# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2007 data_global _journal_name_full Chem.Commun. _journal_coden_cambridge 0182 _publ_contact_author_name 'Joseph Mabry' _publ_contact_author_address ; Propulsion Materials Branch Air Force Research Laboratory 10 E. Saturn Blvd. Edwards AFB CA 93524 UNITED STATES OF AMERICA ; _publ_contact_author_email JOSEPH.MABRY@EDWARDS.AF.MIL loop_ _publ_author_name _publ_author_address J.Mabry ;AFRL/PRSM 10 E. Saturn Blvd., BLDG 8451, Edwards AFB, CA 93524 ; S.T.Iacono ;AFRL/PRSM 10 E. Saturn Blvd., BLDG 8451, Edwards AFB, CA 93524 and Department of Chemistry and Center for Optical Material Science" & Engineering Technologies (COMSET), Advanced Materials research Laboratory Clemson University, Clemson, SC 29634 ; A.Vij ;AFRL/PRSP 10 E. Saturn Blvd., BLDG 8451, Edwards AFB, CA 93524 ; W.Grabow ;AFRL/PRSP 10 E. Saturn Blvd., BLDG 8451, Edwards AFB, CA 93524 ; 'D.Smith Junior' ;Department of Chemistry and Center for Optical Material Science" & Engineering Technologies (COMSET), Advanced Materials research Laboratory Clemson University, Clemson, SC 29634 ; _publ_section_title ; Facile Synthesis of Hydrophobic Fluoroalkyl Functionalized Silsesquioxane Nanostructures via Novel Corner-Capping Methodology ; # Attachment 'CCDC629369.cif' data_Octa(3,3,3-trifluropropyl)-T8-Silsesquioxane _database_code_depnum_ccdc_archive 'CCDC 629369' _audit_creation_method SHELXL-97 _chemical_name_systematic Octa(3,3,3-trifluropropyl)-T8-Silsesquioxane _chemical_name_common Octa(3,3,3-trifluropropyl)-T8-Silsesquioxane _chemical_melting_point 507 _chemical_formula_moiety Si8O12(CH2CH2CF3)8.THF _chemical_formula_sum 'C28 H40 F24 O13 Si8' _chemical_formula_weight 1265.32 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 '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 tetragonal _symmetry_space_group_name_H-M 'I 41/a' _symmetry_int_tables_number 88 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-y+3/4, x+1/4, z+1/4' 'y+3/4, -x+3/4, z+3/4' 'x+1/2, y+1/2, z+1/2' '-x+1, -y+1/2, z+1' '-y+5/4, x+3/4, z+3/4' 'y+5/4, -x+5/4, z+5/4' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'y-3/4, -x-1/4, -z-1/4' '-y-3/4, x-3/4, -z-3/4' '-x+1/2, -y+1/2, -z+1/2' 'x, y+1/2, -z' 'y-1/4, -x+1/4, -z+1/4' '-y-1/4, x-1/4, -z-1/4' _cell_length_a 21.1129(7) _cell_length_b 21.1129(7) _cell_length_c 11.1505(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4970.4(4) _cell_formula_units_Z 4 _cell_measurement_temperature 103(2) _cell_measurement_reflns_used 2275 _cell_measurement_theta_min 2.07 _cell_measurement_theta_max 25.35 _exptl_crystal_description Block _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.37 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.686 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2544 _exptl_absorpt_coefficient_mu 0.361 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 103.0(1) _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_source_type 'Bruker APEX' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 23774 _diffrn_reflns_av_R_equivalents 0.0219 _diffrn_reflns_av_sigmaI/netI 0.0108 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.07 _diffrn_reflns_theta_max 25.35 _reflns_number_total 2275 _reflns_number_gt 2096 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SMART' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'X-Seed and Mercury' _computing_publication_material 'Encifer v1.2' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The asymmetric unit shows an ordered (C1-C3) and a disordered (C4-C6) trifluoropropyl chains, which were refined with occupancies of 67% and 33%, respectively. During the refinement of disordered trifluoropropyl groups, the disorder originates from the alpha carbon (C4). Therefore, in order to have an effective convergence, the C-C distances as well as the C-F distances in these chains were restrained to be same using SADI while the thermal behavior was restrained using SIMU and DELU commands. After a stable minimum was reached, hydrogen atoms were added at calculated positions to the alpha and beta carbon atoms. The disorder in the THF molecule was much more difficult to model as this molecule shows both positional as well as rotational disorder. The positional disorder stems from the two different envelope conformations of the THF molecules with oxygen atoms lying above and below the mean plane formed by the carbon atoms. In the major component, refined with an occupancy of 83%, the oxygen atoms is located 0.3758 angstrom above the mean plane, whereas in the minor component, the oxygen atoms is located -0.4165 angstrom below this plane. This model was further further rotationally disordered due to the four- fold axis passing through the THF molecule. The final model refined satisfactorily by fixing the site occupancy for each of the four disordered positions to 0.25 (with total occupancy as 1.0), and constraining all C-C and C-O distances to 1.52(01) and 1.43(01) angstrom, respectively. The thermal behavior was modeled for all the carbon and oxygen atoms using SIMU, DELU and ISOR commands. Without the use of these restraints, the structure showed unusually large thermal motion of the fluoroalkyl chains and the THF ring. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0527P)^2^+4.2862P] where P=(Fo^2^+2Fc^2^)/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 2276 _refine_ls_number_parameters 244 _refine_ls_number_restraints 160 _refine_ls_R_factor_all 0.0306 _refine_ls_R_factor_gt 0.0286 _refine_ls_wR_factor_ref 0.0880 _refine_ls_wR_factor_gt 0.0857 _refine_ls_goodness_of_fit_ref 1.090 _refine_ls_restrained_S_all 1.061 _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 Si1 Si 0.023200(17) 0.850639(17) 0.01695(3) 0.01684(14) Uani 1 1 d . . . C1 C 0.04210(7) 0.92197(7) 0.10521(12) 0.0198(3) Uani 1 1 d . . . H1A H 0.0139 0.9570 0.0801 0.024 Uiso 1 1 calc R . . H1B H 0.0341 0.9134 0.1912 0.024 Uiso 1 1 calc R . . C2 C 0.11109(7) 0.94223(7) 0.08883(14) 0.0234(3) Uani 1 1 d . . . H2A H 0.1391 0.9088 0.1214 0.028 Uiso 1 1 calc R . . H2B H 0.1201 0.9463 0.0020 0.028 Uiso 1 1 calc R . . C3 C 0.12629(7) 1.00333(7) 0.14905(15) 0.0274(3) Uani 1 1 d . . . F1 F 0.18772(5) 1.01875(5) 0.13822(10) 0.0401(3) Uani 1 1 d . . . F2 F 0.11325(5) 1.00247(5) 0.26640(9) 0.0437(3) Uani 1 1 d . . . F3 F 0.09363(5) 1.05226(5) 0.10422(11) 0.0461(3) Uani 1 1 d . . . Si2 Si 0.101123(17) 0.725957(17) 0.01614(3) 0.01654(14) Uani 1 1 d . A . C4 C 0.17434(7) 0.71016(7) 0.10097(13) 0.0225(3) Uani 1 1 d D . . H4A H 0.2081 0.7392 0.0730 0.027 Uiso 0.673(16) 1 calc PR A 1 H4B H 0.1668 0.7187 0.1871 0.027 Uiso 0.673(16) 1 calc PR A 1 H4C H 0.2033 0.7465 0.0898 0.027 Uiso 0.327(16) 1 d PR A 2 H4D H 0.1635 0.7081 0.1873 0.027 Uiso 0.327(16) 1 d PR A 2 C5 C 0.1965(3) 0.6417(3) 0.0856(8) 0.0277(11) Uani 0.673(16) 1 d PDU A 1 H5A H 0.1707 0.6138 0.1378 0.033 Uiso 0.673(16) 1 calc PR A 1 H5B H 0.1895 0.6284 0.0015 0.033 Uiso 0.673(16) 1 calc PR A 1 C6 C 0.2646(4) 0.6333(3) 0.1160(6) 0.0329(15) Uani 0.673(16) 1 d PDU A 1 F4 F 0.2803(4) 0.6532(3) 0.2266(6) 0.0548(13) Uani 0.673(16) 1 d PDU A 1 F5 F 0.2842(2) 0.57273(16) 0.1082(6) 0.0603(10) Uani 0.673(16) 1 d PDU A 1 F6 F 0.3031(2) 0.66494(18) 0.0409(5) 0.0569(11) Uani 0.673(16) 1 d PDU A 1 C5D C 0.2095(8) 0.6498(6) 0.0674(16) 0.038(3) Uani 0.327(16) 1 d PDU A 2 H5DA H 0.1830 0.6130 0.0897 0.046 Uiso 0.327(16) 1 calc PR A 2 H5DB H 0.2152 0.6489 -0.0207 0.046 Uiso 0.327(16) 1 calc PR A 2 C6D C 0.2730(8) 0.6428(7) 0.1256(14) 0.042(4) Uani 0.327(16) 1 d PDU A 2 F4D F 0.2676(7) 0.6416(7) 0.2406(11) 0.062(3) Uani 0.327(16) 1 d PDU A 2 F5D F 0.2996(9) 0.5905(10) 0.0939(14) 0.117(5) Uani 0.327(16) 1 d PDU A 2 F6D F 0.3092(3) 0.6896(9) 0.0970(17) 0.088(5) Uani 0.327(16) 1 d PDU A 2 O1 O 0.07412(5) 0.79550(4) 0.04850(9) 0.0212(2) Uani 1 1 d . . . O2 O 0.04752(4) 0.67357(5) 0.04830(9) 0.0209(2) Uani 1 1 d . . . O3 O 0.11676(5) 0.72151(5) -0.12559(8) 0.0217(2) Uani 1 1 d . . . O1T O 0.4913(4) 0.6754(6) 0.1686(12) 0.059(3) Uani 0.175(4) 1 d PDU B -3 C2T C 0.5486(5) 0.7029(7) 0.1279(11) 0.048(3) Uani 0.25 1 d PDU B -3 H2TA H 0.5605 0.6837 0.0501 0.057 Uiso 0.175(4) 1 d PR B -3 H2TB H 0.5827 0.6936 0.1860 0.057 Uiso 0.175(4) 1 d PR B -3 H2TC H 0.5603 0.6940 0.2093 0.057 Uiso 0.075(4) 1 d PR C -3 H2TD H 0.5819 0.6877 0.0770 0.057 Uiso 0.075(4) 1 d PR C -3 C3T C 0.5434(6) 0.7744(8) 0.1134(19) 0.042(3) Uani 0.25 1 d PDU B -3 H3TA H 0.5586 0.7890 0.0341 0.050 Uiso 0.25 1 calc PR B -3 H3TB H 0.5656 0.7977 0.1780 0.050 Uiso 0.25 1 calc PR B -3 C4T C 0.4716(6) 0.7785(6) 0.1250(16) 0.048(3) Uani 0.25 1 d PDU B -3 H4TA H 0.4545 0.8020 0.0553 0.057 Uiso 0.25 1 calc PR B -3 H4TB H 0.4610 0.8029 0.1982 0.057 Uiso 0.25 1 calc PR B -3 C5T C 0.4395(5) 0.7139(6) 0.1317(13) 0.042(3) Uani 0.25 1 d PDU B -3 H5TA H 0.4051 0.7137 0.1921 0.050 Uiso 0.175(4) 1 d PR B -3 H5TB H 0.4224 0.7002 0.0532 0.050 Uiso 0.175(4) 1 d PR B -3 H5TC H 0.4043 0.7115 0.0773 0.050 Uiso 0.075(4) 1 d PR C -3 H5TD H 0.4245 0.7060 0.2117 0.050 Uiso 0.075(4) 1 d PR C -3 O1TD O 0.4900(6) 0.6719(10) 0.098(3) 0.057(7) Uani 0.075(4) 1 d PD B -3 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Si1 0.0166(2) 0.0152(2) 0.0187(2) -0.00193(13) -0.00068(13) -0.00027(13) C1 0.0197(7) 0.0179(7) 0.0219(7) -0.0034(5) -0.0001(5) 0.0002(5) C2 0.0194(7) 0.0208(7) 0.0299(8) -0.0066(6) -0.0006(6) 0.0007(5) C3 0.0210(7) 0.0223(8) 0.0388(9) -0.0053(6) -0.0010(6) -0.0004(6) F1 0.0228(5) 0.0339(5) 0.0637(7) -0.0148(5) 0.0000(4) -0.0085(4) F2 0.0471(6) 0.0480(6) 0.0360(6) -0.0192(5) 0.0003(5) -0.0125(5) F3 0.0386(6) 0.0186(5) 0.0812(8) 0.0025(5) -0.0099(5) 0.0019(4) Si2 0.0152(2) 0.0162(2) 0.0182(2) 0.00028(13) -0.00153(13) 0.00039(13) C4 0.0199(7) 0.0223(7) 0.0253(7) 0.0007(6) -0.0044(6) -0.0001(5) C5 0.019(2) 0.0217(16) 0.043(3) 0.0058(14) -0.0065(16) 0.0016(13) C6 0.029(3) 0.034(2) 0.036(2) 0.0065(16) -0.0041(19) 0.0015(17) F4 0.041(3) 0.075(2) 0.048(2) -0.0063(19) -0.0226(17) 0.0189(19) F5 0.0486(15) 0.0335(13) 0.099(2) 0.0080(14) -0.0155(13) 0.0206(12) F6 0.0321(12) 0.0631(17) 0.075(2) 0.0205(14) 0.0175(13) 0.0104(10) C5D 0.032(6) 0.042(6) 0.041(5) -0.010(5) -0.009(4) 0.007(4) C6D 0.023(5) 0.054(6) 0.050(7) 0.000(5) -0.011(4) 0.025(5) F4D 0.040(5) 0.103(7) 0.044(3) 0.029(3) -0.013(3) 0.013(4) F5D 0.111(9) 0.120(8) 0.120(8) -0.055(7) -0.061(7) 0.099(8) F6D 0.017(2) 0.131(9) 0.114(8) 0.066(8) -0.002(3) 0.003(3) O1 0.0208(5) 0.0183(5) 0.0244(5) -0.0019(4) -0.0022(4) 0.0022(4) O2 0.0190(5) 0.0198(5) 0.0238(5) 0.0028(4) -0.0013(4) -0.0018(4) O3 0.0213(5) 0.0231(5) 0.0208(6) 0.0002(4) 0.0005(4) 0.0009(4) O1T 0.037(4) 0.072(6) 0.067(7) 0.042(6) 0.002(5) 0.012(4) C2T 0.025(5) 0.065(6) 0.054(6) -0.017(6) -0.007(3) 0.014(4) C3T 0.032(4) 0.075(6) 0.018(4) 0.013(5) 0.011(3) 0.014(4) C4T 0.025(5) 0.065(6) 0.054(6) -0.017(6) -0.007(3) 0.014(4) C5T 0.032(4) 0.075(6) 0.018(4) 0.013(5) 0.011(3) 0.014(4) O1TD 0.027(10) 0.090(19) 0.053(15) -0.029(14) -0.011(10) 0.008(12) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Si1 O2 1.6163(10) 6_464 ? Si1 O3 1.6165(10) 16_665 ? Si1 O1 1.6231(10) . ? Si1 C1 1.8428(14) . ? C1 C2 1.5289(19) . ? C2 C3 1.489(2) . ? C3 F2 1.337(2) . ? C3 F3 1.3389(19) . ? C3 F1 1.3427(18) . ? Si2 O1 1.6159(10) . ? Si2 O3 1.6172(10) . ? Si2 O2 1.6227(10) . ? Si2 C4 1.8427(14) . ? C4 C5D 1.521(11) . ? C4 C5 1.529(5) . ? C5 C6 1.487(7) . ? C6 F4 1.344(7) . ? C6 F6 1.345(6) . ? C6 F5 1.347(7) . ? C5D C6D 1.498(13) . ? C6D F5D 1.287(13) . ? C6D F4D 1.288(14) . ? C6D F6D 1.290(13) . ? O2 Si1 1.6163(10) 6_464 ? O3 Si1 1.6165(10) 11_565 ? O1T C2T 1.417(9) . ? O1T C5T 1.423(9) . ? C2T O1TD 1.440(10) . ? C2T C3T 1.521(9) . ? C3T C4T 1.524(9) . ? C4T C5T 1.526(9) . ? C5T O1TD 1.437(10) . ? 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 O2 Si1 O3 109.95(6) 6_464 16_665 ? O2 Si1 O1 109.76(6) 6_464 . ? O3 Si1 O1 108.46(5) 16_665 . ? O2 Si1 C1 110.06(6) 6_464 . ? O3 Si1 C1 109.50(6) 16_665 . ? O1 Si1 C1 109.09(6) . . ? C2 C1 Si1 111.79(9) . . ? C3 C2 C1 113.18(12) . . ? F2 C3 F3 105.65(13) . . ? F2 C3 F1 106.86(13) . . ? F3 C3 F1 106.07(13) . . ? F2 C3 C2 112.65(13) . . ? F3 C3 C2 112.90(13) . . ? F1 C3 C2 112.18(13) . . ? O1 Si2 O3 110.06(6) . . ? O1 Si2 O2 108.90(6) . . ? O3 Si2 O2 108.59(5) . . ? O1 Si2 C4 110.23(6) . . ? O3 Si2 C4 108.66(6) . . ? O2 Si2 C4 110.38(6) . . ? C5D C4 C5 14.4(7) . . ? C5D C4 Si2 115.7(7) . . ? C5 C4 Si2 111.7(3) . . ? C6 C5 C4 112.5(5) . . ? F4 C6 F6 105.5(6) . . ? F4 C6 F5 106.2(6) . . ? F6 C6 F5 104.2(5) . . ? F4 C6 C5 114.3(6) . . ? F6 C6 C5 112.5(5) . . ? F5 C6 C5 113.2(5) . . ? C6D C5D C4 114.4(10) . . ? F5D C6D F4D 107.2(12) . . ? F5D C6D F6D 109.3(11) . . ? F4D C6D F6D 108.3(12) . . ? F5D C6D C5D 110.9(12) . . ? F4D C6D C5D 110.7(12) . . ? F6D C6D C5D 110.3(10) . . ? Si2 O1 Si1 146.82(7) . . ? Si1 O2 Si2 144.29(7) 6_464 . ? Si1 O3 Si2 154.95(8) 11_565 . ? C2T O1T C5T 109.2(9) . . ? O1T C2T O1TD 32.2(9) . . ? O1T C2T C3T 112.4(12) . . ? O1TD C2T C3T 111.5(17) . . ? C2T C3T C4T 96.8(13) . . ? C3T C4T C5T 113.3(13) . . ? O1T C5T O1TD 32.2(9) . . ? O1T C5T C4T 100.6(11) . . ? O1TD C5T C4T 102.1(13) . . ? C5T O1TD C2T 107.2(11) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.35 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.351 _refine_diff_density_min -0.478 _refine_diff_density_rms 0.060 _chemical_compound_source 'Synthesis via corner capping' _exptl_crystal_recrystallization_method 'Diffusion - THF Solvent' _diffrn_ambient_pressure 100 # Attachment 'CCDC642077.cif' data_Methyl-hepta(3,3,3-trifluropropyl)-T8-Silsesquioxane _database_code_depnum_ccdc_archive 'CCDC 642077' _audit_creation_method SHELXL-97 _chemical_name_systematic Methylhepta(3,3,3-trifluropropyl)-T8-Silsesquioxane _chemical_name_common Methylhepta(3,3,3-trifluropropyl)-T8-Silsesquioxane _chemical_melting_point 443 _chemical_formula_moiety Si8O12(CH3)(CH2CH2CF3)7 _chemical_formula_sum 'C22 H31 F21 O12 Si8' _chemical_formula_weight 1111.19 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 '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 'C c' _symmetry_int_tables_number 9 loop_ _symmetry_equiv_pos_as_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 13.3164(16) _cell_length_b 17.129(2) _cell_length_c 20.726(3) _cell_angle_alpha 90.00 _cell_angle_beta 105.007(2) _cell_angle_gamma 90.00 _cell_volume 4566.2(10) _cell_formula_units_Z 4 _cell_measurement_temperature 193(2) _cell_measurement_reflns_used 7818 _cell_measurement_theta_min 1.98 _cell_measurement_theta_max 25.35 _exptl_crystal_description Block _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.34 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.616 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2240 _exptl_absorpt_coefficient_mu 0.370 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 193(2) _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_source_type 'Bruker APEX' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 16235 _diffrn_reflns_av_R_equivalents 0.0168 _diffrn_reflns_av_sigmaI/netI 0.0231 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.98 _diffrn_reflns_theta_max 25.35 _reflns_number_total 7818 _reflns_number_gt 7226 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SMART' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'X-Seed and Mercury' _computing_publication_material 'Encifer v1.2' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The Si8O12 ring shows positional disorder with two components refined with an occupancy ratio of 36:64. The two POSS ring conformations were stabilized using the ISOR and BUMP commands in the refinement file. The only ordered trifluoropropyl chain is located on Si2, which is also the common atom for the two disordered POSS cubes. This ordered fragment was used to model the trifluoropropyl groups C13, C14, C15 (F13, F14 and F15) and its disordered component C13'> F15' using the SAME command (ratio 57:43), where the C-C and C-F distances were restrained using SADI. The CF3 group located on C21 shows rotational disorder where two orientations were refined with occupancies of 66:34, restraining all the C-F and F...F distances with SADI. The C-F distances in the trifluoropropyl group on C15 and C21 were fixed using DFIX with a distance of 1.32(01) angstrom. The trifluoropropyl groups located on Si1 and Si6 show disorder in the alpha and beta carbon positions, which share the terminal CF3 group. For C1 and C2, this disorder is refined with an occupancy of 71:29, whereas in the case of C16 and C17, the disorder is of the ratio of 80:20. In both these cases the C-C distances are restrained to be the same using SADI. In order to model the thermal motion effectively, SIMU and DELU commands were used to generate thermal restrains. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1010P)^2^+2.2600P] where P=(Fo^2^+2Fc^2^)/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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.08(13) _refine_ls_number_reflns 7818 _refine_ls_number_parameters 756 _refine_ls_number_restraints 649 _refine_ls_R_factor_all 0.0514 _refine_ls_R_factor_gt 0.0480 _refine_ls_wR_factor_ref 0.1395 _refine_ls_wR_factor_gt 0.1332 _refine_ls_goodness_of_fit_ref 1.022 _refine_ls_restrained_S_all 1.030 _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 Si2 Si 0.94334(10) 0.60712(6) 0.47515(5) 0.0524(3) Uani 1 1 d U A . Si1 Si 0.7431(6) 0.6151(6) 0.6144(5) 0.0314(16) Uani 0.36(2) 1 d PU A 1 Si3 Si 0.8668(8) 0.8356(8) 0.5485(7) 0.043(2) Uani 0.36(2) 1 d PU A 1 Si4 Si 0.6434(5) 0.7726(4) 0.5460(4) 0.0300(17) Uani 0.36(2) 1 d PU A 1 Si5 Si 0.8474(13) 0.7591(7) 0.4117(7) 0.045(2) Uani 0.36(2) 1 d PU A 1 Si6 Si 0.6217(7) 0.7015(4) 0.4083(4) 0.0369(17) Uani 0.36(2) 1 d PU A 1 Si7 Si 0.7220(5) 0.5446(4) 0.4768(3) 0.0318(18) Uani 0.36(2) 1 d PU A 1 Si8 Si 0.9651(7) 0.6802(4) 0.6173(3) 0.0292(18) Uani 0.36(2) 1 d PU A 1 Si1' Si 0.7645(8) 0.6177(5) 0.6225(4) 0.0627(16) Uani 0.64(2) 1 d PU A 2 Si3' Si 0.8590(7) 0.8299(6) 0.5469(5) 0.065(2) Uani 0.64(2) 1 d PU A 2 Si4' Si 0.6515(5) 0.7632(5) 0.5537(4) 0.078(2) Uani 0.64(2) 1 d PU A 2 Si5' Si 0.8320(9) 0.7568(5) 0.4044(5) 0.062(2) Uani 0.64(2) 1 d PU A 2 Si6' Si 0.6262(6) 0.6870(6) 0.4111(3) 0.0811(19) Uani 0.64(2) 1 d PU A 2 Si7' Si 0.7351(7) 0.5404(4) 0.4789(3) 0.080(2) Uani 0.64(2) 1 d PU A 2 Si8' Si 0.9735(7) 0.6832(5) 0.6150(4) 0.077(2) Uani 0.64(2) 1 d PU A 2 O1 O 0.6853(2) 0.69529(17) 0.59943(15) 0.0614(7) Uani 1 1 d . . . O2 O 0.7448(3) 0.82526(18) 0.55455(16) 0.0661(8) Uani 1 1 d . . . O3 O 0.8753(3) 0.63943(18) 0.63995(13) 0.0626(7) Uani 1 1 d . . . O4 O 0.8622(3) 0.81480(18) 0.47049(16) 0.0706(8) Uani 1 1 d . . . O5 O 0.8446(2) 0.54940(17) 0.46890(14) 0.0634(7) Uani 1 1 d . . . O6 O 0.9072(2) 0.67999(17) 0.42539(14) 0.0578(6) Uani 1 1 d . . . O7 O 0.7311(3) 0.55972(16) 0.55405(13) 0.0621(7) Uani 1 1 d . . . O8 O 0.6038(3) 0.7385(2) 0.47419(16) 0.0737(8) Uani 1 1 d . . . O9 O 0.7164(3) 0.7353(2) 0.38749(14) 0.0688(8) Uani 1 1 d . . . O10 O 0.9839(2) 0.6371(2) 0.55046(13) 0.0658(7) Uani 1 1 d . . . O11 O 0.9356(3) 0.77089(17) 0.59604(16) 0.0682(7) Uani 1 1 d . . . O12 O 0.6537(3) 0.6049(2) 0.42894(14) 0.0712(8) Uani 1 1 d . . . F1 F 0.6141(4) 0.4320(4) 0.7382(3) 0.1527(19) Uani 1 1 d U . . F2 F 0.7233(5) 0.4899(3) 0.80987(18) 0.1359(17) Uani 1 1 d U . . F3 F 0.7688(5) 0.3874(3) 0.7729(3) 0.150(2) Uani 1 1 d U . . F7 F 0.8391(4) 1.1202(3) 0.4904(3) 0.1369(16) Uani 1 1 d U A . F8 F 0.9374(5) 1.0975(2) 0.5887(3) 0.161(2) Uani 1 1 d U A . F9 F 0.9812(5) 1.0678(4) 0.5058(5) 0.193(3) Uani 1 1 d U A . F10 F 0.4580(5) 0.9527(4) 0.6293(3) 0.182(3) Uani 1 1 d U A . F11 F 0.5144(5) 0.9079(6) 0.7291(3) 0.246(5) Uani 1 1 d U A . F12 F 0.4006(5) 0.8494(5) 0.6558(3) 0.174(3) Uani 1 1 d U A . F16 F 0.3344(6) 0.6637(7) 0.2327(4) 0.235(5) Uani 1 1 d U . . F17 F 0.2948(6) 0.7601(8) 0.2773(7) 0.295(8) Uani 1 1 d U . . F18 F 0.2432(6) 0.6537(7) 0.3029(4) 0.262(6) Uani 1 1 d U . . F19 F 0.6023(6) 0.2988(7) 0.5009(7) 0.195(7) Uani 0.659(17) 1 d PDU A 1 F20 F 0.6968(11) 0.2764(5) 0.4349(4) 0.184(6) Uani 0.659(17) 1 d PDU A 1 F21 F 0.7521(6) 0.2538(4) 0.5391(4) 0.127(3) Uani 0.659(17) 1 d PDU A 1 F19' F 0.7715(12) 0.2581(11) 0.4849(7) 0.218(13) Uani 0.341(17) 1 d PDU A 2 F21' F 0.6687(14) 0.270(2) 0.5458(13) 0.36(2) Uani 0.341(17) 1 d PDU A 2 F20' F 0.6189(10) 0.2856(9) 0.4460(7) 0.202(14) Uani 0.341(17) 1 d PDU A 2 C1 C 0.7052(6) 0.5704(3) 0.6847(3) 0.0483(17) Uani 0.711(16) 1 d PU A 1 H1A H 0.7237 0.6060 0.7236 0.058 Uiso 0.711(16) 1 calc PR A 1 H1B H 0.6288 0.5631 0.6726 0.058 Uiso 0.711(16) 1 calc PR A 1 C2 C 0.7574(6) 0.4924(4) 0.7042(3) 0.061(2) Uani 0.711(16) 1 d PU A 1 H2A H 0.8326 0.5008 0.7241 0.073 Uiso 0.711(16) 1 calc PR A 1 H2B H 0.7497 0.4600 0.6636 0.073 Uiso 0.711(16) 1 calc PR A 1 C1' C 0.773(2) 0.5573(9) 0.7015(8) 0.063(6) Uani 0.289(16) 1 d PU A 2 H1'A H 0.8384 0.5267 0.7129 0.075 Uiso 0.289(16) 1 calc PR A 2 H1'B H 0.7726 0.5922 0.7395 0.075 Uiso 0.289(16) 1 calc PR A 2 C2' C 0.6825(17) 0.5043(12) 0.6885(8) 0.077(6) Uani 0.289(16) 1 d PU A 2 H2'A H 0.6760 0.4739 0.6470 0.092 Uiso 0.289(16) 1 calc PR A 2 H2'B H 0.6171 0.5334 0.6854 0.092 Uiso 0.289(16) 1 calc PR A 2 C3 C 0.7115(5) 0.4491(3) 0.7536(3) 0.0860(15) Uani 1 1 d U . . C4 C 1.0442(4) 0.5515(3) 0.4497(2) 0.0675(11) Uani 1 1 d DU . . H4A H 1.1032 0.5867 0.4500 0.081 Uiso 1 1 calc R A . H4B H 1.0700 0.5099 0.4831 0.081 Uiso 1 1 calc R . . C5 C 1.0083(4) 0.5148(3) 0.3821(2) 0.0761(13) Uani 1 1 d DU A . H5A H 0.9432 0.4858 0.3797 0.091 Uiso 1 1 calc R . . H5B H 0.9921 0.5568 0.3481 0.091 Uiso 1 1 calc R . . C6 C 1.0846(6) 0.4608(4) 0.3651(3) 0.100(2) Uani 1 1 d DU . . F4 F 1.1172(6) 0.4073(3) 0.4097(2) 0.157(2) Uani 1 1 d DU A . F5 F 1.0485(4) 0.4263(3) 0.3074(2) 0.1410(18) Uani 1 1 d DU A . F6 F 1.1727(4) 0.4992(4) 0.3632(3) 0.1516(19) Uani 1 1 d DU A . C7 C 0.9155(4) 0.9306(3) 0.5695(2) 0.0715(11) Uani 1 1 d U . . H7A H 0.9217 0.9395 0.6176 0.086 Uiso 1 1 calc R A 1 H7B H 0.9862 0.9339 0.5626 0.086 Uiso 1 1 calc R A 1 C8 C 0.8500(4) 0.9949(3) 0.5301(4) 0.100(2) Uani 1 1 d U A . H8A H 0.8216 0.9761 0.4838 0.120 Uiso 1 1 calc R . . H8B H 0.7904 1.0041 0.5494 0.120 Uiso 1 1 calc R . . C9 C 0.9008(5) 1.0680(3) 0.5274(3) 0.0881(15) Uani 1 1 d U . . C10 C 0.5423(4) 0.8213(3) 0.5743(2) 0.0711(12) Uani 1 1 d U . . H10A H 0.5199 0.8681 0.5463 0.085 Uiso 1 1 calc R A 1 H10B H 0.4817 0.7859 0.5676 0.085 Uiso 1 1 calc R A 1 C11 C 0.5743(5) 0.8462(5) 0.6471(3) 0.108(2) Uani 1 1 d U A . H11A H 0.5903 0.7991 0.6757 0.130 Uiso 1 1 calc R . . H11B H 0.6383 0.8781 0.6550 0.130 Uiso 1 1 calc R . . C12 C 0.4909(7) 0.8925(7) 0.6667(4) 0.148(4) Uani 1 1 d U . . C16 C 0.5089(5) 0.7060(5) 0.3369(3) 0.066(2) Uani 0.80(2) 1 d PDU A 1 H16A H 0.4931 0.7614 0.3247 0.080 Uiso 0.80(2) 1 calc PR A 1 H16B H 0.5257 0.6799 0.2985 0.080 Uiso 0.80(2) 1 calc PR A 1 C16' C 0.4978(19) 0.658(2) 0.3570(13) 0.080(11) Uani 0.20(2) 1 d PDU A 2 H16C H 0.5071 0.6417 0.3132 0.097 Uiso 0.20(2) 1 calc PR A 2 H16D H 0.4721 0.6128 0.3773 0.097 Uiso 0.20(2) 1 calc PR A 2 C17 C 0.4149(8) 0.6686(9) 0.3498(6) 0.128(5) Uani 0.79(3) 1 d PDU A 1 H17A H 0.4051 0.6868 0.3930 0.153 Uiso 0.79(3) 1 calc PR A 1 H17B H 0.4238 0.6112 0.3520 0.153 Uiso 0.79(3) 1 calc PR A 1 C17' C 0.4180(18) 0.720(2) 0.3457(14) 0.13(2) Uani 0.21(3) 1 d PDU A 2 H17C H 0.4450 0.7680 0.3297 0.157 Uiso 0.21(3) 1 calc PR A 2 H17D H 0.4002 0.7321 0.3881 0.157 Uiso 0.21(3) 1 calc PR A 2 C18 C 0.3167(8) 0.6908(10) 0.2914(6) 0.180(6) Uani 1 1 d DU . . C19 C 0.6745(4) 0.4441(3) 0.4549(2) 0.0674(10) Uani 1 1 d U . . H19A H 0.6013 0.4405 0.4572 0.081 Uiso 1 1 calc R A 1 H19B H 0.6762 0.4331 0.4083 0.081 Uiso 1 1 calc R A 1 C20 C 0.7374(5) 0.3830(4) 0.5001(4) 0.106(2) Uani 1 1 d U A . H20A H 0.8070 0.3809 0.4913 0.127 Uiso 1 1 calc R . . H20B H 0.7474 0.4007 0.5468 0.127 Uiso 1 1 calc R . . C21 C 0.6953(5) 0.3025(4) 0.4948(4) 0.120(3) Uani 1 1 d DU . . C22 C 1.0902(4) 0.6798(3) 0.6826(2) 0.0745(12) Uani 1 1 d U . . H22A H 1.1108 0.6258 0.6951 0.112 Uiso 1 1 calc R A 1 H22B H 1.0821 0.7084 0.7219 0.112 Uiso 1 1 calc R A 1 H22C H 1.1439 0.7050 0.6653 0.112 Uiso 1 1 calc R A 1 C13 C 0.8567(12) 0.8014(7) 0.3307(6) 0.091(5) Uani 0.566(11) 1 d PDU A 1 H13A H 0.9243 0.7847 0.3239 0.109 Uiso 0.566(11) 1 calc PR A 1 H13B H 0.8021 0.7760 0.2952 0.109 Uiso 0.566(11) 1 calc PR A 1 C14 C 0.8485(10) 0.8812(6) 0.3185(5) 0.093(3) Uani 0.566(11) 1 d PDU A 1 H14A H 0.8855 0.9081 0.3602 0.111 Uiso 0.566(11) 1 calc PR A 1 H14B H 0.7741 0.8954 0.3098 0.111 Uiso 0.566(11) 1 calc PR A 1 C15 C 0.8875(10) 0.9136(7) 0.2637(5) 0.169(11) Uani 0.566(11) 1 d PDU A 1 F13 F 0.8518(13) 0.9844(7) 0.2467(7) 0.242(8) Uani 0.566(11) 1 d PDU A 1 F14 F 0.8584(10) 0.8712(8) 0.2084(4) 0.169(7) Uani 0.566(11) 1 d PDU A 1 F15 F 0.9893(9) 0.9188(11) 0.2754(7) 0.237(10) Uani 0.566(11) 1 d PDU A 1 C13' C 0.8884(12) 0.8175(13) 0.3457(7) 0.081(6) Uani 0.434(11) 1 d PDU A 2 H13C H 0.8326 0.8534 0.3223 0.098 Uiso 0.434(11) 1 calc PR A 2 H13D H 0.9433 0.8505 0.3743 0.098 Uiso 0.434(11) 1 calc PR A 2 C14' C 0.930(2) 0.7865(11) 0.2983(13) 0.214(16) Uani 0.434(11) 1 d PDU A 2 H14C H 0.8795 0.7493 0.2709 0.257 Uiso 0.434(11) 1 calc PR A 2 H14D H 0.9935 0.7572 0.3201 0.257 Uiso 0.434(11) 1 calc PR A 2 C15' C 0.9556(14) 0.8482(10) 0.2540(10) 0.138(9) Uani 0.434(11) 1 d PDU A 2 F13' F 0.967(2) 0.8069(12) 0.2040(10) 0.313(18) Uani 0.434(11) 1 d PDU A 2 F14' F 0.8894(19) 0.9047(12) 0.2320(15) 0.271(15) Uani 0.434(11) 1 d PDU A 2 F15' F 1.045(2) 0.8817(17) 0.2823(12) 0.294(18) Uani 0.434(11) 1 d PDU A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Si2 0.0570(6) 0.0625(6) 0.0412(5) -0.0010(4) 0.0189(4) 0.0118(4) Si1 0.029(3) 0.040(3) 0.024(2) 0.0040(17) 0.0054(14) 0.010(2) Si3 0.040(3) 0.043(4) 0.045(4) 0.007(3) 0.009(2) 0.010(2) Si4 0.029(2) 0.029(2) 0.0308(19) 0.0044(13) 0.0058(13) 0.0026(14) Si5 0.047(3) 0.059(3) 0.031(3) 0.017(2) 0.015(3) -0.004(2) Si6 0.040(3) 0.033(3) 0.036(2) 0.0133(17) 0.0062(15) 0.0089(13) Si7 0.032(3) 0.038(2) 0.024(2) 0.0084(18) 0.0070(16) 0.0091(17) Si8 0.030(2) 0.038(3) 0.017(2) 0.0051(17) 0.0008(15) 0.0134(16) Si1' 0.094(4) 0.061(2) 0.041(2) -0.0075(15) 0.032(3) -0.019(2) Si3' 0.099(5) 0.043(2) 0.055(3) 0.0001(16) 0.022(2) -0.006(2) Si4' 0.075(2) 0.105(4) 0.056(2) -0.014(2) 0.0186(16) 0.034(2) Si5' 0.089(5) 0.061(2) 0.0365(19) 0.0053(12) 0.014(2) 0.018(2) Si6' 0.072(2) 0.113(4) 0.049(2) -0.027(2) -0.0009(16) 0.027(3) Si7' 0.115(4) 0.074(3) 0.069(3) -0.030(2) 0.053(3) -0.030(2) Si8' 0.081(4) 0.088(4) 0.058(3) -0.006(2) 0.013(2) 0.009(2) O1 0.0614(16) 0.0655(16) 0.0634(16) -0.0065(13) 0.0269(13) 0.0036(13) O2 0.071(2) 0.0684(17) 0.0627(18) -0.0016(13) 0.0237(14) 0.0032(14) O3 0.075(2) 0.0676(16) 0.0436(12) 0.0054(12) 0.0125(12) 0.0183(14) O4 0.096(2) 0.0584(16) 0.0583(17) 0.0047(12) 0.0208(16) 0.0082(15) O5 0.0753(18) 0.0637(16) 0.0582(15) -0.0080(12) 0.0299(13) -0.0001(13) O6 0.0624(16) 0.0673(15) 0.0504(13) 0.0041(11) 0.0263(12) 0.0099(12) O7 0.091(2) 0.0582(15) 0.0461(14) -0.0060(11) 0.0335(13) -0.0032(14) O8 0.0674(19) 0.093(2) 0.0624(17) -0.0150(15) 0.0198(14) 0.0093(16) O9 0.067(2) 0.090(2) 0.0477(14) 0.0066(13) 0.0120(13) 0.0223(15) O10 0.0648(17) 0.086(2) 0.0447(13) -0.0085(13) 0.0117(12) 0.0135(15) O11 0.0771(19) 0.0628(17) 0.0595(16) 0.0060(13) 0.0081(13) 0.0089(14) O12 0.079(2) 0.083(2) 0.0502(15) -0.0073(14) 0.0134(14) -0.0019(17) F1 0.127(4) 0.179(5) 0.151(4) 0.057(4) 0.035(3) -0.013(3) F2 0.212(5) 0.153(3) 0.0582(17) 0.029(2) 0.063(2) 0.021(3) F3 0.187(5) 0.130(4) 0.153(4) 0.068(3) 0.082(4) 0.059(3) F7 0.153(4) 0.086(2) 0.165(4) 0.030(3) 0.028(3) 0.020(2) F8 0.225(6) 0.078(2) 0.155(4) -0.032(3) 0.005(4) -0.014(3) F9 0.147(4) 0.168(5) 0.308(9) 0.098(6) 0.138(5) 0.024(4) F10 0.164(5) 0.195(6) 0.175(5) -0.049(4) 0.023(4) 0.106(5) F11 0.170(5) 0.443(13) 0.104(3) -0.126(5) -0.005(3) 0.153(7) F12 0.127(4) 0.296(9) 0.108(3) -0.021(4) 0.044(3) 0.092(5) F16 0.161(6) 0.374(14) 0.117(5) 0.031(6) -0.057(4) -0.048(7) F17 0.133(5) 0.347(13) 0.338(14) 0.249(13) -0.060(6) -0.028(7) F18 0.151(5) 0.387(13) 0.199(7) 0.144(8) -0.047(5) -0.108(7) F19 0.096(5) 0.171(9) 0.294(17) 0.108(11) 0.005(8) -0.037(5) F20 0.321(18) 0.085(5) 0.139(7) -0.051(5) 0.046(9) 0.000(8) F21 0.136(6) 0.067(3) 0.165(7) 0.020(4) 0.013(5) 0.010(3) F19' 0.140(14) 0.136(13) 0.34(3) 0.06(2) -0.014(18) 0.041(11) F21' 0.35(4) 0.38(4) 0.33(4) 0.10(3) 0.05(3) -0.05(4) F20' 0.155(16) 0.097(10) 0.27(3) 0.025(13) -0.098(17) -0.095(12) C1 0.051(4) 0.057(3) 0.045(3) 0.008(2) 0.025(2) 0.014(3) C2 0.074(5) 0.065(4) 0.052(3) 0.019(2) 0.034(3) 0.018(3) C1' 0.092(16) 0.064(10) 0.043(7) -0.001(6) 0.039(8) 0.003(8) C2' 0.065(12) 0.098(13) 0.058(8) 0.023(8) -0.001(7) -0.025(9) C3 0.106(4) 0.091(3) 0.071(3) 0.030(3) 0.042(3) 0.011(3) C4 0.067(2) 0.081(3) 0.057(2) 0.0012(19) 0.0202(19) 0.024(2) C5 0.086(3) 0.089(3) 0.057(2) 0.002(2) 0.025(2) 0.035(3) C6 0.131(5) 0.101(4) 0.069(3) -0.006(3) 0.030(3) 0.044(4) F4 0.245(6) 0.114(3) 0.111(3) 0.011(2) 0.045(3) 0.106(4) F5 0.202(5) 0.140(3) 0.085(2) -0.034(2) 0.045(3) 0.056(3) F6 0.123(3) 0.192(5) 0.173(4) -0.022(4) 0.097(3) 0.025(3) C7 0.089(3) 0.057(2) 0.069(3) -0.0004(19) 0.021(2) 0.002(2) C8 0.066(3) 0.071(3) 0.150(6) 0.019(3) 0.003(3) 0.000(2) C9 0.101(4) 0.071(3) 0.094(4) 0.011(3) 0.029(3) -0.008(3) C10 0.058(2) 0.096(3) 0.057(2) -0.016(2) 0.0120(19) 0.024(2) C11 0.091(4) 0.166(6) 0.060(3) -0.034(3) 0.008(3) 0.057(4) C12 0.109(6) 0.232(11) 0.083(4) -0.069(5) -0.011(4) 0.084(6) C16 0.067(4) 0.078(4) 0.044(3) 0.010(3) -0.002(2) 0.005(3) C16' 0.047(13) 0.13(3) 0.060(13) 0.035(15) 0.012(10) 0.028(13) C17 0.101(8) 0.163(10) 0.090(6) 0.062(6) -0.029(5) -0.038(7) C17' 0.08(2) 0.26(6) 0.038(12) 0.03(2) 0.005(12) 0.05(3) C18 0.107(6) 0.287(16) 0.111(7) 0.082(9) -0.032(5) -0.059(8) C19 0.071(3) 0.062(2) 0.071(2) -0.0127(19) 0.023(2) -0.007(2) C20 0.087(4) 0.079(3) 0.134(5) -0.019(3) -0.001(4) 0.001(3) C21 0.116(6) 0.067(3) 0.173(8) 0.007(4) 0.030(5) 0.021(3) C22 0.070(3) 0.090(3) 0.054(2) 0.000(2) 0.000(2) 0.015(2) C13 0.155(15) 0.083(6) 0.031(5) 0.008(4) 0.018(7) -0.030(9) C14 0.127(9) 0.086(6) 0.072(6) 0.017(5) 0.037(5) -0.004(6) C15 0.25(3) 0.171(19) 0.130(15) 0.068(13) 0.119(17) -0.030(18) F13 0.39(2) 0.174(11) 0.192(12) 0.117(10) 0.128(13) 0.033(12) F14 0.184(10) 0.269(18) 0.065(4) 0.042(6) 0.050(5) -0.072(10) F15 0.151(9) 0.37(2) 0.184(12) 0.154(15) 0.035(8) -0.108(12) C13' 0.066(7) 0.126(15) 0.044(9) 0.017(7) -0.002(6) -0.034(7) C14' 0.25(3) 0.18(2) 0.27(3) 0.14(2) 0.15(3) 0.03(2) C15' 0.127(16) 0.138(17) 0.18(2) 0.067(17) 0.088(17) 0.018(14) F13' 0.40(4) 0.23(2) 0.33(4) 0.16(3) 0.13(3) 0.05(2) F14' 0.33(3) 0.23(2) 0.27(2) 0.181(19) 0.11(2) -0.06(2) F15' 0.41(4) 0.30(3) 0.180(19) -0.03(2) 0.09(2) -0.19(3) _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 Si2 O10 1.599(3) . ? Si2 O6 1.611(3) . ? Si2 O5 1.623(3) . ? Si2 C4 1.832(4) . ? Si1 O7 1.545(10) . ? Si1 O1 1.566(8) . ? Si1 O3 1.753(9) . ? Si1 C1 1.830(12) . ? Si3 O11 1.603(10) . ? Si3 O4 1.642(14) . ? Si3 O2 1.671(12) . ? Si3 C7 1.763(16) . ? Si4 O8 1.557(7) . ? Si4 O2 1.595(6) . ? Si4 O1 1.724(8) . ? Si4 C10 1.807(8) . ? Si5 O4 1.520(15) . ? Si5 O6 1.560(14) . ? Si5 O9 1.734(16) . ? Si5 C13 1.862(16) . ? Si6 O9 1.547(9) . ? Si6 O8 1.578(9) . ? Si6 O12 1.735(7) . ? Si6 C16 1.817(10) . ? Si7 O12 1.553(6) . ? Si7 O7 1.596(7) . ? Si7 O5 1.685(7) . ? Si7 C19 1.849(8) . ? Si8 O3 1.559(10) . ? Si8 O11 1.634(7) . ? Si8 O10 1.645(8) . ? Si8 C22 1.855(9) . ? Si1' O3 1.473(13) . ? Si1' O1 1.687(9) . ? Si1' O7 1.694(10) . ? Si1' C1' 1.915(17) . ? Si3' O2 1.571(10) . ? Si3' O11 1.600(9) . ? Si3' O4 1.617(10) . ? Si3' C7 1.891(11) . ? Si4' O1 1.494(11) . ? Si4' O2 1.632(7) . ? Si4' O8 1.660(8) . ? Si4' C10 1.899(8) . ? Si5' O9 1.533(12) . ? Si5' O6 1.642(9) . ? Si5' O4 1.656(10) . ? Si5' C13' 1.897(19) . ? Si6' O12 1.476(12) . ? Si6' O9 1.635(9) . ? Si6' O8 1.668(8) . ? Si6' C16' 1.85(3) . ? Si7' O5 1.534(9) . ? Si7' O7 1.607(6) . ? Si7' O12 1.698(9) . ? Si7' C19 1.847(7) . ? Si8' O10 1.590(9) . ? Si8' O11 1.600(8) . ? Si8' O3 1.700(11) . ? Si8' C22 1.805(9) . ? F1 C3 1.287(8) . ? F2 C3 1.333(8) . ? F3 C3 1.304(7) . ? F7 C9 1.317(7) . ? F8 C9 1.335(8) . ? F9 C9 1.263(8) . ? F10 C12 1.296(13) . ? F11 C12 1.277(8) . ? F12 C12 1.380(14) . ? F16 C18 1.378(18) . ? F17 C18 1.240(19) . ? F18 C18 1.240(11) . ? F19 C21 1.278(8) . ? F20 C21 1.325(8) . ? F21 C21 1.324(7) . ? F19' C21 1.327(9) . ? F21' C21 1.322(10) . ? F20' C21 1.269(9) . ? C1 C2 1.512(9) . ? C2 C3 1.516(7) . ? C1' C2' 1.48(3) . ? C2' C3 1.611(16) . ? C4 C5 1.497(6) . ? C5 C6 1.483(7) . ? C6 F4 1.294(7) . ? C6 F5 1.309(6) . ? C6 F6 1.355(8) . ? C7 C8 1.506(7) . ? C8 C9 1.432(8) . ? C10 C11 1.518(6) . ? C11 C12 1.504(9) . ? C16 C17 1.490(12) . ? C16' C17' 1.47(2) . ? C17 C18 1.581(11) . ? C17' C18 1.60(2) . ? C19 C20 1.505(8) . ? C20 C21 1.482(9) . ? C13 C14 1.389(14) . ? C14 C15 1.473(12) . ? C15 F15 1.318(8) . ? C15 F13 1.318(8) . ? C15 F14 1.327(8) . ? C13' C14' 1.351(18) . ? C14' C15' 1.497(15) . ? C15' F13' 1.299(8) . ? C15' F14' 1.309(8) . ? C15' F15' 1.317(8) . ? 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 O10 Si2 O6 110.20(17) . . ? O10 Si2 O5 109.63(17) . . ? O6 Si2 O5 108.64(16) . . ? O10 Si2 C4 111.12(18) . . ? O6 Si2 C4 109.78(19) . . ? O5 Si2 C4 107.4(2) . . ? O7 Si1 O1 115.8(5) . . ? O7 Si1 O3 106.0(5) . . ? O1 Si1 O3 104.7(6) . . ? O7 Si1 C1 113.4(6) . . ? O1 Si1 C1 107.6(6) . . ? O3 Si1 C1 108.8(5) . . ? O11 Si3 O4 108.9(7) . . ? O11 Si3 O2 107.0(9) . . ? O4 Si3 O2 105.1(7) . . ? O11 Si3 C7 111.8(8) . . ? O4 Si3 C7 111.2(8) . . ? O2 Si3 C7 112.5(6) . . ? O8 Si4 O2 112.7(4) . . ? O8 Si4 O1 107.5(4) . . ? O2 Si4 O1 103.8(4) . . ? O8 Si4 C10 112.7(5) . . ? O2 Si4 C10 112.5(4) . . ? O1 Si4 C10 106.9(4) . . ? O4 Si5 O6 116.4(10) . . ? O4 Si5 O9 106.9(7) . . ? O6 Si5 O9 106.1(7) . . ? O4 Si5 C13 116.9(8) . . ? O6 Si5 C13 110.6(8) . . ? O9 Si5 C13 97.3(9) . . ? O9 Si6 O8 114.1(5) . . ? O9 Si6 O12 105.1(5) . . ? O8 Si6 O12 104.6(4) . . ? O9 Si6 C16 108.6(5) . . ? O8 Si6 C16 114.1(6) . . ? O12 Si6 C16 109.8(5) . . ? O12 Si7 O7 114.3(4) . . ? O12 Si7 O5 109.1(4) . . ? O7 Si7 O5 105.4(4) . . ? O12 Si7 C19 110.9(4) . . ? O7 Si7 C19 109.2(4) . . ? O5 Si7 C19 107.5(4) . . ? O3 Si8 O11 110.9(5) . . ? O3 Si8 O10 110.4(5) . . ? O11 Si8 O10 106.2(4) . . ? O3 Si8 C22 113.1(4) . . ? O11 Si8 C22 107.9(5) . . ? O10 Si8 C22 108.0(5) . . ? O3 Si1' O1 112.5(5) . . ? O3 Si1' O7 112.5(5) . . ? O1 Si1' O7 102.4(6) . . ? O3 Si1' C1' 95.3(9) . . ? O1 Si1' C1' 124.2(8) . . ? O7 Si1' C1' 110.2(6) . . ? O2 Si3' O11 112.2(6) . . ? O2 Si3' O4 111.2(6) . . ? O11 Si3' O4 110.4(5) . . ? O2 Si3' C7 110.8(5) . . ? O11 Si3' C7 105.8(5) . . ? O4 Si3' C7 106.2(6) . . ? O1 Si4' O2 113.4(5) . . ? O1 Si4' O8 114.0(5) . . ? O2 Si4' O8 105.7(5) . . ? O1 Si4' C10 112.8(5) . . ? O2 Si4' C10 106.4(4) . . ? O8 Si4' C10 103.8(5) . . ? O9 Si5' O6 112.1(5) . . ? O9 Si5' O4 110.3(5) . . ? O6 Si5' O4 105.1(7) . . ? O9 Si5' C13' 121.8(8) . . ? O6 Si5' C13' 107.1(8) . . ? O4 Si5' C13' 98.6(7) . . ? O12 Si6' O9 113.8(6) . . ? O12 Si6' O8 113.0(5) . . ? O9 Si6' O8 105.1(5) . . ? O12 Si6' C16' 91.7(13) . . ? O9 Si6' C16' 126.0(11) . . ? O8 Si6' C16' 106.9(9) . . ? O5 Si7' O7 112.4(5) . . ? O5 Si7' O12 109.4(4) . . ? O7 Si7' O12 106.3(5) . . ? O5 Si7' C19 114.7(5) . . ? O7 Si7' C19 108.8(4) . . ? O12 Si7' C19 104.6(4) . . ? O10 Si8' O11 110.5(5) . . ? O10 Si8' O3 106.2(5) . . ? O11 Si8' O3 105.7(5) . . ? O10 Si8' C22 113.0(5) . . ? O11 Si8' C22 112.0(5) . . ? O3 Si8' C22 109.0(5) . . ? Si4' O1 Si1 149.4(5) . . ? Si4' O1 Si1' 149.0(4) . . ? Si1 O1 Si1' 9.5(6) . . ? Si4' O1 Si4 1.4(4) . . ? Si1 O1 Si4 149.5(5) . . ? Si1' O1 Si4 149.5(4) . . ? Si3' O2 Si4 146.2(5) . . ? Si3' O2 Si4' 141.8(5) . . ? Si4 O2 Si4' 8.2(5) . . ? Si3' O2 Si3 3.5(8) . . ? Si4 O2 Si3 149.7(6) . . ? Si4' O2 Si3 145.2(6) . . ? Si1' O3 Si8 146.8(4) . . ? Si1' O3 Si8' 146.8(4) . . ? Si8 O3 Si8' 0.5(6) . . ? Si1' O3 Si1 3.3(6) . . ? Si8 O3 Si1 143.6(4) . . ? Si8' O3 Si1 143.6(4) . . ? Si5 O4 Si3' 148.8(6) . . ? Si5 O4 Si3 152.9(7) . . ? Si3' O4 Si3 4.9(8) . . ? Si5 O4 Si5' 6.5(9) . . ? Si3' O4 Si5' 147.6(5) . . ? Si3 O4 Si5' 152.2(7) . . ? Si7' O5 Si2 146.1(3) . . ? Si7' O5 Si7 3.6(4) . . ? Si2 O5 Si7 143.9(3) . . ? Si5 O6 Si2 147.5(4) . . ? Si5 O6 Si5' 7.5(10) . . ? Si2 O6 Si5' 148.3(3) . . ? Si1 O7 Si7 151.4(5) . . ? Si1 O7 Si7' 152.8(5) . . ? Si7 O7 Si7' 6.5(4) . . ? Si1 O7 Si1' 9.0(5) . . ? Si7 O7 Si1' 150.6(4) . . ? Si7' O7 Si1' 149.9(4) . . ? Si4 O8 Si6 152.5(5) . . ? Si4 O8 Si4' 7.4(4) . . ? Si6 O8 Si4' 148.9(5) . . ? Si4 O8 Si6' 149.6(5) . . ? Si6 O8 Si6' 8.6(4) . . ? Si4' O8 Si6' 144.4(5) . . ? Si5' O9 Si6 150.4(5) . . ? Si5' O9 Si6' 145.7(4) . . ? Si6 O9 Si6' 8.8(5) . . ? Si5' O9 Si5 3.5(7) . . ? Si6 O9 Si5 147.0(5) . . ? Si6' O9 Si5 142.6(5) . . ? Si8' O10 Si2 154.1(4) . . ? Si8' O10 Si8 4.6(6) . . ? Si2 O10 Si8 151.6(3) . . ? Si3' O11 Si8' 149.0(5) . . ? Si3' O11 Si3 5.0(9) . . ? Si8' O11 Si3 153.3(6) . . ? Si3' O11 Si8 147.3(5) . . ? Si8' O11 Si8 4.9(6) . . ? Si3 O11 Si8 151.9(7) . . ? Si6' O12 Si7 149.4(4) . . ? Si6' O12 Si7' 148.2(4) . . ? Si7 O12 Si7' 3.9(5) . . ? Si6' O12 Si6 0.3(6) . . ? Si7 O12 Si6 149.1(4) . . ? Si7' O12 Si6 148.0(4) . . ? C2 C1 Si1 112.3(5) . . ? C1 C2 C3 111.9(5) . . ? C2' C1' Si1' 108.1(14) . . ? C1' C2' C3 101.5(13) . . ? F1 C3 F3 111.3(6) . . ? F1 C3 F2 102.6(6) . . ? F3 C3 F2 103.3(5) . . ? F1 C3 C2 120.0(6) . . ? F3 C3 C2 107.3(5) . . ? F2 C3 C2 111.0(6) . . ? F1 C3 C2' 85.3(8) . . ? F3 C3 C2' 136.7(10) . . ? F2 C3 C2' 111.9(9) . . ? C2 C3 C2' 36.7(7) . . ? C5 C4 Si2 114.0(3) . . ? C6 C5 C4 114.4(4) . . ? F4 C6 F5 108.0(5) . . ? F4 C6 F6 103.4(6) . . ? F5 C6 F6 108.0(6) . . ? F4 C6 C5 113.3(5) . . ? F5 C6 C5 112.8(5) . . ? F6 C6 C5 110.8(5) . . ? C8 C7 Si3 114.6(5) . . ? C8 C7 Si3' 113.3(5) . . ? Si3 C7 Si3' 1.8(5) . . ? C9 C8 C7 116.6(5) . . ? F9 C9 F7 104.6(6) . . ? F9 C9 F8 101.8(7) . . ? F7 C9 F8 108.5(6) . . ? F9 C9 C8 117.6(6) . . ? F7 C9 C8 112.8(5) . . ? F8 C9 C8 110.7(6) . . ? C11 C10 Si4 114.3(4) . . ? C11 C10 Si4' 109.7(4) . . ? Si4 C10 Si4' 6.6(4) . . ? C12 C11 C10 112.4(4) . . ? F11 C12 F10 113.5(9) . . ? F11 C12 F12 104.5(10) . . ? F10 C12 F12 100.5(6) . . ? F11 C12 C11 112.3(6) . . ? F10 C12 C11 114.6(9) . . ? F12 C12 C11 110.3(8) . . ? C17 C16 Si6 113.1(6) . . ? C17' C16' Si6' 115(2) . . ? C16 C17 C18 109.1(7) . . ? C16' C17' C18 109(2) . . ? F18 C18 F17 112.7(14) . . ? F18 C18 F16 108.7(13) . . ? F17 C18 F16 101.4(10) . . ? F18 C18 C17 105.6(8) . . ? F17 C18 C17 120.6(13) . . ? F16 C18 C17 107.3(13) . . ? F18 C18 C17' 126.2(17) . . ? F17 C18 C17' 88.4(17) . . ? F16 C18 C17' 114.9(14) . . ? C17 C18 C17' 32.4(14) . . ? C20 C19 Si7' 108.7(4) . . ? C20 C19 Si7 113.3(4) . . ? Si7' C19 Si7 5.7(4) . . ? C21 C20 C19 117.5(5) . . ? F20' C21 F19 58.0(6) . . ? F20' C21 F21' 102.4(15) . . ? F19 C21 F21' 55.5(6) . . ? F20' C21 F21 127.2(9) . . ? F19 C21 F21 107.1(7) . . ? F21' C21 F21 53.2(6) . . ? F20' C21 F20 51.6(6) . . ? F19 C21 F20 109.0(8) . . ? F21' C21 F20 133(2) . . ? F21 C21 F20 107.0(6) . . ? F20' C21 F19' 103.4(10) . . ? F19 C21 F19' 141.8(12) . . ? F21' C21 F19' 104.7(13) . . ? F21 C21 F19' 54.8(6) . . ? F20 C21 F19' 57.5(6) . . ? F20' C21 C20 118.8(9) . . ? F19 C21 C20 113.4(8) . . ? F21' C21 C20 121(2) . . ? F21 C21 C20 113.5(6) . . ? F20 C21 C20 106.6(8) . . ? F19' C21 C20 104.8(11) . . ? Si8' C22 Si8 4.1(5) . . ? C14 C13 Si5 121.8(9) . . ? C13 C14 C15 118.9(10) . . ? F15 C15 F13 105.5(10) . . ? F15 C15 F14 104.6(9) . . ? F13 C15 F14 105.5(10) . . ? F15 C15 C14 115.8(10) . . ? F13 C15 C14 112.3(10) . . ? F14 C15 C14 112.2(9) . . ? C14' C13' Si5' 123.6(15) . . ? C13' C14' C15' 111.7(16) . . ? F13' C15' F14' 109.5(12) . . ? F13' C15' F15' 107.9(12) . . ? F14' C15' F15' 106.5(12) . . ? F13' C15' C14' 101.6(15) . . ? F14' C15' C14' 119.6(14) . . ? F15' C15' C14' 111.2(18) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.35 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.413 _refine_diff_density_min -0.252 _refine_diff_density_rms 0.060 _chemical_compound_source 'Chemical synthesis via corner capping technique' _exptl_crystal_recrystallization_method 'Diffusion THF Solvent' _diffrn_ambient_pressure 100