Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_coden_Cambridge 222 loop_ _publ_author_name 'David Atwood' 'Amithaba Mitra' 'Sean Parkin' 'Jeffrey Struss' 'Yuzhong Wang' _publ_contact_author_name 'David Atwood' _publ_contact_author_address ; Department of Chemistry University of Kentucky Lexington Kentucky 40506 0055 UNITED STATES OF AMERICA ; _publ_contact_author_email DATWOOD@UKY.EDU _publ_requested_journal 'Dalton Transactions' _publ_section_title ; Halogen-Containing Tetrametallic Aluminum Alkoxides ; data_k02073 _database_code_depnum_ccdc_archive 'CCDC 192160' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C15 H39 Al4 Cl3 O6' _chemical_formula_weight 529.73 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C .0033 .0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H .0000 .0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Al Al .0645 .0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl .1484 .1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O .0106 .0060 '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 14.2120(5) _cell_length_b 11.5650(4) _cell_length_c 16.7880(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.646(2) _cell_angle_gamma 90.00 _cell_volume 2759.13(16) _cell_formula_units_Z 4 _cell_measurement_temperature 90.0(2) _cell_measurement_reflns_used 31265 _cell_measurement_theta_min 1.00 _cell_measurement_theta_max 27.48 _exptl_crystal_description 'irregular block' _exptl_crystal_colour colourless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.275 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1120 _exptl_absorpt_coefficient_mu 0.484 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8885 _exptl_absorpt_correction_T_max 0.9179 _exptl_absorpt_process_details 'Scalepack (Otwinowski & Minor, 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 90.0(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 'Nonius KappaCCD diffractometer' _diffrn_measurement_method '\w scans at fixed \c = 55\%' _diffrn_detector_area_resol_mean 18 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% <1 _diffrn_reflns_number 9273 _diffrn_reflns_av_R_equivalents 0.0351 _diffrn_reflns_av_sigmaI/netI 0.0562 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.87 _diffrn_reflns_theta_max 25.00 _reflns_number_total 4856 _reflns_number_gt 3979 _reflns_threshold_expression >2\s(I) _computing_data_collection 'COLLECT (Nonius, 1998)' _computing_cell_refinement 'SCALEPACK (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XP in Siemens SHELXTL (Sheldrick, 1994)' _computing_publication_material ; SHELX97-2 (Sheldrick, 1997) and local procedures ; _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The Cl and Me groups on Al2 and Al4 appear to be disordered so that their positions are interchanged. This has been modelled, but as a result, the bond lengths will not be very accurate for these groups The geometries were fixed and ADPs restrained. ; _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^)+(0.0402P)^2^+3.5577P] 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 4856 _refine_ls_number_parameters 273 _refine_ls_number_restraints 353 _refine_ls_R_factor_all 0.0746 _refine_ls_R_factor_gt 0.0561 _refine_ls_wR_factor_ref 0.1211 _refine_ls_wR_factor_gt 0.1147 _refine_ls_goodness_of_fit_ref 1.085 _refine_ls_restrained_S_all 1.056 _refine_ls_shift/su_max 0.029 _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 Al1 Al 0.51358(6) 0.69895(7) 0.24599(5) 0.0171(2) Uani 1 1 d U A . Al2 Al 0.40240(6) 0.49828(8) 0.27814(6) 0.0255(2) Uani 1 1 d DU . . Al3 Al 0.59678(7) 0.82860(9) 0.37280(5) 0.0282(3) Uani 1 1 d DU . . Al4 Al 0.54302(6) 0.78290(8) 0.08805(5) 0.0232(2) Uani 1 1 d DU . . O1 O 0.39125(12) 0.63649(17) 0.23003(11) 0.0190(4) Uani 1 1 d U A . O2 O 0.52071(13) 0.54911(17) 0.29395(11) 0.0203(5) Uani 1 1 d U A . O3 O 0.48219(13) 0.78034(17) 0.34081(11) 0.0223(5) Uani 1 1 d U A . O4 O 0.63261(13) 0.74423(17) 0.28863(11) 0.0209(5) Uani 1 1 d U A . O5 O 0.49385(13) 0.83106(16) 0.18039(11) 0.0197(5) Uani 1 1 d U A . O6 O 0.56305(13) 0.65380(17) 0.14640(11) 0.0197(4) Uani 1 1 d U A . C1 C 0.3146(2) 0.6766(4) 0.1810(2) 0.0500(11) Uani 1 1 d U . . H1A H 0.3337 0.6716 0.1246 0.060 Uiso 1 1 calc R A . H1B H 0.3037 0.7593 0.1932 0.060 Uiso 1 1 calc R . . C2 C 0.2272(2) 0.6155(4) 0.1898(2) 0.0522(11) Uani 1 1 d U A . H2A H 0.2359 0.5342 0.1752 0.078 Uiso 1 1 calc R . . H2B H 0.1792 0.6503 0.1549 0.078 Uiso 1 1 calc R . . H2C H 0.2068 0.6204 0.2453 0.078 Uiso 1 1 calc R . . C3 C 0.5952(2) 0.4992(3) 0.3417(2) 0.0399(9) Uani 1 1 d U . . H3A H 0.6104 0.5525 0.3862 0.048 Uiso 1 1 calc R A . H3B H 0.6522 0.4918 0.3087 0.048 Uiso 1 1 calc R . . C4 C 0.5716(3) 0.3843(3) 0.3749(3) 0.0523(11) Uani 1 1 d U A . H4A H 0.5179 0.3917 0.4107 0.078 Uiso 1 1 calc R . . H4B H 0.6259 0.3539 0.4047 0.078 Uiso 1 1 calc R . . H4C H 0.5554 0.3312 0.3314 0.078 Uiso 1 1 calc R . . C5 C 0.3922(2) 0.7918(3) 0.3778(2) 0.0442(10) Uani 1 1 d U . . H5A H 0.3735 0.7162 0.4004 0.053 Uiso 1 1 calc R A . H5B H 0.3447 0.8135 0.3369 0.053 Uiso 1 1 calc R . . C6 C 0.3930(3) 0.8802(4) 0.4421(2) 0.0577(12) Uani 1 1 d U A . H6A H 0.4373 0.8567 0.4843 0.086 Uiso 1 1 calc R . . H6B H 0.3298 0.8873 0.4643 0.086 Uiso 1 1 calc R . . H6C H 0.4125 0.9549 0.4202 0.086 Uiso 1 1 calc R . . C7 C 0.7245(2) 0.7419(3) 0.25305(19) 0.0362(9) Uani 1 1 d U . . H7A H 0.7337 0.8136 0.2218 0.043 Uiso 1 1 calc R A . H7B H 0.7283 0.6755 0.2160 0.043 Uiso 1 1 calc R . . C8 C 0.8012(2) 0.7321(3) 0.3146(2) 0.0371(9) Uani 1 1 d U A . H8A H 0.8001 0.8001 0.3494 0.056 Uiso 1 1 calc R . . H8B H 0.8623 0.7276 0.2882 0.056 Uiso 1 1 calc R . . H8C H 0.7915 0.6622 0.3465 0.056 Uiso 1 1 calc R . . C9 C 0.4443(2) 0.9374(3) 0.1964(2) 0.0339(8) Uani 1 1 d U . . H9A H 0.4574 0.9613 0.2520 0.041 Uiso 1 1 calc R A . H9B H 0.3757 0.9234 0.1911 0.041 Uiso 1 1 calc R . . C10 C 0.4708(3) 1.0318(3) 0.1426(2) 0.0584(12) Uani 1 1 d U A . H10A H 0.5390 1.0441 0.1461 0.088 Uiso 1 1 calc R . . H10B H 0.4381 1.1027 0.1581 0.088 Uiso 1 1 calc R . . H10C H 0.4532 1.0114 0.0878 0.088 Uiso 1 1 calc R . . C11 C 0.5907(3) 0.5410(3) 0.1191(2) 0.0393(9) Uani 1 1 d U . . H11A H 0.5337 0.4935 0.1094 0.047 Uiso 1 1 calc R A . H11B H 0.6288 0.5026 0.1611 0.047 Uiso 1 1 calc R . . C12 C 0.6463(2) 0.5469(3) 0.0446(2) 0.0400(9) Uani 1 1 d U A . H12A H 0.6082 0.5827 0.0023 0.060 Uiso 1 1 calc R . . H12B H 0.6642 0.4686 0.0284 0.060 Uiso 1 1 calc R . . H12C H 0.7031 0.5932 0.0540 0.060 Uiso 1 1 calc R . . C13 C 0.3311(17) 0.480(2) 0.3756(11) 0.0381(8) Uani 0.612(4) 1 d PDU A 1 H13A H 0.3417 0.4021 0.3973 0.057 Uiso 0.612(4) 1 calc PR A 1 H13B H 0.2639 0.4902 0.3639 0.057 Uiso 0.612(4) 1 calc PR A 1 H13C H 0.3517 0.5376 0.4147 0.057 Uiso 0.612(4) 1 calc PR A 1 Cl1 Cl 0.3873(2) 0.3628(3) 0.19568(18) 0.0402(6) Uani 0.612(4) 1 d PDU A 1 C13' C 0.4047(16) 0.3612(18) 0.2092(14) 0.0402(6) Uani 0.388(4) 1 d PDU A 2 H13D H 0.4111 0.2916 0.2421 0.060 Uiso 0.388(4) 1 calc PR A 2 H13E H 0.4582 0.3665 0.1730 0.060 Uiso 0.388(4) 1 calc PR A 2 H13F H 0.3461 0.3572 0.1780 0.060 Uiso 0.388(4) 1 calc PR A 2 Cl1' Cl 0.3225(6) 0.4762(9) 0.3775(4) 0.0381(8) Uani 0.388(4) 1 d PDU A 2 C14 C 0.6374(2) 0.7832(3) 0.47995(16) 0.0307(8) Uani 1 1 d DU A . H14A H 0.6120 0.8379 0.5188 0.046 Uiso 1 1 calc R . . H14B H 0.7063 0.7838 0.4832 0.046 Uiso 1 1 calc R . . H14C H 0.6142 0.7053 0.4916 0.046 Uiso 1 1 calc R . . Cl2 Cl 0.62168(7) 1.00694(8) 0.34650(6) 0.0506(3) Uani 1 1 d DU A . C15 C 0.6557(14) 0.862(2) 0.0481(14) 0.0481(10) Uani 0.559(4) 1 d PDU A 1 H15A H 0.6741 0.8281 -0.0028 0.072 Uiso 0.559(4) 1 calc PR A 1 H15B H 0.7074 0.8540 0.0868 0.072 Uiso 0.559(4) 1 calc PR A 1 H15C H 0.6417 0.9447 0.0403 0.072 Uiso 0.559(4) 1 calc PR A 1 Cl3 Cl 0.4401(3) 0.7573(5) -0.0016(3) 0.0385(7) Uani 0.559(4) 1 d PDU A 1 C15' C 0.4525(18) 0.766(3) -0.0001(15) 0.0385(7) Uani 0.441(4) 1 d PDU A 2 H15D H 0.4854 0.7401 -0.0479 0.058 Uiso 0.441(4) 1 calc PR A 2 H15E H 0.4220 0.8404 -0.0107 0.058 Uiso 0.441(4) 1 calc PR A 2 H15F H 0.4047 0.7086 0.0142 0.058 Uiso 0.441(4) 1 calc PR A 2 Cl3' Cl 0.6658(4) 0.8724(7) 0.0577(4) 0.0481(10) Uani 0.441(4) 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 Al1 0.0152(4) 0.0195(5) 0.0166(4) 0.0010(4) 0.0005(3) 0.0014(4) Al2 0.0221(5) 0.0224(5) 0.0318(5) 0.0048(4) -0.0031(4) -0.0044(4) Al3 0.0378(6) 0.0282(6) 0.0185(5) 0.0006(4) -0.0041(4) -0.0069(5) Al4 0.0200(5) 0.0313(6) 0.0183(5) 0.0051(4) -0.0006(4) -0.0025(4) O1 0.0150(10) 0.0220(11) 0.0201(10) 0.0036(9) -0.0030(8) 0.0004(9) O2 0.0181(10) 0.0217(11) 0.0211(11) 0.0055(9) -0.0030(8) 0.0024(9) O3 0.0253(11) 0.0230(11) 0.0188(10) -0.0025(9) 0.0044(8) 0.0022(9) O4 0.0156(10) 0.0285(12) 0.0188(10) 0.0019(9) -0.0008(8) -0.0026(9) O5 0.0201(11) 0.0179(11) 0.0211(10) 0.0025(9) -0.0018(8) 0.0028(9) O6 0.0187(10) 0.0227(11) 0.0179(10) -0.0012(9) 0.0006(8) 0.0038(9) C1 0.0176(17) 0.069(3) 0.063(3) 0.038(2) -0.0118(17) -0.0048(18) C2 0.031(2) 0.055(3) 0.070(3) 0.019(2) -0.0253(19) -0.0102(19) C3 0.033(2) 0.033(2) 0.053(2) 0.0144(18) -0.0171(17) 0.0022(17) C4 0.033(2) 0.052(3) 0.072(3) 0.038(2) 0.0011(19) 0.0054(19) C5 0.040(2) 0.045(2) 0.048(2) -0.0147(19) 0.0260(17) -0.0065(18) C6 0.060(3) 0.067(3) 0.047(2) -0.021(2) 0.020(2) 0.014(2) C7 0.0181(16) 0.059(3) 0.0317(18) 0.0056(18) 0.0001(13) -0.0018(17) C8 0.0229(17) 0.048(2) 0.040(2) 0.0029(18) -0.0084(15) -0.0026(17) C9 0.039(2) 0.0228(18) 0.040(2) 0.0017(15) -0.0048(16) 0.0100(16) C10 0.097(3) 0.027(2) 0.052(3) 0.0111(19) 0.017(2) 0.014(2) C11 0.047(2) 0.032(2) 0.039(2) -0.0061(17) 0.0153(17) 0.0061(18) C12 0.040(2) 0.046(2) 0.034(2) -0.0085(18) 0.0073(16) 0.0098(18) C13 0.028(2) 0.0470(14) 0.0398(11) 0.0134(9) 0.0058(9) -0.0042(11) Cl1 0.0430(14) 0.0300(8) 0.0476(14) -0.0094(8) -0.0011(9) -0.0062(8) C13' 0.0430(14) 0.0300(8) 0.0476(14) -0.0094(8) -0.0011(9) -0.0062(8) Cl1' 0.028(2) 0.0470(14) 0.0398(11) 0.0134(9) 0.0058(9) -0.0042(11) C14 0.046(2) 0.0333(19) 0.0126(15) -0.0002(14) -0.0087(14) -0.0064(17) Cl2 0.0715(7) 0.0339(5) 0.0463(6) 0.0007(4) -0.0039(5) -0.0161(5) C15 0.0313(16) 0.071(2) 0.0422(19) 0.0207(15) -0.0011(14) -0.0099(11) Cl3 0.0374(15) 0.0505(13) 0.0274(8) 0.0068(8) -0.0099(8) -0.0070(12) C15' 0.0374(15) 0.0505(13) 0.0274(8) 0.0068(8) -0.0099(8) -0.0070(12) Cl3' 0.0313(16) 0.071(2) 0.0422(19) 0.0207(15) -0.0011(14) -0.0099(11) _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 O6 1.894(2) . ? Al1 O1 1.899(2) . ? Al1 O5 1.902(2) . ? Al1 O4 1.903(2) . ? Al1 O3 1.907(2) . ? Al1 O2 1.913(2) . ? Al1 Al3 2.8500(12) . ? Al1 Al4 2.8589(12) . ? Al1 Al2 2.8623(12) . ? Al2 O1 1.797(2) . ? Al2 O2 1.798(2) . ? Al2 C13 1.946(13) . ? Al2 C13' 1.964(14) . ? Al2 Cl1' 2.044(5) . ? Al2 Cl1 2.100(2) . ? Al3 O4 1.796(2) . ? Al3 O3 1.798(2) . ? Al3 C14 1.954(3) . ? Al3 Cl2 2.1396(13) . ? Al4 O5 1.796(2) . ? Al4 O6 1.807(2) . ? Al4 C15' 1.960(14) . ? Al4 C15 1.971(14) . ? Al4 Cl3' 2.096(4) . ? Al4 Cl3 2.108(3) . ? O1 C1 1.434(4) . ? O2 C3 1.442(4) . ? O3 C5 1.434(4) . ? O4 C7 1.443(3) . ? O5 C9 1.444(4) . ? O6 C11 1.439(4) . ? C1 C2 1.439(5) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 C4 1.481(5) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 C6 1.488(5) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 C8 1.498(4) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 C10 1.468(5) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 C12 1.488(4) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C13' H13D 0.9800 . ? C13' H13E 0.9800 . ? C13' H13F 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C15' H15D 0.9800 . ? C15' H15E 0.9800 . ? C15' H15F 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O6 Al1 O1 96.84(9) . . ? O6 Al1 O5 76.36(9) . . ? O1 Al1 O5 95.46(9) . . ? O6 Al1 O4 94.05(9) . . ? O1 Al1 O4 165.10(9) . . ? O5 Al1 O4 96.97(9) . . ? O6 Al1 O3 164.93(10) . . ? O1 Al1 O3 94.77(9) . . ? O5 Al1 O3 93.01(9) . . ? O4 Al1 O3 76.43(9) . . ? O6 Al1 O2 95.93(9) . . ? O1 Al1 O2 76.05(8) . . ? O5 Al1 O2 167.95(9) . . ? O4 Al1 O2 92.77(9) . . ? O3 Al1 O2 96.17(9) . . ? O6 Al1 Al3 130.49(7) . . ? O1 Al1 Al3 132.61(7) . . ? O5 Al1 Al3 93.85(7) . . ? O4 Al1 Al3 38.24(6) . . ? O3 Al1 Al3 38.33(6) . . ? O2 Al1 Al3 98.20(7) . . ? O6 Al1 Al4 38.32(6) . . ? O1 Al1 Al4 98.15(6) . . ? O5 Al1 Al4 38.05(6) . . ? O4 Al1 Al4 96.70(7) . . ? O3 Al1 Al4 130.15(7) . . ? O2 Al1 Al4 133.66(7) . . ? Al3 Al1 Al4 116.77(4) . . ? O6 Al1 Al2 98.87(7) . . ? O1 Al1 Al2 37.97(6) . . ? O5 Al1 Al2 133.02(7) . . ? O4 Al1 Al2 129.97(7) . . ? O3 Al1 Al2 96.20(7) . . ? O2 Al1 Al2 38.09(6) . . ? Al3 Al1 Al2 120.72(4) . . ? Al4 Al1 Al2 122.49(4) . . ? O1 Al2 O2 81.55(9) . . ? O1 Al2 C13 115.6(9) . . ? O2 Al2 C13 114.0(8) . . ? O1 Al2 C13' 117.1(8) . . ? O2 Al2 C13' 109.2(7) . . ? C13 Al2 C13' 114.8(12) . . ? O1 Al2 Cl1' 115.5(3) . . ? O2 Al2 Cl1' 116.6(3) . . ? C13 Al2 Cl1' 2.6(11) . . ? C13' Al2 Cl1' 113.2(9) . . ? O1 Al2 Cl1 111.07(12) . . ? O2 Al2 Cl1 115.46(11) . . ? C13 Al2 Cl1 114.9(8) . . ? C13' Al2 Cl1 8.6(7) . . ? Cl1' Al2 Cl1 113.0(3) . . ? O1 Al2 Al1 40.55(6) . . ? O2 Al2 Al1 41.02(6) . . ? C13 Al2 Al1 122.8(8) . . ? C13' Al2 Al1 122.0(8) . . ? Cl1' Al2 Al1 124.6(3) . . ? Cl1 Al2 Al1 122.22(12) . . ? O4 Al3 O3 81.96(9) . . ? O4 Al3 C14 119.68(13) . . ? O3 Al3 C14 116.65(13) . . ? O4 Al3 Cl2 108.20(8) . . ? O3 Al3 Cl2 112.89(8) . . ? C14 Al3 Cl2 113.63(11) . . ? O4 Al3 Al1 40.99(6) . . ? O3 Al3 Al1 41.12(6) . . ? C14 Al3 Al1 131.45(11) . . ? Cl2 Al3 Al1 114.91(5) . . ? O5 Al4 O6 81.30(9) . . ? O5 Al4 C15' 115.1(10) . . ? O6 Al4 C15' 115.1(10) . . ? O5 Al4 C15 118.3(8) . . ? O6 Al4 C15 116.5(8) . . ? C15' Al4 C15 108.6(12) . . ? O5 Al4 Cl3' 112.9(2) . . ? O6 Al4 Cl3' 114.4(2) . . ? C15' Al4 Cl3' 114.0(10) . . ? C15 Al4 Cl3' 5.9(9) . . ? O5 Al4 Cl3 112.71(18) . . ? O6 Al4 Cl3 112.03(18) . . ? C15' Al4 Cl3 3.9(11) . . ? C15 Al4 Cl3 112.5(7) . . ? Cl3' Al4 Cl3 117.9(2) . . ? O5 Al4 Al1 40.75(6) . . ? O6 Al4 Al1 40.55(6) . . ? C15' Al4 Al1 124.4(9) . . ? C15 Al4 Al1 127.0(7) . . ? Cl3' Al4 Al1 121.60(18) . . ? Cl3 Al4 Al1 120.46(15) . . ? C1 O1 Al2 127.5(2) . . ? C1 O1 Al1 130.21(19) . . ? Al2 O1 Al1 101.47(9) . . ? C3 O2 Al2 129.12(19) . . ? C3 O2 Al1 129.19(18) . . ? Al2 O2 Al1 100.90(9) . . ? C5 O3 Al3 130.7(2) . . ? C5 O3 Al1 128.67(19) . . ? Al3 O3 Al1 100.55(10) . . ? C7 O4 Al3 127.00(19) . . ? C7 O4 Al1 130.12(18) . . ? Al3 O4 Al1 100.77(9) . . ? C9 O5 Al4 128.31(18) . . ? C9 O5 Al1 130.20(18) . . ? Al4 O5 Al1 101.20(10) . . ? C11 O6 Al4 128.20(18) . . ? C11 O6 Al1 129.53(18) . . ? Al4 O6 Al1 101.13(10) . . ? O1 C1 C2 115.7(3) . . ? O1 C1 H1A 108.4 . . ? C2 C1 H1A 108.4 . . ? O1 C1 H1B 108.4 . . ? C2 C1 H1B 108.4 . . ? H1A C1 H1B 107.4 . . ? C1 C2 H2A 109.5 . . ? C1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? O2 C3 C4 113.6(3) . . ? O2 C3 H3A 108.8 . . ? C4 C3 H3A 108.8 . . ? O2 C3 H3B 108.8 . . ? C4 C3 H3B 108.8 . . ? H3A C3 H3B 107.7 . . ? C3 C4 H4A 109.5 . . ? C3 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C3 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? O3 C5 C6 112.2(3) . . ? O3 C5 H5A 109.2 . . ? C6 C5 H5A 109.2 . . ? O3 C5 H5B 109.2 . . ? C6 C5 H5B 109.2 . . ? H5A C5 H5B 107.9 . . ? C5 C6 H6A 109.5 . . ? C5 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C5 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? O4 C7 C8 111.8(3) . . ? O4 C7 H7A 109.3 . . ? C8 C7 H7A 109.3 . . ? O4 C7 H7B 109.3 . . ? C8 C7 H7B 109.3 . . ? H7A C7 H7B 107.9 . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? O5 C9 C10 112.9(3) . . ? O5 C9 H9A 109.0 . . ? C10 C9 H9A 109.0 . . ? O5 C9 H9B 109.0 . . ? C10 C9 H9B 109.0 . . ? H9A C9 H9B 107.8 . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? O6 C11 C12 112.1(3) . . ? O6 C11 H11A 109.2 . . ? C12 C11 H11A 109.2 . . ? O6 C11 H11B 109.2 . . ? C12 C11 H11B 109.2 . . ? H11A C11 H11B 107.9 . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? Al2 C13 H13A 109.5 . . ? Al2 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? Al2 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? Al2 C13' H13D 109.5 . . ? Al2 C13' H13E 109.5 . . ? H13D C13' H13E 109.5 . . ? Al2 C13' H13F 109.5 . . ? H13D C13' H13F 109.5 . . ? H13E C13' H13F 109.5 . . ? Al3 C14 H14A 109.5 . . ? Al3 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? Al3 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? Al4 C15 H15A 109.5 . . ? Al4 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? Al4 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? Al4 C15' H15D 109.5 . . ? Al4 C15' H15E 109.5 . . ? H15D C15' H15E 109.5 . . ? Al4 C15' H15F 109.5 . . ? H15D C15' H15F 109.5 . . ? H15E C15' H15F 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O6 Al1 Al2 O1 -89.76(11) . . . . ? O5 Al1 Al2 O1 -10.18(13) . . . . ? O4 Al1 Al2 O1 167.28(13) . . . . ? O3 Al1 Al2 O1 89.81(11) . . . . ? O2 Al1 Al2 O1 -178.08(14) . . . . ? Al3 Al1 Al2 O1 121.23(10) . . . . ? Al4 Al1 Al2 O1 -57.12(10) . . . . ? O6 Al1 Al2 O2 88.31(11) . . . . ? O1 Al1 Al2 O2 178.08(14) . . . . ? O5 Al1 Al2 O2 167.90(13) . . . . ? O4 Al1 Al2 O2 -14.64(13) . . . . ? O3 Al1 Al2 O2 -92.11(12) . . . . ? Al3 Al1 Al2 O2 -60.69(10) . . . . ? Al4 Al1 Al2 O2 120.95(10) . . . . ? O6 Al1 Al2 C13 178.1(10) . . . . ? O1 Al1 Al2 C13 -92.1(10) . . . . ? O5 Al1 Al2 C13 -102.3(10) . . . . ? O4 Al1 Al2 C13 75.2(10) . . . . ? O3 Al1 Al2 C13 -2.3(10) . . . . ? O2 Al1 Al2 C13 89.8(10) . . . . ? Al3 Al1 Al2 C13 29.1(10) . . . . ? Al4 Al1 Al2 C13 -149.2(10) . . . . ? O6 Al1 Al2 C13' 5.7(7) . . . . ? O1 Al1 Al2 C13' 95.4(7) . . . . ? O5 Al1 Al2 C13' 85.2(7) . . . . ? O4 Al1 Al2 C13' -97.3(7) . . . . ? O3 Al1 Al2 C13' -174.8(7) . . . . ? O2 Al1 Al2 C13' -82.7(7) . . . . ? Al3 Al1 Al2 C13' -143.3(7) . . . . ? Al4 Al1 Al2 C13' 38.3(7) . . . . ? O6 Al1 Al2 Cl1' -179.7(4) . . . . ? O1 Al1 Al2 Cl1' -89.9(4) . . . . ? O5 Al1 Al2 Cl1' -100.1(4) . . . . ? O4 Al1 Al2 Cl1' 77.4(4) . . . . ? O3 Al1 Al2 Cl1' -0.1(4) . . . . ? O2 Al1 Al2 Cl1' 92.0(4) . . . . ? Al3 Al1 Al2 Cl1' 31.3(4) . . . . ? Al4 Al1 Al2 Cl1' -147.0(4) . . . . ? O6 Al1 Al2 Cl1 -4.52(11) . . . . ? O1 Al1 Al2 Cl1 85.24(13) . . . . ? O5 Al1 Al2 Cl1 75.06(13) . . . . ? O4 Al1 Al2 Cl1 -107.48(12) . . . . ? O3 Al1 Al2 Cl1 175.05(10) . . . . ? O2 Al1 Al2 Cl1 -92.84(13) . . . . ? Al3 Al1 Al2 Cl1 -153.53(9) . . . . ? Al4 Al1 Al2 Cl1 28.12(10) . . . . ? O6 Al1 Al3 O4 -21.06(13) . . . . ? O1 Al1 Al3 O4 162.58(14) . . . . ? O5 Al1 Al3 O4 -96.39(12) . . . . ? O3 Al1 Al3 O4 173.63(15) . . . . ? O2 Al1 Al3 O4 84.03(12) . . . . ? Al4 Al1 Al3 O4 -64.60(10) . . . . ? Al2 Al1 Al3 O4 116.95(11) . . . . ? O6 Al1 Al3 O3 165.31(14) . . . . ? O1 Al1 Al3 O3 -11.05(13) . . . . ? O5 Al1 Al3 O3 89.98(12) . . . . ? O4 Al1 Al3 O3 -173.63(15) . . . . ? O2 Al1 Al3 O3 -89.60(12) . . . . ? Al4 Al1 Al3 O3 121.76(11) . . . . ? Al2 Al1 Al3 O3 -56.68(11) . . . . ? O6 Al1 Al3 C14 -110.52(17) . . . . ? O1 Al1 Al3 C14 73.12(18) . . . . ? O5 Al1 Al3 C14 174.15(16) . . . . ? O4 Al1 Al3 C14 -89.47(18) . . . . ? O3 Al1 Al3 C14 84.17(18) . . . . ? O2 Al1 Al3 C14 -5.43(16) . . . . ? Al4 Al1 Al3 C14 -154.07(15) . . . . ? Al2 Al1 Al3 C14 27.49(16) . . . . ? O6 Al1 Al3 Cl2 68.41(11) . . . . ? O1 Al1 Al3 Cl2 -107.95(10) . . . . ? O5 Al1 Al3 Cl2 -6.92(8) . . . . ? O4 Al1 Al3 Cl2 89.47(11) . . . . ? O3 Al1 Al3 Cl2 -96.90(11) . . . . ? O2 Al1 Al3 Cl2 173.50(8) . . . . ? Al4 Al1 Al3 Cl2 24.86(7) . . . . ? Al2 Al1 Al3 Cl2 -153.58(5) . . . . ? O6 Al1 Al4 O5 179.18(14) . . . . ? O1 Al1 Al4 O5 88.45(11) . . . . ? O4 Al1 Al4 O5 -92.76(12) . . . . ? O3 Al1 Al4 O5 -14.88(13) . . . . ? O2 Al1 Al4 O5 166.91(14) . . . . ? Al3 Al1 Al4 O5 -58.50(10) . . . . ? Al2 Al1 Al4 O5 119.92(10) . . . . ? O1 Al1 Al4 O6 -90.73(12) . . . . ? O5 Al1 Al4 O6 -179.18(14) . . . . ? O4 Al1 Al4 O6 88.06(12) . . . . ? O3 Al1 Al4 O6 165.94(14) . . . . ? O2 Al1 Al4 O6 -12.27(13) . . . . ? Al3 Al1 Al4 O6 122.32(10) . . . . ? Al2 Al1 Al4 O6 -59.26(10) . . . . ? O6 Al1 Al4 C15' 89.5(13) . . . . ? O1 Al1 Al4 C15' -1.2(13) . . . . ? O5 Al1 Al4 C15' -89.7(13) . . . . ? O4 Al1 Al4 C15' 177.6(13) . . . . ? O3 Al1 Al4 C15' -104.5(13) . . . . ? O2 Al1 Al4 C15' 77.3(13) . . . . ? Al3 Al1 Al4 C15' -148.1(13) . . . . ? Al2 Al1 Al4 C15' 30.3(13) . . . . ? O6 Al1 Al4 C15 -88.8(11) . . . . ? O1 Al1 Al4 C15 -179.5(11) . . . . ? O5 Al1 Al4 C15 92.0(11) . . . . ? O4 Al1 Al4 C15 -0.7(11) . . . . ? O3 Al1 Al4 C15 77.2(11) . . . . ? O2 Al1 Al4 C15 -101.1(11) . . . . ? Al3 Al1 Al4 C15 33.5(11) . . . . ? Al2 Al1 Al4 C15 -148.0(11) . . . . ? O6 Al1 Al4 Cl3' -91.6(3) . . . . ? O1 Al1 Al4 Cl3' 177.7(3) . . . . ? O5 Al1 Al4 Cl3' 89.2(3) . . . . ? O4 Al1 Al4 Cl3' -3.5(3) . . . . ? O3 Al1 Al4 Cl3' 74.4(3) . . . . ? O2 Al1 Al4 Cl3' -103.9(3) . . . . ? Al3 Al1 Al4 Cl3' 30.7(3) . . . . ? Al2 Al1 Al4 Cl3' -150.8(3) . . . . ? O6 Al1 Al4 Cl3 89.0(2) . . . . ? O1 Al1 Al4 Cl3 -1.8(2) . . . . ? O5 Al1 Al4 Cl3 -90.2(2) . . . . ? O4 Al1 Al4 Cl3 177.0(2) . . . . ? O3 Al1 Al4 Cl3 -105.1(2) . . . . ? O2 Al1 Al4 Cl3 76.7(2) . . . . ? Al3 Al1 Al4 Cl3 -148.7(2) . . . . ? Al2 Al1 Al4 Cl3 29.7(2) . . . . ? O2 Al2 O1 C1 169.0(3) . . . . ? C13 Al2 O1 C1 -78.4(9) . . . . ? C13' Al2 O1 C1 61.6(8) . . . . ? Cl1' Al2 O1 C1 -75.5(4) . . . . ? Cl1 Al2 O1 C1 54.8(3) . . . . ? Al1 Al2 O1 C1 170.2(3) . . . . ? O2 Al2 O1 Al1 -1.28(9) . . . . ? C13 Al2 O1 Al1 111.4(9) . . . . ? C13' Al2 O1 Al1 -108.6(8) . . . . ? Cl1' Al2 O1 Al1 114.3(3) . . . . ? Cl1 Al2 O1 Al1 -115.38(12) . . . . ? O6 Al1 O1 C1 -74.2(3) . . . . ? O5 Al1 O1 C1 2.7(3) . . . . ? O4 Al1 O1 C1 149.1(4) . . . . ? O3 Al1 O1 C1 96.2(3) . . . . ? O2 Al1 O1 C1 -168.6(3) . . . . ? Al3 Al1 O1 C1 103.0(3) . . . . ? Al4 Al1 O1 C1 -35.5(3) . . . . ? Al2 Al1 O1 C1 -169.8(3) . . . . ? O6 Al1 O1 Al2 95.67(10) . . . . ? O5 Al1 O1 Al2 172.54(9) . . . . ? O4 Al1 O1 Al2 -41.0(4) . . . . ? O3 Al1 O1 Al2 -93.97(10) . . . . ? O2 Al1 O1 Al2 1.22(9) . . . . ? Al3 Al1 O1 Al2 -87.12(11) . . . . ? Al4 Al1 O1 Al2 134.31(8) . . . . ? O1 Al2 O2 C3 171.6(3) . . . . ? C13 Al2 O2 C3 57.3(10) . . . . ? C13' Al2 O2 C3 -72.5(9) . . . . ? Cl1' Al2 O2 C3 57.3(4) . . . . ? Cl1 Al2 O2 C3 -79.0(3) . . . . ? Al1 Al2 O2 C3 170.4(3) . . . . ? O1 Al2 O2 Al1 1.26(9) . . . . ? C13 Al2 O2 Al1 -113.0(9) . . . . ? C13' Al2 O2 Al1 117.1(8) . . . . ? Cl1' Al2 O2 Al1 -113.1(4) . . . . ? Cl1 Al2 O2 Al1 110.65(13) . . . . ? O6 Al1 O2 C3 92.8(3) . . . . ? O1 Al1 O2 C3 -171.6(3) . . . . ? O5 Al1 O2 C3 142.4(4) . . . . ? O4 Al1 O2 C3 -1.5(3) . . . . ? O3 Al1 O2 C3 -78.2(3) . . . . ? Al3 Al1 O2 C3 -39.6(3) . . . . ? Al4 Al1 O2 C3 100.4(3) . . . . ? Al2 Al1 O2 C3 -170.4(3) . . . . ? O6 Al1 O2 Al2 -96.81(10) . . . . ? O1 Al1 O2 Al2 -1.22(9) . . . . ? O5 Al1 O2 Al2 -47.2(5) . . . . ? O4 Al1 O2 Al2 168.82(10) . . . . ? O3 Al1 O2 Al2 92.18(10) . . . . ? Al3 Al1 O2 Al2 130.77(8) . . . . ? Al4 Al1 O2 Al2 -89.20(11) . . . . ? O4 Al3 O3 C5 172.0(3) . . . . ? C14 Al3 O3 C5 52.8(3) . . . . ? Cl2 Al3 O3 C5 -81.6(3) . . . . ? Al1 Al3 O3 C5 176.2(3) . . . . ? O4 Al3 O3 Al1 -4.21(10) . . . . ? C14 Al3 O3 Al1 -123.46(14) . . . . ? Cl2 Al3 O3 Al1 102.21(9) . . . . ? O6 Al1 O3 C5 135.8(4) . . . . ? O1 Al1 O3 C5 -4.5(3) . . . . ? O5 Al1 O3 C5 91.3(3) . . . . ? O4 Al1 O3 C5 -172.3(3) . . . . ? O2 Al1 O3 C5 -80.9(3) . . . . ? Al3 Al1 O3 C5 -176.3(3) . . . . ? Al4 Al1 O3 C5 100.4(3) . . . . ? Al2 Al1 O3 C5 -42.6(3) . . . . ? O6 Al1 O3 Al3 -47.9(4) . . . . ? O1 Al1 O3 Al3 171.86(10) . . . . ? O5 Al1 O3 Al3 -92.40(10) . . . . ? O4 Al1 O3 Al3 4.05(9) . . . . ? O2 Al1 O3 Al3 95.42(10) . . . . ? Al4 Al1 O3 Al3 -83.28(11) . . . . ? Al2 Al1 O3 Al3 133.73(8) . . . . ? O3 Al3 O4 C7 169.0(2) . . . . ? C14 Al3 O4 C7 -74.9(3) . . . . ? Cl2 Al3 O4 C7 57.4(2) . . . . ? Al1 Al3 O4 C7 164.7(3) . . . . ? O3 Al3 O4 Al1 4.22(10) . . . . ? C14 Al3 O4 Al1 120.38(14) . . . . ? Cl2 Al3 O4 Al1 -107.31(9) . . . . ? O6 Al1 O4 C7 0.1(3) . . . . ? O1 Al1 O4 C7 137.0(4) . . . . ? O5 Al1 O4 C7 -76.7(3) . . . . ? O3 Al1 O4 C7 -168.1(3) . . . . ? O2 Al1 O4 C7 96.2(3) . . . . ? Al3 Al1 O4 C7 -164.0(3) . . . . ? Al4 Al1 O4 C7 -38.3(3) . . . . ? Al2 Al1 O4 C7 105.2(2) . . . . ? O6 Al1 O4 Al3 164.10(10) . . . . ? O1 Al1 O4 Al3 -59.0(4) . . . . ? O5 Al1 O4 Al3 87.37(10) . . . . ? O3 Al1 O4 Al3 -4.06(9) . . . . ? O2 Al1 O4 Al3 -99.75(10) . . . . ? Al4 Al1 O4 Al3 125.70(8) . . . . ? Al2 Al1 O4 Al3 -90.76(11) . . . . ? O6 Al4 O5 C9 -173.8(2) . . . . ? C15' Al4 O5 C9 -60.1(11) . . . . ? C15 Al4 O5 C9 70.7(10) . . . . ? Cl3' Al4 O5 C9 73.3(3) . . . . ? Cl3 Al4 O5 C9 -63.5(3) . . . . ? Al1 Al4 O5 C9 -174.3(3) . . . . ? O6 Al4 O5 Al1 0.54(9) . . . . ? C15' Al4 O5 Al1 114.3(11) . . . . ? C15 Al4 O5 Al1 -115.0(9) . . . . ? Cl3' Al4 O5 Al1 -112.4(3) . . . . ? Cl3 Al4 O5 Al1 110.9(2) . . . . ? O6 Al1 O5 C9 173.6(2) . . . . ? O1 Al1 O5 C9 77.9(2) . . . . ? O4 Al1 O5 C9 -93.9(2) . . . . ? O3 Al1 O5 C9 -17.2(2) . . . . ? O2 Al1 O5 C9 122.5(4) . . . . ? Al3 Al1 O5 C9 -55.6(2) . . . . ? Al4 Al1 O5 C9 174.2(3) . . . . ? Al2 Al1 O5 C9 84.2(2) . . . . ? O6 Al1 O5 Al4 -0.52(9) . . . . ? O1 Al1 O5 Al4 -96.25(10) . . . . ? O4 Al1 O5 Al4 91.98(10) . . . . ? O3 Al1 O5 Al4 168.66(10) . . . . ? O2 Al1 O5 Al4 -51.7(5) . . . . ? Al3 Al1 O5 Al4 130.27(8) . . . . ? Al2 Al1 O5 Al4 -89.98(11) . . . . ? O5 Al4 O6 C11 168.1(3) . . . . ? C15' Al4 O6 C11 54.3(11) . . . . ? C15 Al4 O6 C11 -74.5(9) . . . . ? Cl3' Al4 O6 C11 -80.6(3) . . . . ? Cl3 Al4 O6 C11 57.0(3) . . . . ? Al1 Al4 O6 C11 168.6(3) . . . . ? O5 Al4 O6 Al1 -0.54(9) . . . . ? C15' Al4 O6 Al1 -114.3(11) . . . . ? C15 Al4 O6 Al1 116.9(9) . . . . ? Cl3' Al4 O6 Al1 110.8(2) . . . . ? Cl3 Al4 O6 Al1 -111.61(19) . . . . ? O1 Al1 O6 C11 -73.9(3) . . . . ? O5 Al1 O6 C11 -167.9(3) . . . . ? O4 Al1 O6 C11 95.9(3) . . . . ? O3 Al1 O6 C11 146.0(4) . . . . ? O2 Al1 O6 C11 2.7(3) . . . . ? Al3 Al1 O6 C11 108.8(2) . . . . ? Al4 Al1 O6 C11 -168.4(3) . . . . ? Al2 Al1 O6 C11 -35.6(3) . . . . ? O1 Al1 O6 Al4 94.50(10) . . . . ? O5 Al1 O6 Al4 0.52(9) . . . . ? O4 Al1 O6 Al4 -95.68(10) . . . . ? O3 Al1 O6 Al4 -45.6(4) . . . . ? O2 Al1 O6 Al4 171.10(9) . . . . ? Al3 Al1 O6 Al4 -82.80(11) . . . . ? Al2 Al1 O6 Al4 132.80(8) . . . . ? Al2 O1 C1 C2 19.5(5) . . . . ? Al1 O1 C1 C2 -173.1(3) . . . . ? Al2 O2 C3 C4 6.8(5) . . . . ? Al1 O2 C3 C4 174.6(2) . . . . ? Al3 O3 C5 C6 15.7(5) . . . . ? Al1 O3 C5 C6 -169.1(2) . . . . ? Al3 O4 C7 C8 46.1(4) . . . . ? Al1 O4 C7 C8 -153.7(2) . . . . ? Al4 O5 C9 C10 -26.5(4) . . . . ? Al1 O5 C9 C10 160.8(2) . . . . ? Al4 O6 C11 C12 27.8(4) . . . . ? Al1 O6 C11 C12 -166.7(2) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max .448 _refine_diff_density_min -.441 _refine_diff_density_rms .060 # Attachment 'Compound_4-cif.htm' data_k05036 _database_code_depnum_ccdc_archive 'CCDC 665929' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C12 H30 Al4 Br6 O6' _chemical_formula_weight 857.74 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' Al Al 0.0645 0.0514 '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' Br Br -0.2901 2.4595 '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 14.3134(2) _cell_length_b 11.7178(2) _cell_length_c 17.0046(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.2588(6) _cell_angle_gamma 90.00 _cell_volume 2852.01(8) _cell_formula_units_Z 4 _cell_measurement_temperature 90.0(2) _cell_measurement_reflns_used 6821 _cell_measurement_theta_min 1.00 _cell_measurement_theta_max 27.5 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.998 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1648 _exptl_absorpt_coefficient_mu 8.593 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.2225 _exptl_absorpt_correction_T_max 0.2783 _exptl_absorpt_process_details 'Scalepack (Otwinowski & Minor, 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 90.0(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 'Nonius KappaCCD diffractometer' _diffrn_measurement_method '\w scans at \c = 55\%' _diffrn_detector_area_resol_mean 18 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12649 _diffrn_reflns_av_R_equivalents 0.0470 _diffrn_reflns_av_sigmaI/netI 0.0596 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.86 _diffrn_reflns_theta_max 27.48 _reflns_number_total 6533 _reflns_number_gt 4643 _reflns_threshold_expression >2\s(I) _computing_data_collection 'Collect (Nonius, 1998)' _computing_cell_refinement 'Collect (Nonius, 1998)' _computing_data_reduction 'Denzo-SMN (Nonius, 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XP in SHELXTL (Sheldrick, 1995)' _computing_publication_material ; SHELX97-2 (Sheldrick, 1997) and local procedures' ; _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^)+(0.0302P)^2^+0.4555P] 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 6533 _refine_ls_number_parameters 259 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0660 _refine_ls_R_factor_gt 0.0340 _refine_ls_wR_factor_ref 0.0729 _refine_ls_wR_factor_gt 0.0650 _refine_ls_goodness_of_fit_ref 1.016 _refine_ls_restrained_S_all 1.016 _refine_ls_shift/su_max 0.033 _refine_ls_shift/su_mean 0.001 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 0.51026(7) 0.70041(9) 0.24558(6) 0.0121(2) Uani 1 1 d . . . Al2 Al 0.54118(7) 0.77956(9) 0.09041(6) 0.0157(2) Uani 1 1 d . . . Al3 Al 0.40260(7) 0.50268(9) 0.27564(6) 0.0156(2) Uani 1 1 d . . . Al4 Al 0.58911(8) 0.83390(9) 0.36740(6) 0.0190(3) Uani 1 1 d . . . O1 O 0.49221(15) 0.82995(19) 0.17955(13) 0.0134(5) Uani 1 1 d . . . O2 O 0.56228(15) 0.65422(19) 0.14752(13) 0.0139(5) Uani 1 1 d . . . O3 O 0.38920(15) 0.63783(19) 0.22965(13) 0.0141(5) Uani 1 1 d . . . O4 O 0.51802(15) 0.55286(19) 0.29344(13) 0.0148(5) Uani 1 1 d . . . O5 O 0.47772(16) 0.78275(19) 0.33799(13) 0.0158(5) Uani 1 1 d . . . O6 O 0.62819(15) 0.74778(19) 0.28765(13) 0.0148(5) Uani 1 1 d . . . C1 C 0.4406(2) 0.9343(3) 0.1924(2) 0.0223(9) Uani 1 1 d . . . H1A H 0.4469 0.9570 0.2483 0.027 Uiso 1 1 calc R . . H1B H 0.3736 0.9204 0.1815 0.027 Uiso 1 1 calc R . . C2 C 0.4741(3) 1.0294(3) 0.1415(2) 0.0310(10) Uani 1 1 d . . . H2A H 0.5397 1.0457 0.1537 0.047 Uiso 1 1 calc R . . H2B H 0.4364 1.0977 0.1512 0.047 Uiso 1 1 calc R . . H2C H 0.4682 1.0072 0.0861 0.047 Uiso 1 1 calc R . . C3 C 0.5932(3) 0.5429(3) 0.1225(2) 0.0264(9) Uani 1 1 d . . . H3A H 0.5381 0.4930 0.1146 0.032 Uiso 1 1 calc R . . H3B H 0.6325 0.5087 0.1644 0.032 Uiso 1 1 calc R . . C4 C 0.6484(3) 0.5486(3) 0.0473(2) 0.0286(10) Uani 1 1 d . . . H4A H 0.6101 0.5839 0.0060 0.043 Uiso 1 1 calc R . . H4B H 0.6661 0.4713 0.0312 0.043 Uiso 1 1 calc R . . H4C H 0.7048 0.5944 0.0558 0.043 Uiso 1 1 calc R . . C5 C 0.3116(3) 0.6798(4) 0.1836(3) 0.0385(12) Uani 1 1 d . . . H5A H 0.3292 0.6783 0.1273 0.046 Uiso 1 1 calc R . . H5B H 0.2998 0.7603 0.1981 0.046 Uiso 1 1 calc R . . C6 C 0.2251(2) 0.6148(3) 0.1935(2) 0.0329(10) Uani 1 1 d . . . H6A H 0.2353 0.5355 0.1774 0.049 Uiso 1 1 calc R . . H6B H 0.1757 0.6486 0.1610 0.049 Uiso 1 1 calc R . . H6C H 0.2064 0.6168 0.2489 0.049 Uiso 1 1 calc R . . C7 C 0.5916(3) 0.5055(3) 0.3414(2) 0.0292(10) Uani 1 1 d . . . H7A H 0.6011 0.5549 0.3880 0.035 Uiso 1 1 calc R . . H7B H 0.6504 0.5054 0.3109 0.035 Uiso 1 1 calc R . . C8 C 0.5713(3) 0.3866(4) 0.3683(3) 0.0407(12) Uani 1 1 d . . . H8A H 0.5138 0.3863 0.3994 0.061 Uiso 1 1 calc R . . H8B H 0.6233 0.3589 0.4008 0.061 Uiso 1 1 calc R . . H8C H 0.5635 0.3367 0.3225 0.061 Uiso 1 1 calc R . . C9 C 0.3861(3) 0.7948(4) 0.3744(3) 0.0355(11) Uani 1 1 d . . . H9A H 0.3675 0.7208 0.3977 0.043 Uiso 1 1 calc R . . H9B H 0.3395 0.8149 0.3335 0.043 Uiso 1 1 calc R . . C10 C 0.3859(3) 0.8838(4) 0.4365(2) 0.0407(12) Uani 1 1 d . . . H10A H 0.4281 0.8610 0.4792 0.061 Uiso 1 1 calc R . . H10B H 0.3225 0.8927 0.4571 0.061 Uiso 1 1 calc R . . H10C H 0.4070 0.9564 0.4142 0.061 Uiso 1 1 calc R . . C11 C 0.7195(2) 0.7477(3) 0.2535(2) 0.0242(9) Uani 1 1 d . . . H11A H 0.7282 0.8188 0.2231 0.029 Uiso 1 1 calc R . . H11B H 0.7247 0.6826 0.2166 0.029 Uiso 1 1 calc R . . C12 C 0.7954(3) 0.7387(3) 0.3143(2) 0.0278(9) Uani 1 1 d . . . H12A H 0.7929 0.8052 0.3492 0.042 Uiso 1 1 calc R . . H12B H 0.8563 0.7359 0.2883 0.042 Uiso 1 1 calc R . . H12C H 0.7865 0.6690 0.3453 0.042 Uiso 1 1 calc R . . Br1 Br 0.67141(3) 0.87132(4) 0.04853(2) 0.02916(11) Uani 1 1 d . . . Br2 Br 0.43487(3) 0.75692(3) -0.00702(2) 0.02573(10) Uani 1 1 d . . . Br3 Br 0.39120(3) 0.35422(3) 0.19031(2) 0.02934(11) Uani 1 1 d . . . Br4 Br 0.31534(3) 0.47641(3) 0.38483(2) 0.02427(10) Uani 1 1 d . . . Br5 Br 0.63469(3) 0.77984(4) 0.48891(2) 0.03197(11) Uani 1 1 d . . . Br6 Br 0.61721(3) 1.02171(3) 0.34335(2) 0.02997(11) 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 0.0116(5) 0.0130(6) 0.0117(5) 0.0006(4) 0.0009(4) 0.0007(4) Al2 0.0152(5) 0.0201(6) 0.0119(5) 0.0043(5) 0.0009(5) -0.0021(5) Al3 0.0143(5) 0.0152(6) 0.0173(6) 0.0023(5) 0.0020(5) -0.0004(5) Al4 0.0236(6) 0.0183(6) 0.0150(6) -0.0001(5) -0.0004(5) -0.0015(5) O1 0.0147(12) 0.0118(13) 0.0136(12) 0.0025(10) 0.0001(10) 0.0026(10) O2 0.0151(12) 0.0135(13) 0.0130(12) -0.0016(10) 0.0033(10) 0.0012(10) O3 0.0112(12) 0.0153(13) 0.0157(13) 0.0044(11) -0.0003(10) -0.0005(10) O4 0.0132(12) 0.0145(13) 0.0167(13) 0.0042(11) 0.0004(10) 0.0020(10) O5 0.0182(13) 0.0162(13) 0.0131(12) -0.0014(10) 0.0062(10) 0.0012(11) O6 0.0109(12) 0.0199(13) 0.0136(12) 0.0006(11) -0.0002(10) -0.0009(11) C1 0.019(2) 0.016(2) 0.032(2) 0.0002(17) -0.0009(17) 0.0032(16) C2 0.045(3) 0.017(2) 0.031(2) 0.0047(19) 0.005(2) 0.0064(19) C3 0.031(2) 0.022(2) 0.027(2) -0.0045(18) 0.0102(19) 0.0045(18) C4 0.031(2) 0.028(2) 0.026(2) -0.0034(19) 0.0081(19) 0.0030(19) C5 0.0127(19) 0.054(3) 0.049(3) 0.029(2) -0.0103(19) -0.004(2) C6 0.019(2) 0.032(2) 0.047(3) 0.009(2) -0.014(2) -0.0017(19) C7 0.022(2) 0.029(2) 0.037(3) 0.0090(19) -0.0106(19) 0.0004(18) C8 0.023(2) 0.040(3) 0.059(3) 0.027(2) -0.003(2) 0.008(2) C9 0.031(2) 0.034(3) 0.042(3) -0.010(2) 0.027(2) -0.002(2) C10 0.041(3) 0.052(3) 0.030(2) -0.015(2) 0.013(2) 0.010(2) C11 0.0114(17) 0.037(2) 0.024(2) 0.0028(19) 0.0009(16) -0.0020(17) C12 0.019(2) 0.033(2) 0.032(2) -0.002(2) -0.0082(18) -0.0010(18) Br1 0.0192(2) 0.0395(3) 0.0288(2) 0.0139(2) 0.00285(17) -0.00814(18) Br2 0.0257(2) 0.0325(2) 0.0189(2) 0.00393(18) -0.00728(17) -0.00469(18) Br3 0.0340(2) 0.0187(2) 0.0354(2) -0.00662(18) 0.00660(19) -0.00437(18) Br4 0.01995(19) 0.0303(2) 0.0226(2) 0.00736(18) 0.00489(16) -0.00333(17) Br5 0.0440(3) 0.0360(3) 0.0159(2) 0.00255(18) -0.00666(19) -0.0002(2) Br6 0.0413(3) 0.0203(2) 0.0283(2) 0.00070(18) -0.00401(19) -0.00952(19) _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 O3 1.900(2) . ? Al1 O5 1.904(2) . ? Al1 O1 1.905(2) . ? Al1 O2 1.908(2) . ? Al1 O6 1.913(2) . ? Al1 O4 1.914(2) . ? Al1 Al4 2.8268(15) . ? Al1 Al3 2.8305(14) . ? Al1 Al2 2.8334(14) . ? Al2 O1 1.774(2) . ? Al2 O2 1.786(2) . ? Al2 Br2 2.2600(11) . ? Al2 Br1 2.2694(11) . ? Al3 O3 1.776(2) . ? Al3 O4 1.778(2) . ? Al3 Br4 2.2634(10) . ? Al3 Br3 2.2708(11) . ? Al4 O5 1.773(3) . ? Al4 O6 1.783(2) . ? Al4 Br5 2.2546(11) . ? Al4 Br6 2.2746(12) . ? O1 C1 1.445(4) . ? O2 C3 1.441(4) . ? O3 C5 1.442(4) . ? O4 C7 1.440(4) . ? O5 C9 1.459(4) . ? O6 C11 1.433(4) . ? C1 C2 1.491(5) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 C4 1.508(5) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 C6 1.464(5) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 C8 1.496(5) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 C10 1.485(5) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 C12 1.499(5) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O3 Al1 O5 94.99(11) . . ? O3 Al1 O1 95.87(10) . . ? O5 Al1 O1 92.85(10) . . ? O3 Al1 O2 97.19(10) . . ? O5 Al1 O2 164.43(11) . . ? O1 Al1 O2 76.31(10) . . ? O3 Al1 O6 165.50(11) . . ? O5 Al1 O6 76.29(10) . . ? O1 Al1 O6 96.11(11) . . ? O2 Al1 O6 93.55(10) . . ? O3 Al1 O4 76.30(10) . . ? O5 Al1 O4 96.93(10) . . ? O1 Al1 O4 167.93(11) . . ? O2 Al1 O4 95.35(10) . . ? O6 Al1 O4 93.07(10) . . ? O3 Al1 Al4 132.76(8) . . ? O5 Al1 Al4 38.09(7) . . ? O1 Al1 Al4 92.51(8) . . ? O2 Al1 Al4 129.90(8) . . ? O6 Al1 Al4 38.42(7) . . ? O4 Al1 Al4 99.55(8) . . ? O3 Al1 Al3 38.08(7) . . ? O5 Al1 Al3 97.49(8) . . ? O1 Al1 Al3 133.33(8) . . ? O2 Al1 Al3 98.08(8) . . ? O6 Al1 Al3 130.56(8) . . ? O4 Al1 Al3 38.22(7) . . ? Al4 Al1 Al3 122.44(5) . . ? O3 Al1 Al2 98.03(8) . . ? O5 Al1 Al2 129.99(8) . . ? O1 Al1 Al2 37.97(7) . . ? O2 Al1 Al2 38.35(7) . . ? O6 Al1 Al2 96.44(8) . . ? O4 Al1 Al2 133.05(8) . . ? Al4 Al1 Al2 115.97(5) . . ? Al3 Al1 Al2 121.57(5) . . ? O1 Al2 O2 82.85(11) . . ? O1 Al2 Br2 113.46(9) . . ? O2 Al2 Br2 114.45(9) . . ? O1 Al2 Br1 116.02(9) . . ? O2 Al2 Br1 115.03(9) . . ? Br2 Al2 Br1 112.14(4) . . ? O1 Al2 Al1 41.35(8) . . ? O2 Al2 Al1 41.51(7) . . ? Br2 Al2 Al1 122.46(5) . . ? Br1 Al2 Al1 125.40(5) . . ? O3 Al3 O4 83.02(11) . . ? O3 Al3 Br4 115.06(8) . . ? O4 Al3 Br4 114.90(9) . . ? O3 Al3 Br3 113.23(9) . . ? O4 Al3 Br3 115.22(9) . . ? Br4 Al3 Br3 112.44(5) . . ? O3 Al3 Al1 41.27(7) . . ? O4 Al3 Al1 41.75(8) . . ? Br4 Al3 Al1 124.22(5) . . ? Br3 Al3 Al1 123.32(5) . . ? O5 Al4 O6 83.04(11) . . ? O5 Al4 Br5 114.81(9) . . ? O6 Al4 Br5 116.59(9) . . ? O5 Al4 Br6 115.84(9) . . ? O6 Al4 Br6 110.77(9) . . ? Br5 Al4 Br6 112.70(5) . . ? O5 Al4 Al1 41.47(8) . . ? O6 Al4 Al1 41.82(8) . . ? Br5 Al4 Al1 128.98(5) . . ? Br6 Al4 Al1 118.29(5) . . ? C1 O1 Al2 127.9(2) . . ? C1 O1 Al1 130.8(2) . . ? Al2 O1 Al1 100.68(11) . . ? C3 O2 Al2 129.4(2) . . ? C3 O2 Al1 129.5(2) . . ? Al2 O2 Al1 100.15(11) . . ? C5 O3 Al3 128.6(2) . . ? C5 O3 Al1 130.2(2) . . ? Al3 O3 Al1 100.65(11) . . ? C7 O4 Al3 130.2(2) . . ? C7 O4 Al1 129.0(2) . . ? Al3 O4 Al1 100.03(11) . . ? C9 O5 Al4 131.0(2) . . ? C9 O5 Al1 128.5(2) . . ? Al4 O5 Al1 100.44(11) . . ? C11 O6 Al4 126.8(2) . . ? C11 O6 Al1 130.8(2) . . ? Al4 O6 Al1 99.75(11) . . ? O1 C1 C2 112.3(3) . . ? O1 C1 H1A 109.2 . . ? C2 C1 H1A 109.2 . . ? O1 C1 H1B 109.2 . . ? C2 C1 H1B 109.2 . . ? H1A C1 H1B 107.9 . . ? C1 C2 H2A 109.5 . . ? C1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? O2 C3 C4 111.9(3) . . ? O2 C3 H3A 109.2 . . ? C4 C3 H3A 109.2 . . ? O2 C3 H3B 109.2 . . ? C4 C3 H3B 109.2 . . ? H3A C3 H3B 107.9 . . ? C3 C4 H4A 109.5 . . ? C3 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C3 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? O3 C5 C6 114.2(3) . . ? O3 C5 H5A 108.7 . . ? C6 C5 H5A 108.7 . . ? O3 C5 H5B 108.7 . . ? C6 C5 H5B 108.7 . . ? H5A C5 H5B 107.6 . . ? C5 C6 H6A 109.5 . . ? C5 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C5 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? O4 C7 C8 113.0(3) . . ? O4 C7 H7A 109.0 . . ? C8 C7 H7A 109.0 . . ? O4 C7 H7B 109.0 . . ? C8 C7 H7B 109.0 . . ? H7A C7 H7B 107.8 . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? O5 C9 C10 112.0(3) . . ? O5 C9 H9A 109.2 . . ? C10 C9 H9A 109.2 . . ? O5 C9 H9B 109.2 . . ? C10 C9 H9B 109.2 . . ? H9A C9 H9B 107.9 . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? O6 C11 C12 112.3(3) . . ? O6 C11 H11A 109.1 . . ? C12 C11 H11A 109.1 . . ? O6 C11 H11B 109.1 . . ? C12 C11 H11B 109.1 . . ? H11A C11 H11B 107.9 . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O3 Al1 Al2 O1 89.26(14) . . . . ? O5 Al1 Al2 O1 -14.21(15) . . . . ? O2 Al1 Al2 O1 -179.28(17) . . . . ? O6 Al1 Al2 O1 -91.69(14) . . . . ? O4 Al1 Al2 O1 167.98(16) . . . . ? Al4 Al1 Al2 O1 -56.98(12) . . . . ? Al3 Al1 Al2 O1 121.44(13) . . . . ? O3 Al1 Al2 O2 -91.46(13) . . . . ? O5 Al1 Al2 O2 165.07(16) . . . . ? O1 Al1 Al2 O2 179.28(17) . . . . ? O6 Al1 Al2 O2 87.59(14) . . . . ? O4 Al1 Al2 O2 -12.73(15) . . . . ? Al4 Al1 Al2 O2 122.30(12) . . . . ? Al3 Al1 Al2 O2 -59.27(12) . . . . ? O3 Al1 Al2 Br2 -0.24(9) . . . . ? O5 Al1 Al2 Br2 -103.71(12) . . . . ? O1 Al1 Al2 Br2 -89.50(13) . . . . ? O2 Al1 Al2 Br2 91.21(12) . . . . ? O6 Al1 Al2 Br2 178.80(8) . . . . ? O4 Al1 Al2 Br2 78.48(12) . . . . ? Al4 Al1 Al2 Br2 -146.48(5) . . . . ? Al3 Al1 Al2 Br2 31.94(8) . . . . ? O3 Al1 Al2 Br1 179.67(8) . . . . ? O5 Al1 Al2 Br1 76.20(12) . . . . ? O1 Al1 Al2 Br1 90.41(13) . . . . ? O2 Al1 Al2 Br1 -88.87(12) . . . . ? O6 Al1 Al2 Br1 -1.28(10) . . . . ? O4 Al1 Al2 Br1 -101.60(12) . . . . ? Al4 Al1 Al2 Br1 33.43(8) . . . . ? Al3 Al1 Al2 Br1 -148.14(5) . . . . ? O5 Al1 Al3 O3 88.53(14) . . . . ? O1 Al1 Al3 O3 -12.59(15) . . . . ? O2 Al1 Al3 O3 -91.37(13) . . . . ? O6 Al1 Al3 O3 166.87(16) . . . . ? O4 Al1 Al3 O3 -179.76(16) . . . . ? Al4 Al1 Al3 O3 119.54(12) . . . . ? Al2 Al1 Al3 O3 -58.77(12) . . . . ? O3 Al1 Al3 O4 179.76(16) . . . . ? O5 Al1 Al3 O4 -91.71(13) . . . . ? O1 Al1 Al3 O4 167.17(16) . . . . ? O2 Al1 Al3 O4 88.39(13) . . . . ? O6 Al1 Al3 O4 -13.38(15) . . . . ? Al4 Al1 Al3 O4 -60.70(12) . . . . ? Al2 Al1 Al3 O4 120.98(12) . . . . ? O3 Al1 Al3 Br4 -90.09(12) . . . . ? O5 Al1 Al3 Br4 -1.56(10) . . . . ? O1 Al1 Al3 Br4 -102.68(12) . . . . ? O2 Al1 Al3 Br4 178.54(8) . . . . ? O6 Al1 Al3 Br4 76.77(12) . . . . ? O4 Al1 Al3 Br4 90.15(12) . . . . ? Al4 Al1 Al3 Br4 29.45(8) . . . . ? Al2 Al1 Al3 Br4 -148.87(5) . . . . ? O3 Al1 Al3 Br3 88.08(12) . . . . ? O5 Al1 Al3 Br3 176.61(8) . . . . ? O1 Al1 Al3 Br3 75.49(12) . . . . ? O2 Al1 Al3 Br3 -3.29(10) . . . . ? O6 Al1 Al3 Br3 -105.05(11) . . . . ? O4 Al1 Al3 Br3 -91.68(12) . . . . ? Al4 Al1 Al3 Br3 -152.38(5) . . . . ? Al2 Al1 Al3 Br3 29.30(8) . . . . ? O3 Al1 Al4 O5 -8.95(15) . . . . ? O1 Al1 Al4 O5 91.42(14) . . . . ? O2 Al1 Al4 O5 165.63(16) . . . . ? O6 Al1 Al4 O5 -171.90(17) . . . . ? O4 Al1 Al4 O5 -89.07(14) . . . . ? Al3 Al1 Al4 O5 -55.90(12) . . . . ? Al2 Al1 Al4 O5 122.51(13) . . . . ? O3 Al1 Al4 O6 162.96(16) . . . . ? O5 Al1 Al4 O6 171.90(17) . . . . ? O1 Al1 Al4 O6 -96.67(14) . . . . ? O2 Al1 Al4 O6 -22.47(15) . . . . ? O4 Al1 Al4 O6 82.84(13) . . . . ? Al3 Al1 Al4 O6 116.01(13) . . . . ? Al2 Al1 Al4 O6 -65.59(12) . . . . ? O3 Al1 Al4 Br5 75.29(13) . . . . ? O5 Al1 Al4 Br5 84.24(13) . . . . ? O1 Al1 Al4 Br5 175.66(8) . . . . ? O2 Al1 Al4 Br5 -110.13(12) . . . . ? O6 Al1 Al4 Br5 -87.66(13) . . . . ? O4 Al1 Al4 Br5 -4.83(10) . . . . ? Al3 Al1 Al4 Br5 28.34(9) . . . . ? Al2 Al1 Al4 Br5 -153.25(6) . . . . ? O3 Al1 Al4 Br6 -106.90(11) . . . . ? O5 Al1 Al4 Br6 -97.96(13) . . . . ? O1 Al1 Al4 Br6 -6.54(9) . . . . ? O2 Al1 Al4 Br6 67.67(12) . . . . ? O6 Al1 Al4 Br6 90.14(12) . . . . ? O4 Al1 Al4 Br6 172.98(8) . . . . ? Al3 Al1 Al4 Br6 -153.86(5) . . . . ? Al2 Al1 Al4 Br6 24.55(7) . . . . ? O2 Al2 O1 C1 -172.2(3) . . . . ? Br2 Al2 O1 C1 -58.6(3) . . . . ? Br1 Al2 O1 C1 73.4(3) . . . . ? Al1 Al2 O1 C1 -171.7(3) . . . . ? O2 Al2 O1 Al1 -0.48(11) . . . . ? Br2 Al2 O1 Al1 113.11(9) . . . . ? Br1 Al2 O1 Al1 -114.90(9) . . . . ? O3 Al1 O1 C1 75.8(3) . . . . ? O5 Al1 O1 C1 -19.5(3) . . . . ? O2 Al1 O1 C1 171.8(3) . . . . ? O6 Al1 O1 C1 -96.0(3) . . . . ? O4 Al1 O1 C1 124.6(5) . . . . ? Al4 Al1 O1 C1 -57.7(3) . . . . ? Al3 Al1 O1 C1 83.6(3) . . . . ? Al2 Al1 O1 C1 171.3(3) . . . . ? O3 Al1 O1 Al2 -95.54(12) . . . . ? O5 Al1 O1 Al2 169.15(12) . . . . ? O2 Al1 O1 Al2 0.46(11) . . . . ? O6 Al1 O1 Al2 92.64(12) . . . . ? O4 Al1 O1 Al2 -46.7(5) . . . . ? Al4 Al1 O1 Al2 131.01(10) . . . . ? Al3 Al1 O1 Al2 -87.77(13) . . . . ? O1 Al2 O2 C3 170.0(3) . . . . ? Br2 Al2 O2 C3 57.4(3) . . . . ? Br1 Al2 O2 C3 -74.6(3) . . . . ? Al1 Al2 O2 C3 169.5(3) . . . . ? O1 Al2 O2 Al1 0.48(11) . . . . ? Br2 Al2 O2 Al1 -112.09(9) . . . . ? Br1 Al2 O2 Al1 115.91(9) . . . . ? O3 Al1 O2 C3 -75.6(3) . . . . ? O5 Al1 O2 C3 143.1(4) . . . . ? O1 Al1 O2 C3 -170.0(3) . . . . ? O6 Al1 O2 C3 94.6(3) . . . . ? O4 Al1 O2 C3 1.2(3) . . . . ? Al4 Al1 O2 C3 108.4(3) . . . . ? Al3 Al1 O2 C3 -37.2(3) . . . . ? Al2 Al1 O2 C3 -169.5(3) . . . . ? O3 Al1 O2 Al2 93.87(12) . . . . ? O5 Al1 O2 Al2 -47.3(5) . . . . ? O1 Al1 O2 Al2 -0.46(11) . . . . ? O6 Al1 O2 Al2 -95.88(12) . . . . ? O4 Al1 O2 Al2 170.69(11) . . . . ? Al4 Al1 O2 Al2 -82.12(13) . . . . ? Al3 Al1 O2 Al2 132.29(9) . . . . ? O4 Al3 O3 C5 172.1(3) . . . . ? Br4 Al3 O3 C5 -73.7(3) . . . . ? Br3 Al3 O3 C5 57.6(3) . . . . ? Al1 Al3 O3 C5 172.2(4) . . . . ? O4 Al3 O3 Al1 -0.16(11) . . . . ? Br4 Al3 O3 Al1 114.11(9) . . . . ? Br3 Al3 O3 Al1 -114.66(9) . . . . ? O5 Al1 O3 C5 92.2(3) . . . . ? O1 Al1 O3 C5 -1.2(3) . . . . ? O2 Al1 O3 C5 -78.1(3) . . . . ? O6 Al1 O3 C5 144.4(5) . . . . ? O4 Al1 O3 C5 -171.9(3) . . . . ? Al4 Al1 O3 C5 97.7(3) . . . . ? Al3 Al1 O3 C5 -172.0(4) . . . . ? Al2 Al1 O3 C5 -39.4(3) . . . . ? O5 Al1 O3 Al3 -95.78(12) . . . . ? O1 Al1 O3 Al3 170.83(11) . . . . ? O2 Al1 O3 Al3 93.94(12) . . . . ? O6 Al1 O3 Al3 -43.6(5) . . . . ? O4 Al1 O3 Al3 0.16(10) . . . . ? Al4 Al1 O3 Al3 -90.25(13) . . . . ? Al2 Al1 O3 Al3 132.63(9) . . . . ? O3 Al3 O4 C7 170.8(3) . . . . ? Br4 Al3 O4 C7 56.4(3) . . . . ? Br3 Al3 O4 C7 -76.8(3) . . . . ? Al1 Al3 O4 C7 170.6(3) . . . . ? O3 Al3 O4 Al1 0.16(11) . . . . ? Br4 Al3 O4 Al1 -114.27(9) . . . . ? Br3 Al3 O4 Al1 112.59(9) . . . . ? O3 Al1 O4 C7 -170.9(3) . . . . ? O5 Al1 O4 C7 -77.5(3) . . . . ? O1 Al1 O4 C7 138.6(5) . . . . ? O2 Al1 O4 C7 92.9(3) . . . . ? O6 Al1 O4 C7 -0.9(3) . . . . ? Al4 Al1 O4 C7 -39.1(3) . . . . ? Al3 Al1 O4 C7 -170.8(3) . . . . ? Al2 Al1 O4 C7 100.8(3) . . . . ? O3 Al1 O4 Al3 -0.16(10) . . . . ? O5 Al1 O4 Al3 93.31(12) . . . . ? O1 Al1 O4 Al3 -50.6(5) . . . . ? O2 Al1 O4 Al3 -96.28(12) . . . . ? O6 Al1 O4 Al3 169.86(11) . . . . ? Al4 Al1 O4 Al3 131.73(9) . . . . ? Al2 Al1 O4 Al3 -88.38(12) . . . . ? O6 Al4 O5 C9 172.4(3) . . . . ? Br5 Al4 O5 C9 56.3(3) . . . . ? Br6 Al4 O5 C9 -77.8(3) . . . . ? Al1 Al4 O5 C9 177.9(4) . . . . ? O6 Al4 O5 Al1 -5.43(12) . . . . ? Br5 Al4 O5 Al1 -121.56(9) . . . . ? Br6 Al4 O5 Al1 104.31(10) . . . . ? O3 Al1 O5 C9 -4.5(3) . . . . ? O1 Al1 O5 C9 91.6(3) . . . . ? O2 Al1 O5 C9 136.9(4) . . . . ? O6 Al1 O5 C9 -172.8(3) . . . . ? O4 Al1 O5 C9 -81.3(3) . . . . ? Al4 Al1 O5 C9 -177.9(3) . . . . ? Al3 Al1 O5 C9 -42.8(3) . . . . ? Al2 Al1 O5 C9 100.3(3) . . . . ? O3 Al1 O5 Al4 173.42(11) . . . . ? O1 Al1 O5 Al4 -90.43(12) . . . . ? O2 Al1 O5 Al4 -45.2(5) . . . . ? O6 Al1 O5 Al4 5.17(11) . . . . ? O4 Al1 O5 Al4 96.65(12) . . . . ? Al3 Al1 O5 Al4 135.18(9) . . . . ? Al2 Al1 O5 Al4 -81.73(13) . . . . ? O5 Al4 O6 C11 168.4(3) . . . . ? Br5 Al4 O6 C11 -77.2(3) . . . . ? Br6 Al4 O6 C11 53.4(3) . . . . ? Al1 Al4 O6 C11 163.0(3) . . . . ? O5 Al4 O6 Al1 5.39(11) . . . . ? Br5 Al4 O6 Al1 119.70(9) . . . . ? Br6 Al4 O6 Al1 -109.65(9) . . . . ? O3 Al1 O6 C11 138.7(4) . . . . ? O5 Al1 O6 C11 -167.2(3) . . . . ? O1 Al1 O6 C11 -75.7(3) . . . . ? O2 Al1 O6 C11 0.9(3) . . . . ? O4 Al1 O6 C11 96.4(3) . . . . ? Al4 Al1 O6 C11 -162.0(3) . . . . ? Al3 Al1 O6 C11 104.7(3) . . . . ? Al2 Al1 O6 C11 -37.5(3) . . . . ? O3 Al1 O6 Al4 -59.3(5) . . . . ? O5 Al1 O6 Al4 -5.13(11) . . . . ? O1 Al1 O6 Al4 86.32(12) . . . . ? O2 Al1 O6 Al4 162.92(12) . . . . ? O4 Al1 O6 Al4 -101.52(12) . . . . ? Al3 Al1 O6 Al4 -93.28(12) . . . . ? Al2 Al1 O6 Al4 124.53(10) . . . . ? Al2 O1 C1 C2 -33.4(4) . . . . ? Al1 O1 C1 C2 157.4(3) . . . . ? Al2 O2 C3 C4 25.6(5) . . . . ? Al1 O2 C3 C4 -167.8(2) . . . . ? Al3 O3 C5 C6 17.3(5) . . . . ? Al1 O3 C5 C6 -172.7(3) . . . . ? Al3 O4 C7 C8 11.6(5) . . . . ? Al1 O4 C7 C8 179.7(3) . . . . ? Al4 O5 C9 C10 13.9(5) . . . . ? Al1 O5 C9 C10 -168.8(3) . . . . ? Al4 O6 C11 C12 49.2(4) . . . . ? Al1 O6 C11 C12 -153.1(3) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.762 _refine_diff_density_min -0.647 _refine_diff_density_rms 0.128