# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_name_full Chem.Commun. _journal_coden_cambridge 0182 _publ_section_title ;Base free lithium-organoaluminate and the gallium congener: potencial precursors to heterometallic assemblies ; loop_ _publ_author_name _publ_author_address S.Singh ;Institute of Inorganic Chemistry Georg-August-University of G\"ottingen Tammannstr. 4 D-37077 G\"ottingen Germany ; 'Jianfang Chai.' ;Institute of Inorganic Chemistry Georg-August-University of G\"ottingen Tammannstr. 4 D-37077 G\"ottingen Germany ; A.Pal ;Institute of Inorganic Chemistry Georg-August-University of G\"ottingen Tammannstr. 4 D-37077 G\"ottingen Germany ; V.Jancik ;Institute of Inorganic Chemistry Georg-August-University of G\"ottingen Tammannstr. 4 D-37077 G\"ottingen Germany ; H.W.Roesky ;Institute of Inorganic Chemistry Georg-August-University of G\"ottingen Tammannstr. 4 D-37077 G\"ottingen Germany ; R.Herbst-Irmer ;Institute of Inorganic Chemistry Georg-August-University of G\"ottingen Tammannstr. 4 D-37077 G\"ottingen Germany ; _publ_contact_author_address ;Institute of Inorganic Chemistry Georg-August-University of G\"ottingen Tammannstr. 4 D-37077 G\"ottingen Germany ; _publ_contact_author_email rherbst@shelx.uni-ac.gwdg.de _publ_contact_author_fax +49-551-392582 _publ_contact_author_phone +49-551-393007 _publ_contact_author_name 'Prof. H.Roesky' # Attachment 'new cif files for 3 nad 4.txt' data_final _database_code_depnum_ccdc_archive 'CCDC 654337' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C96 H146 Al3 Li3 N6 O3' _chemical_formula_weight 1533.95 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0008 0.0003 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Al Al 0.2130 0.2455 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Hexagonal _symmetry_space_group_name_H-M P6(3) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' '-x, -y, z+1/2' 'y, -x+y, z+1/2' 'x-y, x, z+1/2' _cell_length_a 15.847(2) _cell_length_b 15.847(2) _cell_length_c 21.396(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 4653.3(12) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9880 _cell_measurement_theta_min 3.83 _cell_measurement_theta_max 58.89 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.095 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1672 _exptl_absorpt_coefficient_mu 0.746 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8355 _exptl_absorpt_correction_T_max 0.9291 _exptl_absorpt_process_details 'Sadabs, Sheldrick 2007' _exptl_special_details ; The intensities were measured with Smart6000 CCD area detector ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator 'mirror system' _diffrn_measurement_device_type 'Bruker three circle diffractometer' _diffrn_measurement_method 'phi and omega scan' _diffrn_detector_area_resol_mean 5.602 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 26482 _diffrn_reflns_av_R_equivalents 0.0275 _diffrn_reflns_av_sigmaI/netI 0.0202 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 3.22 _diffrn_reflns_theta_max 58.93 _reflns_number_total 4395 _reflns_number_gt 4290 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Proteum (Version 1.40, Bruker 2002)' _computing_cell_refinement 'Bruker SAINT (V. 7.12A, Siemens 2003)' _computing_data_reduction 'Bruker SAINT (V. 7.12A, Siemens 2003)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker AXS SHELXTL (V. 6.12)' _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. The hexane molecule was disordered along the 3-fold axis. Distance restraints and restraints for the anisotropic displacment parameters were used to refine it. The found position of the hydrogen atom bond to C3 deviates from its calculated position. Therefore it was refined with a distance restraint. ; _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^)+(0.0426P)^2^+0.4959P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.02(2) _refine_ls_number_reflns 4395 _refine_ls_number_parameters 440 _refine_ls_number_restraints 219 _refine_ls_R_factor_all 0.0258 _refine_ls_R_factor_gt 0.0249 _refine_ls_wR_factor_ref 0.0667 _refine_ls_wR_factor_gt 0.0661 _refine_ls_goodness_of_fit_ref 1.069 _refine_ls_restrained_S_all 1.071 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Al1 Al 0.91348(3) 0.37014(3) 0.19556(2) 0.02569(11) Uani 1 1 d . . . O1 O 0.79644(7) 0.34568(7) 0.20067(5) 0.0297(2) Uani 1 1 d . . . Li1 Li 0.67714(18) 0.24018(18) 0.20105(15) 0.0383(6) Uani 1 1 d . . . N1 N 0.92119(9) 0.26453(9) 0.15392(6) 0.0273(3) Uani 1 1 d . . . N2 N 0.96060(8) 0.35019(9) 0.27451(6) 0.0276(3) Uani 1 1 d . . . C1 C 0.89029(14) 0.09519(12) 0.15469(8) 0.0392(4) Uani 1 1 d . . . H1A H 0.8980 0.1064 0.1095 0.059 Uiso 0.50 1 calc PR . . H1B H 0.8256 0.0395 0.1635 0.059 Uiso 0.50 1 calc PR . . H1C H 0.9404 0.0814 0.1702 0.059 Uiso 0.50 1 calc PR . . H1D H 0.8780 0.0452 0.1860 0.059 Uiso 0.50 1 calc PR . . H1E H 0.9504 0.1120 0.1319 0.059 Uiso 0.50 1 calc PR . . H1F H 0.8356 0.0702 0.1253 0.059 Uiso 0.50 1 calc PR . . C2 C 0.90097(10) 0.18503(10) 0.18690(7) 0.0298(3) Uani 1 1 d . . . C3 C 0.89182(11) 0.18008(11) 0.25217(7) 0.0320(3) Uani 1 1 d D . . H3 H 0.8710(12) 0.1193(11) 0.2710(8) 0.036(4) Uiso 1 1 d D . . C4 C 0.92735(11) 0.25868(11) 0.29352(7) 0.0298(3) Uani 1 1 d . . . C5 C 0.92909(12) 0.23705(12) 0.36258(8) 0.0383(4) Uani 1 1 d . . . H5A H 0.8923 0.2610 0.3862 0.057 Uiso 1 1 calc R . . H5B H 0.9967 0.2696 0.3774 0.057 Uiso 1 1 calc R . . H5C H 0.8994 0.1666 0.3686 0.057 Uiso 1 1 calc R . . C6 C 1.01012(12) 0.49843(12) 0.16154(8) 0.0351(4) Uani 1 1 d . . . H6A H 0.9889 0.5457 0.1700 0.053 Uiso 1 1 calc R . . H6B H 1.0160 0.4931 0.1163 0.053 Uiso 1 1 calc R . . H6C H 1.0735 0.5202 0.1814 0.053 Uiso 1 1 calc R . . C11 C 0.93602(11) 0.26317(11) 0.08678(7) 0.0286(3) Uani 1 1 d . . . C12 C 0.85631(11) 0.21239(11) 0.04652(7) 0.0309(3) Uani 1 1 d . . . C13 C 0.87436(12) 0.21158(12) -0.01729(8) 0.0347(4) Uani 1 1 d . . . H13 H 0.8211 0.1788 -0.0453 0.042 Uiso 1 1 calc R . . C14 C 0.96845(13) 0.25758(13) -0.04053(8) 0.0386(4) Uani 1 1 d . . . H14 H 0.9795 0.2545 -0.0839 0.046 Uiso 1 1 calc R . . C15 C 1.04583(12) 0.30775(12) -0.00078(7) 0.0363(4) Uani 1 1 d . . . H15 H 1.1102 0.3396 -0.0172 0.044 Uiso 1 1 calc R . . C16 C 1.03196(12) 0.31295(11) 0.06352(7) 0.0320(4) Uani 1 1 d . . . C120 C 0.75082(11) 0.15744(11) 0.06890(7) 0.0310(3) Uani 1 1 d . . . H120 H 0.7510 0.1454 0.1148 0.037 Uiso 1 1 calc R . . C121 C 0.69234(12) 0.05852(12) 0.03627(8) 0.0382(4) Uani 1 1 d . . . H12A H 0.6799 0.0686 -0.0072 0.057 Uiso 1 1 calc R . . H12B H 0.6302 0.0194 0.0580 0.057 Uiso 1 1 calc R . . H12C H 0.7296 0.0243 0.0371 0.057 Uiso 1 1 calc R . . C122 C 0.70127(12) 0.21790(12) 0.05887(8) 0.0363(4) Uani 1 1 d . . . H12D H 0.7038 0.2340 0.0144 0.054 Uiso 1 1 calc R . . H12E H 0.7351 0.2781 0.0833 0.054 Uiso 1 1 calc R . . H12F H 0.6332 0.1804 0.0724 0.054 Uiso 1 1 calc R . . C160 C 1.12014(12) 0.36644(12) 0.10595(7) 0.0340(3) Uani 1 1 d . . . H160 H 1.1003 0.3916 0.1426 0.041 Uiso 1 1 calc R . . C161 C 1.15036(13) 0.29457(13) 0.13044(9) 0.0421(4) Uani 1 1 d . . . H16A H 1.1600 0.2609 0.0951 0.063 Uiso 1 1 calc R . . H16B H 1.0991 0.2467 0.1578 0.063 Uiso 1 1 calc R . . H16C H 1.2112 0.3301 0.1541 0.063 Uiso 1 1 calc R . . C162 C 1.20614(14) 0.45306(15) 0.07444(9) 0.0491(5) Uani 1 1 d . . . H16D H 1.1847 0.4962 0.0567 0.074 Uiso 1 1 calc R . . H16E H 1.2315 0.4297 0.0410 0.074 Uiso 1 1 calc R . . H16F H 1.2575 0.4889 0.1053 0.074 Uiso 1 1 calc R . . C21 C 1.02177(11) 0.42717(10) 0.31746(7) 0.0282(3) Uani 1 1 d . . . C22 C 0.98230(11) 0.46995(11) 0.35658(8) 0.0326(3) Uani 1 1 d . . . C23 C 1.04342(12) 0.54042(11) 0.39923(8) 0.0332(3) Uani 1 1 d . . . H23 H 1.0175 0.5698 0.4259 0.040 Uiso 1 1 calc R . . C24 C 1.14077(11) 0.56846(11) 0.40361(7) 0.0330(3) Uani 1 1 d . . . H24 H 1.1811 0.6156 0.4337 0.040 Uiso 1 1 calc R . . C25 C 1.17914(11) 0.52768(11) 0.36413(7) 0.0325(4) Uani 1 1 d . . . H25 H 1.2464 0.5479 0.3670 0.039 Uiso 1 1 calc R . . C26 C 1.12170(11) 0.45741(11) 0.31991(7) 0.0287(3) Uani 1 1 d . . . C220 C 0.87610(12) 0.44313(13) 0.35302(9) 0.0432(4) Uani 1 1 d . . . H220 H 0.8405 0.3827 0.3272 0.052 Uiso 1 1 calc R . . C221 C 0.82888(15) 0.42205(18) 0.41773(11) 0.0655(6) Uani 1 1 d . . . H22A H 0.8645 0.4795 0.4444 0.098 Uiso 1 1 calc R . . H22B H 0.8309 0.3666 0.4364 0.098 Uiso 1 1 calc R . . H22C H 0.7610 0.4065 0.4138 0.098 Uiso 1 1 calc R . . C222 C 0.86715(15) 0.52447(15) 0.32077(12) 0.0568(5) Uani 1 1 d . . . H22D H 0.8970 0.5829 0.3471 0.085 Uiso 1 1 calc R . . H22E H 0.7982 0.5033 0.3143 0.085 Uiso 1 1 calc R . . H22F H 0.9006 0.5393 0.2803 0.085 Uiso 1 1 calc R . . C260 C 1.16902(11) 0.41761(12) 0.27615(8) 0.0317(3) Uani 1 1 d . . . H260 H 1.1203 0.3783 0.2432 0.038 Uiso 1 1 calc R . . C261 C 1.25837(12) 0.50012(13) 0.24347(8) 0.0399(4) Uani 1 1 d . . . H26A H 1.3079 0.5391 0.2747 0.060 Uiso 1 1 calc R . . H26B H 1.2392 0.5417 0.2209 0.060 Uiso 1 1 calc R . . H26C H 1.2851 0.4723 0.2139 0.060 Uiso 1 1 calc R . . C262 C 1.19806(13) 0.35072(13) 0.30989(8) 0.0417(4) Uani 1 1 d . . . H26D H 1.1405 0.2970 0.3297 0.063 Uiso 1 1 calc R . . H26E H 1.2470 0.3880 0.3419 0.063 Uiso 1 1 calc R . . H26F H 1.2253 0.3243 0.2797 0.063 Uiso 1 1 calc R . . C1S C 1.011(3) -0.009(3) -0.2146(5) 0.053(4) Uani 0.244(4) 1 d PDU A -1 H1S1 H 1.0218 0.0240 -0.2550 0.079 Uiso 0.244(4) 1 calc PR A -1 H1S2 H 0.9669 -0.0792 -0.2203 0.079 Uiso 0.244(4) 1 calc PR A -1 H1S3 H 1.0733 0.0022 -0.1978 0.079 Uiso 0.244(4) 1 calc PR A -1 C2S C 0.9660(9) 0.0303(10) -0.1698(5) 0.066(3) Uani 0.244(4) 1 d PDU A -1 H2S1 H 1.0069 0.1022 -0.1683 0.079 Uiso 0.244(4) 1 calc PR A -1 H2S2 H 0.9009 0.0143 -0.1856 0.079 Uiso 0.244(4) 1 calc PR A -1 C3S C 0.9554(7) -0.0093(14) -0.1050(5) 0.080(3) Uani 0.244(4) 1 d PDU A -1 H3S1 H 0.9142 -0.0811 -0.1073 0.096 Uiso 0.244(4) 1 calc PR A -1 H3S2 H 0.9193 0.0148 -0.0799 0.096 Uiso 0.244(4) 1 calc PR A -1 C4S C 1.0470(8) 0.0138(11) -0.0697(5) 0.075(3) Uani 0.244(4) 1 d PDU A -1 H4S1 H 1.0884 0.0854 -0.0658 0.090 Uiso 0.244(4) 1 calc PR A -1 H4S2 H 1.0838 -0.0104 -0.0939 0.090 Uiso 0.244(4) 1 calc PR A -1 C5S C 1.0264(13) -0.0319(12) -0.0036(5) 0.074(2) Uani 0.244(4) 1 d PDU A -1 H5S1 H 0.9778 -0.1023 -0.0061 0.089 Uiso 0.244(4) 1 calc PR A -1 H5S2 H 1.0871 -0.0247 0.0146 0.089 Uiso 0.244(4) 1 calc PR A -1 C6S C 0.989(3) 0.018(2) 0.0362(6) 0.075(4) Uani 0.244(4) 1 d PDU A -1 H6S1 H 0.9760 -0.0093 0.0784 0.113 Uiso 0.244(4) 1 calc PR A -1 H6S2 H 0.9279 0.0099 0.0183 0.113 Uiso 0.244(4) 1 calc PR A -1 H6S3 H 1.0369 0.0881 0.0382 0.113 Uiso 0.244(4) 1 calc PR A -1 C1SA C 0.978(4) 0.023(4) -0.201(2) 0.071(7) Uani 0.090(4) 1 d PDU A -2 H1S4 H 0.9830 0.0088 -0.2445 0.106 Uiso 0.090(4) 1 calc PR A -2 H1S5 H 0.9927 0.0908 -0.1967 0.106 Uiso 0.090(4) 1 calc PR A -2 H1S6 H 0.9112 -0.0207 -0.1858 0.106 Uiso 0.090(4) 1 calc PR A -2 C2SA C 1.048(3) 0.008(3) -0.1621(13) 0.072(4) Uani 0.090(4) 1 d PDU A -2 H2S3 H 1.0299 -0.0610 -0.1678 0.087 Uiso 0.090(4) 1 calc PR A -2 H2S4 H 1.1127 0.0473 -0.1824 0.087 Uiso 0.090(4) 1 calc PR A -2 C3SA C 1.065(2) 0.028(2) -0.0942(13) 0.076(4) Uani 0.090(4) 1 d PDU A -2 H3S3 H 1.0407 0.0723 -0.0817 0.091 Uiso 0.090(4) 1 calc PR A -2 H3S4 H 1.1361 0.0624 -0.0860 0.091 Uiso 0.090(4) 1 calc PR A -2 C4SA C 1.015(2) -0.064(2) -0.0534(13) 0.075(4) Uani 0.090(4) 1 d PDU A -2 H4S3 H 0.9702 -0.1196 -0.0798 0.090 Uiso 0.090(4) 1 calc PR A -2 H4S4 H 1.0659 -0.0779 -0.0375 0.090 Uiso 0.090(4) 1 calc PR A -2 C5SA C 0.960(3) -0.057(3) 0.0015(14) 0.076(5) Uani 0.090(4) 1 d PDU A -2 H5S3 H 1.0042 -0.0256 0.0373 0.091 Uiso 0.090(4) 1 calc PR A -2 H5S4 H 0.9085 -0.1227 0.0145 0.091 Uiso 0.090(4) 1 calc PR A -2 C6SA C 0.913(2) 0.003(2) -0.0166(16) 0.078(6) Uani 0.090(4) 1 d PDU A -2 H6S4 H 0.8880 0.0192 0.0210 0.116 Uiso 0.090(4) 1 calc PR A -2 H6S5 H 0.8588 -0.0341 -0.0455 0.116 Uiso 0.090(4) 1 calc PR A -2 H6S6 H 0.9614 0.0638 -0.0369 0.116 Uiso 0.090(4) 1 calc PR 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 0.0241(2) 0.0246(2) 0.0282(2) -0.00060(18) -0.00148(19) 0.01207(17) O1 0.0272(5) 0.0297(5) 0.0339(6) -0.0026(5) -0.0019(4) 0.0154(4) Li1 0.0319(13) 0.0322(13) 0.0517(16) -0.0027(13) -0.0013(12) 0.0166(11) N1 0.0289(7) 0.0287(7) 0.0261(7) 0.0009(5) -0.0012(5) 0.0157(6) N2 0.0248(6) 0.0284(7) 0.0293(7) -0.0016(5) -0.0018(5) 0.0130(5) C1 0.0517(10) 0.0309(9) 0.0378(9) -0.0027(7) -0.0060(7) 0.0229(8) C2 0.0303(8) 0.0270(7) 0.0327(9) -0.0010(7) -0.0031(7) 0.0148(6) C3 0.0352(8) 0.0254(8) 0.0320(9) 0.0041(7) -0.0013(7) 0.0126(7) C4 0.0286(8) 0.0322(8) 0.0275(8) 0.0032(6) 0.0011(6) 0.0143(7) C5 0.0430(9) 0.0350(9) 0.0292(9) 0.0035(7) -0.0018(7) 0.0137(7) C6 0.0322(8) 0.0311(8) 0.0423(9) 0.0018(7) -0.0026(7) 0.0161(7) C11 0.0340(8) 0.0304(8) 0.0263(8) 0.0017(6) 0.0009(6) 0.0197(7) C12 0.0350(8) 0.0300(8) 0.0294(8) 0.0012(7) -0.0001(7) 0.0175(7) C13 0.0381(9) 0.0361(8) 0.0293(8) -0.0015(7) -0.0038(7) 0.0182(7) C14 0.0455(10) 0.0447(9) 0.0268(8) 0.0007(7) 0.0031(7) 0.0234(8) C15 0.0368(9) 0.0430(9) 0.0306(9) 0.0029(7) 0.0031(7) 0.0210(8) C16 0.0365(9) 0.0324(8) 0.0315(9) 0.0012(6) 0.0011(6) 0.0205(7) C120 0.0329(8) 0.0311(8) 0.0275(8) 0.0016(6) 0.0011(6) 0.0150(7) C121 0.0403(9) 0.0340(9) 0.0381(9) -0.0024(7) -0.0005(7) 0.0169(7) C122 0.0369(9) 0.0368(9) 0.0362(9) -0.0043(7) -0.0016(7) 0.0192(7) C160 0.0321(8) 0.0429(9) 0.0283(8) 0.0029(7) 0.0023(7) 0.0198(7) C161 0.0424(9) 0.0517(11) 0.0418(10) -0.0041(8) -0.0035(8) 0.0308(9) C162 0.0389(10) 0.0557(11) 0.0400(10) 0.0055(8) -0.0019(8) 0.0141(9) C21 0.0296(8) 0.0249(7) 0.0275(8) 0.0010(6) -0.0033(6) 0.0116(6) C22 0.0305(8) 0.0311(8) 0.0329(8) -0.0009(7) 0.0000(6) 0.0131(7) C23 0.0379(9) 0.0284(8) 0.0312(8) -0.0010(6) -0.0006(7) 0.0151(7) C24 0.0371(9) 0.0277(8) 0.0280(8) 0.0007(6) -0.0055(7) 0.0115(7) C25 0.0297(8) 0.0307(8) 0.0319(8) 0.0029(7) -0.0062(6) 0.0112(7) C26 0.0291(8) 0.0275(8) 0.0282(8) 0.0049(6) -0.0020(6) 0.0132(7) C220 0.0318(9) 0.0447(10) 0.0500(10) -0.0182(8) -0.0035(8) 0.0167(8) C221 0.0395(11) 0.0705(14) 0.0677(14) -0.0244(11) 0.0126(10) 0.0132(10) C222 0.0475(11) 0.0573(12) 0.0784(14) -0.0267(10) -0.0217(10) 0.0358(10) C260 0.0268(8) 0.0350(9) 0.0315(8) -0.0016(7) -0.0055(6) 0.0142(7) C261 0.0357(9) 0.0433(9) 0.0368(9) -0.0008(7) 0.0014(7) 0.0168(8) C262 0.0447(10) 0.0495(10) 0.0391(10) 0.0002(8) -0.0016(8) 0.0297(9) C1S 0.057(10) 0.045(7) 0.064(5) -0.004(8) -0.010(8) 0.031(5) C2S 0.059(6) 0.057(5) 0.074(5) -0.005(5) 0.012(4) 0.023(4) C3S 0.061(4) 0.078(6) 0.073(4) 0.002(5) 0.002(4) 0.013(6) C4S 0.072(4) 0.071(6) 0.076(4) -0.009(5) 0.000(4) 0.031(5) C5S 0.080(6) 0.065(6) 0.077(5) -0.007(5) 0.001(5) 0.034(5) C6S 0.084(10) 0.071(10) 0.068(5) -0.009(7) -0.001(8) 0.037(5) C1SA 0.068(12) 0.057(11) 0.068(11) -0.007(11) 0.006(9) 0.016(9) C2SA 0.069(7) 0.055(7) 0.081(6) -0.008(7) 0.007(6) 0.023(7) C3SA 0.071(6) 0.069(6) 0.080(5) -0.003(6) 0.001(6) 0.029(6) C4SA 0.076(6) 0.068(7) 0.080(6) -0.005(6) 0.001(6) 0.036(6) C5SA 0.083(7) 0.069(8) 0.070(7) -0.005(6) -0.002(7) 0.034(7) C6SA 0.102(12) 0.055(11) 0.078(12) -0.005(10) 0.014(11) 0.041(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Al1 O1 1.6980(10) . ? Al1 N2 1.9357(13) . ? Al1 N1 1.9528(13) . ? Al1 C6 1.9736(17) . ? Al1 Li1 3.105(3) 2_655 ? Al1 Li1 3.251(3) . ? O1 Li1 1.791(3) . ? O1 Li1 1.808(3) 2_655 ? Li1 O1 1.808(3) 3_665 ? Li1 Li1 2.712(4) 2_655 ? Li1 Li1 2.712(4) 3_665 ? Li1 Al1 3.105(3) 3_665 ? N1 C2 1.3356(19) . ? N1 C11 1.457(2) . ? N2 C4 1.335(2) . ? N2 C21 1.446(2) . ? C1 C2 1.513(2) . ? C2 C3 1.402(2) . ? C3 C4 1.396(2) . ? C4 C5 1.520(2) . ? C11 C12 1.403(2) . ? C11 C16 1.408(2) . ? C12 C13 1.396(2) . ? C12 C120 1.525(2) . ? C13 C14 1.384(2) . ? C14 C15 1.373(2) . ? C15 C16 1.402(2) . ? C16 C160 1.520(2) . ? C120 C122 1.527(2) . ? C120 C121 1.533(2) . ? C160 C162 1.525(2) . ? C160 C161 1.532(2) . ? C21 C22 1.405(2) . ? C21 C26 1.408(2) . ? C22 C23 1.391(2) . ? C22 C220 1.518(2) . ? C23 C24 1.379(2) . ? C24 C25 1.376(2) . ? C25 C26 1.397(2) . ? C26 C260 1.520(2) . ? C220 C221 1.529(3) . ? C220 C222 1.530(3) . ? C260 C262 1.531(2) . ? C260 C261 1.534(2) . ? C1S C2S 1.504(12) . ? C2S C3S 1.497(12) . ? C3S C4S 1.510(11) . ? C4S C5S 1.546(12) . ? C5S C6S 1.484(12) . ? C1SA C2SA 1.500(16) . ? C2SA C3SA 1.484(16) . ? C3SA C4SA 1.536(16) . ? C4SA C5SA 1.510(15) . ? C5SA C6SA 1.519(16) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Al1 N2 111.90(5) . . ? O1 Al1 N1 111.28(5) . . ? N2 Al1 N1 93.65(5) . . ? O1 Al1 C6 117.09(6) . . ? N2 Al1 C6 109.03(6) . . ? N1 Al1 C6 111.46(7) . . ? O1 Al1 Li1 28.62(5) . 2_655 ? N2 Al1 Li1 117.06(7) . 2_655 ? N1 Al1 Li1 134.84(6) . 2_655 ? C6 Al1 Li1 89.98(6) . 2_655 ? O1 Al1 Li1 21.90(5) . . ? N2 Al1 Li1 106.34(7) . . ? N1 Al1 Li1 91.12(6) . . ? C6 Al1 Li1 136.11(7) . . ? Li1 Al1 Li1 50.45(9) 2_655 . ? Al1 O1 Li1 137.40(10) . . ? Al1 O1 Li1 124.65(9) . 2_655 ? Li1 O1 Li1 97.78(15) . 2_655 ? O1 Li1 O1 142.21(15) . 3_665 ? O1 Li1 Li1 41.34(10) . 2_655 ? O1 Li1 Li1 100.87(10) 3_665 2_655 ? O1 Li1 Li1 101.34(10) . 3_665 ? O1 Li1 Li1 40.87(10) 3_665 3_665 ? Li1 Li1 Li1 60.0 2_655 3_665 ? O1 Li1 Al1 168.63(13) . 3_665 ? O1 Li1 Al1 26.73(5) 3_665 3_665 ? Li1 Li1 Al1 127.51(11) 2_655 3_665 ? Li1 Li1 Al1 67.56(11) 3_665 3_665 ? O1 Li1 Al1 20.71(5) . . ? O1 Li1 Al1 162.69(12) 3_665 . ? Li1 Li1 Al1 61.99(10) 2_655 . ? Li1 Li1 Al1 121.95(10) 3_665 . ? Al1 Li1 Al1 169.58(9) 3_665 . ? C2 N1 C11 118.10(12) . . ? C2 N1 Al1 118.62(10) . . ? C11 N1 Al1 122.81(10) . . ? C4 N2 C21 117.19(12) . . ? C4 N2 Al1 117.93(10) . . ? C21 N2 Al1 124.58(9) . . ? N1 C2 C3 123.25(14) . . ? N1 C2 C1 120.54(14) . . ? C3 C2 C1 116.17(14) . . ? C4 C3 C2 126.64(14) . . ? N2 C4 C3 122.69(14) . . ? N2 C4 C5 119.96(14) . . ? C3 C4 C5 117.34(14) . . ? C12 C11 C16 120.97(14) . . ? C12 C11 N1 120.53(13) . . ? C16 C11 N1 118.50(13) . . ? C13 C12 C11 118.41(14) . . ? C13 C12 C120 118.22(14) . . ? C11 C12 C120 123.37(14) . . ? C14 C13 C12 121.22(15) . . ? C15 C14 C13 119.85(15) . . ? C14 C15 C16 121.40(15) . . ? C15 C16 C11 118.11(15) . . ? C15 C16 C160 119.43(14) . . ? C11 C16 C160 122.36(14) . . ? C12 C120 C122 110.99(13) . . ? C12 C120 C121 111.74(13) . . ? C122 C120 C121 109.87(13) . . ? C16 C160 C162 113.36(14) . . ? C16 C160 C161 109.37(13) . . ? C162 C160 C161 110.46(14) . . ? C22 C21 C26 120.66(13) . . ? C22 C21 N2 120.89(13) . . ? C26 C21 N2 118.45(13) . . ? C23 C22 C21 118.59(14) . . ? C23 C22 C220 119.15(14) . . ? C21 C22 C220 122.25(14) . . ? C24 C23 C22 121.40(15) . . ? C25 C24 C23 119.53(14) . . ? C24 C25 C26 121.70(14) . . ? C25 C26 C21 118.06(14) . . ? C25 C26 C260 119.22(13) . . ? C21 C26 C260 122.71(13) . . ? C22 C220 C221 111.63(17) . . ? C22 C220 C222 110.10(15) . . ? C221 C220 C222 110.55(17) . . ? C26 C260 C262 112.23(14) . . ? C26 C260 C261 111.33(13) . . ? C262 C260 C261 109.65(13) . . ? C3S C2S C1S 113.2(12) . . ? C2S C3S C4S 118.0(9) . . ? C3S C4S C5S 113.1(10) . . ? C6S C5S C4S 108.7(11) . . ? C3SA C2SA C1SA 125(3) . . ? C2SA C3SA C4SA 114(2) . . ? C5SA C4SA C3SA 114.3(18) . . ? C4SA C5SA C6SA 109.7(18) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 58.93 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.306 _refine_diff_density_min -0.132 _refine_diff_density_rms 0.026 data_test _database_code_depnum_ccdc_archive 'CCDC 654338' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C96 H146 Ga3 Li3 N6 O3' _chemical_formula_weight 1662.17 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0008 0.0003 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ga Ga -1.2846 0.7763 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting hexagonal _symmetry_space_group_name_H-M P6(3) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' '-x, -y, z+1/2' 'y, -x+y, z+1/2' 'x-y, x, z+1/2' _cell_length_a 15.902(2) _cell_length_b 15.902(2) _cell_length_c 21.419(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 4690.7(11) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 7032 _cell_measurement_theta_min 3.216 _cell_measurement_theta_max 58.892 _exptl_crystal_description blocks _exptl_crystal_colour colorless _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.177 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1780 _exptl_absorpt_coefficient_mu 1.376 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7705 _exptl_absorpt_correction_T_max 0.8202 _exptl_absorpt_process_details 'Sadabs, Sheldrick 2007' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator 'mirror system' _diffrn_measurement_device_type 'Bruker three circle diffractometer' _diffrn_measurement_method 'phi and omega scan' _diffrn_detector_area_resol_mean 5.602 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 33693 _diffrn_reflns_av_R_equivalents 0.0330 _diffrn_reflns_av_sigmaI/netI 0.0203 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 3.21 _diffrn_reflns_theta_max 59.07 _reflns_number_total 4490 _reflns_number_gt 4404 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Proteum (v 1.40, Bruker 2002)' _computing_cell_refinement 'Bruker AXS SAINT (v 7.01A, Bruker 2003)' _computing_data_reduction 'Bruker AXS SAINT (v 7.01A, Bruker 2003)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker AXS SHELXTL (v 6.12)' _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. The hexane molecule was disordered along the 3-fold axis. Distance restraints and restraints for the anisotropic displacment parameters were used to refine it. The found position of the hydrogen atom bond to C3 deviates from its calculated position. Therefore it was refined with a distance restraint. ; _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^)+(0.0428P)^2^+0.5250P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00024(5) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.016(16) _refine_ls_number_reflns 4490 _refine_ls_number_parameters 386 _refine_ls_number_restraints 57 _refine_ls_R_factor_all 0.0224 _refine_ls_R_factor_gt 0.0218 _refine_ls_wR_factor_ref 0.0606 _refine_ls_wR_factor_gt 0.0601 _refine_ls_goodness_of_fit_ref 1.050 _refine_ls_restrained_S_all 1.082 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ga1 Ga 0.080629(13) 0.622938(13) 0.805814(16) 0.02271(9) Uani 1 1 d . . . O1 O 0.20349(8) 0.65008(8) 0.79908(7) 0.0276(3) Uani 1 1 d . . . Li1 Li 0.3187(2) 0.7578(2) 0.7985(2) 0.0361(8) Uani 1 1 d . . . N1 N 0.07699(11) 0.73528(11) 0.84686(7) 0.0239(3) Uani 1 1 d . . . N2 N 0.03740(10) 0.64828(11) 0.72388(8) 0.0247(3) Uani 1 1 d . . . C1 C 0.10954(17) 0.90375(15) 0.84447(11) 0.0355(5) Uani 1 1 d . . . H1A H 0.0805 0.8870 0.8862 0.053 Uiso 0.50 1 calc PR . . H1B H 0.0767 0.9304 0.8196 0.053 Uiso 0.50 1 calc PR . . H1C H 0.1786 0.9522 0.8481 0.053 Uiso 0.50 1 calc PR . . H1D H 0.1434 0.9595 0.8163 0.053 Uiso 0.50 1 calc PR . . H1E H 0.1472 0.9160 0.8830 0.053 Uiso 0.50 1 calc PR . . H1F H 0.0452 0.8942 0.8545 0.053 Uiso 0.50 1 calc PR . . C2 C 0.09849(12) 0.81339(12) 0.81288(11) 0.0274(4) Uani 1 1 d . . . C3 C 0.10816(14) 0.81785(13) 0.74792(10) 0.0286(4) Uani 1 1 d D . . H3 H 0.1267(16) 0.8800(13) 0.7287(11) 0.035(6) Uiso 1 1 d D . . C4 C 0.07208(14) 0.74014(15) 0.70604(10) 0.0281(5) Uani 1 1 d . . . C5 C 0.07194(16) 0.76332(15) 0.63749(10) 0.0354(5) Uani 1 1 d . . . H5A H 0.1082 0.7391 0.6138 0.053 Uiso 1 1 calc R . . H5B H 0.1026 0.8338 0.6320 0.053 Uiso 1 1 calc R . . H5C H 0.0049 0.7321 0.6222 0.053 Uiso 1 1 calc R . . C6 C -0.01802(14) 0.49586(14) 0.83949(11) 0.0325(5) Uani 1 1 d . . . H6A H 0.0023 0.4479 0.8318 0.049 Uiso 1 1 calc R . . H6B H -0.0804 0.4750 0.8189 0.049 Uiso 1 1 calc R . . H6C H -0.0249 0.5016 0.8845 0.049 Uiso 1 1 calc R . . C11 C 0.06224(15) 0.73707(15) 0.91325(9) 0.0253(4) Uani 1 1 d . . . C12 C 0.14145(15) 0.78718(14) 0.95392(10) 0.0284(4) Uani 1 1 d . . . C13 C 0.12322(15) 0.78790(15) 1.01728(10) 0.0333(5) Uani 1 1 d . . . H13 H 0.1762 0.8205 1.0453 0.040 Uiso 1 1 calc R . . C14 C 0.02924(16) 0.74201(16) 1.04051(10) 0.0354(5) Uani 1 1 d . . . H14 H 0.0181 0.7449 1.0838 0.042 Uiso 1 1 calc R . . C15 C -0.04778(15) 0.69229(15) 1.00051(10) 0.0324(5) Uani 1 1 d . . . H15 H -0.1119 0.6606 1.0168 0.039 Uiso 1 1 calc R . . C16 C -0.03405(14) 0.68715(13) 0.93666(10) 0.0273(4) Uani 1 1 d . . . C120 C 0.24627(15) 0.84066(14) 0.93152(10) 0.0308(5) Uani 1 1 d . . . H120 H 0.2462 0.8532 0.8858 0.037 Uiso 1 1 calc R . . C121 C 0.30688(16) 0.93966(15) 0.96484(11) 0.0379(5) Uani 1 1 d . . . H12A H 0.3192 0.9287 1.0081 0.057 Uiso 1 1 calc R . . H12B H 0.2709 0.9749 0.9645 0.057 Uiso 1 1 calc R . . H12C H 0.3688 0.9780 0.9430 0.057 Uiso 1 1 calc R . . C122 C 0.29377(16) 0.77901(15) 0.94116(11) 0.0361(5) Uani 1 1 d . . . H12D H 0.2895 0.7611 0.9853 0.054 Uiso 1 1 calc R . . H12E H 0.3621 0.8161 0.9287 0.054 Uiso 1 1 calc R . . H12F H 0.2603 0.7201 0.9157 0.054 Uiso 1 1 calc R . . C160 C -0.12136(15) 0.63452(15) 0.89377(10) 0.0304(4) Uani 1 1 d . . . H160 H -0.1015 0.6090 0.8574 0.037 Uiso 1 1 calc R . . C161 C -0.15091(16) 0.70673(16) 0.86880(11) 0.0385(5) Uani 1 1 d . . . H16A H -0.1607 0.7405 0.9039 0.058 Uiso 1 1 calc R . . H16B H -0.2114 0.6715 0.8450 0.058 Uiso 1 1 calc R . . H16C H -0.0995 0.7542 0.8416 0.058 Uiso 1 1 calc R . . C162 C -0.20784(17) 0.54835(18) 0.92550(12) 0.0454(6) Uani 1 1 d . . . H16D H -0.1869 0.5051 0.9434 0.068 Uiso 1 1 calc R . . H16E H -0.2590 0.5126 0.8946 0.068 Uiso 1 1 calc R . . H16F H -0.2329 0.5722 0.9587 0.068 Uiso 1 1 calc R . . C21 C -0.02299(13) 0.57240(13) 0.68102(9) 0.0260(4) Uani 1 1 d . . . C22 C 0.01658(14) 0.52954(14) 0.64208(10) 0.0303(4) Uani 1 1 d . . . C23 C -0.04388(14) 0.45959(14) 0.59972(10) 0.0305(4) Uani 1 1 d . . . H23 H -0.0179 0.4302 0.5733 0.037 Uiso 1 1 calc R . . C24 C -0.14123(14) 0.43134(14) 0.59487(10) 0.0303(5) Uani 1 1 d . . . H24 H -0.1811 0.3847 0.5646 0.036 Uiso 1 1 calc R . . C25 C -0.17982(14) 0.47175(13) 0.63454(10) 0.0295(4) Uani 1 1 d . . . H25 H -0.2470 0.4513 0.6317 0.035 Uiso 1 1 calc R . . C26 C -0.12294(13) 0.54164(13) 0.67853(9) 0.0258(4) Uani 1 1 d . . . C220 C 0.12286(15) 0.55669(16) 0.64599(12) 0.0412(6) Uani 1 1 d . . . H220 H 0.1577 0.6163 0.6724 0.049 Uiso 1 1 calc R . . C221 C 0.17089(18) 0.5794(2) 0.58193(15) 0.0646(8) Uani 1 1 d . . . H22A H 0.1381 0.5217 0.5553 0.097 Uiso 1 1 calc R . . H22B H 0.2394 0.5982 0.5864 0.097 Uiso 1 1 calc R . . H22C H 0.1661 0.6329 0.5629 0.097 Uiso 1 1 calc R . . C222 C 0.13131(18) 0.47523(19) 0.67773(15) 0.0549(7) Uani 1 1 d . . . H22D H 0.0959 0.4155 0.6532 0.082 Uiso 1 1 calc R . . H22E H 0.1035 0.4645 0.7198 0.082 Uiso 1 1 calc R . . H22F H 0.1999 0.4934 0.6805 0.082 Uiso 1 1 calc R . . C260 C -0.16934(14) 0.58180(15) 0.72245(10) 0.0284(4) Uani 1 1 d . . . H260 H -0.1207 0.6208 0.7553 0.034 Uiso 1 1 calc R . . C261 C -0.25893(15) 0.49964(16) 0.75503(11) 0.0365(5) Uani 1 1 d . . . H26A H -0.3080 0.4607 0.7237 0.055 Uiso 1 1 calc R . . H26B H -0.2858 0.5276 0.7842 0.055 Uiso 1 1 calc R . . H26C H -0.2401 0.4583 0.7780 0.055 Uiso 1 1 calc R . . C262 C -0.19837(16) 0.64856(16) 0.68891(11) 0.0377(5) Uani 1 1 d . . . H26D H -0.1409 0.7025 0.6695 0.057 Uiso 1 1 calc R . . H26E H -0.2262 0.6741 0.7191 0.057 Uiso 1 1 calc R . . H26F H -0.2466 0.6117 0.6566 0.057 Uiso 1 1 calc R . . C1S C 0.011(2) 0.988(2) 1.2083(6) 0.107(10) Uani 0.33 1 d PDU A -1 H1S1 H -0.0102 0.9985 1.2489 0.161 Uiso 0.33 1 calc PR A -1 H1S2 H 0.0727 1.0458 1.1968 0.161 Uiso 0.33 1 calc PR A -1 H1S3 H 0.0211 0.9319 1.2110 0.161 Uiso 0.33 1 calc PR A -1 C2S C -0.0570(10) 0.9710(11) 1.1644(7) 0.096(3) Uani 0.33 1 d PDU A -1 H2S1 H -0.0694 1.0260 1.1607 0.115 Uiso 0.33 1 calc PR A -1 H2S2 H -0.1188 0.9105 1.1730 0.115 Uiso 0.33 1 calc PR A -1 C3S C -0.008(3) 0.9617(15) 1.1083(7) 0.138(6) Uani 0.33 1 d PDU A -1 H3S1 H 0.0621 1.0117 1.1070 0.165 Uiso 0.33 1 calc PR A -1 H3S2 H -0.0151 0.8963 1.1045 0.165 Uiso 0.33 1 calc PR A -1 C4S C -0.0574(17) 0.977(2) 1.0672(7) 0.153(7) Uani 0.33 1 d PDU A -1 H4S1 H -0.0309 1.0472 1.0607 0.183 Uiso 0.33 1 calc PR A -1 H4S2 H -0.1261 0.9471 1.0803 0.183 Uiso 0.33 1 calc PR A -1 C5S C -0.049(2) 0.9328(14) 1.0127(7) 0.163(8) Uani 0.33 1 d PDU A -1 H5S1 H 0.0022 0.9155 1.0162 0.196 Uiso 0.33 1 calc PR A -1 H5S2 H -0.1115 0.8744 1.0016 0.196 Uiso 0.33 1 calc PR A -1 C6S C -0.025(2) 1.008(3) 0.9710(8) 0.159(12) Uani 0.33 1 d PDU A -1 H6S1 H -0.0102 0.9899 0.9303 0.239 Uiso 0.33 1 calc PR A -1 H6S2 H 0.0325 1.0665 0.9864 0.239 Uiso 0.33 1 calc PR A -1 H6S3 H -0.0791 1.0198 0.9668 0.239 Uiso 0.33 1 calc PR A -1 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 Ga1 0.02026(12) 0.02049(12) 0.02711(14) -0.00005(11) -0.00147(11) 0.00999(8) O1 0.0227(6) 0.0258(6) 0.0353(8) -0.0028(6) -0.0024(6) 0.0129(5) Li1 0.0281(15) 0.0299(15) 0.050(2) -0.0018(17) -0.0002(18) 0.0142(13) N1 0.0258(8) 0.0251(8) 0.0222(9) 0.0024(6) -0.0007(6) 0.0139(7) N2 0.0224(8) 0.0228(8) 0.0268(9) -0.0027(7) -0.0020(7) 0.0098(6) C1 0.0485(12) 0.0258(10) 0.0332(13) -0.0011(9) -0.0057(9) 0.0193(10) C2 0.0279(9) 0.0234(8) 0.0305(13) -0.0016(9) -0.0040(9) 0.0126(7) C3 0.0301(10) 0.0206(10) 0.0304(13) 0.0037(8) -0.0012(9) 0.0091(8) C4 0.0234(10) 0.0291(11) 0.0297(12) 0.0026(9) 0.0010(8) 0.0117(9) C5 0.0406(12) 0.0311(11) 0.0265(12) 0.0000(9) -0.0023(10) 0.0120(9) C6 0.0279(10) 0.0253(10) 0.0439(12) 0.0036(9) -0.0010(9) 0.0131(9) C11 0.0330(11) 0.0247(10) 0.0236(11) 0.0020(8) -0.0002(8) 0.0185(9) C12 0.0310(11) 0.0259(10) 0.0287(12) 0.0017(8) -0.0003(9) 0.0145(8) C13 0.0380(12) 0.0325(11) 0.0291(12) -0.0010(9) -0.0061(9) 0.0174(9) C14 0.0424(12) 0.0394(12) 0.0244(11) 0.0017(9) 0.0012(9) 0.0206(10) C15 0.0334(11) 0.0380(12) 0.0288(12) 0.0035(9) 0.0024(9) 0.0201(10) C16 0.0313(11) 0.0284(10) 0.0261(12) 0.0020(8) 0.0002(8) 0.0178(9) C120 0.0314(11) 0.0338(11) 0.0251(11) 0.0021(9) -0.0022(9) 0.0147(9) C121 0.0406(12) 0.0308(11) 0.0379(13) -0.0024(9) -0.0018(10) 0.0146(10) C122 0.0342(11) 0.0371(12) 0.0352(13) -0.0061(9) -0.0024(9) 0.0165(10) C160 0.0309(11) 0.0370(11) 0.0267(11) 0.0039(9) 0.0010(9) 0.0195(9) C161 0.0396(11) 0.0475(13) 0.0399(13) -0.0051(10) -0.0080(10) 0.0304(11) C162 0.0349(12) 0.0515(14) 0.0361(14) 0.0046(11) -0.0019(10) 0.0113(11) C21 0.0270(9) 0.0240(9) 0.0242(10) 0.0014(8) -0.0009(8) 0.0106(8) C22 0.0272(10) 0.0284(10) 0.0326(12) -0.0003(9) 0.0004(9) 0.0119(8) C23 0.0337(11) 0.0263(10) 0.0291(12) -0.0018(8) 0.0009(9) 0.0132(9) C24 0.0339(11) 0.0253(9) 0.0249(11) 0.0005(8) -0.0059(9) 0.0097(8) C25 0.0259(10) 0.0280(10) 0.0290(11) 0.0034(9) -0.0052(8) 0.0093(8) C26 0.0258(10) 0.0243(9) 0.0259(11) 0.0047(8) -0.0005(8) 0.0116(8) C220 0.0298(11) 0.0395(12) 0.0510(15) -0.0194(11) -0.0022(10) 0.0149(9) C221 0.0353(13) 0.0659(17) 0.073(2) -0.0269(15) 0.0139(13) 0.0104(13) C222 0.0431(13) 0.0529(14) 0.081(2) -0.0279(14) -0.0246(13) 0.0331(12) C260 0.0248(10) 0.0308(11) 0.0291(11) -0.0022(9) -0.0045(9) 0.0135(9) C261 0.0324(11) 0.0402(12) 0.0320(12) -0.0001(10) 0.0034(9) 0.0145(9) C262 0.0420(12) 0.0431(12) 0.0359(13) 0.0015(10) -0.0011(10) 0.0271(10) C1S 0.087(16) 0.094(19) 0.083(6) 0.039(12) -0.013(12) 0.002(11) C2S 0.123(9) 0.079(9) 0.096(8) -0.018(8) -0.037(7) 0.057(8) C3S 0.246(16) 0.108(12) 0.097(8) -0.048(9) -0.036(11) 0.116(14) C4S 0.181(16) 0.236(19) 0.107(9) -0.018(11) -0.006(11) 0.154(18) C5S 0.33(3) 0.142(11) 0.103(9) -0.031(10) -0.068(14) 0.179(16) C6S 0.15(2) 0.23(2) 0.128(11) 0.06(2) -0.038(16) 0.114(13) _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 Ga1 O1 1.7835(11) . ? Ga1 C6 1.973(2) . ? Ga1 N2 1.9980(16) . ? Ga1 N1 2.0176(16) . ? Ga1 Li1 3.183(3) 2_665 ? O1 Li1 1.776(3) . ? O1 Li1 1.806(3) 2_665 ? Li1 O1 1.806(3) 3_565 ? Li1 Li1 2.734(5) 2_665 ? Li1 Li1 2.734(5) 3_565 ? Li1 Ga1 3.183(3) 3_565 ? N1 C2 1.329(2) . ? N1 C11 1.444(3) . ? N2 C4 1.334(3) . ? N2 C21 1.436(3) . ? C1 C2 1.517(3) . ? C2 C3 1.398(3) . ? C3 C4 1.397(3) . ? C4 C5 1.514(3) . ? C11 C12 1.406(3) . ? C11 C16 1.418(3) . ? C12 C13 1.389(3) . ? C12 C120 1.521(3) . ? C13 C14 1.387(3) . ? C14 C15 1.375(3) . ? C15 C16 1.394(3) . ? C16 C160 1.520(3) . ? C120 C122 1.522(3) . ? C120 C121 1.549(3) . ? C160 C162 1.532(3) . ? C160 C161 1.538(3) . ? C21 C22 1.409(3) . ? C21 C26 1.411(3) . ? C22 C23 1.384(3) . ? C22 C220 1.523(3) . ? C23 C24 1.383(3) . ? C24 C25 1.381(3) . ? C25 C26 1.391(3) . ? C26 C260 1.519(3) . ? C220 C221 1.523(4) . ? C220 C222 1.527(4) . ? C260 C262 1.532(3) . ? C260 C261 1.537(3) . ? C1S C2S 1.359(19) . ? C2S C3S 1.48(2) . ? C3S C4S 1.28(2) . ? C4S C5S 1.398(19) . ? C5S C6S 1.38(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Ga1 C6 119.41(7) . . ? O1 Ga1 N2 109.02(7) . . ? C6 Ga1 N2 110.49(8) . . ? O1 Ga1 N1 109.50(6) . . ? C6 Ga1 N1 112.79(8) . . ? N2 Ga1 N1 92.24(6) . . ? O1 Ga1 Li1 27.73(6) . 2_665 ? C6 Ga1 Li1 92.98(8) . 2_665 ? N2 Ga1 Li1 115.59(9) . 2_665 ? N1 Ga1 Li1 132.90(8) . 2_665 ? Li1 O1 Ga1 135.32(12) . . ? Li1 O1 Li1 99.52(19) . 2_665 ? Ga1 O1 Li1 124.92(12) . 2_665 ? O1 Li1 O1 140.47(19) . 3_565 ? O1 Li1 Li1 40.64(12) . 2_665 ? O1 Li1 Li1 99.84(12) 3_565 2_665 ? O1 Li1 Li1 100.64(12) . 3_565 ? O1 Li1 Li1 39.84(12) 3_565 3_565 ? Li1 Li1 Li1 60.0 2_665 3_565 ? O1 Li1 Ga1 167.34(16) . 3_565 ? O1 Li1 Ga1 27.36(6) 3_565 3_565 ? Li1 Li1 Ga1 127.05(13) 2_665 3_565 ? Li1 Li1 Ga1 67.13(13) 3_565 3_565 ? C2 N1 C11 119.31(16) . . ? C2 N1 Ga1 118.77(13) . . ? C11 N1 Ga1 121.56(12) . . ? C4 N2 C21 118.28(16) . . ? C4 N2 Ga1 118.49(13) . . ? C21 N2 Ga1 123.03(12) . . ? N1 C2 C3 124.27(17) . . ? N1 C2 C1 119.68(19) . . ? C3 C2 C1 116.00(17) . . ? C4 C3 C2 127.46(18) . . ? N2 C4 C3 123.15(19) . . ? N2 C4 C5 119.63(18) . . ? C3 C4 C5 117.21(18) . . ? C12 C11 C16 120.59(19) . . ? C12 C11 N1 120.87(18) . . ? C16 C11 N1 118.54(18) . . ? C13 C12 C11 118.58(19) . . ? C13 C12 C120 118.59(18) . . ? C11 C12 C120 122.83(19) . . ? C14 C13 C12 121.4(2) . . ? C15 C14 C13 119.6(2) . . ? C14 C15 C16 121.6(2) . . ? C15 C16 C11 118.10(18) . . ? C15 C16 C160 119.92(18) . . ? C11 C16 C160 121.87(18) . . ? C12 C120 C122 110.80(17) . . ? C12 C120 C121 111.95(18) . . ? C122 C120 C121 109.59(17) . . ? C16 C160 C162 112.87(18) . . ? C16 C160 C161 109.58(17) . . ? C162 C160 C161 110.45(18) . . ? C22 C21 C26 120.54(17) . . ? C22 C21 N2 120.80(16) . . ? C26 C21 N2 118.65(16) . . ? C23 C22 C21 118.56(18) . . ? C23 C22 C220 119.35(18) . . ? C21 C22 C220 122.08(17) . . ? C24 C23 C22 121.68(19) . . ? C25 C24 C23 119.22(18) . . ? C24 C25 C26 121.73(18) . . ? C25 C26 C21 118.18(18) . . ? C25 C26 C260 119.77(17) . . ? C21 C26 C260 122.05(17) . . ? C22 C220 C221 111.8(2) . . ? C22 C220 C222 109.86(19) . . ? C221 C220 C222 110.8(2) . . ? C26 C260 C262 112.27(18) . . ? C26 C260 C261 111.25(17) . . ? C262 C260 C261 109.25(17) . . ? C1S C2S C3S 99.8(18) . . ? C4S C3S C2S 97(2) . . ? C3S C4S C5S 105.1(18) . . ? C6S C5S C4S 99.6(18) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 59.07 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.263 _refine_diff_density_min -0.197 _refine_diff_density_rms 0.035