# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2007 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'Ingo Krossing' _publ_contact_author_address ; Albert-Ludwig Universitat Freiburg Institut fur Anorganische Chemie Alberstr.21 Freiburg 79104 GERMANY ; _publ_contact_author_email KROSSING@UNI-FREIBURG.DE _publ_section_title ; Homoleptic Cu-phosphorous and Cu-ethene complexes. ; loop_ _publ_author_name 'Ingo Krossing' 'Andreas Reisinger' 'Gustavo Santiso Quinones' 'John Slattery' data_sad _database_code_depnum_ccdc_archive 'CCDC 654310' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C16 Ag1 Al1 F36 O4 P8' _chemical_formula_sum 'C16 Ag1 Al1 F36 O4 P8' _chemical_formula_weight 1322.77 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' 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M P212121 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 11.614(2) _cell_length_b 17.324(4) _cell_length_c 38.299(8) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 7706(3) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Blocks _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.280 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5056 _exptl_absorpt_coefficient_mu 1.083 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.68745 _exptl_absorpt_correction_T_max 0.805 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'FR590 Sealed Tube Generator' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX II CCD area detector at 100K' _diffrn_measurement_method 'APEXII (Bruker, 2005)' _diffrn_detector_area_resol_mean 'frames each covering 0.5\% in\w' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 293914 _diffrn_reflns_av_R_equivalents 0.1090 _diffrn_reflns_av_sigmaI/netI 0.0458 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -49 _diffrn_reflns_limit_l_max 49 _diffrn_reflns_theta_min 1.29 _diffrn_reflns_theta_max 27.54 _reflns_number_total 17675 _reflns_number_gt 15206 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Bruker AXS BV, 1997-2004)' _computing_cell_refinement 'Dirax/lsq (Duisenberg & Schreurs 1989-2000)' _computing_data_reduction 'EvalCCD (Duisenberg & Schreurs 1990-2000)' _computing_structure_solution 'SHELXTL (Bruker, 2001)' _computing_structure_refinement 'SHELXTL (Bruker, 2001)' _computing_molecular_graphics 'SHELXTL (Bruker, 2001)' _computing_publication_material 'SHELXTL (Bruker, 2001)' _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 structure was refined as an inversion twin with a 0.51:0.49 ratio of twin components. The C(CF3)3 group containing C21 is disordered by rotation around the C-O bond. This was modeled as two positions with a SOF ratio of 0.77:0.33 - refined using a free variable. SIMU restraints were applied to all disordered atoms. ISOR restraints were applied to seven atoms, including one in the disordered residue, to correct for very asymmetric ADPs. ; _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^)+(0.0242P)^2^+44.8770P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens ? _refine_ls_hydrogen_treatment ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.51(3) _refine_ls_number_reflns 17675 _refine_ls_number_parameters 1299 _refine_ls_number_restraints 318 _refine_ls_R_factor_all 0.0784 _refine_ls_R_factor_gt 0.0649 _refine_ls_wR_factor_ref 0.1369 _refine_ls_wR_factor_gt 0.1302 _refine_ls_goodness_of_fit_ref 1.222 _refine_ls_restrained_S_all 1.217 _refine_ls_shift/su_max 0.006 _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 Ag1 Ag 0.27367(6) 0.50924(3) 0.039236(16) 0.03148(14) Uani 1 1 d . . . Ag2 Ag 0.73496(5) 0.99226(3) 0.209223(15) 0.02797(13) Uani 1 1 d . . . Al1 Al 0.78184(16) 0.49761(10) 0.12614(5) 0.0142(4) Uani 1 1 d . . . Al2 Al 0.27580(16) 0.00335(10) 0.12397(5) 0.0142(4) Uani 1 1 d . . . C1 C 0.7812(7) 0.3635(4) 0.07853(17) 0.0181(14) Uani 1 1 d . . . C2 C 0.8311(7) 0.2809(4) 0.0866(2) 0.0246(16) Uani 1 1 d . . . C3 C 0.8511(6) 0.3994(4) 0.04757(19) 0.0226(15) Uani 1 1 d . . . C4 C 0.6530(6) 0.3553(5) 0.0677(2) 0.0282(18) Uani 1 1 d U . . C5 C 0.8162(6) 0.6403(4) 0.08437(18) 0.0171(14) Uani 1 1 d . . . C6 C 0.8799(6) 0.6437(4) 0.04801(19) 0.0211(15) Uani 1 1 d . . . C7 C 0.8835(8) 0.6913(4) 0.1111(2) 0.0284(18) Uani 1 1 d . . . C8 C 0.6948(7) 0.6710(4) 0.0802(2) 0.0269(17) Uani 1 1 d . . . C9 C 0.5596(5) 0.5091(4) 0.16512(17) 0.0186(13) Uani 1 1 d . . . C10 C 0.4598(6) 0.5679(4) 0.1580(2) 0.0250(16) Uani 1 1 d . . . C11 C 0.6106(6) 0.5233(4) 0.20209(19) 0.0250(16) Uani 1 1 d . . . C12 C 0.5087(6) 0.4250(4) 0.1630(2) 0.0247(16) Uani 1 1 d . . . C13 C 0.9716(6) 0.4766(4) 0.17637(19) 0.0203(15) Uani 1 1 d . . . C14 C 1.0790(7) 0.4958(6) 0.1544(3) 0.043(2) Uani 1 1 d . . . C15 C 0.9811(8) 0.5156(6) 0.2132(2) 0.041(2) Uani 1 1 d . . . C16 C 0.9705(8) 0.3871(5) 0.1823(3) 0.045(3) Uani 1 1 d . . . C17 C 0.2626(7) -0.1381(4) 0.16719(18) 0.0203(15) Uani 1 1 d . . . C18 C 0.3123(8) -0.1945(4) 0.1394(2) 0.0303(18) Uani 1 1 d U . . C19 C 0.1320(7) -0.1551(4) 0.1725(2) 0.0283(18) Uani 1 1 d . . . C20 C 0.3264(7) -0.1505(4) 0.2025(2) 0.0270(17) Uani 1 1 d . . . C21 C 0.0801(6) 0.0080(4) 0.07436(17) 0.0183(13) Uani 1 1 d . . . C25 C 0.4984(5) 0.0059(4) 0.08576(17) 0.0172(13) Uani 1 1 d . . . C26 C 0.5229(7) 0.0961(4) 0.0870(2) 0.0274(17) Uani 1 1 d . . . C27 C 0.5168(5) -0.0229(4) 0.04788(19) 0.0193(14) Uani 1 1 d . . . C28 C 0.5844(7) -0.0351(5) 0.1110(2) 0.0302(18) Uani 1 1 d . . . C29 C 0.2684(6) 0.1398(3) 0.16976(18) 0.0157(13) Uani 1 1 d . . . C30 C 0.1382(6) 0.1410(4) 0.1792(2) 0.0237(16) Uani 1 1 d . . . C31 C 0.3393(7) 0.1118(4) 0.20243(18) 0.0226(15) Uani 1 1 d . . . C32 C 0.3066(7) 0.2244(4) 0.1602(2) 0.0247(16) Uani 1 1 d . . . F1 F 0.7948(5) 0.2560(2) 0.11752(12) 0.0344(11) Uani 1 1 d . . . F2 F 0.9445(4) 0.2816(2) 0.08680(13) 0.0327(11) Uani 1 1 d . . . F3 F 0.7966(5) 0.2284(2) 0.06230(13) 0.0389(12) Uani 1 1 d . . . F4 F 0.9521(4) 0.4256(3) 0.05763(12) 0.0278(10) Uani 1 1 d . . . F5 F 0.8697(4) 0.3473(2) 0.02155(11) 0.0330(11) Uani 1 1 d . . . F6 F 0.7913(4) 0.4576(2) 0.03297(11) 0.0332(11) Uani 1 1 d . . . F7 F 0.5955(4) 0.3078(3) 0.08913(14) 0.0397(13) Uani 1 1 d . . . F8 F 0.5998(4) 0.4244(3) 0.06999(13) 0.0393(12) Uani 1 1 d . . . F9 F 0.6387(4) 0.3303(3) 0.03523(13) 0.0398(12) Uani 1 1 d . . . F10 F 0.8117(4) 0.6213(2) 0.02236(11) 0.0299(10) Uani 1 1 d . . . F11 F 0.9148(4) 0.7174(2) 0.04051(12) 0.0319(10) Uani 1 1 d . . . F12 F 0.9744(4) 0.6005(2) 0.04780(12) 0.0304(10) Uani 1 1 d . . . F13 F 0.8516(5) 0.6733(2) 0.14367(11) 0.0357(12) Uani 1 1 d . . . F14 F 0.9973(4) 0.6811(3) 0.10844(13) 0.0338(11) Uani 1 1 d . . . F15 F 0.8623(4) 0.7668(2) 0.10660(13) 0.0351(11) Uani 1 1 d U . . F16 F 0.6250(4) 0.6178(3) 0.06516(14) 0.0352(12) Uani 1 1 d . . . F17 F 0.6463(4) 0.6884(3) 0.11074(14) 0.0358(12) Uani 1 1 d . . . F18 F 0.6876(4) 0.7349(2) 0.06001(13) 0.0340(11) Uani 1 1 d . . . F19 F 0.3651(4) 0.5509(3) 0.17566(13) 0.0333(11) Uani 1 1 d . . . F20 F 0.4370(4) 0.5706(3) 0.12422(13) 0.0357(11) Uani 1 1 d . . . F21 F 0.4951(4) 0.6397(2) 0.16738(13) 0.0324(11) Uani 1 1 d . . . F22 F 0.5288(4) 0.5356(3) 0.22614(12) 0.0350(11) Uani 1 1 d . . . F23 F 0.6805(4) 0.5841(2) 0.20236(11) 0.0279(10) Uani 1 1 d . . . F24 F 0.6720(4) 0.4617(3) 0.21292(11) 0.0337(11) Uani 1 1 d . . . F25 F 0.4411(4) 0.4169(3) 0.13537(12) 0.0326(11) Uani 1 1 d . . . F26 F 0.4498(4) 0.4064(3) 0.19153(13) 0.0385(12) Uani 1 1 d . . . F27 F 0.5956(4) 0.3740(2) 0.15994(12) 0.0326(11) Uani 1 1 d . . . F28 F 1.0601(4) 0.4900(4) 0.12058(13) 0.0506(14) Uani 1 1 d . . . F29 F 1.1051(5) 0.5742(3) 0.15981(19) 0.0657(19) Uani 1 1 d U . . F30 F 1.1738(4) 0.4558(3) 0.16217(16) 0.0477(14) Uani 1 1 d U . . F31 F 0.9555(5) 0.5878(3) 0.21252(16) 0.0559(17) Uani 1 1 d . . . F32 F 1.0916(5) 0.5079(3) 0.22608(14) 0.0518(14) Uani 1 1 d . . . F33 F 0.9097(5) 0.4815(4) 0.23587(14) 0.0669(19) Uani 1 1 d . . . F34 F 1.0001(5) 0.3527(3) 0.15063(19) 0.066(2) Uani 1 1 d . . . F35 F 1.0443(5) 0.3611(3) 0.20537(15) 0.0484(14) Uani 1 1 d . . . F36 F 0.8655(4) 0.3630(3) 0.18867(17) 0.0541(16) Uani 1 1 d . . . F37 F 0.2816(5) -0.1705(2) 0.10730(12) 0.0412(13) Uani 1 1 d . . . F38 F 0.4260(4) -0.1969(3) 0.14078(14) 0.0405(13) Uani 1 1 d . . . F39 F 0.2715(5) -0.2669(2) 0.14316(12) 0.0391(12) Uani 1 1 d . . . F40 F 0.0777(4) -0.1639(3) 0.14177(14) 0.0398(13) Uani 1 1 d . . . F41 F 0.1139(4) -0.2193(3) 0.19151(14) 0.0385(12) Uani 1 1 d . . . F42 F 0.0803(4) -0.0962(3) 0.18919(14) 0.0385(12) Uani 1 1 d . . . F43 F 0.4280(4) -0.1156(3) 0.20244(13) 0.0352(11) Uani 1 1 d . . . F44 F 0.2661(5) -0.1242(2) 0.22916(11) 0.0369(12) Uani 1 1 d . . . F45 F 0.3469(4) -0.2268(2) 0.20862(12) 0.0322(10) Uani 1 1 d . . . F55 F 0.5430(4) 0.1188(3) 0.11925(14) 0.0426(13) Uani 1 1 d . . . F56 F 0.4326(5) 0.1346(3) 0.07453(14) 0.0425(13) Uani 1 1 d . . . F57 F 0.6145(4) 0.1140(3) 0.06754(14) 0.0434(13) Uani 1 1 d . . . F58 F 0.4732(4) -0.0935(3) 0.04341(13) 0.0369(12) Uani 1 1 d . . . F59 F 0.4685(4) 0.0232(3) 0.02433(12) 0.0379(12) Uani 1 1 d . . . F60 F 0.6311(4) -0.0285(3) 0.03944(12) 0.0329(11) Uani 1 1 d . . . F61 F 0.6894(3) -0.0060(4) 0.10938(13) 0.0443(13) Uani 1 1 d U . . F62 F 0.5905(4) -0.1103(3) 0.10334(14) 0.0428(13) Uani 1 1 d . . . F63 F 0.5473(4) -0.0288(3) 0.14379(12) 0.0388(12) Uani 1 1 d . . . F64 F 0.0779(4) 0.1839(3) 0.15653(13) 0.0312(11) Uani 1 1 d . . . F65 F 0.0950(4) 0.0689(2) 0.17741(12) 0.0293(10) Uani 1 1 d . . . F66 F 0.1172(4) 0.1678(3) 0.21116(12) 0.0350(11) Uani 1 1 d . . . F67 F 0.2852(4) 0.0528(2) 0.21800(11) 0.0281(10) Uani 1 1 d . . . F68 F 0.4433(4) 0.0883(2) 0.19305(12) 0.0259(10) Uani 1 1 d . . . F69 F 0.3526(4) 0.1686(2) 0.22647(11) 0.0315(11) Uani 1 1 d . . . F70 F 0.2641(4) 0.2771(2) 0.18262(12) 0.0321(11) Uani 1 1 d . . . F71 F 0.2736(4) 0.2433(2) 0.12836(11) 0.0309(10) Uani 1 1 d . . . F72 F 0.4217(4) 0.2308(2) 0.16142(12) 0.0300(10) Uani 1 1 d . . . O1 O 0.7945(4) 0.4068(2) 0.10762(12) 0.0207(11) Uani 1 1 d . . . O2 O 0.8178(4) 0.5654(3) 0.09430(12) 0.0189(10) Uani 1 1 d . . . O3 O 0.6421(4) 0.5191(3) 0.14024(12) 0.0165(9) Uani 1 1 d . . . O4 O 0.8742(4) 0.5019(3) 0.16159(12) 0.0189(10) Uani 1 1 d . . . O5 O 0.2787(4) -0.0635(2) 0.15777(11) 0.0168(9) Uani 1 1 d . . . O6 O 0.1454(4) -0.0075(3) 0.10265(11) 0.0182(9) Uani 1 1 d . A . O7 O 0.3879(4) -0.0100(3) 0.09437(11) 0.0176(9) Uani 1 1 d . . . O8 O 0.2909(4) 0.0943(2) 0.14184(12) 0.0176(10) Uani 1 1 d . . . P1 P 0.70700(19) 0.85967(11) 0.23761(5) 0.0255(4) Uani 1 1 d . . . P2 P 0.7826(2) 0.86284(11) 0.18095(5) 0.0261(4) Uani 1 1 d . . . P3 P 0.83931(19) 0.78010(11) 0.22007(6) 0.0278(5) Uani 1 1 d . . . P4 P 0.6639(2) 0.77355(12) 0.19865(7) 0.0355(5) Uani 1 1 d . . . P5 P 0.69889(18) 1.12070(10) 0.23997(5) 0.0247(4) Uani 1 1 d . . . P6 P 0.6727(2) 1.21590(12) 0.20388(7) 0.0364(6) Uani 1 1 d . . . P7 P 0.84258(18) 1.19778(11) 0.22857(6) 0.0277(4) Uani 1 1 d . . . P8 P 0.38576(18) 0.72094(12) 0.04410(7) 0.0314(5) Uani 1 1 d . . . P9 P 0.25810(19) 0.64288(11) 0.06663(5) 0.0251(4) Uani 1 1 d . . . P10 P 0.3135(2) 0.63727(11) 0.00788(6) 0.0307(5) Uani 1 1 d . . . P11 P 0.20430(19) 0.72801(12) 0.02841(6) 0.0340(5) Uani 1 1 d . . . P12 P 0.2761(2) 0.38172(11) 0.00600(5) 0.0315(5) Uani 1 1 d . . . P13 P 0.2497(3) 0.37550(12) 0.06622(5) 0.0398(6) Uani 1 1 d . . . P14 P 0.1630(2) 0.29929(13) 0.03017(8) 0.0422(6) Uani 1 1 d . . . P15 P 0.3495(2) 0.29030(13) 0.03715(8) 0.0427(6) Uani 1 1 d . . . P16 P 0.7877(2) 1.12515(11) 0.18520(6) 0.0325(5) Uani 1 1 d . . . C22 C 0.0969(9) -0.0564(6) 0.0462(3) 0.0260(17) Uani 0.766(7) 1 d PU A 1 C23 C -0.0476(8) 0.0106(6) 0.0856(3) 0.0272(17) Uani 0.766(7) 1 d PU A 1 C24 C 0.1130(9) 0.0882(6) 0.0571(3) 0.0253(17) Uani 0.766(7) 1 d PU A 1 F46 F 0.2084(13) -0.0704(7) 0.0409(3) 0.028(2) Uani 0.766(7) 1 d PU A 1 F47 F 0.0527(6) -0.0371(5) 0.0147(2) 0.0332(16) Uani 0.766(7) 1 d PU A 1 F48 F 0.0412(7) -0.1208(4) 0.0562(2) 0.0335(16) Uani 0.766(7) 1 d PU A 1 F49 F -0.1217(8) 0.0057(4) 0.0588(2) 0.0295(16) Uani 0.766(7) 1 d PU A 1 F50 F -0.0711(12) -0.0455(7) 0.1094(3) 0.0257(19) Uani 0.766(7) 1 d PU A 1 F51 F -0.0737(7) 0.0764(5) 0.1024(2) 0.0339(17) Uani 0.766(7) 1 d PU A 1 F52 F 0.0315(6) 0.1135(4) 0.03505(19) 0.0320(15) Uani 0.766(7) 1 d PU A 1 F53 F 0.2099(7) 0.0831(4) 0.0390(2) 0.0319(16) Uani 0.766(7) 1 d PU A 1 F54 F 0.1315(9) 0.1408(8) 0.0817(3) 0.0266(19) Uani 0.766(7) 1 d PU A 1 C22' C 0.147(3) -0.005(2) 0.0402(8) 0.029(2) Uani 0.234(7) 1 d PU A 2 C23' C -0.034(3) -0.047(2) 0.0777(9) 0.028(3) Uani 0.234(7) 1 d PU A 2 C24' C 0.034(3) 0.096(2) 0.0782(9) 0.029(2) Uani 0.234(7) 1 d PU A 2 F46' F 0.224(3) 0.0532(14) 0.0357(7) 0.030(3) Uani 0.234(7) 1 d PU A 2 F47' F 0.079(2) -0.0089(15) 0.0129(7) 0.028(3) Uani 0.234(7) 1 d PU A 2 F48' F 0.200(5) -0.082(3) 0.0479(11) 0.028(3) Uani 0.234(7) 1 d PU A 2 F49' F -0.112(3) -0.0210(15) 0.0551(9) 0.028(3) Uani 0.234(7) 1 d PU A 2 F50' F -0.007(2) -0.1163(14) 0.0663(7) 0.030(4) Uani 0.234(7) 1 d PU A 2 F51' F -0.072(4) -0.059(2) 0.1022(10) 0.026(3) Uani 0.234(7) 1 d PU A 2 F52' F -0.009(2) 0.1212(13) 0.0486(6) 0.027(3) Uani 0.234(7) 1 d PU A 2 F53' F 0.107(3) 0.143(3) 0.0873(11) 0.027(3) Uani 0.234(7) 1 d PU A 2 F54' F -0.043(2) 0.0997(16) 0.1036(9) 0.030(3) Uani 0.234(7) 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 Ag1 0.0439(3) 0.0120(2) 0.0385(3) -0.0001(2) -0.0016(3) -0.0015(3) Ag2 0.0353(3) 0.0114(2) 0.0372(3) -0.0009(2) -0.0052(3) -0.0014(2) Al1 0.0148(9) 0.0096(9) 0.0182(9) 0.0003(7) -0.0004(7) -0.0004(8) Al2 0.0151(8) 0.0094(8) 0.0181(9) -0.0005(7) 0.0011(7) 0.0007(8) C1 0.023(4) 0.016(3) 0.015(3) -0.004(2) 0.002(3) -0.009(3) C2 0.033(5) 0.012(3) 0.029(4) -0.004(3) 0.009(3) 0.000(3) C3 0.021(4) 0.018(3) 0.028(4) -0.002(3) 0.009(3) 0.003(3) C4 0.011(3) 0.045(4) 0.029(4) -0.017(3) 0.000(3) -0.005(3) C5 0.022(4) 0.010(3) 0.019(3) 0.003(3) -0.001(3) -0.008(3) C6 0.026(4) 0.012(3) 0.025(4) 0.005(3) 0.003(3) -0.007(3) C7 0.045(5) 0.012(3) 0.029(4) -0.002(3) -0.008(4) -0.006(3) C8 0.030(5) 0.011(3) 0.040(5) 0.007(3) -0.003(4) -0.007(3) C9 0.014(3) 0.021(3) 0.020(3) 0.000(3) -0.002(3) -0.004(3) C10 0.017(4) 0.022(4) 0.036(4) -0.007(3) -0.002(3) 0.006(3) C11 0.024(4) 0.027(4) 0.023(4) 0.001(3) 0.003(3) -0.001(3) C12 0.021(4) 0.019(4) 0.034(4) -0.002(3) 0.005(3) -0.002(3) C13 0.018(3) 0.012(3) 0.031(4) 0.000(3) -0.005(3) -0.003(3) C14 0.017(4) 0.050(6) 0.064(6) 0.007(5) -0.005(4) -0.008(4) C15 0.040(5) 0.041(5) 0.043(5) -0.010(4) -0.012(4) 0.011(4) C16 0.029(5) 0.018(4) 0.088(8) 0.013(5) -0.016(5) -0.006(3) C17 0.029(4) 0.008(3) 0.024(3) 0.001(2) -0.003(3) 0.002(3) C18 0.055(5) 0.004(3) 0.032(4) 0.000(3) 0.001(4) -0.001(3) C19 0.028(4) 0.015(3) 0.041(5) 0.009(3) 0.006(4) -0.011(3) C20 0.033(4) 0.018(3) 0.030(4) 0.005(3) -0.005(3) 0.006(3) C21 0.017(3) 0.015(3) 0.022(3) 0.004(3) 0.000(3) 0.003(3) C25 0.014(3) 0.011(3) 0.026(3) -0.004(3) 0.001(2) 0.002(3) C26 0.028(4) 0.021(4) 0.033(4) 0.000(3) 0.009(3) -0.003(3) C27 0.008(3) 0.022(3) 0.028(4) -0.003(3) -0.001(3) -0.003(3) C28 0.025(4) 0.035(4) 0.031(4) 0.006(3) -0.002(3) 0.012(3) C29 0.016(3) 0.005(3) 0.026(3) 0.001(2) -0.001(3) -0.002(3) C30 0.019(4) 0.018(3) 0.034(4) 0.000(3) 0.001(3) -0.002(3) C31 0.031(4) 0.017(3) 0.020(3) -0.001(3) -0.001(3) -0.003(3) C32 0.033(4) 0.013(3) 0.028(4) -0.005(3) 0.002(3) -0.002(3) F1 0.055(3) 0.0121(19) 0.036(3) 0.0014(18) 0.010(2) -0.004(2) F2 0.033(3) 0.020(2) 0.045(3) 0.000(2) 0.007(2) 0.0068(19) F3 0.056(3) 0.018(2) 0.043(3) -0.013(2) 0.011(2) -0.006(2) F4 0.022(2) 0.027(2) 0.034(2) -0.0013(19) 0.0059(19) -0.0039(18) F5 0.055(3) 0.021(2) 0.023(2) -0.0107(18) 0.011(2) -0.003(2) F6 0.053(3) 0.023(2) 0.024(2) 0.0026(17) -0.002(2) 0.001(2) F7 0.026(3) 0.044(3) 0.048(3) -0.015(2) 0.010(2) -0.018(2) F8 0.031(3) 0.042(3) 0.045(3) -0.016(2) -0.004(2) 0.013(2) F9 0.028(3) 0.059(3) 0.033(3) -0.019(2) -0.003(2) -0.004(2) F10 0.036(3) 0.031(2) 0.023(2) 0.0024(18) -0.0047(19) -0.008(2) F11 0.039(3) 0.021(2) 0.036(3) 0.007(2) 0.002(2) -0.0051(19) F12 0.032(3) 0.023(2) 0.037(3) 0.0038(19) 0.010(2) -0.0011(19) F13 0.068(4) 0.016(2) 0.023(2) -0.0030(17) 0.000(2) -0.001(2) F14 0.033(3) 0.024(2) 0.044(3) -0.003(2) -0.010(2) -0.009(2) F15 0.054(3) 0.0071(18) 0.044(3) 0.0005(18) -0.004(2) -0.0003(19) F16 0.014(2) 0.035(3) 0.056(3) 0.010(2) -0.007(2) -0.0054(19) F17 0.031(3) 0.023(2) 0.054(3) 0.007(2) 0.016(2) 0.010(2) F18 0.031(3) 0.021(2) 0.051(3) 0.019(2) 0.001(2) 0.0079(19) F19 0.017(2) 0.036(3) 0.048(3) -0.007(2) 0.007(2) 0.0022(19) F20 0.029(3) 0.040(3) 0.038(3) 0.003(2) -0.010(2) 0.010(2) F21 0.030(2) 0.013(2) 0.054(3) -0.003(2) 0.003(2) 0.0078(18) F22 0.030(3) 0.045(3) 0.030(2) -0.011(2) 0.007(2) 0.003(2) F23 0.028(2) 0.025(2) 0.031(2) -0.0104(18) -0.0030(19) -0.0088(18) F24 0.043(3) 0.033(2) 0.025(2) 0.0068(19) 0.000(2) 0.007(2) F25 0.028(2) 0.027(2) 0.043(3) -0.011(2) -0.001(2) -0.016(2) F26 0.041(3) 0.027(2) 0.047(3) -0.003(2) 0.023(2) -0.011(2) F27 0.039(3) 0.013(2) 0.046(3) -0.0016(19) 0.011(2) -0.0024(19) F28 0.035(3) 0.079(4) 0.038(3) 0.004(3) 0.006(2) -0.001(3) F29 0.050(3) 0.040(3) 0.106(5) 0.028(3) -0.015(3) -0.023(3) F30 0.011(2) 0.049(3) 0.083(4) 0.006(3) -0.010(2) 0.000(2) F31 0.053(4) 0.050(3) 0.065(4) -0.030(3) -0.031(3) 0.013(3) F32 0.051(3) 0.045(3) 0.059(3) -0.011(3) -0.038(3) 0.005(3) F33 0.060(4) 0.107(6) 0.034(3) 0.014(3) -0.003(3) 0.000(4) F34 0.058(4) 0.034(3) 0.105(5) -0.030(3) -0.032(4) 0.019(3) F35 0.047(3) 0.031(3) 0.067(4) 0.017(3) -0.025(3) -0.002(2) F36 0.034(3) 0.032(3) 0.096(5) 0.030(3) -0.018(3) -0.018(2) F37 0.080(4) 0.020(2) 0.024(2) -0.0010(18) 0.001(3) 0.004(2) F38 0.037(3) 0.023(2) 0.061(3) 0.001(2) 0.021(3) 0.009(2) F39 0.074(4) 0.0088(18) 0.035(3) -0.0011(17) 0.001(3) -0.001(2) F40 0.043(3) 0.019(2) 0.058(3) 0.005(2) -0.022(3) -0.013(2) F41 0.033(3) 0.020(2) 0.063(3) 0.014(2) 0.005(2) -0.007(2) F42 0.016(2) 0.025(2) 0.074(4) -0.001(2) 0.012(2) -0.0046(19) F43 0.030(3) 0.030(2) 0.046(3) 0.010(2) -0.013(2) -0.006(2) F44 0.063(3) 0.027(2) 0.020(2) -0.0003(18) 0.006(2) -0.008(2) F45 0.042(3) 0.016(2) 0.039(3) 0.0122(19) -0.005(2) 0.0046(19) F55 0.042(3) 0.037(3) 0.050(3) -0.022(2) 0.009(2) -0.020(2) F56 0.053(3) 0.016(2) 0.059(3) 0.012(2) 0.009(3) 0.008(2) F57 0.035(3) 0.031(3) 0.065(3) -0.009(2) 0.023(3) -0.015(2) F58 0.038(3) 0.029(2) 0.044(3) -0.016(2) 0.011(2) -0.015(2) F59 0.039(3) 0.051(3) 0.024(2) 0.004(2) -0.005(2) 0.009(2) F60 0.021(2) 0.041(3) 0.037(3) -0.006(2) 0.009(2) -0.0021(19) F61 0.0081(18) 0.078(4) 0.047(3) 0.003(3) 0.0015(18) -0.005(2) F62 0.036(3) 0.034(3) 0.058(3) 0.016(2) 0.011(3) 0.024(2) F63 0.026(2) 0.065(4) 0.026(2) 0.009(2) 0.002(2) 0.004(2) F64 0.023(2) 0.026(2) 0.045(3) 0.000(2) -0.003(2) 0.0065(19) F65 0.026(2) 0.015(2) 0.046(3) -0.0020(19) 0.010(2) -0.0059(18) F66 0.031(3) 0.036(3) 0.037(3) -0.014(2) 0.014(2) -0.002(2) F67 0.039(3) 0.021(2) 0.025(2) 0.0035(17) -0.002(2) -0.0028(19) F68 0.016(2) 0.026(2) 0.036(2) -0.0011(19) -0.0007(19) 0.0036(17) F69 0.047(3) 0.024(2) 0.024(2) -0.0057(18) -0.009(2) -0.004(2) F70 0.047(3) 0.0116(18) 0.038(2) -0.0077(17) 0.006(2) 0.0045(19) F71 0.049(3) 0.0128(18) 0.031(2) 0.0047(17) -0.003(2) -0.003(2) F72 0.033(3) 0.019(2) 0.038(3) -0.0053(19) 0.004(2) -0.0082(19) O1 0.030(3) 0.012(2) 0.020(2) -0.0032(18) 0.000(2) 0.000(2) O2 0.025(3) 0.011(2) 0.021(2) 0.0054(18) -0.002(2) 0.0019(19) O3 0.011(2) 0.017(2) 0.021(2) 0.0014(19) 0.0054(18) 0.0023(18) O4 0.018(2) 0.013(2) 0.025(2) -0.002(2) -0.0068(18) 0.003(2) O5 0.024(2) 0.0079(19) 0.019(2) 0.0027(17) -0.001(2) -0.0054(19) O6 0.016(2) 0.016(2) 0.023(2) 0.003(2) -0.0052(18) -0.003(2) O7 0.019(2) 0.010(2) 0.024(2) -0.0029(19) 0.0001(19) -0.0005(19) O8 0.022(3) 0.010(2) 0.021(2) -0.0002(18) 0.004(2) 0.0018(19) P1 0.0331(12) 0.0155(8) 0.0278(10) -0.0003(7) 0.0073(9) 0.0015(8) P2 0.0383(12) 0.0176(8) 0.0224(9) 0.0011(7) 0.0040(9) 0.0058(9) P3 0.0252(11) 0.0199(9) 0.0384(12) 0.0076(9) -0.0027(9) 0.0043(8) P4 0.0289(11) 0.0154(9) 0.0623(16) -0.0082(10) -0.0088(11) -0.0043(8) P5 0.0269(11) 0.0136(8) 0.0336(11) 0.0008(8) 0.0077(8) -0.0001(7) P6 0.0337(12) 0.0158(9) 0.0597(15) 0.0104(10) -0.0123(12) 0.0027(8) P7 0.0219(10) 0.0188(9) 0.0425(12) -0.0047(8) -0.0012(9) -0.0046(8) P8 0.0225(10) 0.0199(9) 0.0519(14) -0.0015(9) -0.0049(10) -0.0048(8) P9 0.0335(12) 0.0164(8) 0.0252(10) 0.0009(7) 0.0020(9) -0.0013(8) P10 0.0457(14) 0.0177(9) 0.0287(11) -0.0021(8) 0.0096(10) -0.0048(9) P11 0.0260(11) 0.0236(10) 0.0524(14) 0.0108(9) -0.0003(10) 0.0045(9) P12 0.0543(14) 0.0173(9) 0.0230(9) 0.0018(7) 0.0049(10) -0.0019(10) P13 0.078(2) 0.0195(9) 0.0220(10) 0.0013(8) 0.0046(11) -0.0023(11) P14 0.0289(12) 0.0253(11) 0.0726(18) -0.0134(11) 0.0148(12) -0.0109(9) P15 0.0370(13) 0.0205(10) 0.0706(18) -0.0051(11) -0.0184(13) 0.0106(9) P16 0.0509(14) 0.0203(9) 0.0264(10) 0.0000(8) 0.0074(10) -0.0068(10) C22 0.020(3) 0.030(4) 0.028(4) -0.007(3) 0.001(3) -0.009(3) C23 0.019(3) 0.033(4) 0.029(3) 0.003(3) 0.002(3) 0.003(3) C24 0.022(3) 0.025(3) 0.029(4) 0.004(3) -0.004(3) -0.001(3) F46 0.020(4) 0.034(5) 0.029(5) -0.009(3) 0.002(4) 0.004(3) F47 0.021(3) 0.049(4) 0.030(3) -0.006(3) -0.002(3) -0.009(3) F48 0.037(4) 0.017(3) 0.046(4) -0.010(3) 0.000(3) -0.004(3) F49 0.018(3) 0.037(4) 0.034(3) 0.001(4) -0.005(2) 0.004(4) F50 0.018(3) 0.034(4) 0.025(4) 0.006(3) 0.002(3) -0.002(3) F51 0.023(4) 0.041(4) 0.037(3) -0.002(3) 0.003(3) 0.009(3) F52 0.032(4) 0.032(3) 0.032(4) 0.007(3) -0.008(3) 0.000(3) F53 0.025(3) 0.037(4) 0.034(3) 0.009(3) 0.011(3) 0.001(3) F54 0.026(5) 0.017(3) 0.037(5) -0.004(3) 0.004(3) -0.002(3) C22' 0.022(4) 0.035(5) 0.028(4) -0.002(4) 0.005(4) -0.005(4) C23' 0.020(5) 0.031(5) 0.034(5) -0.001(5) 0.003(5) 0.006(5) C24' 0.023(5) 0.030(4) 0.033(4) 0.000(4) -0.002(4) 0.000(4) F46' 0.029(6) 0.033(6) 0.028(5) 0.005(6) 0.007(5) -0.004(6) F47' 0.024(6) 0.039(7) 0.020(5) -0.004(6) 0.002(5) -0.017(6) F48' 0.021(6) 0.033(7) 0.032(7) -0.001(6) 0.005(6) -0.002(6) F49' 0.016(5) 0.033(7) 0.036(6) 0.001(6) 0.000(5) 0.006(6) F50' 0.026(7) 0.018(6) 0.046(7) -0.007(6) 0.002(6) 0.001(7) F51' 0.020(5) 0.029(7) 0.030(7) 0.005(6) 0.006(6) -0.001(6) F52' 0.023(6) 0.027(5) 0.031(6) 0.004(6) -0.009(5) -0.005(5) F53' 0.027(7) 0.020(5) 0.034(7) 0.001(6) 0.000(6) -0.005(6) F54' 0.022(6) 0.034(6) 0.035(5) -0.001(6) -0.001(6) 0.003(6) _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 Ag1 P9 2.548(2) . ? Ag1 P12 2.550(2) . ? Ag1 P13 2.552(2) . ? Ag1 P10 2.564(2) . ? Ag2 P2 2.551(2) . ? Ag2 P5 2.552(2) . ? Ag2 P16 2.554(2) . ? Ag2 P1 2.562(2) . ? Al1 O4 1.732(5) . ? Al1 O1 1.733(5) . ? Al1 O2 1.744(5) . ? Al1 O3 1.750(5) . ? Al2 O8 1.727(5) . ? Al2 O6 1.731(5) . ? Al2 O5 1.738(5) . ? Al2 O7 1.742(5) . ? C1 O1 1.352(8) . ? C1 C4 1.552(10) . ? C1 C3 1.566(9) . ? C1 C2 1.575(10) . ? C2 F2 1.318(9) . ? C2 F1 1.329(8) . ? C2 F3 1.362(8) . ? C3 F4 1.316(9) . ? C3 F6 1.346(8) . ? C3 F5 1.363(8) . ? C4 F9 1.326(9) . ? C4 F7 1.341(10) . ? C4 F8 1.350(10) . ? C5 O2 1.352(7) . ? C5 C8 1.515(11) . ? C5 C7 1.563(10) . ? C5 C6 1.578(10) . ? C6 F10 1.321(8) . ? C6 F12 1.328(9) . ? C6 F11 1.370(7) . ? C7 F13 1.337(9) . ? C7 F14 1.337(10) . ? C7 F15 1.342(8) . ? C8 F17 1.333(9) . ? C8 F18 1.353(8) . ? C8 F16 1.355(8) . ? C9 O3 1.363(8) . ? C9 C11 1.555(10) . ? C9 C10 1.567(10) . ? C9 C12 1.576(10) . ? C10 F20 1.322(9) . ? C10 F19 1.324(9) . ? C10 F21 1.357(9) . ? C11 F23 1.330(8) . ? C11 F22 1.340(8) . ? C11 F24 1.349(9) . ? C12 F25 1.325(9) . ? C12 F26 1.328(9) . ? C12 F27 1.347(9) . ? C13 O4 1.338(8) . ? C13 C14 1.540(11) . ? C13 C15 1.568(11) . ? C13 C16 1.567(10) . ? C14 F28 1.319(11) . ? C14 F30 1.333(10) . ? C14 F29 1.407(11) . ? C15 F31 1.286(11) . ? C15 F33 1.338(11) . ? C15 F32 1.381(10) . ? C16 F35 1.311(10) . ? C16 F36 1.313(10) . ? C16 F34 1.395(13) . ? C17 O5 1.355(7) . ? C17 C18 1.555(10) . ? C17 C20 1.556(10) . ? C17 C19 1.559(11) . ? C18 F38 1.322(10) . ? C18 F37 1.348(9) . ? C18 F39 1.348(8) . ? C19 F40 1.344(10) . ? C19 F42 1.345(9) . ? C19 F41 1.346(8) . ? C20 F44 1.320(9) . ? C20 F43 1.326(9) . ? C20 F45 1.364(8) . ? C21 O6 1.350(8) . ? C21 C22' 1.53(3) . ? C21 C23 1.544(11) . ? C21 C22 1.563(12) . ? C21 C24 1.585(12) . ? C21 C24' 1.63(4) . ? C21 C23' 1.64(4) . ? C25 O7 1.353(8) . ? C25 C27 1.549(9) . ? C25 C28 1.560(10) . ? C25 C26 1.589(10) . ? C26 F55 1.317(9) . ? C26 F56 1.331(10) . ? C26 F57 1.336(9) . ? C27 F59 1.329(8) . ? C27 F58 1.334(8) . ? C27 F60 1.370(7) . ? C28 F61 1.321(9) . ? C28 F63 1.334(9) . ? C28 F62 1.337(9) . ? C29 O8 1.354(8) . ? C29 C30 1.554(10) . ? C29 C31 1.575(10) . ? C29 C32 1.576(9) . ? C30 F66 1.333(9) . ? C30 F64 1.339(9) . ? C30 F65 1.348(8) . ? C31 F68 1.324(9) . ? C31 F67 1.340(8) . ? C31 F69 1.357(8) . ? C32 F71 1.319(9) . ? C32 F72 1.341(9) . ? C32 F70 1.347(8) . ? P1 P4 2.169(3) . ? P1 P3 2.171(3) . ? P1 P2 2.342(3) . ? P2 P3 2.176(3) . ? P2 P4 2.180(3) . ? P3 P4 2.200(3) . ? P5 P6 2.173(3) . ? P5 P7 2.181(3) . ? P5 P16 2.339(3) . ? P6 P16 2.184(3) . ? P6 P7 2.210(3) . ? P7 P16 2.179(3) . ? P8 P10 2.175(3) . ? P8 P9 2.184(3) . ? P8 P11 2.195(3) . ? P9 P11 2.170(3) . ? P9 P10 2.342(3) . ? P10 P11 2.168(3) . ? P12 P14 2.150(3) . ? P12 P15 2.158(3) . ? P12 P13 2.329(3) . ? P13 P14 2.160(3) . ? P13 P15 2.182(4) . ? P14 P15 2.189(4) . ? C22 F46 1.333(18) . ? C22 F48 1.346(12) . ? C22 F47 1.353(13) . ? C23 F51 1.343(13) . ? C23 F49 1.343(13) . ? C23 F50 1.361(16) . ? C24 F53 1.325(13) . ? C24 F54 1.327(16) . ? C24 F52 1.343(11) . ? C22' F47' 1.31(4) . ? C22' F46' 1.36(4) . ? C22' F48' 1.50(6) . ? C23' F51' 1.06(5) . ? C23' F49' 1.33(5) . ? C23' F50' 1.32(4) . ? C24' F53' 1.22(6) . ? C24' F52' 1.31(4) . ? C24' F54' 1.33(5) . ? 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 P9 Ag1 P12 173.46(7) . . ? P9 Ag1 P13 130.57(7) . . ? P12 Ag1 P13 54.32(7) . . ? P9 Ag1 P10 54.54(7) . . ? P12 Ag1 P10 120.90(7) . . ? P13 Ag1 P10 174.00(8) . . ? P2 Ag2 P5 176.28(8) . . ? P2 Ag2 P16 125.97(7) . . ? P5 Ag2 P16 54.52(7) . . ? P2 Ag2 P1 54.52(6) . . ? P5 Ag2 P1 124.41(7) . . ? P16 Ag2 P1 172.53(8) . . ? O4 Al1 O1 107.9(2) . . ? O4 Al1 O2 111.8(2) . . ? O1 Al1 O2 107.8(2) . . ? O4 Al1 O3 108.9(2) . . ? O1 Al1 O3 113.5(2) . . ? O2 Al1 O3 107.1(2) . . ? O8 Al2 O6 112.0(2) . . ? O8 Al2 O5 108.2(2) . . ? O6 Al2 O5 107.2(2) . . ? O8 Al2 O7 107.7(2) . . ? O6 Al2 O7 109.4(2) . . ? O5 Al2 O7 112.4(2) . . ? O1 C1 C4 112.4(6) . . ? O1 C1 C3 110.1(5) . . ? C4 C1 C3 109.3(6) . . ? O1 C1 C2 107.5(6) . . ? C4 C1 C2 108.8(6) . . ? C3 C1 C2 108.6(6) . . ? F2 C2 F1 108.4(7) . . ? F2 C2 F3 107.7(6) . . ? F1 C2 F3 107.4(6) . . ? F2 C2 C1 111.1(6) . . ? F1 C2 C1 110.6(6) . . ? F3 C2 C1 111.4(6) . . ? F4 C3 F6 108.9(6) . . ? F4 C3 F5 107.5(6) . . ? F6 C3 F5 106.0(6) . . ? F4 C3 C1 112.2(6) . . ? F6 C3 C1 110.2(6) . . ? F5 C3 C1 111.9(6) . . ? F9 C4 F7 108.1(6) . . ? F9 C4 F8 107.1(7) . . ? F7 C4 F8 106.1(6) . . ? F9 C4 C1 113.6(6) . . ? F7 C4 C1 111.6(7) . . ? F8 C4 C1 109.9(6) . . ? O2 C5 C8 112.3(5) . . ? O2 C5 C7 110.6(6) . . ? C8 C5 C7 109.7(6) . . ? O2 C5 C6 106.1(5) . . ? C8 C5 C6 109.3(6) . . ? C7 C5 C6 108.8(6) . . ? F10 C6 F12 109.0(6) . . ? F10 C6 F11 107.2(6) . . ? F12 C6 F11 106.3(6) . . ? F10 C6 C5 111.3(6) . . ? F12 C6 C5 111.8(6) . . ? F11 C6 C5 111.0(6) . . ? F13 C7 F14 108.4(7) . . ? F13 C7 F15 107.3(6) . . ? F14 C7 F15 107.5(6) . . ? F13 C7 C5 109.9(6) . . ? F14 C7 C5 111.6(6) . . ? F15 C7 C5 112.0(6) . . ? F17 C8 F18 106.9(6) . . ? F17 C8 F16 105.8(6) . . ? F18 C8 F16 106.1(6) . . ? F17 C8 C5 112.3(7) . . ? F18 C8 C5 113.9(6) . . ? F16 C8 C5 111.3(6) . . ? O3 C9 C11 110.4(5) . . ? O3 C9 C10 108.5(6) . . ? C11 C9 C10 109.7(6) . . ? O3 C9 C12 110.2(6) . . ? C11 C9 C12 109.6(6) . . ? C10 C9 C12 108.4(6) . . ? F20 C10 F19 110.0(6) . . ? F20 C10 F21 106.6(6) . . ? F19 C10 F21 108.7(6) . . ? F20 C10 C9 109.9(6) . . ? F19 C10 C9 112.4(6) . . ? F21 C10 C9 109.0(6) . . ? F23 C11 F22 107.5(6) . . ? F23 C11 F24 107.6(6) . . ? F22 C11 F24 106.8(6) . . ? F23 C11 C9 111.4(6) . . ? F22 C11 C9 112.4(6) . . ? F24 C11 C9 110.9(6) . . ? F25 C12 F26 109.1(6) . . ? F25 C12 F27 107.8(6) . . ? F26 C12 F27 107.4(6) . . ? F25 C12 C9 111.1(6) . . ? F26 C12 C9 112.0(6) . . ? F27 C12 C9 109.3(6) . . ? O4 C13 C14 112.6(6) . . ? O4 C13 C15 107.4(6) . . ? C14 C13 C15 109.9(7) . . ? O4 C13 C16 112.2(6) . . ? C14 C13 C16 107.4(7) . . ? C15 C13 C16 107.2(7) . . ? F28 C14 F30 108.4(8) . . ? F28 C14 F29 104.7(8) . . ? F30 C14 F29 106.9(7) . . ? F28 C14 C13 112.6(6) . . ? F30 C14 C13 115.8(8) . . ? F29 C14 C13 107.6(8) . . ? F31 C15 F33 107.5(8) . . ? F31 C15 F32 108.4(7) . . ? F33 C15 F32 107.5(7) . . ? F31 C15 C13 112.6(7) . . ? F33 C15 C13 110.5(7) . . ? F32 C15 C13 110.2(7) . . ? F35 C16 F36 111.9(8) . . ? F35 C16 F34 106.1(8) . . ? F36 C16 F34 104.7(8) . . ? F35 C16 C13 115.7(7) . . ? F36 C16 C13 110.5(7) . . ? F34 C16 C13 107.2(8) . . ? O5 C17 C18 111.5(6) . . ? O5 C17 C20 107.3(6) . . ? C18 C17 C20 109.3(6) . . ? O5 C17 C19 110.4(6) . . ? C18 C17 C19 109.4(6) . . ? C20 C17 C19 108.9(6) . . ? F38 C18 F37 108.0(7) . . ? F38 C18 F39 108.6(6) . . ? F37 C18 F39 106.9(6) . . ? F38 C18 C17 111.3(7) . . ? F37 C18 C17 109.3(6) . . ? F39 C18 C17 112.4(7) . . ? F40 C19 F42 107.0(7) . . ? F40 C19 F41 107.9(6) . . ? F42 C19 F41 107.5(6) . . ? F40 C19 C17 111.3(6) . . ? F42 C19 C17 110.7(6) . . ? F41 C19 C17 112.2(6) . . ? F44 C20 F43 108.4(6) . . ? F44 C20 F45 107.0(6) . . ? F43 C20 F45 106.7(6) . . ? F44 C20 C17 111.9(6) . . ? F43 C20 C17 111.1(6) . . ? F45 C20 C17 111.5(6) . . ? O6 C21 C22' 111.8(13) . . ? O6 C21 C23 108.8(6) . . ? C22' C21 C23 136.5(13) . . ? O6 C21 C22 110.0(6) . . ? C22' C21 C22 41.1(13) . . ? C23 C21 C22 109.5(7) . . ? O6 C21 C24 111.9(6) . . ? C22' C21 C24 69.6(14) . . ? C23 C21 C24 108.7(7) . . ? C22 C21 C24 107.9(7) . . ? O6 C21 C24' 107.3(13) . . ? C22' C21 C24' 112.2(19) . . ? C23 C21 C24' 68.5(13) . . ? C22 C21 C24' 140.7(14) . . ? C24 C21 C24' 44.9(13) . . ? O6 C21 C23' 106.1(13) . . ? C22' C21 C23' 113.0(18) . . ? C23 C21 C23' 38.5(12) . . ? C22 C21 C23' 75.0(13) . . ? C24 C21 C23' 137.5(14) . . ? C24' C21 C23' 105.9(18) . . ? O7 C25 C27 107.0(5) . . ? O7 C25 C28 111.3(6) . . ? C27 C25 C28 110.2(6) . . ? O7 C25 C26 111.3(5) . . ? C27 C25 C26 108.7(6) . . ? C28 C25 C26 108.3(6) . . ? F55 C26 F56 109.1(7) . . ? F55 C26 F57 108.2(7) . . ? F56 C26 F57 108.1(6) . . ? F55 C26 C25 110.7(6) . . ? F56 C26 C25 109.9(6) . . ? F57 C26 C25 110.7(6) . . ? F59 C27 F58 107.7(6) . . ? F59 C27 F60 106.9(6) . . ? F58 C27 F60 105.8(6) . . ? F59 C27 C25 112.6(6) . . ? F58 C27 C25 111.3(6) . . ? F60 C27 C25 112.2(5) . . ? F61 C28 F63 108.1(7) . . ? F61 C28 F62 108.2(7) . . ? F63 C28 F62 107.6(7) . . ? F61 C28 C25 112.9(6) . . ? F63 C28 C25 109.9(6) . . ? F62 C28 C25 110.0(6) . . ? O8 C29 C30 112.3(6) . . ? O8 C29 C31 110.3(5) . . ? C30 C29 C31 109.2(6) . . ? O8 C29 C32 107.6(5) . . ? C30 C29 C32 108.4(6) . . ? C31 C29 C32 108.9(5) . . ? F66 C30 F64 107.8(6) . . ? F66 C30 F65 107.5(6) . . ? F64 C30 F65 106.7(6) . . ? F66 C30 C29 113.3(6) . . ? F64 C30 C29 111.5(6) . . ? F65 C30 C29 109.8(6) . . ? F68 C31 F67 108.4(6) . . ? F68 C31 F69 107.7(6) . . ? F67 C31 F69 107.8(6) . . ? F68 C31 C29 110.9(6) . . ? F67 C31 C29 110.0(6) . . ? F69 C31 C29 112.0(6) . . ? F71 C32 F72 107.6(6) . . ? F71 C32 F70 108.3(6) . . ? F72 C32 F70 106.7(6) . . ? F71 C32 C29 111.3(6) . . ? F72 C32 C29 110.4(6) . . ? F70 C32 C29 112.3(6) . . ? C1 O1 Al1 146.3(5) . . ? C5 O2 Al1 147.1(5) . . ? C9 O3 Al1 147.2(4) . . ? C13 O4 Al1 147.3(5) . . ? C17 O5 Al2 146.3(4) . . ? C21 O6 Al2 148.1(4) . . ? C25 O7 Al2 147.2(4) . . ? C29 O8 Al2 145.5(4) . . ? P4 P1 P3 60.90(10) . . ? P4 P1 P2 57.66(10) . . ? P3 P1 P2 57.50(9) . . ? P4 P1 Ag2 110.73(11) . . ? P3 P1 Ag2 110.38(10) . . ? P2 P1 Ag2 62.49(7) . . ? P3 P2 P4 60.65(10) . . ? P3 P2 P1 57.31(9) . . ? P4 P2 P1 57.19(10) . . ? P3 P2 Ag2 110.64(10) . . ? P4 P2 Ag2 110.76(11) . . ? P1 P2 Ag2 62.99(7) . . ? P1 P3 P2 65.20(10) . . ? P1 P3 P4 59.50(10) . . ? P2 P3 P4 59.78(10) . . ? P1 P4 P2 65.15(9) . . ? P1 P4 P3 59.60(10) . . ? P2 P4 P3 59.56(10) . . ? P6 P5 P7 61.01(10) . . ? P6 P5 P16 57.75(10) . . ? P7 P5 P16 57.52(9) . . ? P6 P5 Ag2 113.04(11) . . ? P7 P5 Ag2 108.41(10) . . ? P16 P5 Ag2 62.78(7) . . ? P5 P6 P16 64.93(10) . . ? P5 P6 P7 59.68(10) . . ? P16 P6 P7 59.46(10) . . ? P16 P7 P5 64.87(10) . . ? P16 P7 P6 59.66(11) . . ? P5 P7 P6 59.31(10) . . ? P10 P8 P9 65.01(9) . . ? P10 P8 P11 59.48(10) . . ? P9 P8 P11 59.40(10) . . ? P11 P9 P8 60.54(10) . . ? P11 P9 P10 57.27(10) . . ? P8 P9 P10 57.30(9) . . ? P11 P9 Ag1 111.11(10) . . ? P8 P9 Ag1 110.59(10) . . ? P10 P9 Ag1 63.08(7) . . ? P11 P10 P8 60.73(10) . . ? P11 P10 P9 57.36(9) . . ? P8 P10 P9 57.70(10) . . ? P11 P10 Ag1 110.59(11) . . ? P8 P10 Ag1 110.33(11) . . ? P9 P10 Ag1 62.38(7) . . ? P10 P11 P9 65.37(10) . . ? P10 P11 P8 59.80(10) . . ? P9 P11 P8 60.06(10) . . ? P14 P12 P15 61.06(12) . . ? P14 P12 P13 57.49(11) . . ? P15 P12 P13 58.05(11) . . ? P14 P12 Ag1 110.72(11) . . ? P15 P12 Ag1 111.36(11) . . ? P13 P12 Ag1 62.89(7) . . ? P14 P13 P15 60.53(11) . . ? P14 P13 P12 57.08(10) . . ? P15 P13 P12 57.05(11) . . ? P14 P13 Ag1 110.30(12) . . ? P15 P13 Ag1 110.45(12) . . ? P12 P13 Ag1 62.78(7) . . ? P12 P14 P13 65.44(10) . . ? P12 P14 P15 59.66(11) . . ? P13 P14 P15 60.25(12) . . ? P12 P15 P13 64.90(10) . . ? P12 P15 P14 59.28(11) . . ? P13 P15 P14 59.22(12) . . ? P7 P16 P6 60.88(10) . . ? P7 P16 P5 57.61(9) . . ? P6 P16 P5 57.31(10) . . ? P7 P16 Ag2 108.42(10) . . ? P6 P16 Ag2 112.59(11) . . ? P5 P16 Ag2 62.70(7) . . ? F46 C22 F48 111.0(10) . . ? F46 C22 F47 106.1(9) . . ? F48 C22 F47 106.1(8) . . ? F46 C22 C21 110.8(9) . . ? F48 C22 C21 109.5(8) . . ? F47 C22 C21 113.1(8) . . ? F51 C23 F49 106.0(9) . . ? F51 C23 F50 103.9(9) . . ? F49 C23 F50 109.8(10) . . ? F51 C23 C21 112.1(8) . . ? F49 C23 C21 113.6(8) . . ? F50 C23 C21 111.0(9) . . ? F53 C24 F54 106.2(9) . . ? F53 C24 F52 106.9(8) . . ? F54 C24 F52 109.6(10) . . ? F53 C24 C21 111.4(8) . . ? F54 C24 C21 110.2(9) . . ? F52 C24 C21 112.2(8) . . ? F47' C22' F46' 110(3) . . ? F47' C22' F48' 111(3) . . ? F46' C22' F48' 114(3) . . ? F47' C22' C21 113(2) . . ? F46' C22' C21 110(2) . . ? F48' C22' C21 100(3) . . ? F51' C23' F49' 112(4) . . ? F51' C23' F50' 102(4) . . ? F49' C23' F50' 105(3) . . ? F51' C23' C21 121(4) . . ? F49' C23' C21 108(3) . . ? F50' C23' C21 108(2) . . ? F53' C24' F52' 107(4) . . ? F53' C24' F54' 104(3) . . ? F52' C24' F54' 111(3) . . ? F53' C24' C21 115(3) . . ? F52' C24' C21 111(3) . . ? F54' C24' C21 109(3) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.54 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.382 _refine_diff_density_min -1.307 _refine_diff_density_rms 0.142 data_ns_cu(c2h4)3_chemcom _database_code_depnum_ccdc_archive 'CCDC 654311' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C66 H36 Al3 Cu3 F108 O12' _chemical_formula_sum 'C66 H36 Al3 Cu3 F108 O12' _chemical_formula_weight 3344.51 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' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 12.8455(6) _cell_length_b 44.862(2) _cell_length_c 18.9555(9) _cell_angle_alpha 90.00 _cell_angle_beta 102.506(3) _cell_angle_gamma 90.00 _cell_volume 10664.4(9) _cell_formula_units_Z 4 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description blocks _exptl_crystal_colour colourless _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.083 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 6504 _exptl_absorpt_coefficient_mu 0.861 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.86494 _exptl_absorpt_correction_T_max 0.96 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(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 'Bruker APEX II CCD area detector at 100K' _diffrn_measurement_method 'APEXII (Bruker, 2005)' _diffrn_detector_area_resol_mean 'frames each covering 0.5\% in\w' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 143838 _diffrn_reflns_av_R_equivalents 0.1711 _diffrn_reflns_av_sigmaI/netI 0.0897 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -49 _diffrn_reflns_limit_k_max 49 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 0.91 _diffrn_reflns_theta_max 23.30 _reflns_number_total 15375 _reflns_number_gt 8407 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Bruker AXS BV, 1997-2004)' _computing_cell_refinement 'Saint V7.23A (Bruker AXS BV, 1997-2004)' _computing_data_reduction 'Sadabs 2004/1 (Bruker AXS BV, 1997-2004)' _computing_structure_solution 'SHELXTL (Bruker, 2001)' _computing_structure_refinement 'SHELXTL (Bruker, 2001)' _computing_molecular_graphics 'SHELXTL (Bruker, 2001)' _computing_publication_material 'SHELXTL (Bruker, 2001)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0426P)^2^+69.9242P] 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 15375 _refine_ls_number_parameters 1817 _refine_ls_number_restraints 45 _refine_ls_R_factor_all 0.1529 _refine_ls_R_factor_gt 0.0755 _refine_ls_wR_factor_ref 0.1832 _refine_ls_wR_factor_gt 0.1431 _refine_ls_goodness_of_fit_ref 1.044 _refine_ls_restrained_S_all 1.055 _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 Cu1 Cu 0.26396(6) 0.587220(17) 0.17886(4) 0.0329(2) Uani 1 1 d . . . Cu2 Cu 0.72985(5) 0.420096(17) 0.31291(4) 0.0299(2) Uani 1 1 d . . . Cu3 Cu 0.24244(5) 0.251426(18) 0.16857(4) 0.0344(2) Uani 1 1 d . . . C50 C 0.1777(5) 0.5748(2) 0.2608(4) 0.069(3) Uani 1 1 d . . . C51 C 0.1862(5) 0.60417(19) 0.2599(4) 0.063(2) Uani 1 1 d . . . H51A H 0.2330 0.6134 0.3028 0.076 Uiso 1 1 calc R . . H51B H 0.1193 0.6154 0.2422 0.076 Uiso 1 1 calc R . . C52 C 0.2934(7) 0.63386(17) 0.1576(4) 0.065(3) Uani 1 1 d . . . C53 C 0.3395(6) 0.6176(2) 0.1155(5) 0.074(3) Uani 1 1 d . . . C54 C 0.3278(6) 0.55261(17) 0.1196(4) 0.063(3) Uani 1 1 d . . . C55 C 0.2639(7) 0.53960(16) 0.1563(4) 0.060(3) Uani 1 1 d . . . C60 C 0.6795(6) 0.45990(16) 0.3603(4) 0.055(2) Uani 1 1 d . . . C61 C 0.7474(7) 0.46827(15) 0.3226(4) 0.057(2) Uani 1 1 d . . . C62 C 0.8347(5) 0.4240(2) 0.2379(4) 0.056(2) Uani 1 1 d . . . C63 C 0.8129(6) 0.39541(19) 0.2428(4) 0.057(2) Uani 1 1 d . . . C64 C 0.6737(6) 0.37639(16) 0.3379(4) 0.054(2) Uani 1 1 d . . . C65 C 0.6294(6) 0.39634(19) 0.3726(4) 0.061(2) Uani 1 1 d . . . C70 C 0.2602(8) 0.20541(18) 0.1413(5) 0.089(3) Uani 1 1 d U . . H70A H 0.2966 0.1923 0.1810 0.107 Uiso 1 1 calc R . . H70B H 0.1981 0.1959 0.1090 0.107 Uiso 1 1 calc R . . C71 C 0.3225(7) 0.2221(2) 0.1098(5) 0.093(3) Uani 1 1 d U . . H71A H 0.3019 0.2236 0.0564 0.112 Uiso 1 1 calc R . . H71B H 0.4003 0.2199 0.1283 0.112 Uiso 1 1 calc R . . C72 C 0.3182(7) 0.2854(2) 0.1175(5) 0.097(3) Uani 1 1 d U . . H72A H 0.3963 0.2875 0.1347 0.116 Uiso 1 1 calc R . . H72B H 0.2941 0.2873 0.0644 0.116 Uiso 1 1 calc R . . C73 C 0.2586(8) 0.2985(2) 0.1567(6) 0.107(3) Uani 1 1 d U . . H73A H 0.1948 0.3091 0.1298 0.129 Uiso 1 1 calc R . . H73B H 0.2970 0.3094 0.2000 0.129 Uiso 1 1 calc R . . C74 C 0.1552(8) 0.2647(3) 0.2461(5) 0.114(3) Uani 1 1 d U . . H74A H 0.1973 0.2729 0.2920 0.136 Uiso 1 1 calc R . . H74B H 0.0880 0.2756 0.2275 0.136 Uiso 1 1 calc R . . C75 C 0.1501(6) 0.2353(2) 0.2410(5) 0.088(3) Uani 1 1 d U . . H75A H 0.0796 0.2267 0.2189 0.106 Uiso 1 1 calc R . . H75B H 0.1890 0.2239 0.2834 0.106 Uiso 1 1 calc R . . H50A H 0.110(4) 0.5678(12) 0.236(3) 0.039(17) Uiso 1 1 d . . . H50B H 0.231(5) 0.5641(15) 0.296(4) 0.07(2) Uiso 1 1 d . . . H52A H 0.218(6) 0.6425(17) 0.149(4) 0.10(3) Uiso 1 1 d . . . H52B H 0.323(5) 0.6408(15) 0.205(4) 0.07(2) Uiso 1 1 d . . . H53B H 0.402(6) 0.6152(16) 0.128(4) 0.08(3) Uiso 1 1 d . . . H53A H 0.295(7) 0.6151(19) 0.070(5) 0.11(3) Uiso 1 1 d . . . H54A H 0.290(5) 0.5599(14) 0.065(3) 0.06(2) Uiso 1 1 d . . . H54B H 0.412(6) 0.5558(17) 0.135(4) 0.09(3) Uiso 1 1 d . . . H55A H 0.176(4) 0.5314(12) 0.130(3) 0.043(17) Uiso 1 1 d . . . H55B H 0.292(5) 0.5299(14) 0.203(4) 0.07(2) Uiso 1 1 d . . . H60A H 0.603(6) 0.4586(18) 0.348(4) 0.10(3) Uiso 1 1 d . . . H60B H 0.685(4) 0.4553(12) 0.411(3) 0.035(16) Uiso 1 1 d . . . H61A H 0.727(6) 0.4750(17) 0.269(4) 0.10(3) Uiso 1 1 d . . . H61B H 0.828(6) 0.4737(15) 0.345(4) 0.08(2) Uiso 1 1 d . . . H62A H 0.796(4) 0.4326(12) 0.195(3) 0.038(17) Uiso 1 1 d . . . H62B H 0.897(5) 0.4290(13) 0.265(3) 0.05(2) Uiso 1 1 d . . . H63A H 0.767(4) 0.3889(12) 0.213(3) 0.034(17) Uiso 1 1 d . . . H63B H 0.860(5) 0.3865(13) 0.272(3) 0.05(2) Uiso 1 1 d . . . H64B H 0.747(5) 0.3651(14) 0.361(3) 0.07(2) Uiso 1 1 d . . . H64A H 0.651(6) 0.3686(16) 0.290(4) 0.08(3) Uiso 1 1 d . . . H65A H 0.570(6) 0.4045(16) 0.355(4) 0.08(2) Uiso 1 1 d . . . H65B H 0.668(5) 0.4006(14) 0.428(4) 0.07(2) Uiso 1 1 d . . . Al1 Al 0.73989(11) 0.25060(4) 0.50434(8) 0.0176(4) Uani 1 1 d . . . O1 O 0.6438(3) 0.24462(9) 0.42689(19) 0.0300(11) Uani 1 1 d . . . O2 O 0.8618(3) 0.24234(9) 0.4856(2) 0.0326(11) Uani 1 1 d . . . O3 O 0.7217(3) 0.22790(8) 0.5741(2) 0.0306(11) Uani 1 1 d . . . O4 O 0.7320(3) 0.28726(8) 0.5293(2) 0.0355(12) Uani 1 1 d . . . C1 C 0.5433(4) 0.24868(13) 0.3894(3) 0.0263(15) Uani 1 1 d . . . C2 C 0.5276(5) 0.28127(14) 0.3617(3) 0.0391(19) Uani 1 1 d . . . C3 C 0.5252(5) 0.22685(16) 0.3245(4) 0.045(2) Uani 1 1 d . . . C4 C 0.4611(4) 0.24189(15) 0.4358(3) 0.0393(19) Uani 1 1 d . . . C5 C 0.9288(4) 0.24484(13) 0.4402(3) 0.0264(16) Uani 1 1 d . . . C6 C 0.9002(5) 0.22170(15) 0.3779(3) 0.042(2) Uani 1 1 d . . . C7 C 0.9289(5) 0.27652(15) 0.4089(3) 0.0379(19) Uani 1 1 d . . . C8 C 1.0428(4) 0.23701(15) 0.4850(3) 0.0360(18) Uani 1 1 d . . . C9 C 0.7357(5) 0.20143(13) 0.6083(3) 0.0301(17) Uani 1 1 d . . . C10 C 0.6727(7) 0.2018(2) 0.6687(5) 0.087(3) Uani 1 1 d U . . C11 C 0.8561(7) 0.19707(18) 0.6454(6) 0.121(4) Uani 1 1 d . . . C12 C 0.7057(9) 0.17570(16) 0.5562(4) 0.093(4) Uani 1 1 d . . . C13 C 0.7497(5) 0.30874(13) 0.5805(3) 0.0286(17) Uani 1 1 d . . . C14 C 0.7328(5) 0.33896(14) 0.5417(3) 0.0369(19) Uani 1 1 d . . . C15 C 0.6694(6) 0.30561(14) 0.6298(4) 0.044(2) Uani 1 1 d . . . C16 C 0.8652(5) 0.30779(15) 0.6279(4) 0.044(2) Uani 1 1 d . . . F1 F 0.4412(3) 0.28364(10) 0.3052(2) 0.0691(14) Uani 1 1 d . . . F2 F 0.6100(3) 0.29066(9) 0.3363(2) 0.0596(13) Uani 1 1 d . . . F3 F 0.5135(3) 0.29994(8) 0.4125(2) 0.0567(13) Uani 1 1 d . . . F4 F 0.4199(3) 0.22362(10) 0.2944(2) 0.0665(14) Uani 1 1 d . . . F5 F 0.5707(3) 0.23675(10) 0.2726(2) 0.0668(14) Uani 1 1 d . . . F6 F 0.5628(3) 0.20018(9) 0.3433(2) 0.0608(13) Uani 1 1 d . . . F7 F 0.3631(3) 0.25213(10) 0.4079(2) 0.0665(14) Uani 1 1 d . . . F8 F 0.4523(3) 0.21321(9) 0.4472(2) 0.0584(13) Uani 1 1 d . . . F9 F 0.4921(3) 0.25454(9) 0.5009(2) 0.0578(12) Uani 1 1 d . . . F10 F 0.9798(3) 0.21691(9) 0.3435(2) 0.0599(13) Uani 1 1 d . . . F11 F 0.8159(3) 0.23090(10) 0.32932(19) 0.0625(13) Uani 1 1 d . . . F12 F 0.8759(3) 0.19549(9) 0.4019(2) 0.0618(13) Uani 1 1 d . . . F13 F 1.1196(3) 0.24537(10) 0.4515(2) 0.0634(14) Uani 1 1 d . . . F14 F 1.0616(3) 0.25189(9) 0.54811(19) 0.0565(12) Uani 1 1 d . . . F15 F 1.0548(3) 0.20850(9) 0.4995(2) 0.0571(12) Uani 1 1 d . . . F16 F 0.9763(3) 0.27747(9) 0.3525(2) 0.0563(12) Uani 1 1 d . . . F17 F 0.9794(3) 0.29544(8) 0.4580(2) 0.0539(12) Uani 1 1 d . . . F18 F 0.8299(3) 0.28598(8) 0.3861(2) 0.0509(11) Uani 1 1 d . . . F19 F 0.6607(4) 0.17446(9) 0.6942(3) 0.0932(16) Uani 1 1 d . . . F20 F 0.5855(3) 0.21473(11) 0.6530(3) 0.0952(17) Uani 1 1 d . . . F21 F 0.7489(6) 0.21942(12) 0.7251(2) 0.143(3) Uani 1 1 d . . . F22 F 0.8702(4) 0.17522(9) 0.6935(2) 0.0749(15) Uani 1 1 d . . . F23 F 0.9044(3) 0.21946(10) 0.6669(3) 0.105(2) Uani 1 1 d . . . F24 F 0.8990(5) 0.18544(13) 0.5812(4) 0.180(2) Uani 1 1 d . . . F25 F 0.7324(4) 0.14891(8) 0.5823(2) 0.0664(14) Uani 1 1 d . . . F26 F 0.7192(6) 0.17924(10) 0.4946(2) 0.113(2) Uani 1 1 d . . . F27 F 0.5811(5) 0.17750(13) 0.5505(4) 0.214(3) Uani 1 1 d . . . F28 F 0.7838(3) 0.33998(8) 0.4875(2) 0.0549(12) Uani 1 1 d . . . F29 F 0.6309(3) 0.34382(9) 0.5118(2) 0.0618(13) Uani 1 1 d . . . F30 F 0.7666(3) 0.36197(8) 0.5839(2) 0.0606(13) Uani 1 1 d . . . F31 F 0.5718(3) 0.30048(11) 0.5927(2) 0.0781(15) Uani 1 1 d . . . F32 F 0.6974(4) 0.28298(10) 0.6754(2) 0.0770(14) Uani 1 1 d . . . F33 F 0.6642(3) 0.32947(9) 0.6702(2) 0.0645(13) Uani 1 1 d . . . F34 F 0.8903(3) 0.27968(9) 0.6456(2) 0.0746(15) Uani 1 1 d . . . F35 F 0.9355(3) 0.31674(10) 0.5908(2) 0.0635(14) Uani 1 1 d . . . F36 F 0.8774(3) 0.32413(9) 0.6864(2) 0.0648(14) Uani 1 1 d . . . Al2 Al 0.23615(12) 0.41756(4) 0.48143(8) 0.0193(4) Uani 1 1 d . . . O5 O 0.1112(3) 0.42566(8) 0.49655(19) 0.0260(11) Uani 1 1 d . . . O6 O 0.2434(3) 0.38129(9) 0.4536(2) 0.0323(11) Uani 1 1 d . . . O7 O 0.3282(3) 0.42244(9) 0.5620(2) 0.0301(11) Uani 1 1 d . . . O8 O 0.2588(3) 0.44121(8) 0.41489(19) 0.0263(11) Uani 1 1 d . . . C17 C 0.0420(4) 0.42280(13) 0.5402(3) 0.0255(16) Uani 1 1 d . . . C18 C 0.0419(5) 0.39112(14) 0.5710(3) 0.0355(18) Uani 1 1 d . . . C19 C -0.0705(5) 0.43016(16) 0.4940(3) 0.0398(19) Uani 1 1 d . . . C20 C 0.0678(5) 0.44557(15) 0.6037(3) 0.042(2) Uani 1 1 d . . . C21 C 0.2275(5) 0.36065(12) 0.4002(3) 0.0277(16) Uani 1 1 d . . . C22 C 0.1151(5) 0.36407(15) 0.3490(4) 0.045(2) Uani 1 1 d . . . C23 C 0.3120(6) 0.36415(15) 0.3548(4) 0.045(2) Uani 1 1 d . . . C24 C 0.2380(5) 0.32991(14) 0.4367(4) 0.0382(19) Uani 1 1 d . . . C25 C 0.4276(4) 0.41782(13) 0.6028(3) 0.0279(16) Uani 1 1 d . . . C26 C 0.5126(5) 0.42518(16) 0.5603(4) 0.043(2) Uani 1 1 d . . . C27 C 0.4388(5) 0.38511(15) 0.6294(4) 0.045(2) Uani 1 1 d . . . C28 C 0.4423(5) 0.43858(16) 0.6685(4) 0.046(2) Uani 1 1 d . . . C29 C 0.2510(4) 0.46851(12) 0.3843(3) 0.0250(16) Uani 1 1 d . . . C30 C 0.2452(10) 0.49288(16) 0.4382(5) 0.112(4) Uani 1 1 d . . . C31 C 0.1555(7) 0.4694(2) 0.3203(6) 0.139(4) Uani 1 1 d . . . C32 C 0.3544(7) 0.47397(18) 0.3571(6) 0.124(3) Uani 1 1 d . . . F37 F 0.1404(3) 0.38083(8) 0.5941(2) 0.0467(11) Uani 1 1 d . . . F38 F -0.0069(3) 0.37221(8) 0.5189(2) 0.0547(12) Uani 1 1 d . . . F39 F -0.0086(3) 0.38909(9) 0.6256(2) 0.0503(11) Uani 1 1 d . . . F40 F -0.0806(3) 0.45922(9) 0.4794(2) 0.0516(12) Uani 1 1 d . . . F41 F -0.0868(3) 0.41580(9) 0.43000(19) 0.0511(12) Uani 1 1 d . . . F42 F -0.1495(3) 0.42198(9) 0.5259(2) 0.0579(13) Uani 1 1 d . . . F43 F 0.0931(3) 0.47189(8) 0.5815(2) 0.0536(12) Uani 1 1 d . . . F44 F 0.1519(3) 0.43572(9) 0.65328(18) 0.0555(12) Uani 1 1 d . . . F45 F -0.0121(3) 0.44923(9) 0.63713(19) 0.0537(12) Uani 1 1 d . . . F46 F 0.0948(3) 0.39235(9) 0.3326(2) 0.0653(14) Uani 1 1 d . . . F47 F 0.1064(3) 0.34836(9) 0.2888(2) 0.0673(14) Uani 1 1 d . . . F48 F 0.0396(3) 0.35410(10) 0.3820(2) 0.0638(14) Uani 1 1 d . . . F49 F 0.4092(3) 0.36749(10) 0.3969(2) 0.0676(14) Uani 1 1 d . . . F50 F 0.3194(3) 0.34056(9) 0.3125(2) 0.0669(13) Uani 1 1 d . . . F51 F 0.2945(4) 0.38789(9) 0.3120(2) 0.0658(13) Uani 1 1 d . . . F52 F 0.2046(3) 0.30767(8) 0.3897(2) 0.0642(14) Uani 1 1 d . . . F53 F 0.3380(3) 0.32385(8) 0.4687(2) 0.0531(12) Uani 1 1 d . . . F54 F 0.1808(3) 0.32823(8) 0.4866(2) 0.0525(12) Uani 1 1 d . . . F55 F 0.5235(3) 0.45412(9) 0.5528(2) 0.0687(14) Uani 1 1 d . . . F56 F 0.4873(3) 0.41344(10) 0.4936(2) 0.0653(14) Uani 1 1 d . . . F57 F 0.6095(3) 0.41438(10) 0.5912(2) 0.0603(13) Uani 1 1 d . . . F58 F 0.4565(3) 0.36684(9) 0.5771(2) 0.0665(14) Uani 1 1 d . . . F59 F 0.3546(3) 0.37530(9) 0.6496(2) 0.0674(14) Uani 1 1 d . . . F60 F 0.5235(3) 0.38155(9) 0.6857(2) 0.0616(13) Uani 1 1 d . . . F61 F 0.4057(3) 0.46564(9) 0.6508(2) 0.0725(15) Uani 1 1 d . . . F62 F 0.5445(3) 0.44135(10) 0.7035(2) 0.0665(14) Uani 1 1 d . . . F63 F 0.3896(3) 0.42832(11) 0.7174(2) 0.0716(15) Uani 1 1 d . . . F64 F 0.1332(3) 0.49673(9) 0.2932(2) 0.0777(15) Uani 1 1 d . . . F65 F 0.2107(7) 0.45202(13) 0.2636(3) 0.163(3) Uani 1 1 d . . . F66 F 0.0778(3) 0.45504(10) 0.3241(3) 0.0840(17) Uani 1 1 d . . . F67 F 0.2528(3) 0.52016(8) 0.4162(2) 0.0631(14) Uani 1 1 d . . . F68 F 0.1119(5) 0.49002(12) 0.4285(4) 0.169(2) Uani 1 1 d . . . F69 F 0.2790(5) 0.48834(9) 0.5019(2) 0.103(2) Uani 1 1 d . . . F70 F 0.3499(3) 0.49749(10) 0.3140(2) 0.0773(15) Uani 1 1 d . . . F71 F 0.3992(3) 0.45260(10) 0.3376(3) 0.0726(14) Uani 1 1 d . . . F72 F 0.4276(4) 0.48476(13) 0.4302(4) 0.177(3) Uani 1 1 d . . . Al3 Al 0.23068(12) 0.41656(3) 0.97789(8) 0.0179(4) Uani 1 1 d . . . O9 O 0.1796(3) 0.44832(8) 0.9310(2) 0.0291(11) Uani 1 1 d . . . O10 O 0.3411(3) 0.42665(9) 1.0423(2) 0.0341(12) Uani 1 1 d . . . O11 O 0.1308(3) 0.40103(8) 1.0141(2) 0.0293(11) Uani 1 1 d . . . O12 O 0.2684(3) 0.39047(8) 0.9217(2) 0.0313(11) Uani 1 1 d . . . C33 C 0.1995(4) 0.47384(12) 0.8998(3) 0.0224(15) Uani 1 1 d . . . C34 C 0.2343(5) 0.49868(14) 0.9575(4) 0.0403(19) Uani 1 1 d . . . C35 C 0.0925(5) 0.48380(14) 0.8485(4) 0.041(2) Uani 1 1 d . . . C36 C 0.2838(5) 0.47012(15) 0.8544(4) 0.044(2) Uani 1 1 d . . . C37 C 0.4336(4) 0.41993(15) 1.0889(3) 0.0340(18) Uani 1 1 d . . . C38 C 0.4617(8) 0.4471(3) 1.1389(6) 0.184(4) Uani 1 1 d . . . C39 C 0.4240(7) 0.3928(2) 1.1315(6) 0.144(4) Uani 1 1 d . . . C40 C 0.5225(6) 0.4154(3) 1.0485(4) 0.127(5) Uani 1 1 d . . . C41 C 0.0498(4) 0.40516(13) 1.0493(3) 0.0264(16) Uani 1 1 d . . . C42 C -0.0497(7) 0.4036(5) 0.9959(5) 0.204(9) Uani 1 1 d . . . C43 C 0.0542(9) 0.3805(2) 1.1027(7) 0.208(4) Uani 1 1 d . . . C44 C 0.0565(7) 0.4331(2) 1.0904(6) 0.153(3) Uani 1 1 d . . . C45 C 0.2436(4) 0.36692(12) 0.8766(3) 0.0235(15) Uani 1 1 d . . . C46 C 0.2116(6) 0.33988(16) 0.9152(4) 0.051(2) Uani 1 1 d . . . C47 C 0.1539(6) 0.37554(16) 0.8111(4) 0.055(2) Uani 1 1 d . . . C48 C 0.3451(6) 0.35920(15) 0.8488(4) 0.050(2) Uani 1 1 d . . . F73 F 0.2257(3) 0.52606(7) 0.9303(2) 0.0556(12) Uani 1 1 d . . . F74 F 0.3368(3) 0.49462(8) 0.9900(2) 0.0570(12) Uani 1 1 d . . . F75 F 0.1776(3) 0.49760(9) 1.0078(2) 0.0608(13) Uani 1 1 d . . . F76 F 0.1067(3) 0.50573(9) 0.8037(2) 0.0610(13) Uani 1 1 d . . . F77 F 0.0239(3) 0.49347(9) 0.8860(2) 0.0620(13) Uani 1 1 d . . . F78 F 0.0474(3) 0.46111(9) 0.8089(2) 0.0629(13) Uani 1 1 d . . . F79 F 0.2452(3) 0.45565(10) 0.7934(2) 0.0708(14) Uani 1 1 d . . . F80 F 0.3238(3) 0.49568(9) 0.8374(2) 0.0575(12) Uani 1 1 d . . . F81 F 0.3660(3) 0.45380(9) 0.8901(2) 0.0571(12) Uani 1 1 d . . . F82 F 0.5442(4) 0.44212(12) 1.1937(2) 0.0987(19) Uani 1 1 d . . . F83 F 0.5238(5) 0.46393(16) 1.0726(5) 0.256(4) Uani 1 1 d . . . F84 F 0.4016(4) 0.46406(11) 1.1481(3) 0.1016(19) Uani 1 1 d . . . F85 F 0.5117(4) 0.38276(11) 1.1742(3) 0.0915(17) Uani 1 1 d . . . F86 F 0.3537(4) 0.37554(10) 1.1146(3) 0.100(2) Uani 1 1 d . . . F87 F 0.3707(5) 0.4147(2) 1.1949(3) 0.190(4) Uani 1 1 d . . . F88 F 0.4860(6) 0.37689(16) 1.0386(4) 0.257(3) Uani 1 1 d . . . F89 F 0.6180(3) 0.41378(12) 1.0888(3) 0.0860(18) Uani 1 1 d . . . F90 F 0.5134(4) 0.42222(16) 0.9888(3) 0.126(3) Uani 1 1 d . . . F91 F -0.0608(3) 0.41139(10) 0.9316(2) 0.0627(14) Uani 1 1 d . . . F92 F -0.0609(4) 0.36587(10) 0.9911(3) 0.0888(17) Uani 1 1 d . . . F93 F -0.1382(3) 0.41094(14) 1.0209(3) 0.098(2) Uani 1 1 d . . . F94 F 0.0945(3) 0.35680(8) 1.0945(2) 0.0565(12) Uani 1 1 d . . . F95 F -0.0291(4) 0.37849(10) 1.1317(3) 0.0824(15) Uani 1 1 d . . . F96 F 0.1470(4) 0.39847(15) 1.1683(2) 0.104(2) Uani 1 1 d . . . F97 F -0.0029(3) 0.43791(9) 1.1347(2) 0.0574(12) Uani 1 1 d . . . F98 F 0.1448(3) 0.44737(8) 1.10429(19) 0.0448(11) Uani 1 1 d . . . F99 F -0.0082(3) 0.45420(9) 1.0123(3) 0.0867(16) Uani 1 1 d . . . F100 F 0.2170(3) 0.31407(8) 0.8834(2) 0.0635(13) Uani 1 1 d . . . F101 F 0.1086(4) 0.34322(9) 0.9227(3) 0.0770(15) Uani 1 1 d . . . F102 F 0.2693(4) 0.33772(9) 0.9828(2) 0.0801(16) Uani 1 1 d . . . F103 F 0.1911(4) 0.39282(10) 0.7654(2) 0.0775(16) Uani 1 1 d . . . F104 F 0.1099(4) 0.35096(10) 0.7763(2) 0.0794(16) Uani 1 1 d . . . F105 F 0.0766(3) 0.38983(10) 0.8340(2) 0.0717(15) Uani 1 1 d . . . F106 F 0.3244(3) 0.34024(9) 0.7929(2) 0.0699(14) Uani 1 1 d . . . F107 F 0.3905(3) 0.38311(9) 0.8296(2) 0.0530(12) Uani 1 1 d . . . F108 F 0.4178(3) 0.34601(9) 0.9021(2) 0.0693(14) 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 Cu1 0.0260(4) 0.0424(5) 0.0269(4) -0.0013(4) -0.0017(3) -0.0027(3) Cu2 0.0225(4) 0.0436(4) 0.0212(4) 0.0017(4) -0.0008(3) -0.0005(3) Cu3 0.0228(4) 0.0531(5) 0.0234(4) -0.0044(4) -0.0039(3) 0.0035(4) C50 0.037(4) 0.137(7) 0.039(4) -0.016(5) 0.019(3) -0.051(4) C51 0.033(4) 0.108(6) 0.050(4) -0.047(4) 0.014(3) -0.005(4) C52 0.081(6) 0.048(5) 0.054(5) 0.012(4) -0.010(5) -0.017(4) C53 0.049(5) 0.080(6) 0.092(7) 0.034(5) 0.010(5) -0.025(4) C54 0.072(5) 0.059(5) 0.055(5) -0.016(4) 0.007(4) 0.022(4) C55 0.084(6) 0.038(4) 0.049(5) -0.004(4) -0.007(4) 0.001(4) C60 0.055(4) 0.057(5) 0.051(5) -0.023(4) 0.004(4) 0.023(4) C61 0.081(5) 0.029(4) 0.049(5) 0.007(4) -0.009(4) 0.004(4) C62 0.027(3) 0.113(6) 0.030(4) -0.006(4) 0.010(3) -0.019(4) C63 0.033(4) 0.089(6) 0.043(5) -0.013(4) -0.002(4) 0.008(4) C64 0.065(5) 0.048(4) 0.048(4) 0.016(4) 0.009(4) -0.021(4) C65 0.042(4) 0.090(6) 0.055(5) 0.023(4) 0.020(4) -0.017(4) C70 0.116(5) 0.064(5) 0.065(5) -0.014(4) -0.027(4) 0.013(4) C71 0.079(5) 0.124(6) 0.073(5) -0.030(4) 0.009(4) 0.036(4) C72 0.073(5) 0.112(5) 0.097(5) 0.042(4) 0.000(4) -0.041(4) C73 0.121(6) 0.073(5) 0.096(5) -0.008(4) -0.046(4) 0.005(5) C74 0.087(5) 0.165(5) 0.091(6) -0.028(5) 0.023(5) 0.034(5) C75 0.045(4) 0.156(5) 0.066(5) 0.040(5) 0.017(4) -0.022(4) Al1 0.0132(7) 0.0252(9) 0.0132(8) -0.0002(7) 0.0003(7) -0.0013(7) O1 0.0140(18) 0.045(2) 0.024(2) -0.0032(19) -0.0114(17) -0.0045(18) O2 0.0203(19) 0.048(3) 0.031(2) 0.007(2) 0.0086(18) 0.0120(18) O3 0.040(2) 0.027(2) 0.025(2) 0.0064(18) 0.0071(19) 0.0040(19) O4 0.053(3) 0.026(2) 0.025(2) -0.0037(19) 0.003(2) -0.004(2) C1 0.018(3) 0.038(3) 0.020(3) -0.003(3) -0.002(2) -0.005(3) C2 0.032(3) 0.044(4) 0.038(4) 0.002(3) 0.000(3) 0.013(3) C3 0.037(4) 0.055(4) 0.040(4) -0.004(4) 0.002(3) 0.002(3) C4 0.018(3) 0.053(4) 0.043(4) -0.012(3) 0.000(3) -0.004(3) C5 0.011(3) 0.044(4) 0.025(3) 0.000(3) 0.005(2) -0.001(3) C6 0.035(4) 0.057(4) 0.031(4) -0.011(3) -0.002(3) -0.006(3) C7 0.024(3) 0.062(4) 0.030(4) 0.008(3) 0.012(3) -0.010(3) C8 0.016(3) 0.063(4) 0.031(4) -0.010(3) 0.008(3) 0.002(3) C9 0.033(3) 0.027(3) 0.028(3) 0.008(3) 0.002(3) 0.003(3) C10 0.095(5) 0.082(5) 0.104(5) 0.040(4) 0.068(4) 0.014(4) C11 0.111(6) 0.046(5) 0.148(8) 0.052(5) -0.098(6) -0.038(5) C12 0.210(10) 0.025(4) 0.047(5) 0.000(4) 0.033(6) -0.012(6) C13 0.039(3) 0.025(3) 0.020(3) -0.007(3) 0.002(3) -0.003(3) C14 0.033(3) 0.043(4) 0.033(4) -0.007(3) 0.004(3) -0.001(3) C15 0.061(4) 0.034(4) 0.041(4) -0.008(3) 0.016(4) -0.012(3) C16 0.042(4) 0.047(4) 0.036(4) 0.002(3) -0.007(3) 0.005(3) F1 0.057(2) 0.083(3) 0.050(3) 0.014(2) -0.026(2) 0.018(2) F2 0.062(2) 0.057(3) 0.064(3) 0.019(2) 0.024(2) -0.004(2) F3 0.052(2) 0.043(2) 0.071(3) -0.010(2) 0.005(2) 0.0119(19) F4 0.044(2) 0.093(3) 0.050(2) -0.027(2) -0.018(2) -0.009(2) F5 0.070(3) 0.094(3) 0.039(2) -0.005(2) 0.017(2) 0.002(2) F6 0.056(2) 0.055(3) 0.067(3) -0.025(2) 0.005(2) 0.003(2) F7 0.0178(17) 0.098(3) 0.082(3) -0.009(3) 0.007(2) 0.010(2) F8 0.049(2) 0.059(3) 0.070(3) 0.003(2) 0.021(2) -0.014(2) F9 0.051(2) 0.088(3) 0.040(2) -0.018(2) 0.0210(19) -0.011(2) F10 0.062(2) 0.078(3) 0.044(2) -0.021(2) 0.021(2) -0.005(2) F11 0.047(2) 0.102(3) 0.029(2) -0.011(2) -0.0143(19) -0.006(2) F12 0.078(3) 0.052(2) 0.054(3) -0.014(2) 0.011(2) -0.020(2) F13 0.0188(17) 0.108(3) 0.064(3) -0.004(3) 0.0115(19) 0.002(2) F14 0.040(2) 0.088(3) 0.034(2) -0.022(2) -0.0078(18) 0.009(2) F15 0.051(2) 0.064(3) 0.054(3) 0.001(2) 0.006(2) 0.028(2) F16 0.053(2) 0.072(3) 0.052(2) 0.014(2) 0.031(2) -0.008(2) F17 0.056(2) 0.055(2) 0.053(2) -0.014(2) 0.016(2) -0.016(2) F18 0.041(2) 0.062(2) 0.050(2) 0.021(2) 0.0105(19) 0.0128(19) F19 0.149(4) 0.053(3) 0.102(3) 0.042(2) 0.080(3) 0.006(3) F20 0.061(2) 0.118(4) 0.125(4) 0.067(3) 0.061(3) 0.028(3) F21 0.304(8) 0.078(4) 0.029(3) 0.002(3) -0.001(4) 0.035(5) F22 0.081(3) 0.064(3) 0.063(3) 0.022(2) -0.024(2) 0.011(2) F23 0.057(3) 0.057(3) 0.169(5) 0.018(3) -0.049(3) -0.004(2) F24 0.210(4) 0.143(4) 0.250(5) 0.134(4) 0.193(4) 0.134(3) F25 0.103(3) 0.026(2) 0.066(3) 0.006(2) 0.011(3) -0.006(2) F26 0.248(7) 0.047(3) 0.040(3) -0.017(2) 0.025(4) -0.001(4) F27 0.146(4) 0.111(4) 0.291(7) 0.095(4) -0.161(5) -0.090(3) F28 0.070(3) 0.046(2) 0.054(2) 0.0128(19) 0.025(2) -0.001(2) F29 0.043(2) 0.061(3) 0.071(3) 0.011(2) -0.009(2) 0.010(2) F30 0.088(3) 0.026(2) 0.064(3) -0.007(2) 0.009(2) -0.004(2) F31 0.057(2) 0.112(4) 0.072(3) -0.030(3) 0.030(2) -0.044(2) F32 0.132(3) 0.064(3) 0.055(2) 0.011(2) 0.064(2) 0.000(3) F33 0.075(3) 0.063(3) 0.064(3) -0.028(2) 0.033(2) -0.003(2) F34 0.071(3) 0.056(3) 0.078(3) 0.014(2) -0.025(3) 0.010(2) F35 0.033(2) 0.093(3) 0.064(3) -0.001(2) 0.008(2) 0.002(2) F36 0.063(3) 0.079(3) 0.040(2) -0.022(2) -0.016(2) -0.009(2) Al2 0.0171(8) 0.0236(9) 0.0146(8) 0.0013(7) -0.0020(7) -0.0010(7) O5 0.0133(18) 0.044(2) 0.022(2) 0.0053(18) 0.0052(17) 0.0035(18) O6 0.037(2) 0.037(2) 0.024(2) -0.0039(19) 0.0079(19) 0.001(2) O7 0.020(2) 0.045(2) 0.021(2) -0.0036(19) -0.0036(18) 0.0047(19) O8 0.033(2) 0.025(2) 0.023(2) 0.0069(17) 0.0092(18) 0.0024(18) C17 0.010(3) 0.039(3) 0.024(3) -0.003(3) -0.004(3) -0.001(3) C18 0.035(3) 0.036(4) 0.040(4) -0.001(3) 0.017(3) 0.002(3) C19 0.016(3) 0.065(5) 0.036(4) -0.001(4) 0.002(3) 0.004(3) C20 0.043(4) 0.056(4) 0.022(3) -0.002(3) -0.001(3) -0.003(3) C21 0.035(3) 0.026(3) 0.025(3) -0.007(3) 0.012(3) -0.001(3) C22 0.052(4) 0.037(4) 0.046(4) -0.001(3) 0.007(4) -0.005(3) C23 0.058(4) 0.043(4) 0.039(4) -0.004(3) 0.020(4) 0.000(4) C24 0.043(4) 0.032(4) 0.041(4) -0.001(3) 0.011(3) -0.003(3) C25 0.014(3) 0.037(4) 0.031(3) 0.001(3) 0.000(3) 0.003(3) C26 0.029(3) 0.060(5) 0.038(4) -0.004(4) 0.000(3) -0.002(3) C27 0.024(3) 0.051(4) 0.049(4) 0.007(4) -0.015(3) 0.008(3) C28 0.038(4) 0.055(4) 0.041(4) -0.011(4) 0.003(3) 0.003(3) C29 0.027(3) 0.024(3) 0.023(3) 0.007(3) 0.003(3) -0.003(3) C30 0.278(13) 0.014(4) 0.052(5) 0.007(4) 0.053(7) 0.005(6) C31 0.070(5) 0.096(6) 0.195(9) 0.099(6) -0.095(6) -0.054(5) C32 0.167(6) 0.050(5) 0.214(7) 0.074(5) 0.174(5) 0.056(5) F37 0.0328(19) 0.056(2) 0.054(2) 0.0214(19) 0.0140(18) 0.0119(18) F38 0.053(2) 0.046(2) 0.064(3) -0.012(2) 0.009(2) -0.0213(19) F39 0.041(2) 0.070(3) 0.045(2) 0.011(2) 0.0189(19) -0.003(2) F40 0.039(2) 0.059(2) 0.053(2) 0.011(2) 0.0014(19) 0.0223(19) F41 0.037(2) 0.076(3) 0.031(2) -0.008(2) -0.0129(18) 0.0016(19) F42 0.0208(18) 0.093(3) 0.060(3) 0.007(2) 0.0089(19) 0.003(2) F43 0.072(3) 0.043(2) 0.044(2) -0.0089(19) 0.010(2) -0.013(2) F44 0.050(2) 0.085(3) 0.024(2) -0.008(2) -0.0101(19) 0.001(2) F45 0.057(2) 0.071(3) 0.040(2) -0.015(2) 0.0281(19) 0.005(2) F46 0.060(3) 0.048(2) 0.072(3) 0.011(2) -0.021(2) 0.010(2) F47 0.070(3) 0.079(3) 0.039(2) -0.026(2) -0.019(2) -0.006(2) F48 0.032(2) 0.094(3) 0.064(3) 0.008(2) 0.006(2) 0.002(2) F49 0.045(2) 0.102(3) 0.060(3) -0.012(2) 0.021(2) -0.024(2) F50 0.071(3) 0.074(3) 0.063(3) -0.031(2) 0.031(2) 0.001(2) F51 0.099(3) 0.055(3) 0.053(2) 0.011(2) 0.036(2) -0.006(2) F52 0.090(3) 0.027(2) 0.072(3) -0.014(2) 0.008(2) -0.006(2) F53 0.044(2) 0.049(2) 0.062(3) 0.012(2) 0.001(2) 0.0095(19) F54 0.058(2) 0.047(2) 0.056(2) 0.0174(19) 0.021(2) -0.0035(19) F55 0.049(2) 0.068(3) 0.087(3) 0.026(2) 0.008(2) -0.021(2) F56 0.035(2) 0.125(4) 0.039(2) -0.015(2) 0.0138(19) -0.006(2) F57 0.0146(18) 0.102(3) 0.063(3) 0.007(2) 0.0056(18) 0.004(2) F58 0.066(3) 0.051(2) 0.075(3) -0.015(2) -0.002(2) 0.016(2) F59 0.040(2) 0.070(3) 0.089(3) 0.038(2) 0.007(2) -0.007(2) F60 0.048(2) 0.069(3) 0.055(3) 0.022(2) -0.017(2) 0.018(2) F61 0.083(3) 0.051(3) 0.067(3) -0.022(2) -0.022(2) 0.016(2) F62 0.046(2) 0.087(3) 0.050(2) -0.023(2) -0.024(2) -0.001(2) F63 0.063(3) 0.115(4) 0.038(2) -0.010(2) 0.014(2) 0.020(3) F64 0.068(3) 0.057(3) 0.087(3) 0.035(2) -0.029(3) -0.002(2) F65 0.349(10) 0.102(4) 0.028(3) -0.008(3) 0.017(4) 0.057(5) F66 0.035(2) 0.077(3) 0.118(4) 0.017(3) -0.031(3) -0.009(2) F67 0.076(3) 0.030(2) 0.078(3) 0.004(2) 0.005(2) -0.003(2) F68 0.193(4) 0.098(4) 0.284(6) 0.101(4) 0.203(4) 0.091(3) F69 0.206(6) 0.047(3) 0.042(3) -0.013(2) -0.003(3) 0.029(3) F70 0.078(3) 0.076(3) 0.084(3) 0.050(2) 0.031(2) -0.003(2) F71 0.057(2) 0.072(3) 0.107(3) 0.025(3) 0.057(2) 0.016(2) F72 0.114(4) 0.118(4) 0.222(6) 0.089(4) -0.131(4) -0.074(3) Al3 0.0155(8) 0.0207(9) 0.0157(8) 0.0001(7) -0.0004(7) -0.0006(7) O9 0.030(2) 0.022(2) 0.034(2) 0.0089(18) 0.0027(19) -0.0007(18) O10 0.017(2) 0.056(3) 0.026(2) -0.007(2) -0.0047(18) -0.0028(19) O11 0.029(2) 0.029(2) 0.031(2) 0.0006(18) 0.0080(19) 0.0000(18) O12 0.035(2) 0.031(2) 0.030(2) -0.0063(19) 0.0118(19) -0.0030(19) C33 0.020(3) 0.022(3) 0.025(3) 0.002(3) 0.003(3) -0.002(2) C34 0.045(4) 0.033(4) 0.043(4) -0.002(3) 0.009(3) -0.006(3) C35 0.039(4) 0.036(4) 0.044(4) 0.015(3) -0.001(3) -0.008(3) C36 0.036(4) 0.056(4) 0.039(4) 0.016(4) 0.004(3) -0.005(3) C37 0.019(3) 0.057(4) 0.023(3) 0.002(3) -0.004(3) -0.003(3) C38 0.107(6) 0.226(9) 0.157(8) -0.154(7) -0.111(6) 0.118(6) C39 0.060(6) 0.159(8) 0.173(9) 0.121(7) -0.060(6) -0.049(6) C40 0.018(4) 0.322(14) 0.043(5) 0.077(7) 0.012(4) 0.044(6) C41 0.026(3) 0.031(3) 0.025(3) 0.008(3) 0.012(3) -0.006(3) C42 0.033(5) 0.54(3) 0.036(6) 0.021(10) 0.002(5) 0.055(10) C43 0.269(7) 0.077(5) 0.385(10) 0.144(6) 0.306(7) 0.109(6) C44 0.120(5) 0.164(7) 0.226(8) -0.157(6) 0.153(5) -0.101(5) C45 0.029(3) 0.020(3) 0.021(3) -0.004(3) 0.004(3) 0.001(3) C46 0.065(5) 0.047(4) 0.045(4) 0.001(4) 0.021(4) -0.012(4) C47 0.055(5) 0.058(5) 0.044(4) -0.015(4) -0.008(4) -0.003(4) C48 0.073(5) 0.036(4) 0.043(4) -0.009(3) 0.016(4) 0.001(4) F73 0.070(3) 0.0222(19) 0.068(3) 0.0023(19) 0.002(2) -0.0035(19) F74 0.054(2) 0.055(2) 0.048(2) -0.006(2) -0.020(2) -0.017(2) F75 0.088(3) 0.056(2) 0.043(2) -0.022(2) 0.026(2) -0.013(2) F76 0.053(2) 0.062(3) 0.059(3) 0.036(2) -0.007(2) -0.002(2) F77 0.039(2) 0.062(3) 0.085(3) 0.021(2) 0.015(2) 0.012(2) F78 0.054(2) 0.059(3) 0.058(3) 0.009(2) -0.027(2) -0.016(2) F79 0.081(3) 0.097(3) 0.038(2) -0.019(2) 0.019(2) -0.010(3) F80 0.051(2) 0.067(3) 0.059(2) 0.031(2) 0.021(2) -0.008(2) F81 0.038(2) 0.068(3) 0.070(3) 0.023(2) 0.022(2) 0.010(2) F82 0.084(3) 0.120(4) 0.065(3) -0.030(3) -0.044(3) 0.002(3) F83 0.093(4) 0.253(6) 0.354(8) 0.240(5) -0.103(5) -0.104(4) F84 0.113(4) 0.091(3) 0.075(3) -0.045(3) -0.037(3) 0.026(3) F85 0.061(3) 0.112(4) 0.083(3) 0.053(3) -0.024(3) 0.012(3) F86 0.085(3) 0.064(3) 0.128(4) 0.042(3) -0.030(3) -0.019(3) F87 0.089(4) 0.453(13) 0.037(3) 0.040(5) 0.029(3) 0.031(6) F88 0.215(5) 0.238(5) 0.226(6) -0.185(4) -0.154(5) 0.182(4) F89 0.023(2) 0.150(5) 0.081(3) 0.020(3) 0.002(2) 0.012(3) F90 0.054(3) 0.267(7) 0.065(3) 0.038(4) 0.031(3) 0.051(4) F91 0.049(2) 0.098(3) 0.031(2) 0.003(2) -0.012(2) 0.012(2) F92 0.082(3) 0.074(3) 0.116(4) -0.050(3) 0.034(3) -0.045(3) F93 0.025(2) 0.197(6) 0.070(3) -0.004(3) 0.005(2) 0.012(3) F94 0.063(2) 0.045(2) 0.071(3) 0.022(2) 0.035(2) 0.006(2) F95 0.100(3) 0.065(3) 0.110(3) 0.023(2) 0.083(3) 0.001(2) F96 0.054(3) 0.211(6) 0.035(3) 0.019(3) -0.017(2) -0.013(3) F97 0.064(2) 0.062(3) 0.062(2) -0.017(2) 0.048(2) -0.006(2) F98 0.046(2) 0.044(2) 0.046(2) -0.0111(18) 0.0149(18) -0.0147(18) F99 0.080(3) 0.061(3) 0.137(4) 0.048(3) 0.064(3) 0.036(2) F100 0.088(3) 0.025(2) 0.079(3) -0.016(2) 0.023(2) -0.012(2) F101 0.087(3) 0.057(3) 0.102(3) -0.015(2) 0.056(3) -0.033(2) F102 0.130(4) 0.063(3) 0.041(2) 0.023(2) 0.005(3) -0.028(3) F103 0.106(4) 0.082(3) 0.035(2) 0.024(2) -0.006(2) -0.010(3) F104 0.083(3) 0.076(3) 0.060(3) -0.020(2) -0.025(3) -0.011(3) F105 0.034(2) 0.085(3) 0.085(3) -0.014(3) -0.010(2) 0.015(2) F106 0.084(3) 0.072(3) 0.062(3) -0.041(2) 0.033(2) -0.004(2) F107 0.056(2) 0.056(2) 0.054(2) -0.001(2) 0.029(2) -0.005(2) F108 0.052(2) 0.072(3) 0.078(3) -0.002(2) 0.001(2) 0.027(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 C51 2.145(7) . ? Cu1 C50 2.168(7) . ? Cu1 C54 2.178(8) . ? Cu1 C55 2.179(7) . ? Cu1 C52 2.179(8) . ? Cu1 C53 2.181(9) . ? Cu2 C60 2.160(7) . ? Cu2 C62 2.167(7) . ? Cu2 C65 2.171(8) . ? Cu2 C61 2.176(7) . ? Cu2 C64 2.177(7) . ? Cu2 C63 2.178(8) . ? Cu3 C74 2.118(10) . ? Cu3 C71 2.127(9) . ? Cu3 C75 2.127(8) . ? Cu3 C73 2.138(9) . ? Cu3 C72 2.149(9) . ? Cu3 C70 2.152(8) . ? C50 C51 1.324(12) . ? C50 H50A 0.95(5) . ? C50 H50B 0.98(6) . ? C51 H51A 0.9900 . ? C51 H51B 0.9900 . ? C52 C53 1.313(12) . ? C52 H52A 1.02(8) . ? C52 H52B 0.96(7) . ? C53 H53B 0.79(7) . ? C53 H53A 0.93(8) . ? C54 C55 1.321(12) . ? C54 H54A 1.09(6) . ? C54 H54B 1.06(7) . ? C55 H55A 1.19(5) . ? C55 H55B 0.99(6) . ? C60 C61 1.297(11) . ? C60 H60A 0.96(8) . ? C60 H60B 0.97(5) . ? C61 H61A 1.04(8) . ? C61 H61B 1.06(7) . ? C62 C63 1.321(11) . ? C62 H62A 0.94(5) . ? C62 H62B 0.88(6) . ? C63 H63A 0.78(5) . ? C63 H63B 0.83(6) . ? C64 C65 1.311(11) . ? C64 H64B 1.08(6) . ? C64 H64A 0.95(7) . ? C65 H65A 0.84(7) . ? C65 H65B 1.08(6) . ? C70 C71 1.330(13) . ? C70 H70A 0.9900 . ? C70 H70B 0.9900 . ? C71 H71A 0.9900 . ? C71 H71B 0.9900 . ? C72 C73 1.313(14) . ? C72 H72A 0.9900 . ? C72 H72B 0.9900 . ? C73 H73A 0.9900 . ? C73 H73B 0.9900 . ? C74 C75 1.324(14) . ? C74 H74A 0.9900 . ? C74 H74B 0.9900 . ? C75 H75A 0.9900 . ? C75 H75B 0.9900 . ? Al1 O2 1.720(4) . ? Al1 O4 1.720(4) . ? Al1 O1 1.722(3) . ? Al1 O3 1.725(4) . ? O1 C1 1.345(6) . ? O2 C5 1.347(7) . ? O3 C9 1.346(7) . ? O4 C13 1.351(7) . ? C1 C4 1.543(9) . ? C1 C3 1.550(9) . ? C1 C2 1.552(8) . ? C2 F3 1.318(7) . ? C2 F2 1.324(8) . ? C2 F1 1.369(7) . ? C3 F6 1.311(8) . ? C3 F5 1.326(8) . ? C3 F4 1.356(7) . ? C4 F8 1.313(7) . ? C4 F7 1.337(7) . ? C4 F9 1.337(7) . ? C5 C7 1.540(9) . ? C5 C6 1.556(8) . ? C5 C8 1.565(7) . ? C6 F12 1.322(8) . ? C6 F11 1.326(7) . ? C6 F10 1.344(8) . ? C7 F18 1.321(7) . ? C7 F17 1.321(7) . ? C7 F16 1.341(7) . ? C8 F15 1.310(7) . ? C8 F13 1.338(7) . ? C8 F14 1.346(7) . ? C9 C12 1.514(9) . ? C9 C10 1.539(11) . ? C9 C11 1.567(10) . ? C10 F20 1.239(9) . ? C10 F19 1.340(9) . ? C10 F21 1.507(11) . ? C11 F23 1.204(9) . ? C11 F22 1.325(9) . ? C11 F24 1.532(13) . ? C12 F26 1.227(10) . ? C12 F25 1.317(8) . ? C12 F27 1.582(13) . ? C13 C14 1.534(8) . ? C13 C15 1.542(9) . ? C13 C16 1.560(8) . ? C14 F30 1.320(7) . ? C14 F29 1.328(7) . ? C14 F28 1.333(8) . ? C15 F31 1.317(7) . ? C15 F33 1.326(7) . ? C15 F32 1.332(7) . ? C16 F36 1.310(7) . ? C16 F35 1.321(8) . ? C16 F34 1.327(7) . ? Al2 O6 1.719(4) . ? Al2 O8 1.721(4) . ? Al2 O5 1.729(4) . ? Al2 O7 1.731(4) . ? O5 C17 1.345(7) . ? O6 C21 1.355(7) . ? O7 C25 1.359(6) . ? O8 C29 1.349(6) . ? C17 C18 1.536(8) . ? C17 C19 1.554(7) . ? C17 C20 1.559(8) . ? C18 F37 1.330(7) . ? C18 F39 1.339(7) . ? C18 F38 1.349(7) . ? C19 F40 1.333(8) . ? C19 F42 1.340(7) . ? C19 F41 1.350(7) . ? C20 F43 1.318(7) . ? C20 F45 1.328(8) . ? C20 F44 1.344(7) . ? C21 C23 1.532(9) . ? C21 C24 1.536(8) . ? C21 C22 1.563(8) . ? C22 F46 1.319(7) . ? C22 F47 1.325(8) . ? C22 F48 1.339(8) . ? C23 F51 1.328(7) . ? C23 F49 1.336(7) . ? C23 F50 1.344(8) . ? C24 F54 1.320(8) . ? C24 F53 1.323(7) . ? C24 F52 1.344(7) . ? C25 C26 1.528(9) . ? C25 C28 1.533(9) . ? C25 C27 1.548(9) . ? C26 F55 1.317(8) . ? C26 F56 1.342(7) . ? C26 F57 1.345(7) . ? C27 F59 1.301(8) . ? C27 F58 1.342(8) . ? C27 F60 1.359(7) . ? C28 F61 1.319(8) . ? C28 F63 1.342(8) . ? C28 F62 1.342(7) . ? C29 C30 1.508(10) . ? C29 C31 1.529(10) . ? C29 C32 1.545(10) . ? C30 F69 1.210(9) . ? C30 F67 1.303(8) . ? C30 F68 1.687(14) . ? C31 F66 1.202(9) . ? C31 F64 1.338(9) . ? C31 F65 1.610(14) . ? C32 F71 1.216(9) . ? C32 F70 1.328(9) . ? C32 F72 1.573(12) . ? Al3 O10 1.719(4) . ? Al3 O12 1.721(4) . ? Al3 O11 1.727(4) . ? Al3 O9 1.731(4) . ? O9 C33 1.339(6) . ? O10 C37 1.353(6) . ? O11 C41 1.364(7) . ? O12 C45 1.354(6) . ? C33 C36 1.531(9) . ? C33 C34 1.558(8) . ? C33 C35 1.567(8) . ? C34 F75 1.322(8) . ? C34 F73 1.327(7) . ? C34 F74 1.340(7) . ? C35 F77 1.320(8) . ? C35 F78 1.321(7) . ? C35 F76 1.337(7) . ? C36 F80 1.324(8) . ? C36 F79 1.325(7) . ? C36 F81 1.341(7) . ? C37 C39 1.479(12) . ? C37 C40 1.521(10) . ? C37 C38 1.536(12) . ? C38 F84 1.126(11) . ? C38 F82 1.332(10) . ? C38 F83 1.795(15) . ? C39 F86 1.180(10) . ? C39 F85 1.317(9) . ? C39 F87 1.798(15) . ? C40 F90 1.154(9) . ? C40 F89 1.298(8) . ? C40 F88 1.788(14) . ? C41 C42 1.450(10) . ? C41 C44 1.469(11) . ? C41 C43 1.491(11) . ? C42 F91 1.246(11) . ? C42 F93 1.364(11) . ? C42 F92 1.70(2) . ? C43 F94 1.209(10) . ? C43 F95 1.308(11) . ? C43 F96 1.725(13) . ? C44 F97 1.269(10) . ? C44 F98 1.279(9) . ? C44 F99 1.801(12) . ? C45 C46 1.518(9) . ? C45 C48 1.548(10) . ? C45 C47 1.549(8) . ? C46 F100 1.314(8) . ? C46 F102 1.337(8) . ? C46 F101 1.370(8) . ? C47 F103 1.326(9) . ? C47 F105 1.332(9) . ? C47 F104 1.344(8) . ? C48 F107 1.310(8) . ? C48 F106 1.340(8) . ? C48 F108 1.353(8) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C51 Cu1 C50 35.8(3) . . ? C51 Cu1 C54 155.2(3) . . ? C50 Cu1 C54 119.6(3) . . ? C51 Cu1 C55 120.5(3) . . ? C50 Cu1 C55 84.8(3) . . ? C54 Cu1 C55 35.3(3) . . ? C51 Cu1 C52 85.3(3) . . ? C50 Cu1 C52 121.1(4) . . ? C54 Cu1 C52 119.3(3) . . ? C55 Cu1 C52 153.9(3) . . ? C51 Cu1 C53 120.3(3) . . ? C50 Cu1 C53 156.0(4) . . ? C54 Cu1 C53 84.2(4) . . ? C55 Cu1 C53 119.1(4) . . ? C52 Cu1 C53 35.0(3) . . ? C60 Cu2 C62 119.4(3) . . ? C60 Cu2 C65 85.6(3) . . ? C62 Cu2 C65 154.9(3) . . ? C60 Cu2 C61 34.8(3) . . ? C62 Cu2 C61 84.7(3) . . ? C65 Cu2 C61 120.4(3) . . ? C60 Cu2 C64 120.7(3) . . ? C62 Cu2 C64 119.9(3) . . ? C65 Cu2 C64 35.1(3) . . ? C61 Cu2 C64 155.4(3) . . ? C60 Cu2 C63 154.8(3) . . ? C62 Cu2 C63 35.4(3) . . ? C65 Cu2 C63 119.5(3) . . ? C61 Cu2 C63 120.1(3) . . ? C64 Cu2 C63 84.5(3) . . ? C74 Cu3 C71 157.8(4) . . ? C74 Cu3 C75 36.4(4) . . ? C71 Cu3 C75 121.9(4) . . ? C74 Cu3 C73 82.8(4) . . ? C71 Cu3 C73 119.1(4) . . ? C75 Cu3 C73 119.0(4) . . ? C74 Cu3 C72 118.2(4) . . ? C71 Cu3 C72 83.4(4) . . ? C75 Cu3 C72 154.6(4) . . ? C73 Cu3 C72 35.7(4) . . ? C74 Cu3 C70 122.4(4) . . ? C71 Cu3 C70 36.2(4) . . ? C75 Cu3 C70 86.0(4) . . ? C73 Cu3 C70 154.7(4) . . ? C72 Cu3 C70 119.4(4) . . ? C51 C50 Cu1 71.2(5) . . ? C51 C50 H50A 113(3) . . ? Cu1 C50 H50A 106(4) . . ? C51 C50 H50B 117(4) . . ? Cu1 C50 H50B 103(4) . . ? H50A C50 H50B 128(5) . . ? C50 C51 Cu1 73.1(5) . . ? C50 C51 H51A 116.2 . . ? Cu1 C51 H51A 116.2 . . ? C50 C51 H51B 116.2 . . ? Cu1 C51 H51B 116.2 . . ? H51A C51 H51B 113.2 . . ? C53 C52 Cu1 72.5(5) . . ? C53 C52 H52A 130(5) . . ? Cu1 C52 H52A 101(4) . . ? C53 C52 H52B 128(4) . . ? Cu1 C52 H52B 101(4) . . ? H52A C52 H52B 102(6) . . ? C52 C53 Cu1 72.4(5) . . ? C52 C53 H53B 118(6) . . ? Cu1 C53 H53B 107(6) . . ? C52 C53 H53A 111(6) . . ? Cu1 C53 H53A 100(5) . . ? H53B C53 H53A 129(8) . . ? C55 C54 Cu1 72.4(5) . . ? C55 C54 H54A 116(3) . . ? Cu1 C54 H54A 98(3) . . ? C55 C54 H54B 128(4) . . ? Cu1 C54 H54B 104(4) . . ? H54A C54 H54B 116(6) . . ? C54 C55 Cu1 72.3(5) . . ? C54 C55 H55A 124(3) . . ? Cu1 C55 H55A 110(3) . . ? C54 C55 H55B 121(4) . . ? Cu1 C55 H55B 106(4) . . ? H55A C55 H55B 112(5) . . ? C61 C60 Cu2 73.3(5) . . ? C61 C60 H60A 131(5) . . ? Cu2 C60 H60A 103(5) . . ? C61 C60 H60B 134(3) . . ? Cu2 C60 H60B 106(3) . . ? H60A C60 H60B 94(6) . . ? C60 C61 Cu2 71.9(4) . . ? C60 C61 H61A 125(4) . . ? Cu2 C61 H61A 102(4) . . ? C60 C61 H61B 124(4) . . ? Cu2 C61 H61B 110(4) . . ? H61A C61 H61B 110(6) . . ? C63 C62 Cu2 72.7(5) . . ? C63 C62 H62A 112(3) . . ? Cu2 C62 H62A 108(4) . . ? C63 C62 H62B 113(4) . . ? Cu2 C62 H62B 105(4) . . ? H62A C62 H62B 130(5) . . ? C62 C63 Cu2 71.8(5) . . ? C62 C63 H63A 117(4) . . ? Cu2 C63 H63A 104(4) . . ? C62 C63 H63B 112(4) . . ? Cu2 C63 H63B 102(5) . . ? H63A C63 H63B 129(6) . . ? C65 C64 Cu2 72.2(5) . . ? C65 C64 H64B 124(4) . . ? Cu2 C64 H64B 102(4) . . ? C65 C64 H64A 130(5) . . ? Cu2 C64 H64A 100(5) . . ? H64B C64 H64A 106(6) . . ? C64 C65 Cu2 72.7(5) . . ? C64 C65 H65A 123(5) . . ? Cu2 C65 H65A 99(5) . . ? C64 C65 H65B 117(4) . . ? Cu2 C65 H65B 103(4) . . ? H65A C65 H65B 120(6) . . ? C71 C70 Cu3 70.9(5) . . ? C71 C70 H70A 116.5 . . ? Cu3 C70 H70A 116.5 . . ? C71 C70 H70B 116.5 . . ? Cu3 C70 H70B 116.5 . . ? H70A C70 H70B 113.5 . . ? C70 C71 Cu3 72.9(6) . . ? C70 C71 H71A 116.3 . . ? Cu3 C71 H71A 116.3 . . ? C70 C71 H71B 116.3 . . ? Cu3 C71 H71B 116.3 . . ? H71A C71 H71B 113.3 . . ? C73 C72 Cu3 71.7(6) . . ? C73 C72 H72A 116.4 . . ? Cu3 C72 H72A 116.4 . . ? C73 C72 H72B 116.4 . . ? Cu3 C72 H72B 116.4 . . ? H72A C72 H72B 113.4 . . ? C72 C73 Cu3 72.6(6) . . ? C72 C73 H73A 116.3 . . ? Cu3 C73 H73A 116.3 . . ? C72 C73 H73B 116.3 . . ? Cu3 C73 H73B 116.3 . . ? H73A C73 H73B 113.3 . . ? C75 C74 Cu3 72.2(6) . . ? C75 C74 H74A 116.4 . . ? Cu3 C74 H74A 116.4 . . ? C75 C74 H74B 116.4 . . ? Cu3 C74 H74B 116.4 . . ? H74A C74 H74B 113.3 . . ? C74 C75 Cu3 71.4(6) . . ? C74 C75 H75A 116.5 . . ? Cu3 C75 H75A 116.5 . . ? C74 C75 H75B 116.5 . . ? Cu3 C75 H75B 116.5 . . ? H75A C75 H75B 113.4 . . ? O2 Al1 O4 111.9(2) . . ? O2 Al1 O1 107.9(2) . . ? O4 Al1 O1 108.02(19) . . ? O2 Al1 O3 108.1(2) . . ? O4 Al1 O3 109.1(2) . . ? O1 Al1 O3 111.8(2) . . ? C1 O1 Al1 149.1(4) . . ? C5 O2 Al1 148.2(3) . . ? C9 O3 Al1 149.8(4) . . ? C13 O4 Al1 150.3(4) . . ? O1 C1 C4 111.7(4) . . ? O1 C1 C3 107.2(5) . . ? C4 C1 C3 108.9(5) . . ? O1 C1 C2 110.2(5) . . ? C4 C1 C2 108.9(5) . . ? C3 C1 C2 109.9(5) . . ? F3 C2 F2 108.1(5) . . ? F3 C2 F1 107.8(5) . . ? F2 C2 F1 105.5(5) . . ? F3 C2 C1 112.3(5) . . ? F2 C2 C1 111.6(5) . . ? F1 C2 C1 111.2(5) . . ? F6 C3 F5 108.1(6) . . ? F6 C3 F4 107.0(5) . . ? F5 C3 F4 106.4(5) . . ? F6 C3 C1 112.2(5) . . ? F5 C3 C1 111.3(5) . . ? F4 C3 C1 111.5(5) . . ? F8 C4 F7 107.2(5) . . ? F8 C4 F9 106.4(5) . . ? F7 C4 F9 106.6(5) . . ? F8 C4 C1 112.4(5) . . ? F7 C4 C1 114.1(5) . . ? F9 C4 C1 109.7(5) . . ? O2 C5 C7 112.2(5) . . ? O2 C5 C6 110.5(5) . . ? C7 C5 C6 110.0(5) . . ? O2 C5 C8 106.7(4) . . ? C7 C5 C8 109.7(5) . . ? C6 C5 C8 107.5(5) . . ? F12 C6 F11 107.3(5) . . ? F12 C6 F10 106.6(5) . . ? F11 C6 F10 107.8(5) . . ? F12 C6 C5 111.5(5) . . ? F11 C6 C5 110.1(5) . . ? F10 C6 C5 113.3(5) . . ? F18 C7 F17 108.3(5) . . ? F18 C7 F16 107.5(5) . . ? F17 C7 F16 107.6(5) . . ? F18 C7 C5 109.9(5) . . ? F17 C7 C5 111.2(5) . . ? F16 C7 C5 112.0(5) . . ? F15 C8 F13 107.9(5) . . ? F15 C8 F14 107.9(5) . . ? F13 C8 F14 105.9(5) . . ? F15 C8 C5 112.8(5) . . ? F13 C8 C5 112.3(5) . . ? F14 C8 C5 109.8(5) . . ? O3 C9 C12 111.7(5) . . ? O3 C9 C10 108.2(5) . . ? C12 C9 C10 113.2(7) . . ? O3 C9 C11 110.0(5) . . ? C12 C9 C11 106.5(7) . . ? C10 C9 C11 107.1(6) . . ? F20 C10 F19 110.3(7) . . ? F20 C10 F21 109.8(8) . . ? F19 C10 F21 109.4(7) . . ? F20 C10 C9 114.8(7) . . ? F19 C10 C9 112.3(7) . . ? F21 C10 C9 99.6(6) . . ? F23 C11 F22 113.6(7) . . ? F23 C11 F24 107.8(9) . . ? F22 C11 F24 106.1(7) . . ? F23 C11 C9 115.7(7) . . ? F22 C11 C9 112.1(7) . . ? F24 C11 C9 100.1(6) . . ? F26 C12 F25 113.3(7) . . ? F26 C12 C9 117.0(7) . . ? F25 C12 C9 116.2(6) . . ? F26 C12 F27 106.1(8) . . ? F25 C12 F27 104.5(7) . . ? C9 C12 F27 96.7(7) . . ? O4 C13 C14 107.6(5) . . ? O4 C13 C15 109.9(5) . . ? C14 C13 C15 109.1(5) . . ? O4 C13 C16 112.7(5) . . ? C14 C13 C16 108.6(5) . . ? C15 C13 C16 109.0(5) . . ? F30 C14 F29 107.1(5) . . ? F30 C14 F28 106.8(5) . . ? F29 C14 F28 105.5(5) . . ? F30 C14 C13 114.0(5) . . ? F29 C14 C13 112.0(5) . . ? F28 C14 C13 110.9(5) . . ? F31 C15 F33 106.8(6) . . ? F31 C15 F32 107.8(6) . . ? F33 C15 F32 106.3(5) . . ? F31 C15 C13 112.1(5) . . ? F33 C15 C13 113.6(5) . . ? F32 C15 C13 109.9(6) . . ? F36 C16 F35 108.0(5) . . ? F36 C16 F34 109.9(5) . . ? F35 C16 F34 105.4(6) . . ? F36 C16 C13 113.5(6) . . ? F35 C16 C13 111.0(5) . . ? F34 C16 C13 108.7(5) . . ? O6 Al2 O8 109.3(2) . . ? O6 Al2 O5 111.3(2) . . ? O8 Al2 O5 107.62(19) . . ? O6 Al2 O7 108.55(19) . . ? O8 Al2 O7 112.2(2) . . ? O5 Al2 O7 107.97(19) . . ? C17 O5 Al2 147.4(3) . . ? C21 O6 Al2 150.1(4) . . ? C25 O7 Al2 149.6(4) . . ? C29 O8 Al2 150.0(4) . . ? O5 C17 C18 112.2(5) . . ? O5 C17 C19 106.9(5) . . ? C18 C17 C19 109.4(5) . . ? O5 C17 C20 110.8(5) . . ? C18 C17 C20 109.3(5) . . ? C19 C17 C20 108.1(5) . . ? F37 C18 F39 107.9(5) . . ? F37 C18 F38 106.3(5) . . ? F39 C18 F38 107.3(5) . . ? F37 C18 C17 111.5(5) . . ? F39 C18 C17 113.4(5) . . ? F38 C18 C17 110.0(5) . . ? F40 C19 F42 108.2(5) . . ? F40 C19 F41 106.9(5) . . ? F42 C19 F41 106.8(5) . . ? F40 C19 C17 111.2(5) . . ? F42 C19 C17 113.0(5) . . ? F41 C19 C17 110.4(5) . . ? F43 C20 F45 108.2(5) . . ? F43 C20 F44 107.5(5) . . ? F45 C20 F44 107.2(5) . . ? F43 C20 C17 111.4(5) . . ? F45 C20 C17 113.1(5) . . ? F44 C20 C17 109.2(5) . . ? O6 C21 C23 109.8(5) . . ? O6 C21 C24 106.9(5) . . ? C23 C21 C24 110.0(5) . . ? O6 C21 C22 111.5(5) . . ? C23 C21 C22 108.3(5) . . ? C24 C21 C22 110.3(5) . . ? F46 C22 F47 109.5(6) . . ? F46 C22 F48 107.7(6) . . ? F47 C22 F48 106.9(5) . . ? F46 C22 C21 110.5(5) . . ? F47 C22 C21 112.1(6) . . ? F48 C22 C21 110.0(5) . . ? F51 C23 F49 106.7(6) . . ? F51 C23 F50 106.9(5) . . ? F49 C23 F50 105.5(5) . . ? F51 C23 C21 112.2(6) . . ? F49 C23 C21 111.2(5) . . ? F50 C23 C21 113.8(5) . . ? F54 C24 F53 107.2(5) . . ? F54 C24 F52 106.6(5) . . ? F53 C24 F52 106.9(5) . . ? F54 C24 C21 111.5(5) . . ? F53 C24 C21 111.9(5) . . ? F52 C24 C21 112.5(5) . . ? O7 C25 C26 110.9(5) . . ? O7 C25 C28 107.8(5) . . ? C26 C25 C28 108.7(5) . . ? O7 C25 C27 109.8(5) . . ? C26 C25 C27 110.5(5) . . ? C28 C25 C27 109.0(5) . . ? F55 C26 F56 107.2(6) . . ? F55 C26 F57 107.0(5) . . ? F56 C26 F57 106.4(5) . . ? F55 C26 C25 112.0(6) . . ? F56 C26 C25 110.9(5) . . ? F57 C26 C25 113.0(5) . . ? F59 C27 F58 107.2(5) . . ? F59 C27 F60 107.7(6) . . ? F58 C27 F60 105.8(5) . . ? F59 C27 C25 113.1(5) . . ? F58 C27 C25 111.0(6) . . ? F60 C27 C25 111.6(5) . . ? F61 C28 F63 106.6(6) . . ? F61 C28 F62 107.3(5) . . ? F63 C28 F62 106.1(5) . . ? F61 C28 C25 112.2(5) . . ? F63 C28 C25 111.1(5) . . ? F62 C28 C25 113.1(5) . . ? O8 C29 C30 112.2(5) . . ? O8 C29 C31 109.6(5) . . ? C30 C29 C31 111.8(7) . . ? O8 C29 C32 107.3(5) . . ? C30 C29 C32 106.5(7) . . ? C31 C29 C32 109.3(7) . . ? F69 C30 F67 116.2(7) . . ? F69 C30 C29 119.6(7) . . ? F67 C30 C29 116.5(7) . . ? F69 C30 F68 103.4(8) . . ? F67 C30 F68 100.5(7) . . ? C29 C30 F68 94.0(6) . . ? F66 C31 F64 113.8(7) . . ? F66 C31 C29 118.2(8) . . ? F64 C31 C29 113.3(6) . . ? F66 C31 F65 105.9(8) . . ? F64 C31 F65 106.0(8) . . ? C29 C31 F65 97.1(6) . . ? F71 C32 F70 113.6(8) . . ? F71 C32 C29 118.3(7) . . ? F70 C32 C29 113.9(6) . . ? F71 C32 F72 106.1(7) . . ? F70 C32 F72 103.6(6) . . ? C29 C32 F72 98.5(7) . . ? O10 Al3 O12 108.6(2) . . ? O10 Al3 O11 113.2(2) . . ? O12 Al3 O11 107.7(2) . . ? O10 Al3 O9 108.1(2) . . ? O12 Al3 O9 111.6(2) . . ? O11 Al3 O9 107.71(19) . . ? C33 O9 Al3 147.5(4) . . ? C37 O10 Al3 151.4(4) . . ? C41 O11 Al3 148.2(4) . . ? C45 O12 Al3 149.6(4) . . ? O9 C33 C36 112.4(5) . . ? O9 C33 C34 110.8(5) . . ? C36 C33 C34 110.0(5) . . ? O9 C33 C35 107.0(4) . . ? C36 C33 C35 108.3(5) . . ? C34 C33 C35 108.2(5) . . ? F75 C34 F73 107.5(5) . . ? F75 C34 F74 107.6(5) . . ? F73 C34 F74 107.2(5) . . ? F75 C34 C33 111.2(5) . . ? F73 C34 C33 113.8(5) . . ? F74 C34 C33 109.3(5) . . ? F77 C35 F78 107.2(5) . . ? F77 C35 F76 107.3(5) . . ? F78 C35 F76 108.1(5) . . ? F77 C35 C33 111.0(5) . . ? F78 C35 C33 110.5(5) . . ? F76 C35 C33 112.5(5) . . ? F80 C36 F79 107.7(5) . . ? F80 C36 F81 106.9(5) . . ? F79 C36 F81 106.1(6) . . ? F80 C36 C33 113.7(6) . . ? F79 C36 C33 111.6(5) . . ? F81 C36 C33 110.5(5) . . ? O10 C37 C39 112.0(6) . . ? O10 C37 C40 110.5(5) . . ? C39 C37 C40 109.0(8) . . ? O10 C37 C38 106.4(6) . . ? C39 C37 C38 110.6(8) . . ? C40 C37 C38 108.4(8) . . ? F84 C38 F82 116.7(9) . . ? F84 C38 C37 123.7(8) . . ? F82 C38 C37 112.9(8) . . ? F84 C38 F83 104.3(10) . . ? F82 C38 F83 102.5(8) . . ? C37 C38 F83 89.0(7) . . ? F86 C39 F85 116.3(9) . . ? F86 C39 C37 122.8(8) . . ? F85 C39 C37 117.1(7) . . ? F86 C39 F87 99.3(8) . . ? F85 C39 F87 100.1(8) . . ? C37 C39 F87 90.2(7) . . ? F90 C40 F89 118.3(7) . . ? F90 C40 C37 122.0(7) . . ? F89 C40 C37 115.4(7) . . ? F90 C40 F88 100.7(9) . . ? F89 C40 F88 101.7(8) . . ? C37 C40 F88 88.5(6) . . ? O11 C41 C42 107.6(6) . . ? O11 C41 C44 114.3(5) . . ? C42 C41 C44 110.7(9) . . ? O11 C41 C43 108.1(6) . . ? C42 C41 C43 109.6(9) . . ? C44 C41 C43 106.4(8) . . ? F91 C42 F93 110.2(9) . . ? F91 C42 C41 124.5(10) . . ? F93 C42 C41 114.9(8) . . ? F91 C42 F92 103.7(10) . . ? F93 C42 F92 101.1(10) . . ? C41 C42 F92 97.9(9) . . ? F94 C43 F95 113.8(8) . . ? F94 C43 C41 121.3(9) . . ? F95 C43 C41 115.1(7) . . ? F94 C43 F96 104.8(8) . . ? F95 C43 F96 103.3(8) . . ? C41 C43 F96 93.6(6) . . ? F97 C44 F98 114.3(8) . . ? F97 C44 C41 121.4(8) . . ? F98 C44 C41 118.9(7) . . ? F97 C44 F99 102.6(7) . . ? F98 C44 F99 97.9(7) . . ? C41 C44 F99 92.8(6) . . ? O12 C45 C46 111.7(5) . . ? O12 C45 C48 106.8(5) . . ? C46 C45 C48 108.7(5) . . ? O12 C45 C47 110.1(5) . . ? C46 C45 C47 110.7(5) . . ? C48 C45 C47 108.5(5) . . ? F100 C46 F102 107.6(6) . . ? F100 C46 F101 107.0(6) . . ? F102 C46 F101 104.8(6) . . ? F100 C46 C45 115.9(6) . . ? F102 C46 C45 111.6(5) . . ? F101 C46 C45 109.3(5) . . ? F103 C47 F105 109.4(6) . . ? F103 C47 F104 109.4(6) . . ? F105 C47 F104 106.9(6) . . ? F103 C47 C45 111.0(6) . . ? F105 C47 C45 109.6(6) . . ? F104 C47 C45 110.4(6) . . ? F107 C48 F106 108.9(6) . . ? F107 C48 F108 106.8(6) . . ? F106 C48 F108 107.4(5) . . ? F107 C48 C45 111.7(5) . . ? F106 C48 C45 111.9(6) . . ? F108 C48 C45 109.9(6) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 23.30 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.741 _refine_diff_density_min -0.732 _refine_diff_density_rms 0.097 # Attachment 'cup8+_pf.cif' data_cup8+_pf _database_code_depnum_ccdc_archive 'CCDC 654312' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C16 Al Cu F36 O4 P8' _chemical_formula_sum 'C16 Al Cu F36 O4 P8' _chemical_formula_weight 1278.44 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' 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M P212121 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 11.7609(18) _cell_length_b 16.9425(15) _cell_length_c 38.266(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 7624.8(16) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Platelets _exptl_crystal_colour colourless _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.227 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4912 _exptl_absorpt_coefficient_mu 1.139 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.791 _exptl_absorpt_correction_T_max 0.892 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _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 'Bruker APEX II CCD area detector at 100K' _diffrn_measurement_method 'APEXII (Bruker, 2005)' _diffrn_detector_area_resol_mean 'frames each covering 0.5\% in\w' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 80331 _diffrn_reflns_av_R_equivalents 0.0770 _diffrn_reflns_av_sigmaI/netI 0.0517 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -45 _diffrn_reflns_limit_l_max 45 _diffrn_reflns_theta_min 1.31 _diffrn_reflns_theta_max 25.04 _reflns_number_total 13407 _reflns_number_gt 11418 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Bruker AXS BV, 1997-2004)' _computing_cell_refinement 'Dirax/lsq (Duisenberg & Schreurs 1989-2000)' _computing_data_reduction 'EvalCCD (Duisenberg & Schreurs 1990-2000)' _computing_structure_solution 'SHELXTL (Bruker, 2001)' _computing_structure_refinement 'SHELXTL (Bruker, 2001)' _computing_molecular_graphics 'SHELXTL (Bruker, 2001)' _computing_publication_material 'SHELXTL (Bruker, 2001)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0287P)^2^+23.7122P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens none _refine_ls_hydrogen_treatment none _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.517(15) _refine_ls_number_reflns 13407 _refine_ls_number_parameters 1190 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0671 _refine_ls_R_factor_gt 0.0506 _refine_ls_wR_factor_ref 0.1152 _refine_ls_wR_factor_gt 0.1060 _refine_ls_goodness_of_fit_ref 1.187 _refine_ls_restrained_S_all 1.187 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.74198(7) 0.50910(5) 0.79063(2) 0.02317(18) Uani 1 1 d . . . P1 P 0.79420(19) 0.38842(11) 0.81595(5) 0.0325(5) Uani 1 1 d . . . P2 P 0.69866(16) 0.39048(10) 0.76206(5) 0.0256(4) Uani 1 1 d . . . P3 P 0.83856(16) 0.31018(10) 0.77296(5) 0.0268(4) Uani 1 1 d . . . P4 P 0.67439(19) 0.29673(12) 0.80016(7) 0.0403(5) Uani 1 1 d . . . P5 P 0.78621(17) 0.62741(10) 0.81914(5) 0.0252(4) Uani 1 1 d . . . P6 P 0.70724(17) 0.63021(10) 0.76293(5) 0.0272(4) Uani 1 1 d . . . P7 P 0.66475(17) 0.71652(11) 0.80303(6) 0.0351(5) Uani 1 1 d . . . P8 P 0.83610(16) 0.71392(11) 0.77988(5) 0.0273(4) Uani 1 1 d . . . Cu2 Cu 0.27191(7) -0.00893(4) 0.96146(2) 0.02319(18) Uani 1 1 d . . . P9 P 0.31243(16) -0.12662(10) 0.99118(5) 0.0238(4) Uani 1 1 d . . . P10 P 0.24822(16) -0.13033(10) 0.93306(5) 0.0236(4) Uani 1 1 d . . . P11 P 0.37657(16) -0.21137(11) 0.95331(5) 0.0289(4) Uani 1 1 d . . . P12 P 0.19971(16) -0.21812(11) 0.97178(5) 0.0278(4) Uani 1 1 d . . . P13 P 0.2725(2) 0.10836(10) 0.99353(5) 0.0321(5) Uani 1 1 d . . . P14 P 0.2558(2) 0.11271(11) 0.93298(5) 0.0450(6) Uani 1 1 d . . . P15 P 0.35126(18) 0.20007(11) 0.96266(7) 0.0431(6) Uani 1 1 d . . . P16 P 0.16649(18) 0.19323(12) 0.96716(7) 0.0444(6) Uani 1 1 d . . . Al1 Al 0.27270(14) 0.49788(10) 0.87540(4) 0.0120(4) Uani 1 1 d . . . O1 O 0.2745(3) 0.5655(2) 0.84120(10) 0.0141(9) Uani 1 1 d . . . O2 O 0.3835(3) 0.5126(2) 0.90472(10) 0.0189(9) Uani 1 1 d . . . O3 O 0.2900(4) 0.4045(2) 0.85775(10) 0.0161(9) Uani 1 1 d . . . O4 O 0.1439(3) 0.5077(2) 0.89671(10) 0.0169(9) Uani 1 1 d . . . C1 C 0.2564(6) 0.6427(3) 0.83173(16) 0.0191(14) Uani 1 1 d . . . C2 C 0.1282(6) 0.6582(4) 0.82615(18) 0.0242(16) Uani 1 1 d . . . C3 C 0.3035(6) 0.6994(4) 0.85996(18) 0.0227(15) Uani 1 1 d . . . C4 C 0.3215(6) 0.6559(4) 0.79684(18) 0.0238(15) Uani 1 1 d . . . C5 C 0.4917(5) 0.4965(3) 0.91436(16) 0.0166(13) Uani 1 1 d . . . C6 C 0.5777(6) 0.5368(4) 0.88870(19) 0.0298(17) Uani 1 1 d . . . C7 C 0.5095(5) 0.5286(4) 0.95155(18) 0.0223(15) Uani 1 1 d . . . C8 C 0.5171(6) 0.4044(4) 0.91385(17) 0.0231(15) Uani 1 1 d . . . C9 C 0.2670(5) 0.3578(3) 0.82987(15) 0.0118(12) Uani 1 1 d . . . C10 C 0.3354(5) 0.3850(4) 0.79714(16) 0.0198(14) Uani 1 1 d . . . C11 C 0.3047(6) 0.2703(4) 0.83990(17) 0.0232(15) Uani 1 1 d . . . C12 C 0.1369(5) 0.3565(4) 0.82080(17) 0.0199(14) Uani 1 1 d . . . C13 C 0.0784(5) 0.4920(4) 0.92536(15) 0.0171(13) Uani 1 1 d . . . C14 C 0.1117(6) 0.4117(4) 0.94269(18) 0.0244(15) Uani 1 1 d . . . C15 C -0.0495(5) 0.4889(4) 0.91369(16) 0.0247(15) Uani 1 1 d . . . C16 C 0.0937(6) 0.5587(4) 0.95312(17) 0.0248(16) Uani 1 1 d . . . Al2 Al 0.78086(14) 0.00168(10) 0.87439(4) 0.0132(4) Uani 1 1 d . . . O5 O 0.8155(4) -0.0668(2) 0.90638(10) 0.0174(10) Uani 1 1 d . . . O6 O 0.6433(3) -0.0192(2) 0.86026(10) 0.0143(9) Uani 1 1 d . . . O7 O 0.8730(3) -0.0034(2) 0.83905(10) 0.0181(9) Uani 1 1 d . . . O8 O 0.7940(4) 0.0950(2) 0.89303(11) 0.0183(10) Uani 1 1 d . . . C17 C 0.8133(5) -0.1440(3) 0.91682(16) 0.0158(13) Uani 1 1 d . . . C18 C 0.8724(6) -0.1472(4) 0.95370(17) 0.0220(15) Uani 1 1 d . . . C19 C 0.8810(6) -0.1965(4) 0.89050(17) 0.0230(15) Uani 1 1 d . . . C20 C 0.6894(6) -0.1746(4) 0.92029(19) 0.0267(16) Uani 1 1 d . . . C21 C 0.5641(5) -0.0099(3) 0.83521(15) 0.0157(13) Uani 1 1 d . . . C22 C 0.5159(6) 0.0769(4) 0.83624(18) 0.0232(15) Uani 1 1 d . . . C23 C 0.4637(5) -0.0687(4) 0.84261(17) 0.0212(15) Uani 1 1 d . . . C24 C 0.6119(5) -0.0260(4) 0.79806(17) 0.0230(15) Uani 1 1 d . . . C25 C 0.7831(6) 0.1402(4) 0.92203(16) 0.0191(14) Uani 1 1 d . . . C26 C 0.6543(6) 0.1497(4) 0.93248(18) 0.0267(16) Uani 1 1 d . . . C27 C 0.8481(5) 0.1032(4) 0.95349(17) 0.0205(14) Uani 1 1 d . . . C28 C 0.8330(5) 0.2238(4) 0.91367(17) 0.0200(14) Uani 1 1 d . . . C29 C 0.9689(5) 0.0217(4) 0.82394(17) 0.0185(14) Uani 1 1 d . . . C30 C 1.0746(6) -0.0007(5) 0.8458(2) 0.041(2) Uani 1 1 d . . . C31 C 0.9688(6) 0.1137(4) 0.8186(2) 0.0363(19) Uani 1 1 d . . . C32 C 0.9777(7) -0.0174(5) 0.7871(2) 0.040(2) Uani 1 1 d . . . F1 F 0.0800(3) 0.5980(2) 0.80835(11) 0.0316(10) Uani 1 1 d . . . F2 F 0.0738(4) 0.6660(2) 0.85617(11) 0.0351(10) Uani 1 1 d . . . F3 F 0.1109(3) 0.7242(2) 0.80702(11) 0.0320(10) Uani 1 1 d . . . F4 F 0.2707(4) 0.6755(2) 0.89209(10) 0.0343(10) Uani 1 1 d . . . F5 F 0.4165(4) 0.7017(2) 0.85998(11) 0.0365(11) Uani 1 1 d . . . F6 F 0.2653(4) 0.7738(2) 0.85604(10) 0.0333(10) Uani 1 1 d . . . F7 F 0.3420(4) 0.7338(2) 0.79088(10) 0.0314(10) Uani 1 1 d . . . F8 F 0.4221(3) 0.6204(2) 0.79712(11) 0.0333(10) Uani 1 1 d . . . F9 F 0.2647(4) 0.6289(2) 0.76950(10) 0.0321(10) Uani 1 1 d . . . F10 F 0.5839(3) 0.6147(2) 0.89513(12) 0.0384(11) Uani 1 1 d . . . F11 F 0.6829(3) 0.5064(3) 0.89096(10) 0.0373(10) Uani 1 1 d . . . F12 F 0.5435(3) 0.5283(3) 0.85542(10) 0.0331(10) Uani 1 1 d . . . F13 F 0.4610(3) 0.4821(3) 0.97539(9) 0.0356(10) Uani 1 1 d . . . F14 F 0.4665(3) 0.6007(2) 0.95507(11) 0.0328(10) Uani 1 1 d . . . F15 F 0.6219(3) 0.5335(2) 0.96049(11) 0.0327(10) Uani 1 1 d . . . F16 F 0.6044(4) 0.3855(2) 0.93383(11) 0.0374(11) Uani 1 1 d . . . F17 F 0.4250(3) 0.3660(2) 0.92629(11) 0.0331(10) Uani 1 1 d . . . F18 F 0.5353(3) 0.3787(2) 0.88155(11) 0.0355(10) Uani 1 1 d . . . F19 F 0.4371(3) 0.4104(2) 0.80585(10) 0.0249(9) Uani 1 1 d . . . F20 F 0.3473(4) 0.3277(2) 0.77286(10) 0.0292(9) Uani 1 1 d . . . F21 F 0.2806(3) 0.4455(2) 0.78104(10) 0.0269(9) Uani 1 1 d . . . F22 F 0.4178(3) 0.2653(2) 0.83849(10) 0.0254(9) Uani 1 1 d . . . F23 F 0.2618(3) 0.2169(2) 0.81748(10) 0.0278(9) Uani 1 1 d . . . F24 F 0.2720(4) 0.2529(2) 0.87173(10) 0.0302(10) Uani 1 1 d . . . F25 F 0.1152(3) 0.3273(2) 0.78904(10) 0.0296(9) Uani 1 1 d . . . F26 F 0.0780(3) 0.3141(2) 0.84431(10) 0.0278(9) Uani 1 1 d . . . F27 F 0.0945(3) 0.4303(2) 0.82226(10) 0.0271(9) Uani 1 1 d . . . F28 F 0.1281(3) 0.3570(2) 0.91790(10) 0.0282(9) Uani 1 1 d . . . F29 F 0.2082(3) 0.4189(2) 0.96065(11) 0.0339(10) Uani 1 1 d . . . F30 F 0.0311(3) 0.3843(2) 0.96438(10) 0.0335(10) Uani 1 1 d . . . F31 F -0.0716(3) 0.5473(2) 0.89122(10) 0.0295(9) Uani 1 1 d . . . F32 F -0.0709(3) 0.4208(2) 0.89692(10) 0.0303(9) Uani 1 1 d . . . F33 F -0.1206(3) 0.4951(2) 0.94044(9) 0.0325(9) Uani 1 1 d . . . F34 F 0.0362(4) 0.6244(2) 0.94249(11) 0.0372(10) Uani 1 1 d . . . F35 F 0.0558(3) 0.5393(3) 0.98468(10) 0.0351(10) Uani 1 1 d . . . F36 F 0.2032(3) 0.5781(2) 0.95621(11) 0.0310(9) Uani 1 1 d . . . F37 F 0.8029(3) -0.1235(2) 0.97912(9) 0.0278(9) Uani 1 1 d . . . F38 F 0.9650(3) -0.1025(2) 0.95458(10) 0.0264(9) Uani 1 1 d . . . F39 F 0.9056(3) -0.2219(2) 0.96171(10) 0.0278(9) Uani 1 1 d . . . F40 F 0.9933(3) -0.1862(2) 0.89402(11) 0.0301(9) Uani 1 1 d . . . F41 F 0.8590(4) -0.2738(2) 0.89522(11) 0.0337(10) Uani 1 1 d . . . F42 F 0.8518(4) -0.1789(2) 0.85765(10) 0.0314(10) Uani 1 1 d . . . F43 F 0.6819(3) -0.2394(2) 0.94085(11) 0.0326(10) Uani 1 1 d . . . F44 F 0.6238(3) -0.1196(2) 0.93476(11) 0.0336(10) Uani 1 1 d . . . F45 F 0.6450(3) -0.1927(2) 0.88922(11) 0.0323(10) Uani 1 1 d . . . F46 F 0.4469(3) 0.0869(2) 0.86375(10) 0.0317(10) Uani 1 1 d . . . F47 F 0.6003(3) 0.1286(2) 0.83961(10) 0.0289(9) Uani 1 1 d . . . F48 F 0.4567(4) 0.0952(2) 0.80750(10) 0.0335(10) Uani 1 1 d . . . F49 F 0.4386(3) -0.0699(2) 0.87632(10) 0.0332(10) Uani 1 1 d . . . F50 F 0.3699(3) -0.0508(2) 0.82445(10) 0.0298(9) Uani 1 1 d . . . F51 F 0.4950(3) -0.1421(2) 0.83296(11) 0.0320(10) Uani 1 1 d . . . F52 F 0.5334(3) -0.0390(2) 0.77393(10) 0.0311(9) Uani 1 1 d . . . F53 F 0.6816(3) -0.0888(2) 0.79856(10) 0.0270(9) Uani 1 1 d . . . F54 F 0.6758(3) 0.0359(2) 0.78712(9) 0.0279(9) Uani 1 1 d . . . F55 F 1.0568(4) 0.0077(3) 0.87985(10) 0.0466(12) Uani 1 1 d . . . F56 F 1.0999(4) -0.0799(3) 0.84048(15) 0.0584(15) Uani 1 1 d . . . F57 F 1.1685(3) 0.0399(3) 0.83765(13) 0.0427(11) Uani 1 1 d . . . F58 F 0.8658(4) 0.1394(3) 0.81199(13) 0.0495(13) Uani 1 1 d . . . F59 F 0.9991(4) 0.1481(3) 0.84968(14) 0.0511(13) Uani 1 1 d . . . F60 F 1.0418(4) 0.1391(2) 0.79511(12) 0.0440(12) Uani 1 1 d . . . F61 F 0.9071(4) 0.0180(3) 0.76408(11) 0.0541(13) Uani 1 1 d . . . F62 F 1.0855(4) -0.0106(3) 0.77347(11) 0.0458(11) Uani 1 1 d . . . F63 F 0.9517(4) -0.0918(3) 0.78756(12) 0.0468(13) Uani 1 1 d . . . F64 F 0.6001(3) 0.1978(2) 0.91063(11) 0.0346(10) Uani 1 1 d . . . F65 F 0.6401(3) 0.1760(2) 0.96492(11) 0.0355(10) Uani 1 1 d . . . F66 F 0.6018(3) 0.0788(2) 0.93035(10) 0.0325(10) Uani 1 1 d . . . F67 F 0.7890(4) 0.0440(2) 0.96796(10) 0.0319(10) Uani 1 1 d . . . F68 F 0.8690(4) 0.1564(2) 0.97921(10) 0.0319(10) Uani 1 1 d . . . F69 F 0.9489(3) 0.0748(2) 0.94317(10) 0.0268(9) Uani 1 1 d . . . F70 F 0.9451(3) 0.2218(2) 0.91365(11) 0.0291(9) Uani 1 1 d . . . F71 F 0.7980(3) 0.2489(2) 0.88247(10) 0.0291(9) Uani 1 1 d . . . F72 F 0.7997(4) 0.2778(2) 0.93760(10) 0.0311(10) 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 Cu1 0.0275(4) 0.0124(4) 0.0296(4) 0.0000(3) -0.0001(3) 0.0015(3) P1 0.0519(13) 0.0195(9) 0.0261(10) 0.0004(8) -0.0125(9) 0.0092(9) P2 0.0266(10) 0.0148(8) 0.0356(11) 0.0015(8) -0.0108(8) -0.0012(7) P3 0.0217(10) 0.0193(9) 0.0393(11) -0.0057(8) 0.0003(8) 0.0031(7) P4 0.0343(12) 0.0216(10) 0.0650(15) 0.0146(10) 0.0169(11) -0.0018(8) P5 0.0369(11) 0.0172(9) 0.0216(9) 0.0020(7) -0.0029(8) -0.0053(8) P6 0.0394(11) 0.0153(9) 0.0268(10) 0.0011(7) -0.0134(8) 0.0013(8) P7 0.0260(10) 0.0178(9) 0.0615(14) -0.0090(9) 0.0081(10) 0.0034(8) P8 0.0245(10) 0.0243(10) 0.0330(11) 0.0075(8) 0.0018(8) -0.0049(8) Cu2 0.0309(4) 0.0107(4) 0.0279(4) -0.0003(3) 0.0002(4) 0.0000(3) P9 0.0346(11) 0.0127(8) 0.0241(9) -0.0007(7) -0.0072(8) 0.0008(8) P10 0.0343(11) 0.0144(8) 0.0221(9) -0.0014(7) -0.0055(8) -0.0014(8) P11 0.0224(10) 0.0185(9) 0.0458(12) -0.0034(8) 0.0042(9) 0.0030(7) P12 0.0208(9) 0.0209(9) 0.0418(12) 0.0070(8) -0.0002(8) -0.0032(7) P13 0.0611(14) 0.0131(8) 0.0220(9) 0.0006(7) -0.0007(9) 0.0026(9) P14 0.099(2) 0.0152(9) 0.0204(10) 0.0020(8) -0.0055(11) 0.0018(11) P15 0.0326(12) 0.0195(10) 0.0772(17) -0.0052(10) 0.0169(11) -0.0102(8) P16 0.0292(11) 0.0221(10) 0.0821(17) -0.0079(11) -0.0176(11) 0.0091(8) Al1 0.0109(8) 0.0075(8) 0.0175(8) 0.0001(7) -0.0005(7) -0.0001(7) O1 0.017(2) 0.0050(19) 0.021(2) 0.0024(16) 0.0016(18) -0.0021(16) O2 0.013(2) 0.016(2) 0.027(2) -0.0042(19) -0.0015(18) -0.0005(18) O3 0.020(2) 0.008(2) 0.021(2) -0.0046(17) -0.0046(19) 0.0010(17) O4 0.015(2) 0.014(2) 0.022(2) 0.0013(19) 0.0043(17) -0.0008(18) C1 0.029(4) 0.011(3) 0.017(3) 0.003(2) -0.004(3) 0.000(3) C2 0.028(4) 0.015(3) 0.029(4) 0.007(3) 0.002(3) 0.006(3) C3 0.028(4) 0.011(3) 0.029(4) 0.005(3) -0.004(3) 0.002(3) C4 0.030(4) 0.014(3) 0.027(4) 0.010(3) 0.001(3) -0.002(3) C5 0.016(3) 0.011(3) 0.022(3) 0.001(3) -0.007(2) -0.006(3) C6 0.016(4) 0.039(5) 0.034(4) 0.004(3) -0.003(3) -0.008(3) C7 0.010(3) 0.022(4) 0.035(4) 0.003(3) 0.000(3) 0.003(3) C8 0.020(4) 0.026(4) 0.024(4) 0.001(3) -0.008(3) 0.000(3) C9 0.009(3) 0.009(3) 0.018(3) -0.001(2) 0.000(2) 0.001(2) C10 0.021(3) 0.018(3) 0.021(3) 0.000(3) -0.002(3) 0.001(3) C11 0.034(4) 0.013(3) 0.022(4) -0.005(3) -0.003(3) -0.003(3) C12 0.018(3) 0.020(3) 0.022(4) -0.003(3) 0.004(3) 0.003(3) C13 0.015(3) 0.018(3) 0.018(3) 0.000(3) 0.000(2) -0.002(3) C14 0.022(4) 0.023(4) 0.028(4) 0.003(3) 0.008(3) -0.002(3) C15 0.022(4) 0.030(4) 0.022(3) 0.002(3) 0.001(3) -0.006(3) C16 0.026(4) 0.027(4) 0.022(4) -0.006(3) 0.001(3) 0.002(3) Al2 0.0135(9) 0.0093(9) 0.0167(9) -0.0003(7) 0.0005(7) 0.0001(7) O5 0.022(2) 0.010(2) 0.021(2) 0.0015(17) -0.0019(19) -0.0005(18) O6 0.014(2) 0.013(2) 0.016(2) 0.0023(17) -0.0005(17) 0.0010(17) O7 0.011(2) 0.016(2) 0.027(2) 0.001(2) 0.0041(17) 0.0042(18) O8 0.025(2) 0.010(2) 0.019(2) -0.0021(18) 0.0002(19) -0.0007(18) C17 0.019(3) 0.009(3) 0.020(3) -0.002(3) 0.002(3) 0.003(2) C18 0.022(4) 0.015(3) 0.030(4) 0.001(3) 0.002(3) -0.004(3) C19 0.033(4) 0.011(3) 0.024(4) 0.000(3) 0.003(3) 0.003(3) C20 0.033(4) 0.015(3) 0.032(4) 0.011(3) 0.002(3) -0.002(3) C21 0.017(3) 0.010(3) 0.020(3) 0.003(3) -0.003(3) 0.003(3) C22 0.023(4) 0.017(3) 0.030(4) 0.001(3) -0.009(3) 0.003(3) C23 0.010(3) 0.025(4) 0.029(4) -0.002(3) 0.001(3) -0.007(3) C24 0.018(3) 0.028(4) 0.023(3) -0.001(3) -0.006(3) -0.001(3) C25 0.026(4) 0.014(3) 0.017(3) -0.003(3) 0.001(3) 0.004(3) C26 0.019(4) 0.035(4) 0.026(4) -0.008(3) 0.004(3) -0.002(3) C27 0.019(3) 0.017(3) 0.025(3) 0.002(3) -0.004(3) -0.004(3) C28 0.013(3) 0.020(3) 0.027(4) -0.003(3) -0.005(3) -0.001(3) C29 0.015(3) 0.014(3) 0.027(4) 0.003(3) 0.004(3) 0.000(2) C30 0.020(4) 0.055(6) 0.048(5) 0.011(4) 0.006(3) 0.007(4) C31 0.028(4) 0.015(4) 0.066(6) 0.004(4) 0.013(4) -0.004(3) C32 0.042(5) 0.031(4) 0.046(5) -0.008(4) 0.018(4) -0.004(4) F1 0.016(2) 0.022(2) 0.057(3) -0.0029(19) -0.0123(19) 0.0009(16) F2 0.030(2) 0.025(2) 0.051(3) 0.004(2) 0.017(2) 0.0058(18) F3 0.026(2) 0.025(2) 0.045(2) 0.0082(19) -0.0020(19) 0.0039(17) F4 0.063(3) 0.0184(19) 0.021(2) -0.0008(16) -0.002(2) 0.000(2) F5 0.036(3) 0.021(2) 0.053(3) 0.0024(19) -0.022(2) -0.0068(18) F6 0.058(3) 0.0088(18) 0.033(2) -0.0007(16) -0.001(2) -0.0019(19) F7 0.040(2) 0.018(2) 0.036(2) 0.0105(17) 0.0027(19) -0.0022(18) F8 0.022(2) 0.033(2) 0.045(2) 0.010(2) 0.0145(19) 0.0056(18) F9 0.048(3) 0.025(2) 0.024(2) -0.0006(17) -0.0023(19) 0.007(2) F10 0.029(2) 0.027(2) 0.059(3) 0.013(2) -0.007(2) -0.0152(19) F11 0.0103(18) 0.060(3) 0.042(2) 0.004(2) 0.0003(17) 0.000(2) F12 0.020(2) 0.052(3) 0.027(2) 0.008(2) -0.0011(17) -0.0038(19) F13 0.039(2) 0.045(3) 0.022(2) 0.004(2) 0.0018(18) -0.003(2) F14 0.034(2) 0.025(2) 0.039(2) -0.0129(19) -0.0107(19) 0.0052(18) F15 0.020(2) 0.035(2) 0.044(2) -0.0081(19) -0.0154(19) 0.0039(17) F16 0.038(3) 0.024(2) 0.050(3) -0.0028(19) -0.021(2) 0.0141(19) F17 0.034(2) 0.0144(19) 0.051(3) 0.0080(18) -0.004(2) -0.0057(18) F18 0.035(2) 0.030(2) 0.042(3) -0.015(2) -0.007(2) 0.0152(19) F19 0.017(2) 0.025(2) 0.033(2) 0.0012(17) 0.0004(17) -0.0037(16) F20 0.042(3) 0.022(2) 0.023(2) -0.0074(17) 0.0079(18) 0.0027(18) F21 0.037(2) 0.0179(19) 0.026(2) 0.0087(16) -0.0009(18) 0.0000(17) F22 0.017(2) 0.0151(19) 0.044(2) -0.0020(17) -0.0055(18) 0.0073(15) F23 0.034(2) 0.0127(18) 0.037(2) -0.0095(16) -0.0024(19) -0.0037(17) F24 0.049(3) 0.0120(18) 0.030(2) 0.0011(16) 0.003(2) -0.0003(18) F25 0.027(2) 0.031(2) 0.031(2) -0.0135(18) -0.0094(18) -0.0038(18) F26 0.022(2) 0.021(2) 0.041(2) -0.0012(17) 0.0071(18) -0.0065(16) F27 0.025(2) 0.018(2) 0.038(2) -0.0036(17) -0.0071(18) 0.0036(17) F28 0.039(2) 0.0111(18) 0.034(2) 0.0010(17) 0.0042(19) 0.0017(16) F29 0.025(2) 0.041(2) 0.035(2) 0.0131(19) -0.0117(19) 0.0047(19) F30 0.037(2) 0.027(2) 0.036(2) 0.0124(19) 0.016(2) 0.0011(18) F31 0.018(2) 0.032(2) 0.039(2) 0.0170(19) -0.0021(18) 0.0013(17) F32 0.025(2) 0.031(2) 0.035(2) -0.0056(19) -0.0018(19) -0.0100(18) F33 0.0181(19) 0.047(3) 0.032(2) 0.006(2) 0.0089(16) -0.0022(19) F34 0.043(3) 0.019(2) 0.050(3) -0.0103(19) 0.006(2) 0.0087(19) F35 0.032(2) 0.048(3) 0.026(2) -0.0104(19) 0.0050(18) 0.003(2) F36 0.021(2) 0.034(2) 0.038(2) -0.0129(19) -0.0008(18) -0.0077(17) F37 0.034(2) 0.030(2) 0.0195(19) 0.0025(16) 0.0049(17) 0.0035(18) F38 0.026(2) 0.0182(19) 0.035(2) 0.0035(17) -0.0053(18) 0.0024(16) F39 0.038(2) 0.0141(19) 0.031(2) 0.0087(17) -0.0056(19) 0.0035(17) F40 0.022(2) 0.025(2) 0.044(3) -0.0064(19) 0.0073(19) 0.0055(17) F41 0.054(3) 0.0067(18) 0.040(2) -0.0004(17) 0.002(2) -0.0007(18) F42 0.049(3) 0.019(2) 0.026(2) -0.0016(17) 0.0009(19) -0.0036(19) F43 0.030(2) 0.026(2) 0.042(2) 0.0158(19) -0.0010(19) -0.0089(18) F44 0.019(2) 0.031(2) 0.051(3) 0.005(2) 0.0046(19) 0.0005(18) F45 0.029(2) 0.025(2) 0.043(3) 0.0051(19) -0.016(2) -0.0056(17) F46 0.024(2) 0.028(2) 0.043(3) -0.0116(19) 0.0027(19) 0.0146(17) F47 0.032(2) 0.0129(19) 0.042(2) 0.0011(17) -0.0082(19) -0.0015(17) F48 0.038(2) 0.022(2) 0.041(2) -0.0014(18) -0.020(2) 0.0112(18) F49 0.026(2) 0.038(2) 0.035(2) 0.0015(19) 0.0101(19) -0.0083(19) F50 0.0114(19) 0.036(2) 0.042(2) -0.0016(19) -0.0050(17) 0.0004(16) F51 0.030(2) 0.0119(19) 0.055(3) -0.0038(18) -0.003(2) -0.0072(16) F52 0.028(2) 0.038(2) 0.027(2) -0.0085(18) -0.0063(18) 0.0000(18) F53 0.026(2) 0.022(2) 0.032(2) -0.0086(17) 0.0038(18) 0.0018(17) F54 0.028(2) 0.031(2) 0.025(2) 0.0065(17) 0.0016(17) -0.0062(17) F55 0.037(2) 0.071(3) 0.031(2) 0.001(2) -0.0104(19) -0.005(3) F56 0.036(3) 0.036(3) 0.103(4) 0.023(3) 0.011(3) 0.020(2) F57 0.012(2) 0.043(3) 0.073(3) 0.004(2) 0.003(2) 0.0003(18) F58 0.031(3) 0.027(2) 0.090(4) 0.027(2) 0.016(2) 0.015(2) F59 0.047(3) 0.028(2) 0.079(4) -0.017(3) 0.021(3) -0.013(2) F60 0.045(3) 0.023(2) 0.065(3) 0.013(2) 0.031(2) -0.002(2) F61 0.045(3) 0.085(4) 0.032(2) 0.008(3) 0.003(2) 0.003(3) F62 0.039(3) 0.043(3) 0.055(3) -0.011(2) 0.031(2) -0.006(2) F63 0.046(3) 0.041(3) 0.053(3) -0.024(2) 0.025(2) -0.013(2) F64 0.028(2) 0.035(2) 0.041(2) -0.006(2) -0.010(2) 0.0094(19) F65 0.032(2) 0.042(3) 0.032(2) -0.013(2) 0.0058(19) 0.003(2) F66 0.024(2) 0.033(2) 0.040(2) -0.0084(19) 0.0073(19) -0.0117(18) F67 0.051(3) 0.0219(19) 0.023(2) 0.0034(16) 0.0026(19) -0.0039(19) F68 0.053(3) 0.020(2) 0.023(2) -0.0052(17) -0.0102(19) 0.0066(18) F69 0.025(2) 0.025(2) 0.031(2) -0.0023(17) -0.0052(17) 0.0063(17) F70 0.027(2) 0.0198(19) 0.040(2) -0.0024(18) -0.0028(19) -0.0051(17) F71 0.040(2) 0.0134(18) 0.034(2) 0.0000(16) -0.0067(19) -0.0017(17) F72 0.044(3) 0.0122(18) 0.037(2) -0.0122(17) -0.003(2) 0.0013(18) _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 Cu1 P5 2.3406(19) . ? Cu1 P2 2.3440(19) . ? Cu1 P1 2.3445(19) . ? Cu1 P6 2.3452(19) . ? P1 P3 2.176(3) . ? P1 P4 2.183(3) . ? P1 P2 2.349(3) . ? P2 P4 2.175(3) . ? P2 P3 2.175(3) . ? P3 P4 2.205(3) . ? P5 P7 2.168(3) . ? P5 P8 2.179(3) . ? P5 P6 2.343(3) . ? P6 P8 2.175(3) . ? P6 P7 2.178(3) . ? P7 P8 2.202(3) . ? Cu2 P13 2.3356(19) . ? Cu2 P14 2.339(2) . ? Cu2 P10 2.3430(18) . ? Cu2 P9 2.3444(19) . ? P9 P12 2.171(3) . ? P9 P11 2.175(3) . ? P9 P10 2.350(2) . ? P10 P12 2.175(3) . ? P10 P11 2.183(3) . ? P11 P12 2.200(3) . ? P13 P16 2.154(3) . ? P13 P15 2.161(3) . ? P13 P14 2.327(3) . ? P14 P16 2.162(3) . ? P14 P15 2.177(3) . ? P15 P16 2.183(3) . ? Al1 O4 1.729(4) . ? Al1 O3 1.732(4) . ? Al1 O2 1.738(4) . ? Al1 O1 1.740(4) . ? O1 C1 1.373(7) . ? O2 C5 1.352(7) . ? O3 C9 1.355(7) . ? O4 C13 1.366(7) . ? C1 C2 1.546(9) . ? C1 C3 1.548(9) . ? C1 C4 1.555(9) . ? C2 F2 1.321(8) . ? C2 F1 1.351(8) . ? C2 F3 1.351(7) . ? C3 F5 1.330(8) . ? C3 F6 1.347(7) . ? C3 F4 1.351(8) . ? C4 F9 1.322(8) . ? C4 F8 1.327(8) . ? C4 F7 1.361(7) . ? C5 C7 1.538(9) . ? C5 C6 1.566(9) . ? C5 C8 1.589(9) . ? C6 F12 1.343(8) . ? C6 F11 1.344(8) . ? C6 F10 1.344(8) . ? C7 F14 1.328(7) . ? C7 F13 1.334(8) . ? C7 F15 1.368(7) . ? C8 F16 1.319(7) . ? C8 F18 1.328(8) . ? C8 F17 1.350(8) . ? C9 C10 1.559(8) . ? C9 C12 1.569(8) . ? C9 C11 1.594(8) . ? C10 F19 1.314(7) . ? C10 F20 1.351(7) . ? C10 F21 1.359(7) . ? C11 F24 1.311(8) . ? C11 F22 1.334(8) . ? C11 F23 1.345(7) . ? C12 F25 1.336(7) . ? C12 F26 1.344(7) . ? C12 F27 1.348(7) . ? C13 C16 1.562(9) . ? C13 C14 1.563(9) . ? C13 C15 1.570(9) . ? C14 F29 1.333(8) . ? C14 F28 1.341(8) . ? C14 F30 1.342(7) . ? C15 F33 1.326(7) . ? C15 F31 1.335(8) . ? C15 F32 1.344(8) . ? C16 F35 1.329(8) . ? C16 F36 1.334(8) . ? C16 F34 1.364(8) . ? Al2 O7 1.735(4) . ? Al2 O5 1.735(4) . ? Al2 O8 1.742(4) . ? Al2 O6 1.742(4) . ? O5 C17 1.368(7) . ? O6 C21 1.346(7) . ? O7 C29 1.337(7) . ? O8 C25 1.354(7) . ? C17 C20 1.552(10) . ? C17 C19 1.562(9) . ? C17 C18 1.574(9) . ? C18 F38 1.327(7) . ? C18 F37 1.333(7) . ? C18 F39 1.359(7) . ? C19 F42 1.337(8) . ? C19 F40 1.339(8) . ? C19 F41 1.347(7) . ? C20 F44 1.330(8) . ? C20 F45 1.334(8) . ? C20 F43 1.354(7) . ? C21 C24 1.553(9) . ? C21 C23 1.570(8) . ? C21 C22 1.576(9) . ? C22 F47 1.330(7) . ? C22 F48 1.339(7) . ? C22 F46 1.340(8) . ? C23 F49 1.323(8) . ? C23 F50 1.339(7) . ? C23 F51 1.349(8) . ? C24 F52 1.324(7) . ? C24 F53 1.344(7) . ? C24 F54 1.357(7) . ? C25 C27 1.558(9) . ? C25 C28 1.567(9) . ? C25 C26 1.575(9) . ? C26 F65 1.329(8) . ? C26 F64 1.330(8) . ? C26 F66 1.354(8) . ? C27 F69 1.338(7) . ? C27 F67 1.340(7) . ? C27 F68 1.357(7) . ? C28 F70 1.319(7) . ? C28 F71 1.333(7) . ? C28 F72 1.352(7) . ? C29 C30 1.546(9) . ? C29 C32 1.561(10) . ? C29 C31 1.573(9) . ? C30 F55 1.328(9) . ? C30 F57 1.337(8) . ? C30 F56 1.390(10) . ? C31 F58 1.312(9) . ? C31 F60 1.316(8) . ? C31 F59 1.371(10) . ? C32 F63 1.298(9) . ? C32 F61 1.350(9) . ? C32 F62 1.376(8) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag P5 Cu1 P2 179.72(8) . . ? P5 Cu1 P1 119.74(7) . . ? P2 Cu1 P1 60.13(7) . . ? P5 Cu1 P6 60.01(7) . . ? P2 Cu1 P6 120.10(7) . . ? P1 Cu1 P6 174.51(9) . . ? P3 P1 P4 60.79(9) . . ? P3 P1 Cu1 106.36(10) . . ? P4 P1 Cu1 109.71(10) . . ? P3 P1 P2 57.32(8) . . ? P4 P1 P2 57.23(9) . . ? Cu1 P1 P2 59.93(6) . . ? P4 P2 P3 60.92(9) . . ? P4 P2 Cu1 110.00(10) . . ? P3 P2 Cu1 106.40(9) . . ? P4 P2 P1 57.54(9) . . ? P3 P2 P1 57.35(8) . . ? Cu1 P2 P1 59.95(6) . . ? P2 P3 P1 65.34(9) . . ? P2 P3 P4 59.53(9) . . ? P1 P3 P4 59.75(10) . . ? P2 P4 P1 65.23(9) . . ? P2 P4 P3 59.55(9) . . ? P1 P4 P3 59.46(9) . . ? P7 P5 P8 60.86(9) . . ? P7 P5 Cu1 108.51(10) . . ? P8 P5 Cu1 108.33(9) . . ? P7 P5 P6 57.57(9) . . ? P8 P5 P6 57.34(8) . . ? Cu1 P5 P6 60.09(6) . . ? P8 P6 P7 60.78(9) . . ? P8 P6 P5 57.54(8) . . ? P7 P6 P5 57.17(9) . . ? P8 P6 Cu1 108.33(9) . . ? P7 P6 Cu1 108.01(10) . . ? P5 P6 Cu1 59.90(6) . . ? P5 P7 P6 65.26(9) . . ? P5 P7 P8 59.83(9) . . ? P6 P7 P8 59.54(9) . . ? P6 P8 P5 65.12(8) . . ? P6 P8 P7 59.68(9) . . ? P5 P8 P7 59.32(9) . . ? P13 Cu2 P14 59.70(7) . . ? P13 Cu2 P10 172.31(8) . . ? P14 Cu2 P10 123.21(7) . . ? P13 Cu2 P9 117.92(7) . . ? P14 Cu2 P9 172.68(9) . . ? P10 Cu2 P9 60.17(6) . . ? P12 P9 P11 60.82(8) . . ? P12 P9 Cu2 108.50(9) . . ? P11 P9 Cu2 107.98(9) . . ? P12 P9 P10 57.37(8) . . ? P11 P9 P10 57.52(8) . . ? Cu2 P9 P10 59.89(6) . . ? P12 P10 P11 60.63(8) . . ? P12 P10 Cu2 108.39(9) . . ? P11 P10 Cu2 107.78(9) . . ? P12 P10 P9 57.18(8) . . ? P11 P10 P9 57.22(8) . . ? Cu2 P10 P9 59.95(6) . . ? P9 P11 P10 65.26(8) . . ? P9 P11 P12 59.49(9) . . ? P10 P11 P12 59.53(8) . . ? P9 P12 P10 65.45(8) . . ? P9 P12 P11 59.69(9) . . ? P10 P12 P11 59.84(9) . . ? P16 P13 P15 60.79(10) . . ? P16 P13 P14 57.56(10) . . ? P15 P13 P14 57.91(10) . . ? P16 P13 Cu2 108.68(10) . . ? P15 P13 Cu2 109.01(10) . . ? P14 P13 Cu2 60.23(7) . . ? P16 P14 P15 60.40(10) . . ? P16 P14 P13 57.21(10) . . ? P15 P14 P13 57.22(10) . . ? P16 P14 Cu2 108.25(11) . . ? P15 P14 Cu2 108.31(11) . . ? P13 P14 Cu2 60.08(7) . . ? P13 P15 P14 64.87(9) . . ? P13 P15 P16 59.45(10) . . ? P14 P15 P16 59.47(11) . . ? P13 P16 P14 65.23(9) . . ? P13 P16 P15 59.76(10) . . ? P14 P16 P15 60.13(11) . . ? O4 Al1 O3 112.0(2) . . ? O4 Al1 O2 109.8(2) . . ? O3 Al1 O2 107.2(2) . . ? O4 Al1 O1 107.6(2) . . ? O3 Al1 O1 107.9(2) . . ? O2 Al1 O1 112.4(2) . . ? C1 O1 Al1 145.5(4) . . ? C5 O2 Al1 148.5(4) . . ? C9 O3 Al1 144.7(4) . . ? C13 O4 Al1 148.7(4) . . ? O1 C1 C2 110.5(5) . . ? O1 C1 C3 110.6(5) . . ? C2 C1 C3 109.9(5) . . ? O1 C1 C4 106.7(5) . . ? C2 C1 C4 109.7(5) . . ? C3 C1 C4 109.5(5) . . ? F2 C2 F1 108.1(6) . . ? F2 C2 F3 108.4(5) . . ? F1 C2 F3 106.7(5) . . ? F2 C2 C1 111.7(6) . . ? F1 C2 C1 110.5(5) . . ? F3 C2 C1 111.2(5) . . ? F5 C3 F6 107.8(5) . . ? F5 C3 F4 107.1(5) . . ? F6 C3 F4 106.7(5) . . ? F5 C3 C1 112.1(6) . . ? F6 C3 C1 112.6(5) . . ? F4 C3 C1 110.3(5) . . ? F9 C4 F8 107.4(5) . . ? F9 C4 F7 107.0(5) . . ? F8 C4 F7 106.4(5) . . ? F9 C4 C1 112.4(5) . . ? F8 C4 C1 111.5(5) . . ? F7 C4 C1 111.8(5) . . ? O2 C5 C7 108.0(5) . . ? O2 C5 C6 110.4(5) . . ? C7 C5 C6 109.7(5) . . ? O2 C5 C8 111.9(5) . . ? C7 C5 C8 109.5(5) . . ? C6 C5 C8 107.4(5) . . ? F12 C6 F11 107.2(6) . . ? F12 C6 F10 107.2(6) . . ? F11 C6 F10 108.4(5) . . ? F12 C6 C5 110.7(5) . . ? F11 C6 C5 112.8(6) . . ? F10 C6 C5 110.4(6) . . ? F14 C7 F13 108.1(5) . . ? F14 C7 F15 106.7(5) . . ? F13 C7 F15 106.2(5) . . ? F14 C7 C5 111.6(5) . . ? F13 C7 C5 111.4(5) . . ? F15 C7 C5 112.6(5) . . ? F16 C8 F18 109.5(6) . . ? F16 C8 F17 107.7(5) . . ? F18 C8 F17 107.4(5) . . ? F16 C8 C5 112.2(5) . . ? F18 C8 C5 111.4(5) . . ? F17 C8 C5 108.5(5) . . ? O3 C9 C10 110.9(5) . . ? O3 C9 C12 112.2(5) . . ? C10 C9 C12 109.3(5) . . ? O3 C9 C11 107.3(5) . . ? C10 C9 C11 108.9(5) . . ? C12 C9 C11 108.1(5) . . ? F19 C10 F20 108.4(5) . . ? F19 C10 F21 107.4(5) . . ? F20 C10 F21 106.3(5) . . ? F19 C10 C9 111.3(5) . . ? F20 C10 C9 113.2(5) . . ? F21 C10 C9 110.0(5) . . ? F24 C11 F22 108.4(5) . . ? F24 C11 F23 109.4(5) . . ? F22 C11 F23 107.7(5) . . ? F24 C11 C9 110.6(5) . . ? F22 C11 C9 109.1(5) . . ? F23 C11 C9 111.6(5) . . ? F25 C12 F26 108.3(5) . . ? F25 C12 F27 108.0(5) . . ? F26 C12 F27 106.1(5) . . ? F25 C12 C9 113.1(5) . . ? F26 C12 C9 111.2(5) . . ? F27 C12 C9 109.7(5) . . ? O4 C13 C16 109.9(5) . . ? O4 C13 C14 111.6(5) . . ? C16 C13 C14 108.2(5) . . ? O4 C13 C15 108.6(5) . . ? C16 C13 C15 109.1(5) . . ? C14 C13 C15 109.4(5) . . ? F29 C14 F28 107.8(5) . . ? F29 C14 F30 108.3(5) . . ? F28 C14 F30 107.4(5) . . ? F29 C14 C13 110.6(5) . . ? F28 C14 C13 109.7(5) . . ? F30 C14 C13 112.8(5) . . ? F33 C15 F31 108.4(5) . . ? F33 C15 F32 108.6(5) . . ? F31 C15 F32 107.0(5) . . ? F33 C15 C13 112.5(5) . . ? F31 C15 C13 110.2(5) . . ? F32 C15 C13 110.1(5) . . ? F35 C16 F36 107.7(5) . . ? F35 C16 F34 107.8(5) . . ? F36 C16 F34 107.6(5) . . ? F35 C16 C13 113.6(5) . . ? F36 C16 C13 110.5(5) . . ? F34 C16 C13 109.3(5) . . ? O7 Al2 O5 111.7(2) . . ? O7 Al2 O8 108.0(2) . . ? O5 Al2 O8 107.3(2) . . ? O7 Al2 O6 109.1(2) . . ? O5 Al2 O6 107.5(2) . . ? O8 Al2 O6 113.2(2) . . ? C17 O5 Al2 147.2(4) . . ? C21 O6 Al2 147.1(4) . . ? C29 O7 Al2 148.0(4) . . ? C25 O8 Al2 147.2(4) . . ? O5 C17 C20 111.3(5) . . ? O5 C17 C19 110.3(5) . . ? C20 C17 C19 110.1(5) . . ? O5 C17 C18 106.7(5) . . ? C20 C17 C18 109.0(5) . . ? C19 C17 C18 109.4(5) . . ? F38 C18 F37 108.2(5) . . ? F38 C18 F39 106.8(5) . . ? F37 C18 F39 107.0(5) . . ? F38 C18 C17 111.4(5) . . ? F37 C18 C17 111.9(5) . . ? F39 C18 C17 111.2(5) . . ? F42 C19 F40 108.6(5) . . ? F42 C19 F41 107.0(5) . . ? F40 C19 F41 107.6(5) . . ? F42 C19 C17 110.4(5) . . ? F40 C19 C17 111.4(5) . . ? F41 C19 C17 111.7(5) . . ? F44 C20 F45 107.7(6) . . ? F44 C20 F43 106.7(5) . . ? F45 C20 F43 107.8(5) . . ? F44 C20 C17 110.3(5) . . ? F45 C20 C17 111.6(6) . . ? F43 C20 C17 112.4(6) . . ? O6 C21 C24 112.4(5) . . ? O6 C21 C23 108.5(5) . . ? C24 C21 C23 109.0(5) . . ? O6 C21 C22 109.9(5) . . ? C24 C21 C22 108.5(5) . . ? C23 C21 C22 108.4(5) . . ? F47 C22 F48 108.4(5) . . ? F47 C22 F46 107.0(5) . . ? F48 C22 F46 107.5(5) . . ? F47 C22 C21 110.4(5) . . ? F48 C22 C21 112.5(5) . . ? F46 C22 C21 110.8(5) . . ? F49 C23 F50 109.0(5) . . ? F49 C23 F51 108.2(5) . . ? F50 C23 F51 106.9(5) . . ? F49 C23 C21 110.7(5) . . ? F50 C23 C21 112.5(5) . . ? F51 C23 C21 109.3(5) . . ? F52 C24 F53 107.7(5) . . ? F52 C24 F54 107.4(5) . . ? F53 C24 F54 106.2(5) . . ? F52 C24 C21 114.6(5) . . ? F53 C24 C21 110.3(5) . . ? F54 C24 C21 110.3(5) . . ? O8 C25 C27 111.0(5) . . ? O8 C25 C28 108.0(5) . . ? C27 C25 C28 109.8(5) . . ? O8 C25 C26 110.9(5) . . ? C27 C25 C26 108.5(5) . . ? C28 C25 C26 108.6(5) . . ? F65 C26 F64 108.8(6) . . ? F65 C26 F66 107.2(6) . . ? F64 C26 F66 106.7(5) . . ? F65 C26 C25 113.1(5) . . ? F64 C26 C25 111.4(6) . . ? F66 C26 C25 109.4(5) . . ? F69 C27 F67 108.3(5) . . ? F69 C27 F68 107.0(5) . . ? F67 C27 F68 106.9(5) . . ? F69 C27 C25 110.5(5) . . ? F67 C27 C25 111.5(5) . . ? F68 C27 C25 112.4(5) . . ? F70 C28 F71 108.5(5) . . ? F70 C28 F72 107.9(5) . . ? F71 C28 F72 107.5(5) . . ? F70 C28 C25 110.5(5) . . ? F71 C28 C25 110.8(5) . . ? F72 C28 C25 111.4(5) . . ? O7 C29 C30 111.5(5) . . ? O7 C29 C32 108.1(5) . . ? C30 C29 C32 109.4(6) . . ? O7 C29 C31 111.7(5) . . ? C30 C29 C31 108.3(6) . . ? C32 C29 C31 107.7(6) . . ? F55 C30 F57 107.7(7) . . ? F55 C30 F56 106.3(6) . . ? F57 C30 F56 106.6(6) . . ? F55 C30 C29 112.2(6) . . ? F57 C30 C29 114.3(6) . . ? F56 C30 C29 109.2(6) . . ? F58 C31 F60 111.2(7) . . ? F58 C31 F59 105.5(6) . . ? F60 C31 F59 106.5(6) . . ? F58 C31 C29 110.8(6) . . ? F60 C31 C29 114.3(6) . . ? F59 C31 C29 108.0(6) . . ? F63 C32 F61 107.2(7) . . ? F63 C32 F62 107.6(6) . . ? F61 C32 F62 106.4(6) . . ? F63 C32 C29 112.6(6) . . ? F61 C32 C29 111.1(6) . . ? F62 C32 C29 111.6(6) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.04 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.760 _refine_diff_density_min -0.563 _refine_diff_density_rms 0.111