# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_email erhard.kemnitz@chemie.hu-berlin.de _publ_contact_author_name E.Kemnitz loop_ _publ_author_name E.Kemnitz G.Scholz M.Veiczi C.Jaeger S.Troyanov R.Koenig data_comp1 _database_code_depnum_ccdc_archive 'CCDC 826056' #TrackingRef '- compound1.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C21 H50 Al4 F4 O8' _chemical_formula_weight 614.53 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' Al Al 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c 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' '-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 15.2063(12) _cell_length_b 12.2374(7) _cell_length_c 18.2326(14) _cell_angle_alpha 90.00 _cell_angle_beta 101.606(6) _cell_angle_gamma 90.00 _cell_volume 3323.5(4) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 8900 _cell_measurement_theta_min 3 _cell_measurement_theta_max 27 _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.228 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1312 _exptl_absorpt_coefficient_mu 0.199 _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 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 IPDS(Stoe) _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13593 _diffrn_reflns_av_R_equivalents 0.1048 _diffrn_reflns_av_sigmaI/netI 0.0724 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 3.33 _diffrn_reflns_theta_max 27.88 _reflns_number_total 3926 _reflns_number_gt 2625 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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 molecule has crystallographically imposed two-fold symmetry with oxygen atoms O1 and O5 on the two-fold axis. ; _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^)+(0.1000P)^2^+7.5000P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3926 _refine_ls_number_parameters 194 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.1273 _refine_ls_R_factor_gt 0.0919 _refine_ls_wR_factor_ref 0.2526 _refine_ls_wR_factor_gt 0.2295 _refine_ls_goodness_of_fit_ref 1.026 _refine_ls_restrained_S_all 1.026 _refine_ls_shift/su_max 0.016 _refine_ls_shift/su_mean 0.002 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 0.03364(7) 0.29267(10) 0.34865(6) 0.0568(4) Uani 1 1 d . . . Al2 Al 0.09146(9) 0.15054(11) 0.24321(6) 0.0628(4) Uani 1 1 d . . . F1 F 0.06442(19) 0.3132(3) 0.44140(14) 0.1005(11) Uani 1 1 d . . . F2 F 0.1770(2) 0.0683(3) 0.23574(17) 0.1220(14) Uani 1 1 d . . . O1 O 0.0000 0.2488(2) 0.2500 0.0396(6) Uani 1 2 d S . . O2 O 0.13301(17) 0.2144(3) 0.33432(14) 0.0688(8) Uani 1 1 d . . . O3 O -0.07064(19) 0.2148(3) 0.34924(14) 0.0660(8) Uani 1 1 d . . . O4 O 0.0242(3) 0.4313(3) 0.3174(2) 0.0904(12) Uani 1 1 d D . . H H 0.022(6) 0.417(7) 0.2804(17) 0.050 Uiso 0.50 1 d PD . . O5 O 0.0000 0.0548(3) 0.2500 0.0852(14) Uani 1 2 d S . . C1 C 0.2200(3) 0.2068(7) 0.3869(3) 0.107(2) Uani 1 1 d . . . H1 H 0.2079 0.2532 0.4289 0.129 Uiso 1 1 calc R . . C2 C 0.2306(4) 0.1016(5) 0.4225(3) 0.106(2) Uani 1 1 d . . . H2A H 0.2327 0.0450 0.3849 0.158 Uiso 1 1 calc R . . H2B H 0.1797 0.0877 0.4468 0.158 Uiso 1 1 calc R . . H2C H 0.2865 0.1004 0.4602 0.158 Uiso 1 1 calc R . . C3 C 0.2873(4) 0.2689(6) 0.3633(5) 0.143(3) Uani 1 1 d . . . H3A H 0.3424 0.2665 0.4019 0.214 Uiso 1 1 calc R . . H3B H 0.2671 0.3448 0.3551 0.214 Uiso 1 1 calc R . . H3C H 0.2991 0.2386 0.3165 0.214 Uiso 1 1 calc R . . C4 C -0.1201(5) 0.2046(8) 0.4090(3) 0.134(3) Uani 1 1 d . . . H4 H -0.1706 0.1610 0.3793 0.161 Uiso 1 1 calc R . . C5 C -0.1722(7) 0.2984(7) 0.4156(6) 0.173(5) Uani 1 1 d . . . H5A H -0.2118 0.2836 0.4506 0.259 Uiso 1 1 calc R . . H5B H -0.2084 0.3171 0.3664 0.259 Uiso 1 1 calc R . . H5C H -0.1324 0.3597 0.4342 0.259 Uiso 1 1 calc R . . C6 C -0.0906(8) 0.1250(8) 0.4598(4) 0.188(5) Uani 1 1 d . . . H6A H -0.0919 0.0545 0.4341 0.282 Uiso 1 1 calc R . . H6B H -0.1297 0.1217 0.4965 0.282 Uiso 1 1 calc R . . H6C H -0.0290 0.1413 0.4856 0.282 Uiso 1 1 calc R . . C7 C 0.0555(7) 0.5139(7) 0.3816(5) 0.068(2) Uani 0.50 1 d P A 1 H7 H 0.0758 0.4718 0.4290 0.082 Uiso 0.50 1 calc PR A 1 C8 C 0.1324(3) 0.5684(5) 0.3634(3) 0.0865(15) Uani 0.50 1 d P A 1 H8A H 0.1498 0.6296 0.3979 0.130 Uiso 0.50 1 calc PR A 1 H8B H 0.1172 0.5959 0.3119 0.130 Uiso 0.50 1 calc PR A 1 H8C H 0.1824 0.5167 0.3680 0.130 Uiso 0.50 1 calc PR A 1 C9 C -0.0240(3) 0.5731(4) 0.3877(3) 0.0824(14) Uani 0.50 1 d P A 1 H9A H -0.0640 0.5257 0.4095 0.124 Uiso 0.50 1 calc PR A 1 H9B H -0.0549 0.5971 0.3378 0.124 Uiso 0.50 1 calc PR A 1 H9C H -0.0076 0.6371 0.4199 0.124 Uiso 0.50 1 calc PR A 1 C7A C 0.0362(5) 0.5458(6) 0.3366(5) 0.0558(17) Uani 0.50 1 d P A 2 H7A H 0.0160 0.5887 0.2896 0.067 Uiso 0.50 1 calc PR A 2 C8A C 0.1324(3) 0.5684(5) 0.3634(3) 0.0865(15) Uani 0.50 1 d P A 2 H8A1 H 0.1588 0.5117 0.3991 0.130 Uiso 0.50 1 calc PR A 2 H8A2 H 0.1397 0.6399 0.3881 0.130 Uiso 0.50 1 calc PR A 2 H8A3 H 0.1628 0.5686 0.3208 0.130 Uiso 0.50 1 calc PR A 2 C9A C -0.0240(3) 0.5731(4) 0.3877(3) 0.0824(14) Uani 0.50 1 d P A 2 H9A1 H -0.0865 0.5639 0.3616 0.124 Uiso 0.50 1 calc PR A 2 H9A2 H -0.0141 0.6491 0.4042 0.124 Uiso 0.50 1 calc PR A 2 H9A3 H -0.0116 0.5246 0.4313 0.124 Uiso 0.50 1 calc PR A 2 C10 C 0.0309(6) -0.0627(6) 0.2508(7) 0.080(3) Uani 0.50 1 d P . . H10 H 0.0951 -0.0634 0.2458 0.096 Uiso 0.50 1 calc PR . . C11 C -0.0254(5) -0.1095(5) 0.1800(4) 0.123(2) Uani 1 1 d . . . H11A H -0.0111 -0.1872 0.1762 0.185 Uiso 1 1 calc R . . H11B H -0.0123 -0.0703 0.1365 0.185 Uiso 1 1 calc R . . H11C H -0.0892 -0.1015 0.1813 0.185 Uiso 1 1 calc R . . 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 0.0502(6) 0.0699(8) 0.0491(6) -0.0202(5) 0.0072(4) 0.0023(5) Al2 0.0731(8) 0.0663(8) 0.0488(6) -0.0044(5) 0.0118(5) 0.0309(6) F1 0.0766(17) 0.161(3) 0.0598(15) -0.0487(17) 0.0038(12) 0.0053(18) F2 0.133(3) 0.150(3) 0.085(2) -0.0112(19) 0.0247(18) 0.097(3) O1 0.0357(14) 0.0424(16) 0.0404(15) 0.000 0.0072(11) 0.000 O2 0.0477(14) 0.104(2) 0.0494(14) -0.0045(14) -0.0031(11) 0.0234(14) O3 0.0643(16) 0.092(2) 0.0456(13) 0.0015(13) 0.0203(12) -0.0082(15) O4 0.090(2) 0.0555(18) 0.133(3) -0.046(2) 0.038(2) -0.0154(16) O5 0.152(5) 0.038(2) 0.065(2) 0.000 0.021(3) 0.000 C1 0.055(3) 0.188(7) 0.070(3) 0.034(4) -0.009(2) 0.020(3) C2 0.084(3) 0.109(5) 0.104(4) -0.003(3) -0.029(3) 0.040(3) C3 0.062(3) 0.109(5) 0.229(9) 0.017(5) -0.039(4) 0.018(3) C4 0.105(5) 0.234(10) 0.075(4) 0.018(5) 0.048(3) -0.016(5) C5 0.220(9) 0.120(6) 0.241(10) -0.029(6) 0.195(9) -0.015(6) C6 0.338(14) 0.166(8) 0.090(5) 0.038(5) 0.114(7) -0.016(9) C7 0.087(6) 0.051(5) 0.058(5) -0.017(4) -0.009(4) 0.007(4) C8 0.067(3) 0.087(4) 0.100(4) -0.030(3) 0.003(2) -0.013(2) C9 0.081(3) 0.073(3) 0.092(3) -0.030(3) 0.014(3) 0.009(2) C7A 0.064(4) 0.038(4) 0.059(5) -0.009(3) -0.001(4) 0.001(3) C8A 0.067(3) 0.087(4) 0.100(4) -0.030(3) 0.003(2) -0.013(2) C9A 0.081(3) 0.073(3) 0.092(3) -0.030(3) 0.014(3) 0.009(2) C10 0.087(7) 0.041(4) 0.109(7) 0.002(5) 0.016(8) 0.003(4) C11 0.141(6) 0.061(3) 0.157(6) -0.037(4) 0.005(5) 0.004(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 F1 1.680(3) . ? Al1 O4 1.786(4) . ? Al1 O1 1.8481(14) . ? Al1 O2 1.851(3) . ? Al1 O3 1.852(3) . ? Al1 Al2 2.8579(16) 2 ? Al1 Al2 2.8590(15) . ? Al2 F2 1.672(3) . ? Al2 O3 1.829(3) 2 ? Al2 O2 1.829(3) . ? Al2 O5 1.842(3) . ? Al2 O1 1.861(2) . ? Al2 Al2 2.842(3) 2 ? Al2 Al1 2.8579(16) 2 ? O1 Al1 1.8481(14) 2 ? O1 Al2 1.861(2) 2 ? O2 C1 1.472(5) . ? O3 C4 1.448(6) . ? O3 Al2 1.829(3) 2 ? O4 C7A 1.447(8) . ? O4 C7 1.547(8) . ? O5 C10 1.511(8) 2 ? O5 C10 1.511(8) . ? O5 Al2 1.842(3) 2 ? C1 C3 1.409(9) . ? C1 C2 1.437(9) . ? C4 C6 1.357(11) . ? C4 C5 1.413(11) . ? C7 C9 1.433(10) . ? C7 C8 1.442(11) . ? C10 C11 1.403(13) 2 ? C10 C11 1.511(13) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag F1 Al1 O4 99.63(19) . . ? F1 Al1 O1 171.71(18) . . ? O4 Al1 O1 88.66(16) . . ? F1 Al1 O2 98.61(14) . . ? O4 Al1 O2 117.50(17) . . ? O1 Al1 O2 77.66(10) . . ? F1 Al1 O3 97.86(15) . . ? O4 Al1 O3 118.45(17) . . ? O1 Al1 O3 77.66(10) . . ? O2 Al1 O3 117.31(16) . . ? F1 Al1 Al2 134.33(14) . 2 ? O4 Al1 Al2 112.92(14) . 2 ? O1 Al1 Al2 39.77(6) . 2 ? O2 Al1 Al2 93.93(11) . 2 ? O3 Al1 Al2 38.78(8) . 2 ? F1 Al1 Al2 134.98(13) . . ? O4 Al1 Al2 112.27(13) . . ? O1 Al1 Al2 39.74(6) . . ? O2 Al1 Al2 38.76(9) . . ? O3 Al1 Al2 94.03(10) . . ? Al2 Al1 Al2 59.62(6) 2 . ? F2 Al2 O3 100.19(15) . 2 ? F2 Al2 O2 101.47(15) . . ? O3 Al2 O2 128.12(17) 2 . ? F2 Al2 O5 103.5(2) . . ? O3 Al2 O5 110.02(12) 2 . ? O2 Al2 O5 109.78(12) . . ? F2 Al2 O1 176.71(19) . . ? O3 Al2 O1 77.91(10) 2 . ? O2 Al2 O1 77.87(9) . . ? O5 Al2 O1 79.75(13) . . ? F2 Al2 Al2 142.99(17) . 2 ? O3 Al2 Al2 95.12(10) 2 2 ? O2 Al2 Al2 94.95(10) . 2 ? O5 Al2 Al2 39.52(10) . 2 ? O1 Al2 Al2 40.23(8) . 2 ? F2 Al2 Al1 139.09(12) . 2 ? O3 Al2 Al1 39.36(9) 2 2 ? O2 Al2 Al1 109.86(11) . 2 ? O5 Al2 Al1 90.23(9) . 2 ? O1 Al2 Al1 39.44(4) . 2 ? Al2 Al2 Al1 60.21(4) 2 2 ? F2 Al2 Al1 140.40(13) . . ? O3 Al2 Al1 109.79(11) 2 . ? O2 Al2 Al1 39.31(8) . . ? O5 Al2 Al1 90.20(9) . . ? O1 Al2 Al1 39.41(3) . . ? Al2 Al2 Al1 60.17(4) 2 . ? Al1 Al2 Al1 76.43(5) 2 . ? Al1 O1 Al1 146.20(19) . 2 ? Al1 O1 Al2 100.80(7) . 2 ? Al1 O1 Al2 100.85(6) 2 2 ? Al1 O1 Al2 100.85(6) . . ? Al1 O1 Al2 100.80(7) 2 . ? Al2 O1 Al2 99.55(17) 2 . ? C1 O2 Al2 131.7(3) . . ? C1 O2 Al1 126.4(3) . . ? Al2 O2 Al1 101.92(12) . . ? C4 O3 Al2 129.5(4) . 2 ? C4 O3 Al1 128.6(4) . . ? Al2 O3 Al1 101.86(12) 2 . ? C7A O4 C7 34.9(4) . . ? C7A O4 Al1 147.6(5) . . ? C7 O4 Al1 112.7(5) . . ? C10 O5 C10 36.0(7) 2 . ? C10 O5 Al2 147.3(4) 2 . ? C10 O5 Al2 111.6(4) . . ? C10 O5 Al2 111.6(4) 2 2 ? C10 O5 Al2 147.3(4) . 2 ? Al2 O5 Al2 101.0(2) . 2 ? C3 C1 C2 126.8(5) . . ? C3 C1 O2 112.3(5) . . ? C2 C1 O2 110.8(5) . . ? C6 C4 C5 129.7(7) . . ? C6 C4 O3 115.1(7) . . ? C5 C4 O3 112.3(6) . . ? C9 C7 C8 121.3(7) . . ? C9 C7 O4 104.7(6) . . ? C8 C7 O4 105.6(6) . . ? C11 C10 O5 108.9(8) 2 . ? C11 C10 C11 119.2(8) 2 . ? O5 C10 C11 103.4(7) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 27.88 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.401 _refine_diff_density_min -0.349 _refine_diff_density_rms 0.070 # Attachment '- compound_2_Al4F4 and Al5F5.CIF' data_resch3 _database_code_depnum_ccdc_archive 'CCDC 826057' #TrackingRef '- compound_2_Al4F4 and Al5F5.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C45 H106 Al9 F9 O17' _chemical_formula_weight 1333.12 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' Al Al 0.0645 0.0514 '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 9.7613(7) _cell_length_b 18.6429(14) _cell_length_c 19.1726(15) _cell_angle_alpha 87.900(6) _cell_angle_beta 86.201(6) _cell_angle_gamma 87.603(6) _cell_volume 3476.3(5) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 15800 _cell_measurement_theta_min 3 _cell_measurement_theta_max 27 _exptl_crystal_description needle _exptl_crystal_colour clorless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.274 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1420 _exptl_absorpt_coefficient_mu 0.211 _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 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 IPDS(Stoe) _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 24485 _diffrn_reflns_av_R_equivalents 0.0922 _diffrn_reflns_av_sigmaI/netI 0.1060 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 3.27 _diffrn_reflns_theta_max 27.48 _reflns_number_total 14602 _reflns_number_gt 8367 _reflns_threshold_expression >2sigma(I) _computing_data_collection XDS _computing_cell_refinement XDS _computing_data_reduction XDS _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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. Only one of 106 H atoms was refined, whereas all others were included in the geometrically calculated positions. ; _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^)+(0.0800P)^2^+8.0000P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 14602 _refine_ls_number_parameters 776 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1697 _refine_ls_R_factor_gt 0.1122 _refine_ls_wR_factor_ref 0.2770 _refine_ls_wR_factor_gt 0.2577 _refine_ls_goodness_of_fit_ref 1.195 _refine_ls_restrained_S_all 1.195 _refine_ls_shift/su_max 0.020 _refine_ls_shift/su_mean 0.001 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 0.9426(2) 0.85756(9) 0.35954(10) 0.0385(4) Uani 1 1 d . . . Al2 Al 0.9680(2) 0.66665(9) 0.37018(10) 0.0379(4) Uani 1 1 d . . . Al3 Al 0.7248(2) 0.75874(9) 0.36037(10) 0.0393(4) Uani 1 1 d . . . Al4 Al 0.9315(2) 0.75862(9) 0.24846(10) 0.0389(4) Uani 1 1 d . . . Al5 Al 0.5044(2) 1.27080(10) 0.16984(11) 0.0436(5) Uani 1 1 d . A . Al6 Al 0.3245(2) 1.27293(10) 0.05118(10) 0.0450(5) Uani 1 1 d . A . Al7 Al 0.2562(2) 1.36535(9) 0.16601(11) 0.0423(5) Uani 1 1 d . . . Al8 Al 0.2606(2) 1.24492(11) 0.26501(11) 0.0467(5) Uani 1 1 d . A . Al9 Al 0.3258(2) 1.15204(10) 0.14933(12) 0.0501(5) Uani 1 1 d . A . O1 O 0.9167(4) 0.76122(19) 0.3467(2) 0.0348(9) Uani 1 1 d . . . O2 O 0.7575(5) 0.8494(2) 0.3879(2) 0.0426(10) Uani 1 1 d . . . O3 O 0.9908(5) 0.8493(2) 0.2645(2) 0.0429(10) Uani 1 1 d . . . O4 O 1.0688(5) 0.8321(2) 0.4213(2) 0.0433(11) Uani 1 1 d . . . O5 O 0.7814(5) 0.6713(2) 0.3989(2) 0.0422(10) Uani 1 1 d . . . O6 O 1.0070(5) 0.6698(2) 0.2735(2) 0.0402(10) Uani 1 1 d . . . O7 O 1.0974(5) 0.7015(2) 0.4227(2) 0.0402(10) Uani 1 1 d . . . H H 1.107(7) 0.763(4) 0.434(3) 0.046(18) Uiso 1 1 d . . . O8 O 0.7443(4) 0.7569(2) 0.2643(2) 0.0390(10) Uani 1 1 d . . . O9 O 0.3180(4) 1.2606(2) 0.1590(2) 0.0377(9) Uani 1 1 d . . . O10 O 0.5004(5) 1.2851(2) 0.0689(2) 0.0495(11) Uani 1 1 d . . . O11 O 0.4367(5) 1.3702(2) 0.1786(2) 0.0456(11) Uani 1 1 d . . . O12 O 0.4428(5) 1.2537(2) 0.2680(2) 0.0456(11) Uani 1 1 d . . . O13 O 0.5048(5) 1.1680(2) 0.1590(2) 0.0459(11) Uani 1 1 d . . . O14 O 0.2125(5) 1.3476(2) 0.0777(2) 0.0456(11) Uani 1 1 d . . . O15 O 0.1626(5) 1.3268(2) 0.2426(2) 0.0462(11) Uani 1 1 d . . . O16 O 0.2189(5) 1.1605(2) 0.2300(3) 0.0530(12) Uani 1 1 d . . . O17 O 0.2692(5) 1.1826(2) 0.0645(3) 0.0522(12) Uani 1 1 d . . . F1 F 0.9486(4) 0.94819(17) 0.3614(2) 0.0456(9) Uani 1 1 d . . . F2 F 0.9978(4) 0.57817(17) 0.38568(19) 0.0434(8) Uani 1 1 d . . . F3 F 0.5553(4) 0.75600(18) 0.3808(2) 0.0452(9) Uani 1 1 d . . . F4 F 0.9540(4) 0.75785(18) 0.16087(19) 0.0474(9) Uani 1 1 d . . . F5 F 0.6731(4) 1.2803(2) 0.1786(2) 0.0545(10) Uani 1 1 d . . . F6 F 0.3228(5) 1.2813(2) -0.0363(2) 0.0571(11) Uani 1 1 d . . . F7 F 0.1967(4) 1.45152(19) 0.1674(2) 0.0537(10) Uani 1 1 d . . . F8 F 0.2036(5) 1.2347(2) 0.3488(2) 0.0605(11) Uani 1 1 d . . . F9 F 0.3191(6) 1.0630(2) 0.1416(2) 0.0693(13) Uani 1 1 d . . . C1 C 0.6606(7) 0.8987(3) 0.4256(4) 0.0438(15) Uani 1 1 d . . . H1 H 0.5752 0.8728 0.4403 0.053 Uiso 1 1 calc R . . C2 C 0.6245(8) 0.9612(3) 0.3771(5) 0.059(2) Uani 1 1 d . . . H2A H 0.7088 0.9837 0.3585 0.089 Uiso 1 1 calc R . . H2B H 0.5657 0.9964 0.4029 0.089 Uiso 1 1 calc R . . H2C H 0.5753 0.9440 0.3384 0.089 Uiso 1 1 calc R . . C3 C 0.7281(8) 0.9213(4) 0.4914(4) 0.0542(18) Uani 1 1 d . . . H3A H 0.7657 0.8786 0.5159 0.081 Uiso 1 1 calc R . . H3B H 0.6591 0.9460 0.5225 0.081 Uiso 1 1 calc R . . H3C H 0.8023 0.9538 0.4777 0.081 Uiso 1 1 calc R . . C4 C 1.0440(8) 0.9052(3) 0.2182(3) 0.0458(16) Uani 1 1 d . . . H4 H 1.0605 0.9474 0.2468 0.055 Uiso 1 1 calc R . . C5 C 0.9400(10) 0.9288(4) 0.1657(5) 0.070(2) Uani 1 1 d . . . H5A H 0.9198 0.8878 0.1381 0.105 Uiso 1 1 calc R . . H5B H 0.9777 0.9670 0.1346 0.105 Uiso 1 1 calc R . . H5C H 0.8553 0.9468 0.1907 0.105 Uiso 1 1 calc R . . C6 C 1.1812(9) 0.8798(5) 0.1833(5) 0.077(3) Uani 1 1 d . . . H6A H 1.2347 0.8526 0.2175 0.116 Uiso 1 1 calc R . . H6B H 1.2321 0.9215 0.1652 0.116 Uiso 1 1 calc R . . H6C H 1.1651 0.8490 0.1445 0.116 Uiso 1 1 calc R . . C7 C 1.1372(7) 0.8780(3) 0.4648(4) 0.0479(17) Uani 1 1 d . . . H7 H 1.0932 0.9273 0.4615 0.057 Uiso 1 1 calc R . . C8 C 1.2848(8) 0.8819(4) 0.4400(5) 0.059(2) Uani 1 1 d . . . H8A H 1.3303 0.8343 0.4450 0.088 Uiso 1 1 calc R . . H8B H 1.3295 0.9160 0.4680 0.088 Uiso 1 1 calc R . . H8C H 1.2917 0.8981 0.3907 0.088 Uiso 1 1 calc R . . C9 C 1.1194(9) 0.8502(5) 0.5399(4) 0.071(2) Uani 1 1 d . . . H9A H 1.0216 0.8521 0.5553 0.106 Uiso 1 1 calc R . . H9B H 1.1696 0.8800 0.5698 0.106 Uiso 1 1 calc R . . H9C H 1.1553 0.8004 0.5433 0.106 Uiso 1 1 calc R . . C10 C 0.6952(7) 0.6186(3) 0.4344(4) 0.0464(16) Uani 1 1 d . . . H10 H 0.6026 0.6422 0.4450 0.056 Uiso 1 1 calc R . . C11 C 0.7523(9) 0.5940(4) 0.5038(4) 0.0552(18) Uani 1 1 d . . . H11A H 0.8437 0.5709 0.4950 0.083 Uiso 1 1 calc R . . H11B H 0.6909 0.5595 0.5280 0.083 Uiso 1 1 calc R . . H11C H 0.7593 0.6356 0.5330 0.083 Uiso 1 1 calc R . . C12 C 0.6770(8) 0.5568(3) 0.3867(4) 0.0538(18) Uani 1 1 d . . . H12A H 0.6255 0.5743 0.3469 0.081 Uiso 1 1 calc R . . H12B H 0.6264 0.5191 0.4128 0.081 Uiso 1 1 calc R . . H12C H 0.7674 0.5373 0.3697 0.081 Uiso 1 1 calc R . . C13 C 1.0589(8) 0.6100(3) 0.2309(3) 0.0453(16) Uani 1 1 d . . . H13 H 1.0929 0.5708 0.2631 0.054 Uiso 1 1 calc R . . C14 C 0.9421(9) 0.5823(4) 0.1944(4) 0.0567(19) Uani 1 1 d . . . H14A H 0.8711 0.5658 0.2292 0.085 Uiso 1 1 calc R . . H14B H 0.9755 0.5422 0.1655 0.085 Uiso 1 1 calc R . . H14C H 0.9032 0.6208 0.1646 0.085 Uiso 1 1 calc R . . C15 C 1.1771(8) 0.6325(4) 0.1831(4) 0.058(2) Uani 1 1 d . . . H15A H 1.1463 0.6710 0.1510 0.087 Uiso 1 1 calc R . . H15B H 1.2135 0.5914 0.1563 0.087 Uiso 1 1 calc R . . H15C H 1.2492 0.6499 0.2107 0.087 Uiso 1 1 calc R . . C16 C 1.2137(8) 0.6662(4) 0.4543(4) 0.0549(18) Uani 1 1 d . . . H16 H 1.2738 0.7046 0.4685 0.066 Uiso 1 1 calc R . . C17 C 1.1661(10) 0.6251(5) 0.5197(5) 0.074(3) Uani 1 1 d . . . H17A H 1.1124 0.6574 0.5512 0.111 Uiso 1 1 calc R . . H17B H 1.2460 0.6049 0.5431 0.111 Uiso 1 1 calc R . . H17C H 1.1088 0.5860 0.5075 0.111 Uiso 1 1 calc R . . C18 C 1.2972(9) 0.6214(4) 0.4017(5) 0.072(2) Uani 1 1 d . . . H18A H 1.2399 0.5845 0.3851 0.107 Uiso 1 1 calc R . . H18B H 1.3762 0.5984 0.4238 0.107 Uiso 1 1 calc R . . H18C H 1.3296 0.6523 0.3621 0.107 Uiso 1 1 calc R . . C19 C 0.6411(7) 0.7576(3) 0.2104(4) 0.0463(16) Uani 1 1 d . . . H19 H 0.6920 0.7577 0.1634 0.056 Uiso 1 1 calc R . . C20 C 0.5553(9) 0.8265(4) 0.2154(4) 0.065(2) Uani 1 1 d . . . H20A H 0.5042 0.8277 0.2612 0.098 Uiso 1 1 calc R . . H20B H 0.4905 0.8292 0.1784 0.098 Uiso 1 1 calc R . . H20C H 0.6153 0.8674 0.2100 0.098 Uiso 1 1 calc R . . C21 C 0.5658(9) 0.6897(4) 0.2192(4) 0.063(2) Uani 1 1 d . . . H21A H 0.6311 0.6486 0.2140 0.094 Uiso 1 1 calc R . . H21B H 0.4984 0.6887 0.1836 0.094 Uiso 1 1 calc R . . H21C H 0.5184 0.6873 0.2658 0.094 Uiso 1 1 calc R . . C22 C 0.6144(9) 1.3077(4) 0.0232(5) 0.065(2) Uani 1 1 d . . . H22 H 0.6928 1.3179 0.0519 0.078 Uiso 1 1 calc R . . C23 C 0.5745(9) 1.3759(4) -0.0191(4) 0.0572(19) Uani 1 1 d . . . H23A H 0.5135 1.3637 -0.0551 0.086 Uiso 1 1 calc R . . H23B H 0.6574 1.3969 -0.0413 0.086 Uiso 1 1 calc R . . H23C H 0.5268 1.4106 0.0122 0.086 Uiso 1 1 calc R . . C24 C 0.6593(14) 1.2471(5) -0.0268(7) 0.130(6) Uani 1 1 d . . . H24A H 0.7537 1.2304 -0.0186 0.195 Uiso 1 1 calc R . . H24B H 0.6552 1.2651 -0.0753 0.195 Uiso 1 1 calc R . . H24C H 0.5978 1.2070 -0.0184 0.195 Uiso 1 1 calc R . . C25 C 0.5175(8) 1.4252(4) 0.2057(4) 0.0564(19) Uani 1 1 d . . . H25 H 0.5931 1.4000 0.2309 0.068 Uiso 1 1 calc R . . C26 C 0.4321(9) 1.4698(4) 0.2593(5) 0.069(2) Uani 1 1 d . . . H26A H 0.3620 1.4990 0.2356 0.104 Uiso 1 1 calc R . . H26B H 0.4921 1.5014 0.2820 0.104 Uiso 1 1 calc R . . H26C H 0.3874 1.4377 0.2946 0.104 Uiso 1 1 calc R . . C27 C 0.5838(15) 1.4695(6) 0.1472(5) 0.113(5) Uani 1 1 d . . . H27A H 0.6530 1.4398 0.1209 0.170 Uiso 1 1 calc R . . H27B H 0.6279 1.5100 0.1664 0.170 Uiso 1 1 calc R . . H27C H 0.5138 1.4877 0.1159 0.170 Uiso 1 1 calc R . . C28 C 0.5349(8) 1.2430(4) 0.3257(4) 0.0504(17) Uani 1 1 d . . . H28 H 0.6317 1.2398 0.3051 0.060 Uiso 1 1 calc R . . C29 C 0.5202(12) 1.3064(5) 0.3711(5) 0.086(3) Uani 1 1 d . . . H29A H 0.5391 1.3502 0.3428 0.129 Uiso 1 1 calc R . . H29B H 0.5855 1.3009 0.4078 0.129 Uiso 1 1 calc R . . H29C H 0.4264 1.3100 0.3926 0.129 Uiso 1 1 calc R . . C30 C 0.5069(12) 1.1743(5) 0.3661(6) 0.088(3) Uani 1 1 d . . . H30A H 0.4186 1.1794 0.3933 0.132 Uiso 1 1 calc R . . H30B H 0.5802 1.1635 0.3978 0.132 Uiso 1 1 calc R . . H30C H 0.5035 1.1352 0.3335 0.132 Uiso 1 1 calc R . . C31 C 0.6243(10) 1.1205(4) 0.1659(6) 0.075(4) Uani 0.50(2) 1 d P A . H31 H 0.7076 1.1403 0.1846 0.089 Uiso 0.50(2) 1 calc PR . . C32 C 0.570(3) 1.0403(10) 0.1993(11) 0.069(6) Uani 0.50(2) 1 d P . . H32A H 0.5243 1.0469 0.2459 0.104 Uiso 0.50(2) 1 calc PR A . H32B H 0.6489 1.0065 0.2029 0.104 Uiso 0.50(2) 1 calc PR . . H32C H 0.5050 1.0213 0.1685 0.104 Uiso 0.50(2) 1 calc PR . . C33 C 0.641(3) 1.0838(11) 0.0885(11) 0.087(9) Uani 0.50(2) 1 d P . . H33A H 0.5790 1.0438 0.0880 0.130 Uiso 0.50(2) 1 calc PR A . H33B H 0.7360 1.0660 0.0793 0.130 Uiso 0.50(2) 1 calc PR . . H33C H 0.6174 1.1199 0.0523 0.130 Uiso 0.50(2) 1 calc PR . . C31A C 0.6243(10) 1.1205(4) 0.1659(6) 0.075(4) Uani 0.50 1 d P A 2 H31A H 0.6780 1.1566 0.1888 0.089 Uiso 0.50(2) 1 calc PR A 2 C32A C 0.629(3) 1.0735(12) 0.2174(13) 0.085(9) Uani 0.50(2) 1 d P A 2 H32D H 0.7222 1.0521 0.2185 0.127 Uiso 0.50(2) 1 calc PR A 2 H32E H 0.5642 1.0359 0.2110 0.127 Uiso 0.50(2) 1 calc PR A 2 H32F H 0.6040 1.0971 0.2615 0.127 Uiso 0.50(2) 1 calc PR A 2 C33A C 0.715(2) 1.1145(10) 0.1091(10) 0.061(6) Uani 0.50(2) 1 d P A 2 H33D H 0.8077 1.1049 0.1246 0.092 Uiso 0.50(2) 1 calc PR A 2 H33E H 0.7125 1.1594 0.0809 0.092 Uiso 0.50(2) 1 calc PR A 2 H33F H 0.6895 1.0749 0.0809 0.092 Uiso 0.50(2) 1 calc PR A 2 C34 C 0.1149(8) 1.3923(4) 0.0374(4) 0.0568(19) Uani 1 1 d . . . H34 H 0.0600 1.4228 0.0717 0.068 Uiso 1 1 calc R . . C35 C 0.1910(9) 1.4420(4) -0.0121(4) 0.060(2) Uani 1 1 d . . . H35A H 0.2438 1.4143 -0.0479 0.090 Uiso 1 1 calc R . . H35B H 0.2538 1.4693 0.0136 0.090 Uiso 1 1 calc R . . H35C H 0.1256 1.4753 -0.0345 0.090 Uiso 1 1 calc R . . C36 C 0.0176(9) 1.3459(5) 0.0072(5) 0.067(2) Uani 1 1 d . . . H36A H 0.0677 1.3134 -0.0254 0.100 Uiso 1 1 calc R . . H36B H -0.0496 1.3757 -0.0178 0.100 Uiso 1 1 calc R . . H36C H -0.0303 1.3177 0.0448 0.100 Uiso 1 1 calc R . . C37 C 0.0419(9) 1.3542(5) 0.2849(4) 0.064(2) Uani 1 1 d . . . H37 H 0.0157 1.3149 0.3194 0.077 Uiso 1 1 calc R . . C38 C 0.0794(9) 1.4149(4) 0.3256(4) 0.058(2) Uani 1 1 d . . . H38A H 0.1527 1.3991 0.3559 0.087 Uiso 1 1 calc R . . H38B H -0.0012 1.4321 0.3544 0.087 Uiso 1 1 calc R . . H38C H 0.1116 1.4538 0.2937 0.087 Uiso 1 1 calc R . . C39 C -0.0739(11) 1.3664(6) 0.2400(6) 0.094(3) Uani 1 1 d . . . H39A H -0.0647 1.4124 0.2142 0.141 Uiso 1 1 calc R . . H39B H -0.1604 1.3672 0.2691 0.141 Uiso 1 1 calc R . . H39C H -0.0738 1.3276 0.2069 0.141 Uiso 1 1 calc R . . C40 C 0.1321(10) 1.1032(4) 0.2590(5) 0.069(2) Uani 1 1 d . A . H40 H 0.1309 1.0676 0.2212 0.083 Uiso 1 1 calc R . . C41 C 0.1979(9) 1.0637(4) 0.3184(4) 0.060(2) Uani 1 1 d . . . H41A H 0.2138 1.0975 0.3547 0.091 Uiso 1 1 calc R A . H41B H 0.2858 1.0413 0.3014 0.091 Uiso 1 1 calc R . . H41C H 0.1371 1.0265 0.3381 0.091 Uiso 1 1 calc R . . C42 C -0.0095(10) 1.1291(6) 0.2713(6) 0.086(3) Uani 1 1 d . . . H42A H -0.0151 1.1644 0.3082 0.128 Uiso 1 1 calc R A . H42B H -0.0671 1.0887 0.2858 0.128 Uiso 1 1 calc R . . H42C H -0.0418 1.1518 0.2281 0.128 Uiso 1 1 calc R . . C43 C 0.2131(10) 1.1415(4) 0.0079(4) 0.066(2) Uani 1 1 d . A . H43 H 0.1829 1.1767 -0.0292 0.079 Uiso 1 1 calc R . . C44 C 0.0922(11) 1.1039(6) 0.0371(5) 0.084(3) Uani 1 1 d . . . H44A H 0.1212 1.0651 0.0694 0.127 Uiso 1 1 calc R A . H44B H 0.0453 1.0838 -0.0009 0.127 Uiso 1 1 calc R . . H44C H 0.0294 1.1378 0.0623 0.127 Uiso 1 1 calc R . . C45 C 0.3278(11) 1.0939(5) -0.0237(5) 0.076(3) Uani 1 1 d . . . H45A H 0.3586 1.0589 0.0118 0.113 Uiso 1 1 calc R A . H45B H 0.4047 1.1234 -0.0407 0.113 Uiso 1 1 calc R . . H45C H 0.2946 1.0686 -0.0628 0.113 Uiso 1 1 calc R . . 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 0.0392(12) 0.0307(8) 0.0454(10) -0.0064(7) 0.0024(8) -0.0010(7) Al2 0.0397(12) 0.0308(8) 0.0428(10) -0.0060(7) 0.0013(8) 0.0012(7) Al3 0.0387(12) 0.0304(8) 0.0485(11) -0.0073(7) 0.0011(9) 0.0003(7) Al4 0.0436(12) 0.0311(8) 0.0416(10) -0.0057(7) 0.0001(8) 0.0016(7) Al5 0.0423(13) 0.0384(9) 0.0496(11) -0.0004(8) -0.0011(9) -0.0004(8) Al6 0.0525(14) 0.0418(10) 0.0406(10) -0.0050(8) 0.0001(9) -0.0025(8) Al7 0.0474(13) 0.0333(9) 0.0460(11) -0.0040(8) -0.0022(9) 0.0004(8) Al8 0.0439(13) 0.0465(11) 0.0491(11) 0.0004(8) 0.0003(9) -0.0019(8) Al9 0.0591(15) 0.0356(10) 0.0556(12) -0.0028(8) -0.0021(11) -0.0043(9) O1 0.039(3) 0.0277(18) 0.037(2) -0.0057(15) 0.0041(18) 0.0015(16) O2 0.047(3) 0.031(2) 0.050(3) -0.0102(17) 0.004(2) 0.0039(17) O3 0.051(3) 0.032(2) 0.044(2) -0.0021(17) 0.009(2) -0.0024(18) O4 0.044(3) 0.035(2) 0.052(3) -0.0123(18) -0.002(2) -0.0006(18) O5 0.043(3) 0.0292(19) 0.054(3) -0.0072(18) 0.001(2) -0.0008(17) O6 0.045(3) 0.032(2) 0.043(2) -0.0085(17) 0.005(2) 0.0033(17) O7 0.037(3) 0.038(2) 0.045(2) -0.0019(18) -0.003(2) 0.0030(17) O8 0.042(3) 0.034(2) 0.042(2) -0.0055(17) -0.008(2) 0.0013(17) O9 0.037(3) 0.038(2) 0.038(2) -0.0018(16) 0.0013(19) -0.0011(17) O10 0.046(3) 0.050(3) 0.050(3) 0.003(2) 0.009(2) -0.003(2) O11 0.050(3) 0.035(2) 0.052(3) -0.0015(18) -0.005(2) -0.0077(18) O12 0.046(3) 0.044(2) 0.048(3) 0.0001(19) -0.011(2) -0.0004(19) O13 0.040(3) 0.045(2) 0.052(3) -0.0019(19) -0.002(2) 0.0095(19) O14 0.054(3) 0.038(2) 0.045(2) 0.0021(18) -0.009(2) 0.0028(19) O15 0.042(3) 0.052(3) 0.044(2) -0.0083(19) -0.001(2) 0.005(2) O16 0.057(3) 0.043(2) 0.059(3) 0.008(2) -0.002(2) -0.010(2) O17 0.060(3) 0.048(3) 0.050(3) -0.016(2) -0.009(2) -0.006(2) F1 0.049(2) 0.0344(17) 0.054(2) -0.0072(15) 0.0040(18) -0.0029(15) F2 0.045(2) 0.0365(17) 0.047(2) -0.0046(14) 0.0065(17) 0.0031(15) F3 0.033(2) 0.0394(18) 0.062(2) -0.0081(16) 0.0013(17) 0.0006(14) F4 0.058(3) 0.0417(19) 0.042(2) -0.0058(15) -0.0011(18) 0.0020(16) F5 0.042(3) 0.059(2) 0.061(3) 0.0070(19) -0.004(2) 0.0016(18) F6 0.070(3) 0.063(2) 0.038(2) -0.0008(17) 0.0018(19) -0.006(2) F7 0.064(3) 0.0388(19) 0.059(2) -0.0052(17) -0.007(2) 0.0068(17) F8 0.057(3) 0.077(3) 0.046(2) 0.0080(19) 0.002(2) 0.001(2) F9 0.103(4) 0.040(2) 0.066(3) 0.0009(19) -0.012(3) -0.005(2) C1 0.041(4) 0.030(3) 0.060(4) -0.011(3) 0.005(3) 0.004(2) C2 0.053(5) 0.036(3) 0.087(6) -0.009(3) 0.005(4) 0.009(3) C3 0.059(5) 0.046(4) 0.056(4) -0.017(3) 0.008(4) 0.001(3) C4 0.055(5) 0.037(3) 0.045(4) 0.000(3) 0.005(3) -0.007(3) C5 0.078(7) 0.055(4) 0.076(6) 0.021(4) -0.012(5) 0.007(4) C6 0.056(6) 0.068(5) 0.100(7) 0.023(5) 0.026(5) 0.009(4) C7 0.036(4) 0.040(3) 0.069(5) -0.017(3) -0.005(3) -0.002(3) C8 0.051(5) 0.046(4) 0.081(6) -0.013(4) -0.012(4) 0.002(3) C9 0.060(6) 0.106(7) 0.049(4) -0.025(4) -0.007(4) -0.007(5) C10 0.045(4) 0.035(3) 0.059(4) -0.002(3) -0.001(3) 0.002(3) C11 0.060(5) 0.047(4) 0.058(4) 0.004(3) 0.002(4) -0.004(3) C12 0.053(5) 0.040(3) 0.069(5) -0.004(3) -0.005(4) -0.008(3) C13 0.065(5) 0.027(3) 0.043(3) -0.010(2) 0.003(3) 0.008(3) C14 0.069(6) 0.038(3) 0.063(5) -0.014(3) 0.001(4) 0.001(3) C15 0.055(5) 0.042(4) 0.071(5) -0.005(3) 0.030(4) 0.009(3) C16 0.046(5) 0.048(4) 0.071(5) 0.002(3) -0.012(4) 0.000(3) C17 0.080(7) 0.071(5) 0.073(6) 0.018(4) -0.038(5) -0.016(4) C18 0.045(5) 0.060(5) 0.109(7) -0.011(5) -0.004(5) 0.012(4) C19 0.042(4) 0.053(4) 0.045(4) -0.007(3) -0.009(3) -0.001(3) C20 0.061(6) 0.079(5) 0.054(5) 0.002(4) -0.007(4) 0.014(4) C21 0.064(6) 0.077(5) 0.050(4) -0.005(4) -0.012(4) -0.019(4) C22 0.053(6) 0.066(5) 0.072(5) 0.009(4) 0.010(4) 0.005(4) C23 0.059(5) 0.059(4) 0.052(4) -0.004(3) 0.015(4) -0.008(3) C24 0.152(12) 0.076(6) 0.139(10) 0.036(6) 0.111(9) 0.050(7) C25 0.051(5) 0.051(4) 0.068(5) -0.008(3) -0.005(4) -0.015(3) C26 0.066(6) 0.059(5) 0.085(6) -0.028(4) -0.014(5) -0.002(4) C27 0.191(14) 0.083(7) 0.072(6) -0.004(5) -0.003(7) -0.087(8) C28 0.051(5) 0.055(4) 0.046(4) 0.002(3) -0.014(3) -0.002(3) C29 0.126(9) 0.074(6) 0.061(5) -0.013(4) -0.032(6) 0.013(5) C30 0.096(8) 0.082(6) 0.092(7) 0.019(5) -0.049(6) -0.012(5) C31 0.062(6) 0.045(4) 0.116(9) -0.024(5) -0.003(5) 0.016(4) C32 0.109(18) 0.036(9) 0.060(11) 0.000(7) 0.010(10) 0.004(9) C33 0.12(2) 0.057(11) 0.073(13) -0.011(9) 0.026(13) 0.027(12) C31A 0.062(6) 0.045(4) 0.116(9) -0.024(5) -0.003(5) 0.016(4) C32A 0.097(19) 0.056(13) 0.094(16) 0.011(11) 0.022(13) 0.047(13) C33A 0.057(13) 0.048(10) 0.077(12) 0.004(8) -0.002(9) 0.012(8) C34 0.058(5) 0.055(4) 0.057(4) 0.005(3) -0.013(4) 0.007(3) C35 0.070(6) 0.046(4) 0.066(5) 0.011(3) -0.021(4) -0.005(3) C36 0.065(6) 0.076(5) 0.060(5) 0.008(4) -0.013(4) -0.004(4) C37 0.057(6) 0.075(5) 0.060(5) -0.022(4) 0.007(4) 0.013(4) C38 0.073(6) 0.049(4) 0.051(4) -0.003(3) 0.009(4) 0.008(3) C39 0.055(7) 0.122(9) 0.104(8) -0.028(7) 0.010(6) 0.011(6) C40 0.073(7) 0.056(4) 0.077(6) 0.021(4) -0.010(5) -0.016(4) C41 0.078(6) 0.047(4) 0.058(4) 0.003(3) -0.008(4) -0.022(4) C42 0.055(7) 0.117(8) 0.084(7) 0.027(6) -0.009(5) -0.021(5) C43 0.081(7) 0.058(4) 0.061(5) -0.017(4) -0.010(4) -0.020(4) C44 0.097(8) 0.097(7) 0.062(5) -0.002(5) 0.000(5) -0.041(6) C45 0.101(8) 0.070(5) 0.059(5) -0.028(4) -0.013(5) -0.001(5) _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 F1 1.695(4) . ? Al1 O4 1.803(5) . ? Al1 O1 1.852(4) . ? Al1 O3 1.863(5) . ? Al1 O2 1.862(5) . ? Al1 Al3 2.870(3) . ? Al1 Al4 2.878(2) . ? Al2 F2 1.682(4) . ? Al2 O7 1.821(5) . ? Al2 O1 1.860(4) . ? Al2 O6 1.866(5) . ? Al2 O5 1.867(5) . ? Al2 Al4 2.877(3) . ? Al2 Al3 2.884(3) . ? Al3 F3 1.676(4) . ? Al3 O2 1.837(4) . ? Al3 O8 1.841(5) . ? Al3 O5 1.843(4) . ? Al3 O1 1.876(5) . ? Al3 Al4 2.846(3) . ? Al4 F4 1.680(4) . ? Al4 O8 1.834(5) . ? Al4 O6 1.844(4) . ? Al4 O3 1.852(4) . ? Al4 O1 1.881(4) . ? Al5 F5 1.684(5) . ? Al5 O9 1.863(5) . ? Al5 O13 1.935(5) . ? Al5 O10 1.947(5) . ? Al5 O11 1.950(5) . ? Al5 O12 1.956(5) . ? Al5 Al9 2.928(3) . ? Al5 Al7 2.939(3) . ? Al5 Al8 2.946(3) . ? Al5 Al6 2.963(3) . ? Al6 F6 1.679(4) . ? Al6 O17 1.795(5) . ? Al6 O10 1.797(6) . ? Al6 O14 1.801(5) . ? Al6 O9 2.069(5) . ? Al6 Al7 2.872(3) . ? Al6 Al9 2.883(3) . ? Al7 F7 1.686(4) . ? Al7 O11 1.801(5) . ? Al7 O15 1.818(5) . ? Al7 O14 1.818(5) . ? Al7 O9 2.027(4) . ? Al7 Al8 2.887(3) . ? Al8 F8 1.673(5) . ? Al8 O12 1.798(5) . ? Al8 O16 1.807(5) . ? Al8 O15 1.821(5) . ? Al8 O9 2.085(5) . ? Al8 Al9 2.885(3) . ? Al9 F9 1.676(4) . ? Al9 O13 1.807(5) . ? Al9 O16 1.815(6) . ? Al9 O17 1.817(5) . ? Al9 O9 2.037(4) . ? O2 C1 1.464(7) . ? O3 C4 1.435(8) . ? O4 C7 1.431(7) . ? O5 C10 1.444(8) . ? O6 C13 1.460(6) . ? O7 C16 1.445(8) . ? O8 C19 1.489(8) . ? O10 C22 1.438(10) . ? O11 C25 1.451(8) . ? O12 C28 1.474(8) . ? O13 C31 1.445(9) . ? O14 C34 1.477(8) . ? O15 C37 1.469(9) . ? O16 C40 1.462(9) . ? O17 C43 1.495(8) . ? C1 C2 1.508(10) . ? C1 C3 1.543(10) . ? C4 C5 1.516(11) . ? C4 C6 1.522(11) . ? C7 C8 1.491(11) . ? C7 C9 1.514(11) . ? C10 C12 1.519(9) . ? C10 C11 1.524(10) . ? C13 C15 1.490(10) . ? C13 C14 1.496(10) . ? C16 C17 1.503(12) . ? C16 C18 1.507(11) . ? C19 C21 1.487(10) . ? C19 C20 1.507(10) . ? C22 C23 1.532(11) . ? C22 C24 1.540(13) . ? C25 C27 1.496(12) . ? C25 C26 1.527(11) . ? C28 C29 1.492(11) . ? C28 C30 1.496(11) . ? C31 C33 1.65(2) . ? C31 C32 1.70(2) . ? C34 C36 1.470(11) . ? C34 C35 1.487(11) . ? C37 C38 1.469(10) . ? C37 C39 1.471(13) . ? C40 C42 1.452(13) . ? C40 C41 1.500(11) . ? C43 C44 1.466(12) . ? C43 C45 1.508(12) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag F1 Al1 O4 99.8(2) . . ? F1 Al1 O1 171.0(2) . . ? O4 Al1 O1 89.17(19) . . ? F1 Al1 O3 97.0(2) . . ? O4 Al1 O3 118.7(2) . . ? O1 Al1 O3 78.01(18) . . ? F1 Al1 O2 98.01(19) . . ? O4 Al1 O2 118.4(2) . . ? O1 Al1 O2 77.99(18) . . ? O3 Al1 O2 116.9(2) . . ? F1 Al1 Al3 134.34(16) . . ? O4 Al1 Al3 113.04(17) . . ? O1 Al1 Al3 39.99(14) . . ? O3 Al1 Al3 94.17(16) . . ? O2 Al1 Al3 38.80(12) . . ? F1 Al1 Al4 133.44(16) . . ? O4 Al1 Al4 113.84(15) . . ? O1 Al1 Al4 39.93(13) . . ? O3 Al1 Al4 39.09(13) . . ? O2 Al1 Al4 93.41(14) . . ? Al3 Al1 Al4 59.37(7) . . ? F2 Al2 O7 99.3(2) . . ? F2 Al2 O1 172.8(2) . . ? O7 Al2 O1 87.94(19) . . ? F2 Al2 O6 98.77(18) . . ? O7 Al2 O6 116.3(2) . . ? O1 Al2 O6 78.30(18) . . ? F2 Al2 O5 98.1(2) . . ? O7 Al2 O5 121.8(2) . . ? O1 Al2 O5 77.48(19) . . ? O6 Al2 O5 115.1(2) . . ? F2 Al2 Al4 135.85(15) . . ? O7 Al2 Al4 110.28(16) . . ? O1 Al2 Al4 40.01(13) . . ? O6 Al2 Al4 38.89(13) . . ? O5 Al2 Al4 93.45(16) . . ? F2 Al2 Al3 134.73(16) . . ? O7 Al2 Al3 114.31(15) . . ? O1 Al2 Al3 39.70(14) . . ? O6 Al2 Al3 92.81(15) . . ? O5 Al2 Al3 38.69(13) . . ? Al4 Al2 Al3 59.22(7) . . ? F3 Al3 O2 100.3(2) . . ? F3 Al3 O8 105.5(2) . . ? O2 Al3 O8 109.1(2) . . ? F3 Al3 O5 99.7(2) . . ? O2 Al3 O5 128.8(2) . . ? O8 Al3 O5 110.03(19) . . ? F3 Al3 O1 174.5(2) . . ? O2 Al3 O1 78.00(19) . . ? O8 Al3 O1 80.0(2) . . ? O5 Al3 O1 77.7(2) . . ? F3 Al3 Al4 144.61(17) . . ? O2 Al3 Al4 95.02(16) . . ? O8 Al3 Al4 39.14(15) . . ? O5 Al3 Al4 94.97(16) . . ? O1 Al3 Al4 40.82(13) . . ? F3 Al3 Al1 139.62(14) . . ? O2 Al3 Al1 39.44(15) . . ? O8 Al3 Al1 90.02(16) . . ? O5 Al3 Al1 109.72(16) . . ? O1 Al3 Al1 39.36(12) . . ? Al4 Al3 Al1 60.47(7) . . ? F3 Al3 Al2 138.76(15) . . ? O2 Al3 Al2 110.26(17) . . ? O8 Al3 Al2 90.25(15) . . ? O5 Al3 Al2 39.29(15) . . ? O1 Al3 Al2 39.29(12) . . ? Al4 Al3 Al2 60.28(7) . . ? Al1 Al3 Al2 76.37(7) . . ? F4 Al4 O8 103.2(2) . . ? F4 Al4 O6 101.35(19) . . ? O8 Al4 O6 108.7(2) . . ? F4 Al4 O3 100.4(2) . . ? O8 Al4 O3 109.9(2) . . ? O6 Al4 O3 129.4(2) . . ? F4 Al4 O1 176.7(2) . . ? O8 Al4 O1 80.0(2) . . ? O6 Al4 O1 78.31(18) . . ? O3 Al4 O1 77.52(19) . . ? F4 Al4 Al3 142.47(18) . . ? O8 Al4 Al3 39.32(14) . . ? O6 Al4 Al3 94.49(16) . . ? O3 Al4 Al3 95.16(16) . . ? O1 Al4 Al3 40.69(14) . . ? F4 Al4 Al2 140.57(15) . . ? O8 Al4 Al2 90.58(15) . . ? O6 Al4 Al2 39.44(14) . . ? O3 Al4 Al2 109.42(16) . . ? O1 Al4 Al2 39.47(12) . . ? Al3 Al4 Al2 60.50(7) . . ? F4 Al4 Al1 139.17(15) . . ? O8 Al4 Al1 89.89(14) . . ? O6 Al4 Al1 110.86(15) . . ? O3 Al4 Al1 39.34(14) . . ? O1 Al4 Al1 39.18(12) . . ? Al3 Al4 Al1 60.17(6) . . ? Al2 Al4 Al1 76.34(7) . . ? F5 Al5 O9 179.4(2) . . ? F5 Al5 O13 99.5(2) . . ? O9 Al5 O13 80.60(19) . . ? F5 Al5 O10 99.6(2) . . ? O9 Al5 O10 79.7(2) . . ? O13 Al5 O10 89.6(2) . . ? F5 Al5 O11 100.3(2) . . ? O9 Al5 O11 79.7(2) . . ? O13 Al5 O11 160.2(2) . . ? O10 Al5 O11 87.9(2) . . ? F5 Al5 O12 99.6(2) . . ? O9 Al5 O12 81.1(2) . . ? O13 Al5 O12 87.8(2) . . ? O10 Al5 O12 160.8(2) . . ? O11 Al5 O12 88.1(2) . . ? F5 Al5 Al9 136.45(17) . . ? O9 Al5 Al9 43.63(13) . . ? O13 Al5 Al9 36.98(15) . . ? O10 Al5 Al9 83.94(16) . . ? O11 Al5 Al9 123.27(17) . . ? O12 Al5 Al9 82.55(15) . . ? F5 Al5 Al7 136.86(16) . . ? O9 Al5 Al7 43.05(13) . . ? O13 Al5 Al7 123.65(17) . . ? O10 Al5 Al7 81.34(16) . . ? O11 Al5 Al7 36.63(15) . . ? O12 Al5 Al7 84.32(15) . . ? Al9 Al5 Al7 86.68(8) . . ? F5 Al5 Al8 135.96(18) . . ? O9 Al5 Al8 44.68(14) . . ? O13 Al5 Al8 83.59(16) . . ? O10 Al5 Al8 124.39(18) . . ? O11 Al5 Al8 81.70(16) . . ? O12 Al5 Al8 36.41(15) . . ? Al9 Al5 Al8 58.83(7) . . ? Al7 Al5 Al8 58.75(7) . . ? F5 Al5 Al6 135.55(18) . . ? O9 Al5 Al6 43.81(14) . . ? O13 Al5 Al6 82.84(15) . . ? O10 Al5 Al6 35.96(16) . . ? O11 Al5 Al6 83.65(15) . . ? O12 Al5 Al6 124.88(17) . . ? Al9 Al5 Al6 58.59(7) . . ? Al7 Al5 Al6 58.23(7) . . ? Al8 Al5 Al6 88.49(8) . . ? F6 Al6 O17 99.9(2) . . ? F6 Al6 O10 104.4(2) . . ? O17 Al6 O10 114.7(2) . . ? F6 Al6 O14 101.2(2) . . ? O17 Al6 O14 120.4(3) . . ? O10 Al6 O14 112.6(2) . . ? F6 Al6 O9 177.4(2) . . ? O17 Al6 O9 78.3(2) . . ? O10 Al6 O9 78.0(2) . . ? O14 Al6 O9 78.30(19) . . ? F6 Al6 Al7 135.48(17) . . ? O17 Al6 Al7 115.08(19) . . ? O10 Al6 Al7 85.72(17) . . ? O14 Al6 Al7 37.69(15) . . ? O9 Al6 Al7 44.88(12) . . ? F6 Al6 Al9 133.95(17) . . ? O17 Al6 Al9 37.31(16) . . ? O10 Al6 Al9 87.90(17) . . ? O14 Al6 Al9 114.76(18) . . ? O9 Al6 Al9 44.94(12) . . ? Al7 Al6 Al9 88.82(8) . . ? F6 Al6 Al5 143.9(2) . . ? O17 Al6 Al5 96.66(17) . . ? O10 Al6 Al5 39.50(16) . . ? O14 Al6 Al5 97.58(16) . . ? O9 Al6 Al5 38.56(13) . . ? Al7 Al6 Al5 60.47(7) . . ? Al9 Al6 Al5 60.10(7) . . ? F7 Al7 O11 104.3(2) . . ? F7 Al7 O15 101.3(2) . . ? O11 Al7 O15 111.9(2) . . ? F7 Al7 O14 97.2(2) . . ? O11 Al7 O14 115.9(2) . . ? O15 Al7 O14 121.9(2) . . ? F7 Al7 O9 175.9(2) . . ? O11 Al7 O9 79.10(19) . . ? O15 Al7 O9 79.40(19) . . ? O14 Al7 O9 79.06(18) . . ? F7 Al7 Al6 130.95(17) . . ? O11 Al7 Al6 88.96(16) . . ? O15 Al7 Al6 117.28(16) . . ? O14 Al7 Al6 37.28(15) . . ? O9 Al7 Al6 46.10(13) . . ? F7 Al7 Al8 135.76(18) . . ? O11 Al7 Al8 85.85(16) . . ? O15 Al7 Al8 37.53(15) . . ? O14 Al7 Al8 117.13(16) . . ? O9 Al7 Al8 46.22(13) . . ? Al6 Al7 Al8 91.44(8) . . ? F7 Al7 Al5 144.36(18) . . ? O11 Al7 Al5 40.25(14) . . ? O15 Al7 Al5 97.65(16) . . ? O14 Al7 Al5 97.99(16) . . ? O9 Al7 Al5 38.88(13) . . ? Al6 Al7 Al5 61.30(7) . . ? Al8 Al7 Al5 60.75(7) . . ? F8 Al8 O12 104.5(2) . . ? F8 Al8 O16 101.8(2) . . ? O12 Al8 O16 112.2(2) . . ? F8 Al8 O15 98.9(2) . . ? O12 Al8 O15 115.8(2) . . ? O16 Al8 O15 120.0(2) . . ? F8 Al8 O9 176.0(2) . . ? O12 Al8 O9 79.2(2) . . ? O16 Al8 O9 78.1(2) . . ? O15 Al8 O9 77.8(2) . . ? F8 Al8 Al9 136.34(19) . . ? O12 Al8 Al9 86.47(17) . . ? O16 Al8 Al9 37.28(18) . . ? O15 Al8 Al9 114.30(17) . . ? O9 Al8 Al9 44.89(12) . . ? F8 Al8 Al7 133.03(18) . . ? O12 Al8 Al7 88.68(17) . . ? O16 Al8 Al7 114.58(18) . . ? O15 Al8 Al7 37.46(16) . . ? O9 Al8 Al7 44.58(12) . . ? Al9 Al8 Al7 88.48(8) . . ? F8 Al8 Al5 144.6(2) . . ? O12 Al8 Al5 40.24(16) . . ? O16 Al8 Al5 96.80(19) . . ? O15 Al8 Al5 97.33(18) . . ? O9 Al8 Al5 38.93(13) . . ? Al9 Al8 Al5 60.27(7) . . ? Al7 Al8 Al5 60.50(7) . . ? F9 Al9 O13 105.1(2) . . ? F9 Al9 O16 98.4(2) . . ? O13 Al9 O16 113.5(2) . . ? F9 Al9 O17 99.8(2) . . ? O13 Al9 O17 112.8(3) . . ? O16 Al9 O17 123.1(3) . . ? F9 Al9 O9 175.6(3) . . ? O13 Al9 O9 79.23(19) . . ? O16 Al9 O9 79.2(2) . . ? O17 Al9 O9 78.68(19) . . ? F9 Al9 Al6 133.96(19) . . ? O13 Al9 Al6 87.34(17) . . ? O16 Al9 Al6 117.24(17) . . ? O17 Al9 Al6 36.78(15) . . ? O9 Al9 Al6 45.87(13) . . ? F9 Al9 Al8 132.6(2) . . ? O13 Al9 Al8 87.59(16) . . ? O16 Al9 Al8 37.09(15) . . ? O17 Al9 Al8 117.21(17) . . ? O9 Al9 Al8 46.25(13) . . ? Al6 Al9 Al8 91.26(8) . . ? F9 Al9 Al5 145.2(2) . . ? O13 Al9 Al5 40.09(14) . . ? O16 Al9 Al5 97.24(17) . . ? O17 Al9 Al5 97.33(17) . . ? O9 Al9 Al5 39.14(13) . . ? Al6 Al9 Al5 61.31(7) . . ? Al8 Al9 Al5 60.90(7) . . ? Al1 O1 Al2 146.7(3) . . ? Al1 O1 Al3 100.65(19) . . ? Al2 O1 Al3 101.0(2) . . ? Al1 O1 Al4 100.9(2) . . ? Al2 O1 Al4 100.52(18) . . ? Al3 O1 Al4 98.5(2) . . ? C1 O2 Al3 127.1(4) . . ? C1 O2 Al1 131.1(4) . . ? Al3 O2 Al1 101.8(2) . . ? C4 O3 Al4 132.2(4) . . ? C4 O3 Al1 125.8(4) . . ? Al4 O3 Al1 101.6(2) . . ? C7 O4 Al1 127.7(4) . . ? C10 O5 Al3 126.7(4) . . ? C10 O5 Al2 130.8(4) . . ? Al3 O5 Al2 102.0(2) . . ? C13 O6 Al4 130.9(4) . . ? C13 O6 Al2 126.3(4) . . ? Al4 O6 Al2 101.68(19) . . ? C16 O7 Al2 131.1(4) . . ? C19 O8 Al4 126.7(4) . . ? C19 O8 Al3 131.7(4) . . ? Al4 O8 Al3 101.5(2) . . ? Al5 O9 Al7 98.07(19) . . ? Al5 O9 Al9 97.2(2) . . ? Al7 O9 Al9 164.7(3) . . ? Al5 O9 Al6 97.6(2) . . ? Al7 O9 Al6 89.03(17) . . ? Al9 O9 Al6 89.18(17) . . ? Al5 O9 Al8 96.4(2) . . ? Al7 O9 Al8 89.20(17) . . ? Al9 O9 Al8 88.86(18) . . ? Al6 O9 Al8 166.0(3) . . ? C22 O10 Al6 130.4(5) . . ? C22 O10 Al5 124.8(5) . . ? Al6 O10 Al5 104.5(2) . . ? C25 O11 Al7 132.6(4) . . ? C25 O11 Al5 122.7(4) . . ? Al7 O11 Al5 103.1(2) . . ? C28 O12 Al8 131.6(5) . . ? C28 O12 Al5 124.6(5) . . ? Al8 O12 Al5 103.3(2) . . ? C31 O13 Al9 132.8(5) . . ? C31 O13 Al5 123.9(5) . . ? Al9 O13 Al5 102.9(2) . . ? C34 O14 Al6 130.1(4) . . ? C34 O14 Al7 124.6(4) . . ? Al6 O14 Al7 105.0(2) . . ? C37 O15 Al7 131.1(5) . . ? C37 O15 Al8 123.6(5) . . ? Al7 O15 Al8 105.0(2) . . ? C40 O16 Al8 131.3(5) . . ? C40 O16 Al9 122.7(5) . . ? Al8 O16 Al9 105.6(3) . . ? C43 O17 Al6 122.8(5) . . ? C43 O17 Al9 130.3(5) . . ? Al6 O17 Al9 105.9(2) . . ? O2 C1 C2 108.9(6) . . ? O2 C1 C3 107.8(5) . . ? C2 C1 C3 113.2(5) . . ? O3 C4 C5 110.5(6) . . ? O3 C4 C6 109.6(6) . . ? C5 C4 C6 112.6(7) . . ? O4 C7 C8 109.9(6) . . ? O4 C7 C9 108.9(6) . . ? C8 C7 C9 112.1(7) . . ? O5 C10 C12 110.1(6) . . ? O5 C10 C11 110.5(6) . . ? C12 C10 C11 112.9(5) . . ? O6 C13 C15 110.2(5) . . ? O6 C13 C14 108.6(6) . . ? C15 C13 C14 114.2(6) . . ? O7 C16 C17 109.9(7) . . ? O7 C16 C18 110.5(6) . . ? C17 C16 C18 114.1(7) . . ? O8 C19 C21 108.1(6) . . ? O8 C19 C20 108.4(5) . . ? C21 C19 C20 116.5(7) . . ? O10 C22 C23 110.5(6) . . ? O10 C22 C24 109.3(7) . . ? C23 C22 C24 109.8(8) . . ? O11 C25 C27 110.7(6) . . ? O11 C25 C26 111.2(7) . . ? C27 C25 C26 113.4(8) . . ? O12 C28 C29 109.3(6) . . ? O12 C28 C30 111.0(6) . . ? C29 C28 C30 112.1(8) . . ? O13 C31 C33 101.9(11) . . ? O13 C31 C32 107.9(10) . . ? C33 C31 C32 87.7(12) . . ? C36 C34 O14 109.6(6) . . ? C36 C34 C35 116.7(7) . . ? O14 C34 C35 110.0(6) . . ? O15 C37 C38 110.0(7) . . ? O15 C37 C39 109.2(7) . . ? C38 C37 C39 117.2(7) . . ? C42 C40 O16 111.2(7) . . ? C42 C40 C41 117.3(8) . . ? O16 C40 C41 110.6(7) . . ? C44 C43 O17 108.8(7) . . ? C44 C43 C45 115.2(8) . . ? O17 C43 C45 108.1(7) . . ? _diffrn_measured_fraction_theta_max 0.916 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.916 _refine_diff_density_max 0.717 _refine_diff_density_min -0.694 _refine_diff_density_rms 0.102 # Attachment '- compound3.CIF' data_a2 _database_code_depnum_ccdc_archive 'CCDC 826058' #TrackingRef '- compound3.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C66 H150 Al16 F20 O26' _chemical_formula_weight 2171.54 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' Al Al 0.0645 0.0514 '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 10.7854(5) _cell_length_b 13.6679(6) _cell_length_c 20.0924(9) _cell_angle_alpha 96.679(4) _cell_angle_beta 100.678(4) _cell_angle_gamma 100.788(4) _cell_volume 2824.0(2) _cell_formula_units_Z 1 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 23065 _cell_measurement_theta_min 2 _cell_measurement_theta_max 29 _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.276 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1142 _exptl_absorpt_coefficient_mu 0.226 _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 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 IPDS(Stoe) _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 48389 _diffrn_reflns_av_R_equivalents 0.1033 _diffrn_reflns_av_sigmaI/netI 0.0884 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 2.38 _diffrn_reflns_theta_max 27.88 _reflns_number_total 13450 _reflns_number_gt 8182 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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 compound has crystallographically imposed inversion symmetry, with one HOiPr molecule in the asymmetric unit. Four carbon atoms, C10, C18, C26, and C27, were refined using the ISOR to prevent them from becoming non-positive-definite . ; _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^)+(0.0800P)^2^+1.0000P] 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 SHELXL _refine_ls_extinction_coef 0.0086(12) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 13439 _refine_ls_number_parameters 599 _refine_ls_number_restraints 24 _refine_ls_R_factor_all 0.1304 _refine_ls_R_factor_gt 0.0770 _refine_ls_wR_factor_ref 0.1912 _refine_ls_wR_factor_gt 0.1720 _refine_ls_goodness_of_fit_ref 1.083 _refine_ls_restrained_S_all 1.095 _refine_ls_shift/su_max 0.003 _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 0.23731(11) 0.74410(8) 0.17725(5) 0.0291(2) Uani 1 1 d . . . Al2 Al 0.30374(12) 0.74767(9) 0.04338(6) 0.0362(3) Uani 1 1 d . . . Al3 Al 0.06534(11) 0.60228(7) 0.01365(5) 0.0260(2) Uani 1 1 d . . . Al4 Al 0.07710(13) 0.80897(8) 0.06470(6) 0.0360(3) Uani 1 1 d . . . Al5 Al 0.17073(12) 0.57866(8) 0.25130(5) 0.0323(3) Uani 1 1 d . . . Al6 Al 0.16763(14) 0.66334(11) 0.38999(6) 0.0437(3) Uani 1 1 d . . . Al7 Al 0.38592(13) 0.59259(10) 0.36431(6) 0.0402(3) Uani 1 1 d . . . Al8 Al 0.36902(13) 0.79648(9) 0.34887(6) 0.0403(3) Uani 1 1 d . . . F1 F 0.1053(2) 0.68255(15) 0.21414(10) 0.0322(5) Uani 1 1 d . . . F2 F 0.2842(2) 0.62587(15) 0.19509(10) 0.0314(5) Uani 1 1 d . . . F3 F 0.3323(3) 0.82068(19) 0.26099(13) 0.0512(6) Uani 1 1 d . . . F4 F 0.4326(3) 0.77556(19) 0.00797(12) 0.0508(7) Uani 1 1 d . . . F5 F 0.0297(2) 0.49654(17) 0.05790(12) 0.0430(6) Uani 1 1 d . . . F6 F -0.0129(3) 0.89520(17) 0.05055(12) 0.0538(7) Uani 1 1 d . . . F7 F 0.0752(2) 0.48492(16) 0.18806(10) 0.0376(5) Uani 1 1 d . . . F8 F 0.0676(3) 0.6689(2) 0.44435(13) 0.0620(8) Uani 1 1 d . . . F9 F 0.4986(3) 0.5300(2) 0.39435(13) 0.0536(7) Uani 1 1 d . . . F10 F 0.4629(3) 0.91286(19) 0.38222(13) 0.0575(7) Uani 1 1 d . . . O1 O 0.1602(2) 0.70019(17) 0.08462(12) 0.0299(5) Uani 1 1 d . . . O2 O 0.3802(3) 0.77478(18) 0.13407(13) 0.0335(6) Uani 1 1 d . . . O3 O 0.1417(3) 0.84526(18) 0.15694(13) 0.0342(6) Uani 1 1 d . . . O4 O 0.2169(2) 0.62970(18) -0.01629(12) 0.0314(6) Uani 1 1 d . . . O5 O 0.2115(3) 0.84405(19) 0.02354(14) 0.0457(8) Uani 1 1 d . . . O6 O -0.0337(3) 0.69756(18) 0.00645(12) 0.0309(6) Uani 1 1 d . . . O7 O 0.2723(3) 0.66791(19) 0.32459(12) 0.0335(6) Uani 1 1 d . . . O8 O 0.0616(3) 0.5775(2) 0.31594(14) 0.0429(7) Uani 1 1 d . . . O9 O 0.2888(3) 0.50255(19) 0.28975(13) 0.0375(6) Uani 1 1 d . . . O10 O 0.2893(3) 0.5978(2) 0.42957(14) 0.0458(7) Uani 1 1 d . . . O11 O 0.2434(3) 0.8004(2) 0.40050(14) 0.0497(8) Uani 1 1 d . . . O12 O 0.4920(3) 0.7195(2) 0.37264(15) 0.0472(7) Uani 1 1 d . . . O13 O 0.4971(5) 0.0190(3) 0.2813(2) 0.0879(15) Uani 1 1 d . . . H13A H 0.5144 -0.0019 0.3190 0.132 Uiso 1 1 calc R . . C1 C 0.5144(4) 0.7841(3) 0.1665(2) 0.0389(9) Uani 1 1 d . . . H1 H 0.5211 0.7919 0.2172 0.047 Uiso 1 1 calc R . . C2 C 0.5962(4) 0.8776(3) 0.1507(3) 0.0487(11) Uani 1 1 d . . . H2A H 0.6037 0.8668 0.1027 0.073 Uiso 1 1 calc R . . H2B H 0.6824 0.8915 0.1806 0.073 Uiso 1 1 calc R . . H2C H 0.5556 0.9351 0.1587 0.073 Uiso 1 1 calc R . . C3 C 0.5588(5) 0.6894(3) 0.1448(3) 0.0509(11) Uani 1 1 d . . . H3A H 0.5020 0.6310 0.1553 0.076 Uiso 1 1 calc R . . H3B H 0.6476 0.6943 0.1696 0.076 Uiso 1 1 calc R . . H3C H 0.5558 0.6813 0.0953 0.076 Uiso 1 1 calc R . . C4 C 0.1023(4) 0.9123(3) 0.2063(2) 0.0390(9) Uani 1 1 d . . . H4 H 0.1493 0.9066 0.2530 0.047 Uiso 1 1 calc R . . C5 C -0.0404(5) 0.8789(4) 0.2032(3) 0.0514(11) Uani 1 1 d . . . H5A H -0.0890 0.8859 0.1583 0.077 Uiso 1 1 calc R . . H5B H -0.0651 0.9209 0.2393 0.077 Uiso 1 1 calc R . . H5C H -0.0596 0.8082 0.2099 0.077 Uiso 1 1 calc R . . C6 C 0.1408(6) 1.0204(3) 0.1953(3) 0.0584(13) Uani 1 1 d . . . C7 C 0.2507(4) 0.5829(3) -0.07722(19) 0.0342(8) Uani 1 1 d . . . H7 H 0.1805 0.5226 -0.0986 0.041 Uiso 1 1 calc R . . C8 C 0.2589(5) 0.6549(3) -0.1287(2) 0.0478(11) Uani 1 1 d . . . H8A H 0.1763 0.6756 -0.1402 0.072 Uiso 1 1 calc R . . H8B H 0.2780 0.6213 -0.1702 0.072 Uiso 1 1 calc R . . H8C H 0.3277 0.7144 -0.1089 0.072 Uiso 1 1 calc R . . C9 C 0.3741(5) 0.5471(4) -0.0570(3) 0.0566(12) Uani 1 1 d . . . H9A H 0.4449 0.6053 -0.0370 0.085 Uiso 1 1 calc R . . H9B H 0.3936 0.5112 -0.0976 0.085 Uiso 1 1 calc R . . H9C H 0.3642 0.5016 -0.0232 0.085 Uiso 1 1 calc R . . C10 C 0.2477(8) 0.9355(4) -0.0057(3) 0.092(2) Uani 1 1 d U . . H10 H 0.1706 0.9632 0.0012 0.111 Uiso 1 1 calc R . . C11 C 0.3391(4) 1.0120(3) 0.0422(2) 0.0445(10) Uani 1 1 d . . . H11A H 0.4226 0.9921 0.0509 0.067 Uiso 1 1 calc R . . H11B H 0.3091 1.0210 0.0852 0.067 Uiso 1 1 calc R . . H11C H 0.3485 1.0754 0.0235 0.067 Uiso 1 1 calc R . . C12 C 0.2179(7) 0.9242(4) -0.0749(3) 0.083(2) Uani 1 1 d . . . H12A H 0.2047 0.9882 -0.0892 0.124 Uiso 1 1 calc R . . H12B H 0.1387 0.8723 -0.0923 0.124 Uiso 1 1 calc R . . H12C H 0.2888 0.9037 -0.0933 0.124 Uiso 1 1 calc R . . C13 C -0.1540(4) 0.6945(3) -0.0413(2) 0.0347(8) Uani 1 1 d . . . H13 H -0.1870 0.6241 -0.0664 0.042 Uiso 1 1 calc R . . C14 C -0.1304(4) 0.7636(3) -0.0928(2) 0.0404(9) Uani 1 1 d . . . H14A H -0.0990 0.8332 -0.0691 0.061 Uiso 1 1 calc R . . H14B H -0.2112 0.7588 -0.1260 0.061 Uiso 1 1 calc R . . H14C H -0.0657 0.7439 -0.1169 0.061 Uiso 1 1 calc R . . C15 C -0.2528(5) 0.7207(4) -0.0013(3) 0.0586(13) Uani 1 1 d . . . H15A H -0.2572 0.6790 0.0350 0.088 Uiso 1 1 calc R . . H15B H -0.3377 0.7080 -0.0324 0.088 Uiso 1 1 calc R . . H15C H -0.2274 0.7921 0.0191 0.088 Uiso 1 1 calc R . . C16 C -0.0726(5) 0.5287(4) 0.3054(4) 0.079(2) Uani 1 1 d . . . H16 H -0.0773 0.5554 0.3532 0.095 Uiso 1 1 calc R . . C17 C -0.0908(7) 0.4274(5) 0.3187(4) 0.092(2) Uani 1 1 d . . . H17A H -0.1834 0.3974 0.3096 0.139 Uiso 1 1 calc R . . H17B H -0.0523 0.4268 0.3668 0.139 Uiso 1 1 calc R . . H17C H -0.0492 0.3882 0.2890 0.139 Uiso 1 1 calc R . . C18 C -0.1597(6) 0.5805(6) 0.2774(5) 0.110(3) Uani 1 1 d U . . H18A H -0.1465 0.6462 0.3062 0.164 Uiso 1 1 calc R . . H18B H -0.2474 0.5422 0.2747 0.164 Uiso 1 1 calc R . . H18C H -0.1479 0.5906 0.2313 0.164 Uiso 1 1 calc R . . C19 C 0.3048(5) 0.4050(3) 0.2594(2) 0.0503(12) Uani 1 1 d . . . H19 H 0.2327 0.3797 0.2184 0.060 Uiso 1 1 calc R . . C20 C 0.4274(6) 0.4159(4) 0.2348(3) 0.0658(14) Uani 1 1 d . . . H20A H 0.4330 0.4696 0.2065 0.099 Uiso 1 1 calc R . . H20B H 0.4297 0.3523 0.2075 0.099 Uiso 1 1 calc R . . H20C H 0.5005 0.4331 0.2742 0.099 Uiso 1 1 calc R . . C21 C 0.2917(7) 0.3311(4) 0.3085(3) 0.0762(18) Uani 1 1 d . . . H21A H 0.3599 0.3546 0.3500 0.114 Uiso 1 1 calc R . . H21B H 0.2997 0.2651 0.2869 0.114 Uiso 1 1 calc R . . H21C H 0.2071 0.3252 0.3207 0.114 Uiso 1 1 calc R . . C22 C 0.3041(6) 0.5511(4) 0.4918(2) 0.0579(13) Uani 1 1 d . . . H22 H 0.3839 0.5230 0.4956 0.069 Uiso 1 1 calc R . . C23 C 0.1924(6) 0.4660(4) 0.4853(3) 0.0704(16) Uani 1 1 d . . . H23A H 0.1135 0.4921 0.4842 0.106 Uiso 1 1 calc R . . H23B H 0.2066 0.4301 0.5246 0.106 Uiso 1 1 calc R . . H23C H 0.1833 0.4196 0.4428 0.106 Uiso 1 1 calc R . . C24 C 0.3228(7) 0.6304(5) 0.5533(2) 0.0719(17) Uani 1 1 d . . . H24A H 0.3943 0.6860 0.5525 0.108 Uiso 1 1 calc R . . H24B H 0.3429 0.6010 0.5952 0.108 Uiso 1 1 calc R . . H24C H 0.2436 0.6559 0.5524 0.108 Uiso 1 1 calc R . . C25 C 0.2230(7) 0.8859(5) 0.4438(3) 0.0746(18) Uani 1 1 d . . . H25 H 0.2842 0.9388 0.4286 0.089 Uiso 1 1 calc R . . C26 C 0.2927(9) 0.8983(6) 0.5132(3) 0.111(3) Uani 1 1 d U . . H26A H 0.2729 0.9556 0.5402 0.166 Uiso 1 1 calc R . . H26B H 0.3856 0.9109 0.5143 0.166 Uiso 1 1 calc R . . H26C H 0.2675 0.8369 0.5326 0.166 Uiso 1 1 calc R . . C27 C 0.1123(12) 0.9176(9) 0.4188(6) 0.173(5) Uani 1 1 d U . . H27A H 0.1349 0.9800 0.4000 0.260 Uiso 1 1 calc R . . H27B H 0.0672 0.9300 0.4559 0.260 Uiso 1 1 calc R . . H27C H 0.0560 0.8654 0.3825 0.260 Uiso 1 1 calc R . . C28 C 0.6311(5) 0.7491(5) 0.4045(3) 0.0755(19) Uani 1 1 d . . . H28 H 0.6593 0.6833 0.4023 0.091 Uiso 1 1 calc R . . C29 C 0.6472(6) 0.7823(6) 0.4790(3) 0.096(2) Uani 1 1 d . . . H29A H 0.7393 0.7997 0.5006 0.144 Uiso 1 1 calc R . . H29B H 0.6035 0.7275 0.4994 0.144 Uiso 1 1 calc R . . H29C H 0.6093 0.8414 0.4863 0.144 Uiso 1 1 calc R . . C30 C 0.7039(7) 0.8039(8) 0.3607(4) 0.117(3) Uani 1 1 d . . . H30A H 0.6910 0.7616 0.3161 0.175 Uiso 1 1 calc R . . H30B H 0.7960 0.8207 0.3825 0.175 Uiso 1 1 calc R . . H30C H 0.6735 0.8661 0.3542 0.175 Uiso 1 1 calc R . . C31 C 0.5691(9) 0.1211(5) 0.2871(4) 0.103(3) Uani 1 1 d . . . H31 H 0.5535 0.1666 0.3260 0.123 Uiso 1 1 calc R . . C32 C 0.5411(9) 0.1582(5) 0.2235(5) 0.111(3) Uani 1 1 d . . . H32A H 0.5590 0.1125 0.1869 0.166 Uiso 1 1 calc R . . H32B H 0.5951 0.2255 0.2272 0.166 Uiso 1 1 calc R . . H32C H 0.4498 0.1619 0.2129 0.166 Uiso 1 1 calc R . . C33 C 0.7171(10) 0.1125(6) 0.2978(5) 0.131(4) Uani 1 1 d . . . H33A H 0.7393 0.0798 0.3379 0.197 Uiso 1 1 calc R . . H33B H 0.7722 0.1802 0.3050 0.197 Uiso 1 1 calc R . . H33C H 0.7303 0.0724 0.2570 0.197 Uiso 1 1 calc R . . 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 0.0326(6) 0.0273(5) 0.0273(5) 0.0102(4) 0.0056(4) 0.0034(4) Al2 0.0415(7) 0.0342(6) 0.0288(5) 0.0089(4) 0.0095(5) -0.0068(5) Al3 0.0288(6) 0.0236(5) 0.0259(5) 0.0108(4) 0.0034(4) 0.0048(4) Al4 0.0540(8) 0.0235(5) 0.0302(5) 0.0112(4) 0.0015(5) 0.0102(5) Al5 0.0353(6) 0.0321(5) 0.0282(5) 0.0149(4) 0.0016(4) 0.0024(4) Al6 0.0478(8) 0.0569(8) 0.0315(6) 0.0177(5) 0.0108(5) 0.0146(6) Al7 0.0406(7) 0.0447(7) 0.0337(6) 0.0147(5) -0.0013(5) 0.0087(5) Al8 0.0487(8) 0.0370(6) 0.0295(6) 0.0071(5) -0.0001(5) 0.0025(5) F1 0.0308(12) 0.0346(11) 0.0322(10) 0.0147(9) 0.0047(9) 0.0055(9) F2 0.0329(12) 0.0306(10) 0.0314(10) 0.0121(8) 0.0061(9) 0.0048(8) F3 0.0575(17) 0.0490(14) 0.0442(14) 0.0106(11) 0.0049(12) 0.0079(12) F4 0.0523(16) 0.0542(14) 0.0364(12) 0.0043(11) 0.0169(11) -0.0177(12) F5 0.0483(15) 0.0379(12) 0.0428(13) 0.0135(10) 0.0061(11) 0.0085(10) F6 0.092(2) 0.0303(11) 0.0382(12) 0.0100(10) -0.0042(13) 0.0251(12) F7 0.0439(14) 0.0352(11) 0.0294(10) 0.0149(9) -0.0007(9) -0.0002(9) F8 0.069(2) 0.085(2) 0.0441(14) 0.0240(14) 0.0255(14) 0.0244(16) F9 0.0533(17) 0.0570(15) 0.0482(14) 0.0177(12) -0.0065(12) 0.0180(13) F10 0.074(2) 0.0460(14) 0.0385(13) 0.0051(11) -0.0028(13) -0.0070(13) O1 0.0344(15) 0.0243(11) 0.0307(12) 0.0110(10) 0.0059(10) 0.0028(10) O2 0.0344(15) 0.0328(13) 0.0306(12) 0.0090(10) 0.0059(11) -0.0010(11) O3 0.0463(17) 0.0268(12) 0.0295(12) 0.0070(10) 0.0054(11) 0.0089(11) O4 0.0325(15) 0.0327(13) 0.0285(12) 0.0087(10) 0.0075(10) 0.0024(10) O5 0.069(2) 0.0283(13) 0.0339(14) 0.0160(11) 0.0072(14) -0.0083(13) O6 0.0352(15) 0.0294(12) 0.0284(12) 0.0125(10) 0.0017(10) 0.0078(10) O7 0.0351(15) 0.0366(13) 0.0287(12) 0.0127(10) 0.0042(11) 0.0052(11) O8 0.0363(16) 0.0523(17) 0.0431(15) 0.0247(13) 0.0096(12) 0.0049(13) O9 0.0438(17) 0.0333(13) 0.0338(13) 0.0127(11) 0.0001(12) 0.0078(12) O10 0.056(2) 0.0554(17) 0.0288(13) 0.0205(13) 0.0052(13) 0.0125(15) O11 0.072(2) 0.0472(17) 0.0308(14) 0.0027(12) 0.0095(14) 0.0176(15) O12 0.0363(17) 0.0554(18) 0.0436(16) 0.0149(14) -0.0048(13) 0.0030(13) O13 0.124(4) 0.058(2) 0.066(2) 0.0167(19) 0.025(2) -0.030(2) C1 0.036(2) 0.042(2) 0.039(2) 0.0115(17) 0.0082(17) 0.0053(17) C2 0.036(2) 0.045(2) 0.058(3) 0.008(2) 0.005(2) -0.0043(18) C3 0.057(3) 0.044(2) 0.059(3) 0.016(2) 0.023(2) 0.014(2) C4 0.048(3) 0.036(2) 0.0340(19) 0.0057(16) 0.0090(17) 0.0117(17) C5 0.048(3) 0.057(3) 0.055(3) 0.014(2) 0.011(2) 0.020(2) C6 0.085(4) 0.027(2) 0.064(3) 0.001(2) 0.023(3) 0.011(2) C7 0.032(2) 0.0346(18) 0.0359(19) 0.0025(15) 0.0107(16) 0.0065(15) C8 0.056(3) 0.054(3) 0.032(2) 0.0094(18) 0.0123(19) 0.004(2) C9 0.041(3) 0.046(2) 0.084(4) 0.009(2) 0.014(2) 0.012(2) C10 0.153(6) 0.041(2) 0.050(3) 0.028(2) -0.012(3) -0.040(3) C11 0.047(3) 0.0301(19) 0.054(2) 0.0144(18) 0.008(2) 0.0013(17) C12 0.121(5) 0.055(3) 0.055(3) 0.038(3) -0.005(3) -0.022(3) C13 0.030(2) 0.0301(18) 0.046(2) 0.0119(16) 0.0049(16) 0.0087(15) C14 0.039(2) 0.042(2) 0.039(2) 0.0145(17) -0.0046(17) 0.0125(17) C15 0.054(3) 0.045(2) 0.093(4) 0.026(3) 0.037(3) 0.019(2) C16 0.035(3) 0.071(4) 0.138(6) 0.051(4) 0.024(3) -0.001(2) C17 0.072(4) 0.069(4) 0.116(5) 0.044(4) -0.013(4) -0.020(3) C18 0.049(4) 0.103(5) 0.183(7) 0.071(5) 0.013(4) 0.014(3) C19 0.069(3) 0.034(2) 0.049(2) 0.0110(18) 0.006(2) 0.017(2) C20 0.075(4) 0.058(3) 0.074(4) 0.015(3) 0.025(3) 0.026(3) C21 0.109(5) 0.041(3) 0.079(4) 0.024(3) 0.015(4) 0.013(3) C22 0.077(4) 0.069(3) 0.032(2) 0.026(2) 0.004(2) 0.022(3) C23 0.095(5) 0.071(3) 0.051(3) 0.035(3) 0.018(3) 0.014(3) C24 0.097(5) 0.087(4) 0.033(2) 0.022(2) 0.001(3) 0.028(3) C25 0.100(5) 0.078(4) 0.047(3) -0.008(3) 0.007(3) 0.041(4) C26 0.179(8) 0.083(4) 0.055(3) -0.019(3) -0.013(4) 0.045(5) C27 0.195(9) 0.169(8) 0.149(7) -0.051(6) -0.017(6) 0.125(7) C28 0.048(3) 0.091(4) 0.063(3) 0.031(3) -0.025(3) -0.021(3) C29 0.056(4) 0.144(7) 0.066(4) -0.019(4) -0.024(3) 0.021(4) C30 0.050(4) 0.176(9) 0.111(6) 0.010(6) 0.015(4) 0.004(5) C31 0.124(7) 0.058(4) 0.112(6) 0.028(4) 0.010(5) -0.013(4) C32 0.138(8) 0.057(4) 0.138(7) 0.029(4) 0.041(6) 0.003(4) C33 0.137(9) 0.078(5) 0.149(8) 0.016(5) 0.001(7) -0.021(5) _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 F2 1.835(2) . ? Al1 F1 1.836(2) . ? Al1 O1 1.870(3) . ? Al1 F3 1.878(3) . ? Al1 O2 1.908(3) . ? Al1 O3 1.911(3) . ? Al1 Al5 2.9006(14) . ? Al1 Al4 2.9116(15) . ? Al1 Al2 2.9124(16) . ? Al2 F4 1.678(3) . ? Al2 O2 1.819(3) . ? Al2 O5 1.830(3) . ? Al2 O4 1.866(3) . ? Al2 O1 1.931(3) . ? Al2 Al4 2.8164(19) . ? Al2 Al3 2.8565(16) . ? Al3 F5 1.801(2) . ? Al3 O4 1.834(3) . ? Al3 O6 1.835(3) . ? Al3 O1 1.837(3) . ? Al3 F5 1.851(3) 2_565 ? Al3 Al3 2.826(2) 2_565 ? Al3 Al4 2.8623(15) . ? Al4 F6 1.678(3) . ? Al4 O5 1.814(3) . ? Al4 O3 1.829(3) . ? Al4 O6 1.872(3) . ? Al4 O1 1.918(3) . ? Al5 F7 1.720(2) . ? Al5 O7 1.828(3) . ? Al5 F1 1.870(2) . ? Al5 F2 1.891(2) . ? Al5 O9 1.903(3) . ? Al5 O8 1.907(3) . ? Al5 Al7 2.8913(16) . ? Al5 Al6 2.8991(17) . ? Al6 F8 1.677(3) . ? Al6 O8 1.833(3) . ? Al6 O10 1.837(3) . ? Al6 O11 1.869(3) . ? Al6 O7 1.883(3) . ? Al6 Al7 2.816(2) . ? Al6 Al8 2.872(2) . ? Al7 F9 1.677(3) . ? Al7 O10 1.823(3) . ? Al7 O9 1.834(3) . ? Al7 O12 1.862(3) . ? Al7 O7 1.871(3) . ? Al7 Al8 2.8751(17) . ? Al8 F10 1.703(3) . ? Al8 F3 1.819(3) . ? Al8 O7 1.828(3) . ? Al8 O11 1.857(4) . ? Al8 O12 1.871(3) . ? F5 Al3 1.851(3) 2_565 ? O2 C1 1.448(5) . ? O3 C4 1.447(5) . ? O4 C7 1.453(4) . ? O5 C10 1.461(5) . ? O6 C13 1.454(4) . ? O8 C16 1.441(6) . ? O9 C19 1.454(5) . ? O10 C22 1.466(5) . ? O11 C25 1.449(6) . ? O12 C28 1.476(6) . ? O13 C31 1.445(7) . ? C1 C3 1.508(6) . ? C1 C2 1.513(6) . ? C4 C5 1.508(7) . ? C4 C6 1.512(6) . ? C7 C9 1.505(6) . ? C7 C8 1.510(6) . ? C10 C12 1.350(7) . ? C10 C11 1.421(6) . ? C13 C14 1.505(5) . ? C13 C15 1.517(6) . ? C16 C18 1.359(8) . ? C16 C17 1.425(8) . ? C19 C20 1.483(8) . ? C19 C21 1.497(7) . ? C22 C23 1.484(8) . ? C22 C24 1.502(7) . ? C25 C27 1.374(11) . ? C25 C26 1.431(8) . ? C28 C30 1.464(10) . ? C28 C29 1.482(9) . ? C31 C32 1.430(11) . ? C31 C33 1.598(13) . ? 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 F2 Al1 F1 77.08(10) . . ? F2 Al1 O1 96.83(11) . . ? F1 Al1 O1 98.17(11) . . ? F2 Al1 F3 95.20(11) . . ? F1 Al1 F3 94.55(12) . . ? O1 Al1 F3 164.14(12) . . ? F2 Al1 O2 89.75(11) . . ? F1 Al1 O2 165.80(12) . . ? O1 Al1 O2 77.92(12) . . ? F3 Al1 O2 91.87(12) . . ? F2 Al1 O3 164.06(13) . . ? F1 Al1 O3 88.62(12) . . ? O1 Al1 O3 78.05(11) . . ? F3 Al1 O3 92.89(12) . . ? O2 Al1 O3 103.70(12) . . ? F2 Al1 Al5 39.58(7) . . ? F1 Al1 Al5 38.93(7) . . ? O1 Al1 Al5 107.73(8) . . ? F3 Al1 Al5 88.12(9) . . ? O2 Al1 Al5 128.93(9) . . ? O3 Al1 Al5 127.32(10) . . ? F2 Al1 Al4 136.23(8) . . ? F1 Al1 Al4 97.03(8) . . ? O1 Al1 Al4 40.36(8) . . ? F3 Al1 Al4 128.57(9) . . ? O2 Al1 Al4 88.78(9) . . ? O3 Al1 Al4 37.86(8) . . ? Al5 Al1 Al4 128.99(5) . . ? F2 Al1 Al2 98.31(8) . . ? F1 Al1 Al2 138.49(8) . . ? O1 Al1 Al2 40.78(9) . . ? F3 Al1 Al2 126.93(10) . . ? O2 Al1 Al2 37.54(8) . . ? O3 Al1 Al2 87.68(9) . . ? Al5 Al1 Al2 131.42(5) . . ? Al4 Al1 Al2 57.84(4) . . ? F4 Al2 O2 100.86(13) . . ? F4 Al2 O5 104.53(15) . . ? O2 Al2 O5 108.53(14) . . ? F4 Al2 O4 98.67(13) . . ? O2 Al2 O4 133.75(12) . . ? O5 Al2 O4 106.41(13) . . ? F4 Al2 O1 173.28(14) . . ? O2 Al2 O1 78.54(12) . . ? O5 Al2 O1 81.91(13) . . ? O4 Al2 O1 77.39(11) . . ? F4 Al2 Al4 143.72(12) . . ? O2 Al2 Al4 93.59(10) . . ? O5 Al2 Al4 39.19(10) . . ? O4 Al2 Al4 94.77(10) . . ? O1 Al2 Al4 42.78(8) . . ? F4 Al2 Al3 137.43(10) . . ? O2 Al2 Al3 113.28(10) . . ? O5 Al2 Al3 88.45(10) . . ? O4 Al2 Al3 39.05(9) . . ? O1 Al2 Al3 39.48(8) . . ? Al4 Al2 Al3 60.60(4) . . ? F4 Al2 Al1 140.58(10) . . ? O2 Al2 Al1 39.73(9) . . ? O5 Al2 Al1 92.45(10) . . ? O4 Al2 Al1 110.40(9) . . ? O1 Al2 Al1 39.21(8) . . ? Al4 Al2 Al1 61.07(4) . . ? Al3 Al2 Al1 77.06(4) . . ? F5 Al3 O4 120.73(12) . . ? F5 Al3 O6 122.77(13) . . ? O4 Al3 O6 115.96(12) . . ? F5 Al3 O1 101.37(11) . . ? O4 Al3 O1 80.64(12) . . ? O6 Al3 O1 80.11(11) . . ? F5 Al3 F5 78.62(12) . 2_565 ? O4 Al3 F5 99.19(12) . 2_565 ? O6 Al3 F5 100.06(12) . 2_565 ? O1 Al3 F5 179.80(15) . 2_565 ? F5 Al3 Al3 39.95(8) . 2_565 ? O4 Al3 Al3 115.49(10) . 2_565 ? O6 Al3 Al3 117.35(10) . 2_565 ? O1 Al3 Al3 141.32(9) . 2_565 ? F5 Al3 Al3 38.67(7) 2_565 2_565 ? F5 Al3 Al2 125.35(9) . . ? O4 Al3 Al2 39.89(8) . . ? O6 Al3 Al2 93.77(9) . . ? O1 Al3 Al2 41.96(9) . . ? F5 Al3 Al2 137.89(10) 2_565 . ? Al3 Al3 Al2 148.73(7) 2_565 . ? F5 Al3 Al4 126.26(9) . . ? O4 Al3 Al4 94.02(9) . . ? O6 Al3 Al4 39.91(8) . . ? O1 Al3 Al4 41.39(8) . . ? F5 Al3 Al4 138.77(9) 2_565 . ? Al3 Al3 Al4 150.41(7) 2_565 . ? Al2 Al3 Al4 59.01(4) . . ? F6 Al4 O5 104.90(15) . . ? F6 Al4 O3 100.31(13) . . ? O5 Al4 O3 106.26(14) . . ? F6 Al4 O6 98.76(13) . . ? O5 Al4 O6 105.80(13) . . ? O3 Al4 O6 136.68(12) . . ? F6 Al4 O1 172.20(15) . . ? O5 Al4 O1 82.70(13) . . ? O3 Al4 O1 78.87(11) . . ? O6 Al4 O1 77.14(11) . . ? F6 Al4 Al2 144.49(12) . . ? O5 Al4 Al2 39.60(10) . . ? O3 Al4 Al2 92.27(10) . . ? O6 Al4 Al2 94.24(10) . . ? O1 Al4 Al2 43.16(8) . . ? F6 Al4 Al3 137.55(11) . . ? O5 Al4 Al3 88.57(10) . . ? O3 Al4 Al3 114.45(9) . . ? O6 Al4 Al3 38.97(8) . . ? O1 Al4 Al3 39.29(8) . . ? Al2 Al4 Al3 60.39(4) . . ? F6 Al4 Al1 140.11(10) . . ? O5 Al4 Al1 92.81(10) . . ? O3 Al4 Al1 39.90(8) . . ? O6 Al4 Al1 110.54(8) . . ? O1 Al4 Al1 39.16(8) . . ? Al2 Al4 Al1 61.09(4) . . ? Al3 Al4 Al1 76.98(4) . . ? F7 Al5 O7 173.80(12) . . ? F7 Al5 F1 94.44(10) . . ? O7 Al5 F1 91.06(11) . . ? F7 Al5 F2 94.13(11) . . ? O7 Al5 F2 90.04(12) . . ? F1 Al5 F2 74.92(10) . . ? F7 Al5 O9 97.85(12) . . ? O7 Al5 O9 77.54(12) . . ? F1 Al5 O9 161.24(13) . . ? F2 Al5 O9 90.06(12) . . ? F7 Al5 O8 99.50(13) . . ? O7 Al5 O8 77.53(13) . . ? F1 Al5 O8 90.95(12) . . ? F2 Al5 O8 161.11(13) . . ? O9 Al5 O8 100.88(13) . . ? F7 Al5 Al7 136.03(9) . . ? O7 Al5 Al7 39.12(9) . . ? F1 Al5 Al7 128.89(9) . . ? F2 Al5 Al7 91.05(8) . . ? O9 Al5 Al7 38.44(9) . . ? O8 Al5 Al7 88.18(10) . . ? F7 Al5 Al6 137.29(10) . . ? O7 Al5 Al6 39.32(9) . . ? F1 Al5 Al6 92.66(8) . . ? F2 Al5 Al6 128.31(8) . . ? O9 Al5 Al6 87.88(9) . . ? O8 Al5 Al6 38.26(10) . . ? Al7 Al5 Al6 58.20(4) . . ? F7 Al5 Al1 103.21(8) . . ? O7 Al5 Al1 82.89(9) . . ? F1 Al5 Al1 38.09(7) . . ? F2 Al5 Al1 38.20(7) . . ? O9 Al5 Al1 124.44(10) . . ? O8 Al5 Al1 124.77(10) . . ? Al7 Al5 Al1 107.46(5) . . ? Al6 Al5 Al1 108.06(5) . . ? F8 Al6 O8 101.34(16) . . ? F8 Al6 O10 105.35(15) . . ? O8 Al6 O10 108.24(15) . . ? F8 Al6 O11 99.29(16) . . ? O8 Al6 O11 130.90(14) . . ? O10 Al6 O11 108.38(16) . . ? F8 Al6 O7 173.81(15) . . ? O8 Al6 O7 78.01(13) . . ? O10 Al6 O7 80.61(13) . . ? O11 Al6 O7 76.92(13) . . ? F8 Al6 Al7 144.81(12) . . ? O8 Al6 Al7 91.98(11) . . ? O10 Al6 Al7 39.51(10) . . ? O11 Al6 Al7 96.01(12) . . ? O7 Al6 Al7 41.23(8) . . ? F8 Al6 Al8 138.40(13) . . ? O8 Al6 Al8 111.12(10) . . ? O10 Al6 Al8 88.83(11) . . ? O11 Al6 Al8 39.43(11) . . ? O7 Al6 Al8 38.60(9) . . ? Al7 Al6 Al8 60.72(5) . . ? F8 Al6 Al5 141.30(13) . . ? O8 Al6 Al5 40.11(10) . . ? O10 Al6 Al5 93.84(11) . . ? O11 Al6 Al5 106.15(10) . . ? O7 Al6 Al5 37.94(9) . . ? Al7 Al6 Al5 60.76(4) . . ? Al8 Al6 Al5 73.73(5) . . ? F9 Al7 O10 104.64(14) . . ? F9 Al7 O9 101.63(14) . . ? O10 Al7 O9 107.81(15) . . ? F9 Al7 O12 98.76(15) . . ? O10 Al7 O12 107.79(16) . . ? O9 Al7 O12 132.44(14) . . ? F9 Al7 O7 173.68(15) . . ? O10 Al7 O7 81.31(13) . . ? O9 Al7 O7 78.20(12) . . ? O12 Al7 O7 77.13(13) . . ? F9 Al7 Al6 144.49(12) . . ? O10 Al7 Al6 39.88(9) . . ? O9 Al7 Al6 91.79(11) . . ? O12 Al7 Al6 95.83(12) . . ? O7 Al7 Al6 41.57(9) . . ? F9 Al7 Al8 138.19(12) . . ? O10 Al7 Al8 89.00(11) . . ? O9 Al7 Al8 111.58(9) . . ? O12 Al7 Al8 39.73(10) . . ? O7 Al7 Al8 38.44(9) . . ? Al6 Al7 Al8 60.60(5) . . ? F9 Al7 Al5 141.59(12) . . ? O10 Al7 Al5 94.41(11) . . ? O9 Al7 Al5 40.17(9) . . ? O12 Al7 Al5 106.81(10) . . ? O7 Al7 Al5 38.05(8) . . ? Al6 Al7 Al5 61.04(4) . . ? Al8 Al7 Al5 73.79(4) . . ? F10 Al8 F3 95.95(13) . . ? F10 Al8 O7 172.47(14) . . ? F3 Al8 O7 91.57(12) . . ? F10 Al8 O11 97.64(16) . . ? F3 Al8 O11 117.98(15) . . ? O7 Al8 O11 78.58(14) . . ? F10 Al8 O12 98.42(15) . . ? F3 Al8 O12 118.85(15) . . ? O7 Al8 O12 77.98(13) . . ? O11 Al8 O12 118.34(15) . . ? F10 Al8 Al6 134.76(12) . . ? F3 Al8 Al6 115.58(11) . . ? O7 Al8 Al6 40.01(9) . . ? O11 Al8 Al6 39.72(10) . . ? O12 Al8 Al6 93.82(11) . . ? F10 Al8 Al7 135.41(12) . . ? F3 Al8 Al7 115.62(10) . . ? O7 Al8 Al7 39.53(9) . . ? O11 Al8 Al7 94.35(11) . . ? O12 Al8 Al7 39.51(10) . . ? Al6 Al8 Al7 58.69(5) . . ? Al1 F1 Al5 102.98(12) . . ? Al1 F2 Al5 102.22(12) . . ? Al8 F3 Al1 134.81(15) . . ? Al3 F5 Al3 101.38(12) . 2_565 ? Al3 O1 Al1 151.68(14) . . ? Al3 O1 Al4 99.33(12) . . ? Al1 O1 Al4 100.48(12) . . ? Al3 O1 Al2 98.56(12) . . ? Al1 O1 Al2 100.01(12) . . ? Al4 O1 Al2 94.06(11) . . ? C1 O2 Al2 129.2(2) . . ? C1 O2 Al1 125.3(2) . . ? Al2 O2 Al1 102.74(13) . . ? C4 O3 Al4 129.4(2) . . ? C4 O3 Al1 126.1(2) . . ? Al4 O3 Al1 102.24(13) . . ? C7 O4 Al3 129.2(2) . . ? C7 O4 Al2 129.0(2) . . ? Al3 O4 Al2 101.06(13) . . ? C10 O5 Al4 128.4(4) . . ? C10 O5 Al2 129.5(4) . . ? Al4 O5 Al2 101.21(13) . . ? C13 O6 Al3 129.5(2) . . ? C13 O6 Al4 128.4(2) . . ? Al3 O6 Al4 101.12(13) . . ? Al5 O7 Al8 142.57(15) . . ? Al5 O7 Al7 102.83(14) . . ? Al8 O7 Al7 102.03(14) . . ? Al5 O7 Al6 102.74(14) . . ? Al8 O7 Al6 101.39(14) . . ? Al7 O7 Al6 97.20(12) . . ? C16 O8 Al6 130.2(4) . . ? C16 O8 Al5 127.9(4) . . ? Al6 O8 Al5 101.64(15) . . ? C19 O9 Al7 131.3(3) . . ? C19 O9 Al5 126.7(2) . . ? Al7 O9 Al5 101.39(13) . . ? C22 O10 Al7 126.6(3) . . ? C22 O10 Al6 132.6(3) . . ? Al7 O10 Al6 100.61(13) . . ? C25 O11 Al8 128.5(4) . . ? C25 O11 Al6 130.2(4) . . ? Al8 O11 Al6 100.85(15) . . ? C28 O12 Al7 126.4(3) . . ? C28 O12 Al8 131.6(3) . . ? Al7 O12 Al8 100.76(15) . . ? O2 C1 C3 110.0(3) . . ? O2 C1 C2 110.1(3) . . ? C3 C1 C2 112.6(4) . . ? O3 C4 C5 109.8(3) . . ? O3 C4 C6 110.4(3) . . ? C5 C4 C6 113.2(4) . . ? O4 C7 C9 109.4(3) . . ? O4 C7 C8 110.4(3) . . ? C9 C7 C8 112.7(4) . . ? C12 C10 C11 129.8(5) . . ? C12 C10 O5 115.2(4) . . ? C11 C10 O5 112.3(4) . . ? O6 C13 C14 110.1(3) . . ? O6 C13 C15 109.2(4) . . ? C14 C13 C15 112.6(3) . . ? C18 C16 C17 130.3(6) . . ? C18 C16 O8 116.2(5) . . ? C17 C16 O8 113.0(5) . . ? O9 C19 C20 110.5(4) . . ? O9 C19 C21 110.2(4) . . ? C20 C19 C21 113.9(5) . . ? O10 C22 C23 109.4(4) . . ? O10 C22 C24 109.3(4) . . ? C23 C22 C24 114.2(5) . . ? C27 C25 C26 128.7(7) . . ? C27 C25 O11 113.9(6) . . ? C26 C25 O11 113.2(5) . . ? C30 C28 O12 111.3(5) . . ? C30 C28 C29 123.8(6) . . ? O12 C28 C29 109.2(5) . . ? C32 C31 O13 110.4(6) . . ? C32 C31 C33 105.6(8) . . ? O13 C31 C33 105.1(6) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.88 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.916 _refine_diff_density_min -0.564 _refine_diff_density_rms 0.081