Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2005 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 # 1. SUBMISSION DETAILS _publ_contact_author 'Prof. Dr. Ingo Krossing' _publ_contact_author_address ; Laboratory of Inorganic and Coordination Chemistry, EPFL-BCH, 1015 Lausanne, Switzerland ; _publ_contact_author_phone '++41 21 693 9315' _publ_contact_author_fax '++49 721 608 49 52' _publ_contact_author_email ingo.krossing@epfl.ch _publ_contact_letter ; Please store this CIF submission in the CCDC data base. ; # 3. TITLE AND AUTHOR LIST _publ_section_title ; Preparation of Stable AsBr4+ and I2As-PI3+ Salts. Why didnt we Succeed to Prepare AsI4+ and As2X5+? A Combined Experimental and Theoretical Study. ; loop_ _publ_author_name _publ_author_address M.Gonsior ; Institut fuer anorganische Chemie, Universitaet Karlsruhe, Engesserstr. Geb. 30.45, Germany ; 'Prof. Dr. Ingo Krossing' ; Laboratory of Inorganic and Coordination Chemistry, EPFL-BCH, 1015 Lausanne, Switzerland ; _publ_manuscript_creation 'RTF-File created by CIF6 (H.Schwenk 1996)' _publ_contact_author_name 'Prof. Dr. Ingo Krossing' data_p21n _database_code_depnum_ccdc_archive 'CCDC 256551' _publ_manuscript_creation 'RTF-File created by CIF6 (H.Schwenk 1996)' _audit_creation_method SHELXL-97 _chemical_name_systematic ; [(RO)2AlF(THF)]2 (R = C(CF3)3) ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H16 Al2 F38 O6' _chemical_formula_weight 1176.33 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Al Al 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 '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 9.6522(19) _cell_length_b 12.727(3) _cell_length_c 15.596(3) _cell_angle_alpha 90.00 _cell_angle_beta 96.34(3) _cell_angle_gamma 90.00 _cell_volume 1904.1(7) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 3207 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plates _exptl_crystal_colour colorless _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.6 _exptl_crystal_size_min 0.8 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.052 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1152 _exptl_absorpt_coefficient_mu 0.304 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; crystal mounted in PFE oil ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'IPDS II (STOE)' _diffrn_measurement_method 'Image Plate Technique' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7799 _diffrn_reflns_av_R_equivalents 0.0411 _diffrn_reflns_av_sigmaI/netI 0.0353 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.07 _diffrn_reflns_theta_max 25.85 _reflns_number_total 3426 _reflns_number_gt 2749 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'XPOSE (STOE)' _computing_cell_refinement 'CELL (STOE)' _computing_data_reduction 'XRED (STOE)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics RESVIEW _computing_publication_material RESVIEW _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^)+(0.0446P)^2^+0.1223P] 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 SHELXL _refine_ls_extinction_coef 0.0004(7) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 3426 _refine_ls_number_parameters 349 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0435 _refine_ls_R_factor_gt 0.0301 _refine_ls_wR_factor_ref 0.0750 _refine_ls_wR_factor_gt 0.0710 _refine_ls_goodness_of_fit_ref 1.009 _refine_ls_restrained_S_all 1.009 _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 0.05607(6) 0.40927(4) 0.95793(3) 0.01510(14) Uani 1 1 d . . . F10 F -0.25227(13) 0.39318(9) 0.82413(7) 0.0288(3) Uani 1 1 d . . . F01 F 0.06189(11) 0.47282(8) 1.06075(6) 0.0184(2) Uani 1 1 d . . . F15 F -0.30769(14) 0.10270(10) 0.92823(8) 0.0326(3) Uani 1 1 d . . . F4 F -0.04253(12) 0.52624(10) 0.75603(7) 0.0302(3) Uani 1 1 d . . . F13 F -0.23926(13) 0.20204(9) 1.03630(7) 0.0296(3) Uani 1 1 d . . . F1 F 0.30328(15) 0.33474(9) 0.76555(8) 0.0356(3) Uani 1 1 d . . . O2 O -0.07592(13) 0.31711(10) 0.95176(7) 0.0188(3) Uani 1 1 d . . . F11 F -0.37874(12) 0.32151(10) 0.91257(7) 0.0288(3) Uani 1 1 d . . . F16 F -0.06235(13) 0.26036(10) 0.76869(7) 0.0306(3) Uani 1 1 d . . . F17 F 0.05693(12) 0.17211(10) 0.86852(7) 0.0318(3) Uani 1 1 d . . . F7 F 0.30121(14) 0.58256(10) 0.92971(7) 0.0314(3) Uani 1 1 d . . . F14 F -0.09547(14) 0.09441(10) 0.98846(8) 0.0344(3) Uani 1 1 d . . . F2 F 0.32093(14) 0.47099(10) 0.68581(7) 0.0317(3) Uani 1 1 d . . . F5 F 0.07290(13) 0.65121(9) 0.82375(7) 0.0277(3) Uani 1 1 d . . . F6 F 0.11286(13) 0.61025(10) 0.69425(7) 0.0300(3) Uani 1 1 d . . . F12 F -0.35089(13) 0.24467(10) 0.79283(7) 0.0298(3) Uani 1 1 d . . . O3 O 0.19914(14) 0.32059(10) 1.00992(7) 0.0192(3) Uani 1 1 d . . . F18 F -0.13123(14) 0.10650(10) 0.80221(8) 0.0350(3) Uani 1 1 d . . . F8 F 0.43581(13) 0.49006(10) 0.85983(8) 0.0330(3) Uani 1 1 d . . . O1 O 0.14237(14) 0.42742(10) 0.86800(8) 0.0197(3) Uani 1 1 d . . . F3 F 0.12513(15) 0.38894(11) 0.68303(7) 0.0376(3) Uani 1 1 d . . . F9 F 0.35305(13) 0.63531(9) 0.80609(7) 0.0290(3) Uani 1 1 d . . . C6 C -0.2862(2) 0.30251(16) 0.85717(11) 0.0220(4) Uani 1 1 d . . . C5 C -0.1556(2) 0.24677(14) 0.90323(11) 0.0187(4) Uani 1 1 d . . . C7 C -0.2010(2) 0.16008(16) 0.96468(12) 0.0249(4) Uani 1 1 d . . . C8 C -0.0721(2) 0.19457(16) 0.83459(12) 0.0245(4) Uani 1 1 d . . . C2 C 0.2381(2) 0.42001(16) 0.73493(12) 0.0272(5) Uani 1 1 d . . . C03 C 0.2679(2) 0.16272(18) 1.07872(14) 0.0282(5) Uani 1 1 d . . . C3 C 0.0821(2) 0.57019(16) 0.76974(12) 0.0235(4) Uani 1 1 d . . . C04 C 0.1820(2) 0.25922(17) 1.08829(12) 0.0248(4) Uani 1 1 d . . . C02 C 0.3921(2) 0.20600(19) 1.03846(14) 0.0304(5) Uani 1 1 d . . . C1 C 0.1930(2) 0.49051(15) 0.80829(10) 0.0181(4) Uani 1 1 d . . . C4 C 0.3226(2) 0.55104(16) 0.85087(12) 0.0249(4) Uani 1 1 d . . . C01 C 0.3281(2) 0.28700(19) 0.97494(13) 0.0279(5) Uani 1 1 d . . . H7 H 0.086(3) 0.2466(18) 1.0885(13) 0.026(6) Uiso 1 1 d . . . H1 H 0.383(3) 0.346(2) 0.9694(14) 0.029(6) Uiso 1 1 d . . . H2 H 0.298(3) 0.257(2) 0.9188(16) 0.034(6) Uiso 1 1 d . . . H8 H 0.223(3) 0.3011(19) 1.1376(15) 0.033(6) Uiso 1 1 d . . . H3 H 0.440(3) 0.155(2) 1.0082(14) 0.033(6) Uiso 1 1 d . . . H5 H 0.294(3) 0.127(2) 1.1324(17) 0.041(7) Uiso 1 1 d . . . H6 H 0.217(3) 0.117(2) 1.0439(17) 0.040(7) Uiso 1 1 d . . . H4 H 0.461(3) 0.244(2) 1.0856(16) 0.044(7) Uiso 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 0.0140(3) 0.0147(3) 0.0170(2) -0.00010(19) 0.00375(19) 0.0004(2) F10 0.0283(7) 0.0251(6) 0.0320(6) 0.0064(5) -0.0016(5) -0.0005(5) F01 0.0195(6) 0.0177(5) 0.0179(5) -0.0004(4) 0.0017(4) 0.0030(4) F15 0.0302(7) 0.0244(6) 0.0438(6) -0.0016(5) 0.0062(5) -0.0120(6) F4 0.0202(6) 0.0389(7) 0.0309(6) 0.0087(5) 0.0001(5) -0.0029(5) F13 0.0350(7) 0.0288(7) 0.0269(5) 0.0018(5) 0.0122(5) -0.0052(5) F1 0.0509(9) 0.0209(6) 0.0392(6) -0.0007(5) 0.0242(6) 0.0082(6) O2 0.0173(7) 0.0194(7) 0.0200(6) -0.0013(5) 0.0031(5) -0.0025(5) F11 0.0186(6) 0.0383(7) 0.0303(6) -0.0040(5) 0.0062(5) 0.0079(5) F16 0.0294(7) 0.0394(7) 0.0246(5) -0.0043(5) 0.0108(5) -0.0028(6) F17 0.0206(6) 0.0376(7) 0.0378(6) -0.0098(5) 0.0052(5) 0.0075(5) F7 0.0355(7) 0.0350(7) 0.0236(5) -0.0069(5) 0.0023(5) -0.0062(6) F14 0.0336(7) 0.0228(6) 0.0464(7) 0.0079(5) 0.0035(6) 0.0046(6) F2 0.0404(8) 0.0297(7) 0.0289(5) -0.0014(5) 0.0213(5) -0.0050(6) F5 0.0308(7) 0.0208(6) 0.0331(6) 0.0035(5) 0.0110(5) 0.0069(5) F6 0.0324(7) 0.0351(7) 0.0233(5) 0.0122(5) 0.0070(5) 0.0014(5) F12 0.0232(6) 0.0386(7) 0.0266(5) -0.0085(5) -0.0021(5) -0.0049(5) O3 0.0188(7) 0.0209(7) 0.0187(6) 0.0033(5) 0.0057(5) 0.0052(6) F18 0.0344(7) 0.0283(7) 0.0432(7) -0.0183(5) 0.0090(6) -0.0050(6) F8 0.0183(6) 0.0339(7) 0.0468(7) 0.0065(5) 0.0037(5) 0.0030(5) O1 0.0220(7) 0.0172(7) 0.0213(6) 0.0028(5) 0.0084(5) 0.0009(6) F3 0.0469(8) 0.0395(8) 0.0274(6) -0.0115(5) 0.0087(6) -0.0167(6) F9 0.0279(7) 0.0225(6) 0.0371(6) 0.0046(5) 0.0056(5) -0.0076(5) C6 0.0192(10) 0.0242(10) 0.0227(8) -0.0039(7) 0.0034(7) -0.0023(8) C5 0.0172(10) 0.0163(10) 0.0229(8) -0.0030(7) 0.0034(7) -0.0023(8) C7 0.0219(11) 0.0206(10) 0.0329(10) -0.0012(8) 0.0061(8) -0.0019(8) C8 0.0197(10) 0.0241(11) 0.0302(9) -0.0070(8) 0.0047(8) -0.0019(9) C2 0.0343(12) 0.0222(11) 0.0274(9) -0.0014(8) 0.0136(9) -0.0043(9) C03 0.0313(12) 0.0228(11) 0.0304(10) 0.0051(9) 0.0020(9) 0.0041(10) C3 0.0223(10) 0.0250(11) 0.0241(9) 0.0057(8) 0.0058(8) -0.0012(9) C04 0.0254(11) 0.0286(11) 0.0212(9) 0.0084(8) 0.0058(8) 0.0051(9) C02 0.0247(11) 0.0323(12) 0.0347(10) 0.0049(9) 0.0052(9) 0.0117(10) C1 0.0203(10) 0.0169(9) 0.0184(8) 0.0019(7) 0.0071(7) -0.0020(8) C4 0.0255(11) 0.0236(11) 0.0260(9) -0.0005(8) 0.0052(8) -0.0007(9) C01 0.0180(10) 0.0339(13) 0.0334(11) 0.0072(9) 0.0093(8) 0.0098(10) _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 1.7239(13) . ? Al1 O2 1.7266(14) . ? Al1 F01 1.7914(11) . ? Al1 F01 1.8868(12) 3_567 ? Al1 O3 1.8950(15) . ? Al1 Al1 2.9225(11) 3_567 ? F10 C6 1.320(2) . ? F01 Al1 1.8868(12) 3_567 ? F15 C7 1.337(3) . ? F4 C3 1.323(2) . ? F13 C7 1.327(2) . ? F1 C2 1.317(3) . ? O2 C5 1.355(2) . ? F11 C6 1.332(2) . ? F16 C8 1.337(2) . ? F17 C8 1.329(2) . ? F7 C4 1.331(2) . ? F14 C7 1.338(3) . ? F2 C2 1.335(2) . ? F5 C3 1.341(2) . ? F6 C3 1.346(2) . ? F12 C6 1.342(2) . ? O3 C04 1.475(2) . ? O3 C01 1.476(2) . ? F18 C8 1.332(2) . ? F8 C4 1.335(3) . ? O1 C1 1.361(2) . ? F3 C2 1.344(3) . ? F9 C4 1.330(2) . ? C6 C5 1.552(3) . ? C5 C7 1.556(3) . ? C5 C8 1.558(2) . ? C2 C1 1.553(3) . ? C03 C04 1.498(3) . ? C03 C02 1.517(3) . ? C3 C1 1.547(3) . ? C02 C01 1.514(3) . ? C1 C4 1.554(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 O1 Al1 O2 117.75(7) . . ? O1 Al1 F01 134.23(7) . . ? O2 Al1 F01 107.85(6) . . ? O1 Al1 F01 96.05(6) . 3_567 ? O2 Al1 F01 95.90(6) . 3_567 ? F01 Al1 F01 74.80(6) . 3_567 ? O1 Al1 O3 91.90(6) . . ? O2 Al1 O3 96.76(7) . . ? F01 Al1 O3 86.36(6) . . ? F01 Al1 O3 159.82(6) 3_567 . ? O1 Al1 Al1 119.71(5) . 3_567 ? O2 Al1 Al1 104.73(5) . 3_567 ? F01 Al1 Al1 38.54(4) . 3_567 ? F01 Al1 Al1 36.27(3) 3_567 3_567 ? O3 Al1 Al1 124.55(5) . 3_567 ? Al1 F01 Al1 105.20(6) . 3_567 ? C5 O2 Al1 148.15(11) . . ? C04 O3 C01 109.20(14) . . ? C04 O3 Al1 121.80(11) . . ? C01 O3 Al1 128.22(11) . . ? C1 O1 Al1 151.43(12) . . ? F10 C6 F11 107.92(16) . . ? F10 C6 F12 107.62(14) . . ? F11 C6 F12 107.14(16) . . ? F10 C6 C5 110.89(16) . . ? F11 C6 C5 110.58(15) . . ? F12 C6 C5 112.49(15) . . ? O2 C5 C6 109.78(15) . . ? O2 C5 C7 107.78(14) . . ? C6 C5 C7 109.85(15) . . ? O2 C5 C8 111.14(15) . . ? C6 C5 C8 109.41(15) . . ? C7 C5 C8 108.86(16) . . ? F13 C7 F15 107.75(15) . . ? F13 C7 F14 106.99(16) . . ? F15 C7 F14 107.68(17) . . ? F13 C7 C5 110.91(16) . . ? F15 C7 C5 112.43(16) . . ? F14 C7 C5 110.85(15) . . ? F17 C8 F18 108.27(17) . . ? F17 C8 F16 107.37(15) . . ? F18 C8 F16 107.41(15) . . ? F17 C8 C5 110.56(15) . . ? F18 C8 C5 112.75(16) . . ? F16 C8 C5 110.29(16) . . ? F1 C2 F2 108.42(17) . . ? F1 C2 F3 107.42(17) . . ? F2 C2 F3 107.16(16) . . ? F1 C2 C1 111.72(15) . . ? F2 C2 C1 112.09(17) . . ? F3 C2 C1 109.83(17) . . ? C04 C03 C02 102.40(18) . . ? F4 C3 F5 107.73(15) . . ? F4 C3 F6 107.66(16) . . ? F5 C3 F6 107.14(16) . . ? F4 C3 C1 111.33(16) . . ? F5 C3 C1 110.54(15) . . ? F6 C3 C1 112.23(14) . . ? O3 C04 C03 103.75(15) . . ? C01 C02 C03 103.51(18) . . ? O1 C1 C3 111.54(15) . . ? O1 C1 C2 108.32(15) . . ? C3 C1 C2 109.28(15) . . ? O1 C1 C4 109.46(15) . . ? C3 C1 C4 109.32(16) . . ? C2 C1 C4 108.87(15) . . ? F9 C4 F7 107.93(16) . . ? F9 C4 F8 107.35(15) . . ? F7 C4 F8 106.69(16) . . ? F9 C4 C1 112.90(16) . . ? F7 C4 C1 110.14(15) . . ? F8 C4 C1 111.55(17) . . ? O3 C01 C02 104.80(15) . . ? _diffrn_measured_fraction_theta_max 0.928 _diffrn_reflns_theta_full 25.85 _diffrn_measured_fraction_theta_full 0.928 _refine_diff_density_max 0.266 _refine_diff_density_min -0.240 _refine_diff_density_rms 0.049 data_pna21 _database_code_depnum_ccdc_archive 'CCDC 256552' _audit_creation_method SHELXL-97 _chemical_name_systematic ; AsBr4(+)[Al(OR)4](-) (R = C(CF3)3) ; _chemical_name_common 'AsBr4(+)(Al(OR)4)(-) (R = C(CF3)3)' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C16 Al As Br4 F36 O4' _chemical_formula_weight 1361.70 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Al Al 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' As As 0.0499 2.0058 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pna2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x+1/2, -y+1/2, z' '-x+1/2, y+1/2, z+1/2' _cell_length_a 19.062(4) _cell_length_b 13.874(3) _cell_length_c 13.588(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3593.6(12) _cell_formula_units_Z 4 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 1987 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.517 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2552 _exptl_absorpt_coefficient_mu 5.634 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.3910 _exptl_absorpt_correction_T_max 0.5391 _exptl_absorpt_process_details ? _exptl_special_details ; crystal mounted in PFE oil ; _diffrn_ambient_temperature 200(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 'STOE IPDS' _diffrn_measurement_method 'Image Plate Technique' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 22082 _diffrn_reflns_av_R_equivalents 0.0707 _diffrn_reflns_av_sigmaI/netI 0.0701 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.35 _diffrn_reflns_theta_max 25.94 _reflns_number_total 6572 _reflns_number_gt 3485 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'EXPOSE (STOE)' _computing_cell_refinement 'EXPOSE (STOE)' _computing_data_reduction 'INTEGRATE (STOE)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics RESVIEW _computing_publication_material RESVIEW _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^)+(0.0546P)^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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.524(6) _refine_ls_number_reflns 6572 _refine_ls_number_parameters 777 _refine_ls_number_restraints 334 _refine_ls_R_factor_all 0.0925 _refine_ls_R_factor_gt 0.0394 _refine_ls_wR_factor_ref 0.1022 _refine_ls_wR_factor_gt 0.0861 _refine_ls_goodness_of_fit_ref 0.855 _refine_ls_restrained_S_all 0.852 _refine_ls_shift/su_max 0.046 _refine_ls_shift/su_mean 0.002 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group As1 As 0.675488(6) -0.746188(8) 0.98645(4) 0.03266(3) Uani 1 1 d . . . Br4 Br 0.614118(8) -0.609488(8) 0.98601(5) 0.05552(4) Uani 1 1 d . . . Br3 Br 0.742014(11) -0.751067(15) 0.852946(11) 0.06007(6) Uani 1 1 d . . . Br2 Br 0.603847(8) -0.873115(8) 0.98626(5) 0.06097(5) Uani 1 1 d . . . Br1 Br 0.743533(11) -0.750471(14) 1.120036(11) 0.05735(6) Uani 1 1 d . . . Al1 Al 0.943230(15) -0.24571(2) 0.98563(9) 0.02278(7) Uani 1 1 d . . . F10 F 1.00960(5) -0.39514(6) 0.75976(7) 0.0616(4) Uani 1 1 d D . . O3 O 0.91522(5) -0.36216(5) 0.9803(2) 0.0663(4) Uani 1 1 d . A . F11 F 1.07538(7) -0.37639(8) 0.88895(7) 0.0977(5) Uani 1 1 d D . . O1 O 0.98462(9) -0.22395(10) 1.09108(10) 0.0937(6) Uani 1 1 d . . . O2 O 0.99682(8) -0.22373(8) 0.89021(10) 0.0837(5) Uani 1 1 d . . . F1 F 0.93278(6) -0.24236(7) 1.27370(11) 0.1037(5) Uani 1 1 d D . . F13 F 0.99153(7) -0.10331(7) 0.71861(10) 0.1121(6) Uani 1 1 d D . . F12 F 1.11889(5) -0.34784(8) 0.74501(7) 0.0733(4) Uani 1 1 d D . . F2 F 0.98828(6) -0.10829(6) 1.26362(9) 0.0841(4) Uani 1 1 d D . . C1 C 1.03314(6) -0.23334(7) 1.16604(9) 0.0352(4) Uani 1 1 d DU . . F14 F 0.92856(6) -0.23961(9) 0.73192(13) 0.1371(8) Uani 1 1 d D . . F15 F 1.02359(7) -0.23677(9) 0.63534(7) 0.1090(6) Uani 1 1 d D . . C5 C 1.03565(6) -0.23403(7) 0.81135(8) 0.0397(5) Uani 1 1 d D . . C2 C 0.99578(6) -0.20414(7) 1.26290(10) 0.0835(8) Uani 1 1 d D . . C6 C 1.06059(5) -0.33968(8) 0.80016(8) 0.0416(5) Uani 1 1 d D . . C7 C 0.99398(6) -0.20219(8) 0.71854(9) 0.0742(8) Uani 1 1 d D . . F3 F 1.03340(7) -0.22958(8) 1.34040(6) 0.1013(6) Uani 1 1 d D . . O4 O 0.87245(4) -0.17077(5) 0.9823(2) 0.0596(3) Uani 1 1 d . A . F4 F 1.08295(7) -0.08117(6) 1.11997(8) 0.0821(5) Uani 1 1 d D . . F16 F 1.13221(6) -0.14891(8) 0.74383(7) 0.0814(4) Uani 1 1 d D . . F17 F 1.07727(7) -0.08368(7) 0.86284(9) 0.1128(5) Uani 1 1 d D . . F5 F 1.13372(7) -0.15688(9) 1.24000(8) 0.1121(5) Uani 1 1 d D . . C13 C 0.84075(4) -0.08352(6) 0.97757(7) 0.0318(4) Uani 1 1 d D . . F18 F 1.14391(7) -0.20606(9) 0.88971(9) 0.1283(5) Uani 1 1 d D . . F6 F 1.14101(8) -0.21481(13) 1.08958(10) 0.1909(10) Uani 1 1 d D . . C9 C 0.86510(5) -0.43249(6) 0.98137(7) 0.0494(4) Uani 1 1 d D . . C8 C 1.09923(6) -0.16581(8) 0.82700(8) 0.0568(6) Uani 1 1 d D . . C3 C 1.09890(7) -0.16904(8) 1.15493(9) 0.1168(11) Uani 1 1 d D . . F7 F 1.11336(6) -0.34469(8) 1.23687(8) 0.0942(5) Uani 1 1 d D . . F8 F 1.00495(6) -0.39087(9) 1.21721(10) 0.1407(6) Uani 1 1 d D . . F9 F 1.07480(7) -0.37861(7) 1.09255(7) 0.0964(5) Uani 1 1 d D . . C4 C 1.05756(6) -0.33896(9) 1.17779(8) 0.1371(10) Uani 1 1 d D . . F36 F 0.80385(10) -0.12474(12) 1.13707(10) 0.1404(11) Uani 0.7149(6) 1 d PD A 1 F34 F 0.72970(6) -0.13908(8) 1.01635(10) 0.0810(6) Uani 0.7149(6) 1 d PDU A 1 F33 F 0.77287(7) -0.14491(8) 0.84913(11) 0.0833(5) Uani 0.7149(6) 1 d PD A 1 F27 F 0.84787(10) -0.40300(14) 1.14160(11) 0.1788(13) Uani 0.7149(6) 1 d PD A 1 F31 F 0.76321(8) 0.01208(9) 0.89508(14) 0.1085(8) Uani 0.7149(6) 1 d PD A 1 F24 F 0.79588(8) -0.34363(8) 0.86562(14) 0.1305(7) Uani 0.7149(6) 1 d PD A 1 F26 F 0.77656(8) -0.34887(10) 1.04539(15) 0.1745(11) Uani 0.7149(6) 1 d PD A 1 C16 C 0.78063(7) -0.08333(8) 1.05437(9) 0.0507(8) Uani 0.7149(6) 1 d PD A 1 F23 F 0.86165(8) -0.45348(11) 0.80402(10) 0.1048(8) Uani 0.7149(6) 1 d PD A 1 C11 C 0.82506(6) -0.42925(8) 0.88352(9) 0.0393(6) Uani 0.7149(6) 1 d PDU A 1 C12 C 0.81276(7) -0.42313(9) 1.06516(9) 0.0685(9) Uani 0.7149(6) 1 d PDU A 1 C15 C 0.80730(6) -0.06302(8) 0.87437(9) 0.0545(8) Uani 0.7149(6) 1 d PD A 1 F22 F 0.77324(8) -0.49326(9) 0.89256(15) 0.1193(8) Uani 0.7149(6) 1 d PD A 1 F25 F 0.76953(6) -0.48823(8) 1.08973(13) 0.1123(7) Uani 0.7149(6) 1 d PD A 1 F35 F 0.75224(7) 0.00239(8) 1.07720(12) 0.0799(7) Uani 0.7149(6) 1 d PD A 1 F32 F 0.86114(6) -0.03900(10) 0.81387(11) 0.1243(9) Uani 0.7149(6) 1 d PD A 1 F30 F 0.86548(5) 0.08520(5) 0.98533(16) 0.0766(5) Uani 0.7149(6) 1 d PD A 1 F21 F 0.86289(6) -0.60493(6) 0.99969(13) 0.0769(5) Uani 0.7149(6) 1 d PD A 1 F20 F 0.95459(6) -0.53631(8) 1.05667(9) 0.0715(5) Uani 0.7149(6) 1 d PD A 1 F19 F 0.93567(9) -0.53784(12) 0.90188(8) 0.1094(8) Uani 0.7149(6) 1 d PD A 1 C10 C 0.90412(6) -0.52806(7) 0.98915(9) 0.0311(4) Uani 0.7149(6) 1 d PDU A 1 C14 C 0.89290(6) -0.00071(7) 1.00047(9) 0.0463(7) Uani 0.7149(6) 1 d PD A 1 F29 F 0.91712(10) -0.00291(14) 1.09103(10) 0.2123(10) Uani 0.7149(6) 1 d PD A 1 F28 F 0.94701(7) -0.00932(9) 0.93987(11) 0.1400(9) Uani 0.7149(6) 1 d PD A 1 F36A F 0.85137(10) -0.06837(15) 1.16053(14) 0.0921(13) Uani 0.2851(6) 1 d PDU A 2 F27A F 0.86559(9) -0.46444(12) 1.17766(12) 0.0397(9) Uani 0.2851(6) 1 d PDU A 2 F26A F 0.80373(9) -0.33960(9) 1.12685(16) 0.0326(8) Uani 0.2851(6) 1 d PDU A 2 F24A F 0.76811(10) -0.34659(11) 0.93716(16) 0.0517(9) Uani 0.2851(6) 1 d PDU A 2 C16A C 0.81216(7) -0.08601(11) 1.08147(10) 0.0442(12) Uani 0.2851(6) 1 d PDU A 2 F23A F 0.84874(9) -0.39388(14) 0.83645(14) 0.0520(10) Uani 0.2851(6) 1 d PDU A 2 C11A C 0.80207(7) -0.41703(10) 0.89975(10) 0.2637(17) Uani 0.2851(6) 1 d PDU A 2 F34A F 0.76972(9) -0.12960(13) 1.14411(15) 0.0469(9) Uani 0.2851(6) 1 d PDU A 2 C12A C 0.83403(8) -0.42446(9) 1.09541(10) 0.1205(16) Uani 0.2851(6) 1 d PDU A 2 C15A C 0.78302(7) -0.08074(10) 0.90291(11) 0.1806(16) Uani 0.2851(6) 1 d PDU A 2 F31A F 0.76090(8) -0.00009(11) 0.86500(16) 0.0632(11) Uani 0.2851(6) 1 d PDU A 2 F33A F 0.72812(9) -0.13228(12) 0.92508(18) 0.0647(10) Uani 0.2851(6) 1 d PDU A 2 F35A F 0.77851(10) -0.00638(11) 1.1084(2) 0.0715(11) Uani 0.2851(6) 1 d PDU A 2 F32A F 0.81688(10) -0.12688(13) 0.83400(14) 0.0741(11) Uani 0.2851(6) 1 d PDU A 2 F25A F 0.78088(12) -0.49169(11) 1.0886(3) 0.1000(13) Uani 0.2851(6) 1 d PDU A 2 F22A F 0.76608(11) -0.49198(12) 0.8797(2) 0.0919(13) Uani 0.2851(6) 1 d PDU A 2 F30A F 0.94878(9) -0.01900(13) 1.01057(13) 0.0477(9) Uani 0.2851(6) 1 d PDU A 2 F29A F 0.87752(12) 0.09155(11) 0.98847(17) 0.0713(9) Uani 0.2851(6) 1 d PDU A 2 F28A F 0.90301(13) 0.00010(15) 0.87326(11) 0.0494(9) Uani 0.2851(6) 1 d PDU A 2 C14A C 0.88981(8) 0.00179(10) 0.96662(9) 0.0999(15) Uani 0.2851(6) 1 d PDU A 2 C10A C 0.90527(7) -0.53725(11) 0.96576(9) 0.1082(15) Uani 0.2851(6) 1 d PDU A 2 F21A F 0.86626(9) -0.60573(12) 0.94659(13) 0.0340(8) Uani 0.2851(6) 1 d PDU A 2 F20A F 0.95737(9) -0.53852(19) 0.91193(13) 0.0514(10) Uani 0.2851(6) 1 d PDU A 2 F19A F 0.92357(12) -0.5413(2) 1.05317(11) 0.0664(11) Uani 0.2851(6) 1 d PDU A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 As1 0.02753(6) 0.03075(4) 0.03969(5) -0.0014(2) -0.0013(2) -0.00028(5) Br4 0.05379(9) 0.03706(5) 0.07570(9) -0.0026(3) -0.0030(3) 0.01429(6) Br3 0.05847(12) 0.07352(11) 0.04822(8) -0.00251(11) 0.01557(8) 0.00245(11) Br2 0.04525(8) 0.04143(6) 0.09622(10) -0.0010(3) -0.0023(3) -0.01449(6) Br1 0.05839(12) 0.05913(9) 0.05453(9) 0.00567(11) -0.02223(8) -0.00293(10) Al1 0.01994(15) 0.02156(11) 0.02684(12) 0.0008(6) -0.0058(5) -0.00038(14) F10 0.0882(8) 0.0253(4) 0.0713(6) -0.0156(4) -0.0076(6) -0.0066(5) O3 0.0262(5) 0.0252(3) 0.1475(9) -0.0158(13) 0.0290(13) -0.0053(4) F11 0.1347(12) 0.0962(8) 0.0623(7) 0.0170(6) 0.0083(8) 0.0476(7) O1 0.1476(13) 0.0765(9) 0.0572(7) -0.0131(7) -0.0654(7) 0.0253(8) O2 0.1148(10) 0.0369(6) 0.0993(8) 0.0050(6) 0.0882(6) -0.0012(6) F1 0.0905(9) 0.0784(7) 0.1423(10) -0.0296(8) 0.0498(8) -0.0368(7) F13 0.1419(12) 0.0680(6) 0.1265(10) 0.0498(6) 0.0490(9) 0.0357(7) F12 0.0547(7) 0.0797(6) 0.0855(8) -0.0045(6) 0.0286(6) 0.0213(5) F2 0.0867(9) 0.0614(6) 0.1042(8) -0.0176(6) 0.0462(6) -0.0028(6) C1 0.0339(8) 0.0273(7) 0.0444(7) 0.0007(6) -0.0157(6) -0.0009(6) F14 0.0285(8) 0.1528(13) 0.2300(17) -0.0067(12) -0.0576(8) -0.0049(8) F15 0.1395(13) 0.1383(11) 0.0490(6) -0.0292(7) -0.0218(7) 0.0413(9) C5 0.0497(10) 0.0570(9) 0.0123(6) 0.0034(7) 0.0003(6) 0.0050(8) C2 0.0997(18) 0.0384(8) 0.1125(16) -0.0426(9) -0.0056(14) -0.0085(10) C6 0.0215(9) 0.0505(8) 0.0527(9) -0.0113(8) 0.0023(7) -0.0114(7) C7 0.0508(14) 0.1184(16) 0.0534(11) -0.0154(11) -0.0275(9) -0.0127(12) F3 0.1594(13) 0.1242(10) 0.0204(4) -0.0151(6) 0.0070(6) -0.0375(9) O4 0.0289(5) 0.0262(3) 0.1235(8) -0.0015(15) -0.0218(15) 0.0084(3) F4 0.1126(10) 0.0514(5) 0.0823(8) 0.0139(6) -0.0291(7) -0.0171(6) F16 0.0582(7) 0.0759(6) 0.1100(9) -0.0019(7) 0.0268(6) -0.0323(6) F17 0.1114(11) 0.0786(7) 0.1483(10) -0.0659(7) -0.0356(8) -0.0191(7) F5 0.0844(9) 0.0870(8) 0.1649(12) 0.0158(9) -0.0784(7) -0.0106(7) C13 0.0252(7) 0.0229(4) 0.0474(7) -0.0049(10) 0.0096(10) 0.0039(4) F18 0.1421(10) 0.0825(8) 0.1604(10) 0.0054(8) -0.1201(7) -0.0230(7) F6 0.1249(12) 0.268(2) 0.1793(13) 0.0068(15) 0.1210(8) 0.0085(14) C9 0.0375(8) 0.0245(5) 0.0861(10) 0.0009(19) 0.0207(18) -0.0062(5) C8 0.0272(10) 0.0820(11) 0.0613(11) -0.0094(10) -0.0183(8) 0.0191(9) C3 0.190(3) 0.0595(10) 0.1013(17) 0.0356(11) -0.0201(18) -0.0702(12) F7 0.0799(9) 0.0529(5) 0.1498(11) 0.0343(7) -0.0355(8) 0.0158(6) F8 0.1600(12) 0.0957(9) 0.1664(12) 0.0522(8) -0.0943(9) -0.0709(8) F9 0.1545(13) 0.0458(5) 0.0890(8) -0.0288(6) 0.0312(8) 0.0052(7) C4 0.256(2) 0.0696(11) 0.0853(12) -0.0424(10) -0.1157(13) 0.0849(13) F36 0.1201(19) 0.244(3) 0.0572(10) 0.0410(14) 0.0342(11) -0.0072(18) F34 0.0473(9) 0.0899(9) 0.1058(13) -0.0150(8) 0.0425(7) -0.0119(7) F33 0.1057(11) 0.0584(8) 0.0857(9) -0.0032(8) -0.0709(7) 0.0061(8) F27 0.160(2) 0.266(3) 0.1108(15) -0.0885(16) 0.0544(14) -0.014(2) F31 0.1291(15) 0.0684(9) 0.1280(15) 0.0119(10) -0.0519(11) 0.0476(9) F24 0.1631(14) 0.0587(8) 0.1698(15) 0.0165(9) -0.1051(10) 0.0516(8) F26 0.1184(14) 0.1217(15) 0.283(2) -0.0161(15) 0.1424(12) 0.0183(12) C16 0.0413(15) 0.0361(10) 0.0749(17) 0.0066(11) -0.0092(13) 0.0142(10) F23 0.1202(17) 0.1168(14) 0.0774(13) 0.0084(11) -0.0130(12) 0.0402(11) C11 0.0179(11) 0.0210(8) 0.0789(14) 0.0154(9) -0.0098(10) -0.0091(8) C12 0.0580(16) 0.0538(13) 0.0936(17) -0.0120(13) 0.0017(14) -0.0027(12) C15 0.0556(16) 0.0216(9) 0.0862(17) -0.0009(11) -0.0361(12) 0.0187(9) F22 0.1121(14) 0.0788(10) 0.1671(18) 0.0056(12) -0.0766(12) -0.0427(9) F25 0.0704(10) 0.1123(10) 0.1542(18) 0.0097(11) 0.0286(11) -0.0792(7) F35 0.0581(11) 0.0732(10) 0.1084(13) -0.0051(10) 0.0317(9) 0.0249(8) F32 0.214(2) 0.0726(10) 0.0858(12) 0.0318(9) 0.0619(12) -0.0205(12) F30 0.0637(8) 0.0070(3) 0.1591(11) -0.003(2) 0.007(3) -0.0049(4) F21 0.0924(9) 0.0231(4) 0.1152(11) 0.0056(11) -0.0198(14) -0.0189(5) F20 0.0487(9) 0.0393(6) 0.1265(12) -0.0128(7) -0.0329(9) 0.0272(6) F19 0.1839(19) 0.0856(11) 0.0588(9) -0.0133(8) 0.0696(10) 0.0176(12) C10 0.0361(9) 0.0264(6) 0.0308(7) 0.0005(15) -0.0211(15) 0.0025(6) C14 0.0101(9) 0.0220(6) 0.1067(18) 0.0104(14) -0.0070(16) 0.0056(6) F29 0.289(2) 0.1004(15) 0.2472(17) -0.0413(13) -0.2239(13) 0.0052(15) F28 0.0814(10) 0.0571(8) 0.282(3) -0.0171(11) 0.1151(10) -0.0352(7) F36A 0.098(2) 0.096(2) 0.082(2) -0.0004(18) -0.0016(18) -0.0029(18) F27A 0.0422(17) 0.0429(14) 0.0341(14) 0.0081(12) 0.0008(13) 0.0008(12) F26A 0.0366(16) 0.0254(11) 0.0358(13) -0.0072(11) -0.0078(12) -0.0037(11) F24A 0.0363(17) 0.0559(15) 0.0629(16) 0.0127(13) 0.0052(13) 0.0070(13) C16A 0.041(2) 0.0387(19) 0.053(2) 0.0023(17) 0.0000(18) 0.0143(17) F23A 0.0588(18) 0.0541(15) 0.0430(16) 0.0128(13) -0.0109(14) -0.0001(13) C11A 0.262(3) 0.264(3) 0.265(3) 0.000(2) 0.002(2) 0.000(2) F34A 0.0485(18) 0.0550(15) 0.0370(14) 0.0018(12) 0.0116(13) 0.0115(13) C12A 0.116(3) 0.121(3) 0.124(3) -0.002(2) 0.000(2) 0.000(2) C15A 0.180(3) 0.180(3) 0.182(3) 0.001(2) 0.001(2) 0.000(2) F31A 0.067(2) 0.0612(17) 0.0612(18) 0.0037(15) -0.0161(16) 0.0125(15) F33A 0.0622(19) 0.0683(17) 0.0638(17) -0.0012(15) -0.0243(15) -0.0077(15) F35A 0.075(2) 0.0690(18) 0.0709(19) -0.0038(16) 0.0053(17) -0.0016(16) F32A 0.074(2) 0.0846(19) 0.0636(19) -0.0058(16) -0.0028(16) -0.0089(16) F25A 0.097(2) 0.100(2) 0.103(2) 0.0032(19) 0.0078(19) -0.0082(18) F22A 0.092(2) 0.091(2) 0.092(2) -0.0125(18) -0.0090(18) -0.0066(18) F30A 0.0418(16) 0.0413(12) 0.060(2) 0.0057(12) 0.0175(13) -0.0123(11) F29A 0.0695(17) 0.0699(14) 0.0747(16) 0.000(2) 0.000(2) 0.0115(13) F28A 0.0565(18) 0.0476(14) 0.0441(15) 0.0018(12) 0.0186(14) -0.0001(13) C14A 0.098(3) 0.101(2) 0.100(3) 0.003(2) -0.001(2) 0.002(2) C10A 0.111(3) 0.107(3) 0.107(3) -0.003(2) 0.000(2) 0.000(2) F21A 0.0376(16) 0.0235(11) 0.0410(14) -0.0085(10) -0.0009(11) -0.0018(10) F20A 0.0505(18) 0.0493(15) 0.0544(16) 0.0092(13) -0.0026(14) 0.0073(13) F19A 0.065(2) 0.0640(17) 0.0703(18) -0.0050(15) -0.0030(16) -0.0067(15) _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 As1 Br3 2.2144(5) . ? As1 Br4 2.2283(4) . ? As1 Br2 2.2284(4) . ? As1 Br1 2.2318(5) . ? Al1 O1 1.6635(18) . ? Al1 O2 1.6785(17) . ? Al1 O3 1.7030(9) . ? Al1 O4 1.7039(9) . ? F10 C6 1.3557(14) . ? O3 C9 1.3656(12) . ? F11 C6 1.3396(14) . ? O1 C1 1.382(2) . ? O2 C5 1.3103(18) . ? F1 C2 1.3210(16) . ? F13 C7 1.3726(15) . ? F12 C6 1.3452(14) . ? F2 C2 1.3375(14) . ? C1 C4 1.5457(16) . ? C1 C3 1.5460(17) . ? C1 C2 1.5504(18) . ? F14 C7 1.3630(16) . ? F15 C7 1.3517(16) . ? C5 C6 1.5483(15) . ? C5 C8 1.5524(16) . ? C5 C7 1.5545(16) . ? C2 F3 1.3220(17) . ? O4 C13 1.3545(12) . ? F4 C3 1.3433(14) . ? F16 C8 1.3144(15) . ? F17 C8 1.3078(15) . ? F5 C3 1.3435(17) . ? C13 C15A 1.4973(16) . ? C13 C16A 1.5137(17) . ? C13 C14A 1.5158(17) . ? C13 C16 1.5499(15) . ? C13 C14 1.5508(14) . ? C13 C15 1.5665(15) . ? F18 C8 1.3280(16) . ? F6 C3 1.3551(19) . ? C9 C12 1.5194(16) . ? C9 C10 1.5240(14) . ? C9 C11 1.5338(16) . ? C9 C11A 1.6492(17) . ? C9 C10A 1.6564(17) . ? C9 C12A 1.6626(17) . ? F7 C4 1.3350(16) . ? F8 C4 1.3459(17) . ? F9 C4 1.3237(15) . ? F36 C16 1.3374(19) . ? F34 C16 1.3446(17) . ? F33 C15 1.3561(17) . ? F27 C12 1.267(2) . ? F31 C15 1.3679(17) . ? F24 C11 1.3340(16) . ? F26 C12 1.2688(19) . ? C16 F35 1.3429(17) . ? F23 C11 1.3292(19) . ? C11 F22 1.3341(18) . ? C12 F25 1.2674(17) . ? C15 F32 1.3564(18) . ? F30 C14 1.3176(14) . ? F21 C10 1.3326(14) . ? F20 C10 1.3341(16) . ? F19 C10 1.3366(17) . ? C14 F29 1.3147(18) . ? C14 F28 1.3251(18) . ? F36A C16A 1.331(2) . ? F27A C12A 1.385(2) . ? F26A C12A 1.379(2) . ? F24A C11A 1.278(2) . ? C16A F34A 1.321(2) . ? C16A F35A 1.329(2) . ? F23A C11A 1.279(2) . ? C11A F22A 1.275(2) . ? C12A F25A 1.380(2) . ? C15A F31A 1.302(2) . ? C15A F33A 1.303(2) . ? C15A F32A 1.305(2) . ? F30A C14A 1.305(2) . ? F29A C14A 1.301(2) . ? F28A C14A 1.294(2) . ? C10A F20A 1.233(2) . ? C10A F21A 1.234(2) . ? C10A F19A 1.239(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 Br3 As1 Br4 108.93(2) . . ? Br3 As1 Br2 109.02(2) . . ? Br4 As1 Br2 110.537(17) . . ? Br3 As1 Br1 109.429(17) . . ? Br4 As1 Br1 109.27(2) . . ? Br2 As1 Br1 109.64(2) . . ? O1 Al1 O2 110.10(8) . . ? O1 Al1 O3 110.94(11) . . ? O2 Al1 O3 109.30(10) . . ? O1 Al1 O4 106.71(12) . . ? O2 Al1 O4 110.53(11) . . ? O3 Al1 O4 109.24(4) . . ? C9 O3 Al1 153.73(8) . . ? C1 O1 Al1 159.27(12) . . ? C5 O2 Al1 162.89(10) . . ? O1 C1 C4 111.54(10) . . ? O1 C1 C3 114.60(11) . . ? C4 C1 C3 108.23(10) . . ? O1 C1 C2 107.08(11) . . ? C4 C1 C2 107.36(9) . . ? C3 C1 C2 107.73(9) . . ? O2 C5 C6 110.92(10) . . ? O2 C5 C8 105.22(10) . . ? C6 C5 C8 110.55(9) . . ? O2 C5 C7 110.10(11) . . ? C6 C5 C7 110.26(9) . . ? C8 C5 C7 109.68(9) . . ? F1 C2 F3 107.31(12) . . ? F1 C2 F2 107.53(10) . . ? F3 C2 F2 108.52(11) . . ? F1 C2 C1 114.01(11) . . ? F3 C2 C1 110.93(10) . . ? F2 C2 C1 108.36(10) . . ? F11 C6 F12 107.21(10) . . ? F11 C6 F10 107.45(10) . . ? F12 C6 F10 108.60(9) . . ? F11 C6 C5 109.64(9) . . ? F12 C6 C5 112.83(9) . . ? F10 C6 C5 110.91(9) . . ? F15 C7 F14 111.01(12) . . ? F15 C7 F13 111.68(11) . . ? F14 C7 F13 110.45(11) . . ? F15 C7 C5 111.36(10) . . ? F14 C7 C5 104.55(11) . . ? F13 C7 C5 107.51(10) . . ? C13 O4 Al1 154.13(7) . . ? O4 C13 C15A 112.53(13) . . ? O4 C13 C16A 95.49(15) . . ? C15A C13 C16A 111.58(9) . . ? O4 C13 C14A 115.30(9) . . ? C15A C13 C14A 111.52(9) . . ? C16A C13 C14A 109.36(9) . . ? O4 C13 C16 107.41(13) . . ? C15A C13 C16 84.99(8) . . ? C16A C13 C16 26.60(7) . . ? C14A C13 C16 121.39(9) . . ? O4 C13 C14 111.50(8) . . ? C15A C13 C14 126.02(9) . . ? C16A C13 C14 93.48(9) . . ? C14A C13 C14 17.40(7) . . ? C16 C13 C14 109.73(8) . . ? O4 C13 C15 112.74(15) . . ? C15A C13 C15 24.44(7) . . ? C16A C13 C15 133.83(9) . . ? C14A C13 C15 91.23(8) . . ? C16 C13 C15 107.54(8) . . ? C14 C13 C15 107.82(8) . . ? O3 C9 C12 113.96(13) . . ? O3 C9 C10 106.31(8) . . ? C12 C9 C10 110.05(9) . . ? O3 C9 C11 108.56(14) . . ? C12 C9 C11 108.68(9) . . ? C10 C9 C11 109.18(8) . . ? O3 C9 C11A 114.19(12) . . ? C12 C9 C11A 90.82(8) . . ? C10 C9 C11A 121.03(9) . . ? C11 C9 C11A 18.31(7) . . ? O3 C9 C10A 107.59(9) . . ? C12 C9 C10A 118.33(9) . . ? C10 C9 C10A 11.44(6) . . ? C11 C9 C10A 98.32(8) . . ? C11A C9 C10A 111.39(8) . . ? O3 C9 C12A 102.18(14) . . ? C12 C9 C12A 20.28(7) . . ? C10 C9 C12A 99.64(8) . . ? C11 C9 C12A 128.95(9) . . ? C11A C9 C12A 111.01(9) . . ? C10A C9 C12A 110.05(8) . . ? F17 C8 F16 108.53(10) . . ? F17 C8 F18 109.44(11) . . ? F16 C8 F18 108.65(11) . . ? F17 C8 C5 109.42(10) . . ? F16 C8 C5 111.37(10) . . ? F18 C8 C5 109.40(10) . . ? F4 C3 F5 107.58(10) . . ? F4 C3 F6 109.13(12) . . ? F5 C3 F6 109.27(13) . . ? F4 C3 C1 112.00(11) . . ? F5 C3 C1 112.90(11) . . ? F6 C3 C1 105.90(11) . . ? F9 C4 F7 107.67(11) . . ? F9 C4 F8 108.11(11) . . ? F7 C4 F8 108.81(11) . . ? F9 C4 C1 112.23(10) . . ? F7 C4 C1 111.02(10) . . ? F8 C4 C1 108.90(11) . . ? F36 C16 F35 108.64(13) . . ? F36 C16 F34 108.34(13) . . ? F35 C16 F34 107.88(12) . . ? F36 C16 C13 108.68(12) . . ? F35 C16 C13 117.07(11) . . ? F34 C16 C13 105.92(10) . . ? F23 C11 F24 107.21(13) . . ? F23 C11 F22 107.16(13) . . ? F24 C11 F22 107.50(12) . . ? F23 C11 C9 115.85(11) . . ? F24 C11 C9 113.06(11) . . ? F22 C11 C9 105.62(12) . . ? F27 C12 F25 106.54(14) . . ? F27 C12 F26 106.38(15) . . ? F25 C12 F26 106.31(13) . . ? F27 C12 C9 106.63(12) . . ? F25 C12 C9 124.30(12) . . ? F26 C12 C9 105.53(13) . . ? F33 C15 F32 114.75(12) . . ? F33 C15 F31 113.12(12) . . ? F32 C15 F31 113.73(12) . . ? F33 C15 C13 105.74(10) . . ? F32 C15 C13 106.21(10) . . ? F31 C15 C13 101.78(11) . . ? F21 C10 F20 106.42(11) . . ? F21 C10 F19 106.23(12) . . ? F20 C10 F19 106.08(11) . . ? F21 C10 C9 114.57(9) . . ? F20 C10 C9 118.31(10) . . ? F19 C10 C9 104.26(11) . . ? F29 C14 F30 107.85(14) . . ? F29 C14 F28 107.83(13) . . ? F30 C14 F28 107.05(12) . . ? F29 C14 C13 113.31(12) . . ? F30 C14 C13 112.61(9) . . ? F28 C14 C13 107.91(10) . . ? F34A C16A F35A 84.70(15) . . ? F34A C16A F36A 84.73(14) . . ? F35A C16A F36A 84.03(17) . . ? F34A C16A C13 146.31(14) . . ? F35A C16A C13 114.30(16) . . ? F36A C16A C13 123.10(13) . . ? F22A C11A F24A 115.86(16) . . ? F22A C11A F23A 115.79(18) . . ? F24A C11A F23A 115.35(16) . . ? F22A C11A C9 115.46(15) . . ? F24A C11A C9 101.60(13) . . ? F23A C11A C9 88.74(12) . . ? F26A C12A F25A 106.86(16) . . ? F26A C12A F27A 105.89(14) . . ? F25A C12A F27A 95.86(19) . . ? F26A C12A C9 119.67(12) . . ? F25A C12A C9 98.9(2) . . ? F27A C12A C9 124.79(12) . . ? F31A C15A F33A 107.64(14) . . ? F31A C15A F32A 107.32(16) . . ? F33A C15A F32A 107.10(16) . . ? F31A C15A C13 121.89(13) . . ? F33A C15A C13 114.81(14) . . ? F32A C15A C13 96.32(12) . . ? F28A C14A F29A 106.03(17) . . ? F28A C14A F30A 106.09(17) . . ? F29A C14A F30A 105.20(16) . . ? F28A C14A C13 101.66(14) . . ? F29A C14A C13 127.86(15) . . ? F30A C14A C13 108.29(13) . . ? F20A C10A F21A 110.43(17) . . ? F20A C10A F19A 109.94(16) . . ? F21A C10A F19A 109.67(18) . . ? F20A C10A C9 117.43(16) . . ? F21A C10A C9 115.08(13) . . ? F19A C10A C9 92.71(16) . . ? _diffrn_measured_fraction_theta_max 0.942 _diffrn_reflns_theta_full 25.94 _diffrn_measured_fraction_theta_full 0.942 _refine_diff_density_max 0.529 _refine_diff_density_min -0.491 _refine_diff_density_rms 0.081