# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Eugene Y.-X. Chen' _publ_contact_author_email eugene.chen@colostate.edu loop_ _publ_author_name Y.Zhang E.Y.-X.Chen # Attachment '- cif_zwitterion 2.txt' data_ec65 _database_code_depnum_ccdc_archive 'CCDC 865898' #TrackingRef '- cif_zwitterion 2.txt' _audit_creation_method 'Bruker SHELXTL' _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C35 H34 Al F15 O2 P' _chemical_formula_sum 'C35 H34 Al F15 O2 P' _chemical_formula_weight 829.57 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21/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 15.9769(3) _cell_length_b 12.0995(2) _cell_length_c 18.1623(3) _cell_angle_alpha 90.00 _cell_angle_beta 93.4810(10) _cell_angle_gamma 90.00 _cell_volume 3504.52(11) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 9073 _cell_measurement_theta_min 2.36 _cell_measurement_theta_max 33.15 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.41 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.572 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1692 _exptl_absorpt_coefficient_mu 0.217 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9160 _exptl_absorpt_correction_T_max 0.9803 _exptl_absorpt_process_details 'SADABS, Sheldrick, 1997' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(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' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 52285 _diffrn_reflns_av_R_equivalents 0.0419 _diffrn_reflns_av_sigmaI/netI 0.0464 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.65 _diffrn_reflns_theta_max 33.22 _reflns_number_total 13439 _reflns_number_gt 9144 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0826P)^2^+0.3389P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 13439 _refine_ls_number_parameters 496 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0765 _refine_ls_R_factor_gt 0.0442 _refine_ls_wR_factor_ref 0.1483 _refine_ls_wR_factor_gt 0.1205 _refine_ls_goodness_of_fit_ref 1.013 _refine_ls_restrained_S_all 1.013 _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 Al2 Al 0.03666(3) 0.89378(4) 0.24433(2) 0.01544(9) Uani 1 1 d . . . C1 C 0.01531(9) 0.73578(12) 0.21494(9) 0.0193(3) Uani 1 1 d . . . C2 C 0.03721(11) 0.64320(13) 0.25650(10) 0.0251(3) Uani 1 1 d . . . C3 C 0.02555(12) 0.53552(14) 0.23188(12) 0.0324(4) Uani 1 1 d . . . C4 C -0.00962(11) 0.51771(14) 0.16181(12) 0.0311(4) Uani 1 1 d . . . C5 C -0.03258(10) 0.60591(14) 0.11755(10) 0.0257(3) Uani 1 1 d . . . C6 C -0.02080(9) 0.71177(12) 0.14575(9) 0.0203(3) Uani 1 1 d . . . C7 C -0.06766(9) 0.97306(12) 0.27210(8) 0.0176(3) Uani 1 1 d . . . C8 C -0.14645(9) 0.92575(13) 0.27339(8) 0.0195(3) Uani 1 1 d . . . C9 C -0.21743(9) 0.98234(14) 0.29231(9) 0.0224(3) Uani 1 1 d . . . C10 C -0.21086(10) 1.09260(14) 0.31056(9) 0.0239(3) Uani 1 1 d . . . C11 C -0.13379(11) 1.14393(13) 0.31122(8) 0.0226(3) Uani 1 1 d . . . C12 C -0.06483(10) 1.08282(13) 0.29363(8) 0.0193(3) Uani 1 1 d . . . C13 C 0.11899(9) 0.90496(12) 0.33244(8) 0.0175(3) Uani 1 1 d . . . C14 C 0.20171(9) 0.93902(12) 0.33422(8) 0.0178(3) Uani 1 1 d . . . C15 C 0.25184(9) 0.95301(12) 0.39813(9) 0.0200(3) Uani 1 1 d . . . C16 C 0.21891(10) 0.93279(13) 0.46516(9) 0.0225(3) Uani 1 1 d . . . C17 C 0.13719(10) 0.89715(14) 0.46685(9) 0.0241(3) Uani 1 1 d . . . C18 C 0.09048(10) 0.88363(14) 0.40142(9) 0.0221(3) Uani 1 1 d . . . C19 C 0.11671(9) 1.04090(12) 0.14602(8) 0.0178(3) Uani 1 1 d . . . C20 C 0.18706(9) 1.05210(11) 0.10991(8) 0.0173(3) Uani 1 1 d . . . H20 H 0.1592 1.0510 0.0603 0.021 Uiso 1 1 calc R . . C21 C 0.20920(11) 1.17327(13) 0.10928(11) 0.0281(3) Uani 1 1 d . . . H21A H 0.2216 1.1979 0.0603 0.034 Uiso 1 1 calc R . . H21B H 0.2565 1.1896 0.1436 0.034 Uiso 1 1 calc R . . C22 C 0.12838(12) 1.22520(14) 0.13401(12) 0.0336(4) Uani 1 1 d . . . H22A H 0.1412 1.2816 0.1710 0.040 Uiso 1 1 calc R . . H22B H 0.0974 1.2592 0.0924 0.040 Uiso 1 1 calc R . . C23 C 0.24263(9) 0.95500(12) 0.09817(8) 0.0173(3) Uani 1 1 d . . . H23A H 0.2229 0.8956 0.1285 0.021 Uiso 1 1 calc R . . H23B H 0.2980 0.9749 0.1189 0.021 Uiso 1 1 calc R . . C24 C 0.15494(9) 0.83758(12) -0.03262(8) 0.0165(3) Uani 1 1 d . . . C25 C 0.15863(11) 0.80828(14) -0.11494(9) 0.0250(3) Uani 1 1 d . . . H25A H 0.1065 0.7754 -0.1325 0.038 Uiso 1 1 calc R . . H25B H 0.2035 0.7570 -0.1210 0.038 Uiso 1 1 calc R . . H25C H 0.1682 0.8742 -0.1426 0.038 Uiso 1 1 calc R . . C26 C 0.13030(10) 0.73362(13) 0.01015(9) 0.0215(3) Uani 1 1 d . . . H26A H 0.0750 0.7105 -0.0069 0.032 Uiso 1 1 calc R . . H26B H 0.1311 0.7503 0.0619 0.032 Uiso 1 1 calc R . . H26C H 0.1695 0.6754 0.0021 0.032 Uiso 1 1 calc R . . C27 C 0.08271(9) 0.92030(13) -0.02455(9) 0.0211(3) Uani 1 1 d . . . H27A H 0.0959 0.9888 -0.0478 0.032 Uiso 1 1 calc R . . H27B H 0.0753 0.9329 0.0268 0.032 Uiso 1 1 calc R . . H27C H 0.0319 0.8906 -0.0476 0.032 Uiso 1 1 calc R . . C28 C 0.33609(9) 0.78112(12) 0.02926(9) 0.0200(3) Uani 1 1 d . . . C29 C 0.33770(10) 0.69645(14) -0.03394(10) 0.0269(3) Uani 1 1 d . . . H29A H 0.3799 0.6417 -0.0220 0.040 Uiso 1 1 calc R . . H29B H 0.3503 0.7335 -0.0787 0.040 Uiso 1 1 calc R . . H29C H 0.2839 0.6613 -0.0406 0.040 Uiso 1 1 calc R . . C30 C 0.31610(10) 0.72183(13) 0.10121(9) 0.0241(3) Uani 1 1 d . . . H30A H 0.2587 0.6980 0.0979 0.036 Uiso 1 1 calc R . . H30B H 0.3250 0.7717 0.1420 0.036 Uiso 1 1 calc R . . H30C H 0.3521 0.6588 0.1085 0.036 Uiso 1 1 calc R . . C31 C 0.42549(10) 0.82737(15) 0.04301(11) 0.0281(4) Uani 1 1 d . . . H31A H 0.4628 0.7687 0.0589 0.042 Uiso 1 1 calc R . . H31B H 0.4256 0.8834 0.0805 0.042 Uiso 1 1 calc R . . H31C H 0.4438 0.8588 -0.0018 0.042 Uiso 1 1 calc R . . C32 C 0.30125(9) 1.00353(13) -0.05373(8) 0.0203(3) Uani 1 1 d . . . C33 C 0.34409(11) 0.95456(15) -0.11996(9) 0.0287(4) Uani 1 1 d . . . H33A H 0.3627 1.0134 -0.1504 0.043 Uiso 1 1 calc R . . H33B H 0.3049 0.9089 -0.1482 0.043 Uiso 1 1 calc R . . H33C H 0.3914 0.9108 -0.1026 0.043 Uiso 1 1 calc R . . C34 C 0.23039(11) 1.08124(14) -0.08321(10) 0.0267(3) Uani 1 1 d . . . H34A H 0.2006 1.1088 -0.0427 0.040 Uiso 1 1 calc R . . H34B H 0.1924 1.0412 -0.1164 0.040 Uiso 1 1 calc R . . H34C H 0.2540 1.1420 -0.1089 0.040 Uiso 1 1 calc R . . C35 C 0.36534(10) 1.07543(14) -0.00858(10) 0.0250(3) Uani 1 1 d . . . H35A H 0.4125 1.0309 0.0080 0.037 Uiso 1 1 calc R . . H35B H 0.3395 1.1057 0.0333 0.037 Uiso 1 1 calc R . . H35C H 0.3839 1.1345 -0.0389 0.037 Uiso 1 1 calc R . . F1 F 0.07241(8) 0.65417(9) 0.32604(6) 0.0405(3) Uani 1 1 d . . . F2 F 0.04862(10) 0.44905(9) 0.27512(8) 0.0537(4) Uani 1 1 d . . . F3 F -0.02066(8) 0.41415(9) 0.13653(8) 0.0470(3) Uani 1 1 d . . . F4 F -0.06499(7) 0.58953(10) 0.04892(7) 0.0407(3) Uani 1 1 d . . . F5 F -0.04721(6) 0.79577(8) 0.10065(6) 0.0283(2) Uani 1 1 d . . . F6 F -0.15755(6) 0.81777(8) 0.25604(6) 0.0288(2) Uani 1 1 d . . . F7 F -0.29225(6) 0.93140(10) 0.29269(6) 0.0344(2) Uani 1 1 d . . . F8 F -0.27875(7) 1.14872(10) 0.32886(6) 0.0363(3) Uani 1 1 d . . . F9 F -0.12658(7) 1.25084(8) 0.33060(6) 0.0338(2) Uani 1 1 d . . . F10 F 0.00957(6) 1.13616(8) 0.30016(6) 0.0275(2) Uani 1 1 d . . . F11 F 0.23813(6) 0.96145(9) 0.27040(5) 0.0281(2) Uani 1 1 d . . . F12 F 0.33147(6) 0.98887(9) 0.39612(6) 0.0295(2) Uani 1 1 d . . . F13 F 0.26532(7) 0.94809(9) 0.52810(6) 0.0333(2) Uani 1 1 d . . . F14 F 0.10437(7) 0.87627(11) 0.53185(6) 0.0389(3) Uani 1 1 d . . . F15 F 0.01070(6) 0.84692(10) 0.40633(6) 0.0332(2) Uani 1 1 d . . . O1 O 0.07947(7) 0.95026(9) 0.16561(6) 0.0193(2) Uani 1 1 d . . . O2 O 0.07918(7) 1.13766(9) 0.16455(7) 0.0254(2) Uani 1 1 d . . . P1 P 0.25741(2) 0.89507(3) 0.00717(2) 0.01383(8) 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 Al2 0.01566(19) 0.0150(2) 0.0159(2) -0.00189(15) 0.00284(15) -0.00159(15) C1 0.0170(6) 0.0177(6) 0.0234(7) -0.0015(5) 0.0046(5) -0.0014(5) C2 0.0274(8) 0.0195(7) 0.0283(8) 0.0007(6) 0.0021(6) -0.0019(6) C3 0.0343(9) 0.0157(7) 0.0472(11) 0.0033(7) 0.0026(8) -0.0009(6) C4 0.0243(8) 0.0174(7) 0.0523(11) -0.0119(7) 0.0067(7) -0.0032(6) C5 0.0172(7) 0.0271(8) 0.0329(9) -0.0115(7) 0.0018(6) -0.0040(6) C6 0.0147(6) 0.0193(7) 0.0270(8) -0.0029(6) 0.0033(5) -0.0010(5) C7 0.0178(6) 0.0204(6) 0.0146(6) -0.0025(5) 0.0013(5) 0.0003(5) C8 0.0203(6) 0.0204(7) 0.0180(7) -0.0014(5) 0.0016(5) 0.0000(5) C9 0.0164(6) 0.0320(8) 0.0191(7) 0.0055(6) 0.0032(5) 0.0023(6) C10 0.0245(7) 0.0302(8) 0.0176(7) 0.0050(6) 0.0065(6) 0.0115(6) C11 0.0321(8) 0.0203(7) 0.0158(7) -0.0005(5) 0.0041(6) 0.0058(6) C12 0.0218(7) 0.0206(7) 0.0156(6) -0.0013(5) 0.0018(5) -0.0010(5) C13 0.0177(6) 0.0175(6) 0.0175(6) -0.0012(5) 0.0024(5) -0.0008(5) C14 0.0180(6) 0.0163(6) 0.0193(7) -0.0007(5) 0.0033(5) 0.0004(5) C15 0.0163(6) 0.0163(6) 0.0273(8) -0.0002(5) -0.0006(5) 0.0000(5) C16 0.0264(7) 0.0208(7) 0.0194(7) -0.0019(5) -0.0050(6) 0.0022(6) C17 0.0272(8) 0.0291(8) 0.0162(7) 0.0008(6) 0.0031(6) 0.0004(6) C18 0.0200(7) 0.0268(8) 0.0197(7) 0.0000(6) 0.0030(5) -0.0037(6) C19 0.0203(6) 0.0158(6) 0.0173(6) -0.0020(5) 0.0005(5) -0.0006(5) C20 0.0211(6) 0.0127(6) 0.0182(7) -0.0006(5) 0.0018(5) -0.0015(5) C21 0.0309(8) 0.0153(7) 0.0392(10) -0.0049(6) 0.0115(7) -0.0055(6) C22 0.0376(9) 0.0156(7) 0.0487(11) -0.0028(7) 0.0124(8) -0.0006(6) C23 0.0183(6) 0.0167(6) 0.0167(6) 0.0007(5) 0.0011(5) -0.0002(5) C24 0.0156(6) 0.0172(6) 0.0166(6) -0.0009(5) 0.0009(5) -0.0015(5) C25 0.0268(8) 0.0291(8) 0.0191(7) -0.0040(6) 0.0004(6) -0.0031(6) C26 0.0189(6) 0.0188(7) 0.0271(8) 0.0013(6) 0.0031(6) -0.0041(5) C27 0.0149(6) 0.0222(7) 0.0258(8) -0.0026(6) -0.0014(5) 0.0018(5) C28 0.0146(6) 0.0181(6) 0.0277(8) 0.0040(6) 0.0041(5) 0.0026(5) C29 0.0226(7) 0.0221(7) 0.0371(9) -0.0014(7) 0.0097(7) 0.0041(6) C30 0.0216(7) 0.0207(7) 0.0297(8) 0.0073(6) -0.0005(6) 0.0044(5) C31 0.0157(7) 0.0278(8) 0.0407(10) 0.0054(7) -0.0004(6) 0.0009(6) C32 0.0198(6) 0.0203(7) 0.0212(7) 0.0058(5) 0.0044(5) -0.0029(5) C33 0.0301(8) 0.0324(9) 0.0248(8) 0.0053(7) 0.0117(7) -0.0041(7) C34 0.0276(8) 0.0215(7) 0.0307(9) 0.0109(6) -0.0004(7) -0.0008(6) C35 0.0210(7) 0.0226(7) 0.0316(9) 0.0047(6) 0.0035(6) -0.0065(6) F1 0.0610(8) 0.0272(6) 0.0314(6) 0.0066(4) -0.0111(5) -0.0049(5) F2 0.0723(9) 0.0183(5) 0.0691(9) 0.0126(6) -0.0076(7) 0.0007(6) F3 0.0445(7) 0.0201(5) 0.0763(9) -0.0189(6) 0.0033(7) -0.0052(5) F4 0.0362(6) 0.0427(7) 0.0419(7) -0.0208(5) -0.0077(5) -0.0068(5) F5 0.0278(5) 0.0278(5) 0.0283(5) 0.0005(4) -0.0072(4) 0.0001(4) F6 0.0253(5) 0.0220(5) 0.0397(6) -0.0066(4) 0.0059(4) -0.0067(4) F7 0.0179(4) 0.0426(6) 0.0432(6) 0.0084(5) 0.0068(4) -0.0010(4) F8 0.0324(6) 0.0400(6) 0.0379(6) 0.0115(5) 0.0145(5) 0.0216(5) F9 0.0489(6) 0.0197(5) 0.0338(6) -0.0056(4) 0.0107(5) 0.0078(4) F10 0.0273(5) 0.0244(5) 0.0312(5) -0.0101(4) 0.0039(4) -0.0066(4) F11 0.0207(4) 0.0418(6) 0.0224(5) 0.0025(4) 0.0060(4) -0.0051(4) F12 0.0179(4) 0.0342(5) 0.0359(6) -0.0024(4) -0.0034(4) -0.0044(4) F13 0.0330(5) 0.0430(6) 0.0226(5) -0.0025(4) -0.0109(4) 0.0017(5) F14 0.0400(6) 0.0609(8) 0.0163(5) 0.0056(5) 0.0053(4) -0.0054(5) F15 0.0226(5) 0.0533(7) 0.0241(5) 0.0046(5) 0.0050(4) -0.0120(4) O1 0.0218(5) 0.0192(5) 0.0171(5) -0.0005(4) 0.0041(4) -0.0050(4) O2 0.0278(6) 0.0177(5) 0.0316(6) -0.0026(4) 0.0095(5) 0.0023(4) P1 0.01252(15) 0.01371(15) 0.01543(16) 0.00156(12) 0.00229(12) -0.00017(12) _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 Al2 O1 1.7599(11) . ? Al2 C1 2.0085(15) . ? Al2 C13 2.0134(15) . ? Al2 C7 2.0136(15) . ? C1 C6 1.381(2) . ? C1 C2 1.384(2) . ? C2 F1 1.357(2) . ? C2 C3 1.386(2) . ? C3 F2 1.346(2) . ? C3 C4 1.376(3) . ? C4 F3 1.3425(19) . ? C4 C5 1.373(3) . ? C5 F4 1.335(2) . ? C5 C6 1.388(2) . ? C6 F5 1.3565(18) . ? C7 C12 1.384(2) . ? C7 C8 1.384(2) . ? C8 F6 1.3532(18) . ? C8 C9 1.386(2) . ? C9 F7 1.3454(18) . ? C9 C10 1.377(2) . ? C10 F8 1.3386(18) . ? C10 C11 1.378(2) . ? C11 F9 1.3438(19) . ? C11 C12 1.380(2) . ? C12 F10 1.3514(18) . ? C13 C14 1.383(2) . ? C13 C18 1.383(2) . ? C14 F11 1.3556(18) . ? C14 C15 1.380(2) . ? C15 F12 1.3467(17) . ? C15 C16 1.377(2) . ? C16 F13 1.3371(18) . ? C16 C17 1.377(2) . ? C17 F14 1.3445(19) . ? C17 C18 1.374(2) . ? C18 F15 1.3578(18) . ? C19 O1 1.3073(17) . ? C19 C20 1.342(2) . ? C19 O2 1.3666(18) . ? C20 C23 1.496(2) . ? C20 C21 1.508(2) . ? C21 C22 1.528(3) . ? C22 O2 1.449(2) . ? C23 P1 1.8332(15) . ? C24 C25 1.541(2) . ? C24 C27 1.541(2) . ? C24 C26 1.542(2) . ? C24 P1 1.8823(14) . ? C28 C29 1.540(2) . ? C28 C31 1.540(2) . ? C28 C30 1.541(2) . ? C28 P1 1.8922(15) . ? C32 C33 1.538(2) . ? C32 C35 1.541(2) . ? C32 C34 1.542(2) . ? C32 P1 1.8789(15) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Al2 C1 102.82(6) . . ? O1 Al2 C13 110.63(6) . . ? C1 Al2 C13 111.56(6) . . ? O1 Al2 C7 112.76(6) . . ? C1 Al2 C7 112.97(6) . . ? C13 Al2 C7 106.24(6) . . ? C6 C1 C2 113.82(14) . . ? C6 C1 Al2 119.78(11) . . ? C2 C1 Al2 126.32(12) . . ? F1 C2 C1 120.35(14) . . ? F1 C2 C3 115.59(15) . . ? C1 C2 C3 124.07(16) . . ? F2 C3 C4 119.98(16) . . ? F2 C3 C2 121.03(18) . . ? C4 C3 C2 118.99(16) . . ? F3 C4 C5 120.03(18) . . ? F3 C4 C3 120.01(17) . . ? C5 C4 C3 119.96(15) . . ? F4 C5 C4 120.40(15) . . ? F4 C5 C6 121.18(16) . . ? C4 C5 C6 118.42(16) . . ? F5 C6 C1 119.29(13) . . ? F5 C6 C5 115.99(14) . . ? C1 C6 C5 124.72(15) . . ? C12 C7 C8 113.95(14) . . ? C12 C7 Al2 120.96(11) . . ? C8 C7 Al2 125.08(11) . . ? F6 C8 C7 120.11(13) . . ? F6 C8 C9 115.93(14) . . ? C7 C8 C9 123.96(15) . . ? F7 C9 C10 119.83(14) . . ? F7 C9 C8 121.04(15) . . ? C10 C9 C8 119.13(14) . . ? F8 C10 C9 120.01(15) . . ? F8 C10 C11 120.40(15) . . ? C9 C10 C11 119.57(14) . . ? F9 C11 C10 119.89(14) . . ? F9 C11 C12 121.29(15) . . ? C10 C11 C12 118.80(15) . . ? F10 C12 C11 115.73(14) . . ? F10 C12 C7 119.76(13) . . ? C11 C12 C7 124.50(15) . . ? C14 C13 C18 113.66(14) . . ? C14 C13 Al2 128.02(11) . . ? C18 C13 Al2 118.18(11) . . ? F11 C14 C15 115.93(13) . . ? F11 C14 C13 119.93(13) . . ? C15 C14 C13 124.14(14) . . ? F12 C15 C16 119.56(14) . . ? F12 C15 C14 121.18(14) . . ? C16 C15 C14 119.23(14) . . ? F13 C16 C17 120.11(15) . . ? F13 C16 C15 120.62(15) . . ? C17 C16 C15 119.27(14) . . ? F14 C17 C18 121.11(15) . . ? F14 C17 C16 119.95(14) . . ? C18 C17 C16 118.94(15) . . ? F15 C18 C17 116.42(14) . . ? F15 C18 C13 118.86(14) . . ? C17 C18 C13 124.72(15) . . ? O1 C19 C20 128.77(13) . . ? O1 C19 O2 115.97(13) . . ? C20 C19 O2 115.27(13) . . ? C19 C20 C23 120.81(13) . . ? C19 C20 C21 107.79(13) . . ? C23 C20 C21 128.39(13) . . ? C20 C21 C22 101.23(13) . . ? O2 C22 C21 107.43(13) . . ? C20 C23 P1 123.32(11) . . ? C25 C24 C27 108.33(12) . . ? C25 C24 C26 109.09(12) . . ? C27 C24 C26 105.45(12) . . ? C25 C24 P1 111.95(10) . . ? C27 C24 P1 111.24(10) . . ? C26 C24 P1 110.53(10) . . ? C29 C28 C31 107.78(13) . . ? C29 C28 C30 109.63(13) . . ? C31 C28 C30 105.63(13) . . ? C29 C28 P1 111.57(11) . . ? C31 C28 P1 111.55(10) . . ? C30 C28 P1 110.47(10) . . ? C33 C32 C35 108.70(13) . . ? C33 C32 C34 108.38(14) . . ? C35 C32 C34 106.89(13) . . ? C33 C32 P1 113.00(11) . . ? C35 C32 P1 109.90(11) . . ? C34 C32 P1 109.76(10) . . ? C19 O1 Al2 138.81(10) . . ? C19 O2 C22 105.99(12) . . ? C23 P1 C32 109.12(7) . . ? C23 P1 C24 109.61(7) . . ? C32 P1 C24 112.26(7) . . ? C23 P1 C28 102.56(7) . . ? C32 P1 C28 111.54(7) . . ? C24 P1 C28 111.30(7) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 33.22 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.517 _refine_diff_density_min -0.975 _refine_diff_density_rms 0.090 data_ec64 _database_code_depnum_ccdc_archive 'CCDC 865899' #TrackingRef 'CCDC-865899-Rev.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C35 H35 Al F15 O2 P' _chemical_formula_sum 'C35 H35 Al F15 O2 P' _chemical_formula_weight 830.58 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' 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 10.7749(4) _cell_length_b 12.9668(4) _cell_length_c 15.2829(5) _cell_angle_alpha 92.432(2) _cell_angle_beta 97.632(2) _cell_angle_gamma 111.204(2) _cell_volume 1963.59(11) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9950 _cell_measurement_theta_min 2.27 _cell_measurement_theta_max 33.11 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.34 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.405 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 848 _exptl_absorpt_coefficient_mu 0.194 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9378 _exptl_absorpt_correction_T_max 0.9873 _exptl_absorpt_process_details 'SCALE (Bruker, 2009)' _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' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 48867 _diffrn_reflns_av_R_equivalents 0.0292 _diffrn_reflns_av_sigmaI/netI 0.0334 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.69 _diffrn_reflns_theta_max 30.51 _reflns_number_total 11898 _reflns_number_gt 8699 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2 (Bruker, 2009)' _computing_cell_refinement 'Bruker APEX2 (Bruker, 2009)' _computing_data_reduction 'Bruker APEX2 (Bruker, 2009)' _computing_structure_solution 'SHELXTL (Sheldrick, 2008)' _computing_structure_refinement 'SHELXTL (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 2008)' _computing_publication_material 'SHELXTL (Sheldrick, 2008)' _refine_special_details ; A disordered CH2Cl2 solvent molecule was found in the crystal lattice, and the Platon Squeeze program was applied to take care of the solvent void (203 Ang^3) in the structure refinement. The SAME command was implemented to restrain the bond distances and angles of the disordered fluorophenyl ring(C13-C18 and F11-F15).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^)+(0.0874P)^2^+0.1053P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11898 _refine_ls_number_parameters 666 _refine_ls_number_restraints 81 _refine_ls_R_factor_all 0.0681 _refine_ls_R_factor_gt 0.0488 _refine_ls_wR_factor_ref 0.1545 _refine_ls_wR_factor_gt 0.1446 _refine_ls_goodness_of_fit_ref 1.115 _refine_ls_restrained_S_all 1.113 _refine_ls_shift/su_max 0.002 _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 0.49356(4) 0.21950(3) 0.29155(3) 0.02236(11) Uani 1 1 d . . . C1 C 0.53859(16) 0.08186(11) 0.29017(11) 0.0303(3) Uani 1 1 d D A . C2 C 0.53334(19) 0.01464(13) 0.21550(13) 0.0390(4) Uani 1 1 d D . . C3 C 0.5759(2) -0.07415(14) 0.21892(17) 0.0515(5) Uani 1 1 d D A . C4 C 0.6236(2) -0.09964(15) 0.29899(18) 0.0538(6) Uani 1 1 d D . . C5 C 0.62923(18) -0.03750(15) 0.37587(16) 0.0470(5) Uani 1 1 d D A . C6 C 0.58569(17) 0.05052(13) 0.36889(13) 0.0360(4) Uani 1 1 d D . . F1 F 0.48148(14) 0.03222(9) 0.13449(8) 0.0521(3) Uani 1 1 d D A . F2 F 0.56663(18) -0.13675(10) 0.14364(11) 0.0786(5) Uani 1 1 d D . . F3 F 0.66443(15) -0.18611(10) 0.30389(14) 0.0817(5) Uani 1 1 d D A . F4 F 0.67460(13) -0.06182(11) 0.45494(11) 0.0667(4) Uani 1 1 d D . . F5 F 0.59039(12) 0.10883(8) 0.44627(7) 0.0456(3) Uani 1 1 d D A . C7 C 0.47678(16) 0.26789(12) 0.16882(11) 0.0293(3) Uani 1 1 d . A . C8 C 0.3775(2) 0.30127(19) 0.12981(13) 0.0466(5) Uani 1 1 d . . . C9 C 0.3711(2) 0.3369(2) 0.04590(14) 0.0531(5) Uani 1 1 d . A . C10 C 0.4685(2) 0.33808(15) -0.00352(12) 0.0443(4) Uani 1 1 d . . . C11 C 0.56960(18) 0.30617(14) 0.03126(12) 0.0367(4) Uani 1 1 d . A . C12 C 0.57236(16) 0.27304(12) 0.11613(11) 0.0302(3) Uani 1 1 d . . . F6 F 0.27689(16) 0.30100(18) 0.17474(10) 0.0879(6) Uani 1 1 d . A . F7 F 0.27240(19) 0.37056(19) 0.01322(11) 0.0974(6) Uani 1 1 d . . . F8 F 0.46485(15) 0.37382(11) -0.08497(8) 0.0607(4) Uani 1 1 d . A . F9 F 0.66716(12) 0.30929(11) -0.01623(8) 0.0557(3) Uani 1 1 d . . . F10 F 0.67854(10) 0.24610(9) 0.14854(7) 0.0411(2) Uani 1 1 d . A . C13 C 0.3225(8) 0.1898(11) 0.3411(7) 0.029(3) Uani 0.604(7) 1 d PD A 1 C14 C 0.3020(7) 0.2305(8) 0.4197(6) 0.036(2) Uani 0.604(7) 1 d PD A 1 C15 C 0.1831(7) 0.2012(10) 0.4535(6) 0.0288(18) Uani 0.604(7) 1 d PD A 1 C16 C 0.0750(4) 0.1169(4) 0.4067(3) 0.0392(10) Uani 0.604(7) 1 d PD A 1 C17 C 0.0871(3) 0.0636(3) 0.3307(2) 0.0364(8) Uani 0.604(7) 1 d PD A 1 C18 C 0.2099(3) 0.0976(3) 0.3012(2) 0.0291(7) Uani 0.604(7) 1 d PD A 1 F11 F 0.4077(7) 0.3148(7) 0.4697(6) 0.0383(14) Uani 0.604(7) 1 d PD A 1 F12 F 0.1780(8) 0.2519(7) 0.5306(4) 0.048(3) Uani 0.604(7) 1 d PD A 1 F13 F -0.0434(6) 0.0851(4) 0.4374(5) 0.0513(11) Uani 0.604(7) 1 d PD A 1 F14 F -0.0217(2) -0.0196(3) 0.2858(2) 0.0611(11) Uani 0.604(7) 1 d PD A 1 F15 F 0.2157(2) 0.0439(3) 0.2243(2) 0.0413(7) Uani 0.604(7) 1 d PD A 1 C13A C 0.3228(12) 0.1851(16) 0.3445(11) 0.021(4) Uiso 0.396(7) 1 d PD A 2 C14A C 0.3123(9) 0.2360(9) 0.4235(7) 0.0134(19) Uiso 0.396(7) 1 d PD A 2 C15A C 0.1894(11) 0.2126(15) 0.4517(9) 0.029(3) Uiso 0.396(7) 1 d PD A 2 C16A C 0.0700(7) 0.1424(5) 0.4017(4) 0.0272(16) Uiso 0.396(7) 1 d PD A 2 C17A C 0.0730(4) 0.1015(4) 0.3170(3) 0.0272(11) Uiso 0.396(7) 1 d PD A 2 C18A C 0.1971(4) 0.1299(4) 0.2908(3) 0.0218(11) Uiso 0.396(7) 1 d PD A 2 F11A F 0.4231(13) 0.2999(12) 0.4799(10) 0.039(2) Uani 0.396(7) 1 d PD A 2 F12A F 0.1753(12) 0.2540(9) 0.5302(7) 0.047(4) Uani 0.396(7) 1 d PD A 2 F13A F -0.0507(8) 0.1161(6) 0.4296(7) 0.0397(12) Uani 0.396(7) 1 d PD A 2 F14A F -0.0418(3) 0.0393(4) 0.2641(2) 0.0426(11) Uani 0.396(7) 1 d PD A 2 F15A F 0.1977(3) 0.0875(4) 0.2074(2) 0.0334(9) Uani 0.396(7) 1 d PD A 2 C19 C 0.73017(14) 0.41771(11) 0.35690(10) 0.0259(3) Uani 1 1 d . . . C20 C 0.85831(14) 0.42357(12) 0.36356(10) 0.0255(3) Uani 1 1 d . A . C21 C 0.88853(17) 0.32090(14) 0.37800(13) 0.0358(4) Uani 1 1 d . . . H21A H 0.8040 0.2560 0.3699 0.054 Uiso 1 1 calc R A . H21B H 0.9366 0.3277 0.4384 0.054 Uiso 1 1 calc R . . H21C H 0.9448 0.3118 0.3351 0.054 Uiso 1 1 calc R . . C22 C 0.57836(17) 0.51486(15) 0.35028(16) 0.0463(5) Uani 1 1 d . . . H22A H 0.5792 0.5898 0.3432 0.069 Uiso 1 1 calc R A . H22B H 0.5500 0.4919 0.4070 0.069 Uiso 1 1 calc R . . H22C H 0.5152 0.4629 0.3017 0.069 Uiso 1 1 calc R . . C23 C 0.97017(14) 0.53712(12) 0.37175(10) 0.0271(3) Uani 1 1 d . . . H23A H 1.0380 0.5381 0.4226 0.032 Uiso 1 1 calc R A . H23B H 0.9307 0.5912 0.3900 0.032 Uiso 1 1 calc R . . O1 O 0.62341(10) 0.32754(8) 0.35933(8) 0.0290(2) Uani 1 1 d . A . O2 O 0.70765(12) 0.51470(9) 0.34879(11) 0.0475(4) Uani 1 1 d . A . P1 P 1.06579(3) 0.59636(3) 0.28216(2) 0.02232(10) Uani 1 1 d . A . C24 C 0.9478(2) 0.61799(19) 0.19289(17) 0.0246(5) Uani 0.592(2) 1 d P A 3 C25 C 0.9051(3) 0.7122(3) 0.2258(2) 0.0347(6) Uani 0.592(2) 1 d P A 3 H25A H 0.8419 0.7242 0.1788 0.052 Uiso 0.592(2) 1 calc PR A 3 H25B H 0.9849 0.7806 0.2415 0.052 Uiso 0.592(2) 1 calc PR A 3 H25C H 0.8612 0.6916 0.2781 0.052 Uiso 0.592(2) 1 calc PR A 3 C26 C 1.0141(3) 0.6504(3) 0.1088(2) 0.0340(7) Uani 0.592(2) 1 d P A 3 H26A H 0.9492 0.6615 0.0625 0.051 Uiso 0.592(2) 1 calc PR A 3 H26B H 1.0415 0.5909 0.0873 0.051 Uiso 0.592(2) 1 calc PR A 3 H26C H 1.0935 0.7194 0.1235 0.051 Uiso 0.592(2) 1 calc PR A 3 C27 C 0.8146(10) 0.5186(9) 0.1649(7) 0.0244(13) Uani 0.592(2) 1 d P A 3 H27A H 0.7584 0.5374 0.1174 0.037 Uiso 0.592(2) 1 calc PR A 3 H27B H 0.7670 0.5006 0.2159 0.037 Uiso 0.592(2) 1 calc PR A 3 H27C H 0.8335 0.4542 0.1436 0.037 Uiso 0.592(2) 1 calc PR A 3 C28 C 1.1986(2) 0.7248(2) 0.33907(17) 0.0264(5) Uani 0.592(2) 1 d P A 3 C29 C 1.1411(10) 0.7869(8) 0.4017(8) 0.0353(16) Uani 0.592(2) 1 d P A 3 H29A H 1.2137 0.8545 0.4312 0.053 Uiso 0.592(2) 1 calc PR A 3 H29B H 1.1018 0.7385 0.4464 0.053 Uiso 0.592(2) 1 calc PR A 3 H29C H 1.0713 0.8070 0.3671 0.053 Uiso 0.592(2) 1 calc PR A 3 C30 C 1.2610(3) 0.8047(3) 0.2704(2) 0.0352(7) Uani 0.592(2) 1 d P A 3 H30A H 1.3318 0.8723 0.3014 0.053 Uiso 0.592(2) 1 calc PR A 3 H30B H 1.1907 0.8242 0.2358 0.053 Uiso 0.592(2) 1 calc PR A 3 H30C H 1.2999 0.7680 0.2305 0.053 Uiso 0.592(2) 1 calc PR A 3 C31 C 1.3146(6) 0.7044(4) 0.3970(4) 0.0332(10) Uani 0.592(2) 1 d P A 3 H31A H 1.3817 0.7757 0.4251 0.050 Uiso 0.592(2) 1 calc PR A 3 H31B H 1.3572 0.6680 0.3598 0.050 Uiso 0.592(2) 1 calc PR A 3 H31C H 1.2788 0.6567 0.4429 0.050 Uiso 0.592(2) 1 calc PR A 3 C32 C 1.1425(2) 0.4930(2) 0.24243(17) 0.0257(5) Uani 0.592(2) 1 d P A 3 C33 C 1.2577(3) 0.5498(3) 0.1905(2) 0.0335(6) Uani 0.592(2) 1 d P A 3 H33A H 1.2952 0.4958 0.1713 0.050 Uiso 0.592(2) 1 calc PR A 3 H33B H 1.3284 0.6113 0.2287 0.050 Uiso 0.592(2) 1 calc PR A 3 H33C H 1.2229 0.5786 0.1385 0.050 Uiso 0.592(2) 1 calc PR A 3 C34 C 1.1987(9) 0.4438(7) 0.3214(6) 0.0277(12) Uani 0.592(2) 1 d P A 3 H34A H 1.2377 0.3922 0.2993 0.041 Uiso 0.592(2) 1 calc PR A 3 H34B H 1.1255 0.4039 0.3536 0.041 Uiso 0.592(2) 1 calc PR A 3 H34C H 1.2684 0.5039 0.3613 0.041 Uiso 0.592(2) 1 calc PR A 3 C35 C 1.0336(3) 0.3958(2) 0.1809(2) 0.0322(6) Uani 0.592(2) 1 d P A 3 H35A H 1.0736 0.3439 0.1609 0.048 Uiso 0.592(2) 1 calc PR A 3 H35B H 0.9979 0.4249 0.1293 0.048 Uiso 0.592(2) 1 calc PR A 3 H35C H 0.9603 0.3571 0.2133 0.048 Uiso 0.592(2) 1 calc PR A 3 C24A C 0.9795(4) 0.5376(3) 0.1659(2) 0.0264(8) Uani 0.408(2) 1 d P A 4 C25A C 1.0395(5) 0.6077(5) 0.0910(3) 0.0379(11) Uani 0.408(2) 1 d P A 4 H25D H 0.9888 0.5697 0.0333 0.057 Uiso 0.408(2) 1 calc PR A 4 H25E H 1.1342 0.6165 0.0939 0.057 Uiso 0.408(2) 1 calc PR A 4 H25F H 1.0333 0.6810 0.0987 0.057 Uiso 0.408(2) 1 calc PR A 4 C26A C 0.9867(5) 0.4215(4) 0.1494(3) 0.0330(9) Uani 0.408(2) 1 d P A 4 H26D H 0.9431 0.3896 0.0889 0.050 Uiso 0.408(2) 1 calc PR A 4 H26E H 0.9404 0.3729 0.1919 0.050 Uiso 0.408(2) 1 calc PR A 4 H26F H 1.0813 0.4286 0.1572 0.050 Uiso 0.408(2) 1 calc PR A 4 C27A C 0.8329(15) 0.5120(14) 0.1556(11) 0.026(2) Uani 0.408(2) 1 d P A 4 H27D H 0.7915 0.4818 0.0943 0.039 Uiso 0.408(2) 1 calc PR A 4 H27E H 0.8167 0.5800 0.1695 0.039 Uiso 0.408(2) 1 calc PR A 4 H27F H 0.7931 0.4571 0.1960 0.039 Uiso 0.408(2) 1 calc PR A 4 C28A C 1.0897(4) 0.7570(3) 0.2909(3) 0.0285(8) Uani 0.408(2) 1 d P A 4 C29A C 0.9579(4) 0.7713(4) 0.2505(4) 0.0396(11) Uani 0.408(2) 1 d P A 4 H29D H 0.9714 0.8504 0.2552 0.059 Uiso 0.408(2) 1 calc PR A 4 H29E H 0.8851 0.7309 0.2828 0.059 Uiso 0.408(2) 1 calc PR A 4 H29F H 0.9336 0.7416 0.1879 0.059 Uiso 0.408(2) 1 calc PR A 4 C30A C 1.2059(5) 0.8294(3) 0.2452(4) 0.0355(10) Uani 0.408(2) 1 d P A 4 H30D H 1.2128 0.9069 0.2517 0.053 Uiso 0.408(2) 1 calc PR A 4 H30E H 1.1881 0.8030 0.1821 0.053 Uiso 0.408(2) 1 calc PR A 4 H30F H 1.2907 0.8244 0.2728 0.053 Uiso 0.408(2) 1 calc PR A 4 C31A C 1.1173(14) 0.8007(12) 0.3888(10) 0.035(2) Uani 0.408(2) 1 d P A 4 H31D H 1.1293 0.8795 0.3938 0.052 Uiso 0.408(2) 1 calc PR A 4 H31E H 1.1993 0.7923 0.4179 0.052 Uiso 0.408(2) 1 calc PR A 4 H31F H 1.0409 0.7585 0.4175 0.052 Uiso 0.408(2) 1 calc PR A 4 C32A C 1.2342(3) 0.5880(3) 0.3083(2) 0.0236(7) Uani 0.408(2) 1 d P A 4 C33A C 1.3171(4) 0.6107(4) 0.2307(3) 0.0330(9) Uani 0.408(2) 1 d P A 4 H33D H 1.4048 0.6052 0.2498 0.050 Uiso 0.408(2) 1 calc PR A 4 H33E H 1.3308 0.6855 0.2135 0.050 Uiso 0.408(2) 1 calc PR A 4 H33F H 1.2681 0.5558 0.1800 0.050 Uiso 0.408(2) 1 calc PR A 4 C34A C 1.3195(8) 0.6667(5) 0.3913(6) 0.0305(13) Uani 0.408(2) 1 d P A 4 H34D H 1.4081 0.6605 0.4027 0.046 Uiso 0.408(2) 1 calc PR A 4 H34E H 1.2734 0.6460 0.4426 0.046 Uiso 0.408(2) 1 calc PR A 4 H34F H 1.3310 0.7435 0.3810 0.046 Uiso 0.408(2) 1 calc PR A 4 C35A C 1.2131(16) 0.4707(9) 0.3336(11) 0.037(3) Uani 0.408(2) 1 d P A 4 H35D H 1.3007 0.4633 0.3475 0.055 Uiso 0.408(2) 1 calc PR A 4 H35E H 1.1578 0.4163 0.2839 0.055 Uiso 0.408(2) 1 calc PR A 4 H35F H 1.1673 0.4575 0.3857 0.055 Uiso 0.408(2) 1 calc PR A 4 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 0.0189(2) 0.01980(19) 0.0269(2) 0.00554(16) 0.00283(16) 0.00538(15) C1 0.0267(7) 0.0200(6) 0.0416(9) 0.0074(6) 0.0031(6) 0.0058(6) C2 0.0407(9) 0.0252(7) 0.0497(11) 0.0037(7) 0.0090(8) 0.0100(7) C3 0.0521(12) 0.0271(8) 0.0793(16) 0.0031(9) 0.0238(11) 0.0152(8) C4 0.0436(10) 0.0265(8) 0.1013(19) 0.0207(10) 0.0236(11) 0.0191(8) C5 0.0321(9) 0.0331(8) 0.0761(15) 0.0282(9) 0.0047(9) 0.0115(7) C6 0.0324(8) 0.0247(7) 0.0480(10) 0.0101(7) 0.0044(7) 0.0071(6) F1 0.0721(8) 0.0359(5) 0.0415(6) -0.0037(4) 0.0014(6) 0.0155(5) F2 0.1034(12) 0.0401(6) 0.0994(12) -0.0105(7) 0.0375(9) 0.0296(7) F3 0.0732(10) 0.0421(7) 0.1531(16) 0.0322(8) 0.0357(10) 0.0401(7) F4 0.0561(8) 0.0562(7) 0.0928(11) 0.0455(7) 0.0034(7) 0.0256(6) F5 0.0518(7) 0.0384(5) 0.0406(6) 0.0144(4) -0.0011(5) 0.0114(5) C7 0.0303(8) 0.0286(7) 0.0300(8) 0.0092(6) 0.0066(6) 0.0108(6) C8 0.0474(11) 0.0717(13) 0.0378(10) 0.0253(9) 0.0165(8) 0.0367(10) C9 0.0627(13) 0.0746(14) 0.0411(11) 0.0283(10) 0.0116(10) 0.0445(12) C10 0.0621(12) 0.0410(9) 0.0293(9) 0.0153(7) 0.0111(8) 0.0160(9) C11 0.0394(9) 0.0337(8) 0.0321(9) 0.0065(7) 0.0139(7) 0.0044(7) C12 0.0277(7) 0.0272(7) 0.0323(8) 0.0052(6) 0.0067(6) 0.0052(6) F6 0.0821(10) 0.1837(18) 0.0575(8) 0.0658(10) 0.0404(8) 0.1037(12) F7 0.1129(13) 0.1770(18) 0.0619(9) 0.0678(11) 0.0292(9) 0.1127(14) F8 0.0889(10) 0.0632(7) 0.0314(6) 0.0237(5) 0.0140(6) 0.0262(7) F9 0.0517(7) 0.0690(8) 0.0440(7) 0.0135(6) 0.0276(5) 0.0117(6) F10 0.0280(5) 0.0510(6) 0.0456(6) 0.0098(5) 0.0112(4) 0.0137(4) C13 0.022(3) 0.030(4) 0.027(3) 0.0088(16) 0.0034(11) 0.0005(11) C14 0.026(3) 0.034(3) 0.035(3) 0.0085(14) -0.0049(15) -0.0001(16) C15 0.031(3) 0.031(3) 0.027(2) 0.0116(18) 0.0134(14) 0.0114(15) C16 0.0253(16) 0.031(2) 0.062(3) 0.0087(18) 0.0216(14) 0.0058(15) C17 0.0208(13) 0.0258(15) 0.054(2) -0.0052(13) 0.0011(12) 0.0009(11) C18 0.0261(13) 0.0232(14) 0.0378(16) -0.0020(12) 0.0038(11) 0.0099(11) F11 0.024(2) 0.048(2) 0.030(3) -0.0120(19) 0.0003(15) 0.0017(18) F12 0.047(4) 0.073(5) 0.027(3) -0.011(3) 0.007(3) 0.025(3) F13 0.0294(13) 0.049(2) 0.075(2) 0.003(2) 0.0279(14) 0.0083(15) F14 0.0227(9) 0.0486(18) 0.0907(19) -0.0292(14) 0.0097(10) -0.0080(10) F15 0.0320(10) 0.0389(13) 0.0465(14) -0.0170(11) 0.0054(9) 0.0080(9) F11A 0.027(2) 0.058(4) 0.027(3) -0.004(2) -0.0083(16) 0.0158(19) F12A 0.043(6) 0.043(5) 0.055(7) 0.002(4) 0.027(5) 0.008(4) F13A 0.0268(17) 0.040(3) 0.054(2) 0.003(2) 0.0170(15) 0.011(2) F14A 0.0186(12) 0.035(2) 0.063(2) -0.0135(14) -0.0017(11) 0.0017(11) F15A 0.0298(14) 0.0373(19) 0.0293(15) -0.0071(13) 0.0034(11) 0.0096(13) C19 0.0206(6) 0.0210(6) 0.0337(8) 0.0009(5) 0.0069(6) 0.0041(5) C20 0.0199(6) 0.0268(6) 0.0276(7) 0.0012(5) 0.0044(5) 0.0061(5) C21 0.0284(8) 0.0372(8) 0.0441(10) 0.0089(7) 0.0037(7) 0.0152(7) C22 0.0275(8) 0.0325(8) 0.0838(15) 0.0007(9) 0.0181(9) 0.0145(7) C23 0.0181(6) 0.0327(7) 0.0244(7) -0.0024(6) 0.0072(5) 0.0018(5) O1 0.0210(5) 0.0232(5) 0.0373(6) 0.0043(4) 0.0050(4) 0.0015(4) O2 0.0262(6) 0.0235(5) 0.0988(12) 0.0114(6) 0.0265(7) 0.0102(5) P1 0.01507(16) 0.03025(18) 0.01957(18) 0.00035(13) 0.00288(13) 0.00616(13) C24 0.0216(11) 0.0223(10) 0.0256(12) 0.0041(9) -0.0018(9) 0.0050(9) C25 0.0293(14) 0.0280(14) 0.0466(18) 0.0064(12) 0.0003(12) 0.0121(12) C26 0.0266(15) 0.0384(17) 0.0293(17) 0.0134(13) -0.0039(12) 0.0045(13) C27 0.015(3) 0.0286(19) 0.027(2) -0.0020(16) -0.0033(19) 0.008(2) C28 0.0161(10) 0.0306(12) 0.0270(13) 0.0015(9) 0.0026(9) 0.0024(9) C29 0.026(3) 0.033(3) 0.035(3) -0.009(2) 0.002(2) 0.0000(18) C30 0.0276(15) 0.0293(14) 0.0399(17) 0.0043(12) 0.0080(13) -0.0008(12) C31 0.0259(17) 0.034(2) 0.0297(17) -0.003(2) -0.0032(12) 0.0033(18) C32 0.0216(11) 0.0321(12) 0.0249(12) 0.0049(9) 0.0054(9) 0.0110(9) C33 0.0304(14) 0.0439(16) 0.0308(15) 0.0083(13) 0.0153(12) 0.0152(13) C34 0.0191(19) 0.038(3) 0.031(3) 0.014(2) 0.0044(17) 0.016(2) C35 0.0333(15) 0.0292(13) 0.0335(16) -0.0031(11) 0.0020(12) 0.0126(12) C24A 0.0249(17) 0.0336(18) 0.0198(17) 0.0043(13) 0.0044(13) 0.0095(14) C25A 0.037(3) 0.051(3) 0.024(2) 0.018(2) 0.0083(18) 0.012(2) C26A 0.035(2) 0.033(2) 0.027(2) -0.0015(16) 0.0055(18) 0.0090(18) C27A 0.017(4) 0.033(4) 0.031(4) 0.008(3) 0.005(2) 0.013(2) C28A 0.0237(17) 0.0217(15) 0.037(2) 0.0035(14) 0.0047(15) 0.0046(13) C29A 0.027(2) 0.026(2) 0.067(3) 0.008(2) 0.006(2) 0.0111(19) C30A 0.029(2) 0.0264(19) 0.048(3) 0.0101(18) 0.015(2) 0.0026(17) C31A 0.033(5) 0.028(3) 0.037(5) -0.006(3) 0.009(4) 0.003(3) C32A 0.0157(14) 0.0326(17) 0.0228(17) 0.0031(13) 0.0047(12) 0.0088(13) C33A 0.0210(18) 0.045(2) 0.038(2) 0.0058(19) 0.0157(17) 0.0134(18) C34A 0.018(2) 0.035(3) 0.031(3) 0.000(3) -0.0046(16) 0.005(3) C35A 0.028(4) 0.040(5) 0.047(5) 0.006(4) 0.012(3) 0.017(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 O1 1.7513(11) . ? Al1 C13 2.000(9) . ? Al1 C7 2.0091(16) . ? Al1 C1 2.0117(16) . ? Al1 C13A 2.018(13) . ? C1 C6 1.378(2) . ? C1 C2 1.388(2) . ? C2 F1 1.353(2) . ? C2 C3 1.385(3) . ? C3 F2 1.351(3) . ? C3 C4 1.364(3) . ? C4 F3 1.346(2) . ? C4 C5 1.378(3) . ? C5 F4 1.336(2) . ? C5 C6 1.385(2) . ? C6 F5 1.361(2) . ? C7 C8 1.369(2) . ? C7 C12 1.374(2) . ? C8 F6 1.358(2) . ? C8 C9 1.383(3) . ? C9 F7 1.336(2) . ? C9 C10 1.368(3) . ? C10 F8 1.347(2) . ? C10 C11 1.353(3) . ? C11 F9 1.345(2) . ? C11 C12 1.384(2) . ? C12 F10 1.353(2) . ? C13 C14 1.369(8) . ? C13 C18 1.401(8) . ? C14 F11 1.368(7) . ? C14 C15 1.377(7) . ? C15 F12 1.342(7) . ? C15 C16 1.362(7) . ? C16 F13 1.346(5) . ? C16 C17 1.371(5) . ? C17 F14 1.348(3) . ? C17 C18 1.380(4) . ? C18 F15 1.360(3) . ? C13A C14A 1.389(9) . ? C13A C18A 1.406(11) . ? C14A F11A 1.343(10) . ? C14A C15A 1.380(10) . ? C15A F12A 1.342(10) . ? C15A C16A 1.379(10) . ? C16A F13A 1.352(9) . ? C16A C17A 1.387(7) . ? C17A F14A 1.339(5) . ? C17A C18A 1.372(6) . ? C18A F15A 1.368(5) . ? C19 O1 1.3167(16) . ? C19 C20 1.345(2) . ? C19 O2 1.3718(18) . ? C20 C21 1.499(2) . ? C20 C23 1.5155(19) . ? C22 O2 1.397(2) . ? C23 P1 1.8487(14) . ? P1 C24 1.840(2) . ? P1 C28 1.844(2) . ? P1 C32A 1.848(3) . ? P1 C24A 1.881(4) . ? P1 C32 1.927(3) . ? P1 C28A 2.001(4) . ? C24 C27 1.535(11) . ? C24 C25 1.540(4) . ? C24 C26 1.553(4) . ? C28 C31 1.543(6) . ? C28 C29 1.550(11) . ? C28 C30 1.550(4) . ? C32 C33 1.537(3) . ? C32 C34 1.543(9) . ? C32 C35 1.545(4) . ? C24A C27A 1.477(15) . ? C24A C26A 1.547(6) . ? C24A C25A 1.552(6) . ? C28A C31A 1.529(17) . ? C28A C30A 1.541(5) . ? C28A C29A 1.550(6) . ? C32A C35A 1.529(13) . ? C32A C34A 1.548(8) . ? C32A C33A 1.553(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 O1 Al1 C13 108.7(2) . . ? O1 Al1 C7 107.97(6) . . ? C13 Al1 C7 110.8(4) . . ? O1 Al1 C1 109.38(6) . . ? C13 Al1 C1 109.5(5) . . ? C7 Al1 C1 110.51(7) . . ? O1 Al1 C13A 108.6(3) . . ? C13 Al1 C13A 2.3(12) . . ? C7 Al1 C13A 112.8(6) . . ? C1 Al1 C13A 107.5(7) . . ? C6 C1 C2 114.22(15) . . ? C6 C1 Al1 119.37(12) . . ? C2 C1 Al1 126.33(13) . . ? F1 C2 C3 116.48(17) . . ? F1 C2 C1 120.23(15) . . ? C3 C2 C1 123.27(19) . . ? F2 C3 C4 120.36(18) . . ? F2 C3 C2 120.1(2) . . ? C4 C3 C2 119.5(2) . . ? F3 C4 C3 120.5(2) . . ? F3 C4 C5 119.3(2) . . ? C3 C4 C5 120.17(17) . . ? F4 C5 C4 120.99(17) . . ? F4 C5 C6 120.9(2) . . ? C4 C5 C6 118.08(19) . . ? F5 C6 C1 118.81(14) . . ? F5 C6 C5 116.49(17) . . ? C1 C6 C5 124.70(18) . . ? C8 C7 C12 113.30(15) . . ? C8 C7 Al1 126.19(13) . . ? C12 C7 Al1 120.49(12) . . ? F6 C8 C7 119.54(16) . . ? F6 C8 C9 115.82(17) . . ? C7 C8 C9 124.64(18) . . ? F7 C9 C10 120.03(18) . . ? F7 C9 C8 121.05(19) . . ? C10 C9 C8 118.92(19) . . ? F8 C10 C11 120.82(18) . . ? F8 C10 C9 119.78(19) . . ? C11 C10 C9 119.37(17) . . ? F9 C11 C10 119.69(16) . . ? F9 C11 C12 121.01(17) . . ? C10 C11 C12 119.28(16) . . ? F10 C12 C7 118.95(14) . . ? F10 C12 C11 116.58(15) . . ? C7 C12 C11 124.46(16) . . ? C14 C13 C18 111.7(7) . . ? C14 C13 Al1 129.8(5) . . ? C18 C13 Al1 116.9(5) . . ? F11 C14 C13 118.1(7) . . ? F11 C14 C15 114.3(7) . . ? C13 C14 C15 127.4(7) . . ? F12 C15 C16 122.9(6) . . ? F12 C15 C14 120.4(6) . . ? C16 C15 C14 116.6(6) . . ? F13 C16 C15 118.8(5) . . ? F13 C16 C17 120.5(4) . . ? C15 C16 C17 120.7(4) . . ? F14 C17 C16 119.3(3) . . ? F14 C17 C18 121.5(3) . . ? C16 C17 C18 119.2(3) . . ? F15 C18 C17 116.9(2) . . ? F15 C18 C13 119.3(4) . . ? C17 C18 C13 123.5(4) . . ? C14A C13A C18A 112.7(10) . . ? C14A C13A Al1 125.3(7) . . ? C18A C13A Al1 119.7(8) . . ? F11A C14A C15A 117.4(10) . . ? F11A C14A C13A 120.8(10) . . ? C15A C14A C13A 121.3(9) . . ? F12A C15A C16A 114.1(9) . . ? F12A C15A C14A 123.5(9) . . ? C16A C15A C14A 122.4(9) . . ? F13A C16A C15A 123.1(8) . . ? F13A C16A C17A 118.4(6) . . ? C15A C16A C17A 118.4(7) . . ? F14A C17A C18A 122.8(4) . . ? F14A C17A C16A 120.2(4) . . ? C18A C17A C16A 117.0(5) . . ? F15A C18A C17A 115.9(4) . . ? F15A C18A C13A 117.1(6) . . ? C17A C18A C13A 126.4(7) . . ? O1 C19 C20 126.13(14) . . ? O1 C19 O2 116.33(13) . . ? C20 C19 O2 117.52(12) . . ? C19 C20 C21 119.32(13) . . ? C19 C20 C23 118.56(13) . . ? C21 C20 C23 121.31(13) . . ? C20 C23 P1 124.86(11) . . ? C19 O1 Al1 142.69(11) . . ? C19 O2 C22 119.66(12) . . ? C24 P1 C28 114.84(11) . . ? C24 P1 C32A 143.39(14) . . ? C28 P1 C32A 65.44(14) . . ? C24 P1 C23 107.79(9) . . ? C28 P1 C23 102.78(9) . . ? C32A P1 C23 107.57(12) . . ? C24 P1 C24A 40.14(14) . . ? C28 P1 C24A 138.34(14) . . ? C32A P1 C24A 113.17(16) . . ? C23 P1 C24A 115.94(12) . . ? C24 P1 C32 111.87(11) . . ? C28 P1 C32 110.94(11) . . ? C32A P1 C32 46.85(13) . . ? C23 P1 C32 107.96(9) . . ? C24A P1 C32 72.19(14) . . ? C24 P1 C28A 71.07(14) . . ? C28 P1 C28A 45.63(14) . . ? C32A P1 C28A 107.98(16) . . ? C23 P1 C28A 105.37(12) . . ? C24A P1 C28A 106.26(16) . . ? C32 P1 C28A 143.28(13) . . ? C27 C24 C25 104.4(4) . . ? C27 C24 C26 107.9(4) . . ? C25 C24 C26 108.9(2) . . ? C27 C24 P1 115.1(5) . . ? C25 C24 P1 108.84(18) . . ? C26 C24 P1 111.28(19) . . ? C31 C28 C29 106.3(4) . . ? C31 C28 C30 107.6(3) . . ? C29 C28 C30 107.7(4) . . ? C31 C28 P1 113.5(2) . . ? C29 C28 P1 111.2(4) . . ? C30 C28 P1 110.27(18) . . ? C33 C32 C34 108.3(4) . . ? C33 C32 C35 108.2(2) . . ? C34 C32 C35 107.9(4) . . ? C33 C32 P1 111.02(18) . . ? C34 C32 P1 111.2(4) . . ? C35 C32 P1 110.07(18) . . ? C27A C24A C26A 102.6(7) . . ? C27A C24A C25A 110.0(7) . . ? C26A C24A C25A 107.8(4) . . ? C27A C24A P1 111.8(6) . . ? C26A C24A P1 108.0(3) . . ? C25A C24A P1 115.7(3) . . ? C31A C28A C30A 108.9(7) . . ? C31A C28A C29A 106.2(6) . . ? C30A C28A C29A 108.9(4) . . ? C31A C28A P1 108.9(5) . . ? C30A C28A P1 113.2(3) . . ? C29A C28A P1 110.6(3) . . ? C35A C32A C34A 105.3(7) . . ? C35A C32A C33A 108.6(7) . . ? C34A C32A C33A 108.9(4) . . ? C35A C32A P1 107.3(6) . . ? C34A C32A P1 111.8(3) . . ? C33A C32A P1 114.4(3) . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 30.51 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.614 _refine_diff_density_min -0.515 _refine_diff_density_rms 0.061 loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.000 0.000 0.000 202 58 ' ' _platon_squeeze_details ; ;