# Supplementary Material (ESI) for New Journal of Chemistry # This journal is © The Royal Society of Chemistry and # The Centre National de la Recherche Scientifique, 2004 data_global _journal_coden_Cambridge 440 loop_ _publ_author_name 'Peter Junk' 'Rene Boere' 'Marcus L. Cole' _publ_contact_author_name 'Assoc. Prof. Peter Junk' _publ_contact_author_address ; School of CHemistry Monash University Monash University Clayton Victoria AUSTRALIA ; _publ_contact_author_email Peter.Junk@sci.monash.edu.au _publ_contact_author_fax 61399054597 _publ_contact_author_phone 61399054570 _publ_requested_journal 'New Journal of Chemistry' _publ_section_title ; The syntheses and structures of some main group complexes of the sterically hindered N,N'-bis(2,6-diisopropylphenyl)-4-toluamidinate ligand ; data_Compound_1 _database_code_depnum_ccdc_archive 'CCDC 242105' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common "[Li(N,N'-Dipamidine)(THF)2]" _chemical_melting_point 434 _chemical_formula_moiety 'C40 H57 Li N2 O2' _chemical_formula_sum 'C40 H57 Li N2 O2' _chemical_formula_weight 604.82 _ccdc_chemical_compound_source_recrystallisation THF loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Li Li -0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.922(3) _cell_length_b 11.627(2) _cell_length_c 15.562(4) _cell_angle_alpha 80.772(9) _cell_angle_beta 77.567(13) _cell_angle_gamma 77.758(11) _cell_volume 1872.3(8) _cell_formula_units_Z 2 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'rectangular block' _exptl_crystal_colour colourless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.073 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 660 _exptl_absorpt_coefficient_mu 0.064 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.9873 _exptl_absorpt_correction_T_max 0.9873 _exptl_absorpt_process_details 'performed as part of the DENZO-SMN package' _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_probe x-ray _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_measurement_method 'psi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 22064 _diffrn_reflns_av_R_equivalents 0.1829 _diffrn_reflns_av_sigmaI/netI 0.2350 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.94 _diffrn_reflns_theta_max 27.73 _reflns_number_total 8589 _reflns_number_gt 3195 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Nonius Collect' _computing_cell_refinement DENZO-SMN _computing_data_reduction X-Seed _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'X-Seed / POV-Ray' _computing_publication_material 'Microsoft Office 2000' _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^)+(0.0857P)^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_number_reflns 8589 _refine_ls_number_parameters 415 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.2305 _refine_ls_R_factor_gt 0.0719 _refine_ls_wR_factor_ref 0.2172 _refine_ls_wR_factor_gt 0.1563 _refine_ls_goodness_of_fit_ref 0.893 _refine_ls_restrained_S_all 0.893 _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 O1 O 0.5550(2) 0.0857(2) 0.16434(16) 0.0471(7) Uani 1 1 d . . . N1 N 0.3114(2) 0.2638(2) 0.30317(16) 0.0231(6) Uani 1 1 d . . . C1 C 0.2971(3) 0.3325(2) 0.3736(2) 0.0235(7) Uani 1 1 d . . . Li1 Li 0.3936(5) 0.1119(5) 0.2485(4) 0.0360(14) Uani 1 1 d . . . O2 O 0.4237(2) -0.03895(19) 0.32536(16) 0.0412(6) Uani 1 1 d . . . N2 N 0.2340(2) 0.1997(2) 0.19950(16) 0.0239(6) Uani 1 1 d . . . C2 C 0.3872(3) 0.4026(3) 0.3714(2) 0.0269(8) Uani 1 1 d . . . C3 C 0.3760(3) 0.4667(3) 0.4411(2) 0.0330(8) Uani 1 1 d . . . H3 H 0.4380 0.5136 0.4397 0.040 Uiso 1 1 calc R . . C4 C 0.2758(3) 0.4638(3) 0.5131(2) 0.0344(8) Uani 1 1 d . . . H4 H 0.2681 0.5098 0.5598 0.041 Uiso 1 1 calc R . . C5 C 0.1883(3) 0.3942(3) 0.5159(2) 0.0328(8) Uani 1 1 d . . . H5 H 0.1200 0.3925 0.5653 0.039 Uiso 1 1 calc R . . C6 C 0.1962(3) 0.3253(3) 0.4482(2) 0.0256(7) Uani 1 1 d . . . C7 C 0.4962(3) 0.4079(3) 0.2924(2) 0.0334(8) Uani 1 1 d . . . H7 H 0.4685 0.3858 0.2410 0.040 Uiso 1 1 calc R . . C8 C 0.6146(3) 0.3169(3) 0.3101(2) 0.0404(9) Uani 1 1 d . . . H8A H 0.6434 0.3353 0.3609 0.061 Uiso 1 1 calc R . . H8B H 0.6827 0.3198 0.2577 0.061 Uiso 1 1 calc R . . H8C H 0.5934 0.2374 0.3231 0.061 Uiso 1 1 calc R . . C9 C 0.5303(3) 0.5306(3) 0.2653(3) 0.0482(10) Uani 1 1 d . . . H9A H 0.4537 0.5885 0.2555 0.072 Uiso 1 1 calc R . . H9B H 0.5945 0.5301 0.2105 0.072 Uiso 1 1 calc R . . H9C H 0.5648 0.5521 0.3124 0.072 Uiso 1 1 calc R . . C10 C 0.1076(3) 0.2379(3) 0.4575(2) 0.0329(8) Uani 1 1 d . . . H10 H 0.0879 0.2378 0.3977 0.039 Uiso 1 1 calc R . . C11 C 0.1753(4) 0.1135(3) 0.4864(3) 0.0493(10) Uani 1 1 d . . . H11A H 0.2525 0.0917 0.4424 0.074 Uiso 1 1 calc R . . H11B H 0.1183 0.0571 0.4914 0.074 Uiso 1 1 calc R . . H11C H 0.1987 0.1118 0.5440 0.074 Uiso 1 1 calc R . . C12 C -0.0194(3) 0.2661(3) 0.5218(3) 0.0572(12) Uani 1 1 d . . . H12A H -0.0036 0.2574 0.5823 0.086 Uiso 1 1 calc R . . H12B H -0.0746 0.2113 0.5183 0.086 Uiso 1 1 calc R . . H12C H -0.0613 0.3477 0.5057 0.086 Uiso 1 1 calc R . . C13 C 0.1585(3) 0.2153(3) 0.13388(19) 0.0224(7) Uani 1 1 d . . . C14 C 0.0702(3) 0.1412(3) 0.1431(2) 0.0282(8) Uani 1 1 d . . . C15 C -0.0010(3) 0.1495(3) 0.0771(2) 0.0343(8) Uani 1 1 d . . . H15 H -0.0600 0.0980 0.0833 0.041 Uiso 1 1 calc R . . C16 C 0.0139(3) 0.2323(3) 0.0027(2) 0.0380(9) Uani 1 1 d . . . H16 H -0.0355 0.2384 -0.0417 0.046 Uiso 1 1 calc R . . C17 C 0.1008(3) 0.3058(3) -0.0063(2) 0.0329(8) Uani 1 1 d . . . H17 H 0.1094 0.3632 -0.0570 0.039 Uiso 1 1 calc R . . C18 C 0.1764(3) 0.2985(3) 0.0566(2) 0.0251(7) Uani 1 1 d . . . C19 C 0.0511(3) 0.0506(3) 0.2245(2) 0.0354(9) Uani 1 1 d . . . H19 H 0.0867 0.0750 0.2714 0.042 Uiso 1 1 calc R . . C20 C 0.1264(4) -0.0716(3) 0.2046(2) 0.0504(11) Uani 1 1 d . . . H20A H 0.0932 -0.0986 0.1592 0.076 Uiso 1 1 calc R . . H20B H 0.1177 -0.1277 0.2588 0.076 Uiso 1 1 calc R . . H20C H 0.2166 -0.0669 0.1831 0.076 Uiso 1 1 calc R . . C21 C -0.0891(4) 0.0441(4) 0.2624(3) 0.0614(12) Uani 1 1 d . . . H21A H -0.1369 0.1235 0.2731 0.092 Uiso 1 1 calc R . . H21B H -0.0953 -0.0087 0.3184 0.092 Uiso 1 1 calc R . . H21C H -0.1249 0.0133 0.2201 0.092 Uiso 1 1 calc R . . C22 C 0.2789(3) 0.3722(3) 0.0388(2) 0.0296(8) Uani 1 1 d . . . H22 H 0.3093 0.3690 0.0954 0.035 Uiso 1 1 calc R . . C23 C 0.3918(3) 0.3156(3) -0.0286(3) 0.0479(10) Uani 1 1 d . . . H23A H 0.4227 0.2338 -0.0049 0.072 Uiso 1 1 calc R . . H23B H 0.4608 0.3611 -0.0393 0.072 Uiso 1 1 calc R . . H23C H 0.3639 0.3160 -0.0844 0.072 Uiso 1 1 calc R . . C24 C 0.2350(4) 0.5025(3) 0.0058(3) 0.0460(10) Uani 1 1 d . . . H24A H 0.2145 0.5087 -0.0533 0.069 Uiso 1 1 calc R . . H24B H 0.3034 0.5466 0.0026 0.069 Uiso 1 1 calc R . . H24C H 0.1591 0.5358 0.0468 0.069 Uiso 1 1 calc R . . C25 C 0.2253(3) 0.2824(2) 0.2515(2) 0.0215(7) Uani 1 1 d . . . C26 C 0.1241(3) 0.3930(2) 0.25013(19) 0.0215(7) Uani 1 1 d . . . C27 C 0.1574(3) 0.5038(3) 0.2414(2) 0.0279(8) Uani 1 1 d . . . H27 H 0.2440 0.5098 0.2370 0.033 Uiso 1 1 calc R . . C28 C 0.0641(3) 0.6063(3) 0.2391(2) 0.0315(8) Uani 1 1 d . . . H28 H 0.0886 0.6814 0.2327 0.038 Uiso 1 1 calc R . . C29 C -0.0627(3) 0.6015(3) 0.2458(2) 0.0270(8) Uani 1 1 d . . . C30 C -0.0949(3) 0.4913(3) 0.2547(2) 0.0297(8) Uani 1 1 d . . . H30 H -0.1816 0.4855 0.2595 0.036 Uiso 1 1 calc R . . C31 C -0.0029(3) 0.3885(3) 0.2569(2) 0.0263(7) Uani 1 1 d . . . H31 H -0.0280 0.3138 0.2632 0.032 Uiso 1 1 calc R . . C32 C -0.1632(3) 0.7131(3) 0.2456(2) 0.0378(9) Uani 1 1 d . . . H32A H -0.2427 0.6950 0.2364 0.057 Uiso 1 1 calc R . . H32B H -0.1338 0.7725 0.1978 0.057 Uiso 1 1 calc R . . H32C H -0.1782 0.7443 0.3027 0.057 Uiso 1 1 calc R . . C33 C 0.6231(4) 0.1730(3) 0.1116(2) 0.0438(10) Uani 1 1 d . . . H33A H 0.6879 0.1878 0.1422 0.053 Uiso 1 1 calc R . . H33B H 0.5638 0.2485 0.1002 0.053 Uiso 1 1 calc R . . C34 C 0.6869(4) 0.1222(3) 0.0248(2) 0.0454(10) Uani 1 1 d . . . H34A H 0.6328 0.1488 -0.0207 0.055 Uiso 1 1 calc R . . H34B H 0.7712 0.1453 0.0017 0.055 Uiso 1 1 calc R . . C35 C 0.7002(5) -0.0088(4) 0.0519(3) 0.0775(15) Uani 1 1 d . . . H35A H 0.6988 -0.0504 0.0015 0.093 Uiso 1 1 calc R . . H35B H 0.7808 -0.0410 0.0737 0.093 Uiso 1 1 calc R . . C36 C 0.5890(4) -0.0220(3) 0.1233(3) 0.0660(13) Uani 1 1 d . . . H36A H 0.5170 -0.0341 0.0986 0.079 Uiso 1 1 calc R . . H36B H 0.6110 -0.0909 0.1672 0.079 Uiso 1 1 calc R . . C37 C 0.5246(4) -0.0601(3) 0.3748(3) 0.0477(10) Uani 1 1 d . . . H37A H 0.5127 0.0030 0.4132 0.057 Uiso 1 1 calc R . . H37B H 0.6084 -0.0629 0.3345 0.057 Uiso 1 1 calc R . . C38 C 0.5164(4) -0.1795(4) 0.4305(3) 0.0621(12) Uani 1 1 d . . . H38A H 0.5696 -0.2453 0.3984 0.075 Uiso 1 1 calc R . . H38B H 0.5439 -0.1828 0.4876 0.075 Uiso 1 1 calc R . . C39 C 0.3808(4) -0.1851(4) 0.4444(3) 0.0655(13) Uani 1 1 d . . . H39A H 0.3310 -0.1410 0.4939 0.079 Uiso 1 1 calc R . . H39B H 0.3673 -0.2682 0.4568 0.079 Uiso 1 1 calc R . . C40 C 0.3449(4) -0.1271(3) 0.3573(3) 0.0537(11) Uani 1 1 d . . . H40A H 0.3613 -0.1860 0.3149 0.064 Uiso 1 1 calc R . . H40B H 0.2535 -0.0899 0.3659 0.064 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 O1 0.0498(16) 0.0364(14) 0.0481(16) -0.0166(13) 0.0072(13) -0.0007(13) N1 0.0244(15) 0.0241(14) 0.0193(14) -0.0041(11) -0.0052(12) 0.0007(12) C1 0.0267(18) 0.0221(16) 0.0209(17) -0.0005(13) -0.0110(14) 0.0023(14) Li1 0.037(3) 0.032(3) 0.034(3) 0.000(3) -0.007(3) 0.003(3) O2 0.0418(15) 0.0342(13) 0.0448(16) 0.0036(12) -0.0158(12) 0.0005(12) N2 0.0291(15) 0.0198(13) 0.0237(15) -0.0040(11) -0.0092(12) -0.0008(12) C2 0.0294(19) 0.0271(17) 0.0231(18) -0.0015(14) -0.0067(15) -0.0025(15) C3 0.039(2) 0.0311(19) 0.032(2) -0.0039(16) -0.0130(17) -0.0069(16) C4 0.044(2) 0.0355(19) 0.028(2) -0.0106(16) -0.0141(18) -0.0031(18) C5 0.037(2) 0.036(2) 0.0192(18) -0.0032(15) -0.0042(15) 0.0046(17) C6 0.0249(18) 0.0289(17) 0.0207(18) -0.0022(14) -0.0062(14) 0.0016(15) C7 0.033(2) 0.040(2) 0.032(2) -0.0036(16) -0.0093(16) -0.0125(17) C8 0.040(2) 0.039(2) 0.042(2) -0.0097(18) -0.0012(18) -0.0093(18) C9 0.041(2) 0.045(2) 0.055(3) 0.008(2) -0.008(2) -0.0108(19) C10 0.037(2) 0.0337(19) 0.0240(19) -0.0006(15) -0.0004(16) -0.0049(17) C11 0.050(3) 0.035(2) 0.055(3) 0.0052(19) 0.001(2) -0.0076(19) C12 0.039(2) 0.048(2) 0.073(3) -0.007(2) 0.011(2) -0.003(2) C13 0.0244(17) 0.0226(16) 0.0191(17) -0.0059(13) -0.0052(14) 0.0016(14) C14 0.033(2) 0.0259(17) 0.0263(19) -0.0047(15) -0.0066(16) -0.0050(15) C15 0.038(2) 0.0351(19) 0.034(2) -0.0029(17) -0.0117(17) -0.0121(17) C16 0.046(2) 0.042(2) 0.029(2) 0.0001(17) -0.0190(18) -0.0076(19) C17 0.040(2) 0.0302(19) 0.0265(19) -0.0003(15) -0.0062(16) -0.0036(17) C18 0.0290(19) 0.0244(17) 0.0206(17) -0.0037(14) -0.0051(15) -0.0011(15) C19 0.051(2) 0.0272(18) 0.032(2) -0.0005(16) -0.0134(18) -0.0117(17) C20 0.083(3) 0.032(2) 0.038(2) 0.0031(17) -0.019(2) -0.012(2) C21 0.063(3) 0.063(3) 0.052(3) 0.016(2) -0.001(2) -0.028(2) C22 0.034(2) 0.0278(18) 0.0253(19) -0.0013(15) -0.0035(15) -0.0051(15) C23 0.039(2) 0.049(2) 0.051(3) -0.004(2) -0.0004(19) -0.0060(19) C24 0.057(3) 0.0280(19) 0.051(2) 0.0056(18) -0.015(2) -0.0068(19) C25 0.0222(17) 0.0190(16) 0.0219(17) 0.0009(13) -0.0047(14) -0.0026(13) C26 0.0278(19) 0.0192(16) 0.0177(16) -0.0019(13) -0.0071(14) -0.0024(14) C27 0.0309(19) 0.0251(17) 0.0274(19) -0.0019(14) -0.0085(15) -0.0026(15) C28 0.044(2) 0.0196(17) 0.029(2) -0.0011(14) -0.0094(16) -0.0008(16) C29 0.031(2) 0.0216(17) 0.0229(18) -0.0024(14) -0.0057(15) 0.0068(15) C30 0.0252(18) 0.0340(19) 0.0269(19) -0.0074(15) -0.0035(15) 0.0026(16) C31 0.031(2) 0.0222(17) 0.0245(18) -0.0026(14) -0.0041(15) -0.0029(15) C32 0.045(2) 0.0302(19) 0.031(2) -0.0049(16) -0.0069(17) 0.0100(17) C33 0.048(2) 0.042(2) 0.039(2) -0.0091(18) -0.0055(19) -0.0038(19) C34 0.038(2) 0.055(2) 0.042(2) -0.0151(19) -0.0062(18) 0.0001(19) C35 0.089(4) 0.057(3) 0.076(4) -0.031(3) 0.024(3) -0.011(3) C36 0.068(3) 0.040(2) 0.078(3) -0.031(2) 0.022(3) -0.002(2) C37 0.042(2) 0.048(2) 0.052(3) 0.005(2) -0.018(2) -0.005(2) C38 0.055(3) 0.061(3) 0.058(3) 0.024(2) -0.018(2) 0.000(2) C39 0.081(4) 0.047(3) 0.068(3) 0.013(2) -0.030(3) -0.009(2) C40 0.064(3) 0.041(2) 0.059(3) -0.004(2) -0.024(2) -0.006(2) _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 O1 C33 1.431(4) . ? O1 C36 1.439(4) . ? O1 Li1 1.955(6) . ? N1 C25 1.327(4) . ? N1 C1 1.421(3) . ? N1 Li1 2.032(6) . ? C1 C2 1.397(4) . ? C1 C6 1.424(4) . ? Li1 O2 1.966(6) . ? Li1 N2 2.057(6) . ? Li1 C25 2.400(6) . ? O2 C37 1.434(4) . ? O2 C40 1.437(4) . ? N2 C25 1.330(3) . ? N2 C13 1.412(4) . ? C2 C3 1.382(4) . ? C2 C7 1.520(5) . ? C3 C4 1.389(5) . ? C4 C5 1.367(4) . ? C5 C6 1.401(4) . ? C6 C10 1.516(4) . ? C7 C9 1.522(4) . ? C7 C8 1.532(4) . ? C10 C11 1.524(4) . ? C10 C12 1.532(5) . ? C13 C14 1.395(4) . ? C13 C18 1.423(4) . ? C14 C15 1.395(4) . ? C14 C19 1.520(4) . ? C15 C16 1.386(5) . ? C16 C17 1.378(4) . ? C17 C18 1.393(4) . ? C18 C22 1.504(4) . ? C19 C20 1.525(4) . ? C19 C21 1.532(5) . ? C22 C24 1.529(4) . ? C22 C23 1.540(5) . ? C25 C26 1.508(4) . ? C26 C31 1.380(4) . ? C26 C27 1.390(4) . ? C27 C28 1.395(4) . ? C28 C29 1.379(4) . ? C29 C30 1.377(4) . ? C29 C32 1.511(4) . ? C30 C31 1.390(4) . ? C33 C34 1.528(5) . ? C34 C35 1.498(5) . ? C35 C36 1.475(6) . ? C37 C38 1.523(5) . ? C38 C39 1.463(6) . ? C39 C40 1.506(5) . ? 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 C33 O1 C36 109.7(3) . . ? C33 O1 Li1 127.8(3) . . ? C36 O1 Li1 118.2(3) . . ? C25 N1 C1 121.6(2) . . ? C25 N1 Li1 88.6(2) . . ? C1 N1 Li1 148.1(2) . . ? C2 C1 N1 119.3(3) . . ? C2 C1 C6 120.0(3) . . ? N1 C1 C6 120.6(3) . . ? O1 Li1 O2 96.8(3) . . ? O1 Li1 N1 126.3(3) . . ? O2 Li1 N1 119.9(3) . . ? O1 Li1 N2 117.6(3) . . ? O2 Li1 N2 130.9(3) . . ? N1 Li1 N2 67.16(19) . . ? O1 Li1 C25 128.6(3) . . ? O2 Li1 C25 134.5(3) . . ? N1 Li1 C25 33.56(12) . . ? N2 Li1 C25 33.61(12) . . ? C37 O2 C40 109.2(3) . . ? C37 O2 Li1 118.9(3) . . ? C40 O2 Li1 130.5(3) . . ? C25 N2 C13 122.3(2) . . ? C25 N2 Li1 87.5(2) . . ? C13 N2 Li1 148.8(2) . . ? C3 C2 C1 119.6(3) . . ? C3 C2 C7 120.7(3) . . ? C1 C2 C7 119.7(3) . . ? C2 C3 C4 121.2(3) . . ? C5 C4 C3 119.4(3) . . ? C4 C5 C6 122.0(3) . . ? C5 C6 C1 117.8(3) . . ? C5 C6 C10 121.2(3) . . ? C1 C6 C10 120.8(3) . . ? C2 C7 C9 113.5(3) . . ? C2 C7 C8 110.7(3) . . ? C9 C7 C8 110.0(3) . . ? C6 C10 C11 109.7(3) . . ? C6 C10 C12 114.9(3) . . ? C11 C10 C12 108.9(3) . . ? C14 C13 N2 118.4(3) . . ? C14 C13 C18 119.7(3) . . ? N2 C13 C18 121.7(3) . . ? C13 C14 C15 120.1(3) . . ? C13 C14 C19 120.5(3) . . ? C15 C14 C19 119.5(3) . . ? C16 C15 C14 120.5(3) . . ? C17 C16 C15 119.5(3) . . ? C16 C17 C18 122.0(3) . . ? C17 C18 C13 118.2(3) . . ? C17 C18 C22 119.6(3) . . ? C13 C18 C22 122.1(3) . . ? C14 C19 C20 110.6(3) . . ? C14 C19 C21 113.6(3) . . ? C20 C19 C21 110.3(3) . . ? C18 C22 C24 114.2(3) . . ? C18 C22 C23 108.5(3) . . ? C24 C22 C23 110.3(3) . . ? N1 C25 N2 116.7(3) . . ? N1 C25 C26 121.9(3) . . ? N2 C25 C26 121.4(3) . . ? N1 C25 Li1 57.8(2) . . ? N2 C25 Li1 58.9(2) . . ? C26 C25 Li1 177.1(3) . . ? C31 C26 C27 117.8(3) . . ? C31 C26 C25 122.0(3) . . ? C27 C26 C25 120.2(3) . . ? C26 C27 C28 120.3(3) . . ? C29 C28 C27 121.7(3) . . ? C30 C29 C28 117.7(3) . . ? C30 C29 C32 121.2(3) . . ? C28 C29 C32 121.1(3) . . ? C29 C30 C31 121.2(3) . . ? C26 C31 C30 121.3(3) . . ? O1 C33 C34 106.0(3) . . ? C35 C34 C33 102.6(3) . . ? C36 C35 C34 104.5(3) . . ? O1 C36 C35 106.7(3) . . ? O2 C37 C38 105.3(3) . . ? C39 C38 C37 103.2(3) . . ? C38 C39 C40 102.8(4) . . ? O2 C40 C39 105.6(3) . . ? _diffrn_measured_fraction_theta_max 0.974 _diffrn_reflns_theta_full 27.73 _diffrn_measured_fraction_theta_full 0.974 _refine_diff_density_max 0.405 _refine_diff_density_min -0.323 _refine_diff_density_rms 0.066 #===END data_Compound_2 _database_code_depnum_ccdc_archive 'CCDC 242106' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common "[Mg(N,N'-Dipamidine)2]" _chemical_melting_point '551 dec.' _chemical_formula_moiety 'C64 H82 Mg N4' _chemical_formula_sum 'C32 H41 Mg0.50 N2' _chemical_formula_weight 465.82 _ccdc_chemical_compound_source_recrystallisation THF 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' Mg Mg 0.0486 0.0363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c _symmetry_Int_Tables_number 15 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 23.4090(11) _cell_length_b 10.6758(4) _cell_length_c 25.0402(12) _cell_angle_alpha 90.00 _cell_angle_beta 114.337(3) _cell_angle_gamma 90.00 _cell_volume 5701.7(4) _cell_formula_units_Z 8 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour 'light yellow' _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.085 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2024 _exptl_absorpt_coefficient_mu 0.072 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.9857 _exptl_absorpt_correction_T_max 0.9964 _exptl_absorpt_process_details 'performed as part of the DENZO-SMN package' _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_probe x-ray _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_measurement_method 'psi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 30267 _diffrn_reflns_av_R_equivalents 0.1902 _diffrn_reflns_av_sigmaI/netI 0.2368 _diffrn_reflns_limit_h_min -30 _diffrn_reflns_limit_h_max 30 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 2.01 _diffrn_reflns_theta_max 27.84 _reflns_number_total 6614 _reflns_number_gt 2563 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Nonius Collect' _computing_cell_refinement DENZO-SMN _computing_data_reduction X-Seed _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'X-Seed / POV-Ray' _computing_publication_material 'Microsoft Office 2000' _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^)+(0.0865P)^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_number_reflns 6614 _refine_ls_number_parameters 332 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.2285 _refine_ls_R_factor_gt 0.0666 _refine_ls_wR_factor_ref 0.1947 _refine_ls_wR_factor_gt 0.1387 _refine_ls_goodness_of_fit_ref 0.908 _refine_ls_restrained_S_all 0.908 _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 Mg1 Mg 0.5000 0.27415(12) 0.2500 0.0204(3) Uani 1 2 d S . . N1 N 0.58231(10) 0.25942(19) 0.24018(9) 0.0198(5) Uani 1 1 d . . . N2 N 0.49013(10) 0.28332(19) 0.16408(9) 0.0191(5) Uani 1 1 d . . . C1 C 0.64503(12) 0.2165(3) 0.26975(11) 0.0196(6) Uani 1 1 d . . . C2 C 0.68778(13) 0.2946(2) 0.31385(11) 0.0224(7) Uani 1 1 d . . . C3 C 0.74976(14) 0.2539(3) 0.34214(12) 0.0292(8) Uani 1 1 d . . . H3 H 0.7795 0.3051 0.3715 0.035 Uiso 1 1 calc R . . C4 C 0.76889(15) 0.1399(3) 0.32820(13) 0.0356(8) Uani 1 1 d . . . H4 H 0.8117 0.1154 0.3467 0.043 Uiso 1 1 calc R . . C5 C 0.72573(14) 0.0627(3) 0.28762(12) 0.0320(8) Uani 1 1 d . . . H5 H 0.7390 -0.0159 0.2789 0.038 Uiso 1 1 calc R . . C6 C 0.66291(13) 0.0972(3) 0.25888(11) 0.0245(7) Uani 1 1 d . . . C7 C 0.66642(14) 0.4180(3) 0.33016(11) 0.0281(7) Uani 1 1 d . . . H7 H 0.6233 0.4038 0.3281 0.034 Uiso 1 1 calc R . . C8 C 0.70735(15) 0.4622(3) 0.39264(13) 0.0400(9) Uani 1 1 d . . . H8A H 0.7112 0.3947 0.4204 0.060 Uiso 1 1 calc R . . H8B H 0.6880 0.5355 0.4020 0.060 Uiso 1 1 calc R . . H8C H 0.7491 0.4848 0.3954 0.060 Uiso 1 1 calc R . . C9 C 0.66118(16) 0.5231(3) 0.28673(13) 0.0373(8) Uani 1 1 d . . . H9A H 0.7026 0.5394 0.2871 0.056 Uiso 1 1 calc R . . H9B H 0.6456 0.5993 0.2980 0.056 Uiso 1 1 calc R . . H9C H 0.6321 0.4978 0.2472 0.056 Uiso 1 1 calc R . . C10 C 0.61537(15) 0.0027(3) 0.21952(13) 0.0330(8) Uani 1 1 d . . . H10 H 0.5757 0.0492 0.1964 0.040 Uiso 1 1 calc R . . C11 C 0.6010(2) -0.0933(3) 0.25741(16) 0.0721(13) Uani 1 1 d . . . H11A H 0.5695 -0.1527 0.2322 0.108 Uiso 1 1 calc R . . H11B H 0.5849 -0.0503 0.2829 0.108 Uiso 1 1 calc R . . H11C H 0.6394 -0.1387 0.2815 0.108 Uiso 1 1 calc R . . C12 C 0.63629(18) -0.0603(4) 0.17613(16) 0.0661(12) Uani 1 1 d . . . H12A H 0.6482 0.0037 0.1546 0.099 Uiso 1 1 calc R . . H12B H 0.6018 -0.1107 0.1485 0.099 Uiso 1 1 calc R . . H12C H 0.6723 -0.1146 0.1973 0.099 Uiso 1 1 calc R . . C13 C 0.44840(12) 0.3202(3) 0.10646(11) 0.0202(7) Uani 1 1 d . . . C14 C 0.39828(13) 0.2386(3) 0.07461(11) 0.0244(7) Uani 1 1 d . . . C15 C 0.35692(14) 0.2744(3) 0.01819(12) 0.0318(8) Uani 1 1 d . . . H15 H 0.3236 0.2201 -0.0044 0.038 Uiso 1 1 calc R . . C16 C 0.36369(14) 0.3873(3) -0.00524(13) 0.0367(8) Uani 1 1 d . . . H16 H 0.3356 0.4094 -0.0439 0.044 Uiso 1 1 calc R . . C17 C 0.41126(14) 0.4683(3) 0.02741(12) 0.0321(8) Uani 1 1 d . . . H17 H 0.4152 0.5462 0.0109 0.039 Uiso 1 1 calc R . . C18 C 0.45369(13) 0.4382(3) 0.08419(11) 0.0235(7) Uani 1 1 d . B . C19 C 0.38935(13) 0.1155(3) 0.10093(13) 0.0281(7) Uani 1 1 d . . . H19 H 0.4021 0.1305 0.1437 0.034 Uiso 1 1 calc R . . C20 C 0.32174(14) 0.0687(3) 0.07609(13) 0.0379(8) Uani 1 1 d . . . H20A H 0.2941 0.1362 0.0778 0.057 Uiso 1 1 calc R . . H20B H 0.3185 -0.0027 0.0993 0.057 Uiso 1 1 calc R . . H20C H 0.3092 0.0426 0.0353 0.057 Uiso 1 1 calc R . . C21 C 0.43200(15) 0.0116(3) 0.09560(14) 0.0404(9) Uani 1 1 d . . . H21A H 0.4230 -0.0017 0.0542 0.061 Uiso 1 1 calc R . . H21B H 0.4243 -0.0661 0.1124 0.061 Uiso 1 1 calc R . . H21C H 0.4760 0.0364 0.1168 0.061 Uiso 1 1 calc R . . C22 C 0.50114(14) 0.5344(3) 0.12055(13) 0.0293(7) Uani 1 1 d . . . H22 H 0.5323 0.4941 0.1570 0.035 Uiso 1 1 calc R A 1 C23A C 0.4653(4) 0.6386(14) 0.1372(7) 0.051(3) Uani 0.72(3) 1 d P B 1 H23A H 0.4361 0.6806 0.1016 0.076 Uiso 0.72(3) 1 calc PR B 1 H23B H 0.4953 0.6999 0.1628 0.076 Uiso 0.72(3) 1 calc PR B 1 H23C H 0.4417 0.6013 0.1577 0.076 Uiso 0.72(3) 1 calc PR B 1 C23B C 0.4802(15) 0.598(3) 0.167(2) 0.053(8) Uani 0.28(3) 1 d P B 2 H23D H 0.4410 0.6443 0.1462 0.079 Uiso 0.28(3) 1 calc PR B 2 H23E H 0.5129 0.6563 0.1915 0.079 Uiso 0.28(3) 1 calc PR B 2 H23F H 0.4737 0.5335 0.1916 0.079 Uiso 0.28(3) 1 calc PR B 2 C24 C 0.53485(18) 0.5984(4) 0.08849(16) 0.0776(14) Uani 1 1 d . B . H24A H 0.5559 0.5355 0.0744 0.116 Uiso 1 1 calc R . . H24B H 0.5660 0.6565 0.1151 0.116 Uiso 1 1 calc R . . H24C H 0.5046 0.6449 0.0550 0.116 Uiso 1 1 calc R . . C25 C 0.55228(13) 0.2701(2) 0.18149(11) 0.0192(6) Uani 1 1 d . . . C26 C 0.58482(13) 0.2665(2) 0.14107(11) 0.0212(7) Uani 1 1 d . . . C27 C 0.64524(13) 0.3147(2) 0.15835(12) 0.0246(7) Uani 1 1 d . . . H27 H 0.6654 0.3524 0.1959 0.029 Uiso 1 1 calc R . . C28 C 0.67651(14) 0.3085(3) 0.12166(12) 0.0283(7) Uani 1 1 d . . . H28 H 0.7175 0.3429 0.1345 0.034 Uiso 1 1 calc R . . C29 C 0.64900(14) 0.2530(2) 0.06650(12) 0.0250(7) Uani 1 1 d . . . C30 C 0.58901(14) 0.2058(3) 0.04965(12) 0.0277(7) Uani 1 1 d . . . H30 H 0.5690 0.1676 0.0122 0.033 Uiso 1 1 calc R . . C31 C 0.55717(14) 0.2124(2) 0.08561(11) 0.0249(7) Uani 1 1 d . . . H31 H 0.5159 0.1796 0.0722 0.030 Uiso 1 1 calc R . . C32 C 0.68357(15) 0.2462(3) 0.02761(13) 0.0344(8) Uani 1 1 d . . . H32A H 0.6579 0.2014 -0.0085 0.052 Uiso 1 1 calc R . . H32B H 0.7232 0.2015 0.0480 0.052 Uiso 1 1 calc R . . H32C H 0.6921 0.3311 0.0180 0.052 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 Mg1 0.0148(8) 0.0289(7) 0.0163(7) 0.000 0.0054(6) 0.000 N1 0.0125(13) 0.0289(13) 0.0146(13) -0.0010(10) 0.0023(11) 0.0009(10) N2 0.0096(13) 0.0284(13) 0.0165(13) -0.0023(10) 0.0026(11) -0.0001(11) C1 0.0120(15) 0.0309(16) 0.0163(15) 0.0035(12) 0.0062(13) 0.0008(13) C2 0.0175(16) 0.0319(17) 0.0182(16) 0.0035(13) 0.0077(14) -0.0041(14) C3 0.0152(17) 0.048(2) 0.0202(16) 0.0049(14) 0.0028(14) -0.0069(14) C4 0.0216(19) 0.054(2) 0.0298(19) 0.0137(16) 0.0096(16) 0.0079(17) C5 0.0258(19) 0.0425(19) 0.0268(18) 0.0055(15) 0.0098(16) 0.0097(16) C6 0.0186(17) 0.0334(17) 0.0204(16) 0.0031(13) 0.0070(14) 0.0034(14) C7 0.0231(18) 0.0403(19) 0.0197(16) -0.0037(14) 0.0076(14) -0.0068(14) C8 0.030(2) 0.053(2) 0.034(2) -0.0119(16) 0.0101(17) -0.0124(17) C9 0.045(2) 0.0362(19) 0.0349(19) -0.0034(15) 0.0202(18) -0.0026(16) C10 0.031(2) 0.0295(17) 0.0346(19) -0.0032(14) 0.0092(17) 0.0055(15) C11 0.092(4) 0.056(2) 0.056(3) -0.007(2) 0.018(2) -0.038(2) C12 0.061(3) 0.074(3) 0.061(3) -0.029(2) 0.023(2) 0.012(2) C13 0.0101(15) 0.0356(17) 0.0135(15) 0.0002(13) 0.0034(13) 0.0031(13) C14 0.0188(17) 0.0345(17) 0.0174(16) -0.0030(13) 0.0050(14) 0.0034(14) C15 0.0163(17) 0.052(2) 0.0221(17) -0.0073(15) 0.0026(14) -0.0017(15) C16 0.0236(19) 0.062(2) 0.0182(17) 0.0068(16) 0.0018(15) 0.0054(17) C17 0.028(2) 0.0407(19) 0.0261(18) 0.0086(15) 0.0094(16) 0.0052(16) C18 0.0170(17) 0.0327(17) 0.0188(16) 0.0000(13) 0.0052(14) 0.0030(14) C19 0.0200(18) 0.0349(18) 0.0265(17) -0.0057(13) 0.0066(14) -0.0008(14) C20 0.0255(19) 0.047(2) 0.040(2) -0.0106(16) 0.0127(17) -0.0088(16) C21 0.033(2) 0.0362(19) 0.051(2) -0.0046(16) 0.0169(18) -0.0034(16) C22 0.0264(18) 0.0306(17) 0.0295(18) 0.0049(14) 0.0099(16) -0.0017(15) C23A 0.037(5) 0.042(6) 0.070(6) -0.020(4) 0.018(4) -0.009(4) C23B 0.038(13) 0.035(11) 0.09(2) -0.016(11) 0.026(15) 0.000(10) C24 0.054(3) 0.117(4) 0.050(3) 0.020(2) 0.009(2) -0.043(3) C25 0.0168(16) 0.0202(15) 0.0181(16) -0.0019(12) 0.0046(13) -0.0015(13) C26 0.0169(16) 0.0286(16) 0.0177(15) -0.0024(13) 0.0066(13) 0.0006(13) C27 0.0198(17) 0.0349(18) 0.0204(16) -0.0043(13) 0.0096(14) -0.0040(14) C28 0.0198(17) 0.0383(18) 0.0283(18) -0.0026(14) 0.0114(15) -0.0033(14) C29 0.0234(18) 0.0335(17) 0.0230(17) 0.0024(13) 0.0145(15) 0.0046(14) C30 0.0274(19) 0.0392(18) 0.0192(16) -0.0048(13) 0.0122(15) 0.0032(15) C31 0.0188(16) 0.0335(17) 0.0226(17) -0.0048(13) 0.0088(14) -0.0030(14) C32 0.034(2) 0.044(2) 0.0326(19) 0.0023(15) 0.0213(16) 0.0036(16) _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 Mg1 N1 2.047(2) . ? Mg1 N1 2.047(2) 2_655 ? Mg1 N2 2.069(2) 2_655 ? Mg1 N2 2.069(2) . ? Mg1 C25 2.485(3) . ? Mg1 C25 2.485(3) 2_655 ? N1 C25 1.347(3) . ? N1 C1 1.420(3) . ? N2 C25 1.343(3) . ? N2 C13 1.424(3) . ? C1 C6 1.402(4) . ? C1 C2 1.416(4) . ? C2 C3 1.396(4) . ? C2 C7 1.523(4) . ? C3 C4 1.390(4) . ? C4 C5 1.373(4) . ? C5 C6 1.394(4) . ? C6 C10 1.524(4) . ? C7 C9 1.532(4) . ? C7 C8 1.534(4) . ? C10 C12 1.520(4) . ? C10 C11 1.526(4) . ? C13 C18 1.404(4) . ? C13 C14 1.414(4) . ? C14 C15 1.397(4) . ? C14 C19 1.523(4) . ? C15 C16 1.378(4) . ? C16 C17 1.381(4) . ? C17 C18 1.396(4) . ? C18 C22 1.512(4) . ? C19 C20 1.526(4) . ? C19 C21 1.534(4) . ? C22 C24 1.502(4) . ? C22 C23A 1.551(10) . ? C22 C23B 1.59(3) . ? C25 C26 1.497(4) . ? C26 C31 1.393(4) . ? C26 C27 1.395(4) . ? C27 C28 1.393(4) . ? C28 C29 1.393(4) . ? C29 C30 1.384(4) . ? C29 C32 1.503(4) . ? C30 C31 1.387(4) . ? 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 Mg1 N1 171.19(13) . 2_655 ? N1 Mg1 N2 114.91(8) . 2_655 ? N1 Mg1 N2 65.54(8) 2_655 2_655 ? N1 Mg1 N2 65.54(8) . . ? N1 Mg1 N2 114.91(8) 2_655 . ? N2 Mg1 N2 174.58(13) 2_655 . ? N1 Mg1 C25 32.82(8) . . ? N1 Mg1 C25 146.89(8) 2_655 . ? N2 Mg1 C25 147.45(8) 2_655 . ? N2 Mg1 C25 32.72(8) . . ? N1 Mg1 C25 146.89(8) . 2_655 ? N1 Mg1 C25 32.82(8) 2_655 2_655 ? N2 Mg1 C25 32.72(8) 2_655 2_655 ? N2 Mg1 C25 147.45(8) . 2_655 ? C25 Mg1 C25 178.01(13) . 2_655 ? C25 N1 C1 123.9(2) . . ? C25 N1 Mg1 91.76(16) . . ? C1 N1 Mg1 141.65(17) . . ? C25 N2 C13 123.8(2) . . ? C25 N2 Mg1 90.89(16) . . ? C13 N2 Mg1 143.35(18) . . ? C6 C1 C2 121.0(2) . . ? C6 C1 N1 121.3(2) . . ? C2 C1 N1 117.6(2) . . ? C3 C2 C1 117.7(3) . . ? C3 C2 C7 121.4(3) . . ? C1 C2 C7 120.9(2) . . ? C4 C3 C2 121.3(3) . . ? C5 C4 C3 119.7(3) . . ? C4 C5 C6 121.4(3) . . ? C5 C6 C1 118.4(3) . . ? C5 C6 C10 119.5(3) . . ? C1 C6 C10 122.0(2) . . ? C2 C7 C9 112.5(2) . . ? C2 C7 C8 113.8(2) . . ? C9 C7 C8 109.4(2) . . ? C12 C10 C6 113.0(3) . . ? C12 C10 C11 111.4(3) . . ? C6 C10 C11 109.4(2) . . ? C18 C13 C14 121.1(2) . . ? C18 C13 N2 121.0(2) . . ? C14 C13 N2 117.7(2) . . ? C15 C14 C13 118.0(3) . . ? C15 C14 C19 120.8(3) . . ? C13 C14 C19 121.1(2) . . ? C16 C15 C14 121.1(3) . . ? C15 C16 C17 120.1(3) . . ? C16 C17 C18 121.4(3) . . ? C17 C18 C13 118.0(3) . . ? C17 C18 C22 119.6(3) . . ? C13 C18 C22 122.3(2) . . ? C14 C19 C20 114.2(2) . . ? C14 C19 C21 112.1(2) . . ? C20 C19 C21 109.3(2) . . ? C24 C22 C18 113.9(3) . . ? C24 C22 C23A 106.2(7) . . ? C18 C22 C23A 107.7(4) . . ? C24 C22 C23B 125.8(11) . . ? C18 C22 C23B 111.1(9) . . ? C23A C22 C23B 29.7(12) . . ? N2 C25 N1 111.8(2) . . ? N2 C25 C26 124.6(2) . . ? N1 C25 C26 123.6(2) . . ? N2 C25 Mg1 56.39(13) . . ? N1 C25 Mg1 55.42(14) . . ? C26 C25 Mg1 178.9(2) . . ? C31 C26 C27 117.2(3) . . ? C31 C26 C25 121.9(2) . . ? C27 C26 C25 120.9(2) . . ? C28 C27 C26 121.3(3) . . ? C27 C28 C29 121.3(3) . . ? C30 C29 C28 117.0(3) . . ? C30 C29 C32 122.3(3) . . ? C28 C29 C32 120.7(3) . . ? C29 C30 C31 122.2(3) . . ? C30 C31 C26 121.0(3) . . ? _diffrn_measured_fraction_theta_max 0.976 _diffrn_reflns_theta_full 27.84 _diffrn_measured_fraction_theta_full 0.976 _refine_diff_density_max 0.323 _refine_diff_density_min -0.378 _refine_diff_density_rms 0.075 #===END data_Compound_3 _database_code_depnum_ccdc_archive 'CCDC 242107' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common "[Al(N,N'-Dipamidine)(Me)2]" _chemical_melting_point '> 633' _chemical_formula_moiety 'C34 H47 Al N2' _chemical_formula_sum 'C34 H47 Al N2' _chemical_formula_weight 510.72 _ccdc_chemical_compound_source_recrystallisation Et2O 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 trigonal _symmetry_space_group_name_H-M P31 _symmetry_Int_Tables_number 144 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z+1/3' '-x+y, -x, z+2/3' _cell_length_a 15.2283(4) _cell_length_b 15.2283(4) _cell_length_c 12.0910(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 2428.26(10) _cell_formula_units_Z 3 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'irregular plate' _exptl_crystal_colour colourless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.048 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 834 _exptl_absorpt_coefficient_mu 0.085 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.9668 _exptl_absorpt_correction_T_max 0.9915 _exptl_absorpt_process_details 'performed as part of the DENZO-SMN package' _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_probe x-ray _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_measurement_method 'psi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17025 _diffrn_reflns_av_R_equivalents 0.0674 _diffrn_reflns_av_sigmaI/netI 0.0764 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 4.30 _diffrn_reflns_theta_max 28.09 _reflns_number_total 7271 _reflns_number_gt 5655 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Nonius Collect' _computing_cell_refinement DENZO-SMN _computing_data_reduction X-Seed _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'X-Seed / POV-Ray' _computing_publication_material 'Microsoft Office 2000' _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^)+(0.0368P)^2^+0.5040P] 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 0.0055(15) _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.01(15) _refine_ls_number_reflns 7271 _refine_ls_number_parameters 365 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0783 _refine_ls_R_factor_gt 0.0477 _refine_ls_wR_factor_ref 0.1117 _refine_ls_wR_factor_gt 0.0946 _refine_ls_goodness_of_fit_ref 1.063 _refine_ls_restrained_S_all 1.063 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Al1 Al 0.51392(4) 0.51406(4) 0.03170(7) 0.02359(14) Uani 1 1 d . . . N1 N 0.59173(12) 0.64684(12) -0.03627(14) 0.0189(4) Uani 1 1 d . . . N2 N 0.64659(12) 0.59152(12) 0.09985(14) 0.0193(4) Uani 1 1 d . . . C1 C 0.60170(15) 0.70255(15) -0.13532(18) 0.0204(4) Uani 1 1 d . . . C2 C 0.55237(16) 0.75986(16) -0.14164(19) 0.0251(5) Uani 1 1 d . . . C3 C 0.56362(18) 0.81422(18) -0.2382(2) 0.0333(5) Uani 1 1 d . . . H3 H 0.5306 0.8529 -0.2445 0.040 Uiso 1 1 calc R . . C4 C 0.6219(2) 0.81307(19) -0.3251(2) 0.0369(6) Uani 1 1 d . . . H4 H 0.6299 0.8519 -0.3897 0.044 Uiso 1 1 calc R . . C5 C 0.66843(19) 0.75555(18) -0.3181(2) 0.0331(5) Uani 1 1 d . . . H5 H 0.7083 0.7552 -0.3783 0.040 Uiso 1 1 calc R . . C6 C 0.65823(16) 0.69781(16) -0.22428(19) 0.0248(5) Uani 1 1 d . . . C7 C 0.48633(17) 0.76012(18) -0.0476(2) 0.0298(5) Uani 1 1 d . . . H7 H 0.5059 0.7370 0.0207 0.036 Uiso 1 1 calc R . . C8 C 0.37515(19) 0.6843(2) -0.0713(2) 0.0459(7) Uani 1 1 d . . . H8A H 0.3536 0.7052 -0.1377 0.069 Uiso 1 1 calc R . . H8B H 0.3336 0.6819 -0.0083 0.069 Uiso 1 1 calc R . . H8C H 0.3669 0.6169 -0.0831 0.069 Uiso 1 1 calc R . . C9 C 0.4999(2) 0.8647(2) -0.0235(3) 0.0479(7) Uani 1 1 d . . . H9A H 0.5718 0.9133 -0.0107 0.072 Uiso 1 1 calc R . . H9B H 0.4608 0.8610 0.0425 0.072 Uiso 1 1 calc R . . H9C H 0.4757 0.8870 -0.0868 0.072 Uiso 1 1 calc R . . C10 C 0.70433(17) 0.62904(17) -0.2245(2) 0.0281(5) Uani 1 1 d . . . H10 H 0.6912 0.5955 -0.1504 0.034 Uiso 1 1 calc R . . C11 C 0.6524(2) 0.54586(19) -0.3116(2) 0.0384(6) Uani 1 1 d . . . H11A H 0.5790 0.5095 -0.2992 0.058 Uiso 1 1 calc R . . H11B H 0.6778 0.4983 -0.3061 0.058 Uiso 1 1 calc R . . H11C H 0.6671 0.5765 -0.3855 0.058 Uiso 1 1 calc R . . C12 C 0.81865(19) 0.6871(2) -0.2428(3) 0.0451(7) Uani 1 1 d . . . H12A H 0.8334 0.7156 -0.3176 0.068 Uiso 1 1 calc R . . H12B H 0.8455 0.6409 -0.2341 0.068 Uiso 1 1 calc R . . H12C H 0.8506 0.7420 -0.1885 0.068 Uiso 1 1 calc R . . C13 C 0.70225(15) 0.60152(15) 0.19919(18) 0.0206(4) Uani 1 1 d . . . C14 C 0.75953(16) 0.55185(16) 0.20517(19) 0.0247(5) Uani 1 1 d . . . C15 C 0.81407(18) 0.56324(18) 0.3018(2) 0.0329(5) Uani 1 1 d . . . H15 H 0.8529 0.5304 0.3079 0.039 Uiso 1 1 calc R . . C16 C 0.81286(19) 0.6212(2) 0.3888(2) 0.0366(6) Uani 1 1 d . . . H16 H 0.8516 0.6291 0.4535 0.044 Uiso 1 1 calc R . . C17 C 0.75502(18) 0.66776(18) 0.3816(2) 0.0329(5) Uani 1 1 d . . . H17 H 0.7543 0.7074 0.4420 0.039 Uiso 1 1 calc R . . C18 C 0.69777(15) 0.65780(16) 0.28792(19) 0.0236(5) Uani 1 1 d . . . C19 C 0.75980(18) 0.48628(17) 0.1108(2) 0.0299(5) Uani 1 1 d . . . H19 H 0.7367 0.5061 0.0427 0.036 Uiso 1 1 calc R . . C20 C 0.6836(2) 0.37486(19) 0.1347(3) 0.0465(7) Uani 1 1 d . . . H20A H 0.7042 0.3534 0.2015 0.070 Uiso 1 1 calc R . . H20B H 0.6817 0.3332 0.0720 0.070 Uiso 1 1 calc R . . H20C H 0.6162 0.3666 0.1459 0.070 Uiso 1 1 calc R . . C21 C 0.8645(2) 0.4997(2) 0.0868(3) 0.0483(7) Uani 1 1 d . . . H21A H 0.9127 0.5714 0.0720 0.073 Uiso 1 1 calc R . . H21B H 0.8604 0.4591 0.0220 0.073 Uiso 1 1 calc R . . H21C H 0.8876 0.4773 0.1509 0.073 Uiso 1 1 calc R . . C22 C 0.62889(17) 0.70423(17) 0.2881(2) 0.0281(5) Uani 1 1 d . . . H22 H 0.5954 0.6912 0.2140 0.034 Uiso 1 1 calc R . . C23 C 0.54576(19) 0.6523(2) 0.3755(2) 0.0380(6) Uani 1 1 d . . . H23A H 0.5087 0.5790 0.3625 0.057 Uiso 1 1 calc R . . H23B H 0.4988 0.6785 0.3709 0.057 Uiso 1 1 calc R . . H23C H 0.5766 0.6662 0.4493 0.057 Uiso 1 1 calc R . . C24 C 0.6874(2) 0.81898(19) 0.3069(3) 0.0426(7) Uani 1 1 d . . . H24A H 0.7159 0.8334 0.3818 0.064 Uiso 1 1 calc R . . H24B H 0.6414 0.8460 0.2983 0.064 Uiso 1 1 calc R . . H24C H 0.7425 0.8510 0.2528 0.064 Uiso 1 1 calc R . . C25 C 0.66938(14) 0.66937(14) 0.03190(19) 0.0181(4) Uani 1 1 d . . . C26 C 0.76618(14) 0.76646(15) 0.0319(2) 0.0242(4) Uani 1 1 d . . . C27 C 0.76767(19) 0.85751(17) 0.0169(2) 0.0369(6) Uani 1 1 d . B . H27 H 0.7060 0.8575 0.0051 0.044 Uiso 1 1 calc R . . C28 C 0.8582(2) 0.9480(2) 0.0189(4) 0.0775(13) Uani 1 1 d . . . H28 H 0.8605 1.0077 -0.0082 0.093 Uiso 1 1 calc R A 1 C29A C 0.9464(12) 0.9535(13) 0.060(3) 0.057(5) Uani 0.47(5) 1 d P B 1 C29B C 0.9522(12) 0.9461(11) 0.007(3) 0.066(4) Uani 0.53(5) 1 d P B 2 C30 C 0.9477(2) 0.8583(2) 0.0477(4) 0.0774(13) Uani 1 1 d . . . H30 H 1.0103 0.8593 0.0399 0.093 Uiso 1 1 calc R B 1 C31 C 0.85743(17) 0.76748(19) 0.0477(2) 0.0379(6) Uani 1 1 d . B . H31 H 0.8574 0.7056 0.0583 0.046 Uiso 1 1 calc R . . C32A C 1.0417(11) 1.0556(11) 0.073(4) 0.105(8) Uani 0.47(5) 1 d P B 1 H32A H 1.0997 1.0457 0.0857 0.157 Uiso 0.47(5) 1 calc PR B 1 H32B H 1.0339 1.0912 0.1370 0.157 Uiso 0.47(5) 1 calc PR B 1 H32C H 1.0530 1.0961 0.0064 0.157 Uiso 0.47(5) 1 calc PR B 1 C32B C 1.0579(16) 1.0431(13) -0.003(4) 0.118(11) Uani 0.53(5) 1 d P B 2 H32D H 1.0592 1.0978 0.0405 0.177 Uiso 0.53(5) 1 calc PR B 2 H32E H 1.0710 1.0637 -0.0813 0.177 Uiso 0.53(5) 1 calc PR B 2 H32F H 1.1102 1.0289 0.0235 0.177 Uiso 0.53(5) 1 calc PR B 2 C33 C 0.40364(17) 0.4930(2) 0.1303(2) 0.0409(6) Uani 1 1 d . . . H33A H 0.3975 0.4468 0.1901 0.061 Uiso 1 1 calc R . . H33B H 0.3400 0.4636 0.0886 0.061 Uiso 1 1 calc R . . H33C H 0.4180 0.5582 0.1618 0.061 Uiso 1 1 calc R . . C34 C 0.4929(2) 0.40399(17) -0.0673(2) 0.0415(6) Uani 1 1 d . . . H34A H 0.5585 0.4164 -0.0955 0.062 Uiso 1 1 calc R . . H34B H 0.4499 0.4007 -0.1294 0.062 Uiso 1 1 calc R . . H34C H 0.4596 0.3396 -0.0268 0.062 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 0.0223(3) 0.0223(3) 0.0204(3) 0.0005(3) -0.0011(3) 0.0068(2) N1 0.0207(8) 0.0222(8) 0.0154(10) 0.0004(7) -0.0022(7) 0.0120(7) N2 0.0221(8) 0.0213(8) 0.0149(10) 0.0014(7) 0.0002(7) 0.0112(7) C1 0.0211(10) 0.0199(10) 0.0189(12) -0.0008(8) -0.0036(8) 0.0093(8) C2 0.0284(11) 0.0281(11) 0.0222(13) -0.0009(9) -0.0041(9) 0.0167(9) C3 0.0404(13) 0.0388(13) 0.0320(15) 0.0043(11) -0.0034(11) 0.0282(11) C4 0.0521(15) 0.0408(14) 0.0238(14) 0.0117(11) 0.0012(12) 0.0277(12) C5 0.0432(13) 0.0421(13) 0.0187(13) 0.0063(10) 0.0048(10) 0.0250(12) C6 0.0273(11) 0.0273(11) 0.0219(13) 0.0012(9) -0.0005(9) 0.0152(9) C7 0.0369(12) 0.0418(13) 0.0237(13) 0.0006(10) -0.0009(10) 0.0293(11) C8 0.0362(14) 0.0633(18) 0.0382(17) -0.0037(14) 0.0041(12) 0.0248(13) C9 0.0638(18) 0.0535(16) 0.0463(19) -0.0067(13) 0.0027(14) 0.0442(15) C10 0.0361(12) 0.0343(12) 0.0222(13) 0.0032(10) 0.0041(10) 0.0239(10) C11 0.0516(15) 0.0359(13) 0.0316(16) -0.0023(11) 0.0027(12) 0.0250(12) C12 0.0391(14) 0.0515(16) 0.052(2) -0.0045(14) 0.0057(13) 0.0284(13) C13 0.0219(10) 0.0226(10) 0.0177(12) 0.0042(8) -0.0006(8) 0.0115(8) C14 0.0297(11) 0.0278(11) 0.0213(12) 0.0052(9) 0.0021(9) 0.0179(9) C15 0.0365(12) 0.0387(13) 0.0332(15) 0.0044(11) -0.0037(10) 0.0261(11) C16 0.0454(14) 0.0503(15) 0.0234(14) -0.0009(12) -0.0123(11) 0.0309(12) C17 0.0432(14) 0.0405(13) 0.0196(13) -0.0042(10) -0.0050(10) 0.0244(11) C18 0.0264(11) 0.0282(11) 0.0196(12) 0.0001(9) -0.0002(9) 0.0162(9) C19 0.0409(13) 0.0376(12) 0.0239(13) 0.0002(10) -0.0015(10) 0.0291(11) C20 0.0622(18) 0.0335(13) 0.0418(18) -0.0063(12) 0.0017(14) 0.0223(13) C21 0.0512(16) 0.0649(18) 0.0475(19) -0.0028(14) 0.0052(13) 0.0429(15) C22 0.0327(12) 0.0358(12) 0.0225(13) -0.0040(10) -0.0020(10) 0.0221(10) C23 0.0353(13) 0.0511(15) 0.0325(16) -0.0039(12) 0.0022(11) 0.0251(12) C24 0.0498(16) 0.0382(14) 0.0442(18) -0.0066(12) 0.0038(13) 0.0253(13) C25 0.0217(10) 0.0216(10) 0.0152(10) -0.0008(8) 0.0010(8) 0.0139(8) C26 0.0222(11) 0.0243(11) 0.0240(12) 0.0043(10) -0.0025(10) 0.0100(8) C27 0.0355(12) 0.0238(11) 0.0486(17) 0.0009(11) -0.0122(12) 0.0128(10) C28 0.0507(18) 0.0207(13) 0.139(4) 0.0175(17) -0.031(2) 0.0016(12) C29A 0.033(4) 0.033(5) 0.072(12) 0.019(7) -0.017(7) -0.008(3) C29B 0.043(4) 0.038(4) 0.080(12) 0.014(7) -0.021(7) -0.007(3) C30 0.0237(14) 0.0504(18) 0.139(4) 0.032(2) -0.0127(18) 0.0038(13) C31 0.0229(11) 0.0344(12) 0.0522(18) 0.0128(12) -0.0022(11) 0.0111(10) C32A 0.043(5) 0.046(6) 0.17(2) 0.025(9) -0.007(8) -0.021(4) C32B 0.052(6) 0.061(6) 0.19(2) 0.031(11) -0.025(11) -0.013(5) C33 0.0237(12) 0.0542(16) 0.0336(16) 0.0041(12) 0.0042(10) 0.0110(11) C34 0.0536(16) 0.0227(12) 0.0340(16) -0.0048(10) -0.0058(12) 0.0084(11) _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 1.9414(17) . ? Al1 N1 1.9422(17) . ? Al1 C33 1.951(3) . ? Al1 C34 1.952(3) . ? Al1 C25 2.3663(19) . ? N1 C25 1.338(3) . ? N1 C1 1.431(3) . ? N2 C25 1.338(3) . ? N2 C13 1.434(3) . ? C1 C6 1.402(3) . ? C1 C2 1.410(3) . ? C2 C3 1.392(3) . ? C2 C7 1.520(3) . ? C3 C4 1.381(4) . ? C4 C5 1.377(3) . ? C5 C6 1.395(3) . ? C6 C10 1.525(3) . ? C7 C8 1.526(3) . ? C7 C9 1.528(3) . ? C10 C12 1.524(3) . ? C10 C11 1.529(3) . ? C13 C18 1.396(3) . ? C13 C14 1.413(3) . ? C14 C15 1.393(3) . ? C14 C19 1.517(3) . ? C15 C16 1.380(4) . ? C16 C17 1.382(3) . ? C17 C18 1.391(3) . ? C18 C22 1.530(3) . ? C19 C20 1.530(3) . ? C19 C21 1.531(3) . ? C22 C24 1.531(3) . ? C22 C23 1.532(3) . ? C25 C26 1.476(3) . ? C26 C27 1.387(3) . ? C26 C31 1.395(3) . ? C27 C28 1.378(4) . ? C28 C29A 1.394(17) . ? C28 C29B 1.45(2) . ? C29A C30 1.47(2) . ? C29A C32A 1.515(19) . ? C29B C30 1.393(16) . ? C29B C32B 1.553(18) . ? C30 C31 1.379(4) . ? 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 68.85(6) . . ? N2 Al1 C33 112.90(10) . . ? N1 Al1 C33 117.15(10) . . ? N2 Al1 C34 117.16(10) . . ? N1 Al1 C34 112.79(10) . . ? C33 Al1 C34 118.41(11) . . ? N2 Al1 C25 34.42(7) . . ? N1 Al1 C25 34.42(7) . . ? C33 Al1 C25 120.81(10) . . ? C34 Al1 C25 120.78(10) . . ? C25 N1 C1 123.05(17) . . ? C25 N1 Al1 90.42(12) . . ? C1 N1 Al1 143.12(14) . . ? C25 N2 C13 122.88(17) . . ? C25 N2 Al1 90.45(12) . . ? C13 N2 Al1 143.18(14) . . ? C6 C1 C2 121.4(2) . . ? C6 C1 N1 119.83(17) . . ? C2 C1 N1 118.74(19) . . ? C3 C2 C1 117.9(2) . . ? C3 C2 C7 120.76(19) . . ? C1 C2 C7 121.28(19) . . ? C4 C3 C2 121.3(2) . . ? C5 C4 C3 119.9(2) . . ? C4 C5 C6 121.4(2) . . ? C5 C6 C1 117.96(19) . . ? C5 C6 C10 119.1(2) . . ? C1 C6 C10 122.83(19) . . ? C2 C7 C8 110.0(2) . . ? C2 C7 C9 113.6(2) . . ? C8 C7 C9 110.2(2) . . ? C12 C10 C6 112.8(2) . . ? C12 C10 C11 110.4(2) . . ? C6 C10 C11 110.18(19) . . ? C18 C13 C14 121.46(19) . . ? C18 C13 N2 120.08(17) . . ? C14 C13 N2 118.45(19) . . ? C15 C14 C13 117.7(2) . . ? C15 C14 C19 120.97(19) . . ? C13 C14 C19 121.28(19) . . ? C16 C15 C14 121.4(2) . . ? C15 C16 C17 119.7(2) . . ? C16 C17 C18 121.4(2) . . ? C17 C18 C13 118.21(19) . . ? C17 C18 C22 119.1(2) . . ? C13 C18 C22 122.66(19) . . ? C14 C19 C20 109.8(2) . . ? C14 C19 C21 113.6(2) . . ? C20 C19 C21 110.2(2) . . ? C18 C22 C24 112.7(2) . . ? C18 C22 C23 110.06(19) . . ? C24 C22 C23 110.2(2) . . ? N1 C25 N2 110.29(16) . . ? N1 C25 C26 124.67(18) . . ? N2 C25 C26 125.04(18) . . ? N1 C25 Al1 55.16(10) . . ? N2 C25 Al1 55.13(10) . . ? C26 C25 Al1 179.80(17) . . ? C27 C26 C31 119.23(19) . . ? C27 C26 C25 120.67(19) . . ? C31 C26 C25 120.09(19) . . ? C28 C27 C26 120.3(2) . . ? C27 C28 C29A 121.2(6) . . ? C27 C28 C29B 118.8(7) . . ? C29A C28 C29B 26.7(6) . . ? C28 C29A C30 113.1(15) . . ? C28 C29A C32A 120.0(14) . . ? C30 C29A C32A 123.1(13) . . ? C30 C29B C28 114.2(14) . . ? C30 C29B C32B 118.1(13) . . ? C28 C29B C32B 123.6(14) . . ? C31 C30 C29B 120.5(6) . . ? C31 C30 C29A 119.4(7) . . ? C29B C30 C29A 26.5(6) . . ? C30 C31 C26 119.9(2) . . ? _diffrn_measured_fraction_theta_max 0.982 _diffrn_reflns_theta_full 28.09 _diffrn_measured_fraction_theta_full 0.982 _refine_diff_density_max 0.245 _refine_diff_density_min -0.235 _refine_diff_density_rms 0.045