 . . ?
C28 C29 H29B 108.0 . . ?
H29A C29 H29B 107.2 . . ?
C29 C30 C31 112.3(6) . . ?
C29 C30 H30A 109.1 . . ?
C31 C30 H30A 109.1 . . ?
C29 C30 H30B 109.1 . . ?
C31 C30 H30B 109.1 . . ?
H30A C30 H30B 107.9 . . ?
C32 C31 C30 122.7(9) . . ?
C32 C31 H31A 106.6 . . ?
C30 C31 H31A 106.6 . . ?
C32 C31 H31B 106.6 . . ?
C30 C31 H31B 106.6 . . ?
H31A C31 H31B 106.6 . . ?
C31 C32 C133 121.0(11) . . ?
C31 C32 C33 92.2(9) . . ?
C31 C32 H32A 113.3 . . ?
C33 C32 H32A 113.3 . . ?
C31 C32 H32B 113.3 . . ?
C33 C32 H32B 113.3 . . ?
H32A C32 H32B 110.6 . . ?
C31 C32 H32C 107.1 . . ?
C133 C32 H32C 107.1 . . ?
C31 C32 H32D 107.1 . . ?
C133 C32 H32D 107.1 . . ?
H32C C32 H32D 106.8 . . ?
C33 C33 C32 98.8(14) 2_655 . ?
C33 C33 H33A 112.0 2_655 . ?
C32 C33 H33A 112.0 . . ?
C33 C33 H33B 112.0 2_655 . ?
C32 C33 H33B 112.0 . . ?
H33A C33 H33B 109.7 . . ?
C133 C133 C32 122(2) 2_655 . ?
C133 C133 H13C 106.7 2_655 . ?
C32 C133 H13C 106.7 . . ?
C133 C133 H13D 106.7 2_655 . ?
C32 C133 H13D 106.7 . . ?
H13C C133 H13D 106.6 . . ?

_refine_diff_density_max         0.558
_refine_diff_density_min         -0.629
_refine_diff_density_rms         0.057

_shelxl_version_number           2013-4


_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: tetrahydrofuran/methanol (4:1 v/v)'
_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_shelx_CCDC2
_audit_block_doi                 10.5517/ccdc.csd.cc1p5yzs
_database_code_depnum_ccdc_archive 'CCDC 1554866'
_audit_update_record             
;
2017-06-08 deposited with the CCDC.
2017-09-14 downloaded from the CCDC.
;

# start Validation Reply Form
_vrf_RFACR01_I                   
;
PROBLEM: The value of the weighted R factor is > 0.45
RESPONSE: Due to high collection temperature, reflections at high resolution cannot be collected.
;
_vrf_SHFSU01_I                   
;
PROBLEM: The absolute value of parameter shift to su ratio > 0.20
RESPONSE: Due to high collection temperature, reflections at high resolution cannot be collected.
;
_vrf_PLAT026_I                   
;
PROBLEM: Ratio Observed / Unique Reflections too Low ....         18 %     
RESPONSE: Due to high collection temperature, reflections at high resolution cannot be collected.
;
_vrf_PLAT080_I                   
;
PROBLEM: Maximum Shift/Error ............................       1.44       
RESPONSE: This parameter was oscillated during the refinements due to many restraints.
;
_vrf_PLAT084_I                   
;
PROBLEM: High wR2 Value (i.e. > 0.25) ...................       0.47 Report
RESPONSE: Due to high collection temperature, reflections at high resolution cannot be collected.
;
_vrf_PLAT410_I                   
;
PROBLEM: Short Intra H...H Contact  H14B   ..  H17B    ..       1.79 Ang.  
RESPONSE: Due to many restraints
;
# end Validation Reply Form

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        C18BiPhcage
_chemical_name_common            C18BiPhcage
_chemical_melting_point          '274-276 deg.C'
_chemical_formula_moiety         'C66 H116 Si2'
_chemical_formula_sum            'C66 H116 Si2'
_chemical_formula_weight         965.76

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

_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_H-M_alt        'C c'
_space_group_name_Hall           'C -2yc'

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

_cell_length_a                   36.52(3)
_cell_length_b                   10.968(9)
_cell_length_c                   19.057(16)
_cell_angle_alpha                90
_cell_angle_beta                 120.161(12)
_cell_angle_gamma                90
_cell_volume                     6600(10)
_cell_formula_units_Z            4
_cell_measurement_temperature    280(2)
_cell_measurement_reflns_used    963
_cell_measurement_theta_min      2.51
_cell_measurement_theta_max      15.04

_exptl_crystal_description       plate
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    0.972
_exptl_crystal_F_000             2160
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.400
_exptl_crystal_size_min          0.300
_exptl_absorpt_coefficient_mu    0.088
_shelx_estimated_absorpt_T_min   0.966
_shelx_estimated_absorpt_T_max   0.974
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6888
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_process_details   'SADABS (bruker)'

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      280(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker SMART CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean 8.333
_diffrn_reflns_number            17562
_diffrn_reflns_av_unetI/netI     0.0818
_diffrn_reflns_av_R_equivalents  0.0377
_diffrn_reflns_limit_h_min       -47
_diffrn_reflns_limit_h_max       46
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         1.290
_diffrn_reflns_theta_max         27.775
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.915
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.915
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.731
_diffrn_reflns_point_group_measured_fraction_full 0.830
_reflns_number_total             11397
_reflns_number_gt                2038
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.598
_reflns_Friedel_fraction_max     0.547
_reflns_Friedel_fraction_full    0.663

_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, 1997)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX (Farrugia, 1999)'

_refine_special_details          
;
  The structure was refined in Cc, because the molecule has no center of symmetry due to
   unsymmetrical structure in alkyl chains.
  The structure was refined by applying many restraints because of the poor quality of the reflection data, 
   these restraints are required for the correct analysis.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.2000P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Flack x determined using 709 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.46(16)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         11397
_refine_ls_number_parameters     613
_refine_ls_number_restraints     653
_refine_ls_R_factor_all          0.3565
_refine_ls_R_factor_gt           0.1208
_refine_ls_wR_factor_ref         0.4710
_refine_ls_wR_factor_gt          0.3104
_refine_ls_goodness_of_fit_ref   0.955
_refine_ls_restrained_S_all      1.033
_refine_ls_shift/su_max          1.439
_refine_ls_shift/su_mean         0.296

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
Si01 Si 0.29365(15) 0.5030(5) 0.0297(3) 0.202(2) Uani 1 1 d D U . . .
Si02 Si 0.62752(15) 0.5042(5) 0.4929(3) 0.190(2) Uani 1 1 d D U . . .
C01 C 0.3527(4) 0.5199(15) 0.1126(10) 0.167(6) Uani 1 1 d D U . . .
C02 C 0.3681(5) 0.570(2) 0.1792(14) 0.37(2) Uani 1 1 d D U . . .
H02 H 0.3491 0.6125 0.1892 0.448 Uiso 1 1 calc R U . . .
C03 C 0.4097(5) 0.572(2) 0.2409(13) 0.329(15) Uani 1 1 d D U . . .
H03 H 0.4171 0.6056 0.2911 0.394 Uiso 1 1 calc R U . . .
C04 C 0.4407(5) 0.5232(14) 0.2269(11) 0.165(5) Uani 1 1 d . U . . .
C05 C 0.4249(5) 0.477(2) 0.1569(12) 0.300(14) Uani 1 1 d D U . . .
H05 H 0.4434 0.4391 0.1437 0.359 Uiso 1 1 calc R U . . .
C06 C 0.3835(5) 0.477(2) 0.0997(9) 0.336(18) Uani 1 1 d D U . . .
H06 H 0.3758 0.4461 0.0487 0.403 Uiso 1 1 calc R U . . .
C07 C 0.4854(5) 0.5311(14) 0.2935(10) 0.157(5) Uani 1 1 d . U . . .
C08 C 0.4983(7) 0.471(3) 0.3640(14) 0.39(2) Uani 1 1 d D U . . .
H08 H 0.4783 0.4353 0.3738 0.471 Uiso 1 1 calc R U . . .
C09 C 0.5400(7) 0.462(2) 0.4210(15) 0.38(2) Uani 1 1 d D U . . .
H09 H 0.5465 0.4084 0.4634 0.462 Uiso 1 1 calc R U . . .
C10 C 0.5728(6) 0.5203(14) 0.4243(10) 0.183(6) Uani 1 1 d . U . . .
C11 C 0.5573(6) 0.582(2) 0.3507(11) 0.298(13) Uani 1 1 d D U . . .
H11 H 0.5768 0.6187 0.3397 0.357 Uiso 1 1 calc R U . . .
C12 C 0.5156(6) 0.592(2) 0.2941(12) 0.313(15) Uani 1 1 d D U . . .
H12 H 0.5083 0.6469 0.2521 0.375 Uiso 1 1 calc R U . . .
C13 C 0.2697(5) 0.645(2) 0.0126(16) 0.304(12) Uani 1 1 d D U . . .
H13A H 0.2401 0.6336 -0.0281 0.364 Uiso 1 1 calc R U . . .
H13B H 0.2702 0.6676 0.0624 0.364 Uiso 1 1 calc R U . . .
C14 C 0.2827(8) 0.7442(19) -0.0104(16) 0.323(12) Uani 1 1 d D U . . .
H14A H 0.2798 0.7265 -0.0629 0.388 Uiso 1 1 calc R U . . .
H14B H 0.3127 0.7543 0.0276 0.388 Uiso 1 1 calc R U . . .
C15 C 0.2595(7) 0.8763(19) -0.0177(15) 0.302(10) Uani 1 1 d D U . . .
H15A H 0.2305 0.8768 -0.0624 0.362 Uiso 1 1 calc R U . . .
H15B H 0.2599 0.8968 0.0322 0.362 Uiso 1 1 calc R U . . .
C16 C 0.2869(9) 0.961(2) -0.0333(16) 0.346(12) Uani 1 1 d D U . . .
H16A H 0.2734 1.0388 -0.0558 0.416 Uiso 1 1 calc R U . . .
H16B H 0.2970 0.9248 -0.0669 0.416 Uiso 1 1 calc R U . . .
C17 C 0.3222(10) 0.970(2) 0.0583(19) 0.421(18) Uani 1 1 d D U . . .
H17A H 0.3103 0.9925 0.0920 0.505 Uiso 1 1 calc R U . . .
H17B H 0.3374 0.8936 0.0776 0.505 Uiso 1 1 calc R U . . .
C18 C 0.3495(10) 1.064(3) 0.058(2) 0.413(14) Uani 1 1 d D U . . .
H18A H 0.3449 1.1391 0.0798 0.495 Uiso 1 1 calc R U . . .
H18B H 0.3430 1.0801 0.0029 0.495 Uiso 1 1 calc R U . . .
C19 C 0.3946(10) 1.026(3) 0.108(2) 0.48(2) Uani 1 1 d D U . . .
H19A H 0.4088 1.0243 0.0769 0.573 Uiso 1 1 calc R U . . .
H19B H 0.3972 0.9475 0.1335 0.573 Uiso 1 1 calc R U . . .
C20 C 0.4116(11) 1.129(3) 0.171(2) 0.485(19) Uani 1 1 d D U . . .
H20A H 0.3938 1.1491 0.1941 0.582 Uiso 1 1 calc R U . . .
H20B H 0.4207 1.2014 0.1549 0.582 Uiso 1 1 calc R U . . .
C21 C 0.4497(9) 1.029(4) 0.224(2) 0.53(2) Uani 1 1 d D U . . .
H21A H 0.4414 0.9680 0.2506 0.637 Uiso 1 1 calc R U . . .
H21B H 0.4605 0.9903 0.1928 0.637 Uiso 1 1 calc R U . . .
C22 C 0.4796(11) 1.124(4) 0.283(3) 0.55(2) Uani 1 1 d D U . . .
H22A H 0.4691 1.1645 0.3146 0.665 Uiso 1 1 calc R U . . .
H22B H 0.4902 1.1815 0.2590 0.665 Uiso 1 1 calc R U . . .
C23 C 0.5122(10) 1.009(3) 0.331(2) 0.53(2) Uani 1 1 d D U . . .
H23A H 0.4985 0.9406 0.3402 0.632 Uiso 1 1 calc R U . . .
H23B H 0.5278 0.9823 0.3047 0.632 Uiso 1 1 calc R U . . .
C24 C 0.5385(10) 1.084(4) 0.406(2) 0.50(2) Uani 1 1 d D U . . .
H24A H 0.5313 1.0691 0.4474 0.603 Uiso 1 1 calc R U . . .
H24B H 0.5363 1.1709 0.3936 0.603 Uiso 1 1 calc R U . . .
C25 C 0.5832(9) 1.031(3) 0.429(2) 0.442(19) Uani 1 1 d D U . . .
H25A H 0.5810 0.9636 0.3941 0.531 Uiso 1 1 calc R U . . .
H25B H 0.6016 1.0935 0.4268 0.531 Uiso 1 1 calc R U . . .
C26 C 0.5974(8) 0.992(3) 0.5127(19) 0.389(14) Uani 1 1 d D U . . .
H26A H 0.5833 0.9190 0.5162 0.467 Uiso 1 1 calc R U . . .
H26B H 0.5972 1.0559 0.5476 0.467 Uiso 1 1 calc R U . . .
C27 C 0.6445(7) 0.966(3) 0.5227(19) 0.378(14) Uani 1 1 d D U . . .
H27A H 0.6420 0.9509 0.4703 0.454 Uiso 1 1 calc R U . . .
H27B H 0.6632 1.0347 0.5481 0.454 Uiso 1 1 calc R U . . .
C28 C 0.6593(7) 0.865(2) 0.5706(19) 0.378(14) Uani 1 1 d D U . . .
H28A H 0.6633 0.8913 0.6226 0.453 Uiso 1 1 calc R U . . .
H28B H 0.6876 0.8534 0.5790 0.453 Uiso 1 1 calc R U . . .
C29 C 0.6413(6) 0.735(2) 0.5595(13) 0.280(10) Uani 1 1 d D U . . .
H29A H 0.6494 0.6997 0.6119 0.337 Uiso 1 1 calc R U . . .
H29B H 0.6106 0.7375 0.5274 0.337 Uiso 1 1 calc R U . . .
C30 C 0.6586(6) 0.662(2) 0.5177(11) 0.281(10) Uani 1 1 d D U . . .
H30A H 0.6889 0.6499 0.5526 0.337 Uiso 1 1 calc R U . . .
H30B H 0.6536 0.7024 0.4683 0.337 Uiso 1 1 calc R U . . .
C31 C 0.2899(6) 0.4257(19) -0.0580(12) 0.250(9) Uani 1 1 d . U . . .
H31A H 0.3044 0.4763 -0.0781 0.300 Uiso 1 1 calc R U . . .
H31B H 0.3060 0.3507 -0.0386 0.300 Uiso 1 1 calc R U . . .
C32 C 0.2448(5) 0.391(2) -0.1344(11) 0.273(8) Uani 1 1 d D U . . .
H32A H 0.2259 0.4600 -0.1478 0.328 Uiso 1 1 calc R U . . .
H32B H 0.2328 0.3235 -0.1197 0.328 Uiso 1 1 calc R U . . .
C33 C 0.2479(8) 0.352(2) -0.2161(12) 0.376(12) Uani 1 1 d D U . . .
H33A H 0.2212 0.3604 -0.2665 0.451 Uiso 1 1 calc R U . . .
H33B H 0.2703 0.3943 -0.2195 0.451 Uiso 1 1 calc R U . . .
C34 C 0.2588(8) 0.221(2) -0.1876(15) 0.330(10) Uani 1 1 d D U . . .
H34A H 0.2818 0.2214 -0.1317 0.397 Uiso 1 1 calc R U . . .
H34B H 0.2344 0.1840 -0.1887 0.397 Uiso 1 1 calc R U . . .
C35 C 0.2711(9) 0.147(3) -0.2353(18) 0.412(13) Uani 1 1 d D U . . .
H35A H 0.2467 0.1416 -0.2895 0.494 Uiso 1 1 calc R U . . .
H35B H 0.2766 0.0658 -0.2125 0.494 Uiso 1 1 calc R U . . .
C36 C 0.3070(12) 0.181(4) -0.244(2) 0.455(14) Uani 1 1 d D U . . .
H36A H 0.3091 0.2697 -0.2437 0.545 Uiso 1 1 calc R U . . .
H36B H 0.3023 0.1525 -0.2961 0.545 Uiso 1 1 calc R U . . .
C37 C 0.3486(10) 0.128(3) -0.176(2) 0.436(15) Uani 1 1 d D U . . .
H37A H 0.3441 0.0967 -0.1334 0.523 Uiso 1 1 calc R U . . .
H37B H 0.3575 0.0612 -0.1972 0.523 Uiso 1 1 calc R U . . .
C38 C 0.3820(11) 0.221(3) -0.142(2) 0.448(17) Uani 1 1 d D U . . .
H38A H 0.3802 0.2660 -0.1002 0.538 Uiso 1 1 calc R U . . .
H38B H 0.3776 0.2783 -0.1845 0.538 Uiso 1 1 calc R U . . .
C39 C 0.4256(10) 0.166(4) -0.107(2) 0.507(19) Uani 1 1 d D U . . .
H39A H 0.4405 0.1943 -0.1339 0.609 Uiso 1 1 calc R U . . .
H39B H 0.4251 0.0778 -0.1062 0.609 Uiso 1 1 calc R U . . .
C40 C 0.4433(9) 0.220(4) -0.0231(19) 0.461(16) Uani 1 1 d D U . . .
H40A H 0.4436 0.1612 0.0150 0.554 Uiso 1 1 calc R U . . .
H40B H 0.4273 0.2914 -0.0239 0.554 Uiso 1 1 calc R U . . .
C41 C 0.4904(11) 0.257(5) -0.002(2) 0.515(18) Uani 1 1 d D U . . .
H41A H 0.5038 0.1919 -0.0153 0.618 Uiso 1 1 calc R U . . .
H41B H 0.4909 0.3315 -0.0281 0.618 Uiso 1 1 calc R U . . .
C42 C 0.5101(8) 0.272(4) 0.0871(19) 0.429(13) Uani 1 1 d D U . . .
H42A H 0.5085 0.1960 0.1113 0.515 Uiso 1 1 calc R U . . .
H42B H 0.4946 0.3335 0.0985 0.515 Uiso 1 1 calc R U . . .
C43 C 0.5554(10) 0.310(4) 0.1237(19) 0.465(14) Uani 1 1 d D U . . .
H43A H 0.5695 0.2617 0.1016 0.558 Uiso 1 1 calc R U . . .
H43B H 0.5572 0.3954 0.1122 0.558 Uiso 1 1 calc R U . . .
C44 C 0.5756(9) 0.290(4) 0.213(2) 0.456(14) Uani 1 1 d D U . . .
H44A H 0.5774 0.2029 0.2219 0.547 Uiso 1 1 calc R U . . .
H44B H 0.5566 0.3227 0.2298 0.547 Uiso 1 1 calc R U . . .
C45 C 0.6187(11) 0.343(4) 0.2668(19) 0.497(15) Uani 1 1 d D U . . .
H45A H 0.6155 0.4256 0.2813 0.596 Uiso 1 1 calc R U . . .
H45B H 0.6337 0.3474 0.2370 0.596 Uiso 1 1 calc R U . . .
C46 C 0.6461(10) 0.268(3) 0.3470(19) 0.468(15) Uani 1 1 d D U . . .
H46A H 0.6757 0.2731 0.3620 0.562 Uiso 1 1 calc R U . . .
H46B H 0.6378 0.1825 0.3364 0.562 Uiso 1 1 calc R U . . .
C47 C 0.6412(8) 0.313(2) 0.4209(18) 0.370(11) Uani 1 1 d D U . . .
H47A H 0.6120 0.3060 0.4079 0.444 Uiso 1 1 calc R U . . .
H47B H 0.6588 0.2648 0.4690 0.444 Uiso 1 1 calc R U . . .
C48 C 0.6541(6) 0.436(2) 0.4337(19) 0.353(12) Uani 1 1 d D U . . .
H48A H 0.6444 0.4775 0.3825 0.423 Uiso 1 1 calc R U . . .
H48B H 0.6848 0.4417 0.4657 0.423 Uiso 1 1 calc R U . . .
C49 C 0.2690(6) 0.402(3) 0.0709(13) 0.345(14) Uani 1 1 d D U . . .
H49A H 0.2588 0.4561 0.0976 0.414 Uiso 1 1 calc R U . . .
H49B H 0.2438 0.3706 0.0236 0.414 Uiso 1 1 calc R U . . .
C50 C 0.2864(13) 0.297(3) 0.126(2) 0.430(16) Uani 1 1 d D U . . .
H50A H 0.3171 0.2938 0.1550 0.516 Uiso 1 1 calc R U . . .
H50B H 0.2745 0.2194 0.0996 0.516 Uiso 1 1 calc R U . . .
C51 C 0.2673(11) 0.348(4) 0.1761(18) 0.471(14) Uani 1 1 d D U . . .
H51A H 0.2722 0.4348 0.1855 0.566 Uiso 1 1 calc R U . . .
H51B H 0.2372 0.3314 0.1504 0.566 Uiso 1 1 calc R U . . .
C52 C 0.2920(9) 0.277(3) 0.2526(17) 0.401(13) Uani 1 1 d D U . . .
H52A H 0.2932 0.3219 0.2974 0.482 Uiso 1 1 calc R U . . .
H52B H 0.2775 0.2001 0.2478 0.482 Uiso 1 1 calc R U . . .
C53 C 0.3344(9) 0.251(4) 0.2700(19) 0.417(14) Uani 1 1 d D U . . .
H53A H 0.3425 0.3005 0.2377 0.501 Uiso 1 1 calc R U . . .
H53B H 0.3389 0.1656 0.2641 0.501 Uiso 1 1 calc R U . . .
C54 C 0.3563(9) 0.292(3) 0.3589(18) 0.394(13) Uani 1 1 d D U . . .
H54A H 0.3548 0.3793 0.3641 0.473 Uiso 1 1 calc R U . . .
H54B H 0.3450 0.2505 0.3888 0.473 Uiso 1 1 calc R U . . .
C55 C 0.4002(11) 0.250(5) 0.384(2) 0.535(19) Uani 1 1 d D U . . .
H55A H 0.4082 0.2704 0.3440 0.643 Uiso 1 1 calc R U . . .
H55B H 0.4040 0.1638 0.3959 0.643 Uiso 1 1 calc R U . . .
C56 C 0.4233(11) 0.329(4) 0.461(2) 0.515(19) Uani 1 1 d D U . . .
H56A H 0.4042 0.3727 0.4728 0.618 Uiso 1 1 calc R U . . .
H56B H 0.4435 0.3846 0.4589 0.618 Uiso 1 1 calc R U . . .
C57 C 0.4450(10) 0.218(3) 0.518(2) 0.486(17) Uani 1 1 d D U . . .
H57A H 0.4361 0.2104 0.5582 0.583 Uiso 1 1 calc R U . . .
H57B H 0.4394 0.1424 0.4882 0.583 Uiso 1 1 calc R U . . .
C58 C 0.4920(9) 0.256(4) 0.558(2) 0.454(16) Uani 1 1 d D U . . .
H58A H 0.4966 0.3366 0.5810 0.545 Uiso 1 1 calc R U . . .
H58B H 0.5016 0.2534 0.5186 0.545 Uiso 1 1 calc R U . . .
C59 C 0.5151(9) 0.157(4) 0.625(2) 0.480(18) Uani 1 1 d D U . . .
H59A H 0.5097 0.1679 0.6695 0.576 Uiso 1 1 calc R U . . .
H59B H 0.5076 0.0753 0.6036 0.576 Uiso 1 1 calc R U . . .
C60 C 0.5604(9) 0.188(4) 0.649(2) 0.428(15) Uani 1 1 d D U . . .
H60A H 0.5696 0.1405 0.6184 0.514 Uiso 1 1 calc R U . . .
H60B H 0.5630 0.2741 0.6405 0.514 Uiso 1 1 calc R U . . .
C61 C 0.5850(9) 0.160(4) 0.7335(19) 0.390(13) Uani 1 1 d D U . . .
H61A H 0.5743 0.0839 0.7426 0.468 Uiso 1 1 calc R U . . .
H61B H 0.5800 0.2227 0.7635 0.468 Uiso 1 1 calc R U . . .
C62 C 0.6318(10) 0.147(4) 0.7698(19) 0.381(13) Uani 1 1 d D U . . .
H62A H 0.6375 0.0697 0.7520 0.457 Uiso 1 1 calc R U . . .
H62B H 0.6448 0.1430 0.8284 0.457 Uiso 1 1 calc R U . . .
C63 C 0.6526(8) 0.248(3) 0.7483(17) 0.376(14) Uani 1 1 d D U . . .
H63A H 0.6273 0.2984 0.7241 0.452 Uiso 1 1 calc R U . . .
H63B H 0.6683 0.2781 0.8036 0.452 Uiso 1 1 calc R U . . .
C64 C 0.6751(10) 0.328(4) 0.7197(17) 0.411(16) Uani 1 1 d D U . . .
H64A H 0.6999 0.2780 0.7352 0.493 Uiso 1 1 calc R U . . .
H64B H 0.6850 0.3901 0.7617 0.493 Uiso 1 1 calc R U . . .
C65 C 0.6754(6) 0.404(2) 0.6515(14) 0.292(10) Uani 1 1 d D U . . .
H65A H 0.6899 0.4805 0.6732 0.350 Uiso 1 1 calc R U . . .
H65B H 0.6904 0.3595 0.6294 0.350 Uiso 1 1 calc R U . . .
C66 C 0.6318(6) 0.427(2) 0.5875(10) 0.239(7) Uani 1 1 d . U . . .
H66A H 0.6181 0.4780 0.6090 0.287 Uiso 1 1 calc R U . . .
H66B H 0.6166 0.3498 0.5714 0.287 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
Si01 C13 1.74(2) . ?
Si01 C31 1.816(19) . ?
Si01 C49 1.84(2) . ?
Si01 C01 1.938(14) . ?
Si02 C10 1.764(19) . ?
Si02 C66 1.927(18) . ?
Si02 C48 1.97(3) . ?
Si02 C30 2.00(2) . ?
C01 C02 1.23(2) . ?
C01 C06 1.350(16) . ?
C02 C03 1.378(17) . ?
C03 C04 1.39(2) . ?
C04 C05 1.26(2) . ?
C04 C07 1.483(14) . ?
C05 C06 1.347(17) . ?
C07 C12 1.282(19) . ?
C07 C08 1.35(2) . ?
C08 C09 1.358(18) . ?
C09 C10 1.33(2) . ?
C10 C11 1.39(2) . ?
C11 C12 1.358(16) . ?
C13 C14 1.343(18) . ?
C14 C15 1.65(2) . ?
C15 C16 1.50(2) . ?
C16 C17 1.57(2) . ?
C17 C18 1.44(2) . ?
C18 C19 1.49(2) . ?
C19 C20 1.53(2) . ?
C20 C21 1.66(2) . ?
C21 C22 1.51(2) . ?
C22 C23 1.65(2) . ?
C23 C24 1.50(2) . ?
C24 C25 1.57(2) . ?
C25 C26 1.48(2) . ?
C26 C27 1.66(2) . ?
C27 C28 1.36(2) . ?
C28 C29 1.54(2) . ?
C29 C30 1.478(19) . ?
C31 C32 1.60(2) . ?
C32 C33 1.67(2) . ?
C33 C34 1.52(2) . ?
C34 C35 1.45(3) . ?
C35 C36 1.45(2) . ?
C36 C37 1.53(2) . ?
C37 C38 1.47(2) . ?
C38 C39 1.51(2) . ?
C39 C40 1.51(2) . ?
C40 C41 1.61(2) . ?
C41 C42 1.48(2) . ?
C42 C43 1.50(2) . ?
C43 C44 1.48(2) . ?
C44 C45 1.50(2) . ?
C45 C46 1.58(2) . ?
C46 C47 1.59(2) . ?
C47 C48 1.41(2) . ?
C49 C50 1.47(2) . ?
C50 C51 1.55(2) . ?
C51 C52 1.49(2) . ?
C52 C53 1.44(2) . ?
C53 C54 1.53(2) . ?
C54 C55 1.49(2) . ?
C55 C56 1.53(2) . ?
C56 C57 1.56(2) . ?
C57 C58 1.54(2) . ?
C58 C59 1.56(2) . ?
C59 C60 1.51(2) . ?
C60 C61 1.42(2) . ?
C61 C62 1.49(2) . ?
C62 C63 1.51(4) . ?
C63 C64 1.48(2) . ?
C64 C65 1.55(2) . ?
C65 C66 1.46(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
C13 Si01 C31 116.7(12) . . ?
C13 Si01 C49 108.2(13) . . ?
C31 Si01 C49 106.6(13) . . ?
C13 Si01 C01 108.4(8) . . ?
C31 Si01 C01 109.5(8) . . ?
C49 Si01 C01 107.0(8) . . ?
C10 Si02 C66 105.4(8) . . ?
C10 Si02 C48 108.4(9) . . ?
C66 Si02 C48 122.4(11) . . ?
C10 Si02 C30 112.8(9) . . ?
C66 Si02 C30 113.1(10) . . ?
C48 Si02 C30 94.7(10) . . ?
C02 C01 C06 110.6(14) . . ?
C02 C01 Si01 128.9(14) . . ?
C06 C01 Si01 120.4(14) . . ?
C01 C02 C03 128.5(17) . . ?
C02 C03 C04 119.0(17) . . ?
C05 C04 C03 111.9(18) . . ?
C05 C04 C07 130.5(16) . . ?
C03 C04 C07 117.6(15) . . ?
C04 C05 C06 125.7(18) . . ?
C01 C06 C05 123.6(15) . . ?
C12 C07 C08 112(2) . . ?
C12 C07 C04 127.5(15) . . ?
C08 C07 C04 120.6(17) . . ?
C07 C08 C09 122(2) . . ?
C10 C09 C08 129(2) . . ?
C09 C10 C11 106.5(18) . . ?
C09 C10 Si02 130.2(15) . . ?
C11 C10 Si02 122.0(14) . . ?
C12 C11 C10 124.3(19) . . ?
C07 C12 C11 126(2) . . ?
C14 C13 Si01 123.8(19) . . ?
C13 C14 C15 119(2) . . ?
C16 C15 C14 101(2) . . ?
C15 C16 C17 94.4(18) . . ?
C18 C17 C16 103(2) . . ?
C17 C18 C19 110(3) . . ?
C18 C19 C20 100(2) . . ?
C19 C20 C21 83(2) . . ?
C22 C21 C20 94(2) . . ?
C21 C22 C23 87(2) . . ?
C24 C23 C22 93(2) . . ?
C23 C24 C25 98(2) . . ?
C26 C25 C24 99(2) . . ?
C25 C26 C27 87.4(19) . . ?
C28 C27 C26 105(2) . . ?
C27 C28 C29 131(3) . . ?
C30 C29 C28 108(2) . . ?
C29 C30 Si02 104.6(14) . . ?
C32 C31 Si01 121.0(14) . . ?
C31 C32 C33 112.8(15) . . ?
C34 C33 C32 92(2) . . ?
C35 C34 C33 114(2) . . ?
C34 C35 C36 121(3) . . ?
C35 C36 C37 112(3) . . ?
C38 C37 C36 111(3) . . ?
C37 C38 C39 112(3) . . ?
C38 C39 C40 96(2) . . ?
C39 C40 C41 102(2) . . ?
C42 C41 C40 99(2) . . ?
C41 C42 C43 111(2) . . ?
C44 C43 C42 107(2) . . ?
C43 C44 C45 118(2) . . ?
C44 C45 C46 114(3) . . ?
C45 C46 C47 113(3) . . ?
C48 C47 C46 106(2) . . ?
C47 C48 Si02 104.2(19) . . ?
C50 C49 Si01 130(2) . . ?
C49 C50 C51 89.2(19) . . ?
C52 C51 C50 100(2) . . ?
C53 C52 C51 112(2) . . ?
C52 C53 C54 96(2) . . ?
C55 C54 C53 98(2) . . ?
C54 C55 C56 97(2) . . ?
C55 C56 C57 94(3) . . ?
C58 C57 C56 101(3) . . ?
C57 C58 C59 103(2) . . ?
C60 C59 C58 99(2) . . ?
C61 C60 C59 106(3) . . ?
C60 C61 C62 118(3) . . ?
C61 C62 C63 115(3) . . ?
C64 C63 C62 169(4) . . ?
C63 C64 C65 150(2) . . ?
C66 C65 C64 109.1(18) . . ?
C65 C66 Si02 113.4(15) . . ?

_refine_diff_density_max         0.253
_refine_diff_density_min         -0.126
_refine_diff_density_rms         0.047

_shelxl_version_number           2013-4


_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: tetrahydrofuran/methanol=4:1'
_chemical_compound_source        no
