Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2004 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _journal_volume ? _journal_year ? _journal_page_first ? _publ_contact_author_name 'ProfD Norbert Mitzel' _publ_contact_author_address ; Institut fur Anorganische und Analytische Chemie Universitat Munster Corrensstr.8 Munster D-48149 GERMANY ; _publ_contact_author_email MITZEL@UNI-MUENSTER.DE _publ_section_title ; Organoaluminium and -gallium compounds with N,N-diisopropylaminomethyl groups ; loop_ _publ_author_name 'Norbert Mitzel' 'Roland Frohlich' 'Xin Tian' data_fro2694 _database_code_depnum_ccdc_archive 'CCDC 252361' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C27 H62 Cl Ga2 N' _chemical_formula_weight 575.67 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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ga Ga 0.2307 1.6083 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/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 8.852(1) _cell_length_b 17.740(1) _cell_length_c 21.202(1) _cell_angle_alpha 90.00 _cell_angle_beta 93.25(1) _cell_angle_gamma 90.00 _cell_volume 3324.1(4) _cell_formula_units_Z 4 _cell_measurement_temperature 198(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description pyramide _exptl_crystal_colour colourless _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.150 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1240 _exptl_absorpt_coefficient_mu 1.714 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.4261 _exptl_absorpt_correction_T_max 0.7255 _exptl_absorpt_process_details 'SORTAV (Blessing, 1995 & 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 198(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode Nonius FR591' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method '\w and \f scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 25982 _diffrn_reflns_av_R_equivalents 0.0563 _diffrn_reflns_av_sigmaI/netI 0.0439 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 2.24 _diffrn_reflns_theta_max 27.87 _reflns_number_total 7871 _reflns_number_gt 6185 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius B.V., 1998)' _computing_cell_refinement 'Collect (Nonius B.V., 1998)' _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 'SCHAKAL (Keller, 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^)+(0.0460P)^2^+0.0000P] where P==(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7871 _refine_ls_number_parameters 302 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0489 _refine_ls_R_factor_gt 0.0334 _refine_ls_wR_factor_ref 0.0871 _refine_ls_wR_factor_gt 0.0813 _refine_ls_goodness_of_fit_ref 1.046 _refine_ls_restrained_S_all 1.046 _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 -0.07903(2) 0.133952(11) 0.360482(9) 0.03549(7) Uani 1 1 d . . . C1 C -0.2060(2) 0.22419(11) 0.38729(9) 0.0433(4) Uani 1 1 d . . . H1A H -0.3135 0.2086 0.3853 0.052 Uiso 1 1 calc R . . H1B H -0.1769 0.2358 0.4320 0.052 Uiso 1 1 calc R . . N1 N -0.19361(17) 0.29547(9) 0.34969(8) 0.0364(3) Uani 1 1 d . . . H1 H -0.173(2) 0.2785(12) 0.3113(9) 0.044 Uiso 1 1 d . . . C11 C -0.0538(2) 0.34035(13) 0.36940(11) 0.0525(6) Uani 1 1 d . . . H11 H 0.0307 0.3034 0.3765 0.063 Uiso 1 1 calc R . . C12 C -0.0108(3) 0.39169(15) 0.31678(14) 0.0757(8) Uani 1 1 d . . . H12A H -0.0127 0.3633 0.2771 0.114 Uiso 1 1 calc R . . H12B H 0.0912 0.4116 0.3263 0.114 Uiso 1 1 calc R . . H12C H -0.0830 0.4335 0.3127 0.114 Uiso 1 1 calc R . . C13 C -0.0677(3) 0.38264(14) 0.43131(11) 0.0640(7) Uani 1 1 d . . . H13A H 0.0294 0.4064 0.4439 0.096 Uiso 1 1 calc R . . H13B H -0.0954 0.3472 0.4642 0.096 Uiso 1 1 calc R . . H13C H -0.1459 0.4215 0.4257 0.096 Uiso 1 1 calc R . . C14 C -0.3389(2) 0.34243(12) 0.34090(9) 0.0424(5) Uani 1 1 d . . . H14 H -0.3090 0.3952 0.3306 0.051 Uiso 1 1 calc R . . C15 C -0.4316(3) 0.31181(14) 0.28464(11) 0.0624(6) Uani 1 1 d . . . H15A H -0.4608 0.2596 0.2930 0.094 Uiso 1 1 calc R . . H15B H -0.3715 0.3133 0.2473 0.094 Uiso 1 1 calc R . . H15C H -0.5228 0.3426 0.2771 0.094 Uiso 1 1 calc R . . C16 C -0.4278(2) 0.34552(14) 0.39944(11) 0.0542(5) Uani 1 1 d . . . H16A H -0.4708 0.2957 0.4073 0.081 Uiso 1 1 calc R . . H16B H -0.5097 0.3824 0.3934 0.081 Uiso 1 1 calc R . . H16C H -0.3607 0.3604 0.4357 0.081 Uiso 1 1 calc R . . C21 C -0.2261(2) 0.04753(11) 0.35027(10) 0.0453(5) Uani 1 1 d . . . C22 C -0.3635(3) 0.06945(15) 0.30740(12) 0.0661(7) Uani 1 1 d . . . H22A H -0.3314 0.0795 0.2647 0.099 Uiso 1 1 calc R . . H22B H -0.4102 0.1148 0.3240 0.099 Uiso 1 1 calc R . . H22C H -0.4369 0.0281 0.3059 0.099 Uiso 1 1 calc R . . C23 C -0.1597(3) -0.02410(14) 0.32420(14) 0.0762(8) Uani 1 1 d . . . H23A H -0.0728 -0.0401 0.3516 0.114 Uiso 1 1 calc R . . H23B H -0.1268 -0.0146 0.2816 0.114 Uiso 1 1 calc R . . H23C H -0.2367 -0.0639 0.3226 0.114 Uiso 1 1 calc R . . C24 C -0.2803(3) 0.03250(15) 0.41626(11) 0.0703(7) Uani 1 1 d . . . H24A H -0.3610 -0.0054 0.4136 0.106 Uiso 1 1 calc R . . H24B H -0.3191 0.0793 0.4337 0.106 Uiso 1 1 calc R . . H24C H -0.1956 0.0139 0.4437 0.106 Uiso 1 1 calc R . . C25 C 0.1290(2) 0.12302(12) 0.40330(10) 0.0483(5) Uani 1 1 d . . . C26 C 0.1114(3) 0.13899(17) 0.47365(11) 0.0763(8) Uani 1 1 d . . . H26A H 0.0382 0.1036 0.4901 0.114 Uiso 1 1 calc R . . H26B H 0.0753 0.1907 0.4788 0.114 Uiso 1 1 calc R . . H26C H 0.2094 0.1328 0.4969 0.114 Uiso 1 1 calc R . . C27 C 0.2455(3) 0.17693(15) 0.37931(14) 0.0711(8) Uani 1 1 d . . . H27A H 0.3423 0.1696 0.4033 0.107 Uiso 1 1 calc R . . H27B H 0.2111 0.2289 0.3847 0.107 Uiso 1 1 calc R . . H27C H 0.2584 0.1672 0.3344 0.107 Uiso 1 1 calc R . . C28 C 0.1883(3) 0.04273(15) 0.39709(14) 0.0799(9) Uani 1 1 d . . . H28A H 0.2008 0.0314 0.3525 0.120 Uiso 1 1 calc R . . H28B H 0.1160 0.0072 0.4140 0.120 Uiso 1 1 calc R . . H28C H 0.2861 0.0380 0.4208 0.120 Uiso 1 1 calc R . . Cl1 Cl -0.04331(5) 0.18568(3) 0.25547(2) 0.04181(12) Uani 1 1 d . . . Ga2 Ga 0.02893(2) 0.173244(11) 0.139799(9) 0.03409(7) Uani 1 1 d . . . C31 C 0.1671(2) 0.08211(12) 0.14711(10) 0.0446(5) Uani 1 1 d . . . C32 C 0.3253(2) 0.10303(14) 0.17501(13) 0.0629(6) Uani 1 1 d . . . H32A H 0.3170 0.1252 0.2170 0.094 Uiso 1 1 calc R . . H32B H 0.3716 0.1396 0.1474 0.094 Uiso 1 1 calc R . . H32C H 0.3883 0.0576 0.1785 0.094 Uiso 1 1 calc R . . C33 C 0.1051(2) 0.02100(12) 0.18956(11) 0.0545(6) Uani 1 1 d . . . H33A H 0.0058 0.0044 0.1720 0.082 Uiso 1 1 calc R . . H33B H 0.0949 0.0414 0.2321 0.082 Uiso 1 1 calc R . . H33C H 0.1748 -0.0220 0.1918 0.082 Uiso 1 1 calc R . . C34 C 0.1811(3) 0.04921(14) 0.08085(11) 0.0647(7) Uani 1 1 d . . . H34A H 0.2397 0.0023 0.0839 0.097 Uiso 1 1 calc R . . H34B H 0.2326 0.0855 0.0547 0.097 Uiso 1 1 calc R . . H34C H 0.0800 0.0387 0.0617 0.097 Uiso 1 1 calc R . . C35 C 0.1281(2) 0.27524(11) 0.12728(9) 0.0397(4) Uani 1 1 d . . . C36 C 0.2441(2) 0.29491(13) 0.18081(10) 0.0537(5) Uani 1 1 d . . . H36A H 0.3253 0.2573 0.1825 0.081 Uiso 1 1 calc R . . H36B H 0.1947 0.2952 0.2210 0.081 Uiso 1 1 calc R . . H36C H 0.2867 0.3449 0.1732 0.081 Uiso 1 1 calc R . . C37 C 0.0124(2) 0.33922(13) 0.12204(12) 0.0578(6) Uani 1 1 d . . . H37A H 0.0650 0.3873 0.1173 0.087 Uiso 1 1 calc R . . H37B H -0.0447 0.3406 0.1603 0.087 Uiso 1 1 calc R . . H37C H -0.0573 0.3308 0.0852 0.087 Uiso 1 1 calc R . . C38 C 0.2105(3) 0.27203(15) 0.06574(11) 0.0613(6) Uani 1 1 d . . . H38A H 0.2634 0.3198 0.0597 0.092 Uiso 1 1 calc R . . H38B H 0.1369 0.2636 0.0302 0.092 Uiso 1 1 calc R . . H38C H 0.2840 0.2307 0.0680 0.092 Uiso 1 1 calc R . . C39 C -0.1815(2) 0.15740(12) 0.09850(9) 0.0426(5) Uani 1 1 d . . . C40 C -0.2983(2) 0.21262(14) 0.12207(11) 0.0565(6) Uani 1 1 d . . . H40A H -0.2612 0.2643 0.1178 0.085 Uiso 1 1 calc R . . H40B H -0.3146 0.2022 0.1666 0.085 Uiso 1 1 calc R . . H40C H -0.3939 0.2067 0.0970 0.085 Uiso 1 1 calc R . . C41 C -0.1684(3) 0.17003(15) 0.02759(10) 0.0615(7) Uani 1 1 d . . . H41A H -0.2676 0.1626 0.0055 0.092 Uiso 1 1 calc R . . H41B H -0.0959 0.1341 0.0115 0.092 Uiso 1 1 calc R . . H41C H -0.1334 0.2215 0.0203 0.092 Uiso 1 1 calc R . . C42 C -0.2415(2) 0.07762(14) 0.10798(11) 0.0598(6) Uani 1 1 d . . . H42A H -0.3415 0.0726 0.0861 0.090 Uiso 1 1 calc R . . H42B H -0.2496 0.0681 0.1532 0.090 Uiso 1 1 calc R . . H42C H -0.1719 0.0410 0.0907 0.090 Uiso 1 1 calc R . . 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 0.03834(13) 0.03079(12) 0.03720(13) 0.00233(8) 0.00098(8) -0.00129(8) C1 0.0533(12) 0.0362(11) 0.0412(11) 0.0050(9) 0.0097(9) 0.0015(9) N1 0.0412(9) 0.0315(9) 0.0368(9) -0.0001(7) 0.0059(6) 0.0015(6) C11 0.0424(11) 0.0387(12) 0.0763(16) -0.0037(11) 0.0031(10) -0.0024(9) C12 0.0769(18) 0.0502(15) 0.103(2) -0.0008(15) 0.0331(15) -0.0202(12) C13 0.0636(15) 0.0536(15) 0.0724(17) -0.0116(13) -0.0187(12) -0.0018(11) C14 0.0446(11) 0.0377(11) 0.0447(11) 0.0013(9) 0.0000(8) 0.0035(8) C15 0.0620(15) 0.0637(16) 0.0590(14) -0.0040(12) -0.0175(11) 0.0053(11) C16 0.0472(12) 0.0577(14) 0.0588(14) 0.0034(11) 0.0127(10) 0.0112(10) C21 0.0504(11) 0.0352(11) 0.0507(12) 0.0003(9) 0.0064(9) -0.0089(8) C22 0.0573(14) 0.0662(17) 0.0732(17) 0.0026(13) -0.0111(11) -0.0211(12) C23 0.0690(16) 0.0447(15) 0.117(2) -0.0220(15) 0.0209(15) -0.0174(12) C24 0.0884(18) 0.0654(17) 0.0582(15) 0.0068(13) 0.0127(13) -0.0308(14) C25 0.0459(12) 0.0454(13) 0.0525(13) 0.0018(10) -0.0083(9) 0.0018(9) C26 0.0708(17) 0.102(2) 0.0538(15) -0.0018(15) -0.0183(12) 0.0000(15) C27 0.0394(13) 0.0775(19) 0.095(2) 0.0152(15) -0.0089(12) -0.0038(11) C28 0.0706(17) 0.0599(17) 0.105(2) -0.0055(15) -0.0299(15) 0.0194(13) Cl1 0.0531(3) 0.0399(3) 0.0332(2) 0.00173(19) 0.00976(19) 0.0044(2) Ga2 0.03103(12) 0.03506(13) 0.03633(12) 0.00045(9) 0.00307(8) 0.00069(8) C31 0.0443(11) 0.0395(12) 0.0508(12) 0.0014(9) 0.0095(9) 0.0078(8) C32 0.0402(12) 0.0560(15) 0.0922(19) 0.0107(13) 0.0010(11) 0.0115(10) C33 0.0575(13) 0.0386(12) 0.0684(15) 0.0065(11) 0.0115(11) 0.0076(9) C34 0.0739(16) 0.0592(16) 0.0628(16) -0.0057(13) 0.0203(12) 0.0179(12) C35 0.0387(10) 0.0368(11) 0.0438(11) 0.0005(9) 0.0030(8) -0.0031(8) C36 0.0495(12) 0.0517(14) 0.0592(14) -0.0016(11) -0.0039(10) -0.0083(10) C37 0.0582(14) 0.0422(13) 0.0717(16) 0.0043(12) -0.0071(11) 0.0026(10) C38 0.0636(14) 0.0654(16) 0.0562(14) 0.0076(12) 0.0155(11) -0.0132(12) C39 0.0355(10) 0.0511(13) 0.0411(11) -0.0018(9) 0.0018(8) -0.0048(8) C40 0.0343(11) 0.0688(16) 0.0662(15) -0.0020(12) 0.0005(9) 0.0035(10) C41 0.0528(14) 0.088(2) 0.0431(13) -0.0016(12) -0.0056(10) -0.0069(12) C42 0.0482(12) 0.0607(16) 0.0705(16) -0.0057(13) 0.0031(11) -0.0146(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ga1 C21 2.0148(19) . ? Ga1 C25 2.016(2) . ? Ga1 C1 2.054(2) . ? Ga1 Cl1 2.4453(5) . ? C1 N1 1.502(2) . ? N1 C11 1.511(2) . ? N1 C14 1.535(2) . ? C11 C12 1.506(3) . ? C11 C13 1.523(3) . ? C14 C16 1.508(3) . ? C14 C15 1.510(3) . ? C21 C23 1.517(3) . ? C21 C22 1.527(3) . ? C21 C24 1.528(3) . ? C25 C27 1.515(3) . ? C25 C28 1.526(3) . ? C25 C26 1.535(3) . ? Cl1 Ga2 2.5786(5) . ? Ga2 C31 2.0281(19) . ? Ga2 C39 2.0321(18) . ? Ga2 C35 2.0352(19) . ? C31 C33 1.531(3) . ? C31 C34 1.533(3) . ? C31 C32 1.534(3) . ? C35 C36 1.527(3) . ? C35 C37 1.529(3) . ? C35 C38 1.531(3) . ? C39 C40 1.529(3) . ? C39 C42 1.529(3) . ? C39 C41 1.531(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C21 Ga1 C25 122.91(9) . . ? C21 Ga1 C1 105.22(8) . . ? C25 Ga1 C1 116.77(9) . . ? C21 Ga1 Cl1 107.69(6) . . ? C25 Ga1 Cl1 106.51(7) . . ? C1 Ga1 Cl1 93.47(6) . . ? N1 C1 Ga1 116.85(12) . . ? C1 N1 C11 112.33(16) . . ? C1 N1 C14 115.82(14) . . ? C11 N1 C14 114.55(16) . . ? C12 C11 N1 110.56(19) . . ? C12 C11 C13 112.1(2) . . ? N1 C11 C13 113.16(18) . . ? C16 C14 C15 112.20(19) . . ? C16 C14 N1 113.12(16) . . ? C15 C14 N1 108.34(17) . . ? C23 C21 C22 107.9(2) . . ? C23 C21 C24 109.6(2) . . ? C22 C21 C24 107.97(19) . . ? C23 C21 Ga1 114.54(14) . . ? C22 C21 Ga1 110.98(14) . . ? C24 C21 Ga1 105.60(14) . . ? C27 C25 C28 108.4(2) . . ? C27 C25 C26 108.6(2) . . ? C28 C25 C26 108.1(2) . . ? C27 C25 Ga1 114.19(15) . . ? C28 C25 Ga1 111.15(15) . . ? C26 C25 Ga1 106.23(15) . . ? Ga1 Cl1 Ga2 152.34(2) . . ? C31 Ga2 C39 117.18(9) . . ? C31 Ga2 C35 117.12(8) . . ? C39 Ga2 C35 117.28(8) . . ? C31 Ga2 Cl1 100.17(6) . . ? C39 Ga2 Cl1 98.68(6) . . ? C35 Ga2 Cl1 100.38(6) . . ? C33 C31 C34 108.64(18) . . ? C33 C31 C32 107.15(18) . . ? C34 C31 C32 109.03(17) . . ? C33 C31 Ga2 111.99(13) . . ? C34 C31 Ga2 108.25(14) . . ? C32 C31 Ga2 111.71(15) . . ? C36 C35 C37 107.69(18) . . ? C36 C35 C38 108.01(17) . . ? C37 C35 C38 108.38(18) . . ? C36 C35 Ga2 112.52(14) . . ? C37 C35 Ga2 112.16(13) . . ? C38 C35 Ga2 107.93(14) . . ? C40 C39 C42 107.67(17) . . ? C40 C39 C41 108.51(18) . . ? C42 C39 C41 108.10(18) . . ? C40 C39 Ga2 113.01(14) . . ? C42 C39 Ga2 112.85(14) . . ? C41 C39 Ga2 106.53(13) . . ? 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 C21 Ga1 C1 N1 -128.08(14) . . . . ? C25 Ga1 C1 N1 91.76(15) . . . . ? Cl1 Ga1 C1 N1 -18.69(14) . . . . ? Ga1 C1 N1 C11 -80.46(18) . . . . ? Ga1 C1 N1 C14 145.30(14) . . . . ? C1 N1 C11 C12 157.15(19) . . . . ? C14 N1 C11 C12 -68.0(2) . . . . ? C1 N1 C11 C13 -76.1(2) . . . . ? C14 N1 C11 C13 58.7(2) . . . . ? C1 N1 C14 C16 40.0(2) . . . . ? C11 N1 C14 C16 -93.3(2) . . . . ? C1 N1 C14 C15 -85.1(2) . . . . ? C11 N1 C14 C15 141.69(19) . . . . ? C25 Ga1 C21 C23 -48.6(2) . . . . ? C1 Ga1 C21 C23 174.32(18) . . . . ? Cl1 Ga1 C21 C23 75.54(18) . . . . ? C25 Ga1 C21 C22 -171.17(15) . . . . ? C1 Ga1 C21 C22 51.78(17) . . . . ? Cl1 Ga1 C21 C22 -47.00(16) . . . . ? C25 Ga1 C21 C24 72.08(18) . . . . ? C1 Ga1 C21 C24 -64.97(16) . . . . ? Cl1 Ga1 C21 C24 -163.75(14) . . . . ? C21 Ga1 C25 C27 150.92(17) . . . . ? C1 Ga1 C25 C27 -76.50(19) . . . . ? Cl1 Ga1 C25 C27 26.22(19) . . . . ? C21 Ga1 C25 C28 27.9(2) . . . . ? C1 Ga1 C25 C28 160.45(17) . . . . ? Cl1 Ga1 C25 C28 -96.83(18) . . . . ? C21 Ga1 C25 C26 -89.47(17) . . . . ? C1 Ga1 C25 C26 43.11(18) . . . . ? Cl1 Ga1 C25 C26 145.84(15) . . . . ? C21 Ga1 Cl1 Ga2 -56.70(8) . . . . ? C25 Ga1 Cl1 Ga2 76.87(8) . . . . ? C1 Ga1 Cl1 Ga2 -163.88(7) . . . . ? Ga1 Cl1 Ga2 C31 -24.29(8) . . . . ? Ga1 Cl1 Ga2 C39 95.51(8) . . . . ? Ga1 Cl1 Ga2 C35 -144.53(7) . . . . ? C39 Ga2 C31 C33 -63.62(17) . . . . ? C35 Ga2 C31 C33 149.02(15) . . . . ? Cl1 Ga2 C31 C33 41.71(15) . . . . ? C39 Ga2 C31 C34 56.12(17) . . . . ? C35 Ga2 C31 C34 -91.24(16) . . . . ? Cl1 Ga2 C31 C34 161.46(14) . . . . ? C39 Ga2 C31 C32 176.18(14) . . . . ? C35 Ga2 C31 C32 28.82(18) . . . . ? Cl1 Ga2 C31 C32 -78.49(15) . . . . ? C31 Ga2 C35 C36 -58.75(17) . . . . ? C39 Ga2 C35 C36 153.92(14) . . . . ? Cl1 Ga2 C35 C36 48.43(14) . . . . ? C31 Ga2 C35 C37 179.65(14) . . . . ? C39 Ga2 C35 C37 32.32(18) . . . . ? Cl1 Ga2 C35 C37 -73.17(15) . . . . ? C31 Ga2 C35 C38 60.32(16) . . . . ? C39 Ga2 C35 C38 -87.00(15) . . . . ? Cl1 Ga2 C35 C38 167.51(13) . . . . ? C31 Ga2 C39 C40 152.08(15) . . . . ? C35 Ga2 C39 C40 -60.61(17) . . . . ? Cl1 Ga2 C39 C40 45.87(15) . . . . ? C31 Ga2 C39 C42 29.62(18) . . . . ? C35 Ga2 C39 C42 176.92(14) . . . . ? Cl1 Ga2 C39 C42 -76.59(15) . . . . ? C31 Ga2 C39 C41 -88.85(16) . . . . ? C35 Ga2 C39 C41 58.45(17) . . . . ? Cl1 Ga2 C39 C41 164.94(14) . . . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 27.87 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.405 _refine_diff_density_min -0.330 _refine_diff_density_rms 0.055 data_fro2758 _database_code_depnum_ccdc_archive 'CCDC 252362' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C22 H50 Ga Li N2' _chemical_formula_weight 419.30 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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ga Ga 0.2307 1.6083 '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' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.162(1) _cell_length_b 10.082(1) _cell_length_c 15.995(1) _cell_angle_alpha 85.81(1) _cell_angle_beta 87.62(1) _cell_angle_gamma 82.59(1) _cell_volume 1301.1(2) _cell_formula_units_Z 2 _cell_measurement_temperature 198(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description needle _exptl_crystal_colour colourless _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.070 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 460 _exptl_absorpt_coefficient_mu 1.065 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.6458 _exptl_absorpt_correction_T_max 0.9010 _exptl_absorpt_process_details 'SORTAV (Blessing, 1995 & 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 198(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode Nonius FR591' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method '\w and \f scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14186 _diffrn_reflns_av_R_equivalents 0.052 _diffrn_reflns_av_sigmaI/netI 0.0491 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.28 _diffrn_reflns_theta_max 28.34 _reflns_number_total 6341 _reflns_number_gt 4953 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius B.V., 1998)' _computing_cell_refinement 'Collect (Nonius B.V., 1998)' _computing_data_reduction 'Denzo-SMN (Otwinwoski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SCHAKAL (Keller, 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^)+(0.0897P)^2^+1.4005P] 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 riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6341 _refine_ls_number_parameters 249 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0757 _refine_ls_R_factor_gt 0.0555 _refine_ls_wR_factor_ref 0.1728 _refine_ls_wR_factor_gt 0.1606 _refine_ls_goodness_of_fit_ref 1.021 _refine_ls_restrained_S_all 1.021 _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 0.74759(4) 0.04182(3) 0.25547(2) 0.03979(15) Uani 1 1 d . . . N1* N 0.5904(4) 0.3039(3) 0.3415(2) 0.0467(7) Uani 1 1 d . . . C1* C 0.5612(5) 0.1716(4) 0.3123(3) 0.0517(9) Uani 1 1 d . . . H1*A H 0.4703 0.1902 0.2724 0.062 Uiso 1 1 calc R . . H1*B H 0.5181 0.1202 0.3617 0.062 Uiso 1 1 calc R . . C11* C 0.6923(5) 0.2890(5) 0.4164(3) 0.0701(13) Uani 1 1 d . . . H11* H 0.7810 0.2127 0.4074 0.084 Uiso 1 1 calc R . . C12* C 0.6044(7) 0.2538(7) 0.4999(3) 0.0944(19) Uani 1 1 d . . . H12*A H 0.5229 0.3295 0.5143 0.142 Uiso 1 1 calc R . . H12*B H 0.6857 0.2346 0.5439 0.142 Uiso 1 1 calc R . . H12*C H 0.5482 0.1746 0.4947 0.142 Uiso 1 1 calc R . . C13* C 0.7802(6) 0.4122(7) 0.4232(4) 0.093(2) Uani 1 1 d . . . H13*A H 0.8342 0.4349 0.3691 0.140 Uiso 1 1 calc R . . H13*B H 0.8634 0.3931 0.4663 0.140 Uiso 1 1 calc R . . H13*C H 0.6994 0.4879 0.4384 0.140 Uiso 1 1 calc R . . C14* C 0.4376(5) 0.4030(4) 0.3476(3) 0.0571(10) Uani 1 1 d . . . H14* H 0.4611 0.4712 0.3864 0.069 Uiso 1 1 calc R . . C15* C 0.4070(6) 0.4751(5) 0.2632(4) 0.0735(13) Uani 1 1 d . . . H15*A H 0.5032 0.5198 0.2447 0.110 Uiso 1 1 calc R . . H15*B H 0.3091 0.5420 0.2671 0.110 Uiso 1 1 calc R . . H15*C H 0.3887 0.4105 0.2228 0.110 Uiso 1 1 calc R . . C16* C 0.2802(5) 0.3465(5) 0.3819(3) 0.0711(13) Uani 1 1 d . . . H16*A H 0.2465 0.2863 0.3423 0.107 Uiso 1 1 calc R . . H16*B H 0.1915 0.4204 0.3893 0.107 Uiso 1 1 calc R . . H16*C H 0.3023 0.2967 0.4361 0.107 Uiso 1 1 calc R . . N1 N 0.8369(3) 0.2790(3) 0.12923(19) 0.0416(6) Uani 1 1 d . . . C1 C 0.9040(4) 0.1601(3) 0.1848(2) 0.0438(8) Uani 1 1 d . . . H1A H 0.9765 0.1928 0.2247 0.053 Uiso 1 1 calc R . . H1B H 0.9762 0.0995 0.1489 0.053 Uiso 1 1 calc R . . C11 C 0.7529(5) 0.2398(4) 0.0565(3) 0.0538(9) Uani 1 1 d . . . H11 H 0.6930 0.1629 0.0777 0.065 Uiso 1 1 calc R . . C12 C 0.8666(6) 0.1895(6) -0.0160(3) 0.0752(13) Uani 1 1 d . . . H12A H 0.9225 0.2633 -0.0419 0.113 Uiso 1 1 calc R . . H12B H 0.8009 0.1559 -0.0579 0.113 Uiso 1 1 calc R . . H12C H 0.9492 0.1170 0.0053 0.113 Uiso 1 1 calc R . . C13 C 0.6214(6) 0.3509(5) 0.0263(3) 0.0751(14) Uani 1 1 d . . . H13A H 0.5465 0.3771 0.0734 0.113 Uiso 1 1 calc R . . H13B H 0.5586 0.3191 -0.0174 0.113 Uiso 1 1 calc R . . H13C H 0.6741 0.4284 0.0035 0.113 Uiso 1 1 calc R . . C14 C 0.9562(5) 0.3778(4) 0.1070(3) 0.0516(9) Uani 1 1 d . . . H14 H 0.9175 0.4305 0.0545 0.062 Uiso 1 1 calc R . . C15 C 0.9480(6) 0.4755(4) 0.1757(3) 0.0703(13) Uani 1 1 d . . . H15A H 0.8343 0.5189 0.1829 0.105 Uiso 1 1 calc R . . H15B H 1.0211 0.5438 0.1599 0.105 Uiso 1 1 calc R . . H15C H 0.9836 0.4268 0.2284 0.105 Uiso 1 1 calc R . . C16 C 1.1352(5) 0.3180(5) 0.0903(3) 0.0623(11) Uani 1 1 d . . . H16A H 1.1782 0.2674 0.1410 0.093 Uiso 1 1 calc R . . H16B H 1.2023 0.3904 0.0746 0.093 Uiso 1 1 calc R . . H16C H 1.1399 0.2580 0.0445 0.093 Uiso 1 1 calc R . . C21 C 0.9127(5) -0.0702(4) 0.3344(2) 0.0533(9) Uani 1 1 d . . . C22 C 1.0512(5) 0.0114(5) 0.3561(3) 0.0626(11) Uani 1 1 d . . . H22A H 1.1271 -0.0434 0.3946 0.094 Uiso 1 1 calc R . . H22B H 1.0022 0.0922 0.3830 0.094 Uiso 1 1 calc R . . H22C H 1.1120 0.0371 0.3046 0.094 Uiso 1 1 calc R . . C23 C 0.9980(6) -0.1929(5) 0.2913(3) 0.0718(13) Uani 1 1 d . . . H23A H 1.0549 -0.1633 0.2395 0.108 Uiso 1 1 calc R . . H23B H 0.9150 -0.2496 0.2780 0.108 Uiso 1 1 calc R . . H23C H 1.0784 -0.2442 0.3289 0.108 Uiso 1 1 calc R . . C24 C 0.8250(7) -0.1202(6) 0.4153(3) 0.0776(14) Uani 1 1 d . . . H24A H 0.9065 -0.1723 0.4521 0.116 Uiso 1 1 calc R . . H24B H 0.7426 -0.1770 0.4014 0.116 Uiso 1 1 calc R . . H24C H 0.7701 -0.0433 0.4441 0.116 Uiso 1 1 calc R . . C25 C 0.6077(5) -0.0694(4) 0.1901(3) 0.0530(9) Uani 1 1 d . . . C26 C 0.7102(6) -0.1368(5) 0.1185(3) 0.0708(13) Uani 1 1 d . . . H26A H 0.6439 -0.1952 0.0918 0.106 Uiso 1 1 calc R . . H26B H 0.8094 -0.1903 0.1411 0.106 Uiso 1 1 calc R . . H26C H 0.7428 -0.0679 0.0770 0.106 Uiso 1 1 calc R . . C27 C 0.5466(7) -0.1792(5) 0.2516(4) 0.0819(15) Uani 1 1 d . . . H27A H 0.4845 -0.1374 0.2986 0.123 Uiso 1 1 calc R . . H27B H 0.6417 -0.2399 0.2727 0.123 Uiso 1 1 calc R . . H27C H 0.4748 -0.2301 0.2224 0.123 Uiso 1 1 calc R . . C28 C 0.4498(5) 0.0156(5) 0.1547(3) 0.0583(10) Uani 1 1 d . . . H28A H 0.4808 0.0949 0.1218 0.087 Uiso 1 1 calc R . . H28B H 0.3745 0.0438 0.2013 0.087 Uiso 1 1 calc R . . H28C H 0.3945 -0.0384 0.1188 0.087 Uiso 1 1 calc R . . Li1 Li 0.7034(9) 0.3109(7) 0.2326(5) 0.0619(18) 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 Ga1 0.0447(2) 0.0298(2) 0.0442(2) -0.00382(14) 0.00751(15) -0.00446(14) N1* 0.0407(15) 0.0447(16) 0.0551(18) -0.0184(14) 0.0065(13) -0.0016(12) C1* 0.052(2) 0.0407(19) 0.063(2) -0.0113(17) 0.0128(17) -0.0072(15) C11* 0.057(2) 0.088(3) 0.063(3) -0.031(2) -0.006(2) 0.018(2) C12* 0.091(4) 0.123(5) 0.060(3) -0.019(3) -0.002(3) 0.025(4) C13* 0.060(3) 0.123(5) 0.106(4) -0.065(4) -0.010(3) -0.008(3) C14* 0.047(2) 0.053(2) 0.073(3) -0.027(2) 0.0016(18) 0.0012(16) C15* 0.060(3) 0.048(2) 0.110(4) -0.001(2) -0.001(3) 0.0009(19) C16* 0.045(2) 0.083(3) 0.083(3) -0.015(3) 0.017(2) 0.001(2) N1 0.0375(14) 0.0357(14) 0.0504(16) 0.0045(12) 0.0017(12) -0.0049(11) C1 0.0393(16) 0.0377(17) 0.053(2) 0.0004(15) 0.0049(14) -0.0033(13) C11 0.047(2) 0.057(2) 0.057(2) 0.0056(18) -0.0033(17) -0.0083(17) C12 0.076(3) 0.093(4) 0.058(3) -0.015(3) 0.001(2) -0.015(3) C13 0.058(3) 0.078(3) 0.088(3) 0.018(3) -0.019(2) -0.008(2) C14 0.0461(19) 0.0417(19) 0.067(2) 0.0083(17) -0.0001(17) -0.0115(15) C15 0.067(3) 0.045(2) 0.102(4) -0.011(2) 0.009(2) -0.0168(19) C16 0.044(2) 0.070(3) 0.072(3) 0.008(2) 0.0067(18) -0.0131(18) C21 0.064(2) 0.045(2) 0.048(2) 0.0040(16) 0.0046(17) -0.0002(17) C22 0.049(2) 0.063(3) 0.075(3) -0.018(2) -0.0166(19) 0.0089(18) C23 0.080(3) 0.050(2) 0.080(3) -0.003(2) -0.007(2) 0.017(2) C24 0.092(4) 0.077(3) 0.059(3) 0.019(2) 0.005(2) -0.006(3) C25 0.056(2) 0.0421(19) 0.063(2) -0.0128(17) 0.0064(18) -0.0134(16) C26 0.078(3) 0.061(3) 0.077(3) -0.033(2) 0.003(2) -0.009(2) C27 0.089(3) 0.053(3) 0.108(4) -0.003(3) 0.008(3) -0.035(2) C28 0.0425(19) 0.063(3) 0.074(3) -0.012(2) -0.0053(18) -0.0188(17) Li1 0.070(4) 0.048(4) 0.065(4) -0.010(3) 0.027(3) -0.006(3) _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 C21 2.056(4) . ? Ga1 C25 2.062(4) . ? Ga1 C1* 2.098(3) . ? Ga1 C1 2.099(3) . ? Ga1 Li1 2.691(7) . ? N1* C11* 1.475(5) . ? N1* C1* 1.495(5) . ? N1* C14* 1.499(4) . ? N1* Li1 1.937(7) . ? C11* C13* 1.525(8) . ? C11* C12* 1.530(7) . ? C14* C15* 1.500(7) . ? C14* C16* 1.536(6) . ? N1 C11 1.477(5) . ? N1 C14 1.495(4) . ? N1 C1 1.497(4) . ? N1 Li1 1.965(7) . ? C11 C13 1.515(6) . ? C11 C12 1.529(6) . ? C14 C15 1.523(6) . ? C14 C16 1.528(5) . ? C21 C23 1.534(6) . ? C21 C24 1.536(6) . ? C21 C22 1.546(6) . ? C25 C26 1.537(6) . ? C25 C27 1.544(6) . ? C25 C28 1.556(6) . ? 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 C21 Ga1 C25 114.48(17) . . ? C21 Ga1 C1* 116.34(16) . . ? C25 Ga1 C1* 100.72(16) . . ? C21 Ga1 C1 101.05(15) . . ? C25 Ga1 C1 117.11(16) . . ? C1* Ga1 C1 107.68(14) . . ? C21 Ga1 Li1 125.9(2) . . ? C25 Ga1 Li1 119.6(2) . . ? C1* Ga1 Li1 53.86(17) . . ? C1 Ga1 Li1 53.97(17) . . ? C11* N1* C1* 112.2(3) . . ? C11* N1* C14* 114.3(3) . . ? C1* N1* C14* 114.2(3) . . ? C11* N1* Li1 117.7(4) . . ? C1* N1* Li1 80.0(3) . . ? C14* N1* Li1 113.9(3) . . ? N1* C1* Ga1 122.8(2) . . ? N1* C11* C13* 111.0(5) . . ? N1* C11* C12* 116.2(4) . . ? C13* C11* C12* 110.2(4) . . ? N1* C14* C15* 109.0(3) . . ? N1* C14* C16* 116.2(4) . . ? C15* C14* C16* 109.9(4) . . ? C11 N1 C14 113.9(3) . . ? C11 N1 C1 112.1(3) . . ? C14 N1 C1 114.6(3) . . ? C11 N1 Li1 117.7(3) . . ? C14 N1 Li1 114.8(3) . . ? C1 N1 Li1 79.2(3) . . ? N1 C1 Ga1 121.7(2) . . ? N1 C11 C13 110.8(4) . . ? N1 C11 C12 115.6(3) . . ? C13 C11 C12 111.4(4) . . ? N1 C14 C15 109.0(3) . . ? N1 C14 C16 115.8(3) . . ? C15 C14 C16 110.0(4) . . ? C23 C21 C24 108.1(4) . . ? C23 C21 C22 106.5(4) . . ? C24 C21 C22 109.9(4) . . ? C23 C21 Ga1 110.2(3) . . ? C24 C21 Ga1 111.1(3) . . ? C22 C21 Ga1 111.0(3) . . ? C26 C25 C27 108.8(4) . . ? C26 C25 C28 109.8(4) . . ? C27 C25 C28 106.1(4) . . ? C26 C25 Ga1 111.2(3) . . ? C27 C25 Ga1 108.3(3) . . ? C28 C25 Ga1 112.5(3) . . ? N1* Li1 N1 167.9(4) . . ? N1* Li1 Ga1 84.7(3) . . ? N1 Li1 Ga1 83.7(2) . . ? 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 C11* N1* C1* Ga1 -71.2(4) . . . . ? C14* N1* C1* Ga1 156.6(3) . . . . ? Li1 N1* C1* Ga1 44.8(4) . . . . ? C21 Ga1 C1* N1* 78.5(4) . . . . ? C25 Ga1 C1* N1* -157.2(3) . . . . ? C1 Ga1 C1* N1* -34.0(4) . . . . ? Li1 Ga1 C1* N1* -38.2(3) . . . . ? C1* N1* C11* C13* 155.9(3) . . . . ? C14* N1* C11* C13* -72.0(5) . . . . ? Li1 N1* C11* C13* 65.7(4) . . . . ? C1* N1* C11* C12* -77.2(5) . . . . ? C14* N1* C11* C12* 54.9(6) . . . . ? Li1 N1* C11* C12* -167.3(4) . . . . ? C11* N1* C14* C15* 143.7(4) . . . . ? C1* N1* C14* C15* -85.2(4) . . . . ? Li1 N1* C14* C15* 4.3(5) . . . . ? C11* N1* C14* C16* -91.6(5) . . . . ? C1* N1* C14* C16* 39.6(5) . . . . ? Li1 N1* C14* C16* 129.1(4) . . . . ? C11 N1 C1 Ga1 -68.1(3) . . . . ? C14 N1 C1 Ga1 160.0(3) . . . . ? Li1 N1 C1 Ga1 47.5(3) . . . . ? C21 Ga1 C1 N1 -167.6(3) . . . . ? C25 Ga1 C1 N1 67.4(3) . . . . ? C1* Ga1 C1 N1 -45.1(3) . . . . ? Li1 Ga1 C1 N1 -40.9(3) . . . . ? C14 N1 C11 C13 -74.9(4) . . . . ? C1 N1 C11 C13 152.8(3) . . . . ? Li1 N1 C11 C13 63.7(4) . . . . ? C14 N1 C11 C12 53.0(5) . . . . ? C1 N1 C11 C12 -79.3(4) . . . . ? Li1 N1 C11 C12 -168.4(4) . . . . ? C11 N1 C14 C15 143.0(3) . . . . ? C1 N1 C14 C15 -86.0(4) . . . . ? Li1 N1 C14 C15 3.1(5) . . . . ? C11 N1 C14 C16 -92.4(4) . . . . ? C1 N1 C14 C16 38.6(5) . . . . ? Li1 N1 C14 C16 127.7(4) . . . . ? C25 Ga1 C21 C23 42.3(4) . . . . ? C1* Ga1 C21 C23 159.2(3) . . . . ? C1 Ga1 C21 C23 -84.5(3) . . . . ? Li1 Ga1 C21 C23 -137.8(3) . . . . ? C25 Ga1 C21 C24 -77.5(4) . . . . ? C1* Ga1 C21 C24 39.5(4) . . . . ? C1 Ga1 C21 C24 155.7(3) . . . . ? Li1 Ga1 C21 C24 102.5(4) . . . . ? C25 Ga1 C21 C22 159.9(3) . . . . ? C1* Ga1 C21 C22 -83.1(3) . . . . ? C1 Ga1 C21 C22 33.1(3) . . . . ? Li1 Ga1 C21 C22 -20.1(4) . . . . ? C21 Ga1 C25 C26 -75.0(3) . . . . ? C1* Ga1 C25 C26 159.4(3) . . . . ? C1 Ga1 C25 C26 43.0(4) . . . . ? Li1 Ga1 C25 C26 105.0(3) . . . . ? C21 Ga1 C25 C27 44.5(3) . . . . ? C1* Ga1 C25 C27 -81.2(3) . . . . ? C1 Ga1 C25 C27 162.5(3) . . . . ? Li1 Ga1 C25 C27 -135.5(3) . . . . ? C21 Ga1 C25 C28 161.4(3) . . . . ? C1* Ga1 C25 C28 35.8(3) . . . . ? C1 Ga1 C25 C28 -80.6(3) . . . . ? Li1 Ga1 C25 C28 -18.6(4) . . . . ? C11* N1* Li1 N1 66(2) . . . . ? C1* N1* Li1 N1 -44(2) . . . . ? C14* N1* Li1 N1 -156(2) . . . . ? C11* N1* Li1 Ga1 82.3(4) . . . . ? C1* N1* Li1 Ga1 -27.6(2) . . . . ? C14* N1* Li1 Ga1 -139.8(3) . . . . ? C11 N1 Li1 N1* 97(2) . . . . ? C14 N1 Li1 N1* -125(2) . . . . ? C1 N1 Li1 N1* -13(2) . . . . ? C11 N1 Li1 Ga1 79.9(3) . . . . ? C14 N1 Li1 Ga1 -141.8(2) . . . . ? C1 N1 Li1 Ga1 -29.5(2) . . . . ? C21 Ga1 Li1 N1* -74.8(3) . . . . ? C25 Ga1 Li1 N1* 105.1(3) . . . . ? C1* Ga1 Li1 N1* 23.8(2) . . . . ? C1 Ga1 Li1 N1* -151.3(4) . . . . ? C21 Ga1 Li1 N1 101.7(3) . . . . ? C25 Ga1 Li1 N1 -78.3(3) . . . . ? C1* Ga1 Li1 N1 -159.7(4) . . . . ? C1 Ga1 Li1 N1 25.26(19) . . . . ? _diffrn_measured_fraction_theta_max 0.975 _diffrn_reflns_theta_full 28.34 _diffrn_measured_fraction_theta_full 0.975 _refine_diff_density_max 1.037 _refine_diff_density_min -0.458 _refine_diff_density_rms 0.073 data_fro2690 _database_code_depnum_ccdc_archive 'CCDC 252363' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C15 H34 Al Cl Li N' _chemical_formula_weight 297.80 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' 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' Li Li -0.0003 0.0001 '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 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.658(1) _cell_length_b 10.199(1) _cell_length_c 13.383(1) _cell_angle_alpha 98.03(1) _cell_angle_beta 103.95(1) _cell_angle_gamma 102.73(1) _cell_volume 968.76(17) _cell_formula_units_Z 2 _cell_measurement_temperature 198(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.021 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 328 _exptl_absorpt_coefficient_mu 0.232 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.9443 _exptl_absorpt_correction_T_max 0.9885 _exptl_absorpt_process_details 'SORTAV (Blessing, 1995 & 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 198(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode Nonius FR591' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method '\w and \f scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9206 _diffrn_reflns_av_R_equivalents 0.0532 _diffrn_reflns_av_sigmaI/netI 0.0728 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.60 _diffrn_reflns_theta_max 26.30 _reflns_number_total 3940 _reflns_number_gt 2659 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius B.V., 1998)' _computing_cell_refinement 'Collect (Nonius B.V., 1998)' _computing_data_reduction 'Denzo-SMN (Otwinwoski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SCHAKAL (Keller, 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^)+(0.0514P)^2^+0.0819P] 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 riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3940 _refine_ls_number_parameters 182 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0841 _refine_ls_R_factor_gt 0.0467 _refine_ls_wR_factor_ref 0.1188 _refine_ls_wR_factor_gt 0.1039 _refine_ls_goodness_of_fit_ref 1.018 _refine_ls_restrained_S_all 1.018 _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 Li1 Li 0.6056(6) -0.0590(5) 0.5872(3) 0.0514(11) Uani 1 1 d . . . Al1 Al 0.68994(8) 0.23423(6) 0.73304(5) 0.02960(18) Uani 1 1 d . . . Cl1 Cl 0.42789(6) 0.10402(6) 0.59360(4) 0.03629(17) Uani 1 1 d . . . C1 C 0.8178(3) 0.0884(2) 0.77424(18) 0.0367(5) Uani 1 1 d . . . H1A H 0.9339 0.1052 0.7522 0.044 Uiso 1 1 calc R . . H1B H 0.8560 0.1052 0.8520 0.044 Uiso 1 1 calc R . . N1 N 0.7212(2) -0.06132(17) 0.73567(13) 0.0287(4) Uani 1 1 d . . . C11 C 0.5613(3) -0.1031(2) 0.78009(17) 0.0347(5) Uani 1 1 d . . . H11 H 0.4932 -0.0301 0.7745 0.042 Uiso 1 1 calc R . . C12 C 0.6109(3) -0.1130(3) 0.89544(19) 0.0553(7) Uani 1 1 d . . . H12A H 0.4980 -0.1267 0.9193 0.083 Uiso 1 1 calc R . . H12B H 0.7017 -0.0280 0.9374 0.083 Uiso 1 1 calc R . . H12C H 0.6650 -0.1908 0.9040 0.083 Uiso 1 1 calc R . . C13 C 0.4246(3) -0.2348(2) 0.7126(2) 0.0496(7) Uani 1 1 d . . . H13A H 0.3853 -0.2233 0.6398 0.074 Uiso 1 1 calc R . . H13B H 0.3153 -0.2561 0.7392 0.074 Uiso 1 1 calc R . . H13C H 0.4849 -0.3102 0.7151 0.074 Uiso 1 1 calc R . . C14 C 0.8505(3) -0.1530(2) 0.74603(17) 0.0351(5) Uani 1 1 d . . . H14 H 0.7742 -0.2471 0.7437 0.042 Uiso 1 1 calc R . . C15 C 0.9257(3) -0.1615(3) 0.6505(2) 0.0549(7) Uani 1 1 d . . . H15A H 0.8213 -0.1955 0.5863 0.082 Uiso 1 1 calc R . . H15B H 1.0060 -0.2244 0.6548 0.082 Uiso 1 1 calc R . . H15C H 0.9981 -0.0701 0.6489 0.082 Uiso 1 1 calc R . . C16 C 1.0124(3) -0.1141(3) 0.84654(19) 0.0470(6) Uani 1 1 d . . . H16A H 1.0998 -0.0279 0.8467 0.071 Uiso 1 1 calc R . . H16B H 1.0771 -0.1869 0.8496 0.071 Uiso 1 1 calc R . . H16C H 0.9642 -0.1025 0.9078 0.071 Uiso 1 1 calc R . . C21 C 0.8367(3) 0.3557(2) 0.65933(19) 0.0401(6) Uani 1 1 d . . . C22 C 0.9177(3) 0.2714(3) 0.5872(2) 0.0537(7) Uani 1 1 d . . . H22A H 0.9826 0.3315 0.5489 0.081 Uiso 1 1 calc R . . H22B H 0.8164 0.1986 0.5369 0.081 Uiso 1 1 calc R . . H22C H 1.0059 0.2303 0.6296 0.081 Uiso 1 1 calc R . . C23 C 1.0007(3) 0.4609(3) 0.7416(2) 0.0615(8) Uani 1 1 d . . . H23A H 1.0772 0.5171 0.7061 0.092 Uiso 1 1 calc R . . H23B H 1.0769 0.4128 0.7850 0.092 Uiso 1 1 calc R . . H23C H 0.9529 0.5201 0.7865 0.092 Uiso 1 1 calc R . . C24 C 0.7209(4) 0.4344(3) 0.5921(2) 0.0570(7) Uani 1 1 d . . . H24A H 0.6741 0.4939 0.6373 0.085 Uiso 1 1 calc R . . H24B H 0.6155 0.3688 0.5387 0.085 Uiso 1 1 calc R . . H24C H 0.7995 0.4905 0.5575 0.085 Uiso 1 1 calc R . . C25 C 0.5857(3) 0.3205(2) 0.84109(17) 0.0373(5) Uani 1 1 d . . . C26 C 0.7316(4) 0.3549(3) 0.9481(2) 0.0691(8) Uani 1 1 d . . . H26A H 0.6859 0.4028 1.0010 0.104 Uiso 1 1 calc R . . H26B H 0.8481 0.4141 0.9439 0.104 Uiso 1 1 calc R . . H26C H 0.7541 0.2700 0.9680 0.104 Uiso 1 1 calc R . . C27 C 0.5387(4) 0.4529(3) 0.8158(2) 0.0628(8) Uani 1 1 d . . . H27A H 0.4461 0.4321 0.7470 0.094 Uiso 1 1 calc R . . H27B H 0.6521 0.5188 0.8144 0.094 Uiso 1 1 calc R . . H27C H 0.4880 0.4925 0.8699 0.094 Uiso 1 1 calc R . . C28 C 0.4076(3) 0.2267(3) 0.8509(2) 0.0490(6) Uani 1 1 d . . . H28A H 0.4340 0.1429 0.8714 0.073 Uiso 1 1 calc R . . H28B H 0.3114 0.2025 0.7832 0.073 Uiso 1 1 calc R . . H28C H 0.3632 0.2745 0.9045 0.073 Uiso 1 1 calc R . . 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 Li1 0.064(2) 0.057(3) 0.033(2) 0.007(2) 0.0037(19) 0.029(2) Al1 0.0316(3) 0.0267(4) 0.0297(4) 0.0049(3) 0.0086(3) 0.0066(3) Cl1 0.0372(3) 0.0389(3) 0.0286(3) 0.0034(2) 0.0039(2) 0.0095(2) C1 0.0333(11) 0.0308(13) 0.0417(14) 0.0076(11) 0.0051(10) 0.0056(9) N1 0.0292(8) 0.0248(10) 0.0320(10) 0.0057(8) 0.0075(7) 0.0079(7) C11 0.0350(11) 0.0371(14) 0.0350(13) 0.0129(11) 0.0116(10) 0.0101(9) C12 0.0608(15) 0.074(2) 0.0396(16) 0.0263(14) 0.0206(12) 0.0187(13) C13 0.0373(12) 0.0405(15) 0.0653(19) 0.0128(13) 0.0077(12) 0.0046(10) C14 0.0351(11) 0.0341(13) 0.0380(14) 0.0100(11) 0.0073(10) 0.0149(9) C15 0.0586(15) 0.071(2) 0.0519(17) 0.0173(15) 0.0209(13) 0.0415(14) C16 0.0408(12) 0.0508(16) 0.0470(16) 0.0127(13) 0.0000(11) 0.0186(11) C21 0.0431(12) 0.0358(14) 0.0436(15) 0.0114(12) 0.0167(11) 0.0076(10) C22 0.0620(15) 0.0541(18) 0.0565(18) 0.0157(14) 0.0343(14) 0.0163(13) C23 0.0537(15) 0.0471(17) 0.075(2) 0.0080(15) 0.0227(14) -0.0073(12) C24 0.0780(17) 0.0455(17) 0.0594(19) 0.0256(15) 0.0312(15) 0.0185(13) C25 0.0434(12) 0.0357(14) 0.0321(13) 0.0028(11) 0.0120(10) 0.0099(10) C26 0.0616(16) 0.092(2) 0.0399(17) -0.0150(15) 0.0067(13) 0.0186(15) C27 0.0802(19) 0.0440(17) 0.085(2) 0.0154(16) 0.0489(17) 0.0287(14) C28 0.0559(14) 0.0514(17) 0.0475(16) 0.0091(13) 0.0276(12) 0.0166(12) _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 Li1 N1 1.977(4) . ? Li1 Cl1 2.339(4) 2_656 ? Li1 Cl1 2.374(4) . ? Li1 C1 2.661(5) . ? Li1 C11 2.768(5) . ? Li1 Li1 3.055(8) 2_656 ? Li1 Al1 3.175(4) . ? Al1 C25 2.003(2) . ? Al1 C21 2.009(2) . ? Al1 C1 2.021(2) . ? Al1 Cl1 2.3666(9) . ? Cl1 Li1 2.339(4) 2_656 ? C1 N1 1.498(3) . ? N1 C11 1.492(2) . ? N1 C14 1.500(2) . ? C11 C13 1.517(3) . ? C11 C12 1.522(3) . ? C14 C15 1.523(3) . ? C14 C16 1.528(3) . ? C21 C22 1.532(3) . ? C21 C23 1.533(3) . ? C21 C24 1.539(3) . ? C25 C26 1.529(3) . ? C25 C28 1.530(3) . ? C25 C27 1.533(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Li1 Cl1 154.6(2) . 2_656 ? N1 Li1 Cl1 105.24(19) . . ? Cl1 Li1 Cl1 99.19(14) 2_656 . ? N1 Li1 C1 33.78(9) . . ? Cl1 Li1 C1 145.7(2) 2_656 . ? Cl1 Li1 C1 85.04(14) . . ? N1 Li1 C11 31.38(9) . . ? Cl1 Li1 C11 158.9(2) 2_656 . ? Cl1 Li1 C11 88.41(14) . . ? C1 Li1 C11 54.11(10) . . ? N1 Li1 Li1 153.6(3) . 2_656 ? Cl1 Li1 Li1 50.10(12) 2_656 2_656 ? Cl1 Li1 Li1 49.09(11) . 2_656 ? C1 Li1 Li1 124.4(2) . 2_656 ? C11 Li1 Li1 133.8(2) . 2_656 ? N1 Li1 Al1 68.99(13) . . ? Cl1 Li1 Al1 126.28(17) 2_656 . ? Cl1 Li1 Al1 47.85(8) . . ? C1 Li1 Al1 39.30(8) . . ? C11 Li1 Al1 73.05(11) . . ? Li1 Li1 Al1 86.07(18) 2_656 . ? C25 Al1 C21 118.88(10) . . ? C25 Al1 C1 115.57(10) . . ? C21 Al1 C1 110.20(9) . . ? C25 Al1 Cl1 105.56(7) . . ? C21 Al1 Cl1 102.33(7) . . ? C1 Al1 Cl1 101.68(7) . . ? C25 Al1 Li1 136.93(10) . . ? C21 Al1 Li1 101.65(11) . . ? C1 Al1 Li1 56.48(9) . . ? Cl1 Al1 Li1 48.05(7) . . ? Li1 Cl1 Al1 129.31(11) 2_656 . ? Li1 Cl1 Li1 80.81(14) 2_656 . ? Al1 Cl1 Li1 84.09(11) . . ? N1 C1 Al1 121.47(13) . . ? N1 C1 Li1 47.21(13) . . ? Al1 C1 Li1 84.22(11) . . ? C11 N1 C1 111.47(16) . . ? C11 N1 C14 113.86(15) . . ? C1 N1 C14 114.02(15) . . ? C11 N1 Li1 105.00(17) . . ? C1 N1 Li1 99.01(18) . . ? C14 N1 Li1 112.15(17) . . ? N1 C11 C13 110.65(18) . . ? N1 C11 C12 116.30(17) . . ? C13 C11 C12 110.77(19) . . ? N1 C11 Li1 43.62(12) . . ? C13 C11 Li1 82.17(16) . . ? C12 C11 Li1 159.92(16) . . ? N1 C14 C15 108.69(17) . . ? N1 C14 C16 116.35(19) . . ? C15 C14 C16 109.71(18) . . ? C22 C21 C23 107.62(19) . . ? C22 C21 C24 107.8(2) . . ? C23 C21 C24 108.2(2) . . ? C22 C21 Al1 110.67(16) . . ? C23 C21 Al1 109.00(17) . . ? C24 C21 Al1 113.39(15) . . ? C26 C25 C28 107.65(19) . . ? C26 C25 C27 108.8(2) . . ? C28 C25 C27 107.02(18) . . ? C26 C25 Al1 108.51(15) . . ? C28 C25 Al1 113.26(16) . . ? C27 C25 Al1 111.44(15) . . ? 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 N1 Li1 Al1 C25 -72.33(18) . . . . ? Cl1 Li1 Al1 C25 130.95(17) 2_656 . . . ? Cl1 Li1 Al1 C25 64.34(15) . . . . ? C1 Li1 Al1 C25 -92.84(15) . . . . ? C11 Li1 Al1 C25 -39.36(16) . . . . ? Li1 Li1 Al1 C25 98.93(19) 2_656 . . . ? N1 Li1 Al1 C21 127.15(12) . . . . ? Cl1 Li1 Al1 C21 -29.6(2) 2_656 . . . ? Cl1 Li1 Al1 C21 -96.19(10) . . . . ? C1 Li1 Al1 C21 106.64(11) . . . . ? C11 Li1 Al1 C21 160.11(9) . . . . ? Li1 Li1 Al1 C21 -61.59(18) 2_656 . . . ? N1 Li1 Al1 C1 20.51(10) . . . . ? Cl1 Li1 Al1 C1 -136.2(2) 2_656 . . . ? Cl1 Li1 Al1 C1 157.17(14) . . . . ? C11 Li1 Al1 C1 53.48(10) . . . . ? Li1 Li1 Al1 C1 -168.2(2) 2_656 . . . ? N1 Li1 Al1 Cl1 -136.67(17) . . . . ? Cl1 Li1 Al1 Cl1 66.61(16) 2_656 . . . ? C1 Li1 Al1 Cl1 -157.17(14) . . . . ? C11 Li1 Al1 Cl1 -103.70(12) . . . . ? Li1 Li1 Al1 Cl1 34.60(10) 2_656 . . . ? C25 Al1 Cl1 Li1 146.71(15) . . . 2_656 ? C21 Al1 Cl1 Li1 21.67(15) . . . 2_656 ? C1 Al1 Cl1 Li1 -92.29(15) . . . 2_656 ? Li1 Al1 Cl1 Li1 -73.0(2) . . . 2_656 ? C25 Al1 Cl1 Li1 -140.28(12) . . . . ? C21 Al1 Cl1 Li1 94.68(13) . . . . ? C1 Al1 Cl1 Li1 -19.28(12) . . . . ? N1 Li1 Cl1 Li1 173.1(3) . . . 2_656 ? Cl1 Li1 Cl1 Li1 0.0 2_656 . . 2_656 ? C1 Li1 Cl1 Li1 145.7(2) . . . 2_656 ? C11 Li1 Cl1 Li1 -160.2(2) . . . 2_656 ? Al1 Li1 Cl1 Li1 131.45(14) . . . 2_656 ? N1 Li1 Cl1 Al1 41.61(17) . . . . ? Cl1 Li1 Cl1 Al1 -131.45(14) 2_656 . . . ? C1 Li1 Cl1 Al1 14.28(9) . . . . ? C11 Li1 Cl1 Al1 68.39(10) . . . . ? Li1 Li1 Cl1 Al1 -131.45(14) 2_656 . . . ? C25 Al1 C1 N1 100.47(18) . . . . ? C21 Al1 C1 N1 -121.23(17) . . . . ? Cl1 Al1 C1 N1 -13.27(17) . . . . ? Li1 Al1 C1 N1 -30.40(16) . . . . ? C25 Al1 C1 Li1 130.87(12) . . . . ? C21 Al1 C1 Li1 -90.83(13) . . . . ? Cl1 Al1 C1 Li1 17.14(11) . . . . ? Cl1 Li1 C1 N1 -133.8(4) 2_656 . . . ? Cl1 Li1 C1 N1 127.19(19) . . . . ? C11 Li1 C1 N1 35.56(12) . . . . ? Li1 Li1 C1 N1 158.3(3) 2_656 . . . ? Al1 Li1 C1 N1 143.97(17) . . . . ? N1 Li1 C1 Al1 -143.97(17) . . . . ? Cl1 Li1 C1 Al1 82.3(3) 2_656 . . . ? Cl1 Li1 C1 Al1 -16.78(11) . . . . ? C11 Li1 C1 Al1 -108.41(10) . . . . ? Li1 Li1 C1 Al1 14.3(3) 2_656 . . . ? Al1 C1 N1 C11 -66.8(2) . . . . ? Li1 C1 N1 C11 -110.12(19) . . . . ? Al1 C1 N1 C14 162.58(14) . . . . ? Li1 C1 N1 C14 119.3(2) . . . . ? Al1 C1 N1 Li1 43.3(2) . . . . ? Cl1 Li1 N1 C11 -136.3(5) 2_656 . . . ? Cl1 Li1 N1 C11 59.9(2) . . . . ? C1 Li1 N1 C11 115.22(18) . . . . ? Li1 Li1 N1 C11 71.8(7) 2_656 . . . ? Al1 Li1 N1 C11 91.71(13) . . . . ? Cl1 Li1 N1 C1 108.5(6) 2_656 . . . ? Cl1 Li1 N1 C1 -55.35(19) . . . . ? C11 Li1 N1 C1 -115.22(18) . . . . ? Li1 Li1 N1 C1 -43.5(7) 2_656 . . . ? Al1 Li1 N1 C1 -23.52(11) . . . . ? Cl1 Li1 N1 C14 -12.2(6) 2_656 . . . ? Cl1 Li1 N1 C14 -175.99(15) . . . . ? C1 Li1 N1 C14 -120.64(18) . . . . ? C11 Li1 N1 C14 124.1(2) . . . . ? Li1 Li1 N1 C14 -164.1(6) 2_656 . . . ? Al1 Li1 N1 C14 -144.16(13) . . . . ? C1 N1 C11 C13 158.91(17) . . . . ? C14 N1 C11 C13 -70.4(2) . . . . ? Li1 N1 C11 C13 52.7(2) . . . . ? C1 N1 C11 C12 -73.6(2) . . . . ? C14 N1 C11 C12 57.1(3) . . . . ? Li1 N1 C11 C12 -179.8(2) . . . . ? C1 N1 C11 Li1 106.2(2) . . . . ? C14 N1 C11 Li1 -123.0(2) . . . . ? Cl1 Li1 C11 N1 124.8(5) 2_656 . . . ? Cl1 Li1 C11 N1 -123.4(2) . . . . ? C1 Li1 C11 N1 -38.38(14) . . . . ? Li1 Li1 C11 N1 -144.2(4) 2_656 . . . ? Al1 Li1 C11 N1 -77.29(16) . . . . ? N1 Li1 C11 C13 -131.3(2) . . . . ? Cl1 Li1 C11 C13 -6.5(5) 2_656 . . . ? Cl1 Li1 C11 C13 105.28(16) . . . . ? C1 Li1 C11 C13 -169.70(16) . . . . ? Li1 Li1 C11 C13 84.5(4) 2_656 . . . ? Al1 Li1 C11 C13 151.39(14) . . . . ? N1 Li1 C11 C12 0.5(6) . . . . ? Cl1 Li1 C11 C12 125.3(6) 2_656 . . . ? Cl1 Li1 C11 C12 -122.9(5) . . . . ? C1 Li1 C11 C12 -37.9(6) . . . . ? Li1 Li1 C11 C12 -143.8(5) 2_656 . . . ? Al1 Li1 C11 C12 -76.8(6) . . . . ? C11 N1 C14 C15 145.97(19) . . . . ? C1 N1 C14 C15 -84.6(2) . . . . ? Li1 N1 C14 C15 26.9(3) . . . . ? C11 N1 C14 C16 -89.6(2) . . . . ? C1 N1 C14 C16 39.8(2) . . . . ? Li1 N1 C14 C16 151.3(2) . . . . ? C25 Al1 C21 C22 175.16(15) . . . . ? C1 Al1 C21 C22 38.42(19) . . . . ? Cl1 Al1 C21 C22 -69.11(17) . . . . ? Li1 Al1 C21 C22 -19.92(18) . . . . ? C25 Al1 C21 C23 56.98(19) . . . . ? C1 Al1 C21 C23 -79.75(18) . . . . ? Cl1 Al1 C21 C23 172.72(15) . . . . ? Li1 Al1 C21 C23 -138.09(17) . . . . ? C25 Al1 C21 C24 -63.6(2) . . . . ? C1 Al1 C21 C24 159.66(18) . . . . ? Cl1 Al1 C21 C24 52.13(19) . . . . ? Li1 Al1 C21 C24 101.32(19) . . . . ? C21 Al1 C25 C26 -89.23(19) . . . . ? C1 Al1 C25 C26 45.3(2) . . . . ? Cl1 Al1 C25 C26 156.77(16) . . . . ? Li1 Al1 C25 C26 112.7(2) . . . . ? C21 Al1 C25 C28 151.30(15) . . . . ? C1 Al1 C25 C28 -74.18(17) . . . . ? Cl1 Al1 C25 C28 37.30(16) . . . . ? Li1 Al1 C25 C28 -6.8(2) . . . . ? C21 Al1 C25 C27 30.6(2) . . . . ? C1 Al1 C25 C27 165.09(16) . . . . ? Cl1 Al1 C25 C27 -83.44(17) . . . . ? Li1 Al1 C25 C27 -127.53(18) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 26.30 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.235 _refine_diff_density_min -0.237 _refine_diff_density_rms 0.048