Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2002 data_global _journal_coden_Cambridge 186 _publ_requested_journal 'Dalton Transactions' loop_ _publ_author_name 'Arnold, John' 'Cui, Chunming' 'Schmidt, Joseph A. R.' #------------------------------------------------------------------------------ # SUBMISSION DETAILS _publ_contact_author_name 'Prof John Arnold ' _publ_contact_author_address ; Department of Chemistry University of California at Berkeley & Chemical Sciences Division Lawrence Berkeley National Laborato Berkeley California 94720-1460 UNITED STATES OF AMERICA ; _publ_contact_author_email ' arnold@socrates.berkeley.edu ' _publ_contact_author_fax ' (510) 643-5482 ' #------------------------------------------------------------------------------ # TITLE AND AUTHOR LIST _publ_section_title ; An Unsolvated Lithium Trihydroaluminate and the Corresponding Alkynylaluminates Supported by an Anionic Triazacyclononane Ligand ; #------------------------------------------------------------------------------ # TEXT _publ_section_references ; SIR92: Altomare, A., Cascarano, M., Giacovazzo, C., Guagliardi, A. (1993). J. Appl. Cryst., 26, 343. SMART v5.052d: Area-Detector Software Package, Bruker Analytical X-ray Systems, Inc.: Madison, WI, (1995-99). SAINT: SAX Area-Detector Integration Program, V5.04; Siemens Industrial Automation, Inc.: Madison, WI, (1995). teXsan: Crystal Structure Analysis Package, Molecular Structure Corporation, (1985 & 1992). ; data_(iPr2-tacn)LiAlH3_1 _database_code_CSD 173850 #------------------------------------------------------------------------------ _audit_creation_date 'Sat Oct 20 10:36:58 2001' _audit_creation_method 'by teXsan' _audit_update_record ? #------------------------------------------------------------------------------ _cell_length_a 9.1950(1) _cell_length_b 13.4305(3) _cell_length_c 13.0959(3) _cell_angle_alpha 90 _cell_angle_beta 106.265(1) _cell_angle_gamma 90 _cell_volume 1552.53(5) _cell_formula_units_Z 4 _cell_measurement_temperature 139.2 _cell_measurement_reflns_used 3512 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 45.0 #------------------------------------------------------------------------------ _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n ' _symmetry_Int_Tables_number 14 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' '1/2-x,1/2+y,1/2-z' ' -x, -y, -z' '1/2+x,1/2-y,1/2+z' #------------------------------------------------------------------------------ _exptl_crystal_description 'block' _exptl_crystal_colour 'colorless' _exptl_crystal_size_max 0.320 _exptl_crystal_size_mid 0.280 _exptl_crystal_size_min 0.130 _exptl_crystal_density_diffrn 1.067 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _chemical_formula_weight 249.30 _chemical_formula_analytical ? _chemical_formula_sum 'C12 H29 Al Li N3 ' _chemical_formula_moiety 'C12 H29 Al Li N3 ' _chemical_formula_structural ? _chemical_compound_source ? _exptl_crystal_F_000 552.00 _exptl_absorpt_coefficient_mu 0.115 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details 'Blessing, 1995' _exptl_absorpt_correction_T_max 0.98 _exptl_absorpt_correction_T_min 0.50 #------------------------------------------------------------------------------ _diffrn_special_details none _diffrn_ambient_temperature 139.2 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'X-ray tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'SMART CCD' _diffrn_measurement_method \w-scan _diffrn_reflns_number 6935 _reflns_number_total 2678 _reflns_number_gt 1870 _reflns_threshold_expression 'I>3.00sigma' _diffrn_reflns_av_R_equivalents 0.0415 _diffrn_reflns_av_sigmaI/netI ? _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.5 _diffrn_reflns_theta_max 24.69 _diffrn_reflns_reduction_process ? #------------------------------------------------------------------------------ _refine_special_details ? _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme sigma _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef 0.00000 _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 1870 _refine_ls_number_parameters 166 _refine_ls_number_restraints 0 _refine_ls_number_constraints ? _refine_ls_R_factor_all 0.0590 _refine_ls_R_factor_gt 0.0454 _refine_ls_wR_factor_all 0.0559 _refine_ls_wR_factor_gt 0.0536 _refine_ls_wR_factor_ref 0.0536 _refine_ls_goodness_of_fit_ref 1.771 _refine_ls_shift/su_max 0.0000 _refine_diff_density_min -0.33 _refine_diff_density_max 0.28 #------------------------------------------------------------------------------ # COMPUTATION AND REFINEMENT PROGRAMS _computing_data_collection 'Bruker SMART v5.052d' _computing_cell_refinement 'Bruker SAINT v5.04' _computing_data_reduction 'Bruker SAINT v5.04' _computing_structure_solution SIR92 _computing_structure_refinement 'teXsan' _computing_publication_material 'teXsan' _computing_molecular_graphics ? loop_ _atom_type_symbol _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C 0 48 0.003 0.002 'International Tables' H 0 116 0.000 0.000 'International Tables' N 0 12 0.006 0.003 'International Tables' Li 0 4 0.000 0.000 'International Tables' Al 0 4 0.064 0.051 'International Tables' loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_calc_flag _atom_site_calc_attached_atom Al(1) 0.5296(1) 0.15437(5) 0.44692(6) 0.029 Uij ? ? N(1) 0.5125(2) 0.1789(1) 0.5842(2) 0.022 Uij ? ? N(2) 0.6056(2) 0.0656(1) 0.7846(2) 0.019 Uij ? ? N(3) 0.2978(2) 0.1435(1) 0.7085(2) 0.022 Uij ? ? C(1) 0.6536(3) 0.2029(2) 0.6670(2) 0.025 Uij ? ? C(2) 0.7186(3) 0.1162(2) 0.7408(2) 0.025 Uij ? ? C(3) 0.5435(3) 0.1320(2) 0.8530(2) 0.022 Uij ? ? C(4) 0.3717(3) 0.1286(2) 0.8241(2) 0.025 Uij ? ? C(5) 0.3282(3) 0.2465(2) 0.6780(2) 0.027 Uij ? ? C(6) 0.3894(3) 0.2504(2) 0.5815(2) 0.028 Uij ? ? C(7) 0.6693(3) -0.0291(2) 0.8387(2) 0.018 Uij ? ? C(8) 0.8025(3) -0.0172(2) 0.9376(2) 0.032 Uij ? ? C(9) 0.5448(3) -0.0919(2) 0.8625(2) 0.026 Uij ? ? C(10) 0.1323(3) 0.1207(2) 0.6797(2) 0.027 Uij ? ? C(11) 0.1038(3) 0.0140(2) 0.7097(2) 0.034 Uij ? ? C(12) 0.0612(3) 0.1344(2) 0.5609(2) 0.035 Uij ? ? Li(1) 0.4342(4) 0.0555(3) 0.6407(3) 0.020 Uij ? ? H(1) 0.627(3) 0.058(2) 0.449(2) 0.036(7) Uij ? ? H(2) 0.613(3) 0.245(2) 0.411(2) 0.055(9) Uij ? ? H(3) 0.362(3) 0.140(2) 0.376(2) 0.054(9) Uij ? ? H(4) 0.727 0.224 0.634 0.030 Uij ? ? H(5) 0.632 0.255 0.709 0.030 Uij ? ? H(6) 0.757 0.068 0.701 0.030 Uij ? ? H(7) 0.798 0.140 0.798 0.030 Uij ? ? H(8) 0.575 0.197 0.845 0.027 Uij ? ? H(9) 0.583 0.111 0.925 0.027 Uij ? ? H(10) 0.340 0.066 0.844 0.030 Uij ? ? H(11) 0.338 0.180 0.861 0.030 Uij ? ? H(12) 0.401 0.277 0.738 0.033 Uij ? ? H(13) 0.237 0.284 0.664 0.033 Uij ? ? H(14) 0.309 0.237 0.520 0.034 Uij ? ? H(15) 0.427 0.316 0.576 0.034 Uij ? ? H(16) 0.706 -0.066 0.789 0.022 Uij ? ? H(17) 0.882 0.020 0.921 0.039 Uij ? ? H(18) 0.840 -0.081 0.964 0.039 Uij ? ? H(19) 0.771 0.018 0.991 0.039 Uij ? ? H(20) 0.580 -0.156 0.886 0.031 Uij ? ? H(21) 0.510 -0.059 0.918 0.031 Uij ? ? H(22) 0.460 -0.096 0.801 0.031 Uij ? ? H(23) 0.084 0.163 0.716 0.032 Uij ? ? H(24) 0.170 -0.031 0.688 0.040 Uij ? ? H(25) 0.125 0.008 0.786 0.040 Uij ? ? H(26) 0.002 -0.005 0.678 0.040 Uij ? ? H(27) 0.114 0.093 0.522 0.042 Uij ? ? H(28) 0.070 0.201 0.543 0.042 Uij ? ? H(29) -0.042 0.115 0.542 0.042 Uij ? ? loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Al(1) 0.0488(5) 0.0214(4) 0.0248(4) -0.0022(4) 0.0153(4) 0.0001(3) N(1) 0.028(1) 0.016(1) 0.024(1) 0.0003(8) 0.0061(9) 0.0006(8) N(2) 0.020(1) 0.016(1) 0.023(1) 0.0005(8) 0.0069(8) 0.0004(8) N(3) 0.022(1) 0.022(1) 0.025(1) 0.0042(8) 0.0062(9) 0.0003(9) C(1) 0.032(1) 0.021(1) 0.031(1) -0.006(1) 0.012(1) 0.000(1) C(2) 0.021(1) 0.026(1) 0.031(1) -0.004(1) 0.008(1) 0.000(1) C(3) 0.034(1) 0.020(1) 0.020(1) 0.002(1) 0.006(1) -0.001(1) C(4) 0.032(1) 0.026(1) 0.027(1) 0.004(1) 0.013(1) -0.003(1) C(5) 0.030(1) 0.020(1) 0.034(2) 0.007(1) 0.007(1) 0.000(1) C(6) 0.037(1) 0.017(1) 0.029(1) 0.005(1) 0.006(1) 0.004(1) C(7) 0.024(1) 0.018(1) 0.026(1) 0.001(1) 0.004(1) 0.000(1) C(8) 0.033(2) 0.028(1) 0.036(2) 0.004(1) -0.002(1) 0.004(1) C(9) 0.032(1) 0.019(1) 0.034(1) 0.001(1) 0.010(1) 0.004(1) C(10) 0.022(1) 0.032(1) 0.033(1) 0.008(1) 0.009(1) -0.003(1) C(11) 0.026(1) 0.040(2) 0.044(2) -0.003(1) 0.011(1) 0.003(1) C(12) 0.028(1) 0.037(2) 0.042(2) 0.005(1) 0.003(1) -0.001(1) Li(1) 0.027(2) 0.016(2) 0.026(2) 0.000(2) 0.008(2) 0.001(2) _geom_special_details ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Al(1) N(1) 1.877(2) ? ? yes N(1) C(1) 1.474(3) ? ? yes N(1) C(6) 1.478(3) ? ? yes N(1) Li(1) 2.028(4) ? ? yes N(2) C(2) 1.485(3) ? ? yes N(2) C(3) 1.486(3) ? ? yes N(2) C(7) 1.493(3) ? ? yes N(2) Li(1) 2.095(4) ? ? yes N(3) C(4) 1.488(3) ? ? yes N(3) C(5) 1.487(3) ? ? yes N(3) C(10) 1.493(3) ? ? yes N(3) Li(1) 2.094(4) ? ? yes C(1) C(2) 1.524(4) ? ? yes C(3) C(4) 1.519(4) ? ? yes C(5) C(6) 1.522(4) ? ? yes C(7) C(8) 1.521(4) ? ? yes C(7) C(9) 1.523(4) ? ? yes C(10) C(11) 1.527(4) ? ? yes C(10) C(12) 1.520(4) ? ? yes 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Al(1) N(1) C(1) 116.7(2) ? ? ? yes Al(1) N(1) C(6) 111.1(1) ? ? ? yes Al(1) N(1) Li(1) 109.9(1) ? ? ? yes C(1) N(1) C(6) 112.7(2) ? ? ? yes C(1) N(1) Li(1) 103.8(2) ? ? ? yes C(6) N(1) Li(1) 101.1(2) ? ? ? yes C(2) N(2) C(3) 112.7(2) ? ? ? yes C(2) N(2) C(7) 110.5(2) ? ? ? yes C(2) N(2) Li(1) 96.5(2) ? ? ? yes C(3) N(2) C(7) 113.1(2) ? ? ? yes C(3) N(2) Li(1) 105.1(2) ? ? ? yes C(7) N(2) Li(1) 117.9(2) ? ? ? yes C(4) N(3) C(5) 109.3(2) ? ? ? yes C(4) N(3) C(10) 111.8(2) ? ? ? yes C(4) N(3) Li(1) 101.4(2) ? ? ? yes C(5) N(3) C(10) 112.2(2) ? ? ? yes C(5) N(3) Li(1) 103.4(2) ? ? ? yes C(10) N(3) Li(1) 117.8(2) ? ? ? yes N(1) C(1) C(2) 114.1(2) ? ? ? yes N(2) C(2) C(1) 113.7(2) ? ? ? yes N(2) C(3) C(4) 112.3(2) ? ? ? yes N(3) C(4) C(3) 113.3(2) ? ? ? yes N(3) C(5) C(6) 113.4(2) ? ? ? yes N(1) C(6) C(5) 114.6(2) ? ? ? yes N(2) C(7) C(8) 115.4(2) ? ? ? yes N(2) C(7) C(9) 110.6(2) ? ? ? yes C(8) C(7) C(9) 110.9(2) ? ? ? yes N(3) C(10) C(11) 111.3(2) ? ? ? yes N(3) C(10) C(12) 110.4(2) ? ? ? yes C(11) C(10) C(12) 108.7(2) ? ? ? yes N(1) Li(1) N(2) 91.2(2) ? ? ? yes N(1) Li(1) N(3) 90.5(2) ? ? ? yes N(2) Li(1) N(3) 88.4(2) ? ? ? yes #===END data_(iPr2-tacn)LiAl(CCPh)3_2 _database_code_CSD 173851 #------------------------------------------------------------------------------ _audit_creation_date 'Tue Oct 23 11:18:38 2001' _audit_creation_method 'by teXsan' _audit_update_record ? #------------------------------------------------------------------------------ _cell_length_a 8.3268(4) _cell_length_b 18.0244(9) _cell_length_c 22.140(1) _cell_angle_alpha 90 _cell_angle_beta 99.666(1) _cell_angle_gamma 90 _cell_volume 3275.7(2) _cell_formula_units_Z 4 _cell_measurement_temperature 130.2 _cell_measurement_reflns_used 5672 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 45.0 #------------------------------------------------------------------------------ _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c ' _symmetry_Int_Tables_number 14 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' ' -x,1/2+y,1/2-z' ' -x, -y, -z' ' +x,1/2-y,1/2+z' #------------------------------------------------------------------------------ _exptl_crystal_description 'block' _exptl_crystal_colour 'colorless' _exptl_crystal_size_max 0.340 _exptl_crystal_size_mid 0.220 _exptl_crystal_size_min 0.180 _exptl_crystal_density_diffrn 1.114 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _chemical_formula_weight 549.66 _chemical_formula_analytical ? _chemical_formula_sum 'C36 H41 Al Li N3 ' _chemical_formula_moiety 'C36 H41 Al Li N3 ' _chemical_formula_structural ? _chemical_compound_source ? _exptl_crystal_F_000 1176.00 _exptl_absorpt_coefficient_mu 0.089 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details 'Blessing, 1995' _exptl_absorpt_correction_T_max 0.98 _exptl_absorpt_correction_T_min 0.55 #------------------------------------------------------------------------------ _diffrn_special_details none _diffrn_ambient_temperature 130.2 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'X-ray tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'SMART CCD' _diffrn_measurement_method \w-scan _diffrn_reflns_number 14627 _reflns_number_total 5617 _reflns_number_gt 3478 _reflns_threshold_expression 'I>3.00sigma' _diffrn_reflns_av_R_equivalents 0.0479 _diffrn_reflns_av_sigmaI/netI ? _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.5 _diffrn_reflns_theta_max 24.71 _diffrn_reflns_reduction_process ? #------------------------------------------------------------------------------ _refine_special_details ? _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme sigma _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef 0.00000 _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 3478 _refine_ls_number_parameters 370 _refine_ls_number_restraints 0 _refine_ls_number_constraints ? _refine_ls_R_factor_all 0.0672 _refine_ls_R_factor_gt 0.0430 _refine_ls_wR_factor_all 0.0534 _refine_ls_wR_factor_gt 0.0489 _refine_ls_wR_factor_ref 0.0489 _refine_ls_goodness_of_fit_ref 1.410 _refine_ls_shift/su_max 0.0000 _refine_diff_density_min -0.36 _refine_diff_density_max 0.27 #------------------------------------------------------------------------------ # COMPUTATION AND REFINEMENT PROGRAMS _computing_data_collection 'Bruker SMART v5.052d' _computing_cell_refinement 'Bruker SAINT v5.04' _computing_data_reduction 'Bruker SAINT v5.04' _computing_structure_solution SIR92 _computing_structure_refinement 'teXsan' _computing_publication_material 'teXsan' _computing_molecular_graphics ? loop_ _atom_type_symbol _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C 0 144 0.003 0.002 'International Tables' H 0 164 0.000 0.000 'International Tables' N 0 12 0.006 0.003 'International Tables' Al 0 4 0.064 0.051 'International Tables' Li 0 4 0.000 0.000 'International Tables' loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_calc_flag _atom_site_calc_attached_atom Al(1) -0.06297(9) -0.10765(4) 0.25182(4) 0.023 Uij ? ? N(1) -0.2670(2) -0.0990(1) 0.27290(9) 0.020 Uij ? ? N(2) -0.5073(2) -0.0548(1) 0.16856(9) 0.020 Uij ? ? N(3) -0.4434(2) 0.0429(1) 0.27401(9) 0.020 Uij ? ? C(1) -0.0473(3) -0.0149(1) 0.2051(1) 0.030 Uij ? ? C(2) -0.0346(3) 0.0408(1) 0.1756(1) 0.025 Uij ? ? C(3) 0.0016(3) 0.1041(1) 0.1396(1) 0.026 Uij ? ? C(4) -0.0078(3) 0.0976(1) 0.0769(1) 0.034 Uij ? ? C(5) 0.0355(4) 0.1563(2) 0.0425(1) 0.047 Uij ? ? C(6) 0.0897(4) 0.2224(2) 0.0716(1) 0.042 Uij ? ? C(7) 0.0989(3) 0.2292(1) 0.1338(1) 0.035 Uij ? ? C(8) 0.0545(3) 0.1710(1) 0.1681(1) 0.031 Uij ? ? C(9) -0.0553(3) -0.1925(1) 0.1979(1) 0.032 Uij ? ? C(10) -0.0357(3) -0.2440(1) 0.1647(1) 0.028 Uij ? ? C(11) -0.0031(3) -0.3040(1) 0.1259(1) 0.026 Uij ? ? C(12) -0.0658(3) -0.3753(1) 0.1309(1) 0.029 Uij ? ? C(13) -0.0286(4) -0.4320(1) 0.0934(1) 0.036 Uij ? ? C(14) 0.0707(4) -0.4188(2) 0.0510(1) 0.039 Uij ? ? C(15) 0.1327(4) -0.3489(2) 0.0452(1) 0.042 Uij ? ? C(16) 0.0956(3) -0.2922(1) 0.0821(1) 0.031 Uij ? ? C(17) 0.1154(3) -0.1142(1) 0.3210(1) 0.027 Uij ? ? C(18) 0.2225(3) -0.1307(1) 0.3626(1) 0.027 Uij ? ? C(19) 0.3483(3) -0.1540(1) 0.4121(1) 0.027 Uij ? ? C(20) 0.3765(4) -0.2295(2) 0.4237(1) 0.042 Uij ? ? C(21) 0.4952(4) -0.2513(2) 0.4718(1) 0.051 Uij ? ? C(22) 0.5869(4) -0.2002(2) 0.5086(1) 0.043 Uij ? ? C(23) 0.5608(4) -0.1255(2) 0.4975(1) 0.043 Uij ? ? C(24) 0.4412(3) -0.1026(2) 0.4498(1) 0.038 Uij ? ? C(25) -0.4020(3) -0.1493(1) 0.2492(1) 0.027 Uij ? ? C(26) -0.4714(3) -0.1348(1) 0.1820(1) 0.027 Uij ? ? C(27) -0.6432(3) -0.0285(1) 0.1985(1) 0.024 Uij ? ? C(28) -0.6057(3) 0.0437(1) 0.2352(1) 0.021 Uij ? ? C(29) -0.4352(3) -0.0109(1) 0.3256(1) 0.025 Uij ? ? C(30) -0.2857(3) -0.0620(1) 0.3306(1) 0.025 Uij ? ? C(31) -0.5317(3) -0.0408(1) 0.1019(1) 0.032 Uij ? ? C(32) -0.6779(4) -0.0807(2) 0.0647(1) 0.044 Uij ? ? C(33) -0.5414(4) 0.0427(2) 0.0885(1) 0.038 Uij ? ? C(34) -0.3874(3) 0.1182(1) 0.2969(1) 0.022 Uij ? ? C(35) -0.3418(3) 0.1656(1) 0.2456(1) 0.032 Uij ? ? C(36) -0.5084(3) 0.1584(1) 0.3303(1) 0.028 Uij ? ? Li(1) -0.3070(5) -0.0054(2) 0.2172(2) 0.025 Uij ? ? H(1) -0.044 0.052 0.057 0.041 Uij ? ? H(2) 0.030 0.152 -0.001 0.057 Uij ? ? H(3) 0.119 0.263 0.048 0.051 Uij ? ? H(4) 0.136 0.275 0.154 0.041 Uij ? ? H(5) 0.061 0.177 0.211 0.037 Uij ? ? H(6) -0.133 -0.385 0.160 0.035 Uij ? ? H(7) -0.072 -0.480 0.097 0.044 Uij ? ? H(8) 0.096 -0.459 0.027 0.047 Uij ? ? H(9) 0.202 -0.341 0.016 0.051 Uij ? ? H(10) 0.138 -0.244 0.077 0.037 Uij ? ? H(11) 0.314 -0.266 0.399 0.051 Uij ? ? H(12) 0.516 -0.303 0.479 0.061 Uij ? ? H(13) 0.666 -0.217 0.542 0.052 Uij ? ? H(14) 0.625 -0.090 0.523 0.051 Uij ? ? H(15) 0.422 -0.051 0.442 0.045 Uij ? ? H(16) -0.362 -0.199 0.254 0.032 Uij ? ? H(17) -0.485 -0.143 0.273 0.032 Uij ? ? H(18) -0.569 -0.163 0.171 0.033 Uij ? ? H(19) -0.394 -0.151 0.157 0.033 Uij ? ? H(20) -0.736 -0.020 0.167 0.029 Uij ? ? H(21) -0.668 -0.066 0.225 0.029 Uij ? ? H(22) -0.686 0.051 0.260 0.025 Uij ? ? H(23) -0.610 0.084 0.207 0.025 Uij ? ? H(24) -0.429 0.016 0.363 0.031 Uij ? ? H(25) -0.531 -0.040 0.320 0.031 Uij ? ? H(26) -0.295 -0.099 0.360 0.030 Uij ? ? H(27) -0.191 -0.033 0.344 0.030 Uij ? ? H(28) -0.436 -0.059 0.088 0.039 Uij ? ? H(29) -0.669 -0.133 0.071 0.052 Uij ? ? H(30) -0.776 -0.064 0.076 0.052 Uij ? ? H(31) -0.683 -0.071 0.022 0.052 Uij ? ? H(32) -0.447 0.068 0.110 0.046 Uij ? ? H(33) -0.551 0.053 0.046 0.046 Uij ? ? H(34) -0.635 0.064 0.103 0.046 Uij ? ? H(35) -0.290 0.111 0.327 0.026 Uij ? ? H(36) -0.268 0.139 0.224 0.038 Uij ? ? H(37) -0.438 0.177 0.217 0.038 Uij ? ? H(38) -0.292 0.211 0.261 0.038 Uij ? ? H(39) -0.538 0.128 0.362 0.034 Uij ? ? H(40) -0.605 0.170 0.302 0.034 Uij ? ? H(41) -0.462 0.203 0.348 0.034 Uij ? ? loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Al(1) 0.0202(4) 0.0209(4) 0.0311(5) 0.0044(3) 0.0044(3) 0.0009(4) N(1) 0.020(1) 0.017(1) 0.027(1) -0.0015(9) 0.0038(9) -0.0031(9) N(2) 0.019(1) 0.021(1) 0.026(1) 0.0011(9) 0.0033(9) -0.0014(9) N(3) 0.018(1) 0.016(1) 0.026(1) 0.0013(9) 0.0033(9) 0.0015(9) C(1) 0.017(1) 0.029(2) 0.038(2) 0.004(1) 0.008(1) 0.002(1) C(2) 0.016(1) 0.029(2) 0.032(2) 0.003(1) 0.004(1) -0.003(1) C(3) 0.017(1) 0.025(1) 0.032(2) 0.004(1) 0.003(1) 0.006(1) C(4) 0.035(2) 0.031(2) 0.035(2) -0.001(1) -0.002(1) 0.003(1) C(5) 0.049(2) 0.046(2) 0.033(2) -0.001(2) 0.004(1) 0.012(2) C(6) 0.035(2) 0.038(2) 0.051(2) 0.001(1) 0.008(2) 0.019(2) C(7) 0.030(2) 0.026(2) 0.053(2) 0.001(1) 0.006(1) 0.003(1) C(8) 0.028(2) 0.028(1) 0.035(2) 0.000(1) 0.004(1) 0.000(1) C(9) 0.025(2) 0.032(2) 0.035(2) 0.012(1) 0.001(1) 0.000(1) C(10) 0.025(2) 0.031(2) 0.033(2) 0.009(1) 0.001(1) 0.001(1) C(11) 0.023(1) 0.027(1) 0.024(2) 0.008(1) 0.000(1) 0.000(1) C(12) 0.021(1) 0.034(2) 0.037(2) 0.003(1) 0.001(1) 0.006(1) C(13) 0.032(2) 0.023(2) 0.055(2) 0.002(1) -0.010(2) -0.005(1) C(14) 0.044(2) 0.039(2) 0.041(2) 0.012(1) -0.004(2) -0.017(1) C(15) 0.047(2) 0.052(2) 0.028(2) 0.012(2) 0.010(1) 0.000(1) C(16) 0.036(2) 0.028(2) 0.034(2) 0.004(1) 0.006(1) 0.007(1) C(17) 0.024(1) 0.025(1) 0.035(2) 0.000(1) 0.008(1) 0.000(1) C(18) 0.024(1) 0.028(2) 0.036(2) -0.002(1) 0.010(1) -0.003(1) C(19) 0.021(1) 0.038(2) 0.024(1) -0.001(1) 0.007(1) 0.000(1) C(20) 0.038(2) 0.040(2) 0.034(2) 0.006(1) -0.004(1) -0.008(1) C(21) 0.055(2) 0.047(2) 0.046(2) 0.020(2) -0.005(2) -0.002(2) C(22) 0.036(2) 0.071(2) 0.028(2) 0.017(2) -0.003(1) -0.002(2) C(23) 0.035(2) 0.062(2) 0.028(2) -0.012(2) 0.005(1) -0.008(2) C(24) 0.034(2) 0.040(2) 0.030(2) -0.008(1) 0.010(1) 0.004(1) C(25) 0.022(1) 0.017(1) 0.038(2) -0.002(1) 0.007(1) -0.003(1) C(26) 0.023(1) 0.021(1) 0.036(2) -0.002(1) 0.004(1) -0.008(1) C(27) 0.017(1) 0.026(1) 0.028(2) 0.000(1) 0.002(1) -0.001(1) C(28) 0.018(1) 0.022(1) 0.032(2) 0.003(1) 0.007(1) -0.002(1) C(29) 0.024(1) 0.019(1) 0.028(1) -0.001(1) 0.009(1) -0.002(1) C(30) 0.025(1) 0.019(1) 0.026(1) 0.001(1) 0.003(1) 0.004(1) C(31) 0.027(2) 0.037(2) 0.030(2) 0.001(1) 0.006(1) -0.005(1) C(32) 0.037(2) 0.057(2) 0.033(2) -0.001(1) -0.004(1) -0.008(1) C(33) 0.044(2) 0.043(2) 0.031(2) 0.003(1) 0.003(1) 0.005(1) C(34) 0.021(1) 0.014(1) 0.032(2) -0.001(1) 0.004(1) -0.003(1) C(35) 0.031(2) 0.020(1) 0.039(2) -0.002(1) 0.009(1) -0.001(1) C(36) 0.033(2) 0.022(1) 0.035(2) 0.002(1) 0.008(1) -0.001(1) Li(1) 0.021(2) 0.019(2) 0.032(2) 0.001(2) 0.004(2) 0.000(2) _geom_special_details ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Al(1) N(1) 1.843(2) ? ? yes Al(1) C(1) 1.981(3) ? ? yes Al(1) C(9) 1.948(3) ? ? yes Al(1) C(17) 1.950(3) ? ? yes N(1) C(25) 1.472(3) ? ? yes N(1) C(30) 1.472(3) ? ? yes N(1) Li(1) 2.083(4) ? ? yes N(2) C(26) 1.493(3) ? ? yes N(2) C(27) 1.481(3) ? ? yes N(2) C(31) 1.477(3) ? ? yes N(2) Li(1) 2.032(4) ? ? yes N(3) C(28) 1.475(3) ? ? yes N(3) C(29) 1.492(3) ? ? yes N(3) C(34) 1.496(3) ? ? yes N(3) Li(1) 2.027(5) ? ? yes C(1) C(2) 1.212(3) ? ? yes C(1) Li(1) 2.230(5) ? ? yes C(2) C(3) 1.453(4) ? ? yes C(3) C(4) 1.383(4) ? ? yes C(3) C(8) 1.397(3) ? ? yes C(4) C(5) 1.385(4) ? ? yes C(5) C(6) 1.392(4) ? ? yes C(6) C(7) 1.372(4) ? ? yes C(7) C(8) 1.382(4) ? ? yes C(9) C(10) 1.212(3) ? ? yes C(10) C(11) 1.435(4) ? ? yes C(11) C(12) 1.398(3) ? ? yes C(11) C(16) 1.388(4) ? ? yes C(12) C(13) 1.385(4) ? ? yes C(13) C(14) 1.372(4) ? ? yes C(14) C(15) 1.375(4) ? ? yes C(15) C(16) 1.377(4) ? ? yes C(17) C(18) 1.207(4) ? ? yes C(18) C(19) 1.446(4) ? ? yes C(19) C(20) 1.396(4) ? ? yes C(19) C(24) 1.391(4) ? ? yes C(20) C(21) 1.383(4) ? ? yes C(21) C(22) 1.374(4) ? ? yes C(22) C(23) 1.381(4) ? ? yes C(23) C(24) 1.387(4) ? ? yes C(25) C(26) 1.526(4) ? ? yes C(27) C(28) 1.537(3) ? ? yes C(29) C(30) 1.537(3) ? ? yes C(31) C(32) 1.531(4) ? ? yes C(31) C(33) 1.533(4) ? ? yes C(34) C(35) 1.519(4) ? ? yes C(34) C(36) 1.529(4) ? ? yes 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N(1) Al(1) C(1) 101.8(1) ? ? ? yes N(1) Al(1) C(9) 110.4(1) ? ? ? yes N(1) Al(1) C(17) 114.8(1) ? ? ? yes C(1) Al(1) C(9) 109.3(1) ? ? ? yes C(1) Al(1) C(17) 110.7(1) ? ? ? yes C(9) Al(1) C(17) 109.6(1) ? ? ? yes Al(1) N(1) C(25) 122.6(2) ? ? ? yes Al(1) N(1) C(30) 119.6(2) ? ? ? yes Al(1) N(1) Li(1) 88.9(1) ? ? ? yes C(25) N(1) C(30) 113.8(2) ? ? ? yes C(25) N(1) Li(1) 104.6(2) ? ? ? yes C(30) N(1) Li(1) 96.8(2) ? ? ? yes C(26) N(2) C(27) 111.3(2) ? ? ? yes C(26) N(2) C(31) 110.7(2) ? ? ? yes C(26) N(2) Li(1) 101.4(2) ? ? ? yes C(27) N(2) C(31) 113.9(2) ? ? ? yes C(27) N(2) Li(1) 104.1(2) ? ? ? yes C(31) N(2) Li(1) 114.6(2) ? ? ? yes C(28) N(3) C(29) 111.9(2) ? ? ? yes C(28) N(3) C(34) 113.0(2) ? ? ? yes C(28) N(3) Li(1) 101.3(2) ? ? ? yes C(29) N(3) C(34) 111.0(2) ? ? ? yes C(29) N(3) Li(1) 103.8(2) ? ? ? yes C(34) N(3) Li(1) 115.1(2) ? ? ? yes Al(1) C(1) C(2) 178.1(2) ? ? ? yes Al(1) C(1) Li(1) 81.5(1) ? ? ? yes C(2) C(1) Li(1) 100.1(2) ? ? ? yes C(1) C(2) C(3) 172.6(3) ? ? ? yes C(2) C(3) C(4) 120.1(2) ? ? ? yes C(2) C(3) C(8) 120.6(2) ? ? ? yes C(4) C(3) C(8) 119.1(2) ? ? ? yes C(3) C(4) C(5) 120.7(2) ? ? ? yes C(4) C(5) C(6) 119.6(3) ? ? ? yes C(5) C(6) C(7) 120.0(3) ? ? ? yes C(6) C(7) C(8) 120.6(3) ? ? ? yes C(3) C(8) C(7) 120.0(3) ? ? ? yes Al(1) C(9) C(10) 174.1(2) ? ? ? yes C(9) C(10) C(11) 176.9(3) ? ? ? yes C(10) C(11) C(12) 122.3(2) ? ? ? yes C(10) C(11) C(16) 119.7(2) ? ? ? yes C(12) C(11) C(16) 118.0(2) ? ? ? yes C(11) C(12) C(13) 120.4(3) ? ? ? yes C(12) C(13) C(14) 120.2(3) ? ? ? yes C(13) C(14) C(15) 120.2(3) ? ? ? yes C(14) C(15) C(16) 120.0(3) ? ? ? yes C(11) C(16) C(15) 121.3(3) ? ? ? yes Al(1) C(17) C(18) 169.2(2) ? ? ? yes C(17) C(18) C(19) 177.3(3) ? ? ? yes C(18) C(19) C(20) 120.0(2) ? ? ? yes C(18) C(19) C(24) 121.3(2) ? ? ? yes C(20) C(19) C(24) 118.6(3) ? ? ? yes C(19) C(20) C(21) 119.7(3) ? ? ? yes C(20) C(21) C(22) 121.3(3) ? ? ? yes C(21) C(22) C(23) 119.6(3) ? ? ? yes C(22) C(23) C(24) 119.8(3) ? ? ? yes C(19) C(24) C(23) 121.0(3) ? ? ? yes N(1) C(25) C(26) 112.6(2) ? ? ? yes N(2) C(26) C(25) 113.0(2) ? ? ? yes N(2) C(27) C(28) 113.9(2) ? ? ? yes N(3) C(28) C(27) 112.6(2) ? ? ? yes N(3) C(29) C(30) 112.1(2) ? ? ? yes N(1) C(30) C(29) 114.3(2) ? ? ? yes N(2) C(31) C(32) 114.9(2) ? ? ? yes N(2) C(31) C(33) 110.8(2) ? ? ? yes C(32) C(31) C(33) 110.2(2) ? ? ? yes N(3) C(34) C(35) 111.1(2) ? ? ? yes N(3) C(34) C(36) 113.6(2) ? ? ? yes C(35) C(34) C(36) 111.2(2) ? ? ? yes N(1) Li(1) N(2) 89.7(2) ? ? ? yes N(1) Li(1) N(3) 91.7(2) ? ? ? yes N(1) Li(1) C(1) 86.9(2) ? ? ? yes N(2) Li(1) N(3) 91.2(2) ? ? ? yes N(2) Li(1) C(1) 129.0(2) ? ? ? yes N(3) Li(1) C(1) 139.7(2) ? ? ? yes #===END