Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2001 data_global _journal_coden_Cambridge 186 loop_ _publ_author_name 'Armstrong, David R.' 'Davies, Robert P.' 'Linton, David J.' 'Schooler, Paul' 'Wheatley, Andrew' _publ_contact_author_name 'Dr Andrew Wheatley' _publ_contact_author_address ; Department of Chemistry University of Cambridge Lensfield Road Cambridge CB2 1EW UNITED KINGDOM ; _publ_contact_author_email AEHW2@CAM.AC.UK data_rs9831 _database_code_CSD 165070 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C26 H30 Al2 N4' _chemical_formula_weight 452.50 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' _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 8.198(4) _cell_length_b 8.531(4) _cell_length_c 9.462(6) _cell_angle_alpha 107.85(4) _cell_angle_beta 106.44(5) _cell_angle_gamma 94.05(4) _cell_volume 595.1(6) _cell_formula_units_Z 1 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.263 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 240 _exptl_absorpt_coefficient_mu 0.144 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.9515 _exptl_absorpt_correction_T_max 0.9582 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 180(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 3828 _diffrn_reflns_av_R_equivalents 0.0270 _diffrn_reflns_av_sigmaI/netI 0.0284 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 3.64 _diffrn_reflns_theta_max 25.00 _reflns_number_total 2095 _reflns_number_gt 1942 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^+0.9642P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2095 _refine_ls_number_parameters 145 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0397 _refine_ls_R_factor_gt 0.0367 _refine_ls_wR_factor_ref 0.1106 _refine_ls_wR_factor_gt 0.1060 _refine_ls_goodness_of_fit_ref 0.688 _refine_ls_restrained_S_all 0.688 _refine_ls_shift/su_max 0.068 _refine_ls_shift/su_mean 0.012 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 0.30206(6) 0.60691(6) 0.49002(6) 0.02112(18) Uani 1 1 d . . . N1 N 0.53202(18) 0.70351(17) 0.52793(16) 0.0218(3) Uani 1 1 d . . . C1 C 0.4089(2) 0.3337(2) 0.60209(19) 0.0215(4) Uani 1 1 d . . . N2 N 0.32769(18) 0.46651(17) 0.62770(16) 0.0210(3) Uani 1 1 d . . . C2 C 0.2692(2) 0.5076(2) 0.7523(2) 0.0282(4) Uani 1 1 d . . . H2A H 0.2127 0.6018 0.7706 0.034 Uiso 1 1 calc R . . C3 C 0.2881(3) 0.4193(2) 0.8531(2) 0.0319(4) Uani 1 1 d . . . H3A H 0.2439 0.4502 0.9385 0.038 Uiso 1 1 calc R . . C4 C 0.3728(3) 0.2845(3) 0.8277(2) 0.0342(5) Uani 1 1 d . . . H4A H 0.3887 0.2216 0.8963 0.041 Uiso 1 1 calc R . . C5 C 0.4339(3) 0.2419(2) 0.7024(2) 0.0305(4) Uani 1 1 d . . . H5A H 0.4931 0.1496 0.6845 0.037 Uiso 1 1 calc R . . C6 C 0.6322(2) 0.8405(2) 0.6588(2) 0.0217(4) Uani 1 1 d . . . C7 C 0.5917(2) 0.8808(2) 0.7984(2) 0.0259(4) Uani 1 1 d . . . H7A H 0.4947 0.8167 0.8026 0.031 Uiso 1 1 calc R . . C8 C 0.6901(3) 1.0121(2) 0.9302(2) 0.0321(4) Uani 1 1 d . . . H8A H 0.6599 1.0365 1.0235 0.038 Uiso 1 1 calc R . . C9 C 0.8317(3) 1.1084(2) 0.9287(2) 0.0368(5) Uani 1 1 d . . . H9A H 0.8983 1.1995 1.0192 0.044 Uiso 1 1 calc R . . C10 C 0.8739(3) 1.0691(2) 0.7925(2) 0.0358(5) Uani 1 1 d . . . H10A H 0.9716 1.1335 0.7899 0.043 Uiso 1 1 calc R . . C11 C 0.7773(2) 0.9380(2) 0.6598(2) 0.0278(4) Uani 1 1 d . . . H11A H 0.8098 0.9137 0.5677 0.033 Uiso 1 1 calc R . . C12 C 0.1611(3) 0.7688(2) 0.5681(2) 0.0319(4) Uani 1 1 d . . . H12A H 0.1421 0.8436 0.5067 0.048 Uiso 1 1 calc R . . H12B H 0.2214 0.8345 0.6786 0.048 Uiso 1 1 calc R . . H12C H 0.0496 0.7089 0.5580 0.048 Uiso 1 1 calc R . . C13 C 0.1957(2) 0.4769(2) 0.2669(2) 0.0302(4) Uani 1 1 d . . . H13A H 0.1862 0.5521 0.2058 0.045 Uiso 1 1 calc R . . H13B H 0.0804 0.4189 0.2491 0.045 Uiso 1 1 calc R . . H13C H 0.2673 0.3947 0.2340 0.045 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 Al1 0.0231(3) 0.0201(3) 0.0201(3) 0.0054(2) 0.0086(2) 0.0031(2) N1 0.0259(7) 0.0192(7) 0.0198(7) 0.0037(6) 0.0104(6) 0.0017(6) C1 0.0216(8) 0.0198(8) 0.0205(8) 0.0039(7) 0.0069(7) -0.0005(6) N2 0.0227(7) 0.0208(7) 0.0191(7) 0.0049(6) 0.0087(6) 0.0016(6) C2 0.0316(9) 0.0290(9) 0.0261(9) 0.0066(7) 0.0152(8) 0.0064(7) C3 0.0373(10) 0.0380(10) 0.0230(9) 0.0093(8) 0.0157(8) 0.0030(8) C4 0.0430(11) 0.0381(11) 0.0287(10) 0.0185(8) 0.0149(9) 0.0067(9) C5 0.0379(10) 0.0279(9) 0.0313(10) 0.0137(8) 0.0148(8) 0.0093(8) C6 0.0241(8) 0.0175(8) 0.0228(8) 0.0059(7) 0.0069(7) 0.0063(6) C7 0.0293(9) 0.0237(9) 0.0238(9) 0.0062(7) 0.0096(7) 0.0032(7) C8 0.0386(10) 0.0302(10) 0.0228(9) 0.0031(8) 0.0093(8) 0.0061(8) C9 0.0368(11) 0.0297(10) 0.0288(10) -0.0018(8) 0.0022(8) -0.0012(8) C10 0.0303(10) 0.0302(10) 0.0400(11) 0.0062(8) 0.0092(8) -0.0041(8) C11 0.0288(9) 0.0254(9) 0.0290(9) 0.0068(7) 0.0120(7) 0.0029(7) C12 0.0355(10) 0.0309(10) 0.0342(10) 0.0120(8) 0.0163(8) 0.0118(8) C13 0.0321(10) 0.0296(9) 0.0246(9) 0.0068(7) 0.0051(7) 0.0046(8) _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 N1 1.8916(18) . ? Al1 C13 1.958(2) . ? Al1 C12 1.968(2) . ? Al1 N2 2.0033(18) . ? N1 C1 1.403(2) 2_666 ? N1 C6 1.406(2) . ? C1 N2 1.347(2) . ? C1 C5 1.388(3) . ? C1 N1 1.403(2) 2_666 ? N2 C2 1.354(2) . ? C2 C3 1.369(3) . ? C3 C4 1.378(3) . ? C4 C5 1.373(3) . ? C6 C7 1.400(3) . ? C6 C11 1.399(3) . ? C7 C8 1.381(3) . ? C8 C9 1.380(3) . ? C9 C10 1.377(3) . ? C10 C11 1.380(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 Al1 C13 109.66(9) . . ? N1 Al1 C12 113.89(9) . . ? C13 Al1 C12 112.16(10) . . ? N1 Al1 N2 103.59(8) . . ? C13 Al1 N2 113.25(9) . . ? C12 Al1 N2 103.95(8) . . ? C1 N1 C6 115.26(14) 2_666 . ? C1 N1 Al1 116.32(12) 2_666 . ? C6 N1 Al1 126.10(12) . . ? N2 C1 C5 120.67(16) . . ? N2 C1 N1 116.67(15) . 2_666 ? C5 C1 N1 122.65(16) . 2_666 ? C1 N2 C2 118.73(15) . . ? C1 N2 Al1 120.91(12) . . ? C2 N2 Al1 120.31(12) . . ? N2 C2 C3 122.80(17) . . ? C2 C3 C4 118.41(17) . . ? C5 C4 C3 119.51(18) . . ? C4 C5 C1 119.87(17) . . ? C7 C6 C11 116.99(17) . . ? C7 C6 N1 119.80(16) . . ? C11 C6 N1 123.17(16) . . ? C8 C7 C6 121.18(17) . . ? C9 C8 C7 121.13(18) . . ? C8 C9 C10 118.24(18) . . ? C9 C10 C11 121.46(18) . . ? C10 C11 C6 121.00(18) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.414 _refine_diff_density_min -0.350 _refine_diff_density_rms 0.051 data_rs0024 _database_code_CSD 165071 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common rs0024 _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C19 H33 Al Li N3 Si2' _chemical_formula_weight 393.58 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' 'Si' 'Si' 0.0817 0.0704 '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 Monoclinic _symmetry_space_group_name_H-M P2(1)/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 13.8140(4) _cell_length_b 17.6740(5) _cell_length_c 19.7500(5) _cell_angle_alpha 90.00 _cell_angle_beta 99.5570(18) _cell_angle_gamma 90.00 _cell_volume 4755.0(2) _cell_formula_units_Z 8 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 24634 _cell_measurement_theta_min 2.910 _cell_measurement_theta_max 25.028 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.29 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.100 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1696 _exptl_absorpt_coefficient_mu 0.193 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.9461 _exptl_absorpt_correction_T_max 0.9753 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 180(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16045 _diffrn_reflns_av_R_equivalents 0.0379 _diffrn_reflns_av_sigmaI/netI 0.0535 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 3.00 _diffrn_reflns_theta_max 25.03 _reflns_number_total 8324 _reflns_number_gt 6217 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 19' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0840P)^2^+2.7025P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8324 _refine_ls_number_parameters 485 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0792 _refine_ls_R_factor_gt 0.0543 _refine_ls_wR_factor_ref 0.1662 _refine_ls_wR_factor_gt 0.1480 _refine_ls_goodness_of_fit_ref 1.063 _refine_ls_restrained_S_all 1.063 _refine_ls_shift/su_max 0.614 _refine_ls_shift/su_mean 0.007 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 0.25061(6) -0.08271(5) 0.22818(4) 0.0342(2) Uani 1 1 d . . . Li1 Li 0.4623(3) -0.1059(3) 0.2291(3) 0.0468(12) Uani 1 1 d . . . Si1 Si 0.32629(6) -0.24825(5) 0.22050(4) 0.0406(2) Uani 1 1 d . . . N1 N 0.33198(16) -0.15505(13) 0.19049(11) 0.0332(5) Uani 1 1 d . . . C1 C 0.3073(3) -0.24941(19) 0.31240(17) 0.0534(8) Uani 1 1 d . . . H1A H 0.2434 -0.2269 0.3158 0.080 Uiso 1 1 calc R . . H1B H 0.3595 -0.2201 0.3404 0.080 Uiso 1 1 calc R . . H1C H 0.3092 -0.3017 0.3290 0.080 Uiso 1 1 calc R . . Al2 Al -0.25041(6) -0.18549(5) 0.20192(4) 0.0343(2) Uani 1 1 d . . . Li2 Li -0.0430(3) -0.1659(3) 0.2062(3) 0.0496(13) Uani 1 1 d . . . Si2 Si 0.33271(7) -0.14275(5) 0.10248(4) 0.0472(2) Uani 1 1 d . . . N2 N 0.30164(17) -0.06000(14) 0.32256(12) 0.0370(5) Uani 1 1 d . . . C2 C 0.4433(3) -0.3030(2) 0.2222(2) 0.0605(9) Uani 1 1 d . . . H2A H 0.4575 -0.3077 0.1754 0.091 Uiso 1 1 calc R . . H2B H 0.4360 -0.3535 0.2413 0.091 Uiso 1 1 calc R . . H2C H 0.4973 -0.2763 0.2509 0.091 Uiso 1 1 calc R . . Si3 Si -0.16583(6) -0.15172(5) 0.06879(4) 0.0447(2) Uani 1 1 d . . . N3 N 0.45549(17) -0.02871(14) 0.29929(13) 0.0418(6) Uani 1 1 d . . . C3 C 0.2272(2) -0.30498(19) 0.16745(19) 0.0549(9) Uani 1 1 d . . . H3A H 0.1661 -0.2757 0.1600 0.082 Uiso 1 1 calc R . . H3B H 0.2171 -0.3521 0.1915 0.082 Uiso 1 1 calc R . . H3C H 0.2464 -0.3168 0.1231 0.082 Uiso 1 1 calc R . . Si4 Si -0.17420(6) -0.02525(5) 0.16934(5) 0.0468(2) Uani 1 1 d . . . N4 N -0.16939(15) -0.12249(13) 0.15295(12) 0.0348(5) Uani 1 1 d . . . C4 C 0.2058(3) -0.1366(2) 0.05127(17) 0.0642(10) Uani 1 1 d . . . H4A H 0.1693 -0.1828 0.0581 0.096 Uiso 1 1 calc R . . H4B H 0.2100 -0.1312 0.0025 0.096 Uiso 1 1 calc R . . H4C H 0.1717 -0.0928 0.0665 0.096 Uiso 1 1 calc R . . N5 N -0.19061(18) -0.19758(15) 0.29696(13) 0.0451(6) Uani 1 1 d . . . C5 C 0.3985(3) -0.2210(3) 0.0645(2) 0.0744(12) Uani 1 1 d . . . H5A H 0.3621 -0.2684 0.0660 0.112 Uiso 1 1 calc R . . H5B H 0.4647 -0.2267 0.0909 0.112 Uiso 1 1 calc R . . H5C H 0.4029 -0.2087 0.0167 0.112 Uiso 1 1 calc R . . N6 N -0.05753(19) -0.25555(15) 0.26401(15) 0.0499(7) Uani 1 1 d . . . C6 C 0.4017(3) -0.0539(2) 0.08730(18) 0.0605(10) Uani 1 1 d . . . H6A H 0.3652 -0.0096 0.0991 0.091 Uiso 1 1 calc R . . H6B H 0.4091 -0.0512 0.0389 0.091 Uiso 1 1 calc R . . H6C H 0.4667 -0.0548 0.1161 0.091 Uiso 1 1 calc R . . C7 C 0.3897(2) -0.02464(16) 0.34299(15) 0.0362(6) Uani 1 1 d . . . C8 C 0.4137(2) 0.01675(18) 0.40444(16) 0.0475(8) Uani 1 1 d . . . H8A H 0.3680 0.0196 0.4354 0.057 Uiso 1 1 calc R . . C9 C 0.5019(3) 0.0527(2) 0.41985(18) 0.0575(9) Uani 1 1 d . . . H9A H 0.5183 0.0794 0.4620 0.069 Uiso 1 1 calc R . . C10 C 0.5673(3) 0.0504(2) 0.3743(2) 0.0604(10) Uani 1 1 d . . . H10A H 0.6286 0.0759 0.3835 0.073 Uiso 1 1 calc R . . C11 C 0.5407(2) 0.01013(19) 0.31583(19) 0.0540(9) Uani 1 1 d . . . H11A H 0.5852 0.0090 0.2840 0.065 Uiso 1 1 calc R . . C12 C 0.2338(2) -0.05874(18) 0.37015(15) 0.0428(7) Uani 1 1 d . . . C13 C 0.2462(3) -0.1077(2) 0.42570(19) 0.0701(11) Uani 1 1 d . . . H13A H 0.3013 -0.1406 0.4340 0.084 Uiso 1 1 calc R . . C14 C 0.1756(5) -0.1080(3) 0.4695(3) 0.1072(19) Uani 1 1 d . . . H14A H 0.1824 -0.1425 0.5069 0.129 Uiso 1 1 calc R . . C15 C 0.0985(4) -0.0602(3) 0.4595(3) 0.1042(18) Uani 1 1 d . . . H15A H 0.0520 -0.0611 0.4899 0.125 Uiso 1 1 calc R . . C16 C 0.0868(3) -0.0100(3) 0.4053(2) 0.0851(14) Uani 1 1 d . . . H16A H 0.0323 0.0235 0.3980 0.102 Uiso 1 1 calc R . . C17 C 0.1560(2) -0.0089(2) 0.36100(18) 0.0553(9) Uani 1 1 d . . . H17A H 0.1493 0.0265 0.3243 0.066 Uiso 1 1 calc R . . C18 C 0.2379(2) 0.01659(18) 0.18191(18) 0.0498(8) Uani 1 1 d . . . H18A H 0.1828 0.0444 0.1954 0.075 Uiso 1 1 calc R . . H18B H 0.2261 0.0092 0.1321 0.075 Uiso 1 1 calc R . . H18C H 0.2986 0.0455 0.1953 0.075 Uiso 1 1 calc R . . C19 C 0.1165(2) -0.12724(18) 0.22402(17) 0.0435(7) Uani 1 1 d . . . H19A H 0.0742 -0.0910 0.2428 0.065 Uiso 1 1 calc R . . H19B H 0.1211 -0.1740 0.2511 0.065 Uiso 1 1 calc R . . H19C H 0.0886 -0.1385 0.1762 0.065 Uiso 1 1 calc R . . C20 C -0.0899(3) -0.2397(2) 0.07064(18) 0.0566(9) Uani 1 1 d . . . H20A H -0.1146 -0.2778 0.0995 0.085 Uiso 1 1 calc R . . H20B H -0.0214 -0.2279 0.0895 0.085 Uiso 1 1 calc R . . H20C H -0.0939 -0.2595 0.0239 0.085 Uiso 1 1 calc R . . C21 C -0.1041(3) -0.0841(2) 0.0163(2) 0.0727(11) Uani 1 1 d . . . H21A H -0.1404 -0.0362 0.0113 0.109 Uiso 1 1 calc R . . H21B H -0.1029 -0.1059 -0.0291 0.109 Uiso 1 1 calc R . . H21C H -0.0367 -0.0748 0.0394 0.109 Uiso 1 1 calc R . . C22 C -0.2917(3) -0.1671(2) 0.0182(2) 0.0675(10) Uani 1 1 d . . . H22A H -0.3254 -0.1184 0.0100 0.101 Uiso 1 1 calc R . . H22B H -0.3292 -0.2003 0.0440 0.101 Uiso 1 1 calc R . . H22C H -0.2861 -0.1908 -0.0259 0.101 Uiso 1 1 calc R . . C23 C -0.2839(3) 0.0214(2) 0.1178(2) 0.0697(11) Uani 1 1 d . . . H23A H -0.3438 -0.0022 0.1284 0.105 Uiso 1 1 calc R . . H23B H -0.2815 0.0154 0.0687 0.105 Uiso 1 1 calc R . . H23C H -0.2838 0.0753 0.1292 0.105 Uiso 1 1 calc R . . C24 C -0.1748(3) -0.0089(2) 0.2624(2) 0.0676(10) Uani 1 1 d . . . H24A H -0.2349 -0.0301 0.2750 0.101 Uiso 1 1 calc R . . H24B H -0.1724 0.0456 0.2718 0.101 Uiso 1 1 calc R . . H24C H -0.1175 -0.0334 0.2895 0.101 Uiso 1 1 calc R . . C25 C -0.0643(3) 0.0294(2) 0.1514(3) 0.0770(12) Uani 1 1 d . . . H25A H -0.0041 0.0033 0.1721 0.116 Uiso 1 1 calc R . . H25B H -0.0651 0.0803 0.1710 0.116 Uiso 1 1 calc R . . H25C H -0.0663 0.0332 0.1016 0.116 Uiso 1 1 calc R . . C26 C -0.1134(2) -0.24619(17) 0.31518(16) 0.0395(7) Uani 1 1 d . . . C27 C -0.0910(3) -0.2861(2) 0.37567(18) 0.0587(9) Uani 1 1 d . . . H27A H -0.1288 -0.2783 0.4111 0.070 Uiso 1 1 calc R . . C28 C -0.0159(3) -0.3360(2) 0.3854(2) 0.0685(11) Uani 1 1 d . . . H28A H -0.0008 -0.3628 0.4276 0.082 Uiso 1 1 calc R . . C29 C 0.0387(3) -0.3482(2) 0.3341(2) 0.0758(12) Uani 1 1 d . . . H29A H 0.0908 -0.3839 0.3396 0.091 Uiso 1 1 calc R . . C30 C 0.0157(3) -0.3073(2) 0.2754(2) 0.0640(10) Uani 1 1 d . . . H30A H 0.0534 -0.3155 0.2400 0.077 Uiso 1 1 calc R . . C31 C -0.2472(3) -0.1860(2) 0.35147(16) 0.0537(9) Uani 1 1 d . . . C32 C -0.3264(3) -0.2319(3) 0.35654(19) 0.0665(11) Uani 1 1 d . . . H32A H -0.3429 -0.2717 0.3244 0.080 Uiso 1 1 calc R . . C33 C -0.3827(4) -0.2206(3) 0.4082(2) 0.0921(16) Uani 1 1 d . . . H33A H -0.4374 -0.2522 0.4113 0.110 Uiso 1 1 calc R . . C34 C -0.3572(5) -0.1622(4) 0.4550(3) 0.1037(19) Uani 1 1 d . . . H34A H -0.3953 -0.1532 0.4901 0.124 Uiso 1 1 calc R . . C35 C -0.2780(5) -0.1180(3) 0.4506(2) 0.1004(18) Uani 1 1 d . . . H35A H -0.2603 -0.0791 0.4835 0.121 Uiso 1 1 calc R . . C36 C -0.2227(4) -0.1289(3) 0.3991(2) 0.0783(12) Uani 1 1 d . . . H36A H -0.1679 -0.0972 0.3965 0.094 Uiso 1 1 calc R . . C37 C -0.3798(2) -0.13694(18) 0.20674(16) 0.0440(7) Uani 1 1 d . . . H37A H -0.4273 -0.1512 0.1662 0.066 Uiso 1 1 calc R . . H37B H -0.3720 -0.0818 0.2080 0.066 Uiso 1 1 calc R . . H37C H -0.4034 -0.1540 0.2483 0.066 Uiso 1 1 calc R . . C38 C -0.2765(2) -0.28919(18) 0.16574(18) 0.0497(8) Uani 1 1 d . . . H38A H -0.3306 -0.3114 0.1854 0.075 Uiso 1 1 calc R . . H38B H -0.2174 -0.3202 0.1782 0.075 Uiso 1 1 calc R . . H38C H -0.2944 -0.2873 0.1156 0.075 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 Al1 0.0289(4) 0.0347(5) 0.0378(5) 0.0037(4) 0.0015(4) -0.0018(3) Li1 0.030(2) 0.058(3) 0.053(3) -0.014(3) 0.010(2) -0.003(2) Si1 0.0396(4) 0.0348(5) 0.0461(5) -0.0002(4) 0.0037(4) -0.0012(4) N1 0.0318(12) 0.0354(13) 0.0316(12) 0.0004(10) 0.0030(10) -0.0026(10) C1 0.063(2) 0.0437(19) 0.052(2) 0.0134(16) 0.0049(17) 0.0017(16) Al2 0.0277(4) 0.0338(5) 0.0394(5) 0.0006(4) -0.0004(4) 0.0007(3) Li2 0.029(2) 0.054(3) 0.063(3) 0.020(3) 0.000(2) -0.002(2) Si2 0.0497(5) 0.0576(6) 0.0328(4) -0.0018(4) 0.0031(4) -0.0097(4) N2 0.0349(13) 0.0409(14) 0.0361(13) -0.0029(11) 0.0085(10) -0.0002(11) C2 0.051(2) 0.047(2) 0.083(3) 0.0038(19) 0.0091(19) 0.0076(16) Si3 0.0402(5) 0.0495(5) 0.0423(5) 0.0067(4) 0.0008(4) 0.0014(4) N3 0.0331(13) 0.0449(15) 0.0479(15) -0.0091(12) 0.0082(11) -0.0029(11) C3 0.0514(19) 0.0423(19) 0.070(2) -0.0063(17) 0.0053(17) -0.0102(15) Si4 0.0384(5) 0.0314(5) 0.0676(6) 0.0031(4) 0.0000(4) 0.0003(3) N4 0.0262(11) 0.0323(13) 0.0439(14) 0.0039(11) -0.0001(10) -0.0002(9) C4 0.066(2) 0.080(3) 0.0399(18) 0.0087(18) -0.0102(17) -0.019(2) N5 0.0416(14) 0.0501(16) 0.0426(14) -0.0015(12) 0.0037(12) 0.0093(12) C5 0.087(3) 0.089(3) 0.051(2) -0.022(2) 0.022(2) -0.008(2) N6 0.0408(14) 0.0472(16) 0.0638(18) 0.0104(13) 0.0150(13) 0.0035(12) C6 0.062(2) 0.073(3) 0.0462(19) 0.0150(18) 0.0096(17) -0.0127(19) C7 0.0354(15) 0.0345(16) 0.0370(15) 0.0006(13) 0.0006(12) 0.0064(12) C8 0.0514(19) 0.0504(19) 0.0399(17) -0.0080(15) 0.0054(15) 0.0039(15) C9 0.061(2) 0.054(2) 0.052(2) -0.0188(17) -0.0083(17) -0.0010(17) C10 0.0460(19) 0.055(2) 0.078(3) -0.018(2) 0.0045(18) -0.0082(16) C11 0.0403(17) 0.053(2) 0.070(2) -0.0174(18) 0.0124(16) -0.0054(15) C12 0.0451(17) 0.0450(18) 0.0400(17) -0.0023(14) 0.0124(14) -0.0024(14) C13 0.094(3) 0.067(3) 0.056(2) 0.014(2) 0.032(2) 0.016(2) C14 0.169(5) 0.087(4) 0.087(3) 0.026(3) 0.085(4) 0.017(4) C15 0.116(4) 0.113(4) 0.106(4) -0.006(3) 0.082(4) 0.000(3) C16 0.070(3) 0.107(4) 0.089(3) -0.012(3) 0.044(2) 0.015(3) C17 0.0488(19) 0.062(2) 0.058(2) 0.0007(18) 0.0177(17) 0.0107(17) C18 0.0479(18) 0.0431(18) 0.056(2) 0.0109(16) 0.0033(15) -0.0028(15) C19 0.0304(15) 0.0437(18) 0.0554(19) 0.0019(15) 0.0044(14) -0.0025(13) C20 0.058(2) 0.062(2) 0.052(2) -0.0027(17) 0.0157(17) 0.0089(17) C21 0.078(3) 0.077(3) 0.064(2) 0.022(2) 0.014(2) -0.003(2) C22 0.054(2) 0.080(3) 0.059(2) 0.000(2) -0.0168(18) -0.0013(19) C23 0.054(2) 0.046(2) 0.105(3) 0.020(2) 0.002(2) 0.0114(17) C24 0.078(3) 0.047(2) 0.075(3) -0.0184(19) 0.002(2) -0.0041(19) C25 0.055(2) 0.046(2) 0.128(4) 0.006(2) 0.008(2) -0.0111(17) C26 0.0253(14) 0.0382(16) 0.0523(18) 0.0029(14) -0.0020(13) -0.0011(12) C27 0.051(2) 0.073(2) 0.051(2) 0.0088(18) 0.0035(16) 0.0120(18) C28 0.053(2) 0.079(3) 0.071(3) 0.024(2) 0.0037(19) 0.016(2) C29 0.054(2) 0.072(3) 0.105(3) 0.035(2) 0.025(2) 0.023(2) C30 0.0475(19) 0.059(2) 0.090(3) 0.020(2) 0.0267(19) 0.0174(17) C31 0.056(2) 0.064(2) 0.0407(18) 0.0004(17) 0.0060(16) 0.0190(18) C32 0.056(2) 0.092(3) 0.054(2) 0.007(2) 0.0171(18) 0.005(2) C33 0.082(3) 0.132(4) 0.068(3) 0.034(3) 0.028(2) 0.030(3) C34 0.121(5) 0.127(5) 0.074(3) 0.008(3) 0.048(3) 0.057(4) C35 0.148(5) 0.097(4) 0.062(3) -0.007(3) 0.034(3) 0.044(4) C36 0.108(3) 0.069(3) 0.059(2) -0.012(2) 0.016(2) 0.016(2) C37 0.0337(15) 0.0481(19) 0.0503(18) -0.0011(15) 0.0074(14) -0.0004(13) C38 0.0475(18) 0.0390(17) 0.063(2) -0.0044(16) 0.0116(16) -0.0076(14) _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 N2 1.922(2) . ? Al1 N1 1.931(2) . ? Al1 C18 1.973(3) . ? Al1 C19 2.002(3) . ? Al1 Li1 2.950(5) . ? Li1 N3 1.959(6) . ? Li1 N1 2.030(5) . ? Li1 C37 2.361(5) 1_655 ? Li1 C11 2.775(6) . ? Li1 Si2 2.897(5) . ? Li1 Si1 3.128(5) . ? Si1 N1 1.757(2) . ? Si1 C3 1.871(3) . ? Si1 C2 1.879(3) . ? Si1 C1 1.876(3) . ? N1 Si2 1.753(2) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? Al2 N5 1.933(3) . ? Al2 N4 1.946(2) . ? Al2 C38 1.978(3) . ? Al2 C37 1.999(3) . ? Al2 Li2 2.873(5) . ? Li2 N6 1.983(6) . ? Li2 N4 2.033(5) . ? Li2 Si3 2.962(5) . ? Li2 Si4 3.092(5) . ? Si2 C5 1.878(4) . ? Si2 C4 1.876(4) . ? Si2 C6 1.887(4) . ? N2 C7 1.368(4) . ? N2 C12 1.434(4) . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? Si3 N4 1.749(2) . ? Si3 C20 1.873(3) . ? Si3 C22 1.876(3) . ? Si3 C21 1.877(4) . ? N3 C7 1.355(4) . ? N3 C11 1.355(4) . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? Si4 N4 1.752(2) . ? Si4 C24 1.862(4) . ? Si4 C23 1.871(4) . ? Si4 C25 1.883(4) . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? N5 C26 1.370(4) . ? N5 C31 1.447(4) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? N6 C30 1.354(4) . ? N6 C26 1.380(4) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 C8 1.408(4) . ? C8 C9 1.364(5) . ? C8 H8A 0.9500 . ? C9 C10 1.378(5) . ? C9 H9A 0.9500 . ? C10 C11 1.354(5) . ? C10 H10A 0.9500 . ? C11 H11A 0.9500 . ? C12 C17 1.378(5) . ? C12 C13 1.386(5) . ? C13 C14 1.407(5) . ? C13 H13A 0.9500 . ? C14 C15 1.348(7) . ? C14 H14A 0.9500 . ? C15 C16 1.379(7) . ? C15 H15A 0.9500 . ? C16 C17 1.398(5) . ? C16 H16A 0.9500 . ? C17 H17A 0.9500 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 C27 1.377(4) . ? C27 C28 1.351(5) . ? C27 H27A 0.9500 . ? C28 C29 1.377(5) . ? C28 H28A 0.9500 . ? C29 C30 1.358(5) . ? C29 H29A 0.9500 . ? C30 H30A 0.9500 . ? C31 C32 1.379(5) . ? C31 C36 1.382(5) . ? C32 C33 1.396(5) . ? C32 H32A 0.9500 . ? C33 C34 1.391(8) . ? C33 H33A 0.9500 . ? C34 C35 1.359(8) . ? C34 H34A 0.9500 . ? C35 C36 1.383(6) . ? C35 H35A 0.9500 . ? C36 H36A 0.9500 . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Al1 N1 111.63(10) . . ? N2 Al1 C18 104.68(13) . . ? N1 Al1 C18 115.01(12) . . ? N2 Al1 C19 108.05(12) . . ? N1 Al1 C19 108.53(12) . . ? C18 Al1 C19 108.69(14) . . ? N2 Al1 Li1 79.61(12) . . ? N1 Al1 Li1 43.16(12) . . ? C18 Al1 Li1 97.92(15) . . ? C19 Al1 Li1 148.80(15) . . ? N3 Li1 N1 114.8(2) . . ? N3 Li1 C37 116.6(2) . 1_655 ? N1 Li1 C37 128.3(3) . 1_655 ? N3 Li1 C11 26.84(12) . . ? N1 Li1 C11 141.2(2) . . ? C37 Li1 C11 90.50(19) 1_655 . ? N3 Li1 Si2 132.2(2) . . ? N1 Li1 Si2 36.63(11) . . ? C37 Li1 Si2 104.14(19) 1_655 . ? C11 Li1 Si2 145.2(2) . . ? N3 Li1 Al1 75.13(16) . . ? N1 Li1 Al1 40.61(11) . . ? C37 Li1 Al1 167.7(2) 1_655 . ? C11 Li1 Al1 100.73(17) . . ? Si2 Li1 Al1 63.66(10) . . ? N3 Li1 Si1 120.0(2) . . ? N1 Li1 Si1 31.58(11) . . ? C37 Li1 Si1 111.6(2) 1_655 . ? C11 Li1 Si1 142.9(2) . . ? Si2 Li1 Si1 59.53(10) . . ? Al1 Li1 Si1 61.67(10) . . ? N1 Si1 C3 112.52(14) . . ? N1 Si1 C2 113.71(14) . . ? C3 Si1 C2 106.35(17) . . ? N1 Si1 C1 110.97(13) . . ? C3 Si1 C1 109.22(16) . . ? C2 Si1 C1 103.57(17) . . ? N1 Si1 Li1 37.24(12) . . ? C3 Si1 Li1 146.97(16) . . ? C2 Si1 Li1 84.60(15) . . ? C1 Si1 Li1 97.79(15) . . ? Si2 N1 Si1 117.30(13) . . ? Si2 N1 Al1 113.55(12) . . ? Si1 N1 Al1 115.41(12) . . ? Si2 N1 Li1 99.69(18) . . ? Si1 N1 Li1 111.2(2) . . ? Al1 N1 Li1 96.24(17) . . ? Si1 C1 H1A 109.5 . . ? Si1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? Si1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? N5 Al2 N4 110.95(11) . . ? N5 Al2 C38 105.74(14) . . ? N4 Al2 C38 115.84(12) . . ? N5 Al2 C37 104.03(12) . . ? N4 Al2 C37 111.74(12) . . ? C38 Al2 C37 107.71(14) . . ? N5 Al2 Li2 73.84(13) . . ? N4 Al2 Li2 44.98(12) . . ? C38 Al2 Li2 104.07(16) . . ? C37 Al2 Li2 147.34(15) . . ? N6 Li2 N4 116.0(3) . . ? N6 Li2 Al2 74.02(16) . . ? N4 Li2 Al2 42.59(11) . . ? N6 Li2 Si3 119.9(2) . . ? N4 Li2 Si3 35.14(12) . . ? Al2 Li2 Si3 64.32(11) . . ? N6 Li2 Si4 131.8(2) . . ? N4 Li2 Si4 32.34(11) . . ? Al2 Li2 Si4 63.07(10) . . ? Si3 Li2 Si4 59.47(10) . . ? N1 Si2 C5 112.81(16) . . ? N1 Si2 C4 112.51(14) . . ? C5 Si2 C4 107.31(19) . . ? N1 Si2 C6 110.30(14) . . ? C5 Si2 C6 104.99(18) . . ? C4 Si2 C6 108.55(17) . . ? N1 Si2 Li1 43.68(12) . . ? C5 Si2 Li1 103.89(17) . . ? C4 Si2 Li1 147.20(16) . . ? C6 Si2 Li1 72.17(16) . . ? C7 N2 C12 116.5(2) . . ? C7 N2 Al1 123.13(18) . . ? C12 N2 Al1 117.67(19) . . ? Si1 C2 H2A 109.5 . . ? Si1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? Si1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? N4 Si3 C20 109.31(14) . . ? N4 Si3 C22 112.30(15) . . ? C20 Si3 C22 110.88(18) . . ? N4 Si3 C21 115.05(16) . . ? C20 Si3 C21 103.59(18) . . ? C22 Si3 C21 105.33(19) . . ? N4 Si3 Li2 41.99(13) . . ? C20 Si3 Li2 71.21(16) . . ? C22 Si3 Li2 144.59(16) . . ? C21 Si3 Li2 108.40(17) . . ? C7 N3 C11 117.9(3) . . ? C7 N3 Li1 127.2(2) . . ? C11 N3 Li1 112.4(2) . . ? Si1 C3 H3A 109.5 . . ? Si1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? Si1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? N4 Si4 C24 109.97(15) . . ? N4 Si4 C23 112.56(15) . . ? C24 Si4 C23 109.4(2) . . ? N4 Si4 C25 114.34(15) . . ? C24 Si4 C25 104.0(2) . . ? C23 Si4 C25 106.07(19) . . ? N4 Si4 Li2 38.37(12) . . ? C24 Si4 Li2 89.51(17) . . ? C23 Si4 Li2 150.76(17) . . ? C25 Si4 Li2 89.85(15) . . ? Si3 N4 Si4 118.25(13) . . ? Si3 N4 Al2 114.36(12) . . ? Si4 N4 Al2 115.26(13) . . ? Si3 N4 Li2 102.9(2) . . ? Si4 N4 Li2 109.3(2) . . ? Al2 N4 Li2 92.43(17) . . ? Si2 C4 H4A 109.5 . . ? Si2 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? Si2 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C26 N5 C31 112.8(3) . . ? C26 N5 Al2 120.8(2) . . ? C31 N5 Al2 120.7(2) . . ? Si2 C5 H5A 109.5 . . ? Si2 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? Si2 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C30 N6 C26 116.9(3) . . ? C30 N6 Li2 119.4(3) . . ? C26 N6 Li2 116.7(3) . . ? Si2 C6 H6A 109.5 . . ? Si2 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? Si2 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? N3 C7 N2 116.4(2) . . ? N3 C7 C8 119.3(3) . . ? N2 C7 C8 124.2(3) . . ? C9 C8 C7 120.5(3) . . ? C9 C8 H8A 119.7 . . ? C7 C8 H8A 119.7 . . ? C8 C9 C10 119.9(3) . . ? C8 C9 H9A 120.0 . . ? C10 C9 H9A 120.0 . . ? C11 C10 C9 117.3(3) . . ? C11 C10 H10A 121.3 . . ? C9 C10 H10A 121.3 . . ? C10 C11 N3 125.0(3) . . ? C10 C11 Li1 159.7(3) . . ? N3 C11 Li1 40.73(17) . . ? C10 C11 H11A 117.5 . . ? N3 C11 H11A 117.5 . . ? Li1 C11 H11A 78.8 . . ? C17 C12 C13 119.7(3) . . ? C17 C12 N2 120.3(3) . . ? C13 C12 N2 120.1(3) . . ? C12 C13 C14 118.8(4) . . ? C12 C13 H13A 120.6 . . ? C14 C13 H13A 120.6 . . ? C15 C14 C13 121.3(4) . . ? C15 C14 H14A 119.4 . . ? C13 C14 H14A 119.4 . . ? C14 C15 C16 120.3(4) . . ? C14 C15 H15A 119.8 . . ? C16 C15 H15A 119.8 . . ? C15 C16 C17 119.4(4) . . ? C15 C16 H16A 120.3 . . ? C17 C16 H16A 120.3 . . ? C12 C17 C16 120.5(4) . . ? C12 C17 H17A 119.7 . . ? C16 C17 H17A 119.7 . . ? Al1 C18 H18A 109.5 . . ? Al1 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? Al1 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? Al1 C19 H19A 109.5 . . ? Al1 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? Al1 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? Si3 C20 H20A 109.5 . . ? Si3 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? Si3 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? Si3 C21 H21A 109.5 . . ? Si3 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? Si3 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? Si3 C22 H22A 109.5 . . ? Si3 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? Si3 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? Si4 C23 H23A 109.5 . . ? Si4 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? Si4 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? Si4 C24 H24A 109.5 . . ? Si4 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? Si4 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? Si4 C25 H25A 109.5 . . ? Si4 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? Si4 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? N5 C26 C27 127.0(3) . . ? N5 C26 N6 112.9(3) . . ? C27 C26 N6 120.1(3) . . ? C28 C27 C26 121.0(3) . . ? C28 C27 H27A 119.5 . . ? C26 C27 H27A 119.5 . . ? C27 C28 C29 119.9(4) . . ? C27 C28 H28A 120.1 . . ? C29 C28 H28A 120.1 . . ? C30 C29 C28 117.8(3) . . ? C30 C29 H29A 121.1 . . ? C28 C29 H29A 121.1 . . ? C29 C30 N6 124.3(3) . . ? C29 C30 H30A 117.8 . . ? N6 C30 H30A 117.8 . . ? C32 C31 C36 119.2(3) . . ? C32 C31 N5 120.3(3) . . ? C36 C31 N5 120.6(4) . . ? C31 C32 C33 120.9(4) . . ? C31 C32 H32A 119.5 . . ? C33 C32 H32A 119.5 . . ? C34 C33 C32 118.8(5) . . ? C34 C33 H33A 120.6 . . ? C32 C33 H33A 120.6 . . ? C35 C34 C33 120.1(4) . . ? C35 C34 H34A 120.0 . . ? C33 C34 H34A 120.0 . . ? C34 C35 C36 121.1(5) . . ? C34 C35 H35A 119.5 . . ? C36 C35 H35A 119.5 . . ? C35 C36 C31 119.9(5) . . ? C35 C36 H36A 120.0 . . ? C31 C36 H36A 120.0 . . ? Al2 C37 H37A 109.5 . . ? Al2 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? Al2 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? Al2 C38 H38A 109.5 . . ? Al2 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? Al2 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 0.453 _refine_diff_density_min -0.311 _refine_diff_density_rms 0.060 data_rs9911 _database_code_CSD 165072 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C34 H46 Al2 Li2 N4 O3' _chemical_formula_weight 626.59 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' 'O' 'O' 0.0106 0.0060 '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' 'Li' 'Li' -0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pna2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-x+1/2, y+1/2, z+1/2' 'x+1/2, -y+1/2, z' _cell_length_a 20.158(7) _cell_length_b 9.686(4) _cell_length_c 18.129(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3540(2) _cell_formula_units_Z 4 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.176 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1336 _exptl_absorpt_coefficient_mu 0.120 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.9650 _exptl_absorpt_correction_T_max 0.9881 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 180(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4101 _diffrn_reflns_av_R_equivalents 0.0593 _diffrn_reflns_av_sigmaI/netI 0.1467 _diffrn_reflns_limit_h_min -1 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -1 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.59 _diffrn_reflns_theta_max 25.00 _reflns_number_total 3440 _reflns_number_gt 1938 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0468P)^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 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 0.0(4) _refine_ls_number_reflns 3440 _refine_ls_number_parameters 443 _refine_ls_number_restraints 88 _refine_ls_R_factor_all 0.1453 _refine_ls_R_factor_gt 0.0700 _refine_ls_wR_factor_ref 0.1513 _refine_ls_wR_factor_gt 0.1232 _refine_ls_goodness_of_fit_ref 0.978 _refine_ls_restrained_S_all 0.977 _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 0.0858(8) 0.0664(15) 0.1584(8) 0.044(4) Uani 1 1 d . . . Al1 Al 0.05681(11) -0.1528(2) 0.26131(14) 0.0269(6) Uani 1 1 d . . . O1 O 0.1115(2) -0.1146(5) 0.1895(3) 0.0276(13) Uani 1 1 d . . . N1 N 0.0153(3) 0.0260(6) 0.2746(4) 0.0284(16) Uani 1 1 d . . . C1 C -0.0111(4) -0.2901(8) 0.2362(5) 0.042(2) Uani 1 1 d . . . H1A H -0.0453 -0.2913 0.2747 0.063 Uiso 1 1 calc R . . H1B H 0.0094 -0.3815 0.2326 0.063 Uiso 1 1 calc R . . H1C H -0.0315 -0.2660 0.1889 0.063 Uiso 1 1 calc R . . Li2 Li 0.1809(7) -0.0013(16) 0.2238(9) 0.041(4) Uani 1 1 d . . . Al2 Al 0.13937(11) -0.2153(2) 0.11456(15) 0.0279(6) Uani 1 1 d . . . O2 O 0.0319(3) 0.2029(6) 0.1097(4) 0.0472(16) Uani 1 1 d . . . C2 C 0.1054(4) -0.1995(10) 0.3534(5) 0.046(3) Uani 1 1 d . . . H2A H 0.0736 -0.2145 0.3935 0.070 Uiso 1 1 calc R . . H2B H 0.1352 -0.1233 0.3665 0.070 Uiso 1 1 calc R . . H2C H 0.1315 -0.2837 0.3457 0.070 Uiso 1 1 calc R . . N2 N 0.1125(3) 0.1533(7) 0.2715(4) 0.0270(15) Uani 1 1 d . . . N3 N 0.2203(3) -0.1283(7) 0.0844(4) 0.0281(16) Uani 1 1 d . . . C3 C -0.0553(4) 0.0209(8) 0.2900(5) 0.035(2) Uani 1 1 d . . . N4 N 0.1904(3) 0.0978(6) 0.1141(4) 0.0338(17) Uani 1 1 d . . . C4 C -0.0774(4) -0.0073(10) 0.3609(6) 0.047(3) Uani 1 1 d . . . H4A H -0.0467 -0.0193 0.4002 0.056 Uiso 1 1 calc R . . C5 C -0.1454(5) -0.0175(12) 0.3734(7) 0.070(4) Uani 1 1 d . . . H5A H -0.1611 -0.0360 0.4218 0.084 Uiso 1 1 calc R . . C6 C -0.1900(6) -0.0014(12) 0.3170(10) 0.079(4) Uani 1 1 d . . . H6A H -0.2362 -0.0098 0.3262 0.095 Uiso 1 1 calc R . . C7 C -0.1678(5) 0.0267(11) 0.2479(8) 0.064(4) Uani 1 1 d . . . H7A H -0.1987 0.0360 0.2086 0.077 Uiso 1 1 calc R . . C8 C -0.0999(4) 0.0422(9) 0.2339(6) 0.048(3) Uani 1 1 d . . . H8A H -0.0849 0.0671 0.1860 0.058 Uiso 1 1 calc R . . C9 C 0.0489(4) 0.1430(8) 0.2968(4) 0.0270(19) Uani 1 1 d . . . C10 C 0.0221(4) 0.2464(9) 0.3414(5) 0.044(3) Uani 1 1 d . . . H10A H -0.0217 0.2371 0.3602 0.053 Uiso 1 1 calc R . . C11 C 0.0580(4) 0.3586(9) 0.3578(5) 0.043(2) Uani 1 1 d . . . H11A H 0.0395 0.4297 0.3874 0.051 Uiso 1 1 calc R . . C12 C 0.1228(4) 0.3709(9) 0.3315(5) 0.045(3) Uani 1 1 d . . . H12A H 0.1491 0.4494 0.3429 0.054 Uiso 1 1 calc R . . C13 C 0.1471(4) 0.2669(9) 0.2889(5) 0.042(2) Uani 1 1 d . . . H13A H 0.1910 0.2752 0.2705 0.050 Uiso 1 1 calc R . . C14 C 0.0017(5) 0.3234(10) 0.1417(6) 0.057(3) Uani 1 1 d . . . H14A H 0.0342 0.3750 0.1719 0.068 Uiso 1 1 calc R . . H14B H -0.0363 0.2970 0.1734 0.068 Uiso 1 1 calc R . . C15 C -0.0216(6) 0.4100(11) 0.0774(8) 0.089(4) Uani 1 1 d . . . H15A H -0.0689 0.3918 0.0664 0.107 Uiso 1 1 calc R . . H15B H -0.0159 0.5096 0.0880 0.107 Uiso 1 1 calc R . . C16 C 0.0213(7) 0.3667(12) 0.0148(6) 0.090(4) Uani 1 1 d . . . H16A H 0.0636 0.4186 0.0145 0.108 Uiso 1 1 calc R . . H16B H -0.0015 0.3803 -0.0331 0.108 Uiso 1 1 calc R . . C17 C 0.0327(6) 0.2161(11) 0.0300(6) 0.068(3) Uani 1 1 d . . . H17A H -0.0027 0.1593 0.0075 0.082 Uiso 1 1 calc R . . H17B H 0.0760 0.1861 0.0099 0.082 Uiso 1 1 calc R . . C18 C 0.0759(4) -0.2065(11) 0.0325(5) 0.057(3) Uani 1 1 d . . . H18A H 0.0956 -0.2489 -0.0114 0.085 Uiso 1 1 calc R . . H18B H 0.0651 -0.1099 0.0220 0.085 Uiso 1 1 calc R . . H18C H 0.0354 -0.2564 0.0460 0.085 Uiso 1 1 calc R . . C19 C 0.1630(5) -0.4033(8) 0.1478(6) 0.057(3) Uani 1 1 d . . . H19A H 0.1666 -0.4645 0.1050 0.086 Uiso 1 1 calc R . . H19B H 0.1285 -0.4380 0.1811 0.086 Uiso 1 1 calc R . . H19C H 0.2055 -0.4006 0.1739 0.086 Uiso 1 1 calc R . . C20 C 0.2696(4) -0.2182(8) 0.0525(5) 0.032(2) Uani 1 1 d . . . C21 C 0.3297(4) -0.2418(10) 0.0875(5) 0.048(3) Uani 1 1 d . . . H21A H 0.3389 -0.1959 0.1327 0.058 Uiso 1 1 calc R . . C22 C 0.3765(5) -0.3303(10) 0.0586(6) 0.056(3) Uani 1 1 d . . . H22A H 0.4174 -0.3444 0.0835 0.067 Uiso 1 1 calc R . . C23 C 0.3638(5) -0.3977(10) -0.0062(5) 0.044(2) Uani 1 1 d . . . H23A H 0.3955 -0.4598 -0.0263 0.053 Uiso 1 1 calc R . . C24 C 0.3037(4) -0.3744(9) -0.0423(5) 0.044(2) Uani 1 1 d . . . H24A H 0.2946 -0.4205 -0.0875 0.053 Uiso 1 1 calc R . . C25 C 0.2582(4) -0.2863(9) -0.0133(4) 0.035(2) Uani 1 1 d . . . H25A H 0.2177 -0.2711 -0.0388 0.041 Uiso 1 1 calc R . . C26 C 0.2313(4) 0.0106(8) 0.0752(5) 0.028(2) Uani 1 1 d . . . C27 C 0.2820(4) 0.0645(9) 0.0293(5) 0.034(2) Uani 1 1 d . . . H27A H 0.3105 0.0036 0.0032 0.041 Uiso 1 1 calc R . . C28 C 0.2898(4) 0.2041(11) 0.0228(6) 0.051(3) Uani 1 1 d . . . H28A H 0.3245 0.2408 -0.0068 0.061 Uiso 1 1 calc R . . C29 C 0.2461(4) 0.2925(9) 0.0602(5) 0.049(3) Uani 1 1 d . . . H29A H 0.2493 0.3899 0.0549 0.059 Uiso 1 1 calc R . . C30 C 0.1994(4) 0.2351(8) 0.1038(5) 0.040(2) Uani 1 1 d . . . H30A H 0.1705 0.2959 0.1294 0.049 Uiso 1 1 calc R . . O3 O 0.2645(3) -0.0126(6) 0.2702(4) 0.0443(16) Uani 1 1 d D . . C31 C 0.2926(5) -0.1307(11) 0.3096(6) 0.061(3) Uani 1 1 d DU D . H31A H 0.3092 -0.2011 0.2746 0.073 Uiso 0.50 1 calc PR A 1 H31B H 0.2591 -0.1736 0.3423 0.073 Uiso 0.50 1 calc PR A 1 H31C H 0.292(8) -0.242(18) 0.242(10) 0.073 Uiso 0.50 1 d P B 2 H31D H 0.247(9) -0.146(19) 0.328(11) 0.073 Uiso 0.50 1 d P C 2 C32 C 0.3476(10) -0.071(2) 0.3529(11) 0.072(6) Uani 0.50 1 d PDU D 1 H32A H 0.3846 -0.1375 0.3575 0.086 Uiso 0.50 1 calc PR D 1 H32B H 0.3324 -0.0450 0.4030 0.086 Uiso 0.50 1 calc PR D 1 C33 C 0.3691(8) 0.053(2) 0.3114(12) 0.067(6) Uani 0.50 1 d PDU D 1 H33A H 0.3657 0.1370 0.3426 0.081 Uiso 0.50 1 calc PR D 1 H33B H 0.4156 0.0434 0.2946 0.081 Uiso 0.50 1 calc PR D 1 C34 C 0.3239(7) 0.0629(17) 0.2480(10) 0.057(6) Uani 0.50 1 d PDU D 1 H34A H 0.3132 0.1605 0.2369 0.069 Uiso 0.50 1 calc PR D 1 H34B H 0.3441 0.0204 0.2037 0.069 Uiso 0.50 1 calc PR D 1 C32' C 0.3324(12) -0.073(2) 0.3700(10) 0.076(7) Uani 0.50 1 d PDU D 2 H32C H 0.3686 -0.1365 0.3841 0.091 Uiso 0.50 1 calc PR D 2 H32D H 0.3045 -0.0541 0.4138 0.091 Uiso 0.50 1 calc PR D 2 C33' C 0.3592(9) 0.057(2) 0.3389(12) 0.073(6) Uani 0.50 1 d PDU D 2 H33C H 0.3583 0.1315 0.3762 0.088 Uiso 0.50 1 calc PR D 2 H33D H 0.4055 0.0437 0.3222 0.088 Uiso 0.50 1 calc PR D 2 C34' C 0.3162(8) 0.0914(17) 0.2764(12) 0.070(6) Uani 0.50 1 d PDU D 2 H34C H 0.2960 0.1834 0.2840 0.084 Uiso 0.50 1 calc PR D 2 H34D H 0.3426 0.0942 0.2304 0.084 Uiso 0.50 1 calc PR D 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 Li1 0.064(11) 0.028(8) 0.040(9) 0.006(8) -0.008(8) 0.013(8) Al1 0.0280(12) 0.0253(13) 0.0274(13) -0.0007(13) 0.0032(12) -0.0017(12) O1 0.034(3) 0.019(3) 0.030(3) -0.003(3) 0.009(3) -0.003(3) N1 0.027(3) 0.025(4) 0.033(4) -0.003(4) 0.001(4) -0.001(3) C1 0.039(5) 0.036(5) 0.051(6) 0.000(5) 0.001(5) 0.004(5) Li2 0.033(8) 0.045(9) 0.044(9) 0.004(8) 0.009(7) 0.003(8) Al2 0.0305(13) 0.0225(12) 0.0308(13) -0.0035(14) 0.0038(13) -0.0004(12) O2 0.063(4) 0.035(3) 0.043(4) 0.003(3) -0.004(4) 0.019(3) C2 0.054(6) 0.043(6) 0.042(6) 0.000(5) -0.010(5) -0.001(5) N2 0.030(3) 0.027(4) 0.025(4) -0.006(4) 0.003(3) -0.005(3) N3 0.023(3) 0.033(4) 0.028(4) -0.004(3) 0.011(3) 0.002(3) C3 0.026(4) 0.028(5) 0.050(6) -0.008(5) 0.004(5) 0.005(4) N4 0.046(4) 0.022(3) 0.033(4) -0.001(4) 0.016(4) -0.007(3) C4 0.024(5) 0.063(7) 0.053(7) -0.002(6) -0.005(5) 0.009(5) C5 0.050(7) 0.074(9) 0.086(9) -0.025(8) 0.032(7) -0.001(7) C6 0.033(6) 0.059(8) 0.147(14) -0.026(9) 0.023(8) -0.005(6) C7 0.033(6) 0.052(7) 0.107(11) 0.000(8) -0.032(7) -0.002(6) C8 0.040(6) 0.041(6) 0.064(7) 0.003(6) -0.014(5) -0.004(5) C9 0.032(5) 0.021(4) 0.028(5) 0.010(4) -0.010(4) 0.001(4) C10 0.040(5) 0.044(6) 0.048(6) -0.024(5) 0.009(5) 0.002(5) C11 0.050(6) 0.032(5) 0.046(6) -0.018(5) 0.009(5) 0.002(5) C12 0.042(6) 0.031(5) 0.063(7) -0.022(5) 0.002(5) -0.006(5) C13 0.035(5) 0.037(5) 0.053(6) 0.000(5) 0.003(5) -0.002(5) C14 0.059(7) 0.044(6) 0.068(8) 0.000(6) -0.003(6) 0.006(5) C15 0.121(11) 0.045(7) 0.102(10) 0.003(8) -0.029(10) 0.032(7) C16 0.159(13) 0.071(9) 0.041(7) 0.028(7) -0.010(8) 0.006(10) C17 0.089(8) 0.067(8) 0.048(7) 0.007(7) -0.018(7) 0.018(7) C18 0.035(5) 0.086(8) 0.050(6) 0.006(7) 0.001(5) 0.003(6) C19 0.053(6) 0.030(5) 0.089(8) 0.011(6) 0.031(6) 0.006(5) C20 0.026(4) 0.027(4) 0.043(6) 0.001(5) 0.016(4) 0.006(4) C21 0.036(5) 0.068(7) 0.041(6) -0.016(5) 0.005(5) 0.001(5) C22 0.052(6) 0.059(7) 0.056(7) -0.012(6) 0.006(5) 0.028(6) C23 0.036(5) 0.049(6) 0.049(6) -0.007(5) 0.015(5) 0.007(5) C24 0.048(6) 0.039(5) 0.046(6) -0.016(5) 0.015(5) -0.003(5) C25 0.035(5) 0.042(5) 0.026(5) -0.023(5) -0.002(4) 0.008(5) C26 0.030(4) 0.023(4) 0.032(5) 0.005(4) 0.003(4) -0.006(4) C27 0.036(5) 0.024(5) 0.041(6) 0.009(5) 0.008(5) -0.002(4) C28 0.038(5) 0.067(7) 0.048(6) 0.010(6) 0.015(5) -0.016(5) C29 0.054(6) 0.027(5) 0.066(7) -0.003(6) 0.022(6) -0.009(5) C30 0.050(5) 0.026(5) 0.044(6) 0.000(5) 0.012(5) 0.000(5) O3 0.034(3) 0.040(4) 0.059(4) 0.000(4) -0.010(4) -0.007(3) C31 0.056(7) 0.054(7) 0.073(8) 0.020(6) 0.003(6) -0.004(6) C32 0.043(10) 0.133(12) 0.038(11) -0.036(10) 0.017(10) 0.031(10) C33 0.041(9) 0.097(10) 0.064(13) -0.054(10) 0.006(9) 0.001(8) C34 0.056(11) 0.048(10) 0.068(14) -0.042(10) 0.010(9) 0.006(9) C32' 0.061(13) 0.139(13) 0.028(11) -0.022(10) -0.001(11) 0.046(11) C33' 0.047(9) 0.114(11) 0.058(12) -0.061(10) 0.000(9) 0.006(9) C34' 0.057(10) 0.080(11) 0.073(14) -0.019(11) -0.003(10) -0.004(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 Li1 O1 1.913(15) . ? Li1 O2 1.927(15) . ? Li1 N4 2.276(18) . ? Li1 N2 2.281(17) . ? Li1 Li2 2.35(2) . ? Li1 N1 2.572(18) . ? Li1 C9 2.721(18) . ? Li1 Al1 2.887(15) . ? Li1 Al2 3.039(15) . ? Al1 O1 1.746(5) . ? Al1 N1 1.939(6) . ? Al1 C1 1.962(8) . ? Al1 C2 1.988(9) . ? Al1 Li2 2.979(14) . ? O1 Al2 1.763(5) . ? O1 Li2 1.883(16) . ? N1 C9 1.380(9) . ? N1 C3 1.450(9) . ? Li2 O3 1.887(15) . ? Li2 N2 2.212(16) . ? Li2 N4 2.217(18) . ? Li2 Al2 2.986(16) . ? Al2 N3 1.916(6) . ? Al2 C18 1.963(9) . ? Al2 C19 1.977(9) . ? O2 C14 1.438(10) . ? O2 C17 1.450(12) . ? N2 C13 1.340(9) . ? N2 C9 1.365(9) . ? N3 C26 1.374(9) . ? N3 C20 1.442(9) . ? C3 C8 1.375(12) . ? C3 C4 1.388(12) . ? N4 C30 1.355(9) . ? N4 C26 1.375(9) . ? C4 C5 1.393(12) . ? C5 C6 1.371(17) . ? C6 C7 1.358(15) . ? C7 C8 1.400(12) . ? C9 C10 1.396(11) . ? C10 C11 1.340(11) . ? C11 C12 1.394(11) . ? C12 C13 1.360(11) . ? C14 C15 1.511(14) . ? C15 C16 1.486(16) . ? C16 C17 1.503(14) . ? C20 C25 1.383(10) . ? C20 C21 1.386(10) . ? C21 C22 1.378(11) . ? C22 C23 1.367(12) . ? C23 C24 1.396(12) . ? C24 C25 1.359(11) . ? C26 C27 1.416(11) . ? C27 C28 1.366(13) . ? C28 C29 1.404(12) . ? C29 C30 1.350(11) . ? O3 C34' 1.453(10) . ? O3 C34 1.460(10) . ? O3 C31 1.462(9) . ? C31 C32' 1.469(12) . ? C31 C32 1.479(12) . ? C32 C33 1.483(18) . ? C33 C34 1.470(12) . ? C32' C33' 1.480(18) . ? C33' C34' 1.465(12) . ? 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 Li1 O2 156.5(10) . . ? O1 Li1 N4 88.6(6) . . ? O2 Li1 N4 105.7(7) . . ? O1 Li1 N2 90.5(6) . . ? O2 Li1 N2 106.9(7) . . ? N4 Li1 N2 92.8(6) . . ? O1 Li1 Li2 51.2(5) . . ? O2 Li1 Li2 152.2(9) . . ? N4 Li1 Li2 57.3(6) . . ? N2 Li1 Li2 57.1(5) . . ? O1 Li1 N1 76.6(6) . . ? O2 Li1 N1 99.6(7) . . ? N4 Li1 N1 145.2(7) . . ? N2 Li1 N1 56.6(4) . . ? Li2 Li1 N1 89.7(6) . . ? O1 Li1 C9 93.0(6) . . ? O2 Li1 C9 94.6(6) . . ? N4 Li1 C9 122.8(7) . . ? N2 Li1 C9 30.1(3) . . ? Li2 Li1 C9 80.4(6) . . ? N1 Li1 C9 30.1(3) . . ? O1 Li1 Al1 35.9(3) . . ? O2 Li1 Al1 133.4(8) . . ? N4 Li1 Al1 120.9(6) . . ? N2 Li1 Al1 74.8(5) . . ? Li2 Li1 Al1 68.5(5) . . ? N1 Li1 Al1 41.1(3) . . ? C9 Li1 Al1 63.2(4) . . ? O1 Li1 Al2 32.7(3) . . ? O2 Li1 Al2 134.2(7) . . ? N4 Li1 Al2 72.5(4) . . ? N2 Li1 Al2 118.8(6) . . ? Li2 Li1 Al2 65.9(5) . . ? N1 Li1 Al2 105.9(5) . . ? C9 Li1 Al2 125.7(5) . . ? Al1 Li1 Al2 65.2(3) . . ? O1 Al1 N1 100.2(3) . . ? O1 Al1 C1 114.3(3) . . ? N1 Al1 C1 109.4(3) . . ? O1 Al1 C2 111.3(3) . . ? N1 Al1 C2 108.2(4) . . ? C1 Al1 C2 112.6(4) . . ? O1 Al1 Li1 40.0(4) . . ? N1 Al1 Li1 60.7(4) . . ? C1 Al1 Li1 119.3(4) . . ? C2 Al1 Li1 127.6(4) . . ? O1 Al1 Li2 36.4(4) . . ? N1 Al1 Li2 87.2(3) . . ? C1 Al1 Li2 150.1(4) . . ? C2 Al1 Li2 83.7(4) . . ? Li1 Al1 Li2 47.1(4) . . ? Al1 O1 Al2 131.2(3) . . ? Al1 O1 Li2 110.2(5) . . ? Al2 O1 Li2 109.9(5) . . ? Al1 O1 Li1 104.1(6) . . ? Al2 O1 Li1 111.5(5) . . ? Li2 O1 Li1 76.4(7) . . ? C9 N1 C3 117.0(7) . . ? C9 N1 Al1 123.9(5) . . ? C3 N1 Al1 114.6(5) . . ? C9 N1 Li1 80.9(6) . . ? C3 N1 Li1 134.9(7) . . ? Al1 N1 Li1 78.2(4) . . ? O1 Li2 O3 141.0(9) . . ? O1 Li2 N2 93.5(6) . . ? O3 Li2 N2 114.9(8) . . ? O1 Li2 N4 91.2(7) . . ? O3 Li2 N4 110.4(7) . . ? N2 Li2 N4 96.4(6) . . ? O1 Li2 Li1 52.4(5) . . ? O3 Li2 Li1 166.1(9) . . ? N2 Li2 Li1 60.0(5) . . ? N4 Li2 Li1 59.8(6) . . ? O1 Li2 Al1 33.4(3) . . ? O3 Li2 Al1 128.3(7) . . ? N2 Li2 Al1 73.8(4) . . ? N4 Li2 Al1 119.4(6) . . ? Li1 Li2 Al1 64.4(5) . . ? O1 Li2 Al2 33.7(3) . . ? O3 Li2 Al2 120.4(7) . . ? N2 Li2 Al2 123.7(6) . . ? N4 Li2 Al2 74.3(5) . . ? Li1 Li2 Al2 68.3(5) . . ? Al1 Li2 Al2 64.8(3) . . ? O1 Al2 N3 104.3(3) . . ? O1 Al2 C18 110.6(3) . . ? N3 Al2 C18 108.6(4) . . ? O1 Al2 C19 110.6(4) . . ? N3 Al2 C19 106.7(3) . . ? C18 Al2 C19 115.3(4) . . ? O1 Al2 Li2 36.4(3) . . ? N3 Al2 Li2 69.2(3) . . ? C18 Al2 Li2 130.9(4) . . ? C19 Al2 Li2 111.7(5) . . ? O1 Al2 Li1 35.9(3) . . ? N3 Al2 Li1 89.0(4) . . ? C18 Al2 Li1 85.9(4) . . ? C19 Al2 Li1 146.4(4) . . ? Li2 Al2 Li1 45.8(4) . . ? C14 O2 C17 109.6(8) . . ? C14 O2 Li1 127.7(8) . . ? C17 O2 Li1 120.6(8) . . ? C13 N2 C9 117.9(7) . . ? C13 N2 Li2 108.9(6) . . ? C9 N2 Li2 131.9(7) . . ? C13 N2 Li1 129.6(7) . . ? C9 N2 Li1 93.1(6) . . ? Li2 N2 Li1 63.0(6) . . ? C26 N3 C20 115.5(6) . . ? C26 N3 Al2 127.1(5) . . ? C20 N3 Al2 115.9(5) . . ? C8 C3 C4 120.4(8) . . ? C8 C3 N1 119.6(8) . . ? C4 C3 N1 120.0(8) . . ? C30 N4 C26 116.9(7) . . ? C30 N4 Li2 124.0(8) . . ? C26 N4 Li2 104.3(6) . . ? C30 N4 Li1 107.6(6) . . ? C26 N4 Li1 130.9(6) . . ? Li2 N4 Li1 63.0(5) . . ? C3 C4 C5 118.7(10) . . ? C6 C5 C4 121.2(11) . . ? C7 C6 C5 119.6(11) . . ? C6 C7 C8 120.7(11) . . ? C3 C8 C7 119.3(10) . . ? N2 C9 N1 115.0(7) . . ? N2 C9 C10 120.4(8) . . ? N1 C9 C10 124.5(7) . . ? N2 C9 Li1 56.8(5) . . ? N1 C9 Li1 69.0(6) . . ? C10 C9 Li1 146.8(6) . . ? C11 C10 C9 120.0(8) . . ? C10 C11 C12 120.0(8) . . ? C13 C12 C11 117.9(8) . . ? N2 C13 C12 123.7(8) . . ? O2 C14 C15 105.7(8) . . ? C16 C15 C14 104.7(8) . . ? C15 C16 C17 102.8(9) . . ? O2 C17 C16 105.5(9) . . ? C25 C20 C21 117.5(8) . . ? C25 C20 N3 121.3(7) . . ? C21 C20 N3 121.2(8) . . ? C22 C21 C20 121.7(8) . . ? C23 C22 C21 119.7(9) . . ? C22 C23 C24 119.3(9) . . ? C25 C24 C23 120.4(9) . . ? C24 C25 C20 121.4(8) . . ? N3 C26 N4 116.3(7) . . ? N3 C26 C27 123.3(7) . . ? N4 C26 C27 120.4(7) . . ? C28 C27 C26 120.0(8) . . ? C27 C28 C29 119.3(9) . . ? C30 C29 C28 118.0(8) . . ? C29 C30 N4 125.3(8) . . ? C34' O3 C34 23.9(13) . . ? C34' O3 C31 103.1(9) . . ? C34 O3 C31 102.1(9) . . ? C34' O3 Li2 129.4(9) . . ? C34 O3 Li2 125.5(9) . . ? C31 O3 Li2 127.5(7) . . ? O3 C31 C32' 106.1(10) . . ? O3 C31 C32 104.0(9) . . ? C32' C31 C32 17.1(19) . . ? C31 C32 C33 105.5(8) . . ? C34 C33 C32 105.4(8) . . ? O3 C34 C33 105.1(9) . . ? C31 C32' C33' 103.8(9) . . ? C34' C33' C32' 105.8(8) . . ? O3 C34' C33' 109.0(9) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.239 _refine_diff_density_min -0.268 _refine_diff_density_rms 0.060