compound 1 data_p-1 _audit_creation_date 2012-05-09 _audit_creation_method ; Olex2 1.1 (compiled 2011.11.01 svn.r2039, GUI svn.r3906) ; _publ_contact_author_address ? _publ_contact_author_email ? _publ_contact_author_name '' _publ_contact_author_phone ? _chemical_name_common ? _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C18 H Al F32 O4, C7 H8' _chemical_formula_sum 'C25 H9 Al F32 O4' _chemical_formula_weight 1008.30 _chemical_melting_point ? 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' _space_group_crystal_system 'triclinic' _space_group_IT_number 2 _space_group_name_H-M_alt 'P -1' _space_group_name_Hall '-P 1' loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 'x, y, z' 2 '-x, -y, -z' _cell_length_a 10.7030(2) _cell_length_b 10.8399(2) _cell_length_c 15.5105(3) _cell_angle_alpha 72.0560(10) _cell_angle_beta 80.9760(10) _cell_angle_gamma 77.2220(10) _cell_volume 1661.94(5) _cell_formula_units_Z 2 _cell_measurement_reflns_used 8531 _cell_measurement_temperature 100 _cell_measurement_theta_max 27.822 _cell_measurement_theta_min 2.290 _exptl_absorpt_coefficient_mu 0.277 _exptl_absorpt_correction_T_max 0.9782 _exptl_absorpt_correction_T_min 0.9571 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'Sheldrick, G. M., 2003, SADABS' _exptl_crystal_colour 'clear light colourless' _exptl_crystal_colour_lustre clear _exptl_crystal_colour_modifier light _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 2.015 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_method 'not measured' _exptl_crystal_description needle _exptl_crystal_F_000 984 _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.08 _exptl_special_details ; ? ; _diffrn_reflns_av_R_equivalents 0.0337 _diffrn_reflns_av_unetI/netI 0.0355 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_number 33609 _diffrn_reflns_theta_full 29.52 _diffrn_reflns_theta_max 29.52 _diffrn_reflns_theta_min 1.96 _diffrn_ambient_temperature 100(2) _diffrn_detector_area_resol_mean 8 _diffrn_measured_fraction_theta_full 0.987 _diffrn_measured_fraction_theta_max 0.987 _diffrn_measurement_device_type 'Bruker APEX-II CCD area detector' _diffrn_measurement_method '\w and \f scans' _diffrn_radiation_monochromator 'multilayer mirror optics' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'ImuS microsource' _diffrn_source_current 0.6 _diffrn_source_power 0.03 _diffrn_source_target Mo _diffrn_source_voltage 50.0 _diffrn_standards_decay_% ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_number ? _reflns_number_gt 6621 _reflns_number_total 9144 _reflns_threshold_expression >2sigma(I) _computing_cell_refinement ? _computing_data_collection ? _computing_data_reduction 'SAINT v7.68A (Bruker, 2009)' _computing_molecular_graphics ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_publication_material ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_structure_refinement ; XL, G.M. Sheldrick, Acta Cryst. (2008). A64, 112-122 ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _refine_diff_density_max 0.376 _refine_diff_density_min -0.309 _refine_diff_density_rms 0.056 _refine_ls_extinction_coef ? _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.034 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 563 _refine_ls_number_reflns 9144 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0598 _refine_ls_R_factor_gt 0.0375 _refine_ls_restrained_S_all 1.034 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0395P)^2^+0.4779P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0842 _refine_ls_wR_factor_ref 0.0943 _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. ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap 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 0.29828(4) 0.13996(5) 0.23637(3) 0.01832(10) Uani 1 1 d . . . O1 O 0.17774(10) 0.19594(11) 0.30780(7) 0.0227(2) Uani 1 1 d . . . O2 O 0.24803(10) 0.14552(11) 0.13684(7) 0.0218(2) Uani 1 1 d . . . O3 O 0.43802(10) 0.18469(11) 0.24182(8) 0.0232(2) Uani 1 1 d . . . O4 O 0.32956(11) -0.04574(11) 0.27908(8) 0.0232(2) Uani 1 1 d . . . H4 H 0.3683(19) -0.0910(19) 0.3217(14) 0.028 Uiso 1 1 d . . . C1 C 0.14521(14) 0.24330(16) 0.38141(11) 0.0205(3) Uani 1 1 d . . . C2 C 0.18501(16) 0.13271(18) 0.46820(11) 0.0261(4) Uani 1 1 d . . . C3 C -0.00330(16) 0.29027(19) 0.38872(13) 0.0304(4) Uani 1 1 d . . . C4 C 0.21112(16) 0.36174(17) 0.37028(13) 0.0291(4) Uani 1 1 d . . . C5 C 0.17458(14) 0.21608(16) 0.06724(11) 0.0211(3) Uani 1 1 d . . . C6 C 0.21756(17) 0.34999(18) 0.02058(13) 0.0301(4) Uani 1 1 d . . . C7 C 0.03021(16) 0.23836(18) 0.10436(12) 0.0276(4) Uani 1 1 d . . . C8 C 0.19456(16) 0.13412(18) -0.00117(12) 0.0281(4) Uani 1 1 d . . . C9 C 0.56256(14) 0.19602(16) 0.21015(11) 0.0207(3) Uani 1 1 d . . . C10 C 0.61911(15) 0.10312(17) 0.14950(11) 0.0239(3) Uani 1 1 d . . . C11 C 0.64068(15) 0.15726(18) 0.29360(12) 0.0260(4) Uani 1 1 d . . . C12 C 0.56750(16) 0.34109(18) 0.15446(12) 0.0279(4) Uani 1 1 d . . . C13 C 0.26858(15) -0.12485(16) 0.24873(11) 0.0221(3) Uani 1 1 d . . . C14 C 0.33169(16) -0.18294(16) 0.18265(11) 0.0258(4) Uani 1 1 d . . . C15 C 0.27109(19) -0.25889(17) 0.15172(12) 0.0298(4) Uani 1 1 d . . . C16 C 0.14696(18) -0.27512(17) 0.18642(12) 0.0308(4) Uani 1 1 d . . . C17 C 0.08387(17) -0.21713(19) 0.25225(13) 0.0317(4) Uani 1 1 d . . . C18 C 0.14495(17) -0.14198(17) 0.28328(12) 0.0266(4) Uani 1 1 d . . . C19 C 0.57878(16) 0.74499(17) 0.38150(12) 0.0258(4) Uani 1 1 d . . . H19 H 0.6523 0.7859 0.3644 0.031 Uiso 1 1 calc R . . C20 C 0.48017(16) 0.78718(17) 0.44148(12) 0.0270(4) Uani 1 1 d . . . H20 H 0.4872 0.8557 0.4656 0.032 Uiso 1 1 calc R . . C21 C 0.37128(16) 0.72960(18) 0.46638(12) 0.0285(4) Uani 1 1 d . . . H21 H 0.3028 0.7597 0.5062 0.034 Uiso 1 1 calc R . . C22 C 0.36393(17) 0.62760(18) 0.43231(12) 0.0290(4) Uani 1 1 d . . . H22 H 0.2904 0.5867 0.4496 0.035 Uiso 1 1 calc R . . C23 C 0.46283(16) 0.58476(17) 0.37327(12) 0.0281(4) Uani 1 1 d . . . H23 H 0.4567 0.5142 0.3509 0.034 Uiso 1 1 calc R . . C24 C 0.57164(16) 0.64383(17) 0.34609(11) 0.0252(3) Uani 1 1 d . . . C25 C 0.67823(18) 0.5985(2) 0.28068(15) 0.0385(5) Uani 1 1 d . . . H25A H 0.6495 0.6282 0.2194 0.058 Uiso 1 1 calc R . . H25B H 0.7006 0.5019 0.2999 0.058 Uiso 1 1 calc R . . H25C H 0.7539 0.6357 0.2802 0.058 Uiso 1 1 calc R . . F1 F 0.30565(9) 0.07047(10) 0.45285(7) 0.0325(2) Uani 1 1 d . . . F2 F 0.18164(10) 0.17801(12) 0.53917(7) 0.0366(3) Uani 1 1 d . . . F3 F 0.11066(11) 0.04300(11) 0.49125(7) 0.0382(3) Uani 1 1 d . . . F4 F -0.06243(9) 0.20329(12) 0.37517(8) 0.0378(3) Uani 1 1 d . . . F5 F -0.04937(10) 0.30732(13) 0.47009(8) 0.0438(3) Uani 1 1 d . . . F6 F -0.03519(10) 0.40394(12) 0.32610(9) 0.0459(3) Uani 1 1 d . . . F7 F 0.33250(9) 0.32067(10) 0.39157(7) 0.0322(2) Uani 1 1 d . . . F8 F 0.21516(11) 0.43669(11) 0.28486(8) 0.0437(3) Uani 1 1 d . . . F9 F 0.15082(11) 0.43678(12) 0.42353(10) 0.0483(3) Uani 1 1 d . . . F10 F 0.32989(10) 0.33373(11) -0.02932(7) 0.0371(3) Uani 1 1 d . . . F11 F 0.23411(11) 0.40461(11) 0.08325(9) 0.0421(3) Uani 1 1 d . . . F12 F 0.13255(11) 0.43440(11) -0.03337(8) 0.0437(3) Uani 1 1 d . . . F13 F 0.00441(10) 0.33215(11) 0.14678(7) 0.0367(3) Uani 1 1 d . . . F14 F -0.04774(9) 0.27307(11) 0.03870(7) 0.0359(3) Uani 1 1 d . . . F15 F 0.00228(10) 0.12835(11) 0.16489(8) 0.0390(3) Uani 1 1 d . . . F16 F 0.31830(10) 0.08295(11) -0.01449(7) 0.0366(3) Uani 1 1 d . . . F17 F 0.15398(11) 0.20504(12) -0.08158(7) 0.0399(3) Uani 1 1 d . . . F18 F 0.13132(11) 0.03311(11) 0.03081(8) 0.0397(3) Uani 1 1 d . . . F19 F 0.64177(10) -0.02236(10) 0.20045(7) 0.0328(2) Uani 1 1 d . . . F20 F 0.53473(9) 0.11174(11) 0.09232(7) 0.0311(2) Uani 1 1 d . . . F21 F 0.72811(9) 0.13033(10) 0.10089(7) 0.0306(2) Uani 1 1 d . . . F22 F 0.61808(10) 0.25388(11) 0.33334(7) 0.0339(2) Uani 1 1 d . . . F23 F 0.60692(10) 0.05162(11) 0.35628(7) 0.0350(2) Uani 1 1 d . . . F24 F 0.76686(9) 0.12934(12) 0.27184(8) 0.0385(3) Uani 1 1 d . . . F25 F 0.49206(10) 0.42414(10) 0.19670(7) 0.0348(2) Uani 1 1 d . . . F26 F 0.52710(11) 0.36791(11) 0.07312(7) 0.0380(3) Uani 1 1 d . . . F27 F 0.68653(10) 0.36581(11) 0.14294(8) 0.0393(3) Uani 1 1 d . . . F28 F 0.45064(10) -0.16601(11) 0.14859(7) 0.0360(3) Uani 1 1 d . . . F29 F 0.33181(12) -0.31592(11) 0.08797(8) 0.0445(3) Uani 1 1 d . . . F30 F 0.08808(12) -0.34782(11) 0.15623(8) 0.0436(3) Uani 1 1 d . . . F31 F -0.03649(11) -0.23329(13) 0.28604(9) 0.0491(3) Uani 1 1 d . . . F32 F 0.08411(10) -0.08509(11) 0.34729(8) 0.0379(3) Uani 1 1 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 0.0151(2) 0.0208(2) 0.0191(2) -0.00549(18) -0.00122(17) -0.00388(17) O1 0.0174(5) 0.0309(6) 0.0218(6) -0.0113(5) 0.0009(4) -0.0048(5) O2 0.0187(5) 0.0252(6) 0.0208(5) -0.0070(5) -0.0042(4) -0.0001(4) O3 0.0153(5) 0.0313(6) 0.0257(6) -0.0116(5) 0.0023(4) -0.0080(5) O4 0.0247(6) 0.0217(6) 0.0239(6) -0.0040(5) -0.0094(5) -0.0038(5) C1 0.0153(7) 0.0252(8) 0.0229(8) -0.0101(6) 0.0011(6) -0.0048(6) C2 0.0260(8) 0.0306(9) 0.0244(8) -0.0101(7) 0.0011(7) -0.0104(7) C3 0.0191(8) 0.0397(11) 0.0344(10) -0.0163(8) 0.0001(7) -0.0030(7) C4 0.0249(8) 0.0252(9) 0.0382(10) -0.0117(8) -0.0001(7) -0.0049(7) C5 0.0178(7) 0.0226(8) 0.0204(7) -0.0052(6) -0.0026(6) 0.0005(6) C6 0.0259(9) 0.0271(9) 0.0322(9) -0.0033(7) -0.0022(7) -0.0022(7) C7 0.0207(8) 0.0332(10) 0.0247(8) -0.0048(7) -0.0029(6) -0.0006(7) C8 0.0247(8) 0.0330(10) 0.0268(9) -0.0103(7) -0.0063(7) -0.0003(7) C9 0.0156(7) 0.0253(8) 0.0225(8) -0.0083(6) 0.0013(6) -0.0066(6) C10 0.0188(7) 0.0278(9) 0.0258(8) -0.0098(7) 0.0015(6) -0.0054(6) C11 0.0193(8) 0.0335(10) 0.0274(9) -0.0112(7) -0.0013(6) -0.0065(7) C12 0.0263(8) 0.0292(9) 0.0287(9) -0.0108(7) 0.0037(7) -0.0067(7) C13 0.0258(8) 0.0190(8) 0.0226(8) -0.0050(6) -0.0063(6) -0.0047(6) C14 0.0269(8) 0.0220(8) 0.0253(8) -0.0036(7) -0.0038(7) -0.0016(7) C15 0.0447(11) 0.0210(8) 0.0239(8) -0.0081(7) -0.0094(8) 0.0005(7) C16 0.0422(10) 0.0221(9) 0.0321(9) -0.0054(7) -0.0170(8) -0.0076(8) C17 0.0298(9) 0.0319(10) 0.0346(10) -0.0047(8) -0.0067(8) -0.0125(8) C18 0.0304(9) 0.0267(9) 0.0240(8) -0.0091(7) 0.0002(7) -0.0074(7) C19 0.0226(8) 0.0242(9) 0.0305(9) -0.0035(7) -0.0069(7) -0.0071(7) C20 0.0306(9) 0.0254(9) 0.0267(9) -0.0067(7) -0.0104(7) -0.0039(7) C21 0.0252(8) 0.0368(10) 0.0228(8) -0.0082(7) -0.0048(7) -0.0032(7) C22 0.0258(8) 0.0333(10) 0.0293(9) -0.0063(7) -0.0032(7) -0.0116(7) C23 0.0291(9) 0.0241(9) 0.0331(9) -0.0086(7) -0.0067(7) -0.0061(7) C24 0.0233(8) 0.0248(9) 0.0265(8) -0.0053(7) -0.0059(7) -0.0030(7) C25 0.0266(9) 0.0411(12) 0.0504(12) -0.0202(10) 0.0008(8) -0.0043(8) F1 0.0275(5) 0.0314(6) 0.0334(6) -0.0043(4) -0.0061(4) 0.0002(4) F2 0.0378(6) 0.0538(7) 0.0245(5) -0.0171(5) -0.0011(4) -0.0138(5) F3 0.0426(6) 0.0385(6) 0.0347(6) -0.0024(5) 0.0012(5) -0.0246(5) F4 0.0184(5) 0.0591(7) 0.0453(7) -0.0257(6) 0.0010(4) -0.0137(5) F5 0.0236(5) 0.0690(8) 0.0470(7) -0.0367(6) 0.0093(5) -0.0057(5) F6 0.0290(6) 0.0438(7) 0.0575(8) -0.0132(6) -0.0103(5) 0.0110(5) F7 0.0242(5) 0.0372(6) 0.0413(6) -0.0147(5) -0.0010(4) -0.0145(4) F8 0.0463(7) 0.0281(6) 0.0486(7) 0.0056(5) -0.0061(6) -0.0132(5) F9 0.0411(7) 0.0406(7) 0.0764(9) -0.0398(7) 0.0074(6) -0.0109(5) F10 0.0280(5) 0.0409(6) 0.0352(6) -0.0009(5) 0.0045(4) -0.0110(5) F11 0.0462(7) 0.0309(6) 0.0556(7) -0.0204(5) -0.0013(6) -0.0108(5) F12 0.0369(6) 0.0297(6) 0.0489(7) 0.0085(5) -0.0089(5) 0.0013(5) F13 0.0286(5) 0.0439(7) 0.0332(6) -0.0169(5) -0.0020(4) 0.0102(5) F14 0.0201(5) 0.0496(7) 0.0344(6) -0.0084(5) -0.0089(4) 0.0002(4) F15 0.0237(5) 0.0447(7) 0.0378(6) 0.0028(5) 0.0034(4) -0.0092(5) F16 0.0279(5) 0.0480(7) 0.0355(6) -0.0238(5) -0.0045(4) 0.0075(5) F17 0.0414(6) 0.0531(7) 0.0230(5) -0.0120(5) -0.0113(5) 0.0031(5) F18 0.0425(6) 0.0356(6) 0.0482(7) -0.0163(5) -0.0121(5) -0.0105(5) F19 0.0368(6) 0.0248(5) 0.0358(6) -0.0109(4) 0.0007(5) -0.0034(4) F20 0.0241(5) 0.0432(6) 0.0328(6) -0.0221(5) -0.0038(4) -0.0031(4) F21 0.0202(5) 0.0413(6) 0.0326(5) -0.0173(5) 0.0078(4) -0.0081(4) F22 0.0344(6) 0.0437(6) 0.0330(6) -0.0216(5) -0.0024(5) -0.0116(5) F23 0.0380(6) 0.0358(6) 0.0277(5) -0.0010(4) -0.0061(4) -0.0090(5) F24 0.0173(5) 0.0623(8) 0.0400(6) -0.0213(6) -0.0038(4) -0.0052(5) F25 0.0387(6) 0.0260(5) 0.0391(6) -0.0142(5) 0.0058(5) -0.0046(5) F26 0.0486(7) 0.0340(6) 0.0254(5) -0.0039(4) -0.0021(5) -0.0029(5) F27 0.0328(6) 0.0365(6) 0.0503(7) -0.0125(5) 0.0114(5) -0.0199(5) F28 0.0297(5) 0.0382(6) 0.0384(6) -0.0134(5) 0.0033(5) -0.0037(5) F29 0.0624(8) 0.0383(7) 0.0365(6) -0.0213(5) -0.0058(6) -0.0009(6) F30 0.0596(8) 0.0322(6) 0.0483(7) -0.0109(5) -0.0276(6) -0.0126(5) F31 0.0364(6) 0.0585(8) 0.0608(8) -0.0204(7) 0.0030(6) -0.0263(6) F32 0.0355(6) 0.0456(7) 0.0381(6) -0.0209(5) 0.0093(5) -0.0149(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 O1 1.6970(12) . ? Al1 O2 1.6925(12) . ? Al1 O3 1.6926(11) . ? Al1 O4 1.8849(12) . ? O1 C1 1.3586(19) . ? O2 C5 1.3637(18) . ? O3 C9 1.3648(18) . ? O4 H4 0.80(2) . ? O4 C13 1.4056(19) . ? C1 C2 1.546(2) . ? C1 C3 1.556(2) . ? C1 C4 1.550(2) . ? C2 F1 1.340(2) . ? C2 F2 1.329(2) . ? C2 F3 1.3213(19) . ? C3 F4 1.327(2) . ? C3 F5 1.333(2) . ? C3 F6 1.326(2) . ? C4 F7 1.3353(19) . ? C4 F8 1.324(2) . ? C4 F9 1.332(2) . ? C5 C6 1.545(2) . ? C5 C7 1.555(2) . ? C5 C8 1.545(2) . ? C6 F10 1.332(2) . ? C6 F11 1.335(2) . ? C6 F12 1.328(2) . ? C7 F13 1.332(2) . ? C7 F14 1.3290(19) . ? C7 F15 1.331(2) . ? C8 F16 1.3282(19) . ? C8 F17 1.3292(19) . ? C8 F18 1.338(2) . ? C9 C10 1.549(2) . ? C9 C11 1.549(2) . ? C9 C12 1.552(2) . ? C10 F19 1.3362(19) . ? C10 F20 1.3319(18) . ? C10 F21 1.3250(18) . ? C11 F22 1.332(2) . ? C11 F23 1.332(2) . ? C11 F24 1.3299(19) . ? C12 F25 1.329(2) . ? C12 F26 1.324(2) . ? C12 F27 1.333(2) . ? C13 C14 1.377(2) . ? C13 C18 1.377(2) . ? C14 C15 1.381(2) . ? C14 F28 1.329(2) . ? C15 C16 1.381(3) . ? C15 F29 1.334(2) . ? C16 C17 1.373(3) . ? C16 F30 1.333(2) . ? C17 C18 1.378(2) . ? C17 F31 1.340(2) . ? C18 F32 1.337(2) . ? C19 H19 0.9500 . ? C19 C20 1.389(3) . ? C19 C24 1.390(2) . ? C20 H20 0.9500 . ? C20 C21 1.389(2) . ? C21 H21 0.9500 . ? C21 C22 1.385(3) . ? C22 H22 0.9500 . ? C22 C23 1.384(3) . ? C23 H23 0.9500 . ? C23 C24 1.398(2) . ? C24 C25 1.506(3) . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Al1 O4 107.08(6) . . ? O2 Al1 O1 112.92(6) . . ? O2 Al1 O3 122.56(6) . . ? O2 Al1 O4 94.45(6) . . ? O3 Al1 O1 111.55(6) . . ? O3 Al1 O4 105.32(6) . . ? C1 O1 Al1 146.82(10) . . ? C5 O2 Al1 146.81(11) . . ? C9 O3 Al1 151.35(11) . . ? Al1 O4 H4 127.0(14) . . ? C13 O4 Al1 123.11(9) . . ? C13 O4 H4 109.2(14) . . ? O1 C1 C2 109.70(13) . . ? O1 C1 C3 107.37(13) . . ? O1 C1 C4 111.09(13) . . ? C2 C1 C3 110.04(13) . . ? C2 C1 C4 109.59(13) . . ? C4 C1 C3 109.02(14) . . ? F1 C2 C1 109.66(13) . . ? F2 C2 C1 112.81(14) . . ? F2 C2 F1 107.47(13) . . ? F3 C2 C1 111.47(13) . . ? F3 C2 F1 106.95(14) . . ? F3 C2 F2 108.22(14) . . ? F4 C3 C1 110.93(14) . . ? F4 C3 F5 107.70(15) . . ? F5 C3 C1 112.14(14) . . ? F6 C3 C1 110.28(14) . . ? F6 C3 F4 107.62(15) . . ? F6 C3 F5 108.01(15) . . ? F7 C4 C1 111.04(14) . . ? F8 C4 C1 110.74(14) . . ? F8 C4 F7 107.02(14) . . ? F8 C4 F9 108.35(15) . . ? F9 C4 C1 112.27(14) . . ? F9 C4 F7 107.21(15) . . ? O2 C5 C6 109.79(13) . . ? O2 C5 C7 109.86(13) . . ? O2 C5 C8 107.36(12) . . ? C6 C5 C7 110.16(13) . . ? C6 C5 C8 110.15(14) . . ? C8 C5 C7 109.47(13) . . ? F10 C6 C5 110.67(14) . . ? F10 C6 F11 107.19(15) . . ? F11 C6 C5 110.06(14) . . ? F12 C6 C5 112.37(14) . . ? F12 C6 F10 108.07(15) . . ? F12 C6 F11 108.30(15) . . ? F13 C7 C5 110.74(14) . . ? F14 C7 C5 112.26(14) . . ? F14 C7 F13 108.19(13) . . ? F14 C7 F15 108.19(14) . . ? F15 C7 C5 110.05(13) . . ? F15 C7 F13 107.25(14) . . ? F16 C8 C5 110.52(13) . . ? F16 C8 F17 108.03(14) . . ? F16 C8 F18 106.99(14) . . ? F17 C8 C5 112.62(14) . . ? F17 C8 F18 107.66(14) . . ? F18 C8 C5 110.80(14) . . ? O3 C9 C10 110.44(13) . . ? O3 C9 C11 107.75(13) . . ? O3 C9 C12 109.23(13) . . ? C10 C9 C12 109.89(13) . . ? C11 C9 C10 109.75(13) . . ? C11 C9 C12 109.75(13) . . ? F19 C10 C9 110.51(13) . . ? F20 C10 C9 109.96(13) . . ? F20 C10 F19 107.04(13) . . ? F21 C10 C9 113.02(13) . . ? F21 C10 F19 107.95(13) . . ? F21 C10 F20 108.15(13) . . ? F22 C11 C9 111.05(14) . . ? F23 C11 C9 110.75(13) . . ? F23 C11 F22 106.73(14) . . ? F24 C11 C9 112.58(14) . . ? F24 C11 F22 107.93(13) . . ? F24 C11 F23 107.54(14) . . ? F25 C12 C9 110.71(14) . . ? F25 C12 F27 107.76(14) . . ? F26 C12 C9 111.01(14) . . ? F26 C12 F25 107.51(14) . . ? F26 C12 F27 108.21(14) . . ? F27 C12 C9 111.49(14) . . ? C14 C13 O4 119.80(15) . . ? C14 C13 C18 119.90(16) . . ? C18 C13 O4 120.29(15) . . ? C13 C14 C15 119.85(16) . . ? F28 C14 C13 120.18(15) . . ? F28 C14 C15 119.97(16) . . ? C14 C15 C16 119.89(17) . . ? F29 C15 C14 120.19(17) . . ? F29 C15 C16 119.92(16) . . ? C17 C16 C15 120.31(16) . . ? F30 C16 C15 119.95(17) . . ? F30 C16 C17 119.74(17) . . ? C16 C17 C18 119.60(17) . . ? F31 C17 C16 120.23(16) . . ? F31 C17 C18 120.17(18) . . ? C13 C18 C17 120.44(17) . . ? F32 C18 C13 119.61(15) . . ? F32 C18 C17 119.95(16) . . ? C20 C19 H19 119.5 . . ? C20 C19 C24 121.04(16) . . ? C24 C19 H19 119.5 . . ? C19 C20 H20 119.9 . . ? C21 C20 C19 120.30(16) . . ? C21 C20 H20 119.9 . . ? C20 C21 H21 120.5 . . ? C22 C21 C20 119.09(17) . . ? C22 C21 H21 120.5 . . ? C21 C22 H22 119.7 . . ? C23 C22 C21 120.54(16) . . ? C23 C22 H22 119.7 . . ? C22 C23 H23 119.5 . . ? C22 C23 C24 120.93(17) . . ? C24 C23 H23 119.5 . . ? C19 C24 C23 118.07(16) . . ? C19 C24 C25 121.08(16) . . ? C23 C24 C25 120.84(16) . . ? C24 C25 H25A 109.5 . . ? C24 C25 H25B 109.5 . . ? C24 C25 H25C 109.5 . . ? H25A C25 H25B 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? ###end compound 3 data_p21_neu _audit_creation_date 2012-05-16 _audit_creation_method ; Olex2 1.1 (compiled 2011.11.01 svn.r2039, GUI svn.r3906) ; _publ_contact_author_address ? _publ_contact_author_email ? _publ_contact_author_name '' _publ_contact_author_phone ? _chemical_name_common ? _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C22 H20 Al F27 O4' _chemical_formula_sum 'C22 H20 Al F27 O4' _chemical_formula_weight 888.36 _chemical_absolute_configuration unk _chemical_melting_point ? 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' _space_group_crystal_system 'monoclinic' _space_group_IT_number 4 _space_group_name_H-M_alt 'P 1 21 1' _space_group_name_Hall 'P 2yb' loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 'x, y, z' 2 '-x, y+1/2, -z' _cell_length_a 11.4149(3) _cell_length_b 17.9673(6) _cell_length_c 15.8175(4) _cell_angle_alpha 90.00 _cell_angle_beta 96.312(2) _cell_angle_gamma 90.00 _cell_volume 3224.42(16) _cell_formula_units_Z 4 _cell_measurement_reflns_used 5114 _cell_measurement_temperature 100 _cell_measurement_theta_max 19.996 _cell_measurement_theta_min 2.267 _exptl_absorpt_coefficient_mu 0.250 _exptl_absorpt_correction_T_max 0.7451 _exptl_absorpt_correction_T_min 0.6840 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'Sheldrick, G. M., 2003, SADABS' _exptl_crystal_colour 'clear light colourless' _exptl_crystal_colour_lustre clear _exptl_crystal_colour_modifier light _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.830 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_method 'not measured' _exptl_crystal_description plate _exptl_crystal_F_000 1760 _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.1 _exptl_special_details ; ? ; _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_unetI/netI 0.0383 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_number 5104 _diffrn_reflns_theta_full 23.82 _diffrn_reflns_theta_max 23.82 _diffrn_reflns_theta_min 1.72 _diffrn_ambient_temperature 99.98 _diffrn_detector_area_resol_mean 8 _diffrn_measured_fraction_theta_full 0.997 _diffrn_measured_fraction_theta_max 0.997 _diffrn_measurement_device_type 'Bruker APEX-II CCD area detector' _diffrn_measurement_method '\w and \f scans or \w scans' _diffrn_radiation_monochromator 'multilayer mirror optics' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'ImuS microsource' _diffrn_source_target Mo _diffrn_standards_decay_% ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_number ? _reflns_number_gt 4169 _reflns_number_total 5104 _reflns_threshold_expression >2sigma(I) _computing_cell_refinement ? _computing_data_collection ? _computing_data_reduction ? _computing_molecular_graphics ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_publication_material ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_structure_refinement ; XL, G.M. Sheldrick, Acta Cryst. (2008). A64, 112-122 ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _refine_diff_density_max 0.617 _refine_diff_density_min -0.513 _refine_diff_density_rms 0.079 _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.0(5) _refine_ls_extinction_coef ? _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.030 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 993 _refine_ls_number_reflns 5104 _refine_ls_number_restraints 160 _refine_ls_R_factor_all 0.0854 _refine_ls_R_factor_gt 0.0685 _refine_ls_restrained_S_all 1.019 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0969P)^2^+8.6016P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1680 _refine_ls_wR_factor_ref 0.1836 _refine_special_details ; 'Resolution is not high enough, so the flack parameter is not reliable: Friedel opposites were merged; higher symmetry was checked before 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. ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap 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 0.4683(2) 0.37471(15) 0.89693(15) 0.0250(6) Uani 1 1 d . . . Al2 Al 0.98085(19) 0.33960(15) 0.39278(15) 0.0239(5) Uani 1 1 d . . . C1 C 0.5915(8) 0.2508(6) 0.8263(7) 0.041(2) Uani 1 1 d U . . C2 C 0.6474(14) 0.1842(6) 0.8779(10) 0.071(4) Uani 1 1 d U . . C3 C 0.5000(13) 0.2250(10) 0.7548(9) 0.076(4) Uani 1 1 d U . . C4 C 0.6887(10) 0.2924(7) 0.7848(8) 0.053(3) Uani 1 1 d U . . C5 C 0.4894(7) 0.5147(6) 0.8025(6) 0.035(2) Uani 1 1 d U . . C6 C 0.6097(10) 0.5482(6) 0.7842(7) 0.050(3) Uani 1 1 d U . . C7 C 0.4018(10) 0.5137(8) 0.7202(7) 0.053(3) Uani 1 1 d U . . C8 C 0.4388(9) 0.5661(6) 0.8709(7) 0.046(2) Uani 1 1 d U . . C9 C 0.5322(10) 0.3890(6) 1.0820(6) 0.046(2) Uani 1 1 d U . . C10 C 0.5108(17) 0.4621(8) 1.1301(9) 0.082(4) Uani 1 1 d U . . C11 C 0.4930(18) 0.3209(8) 1.1255(9) 0.095(5) Uani 1 1 d U . . C12 C 0.6682(13) 0.3795(9) 1.0738(12) 0.088(4) Uani 1 1 d U . . C13 C 0.9998(10) 0.2078(7) 0.2842(6) 0.053(3) Uani 1 1 d U . . C14 C 0.9660(13) 0.1315(12) 0.3200(9) 0.084(4) Uani 1 1 d U A . C15 C 0.9044(11) 0.2300(7) 0.2100(8) 0.062(3) Uani 1 1 d U A . C16 C 1.1206(10) 0.2008(8) 0.2501(8) 0.061(3) Uani 1 1 d U A . C17 C 1.0581(8) 0.3093(6) 0.5726(5) 0.034(2) Uani 1 1 d U . . C18 C 1.1400(10) 0.2424(8) 0.5577(8) 0.061(3) Uani 1 1 d U A . C19 C 0.9662(10) 0.2830(7) 0.6317(7) 0.052(3) Uani 1 1 d U A . C20 C 1.1320(10) 0.3717(7) 0.6158(7) 0.053(3) Uani 1 1 d U A . C21 C 1.0991(10) 0.4714(7) 0.3272(9) 0.059(3) Uani 1 1 d U . . C22 C 1.2060(14) 0.4444(9) 0.2926(11) 0.083(4) Uani 1 1 d U A . C23 C 1.0204(15) 0.5172(10) 0.2605(13) 0.103(6) Uani 1 1 d U A . C24 C 1.1442(18) 0.5222(12) 0.4032(11) 0.103(5) Uani 1 1 d U A . C50 C 0.2408(7) 0.2409(6) 0.9175(6) 0.034(2) Uani 1 1 d . . . H50A H 0.3242 0.2274 0.9343 0.041 Uiso 1 1 calc R . . H50B H 0.2210 0.2268 0.8571 0.041 Uiso 1 1 calc R . . C51 C 0.1635(8) 0.1974(6) 0.9713(8) 0.048(3) Uani 1 1 d . . . H51 H 0.1911 0.2078 1.0323 0.058 Uiso 1 1 calc R . . C52 C 0.1732(9) 0.1127(6) 0.9571(9) 0.062(3) Uani 1 1 d . . . H52A H 0.1468 0.1009 0.8976 0.092 Uiso 1 1 calc R . . H52B H 0.1236 0.0864 0.9942 0.092 Uiso 1 1 calc R . . H52C H 0.2554 0.0971 0.9707 0.092 Uiso 1 1 calc R . . C53 C 0.0361(8) 0.2255(7) 0.9536(7) 0.049(3) Uani 1 1 d . . . H53A H 0.0044 0.2115 0.8950 0.059 Uiso 1 1 calc R . . H53B H -0.0129 0.2010 0.9933 0.059 Uiso 1 1 calc R . . C54 C 0.0271(8) 0.3084(7) 0.9634(7) 0.051(3) Uani 1 1 d . . . H54A H 0.0524 0.3217 1.0233 0.061 Uiso 1 1 calc R . . H54B H -0.0564 0.3233 0.9505 0.061 Uiso 1 1 calc R . . C55 C 0.1016(7) 0.3524(6) 0.9057(6) 0.034(2) Uani 1 1 d . . . H55 H 0.0748 0.3368 0.8461 0.041 Uiso 1 1 calc R . . C56 C 0.0896(8) 0.4351(6) 0.9081(7) 0.044(2) Uani 1 1 d . . . H56 H 0.1463 0.4562 0.8705 0.053 Uiso 1 1 calc R . . C57 C -0.0344(9) 0.4609(7) 0.8720(8) 0.054(3) Uani 1 1 d . . . H57A H -0.0920 0.4440 0.9094 0.082 Uiso 1 1 calc R . . H57B H -0.0541 0.4398 0.8151 0.082 Uiso 1 1 calc R . . H57C H -0.0361 0.5154 0.8684 0.082 Uiso 1 1 calc R . . C58 C 0.1195(12) 0.4703(8) 0.9969(8) 0.067(4) Uani 1 1 d . . . H58A H 0.1981 0.4542 1.0210 0.101 Uiso 1 1 calc R . . H58B H 0.0611 0.4545 1.0343 0.101 Uiso 1 1 calc R . . H58C H 0.1181 0.5247 0.9918 0.101 Uiso 1 1 calc R . . C59 C 0.2268(7) 0.3228(5) 0.9263(6) 0.030(2) Uani 1 1 d D . . H59 H 0.2532 0.3359 0.9868 0.036 Uiso 1 1 calc R . . C60 C 0.6770(9) 0.2738(6) 0.4239(6) 0.040(2) Uani 1 1 d . A . H60A H 0.7392 0.2357 0.4365 0.047 Uiso 1 1 calc R . . H60B H 0.6416 0.2668 0.3644 0.047 Uiso 1 1 calc R . . C61 C 0.5820(10) 0.2641(7) 0.4844(7) 0.050(3) Uani 1 1 d . . . H61 H 0.6217 0.2669 0.5439 0.061 Uiso 1 1 calc R . . C62 C 0.5247(16) 0.1868(10) 0.4723(10) 0.098(6) Uani 1 1 d . . . H62A H 0.4871 0.1820 0.4138 0.147 Uiso 1 1 calc R . . H62B H 0.4653 0.1808 0.5120 0.147 Uiso 1 1 calc R . . H62C H 0.5853 0.1483 0.4833 0.147 Uiso 1 1 calc R . . C63 C 0.4940(9) 0.3275(8) 0.4726(8) 0.064(4) Uani 1 1 d . . . H63A H 0.4494 0.3236 0.4154 0.077 Uiso 1 1 calc R . . H63B H 0.4370 0.3226 0.5152 0.077 Uiso 1 1 calc R . . C64 C 0.5514(8) 0.4029(7) 0.4818(7) 0.048(3) Uani 1 1 d . . . H64A H 0.5907 0.4083 0.5405 0.057 Uiso 1 1 calc R . . H64B H 0.4899 0.4418 0.4728 0.057 Uiso 1 1 calc R . . C65 C 0.6425(8) 0.4147(6) 0.4184(6) 0.039(2) Uani 1 1 d . A . H65 H 0.6010 0.4085 0.3597 0.046 Uiso 1 1 calc R . . C66 C 0.6981(11) 0.4923(7) 0.4238(7) 0.054(3) Uani 1 1 d . . . H66 H 0.7613 0.4921 0.3847 0.065 Uiso 1 1 calc R . . C67 C 0.7561(13) 0.5124(8) 0.5092(8) 0.078(4) Uani 1 1 d . . . H67A H 0.8165 0.4752 0.5275 0.118 Uiso 1 1 calc R . . H67B H 0.6971 0.5136 0.5498 0.118 Uiso 1 1 calc R . . H67C H 0.7929 0.5615 0.5067 0.118 Uiso 1 1 calc R . . C68 C 0.6101(18) 0.5516(9) 0.3906(11) 0.111(7) Uani 1 1 d . . . H68A H 0.5602 0.5645 0.4351 0.166 Uiso 1 1 calc R . . H68B H 0.5608 0.5326 0.3407 0.166 Uiso 1 1 calc R . . H68C H 0.6525 0.5960 0.3747 0.166 Uiso 1 1 calc R . . C69 C 0.7305(7) 0.3508(6) 0.4343(5) 0.035(2) Uani 1 1 d . . . H69 H 0.7703 0.3554 0.4936 0.043 Uiso 1 1 calc R A . O1 O 0.5412(5) 0.2947(4) 0.8798(4) 0.0381(15) Uani 1 1 d . . . O2 O 0.5033(5) 0.4451(4) 0.8318(4) 0.0373(15) Uani 1 1 d . . . O3 O 0.4731(5) 0.3934(4) 1.0031(4) 0.0329(14) Uani 1 1 d . . . O4 O 0.3089(4) 0.3616(3) 0.8716(3) 0.0287(14) Uani 1 1 d D . . H4 H 0.271(4) 0.370(5) 0.822(2) 0.034 Uiso 1 1 d D . . O6 O 1.0007(6) 0.3336(5) 0.4988(4) 0.0499(19) Uani 1 1 d . A . O8 O 0.8227(5) 0.3569(4) 0.3735(4) 0.0375(16) Uani 1 1 d D A . H8 H 0.795(8) 0.382(5) 0.329(4) 0.045 Uiso 1 1 d D . . F1 F 0.5713(8) 0.1578(4) 0.9286(7) 0.101(2) Uani 1 1 d . . . F2 F 0.7470(6) 0.2045(5) 0.9258(6) 0.092(3) Uani 1 1 d . . . F3 F 0.6701(8) 0.1286(4) 0.8268(7) 0.101(2) Uani 1 1 d . . . F4 F 0.4277(7) 0.1740(5) 0.7821(5) 0.095(3) Uani 1 1 d . . . F5 F 0.5414(10) 0.1980(6) 0.6863(6) 0.128(5) Uani 1 1 d . . . F6 F 0.4280(7) 0.2839(6) 0.7262(5) 0.089(3) Uani 1 1 d . . . F7 F 0.6452(6) 0.3381(4) 0.7222(4) 0.0606(17) Uani 1 1 d . . . F8 F 0.7514(6) 0.3350(5) 0.8412(5) 0.077(2) Uani 1 1 d . . . F9 F 0.7641(7) 0.2463(5) 0.7531(6) 0.098(3) Uani 1 1 d . . . F10 F 0.6919(5) 0.5312(4) 0.8480(5) 0.0652(19) Uani 1 1 d . . . F11 F 0.6437(6) 0.5178(5) 0.7141(5) 0.082(2) Uani 1 1 d . . . F12 F 0.6056(6) 0.6214(4) 0.7740(6) 0.081(2) Uani 1 1 d . . . F13 F 0.3965(7) 0.5789(5) 0.6805(5) 0.090(3) Uani 1 1 d . . . F14 F 0.2948(5) 0.4984(4) 0.7388(4) 0.0596(18) Uani 1 1 d . . . F15 F 0.4327(7) 0.4617(5) 0.6683(5) 0.081(2) Uani 1 1 d . . . F16 F 0.3921(6) 0.6287(4) 0.8392(5) 0.0680(19) Uani 1 1 d . . . F17 F 0.3536(5) 0.5298(4) 0.9052(4) 0.0576(17) Uani 1 1 d . . . F18 F 0.5211(6) 0.5821(4) 0.9323(4) 0.0624(18) Uani 1 1 d . . . F19 F 0.3995(7) 0.4821(4) 1.1160(4) 0.0646(18) Uani 1 1 d . . . F20 F 0.5325(14) 0.4521(6) 1.2138(5) 0.150(6) Uani 1 1 d . . . F21 F 0.5836(8) 0.5156(4) 1.1024(5) 0.087(3) Uani 1 1 d . . . F22 F 0.5623(9) 0.3005(5) 1.1958(5) 0.093(3) Uani 1 1 d . . . F23 F 0.3761(10) 0.3403(6) 1.1503(4) 0.099(3) Uani 1 1 d . . . F24 F 0.4731(7) 0.2618(4) 1.0773(5) 0.071(2) Uani 1 1 d . . . F25 F 0.6903(9) 0.3053(6) 1.0612(7) 0.124(4) Uani 1 1 d . . . F26 F 0.6999(6) 0.4211(6) 1.0145(8) 0.103(3) Uani 1 1 d . . . F27 F 0.7253(9) 0.4011(5) 1.1516(7) 0.135(5) Uani 1 1 d . . . F28 F 0.9302(7) 0.0839(5) 0.2629(6) 0.085(2) Uani 1 1 d . . . F29 F 0.8888(11) 0.1439(11) 0.3725(6) 0.166(6) Uani 1 1 d . . . F30 F 1.0617(10) 0.1053(7) 0.3650(6) 0.129(4) Uani 1 1 d . . . F31 F 0.9062(6) 0.1889(5) 0.1427(4) 0.072(2) Uani 1 1 d . . . F32 F 0.7997(7) 0.2246(7) 0.2352(5) 0.114(4) Uani 1 1 d . . . F33 F 0.9127(11) 0.2988(6) 0.1911(9) 0.159(6) Uani 1 1 d . . . F34 F 1.1282(5) 0.1421(4) 0.2020(4) 0.0622(19) Uani 1 1 d . . . F35 F 1.2070(6) 0.2049(6) 0.3079(6) 0.098(3) Uani 1 1 d . . . F36 F 1.1362(11) 0.2592(6) 0.1953(7) 0.124(4) Uani 1 1 d . . . F37 F 1.2004(5) 0.2573(5) 0.4913(4) 0.067(2) Uani 1 1 d . . . F38 F 1.0754(6) 0.1811(4) 0.5403(5) 0.072(2) Uani 1 1 d . . . F39 F 1.2201(6) 0.2289(5) 0.6235(4) 0.075(2) Uani 1 1 d . . . F40 F 0.9146(5) 0.3442(4) 0.6613(4) 0.0546(16) Uani 1 1 d . . . F41 F 0.8835(5) 0.2429(4) 0.5890(4) 0.0509(15) Uani 1 1 d . . . F42 F 1.0137(5) 0.2433(4) 0.6978(4) 0.0533(16) Uani 1 1 d . . . F43 F 1.1676(6) 0.3575(4) 0.6994(3) 0.0608(19) Uani 1 1 d . . . F44 F 1.0740(6) 0.4356(4) 0.6123(5) 0.0631(18) Uani 1 1 d . . . F45 F 1.2328(5) 0.3804(4) 0.5770(4) 0.0652(19) Uani 1 1 d . . . F46 F 1.2590(8) 0.3907(5) 0.3348(6) 0.097(3) Uani 1 1 d . . . F47 F 1.1734(14) 0.4180(7) 0.2085(8) 0.154(5) Uani 1 1 d . . . F48 F 1.2855(7) 0.4988(6) 0.2855(6) 0.103(3) Uani 1 1 d . . . F49 F 0.9417(8) 0.5575(7) 0.3055(8) 0.129(5) Uani 1 1 d . . . F50 F 1.0771(8) 0.5590(5) 0.2150(6) 0.102(3) Uani 1 1 d . . . F51 F 0.9634(9) 0.4685(6) 0.2050(9) 0.149(5) Uani 1 1 d . . . F52 F 1.1681(13) 0.5893(6) 0.3766(7) 0.133(4) Uani 1 1 d . . . F53 F 1.0498(14) 0.5289(11) 0.4485(7) 0.202(9) Uani 1 1 d . . . F54 F 1.2336(9) 0.4895(7) 0.4488(6) 0.119(4) Uani 1 1 d . . . O5A O 0.9935(9) 0.2493(7) 0.3560(7) 0.031(2) Uani 0.606(12) 1 d PU A 1 O5B O 1.0260(15) 0.2826(10) 0.3236(11) 0.031(2) Uani 0.394(12) 1 d PU A 2 O7A O 1.0434(14) 0.4039(12) 0.3361(15) 0.060(7) Uani 0.59(4) 1 d PU A 1 O7B O 1.0377(14) 0.4291(10) 0.385(2) 0.032(7) Uani 0.41(4) 1 d PU A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Al1 0.0184(11) 0.0284(14) 0.0280(13) -0.0016(11) 0.0015(9) -0.0010(10) Al2 0.0232(12) 0.0265(14) 0.0227(12) 0.0009(11) 0.0060(9) -0.0010(10) C1 0.034(5) 0.033(5) 0.059(6) -0.015(4) 0.023(4) -0.006(4) C2 0.100(10) 0.022(6) 0.105(9) 0.009(6) 0.072(7) 0.014(6) C3 0.067(7) 0.103(12) 0.065(7) -0.050(7) 0.040(5) -0.049(8) C4 0.047(6) 0.043(6) 0.074(8) 0.007(6) 0.028(6) -0.003(5) C5 0.028(4) 0.036(6) 0.041(5) 0.003(4) 0.000(4) -0.007(4) C6 0.048(6) 0.041(7) 0.061(7) 0.002(5) 0.012(5) -0.011(5) C7 0.055(6) 0.063(8) 0.040(5) 0.016(6) 0.000(4) -0.022(6) C8 0.032(5) 0.044(6) 0.060(6) -0.008(5) -0.007(4) -0.006(4) C9 0.066(6) 0.029(5) 0.037(5) -0.001(4) -0.018(5) 0.008(5) C10 0.141(14) 0.043(7) 0.056(8) 0.003(6) -0.014(8) 0.022(8) C11 0.161(13) 0.057(8) 0.053(8) 0.035(7) -0.052(9) -0.037(9) C12 0.066(6) 0.067(10) 0.116(12) -0.005(8) -0.060(7) 0.012(7) C13 0.055(6) 0.068(7) 0.032(5) -0.032(5) -0.020(4) 0.036(5) C14 0.068(8) 0.136(12) 0.049(7) 0.038(9) 0.011(7) 0.035(8) C15 0.063(7) 0.054(8) 0.060(7) -0.010(6) -0.033(6) 0.023(6) C16 0.048(5) 0.063(8) 0.070(8) -0.030(7) -0.005(5) -0.001(5) C17 0.036(5) 0.047(6) 0.018(4) -0.004(4) -0.004(3) 0.003(4) C18 0.044(6) 0.076(8) 0.057(7) -0.022(6) -0.017(5) 0.023(6) C19 0.048(6) 0.057(8) 0.051(7) 0.005(6) 0.003(5) -0.010(5) C20 0.056(6) 0.059(7) 0.046(6) 0.004(5) 0.006(5) -0.016(5) C21 0.048(6) 0.038(6) 0.091(8) 0.040(5) 0.012(5) -0.007(5) C22 0.085(9) 0.066(10) 0.099(11) 0.014(8) 0.024(8) 0.012(8) C23 0.082(10) 0.072(11) 0.146(14) 0.040(11) -0.030(10) -0.002(8) C24 0.138(14) 0.099(13) 0.075(9) 0.009(8) 0.028(8) 0.030(11) C50 0.027(4) 0.040(6) 0.037(5) 0.001(4) 0.004(4) -0.001(4) C51 0.036(5) 0.038(6) 0.068(7) 0.028(6) -0.001(5) -0.005(5) C52 0.037(6) 0.039(7) 0.107(10) 0.026(7) -0.001(6) -0.001(5) C53 0.030(5) 0.063(8) 0.056(6) 0.025(6) 0.010(4) -0.001(5) C54 0.025(5) 0.077(9) 0.051(6) 0.030(6) 0.010(4) 0.000(5) C55 0.025(4) 0.041(6) 0.037(5) 0.009(4) 0.005(3) -0.005(4) C56 0.032(5) 0.049(7) 0.051(6) 0.003(5) 0.007(4) 0.007(5) C57 0.037(5) 0.047(7) 0.081(8) 0.014(6) 0.016(5) 0.005(5) C58 0.072(8) 0.064(9) 0.064(8) -0.032(7) 0.002(6) 0.012(7) C59 0.023(4) 0.032(5) 0.036(5) 0.011(4) 0.007(3) -0.006(4) C60 0.052(6) 0.033(6) 0.033(5) -0.001(4) 0.004(4) -0.002(4) C61 0.060(7) 0.055(7) 0.037(6) -0.005(5) 0.007(5) -0.017(6) C62 0.115(13) 0.111(15) 0.069(10) 0.004(9) 0.014(9) -0.049(11) C63 0.035(5) 0.086(10) 0.075(8) -0.006(7) 0.017(5) -0.005(6) C64 0.030(5) 0.066(8) 0.048(6) -0.013(6) 0.009(4) 0.012(5) C65 0.045(5) 0.040(6) 0.029(5) -0.003(4) -0.004(4) 0.016(5) C66 0.075(8) 0.045(7) 0.040(6) 0.002(5) -0.001(5) 0.003(6) C67 0.102(10) 0.055(8) 0.070(9) 0.003(7) -0.027(7) -0.028(8) C68 0.179(19) 0.049(9) 0.091(11) -0.007(9) -0.039(12) 0.028(11) C69 0.026(4) 0.060(7) 0.021(4) 0.000(4) 0.009(3) 0.008(4) O1 0.034(3) 0.031(4) 0.049(4) -0.010(3) 0.003(3) 0.005(3) O2 0.038(3) 0.024(4) 0.051(4) 0.003(3) 0.007(3) -0.004(3) O3 0.031(3) 0.043(4) 0.024(3) 0.000(3) -0.003(2) 0.004(3) O4 0.020(3) 0.041(4) 0.026(3) 0.005(3) 0.004(2) -0.002(3) O6 0.045(3) 0.082(6) 0.022(3) 0.001(4) 0.000(3) 0.026(4) O8 0.025(3) 0.058(5) 0.031(3) 0.013(3) 0.010(2) 0.013(3) F1 0.133(5) 0.033(3) 0.157(6) 0.008(3) 0.106(5) 0.015(3) F2 0.047(4) 0.085(6) 0.147(8) 0.053(6) 0.025(5) 0.028(4) F3 0.133(5) 0.033(3) 0.157(6) 0.008(3) 0.106(5) 0.015(3) F4 0.102(6) 0.104(7) 0.090(6) -0.062(5) 0.058(5) -0.076(5) F5 0.164(9) 0.137(9) 0.100(6) -0.084(7) 0.097(7) -0.095(8) F6 0.058(4) 0.149(9) 0.056(4) -0.027(5) -0.002(4) -0.027(5) F7 0.066(4) 0.060(4) 0.061(4) 0.006(4) 0.028(3) -0.006(4) F8 0.052(4) 0.077(5) 0.099(5) 0.021(5) -0.006(4) -0.040(4) F9 0.083(5) 0.069(5) 0.161(8) 0.010(5) 0.098(6) 0.005(4) F10 0.028(3) 0.075(5) 0.092(5) 0.000(4) -0.001(3) -0.004(3) F11 0.066(4) 0.104(6) 0.084(5) -0.002(5) 0.041(4) -0.024(4) F12 0.051(4) 0.061(5) 0.131(7) 0.034(5) 0.004(4) -0.023(3) F13 0.097(6) 0.090(6) 0.075(5) 0.043(5) -0.027(4) -0.018(5) F14 0.032(3) 0.073(5) 0.070(4) 0.011(4) -0.010(3) -0.015(3) F15 0.084(5) 0.104(7) 0.056(4) -0.017(5) 0.010(4) -0.015(5) F16 0.064(4) 0.034(4) 0.106(6) 0.007(4) 0.008(4) 0.004(3) F17 0.044(3) 0.053(4) 0.080(4) -0.018(3) 0.027(3) -0.004(3) F18 0.058(4) 0.054(4) 0.073(4) -0.019(4) -0.005(3) 0.003(3) F19 0.086(5) 0.046(4) 0.063(4) -0.011(3) 0.013(4) 0.015(4) F20 0.290(16) 0.100(8) 0.045(5) -0.031(5) -0.057(7) 0.074(9) F21 0.120(7) 0.043(4) 0.092(6) -0.013(4) -0.014(5) -0.024(4) F22 0.146(8) 0.075(6) 0.046(4) 0.020(4) -0.035(4) 0.011(5) F23 0.158(9) 0.097(7) 0.047(4) -0.001(4) 0.035(5) -0.058(7) F24 0.113(6) 0.026(3) 0.069(4) -0.003(3) -0.017(4) 0.008(3) F25 0.111(7) 0.103(8) 0.139(8) -0.047(6) -0.065(6) 0.074(6) F26 0.032(4) 0.093(7) 0.182(10) -0.014(7) 0.007(5) -0.001(4) F27 0.119(7) 0.077(6) 0.177(10) -0.027(6) -0.120(8) 0.018(5) F28 0.080(5) 0.086(6) 0.090(6) 0.004(5) 0.019(4) -0.020(5) F29 0.132(9) 0.30(2) 0.070(6) 0.000(9) 0.050(6) 0.034(11) F30 0.135(9) 0.151(11) 0.091(7) 0.037(7) -0.032(6) 0.039(8) F31 0.069(4) 0.108(6) 0.036(3) -0.024(4) -0.014(3) 0.006(4) F32 0.055(4) 0.198(12) 0.079(5) -0.077(6) -0.030(4) 0.060(6) F33 0.169(11) 0.077(7) 0.197(12) 0.016(8) -0.134(10) 0.006(7) F34 0.049(3) 0.065(5) 0.076(4) -0.035(4) 0.020(3) -0.002(3) F35 0.050(4) 0.140(8) 0.099(6) -0.070(6) -0.015(4) 0.021(5) F36 0.144(9) 0.094(8) 0.131(9) 0.012(7) -0.002(7) -0.055(7) F37 0.035(3) 0.113(6) 0.054(4) -0.024(4) 0.006(3) 0.023(3) F38 0.066(4) 0.046(4) 0.099(6) -0.029(4) -0.009(4) 0.006(3) F39 0.052(4) 0.106(6) 0.061(4) -0.006(4) -0.021(3) 0.036(4) F40 0.050(3) 0.071(4) 0.047(3) -0.006(3) 0.024(3) 0.007(3) F41 0.032(3) 0.052(4) 0.067(4) -0.015(3) -0.003(3) -0.009(3) F42 0.053(3) 0.055(4) 0.050(4) 0.021(3) -0.001(3) -0.013(3) F43 0.070(4) 0.081(5) 0.030(3) -0.010(3) -0.001(3) -0.026(4) F44 0.083(5) 0.036(4) 0.073(5) -0.002(3) 0.025(4) -0.006(3) F45 0.051(3) 0.076(5) 0.072(4) 0.010(4) 0.020(3) -0.025(3) F46 0.108(6) 0.072(6) 0.109(6) 0.001(5) -0.004(5) 0.043(5) F47 0.236(15) 0.112(10) 0.109(8) -0.043(7) 0.000(9) 0.054(10) F48 0.061(4) 0.133(9) 0.122(7) 0.034(6) 0.042(5) -0.003(5) F49 0.072(5) 0.160(11) 0.160(10) 0.066(9) 0.034(6) 0.057(7) F50 0.116(7) 0.095(7) 0.087(6) 0.064(5) -0.019(5) -0.025(6) F51 0.108(8) 0.096(8) 0.216(13) 0.027(8) -0.105(9) -0.023(6) F52 0.239(14) 0.053(6) 0.099(7) -0.018(5) -0.014(8) 0.005(7) F53 0.230(14) 0.30(2) 0.094(7) 0.053(10) 0.089(9) 0.175(15) F54 0.124(8) 0.125(9) 0.094(7) 0.034(6) -0.041(6) 0.009(7) O5A 0.038(5) 0.030(7) 0.023(6) -0.009(4) -0.002(4) 0.011(5) O5B 0.038(5) 0.030(7) 0.023(6) -0.009(4) -0.002(4) 0.011(5) O7A 0.084(10) 0.056(11) 0.042(12) 0.009(10) 0.013(8) -0.048(8) O7B 0.045(9) 0.017(10) 0.036(15) 0.001(9) 0.012(8) -0.009(7) _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 O1 1.697(7) . ? Al1 O2 1.706(7) . ? Al1 O3 1.708(6) . ? Al1 O4 1.835(5) . ? Al2 O6 1.670(7) . ? Al2 O8 1.824(6) . ? Al2 O5A 1.736(11) . ? Al2 O5B 1.623(16) . ? Al2 O7A 1.670(13) . ? Al2 O7B 1.742(17) . ? C1 C2 1.547(17) . ? C1 C3 1.525(17) . ? C1 C4 1.544(14) . ? C1 O1 1.332(11) . ? C2 F1 1.332(13) . ? C2 F2 1.346(19) . ? C2 F3 1.328(15) . ? C3 F4 1.337(15) . ? C3 F5 1.321(13) . ? C3 F6 1.38(2) . ? C4 F7 1.338(14) . ? C4 F8 1.324(14) . ? C4 F9 1.331(13) . ? C5 C6 1.555(14) . ? C5 C7 1.552(14) . ? C5 C8 1.579(15) . ? C5 O2 1.337(12) . ? C6 F10 1.335(13) . ? C6 F11 1.333(13) . ? C6 F12 1.326(13) . ? C7 F13 1.328(15) . ? C7 F14 1.317(12) . ? C7 F15 1.319(15) . ? C8 F16 1.320(13) . ? C8 F17 1.334(13) . ? C8 F18 1.307(12) . ? C9 C10 1.550(18) . ? C9 C11 1.497(18) . ? C9 C12 1.58(2) . ? C9 O3 1.354(11) . ? C10 F19 1.315(18) . ? C10 F20 1.332(16) . ? C10 F21 1.373(19) . ? C11 F22 1.342(14) . ? C11 F23 1.47(2) . ? C11 F24 1.312(17) . ? C12 F25 1.376(18) . ? C12 F26 1.28(2) . ? C12 F27 1.383(17) . ? C13 C14 1.55(2) . ? C13 C15 1.562(14) . ? C13 C16 1.539(16) . ? C13 O5A 1.368(14) . ? C13 O5B 1.50(2) . ? C14 F28 1.28(2) . ? C14 F29 1.295(16) . ? C14 F30 1.322(16) . ? C15 F31 1.299(14) . ? C15 F32 1.304(16) . ? C15 F33 1.278(17) . ? C16 F34 1.309(14) . ? C16 F35 1.272(13) . ? C16 F36 1.384(17) . ? C17 C18 1.556(15) . ? C17 C19 1.554(14) . ? C17 C20 1.521(15) . ? C17 O6 1.347(11) . ? C18 F37 1.344(15) . ? C18 F38 1.337(15) . ? C18 F39 1.331(12) . ? C19 F40 1.354(14) . ? C19 F41 1.314(13) . ? C19 F42 1.332(13) . ? C20 F43 1.364(12) . ? C20 F44 1.323(14) . ? C20 F45 1.371(12) . ? C21 C22 1.473(19) . ? C21 C23 1.546(19) . ? C21 C24 1.55(2) . ? C21 O7A 1.384(19) . ? C21 O7B 1.43(2) . ? C22 F46 1.286(17) . ? C22 F47 1.42(2) . ? C22 F48 1.346(18) . ? C23 F49 1.41(2) . ? C23 F50 1.27(2) . ? C23 F51 1.35(2) . ? C24 F52 1.31(2) . ? C24 F53 1.36(2) . ? C24 F54 1.32(2) . ? C50 H50A 0.9900 . ? C50 H50B 0.9900 . ? C50 C51 1.509(13) . ? C50 C59 1.488(14) . ? C51 H51 1.0000 . ? C51 C52 1.543(17) . ? C51 C53 1.536(14) . ? C52 H52A 0.9800 . ? C52 H52B 0.9800 . ? C52 H52C 0.9800 . ? C53 H53A 0.9900 . ? C53 H53B 0.9900 . ? C53 C54 1.501(17) . ? C54 H54A 0.9900 . ? C54 H54B 0.9900 . ? C54 C55 1.533(12) . ? C55 H55 1.0000 . ? C55 C56 1.493(15) . ? C55 C59 1.527(12) . ? C56 H56 1.0000 . ? C56 C57 1.539(14) . ? C56 C58 1.544(16) . ? C57 H57A 0.9800 . ? C57 H57B 0.9800 . ? C57 H57C 0.9800 . ? C58 H58A 0.9800 . ? C58 H58B 0.9800 . ? C58 H58C 0.9800 . ? C59 H59 1.0000 . ? C59 O4 1.514(10) . ? C60 H60A 0.9900 . ? C60 H60B 0.9900 . ? C60 C61 1.533(14) . ? C60 C69 1.514(14) . ? C61 H61 1.0000 . ? C61 C62 1.539(19) . ? C61 C63 1.517(18) . ? C62 H62A 0.9800 . ? C62 H62B 0.9800 . ? C62 H62C 0.9800 . ? C63 H63A 0.9900 . ? C63 H63B 0.9900 . ? C63 C64 1.505(18) . ? C64 H64A 0.9900 . ? C64 H64B 0.9900 . ? C64 C65 1.538(14) . ? C65 H65 1.0000 . ? C65 C66 1.530(16) . ? C65 C69 1.528(13) . ? C66 H66 1.0000 . ? C66 C67 1.481(16) . ? C66 C68 1.518(19) . ? C67 H67A 0.9800 . ? C67 H67B 0.9800 . ? C67 H67C 0.9800 . ? C68 H68A 0.9800 . ? C68 H68B 0.9800 . ? C68 H68C 0.9800 . ? C69 H69 1.0000 . ? C69 O8 1.507(9) . ? O4 H4 0.870(11) . ? O8 H8 0.870(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 O1 Al1 O2 112.4(3) . . ? O1 Al1 O3 111.1(3) . . ? O1 Al1 O4 110.4(3) . . ? O2 Al1 O3 117.6(4) . . ? O2 Al1 O4 104.8(3) . . ? O3 Al1 O4 99.4(3) . . ? O6 Al2 O8 101.6(3) . . ? O6 Al2 O5A 105.6(5) . . ? O6 Al2 O7B 96.7(11) . . ? O5A Al2 O8 102.8(4) . . ? O5A Al2 O7B 142.6(9) . . ? O5B Al2 O6 128.2(7) . . ? O5B Al2 O8 112.1(6) . . ? O5B Al2 O5A 30.7(6) . . ? O5B Al2 O7A 83.6(13) . . ? O5B Al2 O7B 112.8(12) . . ? O7A Al2 O6 124.4(9) . . ? O7A Al2 O8 105.4(7) . . ? O7A Al2 O5A 114.3(11) . . ? O7A Al2 O7B 30.8(6) . . ? O7B Al2 O8 101.5(6) . . ? C3 C1 C2 111.4(11) . . ? C3 C1 C4 107.3(9) . . ? C4 C1 C2 109.0(9) . . ? O1 C1 C2 107.7(9) . . ? O1 C1 C3 110.1(9) . . ? O1 C1 C4 111.4(9) . . ? F1 C2 C1 109.6(10) . . ? F1 C2 F2 108.9(13) . . ? F2 C2 C1 111.2(10) . . ? F3 C2 C1 110.9(12) . . ? F3 C2 F1 106.4(10) . . ? F3 C2 F2 109.7(11) . . ? F4 C3 C1 111.4(12) . . ? F4 C3 F6 105.3(11) . . ? F5 C3 C1 116.3(11) . . ? F5 C3 F4 107.6(11) . . ? F5 C3 F6 105.4(14) . . ? F6 C3 C1 110.1(10) . . ? F7 C4 C1 112.7(9) . . ? F8 C4 C1 110.7(9) . . ? F8 C4 F7 105.9(10) . . ? F8 C4 F9 106.9(10) . . ? F9 C4 C1 112.5(10) . . ? F9 C4 F7 107.9(9) . . ? C6 C5 C8 107.4(8) . . ? C7 C5 C6 110.4(8) . . ? C7 C5 C8 109.3(8) . . ? O2 C5 C6 110.7(8) . . ? O2 C5 C7 108.7(9) . . ? O2 C5 C8 110.3(8) . . ? F10 C6 C5 109.4(9) . . ? F11 C6 C5 109.9(9) . . ? F11 C6 F10 106.9(9) . . ? F12 C6 C5 112.8(9) . . ? F12 C6 F10 109.4(9) . . ? F12 C6 F11 108.3(10) . . ? F13 C7 C5 112.3(10) . . ? F14 C7 C5 110.1(8) . . ? F14 C7 F13 107.1(10) . . ? F14 C7 F15 108.0(10) . . ? F15 C7 C5 109.8(10) . . ? F15 C7 F13 109.4(9) . . ? F16 C8 C5 113.6(9) . . ? F16 C8 F17 106.7(8) . . ? F17 C8 C5 109.4(8) . . ? F18 C8 C5 110.5(8) . . ? F18 C8 F16 108.8(9) . . ? F18 C8 F17 107.5(9) . . ? C10 C9 C12 109.9(12) . . ? C11 C9 C10 113.3(12) . . ? C11 C9 C12 107.2(12) . . ? O3 C9 C10 108.3(9) . . ? O3 C9 C11 109.1(9) . . ? O3 C9 C12 108.9(10) . . ? F19 C10 C9 110.4(12) . . ? F19 C10 F20 106.0(14) . . ? F19 C10 F21 111.2(11) . . ? F20 C10 C9 110.6(11) . . ? F20 C10 F21 111.1(14) . . ? F21 C10 C9 107.6(13) . . ? F22 C11 C9 115.2(13) . . ? F22 C11 F23 108.3(14) . . ? F23 C11 C9 104.7(12) . . ? F24 C11 C9 115.8(13) . . ? F24 C11 F22 108.0(12) . . ? F24 C11 F23 104.0(12) . . ? F25 C12 C9 108.3(13) . . ? F25 C12 F27 108.9(11) . . ? F26 C12 C9 110.9(10) . . ? F26 C12 F25 112.9(17) . . ? F26 C12 F27 110.1(14) . . ? F27 C12 C9 105.5(14) . . ? C14 C13 C15 108.7(11) . . ? C16 C13 C14 109.0(10) . . ? C16 C13 C15 109.6(10) . . ? O5A C13 C14 98.0(11) . . ? O5A C13 C15 112.9(9) . . ? O5A C13 C16 117.8(10) . . ? O5A C13 O5B 36.0(7) . . ? O5B C13 C14 133.5(12) . . ? O5B C13 C15 100.0(10) . . ? O5B C13 C16 94.2(11) . . ? F28 C14 C13 114.0(10) . . ? F28 C14 F29 112.4(16) . . ? F28 C14 F30 108.8(16) . . ? F29 C14 C13 107.3(16) . . ? F29 C14 F30 107.3(12) . . ? F30 C14 C13 106.7(14) . . ? F31 C15 C13 113.4(9) . . ? F31 C15 F32 107.8(10) . . ? F32 C15 C13 109.8(11) . . ? F33 C15 C13 111.1(11) . . ? F33 C15 F31 110.5(13) . . ? F33 C15 F32 103.7(12) . . ? F34 C16 C13 112.8(10) . . ? F34 C16 F36 103.1(10) . . ? F35 C16 C13 113.4(11) . . ? F35 C16 F34 111.6(11) . . ? F35 C16 F36 105.3(11) . . ? F36 C16 C13 109.8(11) . . ? C19 C17 C18 108.3(9) . . ? C20 C17 C18 108.9(8) . . ? C20 C17 C19 109.3(8) . . ? O6 C17 C18 111.3(8) . . ? O6 C17 C19 108.9(8) . . ? O6 C17 C20 110.1(9) . . ? F37 C18 C17 109.5(11) . . ? F38 C18 C17 109.9(8) . . ? F38 C18 F37 108.7(10) . . ? F39 C18 C17 113.3(9) . . ? F39 C18 F37 106.2(9) . . ? F39 C18 F38 109.1(12) . . ? F40 C19 C17 108.0(9) . . ? F41 C19 C17 110.5(9) . . ? F41 C19 F40 107.9(9) . . ? F41 C19 F42 108.4(9) . . ? F42 C19 C17 113.1(9) . . ? F42 C19 F40 108.7(9) . . ? F43 C20 C17 112.9(9) . . ? F43 C20 F45 106.3(8) . . ? F44 C20 C17 111.7(9) . . ? F44 C20 F43 107.3(10) . . ? F44 C20 F45 108.9(9) . . ? F45 C20 C17 109.5(9) . . ? C22 C21 C23 111.4(13) . . ? C22 C21 C24 105.3(12) . . ? C23 C21 C24 109.5(13) . . ? O7A C21 C22 99.1(15) . . ? O7A C21 C23 107.3(12) . . ? O7A C21 C24 123.6(16) . . ? O7A C21 O7B 37.6(8) . . ? O7B C21 C22 123.2(12) . . ? O7B C21 C23 115.5(13) . . ? O7B C21 C24 87.7(16) . . ? F46 C22 C21 114.5(13) . . ? F46 C22 F47 107.2(13) . . ? F46 C22 F48 107.7(13) . . ? F47 C22 C21 108.3(14) . . ? F48 C22 C21 112.7(13) . . ? F48 C22 F47 105.9(13) . . ? F49 C23 C21 106.6(15) . . ? F50 C23 C21 114.1(13) . . ? F50 C23 F49 112.1(15) . . ? F50 C23 F51 104.7(18) . . ? F51 C23 C21 107.5(14) . . ? F51 C23 F49 111.9(14) . . ? F52 C24 C21 110.7(13) . . ? F52 C24 F53 106.9(17) . . ? F52 C24 F54 114.0(19) . . ? F53 C24 C21 104.2(17) . . ? F54 C24 C21 109.4(15) . . ? F54 C24 F53 111.1(14) . . ? H50A C50 H50B 107.8 . . ? C51 C50 H50A 109.1 . . ? C51 C50 H50B 109.1 . . ? C59 C50 H50A 109.1 . . ? C59 C50 H50B 109.1 . . ? C59 C50 C51 112.6(8) . . ? C50 C51 H51 107.8 . . ? C50 C51 C52 111.9(10) . . ? C50 C51 C53 109.1(8) . . ? C52 C51 H51 107.8 . . ? C53 C51 H51 107.8 . . ? C53 C51 C52 112.3(9) . . ? C51 C52 H52A 109.5 . . ? C51 C52 H52B 109.5 . . ? C51 C52 H52C 109.5 . . ? H52A C52 H52B 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? C51 C53 H53A 109.1 . . ? C51 C53 H53B 109.1 . . ? H53A C53 H53B 107.8 . . ? C54 C53 C51 112.5(9) . . ? C54 C53 H53A 109.1 . . ? C54 C53 H53B 109.1 . . ? C53 C54 H54A 108.8 . . ? C53 C54 H54B 108.8 . . ? C53 C54 C55 113.7(9) . . ? H54A C54 H54B 107.7 . . ? C55 C54 H54A 108.8 . . ? C55 C54 H54B 108.8 . . ? C54 C55 H55 106.5 . . ? C56 C55 C54 116.1(9) . . ? C56 C55 H55 106.5 . . ? C56 C55 C59 115.4(8) . . ? C59 C55 C54 105.1(7) . . ? C59 C55 H55 106.5 . . ? C55 C56 H56 107.1 . . ? C55 C56 C57 111.9(9) . . ? C55 C56 C58 114.8(10) . . ? C57 C56 H56 107.1 . . ? C57 C56 C58 108.5(9) . . ? C58 C56 H56 107.1 . . ? C56 C57 H57A 109.5 . . ? C56 C57 H57B 109.5 . . ? C56 C57 H57C 109.5 . . ? H57A C57 H57B 109.5 . . ? H57A C57 H57C 109.5 . . ? H57B C57 H57C 109.5 . . ? C56 C58 H58A 109.5 . . ? C56 C58 H58B 109.5 . . ? C56 C58 H58C 109.5 . . ? H58A C58 H58B 109.5 . . ? H58A C58 H58C 109.5 . . ? H58B C58 H58C 109.5 . . ? C50 C59 C55 115.6(8) . . ? C50 C59 H59 107.3 . . ? C50 C59 O4 108.9(7) . . ? C55 C59 H59 107.3 . . ? O4 C59 C55 109.9(6) . . ? O4 C59 H59 107.3 . . ? H60A C60 H60B 108.2 . . ? C61 C60 H60A 109.7 . . ? C61 C60 H60B 109.7 . . ? C69 C60 H60A 109.7 . . ? C69 C60 H60B 109.7 . . ? C69 C60 C61 109.9(8) . . ? C60 C61 H61 107.7 . . ? C60 C61 C62 110.2(10) . . ? C62 C61 H61 107.7 . . ? C63 C61 C60 110.1(9) . . ? C63 C61 H61 107.7 . . ? C63 C61 C62 113.3(11) . . ? C61 C62 H62A 109.5 . . ? C61 C62 H62B 109.5 . . ? C61 C62 H62C 109.5 . . ? H62A C62 H62B 109.5 . . ? H62A C62 H62C 109.5 . . ? H62B C62 H62C 109.5 . . ? C61 C63 H63A 109.0 . . ? C61 C63 H63B 109.0 . . ? H63A C63 H63B 107.8 . . ? C64 C63 C61 112.8(8) . . ? C64 C63 H63A 109.0 . . ? C64 C63 H63B 109.0 . . ? C63 C64 H64A 109.1 . . ? C63 C64 H64B 109.1 . . ? C63 C64 C65 112.3(9) . . ? H64A C64 H64B 107.9 . . ? C65 C64 H64A 109.1 . . ? C65 C64 H64B 109.1 . . ? C64 C65 H65 107.7 . . ? C66 C65 C64 113.3(9) . . ? C66 C65 H65 107.7 . . ? C69 C65 C64 105.5(8) . . ? C69 C65 H65 107.7 . . ? C69 C65 C66 114.5(8) . . ? C65 C66 H66 106.5 . . ? C67 C66 C65 114.4(10) . . ? C67 C66 H66 106.5 . . ? C67 C66 C68 110.9(12) . . ? C68 C66 C65 111.4(11) . . ? C68 C66 H66 106.5 . . ? C66 C67 H67A 109.5 . . ? C66 C67 H67B 109.5 . . ? C66 C67 H67C 109.5 . . ? H67A C67 H67B 109.5 . . ? H67A C67 H67C 109.5 . . ? H67B C67 H67C 109.5 . . ? C66 C68 H68A 109.5 . . ? C66 C68 H68B 109.5 . . ? C66 C68 H68C 109.5 . . ? H68A C68 H68B 109.5 . . ? H68A C68 H68C 109.5 . . ? H68B C68 H68C 109.5 . . ? C60 C69 C65 114.8(7) . . ? C60 C69 H69 108.4 . . ? C65 C69 H69 108.4 . . ? O8 C69 C60 107.4(7) . . ? O8 C69 C65 109.4(7) . . ? O8 C69 H69 108.4 . . ? C1 O1 Al1 148.9(7) . . ? C5 O2 Al1 151.2(6) . . ? C9 O3 Al1 148.6(6) . . ? Al1 O4 H4 124(2) . . ? C59 O4 Al1 126.5(5) . . ? C59 O4 H4 109(2) . . ? C17 O6 Al2 152.9(6) . . ? Al2 O8 H8 119(7) . . ? C69 O8 Al2 129.0(5) . . ? C69 O8 H8 110(7) . . ? C13 O5A Al2 143.3(10) . . ? C13 O5B Al2 141.5(15) . . ? C21 O7A Al2 153(2) . . ? C21 O7B Al2 138(2) . . ? ###end compound 4a data_p21c _audit_creation_date 2012-08-09 _audit_creation_method ; Olex2 1.1 (compiled 2011.11.01 svn.r2039, GUI svn.r3906) ; _publ_contact_author_address ? _publ_contact_author_email ? _publ_contact_author_name '' _publ_contact_author_phone ? _chemical_name_common ? _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C24 Al2 F55 O6, C9 H13' _chemical_formula_sum 'C33 H13 Al2 F55 O6' _chemical_formula_weight 1604.39 _chemical_melting_point ? 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' _space_group_crystal_system 'monoclinic' _space_group_IT_number 14 _space_group_name_H-M_alt 'P 1 21/c 1' _space_group_name_Hall '-P 2ybc' loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 'x, y, z' 2 '-x, y+1/2, -z+1/2' 3 '-x, -y, -z' 4 'x, -y-1/2, z-1/2' _cell_length_a 10.447(2) _cell_length_b 33.489(7) _cell_length_c 15.380(3) _cell_angle_alpha 90.00 _cell_angle_beta 105.82(3) _cell_angle_gamma 90.00 _cell_volume 5176.8(18) _cell_formula_units_Z 4 _cell_measurement_reflns_used 1000 _cell_measurement_temperature 113 _cell_measurement_theta_max ? _cell_measurement_theta_min ? _exptl_absorpt_coefficient_mu 0.299 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.92 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(ABSCOR; Higashi, 2001)' _exptl_crystal_colour 'clear light colourless' _exptl_crystal_colour_lustre clear _exptl_crystal_colour_modifier light _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 2.059 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_method 'not measured' _exptl_crystal_description plate _exptl_crystal_F_000 3120 _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.08 _exptl_special_details ; ? ; _diffrn_reflns_av_R_equivalents 0.0525 _diffrn_reflns_av_unetI/netI 0.0357 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_k_max 39 _diffrn_reflns_limit_k_min -39 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_number 55110 _diffrn_reflns_theta_full 24.71 _diffrn_reflns_theta_max 24.71 _diffrn_reflns_theta_min 3.00 _diffrn_ambient_temperature 113 _diffrn_detector 'Image Plate' _diffrn_detector_area_resol_mean 10 _diffrn_detector_type 'Rigaku curved IP' _diffrn_measured_fraction_theta_full 0.984 _diffrn_measured_fraction_theta_max 0.984 _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'Rigaku R-AXIS SPIDER IP' _diffrn_measurement_method '\w scans' _diffrn_radiation_collimation '0.5 mm double pinhole' _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.710747 _diffrn_source 'fine-focus sealed tube' _diffrn_source_current 40.0 _diffrn_source_power 2.0 _diffrn_source_target Mo _diffrn_source_voltage 50.0 _diffrn_standards_decay_% ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_number ? _reflns_number_gt 6506 _reflns_number_total 8677 _reflns_threshold_expression >2sigma(I) _computing_cell_refinement 'CrystalClear (Rigaku, 2007)' _computing_data_collection 'CrystalClear (Rigaku, 2007)' _computing_data_reduction 'CrystalClear/FS-PROCESS (Rigaku, 2007)' _computing_molecular_graphics ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_publication_material ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_structure_refinement ; XL, G.M. Sheldrick, Acta Cryst. (2008). A64, 112-122 ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _refine_diff_density_max 0.574 _refine_diff_density_min -0.466 _refine_diff_density_rms 0.096 _refine_ls_extinction_coef ? _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.068 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 963 _refine_ls_number_reflns 8677 _refine_ls_number_restraints 162 _refine_ls_R_factor_all 0.0902 _refine_ls_R_factor_gt 0.0701 _refine_ls_restrained_S_all 1.060 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0463P)^2^+36.5780P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1820 _refine_ls_wR_factor_ref 0.1921 _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. ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap 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 0.10121(14) 0.61518(4) 0.33139(10) 0.0204(3) Uani 1 1 d . A . Al2 Al -0.07413(15) 0.63233(5) 0.10344(10) 0.0227(3) Uani 1 1 d . A . O1 O 0.1832(4) 0.65864(10) 0.3674(3) 0.0303(9) Uani 1 1 d . . . O2 O 0.2077(4) 0.57635(11) 0.3386(3) 0.0303(9) Uani 1 1 d . . . O3 O -0.0296(4) 0.60738(12) 0.3748(3) 0.0358(10) Uani 1 1 d . . . O4 O -0.1783(4) 0.67049(12) 0.1064(3) 0.0418(11) Uani 1 1 d . . . O5 O -0.1566(4) 0.58925(11) 0.0642(3) 0.0297(9) Uani 1 1 d . . . O6 O 0.0508(4) 0.64171(13) 0.0552(3) 0.0416(11) Uani 1 1 d . . . C1 C 0.3043(5) 0.67726(16) 0.3923(4) 0.0272(12) Uani 1 1 d . . . C2 C 0.2437(5) 0.53861(15) 0.3245(4) 0.0274(12) Uani 1 1 d . . . C3 C -0.0786(6) 0.60848(17) 0.4482(4) 0.0307(13) Uani 1 1 d . . . C4 C -0.2093(6) 0.70952(17) 0.1148(5) 0.0379(15) Uani 1 1 d . . . C6 C 0.1005(6) 0.63720(19) -0.0174(4) 0.0356(14) Uani 1 1 d . A . C11 C 0.2842(6) 0.71848(18) 0.4329(5) 0.0409(15) Uani 1 1 d . . . F11 F 0.1765(4) 0.73603(11) 0.3827(3) 0.0660(13) Uani 1 1 d . . . F12 F 0.3863(4) 0.74310(10) 0.4392(3) 0.0467(9) Uani 1 1 d . . . F13 F 0.2693(5) 0.71359(12) 0.5159(3) 0.0623(12) Uani 1 1 d . . . C12 C 0.3583(6) 0.68313(18) 0.3097(4) 0.0375(14) Uani 1 1 d . . . F14 F 0.3421(5) 0.65010(11) 0.2595(3) 0.0549(11) Uani 1 1 d . . . F15 F 0.2906(5) 0.71185(11) 0.2555(3) 0.0585(12) Uani 1 1 d . . . F16 F 0.4855(4) 0.69332(12) 0.3318(3) 0.0541(10) Uani 1 1 d . . . C13 C 0.4058(6) 0.65270(18) 0.4634(4) 0.0360(14) Uani 1 1 d . . . F17 F 0.5081(4) 0.67488(12) 0.5118(3) 0.0505(10) Uani 1 1 d . . . F18 F 0.3483(4) 0.63597(12) 0.5223(2) 0.0487(10) Uani 1 1 d . . . F19 F 0.4572(3) 0.62282(10) 0.4272(3) 0.0483(10) Uani 1 1 d . . . C21 C 0.3563(6) 0.54098(18) 0.2754(5) 0.0390(15) Uani 1 1 d . . . F21 F 0.3757(4) 0.50557(11) 0.2405(3) 0.0534(10) Uani 1 1 d . . . F22 F 0.4710(3) 0.55159(12) 0.3325(3) 0.0567(11) Uani 1 1 d . . . F23 F 0.3257(5) 0.56712(12) 0.2095(3) 0.0592(11) Uani 1 1 d . . . C22 C 0.2992(6) 0.51821(18) 0.4179(4) 0.0375(14) Uani 1 1 d . . . F24 F 0.3777(4) 0.54279(12) 0.4769(3) 0.0518(10) Uani 1 1 d . . . F25 F 0.2017(4) 0.50757(11) 0.4527(3) 0.0541(10) Uani 1 1 d . . . F26 F 0.3696(4) 0.48531(11) 0.4119(3) 0.0521(10) Uani 1 1 d . . . C23 C 0.1244(6) 0.51441(18) 0.2675(4) 0.0373(14) Uani 1 1 d . . . F27 F 0.1480(4) 0.47543(11) 0.2698(3) 0.0549(11) Uani 1 1 d . . . F28 F 0.0178(3) 0.52070(13) 0.2957(3) 0.0584(11) Uani 1 1 d . . . F29 F 0.0950(4) 0.52600(13) 0.1814(3) 0.0596(11) Uani 1 1 d . . . C31 C -0.2231(6) 0.5915(2) 0.4176(4) 0.0385(15) Uani 1 1 d . . . F31 F -0.2697(3) 0.58377(11) 0.4889(2) 0.0437(9) Uani 1 1 d . . . F32 F -0.2273(4) 0.55806(12) 0.3721(3) 0.0488(10) Uani 1 1 d . . . F33 F -0.3056(4) 0.61746(13) 0.3648(3) 0.0553(11) Uani 1 1 d . . . C32 C 0.0070(6) 0.5827(2) 0.5250(4) 0.0402(15) Uani 1 1 d . . . F34 F 0.1364(3) 0.58929(13) 0.5335(3) 0.0518(10) Uani 1 1 d . . . F35 F -0.0136(4) 0.54395(11) 0.5075(3) 0.0555(11) Uani 1 1 d . . . F36 F -0.0162(4) 0.59040(14) 0.6044(3) 0.0581(11) Uani 1 1 d . . . C33 C -0.0815(8) 0.6522(2) 0.4811(5) 0.0498(18) Uani 1 1 d . . . F37 F -0.1646(5) 0.65662(12) 0.5327(3) 0.0692(14) Uani 1 1 d . . . F38 F 0.0392(5) 0.66371(13) 0.5291(3) 0.0646(13) Uani 1 1 d . . . F39 F -0.1218(5) 0.67677(12) 0.4111(3) 0.0679(13) Uani 1 1 d . . . C41 C -0.0941(8) 0.7322(2) 0.1752(7) 0.065(2) Uani 1 1 d . . . C42 C -0.2488(8) 0.7283(2) 0.0194(6) 0.060(2) Uani 1 1 d . . . C43 C -0.3332(8) 0.7109(2) 0.1514(7) 0.065(2) Uani 1 1 d . . . F41 F -0.1044(5) 0.77158(12) 0.1694(4) 0.0770(14) Uani 1 1 d . . . F42 F 0.0209(4) 0.72235(14) 0.1590(4) 0.0816(16) Uani 1 1 d . . . F43 F -0.0799(6) 0.72147(19) 0.2642(4) 0.102(2) Uani 1 1 d . . . F44 F -0.3129(5) 0.76289(13) 0.0170(4) 0.0865(17) Uani 1 1 d . . . F45 F -0.1369(6) 0.73666(15) -0.0055(4) 0.0859(16) Uani 1 1 d . . . F46 F -0.3248(6) 0.70503(16) -0.0412(3) 0.0890(17) Uani 1 1 d . . . F47 F -0.4426(4) 0.70067(15) 0.0903(4) 0.0821(16) Uani 1 1 d . . . F48 F -0.3156(6) 0.68569(16) 0.2222(4) 0.0860(16) Uani 1 1 d . . . F49 F -0.3512(6) 0.74703(16) 0.1819(5) 0.109(2) Uani 1 1 d . . . C5 C -0.2738(8) 0.5694(2) 0.0447(5) 0.0250(17) Uani 0.788(6) 1 d PDU A 1 C51 C -0.3164(12) 0.5630(3) 0.1325(6) 0.043(2) Uani 0.788(6) 1 d PD A 1 C52 C -0.3858(9) 0.5929(3) -0.0231(6) 0.045(2) Uani 0.788(6) 1 d PD A 1 C53 C -0.2529(10) 0.5287(3) 0.0039(8) 0.053(3) Uani 0.788(6) 1 d PD A 1 F51 F -0.4433(8) 0.5521(2) 0.1168(7) 0.0562(18) Uani 0.788(6) 1 d PD A 1 F52 F -0.2969(6) 0.59611(17) 0.1819(3) 0.0552(16) Uani 0.788(6) 1 d PD A 1 F53 F -0.2410(6) 0.53499(18) 0.1846(4) 0.071(2) Uani 0.788(6) 1 d PD A 1 F54 F -0.4882(10) 0.5694(5) -0.0638(10) 0.0669(18) Uani 0.788(6) 1 d PD A 1 F55 F -0.3387(6) 0.6096(2) -0.0869(4) 0.070(2) Uani 0.788(6) 1 d PD A 1 F56 F -0.4298(5) 0.62290(16) 0.0170(4) 0.0620(17) Uani 0.788(6) 1 d PD A 1 F57 F -0.3486(11) 0.5026(4) 0.0016(11) 0.0689(19) Uani 0.788(6) 1 d PD A 1 F58 F -0.1393(8) 0.5130(3) 0.0478(8) 0.090(4) Uani 0.788(6) 1 d PD A 1 F59 F -0.2538(7) 0.5341(3) -0.0828(5) 0.094(3) Uani 0.788(6) 1 d PD A 1 C5B C -0.272(3) 0.5656(8) 0.0453(15) 0.044(4) Uani 0.212(6) 1 d PDU A 2 C51B C -0.343(3) 0.5699(7) 0.1208(16) 0.042(5) Uani 0.212(6) 1 d PDU A 2 C52B C -0.362(3) 0.5799(7) -0.0468(15) 0.050(5) Uani 0.212(6) 1 d PDU A 2 C53B C -0.236(3) 0.5212(8) 0.0382(18) 0.044(5) Uani 0.212(6) 1 d PDU A 2 F51B F -0.2528(19) 0.5688(8) 0.2012(13) 0.0562(18) Uani 0.212(6) 1 d PDU A 2 F52B F -0.4023(18) 0.6049(5) 0.1155(17) 0.064(6) Uani 0.212(6) 1 d PDU A 2 F53B F -0.429(3) 0.5406(9) 0.123(3) 0.0562(18) Uani 0.212(6) 1 d PDU A 2 F54B F -0.3081(19) 0.5694(8) -0.1122(12) 0.060(5) Uani 0.212(6) 1 d PDU A 2 F55B F -0.365(2) 0.6193(6) -0.0498(17) 0.0562(18) Uani 0.212(6) 1 d PDU A 2 F56B F -0.487(3) 0.5686(16) -0.061(3) 0.0562(18) Uani 0.212(6) 1 d PDU A 2 F57B F -0.1889(18) 0.5048(5) 0.1193(12) 0.050(5) Uani 0.212(6) 1 d PDU A 2 F58B F -0.146(3) 0.5169(9) -0.0044(19) 0.057(8) Uani 0.212(6) 1 d PDU A 2 F59B F -0.348(4) 0.5004(15) 0.003(3) 0.0562(18) Uani 0.212(6) 1 d PDU A 2 C61 C 0.0149(6) 0.6605(2) -0.1002(5) 0.0471(17) Uani 1 1 d . . . F61 F -0.1140(4) 0.65488(13) -0.1073(3) 0.0573(11) Uani 1 1 d . A . F62 F 0.0366(4) 0.69910(13) -0.0924(3) 0.0655(12) Uani 1 1 d . A . F63 F 0.0373(4) 0.64852(14) -0.1783(3) 0.0599(12) Uani 1 1 d . A . C62 C 0.2438(6) 0.6546(2) 0.0105(4) 0.0414(15) Uani 1 1 d . . . F64 F 0.3263(4) 0.62990(13) 0.0671(3) 0.0551(11) Uani 1 1 d . A . F65 F 0.2479(4) 0.68947(12) 0.0514(3) 0.0548(11) Uani 1 1 d . A . F66 F 0.2915(4) 0.65997(13) -0.0614(2) 0.0507(10) Uani 1 1 d . A . C63 C 0.1031(7) 0.5932(2) -0.0434(5) 0.0471(17) Uani 1 1 d . . . F67 F 0.1891(5) 0.58555(13) -0.0924(3) 0.0623(12) Uani 1 1 d . A . F68 F -0.0156(4) 0.57998(12) -0.0903(3) 0.0581(11) Uani 1 1 d . A . F69 F 0.1411(5) 0.57045(12) 0.0311(3) 0.0646(12) Uani 1 1 d . A . F1 F 0.0176(3) 0.62262(9) 0.21638(19) 0.0267(7) Uani 1 1 d . . . C71 C 0.5746(6) 0.62291(19) 0.7089(4) 0.0375(14) Uani 1 1 d . . . C72 C 0.5044(7) 0.58562(19) 0.7062(4) 0.0368(15) Uani 1 1 d . . . H72A H 0.493(7) 0.574(2) 0.663(5) 0.044 Uiso 1 1 d . . . H72B H 0.564(7) 0.567(2) 0.744(5) 0.044 Uiso 1 1 d . . . C73 C 0.3749(7) 0.58569(17) 0.7235(4) 0.0354(14) Uani 1 1 d . . . C74 C 0.3201(7) 0.62122(19) 0.7371(4) 0.0421(16) Uani 1 1 d . . . H74 H 0.2342 0.6217 0.7469 0.051 Uiso 1 1 calc R . . C75 C 0.3886(8) 0.65705(19) 0.7369(4) 0.0461(18) Uani 1 1 d . . . C76 C 0.5160(8) 0.65729(18) 0.7246(4) 0.0442(17) Uani 1 1 d . . . H76 H 0.5623 0.6819 0.7272 0.053 Uiso 1 1 calc R . . C77 C 0.7116(7) 0.6218(3) 0.6939(5) 0.058(2) Uani 1 1 d . . . H77A H 0.7698 0.6047 0.7398 0.088 Uiso 1 1 calc R . . H77B H 0.7483 0.6489 0.6987 0.088 Uiso 1 1 calc R . . H77C H 0.7055 0.6111 0.6337 0.088 Uiso 1 1 calc R . . C78 C 0.3054(8) 0.5465(2) 0.7249(5) 0.0516(18) Uani 1 1 d . . . H78A H 0.3078 0.5309 0.6715 0.077 Uiso 1 1 calc R . . H78B H 0.2128 0.5515 0.7244 0.077 Uiso 1 1 calc R . . H78C H 0.3504 0.5317 0.7796 0.077 Uiso 1 1 calc R . . C79 C 0.3224(11) 0.6956(2) 0.7482(6) 0.080(3) Uani 1 1 d . . . H79A H 0.2269 0.6911 0.7389 0.120 Uiso 1 1 calc R . . H79B H 0.3358 0.7150 0.7038 0.120 Uiso 1 1 calc R . . H79C H 0.3612 0.7060 0.8094 0.120 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 0.0171(7) 0.0195(8) 0.0245(8) 0.0010(6) 0.0056(6) 0.0004(6) Al2 0.0191(8) 0.0238(8) 0.0246(8) 0.0027(6) 0.0051(6) -0.0028(6) O1 0.024(2) 0.0205(19) 0.043(2) -0.0065(17) 0.0021(17) -0.0011(15) O2 0.025(2) 0.0223(19) 0.042(2) 0.0032(17) 0.0052(17) 0.0046(15) O3 0.030(2) 0.045(2) 0.038(2) -0.0028(19) 0.0189(19) -0.0037(18) O4 0.031(2) 0.026(2) 0.068(3) 0.009(2) 0.012(2) 0.0063(17) O5 0.0219(19) 0.030(2) 0.037(2) -0.0026(17) 0.0075(17) -0.0064(16) O6 0.041(2) 0.055(3) 0.039(2) -0.017(2) 0.027(2) -0.024(2) C1 0.028(3) 0.024(3) 0.029(3) -0.001(2) 0.006(2) -0.004(2) C2 0.021(3) 0.021(3) 0.040(3) 0.003(2) 0.007(2) 0.002(2) C3 0.028(3) 0.036(3) 0.033(3) -0.002(2) 0.017(3) -0.004(2) C4 0.032(3) 0.025(3) 0.055(4) 0.005(3) 0.010(3) 0.010(2) C6 0.033(3) 0.042(3) 0.032(3) 0.003(3) 0.011(3) -0.007(3) C11 0.036(4) 0.032(3) 0.053(4) -0.014(3) 0.009(3) -0.009(3) F11 0.045(2) 0.030(2) 0.108(4) -0.023(2) -0.005(2) 0.0065(18) F12 0.047(2) 0.0297(19) 0.057(2) -0.0073(17) 0.0046(18) -0.0149(16) F13 0.078(3) 0.056(3) 0.065(3) -0.030(2) 0.041(2) -0.025(2) C12 0.047(4) 0.029(3) 0.037(3) -0.001(3) 0.014(3) -0.011(3) F14 0.086(3) 0.043(2) 0.047(2) -0.0120(18) 0.037(2) -0.015(2) F15 0.085(3) 0.040(2) 0.040(2) 0.0128(18) -0.002(2) -0.016(2) F16 0.053(2) 0.056(2) 0.063(3) 0.006(2) 0.032(2) -0.0158(19) C13 0.022(3) 0.037(3) 0.044(4) 0.004(3) 0.000(3) -0.010(3) F17 0.037(2) 0.055(2) 0.046(2) 0.0112(18) -0.0106(17) -0.0243(18) F18 0.049(2) 0.058(2) 0.036(2) 0.0152(18) 0.0053(17) -0.0223(19) F19 0.0262(18) 0.037(2) 0.080(3) 0.0095(19) 0.0112(18) 0.0048(15) C21 0.040(4) 0.028(3) 0.055(4) 0.000(3) 0.021(3) 0.005(3) F21 0.062(3) 0.038(2) 0.071(3) -0.0096(19) 0.038(2) 0.0043(18) F22 0.0261(19) 0.062(3) 0.086(3) -0.014(2) 0.022(2) -0.0063(18) F23 0.087(3) 0.045(2) 0.061(3) 0.009(2) 0.046(2) -0.002(2) C22 0.039(3) 0.029(3) 0.044(4) 0.010(3) 0.011(3) 0.011(3) F24 0.054(2) 0.048(2) 0.042(2) 0.0028(18) -0.0052(18) 0.0026(19) F25 0.065(3) 0.047(2) 0.058(2) 0.0156(19) 0.031(2) -0.0006(19) F26 0.055(2) 0.037(2) 0.061(3) 0.0142(18) 0.011(2) 0.0211(18) C23 0.037(3) 0.030(3) 0.042(4) -0.002(3) 0.006(3) 0.004(3) F27 0.057(2) 0.030(2) 0.076(3) -0.0132(19) 0.015(2) -0.0100(17) F28 0.0249(19) 0.063(3) 0.087(3) -0.024(2) 0.015(2) -0.0101(18) F29 0.061(3) 0.059(3) 0.045(2) -0.007(2) -0.009(2) -0.001(2) C31 0.030(3) 0.048(4) 0.043(4) 0.002(3) 0.019(3) 0.001(3) F31 0.0353(19) 0.054(2) 0.050(2) 0.0056(18) 0.0262(17) -0.0061(17) F32 0.036(2) 0.056(2) 0.059(2) -0.0190(19) 0.0197(18) -0.0193(17) F33 0.034(2) 0.078(3) 0.058(2) 0.021(2) 0.0209(19) 0.014(2) C32 0.026(3) 0.051(4) 0.046(4) -0.001(3) 0.013(3) -0.009(3) F34 0.0307(19) 0.070(3) 0.054(2) 0.011(2) 0.0099(18) -0.0084(18) F35 0.043(2) 0.037(2) 0.088(3) 0.015(2) 0.020(2) -0.0005(17) F36 0.050(2) 0.089(3) 0.038(2) 0.006(2) 0.0173(19) -0.009(2) C33 0.069(5) 0.034(4) 0.062(5) -0.006(3) 0.044(4) -0.004(3) F37 0.092(3) 0.047(2) 0.095(3) -0.016(2) 0.070(3) -0.002(2) F38 0.079(3) 0.054(3) 0.072(3) -0.032(2) 0.041(3) -0.035(2) F39 0.093(3) 0.035(2) 0.091(3) 0.017(2) 0.051(3) 0.011(2) C41 0.048(5) 0.046(5) 0.094(7) 0.000(4) 0.008(4) 0.002(4) C42 0.053(5) 0.043(4) 0.077(6) 0.015(4) 0.007(4) 0.011(4) C43 0.057(5) 0.046(4) 0.103(7) -0.009(5) 0.039(5) 0.005(4) F41 0.081(3) 0.034(2) 0.107(4) -0.005(2) 0.011(3) -0.007(2) F42 0.039(2) 0.064(3) 0.131(5) -0.009(3) 0.005(3) -0.010(2) F43 0.113(5) 0.107(4) 0.063(3) -0.004(3) -0.013(3) -0.033(4) F44 0.066(3) 0.045(3) 0.130(5) 0.033(3) -0.005(3) 0.020(2) F45 0.096(4) 0.071(3) 0.107(4) 0.033(3) 0.055(3) 0.003(3) F46 0.101(4) 0.072(3) 0.070(3) 0.017(3) -0.017(3) -0.016(3) F47 0.036(2) 0.077(3) 0.132(5) -0.004(3) 0.021(3) 0.008(2) F48 0.112(4) 0.079(4) 0.088(4) 0.006(3) 0.063(3) -0.008(3) F49 0.109(4) 0.061(3) 0.187(7) -0.031(4) 0.091(5) 0.004(3) C5 0.017(4) 0.031(4) 0.023(4) 0.000(3) -0.003(3) -0.011(3) C51 0.040(5) 0.048(6) 0.039(5) 0.007(5) 0.009(4) -0.014(4) C52 0.032(5) 0.060(7) 0.035(5) 0.005(4) -0.002(4) -0.019(4) C53 0.040(6) 0.050(6) 0.071(8) -0.029(5) 0.017(6) -0.017(4) F51 0.046(3) 0.068(4) 0.059(3) 0.005(4) 0.022(2) -0.023(3) F52 0.074(4) 0.060(4) 0.041(3) -0.015(3) 0.031(3) -0.027(3) F53 0.080(4) 0.060(4) 0.058(4) 0.033(3) -0.007(3) -0.024(3) F54 0.035(3) 0.081(4) 0.060(4) 0.018(3) -0.028(3) -0.023(3) F55 0.056(4) 0.109(6) 0.037(3) 0.038(3) 0.001(3) -0.023(4) F56 0.031(3) 0.048(3) 0.096(5) 0.007(3) -0.002(3) 0.005(2) F57 0.046(3) 0.042(3) 0.105(5) -0.026(3) -0.003(3) -0.024(3) F58 0.039(4) 0.045(4) 0.169(11) -0.044(7) -0.001(6) 0.003(3) F59 0.072(5) 0.133(7) 0.089(5) -0.081(5) 0.042(4) -0.041(5) C5B 0.038(10) 0.052(8) 0.048(8) 0.005(8) 0.021(7) -0.003(8) C51B 0.042(15) 0.037(11) 0.053(10) 0.003(14) 0.024(8) -0.008(9) C52B 0.038(11) 0.060(10) 0.046(11) -0.001(13) 0.000(10) -0.015(12) C53B 0.044(14) 0.048(12) 0.041(13) -0.007(10) 0.013(11) -0.010(10) F51B 0.046(3) 0.068(4) 0.059(3) 0.005(4) 0.022(2) -0.023(3) F52B 0.039(10) 0.046(8) 0.116(18) -0.012(10) 0.037(10) 0.000(7) F53B 0.046(3) 0.068(4) 0.059(3) 0.005(4) 0.022(2) -0.023(3) F54B 0.051(10) 0.089(14) 0.037(8) 0.006(10) 0.005(8) -0.010(11) F55B 0.046(3) 0.068(4) 0.059(3) 0.005(4) 0.022(2) -0.023(3) F56B 0.046(3) 0.068(4) 0.059(3) 0.005(4) 0.022(2) -0.023(3) F57B 0.043(10) 0.034(9) 0.066(10) 0.013(8) 0.004(7) -0.017(8) F58B 0.065(15) 0.034(11) 0.086(18) -0.031(13) 0.042(17) -0.026(11) F59B 0.046(3) 0.068(4) 0.059(3) 0.005(4) 0.022(2) -0.023(3) C61 0.033(4) 0.054(4) 0.055(4) 0.013(3) 0.013(3) -0.007(3) F61 0.0278(19) 0.072(3) 0.070(3) 0.007(2) 0.0100(19) -0.0057(19) F62 0.052(2) 0.050(3) 0.093(3) 0.021(2) 0.016(2) -0.007(2) F63 0.047(2) 0.099(3) 0.035(2) 0.017(2) 0.0130(18) -0.006(2) C62 0.038(4) 0.054(4) 0.036(3) 0.003(3) 0.016(3) -0.008(3) F64 0.039(2) 0.083(3) 0.042(2) 0.015(2) 0.0094(18) 0.002(2) F65 0.049(2) 0.061(3) 0.062(3) -0.010(2) 0.026(2) -0.025(2) F66 0.037(2) 0.078(3) 0.043(2) 0.013(2) 0.0210(17) -0.0080(19) C63 0.059(4) 0.050(4) 0.040(4) 0.000(3) 0.025(3) -0.004(3) F67 0.074(3) 0.060(3) 0.067(3) -0.007(2) 0.043(2) 0.003(2) F68 0.071(3) 0.058(3) 0.052(2) -0.021(2) 0.028(2) -0.030(2) F69 0.096(4) 0.045(2) 0.055(3) 0.013(2) 0.025(2) -0.001(2) F1 0.0230(15) 0.0280(16) 0.0260(16) 0.0046(13) 0.0017(13) -0.0025(12) C71 0.046(4) 0.044(4) 0.022(3) 0.004(3) 0.008(3) 0.002(3) C72 0.048(4) 0.034(3) 0.025(3) -0.002(3) 0.005(3) 0.010(3) C73 0.052(4) 0.031(3) 0.024(3) 0.007(2) 0.011(3) 0.003(3) C74 0.060(4) 0.038(4) 0.034(3) 0.006(3) 0.023(3) 0.013(3) C75 0.085(5) 0.035(4) 0.026(3) 0.002(3) 0.028(3) 0.012(3) C76 0.079(5) 0.029(3) 0.027(3) -0.005(3) 0.019(3) -0.014(3) C77 0.051(4) 0.086(6) 0.039(4) 0.005(4) 0.013(3) -0.006(4) C78 0.059(4) 0.041(4) 0.051(4) 0.009(3) 0.009(4) -0.007(3) C79 0.159(10) 0.034(4) 0.068(6) 0.002(4) 0.065(6) 0.028(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 O1 1.703(4) . ? Al1 O2 1.695(4) . ? Al1 O3 1.697(4) . ? Al1 F1 1.764(3) . ? Al2 O4 1.687(4) . ? Al2 O5 1.704(4) . ? Al2 O6 1.696(4) . ? Al2 F1 1.770(3) . ? O1 C1 1.368(6) . ? O2 C2 1.353(6) . ? O3 C3 1.361(7) . ? O4 C4 1.361(7) . ? O5 C5 1.353(9) . ? O5 C5B 1.40(4) . ? O6 C6 1.363(7) . ? C1 C11 1.552(8) . ? C1 C12 1.537(8) . ? C1 C13 1.538(8) . ? C2 C21 1.563(8) . ? C2 C22 1.553(8) . ? C2 C23 1.544(8) . ? C3 C31 1.562(8) . ? C3 C32 1.537(9) . ? C3 C33 1.553(9) . ? C4 C41 1.509(10) . ? C4 C42 1.545(10) . ? C4 C43 1.546(10) . ? C6 C61 1.552(9) . ? C6 C62 1.553(8) . ? C6 C63 1.528(9) . ? C11 F11 1.317(8) . ? C11 F12 1.331(7) . ? C11 F13 1.337(8) . ? C12 F14 1.333(7) . ? C12 F15 1.341(7) . ? C12 F16 1.324(7) . ? C13 F17 1.347(6) . ? C13 F18 1.338(7) . ? C13 F19 1.328(7) . ? C21 F21 1.340(7) . ? C21 F22 1.327(8) . ? C21 F23 1.311(7) . ? C22 F24 1.330(7) . ? C22 F25 1.322(7) . ? C22 F26 1.342(7) . ? C23 F27 1.327(7) . ? C23 F28 1.318(7) . ? C23 F29 1.332(7) . ? C31 F31 1.340(7) . ? C31 F32 1.314(7) . ? C31 F33 1.334(7) . ? C32 F34 1.341(7) . ? C32 F35 1.332(7) . ? C32 F36 1.334(7) . ? C33 F37 1.334(8) . ? C33 F38 1.332(9) . ? C33 F39 1.329(8) . ? C41 F41 1.324(9) . ? C41 F42 1.334(9) . ? C41 F43 1.384(11) . ? C42 F44 1.333(8) . ? C42 F45 1.356(9) . ? C42 F46 1.306(9) . ? C43 F47 1.313(10) . ? C43 F48 1.352(10) . ? C43 F49 1.328(9) . ? C5 C51 1.548(10) . ? C5 C52 1.552(10) . ? C5 C53 1.541(10) . ? C51 F51 1.332(12) . ? C51 F52 1.328(10) . ? C51 F53 1.341(11) . ? C52 F54 1.336(13) . ? C52 F55 1.335(9) . ? C52 F56 1.325(12) . ? C53 F57 1.321(13) . ? C53 F58 1.306(12) . ? C53 F59 1.343(14) . ? C5B C51B 1.546(18) . ? C5B C52B 1.547(18) . ? C5B C53B 1.542(18) . ? C51B F51B 1.33(2) . ? C51B F52B 1.320(19) . ? C51B F53B 1.34(2) . ? C52B F54B 1.33(2) . ? C52B F55B 1.321(18) . ? C52B F56B 1.32(2) . ? C53B F57B 1.33(2) . ? C53B F58B 1.294(19) . ? C53B F59B 1.34(2) . ? C61 F61 1.334(7) . ? C61 F62 1.313(8) . ? C61 F63 1.346(8) . ? C62 F64 1.332(8) . ? C62 F65 1.322(8) . ? C62 F66 1.345(7) . ? C63 F67 1.346(8) . ? C63 F68 1.329(8) . ? C63 F69 1.343(8) . ? C71 C72 1.443(9) . ? C71 C76 1.356(9) . ? C71 C77 1.510(10) . ? C72 H72A 0.75(7) . ? C72 H72B 0.95(7) . ? C72 C73 1.449(9) . ? C73 C74 1.361(8) . ? C73 C78 1.502(9) . ? C74 H74 0.9500 . ? C74 C75 1.397(10) . ? C75 C76 1.394(10) . ? C75 C79 1.497(9) . ? C76 H76 0.9500 . ? C77 H77A 0.9800 . ? C77 H77B 0.9800 . ? C77 H77C 0.9800 . ? C78 H78A 0.9800 . ? C78 H78B 0.9800 . ? C78 H78C 0.9800 . ? C79 H79A 0.9800 . ? C79 H79B 0.9800 . ? C79 H79C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Al1 F1 105.86(18) . . ? O2 Al1 O1 111.81(19) . . ? O2 Al1 O3 116.2(2) . . ? O2 Al1 F1 108.08(18) . . ? O3 Al1 O1 113.0(2) . . ? O3 Al1 F1 100.64(19) . . ? O4 Al2 O5 112.5(2) . . ? O4 Al2 O6 116.8(2) . . ? O4 Al2 F1 107.1(2) . . ? O5 Al2 F1 106.13(18) . . ? O6 Al2 O5 112.1(2) . . ? O6 Al2 F1 100.8(2) . . ? C1 O1 Al1 145.6(4) . . ? C2 O2 Al1 155.8(4) . . ? C3 O3 Al1 147.9(4) . . ? C4 O4 Al2 154.4(4) . . ? C5 O5 Al2 146.5(4) . . ? C5 O5 C5B 5.1(10) . . ? C5B O5 Al2 151.0(9) . . ? C6 O6 Al2 148.0(4) . . ? O1 C1 C11 107.6(5) . . ? O1 C1 C12 110.3(5) . . ? O1 C1 C13 111.2(4) . . ? C12 C1 C11 109.8(5) . . ? C12 C1 C13 108.6(5) . . ? C13 C1 C11 109.4(5) . . ? O2 C2 C21 108.0(4) . . ? O2 C2 C22 108.2(5) . . ? O2 C2 C23 111.4(4) . . ? C22 C2 C21 109.2(5) . . ? C23 C2 C21 110.4(5) . . ? C23 C2 C22 109.5(5) . . ? O3 C3 C31 107.0(5) . . ? O3 C3 C32 110.5(5) . . ? O3 C3 C33 110.0(5) . . ? C32 C3 C31 109.8(5) . . ? C32 C3 C33 109.7(5) . . ? C33 C3 C31 109.8(5) . . ? O4 C4 C41 111.8(5) . . ? O4 C4 C42 108.1(6) . . ? O4 C4 C43 108.0(5) . . ? C41 C4 C42 109.9(6) . . ? C41 C4 C43 111.5(7) . . ? C42 C4 C43 107.4(6) . . ? O6 C6 C61 110.7(5) . . ? O6 C6 C62 106.6(5) . . ? O6 C6 C63 111.0(5) . . ? C61 C6 C62 109.6(5) . . ? C63 C6 C61 108.5(5) . . ? C63 C6 C62 110.5(5) . . ? F11 C11 C1 110.4(5) . . ? F11 C11 F12 107.8(5) . . ? F11 C11 F13 108.1(6) . . ? F12 C11 C1 112.7(5) . . ? F12 C11 F13 107.8(5) . . ? F13 C11 C1 109.8(5) . . ? F14 C12 C1 110.8(5) . . ? F14 C12 F15 105.8(5) . . ? F15 C12 C1 110.8(5) . . ? F16 C12 C1 113.0(5) . . ? F16 C12 F14 108.8(5) . . ? F16 C12 F15 107.3(5) . . ? F17 C13 C1 112.8(5) . . ? F18 C13 C1 110.8(5) . . ? F18 C13 F17 107.0(5) . . ? F19 C13 C1 112.6(5) . . ? F19 C13 F17 107.2(5) . . ? F19 C13 F18 106.0(5) . . ? F21 C21 C2 111.4(5) . . ? F22 C21 C2 110.9(5) . . ? F22 C21 F21 107.1(5) . . ? F23 C21 C2 110.5(5) . . ? F23 C21 F21 108.2(5) . . ? F23 C21 F22 108.6(5) . . ? F24 C22 C2 111.3(5) . . ? F24 C22 F26 107.9(5) . . ? F25 C22 C2 111.0(5) . . ? F25 C22 F24 106.9(5) . . ? F25 C22 F26 107.7(5) . . ? F26 C22 C2 111.8(5) . . ? F27 C23 C2 112.7(5) . . ? F27 C23 F29 107.7(5) . . ? F28 C23 C2 110.6(5) . . ? F28 C23 F27 108.4(5) . . ? F28 C23 F29 107.1(5) . . ? F29 C23 C2 110.1(5) . . ? F31 C31 C3 111.2(5) . . ? F32 C31 C3 111.1(5) . . ? F32 C31 F31 107.8(5) . . ? F32 C31 F33 108.0(5) . . ? F33 C31 C3 110.9(5) . . ? F33 C31 F31 107.8(5) . . ? F34 C32 C3 110.0(5) . . ? F35 C32 C3 111.3(5) . . ? F35 C32 F34 106.4(5) . . ? F35 C32 F36 108.3(5) . . ? F36 C32 C3 112.5(5) . . ? F36 C32 F34 108.0(5) . . ? F37 C33 C3 111.8(5) . . ? F38 C33 C3 110.7(6) . . ? F38 C33 F37 108.1(6) . . ? F39 C33 C3 110.4(6) . . ? F39 C33 F37 107.4(6) . . ? F39 C33 F38 108.3(6) . . ? F41 C41 C4 115.1(7) . . ? F41 C41 F42 107.2(7) . . ? F41 C41 F43 108.1(7) . . ? F42 C41 C4 111.6(7) . . ? F42 C41 F43 105.1(7) . . ? F43 C41 C4 109.3(7) . . ? F44 C42 C4 112.5(7) . . ? F44 C42 F45 106.2(6) . . ? F45 C42 C4 108.9(6) . . ? F46 C42 C4 112.8(6) . . ? F46 C42 F44 107.2(6) . . ? F46 C42 F45 108.9(8) . . ? F47 C43 C4 112.6(7) . . ? F47 C43 F48 108.2(7) . . ? F47 C43 F49 108.1(7) . . ? F48 C43 C4 109.3(6) . . ? F49 C43 C4 111.7(7) . . ? F49 C43 F48 106.6(8) . . ? O5 C5 C51 109.5(6) . . ? O5 C5 C52 111.9(6) . . ? O5 C5 C53 107.7(7) . . ? C51 C5 C52 108.2(7) . . ? C53 C5 C51 109.8(7) . . ? C53 C5 C52 109.8(7) . . ? F51 C51 C5 112.9(8) . . ? F51 C51 F53 108.1(7) . . ? F52 C51 C5 110.3(7) . . ? F52 C51 F51 108.8(8) . . ? F52 C51 F53 105.6(8) . . ? F53 C51 C5 110.9(8) . . ? F54 C52 C5 112.2(9) . . ? F55 C52 C5 110.1(7) . . ? F55 C52 F54 108.1(9) . . ? F56 C52 C5 111.4(7) . . ? F56 C52 F54 109.2(10) . . ? F56 C52 F55 105.5(9) . . ? F57 C53 C5 114.0(9) . . ? F57 C53 F59 105.1(10) . . ? F58 C53 C5 110.9(8) . . ? F58 C53 F57 108.7(12) . . ? F58 C53 F59 109.0(10) . . ? F59 C53 C5 108.8(9) . . ? O5 C5B C51B 110.5(19) . . ? O5 C5B C52B 106.8(18) . . ? O5 C5B C53B 110.6(19) . . ? C51B C5B C52B 111.2(18) . . ? C53B C5B C51B 108.5(17) . . ? C53B C5B C52B 109.4(18) . . ? F51B C51B C5B 110(2) . . ? F51B C51B F53B 105(2) . . ? F52B C51B C5B 110.6(18) . . ? F52B C51B F51B 106(2) . . ? F52B C51B F53B 110(2) . . ? F53B C51B C5B 114(2) . . ? F54B C52B C5B 109.5(19) . . ? F55B C52B C5B 110.3(19) . . ? F55B C52B F54B 105(2) . . ? F56B C52B C5B 113(2) . . ? F56B C52B F54B 114(3) . . ? F56B C52B F55B 105(3) . . ? F57B C53B C5B 111.5(19) . . ? F57B C53B F59B 103(2) . . ? F58B C53B C5B 111(2) . . ? F58B C53B F57B 107(2) . . ? F58B C53B F59B 114(3) . . ? F59B C53B C5B 109(2) . . ? F61 C61 C6 109.9(5) . . ? F61 C61 F63 107.6(6) . . ? F62 C61 C6 111.9(6) . . ? F62 C61 F61 106.9(6) . . ? F62 C61 F63 107.9(6) . . ? F63 C61 C6 112.4(6) . . ? F64 C62 C6 110.6(5) . . ? F64 C62 F66 107.6(5) . . ? F65 C62 C6 111.5(5) . . ? F65 C62 F64 107.9(5) . . ? F65 C62 F66 107.5(5) . . ? F66 C62 C6 111.6(5) . . ? F67 C63 C6 113.0(5) . . ? F68 C63 C6 112.5(6) . . ? F68 C63 F67 107.3(5) . . ? F68 C63 F69 106.8(6) . . ? F69 C63 C6 110.3(5) . . ? F69 C63 F67 106.4(6) . . ? Al1 F1 Al2 176.0(2) . . ? C72 C71 C77 118.0(6) . . ? C76 C71 C72 119.3(6) . . ? C76 C71 C77 122.7(6) . . ? C71 C72 H72A 116(6) . . ? C71 C72 H72B 107(4) . . ? C71 C72 C73 119.1(6) . . ? H72A C72 H72B 97(6) . . ? C73 C72 H72A 103(6) . . ? C73 C72 H72B 112(4) . . ? C72 C73 C78 118.7(6) . . ? C74 C73 C72 118.9(6) . . ? C74 C73 C78 122.4(6) . . ? C73 C74 H74 119.6 . . ? C73 C74 C75 120.9(7) . . ? C75 C74 H74 119.6 . . ? C74 C75 C79 119.2(7) . . ? C76 C75 C74 120.9(6) . . ? C76 C75 C79 119.9(7) . . ? C71 C76 C75 120.9(6) . . ? C71 C76 H76 119.6 . . ? C75 C76 H76 119.6 . . ? C71 C77 H77A 109.5 . . ? C71 C77 H77B 109.5 . . ? C71 C77 H77C 109.5 . . ? H77A C77 H77B 109.5 . . ? H77A C77 H77C 109.5 . . ? H77B C77 H77C 109.5 . . ? C73 C78 H78A 109.5 . . ? C73 C78 H78B 109.5 . . ? C73 C78 H78C 109.5 . . ? H78A C78 H78B 109.5 . . ? H78A C78 H78C 109.5 . . ? H78B C78 H78C 109.5 . . ? C75 C79 H79A 109.5 . . ? C75 C79 H79B 109.5 . . ? C75 C79 H79C 109.5 . . ? H79A C79 H79B 109.5 . . ? H79A C79 H79C 109.5 . . ? H79B C79 H79C 109.5 . . ?