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

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

data_shelxl
_audit_block_doi                 10.5517/cc1jj9kx
_database_code_depnum_ccdc_archive 'CCDC 1415849'
_audit_update_record             
;
2015-07-30 deposited with the CCDC.
2015-08-26 downloaded from the CCDC.
;




_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            C18Pycage
_chemical_melting_point          553-555
_chemical_formula_moiety         'C70 H116 Si2'
_chemical_formula_sum            'C70 H116 Si2'
_chemical_formula_weight         1013.81

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

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   'P-1   '
_symmetry_space_group_name_Hall  '-P 1   '

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

_cell_length_a                   12.173(3)
_cell_length_b                   17.375(4)
_cell_length_c                   18.275(4)
_cell_angle_alpha                61.920(3)
_cell_angle_beta                 71.547(3)
_cell_angle_gamma                87.263(3)
_cell_volume                     3211.3(14)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    8661
_cell_measurement_theta_min      1.34
_cell_measurement_theta_max      28.71

_exptl_crystal_description       prism
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.048
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1128
_exptl_absorpt_coefficient_mu    0.093
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8702
_exptl_absorpt_correction_T_max  0.9816
_exptl_absorpt_process_details   'SADABS (Bruker)'

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      100(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 8.31
_diffrn_reflns_number            18533
_diffrn_reflns_av_R_equivalents  0.0210
_diffrn_reflns_av_sigmaI/netI    0.0413
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         1.34
_diffrn_reflns_theta_max         28.71
_reflns_number_total             14243
_reflns_number_gt                11827
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0783P)²+1.8633P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.0198(11)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         14243
_refine_ls_number_parameters     650
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0688
_refine_ls_R_factor_gt           0.0575
_refine_ls_wR_factor_ref         0.1553
_refine_ls_wR_factor_gt          0.1454
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_restrained_S_all      1.043
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Si01 Si 0.63676(4) 0.36886(3) 0.15550(3) 0.01525(11) Uani 1 1 d . . .
Si02 Si 0.28667(4) 0.12064(3) 0.86393(3) 0.02032(11) Uani 1 1 d . . .
C01 C 0.57374(13) 0.32705(10) 0.27805(10) 0.0167(3) Uani 1 1 d . . .
C02 C 0.54274(14) 0.23701(10) 0.33727(10) 0.0186(3) Uani 1 1 d . . .
H02 H 0.5539 0.1968 0.3147 0.022 Uiso 1 1 calc R . .
C03 C 0.49594(14) 0.20419(10) 0.42842(10) 0.0181(3) Uani 1 1 d . . .
C04 C 0.47849(13) 0.26412(10) 0.46254(10) 0.0159(3) Uani 1 1 d . . .
C05 C 0.50863(14) 0.35579(10) 0.40366(10) 0.0174(3) Uani 1 1 d . . .
C06 C 0.55625(14) 0.38506(10) 0.31286(10) 0.0180(3) Uani 1 1 d . . .
H06 H 0.5773 0.4463 0.2737 0.022 Uiso 1 1 calc R . .
C07 C 0.43266(13) 0.23229(10) 0.55539(10) 0.0168(3) Uani 1 1 d . . .
C08 C 0.40571(14) 0.14020(10) 0.61431(10) 0.0196(3) Uani 1 1 d . . .
C09 C 0.36458(15) 0.11085(10) 0.70495(11) 0.0219(3) Uani 1 1 d . . .
H09 H 0.3471 0.0494 0.7441 0.026 Uiso 1 1 calc R . .
C10 C 0.34810(14) 0.16847(10) 0.74041(10) 0.0194(3) Uani 1 1 d . . .
C11 C 0.37308(14) 0.25874(10) 0.68122(11) 0.0204(3) Uani 1 1 d . . .
H11 H 0.3610 0.2989 0.7039 0.024 Uiso 1 1 calc R . .
C12 C 0.41535(14) 0.29217(10) 0.58950(10) 0.0181(3) Uani 1 1 d . . .
C13 C 0.46599(17) 0.11144(10) 0.48963(11) 0.0249(4) Uani 1 1 d . . .
H13 H 0.4763 0.0707 0.4677 0.030 Uiso 1 1 calc R . .
C14 C 0.42350(17) 0.08121(11) 0.57773(11) 0.0260(4) Uani 1 1 d . . .
H14 H 0.4050 0.0197 0.6162 0.031 Uiso 1 1 calc R . .
C15 C 0.44434(16) 0.38463(10) 0.52831(11) 0.0229(3) Uani 1 1 d . . .
H15 H 0.4317 0.4255 0.5501 0.027 Uiso 1 1 calc R . .
C16 C 0.48933(16) 0.41485(10) 0.44011(11) 0.0225(3) Uani 1 1 d . . .
H16 H 0.5085 0.4763 0.4016 0.027 Uiso 1 1 calc R . .
C17 C 0.69614(14) 0.27539(10) 0.13676(11) 0.0194(3) Uani 1 1 d . . .
H17A H 0.7399 0.2435 0.1776 0.023 Uiso 1 1 calc R . .
H17B H 0.6300 0.2339 0.1512 0.023 Uiso 1 1 calc R . .
C18 C 0.77682(15) 0.30436(10) 0.04218(11) 0.0216(3) Uani 1 1 d . . .
H18A H 0.8497 0.3369 0.0316 0.026 Uiso 1 1 calc R . .
H18B H 0.7384 0.3454 0.0009 0.026 Uiso 1 1 calc R . .
C19 C 0.80832(16) 0.22835(11) 0.02161(11) 0.0240(3) Uani 1 1 d . . .
H19A H 0.7374 0.2027 0.0216 0.029 Uiso 1 1 calc R . .
H19B H 0.8662 0.2524 -0.0384 0.029 Uiso 1 1 calc R . .
C20 C 0.85815(16) 0.15489(11) 0.08589(12) 0.0251(4) Uani 1 1 d . . .
H20A H 0.7968 0.1261 0.1445 0.030 Uiso 1 1 calc R . .
H20B H 0.8778 0.1103 0.0661 0.030 Uiso 1 1 calc R . .
C21 C 0.96662(16) 0.18462(11) 0.09557(12) 0.0254(4) Uani 1 1 d . . .
H21A H 0.9452 0.2241 0.1217 0.030 Uiso 1 1 calc R . .
H21B H 1.0254 0.2188 0.0364 0.030 Uiso 1 1 calc R . .
C22 C 1.02145(16) 0.10844(12) 0.15276(12) 0.0281(4) Uani 1 1 d . . .
H22A H 1.0908 0.1328 0.1557 0.034 Uiso 1 1 calc R . .
H22B H 1.0485 0.0717 0.1239 0.034 Uiso 1 1 calc R . .
C23 C 0.93954(17) 0.04982(12) 0.24664(12) 0.0281(4) Uani 1 1 d . . .
H23A H 0.8778 0.0165 0.2446 0.034 Uiso 1 1 calc R . .
H23B H 0.9013 0.0874 0.2721 0.034 Uiso 1 1 calc R . .
C24 C 1.00301(19) -0.01529(14) 0.30674(13) 0.0351(4) Uani 1 1 d . . .
H24A H 1.0651 0.0184 0.3080 0.042 Uiso 1 1 calc R . .
H24B H 1.0412 -0.0526 0.2808 0.042 Uiso 1 1 calc R . .
C25 C 0.9238(2) -0.07544(13) 0.40204(13) 0.0369(5) Uani 1 1 d . . .
H25A H 0.8608 -0.1085 0.4010 0.044 Uiso 1 1 calc R . .
H25B H 0.9703 -0.1187 0.4339 0.044 Uiso 1 1 calc R . .
C26 C 0.86906(18) -0.02585(12) 0.45237(12) 0.0316(4) Uani 1 1 d . . .
H26A H 0.8145 0.0116 0.4248 0.038 Uiso 1 1 calc R . .
H26B H 0.9315 0.0135 0.4462 0.038 Uiso 1 1 calc R . .
C27 C 0.80294(18) -0.08451(12) 0.55056(13) 0.0321(4) Uani 1 1 d . . .
H27A H 0.7406 -0.1243 0.5573 0.039 Uiso 1 1 calc R . .
H27B H 0.8574 -0.1213 0.5789 0.039 Uiso 1 1 calc R . .
C28 C 0.74852(17) -0.03168(12) 0.59746(12) 0.0302(4) Uani 1 1 d . . .
H28A H 0.8117 0.0058 0.5930 0.036 Uiso 1 1 calc R . .
H28B H 0.6981 0.0077 0.5665 0.036 Uiso 1 1 calc R . .
C29 C 0.67613(18) -0.08763(12) 0.69437(13) 0.0313(4) Uani 1 1 d . . .
H29A H 0.7225 -0.1333 0.7234 0.038 Uiso 1 1 calc R . .
H29B H 0.6060 -0.1180 0.6984 0.038 Uiso 1 1 calc R . .
C30 C 0.63723(17) -0.03572(12) 0.74469(13) 0.0297(4) Uani 1 1 d . . .
H30A H 0.5965 0.0131 0.7130 0.036 Uiso 1 1 calc R . .
H30B H 0.7072 -0.0097 0.7454 0.036 Uiso 1 1 calc R . .
C31 C 0.55584(19) -0.09190(12) 0.84004(13) 0.0328(4) Uani 1 1 d . . .
H31A H 0.4762 -0.0995 0.8393 0.039 Uiso 1 1 calc R . .
H31B H 0.5822 -0.1509 0.8644 0.039 Uiso 1 1 calc R . .
C32 C 0.54973(19) -0.05411(12) 0.90197(13) 0.0326(4) Uani 1 1 d . . .
H32A H 0.5047 -0.0988 0.9628 0.039 Uiso 1 1 calc R . .
H32B H 0.6299 -0.0437 0.9004 0.039 Uiso 1 1 calc R . .
C33 C 0.49437(17) 0.03157(12) 0.88074(12) 0.0289(4) Uani 1 1 d . . .
H33A H 0.5235 0.0704 0.8162 0.035 Uiso 1 1 calc R . .
H33B H 0.5203 0.0616 0.9080 0.035 Uiso 1 1 calc R . .
C34 C 0.36025(17) 0.01930(12) 0.91254(12) 0.0287(4) Uani 1 1 d . . .
H34A H 0.3316 -0.0053 0.9773 0.034 Uiso 1 1 calc R . .
H34B H 0.3348 -0.0250 0.8997 0.034 Uiso 1 1 calc R . .
C35 C 0.75585(14) 0.46142(10) 0.10697(10) 0.0186(3) Uani 1 1 d . . .
H35A H 0.7833 0.4876 0.0421 0.022 Uiso 1 1 calc R . .
H35B H 0.7230 0.5075 0.1218 0.022 Uiso 1 1 calc R . .
C36 C 0.86048(14) 0.43327(10) 0.13907(11) 0.0209(3) Uani 1 1 d . . .
H36A H 0.8970 0.3907 0.1200 0.025 Uiso 1 1 calc R . .
H36B H 0.8320 0.4027 0.2042 0.025 Uiso 1 1 calc R . .
C37 C 0.95369(15) 0.50935(12) 0.10560(12) 0.0265(4) Uani 1 1 d . . .
H37A H 1.0245 0.4846 0.1184 0.032 Uiso 1 1 calc R . .
H37B H 0.9747 0.5445 0.0409 0.032 Uiso 1 1 calc R . .
C38 C 0.91704(17) 0.57047(11) 0.14543(11) 0.0261(4) Uani 1 1 d . . .
H38A H 0.8489 0.5979 0.1300 0.031 Uiso 1 1 calc R . .
H38B H 0.9816 0.6180 0.1191 0.031 Uiso 1 1 calc R . .
C39 C 0.88545(16) 0.52353(11) 0.24580(11) 0.0241(3) Uani 1 1 d . . .
H39A H 0.8059 0.4915 0.2730 0.029 Uiso 1 1 calc R . .
H39B H 0.9402 0.4797 0.2627 0.029 Uiso 1 1 calc R . .
C40 C 0.88967(17) 0.58597(11) 0.28207(12) 0.0262(4) Uani 1 1 d . . .
H40A H 0.9690 0.6184 0.2543 0.031 Uiso 1 1 calc R . .
H40B H 0.8345 0.6295 0.2654 0.031 Uiso 1 1 calc R . .
C41 C 0.85951(17) 0.54030(12) 0.38134(12) 0.0272(4) Uani 1 1 d . . .
H41A H 0.9107 0.4936 0.3984 0.033 Uiso 1 1 calc R . .
H41B H 0.7780 0.5116 0.4091 0.033 Uiso 1 1 calc R . .
C42 C 0.87223(18) 0.60158(13) 0.41735(13) 0.0305(4) Uani 1 1 d . . .
H42A H 0.9548 0.6272 0.3931 0.037 Uiso 1 1 calc R . .
H42B H 0.8247 0.6503 0.3977 0.037 Uiso 1 1 calc R . .
C43 C 0.83377(18) 0.55395(13) 0.51739(12) 0.0309(4) Uani 1 1 d . . .
H43A H 0.8869 0.5093 0.5363 0.037 Uiso 1 1 calc R . .
H43B H 0.7545 0.5226 0.5410 0.037 Uiso 1 1 calc R . .
C44 C 0.83231(19) 0.61432(14) 0.55743(14) 0.0364(5) Uani 1 1 d . . .
H44A H 0.9134 0.6319 0.5490 0.044 Uiso 1 1 calc R . .
H44B H 0.7988 0.6683 0.5260 0.044 Uiso 1 1 calc R . .
C45 C 0.76127(19) 0.57014(13) 0.65569(13) 0.0346(4) Uani 1 1 d . . .
H45A H 0.7598 0.6130 0.6772 0.041 Uiso 1 1 calc R . .
H45B H 0.6799 0.5537 0.6637 0.041 Uiso 1 1 calc R . .
C46 C 0.80851(17) 0.48931(14) 0.71050(13) 0.0331(4) Uani 1 1 d . . .
H46A H 0.8860 0.5072 0.7083 0.040 Uiso 1 1 calc R . .
H46B H 0.8197 0.4501 0.6839 0.040 Uiso 1 1 calc R . .
C47 C 0.73035(18) 0.43703(14) 0.80770(13) 0.0335(4) Uani 1 1 d . . .
H47A H 0.7690 0.3862 0.8386 0.040 Uiso 1 1 calc R . .
H47B H 0.7229 0.4750 0.8354 0.040 Uiso 1 1 calc R . .
C48 C 0.60904(17) 0.40376(12) 0.82035(12) 0.0292(4) Uani 1 1 d . . .
H48A H 0.6159 0.3800 0.7795 0.035 Uiso 1 1 calc R . .
H48B H 0.5630 0.4540 0.8041 0.035 Uiso 1 1 calc R . .
C49 C 0.54269(17) 0.33288(13) 0.91359(13) 0.0310(4) Uani 1 1 d . . .
H49A H 0.5357 0.3568 0.9543 0.037 Uiso 1 1 calc R . .
H49B H 0.5892 0.2829 0.9298 0.037 Uiso 1 1 calc R . .
C50 C 0.42062(17) 0.29830(13) 0.92736(12) 0.0297(4) Uani 1 1 d . . .
H50A H 0.3758 0.3486 0.9066 0.036 Uiso 1 1 calc R . .
H50B H 0.3801 0.2603 0.9911 0.036 Uiso 1 1 calc R . .
C51 C 0.42124(16) 0.24597(12) 0.87935(11) 0.0262(4) Uani 1 1 d . . .
H51A H 0.4543 0.2857 0.8151 0.031 Uiso 1 1 calc R . .
H51B H 0.4728 0.1994 0.8954 0.031 Uiso 1 1 calc R . .
C52 C 0.30005(17) 0.20361(12) 0.90071(12) 0.0279(4) Uani 1 1 d . . .
H52A H 0.2541 0.2515 0.8750 0.033 Uiso 1 1 calc R . .
H52B H 0.2620 0.1746 0.9654 0.033 Uiso 1 1 calc R . .
C53 C 0.51986(14) 0.40981(10) 0.10448(10) 0.0175(3) Uani 1 1 d . . .
H53A H 0.4959 0.4630 0.1093 0.021 Uiso 1 1 calc R . .
H53B H 0.5535 0.4276 0.0411 0.021 Uiso 1 1 calc R . .
C54 C 0.41059(14) 0.34378(10) 0.14493(11) 0.0203(3) Uani 1 1 d . . .
H54A H 0.4345 0.2891 0.1435 0.024 Uiso 1 1 calc R . .
H54B H 0.3734 0.3289 0.2074 0.024 Uiso 1 1 calc R . .
C55 C 0.32083(14) 0.37768(10) 0.09781(10) 0.0197(3) Uani 1 1 d . . .
H55A H 0.3559 0.3873 0.0369 0.024 Uiso 1 1 calc R . .
H55B H 0.3027 0.4352 0.0943 0.024 Uiso 1 1 calc R . .
C56 C 0.20637(15) 0.31569(11) 0.14254(11) 0.0216(3) Uani 1 1 d . . .
H56A H 0.1580 0.3379 0.1038 0.026 Uiso 1 1 calc R . .
H56B H 0.2245 0.2567 0.1503 0.026 Uiso 1 1 calc R . .
C57 C 0.13687(15) 0.30770(11) 0.23185(11) 0.0233(3) Uani 1 1 d . . .
H57A H 0.1276 0.3676 0.2246 0.028 Uiso 1 1 calc R . .
H57B H 0.1827 0.2799 0.2719 0.028 Uiso 1 1 calc R . .
C58 C 0.01616(15) 0.25497(11) 0.27567(11) 0.0240(3) Uani 1 1 d . . .
H58A H 0.0245 0.1933 0.2886 0.029 Uiso 1 1 calc R . .
H58B H -0.0290 0.2797 0.2348 0.029 Uiso 1 1 calc R . .
C59 C -0.04989(15) 0.25699(12) 0.36106(12) 0.0259(4) Uani 1 1 d . . .
H59A H -0.0105 0.2236 0.4046 0.031 Uiso 1 1 calc R . .
H59B H -0.0446 0.3187 0.3493 0.031 Uiso 1 1 calc R . .
C60 C -0.17853(15) 0.21940(12) 0.40177(12) 0.0261(4) Uani 1 1 d . . .
H60A H -0.1855 0.1611 0.4053 0.031 Uiso 1 1 calc R . .
H60B H -0.2213 0.2585 0.3631 0.031 Uiso 1 1 calc R . .
C61 C -0.23480(15) 0.20973(11) 0.49375(12) 0.0255(4) Uani 1 1 d . . .
H61A H -0.3163 0.1820 0.5180 0.031 Uiso 1 1 calc R . .
H61B H -0.1925 0.1699 0.5325 0.031 Uiso 1 1 calc R . .
C62 C -0.23497(17) 0.29648(12) 0.49577(12) 0.0281(4) Uani 1 1 d . . .
H62A H -0.1534 0.3241 0.4718 0.034 Uiso 1 1 calc R . .
H62B H -0.2769 0.3364 0.4568 0.034 Uiso 1 1 calc R . .
C63 C -0.29150(17) 0.28687(12) 0.58729(13) 0.0300(4) Uani 1 1 d . . .
H63A H -0.3723 0.2577 0.6117 0.036 Uiso 1 1 calc R . .
H63B H -0.2961 0.3463 0.5819 0.036 Uiso 1 1 calc R . .
C64 C -0.22815(17) 0.23480(12) 0.65220(13) 0.0291(4) Uani 1 1 d . . .
H64A H -0.1462 0.2619 0.6273 0.035 Uiso 1 1 calc R . .
H64B H -0.2277 0.1740 0.6612 0.035 Uiso 1 1 calc R . .
C65 C -0.28611(17) 0.23227(13) 0.74090(13) 0.0314(4) Uani 1 1 d . . .
H65A H -0.2749 0.2922 0.7328 0.038 Uiso 1 1 calc R . .
H65B H -0.3710 0.2154 0.7601 0.038 Uiso 1 1 calc R . .
C66 C -0.23998(17) 0.16902(12) 0.81372(12) 0.0302(4) Uani 1 1 d . . .
H66A H -0.2915 0.1634 0.8706 0.036 Uiso 1 1 calc R . .
H66B H -0.2434 0.1103 0.8177 0.036 Uiso 1 1 calc R . .
C67 C -0.11584(17) 0.19783(12) 0.79937(13) 0.0302(4) Uani 1 1 d . . .
H67A H -0.1145 0.2526 0.8034 0.036 Uiso 1 1 calc R . .
H67B H -0.0663 0.2113 0.7392 0.036 Uiso 1 1 calc R . .
C68 C -0.06358(16) 0.12956(11) 0.86498(12) 0.0262(4) Uani 1 1 d . . .
H68A H -0.1118 0.1170 0.9252 0.031 Uiso 1 1 calc R . .
H68B H -0.0658 0.0743 0.8618 0.031 Uiso 1 1 calc R . .
C69 C 0.06167(16) 0.15964(11) 0.84781(12) 0.0276(4) Uani 1 1 d . . .
H69A H 0.0613 0.2066 0.8641 0.033 Uiso 1 1 calc R . .
H69B H 0.1050 0.1855 0.7840 0.033 Uiso 1 1 calc R . .
C70 C 0.12688(15) 0.08697(10) 0.89783(11) 0.0227(3) Uani 1 1 d . . .
H70A H 0.1172 0.0362 0.8888 0.027 Uiso 1 1 calc R . .
H70B H 0.0908 0.0674 0.9615 0.027 Uiso 1 1 calc R . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Si01 C53 1.8760(16) . ?
Si01 C17 1.8796(16) . ?
Si01 C35 1.8816(16) . ?
Si01 C01 1.8882(16) . ?
Si02 C70 1.8746(19) . ?
Si02 C52 1.8869(18) . ?
Si02 C10 1.8894(17) . ?
Si02 C34 1.8901(19) . ?
C01 C06 1.401(2) . ?
C01 C02 1.402(2) . ?
C02 C03 1.400(2) . ?
C02 H02 0.9500 . ?
C03 C04 1.423(2) . ?
C03 C13 1.443(2) . ?
C04 C05 1.422(2) . ?
C04 C07 1.429(2) . ?
C05 C06 1.405(2) . ?
C05 C16 1.440(2) . ?
C06 H06 0.9500 . ?
C07 C12 1.422(2) . ?
C07 C08 1.426(2) . ?
C08 C09 1.399(2) . ?
C08 C14 1.441(2) . ?
C09 C10 1.404(2) . ?
C09 H09 0.9500 . ?
C10 C11 1.401(2) . ?
C11 C12 1.406(2) . ?
C11 H11 0.9500 . ?
C12 C15 1.438(2) . ?
C13 C14 1.356(2) . ?
C13 H13 0.9500 . ?
C14 H14 0.9500 . ?
C15 C16 1.359(2) . ?
C15 H15 0.9500 . ?
C16 H16 0.9500 . ?
C17 C18 1.536(2) . ?
C17 H17A 0.9900 . ?
C17 H17B 0.9900 . ?
C18 C19 1.536(2) . ?
C18 H18A 0.9900 . ?
C18 H18B 0.9900 . ?
C19 C20 1.530(2) . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C20 C21 1.530(2) . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C21 C22 1.531(2) . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C22 C23 1.531(3) . ?
C22 H22A 0.9900 . ?
C22 H22B 0.9900 . ?
C23 C24 1.539(3) . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C24 C25 1.541(3) . ?
C24 H24A 0.9900 . ?
C24 H24B 0.9900 . ?
C25 C26 1.528(3) . ?
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?
C26 C27 1.533(3) . ?
C26 H26A 0.9900 . ?
C26 H26B 0.9900 . ?
C27 C28 1.530(3) . ?
C27 H27A 0.9900 . ?
C27 H27B 0.9900 . ?
C28 C29 1.527(3) . ?
C28 H28A 0.9900 . ?
C28 H28B 0.9900 . ?
C29 C30 1.532(3) . ?
C29 H29A 0.9900 . ?
C29 H29B 0.9900 . ?
C30 C31 1.539(3) . ?
C30 H30A 0.9900 . ?
C30 H30B 0.9900 . ?
C31 C32 1.536(3) . ?
C31 H31A 0.9900 . ?
C31 H31B 0.9900 . ?
C32 C33 1.532(3) . ?
C32 H32A 0.9900 . ?
C32 H32B 0.9900 . ?
C33 C34 1.538(3) . ?
C33 H33A 0.9900 . ?
C33 H33B 0.9900 . ?
C34 H34A 0.9900 . ?
C34 H34B 0.9900 . ?
C35 C36 1.533(2) . ?
C35 H35A 0.9900 . ?
C35 H35B 0.9900 . ?
C36 C37 1.534(2) . ?
C36 H36A 0.9900 . ?
C36 H36B 0.9900 . ?
C37 C38 1.528(2) . ?
C37 H37A 0.9900 . ?
C37 H37B 0.9900 . ?
C38 C39 1.534(2) . ?
C38 H38A 0.9900 . ?
C38 H38B 0.9900 . ?
C39 C40 1.524(2) . ?
C39 H39A 0.9900 . ?
C39 H39B 0.9900 . ?
C40 C41 1.519(2) . ?
C40 H40A 0.9900 . ?
C40 H40B 0.9900 . ?
C41 C42 1.527(2) . ?
C41 H41A 0.9900 . ?
C41 H41B 0.9900 . ?
C42 C43 1.522(3) . ?
C42 H42A 0.9900 . ?
C42 H42B 0.9900 . ?
C43 C44 1.532(3) . ?
C43 H43A 0.9900 . ?
C43 H43B 0.9900 . ?
C44 C45 1.531(3) . ?
C44 H44A 0.9900 . ?
C44 H44B 0.9900 . ?
C45 C46 1.507(3) . ?
C45 H45A 0.9900 . ?
C45 H45B 0.9900 . ?
C46 C47 1.543(3) . ?
C46 H46A 0.9900 . ?
C46 H46B 0.9900 . ?
C47 C48 1.519(3) . ?
C47 H47A 0.9900 . ?
C47 H47B 0.9900 . ?
C48 C49 1.523(3) . ?
C48 H48A 0.9900 . ?
C48 H48B 0.9900 . ?
C49 C50 1.529(3) . ?
C49 H49A 0.9900 . ?
C49 H49B 0.9900 . ?
C50 C51 1.531(2) . ?
C50 H50A 0.9900 . ?
C50 H50B 0.9900 . ?
C51 C52 1.530(3) . ?
C51 H51A 0.9900 . ?
C51 H51B 0.9900 . ?
C52 H52A 0.9900 . ?
C52 H52B 0.9900 . ?
C53 C54 1.535(2) . ?
C53 H53A 0.9900 . ?
C53 H53B 0.9900 . ?
C54 C55 1.529(2) . ?
C54 H54A 0.9900 . ?
C54 H54B 0.9900 . ?
C55 C56 1.537(2) . ?
C55 H55A 0.9900 . ?
C55 H55B 0.9900 . ?
C56 C57 1.524(2) . ?
C56 H56A 0.9900 . ?
C56 H56B 0.9900 . ?
C57 C58 1.527(2) . ?
C57 H57A 0.9900 . ?
C57 H57B 0.9900 . ?
C58 C59 1.529(2) . ?
C58 H58A 0.9900 . ?
C58 H58B 0.9900 . ?
C59 C60 1.528(2) . ?
C59 H59A 0.9900 . ?
C59 H59B 0.9900 . ?
C60 C61 1.529(3) . ?
C60 H60A 0.9900 . ?
C60 H60B 0.9900 . ?
C61 C62 1.525(2) . ?
C61 H61A 0.9900 . ?
C61 H61B 0.9900 . ?
C62 C63 1.523(3) . ?
C62 H62A 0.9900 . ?
C62 H62B 0.9900 . ?
C63 C64 1.524(3) . ?
C63 H63A 0.9900 . ?
C63 H63B 0.9900 . ?
C64 C65 1.529(3) . ?
C64 H64A 0.9900 . ?
C64 H64B 0.9900 . ?
C65 C66 1.527(3) . ?
C65 H65A 0.9900 . ?
C65 H65B 0.9900 . ?
C66 C67 1.517(3) . ?
C66 H66A 0.9900 . ?
C66 H66B 0.9900 . ?
C67 C68 1.523(3) . ?
C67 H67A 0.9900 . ?
C67 H67B 0.9900 . ?
C68 C69 1.522(3) . ?
C68 H68A 0.9900 . ?
C68 H68B 0.9900 . ?
C69 C70 1.529(2) . ?
C69 H69A 0.9900 . ?
C69 H69B 0.9900 . ?
C70 H70A 0.9900 . ?
C70 H70B 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
C53 Si01 C17 109.74(7) . . ?
C53 Si01 C35 109.58(7) . . ?
C17 Si01 C35 110.84(7) . . ?
C53 Si01 C01 109.86(7) . . ?
C17 Si01 C01 108.17(7) . . ?
C35 Si01 C01 108.62(7) . . ?
C70 Si02 C52 106.91(8) . . ?
C70 Si02 C10 107.03(7) . . ?
C52 Si02 C10 112.52(8) . . ?
C70 Si02 C34 108.98(8) . . ?
C52 Si02 C34 114.26(9) . . ?
C10 Si02 C34 106.88(8) . . ?
C06 C01 C02 117.74(14) . . ?
C06 C01 Si01 121.08(11) . . ?
C02 C01 Si01 121.18(12) . . ?
C03 C02 C01 122.38(14) . . ?
C03 C02 H02 118.8 . . ?
C01 C02 H02 118.8 . . ?
C02 C03 C04 119.08(14) . . ?
C02 C03 C13 122.51(14) . . ?
C04 C03 C13 118.41(14) . . ?
C05 C04 C03 119.51(14) . . ?
C05 C04 C07 120.26(14) . . ?
C03 C04 C07 120.22(13) . . ?
C06 C05 C04 119.04(14) . . ?
C06 C05 C16 122.72(14) . . ?
C04 C05 C16 118.24(14) . . ?
C01 C06 C05 122.25(14) . . ?
C01 C06 H06 118.9 . . ?
C05 C06 H06 118.9 . . ?
C12 C07 C08 119.67(14) . . ?
C12 C07 C04 120.23(13) . . ?
C08 C07 C04 120.10(14) . . ?
C09 C08 C07 118.81(14) . . ?
C09 C08 C14 122.81(14) . . ?
C07 C08 C14 118.37(14) . . ?
C08 C09 C10 122.69(14) . . ?
C08 C09 H09 118.7 . . ?
C10 C09 H09 118.7 . . ?
C11 C10 C09 117.47(14) . . ?
C11 C10 Si02 123.93(12) . . ?
C09 C10 Si02 118.52(12) . . ?
C10 C11 C12 122.44(15) . . ?
C10 C11 H11 118.8 . . ?
C12 C11 H11 118.8 . . ?
C11 C12 C07 118.90(14) . . ?
C11 C12 C15 122.80(14) . . ?
C07 C12 C15 118.29(14) . . ?
C14 C13 C03 121.36(15) . . ?
C14 C13 H13 119.3 . . ?
C03 C13 H13 119.3 . . ?
C13 C14 C08 121.53(15) . . ?
C13 C14 H14 119.2 . . ?
C08 C14 H14 119.2 . . ?
C16 C15 C12 121.49(15) . . ?
C16 C15 H15 119.3 . . ?
C12 C15 H15 119.3 . . ?
C15 C16 C05 121.47(14) . . ?
C15 C16 H16 119.3 . . ?
C05 C16 H16 119.3 . . ?
C18 C17 Si01 113.78(11) . . ?
C18 C17 H17A 108.8 . . ?
Si01 C17 H17A 108.8 . . ?
C18 C17 H17B 108.8 . . ?
Si01 C17 H17B 108.8 . . ?
H17A C17 H17B 107.7 . . ?
C17 C18 C19 114.21(13) . . ?
C17 C18 H18A 108.7 . . ?
C19 C18 H18A 108.7 . . ?
C17 C18 H18B 108.7 . . ?
C19 C18 H18B 108.7 . . ?
H18A C18 H18B 107.6 . . ?
C20 C19 C18 114.66(14) . . ?
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 . . ?
C21 C20 C19 114.96(14) . . ?
C21 C20 H20A 108.5 . . ?
C19 C20 H20A 108.5 . . ?
C21 C20 H20B 108.5 . . ?
C19 C20 H20B 108.5 . . ?
H20A C20 H20B 107.5 . . ?
C20 C21 C22 113.49(14) . . ?
C20 C21 H21A 108.9 . . ?
C22 C21 H21A 108.9 . . ?
C20 C21 H21B 108.9 . . ?
C22 C21 H21B 108.9 . . ?
H21A C21 H21B 107.7 . . ?
C21 C22 C23 114.41(15) . . ?
C21 C22 H22A 108.7 . . ?
C23 C22 H22A 108.7 . . ?
C21 C22 H22B 108.7 . . ?
C23 C22 H22B 108.7 . . ?
H22A C22 H22B 107.6 . . ?
C22 C23 C24 112.87(16) . . ?
C22 C23 H23A 109.0 . . ?
C24 C23 H23A 109.0 . . ?
C22 C23 H23B 109.0 . . ?
C24 C23 H23B 109.0 . . ?
H23A C23 H23B 107.8 . . ?
C23 C24 C25 114.61(17) . . ?
C23 C24 H24A 108.6 . . ?
C25 C24 H24A 108.6 . . ?
C23 C24 H24B 108.6 . . ?
C25 C24 H24B 108.6 . . ?
H24A C24 H24B 107.6 . . ?
C26 C25 C24 113.61(17) . . ?
C26 C25 H25A 108.8 . . ?
C24 C25 H25A 108.8 . . ?
C26 C25 H25B 108.8 . . ?
C24 C25 H25B 108.8 . . ?
H25A C25 H25B 107.7 . . ?
C25 C26 C27 114.77(16) . . ?
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 112.63(15) . . ?
C28 C27 H27A 109.1 . . ?
C26 C27 H27A 109.1 . . ?
C28 C27 H27B 109.1 . . ?
C26 C27 H27B 109.1 . . ?
H27A C27 H27B 107.8 . . ?
C29 C28 C27 114.38(15) . . ?
C29 C28 H28A 108.7 . . ?
C27 C28 H28A 108.7 . . ?
C29 C28 H28B 108.7 . . ?
C27 C28 H28B 108.7 . . ?
H28A C28 H28B 107.6 . . ?
C28 C29 C30 114.28(15) . . ?
C28 C29 H29A 108.7 . . ?
C30 C29 H29A 108.7 . . ?
C28 C29 H29B 108.7 . . ?
C30 C29 H29B 108.7 . . ?
H29A C29 H29B 107.6 . . ?
C29 C30 C31 113.44(15) . . ?
C29 C30 H30A 108.9 . . ?
C31 C30 H30A 108.9 . . ?
C29 C30 H30B 108.9 . . ?
C31 C30 H30B 108.9 . . ?
H30A C30 H30B 107.7 . . ?
C32 C31 C30 115.02(16) . . ?
C32 C31 H31A 108.5 . . ?
C30 C31 H31A 108.5 . . ?
C32 C31 H31B 108.5 . . ?
C30 C31 H31B 108.5 . . ?
H31A C31 H31B 107.5 . . ?
C33 C32 C31 115.22(16) . . ?
C33 C32 H32A 108.5 . . ?
C31 C32 H32A 108.5 . . ?
C33 C32 H32B 108.5 . . ?
C31 C32 H32B 108.5 . . ?
H32A C32 H32B 107.5 . . ?
C32 C33 C34 114.34(16) . . ?
C32 C33 H33A 108.7 . . ?
C34 C33 H33A 108.7 . . ?
C32 C33 H33B 108.7 . . ?
C34 C33 H33B 108.7 . . ?
H33A C33 H33B 107.6 . . ?
C33 C34 Si02 116.74(12) . . ?
C33 C34 H34A 108.1 . . ?
Si02 C34 H34A 108.1 . . ?
C33 C34 H34B 108.1 . . ?
Si02 C34 H34B 108.1 . . ?
H34A C34 H34B 107.3 . . ?
C36 C35 Si01 113.79(11) . . ?
C36 C35 H35A 108.8 . . ?
Si01 C35 H35A 108.8 . . ?
C36 C35 H35B 108.8 . . ?
Si01 C35 H35B 108.8 . . ?
H35A C35 H35B 107.7 . . ?
C35 C36 C37 114.21(14) . . ?
C35 C36 H36A 108.7 . . ?
C37 C36 H36A 108.7 . . ?
C35 C36 H36B 108.7 . . ?
C37 C36 H36B 108.7 . . ?
H36A C36 H36B 107.6 . . ?
C38 C37 C36 114.64(14) . . ?
C38 C37 H37A 108.6 . . ?
C36 C37 H37A 108.6 . . ?
C38 C37 H37B 108.6 . . ?
C36 C37 H37B 108.6 . . ?
H37A C37 H37B 107.6 . . ?
C37 C38 C39 113.34(14) . . ?
C37 C38 H38A 108.9 . . ?
C39 C38 H38A 108.9 . . ?
C37 C38 H38B 108.9 . . ?
C39 C38 H38B 108.9 . . ?
H38A C38 H38B 107.7 . . ?
C40 C39 C38 113.19(14) . . ?
C40 C39 H39A 108.9 . . ?
C38 C39 H39A 108.9 . . ?
C40 C39 H39B 108.9 . . ?
C38 C39 H39B 108.9 . . ?
H39A C39 H39B 107.8 . . ?
C41 C40 C39 113.77(14) . . ?
C41 C40 H40A 108.8 . . ?
C39 C40 H40A 108.8 . . ?
C41 C40 H40B 108.8 . . ?
C39 C40 H40B 108.8 . . ?
H40A C40 H40B 107.7 . . ?
C40 C41 C42 114.01(15) . . ?
C40 C41 H41A 108.8 . . ?
C42 C41 H41A 108.8 . . ?
C40 C41 H41B 108.7 . . ?
C42 C41 H41B 108.8 . . ?
H41A C41 H41B 107.6 . . ?
C43 C42 C41 112.03(15) . . ?
C43 C42 H42A 109.2 . . ?
C41 C42 H42A 109.2 . . ?
C43 C42 H42B 109.2 . . ?
C41 C42 H42B 109.2 . . ?
H42A C42 H42B 107.9 . . ?
C42 C43 C44 114.15(16) . . ?
C42 C43 H43A 108.7 . . ?
C44 C43 H43A 108.7 . . ?
C42 C43 H43B 108.7 . . ?
C44 C43 H43B 108.7 . . ?
H43A C43 H43B 107.6 . . ?
C45 C44 C43 112.38(16) . . ?
C45 C44 H44A 109.1 . . ?
C43 C44 H44A 109.1 . . ?
C45 C44 H44B 109.1 . . ?
C43 C44 H44B 109.1 . . ?
H44A C44 H44B 107.9 . . ?
C46 C45 C44 113.51(17) . . ?
C46 C45 H45A 108.9 . . ?
C44 C45 H45A 108.9 . . ?
C46 C45 H45B 108.9 . . ?
C44 C45 H45B 108.9 . . ?
H45A C45 H45B 107.7 . . ?
C45 C46 C47 114.56(16) . . ?
C45 C46 H46A 108.6 . . ?
C47 C46 H46A 108.6 . . ?
C45 C46 H46B 108.6 . . ?
C47 C46 H46B 108.6 . . ?
H46A C46 H46B 107.6 . . ?
C48 C47 C46 113.89(16) . . ?
C48 C47 H47A 108.8 . . ?
C46 C47 H47A 108.8 . . ?
C48 C47 H47B 108.8 . . ?
C46 C47 H47B 108.8 . . ?
H47A C47 H47B 107.7 . . ?
C47 C48 C49 114.36(16) . . ?
C47 C48 H48A 108.7 . . ?
C49 C48 H48A 108.7 . . ?
C47 C48 H48B 108.7 . . ?
C49 C48 H48B 108.7 . . ?
H48A C48 H48B 107.6 . . ?
C48 C49 C50 115.04(16) . . ?
C48 C49 H49A 108.5 . . ?
C50 C49 H49A 108.5 . . ?
C48 C49 H49B 108.5 . . ?
C50 C49 H49B 108.5 . . ?
H49A C49 H49B 107.5 . . ?
C49 C50 C51 113.47(15) . . ?
C49 C50 H50A 108.9 . . ?
C51 C50 H50A 108.9 . . ?
C49 C50 H50B 108.9 . . ?
C51 C50 H50B 108.9 . . ?
H50A C50 H50B 107.7 . . ?
C52 C51 C50 113.32(15) . . ?
C52 C51 H51A 108.9 . . ?
C50 C51 H51A 108.9 . . ?
C52 C51 H51B 108.9 . . ?
C50 C51 H51B 108.9 . . ?
H51A C51 H51B 107.7 . . ?
C51 C52 Si02 119.20(13) . . ?
C51 C52 H52A 107.5 . . ?
Si02 C52 H52A 107.5 . . ?
C51 C52 H52B 107.5 . . ?
Si02 C52 H52B 107.5 . . ?
H52A C52 H52B 107.0 . . ?
C54 C53 Si01 115.30(10) . . ?
C54 C53 H53A 108.4 . . ?
Si01 C53 H53A 108.4 . . ?
C54 C53 H53B 108.4 . . ?
Si01 C53 H53B 108.4 . . ?
H53A C53 H53B 107.5 . . ?
C55 C54 C53 113.61(13) . . ?
C55 C54 H54A 108.8 . . ?
C53 C54 H54A 108.8 . . ?
C55 C54 H54B 108.8 . . ?
C53 C54 H54B 108.8 . . ?
H54A C54 H54B 107.7 . . ?
C54 C55 C56 114.14(13) . . ?
C54 C55 H55A 108.7 . . ?
C56 C55 H55A 108.7 . . ?
C54 C55 H55B 108.7 . . ?
C56 C55 H55B 108.7 . . ?
H55A C55 H55B 107.6 . . ?
C57 C56 C55 112.48(13) . . ?
C57 C56 H56A 109.1 . . ?
C55 C56 H56A 109.1 . . ?
C57 C56 H56B 109.1 . . ?
C55 C56 H56B 109.1 . . ?
H56A C56 H56B 107.8 . . ?
C56 C57 C58 115.30(14) . . ?
C56 C57 H57A 108.4 . . ?
C58 C57 H57A 108.4 . . ?
C56 C57 H57B 108.4 . . ?
C58 C57 H57B 108.4 . . ?
H57A C57 H57B 107.5 . . ?
C57 C58 C59 111.15(14) . . ?
C57 C58 H58A 109.4 . . ?
C59 C58 H58A 109.4 . . ?
C57 C58 H58B 109.4 . . ?
C59 C58 H58B 109.4 . . ?
H58A C58 H58B 108.0 . . ?
C60 C59 C58 115.06(15) . . ?
C60 C59 H59A 108.5 . . ?
C58 C59 H59A 108.5 . . ?
C60 C59 H59B 108.5 . . ?
C58 C59 H59B 108.5 . . ?
H59A C59 H59B 107.5 . . ?
C59 C60 C61 112.57(15) . . ?
C59 C60 H60A 109.1 . . ?
C61 C60 H60A 109.1 . . ?
C59 C60 H60B 109.1 . . ?
C61 C60 H60B 109.1 . . ?
H60A C60 H60B 107.8 . . ?
C62 C61 C60 113.80(15) . . ?
C62 C61 H61A 108.8 . . ?
C60 C61 H61A 108.8 . . ?
C62 C61 H61B 108.8 . . ?
C60 C61 H61B 108.8 . . ?
H61A C61 H61B 107.7 . . ?
C63 C62 C61 113.79(15) . . ?
C63 C62 H62A 108.8 . . ?
C61 C62 H62A 108.8 . . ?
C63 C62 H62B 108.8 . . ?
C61 C62 H62B 108.8 . . ?
H62A C62 H62B 107.7 . . ?
C62 C63 C64 114.77(15) . . ?
C62 C63 H63A 108.6 . . ?
C64 C63 H63A 108.6 . . ?
C62 C63 H63B 108.6 . . ?
C64 C63 H63B 108.6 . . ?
H63A C63 H63B 107.6 . . ?
C63 C64 C65 111.74(15) . . ?
C63 C64 H64A 109.3 . . ?
C65 C64 H64A 109.3 . . ?
C63 C64 H64B 109.3 . . ?
C65 C64 H64B 109.3 . . ?
H64A C64 H64B 107.9 . . ?
C66 C65 C64 114.54(16) . . ?
C66 C65 H65A 108.6 . . ?
C64 C65 H65A 108.6 . . ?
C66 C65 H65B 108.6 . . ?
C64 C65 H65B 108.6 . . ?
H65A C65 H65B 107.6 . . ?
C67 C66 C65 113.48(16) . . ?
C67 C66 H66A 108.9 . . ?
C65 C66 H66A 108.9 . . ?
C67 C66 H66B 108.9 . . ?
C65 C66 H66B 108.9 . . ?
H66A C66 H66B 107.7 . . ?
C66 C67 C68 113.80(15) . . ?
C66 C67 H67A 108.8 . . ?
C68 C67 H67A 108.8 . . ?
C66 C67 H67B 108.8 . . ?
C68 C67 H67B 108.8 . . ?
H67A C67 H67B 107.7 . . ?
C69 C68 C67 112.55(15) . . ?
C69 C68 H68A 109.1 . . ?
C67 C68 H68A 109.1 . . ?
C69 C68 H68B 109.1 . . ?
C67 C68 H68B 109.1 . . ?
H68A C68 H68B 107.8 . . ?
C68 C69 C70 114.51(14) . . ?
C68 C69 H69A 108.6 . . ?
C70 C69 H69A 108.6 . . ?
C68 C69 H69B 108.6 . . ?
C70 C69 H69B 108.6 . . ?
H69A C69 H69B 107.6 . . ?
C69 C70 Si02 114.11(12) . . ?
C69 C70 H70A 108.7 . . ?
Si02 C70 H70A 108.7 . . ?
C69 C70 H70B 108.7 . . ?
Si02 C70 H70B 108.7 . . ?
H70A C70 H70B 107.6 . . ?

_diffrn_measured_fraction_theta_max 0.857
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.978
_refine_diff_density_max         0.602
_refine_diff_density_min         -0.356
_refine_diff_density_rms         0.088
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: methanol/tetrahydrofuran'
_chemical_compound_source        no
_exptl_crystal_preparation       Luminescent
####################################################################### 
# 
# 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/cc1jj9ly
_database_code_depnum_ccdc_archive 'CCDC 1415850'
_audit_update_record             
;
2015-07-30 deposited with the CCDC.
2015-08-26 downloaded from the CCDC.
;



_audit_creation_method           SHELXL-97
_chemical_name_systematic        2,7-bis(trimethylsilyl)pyrene
_chemical_name_common            2,7-TMSpyrene
_chemical_melting_point          '477-479 K'
_chemical_formula_moiety         'C22 H26 Si2'
_chemical_formula_sum            'C22 H26 Si2'
_chemical_formula_weight         346.61

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

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 2(1)/c'
_space_group_name_Hall           '-P 2ybc'

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

_cell_length_a                   6.3540(12)
_cell_length_b                   16.626(3)
_cell_length_c                   9.3688(17)
_cell_angle_alpha                90.00
_cell_angle_beta                 100.456(2)
_cell_angle_gamma                90.00
_cell_volume                     973.3(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    2568
_cell_measurement_theta_min      2.53
_cell_measurement_theta_max      27.83

_exptl_crystal_description       plate
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_exptl_crystal_density_diffrn    1.183
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             372
_exptl_absorpt_coefficient_mu    0.183
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8526
_exptl_absorpt_correction_T_max  0.9644
_exptl_absorpt_process_details   'SADABS Bruker'

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      100(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            5274
_diffrn_reflns_av_R_equivalents  0.0188
_diffrn_reflns_av_sigmaI/netI    0.0241
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_theta_min         2.45
_diffrn_reflns_theta_max         28.06
_reflns_number_total             2118
_reflns_number_gt                1874
_reflns_threshold_expression     >2sigma(I)

_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-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX (Farrugia, 1999)'

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0459P)²+0.3645P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         2118
_refine_ls_number_parameters     109
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0375
_refine_ls_R_factor_gt           0.0331
_refine_ls_wR_factor_ref         0.0905
_refine_ls_wR_factor_gt          0.0875
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_restrained_S_all      1.056
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Si01 Si 0.63630(6) 0.15400(2) 0.01398(4) 0.01800(13) Uani 1 1 d . . .
C01 C 0.5891(2) 0.09906(8) 0.18089(14) 0.0179(3) Uani 1 1 d . . .
C02 C 0.7238(2) 0.03725(8) 0.24373(14) 0.0187(3) Uani 1 1 d . . .
H02 H 0.8414 0.0222 0.1998 0.022 Uiso 1 1 calc R . .
C03 C 0.6917(2) -0.00324(8) 0.36889(14) 0.0169(3) Uani 1 1 d . . .
C04 C 0.5174(2) 0.01972(8) 0.43578(14) 0.0158(3) Uani 1 1 d . . .
C05 C 0.3782(2) 0.08234(8) 0.37370(14) 0.0166(3) Uani 1 1 d . . .
C06 C 0.4160(2) 0.11997(8) 0.24721(14) 0.0183(3) Uani 1 1 d . . .
H06 H 0.3211 0.1611 0.2048 0.022 Uiso 1 1 calc R . .
C07 C 0.8287(2) -0.06729(8) 0.43354(15) 0.0192(3) Uani 1 1 d . . .
H07 H 0.9448 -0.0838 0.3892 0.023 Uiso 1 1 calc R . .
C08 C 0.2038(2) 0.10453(8) 0.44418(15) 0.0188(3) Uani 1 1 d . . .
H08 H 0.1093 0.1463 0.4039 0.023 Uiso 1 1 calc R . .
C09 C 0.3718(2) 0.17513(9) -0.10226(16) 0.0246(3) Uani 1 1 d . . .
H09A H 0.2862 0.2088 -0.0486 0.037 Uiso 1 1 calc R . .
H09B H 0.2966 0.1243 -0.1291 0.037 Uiso 1 1 calc R . .
H09C H 0.3933 0.2034 -0.1903 0.037 Uiso 1 1 calc R . .
C10 C 0.8032(2) 0.09005(9) -0.08518(16) 0.0262(3) Uani 1 1 d . . .
H10A H 0.9415 0.0795 -0.0225 0.039 Uiso 1 1 calc R . .
H10B H 0.8264 0.1181 -0.1731 0.039 Uiso 1 1 calc R . .
H10C H 0.7295 0.0390 -0.1120 0.039 Uiso 1 1 calc R . .
C11 C 0.7740(3) 0.25178(9) 0.06754(18) 0.0298(3) Uani 1 1 d . . .
H11A H 0.9135 0.2414 0.1289 0.045 Uiso 1 1 calc R . .
H11B H 0.6861 0.2842 0.1215 0.045 Uiso 1 1 calc R . .
H11C H 0.7946 0.2810 -0.0198 0.045 Uiso 1 1 calc R . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Si01 C09 1.8629(15) . ?
Si01 C10 1.8645(15) . ?
Si01 C11 1.8712(15) . ?
Si01 C01 1.8814(14) . ?
C01 C02 1.3969(19) . ?
C01 C06 1.4016(18) . ?
C02 C03 1.3988(18) . ?
C02 H02 0.9500 . ?
C03 C04 1.4199(18) . ?
C03 C07 1.4379(18) . ?
C04 C05 1.4207(18) . ?
C04 C04 1.423(3) 3_656 ?
C05 C06 1.3990(18) . ?
C05 C08 1.4372(18) . ?
C06 H06 0.9500 . ?
C07 C08 1.3506(19) 3_656 ?
C07 H07 0.9500 . ?
C08 C07 1.3506(19) 3_656 ?
C08 H08 0.9500 . ?
C09 H09A 0.9800 . ?
C09 H09B 0.9800 . ?
C09 H09C 0.9800 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 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
C09 Si01 C10 110.54(7) . . ?
C09 Si01 C11 108.75(7) . . ?
C10 Si01 C11 110.39(7) . . ?
C09 Si01 C01 108.33(6) . . ?
C10 Si01 C01 109.16(6) . . ?
C11 Si01 C01 109.65(7) . . ?
C02 C01 C06 117.74(12) . . ?
C02 C01 Si01 121.98(10) . . ?
C06 C01 Si01 120.27(10) . . ?
C01 C02 C03 122.41(12) . . ?
C01 C02 H02 118.8 . . ?
C03 C02 H02 118.8 . . ?
C02 C03 C04 118.99(12) . . ?
C02 C03 C07 122.70(12) . . ?
C04 C03 C07 118.31(12) . . ?
C03 C04 C05 119.59(12) . . ?
C03 C04 C04 120.20(15) . 3_656 ?
C05 C04 C04 120.21(14) . 3_656 ?
C06 C05 C04 118.98(12) . . ?
C06 C05 C08 122.67(12) . . ?
C04 C05 C08 118.35(12) . . ?
C01 C06 C05 122.27(12) . . ?
C01 C06 H06 118.9 . . ?
C05 C06 H06 118.9 . . ?
C08 C07 C03 121.52(12) 3_656 . ?
C08 C07 H07 119.2 3_656 . ?
C03 C07 H07 119.2 . . ?
C07 C08 C05 121.42(12) 3_656 . ?
C07 C08 H08 119.3 3_656 . ?
C05 C08 H08 119.3 . . ?
Si01 C09 H09A 109.5 . . ?
Si01 C09 H09B 109.5 . . ?
H09A C09 H09B 109.5 . . ?
Si01 C09 H09C 109.5 . . ?
H09A C09 H09C 109.5 . . ?
H09B C09 H09C 109.5 . . ?
Si01 C10 H10A 109.5 . . ?
Si01 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
Si01 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
Si01 C11 H11A 109.5 . . ?
Si01 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
Si01 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?

_diffrn_measured_fraction_theta_max 0.894
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         0.361
_refine_diff_density_min         -0.195
_refine_diff_density_rms         0.048
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: dichloromethane'
_chemical_compound_source        no
_exptl_crystal_preparation       Luminescent
