# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_coden_Cambridge 222 _journal_volume ? _journal_page_first ? _journal_year ? loop_ _publ_author_name 'Dominic S. Wright' 'Thomas H. Bullock' 'Wesley Ting Kwok Chan.' _publ_contact_author_name 'Dominic S. Wright' _publ_contact_author_email DSW1000@CAM.AC.UK _publ_section_title ; Synergic anion and cation coordination using the tripodal aluminate anion [MeAl(2-py)3] - (py = 2-pyridyl) ; # Attachment 'dw0851.cif' data_dw0851 _database_code_depnum_ccdc_archive 'CCDC 733180' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C32 H30 Al2 Cl Li2 N6, C32 H30 Al3 N6, 2(C4 H8 O)' _chemical_formula_sum 'C72 H76 Al5 Cl Li2 N12 O2' _chemical_formula_weight 1325.68 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' Li Li -0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Al Al 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 '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' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.3535(3) _cell_length_b 11.9457(3) _cell_length_c 13.9801(4) _cell_angle_alpha 100.1982(10) _cell_angle_beta 98.4430(11) _cell_angle_gamma 104.4218(11) _cell_volume 1770.67(8) _cell_formula_units_Z 1 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 17174 _cell_measurement_theta_min 1.02 _cell_measurement_theta_max 27.48 _exptl_crystal_description Needle _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.243 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 696 _exptl_absorpt_coefficient_mu 0.170 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.882 _exptl_absorpt_correction_T_max 0.987 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements Sortav (Blessing 1995) ; _exptl_special_details ; DFIX command was used to restrict the refinement of the disordered THF to avoid bond lengths becoming unrealistic. ; _diffrn_ambient_temperature 180(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_measurement_method 'Thin slice \w and \f scans' _diffrn_standards_number 0 _diffrn_reflns_number 20566 _diffrn_reflns_av_R_equivalents 0.0634 _diffrn_reflns_av_sigmaI/netI 0.0521 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.60 _diffrn_reflns_theta_max 23.25 _reflns_number_total 5076 _reflns_number_gt 3783 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius B.V. 1998)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction ; HKL Denzo and Scalepack (Otwinowski & Minor 1997) ; _computing_structure_solution 'SIR-92 (Altomare et al. 1994)' _computing_structure_refinement 'SHELXL-97 (Sheldrick 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick 1997)' _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^)+(0.0549P)^2^+2.7998P] 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 5076 _refine_ls_number_parameters 419 _refine_ls_number_restraints 10 _refine_ls_R_factor_all 0.0869 _refine_ls_R_factor_gt 0.0578 _refine_ls_wR_factor_ref 0.1516 _refine_ls_wR_factor_gt 0.1330 _refine_ls_goodness_of_fit_ref 1.028 _refine_ls_restrained_S_all 1.033 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cl1 Cl 1.0000 0.0000 0.5000 0.0772(6) Uani 1 2 d S . . Li1 Li 0.9885(6) 0.0884(5) 0.6553(4) 0.0373(14) Uani 1 1 d . . . Al1 Al 0.95012(10) 0.19749(10) 0.86377(8) 0.0351(3) Uani 1 1 d . . . C1 C 0.9282(4) 0.2626(4) 0.9984(3) 0.0530(11) Uani 1 1 d . . . H1A H 0.8479 0.2182 1.0089 0.079 Uiso 1 1 calc R . . H1B H 0.9308 0.3463 1.0049 0.079 Uiso 1 1 calc R . . H1C H 0.9950 0.2557 1.0480 0.079 Uiso 1 1 calc R . . N1 N 1.0936(3) 0.0544(3) 0.7732(2) 0.0366(7) Uani 1 1 d . . . C11 C 1.0749(3) 0.1034(3) 0.8641(3) 0.0351(9) Uani 1 1 d . . . C12 C 1.1458(4) 0.0882(4) 0.9489(3) 0.0547(12) Uani 1 1 d . . . H12 H 1.1330 0.1203 1.0124 0.066 Uiso 1 1 calc R . . C13 C 1.2346(5) 0.0270(5) 0.9421(4) 0.0734(15) Uani 1 1 d . . . H13 H 1.2832 0.0186 1.0003 0.088 Uiso 1 1 calc R . . C14 C 1.2512(5) -0.0211(4) 0.8498(4) 0.0646(13) Uani 1 1 d . . . H14 H 1.3111 -0.0635 0.8426 0.078 Uiso 1 1 calc R . . C15 C 1.1781(4) -0.0057(3) 0.7684(3) 0.0470(10) Uani 1 1 d . . . H15 H 1.1883 -0.0401 0.7046 0.056 Uiso 1 1 calc R . . N2 N 0.8094(3) 0.0474(2) 0.6782(2) 0.0355(7) Uani 1 1 d . . . C21 C 0.7915(3) 0.0942(3) 0.7699(3) 0.0343(9) Uani 1 1 d . . . C22 C 0.6699(4) 0.0743(3) 0.7846(3) 0.0447(10) Uani 1 1 d . . . H22 H 0.6555 0.1051 0.8479 0.054 Uiso 1 1 calc R . . C23 C 0.5701(4) 0.0112(4) 0.7098(3) 0.0500(11) Uani 1 1 d . . . H23 H 0.4879 -0.0003 0.7212 0.060 Uiso 1 1 calc R . . C24 C 0.5902(4) -0.0348(3) 0.6192(3) 0.0487(11) Uani 1 1 d . . . H24 H 0.5229 -0.0790 0.5664 0.058 Uiso 1 1 calc R . . C25 C 0.7104(4) -0.0152(3) 0.6067(3) 0.0417(10) Uani 1 1 d . . . H25 H 0.7248 -0.0477 0.5438 0.050 Uiso 1 1 calc R . . N3 N 1.0290(3) 0.2715(3) 0.6927(2) 0.0351(7) Uani 1 1 d . . . C31 C 1.0128(3) 0.3185(3) 0.7848(3) 0.0357(9) Uani 1 1 d . . . C32 C 1.0375(4) 0.4420(3) 0.8141(3) 0.0462(10) Uani 1 1 d . . . H32 H 1.0288 0.4760 0.8785 0.055 Uiso 1 1 calc R . . C33 C 1.0739(4) 0.5151(4) 0.7514(4) 0.0563(12) Uani 1 1 d . . . H33 H 1.0893 0.5984 0.7719 0.068 Uiso 1 1 calc R . . C34 C 1.0879(4) 0.4649(4) 0.6580(4) 0.0533(11) Uani 1 1 d . . . H34 H 1.1121 0.5127 0.6128 0.064 Uiso 1 1 calc R . . C35 C 1.0658(3) 0.3443(4) 0.6328(3) 0.0435(10) Uani 1 1 d . . . H35 H 1.0772 0.3100 0.5693 0.052 Uiso 1 1 calc R . . Al3 Al 0.5000 0.5000 0.5000 0.0272(3) Uani 1 2 d S . . Al2 Al 0.46827(10) 0.65693(9) 0.71908(8) 0.0320(3) Uani 1 1 d . . . C2 C 0.4522(4) 0.7482(4) 0.8441(3) 0.0461(10) Uani 1 1 d . . . H2A H 0.4805 0.8330 0.8454 0.069 Uiso 1 1 calc R . . H2B H 0.5029 0.7305 0.8993 0.069 Uiso 1 1 calc R . . H2C H 0.3650 0.7269 0.8506 0.069 Uiso 1 1 calc R . . N4 N 0.4272(3) 0.4201(3) 0.6103(2) 0.0389(8) Uani 1 1 d . . . C41 C 0.4181(3) 0.4844(3) 0.7005(2) 0.0231(7) Uani 1 1 d . . . C42 C 0.3728(3) 0.4252(3) 0.7694(3) 0.0383(9) Uani 1 1 d . . . H42 H 0.3684 0.4702 0.8313 0.046 Uiso 1 1 calc R . . C43 C 0.3339(4) 0.3041(4) 0.7519(3) 0.0436(10) Uani 1 1 d . . . H43 H 0.3023 0.2653 0.8004 0.052 Uiso 1 1 calc R . . C44 C 0.3417(4) 0.2398(3) 0.6620(3) 0.0429(10) Uani 1 1 d . . . H44 H 0.3154 0.1556 0.6473 0.051 Uiso 1 1 calc R . . C45 C 0.3882(3) 0.2992(3) 0.5940(3) 0.0349(9) Uani 1 1 d . . . H45 H 0.3935 0.2540 0.5325 0.042 Uiso 1 1 calc R . . N5 N 0.6516(3) 0.6222(3) 0.6045(2) 0.0380(8) Uani 1 1 d . . . C51 C 0.6359(3) 0.6885(3) 0.6905(2) 0.0254(8) Uani 1 1 d . . . C52 C 0.7385(4) 0.7703(3) 0.7532(3) 0.0397(9) Uani 1 1 d . . . H52 H 0.7273 0.8167 0.8120 0.048 Uiso 1 1 calc R . . C53 C 0.8560(4) 0.7873(3) 0.7338(3) 0.0472(11) Uani 1 1 d . . . H53 H 0.9252 0.8439 0.7782 0.057 Uiso 1 1 calc R . . C54 C 0.8705(4) 0.7201(4) 0.6482(3) 0.0456(10) Uani 1 1 d . . . H54 H 0.9504 0.7292 0.6324 0.055 Uiso 1 1 calc R . . C55 C 0.7683(3) 0.6395(3) 0.5857(3) 0.0392(9) Uani 1 1 d . . . H55 H 0.7796 0.5937 0.5266 0.047 Uiso 1 1 calc R . . N6 N 0.3889(3) 0.6191(3) 0.5085(2) 0.0339(7) Uani 1 1 d . . . C61 C 0.3712(3) 0.6772(3) 0.5967(2) 0.0281(8) Uani 1 1 d . . . C62 C 0.2923(3) 0.7491(3) 0.5946(3) 0.0368(9) Uani 1 1 d . . . H62 H 0.2785 0.7881 0.6555 0.044 Uiso 1 1 calc R . . C63 C 0.2332(3) 0.7660(3) 0.5071(3) 0.0426(10) Uani 1 1 d . . . H63 H 0.1797 0.8158 0.5074 0.051 Uiso 1 1 calc R . . C64 C 0.2540(4) 0.7086(3) 0.4191(3) 0.0428(10) Uani 1 1 d . . . H64 H 0.2162 0.7192 0.3573 0.051 Uiso 1 1 calc R . . C65 C 0.3300(3) 0.6361(3) 0.4225(3) 0.0358(9) Uani 1 1 d . . . H65 H 0.3422 0.5955 0.3616 0.043 Uiso 1 1 calc R . . O1 O 0.3823(7) 0.5284(6) 0.0160(6) 0.106(2) Uiso 0.60 1 d PD A 1 C71 C 0.2890(12) 0.4338(10) 0.0287(9) 0.110(3) Uiso 0.60 1 d PD A 1 H71A H 0.3196 0.3639 0.0336 0.132 Uiso 0.60 1 calc PR A 1 H71B H 0.2158 0.4107 -0.0262 0.132 Uiso 0.60 1 calc PR A 1 C72 C 0.2598(13) 0.4848(8) 0.1232(9) 0.103(4) Uiso 0.60 1 d PD A 1 H72A H 0.2904 0.4472 0.1757 0.123 Uiso 0.60 1 calc PR A 1 H72B H 0.1687 0.4678 0.1163 0.123 Uiso 0.60 1 calc PR A 1 C73 C 0.3173(8) 0.6141(6) 0.1527(5) 0.0413(16) Uiso 0.60 1 d PD A 1 H73A H 0.3818 0.6365 0.2141 0.050 Uiso 0.60 1 calc PR A 1 H73B H 0.2547 0.6576 0.1621 0.050 Uiso 0.60 1 calc PR A 1 C74 C 0.3731(7) 0.6357(6) 0.0636(5) 0.0517(16) Uiso 0.60 1 d PD A 1 H74A H 0.3194 0.6665 0.0190 0.062 Uiso 0.60 1 calc PR A 1 H74B H 0.4561 0.6941 0.0848 0.062 Uiso 0.60 1 calc PR A 1 O1' O 0.3053(11) 0.3947(9) 0.1109(7) 0.110(3) Uiso 0.40 1 d PD B 2 C71' C 0.3235(11) 0.4377(9) 0.0293(8) 0.0413(16) Uiso 0.40 1 d PD B 2 H71C H 0.2611 0.3823 -0.0272 0.050 Uiso 0.40 1 calc PR B 2 H71D H 0.4057 0.4310 0.0177 0.050 Uiso 0.40 1 calc PR B 2 C72' C 0.3199(19) 0.5604(11) 0.0210(12) 0.106(2) Uiso 0.40 1 d PD B 2 H72C H 0.2501 0.5608 -0.0304 0.127 Uiso 0.40 1 calc PR B 2 H72D H 0.3993 0.6097 0.0111 0.127 Uiso 0.40 1 calc PR B 2 C73' C 0.298(2) 0.5928(13) 0.1268(12) 0.103(4) Uiso 0.40 1 d PD B 2 H73D H 0.3759 0.6426 0.1724 0.123 Uiso 0.40 1 calc PR B 2 H73E H 0.2345 0.6363 0.1286 0.123 Uiso 0.40 1 calc PR B 2 C74' C 0.2549(12) 0.4782(9) 0.1543(10) 0.0517(16) Uiso 0.40 1 d PD B 2 H74D H 0.2769 0.4899 0.2273 0.062 Uiso 0.40 1 calc PR B 2 H74E H 0.1633 0.4490 0.1343 0.062 Uiso 0.40 1 calc PR B 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 Cl1 0.0858(13) 0.0863(13) 0.0426(9) -0.0184(9) 0.0298(9) 0.0069(10) Li1 0.038(3) 0.042(3) 0.027(3) -0.002(3) 0.007(3) 0.010(3) Al1 0.0384(7) 0.0344(6) 0.0296(6) 0.0008(5) 0.0060(5) 0.0099(5) C1 0.062(3) 0.056(3) 0.039(2) 0.000(2) 0.013(2) 0.017(2) N1 0.0368(18) 0.0296(16) 0.0425(19) 0.0056(14) 0.0094(14) 0.0082(14) C11 0.034(2) 0.0299(19) 0.035(2) 0.0061(16) 0.0039(17) 0.0016(16) C12 0.063(3) 0.060(3) 0.042(2) 0.011(2) 0.002(2) 0.024(2) C13 0.078(4) 0.083(4) 0.068(4) 0.025(3) -0.003(3) 0.043(3) C14 0.063(3) 0.061(3) 0.083(4) 0.023(3) 0.014(3) 0.035(3) C15 0.050(3) 0.036(2) 0.060(3) 0.012(2) 0.018(2) 0.015(2) N2 0.0383(18) 0.0282(16) 0.0345(18) 0.0031(14) 0.0022(14) 0.0052(14) C21 0.039(2) 0.0290(19) 0.035(2) 0.0073(16) 0.0082(17) 0.0103(17) C22 0.047(3) 0.043(2) 0.046(2) 0.0101(19) 0.016(2) 0.0120(19) C23 0.034(2) 0.046(2) 0.069(3) 0.015(2) 0.010(2) 0.0072(19) C24 0.041(3) 0.041(2) 0.052(3) 0.011(2) -0.005(2) -0.0021(19) C25 0.046(3) 0.034(2) 0.036(2) 0.0045(18) -0.0025(19) 0.0032(18) N3 0.0302(17) 0.0374(17) 0.0358(18) 0.0055(15) 0.0059(14) 0.0082(14) C31 0.0266(19) 0.034(2) 0.041(2) 0.0028(17) 0.0014(16) 0.0074(16) C32 0.048(2) 0.036(2) 0.052(3) 0.005(2) 0.009(2) 0.0089(19) C33 0.050(3) 0.032(2) 0.083(4) 0.007(2) 0.011(2) 0.010(2) C34 0.043(3) 0.047(3) 0.075(3) 0.030(2) 0.015(2) 0.008(2) C35 0.037(2) 0.050(3) 0.044(2) 0.016(2) 0.0094(19) 0.0091(19) Al3 0.0282(8) 0.0280(8) 0.0238(8) 0.0045(6) 0.0054(6) 0.0061(6) Al2 0.0381(6) 0.0301(6) 0.0268(6) 0.0046(5) 0.0074(5) 0.0089(5) C2 0.060(3) 0.044(2) 0.038(2) 0.0077(19) 0.012(2) 0.021(2) N4 0.0364(18) 0.0424(19) 0.0361(18) 0.0095(15) 0.0063(14) 0.0081(15) C41 0.0212(17) 0.0278(17) 0.0194(17) 0.0035(14) 0.0031(14) 0.0068(14) C42 0.039(2) 0.045(2) 0.030(2) 0.0097(18) 0.0092(17) 0.0075(18) C43 0.042(2) 0.048(2) 0.041(2) 0.021(2) 0.0112(18) 0.0034(19) C44 0.042(2) 0.031(2) 0.052(3) 0.0135(19) 0.0058(19) 0.0027(18) C45 0.041(2) 0.0265(19) 0.035(2) 0.0058(16) 0.0092(17) 0.0048(16) N5 0.0409(19) 0.0382(18) 0.0317(17) 0.0094(14) 0.0041(14) 0.0065(15) C51 0.0313(19) 0.0186(16) 0.0230(18) 0.0035(14) 0.0012(15) 0.0046(14) C52 0.046(2) 0.029(2) 0.036(2) 0.0041(17) 0.0015(18) 0.0017(18) C53 0.041(2) 0.038(2) 0.049(3) 0.009(2) -0.006(2) -0.0037(19) C54 0.031(2) 0.051(2) 0.050(3) 0.017(2) 0.0052(19) -0.0002(19) C55 0.029(2) 0.047(2) 0.039(2) 0.0104(18) 0.0097(17) 0.0034(18) N6 0.0327(17) 0.0341(16) 0.0335(17) 0.0078(14) 0.0071(14) 0.0067(14) C61 0.0299(19) 0.0217(17) 0.0308(19) 0.0039(15) 0.0077(15) 0.0040(15) C62 0.037(2) 0.0310(19) 0.041(2) 0.0032(17) 0.0117(18) 0.0082(17) C63 0.034(2) 0.040(2) 0.056(3) 0.013(2) 0.0059(19) 0.0146(18) C64 0.042(2) 0.048(2) 0.043(2) 0.019(2) 0.0042(18) 0.016(2) C65 0.035(2) 0.042(2) 0.030(2) 0.0091(17) 0.0028(16) 0.0109(18) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cl1 Li1 2.278(6) . ? Cl1 Li1 2.278(6) 2_756 ? Li1 N1 2.051(7) . ? Li1 N2 2.055(7) . ? Li1 N3 2.071(7) . ? Al1 C1 1.981(4) . ? Al1 C11 2.016(4) . ? Al1 C31 2.024(4) . ? Al1 C21 2.028(4) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? N1 C15 1.337(5) . ? N1 C11 1.371(5) . ? C11 C12 1.398(5) . ? C12 C13 1.389(6) . ? C12 H12 0.9500 . ? C13 C14 1.376(7) . ? C13 H13 0.9500 . ? C14 C15 1.375(6) . ? C14 H14 0.9500 . ? C15 H15 0.9500 . ? N2 C25 1.345(5) . ? N2 C21 1.371(5) . ? C21 C22 1.394(5) . ? C22 C23 1.376(6) . ? C22 H22 0.9500 . ? C23 C24 1.364(6) . ? C23 H23 0.9500 . ? C24 C25 1.369(6) . ? C24 H24 0.9500 . ? C25 H25 0.9500 . ? N3 C35 1.346(5) . ? N3 C31 1.369(5) . ? C31 C32 1.403(5) . ? C32 C33 1.377(6) . ? C32 H32 0.9500 . ? C33 C34 1.387(6) . ? C33 H33 0.9500 . ? C34 C35 1.370(6) . ? C34 H34 0.9500 . ? C35 H35 0.9500 . ? Al3 N4 2.115(3) . ? Al3 N4 2.115(3) 2_666 ? Al3 N5 2.117(3) 2_666 ? Al3 N5 2.117(3) . ? Al3 N6 2.123(3) . ? Al3 N6 2.123(3) 2_666 ? Al2 C2 1.948(4) . ? Al2 C41 1.955(3) . ? Al2 C51 1.960(4) . ? Al2 C61 1.981(4) . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? N4 C45 1.367(5) . ? N4 C41 1.387(4) . ? C41 C42 1.378(5) . ? C42 C43 1.369(5) . ? C42 H42 0.9500 . ? C43 C44 1.380(6) . ? C43 H43 0.9500 . ? C44 C45 1.373(5) . ? C44 H44 0.9500 . ? C45 H45 0.9500 . ? N5 C55 1.362(5) . ? N5 C51 1.378(4) . ? C51 C52 1.382(5) . ? C52 C53 1.374(6) . ? C52 H52 0.9500 . ? C53 C54 1.374(6) . ? C53 H53 0.9500 . ? C54 C55 1.372(5) . ? C54 H54 0.9500 . ? C55 H55 0.9500 . ? N6 C65 1.361(4) . ? N6 C61 1.372(4) . ? C61 C62 1.388(5) . ? C62 C63 1.378(5) . ? C62 H62 0.9500 . ? C63 C64 1.381(6) . ? C63 H63 0.9500 . ? C64 C65 1.367(5) . ? C64 H64 0.9500 . ? C65 H65 0.9500 . ? O1 C74 1.372(7) . ? O1 C71 1.400(9) . ? C71 C72 1.474(9) . ? C71 H71A 0.9900 . ? C71 H71B 0.9900 . ? C72 C73 1.475(8) . ? C72 H72A 0.9900 . ? C72 H72B 0.9900 . ? C73 C74 1.511(7) . ? C73 H73A 0.9900 . ? C73 H73B 0.9900 . ? C74 H74A 0.9900 . ? C74 H74B 0.9900 . ? O1' C71' 1.353(9) . ? O1' C74' 1.364(9) . ? C71' C72' 1.500(9) . ? C71' H71C 0.9900 . ? C71' H71D 0.9900 . ? C72' C73' 1.533(10) . ? C72' H72C 0.9900 . ? C72' H72D 0.9900 . ? C73' C74' 1.473(10) . ? C73' H73D 0.9900 . ? C73' H73E 0.9900 . ? C74' H74D 0.9900 . ? C74' H74E 0.9900 . ? 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 Li1 Cl1 Li1 180.000(1) . 2_756 ? N1 Li1 N2 105.9(3) . . ? N1 Li1 N3 102.0(3) . . ? N2 Li1 N3 98.4(3) . . ? N1 Li1 Cl1 117.6(3) . . ? N2 Li1 Cl1 111.9(3) . . ? N3 Li1 Cl1 118.6(3) . . ? C1 Al1 C11 113.30(18) . . ? C1 Al1 C31 115.77(18) . . ? C11 Al1 C31 103.10(15) . . ? C1 Al1 C21 114.51(18) . . ? C11 Al1 C21 107.46(15) . . ? C31 Al1 C21 101.38(15) . . ? Al1 C1 H1A 109.5 . . ? Al1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? Al1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C15 N1 C11 119.4(3) . . ? C15 N1 Li1 126.3(3) . . ? C11 N1 Li1 114.3(3) . . ? N1 C11 C12 118.2(4) . . ? N1 C11 Al1 116.4(3) . . ? C12 C11 Al1 125.3(3) . . ? C13 C12 C11 121.3(4) . . ? C13 C12 H12 119.3 . . ? C11 C12 H12 119.3 . . ? C14 C13 C12 119.1(4) . . ? C14 C13 H13 120.5 . . ? C12 C13 H13 120.5 . . ? C15 C14 C13 117.7(4) . . ? C15 C14 H14 121.2 . . ? C13 C14 H14 121.2 . . ? N1 C15 C14 124.3(4) . . ? N1 C15 H15 117.9 . . ? C14 C15 H15 117.9 . . ? C25 N2 C21 119.3(3) . . ? C25 N2 Li1 123.5(3) . . ? C21 N2 Li1 117.0(3) . . ? N2 C21 C22 117.8(3) . . ? N2 C21 Al1 113.5(3) . . ? C22 C21 Al1 128.5(3) . . ? C23 C22 C21 121.7(4) . . ? C23 C22 H22 119.1 . . ? C21 C22 H22 119.1 . . ? C24 C23 C22 119.5(4) . . ? C24 C23 H23 120.3 . . ? C22 C23 H23 120.3 . . ? C23 C24 C25 117.8(4) . . ? C23 C24 H24 121.1 . . ? C25 C24 H24 121.1 . . ? N2 C25 C24 123.8(4) . . ? N2 C25 H25 118.1 . . ? C24 C25 H25 118.1 . . ? C35 N3 C31 119.3(3) . . ? C35 N3 Li1 125.0(3) . . ? C31 N3 Li1 115.7(3) . . ? N3 C31 C32 118.4(4) . . ? N3 C31 Al1 114.7(3) . . ? C32 C31 Al1 126.9(3) . . ? C33 C32 C31 121.5(4) . . ? C33 C32 H32 119.3 . . ? C31 C32 H32 119.3 . . ? C32 C33 C34 118.9(4) . . ? C32 C33 H33 120.6 . . ? C34 C33 H33 120.6 . . ? C35 C34 C33 118.0(4) . . ? C35 C34 H34 121.0 . . ? C33 C34 H34 121.0 . . ? N3 C35 C34 123.9(4) . . ? N3 C35 H35 118.1 . . ? C34 C35 H35 118.1 . . ? N4 Al3 N4 180.000(1) . 2_666 ? N4 Al3 N5 87.22(12) . 2_666 ? N4 Al3 N5 92.78(12) 2_666 2_666 ? N4 Al3 N5 92.78(12) . . ? N4 Al3 N5 87.22(12) 2_666 . ? N5 Al3 N5 180.000(1) 2_666 . ? N4 Al3 N6 92.67(12) . . ? N4 Al3 N6 87.33(12) 2_666 . ? N5 Al3 N6 87.08(12) 2_666 . ? N5 Al3 N6 92.92(12) . . ? N4 Al3 N6 87.33(12) . 2_666 ? N4 Al3 N6 92.67(12) 2_666 2_666 ? N5 Al3 N6 92.92(12) 2_666 2_666 ? N5 Al3 N6 87.08(12) . 2_666 ? N6 Al3 N6 180.000(1) . 2_666 ? C2 Al2 C41 116.67(16) . . ? C2 Al2 C51 115.99(17) . . ? C41 Al2 C51 102.29(14) . . ? C2 Al2 C61 116.52(16) . . ? C41 Al2 C61 101.24(14) . . ? C51 Al2 C61 101.71(15) . . ? Al2 C2 H2A 109.5 . . ? Al2 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? Al2 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C45 N4 C41 117.4(3) . . ? C45 N4 Al3 119.4(2) . . ? C41 N4 Al3 123.3(2) . . ? C42 C41 N4 119.5(3) . . ? C42 C41 Al2 124.2(3) . . ? N4 C41 Al2 116.3(2) . . ? C43 C42 C41 122.5(4) . . ? C43 C42 H42 118.8 . . ? C41 C42 H42 118.8 . . ? C42 C43 C44 118.2(4) . . ? C42 C43 H43 120.9 . . ? C44 C43 H43 120.9 . . ? C45 C44 C43 119.1(4) . . ? C45 C44 H44 120.5 . . ? C43 C44 H44 120.5 . . ? N4 C45 C44 123.4(3) . . ? N4 C45 H45 118.3 . . ? C44 C45 H45 118.3 . . ? C55 N5 C51 118.3(3) . . ? C55 N5 Al3 119.6(2) . . ? C51 N5 Al3 122.1(2) . . ? N5 C51 C52 118.9(3) . . ? N5 C51 Al2 117.6(2) . . ? C52 C51 Al2 123.5(3) . . ? C53 C52 C51 122.6(4) . . ? C53 C52 H52 118.7 . . ? C51 C52 H52 118.7 . . ? C52 C53 C54 118.0(4) . . ? C52 C53 H53 121.0 . . ? C54 C53 H53 121.0 . . ? C55 C54 C53 119.4(4) . . ? C55 C54 H54 120.3 . . ? C53 C54 H54 120.3 . . ? N5 C55 C54 122.9(4) . . ? N5 C55 H55 118.6 . . ? C54 C55 H55 118.6 . . ? C65 N6 C61 118.6(3) . . ? C65 N6 Al3 118.5(2) . . ? C61 N6 Al3 122.9(2) . . ? N6 C61 C62 118.7(3) . . ? N6 C61 Al2 116.5(2) . . ? C62 C61 Al2 124.7(3) . . ? C63 C62 C61 122.3(3) . . ? C63 C62 H62 118.8 . . ? C61 C62 H62 118.8 . . ? C62 C63 C64 118.1(4) . . ? C62 C63 H63 120.9 . . ? C64 C63 H63 120.9 . . ? C65 C64 C63 118.8(4) . . ? C65 C64 H64 120.6 . . ? C63 C64 H64 120.6 . . ? N6 C65 C64 123.5(3) . . ? N6 C65 H65 118.3 . . ? C64 C65 H65 118.3 . . ? C74 O1 C71 111.8(8) . . ? O1 C71 C72 101.9(9) . . ? O1 C71 H71A 111.4 . . ? C72 C71 H71A 111.4 . . ? O1 C71 H71B 111.4 . . ? C72 C71 H71B 111.4 . . ? H71A C71 H71B 109.3 . . ? C71 C72 C73 111.2(9) . . ? C71 C72 H72A 109.4 . . ? C73 C72 H72A 109.4 . . ? C71 C72 H72B 109.4 . . ? C73 C72 H72B 109.4 . . ? H72A C72 H72B 108.0 . . ? C72 C73 C74 100.7(7) . . ? C72 C73 H73A 111.6 . . ? C74 C73 H73A 111.6 . . ? C72 C73 H73B 111.6 . . ? C74 C73 H73B 111.6 . . ? H73A C73 H73B 109.4 . . ? O1 C74 C73 106.5(6) . . ? O1 C74 H74A 110.4 . . ? C73 C74 H74A 110.4 . . ? O1 C74 H74B 110.4 . . ? C73 C74 H74B 110.4 . . ? H74A C74 H74B 108.6 . . ? C71' O1' C74' 97.7(10) . . ? O1' C71' C72' 123.1(11) . . ? O1' C71' H71C 106.6 . . ? C72' C71' H71C 106.6 . . ? O1' C71' H71D 106.6 . . ? C72' C71' H71D 106.6 . . ? H71C C71' H71D 106.5 . . ? C71' C72' C73' 93.2(11) . . ? C71' C72' H72C 113.1 . . ? C73' C72' H72C 113.1 . . ? C71' C72' H72D 113.1 . . ? C73' C72' H72D 113.1 . . ? H72C C72' H72D 110.5 . . ? C74' C73' C72' 104.8(12) . . ? C74' C73' H73D 110.8 . . ? C72' C73' H73D 110.8 . . ? C74' C73' H73E 110.8 . . ? C72' C73' H73E 110.8 . . ? H73D C73' H73E 108.9 . . ? O1' C74' C73' 112.5(12) . . ? O1' C74' H74D 109.1 . . ? C73' C74' H74D 109.1 . . ? O1' C74' H74E 109.1 . . ? C73' C74' H74E 109.1 . . ? H74D C74' H74E 107.8 . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 23.25 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.842 _refine_diff_density_min -0.379 _refine_diff_density_rms 0.059