# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_gm072_0m _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C44 H21 Al F27 N' _chemical_formula_weight 1103.60 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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Al Al 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 16.2527(9) _cell_length_b 15.8456(9) _cell_length_c 17.1208(8) _cell_angle_alpha 90.00 _cell_angle_beta 106.582(2) _cell_angle_gamma 90.00 _cell_volume 4225.8(4) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.735 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2192 _exptl_absorpt_coefficient_mu 0.204 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6803 _exptl_absorpt_correction_T_max 0.7457 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 41852 _diffrn_reflns_av_R_equivalents 0.0458 _diffrn_reflns_av_sigmaI/netI 0.0545 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.79 _diffrn_reflns_theta_max 28.38 _reflns_number_total 10516 _reflns_number_gt 6295 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10516 _refine_ls_number_parameters 671 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0972 _refine_ls_R_factor_gt 0.0451 _refine_ls_wR_factor_ref 0.1556 _refine_ls_wR_factor_gt 0.1221 _refine_ls_goodness_of_fit_ref 0.901 _refine_ls_restrained_S_all 0.901 _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 Al1 Al 0.95509(4) 0.84705(4) 0.24855(4) 0.02328(16) Uani 1 1 d . . . C1 C 0.90174(14) 0.87447(14) 0.33884(13) 0.0248(5) Uani 1 1 d . . . C2 C 0.84792(14) 0.81717(14) 0.36448(13) 0.0255(5) Uani 1 1 d . . . C3 C 0.81516(17) 0.83650(16) 0.42801(15) 0.0341(6) Uani 1 1 d . . . C4 C 0.83446(18) 0.91179(16) 0.46998(14) 0.0369(6) Uani 1 1 d . . . C5 C 0.88599(16) 0.96874(14) 0.44728(13) 0.0302(5) Uani 1 1 d . . . C6 C 0.91788(14) 0.94909(14) 0.38244(13) 0.0265(5) Uani 1 1 d . . . C7 C 0.82782(15) 0.73278(14) 0.32412(13) 0.0264(5) Uani 1 1 d . . . C8 C 0.76882(15) 0.72284(16) 0.24905(14) 0.0315(5) Uani 1 1 d . . . C9 C 0.75422(16) 0.64599(17) 0.20939(15) 0.0372(6) Uani 1 1 d . . . C10 C 0.80138(17) 0.57696(16) 0.24470(16) 0.0378(6) Uani 1 1 d . . . C11 C 0.86070(17) 0.58423(16) 0.31930(16) 0.0372(6) Uani 1 1 d . . . C12 C 0.87192(15) 0.66111(15) 0.35850(14) 0.0308(5) Uani 1 1 d . . . C13 C 0.89372(14) 0.90471(13) 0.14180(14) 0.0245(5) Uani 1 1 d . . . C14 C 0.85016(15) 0.98043(14) 0.13636(14) 0.0286(5) Uani 1 1 d . . . C15 C 0.81024(15) 1.02137(14) 0.06424(15) 0.0303(5) Uani 1 1 d . . . C16 C 0.81442(15) 0.98719(15) -0.00801(14) 0.0290(5) Uani 1 1 d . . . C17 C 0.85648(15) 0.91184(15) -0.00638(14) 0.0295(5) Uani 1 1 d . . . C18 C 0.89536(14) 0.87058(13) 0.06599(13) 0.0247(5) Uani 1 1 d . . . C19 C 0.93768(15) 0.78817(14) 0.06162(13) 0.0268(5) Uani 1 1 d . . . C20 C 0.89424(17) 0.71329(16) 0.06018(15) 0.0369(6) Uani 1 1 d . . . C21 C 0.9312(2) 0.63607(16) 0.05681(18) 0.0493(8) Uani 1 1 d . . . C22 C 1.0141(2) 0.63279(18) 0.05472(17) 0.0518(8) Uani 1 1 d . . . C23 C 1.05994(18) 0.7052(2) 0.05574(16) 0.0469(7) Uani 1 1 d . . . C24 C 1.02187(16) 0.78209(16) 0.06021(15) 0.0345(6) Uani 1 1 d . . . C25 C 0.46129(17) 0.72092(15) 0.31686(15) 0.0337(5) Uani 1 1 d . . . H25A H 0.4438 0.7622 0.3525 0.040 Uiso 1 1 calc R . . H25B H 0.4138 0.6799 0.2980 0.040 Uiso 1 1 calc R . . C26 C 0.53944(19) 0.67457(17) 0.36679(17) 0.0457(7) Uani 1 1 d . . . H26A H 0.5632 0.6403 0.3308 0.069 Uiso 1 1 calc R . . H26B H 0.5234 0.6379 0.4062 0.069 Uiso 1 1 calc R . . H26C H 0.5826 0.7154 0.3960 0.069 Uiso 1 1 calc R . . C27 C 0.5503(2) 0.82485(19) 0.26790(18) 0.0507(8) Uani 1 1 d . . . H27A H 0.6024 0.7892 0.2853 0.061 Uiso 1 1 calc R . . H27B H 0.5536 0.8569 0.2192 0.061 Uiso 1 1 calc R . . C28 C 0.5524(2) 0.88706(18) 0.33512(19) 0.0549(8) Uani 1 1 d . . . H28A H 0.5018 0.9236 0.3187 0.082 Uiso 1 1 calc R . . H28B H 0.6045 0.9215 0.3455 0.082 Uiso 1 1 calc R . . H28C H 0.5524 0.8564 0.3848 0.082 Uiso 1 1 calc R . . C29 C 0.48541(19) 0.70124(17) 0.18265(15) 0.0417(6) Uani 1 1 d . . . H29A H 0.5390 0.6698 0.2082 0.050 Uiso 1 1 calc R . . H29B H 0.4373 0.6605 0.1723 0.050 Uiso 1 1 calc R . . C30 C 0.4903(3) 0.7359(2) 0.10199(19) 0.0670(10) Uani 1 1 d . . . H30A H 0.4368 0.7654 0.0750 0.100 Uiso 1 1 calc R . . H30B H 0.4987 0.6893 0.0673 0.100 Uiso 1 1 calc R . . H30C H 0.5386 0.7753 0.1112 0.100 Uiso 1 1 calc R . . C31 C 0.39378(19) 0.82058(16) 0.20637(18) 0.0465(7) Uani 1 1 d . . . H31A H 0.3867 0.8605 0.2485 0.056 Uiso 1 1 calc R . . H31B H 0.4040 0.8545 0.1615 0.056 Uiso 1 1 calc R . . C32 C 1.08030(14) 0.88086(13) 0.28348(13) 0.0244(5) Uani 1 1 d . . . C33 C 1.14667(14) 0.82658(13) 0.32663(13) 0.0232(5) Uani 1 1 d . . . C34 C 1.23087(15) 0.85208(15) 0.34737(14) 0.0296(5) Uani 1 1 d . . . C35 C 1.25394(15) 0.93150(16) 0.32788(15) 0.0342(6) Uani 1 1 d . . . C36 C 1.19139(16) 0.98605(14) 0.28700(15) 0.0315(5) Uani 1 1 d . . . C37 C 1.10719(15) 0.95924(14) 0.26567(15) 0.0293(5) Uani 1 1 d . . . C38 C 1.13028(14) 0.73971(13) 0.35361(13) 0.0242(5) Uani 1 1 d . . . C39 C 1.12546(16) 0.72428(14) 0.43157(14) 0.0306(5) Uani 1 1 d . . . C40 C 1.11642(18) 0.64395(16) 0.45922(15) 0.0369(6) Uani 1 1 d . . . C41 C 1.10929(16) 0.57670(14) 0.40757(16) 0.0341(6) Uani 1 1 d . . . C42 C 1.12491(15) 0.67003(14) 0.30399(14) 0.0293(5) Uani 1 1 d . . . C43 C 1.11361(17) 0.58965(15) 0.32944(15) 0.0346(6) Uani 1 1 d . . . C44 C 0.31112(19) 0.77294(19) 0.1737(2) 0.0580(9) Uani 1 1 d . . . H44A H 0.3166 0.7337 0.1312 0.087 Uiso 1 1 calc R . . H44B H 0.2644 0.8128 0.1506 0.087 Uiso 1 1 calc R . . H44C H 0.2984 0.7412 0.2180 0.087 Uiso 1 1 calc R . . F1 F 0.96822(9) 1.00889(8) 0.36228(8) 0.0351(3) Uani 1 1 d . . . F2 F 0.90594(10) 1.04162(8) 0.48766(8) 0.0403(4) Uani 1 1 d . . . F3 F 0.80312(13) 0.92839(11) 0.53321(10) 0.0602(5) Uani 1 1 d . . . F4 F 0.76375(12) 0.78091(10) 0.45184(10) 0.0551(5) Uani 1 1 d . . . F5 F 0.92960(10) 0.66603(9) 0.43207(9) 0.0459(4) Uani 1 1 d . . . F6 F 0.90592(12) 0.51614(10) 0.35409(11) 0.0593(5) Uani 1 1 d . . . F7 F 0.78829(11) 0.50184(10) 0.20717(10) 0.0550(5) Uani 1 1 d . . . F8 F 0.69386(11) 0.63805(11) 0.13820(9) 0.0559(5) Uani 1 1 d . . . F9 F 0.72359(10) 0.79000(10) 0.21200(9) 0.0483(4) Uani 1 1 d . . . F10 F 0.84585(10) 1.02025(9) 0.20529(8) 0.0406(4) Uani 1 1 d . . . F11 F 0.76938(10) 1.09535(9) 0.06396(9) 0.0436(4) Uani 1 1 d . . . F12 F 0.77775(9) 1.02660(9) -0.07895(8) 0.0408(4) Uani 1 1 d . . . F13 F 0.85912(11) 0.87838(9) -0.07850(8) 0.0443(4) Uani 1 1 d . . . F14 F 1.06837(10) 0.85285(11) 0.06345(10) 0.0505(4) Uani 1 1 d . . . F15 F 1.14146(11) 0.70143(14) 0.05394(11) 0.0724(6) Uani 1 1 d . . . F16 F 1.05215(16) 0.55850(13) 0.05155(13) 0.0923(8) Uani 1 1 d . . . F17 F 0.88670(16) 0.56473(11) 0.05662(13) 0.0826(7) Uani 1 1 d . . . F18 F 0.81227(11) 0.71541(10) 0.06248(11) 0.0538(4) Uani 1 1 d . . . F19 F 1.04877(9) 1.01709(8) 0.22514(10) 0.0421(4) Uani 1 1 d . . . F20 F 1.21216(10) 1.06447(9) 0.26825(10) 0.0477(4) Uani 1 1 d . . . F21 F 1.33715(9) 0.95449(10) 0.34976(10) 0.0510(4) Uani 1 1 d . . . F22 F 1.29461(9) 0.79931(9) 0.38630(10) 0.0441(4) Uani 1 1 d . . . F23 F 1.13212(11) 0.67990(9) 0.22834(8) 0.0474(4) Uani 1 1 d . . . F24 F 1.10713(13) 0.52372(9) 0.27924(10) 0.0593(5) Uani 1 1 d . . . F25 F 1.09892(11) 0.49824(9) 0.43320(10) 0.0510(4) Uani 1 1 d . . . F26 F 1.11362(14) 0.63133(10) 0.53569(10) 0.0615(5) Uani 1 1 d . . . F27 F 1.12955(12) 0.78899(9) 0.48262(9) 0.0527(4) Uani 1 1 d . . . H2 H 0.9521(15) 0.7546(14) 0.2345(13) 0.028(6) Uani 1 1 d . . . N1 N 0.47277(13) 0.76740(12) 0.24305(12) 0.0321(5) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Al1 0.0246(3) 0.0184(3) 0.0277(4) -0.0007(3) 0.0089(3) -0.0001(3) C1 0.0259(12) 0.0222(11) 0.0245(11) 0.0004(8) 0.0042(9) 0.0003(9) C2 0.0280(12) 0.0240(12) 0.0236(11) -0.0004(9) 0.0058(9) -0.0013(9) C3 0.0428(15) 0.0327(14) 0.0315(13) 0.0003(10) 0.0180(11) -0.0027(11) C4 0.0541(17) 0.0355(14) 0.0247(12) -0.0011(10) 0.0171(12) 0.0061(12) C5 0.0411(14) 0.0214(12) 0.0229(11) -0.0024(9) 0.0006(10) 0.0071(10) C6 0.0281(12) 0.0217(11) 0.0264(12) 0.0016(9) 0.0026(9) 0.0005(9) C7 0.0283(12) 0.0274(12) 0.0267(12) -0.0021(9) 0.0129(10) -0.0073(9) C8 0.0282(13) 0.0342(14) 0.0323(13) 0.0013(10) 0.0089(10) -0.0070(10) C9 0.0322(14) 0.0483(16) 0.0296(13) -0.0093(11) 0.0066(11) -0.0176(12) C10 0.0387(15) 0.0343(15) 0.0460(15) -0.0183(12) 0.0214(13) -0.0172(11) C11 0.0368(14) 0.0284(14) 0.0479(16) -0.0034(11) 0.0145(12) -0.0022(11) C12 0.0319(13) 0.0297(13) 0.0302(13) -0.0025(10) 0.0079(10) -0.0071(10) C13 0.0228(11) 0.0206(11) 0.0313(12) 0.0009(9) 0.0098(9) -0.0015(9) C14 0.0299(13) 0.0265(12) 0.0322(12) -0.0021(9) 0.0136(10) 0.0009(10) C15 0.0283(12) 0.0204(12) 0.0421(14) 0.0010(10) 0.0099(11) 0.0048(9) C16 0.0239(12) 0.0294(13) 0.0309(12) 0.0051(9) 0.0034(10) -0.0008(9) C17 0.0334(13) 0.0288(13) 0.0262(12) -0.0030(9) 0.0084(10) -0.0019(10) C18 0.0230(11) 0.0207(11) 0.0309(12) -0.0002(9) 0.0085(9) -0.0011(8) C19 0.0324(13) 0.0256(12) 0.0222(11) -0.0021(9) 0.0076(9) 0.0030(9) C20 0.0473(16) 0.0293(14) 0.0376(14) -0.0045(10) 0.0179(12) 0.0011(11) C21 0.078(2) 0.0257(15) 0.0437(16) -0.0037(11) 0.0162(15) 0.0038(14) C22 0.072(2) 0.0384(17) 0.0358(15) -0.0069(12) 0.0012(14) 0.0312(15) C23 0.0373(16) 0.063(2) 0.0342(15) -0.0124(13) 0.0010(12) 0.0226(14) C24 0.0308(13) 0.0403(15) 0.0296(13) -0.0075(10) 0.0043(10) 0.0030(11) C25 0.0420(15) 0.0274(13) 0.0345(13) -0.0007(10) 0.0158(11) -0.0021(10) C26 0.0551(18) 0.0338(15) 0.0410(15) 0.0017(11) 0.0022(13) 0.0058(13) C27 0.0537(19) 0.0497(18) 0.0511(17) -0.0020(14) 0.0189(14) -0.0230(14) C28 0.060(2) 0.0384(16) 0.060(2) -0.0079(14) 0.0078(16) -0.0167(14) C29 0.0528(17) 0.0414(16) 0.0347(14) -0.0051(11) 0.0187(13) -0.0009(13) C30 0.090(3) 0.076(2) 0.0453(19) -0.0081(16) 0.0358(18) -0.024(2) C31 0.0602(19) 0.0223(13) 0.0502(17) 0.0031(11) 0.0048(14) 0.0039(12) C32 0.0276(12) 0.0179(11) 0.0289(12) -0.0023(8) 0.0103(9) -0.0004(9) C33 0.0264(11) 0.0201(11) 0.0253(11) -0.0027(8) 0.0112(9) 0.0015(9) C34 0.0252(12) 0.0296(13) 0.0334(13) 0.0012(10) 0.0073(10) 0.0050(10) C35 0.0267(13) 0.0352(14) 0.0417(15) -0.0035(11) 0.0114(11) -0.0061(10) C36 0.0360(14) 0.0203(12) 0.0404(14) -0.0018(10) 0.0144(11) -0.0065(10) C37 0.0302(13) 0.0204(12) 0.0372(13) 0.0005(9) 0.0092(10) 0.0028(9) C38 0.0244(11) 0.0208(11) 0.0281(12) 0.0000(9) 0.0085(9) 0.0030(9) C39 0.0396(14) 0.0232(12) 0.0319(13) -0.0066(9) 0.0150(11) 0.0025(10) C40 0.0490(16) 0.0328(14) 0.0349(14) 0.0074(10) 0.0216(12) 0.0073(11) C41 0.0355(14) 0.0186(12) 0.0490(15) 0.0077(10) 0.0131(12) 0.0029(10) C42 0.0354(13) 0.0259(12) 0.0250(12) -0.0007(9) 0.0064(10) 0.0023(10) C43 0.0418(15) 0.0233(12) 0.0375(14) -0.0061(10) 0.0092(11) 0.0020(10) C44 0.0464(18) 0.0459(19) 0.068(2) -0.0049(15) -0.0050(15) 0.0097(14) F1 0.0414(8) 0.0221(7) 0.0413(8) -0.0015(6) 0.0108(6) -0.0064(6) F2 0.0577(10) 0.0267(8) 0.0306(8) -0.0080(6) 0.0031(7) 0.0070(7) F3 0.0995(15) 0.0528(11) 0.0443(10) -0.0130(8) 0.0461(10) -0.0013(10) F4 0.0766(12) 0.0490(10) 0.0586(10) -0.0086(8) 0.0498(9) -0.0194(9) F5 0.0513(10) 0.0367(9) 0.0384(9) -0.0003(7) -0.0052(7) 0.0007(7) F6 0.0655(12) 0.0285(9) 0.0758(12) -0.0041(8) 0.0071(9) 0.0053(8) F7 0.0593(11) 0.0420(10) 0.0679(11) -0.0294(8) 0.0246(9) -0.0190(8) F8 0.0547(10) 0.0644(12) 0.0383(9) -0.0102(8) -0.0036(8) -0.0254(8) F9 0.0456(9) 0.0452(10) 0.0435(9) 0.0065(7) -0.0042(7) -0.0027(7) F10 0.0558(10) 0.0332(8) 0.0373(8) -0.0019(6) 0.0204(7) 0.0164(7) F11 0.0476(9) 0.0310(8) 0.0519(9) 0.0057(7) 0.0137(7) 0.0184(7) F12 0.0436(9) 0.0380(8) 0.0341(8) 0.0111(6) 0.0004(7) 0.0052(7) F13 0.0628(11) 0.0392(9) 0.0279(8) -0.0027(6) 0.0082(7) 0.0081(7) F14 0.0320(8) 0.0618(11) 0.0586(10) -0.0162(8) 0.0143(7) -0.0089(7) F15 0.0391(10) 0.1041(16) 0.0674(12) -0.0267(11) 0.0047(9) 0.0337(10) F16 0.124(2) 0.0583(13) 0.0790(14) -0.0126(10) 0.0044(13) 0.0581(13) F17 0.134(2) 0.0250(10) 0.0974(16) -0.0096(9) 0.0465(14) -0.0111(11) F18 0.0557(11) 0.0418(10) 0.0750(12) -0.0120(8) 0.0363(9) -0.0157(8) F19 0.0342(8) 0.0216(7) 0.0677(10) 0.0124(7) 0.0099(7) 0.0036(6) F20 0.0450(9) 0.0260(8) 0.0731(11) 0.0054(7) 0.0187(8) -0.0124(7) F21 0.0285(8) 0.0518(10) 0.0691(11) 0.0042(8) 0.0083(8) -0.0121(7) F22 0.0255(8) 0.0441(9) 0.0583(10) 0.0139(7) 0.0048(7) 0.0069(6) F23 0.0821(12) 0.0348(9) 0.0272(8) -0.0040(6) 0.0185(8) 0.0012(8) F24 0.0996(15) 0.0240(8) 0.0541(10) -0.0153(7) 0.0216(10) -0.0078(8) F25 0.0645(11) 0.0232(8) 0.0712(11) 0.0137(7) 0.0289(9) 0.0022(7) F26 0.1079(15) 0.0450(10) 0.0463(10) 0.0130(7) 0.0459(10) 0.0091(9) F27 0.0958(13) 0.0323(9) 0.0399(9) -0.0099(7) 0.0356(9) -0.0006(8) H2 0.040(17) 0.018(14) 0.025(15) -0.004(11) 0.010(12) 0.006(12) N1 0.0395(12) 0.0255(11) 0.0322(11) 0.0013(8) 0.0116(9) -0.0042(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Al1 C32 2.023(2) . ? Al1 C1 2.024(2) . ? Al1 C13 2.032(2) . ? C1 C6 1.383(3) . ? C1 C2 1.415(3) . ? C2 C3 1.375(3) . ? C2 C7 1.498(3) . ? C3 F4 1.355(3) . ? C3 C4 1.382(3) . ? C4 F3 1.347(3) . ? C4 C5 1.361(4) . ? C5 F2 1.338(3) . ? C5 C6 1.388(3) . ? C6 F1 1.359(3) . ? C7 C8 1.376(3) . ? C7 C12 1.382(3) . ? C8 F9 1.345(3) . ? C8 C9 1.381(3) . ? C9 F8 1.335(3) . ? C9 C10 1.373(4) . ? C10 F7 1.341(3) . ? C10 C11 1.368(4) . ? C11 F6 1.345(3) . ? C11 C12 1.378(3) . ? C12 F5 1.341(3) . ? C13 C14 1.383(3) . ? C13 C18 1.413(3) . ? C14 F10 1.358(3) . ? C14 C15 1.382(3) . ? C15 F11 1.347(3) . ? C15 C16 1.370(3) . ? C16 F12 1.344(3) . ? C16 C17 1.372(3) . ? C17 F13 1.356(3) . ? C17 C18 1.384(3) . ? C18 C19 1.488(3) . ? C19 C20 1.377(3) . ? C19 C24 1.379(3) . ? C20 F18 1.344(3) . ? C20 C21 1.371(4) . ? C21 F17 1.341(3) . ? C21 C22 1.360(5) . ? C22 F16 1.338(3) . ? C22 C23 1.366(5) . ? C23 F15 1.335(3) . ? C23 C24 1.378(4) . ? C24 F14 1.344(3) . ? C25 C26 1.504(4) . ? C25 N1 1.520(3) . ? C27 C28 1.508(4) . ? C27 N1 1.514(3) . ? C29 C30 1.509(4) . ? C29 N1 1.527(3) . ? C31 C44 1.503(4) . ? C31 N1 1.514(3) . ? C32 C37 1.379(3) . ? C32 C33 1.412(3) . ? C33 C34 1.373(3) . ? C33 C38 1.500(3) . ? C34 F22 1.350(3) . ? C34 C35 1.381(3) . ? C35 F21 1.346(3) . ? C35 C36 1.365(3) . ? C36 F20 1.350(3) . ? C36 C37 1.379(3) . ? C37 F19 1.359(3) . ? C38 C42 1.381(3) . ? C38 C39 1.381(3) . ? C39 F27 1.337(3) . ? C39 C40 1.380(3) . ? C40 F26 1.338(3) . ? C40 C41 1.368(4) . ? C41 F25 1.345(3) . ? C41 C43 1.375(4) . ? C42 F23 1.343(3) . ? C42 C43 1.375(3) . ? C43 F24 1.338(3) . ? 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 C32 Al1 C1 109.36(9) . . ? C32 Al1 C13 109.94(9) . . ? C1 Al1 C13 112.53(9) . . ? C6 C1 C2 114.8(2) . . ? C6 C1 Al1 122.64(17) . . ? C2 C1 Al1 122.47(16) . . ? C3 C2 C1 121.1(2) . . ? C3 C2 C7 118.8(2) . . ? C1 C2 C7 120.17(19) . . ? F4 C3 C2 120.3(2) . . ? F4 C3 C4 118.2(2) . . ? C2 C3 C4 121.5(2) . . ? F3 C4 C5 120.3(2) . . ? F3 C4 C3 120.3(2) . . ? C5 C4 C3 119.4(2) . . ? F2 C5 C4 120.2(2) . . ? F2 C5 C6 121.1(2) . . ? C4 C5 C6 118.7(2) . . ? F1 C6 C1 119.6(2) . . ? F1 C6 C5 115.84(19) . . ? C1 C6 C5 124.5(2) . . ? C8 C7 C12 116.3(2) . . ? C8 C7 C2 122.4(2) . . ? C12 C7 C2 121.3(2) . . ? F9 C8 C7 119.4(2) . . ? F9 C8 C9 118.1(2) . . ? C7 C8 C9 122.4(2) . . ? F8 C9 C10 120.0(2) . . ? F8 C9 C8 120.7(2) . . ? C10 C9 C8 119.3(2) . . ? F7 C10 C11 119.7(3) . . ? F7 C10 C9 120.3(2) . . ? C11 C10 C9 120.0(2) . . ? F6 C11 C10 119.8(2) . . ? F6 C11 C12 120.9(2) . . ? C10 C11 C12 119.3(2) . . ? F5 C12 C11 118.0(2) . . ? F5 C12 C7 119.4(2) . . ? C11 C12 C7 122.6(2) . . ? C14 C13 C18 114.4(2) . . ? C14 C13 Al1 124.14(17) . . ? C18 C13 Al1 121.39(16) . . ? F10 C14 C15 115.5(2) . . ? F10 C14 C13 119.8(2) . . ? C15 C14 C13 124.6(2) . . ? F11 C15 C16 119.5(2) . . ? F11 C15 C14 121.1(2) . . ? C16 C15 C14 119.3(2) . . ? F12 C16 C15 120.6(2) . . ? F12 C16 C17 120.8(2) . . ? C15 C16 C17 118.6(2) . . ? F13 C17 C16 117.8(2) . . ? F13 C17 C18 120.4(2) . . ? C16 C17 C18 121.8(2) . . ? C17 C18 C13 121.2(2) . . ? C17 C18 C19 118.0(2) . . ? C13 C18 C19 120.81(19) . . ? C20 C19 C24 116.5(2) . . ? C20 C19 C18 121.0(2) . . ? C24 C19 C18 122.5(2) . . ? F18 C20 C21 118.2(2) . . ? F18 C20 C19 119.0(2) . . ? C21 C20 C19 122.8(3) . . ? F17 C21 C22 120.4(3) . . ? F17 C21 C20 120.7(3) . . ? C22 C21 C20 119.0(3) . . ? F16 C22 C21 120.5(3) . . ? F16 C22 C23 118.9(3) . . ? C21 C22 C23 120.6(2) . . ? F15 C23 C22 120.2(3) . . ? F15 C23 C24 120.4(3) . . ? C22 C23 C24 119.5(3) . . ? F14 C24 C23 118.9(2) . . ? F14 C24 C19 119.3(2) . . ? C23 C24 C19 121.8(3) . . ? C26 C25 N1 115.2(2) . . ? C28 C27 N1 116.3(2) . . ? C30 C29 N1 115.0(2) . . ? C44 C31 N1 115.9(2) . . ? C37 C32 C33 114.9(2) . . ? C37 C32 Al1 121.91(17) . . ? C33 C32 Al1 123.17(16) . . ? C34 C33 C32 120.8(2) . . ? C34 C33 C38 116.24(19) . . ? C32 C33 C38 122.9(2) . . ? F22 C34 C33 120.9(2) . . ? F22 C34 C35 117.4(2) . . ? C33 C34 C35 121.7(2) . . ? F21 C35 C36 120.9(2) . . ? F21 C35 C34 120.0(2) . . ? C36 C35 C34 119.1(2) . . ? F20 C36 C35 120.3(2) . . ? F20 C36 C37 121.1(2) . . ? C35 C36 C37 118.6(2) . . ? F19 C37 C36 115.1(2) . . ? F19 C37 C32 120.1(2) . . ? C36 C37 C32 124.9(2) . . ? C42 C38 C39 116.2(2) . . ? C42 C38 C33 122.01(19) . . ? C39 C38 C33 121.63(19) . . ? F27 C39 C40 118.3(2) . . ? F27 C39 C38 119.4(2) . . ? C40 C39 C38 122.4(2) . . ? F26 C40 C41 119.7(2) . . ? F26 C40 C39 120.7(2) . . ? C41 C40 C39 119.6(2) . . ? F25 C41 C40 120.3(2) . . ? F25 C41 C43 120.1(2) . . ? C40 C41 C43 119.6(2) . . ? F23 C42 C43 118.0(2) . . ? F23 C42 C38 119.5(2) . . ? C43 C42 C38 122.4(2) . . ? F24 C43 C41 119.5(2) . . ? F24 C43 C42 120.9(2) . . ? C41 C43 C42 119.7(2) . . ? C27 N1 C31 108.7(2) . . ? C27 N1 C25 110.3(2) . . ? C31 N1 C25 108.9(2) . . ? C27 N1 C29 109.9(2) . . ? C31 N1 C29 111.3(2) . . ? C25 N1 C29 107.61(18) . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 28.38 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.255 _refine_diff_density_min -0.256 _refine_diff_density_rms 0.053 _database_code_depnum_ccdc_archive 'CCDC 947825' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_gm040_0m _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C25 H11 Al F12' _chemical_formula_weight 566.32 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Al Al 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.9703(5) _cell_length_b 10.2507(5) _cell_length_c 12.0527(6) _cell_angle_alpha 90.089(3) _cell_angle_beta 113.851(2) _cell_angle_gamma 96.326(3) _cell_volume 1118.32(10) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.682 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 564 _exptl_absorpt_coefficient_mu 0.204 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6758 _exptl_absorpt_correction_T_max 0.7456 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 17319 _diffrn_reflns_av_R_equivalents 0.0226 _diffrn_reflns_av_sigmaI/netI 0.0247 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.00 _diffrn_reflns_theta_max 27.52 _reflns_number_total 4996 _reflns_number_gt 4061 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4996 _refine_ls_number_parameters 344 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0466 _refine_ls_R_factor_gt 0.0344 _refine_ls_wR_factor_ref 0.1262 _refine_ls_wR_factor_gt 0.1128 _refine_ls_goodness_of_fit_ref 0.957 _refine_ls_restrained_S_all 0.957 _refine_ls_shift/su_max 0.009 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Al1 Al 0.64299(5) 0.26034(4) 0.32602(4) 0.01897(13) Uani 1 1 d . . . C1 C 0.80094(16) 0.18225(14) 0.45923(13) 0.0209(3) Uani 1 1 d . . . C2 C 0.77473(16) 0.06764(15) 0.51274(14) 0.0236(3) Uani 1 1 d . . . C3 C 0.88327(18) 0.01455(16) 0.60752(15) 0.0286(4) Uani 1 1 d . . . C4 C 1.02729(18) 0.07215(16) 0.65407(15) 0.0301(4) Uani 1 1 d . . . H4 H 1.1027 0.0353 0.7185 0.036 Uiso 1 1 calc R . . C5 C 1.05770(17) 0.18587(16) 0.60322(14) 0.0265(3) Uani 1 1 d . . . C6 C 0.94757(16) 0.23839(14) 0.50951(13) 0.0214(3) Uani 1 1 d . . . C7 C 0.70893(16) 0.38083(14) 0.22331(13) 0.0203(3) Uani 1 1 d . . . C8 C 0.81508(17) 0.34393(14) 0.18699(13) 0.0226(3) Uani 1 1 d . . . C9 C 0.86453(17) 0.41528(16) 0.11124(14) 0.0253(3) Uani 1 1 d . . . C10 C 0.80765(18) 0.52957(16) 0.06547(15) 0.0289(4) Uani 1 1 d . . . H10 H 0.8410 0.5796 0.0133 0.035 Uiso 1 1 calc R . . C11 C 0.70085(19) 0.56829(16) 0.09831(16) 0.0296(4) Uani 1 1 d . . . C12 C 0.65334(17) 0.49575(15) 0.17514(14) 0.0241(3) Uani 1 1 d . . . C13 C 0.46979(16) 0.14077(14) 0.21276(13) 0.0212(3) Uani 1 1 d . . . C14 C 0.49130(17) 0.02239(15) 0.17036(14) 0.0246(3) Uani 1 1 d . . . C15 C 0.38207(18) -0.05683(15) 0.07860(15) 0.0275(3) Uani 1 1 d . . . C16 C 0.24147(18) -0.02101(16) 0.02234(15) 0.0290(4) Uani 1 1 d . . . H16 H 0.1652 -0.0750 -0.0409 0.035 Uiso 1 1 calc R . . C17 C 0.21677(17) 0.09624(16) 0.06184(15) 0.0267(3) Uani 1 1 d . . . C18 C 0.32768(17) 0.17305(14) 0.15440(14) 0.0234(3) Uani 1 1 d . . . C19 C 0.55145(17) 0.39462(15) 0.42229(14) 0.0238(3) Uani 1 1 d . . . H19 H 0.4961 0.4113 0.3397 0.029 Uiso 1 1 calc R . . C20 C 0.49801(17) 0.29393(15) 0.47853(14) 0.0253(3) Uani 1 1 d . . . H20 H 0.4054 0.2433 0.4343 0.030 Uiso 1 1 calc R . . C21 C 0.58022(19) 0.26887(16) 0.59793(15) 0.0289(4) Uani 1 1 d . . . H21 H 0.5440 0.2001 0.6350 0.035 Uiso 1 1 calc R . . C22 C 0.7159(2) 0.34300(16) 0.66518(15) 0.0312(4) Uani 1 1 d . . . C23 C 0.76860(18) 0.44353(16) 0.60909(15) 0.0287(4) Uani 1 1 d . . . H23 H 0.8613 0.4940 0.6537 0.034 Uiso 1 1 calc R . . C24 C 0.68721(17) 0.47010(15) 0.48939(14) 0.0251(3) Uani 1 1 d . . . H24 H 0.7233 0.5394 0.4527 0.030 Uiso 1 1 calc R . . C25 C 0.8035(2) 0.3140(2) 0.79466(18) 0.0519(6) Uani 1 1 d . . . H25A H 0.7417 0.3154 0.8404 0.078 Uiso 1 1 calc R . . H25B H 0.8897 0.3805 0.8306 0.078 Uiso 1 1 calc R . . H25C H 0.8366 0.2269 0.7977 0.078 Uiso 1 1 calc R . . F1 F 0.62824(10) -0.01714(10) 0.21919(10) 0.0383(3) Uani 1 1 d . . . F2 F 0.41216(12) -0.17079(10) 0.04330(10) 0.0428(3) Uani 1 1 d . . . F3 F 0.08225(11) 0.13797(10) 0.00721(10) 0.0433(3) Uani 1 1 d . . . F4 F 0.29365(10) 0.28922(9) 0.18567(9) 0.0331(2) Uani 1 1 d . . . F5 F 0.87257(11) 0.22955(9) 0.22588(9) 0.0320(2) Uani 1 1 d . . . F6 F 0.96975(12) 0.37157(10) 0.08190(9) 0.0376(3) Uani 1 1 d . . . F7 F 0.64138(13) 0.67933(11) 0.05579(11) 0.0470(3) Uani 1 1 d . . . F8 F 0.54650(11) 0.54100(10) 0.20175(9) 0.0364(3) Uani 1 1 d . . . F9 F 0.98647(10) 0.35234(9) 0.46712(8) 0.0299(2) Uani 1 1 d . . . F10 F 0.84674(12) -0.09705(10) 0.65409(11) 0.0466(3) Uani 1 1 d . . . F11 F 0.63470(10) 0.00517(9) 0.47188(9) 0.0322(2) Uani 1 1 d . . . F12 F 1.19800(10) 0.24635(10) 0.64468(9) 0.0391(3) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Al1 0.0177(2) 0.0185(2) 0.0204(2) 0.00233(17) 0.00706(18) 0.00361(16) C1 0.0207(7) 0.0200(7) 0.0220(7) 0.0018(5) 0.0083(6) 0.0044(6) C2 0.0185(7) 0.0239(7) 0.0279(8) 0.0037(6) 0.0090(6) 0.0022(6) C3 0.0276(8) 0.0261(8) 0.0329(9) 0.0106(7) 0.0125(7) 0.0057(6) C4 0.0245(8) 0.0335(9) 0.0298(9) 0.0097(7) 0.0067(7) 0.0105(7) C5 0.0165(7) 0.0298(8) 0.0286(8) -0.0001(6) 0.0047(6) 0.0020(6) C6 0.0217(7) 0.0186(7) 0.0231(7) 0.0016(6) 0.0085(6) 0.0022(6) C7 0.0208(7) 0.0205(7) 0.0172(7) 0.0007(5) 0.0055(6) 0.0026(6) C8 0.0246(8) 0.0208(7) 0.0197(7) -0.0003(6) 0.0060(6) 0.0038(6) C9 0.0232(8) 0.0339(8) 0.0217(8) -0.0012(6) 0.0108(6) 0.0077(6) C10 0.0317(9) 0.0331(9) 0.0268(8) 0.0086(7) 0.0166(7) 0.0056(7) C11 0.0320(9) 0.0281(8) 0.0314(9) 0.0123(7) 0.0137(7) 0.0115(7) C12 0.0216(8) 0.0283(8) 0.0251(8) 0.0042(6) 0.0113(6) 0.0062(6) C13 0.0204(7) 0.0236(7) 0.0203(7) 0.0033(6) 0.0088(6) 0.0039(6) C14 0.0189(7) 0.0278(8) 0.0273(8) 0.0008(6) 0.0089(6) 0.0054(6) C15 0.0282(8) 0.0252(8) 0.0307(9) -0.0040(6) 0.0134(7) 0.0041(6) C16 0.0255(8) 0.0288(8) 0.0275(8) -0.0033(6) 0.0067(7) -0.0012(6) C17 0.0170(7) 0.0287(8) 0.0298(9) 0.0049(6) 0.0039(6) 0.0060(6) C18 0.0240(8) 0.0190(7) 0.0268(8) 0.0031(6) 0.0090(6) 0.0059(6) C19 0.0275(8) 0.0249(7) 0.0217(7) -0.0010(6) 0.0121(6) 0.0066(6) C20 0.0228(8) 0.0263(8) 0.0289(8) -0.0037(6) 0.0133(7) 0.0009(6) C21 0.0351(9) 0.0267(8) 0.0282(8) 0.0026(6) 0.0170(7) 0.0002(7) C22 0.0354(9) 0.0328(9) 0.0245(8) 0.0007(7) 0.0114(7) 0.0029(7) C23 0.0278(8) 0.0282(8) 0.0291(8) -0.0043(6) 0.0117(7) -0.0011(6) C24 0.0297(8) 0.0212(7) 0.0295(8) -0.0012(6) 0.0174(7) 0.0026(6) C25 0.0542(13) 0.0597(13) 0.0287(10) 0.0082(9) 0.0064(9) -0.0057(11) F1 0.0219(5) 0.0398(6) 0.0471(6) -0.0113(5) 0.0056(5) 0.0123(4) F2 0.0362(6) 0.0344(6) 0.0534(7) -0.0187(5) 0.0129(5) 0.0074(5) F3 0.0211(5) 0.0401(6) 0.0512(7) -0.0045(5) -0.0047(5) 0.0102(4) F4 0.0270(5) 0.0247(5) 0.0399(6) -0.0041(4) 0.0039(4) 0.0106(4) F5 0.0436(6) 0.0268(5) 0.0336(5) 0.0069(4) 0.0205(5) 0.0176(4) F6 0.0417(6) 0.0476(6) 0.0380(6) 0.0098(5) 0.0276(5) 0.0193(5) F7 0.0584(7) 0.0426(6) 0.0614(7) 0.0348(5) 0.0397(6) 0.0311(5) F8 0.0367(6) 0.0412(6) 0.0461(6) 0.0199(5) 0.0276(5) 0.0223(5) F9 0.0252(5) 0.0242(5) 0.0347(5) 0.0071(4) 0.0078(4) -0.0020(4) F10 0.0356(6) 0.0422(6) 0.0575(7) 0.0320(5) 0.0138(5) 0.0064(5) F11 0.0202(5) 0.0295(5) 0.0416(6) 0.0096(4) 0.0084(4) -0.0018(4) F12 0.0181(5) 0.0422(6) 0.0433(6) 0.0077(5) 0.0001(4) -0.0020(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Al1 C1 1.9838(16) . ? Al1 C13 1.9924(16) . ? Al1 C7 1.9936(14) . ? Al1 C19 2.2809(15) . ? C1 C6 1.390(2) . ? C1 C2 1.3912(19) . ? C2 F11 1.3593(17) . ? C2 C3 1.380(2) . ? C3 F10 1.3535(17) . ? C3 C4 1.373(2) . ? C4 C5 1.379(2) . ? C5 F12 1.3540(17) . ? C5 C6 1.379(2) . ? C6 F9 1.3558(15) . ? C7 C8 1.385(2) . ? C7 C12 1.385(2) . ? C8 F5 1.3622(17) . ? C8 C9 1.378(2) . ? C9 F6 1.3526(17) . ? C9 C10 1.376(2) . ? C10 C11 1.372(2) . ? C11 F7 1.3470(18) . ? C11 C12 1.383(2) . ? C12 F8 1.3555(17) . ? C13 C18 1.382(2) . ? C13 C14 1.387(2) . ? C14 F1 1.3592(17) . ? C14 C15 1.377(2) . ? C15 F2 1.3470(18) . ? C15 C16 1.380(2) . ? C16 C17 1.375(2) . ? C17 F3 1.3522(18) . ? C17 C18 1.377(2) . ? C18 F4 1.3661(17) . ? C19 C24 1.402(2) . ? C19 C20 1.408(2) . ? C20 C21 1.379(2) . ? C21 C22 1.396(2) . ? C22 C23 1.402(2) . ? C22 C25 1.498(3) . ? C23 C24 1.385(2) . ? 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 C1 Al1 C13 118.37(6) . . ? C1 Al1 C7 116.11(6) . . ? C13 Al1 C7 106.63(6) . . ? C1 Al1 C19 104.64(6) . . ? C13 Al1 C19 105.90(6) . . ? C7 Al1 C19 103.69(6) . . ? C6 C1 C2 113.73(14) . . ? C6 C1 Al1 123.15(10) . . ? C2 C1 Al1 123.11(11) . . ? F11 C2 C3 117.68(12) . . ? F11 C2 C1 118.84(13) . . ? C3 C2 C1 123.47(14) . . ? F10 C3 C4 119.72(14) . . ? F10 C3 C2 119.13(14) . . ? C4 C3 C2 121.14(13) . . ? C3 C4 C5 117.09(15) . . ? F12 C5 C6 119.29(13) . . ? F12 C5 C4 119.71(14) . . ? C6 C5 C4 120.99(14) . . ? F9 C6 C5 117.09(13) . . ? F9 C6 C1 119.33(13) . . ? C5 C6 C1 123.57(13) . . ? C8 C7 C12 114.25(13) . . ? C8 C7 Al1 118.10(10) . . ? C12 C7 Al1 127.48(11) . . ? F5 C8 C9 117.60(13) . . ? F5 C8 C7 118.70(12) . . ? C9 C8 C7 123.69(14) . . ? F6 C9 C10 120.15(13) . . ? F6 C9 C8 119.23(14) . . ? C10 C9 C8 120.63(14) . . ? C11 C10 C9 117.29(14) . . ? F7 C11 C10 119.63(14) . . ? F7 C11 C12 119.14(14) . . ? C10 C11 C12 121.22(14) . . ? F8 C12 C11 117.08(13) . . ? F8 C12 C7 120.00(13) . . ? C11 C12 C7 122.91(14) . . ? C18 C13 C14 113.88(14) . . ? C18 C13 Al1 125.50(11) . . ? C14 C13 Al1 119.73(11) . . ? F1 C14 C15 117.53(14) . . ? F1 C14 C13 118.79(13) . . ? C15 C14 C13 123.66(14) . . ? F2 C15 C14 119.85(14) . . ? F2 C15 C16 119.43(14) . . ? C14 C15 C16 120.72(15) . . ? C17 C16 C15 117.04(15) . . ? F3 C17 C16 119.44(14) . . ? F3 C17 C18 119.52(14) . . ? C16 C17 C18 121.03(14) . . ? F4 C18 C17 116.84(13) . . ? F4 C18 C13 119.46(14) . . ? C17 C18 C13 123.66(14) . . ? C24 C19 C20 119.38(14) . . ? C24 C19 Al1 95.40(10) . . ? C20 C19 Al1 95.89(10) . . ? C21 C20 C19 119.97(14) . . ? C20 C21 C22 121.03(14) . . ? C21 C22 C23 118.89(15) . . ? C21 C22 C25 120.16(15) . . ? C23 C22 C25 120.95(16) . . ? C24 C23 C22 120.77(15) . . ? C23 C24 C19 119.95(13) . . ? _diffrn_measured_fraction_theta_max 0.970 _diffrn_reflns_theta_full 27.52 _diffrn_measured_fraction_theta_full 0.970 _refine_diff_density_max 0.314 _refine_diff_density_min -0.275 _refine_diff_density_rms 0.047 _database_code_depnum_ccdc_archive 'CCDC 947826' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_gm077_0m _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C99 H35 Al2 F54 P' _chemical_formula_weight 2335.20 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' 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' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.4265(18) _cell_length_b 16.935(3) _cell_length_c 21.347(3) _cell_angle_alpha 88.445(6) _cell_angle_beta 86.663(6) _cell_angle_gamma 83.482(6) _cell_volume 4454.6(11) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.741 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2312 _exptl_absorpt_coefficient_mu 0.216 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.9787 _exptl_absorpt_correction_T_max 0.9787 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 84200 _diffrn_reflns_av_R_equivalents 0.0670 _diffrn_reflns_av_sigmaI/netI 0.0936 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.53 _diffrn_reflns_theta_max 28.49 _reflns_number_total 22314 _reflns_number_gt 11191 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^)+(0.1437P)^2^+2.3660P] 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 22314 _refine_ls_number_parameters 1427 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1682 _refine_ls_R_factor_gt 0.0817 _refine_ls_wR_factor_ref 0.2773 _refine_ls_wR_factor_gt 0.2275 _refine_ls_goodness_of_fit_ref 1.045 _refine_ls_restrained_S_all 1.045 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Al1 Al 0.07563(10) 0.23252(7) 0.30749(6) 0.0236(3) Uani 1 1 d . . . Al2 Al 0.16054(9) 0.22849(7) 0.15088(6) 0.0209(3) Uani 1 1 d . . . H1 H 0.139(4) 0.233(3) 0.234(2) 0.041 Uiso 1 1 d . . . P1 P 0.46323(12) 0.68825(9) 0.26485(8) 0.0338(5) Uani 0.862(5) 1 d P . . H2 H 0.4628 0.6424 0.2198 0.500 Uiso 0.862(5) 1 d P . . P1A P 0.4512(7) 0.7123(5) 0.3076(4) 0.028(3) Uani 0.138(5) 1 d P . . H2A H 0.4518 0.7429 0.3445 0.500 Uiso 0.138(5) 1 d P . . F1 F -0.07574(19) 0.26841(15) 0.16192(11) 0.0297(6) Uani 1 1 d . . . F2 F -0.2162(2) 0.39235(17) 0.13093(13) 0.0404(7) Uani 1 1 d . . . F3 F -0.1421(2) 0.52468(17) 0.07800(14) 0.0490(8) Uani 1 1 d . . . F4 F 0.0701(2) 0.52762(16) 0.05089(13) 0.0428(7) Uani 1 1 d . . . F5 F 0.2336(2) 0.50506(16) 0.14526(12) 0.0412(7) Uani 1 1 d . . . F6 F 0.4435(3) 0.51707(19) 0.11326(15) 0.0529(8) Uani 1 1 d . . . F7 F 0.5499(2) 0.4220(2) 0.02557(16) 0.0552(9) Uani 1 1 d . . . F8 F 0.4554(2) 0.02923(17) 0.18530(13) 0.0444(7) Uani 1 1 d . . . F9 F 0.3536(3) -0.11242(19) 0.01907(18) 0.0683(10) Uani 1 1 d . . . F10 F 0.3140(3) 0.0252(2) -0.04874(15) 0.0598(9) Uani 1 1 d . . . F11 F 0.3439(2) 0.16397(17) 0.00164(13) 0.0431(7) Uani 1 1 d . . . F12 F 0.27462(19) 0.34833(14) 0.20804(11) 0.0302(6) Uani 1 1 d . . . F13 F 0.4817(2) 0.37290(17) 0.21747(14) 0.0447(7) Uani 1 1 d . . . F14 F 0.6434(2) 0.26882(18) 0.16853(14) 0.0469(7) Uani 1 1 d . . . F15 F 0.5958(2) 0.13736(17) 0.11306(14) 0.0442(7) Uani 1 1 d . . . F16 F 0.23284(19) 0.07540(14) 0.20841(11) 0.0309(6) Uani 1 1 d . . . F17 F 0.1918(2) -0.07365(16) 0.19777(15) 0.0499(8) Uani 1 1 d . . . F18 F 0.0441(2) -0.10978(16) 0.11742(16) 0.0523(8) Uani 1 1 d . . . F19 F -0.0662(2) 0.00648(18) 0.05131(14) 0.0448(7) Uani 1 1 d . . . F20 F -0.1871(2) 0.14903(18) 0.10676(14) 0.0432(7) Uani 1 1 d . . . F21 F -0.2970(2) 0.26291(19) 0.03622(16) 0.0534(8) Uani 1 1 d . . . F22 F -0.1897(3) 0.33871(19) -0.05664(16) 0.0590(9) Uani 1 1 d . . . F23 F 0.0237(3) 0.29492(19) -0.08408(14) 0.0532(8) Uani 1 1 d . . . F24 F 0.1315(2) 0.17929(18) -0.01523(13) 0.0424(7) Uani 1 1 d . . . F25 F 0.3090(2) 0.18549(17) 0.30743(14) 0.0436(7) Uani 1 1 d . . . F26 F 0.4396(2) 0.06704(19) 0.35705(16) 0.0534(8) Uani 1 1 d . . . F27 F 0.3531(3) -0.0531(2) 0.42115(17) 0.0609(9) Uani 1 1 d . . . F28 F 0.1358(3) -0.05546(17) 0.43138(14) 0.0524(8) Uani 1 1 d . . . F29 F 0.0069(3) -0.04423(18) 0.31453(14) 0.0515(8) Uani 1 1 d . . . F30 F -0.0368(3) 0.15938(18) 0.46164(14) 0.0494(8) Uani 1 1 d . . . F31 F -0.2529(2) 0.1490(2) 0.46974(16) 0.0595(9) Uani 1 1 d . . . F32 F -0.3373(2) 0.0383(2) 0.40324(17) 0.0690(10) Uani 1 1 d . . . F33 F 0.0822(3) 0.2685(2) 0.48874(16) 0.0680(10) Uani 1 1 d . . . F34 F 0.3979(5) 0.1103(3) 0.5392(2) 0.121(2) Uani 1 1 d . . . F35 F 0.0343(2) 0.39265(15) 0.25290(12) 0.0349(6) Uani 1 1 d . . . F36 F 0.0753(3) 0.53941(17) 0.27989(15) 0.0536(8) Uani 1 1 d . . . F37 F 0.1905(3) 0.56216(17) 0.38056(15) 0.0567(9) Uani 1 1 d . . . F38 F 0.2701(3) 0.43578(19) 0.45026(14) 0.0512(8) Uani 1 1 d . . . F39 F -0.3605(2) 0.3264(2) 0.3338(2) 0.0699(11) Uani 1 1 d . . . F40 F -0.4048(2) 0.1904(2) 0.28613(17) 0.0612(9) Uani 1 1 d . . . F41 F -0.2392(2) 0.08563(19) 0.23968(15) 0.0511(8) Uani 1 1 d . . . F42 F -0.1184(3) 0.3079(2) 0.44895(15) 0.0599(9) Uani 1 1 d . . . F43 F -0.0845(3) 0.4476(2) 0.49580(16) 0.0680(10) Uani 1 1 d . . . F44 F -0.1120(3) 0.5826(2) 0.42339(18) 0.0659(10) Uani 1 1 d . . . F45 F -0.1724(3) 0.5744(2) 0.30484(18) 0.0703(10) Uani 1 1 d . . . F46 F -0.2038(3) 0.43392(19) 0.25783(14) 0.0564(8) Uani 1 1 d . . . F47 F -0.0352(2) 0.11402(15) 0.24899(12) 0.0360(6) Uani 1 1 d . . . F48 F 0.5133(3) 0.1864(3) 0.4501(3) 0.1119(18) Uani 1 1 d . . . F49 F 0.1813(5) 0.1501(3) 0.5572(2) 0.1099(17) Uani 1 1 d . . . F50 F 0.2312(2) 0.31000(16) -0.00643(13) 0.0414(7) Uani 1 1 d . . . F51 F 0.4434(2) 0.31865(19) -0.03529(15) 0.0529(8) Uani 1 1 d . . . F52 F 0.4292(3) -0.10936(17) 0.13438(17) 0.0603(9) Uani 1 1 d . . . F53 F -0.2058(3) -0.0592(2) 0.32718(16) 0.0608(9) Uani 1 1 d . . . F54 F 0.4109(3) 0.2987(2) 0.3775(2) 0.0693(10) Uani 1 1 d . . . C1 C 0.1502(4) 0.1337(3) 0.3465(2) 0.0305(10) Uani 1 1 d . . . C2 C 0.2631(4) 0.1283(3) 0.3386(2) 0.0359(11) Uani 1 1 d . . . C3 C 0.3323(4) 0.0669(3) 0.3635(2) 0.0405(12) Uani 1 1 d . . . C4 C 0.2877(4) 0.0050(3) 0.3945(2) 0.0395(12) Uani 1 1 d . . . C5 C 0.1779(4) 0.0075(3) 0.4015(2) 0.0414(12) Uani 1 1 d . . . C6 C 0.1072(4) 0.0687(3) 0.3774(2) 0.0303(10) Uani 1 1 d . . . C7 C -0.0093(4) 0.0598(3) 0.3855(2) 0.0346(11) Uani 1 1 d . . . C8 C -0.0790(4) 0.1070(3) 0.4261(2) 0.0384(11) Uani 1 1 d . . . C9 C -0.1888(4) 0.1009(3) 0.4320(2) 0.0427(12) Uani 1 1 d . . . C10 C -0.2308(4) 0.0454(4) 0.3982(3) 0.0478(14) Uani 1 1 d . . . C11 C -0.1648(4) -0.0050(3) 0.3602(2) 0.0437(13) Uani 1 1 d . . . C12 C -0.0543(4) 0.0033(3) 0.3538(2) 0.0380(11) Uani 1 1 d . . . C13 C -0.0841(4) 0.2339(3) 0.3024(2) 0.0330(10) Uani 1 1 d . . . C14 C -0.1713(4) 0.2883(3) 0.3219(2) 0.0328(10) Uani 1 1 d . . . C15 C -0.2768(4) 0.2722(3) 0.3164(3) 0.0447(13) Uani 1 1 d . . . C16 C -0.3003(4) 0.2032(4) 0.2905(3) 0.0479(14) Uani 1 1 d . . . C17 C -0.2185(4) 0.1519(3) 0.2671(2) 0.0382(11) Uani 1 1 d . . . C18 C -0.1127(4) 0.1669(3) 0.2742(2) 0.0331(10) Uani 1 1 d . . . C19 C -0.1563(4) 0.3666(3) 0.3506(2) 0.0387(11) Uani 1 1 d . . . C20 C -0.1276(4) 0.3731(3) 0.4115(2) 0.0450(13) Uani 1 1 d . . . C21 C -0.1095(5) 0.4440(4) 0.4363(3) 0.0508(14) Uani 1 1 d . . . C22 C -0.1250(5) 0.5124(3) 0.4001(3) 0.0511(14) Uani 1 1 d . . . C23 C -0.1564(4) 0.5081(3) 0.3396(3) 0.0490(14) Uani 1 1 d . . . C24 C -0.1726(4) 0.4361(3) 0.3163(2) 0.0442(13) Uani 1 1 d . . . C25 C 0.1243(4) 0.3339(3) 0.3388(2) 0.0307(10) Uani 1 1 d . . . C26 C 0.0910(4) 0.4022(3) 0.3035(2) 0.0348(11) Uani 1 1 d . . . C27 C 0.1129(4) 0.4767(3) 0.3166(2) 0.0410(12) Uani 1 1 d . . . C28 C 0.1690(4) 0.4885(3) 0.3665(3) 0.0423(12) Uani 1 1 d . . . C29 C 0.2077(4) 0.4243(3) 0.4021(2) 0.0362(11) Uani 1 1 d . . . C30 C 0.1890(3) 0.3468(3) 0.3882(2) 0.0294(10) Uani 1 1 d . . . C31 C 0.2423(4) 0.2836(3) 0.4288(2) 0.0400(12) Uani 1 1 d . . . C33 C 0.4065(6) 0.2048(4) 0.4582(4) 0.071(2) Uani 1 1 d . . . C34 C 0.3504(8) 0.1645(4) 0.5026(4) 0.083(3) Uani 1 1 d . . . C35 C 0.2387(8) 0.1845(4) 0.5127(3) 0.074(2) Uani 1 1 d . . . C36 C 0.1893(5) 0.2451(3) 0.4754(3) 0.0495(14) Uani 1 1 d . . . C37 C 0.0753(3) 0.3269(2) 0.11856(18) 0.0223(8) Uani 1 1 d . . . C38 C -0.0347(3) 0.3310(3) 0.13170(19) 0.0265(9) Uani 1 1 d . . . C39 C -0.1099(3) 0.3951(3) 0.1179(2) 0.0305(10) Uani 1 1 d . . . C40 C -0.0734(4) 0.4608(3) 0.0911(2) 0.0329(11) Uani 1 1 d . . . C41 C 0.0366(4) 0.4623(3) 0.0780(2) 0.0314(10) Uani 1 1 d . . . C42 C 0.1107(3) 0.3967(2) 0.09011(19) 0.0253(9) Uani 1 1 d . . . C43 C 0.2267(3) 0.4043(3) 0.0723(2) 0.0266(9) Uani 1 1 d . . . C44 C 0.2830(4) 0.4580(3) 0.1008(2) 0.0337(11) Uani 1 1 d . . . C45 C 0.3918(4) 0.4643(3) 0.0852(2) 0.0389(12) Uani 1 1 d . . . C46 C 0.4445(4) 0.4161(3) 0.0400(2) 0.0393(12) Uani 1 1 d . . . C47 C 0.3909(4) 0.3638(3) 0.0097(2) 0.0366(11) Uani 1 1 d . . . C48 C 0.2832(4) 0.3599(3) 0.0253(2) 0.0305(10) Uani 1 1 d . . . C49 C 0.1145(3) 0.1231(2) 0.12977(19) 0.0237(9) Uani 1 1 d . . . C50 C 0.1611(3) 0.0610(2) 0.1662(2) 0.0258(9) Uani 1 1 d . . . C51 C 0.1402(4) -0.0164(3) 0.1629(2) 0.0352(11) Uani 1 1 d . . . C52 C 0.0642(4) -0.0350(3) 0.1221(2) 0.0361(11) Uani 1 1 d . . . C53 C 0.0110(3) 0.0253(3) 0.0877(2) 0.0333(11) Uani 1 1 d . . . C54 C 0.0359(3) 0.1029(3) 0.0896(2) 0.0288(10) Uani 1 1 d . . . C55 C -0.0244(3) 0.1635(3) 0.0492(2) 0.0280(9) Uani 1 1 d . . . C56 C -0.1345(3) 0.1845(3) 0.0596(2) 0.0333(11) Uani 1 1 d . . . C57 C -0.1894(4) 0.2418(3) 0.0248(2) 0.0379(11) Uani 1 1 d . . . C58 C -0.1366(4) 0.2808(3) -0.0227(2) 0.0413(12) Uani 1 1 d . . . C59 C -0.0272(4) 0.2602(3) -0.0366(2) 0.0397(12) Uani 1 1 d . . . C60 C 0.0263(4) 0.2011(3) -0.0006(2) 0.0328(10) Uani 1 1 d . . . C61 C 0.3216(3) 0.2316(2) 0.15058(18) 0.0222(8) Uani 1 1 d . . . C62 C 0.3516(3) 0.2950(2) 0.18108(19) 0.0251(9) Uani 1 1 d . . . C63 C 0.4588(4) 0.3091(3) 0.1873(2) 0.0303(10) Uani 1 1 d . . . C64 C 0.5404(3) 0.2565(3) 0.1628(2) 0.0347(11) Uani 1 1 d . . . C65 C 0.5142(3) 0.1908(3) 0.1336(2) 0.0307(10) Uani 1 1 d . . . C66 C 0.4079(3) 0.1772(2) 0.12690(19) 0.0232(9) Uani 1 1 d . . . C67 C 0.3934(3) 0.1018(3) 0.0968(2) 0.0265(9) Uani 1 1 d . . . C68 C 0.4183(3) 0.0299(3) 0.1281(2) 0.0314(10) Uani 1 1 d . . . C69 C 0.4054(4) -0.0412(3) 0.1021(3) 0.0413(12) Uani 1 1 d . . . C70 C 0.3677(4) -0.0427(3) 0.0432(3) 0.0410(12) Uani 1 1 d . . . C71 C 0.3465(4) 0.0266(3) 0.0097(2) 0.0375(11) Uani 1 1 d . . . C72 C 0.3601(3) 0.0979(3) 0.0360(2) 0.0309(10) Uani 1 1 d . . . C73 C 0.5081(4) 0.6155(3) 0.3240(2) 0.0401(12) Uani 1 1 d . . . C74 C 0.5840(4) 0.6275(3) 0.3687(3) 0.0450(13) Uani 1 1 d . . . C75 C 0.6082(4) 0.5659(4) 0.4109(3) 0.0503(14) Uani 1 1 d . . . H75 H 0.6564 0.5732 0.4415 0.060 Uiso 1 1 calc R . . C76 C 0.4921(4) 0.4840(3) 0.3651(2) 0.0421(12) Uani 1 1 d . . . H76 H 0.4630 0.4359 0.3636 0.051 Uiso 1 1 calc R . . C77 C 0.5657(5) 0.4942(3) 0.4108(2) 0.0488(14) Uani 1 1 d . . . C78 C 0.4621(4) 0.5436(3) 0.3222(2) 0.0365(11) Uani 1 1 d . . . C79 C 0.3819(4) 0.5285(3) 0.2749(2) 0.0445(13) Uani 1 1 d . . . H79A H 0.3562 0.4778 0.2839 0.067 Uiso 1 1 calc R . . H79B H 0.4166 0.5285 0.2335 0.067 Uiso 1 1 calc R . . H79C H 0.3219 0.5695 0.2772 0.067 Uiso 1 1 calc R . . C80 C 0.5943(5) 0.4302(4) 0.4586(3) 0.0661(18) Uani 1 1 d . . . H80A H 0.6691 0.4296 0.4678 0.099 Uiso 1 1 calc R . . H80B H 0.5828 0.3797 0.4424 0.099 Uiso 1 1 calc R . . H80C H 0.5493 0.4402 0.4963 0.099 Uiso 1 1 calc R . . C81 C 0.6391(5) 0.7012(4) 0.3723(3) 0.0673(18) Uani 1 1 d . . . H81A H 0.6741 0.7008 0.4113 0.101 Uiso 1 1 calc R . . H81B H 0.5864 0.7471 0.3700 0.101 Uiso 1 1 calc R . . H81C H 0.6924 0.7030 0.3380 0.101 Uiso 1 1 calc R . . C82 C 0.5571(4) 0.7558(3) 0.2395(2) 0.0394(12) Uani 1 1 d . . . C83 C 0.6447(5) 0.7225(3) 0.2009(3) 0.0517(15) Uani 1 1 d . . . C84 C 0.7212(5) 0.7721(4) 0.1789(3) 0.0570(16) Uani 1 1 d . . . H84 H 0.7797 0.7509 0.1532 0.068 Uiso 1 1 calc R . . C85 C 0.7140(5) 0.8493(4) 0.1934(2) 0.0529(15) Uani 1 1 d . . . C86 C 0.6279(4) 0.8805(3) 0.2309(2) 0.0433(12) Uani 1 1 d . . . H86 H 0.6228 0.9340 0.2409 0.052 Uiso 1 1 calc R . . C87 C 0.5485(4) 0.8360(3) 0.2545(2) 0.0384(11) Uani 1 1 d . . . C88 C 0.4557(5) 0.8778(3) 0.2948(3) 0.0539(15) Uani 1 1 d . . . H88A H 0.3900 0.8811 0.2728 0.081 Uiso 1 1 calc R . . H88B H 0.4715 0.9304 0.3037 0.081 Uiso 1 1 calc R . . H88C H 0.4467 0.8483 0.3334 0.081 Uiso 1 1 calc R . . C89 C 0.8002(5) 0.9018(5) 0.1700(3) 0.080(2) Uani 1 1 d . . . H89A H 0.8540 0.9014 0.2006 0.120 Uiso 1 1 calc R . . H89B H 0.7670 0.9552 0.1636 0.120 Uiso 1 1 calc R . . H89C H 0.8340 0.8820 0.1311 0.120 Uiso 1 1 calc R . . C90 C 0.6615(6) 0.6373(4) 0.1822(4) 0.077(2) Uani 1 1 d . . . H90A H 0.6427 0.6041 0.2175 0.116 Uiso 1 1 calc R . . H90B H 0.7361 0.6233 0.1689 0.116 Uiso 1 1 calc R . . H90C H 0.6163 0.6297 0.1484 0.116 Uiso 1 1 calc R . . C91 C 0.3206(4) 0.7249(3) 0.2811(3) 0.0430(13) Uani 1 1 d . . . C92 C 0.2634(5) 0.7345(3) 0.2271(3) 0.0574(17) Uani 1 1 d . . . C93 C 0.3159(7) 0.7301(4) 0.1620(3) 0.091(3) Uani 1 1 d . . . H93A H 0.3323 0.6755 0.1505 0.137 Uiso 1 1 calc R . . H93B H 0.3818 0.7550 0.1608 0.137 Uiso 1 1 calc R . . H93C H 0.2674 0.7571 0.1330 0.137 Uiso 1 1 calc R . . C94 C 0.2689(6) 0.7310(3) 0.3399(3) 0.0623(17) Uani 1 1 d . . . C95 C 0.3288(7) 0.7236(4) 0.3991(3) 0.083(2) Uani 1 1 d . . . H95A H 0.3474 0.6684 0.4095 0.125 Uiso 1 1 calc R . . H95B H 0.2836 0.7484 0.4327 0.125 Uiso 1 1 calc R . . H95C H 0.3938 0.7492 0.3932 0.125 Uiso 1 1 calc R . . C96 C 0.1557(7) 0.7443(4) 0.3417(5) 0.091(3) Uani 1 1 d . . . H96 H 0.1186 0.7501 0.3807 0.109 Uiso 1 1 calc R . . C97 C 0.0970(6) 0.7492(4) 0.2901(7) 0.112(4) Uani 1 1 d . . . C98 C 0.1518(7) 0.7460(4) 0.2333(5) 0.098(3) Uani 1 1 d . . . H98 H 0.1128 0.7517 0.1972 0.117 Uiso 1 1 calc R . . C99 C 0.3544(5) 0.2637(3) 0.4207(3) 0.0517(15) Uani 1 1 d . . . C100 C -0.0250(7) 0.7592(6) 0.2981(9) 0.215(9) Uani 1 1 d . . . H10A H -0.0546 0.7372 0.2628 0.322 Uiso 1 1 calc R . . H10B H -0.0507 0.8147 0.3007 0.322 Uiso 1 1 calc R . . H10C H -0.0473 0.7321 0.3358 0.322 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Al1 0.0217(6) 0.0235(7) 0.0244(6) 0.0016(5) 0.0001(5) 0.0014(5) Al2 0.0182(6) 0.0218(6) 0.0224(6) 0.0016(5) -0.0014(5) -0.0009(5) P1 0.0409(9) 0.0273(8) 0.0332(11) -0.0021(7) -0.0071(6) -0.0014(6) P1A 0.041(5) 0.022(4) 0.021(6) -0.009(4) -0.004(4) -0.007(4) F1 0.0252(13) 0.0319(14) 0.0313(13) 0.0067(11) 0.0016(10) -0.0031(10) F2 0.0205(13) 0.0484(17) 0.0498(17) 0.0025(13) -0.0024(12) 0.0065(12) F3 0.0432(17) 0.0384(17) 0.0603(19) 0.0108(14) -0.0093(14) 0.0178(13) F4 0.0496(17) 0.0281(15) 0.0491(17) 0.0143(13) -0.0050(14) -0.0001(12) F5 0.0510(17) 0.0372(16) 0.0364(15) -0.0041(12) -0.0034(13) -0.0083(13) F6 0.0551(19) 0.055(2) 0.0551(19) 0.0030(15) -0.0140(15) -0.0312(16) F7 0.0301(15) 0.063(2) 0.071(2) 0.0217(17) 0.0035(15) -0.0115(14) F8 0.0512(18) 0.0362(16) 0.0457(17) 0.0044(13) -0.0174(14) 0.0010(13) F9 0.085(3) 0.0405(19) 0.082(2) -0.0311(17) -0.007(2) -0.0115(18) F10 0.066(2) 0.066(2) 0.0493(19) -0.0175(16) -0.0154(16) -0.0076(17) F11 0.0479(17) 0.0436(17) 0.0379(15) 0.0037(13) -0.0083(13) -0.0043(13) F12 0.0320(13) 0.0252(13) 0.0326(14) -0.0057(11) -0.0019(11) 0.0020(10) F13 0.0433(16) 0.0394(16) 0.0557(18) -0.0167(14) -0.0084(14) -0.0165(13) F14 0.0246(14) 0.0573(19) 0.0625(19) -0.0120(15) -0.0034(13) -0.0180(13) F15 0.0195(13) 0.0448(17) 0.068(2) -0.0167(15) 0.0044(13) -0.0011(12) F16 0.0314(13) 0.0282(14) 0.0325(14) 0.0011(11) -0.0072(11) 0.0011(11) F17 0.0528(18) 0.0242(15) 0.072(2) 0.0067(14) -0.0085(16) -0.0010(13) F18 0.0495(18) 0.0267(15) 0.083(2) -0.0123(15) 0.0005(16) -0.0144(13) F19 0.0328(15) 0.0525(18) 0.0537(18) -0.0155(14) -0.0025(13) -0.0208(13) F20 0.0224(13) 0.0521(18) 0.0544(18) 0.0033(14) 0.0057(12) -0.0054(12) F21 0.0255(15) 0.058(2) 0.076(2) -0.0038(17) -0.0151(14) 0.0052(13) F22 0.066(2) 0.0482(19) 0.067(2) 0.0059(16) -0.0371(17) -0.0077(16) F23 0.065(2) 0.053(2) 0.0426(17) 0.0106(15) -0.0032(15) -0.0147(16) F24 0.0296(14) 0.0530(18) 0.0450(16) -0.0033(14) 0.0093(12) -0.0112(13) F25 0.0310(15) 0.0467(18) 0.0530(18) 0.0060(14) -0.0023(13) -0.0058(13) F26 0.0296(15) 0.0502(19) 0.078(2) -0.0004(16) -0.0052(15) 0.0060(13) F27 0.0507(19) 0.052(2) 0.076(2) 0.0107(17) -0.0111(17) 0.0114(15) F28 0.064(2) 0.0374(17) 0.0533(19) 0.0152(14) -0.0015(16) 0.0005(15) F29 0.063(2) 0.0408(17) 0.0522(19) -0.0078(14) -0.0041(16) -0.0096(15) F30 0.0581(19) 0.0437(18) 0.0457(17) -0.0114(14) 0.0012(15) -0.0027(15) F31 0.0372(17) 0.074(2) 0.064(2) -0.0049(18) 0.0100(15) 0.0026(16) F32 0.0304(17) 0.098(3) 0.080(2) 0.007(2) -0.0021(16) -0.0142(17) F33 0.071(2) 0.082(3) 0.056(2) 0.0041(19) 0.0034(18) -0.033(2) F34 0.175(5) 0.069(3) 0.125(4) 0.020(3) -0.101(4) 0.008(3) F35 0.0408(15) 0.0312(14) 0.0321(14) -0.0001(11) -0.0085(12) 0.0019(12) F36 0.065(2) 0.0352(17) 0.0589(19) 0.0073(14) -0.0116(16) 0.0032(15) F37 0.076(2) 0.0313(17) 0.064(2) -0.0057(15) -0.0083(17) -0.0079(15) F38 0.0560(19) 0.0533(19) 0.0490(18) -0.0037(15) -0.0192(15) -0.0174(15) F39 0.0246(16) 0.065(2) 0.117(3) -0.022(2) 0.0040(17) 0.0093(15) F40 0.0299(16) 0.078(2) 0.078(2) 0.0017(19) -0.0101(15) -0.0106(16) F41 0.0457(17) 0.054(2) 0.0571(19) -0.0023(15) -0.0109(15) -0.0174(15) F42 0.074(2) 0.057(2) 0.0473(18) 0.0026(16) -0.0070(17) 0.0025(17) F43 0.085(3) 0.072(2) 0.049(2) -0.0209(17) -0.0202(18) -0.001(2) F44 0.065(2) 0.047(2) 0.085(3) -0.0259(18) -0.0126(19) 0.0055(16) F45 0.076(2) 0.046(2) 0.086(3) 0.0066(18) -0.017(2) 0.0089(18) F46 0.072(2) 0.0501(19) 0.0444(18) -0.0007(14) -0.0174(16) 0.0108(16) F47 0.0352(14) 0.0339(15) 0.0385(15) -0.0086(12) 0.0089(12) -0.0062(12) F48 0.066(3) 0.079(3) 0.189(5) -0.031(3) -0.068(3) 0.033(2) F49 0.180(5) 0.087(3) 0.070(3) 0.035(2) -0.029(3) -0.039(3) F50 0.0422(16) 0.0377(16) 0.0449(16) -0.0099(13) 0.0040(13) -0.0083(13) F51 0.0419(17) 0.0526(19) 0.061(2) -0.0024(16) 0.0147(15) -0.0015(14) F52 0.075(2) 0.0226(15) 0.082(2) 0.0039(15) -0.0123(19) 0.0015(15) F53 0.064(2) 0.060(2) 0.066(2) 0.0039(17) -0.0216(17) -0.0283(17) F54 0.0408(19) 0.053(2) 0.113(3) -0.010(2) 0.009(2) -0.0055(16) C1 0.028(2) 0.033(2) 0.030(2) -0.0051(19) -0.0022(19) 0.0022(19) C2 0.031(2) 0.026(2) 0.051(3) -0.004(2) -0.007(2) -0.002(2) C3 0.025(2) 0.047(3) 0.049(3) -0.006(2) -0.004(2) 0.002(2) C4 0.032(3) 0.032(3) 0.052(3) 0.011(2) -0.009(2) 0.006(2) C5 0.045(3) 0.039(3) 0.038(3) 0.007(2) 0.000(2) 0.002(2) C6 0.040(3) 0.026(2) 0.023(2) 0.0019(18) 0.0000(19) 0.0033(19) C7 0.037(3) 0.029(2) 0.038(3) 0.004(2) -0.002(2) -0.005(2) C8 0.039(3) 0.040(3) 0.036(3) 0.004(2) -0.005(2) -0.003(2) C9 0.040(3) 0.046(3) 0.041(3) 0.003(2) 0.002(2) -0.002(2) C10 0.035(3) 0.064(4) 0.047(3) 0.014(3) -0.005(2) -0.018(3) C11 0.049(3) 0.044(3) 0.042(3) 0.011(2) -0.012(2) -0.017(3) C12 0.038(3) 0.045(3) 0.032(3) 0.005(2) -0.002(2) -0.008(2) C13 0.028(2) 0.038(3) 0.032(2) -0.001(2) 0.0002(19) 0.000(2) C14 0.026(2) 0.035(3) 0.036(3) -0.004(2) -0.0014(19) 0.0020(19) C15 0.025(2) 0.051(3) 0.055(3) -0.005(3) 0.002(2) 0.008(2) C16 0.020(2) 0.069(4) 0.056(3) 0.007(3) -0.004(2) -0.013(2) C17 0.041(3) 0.036(3) 0.040(3) -0.001(2) -0.003(2) -0.015(2) C18 0.032(2) 0.035(3) 0.032(2) 0.006(2) 0.001(2) -0.006(2) C19 0.027(2) 0.045(3) 0.042(3) -0.007(2) 0.001(2) 0.001(2) C20 0.040(3) 0.050(3) 0.041(3) 0.002(3) 0.000(2) 0.011(2) C21 0.052(3) 0.053(4) 0.046(3) -0.017(3) -0.004(3) 0.006(3) C22 0.046(3) 0.042(3) 0.064(4) -0.011(3) -0.006(3) 0.003(3) C23 0.045(3) 0.040(3) 0.060(4) 0.005(3) -0.007(3) 0.005(2) C24 0.042(3) 0.046(3) 0.043(3) -0.007(2) -0.008(2) 0.007(2) C25 0.027(2) 0.030(2) 0.033(2) -0.0009(19) 0.0017(19) 0.0006(19) C26 0.028(2) 0.040(3) 0.035(3) -0.002(2) -0.003(2) 0.002(2) C27 0.055(3) 0.024(2) 0.043(3) 0.003(2) -0.009(2) 0.004(2) C28 0.046(3) 0.028(3) 0.053(3) -0.003(2) -0.003(3) -0.005(2) C29 0.037(3) 0.035(3) 0.038(3) -0.003(2) -0.006(2) -0.008(2) C30 0.024(2) 0.033(2) 0.031(2) -0.0004(19) -0.0007(18) -0.0033(18) C31 0.044(3) 0.036(3) 0.042(3) -0.006(2) -0.014(2) -0.007(2) C33 0.064(4) 0.045(4) 0.106(6) -0.013(4) -0.051(4) 0.012(3) C34 0.119(7) 0.043(4) 0.091(6) -0.002(4) -0.067(5) 0.011(4) C35 0.135(7) 0.048(4) 0.043(4) 0.017(3) -0.033(4) -0.017(4) C36 0.055(4) 0.050(3) 0.047(3) 0.000(3) -0.011(3) -0.012(3) C37 0.022(2) 0.022(2) 0.022(2) -0.0004(16) -0.0022(16) 0.0004(16) C38 0.029(2) 0.026(2) 0.025(2) 0.0014(17) -0.0055(18) 0.0000(18) C39 0.022(2) 0.040(3) 0.028(2) 0.001(2) -0.0038(18) 0.0046(19) C40 0.033(2) 0.031(3) 0.031(2) 0.003(2) -0.009(2) 0.012(2) C41 0.035(2) 0.024(2) 0.035(2) 0.0058(19) -0.005(2) 0.0000(19) C42 0.028(2) 0.025(2) 0.024(2) 0.0020(17) -0.0042(17) -0.0011(17) C43 0.028(2) 0.024(2) 0.029(2) 0.0069(18) -0.0050(18) -0.0055(18) C44 0.046(3) 0.032(3) 0.024(2) 0.0082(19) -0.006(2) -0.009(2) C45 0.043(3) 0.038(3) 0.038(3) 0.014(2) -0.011(2) -0.017(2) C46 0.029(2) 0.044(3) 0.045(3) 0.017(2) -0.002(2) -0.008(2) C47 0.039(3) 0.036(3) 0.032(3) 0.010(2) 0.009(2) 0.001(2) C48 0.035(2) 0.025(2) 0.032(2) 0.0035(19) -0.003(2) -0.0060(19) C49 0.020(2) 0.025(2) 0.026(2) -0.0047(17) 0.0047(16) -0.0037(16) C50 0.022(2) 0.024(2) 0.031(2) -0.0015(18) 0.0018(18) -0.0012(17) C51 0.035(3) 0.028(2) 0.041(3) 0.004(2) 0.004(2) -0.001(2) C52 0.033(3) 0.026(2) 0.050(3) -0.008(2) 0.010(2) -0.011(2) C53 0.022(2) 0.039(3) 0.040(3) -0.009(2) 0.0022(19) -0.011(2) C54 0.018(2) 0.038(3) 0.030(2) -0.0077(19) 0.0056(17) -0.0053(18) C55 0.021(2) 0.033(2) 0.031(2) -0.0050(19) -0.0041(18) -0.0052(18) C56 0.022(2) 0.043(3) 0.035(3) -0.008(2) -0.0048(19) -0.005(2) C57 0.022(2) 0.046(3) 0.047(3) -0.008(2) -0.009(2) -0.008(2) C58 0.050(3) 0.037(3) 0.039(3) -0.003(2) -0.022(2) -0.001(2) C59 0.049(3) 0.044(3) 0.029(3) -0.003(2) -0.006(2) -0.015(2) C60 0.028(2) 0.039(3) 0.033(2) -0.006(2) -0.0005(19) -0.007(2) C61 0.023(2) 0.022(2) 0.021(2) 0.0039(16) -0.0004(16) -0.0029(16) C62 0.026(2) 0.023(2) 0.026(2) 0.0015(17) -0.0035(17) 0.0008(17) C63 0.032(2) 0.027(2) 0.034(2) -0.0016(19) -0.0052(19) -0.0101(19) C64 0.020(2) 0.045(3) 0.041(3) -0.001(2) -0.0036(19) -0.013(2) C65 0.020(2) 0.032(2) 0.040(3) -0.004(2) -0.0007(19) 0.0002(18) C66 0.019(2) 0.024(2) 0.026(2) 0.0014(17) -0.0022(16) 0.0000(16) C67 0.0162(19) 0.029(2) 0.034(2) -0.0029(19) 0.0019(17) -0.0010(17) C68 0.022(2) 0.031(2) 0.041(3) -0.006(2) -0.0018(19) 0.0009(18) C69 0.035(3) 0.027(3) 0.061(3) -0.004(2) 0.000(2) -0.002(2) C70 0.034(3) 0.033(3) 0.057(3) -0.015(2) 0.002(2) -0.004(2) C71 0.028(2) 0.049(3) 0.036(3) -0.015(2) -0.003(2) -0.006(2) C72 0.022(2) 0.033(3) 0.037(3) -0.002(2) -0.0007(19) 0.0006(18) C73 0.042(3) 0.031(3) 0.046(3) -0.002(2) -0.008(2) 0.004(2) C74 0.044(3) 0.041(3) 0.049(3) -0.010(2) -0.009(2) 0.006(2) C75 0.043(3) 0.064(4) 0.042(3) -0.010(3) -0.005(2) 0.005(3) C76 0.041(3) 0.033(3) 0.049(3) -0.004(2) 0.010(2) 0.004(2) C77 0.047(3) 0.053(4) 0.039(3) 0.006(3) 0.007(2) 0.022(3) C78 0.041(3) 0.029(3) 0.038(3) -0.006(2) 0.003(2) 0.003(2) C79 0.053(3) 0.040(3) 0.042(3) 0.000(2) -0.004(2) -0.012(2) C80 0.062(4) 0.070(4) 0.058(4) 0.018(3) 0.002(3) 0.019(3) C81 0.065(4) 0.055(4) 0.086(5) -0.016(3) -0.038(4) -0.006(3) C82 0.038(3) 0.036(3) 0.044(3) -0.002(2) -0.009(2) -0.002(2) C83 0.065(4) 0.047(3) 0.041(3) -0.015(3) -0.014(3) 0.012(3) C84 0.039(3) 0.086(5) 0.043(3) -0.010(3) 0.004(3) 0.003(3) C85 0.052(3) 0.078(5) 0.030(3) 0.005(3) -0.005(2) -0.013(3) C86 0.046(3) 0.050(3) 0.035(3) 0.005(2) -0.003(2) -0.011(3) C87 0.043(3) 0.038(3) 0.035(3) 0.000(2) -0.004(2) -0.003(2) C88 0.056(4) 0.035(3) 0.067(4) -0.003(3) 0.014(3) 0.001(3) C89 0.061(4) 0.126(7) 0.057(4) 0.012(4) 0.008(3) -0.040(4) C90 0.084(5) 0.066(5) 0.079(5) -0.031(4) -0.007(4) 0.014(4) C91 0.040(3) 0.023(2) 0.066(4) 0.006(2) -0.013(3) -0.005(2) C92 0.063(4) 0.027(3) 0.086(5) 0.018(3) -0.034(3) -0.014(3) C93 0.154(8) 0.052(4) 0.079(5) 0.014(4) -0.058(5) -0.042(5) C94 0.071(4) 0.029(3) 0.084(5) 0.008(3) 0.003(4) 0.006(3) C95 0.114(6) 0.066(5) 0.066(5) -0.009(4) 0.011(4) 0.003(4) C96 0.080(6) 0.029(3) 0.155(8) 0.013(4) 0.045(6) 0.007(3) C97 0.048(5) 0.039(4) 0.243(14) 0.045(6) -0.023(7) 0.006(3) C98 0.074(5) 0.045(4) 0.183(10) 0.044(5) -0.081(6) -0.023(4) C99 0.041(3) 0.039(3) 0.075(4) -0.015(3) -0.024(3) 0.005(2) C100 0.040(5) 0.088(7) 0.51(3) 0.069(11) -0.021(9) 0.017(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Al1 C13 1.991(5) . ? Al1 C1 2.003(5) . ? Al1 C25 2.026(5) . ? Al2 C37 1.999(4) . ? Al2 C49 2.005(4) . ? Al2 C61 2.007(4) . ? P1 P1A 1.005(9) . ? P1 C82 1.778(5) . ? P1 C73 1.806(5) . ? P1 C91 1.827(5) . ? P1A C91 1.738(10) . ? P1A C73 1.744(10) . ? P1A C82 2.080(10) . ? P1A C94 2.318(11) . ? F1 C38 1.359(5) . ? F2 C39 1.339(5) . ? F3 C40 1.334(5) . ? F4 C41 1.332(5) . ? F5 C44 1.332(5) . ? F6 C45 1.333(6) . ? F7 C46 1.341(5) . ? F8 C68 1.330(5) . ? F9 C70 1.335(6) . ? F10 C71 1.334(6) . ? F11 C72 1.324(5) . ? F12 C62 1.352(5) . ? F13 C63 1.339(5) . ? F14 C64 1.332(5) . ? F15 C65 1.342(5) . ? F16 C50 1.350(5) . ? F17 C51 1.335(5) . ? F18 C52 1.325(5) . ? F19 C53 1.340(5) . ? F20 C56 1.334(5) . ? F21 C57 1.354(5) . ? F22 C58 1.339(6) . ? F23 C59 1.324(5) . ? F24 C60 1.338(5) . ? F25 C2 1.324(5) . ? F26 C3 1.332(5) . ? F27 C4 1.340(5) . ? F28 C5 1.366(6) . ? F29 C12 1.324(6) . ? F30 C8 1.352(6) . ? F31 C9 1.327(6) . ? F32 C10 1.340(6) . ? F33 C36 1.360(7) . ? F34 C34 1.302(8) . ? F35 C26 1.347(5) . ? F36 C27 1.358(5) . ? F37 C28 1.350(6) . ? F38 C29 1.355(5) . ? F39 C15 1.349(6) . ? F40 C16 1.350(5) . ? F41 C17 1.337(6) . ? F42 C20 1.343(6) . ? F43 C21 1.329(6) . ? F44 C22 1.331(6) . ? F45 C23 1.330(6) . ? F46 C24 1.331(6) . ? F47 C18 1.337(5) . ? F48 C33 1.330(8) . ? F49 C35 1.318(8) . ? F50 C48 1.340(5) . ? F51 C47 1.336(6) . ? F52 C69 1.340(6) . ? F53 C11 1.336(6) . ? F54 C99 1.298(7) . ? C1 C2 1.395(6) . ? C1 C6 1.410(6) . ? C2 C3 1.387(7) . ? C3 C4 1.378(7) . ? C4 C5 1.359(7) . ? C5 C6 1.388(6) . ? C6 C7 1.473(7) . ? C7 C12 1.373(7) . ? C7 C8 1.390(7) . ? C8 C9 1.378(7) . ? C9 C10 1.366(8) . ? C10 C11 1.364(8) . ? C11 C12 1.395(7) . ? C13 C18 1.390(7) . ? C13 C14 1.392(6) . ? C14 C15 1.380(7) . ? C14 C19 1.511(7) . ? C15 C16 1.375(8) . ? C16 C17 1.343(7) . ? C17 C18 1.384(7) . ? C19 C24 1.371(7) . ? C19 C20 1.379(7) . ? C20 C21 1.372(8) . ? C21 C22 1.377(8) . ? C22 C23 1.377(8) . ? C23 C24 1.370(8) . ? C25 C26 1.399(7) . ? C25 C30 1.399(6) . ? C26 C27 1.360(7) . ? C27 C28 1.339(7) . ? C28 C29 1.367(7) . ? C29 C30 1.401(6) . ? C30 C31 1.480(7) . ? C31 C36 1.355(7) . ? C31 C99 1.397(7) . ? C33 C34 1.359(11) . ? C33 C99 1.387(9) . ? C34 C35 1.397(11) . ? C35 C36 1.391(8) . ? C37 C38 1.374(6) . ? C37 C42 1.416(6) . ? C38 C39 1.386(6) . ? C39 C40 1.350(7) . ? C40 C41 1.382(6) . ? C41 C42 1.389(6) . ? C42 C43 1.488(6) . ? C43 C48 1.380(6) . ? C43 C44 1.382(6) . ? C44 C45 1.388(7) . ? C45 C46 1.370(7) . ? C46 C47 1.365(7) . ? C47 C48 1.369(6) . ? C49 C50 1.384(6) . ? C49 C54 1.414(6) . ? C50 C51 1.368(6) . ? C51 C52 1.389(7) . ? C52 C53 1.372(7) . ? C53 C54 1.384(6) . ? C54 C55 1.488(6) . ? C55 C56 1.381(6) . ? C55 C60 1.381(6) . ? C56 C57 1.352(7) . ? C57 C58 1.371(7) . ? C58 C59 1.381(7) . ? C59 C60 1.379(7) . ? C61 C62 1.368(6) . ? C61 C66 1.412(6) . ? C62 C63 1.395(6) . ? C63 C64 1.361(7) . ? C64 C65 1.371(6) . ? C65 C66 1.382(6) . ? C66 C67 1.478(6) . ? C67 C68 1.385(6) . ? C67 C72 1.391(6) . ? C68 C69 1.369(7) . ? C69 C70 1.369(8) . ? C70 C71 1.365(7) . ? C71 C72 1.378(7) . ? C73 C78 1.406(7) . ? C73 C74 1.414(7) . ? C74 C75 1.379(8) . ? C74 C81 1.496(8) . ? C75 C77 1.377(8) . ? C76 C78 1.378(7) . ? C76 C77 1.404(8) . ? C77 C80 1.496(8) . ? C78 C79 1.506(7) . ? C82 C87 1.395(7) . ? C82 C83 1.402(8) . ? C83 C84 1.392(9) . ? C83 C90 1.496(8) . ? C84 C85 1.343(9) . ? C85 C86 1.365(8) . ? C85 C89 1.523(8) . ? C86 C87 1.372(7) . ? C87 C88 1.518(7) . ? C91 C94 1.376(9) . ? C91 C92 1.385(8) . ? C92 C98 1.377(10) . ? C92 C93 1.501(10) . ? C94 C96 1.398(10) . ? C94 C95 1.500(10) . ? C96 C97 1.352(14) . ? C97 C98 1.356(14) . ? C97 C100 1.506(11) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C13 Al1 C1 115.0(2) . . ? C13 Al1 C25 114.99(19) . . ? C1 Al1 C25 113.44(19) . . ? C37 Al2 C49 118.09(18) . . ? C37 Al2 C61 115.62(17) . . ? C49 Al2 C61 114.95(17) . . ? P1A P1 C82 92.5(5) . . ? P1A P1 C73 70.2(5) . . ? C82 P1 C73 116.0(2) . . ? P1A P1 C91 68.8(5) . . ? C82 P1 C91 119.8(2) . . ? C73 P1 C91 110.1(2) . . ? P1 P1A C91 78.6(6) . . ? P1 P1A C73 77.0(5) . . ? C91 P1A C73 117.6(5) . . ? P1 P1A C82 58.6(5) . . ? C91 P1A C82 109.2(5) . . ? C73 P1A C82 104.9(5) . . ? P1 P1A C94 112.1(6) . . ? C91 P1A C94 36.2(3) . . ? C73 P1A C94 111.4(5) . . ? C82 P1A C94 139.1(5) . . ? C2 C1 C6 116.1(4) . . ? C2 C1 Al1 113.2(3) . . ? C6 C1 Al1 130.6(3) . . ? F25 C2 C3 116.7(4) . . ? F25 C2 C1 119.4(4) . . ? C3 C2 C1 123.8(5) . . ? F26 C3 C4 120.5(4) . . ? F26 C3 C2 121.1(5) . . ? C4 C3 C2 118.4(4) . . ? F27 C4 C5 121.5(5) . . ? F27 C4 C3 119.2(4) . . ? C5 C4 C3 119.1(4) . . ? C4 C5 F28 117.9(4) . . ? C4 C5 C6 123.3(5) . . ? F28 C5 C6 118.7(4) . . ? C5 C6 C1 119.0(4) . . ? C5 C6 C7 116.5(4) . . ? C1 C6 C7 124.5(4) . . ? C12 C7 C8 116.6(4) . . ? C12 C7 C6 121.4(4) . . ? C8 C7 C6 122.0(4) . . ? F30 C8 C9 119.2(5) . . ? F30 C8 C7 118.6(4) . . ? C9 C8 C7 122.2(5) . . ? F31 C9 C10 120.6(5) . . ? F31 C9 C8 120.1(5) . . ? C10 C9 C8 119.3(5) . . ? F32 C10 C11 119.0(5) . . ? F32 C10 C9 120.4(5) . . ? C11 C10 C9 120.6(5) . . ? F53 C11 C10 120.7(5) . . ? F53 C11 C12 120.1(5) . . ? C10 C11 C12 119.2(5) . . ? F29 C12 C7 120.2(4) . . ? F29 C12 C11 117.8(5) . . ? C7 C12 C11 122.0(5) . . ? C18 C13 C14 114.6(4) . . ? C18 C13 Al1 112.9(3) . . ? C14 C13 Al1 132.5(4) . . ? C15 C14 C13 121.0(5) . . ? C15 C14 C19 116.7(4) . . ? C13 C14 C19 122.3(4) . . ? F39 C15 C16 117.8(5) . . ? F39 C15 C14 120.3(5) . . ? C16 C15 C14 121.8(5) . . ? C17 C16 F40 121.4(5) . . ? C17 C16 C15 119.0(4) . . ? F40 C16 C15 119.6(5) . . ? F41 C17 C16 120.2(4) . . ? F41 C17 C18 120.6(5) . . ? C16 C17 C18 119.1(5) . . ? F47 C18 C17 116.0(4) . . ? F47 C18 C13 119.6(4) . . ? C17 C18 C13 124.3(4) . . ? C24 C19 C20 116.5(5) . . ? C24 C19 C14 120.3(5) . . ? C20 C19 C14 123.3(5) . . ? F42 C20 C21 118.0(5) . . ? F42 C20 C19 119.2(5) . . ? C21 C20 C19 122.8(5) . . ? F43 C21 C20 120.6(5) . . ? F43 C21 C22 120.3(5) . . ? C20 C21 C22 119.0(5) . . ? F44 C22 C23 119.9(5) . . ? F44 C22 C21 120.6(5) . . ? C23 C22 C21 119.5(5) . . ? F45 C23 C24 120.9(5) . . ? F45 C23 C22 119.4(5) . . ? C24 C23 C22 119.7(5) . . ? F46 C24 C23 118.3(5) . . ? F46 C24 C19 119.3(5) . . ? C23 C24 C19 122.4(5) . . ? C26 C25 C30 114.5(4) . . ? C26 C25 Al1 114.5(3) . . ? C30 C25 Al1 131.0(3) . . ? F35 C26 C27 118.3(4) . . ? F35 C26 C25 117.1(4) . . ? C27 C26 C25 124.5(4) . . ? C28 C27 F36 120.0(5) . . ? C28 C27 C26 120.0(5) . . ? F36 C27 C26 119.9(5) . . ? C27 C28 F37 120.8(5) . . ? C27 C28 C29 118.9(5) . . ? F37 C28 C29 120.2(5) . . ? F38 C29 C28 118.8(4) . . ? F38 C29 C30 119.2(4) . . ? C28 C29 C30 121.9(4) . . ? C25 C30 C29 119.9(4) . . ? C25 C30 C31 125.0(4) . . ? C29 C30 C31 115.1(4) . . ? C36 C31 C99 117.3(5) . . ? C36 C31 C30 123.8(5) . . ? C99 C31 C30 118.9(5) . . ? F48 C33 C34 119.0(7) . . ? F48 C33 C99 119.7(8) . . ? C34 C33 C99 121.3(7) . . ? F34 C34 C33 122.3(9) . . ? F34 C34 C35 117.8(9) . . ? C33 C34 C35 119.7(6) . . ? F49 C35 C36 120.2(8) . . ? F49 C35 C34 122.2(7) . . ? C36 C35 C34 117.5(7) . . ? C31 C36 F33 118.8(5) . . ? C31 C36 C35 123.9(6) . . ? F33 C36 C35 117.2(6) . . ? C38 C37 C42 114.4(4) . . ? C38 C37 Al2 114.8(3) . . ? C42 C37 Al2 130.4(3) . . ? F1 C38 C37 118.7(4) . . ? F1 C38 C39 115.5(4) . . ? C37 C38 C39 125.7(4) . . ? F2 C39 C40 120.5(4) . . ? F2 C39 C38 121.2(4) . . ? C40 C39 C38 118.3(4) . . ? F3 C40 C39 120.8(4) . . ? F3 C40 C41 119.7(4) . . ? C39 C40 C41 119.6(4) . . ? F4 C41 C40 118.2(4) . . ? F4 C41 C42 120.3(4) . . ? C40 C41 C42 121.5(4) . . ? C41 C42 C37 120.4(4) . . ? C41 C42 C43 116.7(4) . . ? C37 C42 C43 122.8(4) . . ? C48 C43 C44 116.3(4) . . ? C48 C43 C42 122.0(4) . . ? C44 C43 C42 121.7(4) . . ? F5 C44 C43 120.2(4) . . ? F5 C44 C45 117.8(4) . . ? C43 C44 C45 122.0(5) . . ? F6 C45 C46 120.6(5) . . ? F6 C45 C44 120.5(5) . . ? C46 C45 C44 118.9(5) . . ? F7 C46 C47 120.7(5) . . ? F7 C46 C45 118.6(5) . . ? C47 C46 C45 120.8(4) . . ? F51 C47 C46 119.8(4) . . ? F51 C47 C48 121.2(5) . . ? C46 C47 C48 119.0(4) . . ? F50 C48 C47 118.1(4) . . ? F50 C48 C43 118.9(4) . . ? C47 C48 C43 123.0(4) . . ? C50 C49 C54 115.2(4) . . ? C50 C49 Al2 113.0(3) . . ? C54 C49 Al2 131.5(3) . . ? F16 C50 C51 115.8(4) . . ? F16 C50 C49 119.4(4) . . ? C51 C50 C49 124.8(4) . . ? F17 C51 C50 121.2(4) . . ? F17 C51 C52 119.9(4) . . ? C50 C51 C52 118.9(4) . . ? F18 C52 C53 121.6(4) . . ? F18 C52 C51 119.8(5) . . ? C53 C52 C51 118.6(4) . . ? F19 C53 C52 117.4(4) . . ? F19 C53 C54 120.6(4) . . ? C52 C53 C54 122.0(4) . . ? C53 C54 C49 120.5(4) . . ? C53 C54 C55 117.8(4) . . ? C49 C54 C55 121.7(4) . . ? C56 C55 C60 116.8(4) . . ? C56 C55 C54 121.2(4) . . ? C60 C55 C54 121.9(4) . . ? F20 C56 C57 119.3(4) . . ? F20 C56 C55 118.9(4) . . ? C57 C56 C55 121.7(5) . . ? C56 C57 F21 121.2(5) . . ? C56 C57 C58 120.5(4) . . ? F21 C57 C58 118.3(4) . . ? F22 C58 C57 120.9(5) . . ? F22 C58 C59 118.9(5) . . ? C57 C58 C59 120.1(5) . . ? F23 C59 C60 121.2(5) . . ? F23 C59 C58 120.8(5) . . ? C60 C59 C58 118.0(5) . . ? F24 C60 C59 118.1(4) . . ? F24 C60 C55 119.2(4) . . ? C59 C60 C55 122.7(4) . . ? C62 C61 C66 115.4(4) . . ? C62 C61 Al2 114.1(3) . . ? C66 C61 Al2 130.4(3) . . ? F12 C62 C61 119.8(4) . . ? F12 C62 C63 116.0(4) . . ? C61 C62 C63 124.2(4) . . ? F13 C63 C64 120.1(4) . . ? F13 C63 C62 120.8(4) . . ? C64 C63 C62 119.1(4) . . ? F14 C64 C63 120.0(4) . . ? F14 C64 C65 121.4(4) . . ? C63 C64 C65 118.7(4) . . ? F15 C65 C64 117.7(4) . . ? F15 C65 C66 120.0(4) . . ? C64 C65 C66 122.3(4) . . ? C65 C66 C61 120.3(4) . . ? C65 C66 C67 115.5(4) . . ? C61 C66 C67 124.1(4) . . ? C68 C67 C72 116.4(4) . . ? C68 C67 C66 120.2(4) . . ? C72 C67 C66 123.3(4) . . ? F8 C68 C69 118.4(4) . . ? F8 C68 C67 119.5(4) . . ? C69 C68 C67 122.1(5) . . ? F52 C69 C68 120.1(5) . . ? F52 C69 C70 120.0(5) . . ? C68 C69 C70 119.9(5) . . ? F9 C70 C71 120.9(5) . . ? F9 C70 C69 119.1(5) . . ? C71 C70 C69 120.0(5) . . ? F10 C71 C70 120.2(5) . . ? F10 C71 C72 120.0(5) . . ? C70 C71 C72 119.7(5) . . ? F11 C72 C71 118.8(4) . . ? F11 C72 C67 119.4(4) . . ? C71 C72 C67 121.7(4) . . ? C78 C73 C74 121.3(5) . . ? C78 C73 P1A 129.7(5) . . ? C74 C73 P1A 102.4(5) . . ? C78 C73 P1 114.5(4) . . ? C74 C73 P1 124.2(4) . . ? P1A C73 P1 32.8(3) . . ? C75 C74 C73 116.5(5) . . ? C75 C74 C81 119.0(5) . . ? C73 C74 C81 124.5(5) . . ? C77 C75 C74 124.2(5) . . ? C78 C76 C77 121.4(5) . . ? C75 C77 C76 117.6(5) . . ? C75 C77 C80 121.5(6) . . ? C76 C77 C80 120.9(6) . . ? C76 C78 C73 118.9(5) . . ? C76 C78 C79 118.4(5) . . ? C73 C78 C79 122.7(4) . . ? C87 C82 C83 120.2(5) . . ? C87 C82 P1 125.5(4) . . ? C83 C82 P1 114.4(4) . . ? C87 C82 P1A 101.5(4) . . ? C83 C82 P1A 135.3(5) . . ? P1 C82 P1A 28.9(2) . . ? C84 C83 C82 117.5(5) . . ? C84 C83 C90 118.1(6) . . ? C82 C83 C90 124.3(6) . . ? C85 C84 C83 122.7(5) . . ? C84 C85 C86 118.7(5) . . ? C84 C85 C89 121.7(6) . . ? C86 C85 C89 119.6(6) . . ? C85 C86 C87 122.4(6) . . ? C86 C87 C82 118.4(5) . . ? C86 C87 C88 117.6(5) . . ? C82 C87 C88 124.0(5) . . ? C94 C91 C92 121.6(6) . . ? C94 C91 P1A 95.5(5) . . ? C92 C91 P1A 142.7(6) . . ? C94 C91 P1 125.2(5) . . ? C92 C91 P1 112.4(5) . . ? P1A C91 P1 32.6(3) . . ? C98 C92 C91 118.4(7) . . ? C98 C92 C93 117.9(7) . . ? C91 C92 C93 123.7(6) . . ? C91 C94 C96 116.1(7) . . ? C91 C94 C95 122.9(6) . . ? C96 C94 C95 121.1(7) . . ? C91 C94 P1A 48.3(4) . . ? C96 C94 P1A 164.3(7) . . ? C95 C94 P1A 74.6(5) . . ? C97 C96 C94 123.9(9) . . ? C96 C97 C98 117.7(8) . . ? C96 C97 C100 119.1(14) . . ? C98 C97 C100 123.2(13) . . ? C97 C98 C92 122.2(8) . . ? F54 C99 C33 119.0(6) . . ? F54 C99 C31 120.8(5) . . ? C33 C99 C31 120.1(7) . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 28.49 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 1.465 _refine_diff_density_min -0.492 _refine_diff_density_rms 0.099 #==end _database_code_depnum_ccdc_archive 'CCDC 947827'