# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2006 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'Peter Jutzi' _publ_contact_author_address ; Fakultatur Chemie Universitat Bielefeld Bielefeld 33615 GERMANY ; _publ_contact_author_email PETER.JUTZI@UNI-BIELEFELD.DE _publ_section_title ; Novel pi-Complexes of Divalent Silicon: Mixed Substituted Neutral Sandwich Compounds and the Half-Sandwich Cation (iPr5C5)Si+ ; # The loop structure below should contain the names and addresses of all # authors, in the required order of publication. Repeat as necessary. loop_ _publ_author_name _publ_author_address P.Jutzi ; Fakultat f. Chemie Universitat Bielefeld 33615 Bielefeld Germany ; A.Mix ; Fakultat f. Chemie Universitat Bielefeld 33615 Bielefeld Germany ; B.Neumann ; Fakultat f. Chemie Universitat Bielefeld 33615 Bielefeld Germany ; B.Rummel ; Fakultat f. Chemie Universitat Bielefeld 33615 Bielefeld Germany ; H.-G.Stammler ; Fakultat f. Chemie Universitat Bielefeld 33615 Bielefeld Germany ; #========================================================================= data_compound3 _database_code_depnum_ccdc_archive 'CCDC 603837' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C30 H50 Si, 0.5 C6 H14' _chemical_formula_sum 'C33 H57 Si' _chemical_formula_weight 481.88 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' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.8950(10) _cell_length_b 9.9430(8) _cell_length_c 18.0340(18) _cell_angle_alpha 105.747(5) _cell_angle_beta 93.344(4) _cell_angle_gamma 110.354(5) _cell_volume 1578.0(3) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 5097 _cell_measurement_theta_min 2.910 _cell_measurement_theta_max 25.028 _exptl_crystal_description fragment _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.014 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 538 _exptl_absorpt_coefficient_mu 0.092 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9730 _exptl_absorpt_correction_T_max 0.9945 _exptl_absorpt_process_details 'Denzo and Scalepack (Otwinowski & Minor, 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 22941 _diffrn_reflns_av_R_equivalents 0.106 _diffrn_reflns_av_sigmaI/netI 0.0842 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.93 _diffrn_reflns_theta_max 25.00 _reflns_number_total 5509 _reflns_number_gt 3365 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'KappaCCD ' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'Denzo and Scalepack (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL-PLUS (1990)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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. Disorder of i-propylcyclopentadienyl ligand on two positions (62:38), except the methyl-groups. Disorder of hexane on two positions (74:26). All disordered parts were refined isotropically. ; _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^)+(0.0629P)^2^+1.2587P] 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 5509 _refine_ls_number_parameters 279 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.1260 _refine_ls_R_factor_gt 0.0689 _refine_ls_wR_factor_ref 0.1738 _refine_ls_wR_factor_gt 0.1468 _refine_ls_goodness_of_fit_ref 1.022 _refine_ls_restrained_S_all 1.022 _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 0.70880(9) 0.07027(10) 0.80088(5) 0.0251(2) Uani 1 1 d . . . C1A C 0.9485(4) 0.2347(5) 0.7810(2) 0.0215(16) Uiso 0.621(5) 1 d PG A 1 C2A C 0.9062(5) 0.0961(5) 0.7196(3) 0.0233(16) Uiso 0.621(5) 1 d PG A 1 C3A C 0.7803(5) 0.0798(4) 0.6705(2) 0.0218(15) Uiso 0.621(5) 1 d PG A 1 C4A C 0.7447(4) 0.2082(6) 0.7016(3) 0.0209(16) Uiso 0.621(5) 1 d PG A 1 C5A C 0.8487(6) 0.3040(4) 0.7699(3) 0.0200(15) Uiso 0.621(5) 1 d PG A 1 C6A C 1.0832(5) 0.3035(6) 0.8456(3) 0.0270(12) Uiso 0.621(5) 1 d P A 1 H6AA H 1.0766 0.3988 0.8786 0.032 Uiso 0.621(5) 1 calc PR A 1 C9A C 0.9906(6) -0.0089(6) 0.7047(3) 0.0288(13) Uiso 0.621(5) 1 d P A 1 H9AA H 1.0736 0.0392 0.7497 0.035 Uiso 0.621(5) 1 calc PR A 1 C12A C 0.7039(5) -0.0491(6) 0.5951(3) 0.0268(12) Uiso 0.621(5) 1 d P A 1 H12A H 0.7603 -0.1163 0.5907 0.032 Uiso 0.621(5) 1 calc PR A 1 C15A C 0.6223(5) 0.2415(6) 0.6642(3) 0.0261(12) Uiso 0.621(5) 1 d P A 1 H15A H 0.5721 0.1509 0.6172 0.031 Uiso 0.621(5) 1 calc PR A 1 C18A C 0.8592(6) 0.4596(5) 0.8182(3) 0.0271(12) Uiso 0.621(5) 1 d P A 1 H18A H 0.7748 0.4732 0.7923 0.033 Uiso 0.621(5) 1 calc PR A 1 C1B C 0.9544(6) 0.2019(9) 0.7702(4) 0.021(3) Uiso 0.379(5) 1 d PG A 2 C2B C 0.8778(9) 0.0779(7) 0.7023(5) 0.021(3) Uiso 0.379(5) 1 d PG A 2 C3B C 0.7575(7) 0.1036(8) 0.6708(3) 0.023(3) Uiso 0.379(5) 1 d PG A 2 C4B C 0.7596(7) 0.2435(9) 0.7193(5) 0.021(3) Uiso 0.379(5) 1 d PG A 2 C5B C 0.8813(9) 0.3043(6) 0.7807(4) 0.027(3) Uiso 0.379(5) 1 d PG A 2 C6B C 1.0970(8) 0.2304(10) 0.8200(5) 0.027(2) Uiso 0.379(5) 1 d P A 2 H6BA H 1.1191 0.1402 0.7932 0.032 Uiso 0.379(5) 1 calc PR A 2 C9B C 0.9247(10) -0.0518(9) 0.6660(5) 0.027(2) Uiso 0.379(5) 1 d P A 2 H9BA H 0.8490 -0.1131 0.6181 0.032 Uiso 0.379(5) 1 calc PR A 2 C12B C 0.6508(9) 0.0033(9) 0.5947(5) 0.029(2) Uiso 0.379(5) 1 d P A 2 H12B H 0.5836 0.0572 0.5903 0.034 Uiso 0.379(5) 1 calc PR A 2 C15B C 0.6554(8) 0.3204(10) 0.7035(5) 0.0252(19) Uiso 0.379(5) 1 d P A 2 H15B H 0.6921 0.4175 0.7475 0.030 Uiso 0.379(5) 1 calc PR A 2 C18B C 0.9304(10) 0.4589(9) 0.8439(5) 0.029(2) Uiso 0.379(5) 1 d P A 2 H18B H 1.0185 0.4631 0.8760 0.035 Uiso 0.379(5) 1 calc PR A 2 C7 C 1.0849(4) 0.2166(4) 0.90071(19) 0.0390(8) Uani 1 1 d . . . H7A H 0.9905 0.1879 0.9188 0.058 Uiso 0.621(5) 1 calc PR A 1 H7B H 1.1631 0.2792 0.9456 0.058 Uiso 0.621(5) 1 calc PR A 1 H7C H 1.1020 0.1255 0.8741 0.058 Uiso 0.621(5) 1 calc PR A 1 H7D H 1.1817 0.2368 0.9281 0.058 Uiso 0.379(5) 1 calc PR A 2 H7E H 1.0186 0.1142 0.8966 0.058 Uiso 0.379(5) 1 calc PR A 2 H7F H 1.0463 0.2898 0.9299 0.058 Uiso 0.379(5) 1 calc PR A 2 C8 C 1.2252(3) 0.3567(4) 0.8131(2) 0.0376(8) Uani 1 1 d . . . H8A H 1.3088 0.4008 0.8558 0.056 Uiso 0.621(5) 1 calc PR A 1 H8B H 1.2242 0.4328 0.7883 0.056 Uiso 0.621(5) 1 calc PR A 1 H8C H 1.2336 0.2705 0.7743 0.056 Uiso 0.621(5) 1 calc PR A 1 H8D H 1.2216 0.3543 0.7583 0.056 Uiso 0.379(5) 1 calc PR A 2 H8E H 1.3153 0.3464 0.8312 0.056 Uiso 0.379(5) 1 calc PR A 2 H8F H 1.2235 0.4528 0.8451 0.056 Uiso 0.379(5) 1 calc PR A 2 C10 C 0.9156(4) -0.1620(4) 0.7097(2) 0.0407(9) Uani 1 1 d . . . H10A H 0.8715 -0.1556 0.7572 0.061 Uiso 0.621(5) 1 calc PR A 1 H10B H 0.9864 -0.2102 0.7115 0.061 Uiso 0.621(5) 1 calc PR A 1 H10C H 0.8390 -0.2221 0.6638 0.061 Uiso 0.621(5) 1 calc PR A 1 H10D H 0.8219 -0.1891 0.7286 0.061 Uiso 0.379(5) 1 calc PR A 2 H10E H 0.9960 -0.1163 0.7542 0.061 Uiso 0.379(5) 1 calc PR A 2 H10F H 0.9229 -0.2530 0.6748 0.061 Uiso 0.379(5) 1 calc PR A 2 C11 C 1.0662(3) -0.0021(4) 0.63322(19) 0.0344(8) Uani 1 1 d . . . H11A H 1.1196 -0.0701 0.6256 0.052 Uiso 0.621(5) 1 calc PR A 1 H11B H 1.1349 0.1014 0.6416 0.052 Uiso 0.621(5) 1 calc PR A 1 H11C H 0.9926 -0.0333 0.5867 0.052 Uiso 0.621(5) 1 calc PR A 1 H11D H 1.0908 -0.0901 0.6100 0.052 Uiso 0.379(5) 1 calc PR A 2 H11E H 1.1455 0.0716 0.6755 0.052 Uiso 0.379(5) 1 calc PR A 2 H11F H 1.0533 0.0440 0.5931 0.052 Uiso 0.379(5) 1 calc PR A 2 C13 C 0.5505(4) -0.1486(4) 0.5955(2) 0.0388(8) Uani 1 1 d . . . H13A H 0.5472 -0.1785 0.6431 0.058 Uiso 0.621(5) 1 calc PR A 1 H13B H 0.5182 -0.2390 0.5496 0.058 Uiso 0.621(5) 1 calc PR A 1 H13C H 0.4858 -0.0936 0.5941 0.058 Uiso 0.621(5) 1 calc PR A 1 H13D H 0.4869 -0.2035 0.5445 0.058 Uiso 0.379(5) 1 calc PR A 2 H13E H 0.4905 -0.1363 0.6363 0.058 Uiso 0.379(5) 1 calc PR A 2 H13F H 0.6084 -0.2057 0.6063 0.058 Uiso 0.379(5) 1 calc PR A 2 C14 C 0.7226(4) 0.0036(4) 0.52271(18) 0.0352(8) Uani 1 1 d . . . H14A H 0.6729 -0.0826 0.4757 0.053 Uiso 0.621(5) 1 calc PR A 1 H14B H 0.8270 0.0471 0.5202 0.053 Uiso 0.621(5) 1 calc PR A 1 H14C H 0.6801 0.0801 0.5260 0.053 Uiso 0.621(5) 1 calc PR A 1 H14D H 0.6496 -0.0611 0.4759 0.053 Uiso 0.379(5) 1 calc PR A 2 H14E H 0.8009 -0.0348 0.5257 0.053 Uiso 0.379(5) 1 calc PR A 2 H14F H 0.7638 0.1069 0.5201 0.053 Uiso 0.379(5) 1 calc PR A 2 C16 C 0.5035(3) 0.2510(4) 0.7113(2) 0.0365(8) Uani 1 1 d . . . H16A H 0.4695 0.1634 0.7303 0.055 Uiso 0.621(5) 1 calc PR A 1 H16B H 0.4217 0.2520 0.6784 0.055 Uiso 0.621(5) 1 calc PR A 1 H16C H 0.5420 0.3438 0.7559 0.055 Uiso 0.621(5) 1 calc PR A 1 H16D H 0.4991 0.2221 0.7592 0.055 Uiso 0.379(5) 1 calc PR A 2 H16E H 0.4534 0.1610 0.6661 0.055 Uiso 0.379(5) 1 calc PR A 2 H16F H 0.4557 0.3231 0.7140 0.055 Uiso 0.379(5) 1 calc PR A 2 C17 C 0.6825(4) 0.3727(4) 0.63087(19) 0.0354(8) Uani 1 1 d . . . H17A H 0.6011 0.3900 0.6069 0.053 Uiso 0.621(5) 1 calc PR A 1 H17B H 0.7413 0.3481 0.5913 0.053 Uiso 0.621(5) 1 calc PR A 1 H17C H 0.7437 0.4642 0.6731 0.053 Uiso 0.621(5) 1 calc PR A 1 H17D H 0.6151 0.4215 0.6221 0.053 Uiso 0.379(5) 1 calc PR A 2 H17E H 0.6662 0.2853 0.5851 0.053 Uiso 0.379(5) 1 calc PR A 2 H17F H 0.7835 0.4447 0.6392 0.053 Uiso 0.379(5) 1 calc PR A 2 C19 C 0.8330(4) 0.4761(4) 0.90126(19) 0.0384(8) Uani 1 1 d . . . H19A H 0.7451 0.3915 0.9018 0.058 Uiso 0.621(5) 1 calc PR A 1 H19B H 0.8194 0.5712 0.9233 0.058 Uiso 0.621(5) 1 calc PR A 1 H19C H 0.9174 0.4764 0.9327 0.058 Uiso 0.621(5) 1 calc PR A 1 H19D H 0.8752 0.5782 0.9387 0.058 Uiso 0.379(5) 1 calc PR A 2 H19E H 0.8216 0.4020 0.9292 0.058 Uiso 0.379(5) 1 calc PR A 2 H19F H 0.7371 0.4597 0.8741 0.058 Uiso 0.379(5) 1 calc PR A 2 C20 C 0.9925(4) 0.5857(3) 0.8102(2) 0.0383(8) Uani 1 1 d . . . H20A H 1.0021 0.5677 0.7549 0.057 Uiso 0.621(5) 1 calc PR A 1 H20B H 1.0802 0.5884 0.8398 0.057 Uiso 0.621(5) 1 calc PR A 1 H20C H 0.9812 0.6824 0.8307 0.057 Uiso 0.621(5) 1 calc PR A 1 H20D H 1.0230 0.6825 0.8518 0.057 Uiso 0.379(5) 1 calc PR A 2 H20E H 0.9178 0.5803 0.7701 0.057 Uiso 0.379(5) 1 calc PR A 2 H20F H 1.0771 0.5771 0.7867 0.057 Uiso 0.379(5) 1 calc PR A 2 C21 C 0.5545(4) -0.1636(3) 0.82619(19) 0.0335(8) Uani 1 1 d . A . C22 C 0.4666(3) -0.0786(4) 0.82547(19) 0.0337(8) Uani 1 1 d . A . C23 C 0.5271(3) 0.0552(4) 0.89060(19) 0.0316(8) Uani 1 1 d . A . C24 C 0.6513(3) 0.0499(3) 0.93127(18) 0.0298(7) Uani 1 1 d . A . C25 C 0.6692(3) -0.0842(4) 0.89090(19) 0.0323(8) Uani 1 1 d . A . C26 C 0.5261(5) -0.3188(4) 0.7702(2) 0.0613(12) Uani 1 1 d . . . H26A H 0.4992 -0.3935 0.7982 0.092 Uiso 1 1 calc R A . H26B H 0.6146 -0.3183 0.7484 0.092 Uiso 1 1 calc R . . H26C H 0.4460 -0.3449 0.7277 0.092 Uiso 1 1 calc R . . C27 C 0.3276(4) -0.1224(5) 0.7700(2) 0.0579(12) Uani 1 1 d . . . H27A H 0.3229 -0.2018 0.7226 0.087 Uiso 1 1 calc R A . H27B H 0.3262 -0.0341 0.7562 0.087 Uiso 1 1 calc R . . H27C H 0.2432 -0.1599 0.7951 0.087 Uiso 1 1 calc R . . C28 C 0.4616(4) 0.1720(4) 0.9173(2) 0.0511(10) Uani 1 1 d . . . H28A H 0.3972 0.1451 0.9547 0.077 Uiso 1 1 calc R A . H28B H 0.4050 0.1762 0.8722 0.077 Uiso 1 1 calc R . . H28C H 0.5399 0.2709 0.9426 0.077 Uiso 1 1 calc R . . C29 C 0.7426(4) 0.1643(4) 1.0072(2) 0.0471(9) Uani 1 1 d . . . H29A H 0.6869 0.1538 1.0499 0.071 Uiso 1 1 calc R A . H29B H 0.7678 0.2663 1.0034 0.071 Uiso 1 1 calc R . . H29C H 0.8324 0.1468 1.0177 0.071 Uiso 1 1 calc R . . C30 C 0.7808(4) -0.1414(5) 0.9152(2) 0.0540(11) Uani 1 1 d . . . H30A H 0.8533 -0.0623 0.9590 0.081 Uiso 1 1 calc R A . H30B H 0.8299 -0.1687 0.8711 0.081 Uiso 1 1 calc R . . H30C H 0.7323 -0.2304 0.9314 0.081 Uiso 1 1 calc R . . C31A C 0.2474(6) 0.4059(6) 0.5688(3) 0.0881(16) Uiso 0.740(9) 1 d PD B 1 H31A H 0.3241 0.4535 0.6152 0.132 Uiso 0.740(9) 1 calc PR B 1 H31B H 0.2923 0.3933 0.5217 0.132 Uiso 0.740(9) 1 calc PR B 1 H31C H 0.1819 0.3069 0.5701 0.132 Uiso 0.740(9) 1 calc PR B 1 C31B C 0.2474(6) 0.4059(6) 0.5688(3) 0.0881(16) Uiso 0.260(9) 1 d PD B 2 H31D H 0.2651 0.3120 0.5515 0.132 Uiso 0.260(9) 1 calc PR B 2 H31E H 0.2280 0.4229 0.6225 0.132 Uiso 0.260(9) 1 calc PR B 2 H31F H 0.3338 0.4905 0.5668 0.132 Uiso 0.260(9) 1 calc PR B 2 C32A C 0.1625(6) 0.5028(7) 0.5679(4) 0.067(2) Uiso 0.740(9) 1 d PD B 1 H32A H 0.2317 0.6033 0.5689 0.081 Uiso 0.740(9) 1 calc PR B 1 H32B H 0.1214 0.5168 0.6169 0.081 Uiso 0.740(9) 1 calc PR B 1 C32B C 0.1199(16) 0.3940(18) 0.5169(10) 0.066(6) Uiso 0.260(9) 1 d PD B 2 H32C H 0.0378 0.3012 0.5159 0.079 Uiso 0.260(9) 1 calc PR B 2 H32D H 0.1438 0.3780 0.4635 0.079 Uiso 0.260(9) 1 calc PR B 2 C33A C 0.0395(6) 0.4491(7) 0.5008(3) 0.0458(15) Uiso 0.740(9) 1 d PD . 1 H33A H 0.0795 0.4306 0.4516 0.055 Uiso 0.740(9) 1 calc PR B 1 H33B H -0.0324 0.3510 0.5013 0.055 Uiso 0.740(9) 1 calc PR B 1 C33B C 0.0633(18) 0.5199(19) 0.5330(11) 0.057(5) Uiso 0.260(9) 1 d PD . 2 H33C H 0.1427 0.6158 0.5353 0.068 Uiso 0.260(9) 1 calc PR B 2 H33D H 0.0286 0.5330 0.5838 0.068 Uiso 0.260(9) 1 calc PR B 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 Si1 0.0224(4) 0.0273(5) 0.0288(5) 0.0116(4) 0.0069(3) 0.0108(4) C7 0.0349(19) 0.054(2) 0.0323(19) 0.0126(17) 0.0035(15) 0.0226(17) C8 0.0255(18) 0.046(2) 0.038(2) 0.0128(16) 0.0035(15) 0.0102(15) C10 0.045(2) 0.044(2) 0.047(2) 0.0212(17) 0.0181(17) 0.0267(17) C11 0.0331(18) 0.0406(19) 0.036(2) 0.0117(16) 0.0136(15) 0.0207(16) C13 0.037(2) 0.0365(19) 0.0343(19) 0.0073(15) 0.0018(15) 0.0072(16) C14 0.0370(19) 0.042(2) 0.0278(18) 0.0097(15) 0.0045(15) 0.0169(16) C16 0.0312(18) 0.048(2) 0.042(2) 0.0203(17) 0.0094(15) 0.0232(16) C17 0.0379(19) 0.0396(19) 0.0355(19) 0.0166(16) 0.0051(15) 0.0191(16) C19 0.043(2) 0.0340(19) 0.038(2) 0.0079(16) 0.0062(16) 0.0176(16) C20 0.041(2) 0.0290(18) 0.039(2) 0.0115(15) 0.0026(16) 0.0062(16) C21 0.0392(19) 0.0269(17) 0.0344(19) 0.0141(15) 0.0167(16) 0.0074(15) C22 0.0234(17) 0.042(2) 0.038(2) 0.0211(16) 0.0104(14) 0.0064(15) C23 0.0297(18) 0.0386(19) 0.038(2) 0.0218(16) 0.0183(15) 0.0175(15) C24 0.0321(18) 0.0330(17) 0.0275(17) 0.0147(14) 0.0117(14) 0.0110(14) C25 0.0331(18) 0.0377(18) 0.039(2) 0.0241(16) 0.0173(16) 0.0185(15) C26 0.082(3) 0.032(2) 0.057(3) 0.0119(19) 0.031(2) 0.005(2) C27 0.026(2) 0.082(3) 0.056(3) 0.038(2) 0.0006(18) -0.0022(19) C28 0.052(2) 0.065(3) 0.070(3) 0.042(2) 0.038(2) 0.042(2) C29 0.051(2) 0.052(2) 0.031(2) 0.0156(17) 0.0094(17) 0.0080(19) C30 0.058(3) 0.077(3) 0.068(3) 0.054(2) 0.032(2) 0.047(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 Si1 C21 2.476(3) . ? Si1 C22 2.479(3) . ? Si1 C1A 2.479(5) . ? Si1 C23 2.481(3) . ? Si1 C25 2.481(3) . ? Si1 C5A 2.487(4) . ? Si1 C2A 2.494(5) . ? Si1 C24 2.496(3) . ? Si1 C5B 2.496(8) . ? Si1 C4B 2.499(7) . ? Si1 C1B 2.502(8) . ? Si1 C4A 2.507(4) . ? C1A C5A 1.4200 . ? C1A C2A 1.4200 . ? C1A C6A 1.534(5) . ? C2A C3A 1.4200 . ? C2A C9A 1.530(5) . ? C3A C4A 1.4200 . ? C3A C12A 1.524(5) . ? C4A C5A 1.4200 . ? C4A C15A 1.528(5) . ? C5A C18A 1.520(5) . ? C6A C7 1.486(6) . ? C6A C8 1.532(6) . ? C6A H6AA 1.0000 . ? C9A C10 1.474(6) . ? C9A C11 1.532(6) . ? C9A H9AA 1.0000 . ? C12A C13 1.498(6) . ? C12A C14 1.532(6) . ? C12A H12A 1.0000 . ? C15A C16 1.504(6) . ? C15A C17 1.532(5) . ? C15A H15A 1.0000 . ? C18A C19 1.510(6) . ? C18A C20 1.517(6) . ? C18A H18A 1.0000 . ? C1B C5B 1.4200 . ? C1B C2B 1.4200 . ? C1B C6B 1.522(9) . ? C2B C3B 1.4200 . ? C2B C9B 1.517(9) . ? C3B C4B 1.4200 . ? C3B C12B 1.532(9) . ? C4B C5B 1.4200 . ? C4B C15B 1.537(8) . ? C5B C18B 1.537(9) . ? C6B C8 1.483(8) . ? C6B C7 1.506(8) . ? C6B H6BA 1.0000 . ? C9B C10 1.497(8) . ? C9B C11 1.526(8) . ? C9B H9BA 1.0000 . ? C12B C13 1.496(8) . ? C12B C14 1.516(9) . ? C12B H12B 1.0000 . ? C15B C16 1.452(8) . ? C15B C17 1.540(8) . ? C15B H15B 1.0000 . ? C18B C19 1.471(9) . ? C18B C20 1.503(8) . ? C18B H18B 1.0000 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C7 H7D 0.9800 . ? C7 H7E 0.9800 . ? C7 H7F 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C8 H8D 0.9800 . ? C8 H8E 0.9800 . ? C8 H8F 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C10 H10D 0.9800 . ? C10 H10E 0.9800 . ? C10 H10F 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C11 H11D 0.9800 . ? C11 H11E 0.9800 . ? C11 H11F 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C13 H13D 0.9800 . ? C13 H13E 0.9800 . ? C13 H13F 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C14 H14D 0.9800 . ? C14 H14E 0.9800 . ? C14 H14F 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C16 H16D 0.9800 . ? C16 H16E 0.9800 . ? C16 H16F 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C17 H17D 0.9800 . ? C17 H17E 0.9800 . ? C17 H17F 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C19 H19D 0.9800 . ? C19 H19E 0.9800 . ? C19 H19F 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C20 H20D 0.9800 . ? C20 H20E 0.9800 . ? C20 H20F 0.9800 . ? C21 C22 1.410(4) . ? C21 C25 1.412(5) . ? C21 C26 1.516(5) . ? C22 C23 1.423(5) . ? C22 C27 1.506(5) . ? C23 C24 1.418(4) . ? C23 C28 1.502(4) . ? C24 C25 1.411(4) . ? C24 C29 1.510(5) . ? C25 C30 1.501(4) . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31A C32A 1.484(7) . ? C31A H31A 0.9800 . ? C31A H31B 0.9800 . ? C31A H31C 0.9800 . ? C32A C33A 1.502(7) . ? C32A H32A 0.9900 . ? C32A H32B 0.9900 . ? C32B C33B 1.508(14) . ? C32B H32C 0.9900 . ? C32B H32D 0.9900 . ? C33A C33A 1.483(10) 2_566 ? C33A H33A 0.9900 . ? C33A H33B 0.9900 . ? C33B C33B 1.54(3) 2_566 ? C33B H33C 0.9900 . ? C33B H33D 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 C21 Si1 C22 33.06(11) . . ? C21 Si1 C1A 150.10(14) . . ? C22 Si1 C1A 176.15(15) . . ? C21 Si1 C23 54.95(11) . . ? C22 Si1 C23 33.34(11) . . ? C1A Si1 C23 143.36(14) . . ? C21 Si1 C25 33.10(11) . . ? C22 Si1 C25 55.04(10) . . ? C1A Si1 C25 126.21(12) . . ? C23 Si1 C25 55.03(10) . . ? C21 Si1 C5A 176.08(15) . . ? C22 Si1 C5A 143.77(13) . . ? C1A Si1 C5A 33.23(5) . . ? C23 Si1 C5A 123.96(11) . . ? C25 Si1 C5A 150.35(14) . . ? C21 Si1 C2A 126.47(12) . . ? C22 Si1 C2A 150.27(15) . . ? C1A Si1 C2A 33.18(6) . . ? C23 Si1 C2A 175.64(15) . . ? C25 Si1 C2A 123.37(11) . . ? C5A Si1 C2A 54.94(7) . . ? C21 Si1 C24 54.62(11) . . ? C22 Si1 C24 54.90(11) . . ? C1A Si1 C24 123.68(12) . . ? C23 Si1 C24 33.11(10) . . ? C25 Si1 C24 32.94(10) . . ? C5A Si1 C24 127.02(12) . . ? C2A Si1 C24 143.18(13) . . ? C21 Si1 C5B 175.5(2) . . ? C22 Si1 C5B 150.8(2) . . ? C1A Si1 C5B 25.89(18) . . ? C23 Si1 C5B 126.66(17) . . ? C25 Si1 C5B 143.1(2) . . ? C5A Si1 C5B 8.43(18) . . ? C2A Si1 C5B 51.55(17) . . ? C24 Si1 C5B 123.83(16) . . ? C21 Si1 C4B 150.9(2) . . ? C22 Si1 C4B 127.02(16) . . ? C1A Si1 C4B 51.42(16) . . ? C23 Si1 C4B 123.89(15) . . ? C25 Si1 C4B 175.5(2) . . ? C5A Si1 C4B 25.49(18) . . ? C2A Si1 C4B 57.33(16) . . ? C24 Si1 C4B 143.5(2) . . ? C5B Si1 C4B 33.04(9) . . ? C21 Si1 C1B 143.34(19) . . ? C22 Si1 C1B 175.6(2) . . ? C1A Si1 C1B 8.20(19) . . ? C23 Si1 C1B 150.4(2) . . ? C25 Si1 C1B 123.59(15) . . ? C5A Si1 C1B 39.65(17) . . ? C2A Si1 C1B 25.81(18) . . ? C24 Si1 C1B 126.75(16) . . ? C5B Si1 C1B 33.01(9) . . ? C4B Si1 C1B 54.70(11) . . ? C21 Si1 C4A 143.69(14) . . ? C22 Si1 C4A 124.21(11) . . ? C1A Si1 C4A 54.88(7) . . ? C23 Si1 C4A 127.22(12) . . ? C25 Si1 C4A 175.66(15) . . ? C5A Si1 C4A 33.04(5) . . ? C2A Si1 C4A 54.71(7) . . ? C24 Si1 C4A 151.08(14) . . ? C5B Si1 C4A 39.90(17) . . ? C4B Si1 C4A 8.71(18) . . ? C1B Si1 C4A 56.78(16) . . ? C5A C1A C2A 108.0 . . ? C5A C1A C6A 125.4(4) . . ? C2A C1A C6A 126.5(4) . . ? C5A C1A Si1 73.70(17) . . ? C2A C1A Si1 73.97(17) . . ? C6A C1A Si1 121.0(3) . . ? C3A C2A C1A 108.0 . . ? C3A C2A C9A 126.0(4) . . ? C1A C2A C9A 125.7(4) . . ? C3A C2A Si1 74.17(17) . . ? C1A C2A Si1 72.85(17) . . ? C9A C2A Si1 123.4(3) . . ? C2A C3A C4A 108.0 . . ? C2A C3A C12A 125.3(4) . . ? C4A C3A C12A 126.6(4) . . ? C2A C3A Si1 72.86(17) . . ? C4A C3A Si1 73.41(17) . . ? C12A C3A Si1 122.4(3) . . ? C5A C4A C3A 108.0 . . ? C5A C4A C15A 126.4(4) . . ? C3A C4A C15A 125.5(4) . . ? C5A C4A Si1 72.73(17) . . ? C3A C4A Si1 73.71(17) . . ? C15A C4A Si1 122.6(3) . . ? C4A C5A C1A 108.0 . . ? C4A C5A C18A 125.8(4) . . ? C1A C5A C18A 126.0(4) . . ? C4A C5A Si1 74.23(17) . . ? C1A C5A Si1 73.07(17) . . ? C18A C5A Si1 122.7(3) . . ? C7 C6A C8 114.9(4) . . ? C7 C6A C1A 115.9(4) . . ? C8 C6A C1A 111.6(4) . . ? C7 C6A H6AA 104.3 . . ? C8 C6A H6AA 104.3 . . ? C1A C6A H6AA 104.3 . . ? C10 C9A C2A 116.8(4) . . ? C10 C9A C11 115.0(4) . . ? C2A C9A C11 111.7(4) . . ? C10 C9A H9AA 103.8 . . ? C2A C9A H9AA 103.8 . . ? C11 C9A H9AA 103.8 . . ? C13 C12A C3A 115.6(4) . . ? C13 C12A C14 114.1(4) . . ? C3A C12A C14 112.2(4) . . ? C13 C12A H12A 104.5 . . ? C3A C12A H12A 104.5 . . ? C14 C12A H12A 104.5 . . ? C16 C15A C4A 116.1(4) . . ? C16 C15A C17 113.8(4) . . ? C4A C15A C17 111.8(4) . . ? C16 C15A H15A 104.5 . . ? C4A C15A H15A 104.5 . . ? C17 C15A H15A 104.5 . . ? C19 C18A C20 114.1(4) . . ? C19 C18A C5A 115.9(4) . . ? C20 C18A C5A 112.8(4) . . ? C19 C18A H18A 104.1 . . ? C20 C18A H18A 104.1 . . ? C5A C18A H18A 104.1 . . ? C5B C1B C2B 108.0 . . ? C5B C1B C6B 124.7(7) . . ? C2B C1B C6B 127.1(7) . . ? C5B C1B Si1 73.2(3) . . ? C2B C1B Si1 73.8(3) . . ? C6B C1B Si1 122.8(5) . . ? C3B C2B C1B 108.0 . . ? C3B C2B C9B 126.1(7) . . ? C1B C2B C9B 125.7(7) . . ? C3B C2B Si1 73.5(3) . . ? C1B C2B Si1 73.3(3) . . ? C9B C2B Si1 123.2(5) . . ? C2B C3B C4B 108.0 . . ? C2B C3B C12B 125.8(7) . . ? C4B C3B C12B 126.1(7) . . ? C2B C3B Si1 73.6(3) . . ? C4B C3B Si1 73.2(3) . . ? C12B C3B Si1 122.3(5) . . ? C5B C4B C3B 108.0 . . ? C5B C4B C15B 126.4(7) . . ? C3B C4B C15B 125.4(7) . . ? C5B C4B Si1 73.4(3) . . ? C3B C4B Si1 73.8(3) . . ? C15B C4B Si1 122.4(5) . . ? C1B C5B C4B 108.0 . . ? C1B C5B C18B 126.3(7) . . ? C4B C5B C18B 125.6(7) . . ? C1B C5B Si1 73.7(3) . . ? C4B C5B Si1 73.6(3) . . ? C18B C5B Si1 121.7(5) . . ? C8 C6B C7 116.7(6) . . ? C8 C6B C1B 114.6(6) . . ? C7 C6B C1B 115.5(6) . . ? C8 C6B H6BA 102.3 . . ? C7 C6B H6BA 102.3 . . ? C1B C6B H6BA 102.3 . . ? C10 C9B C2B 117.5(6) . . ? C10 C9B C11 114.1(5) . . ? C2B C9B C11 112.9(6) . . ? C10 C9B H9BA 103.3 . . ? C2B C9B H9BA 103.3 . . ? C11 C9B H9BA 103.3 . . ? C13 C12B C14 115.1(6) . . ? C13 C12B C3B 115.8(6) . . ? C14 C12B C3B 112.9(6) . . ? C13 C12B H12B 103.7 . . ? C14 C12B H12B 103.7 . . ? C3B C12B H12B 103.7 . . ? C16 C15B C4B 117.6(6) . . ? C16 C15B C17 116.4(5) . . ? C4B C15B C17 110.9(6) . . ? C16 C15B H15B 103.1 . . ? C4B C15B H15B 103.1 . . ? C17 C15B H15B 103.1 . . ? C19 C18B C20 117.4(6) . . ? C19 C18B C5B 116.5(6) . . ? C20 C18B C5B 111.4(6) . . ? C19 C18B H18B 103.0 . . ? C20 C18B H18B 103.0 . . ? C5B C18B H18B 103.0 . . ? C6A C7 C6B 31.3(3) . . ? C6A C7 H7A 109.5 . . ? C6B C7 H7A 121.8 . . ? C6A C7 H7B 109.5 . . ? C6B C7 H7B 122.2 . . ? H7A C7 H7B 109.5 . . ? C6A C7 H7C 109.5 . . ? C6B C7 H7C 78.1 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C6A C7 H7D 115.5 . . ? C6B C7 H7D 109.5 . . ? H7A C7 H7D 128.7 . . ? H7B C7 H7D 32.4 . . ? H7C C7 H7D 77.8 . . ? C6A C7 H7E 128.2 . . ? C6B C7 H7E 109.5 . . ? H7A C7 H7E 53.1 . . ? H7B C7 H7E 122.3 . . ? H7C C7 H7E 56.4 . . ? H7D C7 H7E 109.5 . . ? C6A C7 H7F 78.8 . . ? C6B C7 H7F 109.5 . . ? H7A C7 H7F 56.5 . . ? H7B C7 H7F 77.0 . . ? H7C C7 H7F 165.9 . . ? H7D C7 H7F 109.5 . . ? H7E C7 H7F 109.5 . . ? C6B C8 C6A 31.0(3) . . ? C6B C8 H8A 116.6 . . ? C6A C8 H8A 109.5 . . ? C6B C8 H8B 127.0 . . ? C6A C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C6B C8 H8C 78.9 . . ? C6A C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C6B C8 H8D 109.5 . . ? C6A C8 H8D 120.1 . . ? H8A C8 H8D 130.0 . . ? H8B C8 H8D 48.9 . . ? H8C C8 H8D 60.9 . . ? C6B C8 H8E 109.5 . . ? C6A C8 H8E 123.7 . . ? H8A C8 H8E 37.2 . . ? H8B C8 H8E 123.1 . . ? H8C C8 H8E 72.3 . . ? H8D C8 H8E 109.5 . . ? C6B C8 H8F 109.5 . . ? C6A C8 H8F 78.5 . . ? H8A C8 H8F 73.0 . . ? H8B C8 H8F 60.6 . . ? H8C C8 H8F 169.5 . . ? H8D C8 H8F 109.5 . . ? H8E C8 H8F 109.5 . . ? C9A C10 C9B 32.3(3) . . ? C9A C10 H10A 109.5 . . ? C9B C10 H10A 120.5 . . ? C9A C10 H10B 109.5 . . ? C9B C10 H10B 124.0 . . ? H10A C10 H10B 109.5 . . ? C9A C10 H10C 109.5 . . ? C9B C10 H10C 77.2 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C9A C10 H10D 120.6 . . ? C9B C10 H10D 109.5 . . ? H10A C10 H10D 36.7 . . ? H10B C10 H10D 125.9 . . ? H10C C10 H10D 72.9 . . ? C9A C10 H10E 77.2 . . ? C9B C10 H10E 109.5 . . ? H10A C10 H10E 72.9 . . ? H10B C10 H10E 61.9 . . ? H10C C10 H10E 171.0 . . ? H10D C10 H10E 109.5 . . ? C9A C10 H10F 123.9 . . ? C9B C10 H10F 109.5 . . ? H10A C10 H10F 126.0 . . ? H10B C10 H10F 47.6 . . ? H10C C10 H10F 61.9 . . ? H10D C10 H10F 109.5 . . ? H10E C10 H10F 109.5 . . ? C9B C11 C9A 31.4(3) . . ? C9B C11 H11A 116.4 . . ? C9A C11 H11A 109.5 . . ? C9B C11 H11B 127.4 . . ? C9A C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C9B C11 H11C 78.6 . . ? C9A C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C9B C11 H11D 109.5 . . ? C9A C11 H11D 114.5 . . ? H11A C11 H11D 20.4 . . ? H11B C11 H11D 122.2 . . ? H11C C11 H11D 89.4 . . ? C9B C11 H11E 109.5 . . ? C9A C11 H11E 79.0 . . ? H11A C11 H11E 89.1 . . ? H11B C11 H11E 45.9 . . ? H11C C11 H11E 154.4 . . ? H11D C11 H11E 109.5 . . ? C9B C11 H11F 109.5 . . ? C9A C11 H11F 129.1 . . ? H11A C11 H11F 120.5 . . ? H11B C11 H11F 63.6 . . ? H11C C11 H11F 46.1 . . ? H11D C11 H11F 109.5 . . ? H11E C11 H11F 109.5 . . ? C12B C13 C12A 33.4(3) . . ? C12B C13 H13A 122.0 . . ? C12A C13 H13A 109.5 . . ? C12B C13 H13B 123.1 . . ? C12A C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12B C13 H13C 76.1 . . ? C12A C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C12B C13 H13D 109.5 . . ? C12A C13 H13D 116.6 . . ? H13A C13 H13D 128.3 . . ? H13B C13 H13D 33.5 . . ? H13C C13 H13D 76.5 . . ? C12B C13 H13E 109.5 . . ? C12A C13 H13E 128.2 . . ? H13A C13 H13E 50.1 . . ? H13B C13 H13E 122.0 . . ? H13C C13 H13E 59.5 . . ? H13D C13 H13E 109.5 . . ? C12B C13 H13F 109.5 . . ? C12A C13 H13F 76.6 . . ? H13A C13 H13F 59.5 . . ? H13B C13 H13F 76.0 . . ? H13C C13 H13F 169.0 . . ? H13D C13 H13F 109.5 . . ? H13E C13 H13F 109.5 . . ? C12B C14 C12A 32.8(3) . . ? C12B C14 H14A 116.3 . . ? C12A C14 H14A 109.5 . . ? C12B C14 H14B 128.2 . . ? C12A C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C12B C14 H14C 77.3 . . ? C12A C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C12B C14 H14D 109.5 . . ? C12A C14 H14D 115.7 . . ? H14A C14 H14D 21.5 . . ? H14B C14 H14D 121.8 . . ? H14C C14 H14D 88.2 . . ? C12B C14 H14E 109.5 . . ? C12A C14 H14E 77.4 . . ? H14A C14 H14E 88.2 . . ? H14B C14 H14E 48.2 . . ? H14C C14 H14E 156.5 . . ? H14D C14 H14E 109.5 . . ? C12B C14 H14F 109.5 . . ? C12A C14 H14F 128.7 . . ? H14A C14 H14F 121.3 . . ? H14B C14 H14F 61.4 . . ? H14C C14 H14F 48.2 . . ? H14D C14 H14F 109.5 . . ? H14E C14 H14F 109.5 . . ? C15B C16 C15A 33.3(3) . . ? C15B C16 H16A 121.8 . . ? C15A C16 H16A 109.5 . . ? C15B C16 H16B 123.2 . . ? C15A C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15B C16 H16C 76.2 . . ? C15A C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C15B C16 H16D 109.5 . . ? C15A C16 H16D 120.5 . . ? H16A C16 H16D 37.4 . . ? H16B C16 H16D 126.4 . . ? H16C C16 H16D 72.2 . . ? C15B C16 H16E 109.5 . . ? C15A C16 H16E 76.3 . . ? H16A C16 H16E 72.1 . . ? H16B C16 H16E 63.5 . . ? H16C C16 H16E 172.5 . . ? H16D C16 H16E 109.5 . . ? C15B C16 H16F 109.5 . . ? C15A C16 H16F 124.5 . . ? H16A C16 H16F 125.1 . . ? H16B C16 H16F 46.0 . . ? H16C C16 H16F 63.5 . . ? H16D C16 H16F 109.5 . . ? H16E C16 H16F 109.5 . . ? C15A C17 C15B 32.0(3) . . ? C15A C17 H17A 109.5 . . ? C15B C17 H17A 114.9 . . ? C15A C17 H17B 109.5 . . ? C15B C17 H17B 129.0 . . ? H17A C17 H17B 109.5 . . ? C15A C17 H17C 109.5 . . ? C15B C17 H17C 78.3 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C15A C17 H17D 115.7 . . ? C15B C17 H17D 109.5 . . ? H17A C17 H17D 19.6 . . ? H17B C17 H17D 120.5 . . ? H17C C17 H17D 90.1 . . ? C15A C17 H17E 78.1 . . ? C15B C17 H17E 109.5 . . ? H17A C17 H17E 90.2 . . ? H17B C17 H17E 45.9 . . ? H17C C17 H17E 153.9 . . ? H17D C17 H17E 109.5 . . ? C15A C17 H17F 128.3 . . ? C15B C17 H17F 109.5 . . ? H17A C17 H17F 121.2 . . ? H17B C17 H17F 63.8 . . ? H17C C17 H17F 45.8 . . ? H17D C17 H17F 109.5 . . ? H17E C17 H17F 109.5 . . ? C18B C19 C18A 32.0(3) . . ? C18B C19 H19A 121.9 . . ? C18A C19 H19A 109.5 . . ? C18B C19 H19B 122.5 . . ? C18A C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C18B C19 H19C 77.4 . . ? C18A C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C18B C19 H19D 109.5 . . ? C18A C19 H19D 116.8 . . ? H19A C19 H19D 128.4 . . ? H19B C19 H19D 34.2 . . ? H19C C19 H19D 75.8 . . ? C18B C19 H19E 109.5 . . ? C18A C19 H19E 127.3 . . ? H19A C19 H19E 50.6 . . ? H19B C19 H19E 123.0 . . ? H19C C19 H19E 58.9 . . ? H19D C19 H19E 109.5 . . ? C18B C19 H19F 109.5 . . ? C18A C19 H19F 77.9 . . ? H19A C19 H19F 59.0 . . ? H19B C19 H19F 75.2 . . ? H19C C19 H19F 168.3 . . ? H19D C19 H19F 109.5 . . ? H19E C19 H19F 109.5 . . ? C18B C20 C18A 31.7(3) . . ? C18B C20 H20A 122.3 . . ? C18A C20 H20A 109.5 . . ? C18B C20 H20B 77.8 . . ? C18A C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C18B C20 H20C 121.9 . . ? C18A C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C18B C20 H20D 109.5 . . ? C18A C20 H20D 116.0 . . ? H20A C20 H20D 128.2 . . ? H20B C20 H20D 77.8 . . ? H20C C20 H20D 32.3 . . ? C18B C20 H20E 109.5 . . ? C18A C20 H20E 78.4 . . ? H20A C20 H20E 56.8 . . ? H20B C20 H20E 166.2 . . ? H20C C20 H20E 77.1 . . ? H20D C20 H20E 109.5 . . ? C18B C20 H20F 109.5 . . ? C18A C20 H20F 127.9 . . ? H20A C20 H20F 52.8 . . ? H20B C20 H20F 56.7 . . ? H20C C20 H20F 122.6 . . ? H20D C20 H20F 109.5 . . ? H20E C20 H20F 109.5 . . ? C22 C21 C25 108.6(3) . . ? C22 C21 C26 126.0(3) . . ? C25 C21 C26 125.4(3) . . ? C22 C21 Si1 73.57(17) . . ? C25 C21 Si1 73.63(17) . . ? C26 C21 Si1 121.8(2) . . ? C21 C22 C23 107.7(3) . . ? C21 C22 C27 127.4(3) . . ? C23 C22 C27 124.8(3) . . ? C21 C22 Si1 73.37(18) . . ? C23 C22 Si1 73.41(17) . . ? C27 C22 Si1 121.9(2) . . ? C24 C23 C22 107.7(3) . . ? C24 C23 C28 125.7(3) . . ? C22 C23 C28 126.3(3) . . ? C24 C23 Si1 74.01(17) . . ? C22 C23 Si1 73.25(18) . . ? C28 C23 Si1 124.0(2) . . ? C25 C24 C23 108.3(3) . . ? C25 C24 C29 126.2(3) . . ? C23 C24 C29 125.5(3) . . ? C25 C24 Si1 72.97(17) . . ? C23 C24 Si1 72.88(17) . . ? C29 C24 Si1 122.7(2) . . ? C24 C25 C21 107.8(3) . . ? C24 C25 C30 126.9(3) . . ? C21 C25 C30 125.1(3) . . ? C24 C25 Si1 74.09(17) . . ? C21 C25 Si1 73.26(17) . . ? C30 C25 Si1 122.6(2) . . ? C21 C26 H26A 109.5 . . ? C21 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C21 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C22 C27 H27A 109.5 . . ? C22 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C22 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C23 C28 H28A 109.5 . . ? C23 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C23 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C24 C29 H29A 109.5 . . ? C24 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C24 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C25 C30 H30A 109.5 . . ? C25 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C25 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C32A C31A H31A 109.5 . . ? C32A C31A H31B 109.5 . . ? H31A C31A H31B 109.5 . . ? C32A C31A H31C 109.5 . . ? H31A C31A H31C 109.5 . . ? H31B C31A H31C 109.5 . . ? C31A C32A C33A 117.6(5) . . ? C31A C32A H32A 107.9 . . ? C33A C32A H32A 107.9 . . ? C31A C32A H32B 107.9 . . ? C33A C32A H32B 107.9 . . ? H32A C32A H32B 107.2 . . ? C33B C32B H32C 107.2 . . ? C33B C32B H32D 107.2 . . ? H32C C32B H32D 106.8 . . ? C33A C33A C32A 116.7(7) 2_566 . ? C33A C33A H33A 108.1 2_566 . ? C32A C33A H33A 108.1 . . ? C33A C33A H33B 108.1 2_566 . ? C32A C33A H33B 108.1 . . ? H33A C33A H33B 107.3 . . ? C32B C33B C33B 108.8(18) . 2_566 ? C32B C33B H33C 109.9 . . ? C33B C33B H33C 109.9 2_566 . ? C32B C33B H33D 109.9 . . ? C33B C33B H33D 109.9 2_566 . ? H33C C33B H33D 108.3 . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 0.287 _refine_diff_density_min -0.313 _refine_diff_density_rms 0.051 # Attachment 'B607236D BRI09.CIF' data_compound8 _database_code_depnum_ccdc_archive 'CCDC 611465' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C20 H35 Si, C16 Al F36 O4' _chemical_formula_sum 'C36 H35 Al F36 O4 Si' _chemical_formula_weight 1270.71 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' Al Al 0.0645 0.0514 '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' O O 0.0106 0.0060 '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' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.2390(14) _cell_length_b 15.481(5) _cell_length_c 15.9790(17) _cell_angle_alpha 92.105(18) _cell_angle_beta 90.523(11) _cell_angle_gamma 102.87(2) _cell_volume 2467.1(9) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 22 _cell_measurement_theta_min 5.87 _cell_measurement_theta_max 18.25 _exptl_crystal_description fragment _exptl_crystal_colour colourless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.711 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1268 _exptl_absorpt_coefficient_mu 0.240 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.9315 _exptl_absorpt_correction_T_max 0.9764 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10994 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.1926 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.18 _diffrn_reflns_theta_max 27.50 _reflns_number_total 10994 _reflns_number_gt 4746 _reflns_threshold_expression >2sigma(I) _computing_data_collection KappaCCD _computing_cell_refinement 'Dirax/lsq (Duisenberg & Schreurs, 1989-2000)' _computing_data_reduction 'EVALCCD (Duisenberg,1998,Thesis.Utrecht University.' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL-PLUS (1990)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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. ; _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^)+(0.1120P)^2^+6.6639P] 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 10994 _refine_ls_number_parameters 814 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.2204 _refine_ls_R_factor_gt 0.1006 _refine_ls_wR_factor_ref 0.2790 _refine_ls_wR_factor_gt 0.2243 _refine_ls_goodness_of_fit_ref 1.011 _refine_ls_restrained_S_all 1.014 _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 Al1 Al 0.01627(18) 0.31323(12) 0.25216(11) 0.0220(4) Uani 1 1 d . . . Si1 Si -0.23656(18) 0.26001(12) -0.23269(12) 0.0329(5) Uani 1 1 d . I . O1 O 0.1035(4) 0.3051(3) 0.3442(2) 0.0274(10) Uani 1 1 d . . . O2 O -0.0504(4) 0.4063(3) 0.2481(2) 0.0253(9) Uani 1 1 d . . . O3 O 0.1269(4) 0.3168(3) 0.1697(2) 0.0291(10) Uani 1 1 d . . . O4 O -0.1179(4) 0.2210(3) 0.2458(3) 0.0313(10) Uani 1 1 d . . . F1 F 0.0861(4) 0.3147(3) 0.5092(2) 0.0490(11) Uani 1 1 d . . . F2 F 0.2999(4) 0.3378(3) 0.5322(2) 0.0585(13) Uani 1 1 d . . . F3 F 0.1898(4) 0.2106(3) 0.4801(2) 0.0498(11) Uani 1 1 d . . . F4 F 0.3969(4) 0.4624(3) 0.4156(3) 0.0607(13) Uani 1 1 d . . . F5 F 0.1937(5) 0.4723(3) 0.4424(2) 0.0516(11) Uani 1 1 d . . . F6 F 0.2577(4) 0.4666(3) 0.3144(2) 0.0451(11) Uani 1 1 d . . . F7 F 0.2793(4) 0.2051(3) 0.3191(3) 0.0524(11) Uani 1 1 d . . . F8 F 0.4342(4) 0.2883(3) 0.3985(3) 0.0593(13) Uani 1 1 d . . . F9 F 0.3821(4) 0.3336(3) 0.2783(2) 0.0472(11) Uani 1 1 d . . . F10A F -0.2937(10) 0.3443(5) 0.1768(6) 0.039(4) Uani 0.54(2) 1 d P . . F10B F -0.3422(10) 0.3303(8) 0.2413(14) 0.079(7) Uani 0.46(2) 1 d P . . F11A F -0.2273(9) 0.4817(9) 0.1388(5) 0.046(4) Uani 0.54(2) 1 d P . . F11B F -0.2463(13) 0.4070(15) 0.1368(9) 0.085(9) Uani 0.46(2) 1 d P . . F12 F -0.3738(4) 0.4553(3) 0.2311(3) 0.0507(11) Uani 1 1 d . . . F13A F -0.1204(10) 0.4028(10) 0.4105(6) 0.041(3) Uani 0.532(19) 1 d P . . F13B F -0.0850(14) 0.4688(15) 0.4191(7) 0.071(5) Uani 0.468(19) 1 d P . . F14A F -0.2975(10) 0.3309(5) 0.3439(5) 0.035(3) Uani 0.532(19) 1 d P . . F14B F -0.1878(19) 0.3395(9) 0.3809(9) 0.082(8) Uani 0.468(19) 1 d P . . F15 F -0.2918(4) 0.4563(3) 0.3930(3) 0.0583(12) Uani 1 1 d . . . F16A F 0.0277(14) 0.5730(9) 0.296(2) 0.074(10) Uani 0.43(4) 1 d P . . F16B F -0.0135(19) 0.5680(8) 0.3519(13) 0.069(5) Uani 0.57(4) 1 d P . . F17A F -0.102(3) 0.5693(9) 0.1862(10) 0.068(8) Uani 0.43(4) 1 d P . . F17B F -0.0161(17) 0.5758(5) 0.2157(10) 0.061(5) Uani 0.57(4) 1 d P . . F18 F -0.1809(5) 0.5957(3) 0.2978(3) 0.0640(13) Uani 1 1 d . . . F19 F 0.2655(5) 0.4728(3) 0.0175(3) 0.0653(14) Uani 1 1 d . . . F20 F 0.3772(4) 0.4346(3) 0.1223(3) 0.0589(13) Uani 1 1 d . . . F21 F 0.2060(4) 0.4931(3) 0.1448(2) 0.0484(11) Uani 1 1 d . . . F22 F 0.2970(5) 0.3056(4) -0.0208(3) 0.0681(14) Uani 1 1 d . . . F23 F 0.1438(5) 0.1978(3) 0.0286(3) 0.0563(12) Uani 1 1 d . . . F24 F 0.3236(4) 0.2562(3) 0.1019(2) 0.0512(11) Uani 1 1 d . . . F25 F -0.0117(5) 0.4194(3) 0.0529(2) 0.0529(12) Uani 1 1 d . . . F26 F -0.0687(4) 0.2759(3) 0.0554(2) 0.0510(11) Uani 1 1 d . . . F27 F 0.0521(5) 0.3385(3) -0.0460(2) 0.0623(14) Uani 1 1 d . . . F28 F -0.1577(5) 0.1719(3) 0.4049(3) 0.0678(14) Uani 1 1 d . . . F29 F -0.2165(5) 0.0307(3) 0.3708(4) 0.0830(18) Uani 1 1 d . . . F30 F -0.0116(5) 0.1018(3) 0.3595(4) 0.0840(18) Uani 1 1 d . . . F31 F -0.3824(4) 0.1427(3) 0.3076(3) 0.0573(12) Uani 1 1 d . . . F32 F -0.3746(4) 0.0234(3) 0.2356(3) 0.0557(12) Uani 1 1 d . . . F33 F -0.3531(5) 0.1480(3) 0.1739(3) 0.0640(14) Uani 1 1 d . . . F34A F 0.0401(7) 0.1085(5) 0.2097(7) 0.031(3) Uiso 0.51(2) 1 d PD . . F34B F 0.0166(10) 0.1088(6) 0.1705(9) 0.053(3) Uiso 0.49(2) 1 d PD . . F35 F -0.1509(6) 0.0770(4) 0.1195(4) 0.088(2) Uani 1 1 d . . . F36A F -0.1398(11) -0.0110(6) 0.1959(9) 0.055(3) Uiso 0.51(2) 1 d PD . . F36B F -0.1100(9) -0.0072(5) 0.2328(7) 0.036(3) Uiso 0.49(2) 1 d PD . . C1 C -0.4459(7) 0.2066(4) -0.2457(5) 0.0402(18) Uani 1 1 d . . . C2 C -0.3940(8) 0.1702(5) -0.1750(4) 0.0405(18) Uani 1 1 d . I . C3 C -0.2992(8) 0.1222(5) -0.2039(4) 0.0410(19) Uani 1 1 d . . . C4 C -0.2888(7) 0.1298(5) -0.2917(5) 0.0396(18) Uani 1 1 d . I . C5 C -0.3809(8) 0.1810(5) -0.3181(4) 0.0388(18) Uani 1 1 d . I . C7 C -0.6918(7) 0.2116(4) -0.2541(4) 0.0379(17) Uani 1 1 d . . . H7A H -0.7133 0.1494 -0.2387 0.057 Uiso 0.50 1 calc PR A 1 H7B H -0.6860 0.2147 -0.3152 0.057 Uiso 0.50 1 calc PR A 1 H7C H -0.7621 0.2407 -0.2343 0.057 Uiso 0.50 1 calc PR A 1 H7D H -0.7276 0.2538 -0.2867 0.057 Uiso 0.50 1 calc PR A 1 H7E H -0.7550 0.1885 -0.2103 0.057 Uiso 0.50 1 calc PR A 1 H7F H -0.6788 0.1625 -0.2912 0.057 Uiso 0.50 1 calc PR A 1 C8 C -0.5140(7) 0.3576(4) -0.2334(5) 0.0398(17) Uani 1 1 d . . . H8A H -0.4282 0.3842 -0.2052 0.060 Uiso 0.50 1 calc PR B 1 H8B H -0.5825 0.3884 -0.2138 0.060 Uiso 0.50 1 calc PR B 1 H8C H -0.5043 0.3632 -0.2941 0.060 Uiso 0.50 1 calc PR B 1 H8D H -0.5818 0.3730 -0.2702 0.060 Uiso 0.50 1 calc PR B 1 H8E H -0.4275 0.3688 -0.2616 0.060 Uiso 0.50 1 calc PR B 1 H8F H -0.5057 0.3940 -0.1813 0.060 Uiso 0.50 1 calc PR B 1 C10 C -0.5463(9) 0.1130(6) -0.0557(5) 0.058(2) Uani 1 1 d . . . H10A H -0.5592 0.0553 -0.0857 0.088 Uiso 0.50 1 calc PR C 1 H10B H -0.6136 0.1442 -0.0753 0.088 Uiso 0.50 1 calc PR C 1 H10C H -0.5561 0.1043 0.0045 0.088 Uiso 0.50 1 calc PR C 1 H10D H -0.5934 0.1473 -0.0186 0.088 Uiso 0.50 1 calc PR C 1 H10E H -0.5390 0.0583 -0.0290 0.088 Uiso 0.50 1 calc PR C 1 H10F H -0.5965 0.0982 -0.1088 0.088 Uiso 0.50 1 calc PR C 1 C11 C -0.3661(9) 0.2591(7) -0.0339(5) 0.066(3) Uani 1 1 d . . . H11A H -0.2758 0.2911 -0.0481 0.100 Uiso 0.50 1 calc PR D 1 H11B H -0.3719 0.2535 0.0269 0.100 Uiso 0.50 1 calc PR D 1 H11C H -0.4317 0.2919 -0.0530 0.100 Uiso 0.50 1 calc PR D 1 H11D H -0.4438 0.2666 -0.0014 0.100 Uiso 0.50 1 calc PR D 1 H11E H -0.3477 0.3041 -0.0764 0.100 Uiso 0.50 1 calc PR D 1 H11F H -0.2879 0.2658 0.0035 0.100 Uiso 0.50 1 calc PR D 1 C13 C -0.0897(8) 0.1172(6) -0.1161(4) 0.052(2) Uani 1 1 d . . . H13A H -0.0413 0.1703 -0.1435 0.078 Uiso 0.50 1 calc PR E 1 H13B H -0.0277 0.0792 -0.1038 0.078 Uiso 0.50 1 calc PR E 1 H13C H -0.1277 0.1348 -0.0638 0.078 Uiso 0.50 1 calc PR E 1 H13D H -0.0899 0.0859 -0.0639 0.078 Uiso 0.50 1 calc PR E 1 H13E H -0.1034 0.1770 -0.1036 0.078 Uiso 0.50 1 calc PR E 1 H13F H -0.0035 0.1214 -0.1436 0.078 Uiso 0.50 1 calc PR E 1 C14 C -0.2856(8) -0.0195(5) -0.1383(5) 0.053(2) Uani 1 1 d . . . H14A H -0.3536 -0.0469 -0.1806 0.079 Uiso 0.50 1 calc PR F 1 H14B H -0.3298 -0.0059 -0.0868 0.079 Uiso 0.50 1 calc PR F 1 H14C H -0.2281 -0.0606 -0.1263 0.079 Uiso 0.50 1 calc PR F 1 H14D H -0.2541 -0.0287 -0.0819 0.079 Uiso 0.50 1 calc PR F 1 H14E H -0.2779 -0.0697 -0.1757 0.079 Uiso 0.50 1 calc PR F 1 H14F H -0.3796 -0.0151 -0.1362 0.079 Uiso 0.50 1 calc PR F 1 C16 C -0.2591(8) 0.0013(5) -0.3860(4) 0.0439(19) Uani 1 1 d . . . H16A H -0.2095 -0.0167 -0.4332 0.066 Uiso 0.50 1 calc PR G 1 H16B H -0.3554 -0.0157 -0.3987 0.066 Uiso 0.50 1 calc PR G 1 H16C H -0.2392 -0.0280 -0.3356 0.066 Uiso 0.50 1 calc PR G 1 H16D H -0.3266 -0.0236 -0.3451 0.066 Uiso 0.50 1 calc PR G 1 H16E H -0.1806 -0.0246 -0.3796 0.066 Uiso 0.50 1 calc PR G 1 H16F H -0.2968 -0.0123 -0.4428 0.066 Uiso 0.50 1 calc PR G 1 C17 C -0.0670(7) 0.1367(5) -0.3650(4) 0.0410(18) Uani 1 1 d . . . H17A H -0.0258 0.1149 -0.4142 0.062 Uiso 0.50 1 calc PR H 1 H17B H -0.0324 0.1154 -0.3141 0.062 Uiso 0.50 1 calc PR H 1 H17C H -0.0452 0.2017 -0.3629 0.062 Uiso 0.50 1 calc PR H 1 H17D H -0.0432 0.1731 -0.3133 0.062 Uiso 0.50 1 calc PR H 1 H17E H -0.0365 0.1726 -0.4133 0.062 Uiso 0.50 1 calc PR H 1 H17F H -0.0237 0.0863 -0.3646 0.062 Uiso 0.50 1 calc PR H 1 C6A C -0.5559(12) 0.2591(8) -0.2134(9) 0.024(3) Uani 0.50 1 d P I 1 H6AA H -0.5628 0.2544 -0.1512 0.029 Uiso 0.50 1 calc PR I 1 C9A C -0.3939(18) 0.1729(11) -0.0740(9) 0.042(4) Uani 0.50 1 d P I 1 H9A H -0.3264 0.1403 -0.0538 0.051 Uiso 0.50 1 calc PR I 1 C12A C -0.1983(16) 0.0683(9) -0.1720(10) 0.034(3) Uani 0.50 1 d P I 1 H12A H -0.1536 0.0502 -0.2230 0.041 Uiso 0.50 1 calc PR I 1 C15A C -0.2166(15) 0.1033(10) -0.3708(9) 0.035(3) Uani 0.50 1 d P I 1 H15A H -0.2497 0.1312 -0.4198 0.042 Uiso 0.50 1 calc PR I 1 C18A C -0.4406(17) 0.2184(10) -0.3987(8) 0.035(3) Uani 0.50 1 d P I 1 H18A H -0.5116 0.2493 -0.3792 0.042 Uiso 0.50 1 calc PR I 1 C6B C -0.5505(13) 0.2632(8) -0.2738(10) 0.025(3) Uani 0.50 1 d P I 2 H6BA H -0.5450 0.2685 -0.3360 0.030 Uiso 0.50 1 calc PR I 2 C9B C -0.4727(17) 0.1932(10) -0.0934(9) 0.037(3) Uani 0.50 1 d P I 2 H9B H -0.5398 0.2267 -0.1123 0.045 Uiso 0.50 1 calc PR I 2 C12B C -0.2486(16) 0.0740(11) -0.1267(10) 0.042(4) Uani 0.50 1 d P I 2 H12B H -0.2935 0.0908 -0.0752 0.050 Uiso 0.50 1 calc PR I 2 C15B C -0.1843(14) 0.0758(9) -0.3256(10) 0.033(3) Uani 0.50 1 d P I 2 H15B H -0.1498 0.0480 -0.2771 0.040 Uiso 0.50 1 calc PR I 2 C18B C -0.3671(17) 0.1924(11) -0.4154(9) 0.040(4) Uani 0.50 1 d P I 2 H18B H -0.2955 0.1626 -0.4356 0.048 Uiso 0.50 1 calc PR I 2 C19 C -0.3313(8) 0.2868(5) -0.4393(5) 0.052(2) Uani 1 1 d . . . H19A H -0.3686 0.3091 -0.4887 0.078 Uiso 0.50 1 calc PR I 1 H19B H -0.2580 0.2591 -0.4563 0.078 Uiso 0.50 1 calc PR I 1 H19C H -0.2972 0.3362 -0.3991 0.078 Uiso 0.50 1 calc PR I 1 H19D H -0.2472 0.2938 -0.4073 0.078 Uiso 0.50 1 calc PR I 1 H19E H -0.3578 0.3438 -0.4397 0.078 Uiso 0.50 1 calc PR I 1 H19F H -0.3187 0.2667 -0.4969 0.078 Uiso 0.50 1 calc PR I 1 C20 C -0.5076(8) 0.1397(5) -0.4554(4) 0.0449(19) Uani 1 1 d . . . H20A H -0.5425 0.1610 -0.5061 0.067 Uiso 0.50 1 calc PR I 1 H20B H -0.5815 0.1025 -0.4258 0.067 Uiso 0.50 1 calc PR I 1 H20C H -0.4419 0.1047 -0.4708 0.067 Uiso 0.50 1 calc PR I 1 H20D H -0.5015 0.0845 -0.4290 0.067 Uiso 0.50 1 calc PR I 1 H20E H -0.4624 0.1430 -0.5094 0.067 Uiso 0.50 1 calc PR I 1 H20F H -0.6020 0.1408 -0.4643 0.067 Uiso 0.50 1 calc PR I 1 C21 C 0.2219(7) 0.3323(4) 0.3875(4) 0.0305(15) Uani 1 1 d . . . C22 C 0.1997(8) 0.2980(5) 0.4786(4) 0.0414(18) Uani 1 1 d . . . C23 C 0.2698(7) 0.4343(5) 0.3903(4) 0.0383(18) Uani 1 1 d . . . C24 C 0.3309(7) 0.2884(6) 0.3452(5) 0.0421(18) Uani 1 1 d . . . C25 C -0.1500(6) 0.4466(4) 0.2731(4) 0.0278(14) Uani 1 1 d . . . C26 C -0.2706(8) 0.4234(6) 0.2101(6) 0.055(2) Uani 1 1 d . . . C27 C -0.2049(9) 0.4165(6) 0.3618(5) 0.053(2) Uani 1 1 d . . . C28 C -0.0934(8) 0.5478(5) 0.2755(6) 0.050(2) Uani 1 1 d . . . C29 C 0.1614(7) 0.3431(4) 0.0905(4) 0.0295(15) Uani 1 1 d . . . C30 C 0.2543(8) 0.4369(5) 0.0931(4) 0.0424(19) Uani 1 1 d . . . C31 C 0.2308(8) 0.2750(6) 0.0497(5) 0.048(2) Uani 1 1 d . . . C32 C 0.0309(8) 0.3458(6) 0.0378(4) 0.048(2) Uani 1 1 d . . . C33 C -0.1662(6) 0.1336(4) 0.2580(5) 0.0343(16) Uani 1 1 d . . . C34 C -0.1371(8) 0.1091(5) 0.3504(6) 0.055(2) Uani 1 1 d . . . C35 C -0.3219(7) 0.1116(5) 0.2431(5) 0.0400(18) Uani 1 1 d . . . C36 C -0.1024(9) 0.0759(6) 0.1982(7) 0.067(3) Uani 1 1 d D . . 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 Al1 0.0195(10) 0.0215(10) 0.0248(10) 0.0030(7) 0.0028(7) 0.0035(7) Si1 0.0244(10) 0.0257(10) 0.0447(12) -0.0026(8) -0.0004(8) -0.0016(8) O1 0.026(2) 0.035(3) 0.021(2) 0.0059(18) 0.0015(18) 0.0043(19) O2 0.023(2) 0.024(2) 0.030(2) 0.0052(17) 0.0071(18) 0.0083(18) O3 0.033(3) 0.035(3) 0.021(2) 0.0044(18) 0.0045(18) 0.008(2) O4 0.032(3) 0.019(2) 0.041(3) 0.0042(18) 0.002(2) 0.0011(19) F1 0.050(3) 0.073(3) 0.029(2) 0.013(2) 0.0146(19) 0.022(2) F2 0.051(3) 0.094(4) 0.031(2) 0.009(2) -0.012(2) 0.019(3) F3 0.059(3) 0.055(3) 0.043(2) 0.029(2) 0.010(2) 0.024(2) F4 0.048(3) 0.060(3) 0.061(3) 0.009(2) -0.025(2) -0.016(2) F5 0.069(3) 0.040(3) 0.044(2) -0.0070(19) -0.007(2) 0.010(2) F6 0.049(3) 0.034(2) 0.045(2) 0.0163(18) -0.0099(19) -0.0077(19) F7 0.049(3) 0.049(3) 0.064(3) 0.004(2) 0.018(2) 0.019(2) F8 0.036(3) 0.100(4) 0.052(3) 0.028(2) 0.002(2) 0.032(2) F9 0.026(2) 0.076(3) 0.038(2) 0.024(2) 0.0101(17) 0.003(2) F10A 0.044(7) 0.024(5) 0.048(7) -0.006(4) -0.015(5) 0.006(4) F10B 0.020(6) 0.055(8) 0.16(2) -0.010(8) 0.008(7) 0.002(5) F11A 0.062(6) 0.058(8) 0.026(5) 0.019(4) 0.000(4) 0.026(5) F11B 0.061(9) 0.13(3) 0.070(10) -0.056(12) -0.037(7) 0.049(11) F12 0.033(2) 0.054(3) 0.068(3) -0.007(2) -0.007(2) 0.019(2) F13A 0.038(6) 0.065(10) 0.032(5) 0.000(5) 0.003(4) 0.035(6) F13B 0.065(8) 0.122(16) 0.037(6) -0.014(8) -0.005(5) 0.043(10) F14A 0.033(6) 0.035(5) 0.041(5) 0.016(3) 0.023(4) 0.010(4) F14B 0.12(2) 0.061(9) 0.086(11) 0.052(8) 0.068(13) 0.056(10) F15 0.044(3) 0.085(4) 0.053(3) -0.002(2) 0.014(2) 0.028(3) F16A 0.028(8) 0.036(7) 0.16(3) -0.019(10) 0.000(11) 0.004(5) F16B 0.042(9) 0.065(7) 0.097(11) -0.044(7) -0.036(8) 0.015(6) F17A 0.090(19) 0.063(8) 0.058(9) 0.024(6) 0.001(9) 0.026(8) F17B 0.050(10) 0.032(5) 0.094(10) 0.036(5) 0.002(9) -0.009(4) F18 0.050(3) 0.026(2) 0.117(4) -0.007(2) 0.001(3) 0.012(2) F19 0.086(4) 0.066(3) 0.041(2) 0.029(2) 0.021(2) 0.005(3) F20 0.035(3) 0.074(3) 0.055(3) 0.015(2) 0.001(2) -0.017(2) F21 0.064(3) 0.034(2) 0.040(2) 0.0060(18) 0.002(2) -0.005(2) F22 0.076(4) 0.100(4) 0.037(2) 0.007(2) 0.030(2) 0.039(3) F23 0.073(3) 0.050(3) 0.049(3) -0.020(2) -0.011(2) 0.024(3) F24 0.049(3) 0.070(3) 0.044(2) -0.002(2) 0.009(2) 0.034(2) F25 0.070(3) 0.058(3) 0.040(2) 0.004(2) -0.007(2) 0.033(3) F26 0.043(3) 0.058(3) 0.047(3) 0.001(2) -0.012(2) 0.001(2) F27 0.078(4) 0.088(4) 0.023(2) 0.004(2) -0.004(2) 0.022(3) F28 0.081(4) 0.061(3) 0.051(3) 0.015(2) 0.000(3) -0.009(3) F29 0.064(3) 0.058(3) 0.114(4) 0.052(3) -0.008(3) -0.021(3) F30 0.046(3) 0.050(3) 0.155(5) 0.047(3) -0.023(3) 0.003(2) F31 0.033(2) 0.040(3) 0.095(4) -0.005(2) 0.027(2) 0.002(2) F32 0.038(3) 0.031(2) 0.087(3) -0.007(2) 0.009(2) -0.0135(19) F33 0.055(3) 0.051(3) 0.076(3) 0.008(2) -0.024(3) -0.010(2) F35 0.099(5) 0.058(3) 0.088(4) -0.025(3) 0.052(3) -0.019(3) C1 0.025(4) 0.017(3) 0.079(6) 0.000(3) -0.001(4) 0.005(3) C2 0.059(5) 0.027(4) 0.028(4) -0.006(3) 0.012(3) -0.005(4) C3 0.051(5) 0.028(4) 0.040(4) 0.002(3) -0.022(4) 0.001(3) C4 0.031(4) 0.030(4) 0.052(5) -0.013(3) 0.010(3) -0.003(3) C5 0.049(5) 0.033(4) 0.025(4) 0.011(3) -0.015(3) -0.011(3) C7 0.026(4) 0.029(4) 0.057(5) 0.006(3) 0.004(3) 0.003(3) C8 0.034(4) 0.029(4) 0.057(5) 0.001(3) 0.000(3) 0.010(3) C10 0.080(6) 0.064(6) 0.045(5) 0.023(4) 0.039(4) 0.040(5) C11 0.050(5) 0.116(8) 0.040(5) -0.026(5) -0.013(4) 0.037(5) C13 0.045(5) 0.088(7) 0.036(4) -0.002(4) -0.005(4) 0.042(5) C14 0.052(5) 0.060(6) 0.062(5) 0.038(4) 0.029(4) 0.042(4) C16 0.051(5) 0.055(5) 0.028(4) -0.006(3) -0.002(3) 0.020(4) C17 0.035(4) 0.051(5) 0.043(4) 0.017(3) 0.018(3) 0.019(4) C6A 0.019(7) 0.021(7) 0.035(8) 0.001(6) 0.003(6) 0.009(5) C9A 0.054(11) 0.054(11) 0.027(8) 0.001(7) 0.007(7) 0.031(9) C12A 0.039(9) 0.037(8) 0.030(8) 0.006(7) -0.012(7) 0.015(7) C15A 0.045(10) 0.037(9) 0.028(8) 0.009(7) 0.013(7) 0.020(7) C18A 0.042(10) 0.051(10) 0.012(7) 0.019(6) -0.006(6) 0.010(8) C6B 0.029(7) 0.014(6) 0.037(8) 0.000(6) 0.003(7) 0.012(5) C9B 0.048(10) 0.033(8) 0.033(8) -0.010(6) 0.018(7) 0.013(7) C12B 0.042(10) 0.059(11) 0.033(9) -0.001(8) 0.012(7) 0.031(8) C15B 0.026(8) 0.028(8) 0.042(9) 0.001(7) 0.008(7) 0.000(6) C18B 0.032(9) 0.048(10) 0.040(9) 0.020(7) -0.003(7) 0.005(8) C19 0.062(6) 0.056(5) 0.042(4) 0.025(4) 0.005(4) 0.018(4) C20 0.054(5) 0.057(5) 0.025(4) 0.005(3) -0.014(3) 0.015(4) C21 0.035(4) 0.033(4) 0.023(3) 0.007(3) 0.001(3) 0.004(3) C22 0.047(5) 0.051(5) 0.027(4) 0.018(3) 0.005(3) 0.011(4) C23 0.040(4) 0.036(4) 0.036(4) 0.005(3) -0.014(3) 0.000(3) C24 0.026(4) 0.060(5) 0.042(4) 0.012(4) 0.001(3) 0.014(4) C25 0.024(4) 0.024(3) 0.037(4) 0.002(3) 0.001(3) 0.008(3) C26 0.035(5) 0.048(6) 0.082(7) -0.024(5) -0.008(4) 0.014(4) C27 0.058(6) 0.060(6) 0.053(5) 0.014(4) 0.021(4) 0.034(5) C28 0.030(5) 0.031(4) 0.091(7) -0.002(4) 0.005(5) 0.011(4) C29 0.035(4) 0.032(4) 0.018(3) 0.001(3) -0.001(3) 0.000(3) C30 0.056(5) 0.040(5) 0.029(4) 0.005(3) 0.007(4) 0.006(4) C31 0.048(5) 0.070(6) 0.034(4) 0.008(4) 0.008(4) 0.024(4) C32 0.053(5) 0.066(6) 0.028(4) 0.004(4) -0.002(4) 0.018(5) C33 0.020(4) 0.013(3) 0.070(5) 0.003(3) 0.007(3) 0.003(3) C34 0.044(5) 0.032(5) 0.086(7) 0.031(4) 0.000(4) -0.006(4) C35 0.028(4) 0.026(4) 0.065(5) -0.006(3) 0.003(4) 0.004(3) C36 0.046(5) 0.033(5) 0.122(9) 0.013(5) 0.048(6) 0.007(4) _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 Al1 O2 1.730(4) . ? Al1 O1 1.737(4) . ? Al1 O3 1.739(4) . ? Al1 O4 1.746(4) . ? Si1 C2 2.122(7) . ? Si1 C1 2.124(7) . ? Si1 C5 2.139(6) . ? Si1 C4 2.147(7) . ? Si1 C3 2.155(7) . ? O1 C21 1.364(7) . ? O2 C25 1.364(7) . ? O3 C29 1.370(7) . ? O4 C33 1.355(7) . ? F1 C22 1.339(8) . ? F2 C22 1.352(8) . ? F3 C22 1.335(8) . ? F4 C23 1.331(8) . ? F5 C23 1.352(9) . ? F6 C23 1.344(7) . ? F7 C24 1.330(9) . ? F8 C24 1.353(8) . ? F9 C24 1.347(8) . ? F10A F10B 1.155(18) . ? F10A F11B 1.19(2) . ? F10A C26 1.287(11) . ? F10B C26 1.566(17) . ? F10B F14A 1.70(2) . ? F11A F11B 1.128(18) . ? F11A C26 1.488(13) . ? F11A F17A 1.79(3) . ? F11B C26 1.228(14) . ? F12 C26 1.304(9) . ? F13A F13B 1.010(17) . ? F13A F14B 1.149(17) . ? F13A C27 1.218(11) . ? F13B C27 1.576(18) . ? F14A F14B 1.243(18) . ? F14A C27 1.464(12) . ? F14B C27 1.290(13) . ? F15 C27 1.284(9) . ? F16A F16B 0.991(18) . ? F16A C28 1.250(15) . ? F16A F17B 1.36(2) . ? F16B C28 1.448(14) . ? F17A F17B 0.975(18) . ? F17A C28 1.483(18) . ? F17B C28 1.273(12) . ? F18 C28 1.327(9) . ? F19 C30 1.344(7) . ? F20 C30 1.346(9) . ? F21 C30 1.353(8) . ? F22 C31 1.365(8) . ? F23 C31 1.351(9) . ? F24 C31 1.346(8) . ? F25 C32 1.322(9) . ? F26 C32 1.351(9) . ? F27 C32 1.363(8) . ? F28 C34 1.334(10) . ? F29 C34 1.355(8) . ? F30 C34 1.322(9) . ? F31 C35 1.336(8) . ? F32 C35 1.353(8) . ? F33 C35 1.327(8) . ? F34A F34B 0.668(11) . ? F34A C36 1.441(12) . ? F34B C36 1.301(11) . ? F35 C36 1.351(11) . ? F36A F36B 0.656(10) . ? F36A C36 1.313(11) . ? F36B C36 1.406(11) . ? C1 C2 1.431(10) . ? C1 C5 1.426(10) . ? C1 C6B 1.599(14) . ? C1 C6A 1.608(14) . ? C2 C3 1.419(11) . ? C2 C9B 1.609(14) . ? C2 C9A 1.612(15) . ? C3 C4 1.415(10) . ? C3 C12A 1.559(15) . ? C3 C12B 1.604(17) . ? C4 C5 1.430(10) . ? C4 C15A 1.557(15) . ? C4 C15B 1.585(16) . ? C5 C18B 1.575(16) . ? C5 C18A 1.602(13) . ? C7 C6B 1.530(15) . ? C7 C6A 1.547(14) . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C7 H7D 0.9800 . ? C7 H7E 0.9800 . ? C7 H7F 0.9800 . ? C8 C6A 1.537(14) . ? C8 C6B 1.541(14) . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C8 H8D 0.9800 . ? C8 H8E 0.9800 . ? C8 H8F 0.9800 . ? C10 C9B 1.455(16) . ? C10 C9A 1.663(19) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C10 H10D 0.9800 . ? C10 H10E 0.9800 . ? C10 H10F 0.9800 . ? C11 C9A 1.427(17) . ? C11 C9B 1.596(17) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C11 H11D 0.9800 . ? C11 H11E 0.9800 . ? C11 H11F 0.9800 . ? C13 C12A 1.471(15) . ? C13 C12B 1.620(18) . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C13 H13D 0.9800 . ? C13 H13E 0.9800 . ? C13 H13F 0.9800 . ? C14 C12B 1.417(18) . ? C14 C12A 1.568(16) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C14 H14D 0.9800 . ? C14 H14E 0.9800 . ? C14 H14F 0.9800 . ? C16 C15B 1.535(15) . ? C16 C15A 1.550(16) . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C16 H16D 0.9800 . ? C16 H16E 0.9800 . ? C16 H16F 0.9800 . ? C17 C15B 1.511(15) . ? C17 C15A 1.504(17) . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C17 H17D 0.9800 . ? C17 H17E 0.9800 . ? C17 H17F 0.9800 . ? C6A H6AA 1.0000 . ? C9A H9A 1.0000 . ? C12A H12A 1.0000 . ? C15A H15A 1.0000 . ? C18A C20 1.521(16) . ? C18A C19 1.526(16) . ? C18A H18A 1.0000 . ? C6B H6BA 1.0000 . ? C9B H9B 1.0000 . ? C12B H12B 1.0000 . ? C15B H15B 1.0000 . ? C18B C19 1.490(17) . ? C18B C20 1.602(17) . ? C18B H18B 1.0000 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C19 H19D 0.9800 . ? C19 H19E 0.9800 . ? C19 H19F 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C20 H20D 0.9800 . ? C20 H20E 0.9800 . ? C20 H20F 0.9800 . ? C21 C23 1.544(9) . ? C21 C24 1.575(10) . ? C21 C22 1.569(9) . ? C25 C28 1.543(10) . ? C25 C26 1.556(10) . ? C25 C27 1.577(10) . ? C29 C31 1.528(10) . ? C29 C30 1.547(10) . ? C29 C32 1.582(10) . ? C33 C36 1.531(11) . ? C33 C35 1.568(9) . ? C33 C34 1.580(11) . ? 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 Al1 O1 114.8(2) . . ? O2 Al1 O3 107.4(2) . . ? O1 Al1 O3 107.8(2) . . ? O2 Al1 O4 107.1(2) . . ? O1 Al1 O4 106.4(2) . . ? O3 Al1 O4 113.4(2) . . ? C2 Si1 C1 39.4(3) . . ? C2 Si1 C5 65.4(3) . . ? C1 Si1 C5 39.1(3) . . ? C2 Si1 C4 65.1(3) . . ? C1 Si1 C4 65.6(3) . . ? C5 Si1 C4 39.0(3) . . ? C2 Si1 C3 38.7(3) . . ? C1 Si1 C3 65.3(3) . . ? C5 Si1 C3 64.8(2) . . ? C4 Si1 C3 38.4(3) . . ? C21 O1 Al1 145.7(4) . . ? C25 O2 Al1 146.7(4) . . ? C29 O3 Al1 148.1(4) . . ? C33 O4 Al1 149.0(4) . . ? F10B F10A F11B 138.3(12) . . ? F10B F10A C26 79.6(9) . . ? F11B F10A C26 59.2(8) . . ? F10A F10B C26 53.9(8) . . ? F10A F10B F14A 139.9(10) . . ? C26 F10B F14A 105.5(8) . . ? F11B F11A C26 53.9(8) . . ? F11B F11A F17A 134.6(10) . . ? C26 F11A F17A 102.6(7) . . ? F11A F11B F10A 141.6(14) . . ? F11A F11B C26 78.2(10) . . ? F10A F11B C26 64.2(11) . . ? F13B F13A F14B 155.5(14) . . ? F13B F13A C27 89.6(12) . . ? F14B F13A C27 66.0(9) . . ? F13A F13B C27 50.6(8) . . ? F14B F14A C27 56.2(7) . . ? F14B F14A F10B 133.1(8) . . ? C27 F14A F10B 106.0(7) . . ? F13A F14B F14A 128.5(12) . . ? F13A F14B C27 59.6(8) . . ? F14A F14B C27 70.6(9) . . ? F16B F16A C28 79.6(14) . . ? F16B F16A F17B 136.1(17) . . ? C28 F16A F17B 58.2(10) . . ? F16A F16B C28 58.1(11) . . ? F17B F17A C28 58.1(10) . . ? F17B F17A F11A 137.7(13) . . ? C28 F17A F11A 106.0(11) . . ? F17A F17B C28 81.4(12) . . ? F17A F17B F16A 137.3(16) . . ? C28 F17B F16A 56.6(8) . . ? F34B F34A C36 64.4(10) . . ? F34A F34B C36 88.0(13) . . ? F36B F36A C36 84.1(12) . . ? F36A F36B C36 68.3(11) . . ? C2 C1 C5 107.4(6) . . ? C2 C1 C6B 143.6(9) . . ? C5 C1 C6B 109.0(8) . . ? C2 C1 C6A 108.3(8) . . ? C5 C1 C6A 144.3(8) . . ? C6B C1 C6A 35.3(6) . . ? C2 C1 Si1 70.3(4) . . ? C5 C1 Si1 71.1(4) . . ? C6B C1 Si1 123.4(6) . . ? C6A C1 Si1 122.7(6) . . ? C1 C2 C3 108.2(6) . . ? C1 C2 C9B 108.1(9) . . ? C3 C2 C9B 143.5(9) . . ? C1 C2 C9A 142.1(9) . . ? C3 C2 C9A 109.3(8) . . ? C9B C2 C9A 35.4(7) . . ? C1 C2 Si1 70.4(4) . . ? C3 C2 Si1 71.9(4) . . ? C9B C2 Si1 125.1(6) . . ? C9A C2 Si1 116.9(7) . . ? C4 C3 C2 108.4(6) . . ? C4 C3 C12A 109.7(9) . . ? C2 C3 C12A 141.8(9) . . ? C4 C3 C12B 142.4(9) . . ? C2 C3 C12B 109.1(8) . . ? C12A C3 C12B 33.2(7) . . ? C4 C3 Si1 70.5(4) . . ? C2 C3 Si1 69.4(4) . . ? C12A C3 Si1 121.9(7) . . ? C12B C3 Si1 127.0(7) . . ? C3 C4 C5 107.9(6) . . ? C3 C4 C15A 144.2(9) . . ? C5 C4 C15A 107.9(8) . . ? C3 C4 C15B 109.3(9) . . ? C5 C4 C15B 142.8(9) . . ? C15A C4 C15B 34.9(6) . . ? C3 C4 Si1 71.1(4) . . ? C5 C4 Si1 70.2(4) . . ? C15A C4 Si1 122.5(7) . . ? C15B C4 Si1 124.8(6) . . ? C4 C5 C1 108.1(6) . . ? C4 C5 C18B 108.4(9) . . ? C1 C5 C18B 143.4(9) . . ? C4 C5 C18A 143.5(9) . . ? C1 C5 C18A 108.4(9) . . ? C18B C5 C18A 35.3(7) . . ? C4 C5 Si1 70.8(4) . . ? C1 C5 Si1 69.9(4) . . ? C18B C5 Si1 120.6(7) . . ? C18A C5 Si1 124.1(6) . . ? C6B C7 C6A 36.8(6) . . ? C6B C7 H7A 124.0 . . ? C6B C7 H7B 72.7 . . ? C6B C7 H7C 122.6 . . ? C6B C7 H7D 88.5 . . ? C6B C7 H7E 146.3 . . ? C6B C7 H7F 89.7 . . ? C6A C8 C6B 36.8(6) . . ? C6B C8 H8A 124.7 . . ? C6B C8 H8B 122.0 . . ? C6B C8 H8C 72.7 . . ? C6B C8 H8D 88.0 . . ? C6B C8 H8E 90.3 . . ? C6B C8 H8F 146.2 . . ? C9B C10 C9A 35.9(7) . . ? C9B C10 H10A 120.8 . . ? C9B C10 H10B 73.7 . . ? C9B C10 H10C 125.4 . . ? C9B C10 H10D 91.6 . . ? C9B C10 H10E 145.2 . . ? C9B C10 H10F 87.7 . . ? C9A C11 C9B 37.3(7) . . ? C9B C11 H11A 127.6 . . ? C9B C11 H11B 119.2 . . ? C9B C11 H11C 72.4 . . ? C9B C11 H11D 85.5 . . ? C9B C11 H11E 92.4 . . ? C9B C11 H11F 146.3 . . ? C12A C13 C12B 33.6(7) . . ? C12B C13 H13A 125.4 . . ? C12B C13 H13B 119.7 . . ? C12B C13 H13C 76.0 . . ? C12B C13 H13D 88.6 . . ? C12B C13 H13E 93.5 . . ? C12B C13 H13F 142.9 . . ? C12B C14 C12A 34.8(7) . . ? C12B C14 H14A 120.3 . . ? C12B C14 H14B 74.7 . . ? C12B C14 H14C 125.4 . . ? C12B C14 H14D 92.5 . . ? C12B C14 H14E 144.1 . . ? C12B C14 H14F 88.1 . . ? C15B C16 C15A 35.6(7) . . ? C15B C16 H16A 117.8 . . ? C15B C16 H16B 128.2 . . ? C15B C16 H16C 74.3 . . ? C15B C16 H16D 94.3 . . ? C15B C16 H16E 85.6 . . ? C15B C16 H16F 144.4 . . ? C15B C17 C15A 36.5(7) . . ? C15B C17 H17A 118.8 . . ? C15B C17 H17B 73.3 . . ? C15B C17 H17C 127.6 . . ? C15B C17 H17D 93.1 . . ? C15B C17 H17E 145.5 . . ? C15B C17 H17F 85.8 . . ? C8 C6A C7 113.3(9) . . ? C8 C6A C1 110.6(9) . . ? C7 C6A C1 107.2(8) . . ? C8 C6A H6AA 108.5 . . ? C7 C6A H6AA 108.5 . . ? C1 C6A H6AA 108.5 . . ? C11 C9A C2 115.8(11) . . ? C11 C9A C10 113.7(11) . . ? C2 C9A C10 101.2(10) . . ? C11 C9A H9A 108.5 . . ? C2 C9A H9A 108.5 . . ? C10 C9A H9A 108.5 . . ? C13 C12A C3 116.0(10) . . ? C13 C12A C14 116.3(10) . . ? C3 C12A C14 106.0(10) . . ? C13 C12A H12A 105.9 . . ? C3 C12A H12A 105.9 . . ? C14 C12A H12A 105.9 . . ? C17 C15A C16 112.8(10) . . ? C17 C15A C4 112.6(10) . . ? C16 C15A C4 108.7(10) . . ? C17 C15A H15A 107.5 . . ? C16 C15A H15A 107.5 . . ? C4 C15A H15A 107.5 . . ? C20 C18A C19 115.3(10) . . ? C20 C18A C5 107.9(10) . . ? C19 C18A C5 110.0(10) . . ? C20 C18A H18A 107.8 . . ? C19 C18A H18A 107.8 . . ? C5 C18A H18A 107.8 . . ? C7 C6B C8 114.0(9) . . ? C7 C6B C1 108.4(8) . . ? C8 C6B C1 110.8(9) . . ? C7 C6B H6BA 107.8 . . ? C8 C6B H6BA 107.8 . . ? C1 C6B H6BA 107.8 . . ? C10 C9B C2 111.4(10) . . ? C10 C9B C11 116.1(11) . . ? C2 C9B C11 107.0(10) . . ? C10 C9B H9B 107.3 . . ? C2 C9B H9B 107.3 . . ? C11 C9B H9B 107.3 . . ? C14 C12B C3 111.3(11) . . ? C14 C12B C13 116.3(11) . . ? C3 C12B C13 105.7(11) . . ? C14 C12B H12B 107.7 . . ? C3 C12B H12B 107.7 . . ? C13 C12B H12B 107.7 . . ? C17 C15B C16 113.3(10) . . ? C17 C15B C4 110.7(10) . . ? C16 C15B C4 108.0(9) . . ? C17 C15B H15B 108.2 . . ? C16 C15B H15B 108.2 . . ? C4 C15B H15B 108.2 . . ? C19 C18B C5 113.5(12) . . ? C19 C18B C20 112.7(10) . . ? C5 C18B C20 105.3(10) . . ? C19 C18B H18B 108.4 . . ? C5 C18B H18B 108.4 . . ? C20 C18B H18B 108.4 . . ? C18B C19 C18A 37.3(7) . . ? C18B C19 H19A 123.7 . . ? C18B C19 H19B 72.2 . . ? C18B C19 H19C 123.1 . . ? C18B C19 H19D 88.6 . . ? C18B C19 H19E 146.7 . . ? C18B C19 H19F 89.1 . . ? C18A C20 C18B 35.9(7) . . ? C18B C20 H20A 119.5 . . ? C18B C20 H20B 126.6 . . ? C18B C20 H20C 73.8 . . ? C18B C20 H20D 92.7 . . ? C18B C20 H20E 86.8 . . ? C18B C20 H20F 145.0 . . ? O1 C21 C23 111.5(5) . . ? O1 C21 C24 109.2(5) . . ? C23 C21 C24 110.0(6) . . ? O1 C21 C22 107.7(5) . . ? C23 C21 C22 110.2(5) . . ? C24 C21 C22 108.2(5) . . ? F3 C22 F1 107.6(6) . . ? F3 C22 F2 107.8(6) . . ? F1 C22 F2 107.0(6) . . ? F3 C22 C21 111.6(6) . . ? F1 C22 C21 110.2(5) . . ? F2 C22 C21 112.4(6) . . ? F4 C23 F6 107.6(6) . . ? F4 C23 F5 107.6(5) . . ? F6 C23 F5 106.4(6) . . ? F4 C23 C21 113.3(6) . . ? F6 C23 C21 110.9(5) . . ? F5 C23 C21 110.8(6) . . ? F7 C24 F8 108.2(6) . . ? F7 C24 F9 107.7(6) . . ? F8 C24 F9 107.2(6) . . ? F7 C24 C21 111.5(6) . . ? F8 C24 C21 111.6(6) . . ? F9 C24 C21 110.5(6) . . ? O2 C25 C28 108.0(5) . . ? O2 C25 C26 110.5(5) . . ? C28 C25 C26 108.8(6) . . ? O2 C25 C27 112.2(5) . . ? C28 C25 C27 110.0(6) . . ? C26 C25 C27 107.2(6) . . ? F11B C26 F10A 56.6(11) . . ? F11B C26 F12 122.3(10) . . ? F10A C26 F12 117.5(8) . . ? F11B C26 F11A 47.9(10) . . ? F10A C26 F11A 104.2(10) . . ? F12 C26 F11A 97.2(7) . . ? F11B C26 F10B 102.9(12) . . ? F10A C26 F10B 46.5(7) . . ? F12 C26 F10B 90.4(7) . . ? F11A C26 F10B 148.7(10) . . ? F11B C26 C25 117.3(9) . . ? F10A C26 C25 115.2(7) . . ? F12 C26 C25 115.0(7) . . ? F11A C26 C25 104.2(7) . . ? F10B C26 C25 99.9(8) . . ? F13A C27 F15 116.0(8) . . ? F13A C27 F14B 54.4(9) . . ? F15 C27 F14B 126.4(9) . . ? F13A C27 F14A 106.5(9) . . ? F15 C27 F14A 96.6(7) . . ? F14B C27 F14A 53.2(10) . . ? F13A C27 C25 114.5(8) . . ? F15 C27 C25 116.2(6) . . ? F14B C27 C25 113.9(8) . . ? F14A C27 C25 103.9(6) . . ? F13A C27 F13B 39.8(7) . . ? F15 C27 F13B 95.1(7) . . ? F14B C27 F13B 94.3(12) . . ? F14A C27 F13B 145.5(9) . . ? C25 C27 F13B 99.7(8) . . ? F16A C28 F17B 65.2(12) . . ? F16A C28 F18 120.7(12) . . ? F17B C28 F18 116.9(9) . . ? F16A C28 F16B 42.3(10) . . ? F17B C28 F16B 106.7(10) . . ? F18 C28 F16B 95.0(9) . . ? F16A C28 F17A 105.4(14) . . ? F17B C28 F17A 40.5(8) . . ? F18 C28 F17A 92.4(10) . . ? F16B C28 F17A 144.5(11) . . ? F16A C28 C25 115.7(9) . . ? F17B C28 C25 114.9(8) . . ? F18 C28 C25 114.5(6) . . ? F16B C28 C25 105.8(8) . . ? F17A C28 C25 102.5(9) . . ? O3 C29 C31 107.7(5) . . ? O3 C29 C30 110.8(5) . . ? C31 C29 C30 111.0(6) . . ? O3 C29 C32 109.7(5) . . ? C31 C29 C32 109.3(5) . . ? C30 C29 C32 108.3(6) . . ? F19 C30 F20 109.1(6) . . ? F19 C30 F21 106.5(6) . . ? F20 C30 F21 107.2(6) . . ? F19 C30 C29 112.2(6) . . ? F20 C30 C29 110.7(6) . . ? F21 C30 C29 111.0(6) . . ? F23 C31 F24 107.3(6) . . ? F23 C31 F22 107.9(6) . . ? F24 C31 F22 106.2(6) . . ? F23 C31 C29 112.2(6) . . ? F24 C31 C29 110.9(6) . . ? F22 C31 C29 112.0(6) . . ? F25 C32 F26 108.4(7) . . ? F25 C32 F27 108.2(6) . . ? F26 C32 F27 106.2(6) . . ? F25 C32 C29 112.7(6) . . ? F26 C32 C29 109.9(6) . . ? F27 C32 C29 111.2(6) . . ? O4 C33 C36 111.2(6) . . ? O4 C33 C35 108.6(5) . . ? C36 C33 C35 109.7(6) . . ? O4 C33 C34 111.5(5) . . ? C36 C33 C34 107.7(7) . . ? C35 C33 C34 108.2(6) . . ? F30 C34 F28 108.1(7) . . ? F30 C34 F29 107.1(6) . . ? F28 C34 F29 108.5(7) . . ? F30 C34 C33 110.9(7) . . ? F28 C34 C33 110.3(6) . . ? F29 C34 C33 111.7(7) . . ? F33 C35 F31 108.5(6) . . ? F33 C35 F32 107.9(6) . . ? F31 C35 F32 106.7(6) . . ? F33 C35 C33 110.6(6) . . ? F31 C35 C33 110.5(6) . . ? F32 C35 C33 112.5(6) . . ? F34B C36 F36A 116.1(9) . . ? F34B C36 F35 88.4(10) . . ? F36A C36 F35 90.0(10) . . ? F34B C36 F36B 111.7(8) . . ? F36A C36 F36B 27.7(5) . . ? F35 C36 F36B 117.6(9) . . ? F34B C36 F34A 27.6(5) . . ? F36A C36 F34A 113.5(8) . . ? F35 C36 F34A 116.0(8) . . ? F36B C36 F34A 96.9(8) . . ? F34B C36 C33 118.4(8) . . ? F36A C36 C33 121.6(8) . . ? F35 C36 C33 110.5(7) . . ? F36B C36 C33 109.3(8) . . ? F34A C36 C33 105.2(8) . . ? _diffrn_measured_fraction_theta_max 0.968 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.968 _refine_diff_density_max 0.610 _refine_diff_density_min -0.566 _refine_diff_density_rms 0.100