# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Marcus Cole' _publ_contact_author_email M.COLE@UNSW.EDU.AU _publ_section_title ; Bulky Triazenide Complexes of Alumino- and Gallohydrides ; loop_ _publ_author_name 'Marcus Cole' 'Sean G Alexander' 'Craig M Forsyth' 'Samantha K. Furfari' 'Kristina Konstas' # Attachment 'Combined rev v2.txt' data_1 _database_code_depnum_ccdc_archive 'CCDC 704415' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common DmpN3(H)Mes _chemical_melting_point 430-432 _chemical_formula_moiety 'C33 H37 N3' _chemical_formula_sum 'C33 H37 N3' _chemical_formula_weight 475.66 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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_int_tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 11.5637(3) _cell_length_b 16.0951(4) _cell_length_c 14.7471(4) _cell_angle_alpha 90.00 _cell_angle_beta 94.6210(10) _cell_angle_gamma 90.00 _cell_volume 2735.79(12) _cell_formula_units_Z 4 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 17849 _cell_measurement_theta_min 1.77 _cell_measurement_theta_max 29.55 _exptl_crystal_description 'hexagonal prism' _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.155 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1024 _exptl_absorpt_coefficient_mu 0.067 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.9900 _exptl_absorpt_correction_T_max 0.9933 _exptl_absorpt_process_details 'performed as part of the DENZO-SMN package' _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _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 17849 _diffrn_reflns_av_R_equivalents 0.0893 _diffrn_reflns_av_sigmaI/netI 0.1240 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.77 _diffrn_reflns_theta_max 29.55 _reflns_number_total 7533 _reflns_number_gt 3422 _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^)+(0.1161P)^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 7533 _refine_ls_number_parameters 338 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1668 _refine_ls_R_factor_gt 0.0718 _refine_ls_wR_factor_ref 0.2235 _refine_ls_wR_factor_gt 0.1704 _refine_ls_goodness_of_fit_ref 0.933 _refine_ls_restrained_S_all 0.933 _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 N1 N 0.81820(14) 0.13911(11) 0.33879(12) 0.0306(4) Uani 1 1 d . . . N2 N 0.81454(16) 0.18451(11) 0.26939(13) 0.0367(5) Uani 1 1 d . . . N3 N 0.90153(16) 0.16936(13) 0.21550(13) 0.0361(5) Uani 1 1 d . . . C1 C 0.72628(18) 0.15667(12) 0.39546(14) 0.0288(5) Uani 1 1 d . . . C2 C 0.62080(18) 0.11502(13) 0.38227(14) 0.0304(5) Uani 1 1 d . . . C3 C 0.53637(18) 0.12978(14) 0.44265(15) 0.0346(5) Uani 1 1 d . . . H3 H 0.4630 0.1034 0.4329 0.042 Uiso 1 1 calc R . . C4 C 0.55742(19) 0.18223(14) 0.51662(15) 0.0343(5) Uani 1 1 d . . . H4 H 0.4993 0.1911 0.5576 0.041 Uiso 1 1 calc R . . C5 C 0.66399(18) 0.22165(13) 0.53030(15) 0.0326(5) Uani 1 1 d . . . H5 H 0.6785 0.2579 0.5808 0.039 Uiso 1 1 calc R . . C6 C 0.75022(17) 0.20879(12) 0.47091(14) 0.0289(5) Uani 1 1 d . . . C7 C 0.59994(17) 0.05019(14) 0.30943(15) 0.0338(5) Uani 1 1 d . . . C8 C 0.63617(18) -0.03136(15) 0.32955(16) 0.0378(6) Uani 1 1 d . . . C9 C 0.61477(19) -0.09298(16) 0.26381(17) 0.0423(6) Uani 1 1 d . . . H9 H 0.6378 -0.1484 0.2780 0.051 Uiso 1 1 calc R . . C10 C 0.5613(2) -0.07591(17) 0.17887(18) 0.0465(7) Uani 1 1 d . . . C11 C 0.5272(2) 0.00520(17) 0.15951(17) 0.0466(7) Uani 1 1 d . . . H11 H 0.4912 0.0178 0.1009 0.056 Uiso 1 1 calc R . . C12 C 0.54416(18) 0.06969(15) 0.22409(16) 0.0394(6) Uani 1 1 d . . . C13 C 0.7006(2) -0.05189(15) 0.41939(17) 0.0450(6) Uani 1 1 d . . . H13A H 0.7041 -0.1123 0.4271 0.068 Uiso 1 1 calc R . . H13B H 0.6602 -0.0272 0.4687 0.068 Uiso 1 1 calc R . . H13C H 0.7795 -0.0295 0.4209 0.068 Uiso 1 1 calc R . . C14 C 0.5408(2) -0.14413(18) 0.1089(2) 0.0631(8) Uani 1 1 d . . . H14A H 0.5161 -0.1196 0.0497 0.095 Uiso 1 1 calc R . . H14B H 0.4802 -0.1816 0.1275 0.095 Uiso 1 1 calc R . . H14C H 0.6128 -0.1754 0.1043 0.095 Uiso 1 1 calc R . . C15 C 0.5043(2) 0.15642(16) 0.20254(17) 0.0492(7) Uani 1 1 d . . . H15A H 0.4364 0.1691 0.2358 0.074 Uiso 1 1 calc R . . H15B H 0.4835 0.1615 0.1370 0.074 Uiso 1 1 calc R . . H15C H 0.5668 0.1955 0.2207 0.074 Uiso 1 1 calc R . . C16 C 0.86646(17) 0.24846(12) 0.48987(13) 0.0286(5) Uani 1 1 d . . . C17 C 0.96299(18) 0.20041(13) 0.52190(14) 0.0305(5) Uani 1 1 d . . . C18 C 1.06877(18) 0.23961(14) 0.54267(14) 0.0347(5) Uani 1 1 d . . . H18 H 1.1331 0.2071 0.5659 0.042 Uiso 1 1 calc R . . C19 C 1.08439(19) 0.32427(14) 0.53085(15) 0.0347(5) Uani 1 1 d . . . C20 C 0.98883(19) 0.37049(14) 0.49696(15) 0.0341(5) Uani 1 1 d . . . H20 H 0.9978 0.4284 0.4874 0.041 Uiso 1 1 calc R . . C21 C 0.87993(19) 0.33421(13) 0.47656(15) 0.0323(5) Uani 1 1 d . . . C22 C 0.9551(2) 0.10712(13) 0.53197(16) 0.0383(6) Uani 1 1 d . . . H22A H 0.9668 0.0806 0.4736 0.058 Uiso 1 1 calc R . . H22B H 0.8784 0.0922 0.5508 0.058 Uiso 1 1 calc R . . H22C H 1.0151 0.0881 0.5781 0.058 Uiso 1 1 calc R . . C23 C 1.2003(2) 0.36446(15) 0.55366(17) 0.0433(6) Uani 1 1 d . . . H23A H 1.1977 0.3975 0.6093 0.065 Uiso 1 1 calc R . . H23B H 1.2190 0.4007 0.5034 0.065 Uiso 1 1 calc R . . H23C H 1.2600 0.3214 0.5632 0.065 Uiso 1 1 calc R . . C24 C 0.7791(2) 0.38700(14) 0.44135(17) 0.0418(6) Uani 1 1 d . . . H24A H 0.7253 0.3935 0.4889 0.063 Uiso 1 1 calc R . . H24B H 0.7389 0.3602 0.3881 0.063 Uiso 1 1 calc R . . H24C H 0.8073 0.4417 0.4241 0.063 Uiso 1 1 calc R . . C25 C 0.99641(18) 0.11482(14) 0.24072(14) 0.0317(5) Uani 1 1 d . . . C26 C 0.98511(18) 0.03041(14) 0.22205(14) 0.0330(5) Uani 1 1 d . . . C27 C 1.07999(19) -0.02081(14) 0.24555(15) 0.0360(5) Uani 1 1 d . . . H27 H 1.0737 -0.0786 0.2331 0.043 Uiso 1 1 calc R . . C28 C 1.18346(19) 0.01012(15) 0.28666(15) 0.0384(6) Uani 1 1 d . . . C29 C 1.19064(19) 0.09480(16) 0.30511(15) 0.0400(6) Uani 1 1 d . . . H29 H 1.2605 0.1166 0.3341 0.048 Uiso 1 1 calc R . . C30 C 1.09898(19) 0.14841(14) 0.28248(15) 0.0362(6) Uani 1 1 d . . . C31 C 0.87334(19) -0.00397(15) 0.17821(17) 0.0416(6) Uani 1 1 d . . . H31A H 0.8105 0.0071 0.2173 0.062 Uiso 1 1 calc R . . H31B H 0.8811 -0.0640 0.1698 0.062 Uiso 1 1 calc R . . H31C H 0.8556 0.0227 0.1190 0.062 Uiso 1 1 calc R . . C32 C 1.2843(2) -0.04785(17) 0.31102(18) 0.0523(7) Uani 1 1 d . . . H32A H 1.3496 -0.0327 0.2759 0.078 Uiso 1 1 calc R . . H32B H 1.2607 -0.1052 0.2967 0.078 Uiso 1 1 calc R . . H32C H 1.3079 -0.0432 0.3762 0.078 Uiso 1 1 calc R . . C33 C 1.1094(2) 0.23985(15) 0.30201(17) 0.0491(7) Uani 1 1 d . . . H33A H 1.1838 0.2511 0.3365 0.074 Uiso 1 1 calc R . . H33B H 1.0458 0.2574 0.3377 0.074 Uiso 1 1 calc R . . H33C H 1.1055 0.2707 0.2446 0.074 Uiso 1 1 calc R . . H1 H 0.901(3) 0.210(2) 0.172(3) 0.122(14) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 N1 0.0335(10) 0.0330(10) 0.0251(10) -0.0005(8) 0.0020(8) -0.0008(8) N2 0.0429(11) 0.0375(11) 0.0302(11) 0.0031(9) 0.0064(9) 0.0027(9) N3 0.0384(11) 0.0416(12) 0.0296(11) 0.0044(9) 0.0104(8) 0.0053(9) C1 0.0348(11) 0.0262(11) 0.0253(11) 0.0044(9) 0.0023(9) 0.0020(9) C2 0.0326(11) 0.0313(12) 0.0268(11) 0.0029(9) -0.0006(9) 0.0031(9) C3 0.0299(11) 0.0391(13) 0.0342(13) 0.0036(11) -0.0011(10) 0.0000(10) C4 0.0361(12) 0.0354(13) 0.0321(12) 0.0040(10) 0.0076(10) 0.0043(10) C5 0.0424(12) 0.0285(12) 0.0268(12) -0.0014(9) 0.0023(9) 0.0041(10) C6 0.0347(11) 0.0245(11) 0.0273(12) 0.0026(9) 0.0019(9) 0.0021(9) C7 0.0291(11) 0.0401(14) 0.0322(12) -0.0040(10) 0.0037(9) -0.0051(10) C8 0.0308(11) 0.0431(14) 0.0398(14) -0.0059(11) 0.0051(10) -0.0061(10) C9 0.0344(12) 0.0423(14) 0.0509(16) -0.0096(12) 0.0080(11) -0.0067(11) C10 0.0358(13) 0.0577(18) 0.0466(16) -0.0151(13) 0.0078(11) -0.0118(12) C11 0.0394(13) 0.0680(19) 0.0322(14) -0.0058(13) 0.0024(11) -0.0157(13) C12 0.0318(11) 0.0533(15) 0.0329(13) -0.0022(12) 0.0006(10) -0.0094(11) C13 0.0471(14) 0.0380(14) 0.0495(16) -0.0011(12) 0.0006(12) 0.0044(11) C14 0.0577(17) 0.071(2) 0.0612(19) -0.0280(16) 0.0096(14) -0.0137(15) C15 0.0476(15) 0.0611(18) 0.0377(14) 0.0099(13) -0.0030(12) -0.0072(13) C16 0.0369(11) 0.0257(11) 0.0231(11) -0.0028(9) 0.0020(9) -0.0009(9) C17 0.0376(12) 0.0299(12) 0.0244(11) 0.0008(9) 0.0051(9) 0.0008(10) C18 0.0375(12) 0.0372(13) 0.0293(12) -0.0009(10) 0.0013(10) 0.0030(10) C19 0.0406(12) 0.0367(13) 0.0267(12) -0.0075(10) 0.0033(10) -0.0052(11) C20 0.0463(13) 0.0259(12) 0.0307(12) -0.0046(10) 0.0064(10) -0.0027(10) C21 0.0391(12) 0.0286(12) 0.0292(12) -0.0016(10) 0.0033(9) 0.0024(10) C22 0.0447(13) 0.0307(13) 0.0389(14) 0.0063(10) -0.0013(11) 0.0005(10) C23 0.0464(14) 0.0444(14) 0.0386(14) -0.0082(12) -0.0004(11) -0.0088(12) C24 0.0481(14) 0.0292(12) 0.0482(15) 0.0065(11) 0.0038(12) 0.0027(11) C25 0.0350(12) 0.0357(13) 0.0255(11) 0.0017(10) 0.0078(9) 0.0007(10) C26 0.0352(12) 0.0386(13) 0.0256(11) 0.0028(10) 0.0047(9) -0.0034(10) C27 0.0421(13) 0.0356(13) 0.0311(13) 0.0021(10) 0.0073(10) 0.0002(10) C28 0.0391(13) 0.0496(15) 0.0268(12) 0.0092(11) 0.0051(10) 0.0039(11) C29 0.0357(12) 0.0564(16) 0.0270(12) 0.0035(11) -0.0029(10) -0.0057(12) C30 0.0425(13) 0.0417(14) 0.0249(11) -0.0017(10) 0.0058(10) -0.0045(11) C31 0.0392(13) 0.0446(15) 0.0412(14) -0.0029(11) 0.0041(11) -0.0063(11) C32 0.0450(14) 0.0670(18) 0.0449(16) 0.0160(14) 0.0032(12) 0.0081(13) C33 0.0620(16) 0.0486(16) 0.0370(14) -0.0048(12) 0.0050(12) -0.0095(13) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag N1 N2 1.256(2) . ? N1 C1 1.432(3) . ? N2 N3 1.353(2) . ? N3 C25 1.431(3) . ? C1 C2 1.392(3) . ? C1 C6 1.403(3) . ? C2 C3 1.394(3) . ? C2 C7 1.503(3) . ? C3 C4 1.385(3) . ? C4 C5 1.386(3) . ? C5 C6 1.395(3) . ? C6 C16 1.494(3) . ? C7 C8 1.402(3) . ? C7 C12 1.403(3) . ? C8 C9 1.395(3) . ? C8 C13 1.504(3) . ? C9 C10 1.379(3) . ? C10 C11 1.387(4) . ? C10 C14 1.512(3) . ? C11 C12 1.412(3) . ? C12 C15 1.496(3) . ? C16 C17 1.408(3) . ? C16 C21 1.404(3) . ? C17 C18 1.389(3) . ? C17 C22 1.512(3) . ? C18 C19 1.387(3) . ? C19 C20 1.391(3) . ? C19 C23 1.502(3) . ? C20 C21 1.399(3) . ? C21 C24 1.501(3) . ? C25 C26 1.390(3) . ? C25 C30 1.400(3) . ? C26 C27 1.394(3) . ? C26 C31 1.503(3) . ? C27 C28 1.389(3) . ? C28 C29 1.391(3) . ? C28 C32 1.514(3) . ? C29 C30 1.386(3) . ? C30 C33 1.503(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 N2 N1 C1 112.52(17) . . ? N1 N2 N3 113.34(18) . . ? N2 N3 C25 123.26(19) . . ? C2 C1 C6 120.9(2) . . ? C2 C1 N1 120.45(18) . . ? C6 C1 N1 118.19(18) . . ? C1 C2 C3 118.7(2) . . ? C1 C2 C7 121.51(19) . . ? C3 C2 C7 119.64(18) . . ? C4 C3 C2 121.3(2) . . ? C3 C4 C5 119.4(2) . . ? C4 C5 C6 120.9(2) . . ? C5 C6 C1 118.77(18) . . ? C5 C6 C16 119.82(18) . . ? C1 C6 C16 121.39(19) . . ? C8 C7 C12 120.5(2) . . ? C8 C7 C2 118.08(19) . . ? C12 C7 C2 121.4(2) . . ? C9 C8 C7 119.0(2) . . ? C9 C8 C13 120.2(2) . . ? C7 C8 C13 120.7(2) . . ? C10 C9 C8 122.1(2) . . ? C9 C10 C11 118.3(2) . . ? C9 C10 C14 120.6(3) . . ? C11 C10 C14 121.1(2) . . ? C10 C11 C12 122.1(2) . . ? C7 C12 C11 118.0(2) . . ? C7 C12 C15 120.7(2) . . ? C11 C12 C15 121.3(2) . . ? C17 C16 C21 119.53(19) . . ? C17 C16 C6 120.33(18) . . ? C21 C16 C6 120.13(18) . . ? C18 C17 C16 119.0(2) . . ? C18 C17 C22 119.23(19) . . ? C16 C17 C22 121.74(19) . . ? C19 C18 C17 122.7(2) . . ? C18 C19 C20 117.56(19) . . ? C18 C19 C23 121.2(2) . . ? C20 C19 C23 121.3(2) . . ? C19 C20 C21 122.0(2) . . ? C20 C21 C16 119.22(19) . . ? C20 C21 C24 119.93(19) . . ? C16 C21 C24 120.85(19) . . ? C26 C25 C30 121.81(19) . . ? C26 C25 N3 119.35(18) . . ? C30 C25 N3 118.8(2) . . ? C25 C26 C27 117.98(19) . . ? C25 C26 C31 120.57(19) . . ? C27 C26 C31 121.4(2) . . ? C28 C27 C26 122.0(2) . . ? C27 C28 C29 118.2(2) . . ? C27 C28 C32 120.2(2) . . ? C29 C28 C32 121.7(2) . . ? C28 C29 C30 122.0(2) . . ? C29 C30 C25 118.0(2) . . ? C29 C30 C33 121.0(2) . . ? C25 C30 C33 121.0(2) . . ? _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 29.55 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 0.316 _refine_diff_density_min -0.330 _refine_diff_density_rms 0.066 _chemical_compound_source Et2O #===END data_Compound2 _database_code_depnum_ccdc_archive 'CCDC 704416' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common (AlH(DitopN3Mes)2) _chemical_melting_point '531 (dec.)' _chemical_formula_moiety 'C58 H57 Al N6' _chemical_formula_sum 'C58 H57 Al N6' _chemical_formula_weight 865.08 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source N N 0.0061 0.0033 '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' Al Al 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' C C 0.0033 0.0016 '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 11.8179(5) _cell_length_b 11.8232(4) _cell_length_c 20.7647(12) _cell_angle_alpha 98.803(2) _cell_angle_beta 99.288(2) _cell_angle_gamma 116.586(3) _cell_volume 2475.7(2) _cell_formula_units_Z 2 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 18948 _cell_measurement_theta_min 1.03 _cell_measurement_theta_max 28.62 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.160 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 920 _exptl_absorpt_coefficient_mu 0.085 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.9791 _exptl_absorpt_correction_T_max 0.9916 _exptl_absorpt_process_details 'performed as part of the DENZO-SMN package' _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _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 18948 _diffrn_reflns_av_R_equivalents 0.1060 _diffrn_reflns_av_sigmaI/netI 0.2911 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.03 _diffrn_reflns_theta_max 28.62 _reflns_number_total 11489 _reflns_number_gt 3334 _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^)+(0.1001P)^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 11489 _refine_ls_number_parameters 600 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.3235 _refine_ls_R_factor_gt 0.0962 _refine_ls_wR_factor_ref 0.2704 _refine_ls_wR_factor_gt 0.1808 _refine_ls_goodness_of_fit_ref 0.945 _refine_ls_restrained_S_all 0.945 _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 Al1 Al 0.16479(16) 0.91496(16) 0.24996(8) 0.0492(5) Uani 1 1 d . . . N1 N 0.1362(4) 0.9819(4) 0.17011(18) 0.0431(11) Uani 1 1 d . . . N2 N 0.1819(4) 0.9198(4) 0.13328(19) 0.0417(10) Uani 1 1 d . . . N3 N 0.2340(4) 0.8721(4) 0.17393(19) 0.0440(11) Uani 1 1 d . . . N4 N 0.3125(4) 0.9657(4) 0.32989(19) 0.0423(11) Uani 1 1 d . . . N5 N 0.2856(4) 1.0473(4) 0.36650(19) 0.0444(11) Uani 1 1 d . . . N6 N 0.1973(4) 1.0594(4) 0.32551(19) 0.0470(11) Uani 1 1 d . . . C1 C 0.0826(5) 1.0528(5) 0.1391(2) 0.0443(13) Uani 1 1 d . . . C2 C -0.0406(5) 1.0324(5) 0.1474(2) 0.0479(14) Uani 1 1 d . . . C3 C -0.0895(5) 1.1095(5) 0.1230(3) 0.0611(16) Uani 1 1 d . . . H3 H -0.1687 1.1017 0.1307 0.073 Uiso 1 1 calc R . . C4 C -0.0246(6) 1.1964(6) 0.0882(3) 0.0709(18) Uani 1 1 d . . . H4 H -0.0595 1.2471 0.0719 0.085 Uiso 1 1 calc R . . C5 C 0.0919(6) 1.2097(5) 0.0770(3) 0.0652(17) Uani 1 1 d . . . H5 H 0.1335 1.2666 0.0511 0.078 Uiso 1 1 calc R . . C6 C 0.1489(5) 1.1410(5) 0.1031(3) 0.0502(14) Uani 1 1 d . . . C7 C -0.1214(5) 0.9271(5) 0.1766(3) 0.0457(14) Uani 1 1 d . . . C8 C -0.1663(5) 0.7961(6) 0.1445(3) 0.0547(15) Uani 1 1 d . . . H8 H -0.1416 0.7760 0.1053 0.066 Uiso 1 1 calc R . . C9 C -0.2450(6) 0.6974(6) 0.1690(3) 0.0632(17) Uani 1 1 d . . . H9 H -0.2736 0.6104 0.1463 0.076 Uiso 1 1 calc R . . C10 C -0.2840(6) 0.7216(7) 0.2261(3) 0.0697(18) Uani 1 1 d . . . C11 C -0.2410(6) 0.8493(7) 0.2582(3) 0.0672(17) Uani 1 1 d . . . H11 H -0.2670 0.8680 0.2971 0.081 Uiso 1 1 calc R . . C12 C -0.1602(5) 0.9506(6) 0.2344(3) 0.0563(15) Uani 1 1 d . . . H12 H -0.1309 1.0374 0.2579 0.068 Uiso 1 1 calc R . . C13 C -0.3748(7) 0.6103(7) 0.2517(4) 0.117(3) Uani 1 1 d . . . H13A H -0.3688 0.6428 0.2986 0.175 Uiso 1 1 calc R . . H13B H -0.3495 0.5425 0.2477 0.175 Uiso 1 1 calc R . . H13C H -0.4642 0.5744 0.2250 0.175 Uiso 1 1 calc R . . C14 C 0.2771(5) 1.1638(5) 0.0917(3) 0.0476(14) Uani 1 1 d . . . C15 C 0.3893(6) 1.2157(6) 0.1440(3) 0.0740(18) Uani 1 1 d . . . H15 H 0.3843 1.2356 0.1887 0.089 Uiso 1 1 calc R . . C16 C 0.5079(6) 1.2389(6) 0.1321(3) 0.0783(19) Uani 1 1 d . . . H16 H 0.5821 1.2747 0.1688 0.094 Uiso 1 1 calc R . . C17 C 0.5208(6) 1.2108(6) 0.0675(3) 0.0675(17) Uani 1 1 d . . . C18 C 0.4095(7) 1.1600(7) 0.0158(3) 0.080(2) Uani 1 1 d . . . H18 H 0.4143 1.1390 -0.0288 0.096 Uiso 1 1 calc R . . C19 C 0.2912(6) 1.1388(6) 0.0275(3) 0.0679(17) Uani 1 1 d . . . H19 H 0.2180 1.1063 -0.0095 0.082 Uiso 1 1 calc R . . C20 C 0.6496(6) 1.2299(8) 0.0540(3) 0.110(3) Uani 1 1 d . . . H20A H 0.6770 1.1756 0.0754 0.165 Uiso 1 1 calc R . . H20B H 0.7158 1.3210 0.0722 0.165 Uiso 1 1 calc R . . H20C H 0.6386 1.2052 0.0057 0.165 Uiso 1 1 calc R . . C21 C 0.2748(5) 0.7855(5) 0.1428(2) 0.0417(13) Uani 1 1 d . . . C22 C 0.1803(5) 0.6597(5) 0.1040(2) 0.0468(13) Uani 1 1 d . . . C23 C 0.2236(5) 0.5755(5) 0.0769(2) 0.0536(14) Uani 1 1 d . . . H23 H 0.1613 0.4911 0.0504 0.064 Uiso 1 1 calc R . . C24 C 0.3560(6) 0.6126(6) 0.0878(3) 0.0536(14) Uani 1 1 d . . . C25 C 0.4453(5) 0.7359(6) 0.1276(3) 0.0538(15) Uani 1 1 d . . . H25 H 0.5351 0.7616 0.1359 0.065 Uiso 1 1 calc R . . C26 C 0.4081(5) 0.8238(5) 0.1558(2) 0.0451(13) Uani 1 1 d . . . C27 C 0.0360(5) 0.6153(5) 0.0921(3) 0.0615(16) Uani 1 1 d . . . H27A H 0.0162 0.6323 0.1349 0.092 Uiso 1 1 calc R . . H27B H -0.0137 0.5223 0.0705 0.092 Uiso 1 1 calc R . . H27C H 0.0125 0.6627 0.0632 0.092 Uiso 1 1 calc R . . C28 C 0.4002(6) 0.5204(6) 0.0560(3) 0.085(2) Uani 1 1 d . . . H28A H 0.4803 0.5702 0.0433 0.127 Uiso 1 1 calc R . . H28B H 0.3325 0.4578 0.0162 0.127 Uiso 1 1 calc R . . H28C H 0.4162 0.4743 0.0881 0.127 Uiso 1 1 calc R . . C29 C 0.5084(5) 0.9584(5) 0.1978(3) 0.0630(16) Uani 1 1 d . . . H29A H 0.5937 0.9777 0.1908 0.095 Uiso 1 1 calc R . . H29B H 0.5113 0.9625 0.2451 0.095 Uiso 1 1 calc R . . H29C H 0.4850 1.0219 0.1846 0.095 Uiso 1 1 calc R . . C30 C 0.4128(5) 0.9421(5) 0.3608(2) 0.0397(13) Uani 1 1 d . . . C31 C 0.3851(5) 0.8118(5) 0.3522(2) 0.0438(13) Uani 1 1 d . . . C32 C 0.4860(6) 0.7862(6) 0.3768(3) 0.0620(16) Uani 1 1 d . . . H32 H 0.4702 0.6993 0.3693 0.074 Uiso 1 1 calc R . . C33 C 0.6080(6) 0.8864(6) 0.4118(3) 0.0675(18) Uani 1 1 d . . . H33 H 0.6752 0.8681 0.4282 0.081 Uiso 1 1 calc R . . C34 C 0.6320(5) 1.0144(6) 0.4230(3) 0.0624(16) Uani 1 1 d . . . H34 H 0.7148 1.0818 0.4490 0.075 Uiso 1 1 calc R . . C35 C 0.5372(5) 1.0463(5) 0.3967(2) 0.0469(14) Uani 1 1 d . . . C36 C 0.2494(5) 0.7015(5) 0.3230(3) 0.0454(14) Uani 1 1 d . . . C37 C 0.2174(6) 0.6059(6) 0.2654(3) 0.0570(15) Uani 1 1 d . . . H37 H 0.2816 0.6119 0.2426 0.068 Uiso 1 1 calc R . . C38 C 0.0910(7) 0.5010(6) 0.2408(3) 0.0673(17) Uani 1 1 d . . . H38 H 0.0700 0.4370 0.2013 0.081 Uiso 1 1 calc R . . C39 C -0.0035(6) 0.4906(6) 0.2742(3) 0.0670(17) Uani 1 1 d . . . C40 C 0.0304(6) 0.5883(7) 0.3324(3) 0.0628(17) Uani 1 1 d . . . H40 H -0.0330 0.5832 0.3557 0.075 Uiso 1 1 calc R . . C41 C 0.1532(6) 0.6896(6) 0.3553(3) 0.0549(15) Uani 1 1 d . . . H41 H 0.1739 0.7541 0.3945 0.066 Uiso 1 1 calc R . . C42 C -0.1406(6) 0.3736(7) 0.2488(4) 0.114(3) Uani 1 1 d . . . H42A H -0.2007 0.4003 0.2276 0.171 Uiso 1 1 calc R . . H42B H -0.1686 0.3399 0.2864 0.171 Uiso 1 1 calc R . . H42C H -0.1399 0.3059 0.2161 0.171 Uiso 1 1 calc R . . C43 C 0.5730(5) 1.1868(5) 0.4086(3) 0.0493(14) Uani 1 1 d . . . C44 C 0.5736(6) 1.2470(6) 0.3564(3) 0.0695(17) Uani 1 1 d . . . H44 H 0.5498 1.1976 0.3117 0.083 Uiso 1 1 calc R . . C45 C 0.6080(6) 1.3766(7) 0.3683(3) 0.0793(19) Uani 1 1 d . . . H45 H 0.6073 1.4145 0.3318 0.095 Uiso 1 1 calc R . . C46 C 0.6437(6) 1.4527(6) 0.4329(4) 0.0728(18) Uani 1 1 d . . . C47 C 0.6446(6) 1.3937(6) 0.4845(3) 0.081(2) Uani 1 1 d . . . H47 H 0.6684 1.4428 0.5293 0.097 Uiso 1 1 calc R . . C48 C 0.6109(6) 1.2632(6) 0.4719(3) 0.0694(17) Uani 1 1 d . . . H48 H 0.6145 1.2260 0.5086 0.083 Uiso 1 1 calc R . . C49 C 0.6766(7) 1.5958(6) 0.4456(3) 0.106(3) Uani 1 1 d . . . H49A H 0.6145 1.6045 0.4128 0.159 Uiso 1 1 calc R . . H49B H 0.7645 1.6481 0.4413 0.159 Uiso 1 1 calc R . . H49C H 0.6719 1.6259 0.4907 0.159 Uiso 1 1 calc R . . C50 C 0.1405(5) 1.1305(5) 0.3568(2) 0.0420(13) Uani 1 1 d . . . C51 C 0.1694(5) 1.2524(5) 0.3439(2) 0.0472(14) Uani 1 1 d . . . C52 C 0.1081(5) 1.3171(5) 0.3726(3) 0.0537(15) Uani 1 1 d . . . H52 H 0.1249 1.3983 0.3640 0.064 Uiso 1 1 calc R . . C53 C 0.0243(6) 1.2686(6) 0.4127(3) 0.0567(15) Uani 1 1 d . . . C54 C -0.0003(5) 1.1471(5) 0.4231(2) 0.0529(14) Uani 1 1 d . . . H54 H -0.0579 1.1111 0.4497 0.063 Uiso 1 1 calc R . . C55 C 0.0555(5) 1.0766(5) 0.3963(2) 0.0449(13) Uani 1 1 d . . . C56 C 0.2610(5) 1.3113(5) 0.3016(3) 0.0625(16) Uani 1 1 d . . . H56A H 0.2781 1.4004 0.3043 0.094 Uiso 1 1 calc R . . H56B H 0.2213 1.2601 0.2550 0.094 Uiso 1 1 calc R . . H56C H 0.3427 1.3115 0.3180 0.094 Uiso 1 1 calc R . . C57 C -0.0348(6) 1.3441(6) 0.4444(3) 0.085(2) Uani 1 1 d . . . H57A H 0.0220 1.4369 0.4506 0.127 Uiso 1 1 calc R . . H57B H -0.0448 1.3265 0.4878 0.127 Uiso 1 1 calc R . . H57C H -0.1200 1.3177 0.4153 0.127 Uiso 1 1 calc R . . C58 C 0.0225(5) 0.9437(5) 0.4075(3) 0.0629(16) Uani 1 1 d . . . H58A H -0.0012 0.8821 0.3645 0.094 Uiso 1 1 calc R . . H58B H -0.0506 0.9143 0.4279 0.094 Uiso 1 1 calc R . . H58C H 0.0980 0.9489 0.4372 0.094 Uiso 1 1 calc R . . H1 H 0.035(3) 0.787(3) 0.2496(14) 0.004(8) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Al1 0.0569(11) 0.0525(11) 0.0458(10) 0.0090(8) 0.0100(8) 0.0350(10) N1 0.048(3) 0.047(3) 0.042(3) 0.008(2) 0.011(2) 0.031(3) N2 0.041(3) 0.041(3) 0.043(3) 0.005(2) 0.008(2) 0.021(2) N3 0.052(3) 0.046(3) 0.042(3) 0.014(2) 0.008(2) 0.031(3) N4 0.047(3) 0.041(3) 0.046(3) 0.007(2) 0.010(2) 0.028(2) N5 0.051(3) 0.048(3) 0.043(3) 0.014(2) 0.016(2) 0.030(3) N6 0.061(3) 0.051(3) 0.043(3) 0.012(2) 0.009(2) 0.041(3) C1 0.049(4) 0.043(3) 0.043(3) 0.008(3) 0.005(3) 0.028(3) C2 0.053(4) 0.040(4) 0.051(3) 0.012(3) 0.010(3) 0.024(3) C3 0.054(4) 0.051(4) 0.086(4) 0.026(4) 0.016(3) 0.031(4) C4 0.073(5) 0.067(5) 0.092(5) 0.034(4) 0.015(4) 0.048(4) C5 0.062(4) 0.063(4) 0.081(4) 0.035(3) 0.015(3) 0.035(4) C6 0.051(4) 0.045(4) 0.055(4) 0.010(3) 0.008(3) 0.026(3) C7 0.045(3) 0.053(4) 0.046(4) 0.012(3) 0.007(3) 0.032(3) C8 0.060(4) 0.050(4) 0.060(4) 0.014(3) 0.017(3) 0.031(4) C9 0.065(4) 0.052(4) 0.077(5) 0.023(4) 0.015(4) 0.032(4) C10 0.078(5) 0.066(5) 0.070(5) 0.032(4) 0.021(4) 0.034(4) C11 0.074(5) 0.073(5) 0.061(4) 0.026(4) 0.028(4) 0.035(4) C12 0.056(4) 0.053(4) 0.056(4) 0.002(3) 0.005(3) 0.031(4) C13 0.136(7) 0.107(6) 0.124(7) 0.069(6) 0.066(5) 0.050(6) C14 0.056(4) 0.038(3) 0.048(4) 0.013(3) 0.007(3) 0.023(3) C15 0.056(4) 0.093(5) 0.062(4) 0.009(4) 0.013(4) 0.030(4) C16 0.058(5) 0.106(6) 0.065(5) 0.022(4) 0.015(4) 0.034(4) C17 0.064(5) 0.086(5) 0.072(5) 0.039(4) 0.028(4) 0.043(4) C18 0.077(5) 0.117(6) 0.061(4) 0.029(4) 0.030(4) 0.053(5) C19 0.068(5) 0.084(5) 0.048(4) 0.013(3) 0.004(3) 0.038(4) C20 0.073(5) 0.181(8) 0.117(6) 0.076(6) 0.051(4) 0.076(6) C21 0.059(4) 0.047(4) 0.033(3) 0.010(3) 0.013(3) 0.037(3) C22 0.050(4) 0.053(4) 0.047(3) 0.016(3) 0.017(3) 0.031(3) C23 0.059(4) 0.046(4) 0.054(4) 0.005(3) 0.013(3) 0.027(3) C24 0.059(4) 0.050(4) 0.053(4) 0.005(3) 0.020(3) 0.029(4) C25 0.051(4) 0.064(4) 0.063(4) 0.018(3) 0.023(3) 0.038(4) C26 0.043(4) 0.045(4) 0.050(3) 0.011(3) 0.010(3) 0.025(3) C27 0.056(4) 0.060(4) 0.060(4) 0.001(3) 0.002(3) 0.030(3) C28 0.083(5) 0.073(5) 0.110(5) -0.002(4) 0.032(4) 0.053(4) C29 0.054(4) 0.059(4) 0.080(4) 0.015(4) 0.020(3) 0.030(4) C30 0.039(3) 0.051(4) 0.036(3) 0.011(3) 0.004(2) 0.030(3) C31 0.052(4) 0.044(4) 0.049(3) 0.020(3) 0.018(3) 0.031(3) C32 0.062(4) 0.058(4) 0.080(4) 0.027(4) 0.016(3) 0.039(4) C33 0.051(4) 0.063(5) 0.105(5) 0.035(4) 0.014(4) 0.039(4) C34 0.050(4) 0.058(4) 0.082(4) 0.020(3) 0.008(3) 0.030(4) C35 0.051(4) 0.051(4) 0.045(3) 0.016(3) 0.012(3) 0.030(3) C36 0.047(4) 0.051(4) 0.049(4) 0.014(3) 0.009(3) 0.034(3) C37 0.069(5) 0.065(4) 0.059(4) 0.028(4) 0.026(3) 0.044(4) C38 0.067(5) 0.060(5) 0.063(4) 0.005(3) 0.005(4) 0.027(4) C39 0.053(4) 0.066(5) 0.076(5) 0.015(4) 0.008(4) 0.027(4) C40 0.056(5) 0.069(5) 0.077(5) 0.030(4) 0.021(4) 0.037(4) C41 0.055(4) 0.052(4) 0.065(4) 0.014(3) 0.015(3) 0.032(4) C42 0.069(5) 0.090(6) 0.132(7) -0.011(5) 0.005(5) 0.015(5) C43 0.037(3) 0.047(4) 0.056(4) 0.011(3) 0.004(3) 0.017(3) C44 0.098(5) 0.052(4) 0.056(4) 0.019(3) 0.022(3) 0.033(4) C45 0.103(5) 0.057(5) 0.073(5) 0.026(4) 0.011(4) 0.036(4) C46 0.069(4) 0.048(4) 0.080(5) 0.003(4) -0.008(4) 0.024(4) C47 0.113(6) 0.062(5) 0.049(4) -0.004(4) -0.007(4) 0.042(4) C48 0.088(5) 0.067(5) 0.053(4) 0.017(4) 0.012(3) 0.039(4) C49 0.125(6) 0.051(5) 0.109(6) 0.002(4) -0.021(5) 0.038(5) C50 0.045(3) 0.044(4) 0.040(3) 0.002(3) 0.006(3) 0.028(3) C51 0.059(4) 0.045(4) 0.040(3) 0.005(3) 0.010(3) 0.030(3) C52 0.062(4) 0.044(4) 0.059(4) 0.004(3) 0.015(3) 0.032(3) C53 0.065(4) 0.051(4) 0.062(4) 0.009(3) 0.021(3) 0.036(4) C54 0.058(4) 0.059(4) 0.051(3) 0.013(3) 0.022(3) 0.034(4) C55 0.046(3) 0.043(4) 0.048(3) 0.006(3) 0.010(3) 0.027(3) C56 0.073(4) 0.052(4) 0.076(4) 0.021(3) 0.031(3) 0.037(4) C57 0.106(5) 0.069(5) 0.113(5) 0.024(4) 0.057(4) 0.061(4) C58 0.076(4) 0.062(4) 0.066(4) 0.025(3) 0.026(3) 0.040(4) _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 N6 1.981(4) . ? Al1 N1 1.987(4) . ? Al1 N3 1.990(4) . ? Al1 N4 1.996(4) . ? N1 N2 1.316(4) . ? N1 C1 1.424(5) . ? N2 N3 1.303(4) . ? N3 C21 1.429(5) . ? N4 N5 1.318(4) . ? N4 C30 1.415(5) . ? N5 N6 1.311(4) . ? N6 C50 1.434(5) . ? C1 C6 1.400(6) . ? C1 C2 1.410(6) . ? C2 C3 1.393(6) . ? C2 C7 1.477(7) . ? C3 C4 1.366(7) . ? C4 C5 1.376(7) . ? C5 C6 1.383(6) . ? C6 C14 1.481(7) . ? C7 C12 1.386(7) . ? C7 C8 1.399(7) . ? C8 C9 1.360(7) . ? C9 C10 1.375(7) . ? C10 C11 1.369(7) . ? C10 C13 1.517(8) . ? C11 C12 1.378(7) . ? C14 C19 1.373(6) . ? C14 C15 1.385(7) . ? C15 C16 1.374(7) . ? C16 C17 1.382(7) . ? C17 C18 1.371(7) . ? C17 C20 1.515(7) . ? C18 C19 1.375(7) . ? C21 C26 1.394(6) . ? C21 C22 1.401(6) . ? C22 C23 1.395(6) . ? C22 C27 1.507(6) . ? C23 C24 1.391(6) . ? C24 C25 1.377(7) . ? C24 C28 1.516(7) . ? C25 C26 1.388(6) . ? C26 C29 1.500(7) . ? C30 C31 1.399(6) . ? C30 C35 1.407(6) . ? C31 C32 1.396(6) . ? C31 C36 1.487(7) . ? C32 C33 1.371(7) . ? C33 C34 1.382(7) . ? C34 C35 1.392(6) . ? C35 C43 1.488(7) . ? C36 C41 1.376(6) . ? C36 C37 1.381(7) . ? C37 C38 1.390(7) . ? C38 C39 1.376(7) . ? C39 C40 1.400(7) . ? C39 C42 1.520(8) . ? C40 C41 1.347(7) . ? C43 C48 1.353(7) . ? C43 C44 1.383(7) . ? C44 C45 1.367(7) . ? C45 C46 1.376(8) . ? C46 C47 1.367(7) . ? C46 C49 1.525(7) . ? C47 C48 1.380(7) . ? C50 C55 1.394(6) . ? C50 C51 1.404(6) . ? C51 C52 1.401(6) . ? C51 C56 1.499(6) . ? C52 C53 1.382(7) . ? C53 C54 1.392(7) . ? C53 C57 1.497(7) . ? C54 C55 1.381(6) . ? C55 C58 1.506(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N6 Al1 N1 102.10(16) . . ? N6 Al1 N3 142.81(19) . . ? N1 Al1 N3 63.42(15) . . ? N6 Al1 N4 63.93(15) . . ? N1 Al1 N4 136.68(18) . . ? N3 Al1 N4 101.92(16) . . ? N2 N1 C1 117.8(4) . . ? N2 N1 Al1 94.6(2) . . ? C1 N1 Al1 147.3(3) . . ? N3 N2 N1 105.9(4) . . ? N2 N3 C21 115.7(4) . . ? N2 N3 Al1 94.9(3) . . ? C21 N3 Al1 145.0(3) . . ? N5 N4 C30 118.3(4) . . ? N5 N4 Al1 93.8(2) . . ? C30 N4 Al1 147.5(3) . . ? N6 N5 N4 106.4(4) . . ? N5 N6 C50 115.7(4) . . ? N5 N6 Al1 94.7(3) . . ? C50 N6 Al1 144.9(3) . . ? C6 C1 C2 120.8(4) . . ? C6 C1 N1 122.3(4) . . ? C2 C1 N1 116.9(5) . . ? C3 C2 C1 118.0(5) . . ? C3 C2 C7 119.9(5) . . ? C1 C2 C7 122.0(4) . . ? C4 C3 C2 121.2(5) . . ? C3 C4 C5 120.1(5) . . ? C4 C5 C6 121.4(5) . . ? C5 C6 C1 118.4(5) . . ? C5 C6 C14 118.8(5) . . ? C1 C6 C14 122.9(4) . . ? C12 C7 C8 116.8(5) . . ? C12 C7 C2 123.0(5) . . ? C8 C7 C2 120.2(5) . . ? C9 C8 C7 121.2(5) . . ? C8 C9 C10 121.7(6) . . ? C11 C10 C9 118.0(6) . . ? C11 C10 C13 121.0(6) . . ? C9 C10 C13 121.0(7) . . ? C10 C11 C12 121.2(6) . . ? C11 C12 C7 121.2(5) . . ? C19 C14 C15 116.5(5) . . ? C19 C14 C6 120.9(5) . . ? C15 C14 C6 122.5(5) . . ? C16 C15 C14 121.5(6) . . ? C15 C16 C17 121.7(6) . . ? C18 C17 C16 116.6(5) . . ? C18 C17 C20 121.3(6) . . ? C16 C17 C20 122.1(6) . . ? C17 C18 C19 121.9(6) . . ? C14 C19 C18 121.8(5) . . ? C26 C21 C22 121.0(4) . . ? C26 C21 N3 119.3(5) . . ? C22 C21 N3 119.5(4) . . ? C23 C22 C21 118.0(5) . . ? C23 C22 C27 120.5(5) . . ? C21 C22 C27 121.4(5) . . ? C24 C23 C22 122.0(5) . . ? C25 C24 C23 117.9(5) . . ? C25 C24 C28 121.2(5) . . ? C23 C24 C28 120.9(5) . . ? C24 C25 C26 122.6(5) . . ? C25 C26 C21 118.4(5) . . ? C25 C26 C29 121.0(5) . . ? C21 C26 C29 120.6(4) . . ? C31 C30 C35 121.5(4) . . ? C31 C30 N4 117.5(4) . . ? C35 C30 N4 121.0(4) . . ? C32 C31 C30 118.6(5) . . ? C32 C31 C36 119.6(5) . . ? C30 C31 C36 121.6(4) . . ? C33 C32 C31 120.7(5) . . ? C32 C33 C34 119.9(5) . . ? C33 C34 C35 121.9(5) . . ? C34 C35 C30 117.2(5) . . ? C34 C35 C43 118.4(5) . . ? C30 C35 C43 124.4(4) . . ? C41 C36 C37 118.2(6) . . ? C41 C36 C31 119.9(5) . . ? C37 C36 C31 121.8(5) . . ? C36 C37 C38 120.6(5) . . ? C39 C38 C37 120.2(6) . . ? C38 C39 C40 118.6(6) . . ? C38 C39 C42 120.3(6) . . ? C40 C39 C42 121.1(6) . . ? C41 C40 C39 120.4(6) . . ? C40 C41 C36 122.0(6) . . ? C48 C43 C44 116.7(5) . . ? C48 C43 C35 120.9(5) . . ? C44 C43 C35 122.3(5) . . ? C45 C44 C43 121.5(6) . . ? C44 C45 C46 121.3(6) . . ? C47 C46 C45 117.3(6) . . ? C47 C46 C49 121.8(6) . . ? C45 C46 C49 120.9(6) . . ? C46 C47 C48 120.9(6) . . ? C43 C48 C47 122.3(5) . . ? C55 C50 C51 121.8(4) . . ? C55 C50 N6 120.3(4) . . ? C51 C50 N6 117.8(5) . . ? C52 C51 C50 116.7(5) . . ? C52 C51 C56 121.2(5) . . ? C50 C51 C56 122.2(4) . . ? C53 C52 C51 123.8(5) . . ? C52 C53 C54 116.4(5) . . ? C52 C53 C57 121.7(5) . . ? C54 C53 C57 121.9(5) . . ? C55 C54 C53 123.4(5) . . ? C54 C55 C50 117.9(4) . . ? C54 C55 C58 121.2(5) . . ? C50 C55 C58 120.8(4) . . ? _diffrn_measured_fraction_theta_max 0.906 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.971 _refine_diff_density_max 0.545 _refine_diff_density_min -0.277 _refine_diff_density_rms 0.058 _chemical_compound_source Et2O #===END data_Compound3b _database_code_depnum_ccdc_archive 'CCDC 704417' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common (AlH(DmpN3pTol)2) _chemical_melting_point '426-430 (dec. 443)' _chemical_formula_moiety 'C62 H64 Al N6' _chemical_formula_sum 'C62 H64 Al N6' _chemical_formula_weight 921.18 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Al Al 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M 'P -4' _symmetry_int_tables_number 81 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'y, -x, -z' '-x, -y, z' '-y, x, -z' _cell_length_a 15.1771(11) _cell_length_b 15.1771(11) _cell_length_c 11.6305(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2679.0(3) _cell_formula_units_Z 2 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 20930 _cell_measurement_theta_min 2.21 _cell_measurement_theta_max 29.11 _exptl_crystal_description tabular _exptl_crystal_colour yellow-orange _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.142 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 984 _exptl_absorpt_coefficient_mu 0.082 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.9798 _exptl_absorpt_correction_T_max 0.9935 _exptl_absorpt_process_details 'Bruker Scalepack' _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker X8 Apex' _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 20930 _diffrn_reflns_av_R_equivalents 0.0658 _diffrn_reflns_av_sigmaI/netI 0.0870 _diffrn_reflns_limit_h_min -20 _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 7 _diffrn_reflns_theta_min 2.21 _diffrn_reflns_theta_max 29.11 _reflns_number_total 7151 _reflns_number_gt 5332 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker AXS Collect Software' _computing_cell_refinement 'Bruker Scalepack' _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^)+(0.0477P)^2^+0.2577P] 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 0.4(2) _refine_ls_number_reflns 7151 _refine_ls_number_parameters 321 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0873 _refine_ls_R_factor_gt 0.0621 _refine_ls_wR_factor_ref 0.1346 _refine_ls_wR_factor_gt 0.1182 _refine_ls_goodness_of_fit_ref 1.024 _refine_ls_restrained_S_all 1.024 _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 Al1 Al 0.5000 1.0000 0.95764(8) 0.0216(2) Uani 1 2 d S . . N1 N 0.55982(12) 0.88030(13) 0.91875(15) 0.0200(4) Uani 1 1 d . . . N2 N 0.48892(13) 0.85264(12) 0.86535(16) 0.0221(4) Uani 1 1 d . . . N3 N 0.43221(12) 0.91920(13) 0.86652(16) 0.0212(4) Uani 1 1 d . . . C1 C 0.63073(15) 0.81863(15) 0.92631(19) 0.0202(5) Uani 1 1 d . . . C2 C 0.69024(16) 0.82852(15) 1.01832(19) 0.0224(5) Uani 1 1 d . . . C3 C 0.76263(18) 0.77166(17) 1.0243(2) 0.0305(6) Uani 1 1 d . . . H3 H 0.8032 0.7777 1.0861 0.037 Uiso 1 1 calc R . . C4 C 0.77674(18) 0.70714(18) 0.9432(2) 0.0347(6) Uani 1 1 d . . . H4 H 0.8266 0.6695 0.9486 0.042 Uiso 1 1 calc R . . C5 C 0.71746(18) 0.69780(17) 0.8537(2) 0.0312(6) Uani 1 1 d . . . H5 H 0.7269 0.6528 0.7983 0.037 Uiso 1 1 calc R . . C6 C 0.64392(16) 0.75290(16) 0.84248(19) 0.0246(5) Uani 1 1 d . . . C7 C 0.67872(16) 0.89257(15) 1.11438(19) 0.0242(5) Uani 1 1 d . . . C8 C 0.61027(18) 0.88103(17) 1.19340(19) 0.0293(6) Uani 1 1 d . . . C9 C 0.6029(2) 0.93809(19) 1.2876(2) 0.0376(7) Uani 1 1 d . . . H9 H 0.5564 0.9297 1.3411 0.045 Uiso 1 1 calc R . . C10 C 0.6621(2) 1.0067(2) 1.3044(2) 0.0417(8) Uani 1 1 d . . . C11 C 0.7294(2) 1.01651(19) 1.2271(3) 0.0405(7) Uani 1 1 d . . . H11 H 0.7700 1.0635 1.2376 0.049 Uiso 1 1 calc R . . C12 C 0.74081(18) 0.95998(16) 1.1333(2) 0.0302(6) Uani 1 1 d . . . C13 C 0.5443(2) 0.80672(19) 1.1809(2) 0.0397(7) Uani 1 1 d . . . H13A H 0.5758 0.7509 1.1707 0.060 Uiso 1 1 calc R . . H13B H 0.5069 0.8177 1.1138 0.060 Uiso 1 1 calc R . . H13C H 0.5077 0.8035 1.2501 0.060 Uiso 1 1 calc R . . C14 C 0.6528(3) 1.0675(2) 1.4079(3) 0.0673(12) Uani 1 1 d . . . H14A H 0.6720 1.1270 1.3869 0.101 Uiso 1 1 calc R . . H14B H 0.6893 1.0455 1.4711 0.101 Uiso 1 1 calc R . . H14C H 0.5910 1.0691 1.4323 0.101 Uiso 1 1 calc R . . C15 C 0.82261(19) 0.97218(19) 1.0609(3) 0.0414(7) Uani 1 1 d . . . H15A H 0.8737 0.9484 1.1020 0.062 Uiso 1 1 calc R . . H15B H 0.8317 1.0351 1.0460 0.062 Uiso 1 1 calc R . . H15C H 0.8155 0.9409 0.9877 0.062 Uiso 1 1 calc R . . C16 C 0.58622(16) 0.73735(16) 0.73946(19) 0.0240(5) Uani 1 1 d . . . C17 C 0.60216(16) 0.78317(16) 0.6374(2) 0.0262(5) Uani 1 1 d . . . C18 C 0.55050(17) 0.76499(17) 0.5412(2) 0.0298(6) Uani 1 1 d . . . H18 H 0.5603 0.7973 0.4724 0.036 Uiso 1 1 calc R . . C19 C 0.48535(17) 0.70116(17) 0.5429(2) 0.0301(6) Uani 1 1 d . . . C20 C 0.47051(18) 0.65604(17) 0.6447(2) 0.0305(6) Uani 1 1 d . . . H20 H 0.4259 0.6122 0.6470 0.037 Uiso 1 1 calc R . . C21 C 0.51930(17) 0.67319(16) 0.7440(2) 0.0277(5) Uani 1 1 d . . . C22 C 0.6736(2) 0.85241(19) 0.6298(2) 0.0415(7) Uani 1 1 d . . . H22A H 0.7290 0.8281 0.6591 0.062 Uiso 1 1 calc R . . H22B H 0.6567 0.9038 0.6758 0.062 Uiso 1 1 calc R . . H22C H 0.6813 0.8702 0.5494 0.062 Uiso 1 1 calc R . . C23 C 0.4304(2) 0.6823(2) 0.4370(2) 0.0425(7) Uani 1 1 d . . . H23A H 0.4647 0.6962 0.3680 0.064 Uiso 1 1 calc R . . H23B H 0.3770 0.7186 0.4386 0.064 Uiso 1 1 calc R . . H23C H 0.4140 0.6199 0.4359 0.064 Uiso 1 1 calc R . . C24 C 0.4978(2) 0.62686(19) 0.8555(2) 0.0402(7) Uani 1 1 d . . . H24A H 0.4518 0.5827 0.8419 0.060 Uiso 1 1 calc R . . H24B H 0.4767 0.6700 0.9118 0.060 Uiso 1 1 calc R . . H24C H 0.5508 0.5978 0.8851 0.060 Uiso 1 1 calc R . . C25 C 0.35357(15) 0.90752(15) 0.80330(18) 0.0210(5) Uani 1 1 d . . . C26 C 0.28651(16) 0.96783(16) 0.8177(2) 0.0269(5) Uani 1 1 d . . . H26 H 0.2936 1.0149 0.8707 0.032 Uiso 1 1 calc R . . C27 C 0.20841(17) 0.96044(17) 0.7552(2) 0.0305(6) Uani 1 1 d . . . H27 H 0.1630 1.0026 0.7663 0.037 Uiso 1 1 calc R . . C28 C 0.19596(17) 0.89222(17) 0.6768(2) 0.0292(6) Uani 1 1 d . . . C29 C 0.26356(17) 0.83145(18) 0.6649(2) 0.0312(6) Uani 1 1 d . . . H29 H 0.2559 0.7835 0.6134 0.037 Uiso 1 1 calc R . . C30 C 0.34186(17) 0.83827(17) 0.7255(2) 0.0288(6) Uani 1 1 d . . . H30 H 0.3873 0.7961 0.7143 0.035 Uiso 1 1 calc R . . C31 C 0.11215(19) 0.8855(2) 0.6062(2) 0.0430(7) Uani 1 1 d . . . H31A H 0.0912 0.8244 0.6066 0.064 Uiso 1 1 calc R . . H31B H 0.1242 0.9037 0.5269 0.064 Uiso 1 1 calc R . . H31C H 0.0670 0.9239 0.6393 0.064 Uiso 1 1 calc R . . H1 H 0.5000 1.0000 1.082(4) 0.058(13) Uiso 1 2 d S . . 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 0.0254(5) 0.0199(5) 0.0194(5) 0.000 0.000 0.0016(4) N1 0.0229(10) 0.0204(10) 0.0168(9) 0.0021(8) -0.0017(8) 0.0018(8) N2 0.0247(10) 0.0220(10) 0.0195(9) 0.0018(8) -0.0016(8) 0.0019(8) N3 0.0203(10) 0.0204(10) 0.0227(9) 0.0020(8) -0.0007(8) 0.0027(8) C1 0.0233(12) 0.0202(11) 0.0172(10) 0.0032(9) -0.0029(9) 0.0020(9) C2 0.0249(12) 0.0229(12) 0.0195(10) 0.0004(10) -0.0047(10) 0.0022(9) C3 0.0340(14) 0.0349(14) 0.0225(12) -0.0009(11) -0.0096(11) 0.0065(11) C4 0.0337(14) 0.0364(15) 0.0340(14) -0.0043(13) -0.0088(12) 0.0159(12) C5 0.0379(15) 0.0301(13) 0.0257(13) -0.0090(11) -0.0047(11) 0.0131(11) C6 0.0315(13) 0.0235(12) 0.0189(11) -0.0004(10) -0.0028(10) 0.0044(10) C7 0.0305(13) 0.0225(12) 0.0196(11) 0.0027(10) -0.0063(10) 0.0064(10) C8 0.0389(15) 0.0318(14) 0.0171(11) 0.0018(11) -0.0049(11) 0.0074(12) C9 0.0478(17) 0.0476(17) 0.0172(11) 0.0013(12) -0.0043(12) 0.0188(14) C10 0.0558(19) 0.0401(16) 0.0292(14) -0.0147(13) -0.0193(14) 0.0173(14) C11 0.0514(18) 0.0278(14) 0.0423(16) -0.0072(13) -0.0197(15) 0.0047(13) C12 0.0350(14) 0.0258(13) 0.0297(12) -0.0004(11) -0.0113(12) 0.0015(11) C13 0.0408(16) 0.0504(18) 0.0278(13) 0.0066(13) 0.0029(13) -0.0033(14) C14 0.096(3) 0.063(2) 0.0434(18) -0.0313(18) -0.022(2) 0.025(2) C15 0.0383(16) 0.0386(16) 0.0473(16) 0.0039(14) -0.0083(14) -0.0064(13) C16 0.0303(13) 0.0226(12) 0.0190(11) -0.0045(10) -0.0037(10) 0.0063(10) C17 0.0295(13) 0.0280(13) 0.0210(11) -0.0018(10) -0.0049(11) 0.0015(10) C18 0.0359(14) 0.0331(14) 0.0203(11) 0.0007(11) -0.0041(11) -0.0017(11) C19 0.0343(14) 0.0319(14) 0.0241(12) -0.0060(11) -0.0083(12) 0.0017(11) C20 0.0356(15) 0.0235(13) 0.0324(13) -0.0063(11) -0.0032(12) -0.0036(11) C21 0.0349(14) 0.0215(12) 0.0266(12) -0.0026(10) 0.0006(11) 0.0041(10) C22 0.0514(18) 0.0474(18) 0.0258(13) 0.0027(13) -0.0059(13) -0.0187(15) C23 0.0490(18) 0.0473(18) 0.0313(14) -0.0020(14) -0.0164(14) -0.0069(14) C24 0.0566(19) 0.0299(15) 0.0341(14) 0.0039(13) -0.0007(14) -0.0061(14) C25 0.0223(12) 0.0221(11) 0.0186(11) 0.0059(10) 0.0008(9) -0.0023(9) C26 0.0278(13) 0.0211(12) 0.0317(13) 0.0005(11) 0.0008(11) -0.0003(10) C27 0.0235(13) 0.0289(14) 0.0391(14) 0.0050(12) 0.0019(11) 0.0006(10) C28 0.0283(13) 0.0359(14) 0.0235(11) 0.0090(11) -0.0019(11) -0.0061(11) C29 0.0320(14) 0.0376(15) 0.0240(12) -0.0025(11) -0.0033(11) -0.0020(11) C30 0.0288(13) 0.0339(14) 0.0238(12) -0.0022(11) -0.0031(11) 0.0032(11) C31 0.0328(16) 0.0551(19) 0.0411(16) 0.0098(15) -0.0109(13) -0.0026(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 N3 1.920(2) . ? Al1 N3 1.920(2) 3_675 ? Al1 N1 2.0807(19) 3_675 ? Al1 N1 2.0807(19) . ? N1 N2 1.311(3) . ? N1 C1 1.429(3) . ? N2 N3 1.327(3) . ? N3 C25 1.413(3) . ? C1 C2 1.408(3) . ? C1 C6 1.409(3) . ? C2 C3 1.399(3) . ? C2 C7 1.491(3) . ? C3 C4 1.376(4) . ? C4 C5 1.383(4) . ? C5 C6 1.401(3) . ? C6 C16 1.503(3) . ? C7 C8 1.398(4) . ? C7 C12 1.408(3) . ? C8 C9 1.400(4) . ? C8 C13 1.515(4) . ? C9 C10 1.390(4) . ? C10 C11 1.369(4) . ? C10 C14 1.523(4) . ? C11 C12 1.399(4) . ? C12 C15 1.511(4) . ? C16 C17 1.397(3) . ? C16 C21 1.408(3) . ? C17 C18 1.394(3) . ? C17 C22 1.512(4) . ? C18 C19 1.384(3) . ? C19 C20 1.386(3) . ? C19 C23 1.515(3) . ? C20 C21 1.396(3) . ? C21 C24 1.511(4) . ? C25 C26 1.379(3) . ? C25 C30 1.398(3) . ? C26 C27 1.395(4) . ? C27 C28 1.392(4) . ? C28 C29 1.386(4) . ? C28 C31 1.518(4) . ? C29 C30 1.386(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 N3 Al1 N3 112.99(12) . 3_675 ? N3 Al1 N1 101.77(8) . 3_675 ? N3 Al1 N1 63.65(8) 3_675 3_675 ? N3 Al1 N1 63.65(8) . . ? N3 Al1 N1 101.77(8) 3_675 . ? N1 Al1 N1 154.89(11) 3_675 . ? N2 N1 C1 115.94(18) . . ? N2 N1 Al1 91.40(13) . . ? C1 N1 Al1 152.52(15) . . ? N1 N2 N3 106.48(17) . . ? N2 N3 C25 116.55(18) . . ? N2 N3 Al1 98.30(13) . . ? C25 N3 Al1 145.09(15) . . ? C2 C1 C6 120.7(2) . . ? C2 C1 N1 117.4(2) . . ? C6 C1 N1 121.9(2) . . ? C3 C2 C1 118.4(2) . . ? C3 C2 C7 117.2(2) . . ? C1 C2 C7 124.3(2) . . ? C4 C3 C2 121.8(2) . . ? C3 C4 C5 119.2(2) . . ? C4 C5 C6 121.8(2) . . ? C5 C6 C1 118.1(2) . . ? C5 C6 C16 116.4(2) . . ? C1 C6 C16 125.5(2) . . ? C8 C7 C12 119.1(2) . . ? C8 C7 C2 119.9(2) . . ? C12 C7 C2 120.8(2) . . ? C7 C8 C9 119.7(3) . . ? C7 C8 C13 121.4(2) . . ? C9 C8 C13 118.9(2) . . ? C10 C9 C8 121.5(3) . . ? C11 C10 C9 118.1(2) . . ? C11 C10 C14 121.5(3) . . ? C9 C10 C14 120.3(3) . . ? C10 C11 C12 122.6(3) . . ? C11 C12 C7 119.0(3) . . ? C11 C12 C15 117.5(2) . . ? C7 C12 C15 123.5(2) . . ? C17 C16 C21 120.1(2) . . ? C17 C16 C6 119.9(2) . . ? C21 C16 C6 119.9(2) . . ? C18 C17 C16 119.1(2) . . ? C18 C17 C22 119.6(2) . . ? C16 C17 C22 121.3(2) . . ? C19 C18 C17 121.9(2) . . ? C18 C19 C20 118.3(2) . . ? C18 C19 C23 120.9(2) . . ? C20 C19 C23 120.8(2) . . ? C19 C20 C21 121.9(2) . . ? C20 C21 C16 118.7(2) . . ? C20 C21 C24 120.6(2) . . ? C16 C21 C24 120.7(2) . . ? C26 C25 C30 118.9(2) . . ? C26 C25 N3 118.5(2) . . ? C30 C25 N3 122.6(2) . . ? C25 C26 C27 120.7(2) . . ? C28 C27 C26 121.1(2) . . ? C29 C28 C27 117.4(2) . . ? C29 C28 C31 121.4(2) . . ? C27 C28 C31 121.2(2) . . ? C30 C29 C28 122.3(2) . . ? C29 C30 C25 119.6(2) . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 29.11 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.307 _refine_diff_density_min -0.244 _refine_diff_density_rms 0.046 _chemical_compound_source Et2O #===END data_Compound4 _database_code_depnum_ccdc_archive 'CCDC 704418' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common (AlH2(DmpN3Mes)(THF)) _chemical_melting_point 398 _chemical_formula_moiety 'C37 H46 Al N3 O' _chemical_formula_sum 'C37 H46 Al N3 O' _chemical_formula_weight 575.75 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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_int_tables_number 14 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 12.1434(5) _cell_length_b 22.3094(10) _cell_length_c 12.2121(6) _cell_angle_alpha 90.00 _cell_angle_beta 94.860(2) _cell_angle_gamma 90.00 _cell_volume 3296.5(3) _cell_formula_units_Z 4 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 25717 _cell_measurement_theta_min 1.91 _cell_measurement_theta_max 30.01 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.160 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1240 _exptl_absorpt_coefficient_mu 0.094 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.9814 _exptl_absorpt_correction_T_max 0.9907 _exptl_absorpt_process_details 'Bruker Scalepack' _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker X8 Apex' _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 25717 _diffrn_reflns_av_R_equivalents 0.0459 _diffrn_reflns_av_sigmaI/netI 0.0704 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -31 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.91 _diffrn_reflns_theta_max 30.01 _reflns_number_total 9228 _reflns_number_gt 7248 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker AXS Collect Software' _computing_cell_refinement 'Bruker Scalepack' _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^)+(0.0230P)^2^+3.5003P] 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 9228 _refine_ls_number_parameters 396 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1154 _refine_ls_R_factor_gt 0.0895 _refine_ls_wR_factor_ref 0.1575 _refine_ls_wR_factor_gt 0.1476 _refine_ls_goodness_of_fit_ref 1.215 _refine_ls_restrained_S_all 1.215 _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 Al1 Al 0.14594(6) 0.06197(3) 0.31648(6) 0.01905(16) Uani 1 1 d . . . O1 O 0.11797(14) -0.01938(8) 0.37861(15) 0.0263(4) Uani 1 1 d . . . N1 N 0.22125(15) 0.12076(8) 0.21192(15) 0.0159(4) Uani 1 1 d . . . N2 N 0.30556(16) 0.08507(9) 0.20537(15) 0.0182(4) Uani 1 1 d . . . N3 N 0.28630(16) 0.03716(8) 0.26414(15) 0.0169(4) Uani 1 1 d . . . C1 C 0.21639(18) 0.16973(10) 0.13756(18) 0.0159(4) Uani 1 1 d . . . C2 C 0.19002(19) 0.22639(10) 0.17740(19) 0.0187(5) Uani 1 1 d . . . C3 C 0.1798(2) 0.27456(11) 0.1048(2) 0.0252(5) Uani 1 1 d . . . H3 H 0.1618 0.3131 0.1312 0.030 Uiso 1 1 calc R . . C4 C 0.1956(2) 0.26702(11) -0.0055(2) 0.0263(6) Uani 1 1 d . . . H4 H 0.1893 0.3003 -0.0541 0.032 Uiso 1 1 calc R . . C5 C 0.2205(2) 0.21072(11) -0.0445(2) 0.0239(5) Uani 1 1 d . . . H5 H 0.2308 0.2058 -0.1203 0.029 Uiso 1 1 calc R . . C6 C 0.23089(19) 0.16102(10) 0.02529(19) 0.0181(5) Uani 1 1 d . . . C7 C 0.1726(2) 0.23447(10) 0.29666(19) 0.0186(5) Uani 1 1 d . . . C8 C 0.0660(2) 0.23012(10) 0.3329(2) 0.0205(5) Uani 1 1 d . . . C9 C 0.0523(2) 0.23872(10) 0.4442(2) 0.0227(5) Uani 1 1 d . . . H9 H -0.0198 0.2358 0.4686 0.027 Uiso 1 1 calc R . . C10 C 0.1403(2) 0.25133(11) 0.5202(2) 0.0242(5) Uani 1 1 d . . . C11 C 0.2451(2) 0.25500(11) 0.4827(2) 0.0249(5) Uani 1 1 d . . . H11 H 0.3063 0.2635 0.5340 0.030 Uiso 1 1 calc R . . C12 C 0.2634(2) 0.24663(11) 0.3731(2) 0.0220(5) Uani 1 1 d . . . C13 C -0.0319(2) 0.21497(13) 0.2532(2) 0.0294(6) Uani 1 1 d . . . H13A H -0.0248 0.1737 0.2272 0.044 Uiso 1 1 calc R . . H13B H -0.0343 0.2425 0.1905 0.044 Uiso 1 1 calc R . . H13C H -0.1001 0.2189 0.2902 0.044 Uiso 1 1 calc R . . C14 C 0.1229(3) 0.25977(13) 0.6401(2) 0.0351(7) Uani 1 1 d . . . H14A H 0.1249 0.2207 0.6769 0.053 Uiso 1 1 calc R . . H14B H 0.0510 0.2787 0.6468 0.053 Uiso 1 1 calc R . . H14C H 0.1816 0.2854 0.6746 0.053 Uiso 1 1 calc R . . C15 C 0.3787(2) 0.25028(13) 0.3363(2) 0.0309(6) Uani 1 1 d . . . H15A H 0.4318 0.2559 0.4006 0.046 Uiso 1 1 calc R . . H15B H 0.3834 0.2842 0.2860 0.046 Uiso 1 1 calc R . . H15C H 0.3958 0.2131 0.2987 0.046 Uiso 1 1 calc R . . C16 C 0.2450(2) 0.10002(10) -0.02249(18) 0.0192(5) Uani 1 1 d . . . C17 C 0.1500(2) 0.06625(11) -0.0543(2) 0.0221(5) Uani 1 1 d . . . C18 C 0.1619(2) 0.00999(11) -0.1021(2) 0.0250(5) Uani 1 1 d . . . H18 H 0.0977 -0.0129 -0.1234 0.030 Uiso 1 1 calc R . . C19 C 0.2649(2) -0.01335(11) -0.1192(2) 0.0242(5) Uani 1 1 d . . . C20 C 0.3582(2) 0.02072(11) -0.0870(2) 0.0220(5) Uani 1 1 d . . . H20 H 0.4292 0.0052 -0.0982 0.026 Uiso 1 1 calc R . . C21 C 0.3502(2) 0.07689(10) -0.03896(18) 0.0189(5) Uani 1 1 d . . . C22 C 0.0363(2) 0.09039(13) -0.0369(2) 0.0314(6) Uani 1 1 d . . . H22A H 0.0318 0.0989 0.0413 0.047 Uiso 1 1 calc R . . H22B H -0.0197 0.0606 -0.0613 0.047 Uiso 1 1 calc R . . H22C H 0.0233 0.1274 -0.0794 0.047 Uiso 1 1 calc R . . C23 C 0.2744(3) -0.07476(12) -0.1703(3) 0.0371(7) Uani 1 1 d . . . H23A H 0.2839 -0.1050 -0.1121 0.056 Uiso 1 1 calc R . . H23B H 0.3385 -0.0756 -0.2141 0.056 Uiso 1 1 calc R . . H23C H 0.2072 -0.0834 -0.2178 0.056 Uiso 1 1 calc R . . C24 C 0.4525(2) 0.11193(11) -0.0030(2) 0.0235(5) Uani 1 1 d . . . H24A H 0.4574 0.1173 0.0769 0.035 Uiso 1 1 calc R . . H24B H 0.4493 0.1512 -0.0390 0.035 Uiso 1 1 calc R . . H24C H 0.5178 0.0901 -0.0234 0.035 Uiso 1 1 calc R . . C25 C 0.37894(19) -0.00242(10) 0.28177(18) 0.0160(4) Uani 1 1 d . . . C26 C 0.3701(2) -0.06105(11) 0.23996(18) 0.0188(5) Uani 1 1 d . . . C27 C 0.4607(2) -0.09937(11) 0.25943(19) 0.0228(5) Uani 1 1 d . . . H27 H 0.4553 -0.1393 0.2326 0.027 Uiso 1 1 calc R . . C28 C 0.5582(2) -0.08088(12) 0.3167(2) 0.0263(6) Uani 1 1 d . . . C29 C 0.5635(2) -0.02271(12) 0.3577(2) 0.0277(6) Uani 1 1 d . . . H29 H 0.6296 -0.0098 0.3980 0.033 Uiso 1 1 calc R . . C30 C 0.4755(2) 0.01736(11) 0.34182(19) 0.0209(5) Uani 1 1 d . . . C31 C 0.2677(2) -0.08154(11) 0.1720(2) 0.0254(5) Uani 1 1 d . . . H31A H 0.2808 -0.1211 0.1409 0.038 Uiso 1 1 calc R . . H31B H 0.2497 -0.0529 0.1123 0.038 Uiso 1 1 calc R . . H31C H 0.2059 -0.0839 0.2185 0.038 Uiso 1 1 calc R . . C32 C 0.6582(3) -0.12157(14) 0.3314(3) 0.0405(7) Uani 1 1 d . . . H32A H 0.7112 -0.1103 0.2788 0.061 Uiso 1 1 calc R . . H32B H 0.6350 -0.1632 0.3185 0.061 Uiso 1 1 calc R . . H32C H 0.6930 -0.1175 0.4064 0.061 Uiso 1 1 calc R . . C33 C 0.4862(2) 0.08029(11) 0.3871(2) 0.0284(6) Uani 1 1 d . . . H33A H 0.5054 0.1077 0.3289 0.043 Uiso 1 1 calc R . . H33B H 0.5444 0.0813 0.4478 0.043 Uiso 1 1 calc R . . H33C H 0.4159 0.0926 0.4139 0.043 Uiso 1 1 calc R . . C34 C 0.1847(2) -0.04689(13) 0.4698(2) 0.0294(6) Uani 1 1 d . . . H34A H 0.2050 -0.0170 0.5280 0.035 Uiso 1 1 calc R . . H34B H 0.2532 -0.0642 0.4445 0.035 Uiso 1 1 calc R . . C35 C 0.1124(2) -0.09554(13) 0.5122(2) 0.0320(6) Uani 1 1 d . . . H35A H 0.0676 -0.0800 0.5700 0.038 Uiso 1 1 calc R . . H35B H 0.1572 -0.1298 0.5419 0.038 Uiso 1 1 calc R . . C36 C 0.0398(2) -0.11334(12) 0.4101(2) 0.0318(6) Uani 1 1 d . . . H36A H 0.0790 -0.1411 0.3635 0.038 Uiso 1 1 calc R . . H36B H -0.0295 -0.1324 0.4295 0.038 Uiso 1 1 calc R . . C37 C 0.0173(2) -0.05417(12) 0.3533(2) 0.0287(6) Uani 1 1 d . . . H37A H 0.0025 -0.0598 0.2730 0.034 Uiso 1 1 calc R . . H37B H -0.0470 -0.0340 0.3818 0.034 Uiso 1 1 calc R . . H1 H 0.165(2) 0.0932(13) 0.428(2) 0.035(8) Uiso 1 1 d . . . H2 H 0.035(2) 0.0586(12) 0.250(2) 0.024(7) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Al1 0.0175(4) 0.0183(4) 0.0220(4) 0.0019(3) 0.0054(3) -0.0005(3) O1 0.0223(9) 0.0252(9) 0.0310(10) 0.0099(8) -0.0007(7) -0.0065(7) N1 0.0167(10) 0.0132(9) 0.0182(9) -0.0001(7) 0.0038(7) 0.0013(7) N2 0.0228(11) 0.0155(9) 0.0163(9) 0.0001(7) 0.0025(8) -0.0007(8) N3 0.0193(10) 0.0124(9) 0.0198(9) 0.0022(7) 0.0059(8) 0.0006(7) C1 0.0159(11) 0.0135(10) 0.0186(11) 0.0019(8) 0.0024(8) -0.0020(8) C2 0.0187(12) 0.0157(11) 0.0219(11) 0.0023(9) 0.0023(9) -0.0005(9) C3 0.0321(15) 0.0159(11) 0.0282(13) 0.0030(10) 0.0068(11) 0.0026(10) C4 0.0316(15) 0.0194(12) 0.0283(13) 0.0091(10) 0.0052(11) 0.0028(11) C5 0.0304(14) 0.0232(13) 0.0183(11) 0.0038(9) 0.0041(10) -0.0001(11) C6 0.0189(12) 0.0174(11) 0.0182(11) -0.0004(9) 0.0030(9) -0.0008(9) C7 0.0245(13) 0.0107(10) 0.0210(11) 0.0002(8) 0.0054(9) 0.0033(9) C8 0.0235(13) 0.0116(10) 0.0268(12) 0.0026(9) 0.0036(10) 0.0044(9) C9 0.0276(14) 0.0137(11) 0.0284(13) 0.0052(9) 0.0117(10) 0.0046(10) C10 0.0392(15) 0.0128(11) 0.0212(12) 0.0031(9) 0.0055(10) 0.0040(10) C11 0.0312(14) 0.0191(12) 0.0236(12) 0.0021(10) -0.0019(10) -0.0006(10) C12 0.0277(13) 0.0141(11) 0.0247(12) 0.0022(9) 0.0057(10) 0.0005(10) C13 0.0223(14) 0.0328(15) 0.0335(15) 0.0012(12) 0.0048(11) 0.0022(11) C14 0.0525(19) 0.0290(15) 0.0249(14) 0.0022(11) 0.0092(12) 0.0026(13) C15 0.0265(14) 0.0321(15) 0.0346(15) -0.0016(12) 0.0047(11) -0.0028(12) C16 0.0253(13) 0.0160(11) 0.0164(10) 0.0021(9) 0.0028(9) -0.0015(9) C17 0.0221(13) 0.0223(12) 0.0220(12) 0.0026(10) 0.0014(9) -0.0018(10) C18 0.0274(14) 0.0225(13) 0.0243(12) 0.0001(10) -0.0027(10) -0.0105(11) C19 0.0340(15) 0.0168(12) 0.0213(12) -0.0023(9) -0.0001(10) -0.0028(10) C20 0.0247(13) 0.0187(12) 0.0232(12) -0.0030(9) 0.0060(10) -0.0001(10) C21 0.0252(13) 0.0161(11) 0.0156(10) -0.0001(8) 0.0025(9) -0.0042(9) C22 0.0225(14) 0.0376(16) 0.0336(15) -0.0014(12) -0.0003(11) -0.0009(12) C23 0.0458(18) 0.0229(14) 0.0417(17) -0.0106(12) -0.0023(13) -0.0020(13) C24 0.0212(13) 0.0227(12) 0.0277(13) -0.0054(10) 0.0080(10) -0.0071(10) C25 0.0205(12) 0.0137(10) 0.0144(10) 0.0036(8) 0.0051(8) 0.0001(9) C26 0.0229(12) 0.0170(11) 0.0176(11) 0.0022(9) 0.0077(9) -0.0004(9) C27 0.0339(15) 0.0147(11) 0.0210(12) 0.0008(9) 0.0105(10) 0.0017(10) C28 0.0297(14) 0.0243(13) 0.0251(13) 0.0045(10) 0.0028(10) 0.0090(11) C29 0.0238(14) 0.0285(14) 0.0301(14) -0.0022(11) -0.0025(10) 0.0033(11) C30 0.0235(13) 0.0199(12) 0.0195(11) -0.0003(9) 0.0026(9) 0.0012(10) C31 0.0274(14) 0.0187(12) 0.0302(13) -0.0057(10) 0.0036(10) -0.0050(10) C32 0.0413(18) 0.0355(17) 0.0435(18) 0.0002(14) -0.0032(14) 0.0198(14) C33 0.0347(15) 0.0213(13) 0.0283(13) -0.0057(10) -0.0024(11) -0.0007(11) C34 0.0243(14) 0.0347(15) 0.0292(14) 0.0123(11) 0.0028(11) 0.0011(11) C35 0.0354(16) 0.0283(14) 0.0336(15) 0.0117(12) 0.0114(12) 0.0028(12) C36 0.0407(17) 0.0195(13) 0.0370(15) -0.0032(11) 0.0142(12) -0.0065(12) C37 0.0264(14) 0.0237(13) 0.0359(15) 0.0022(11) 0.0018(11) -0.0096(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 N3 1.950(2) . ? Al1 O1 2.0071(18) . ? Al1 N1 2.094(2) . ? O1 C34 1.456(3) . ? O1 C37 1.459(3) . ? N1 N2 1.305(3) . ? N1 C1 1.419(3) . ? N2 N3 1.319(3) . ? N3 C25 1.432(3) . ? C1 C2 1.401(3) . ? C1 C6 1.410(3) . ? C2 C3 1.392(3) . ? C2 C7 1.500(3) . ? C3 C4 1.387(3) . ? C4 C5 1.386(4) . ? C5 C6 1.398(3) . ? C6 C16 1.496(3) . ? C7 C8 1.406(3) . ? C7 C12 1.409(3) . ? C8 C9 1.397(3) . ? C8 C13 1.510(4) . ? C9 C10 1.383(4) . ? C10 C11 1.391(4) . ? C10 C14 1.509(3) . ? C11 C12 1.388(3) . ? C12 C15 1.509(4) . ? C16 C17 1.405(3) . ? C16 C21 1.407(3) . ? C17 C18 1.397(4) . ? C17 C22 1.514(4) . ? C18 C19 1.387(4) . ? C19 C20 1.394(3) . ? C19 C23 1.514(4) . ? C20 C21 1.391(3) . ? C21 C24 1.502(3) . ? C25 C30 1.401(3) . ? C25 C26 1.405(3) . ? C26 C27 1.398(3) . ? C26 C31 1.507(3) . ? C27 C28 1.386(4) . ? C28 C29 1.390(4) . ? C28 C32 1.515(4) . ? C29 C30 1.394(3) . ? C30 C33 1.510(3) . ? C34 C35 1.515(4) . ? C35 C36 1.517(4) . ? C36 C37 1.505(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 N3 Al1 O1 92.74(8) . . ? N3 Al1 N1 62.55(8) . . ? O1 Al1 N1 153.32(8) . . ? C34 O1 C37 109.86(19) . . ? C34 O1 Al1 124.69(15) . . ? C37 O1 Al1 124.51(15) . . ? N2 N1 C1 114.89(18) . . ? N2 N1 Al1 92.33(13) . . ? C1 N1 Al1 151.17(15) . . ? N1 N2 N3 106.54(18) . . ? N2 N3 C25 114.08(18) . . ? N2 N3 Al1 98.54(14) . . ? C25 N3 Al1 145.38(15) . . ? C2 C1 C6 120.9(2) . . ? C2 C1 N1 118.1(2) . . ? C6 C1 N1 120.9(2) . . ? C3 C2 C1 119.1(2) . . ? C3 C2 C7 120.9(2) . . ? C1 C2 C7 120.0(2) . . ? C4 C3 C2 120.8(2) . . ? C5 C4 C3 119.7(2) . . ? C4 C5 C6 121.3(2) . . ? C5 C6 C1 118.1(2) . . ? C5 C6 C16 119.4(2) . . ? C1 C6 C16 122.2(2) . . ? C8 C7 C12 119.6(2) . . ? C8 C7 C2 120.4(2) . . ? C12 C7 C2 120.0(2) . . ? C9 C8 C7 119.1(2) . . ? C9 C8 C13 120.4(2) . . ? C7 C8 C13 120.5(2) . . ? C10 C9 C8 122.1(2) . . ? C9 C10 C11 117.9(2) . . ? C9 C10 C14 120.9(2) . . ? C11 C10 C14 121.3(2) . . ? C12 C11 C10 122.3(2) . . ? C11 C12 C7 119.0(2) . . ? C11 C12 C15 120.5(2) . . ? C7 C12 C15 120.5(2) . . ? C17 C16 C21 119.8(2) . . ? C17 C16 C6 118.5(2) . . ? C21 C16 C6 121.6(2) . . ? C18 C17 C16 119.1(2) . . ? C18 C17 C22 120.4(2) . . ? C16 C17 C22 120.5(2) . . ? C19 C18 C17 121.8(2) . . ? C18 C19 C20 118.3(2) . . ? C18 C19 C23 120.3(2) . . ? C20 C19 C23 121.4(2) . . ? C21 C20 C19 121.7(2) . . ? C20 C21 C16 119.2(2) . . ? C20 C21 C24 120.4(2) . . ? C16 C21 C24 120.4(2) . . ? C30 C25 C26 121.2(2) . . ? C30 C25 N3 119.8(2) . . ? C26 C25 N3 119.0(2) . . ? C27 C26 C25 118.2(2) . . ? C27 C26 C31 120.6(2) . . ? C25 C26 C31 121.1(2) . . ? C28 C27 C26 122.0(2) . . ? C27 C28 C29 118.1(2) . . ? C27 C28 C32 121.6(2) . . ? C29 C28 C32 120.3(3) . . ? C28 C29 C30 122.5(2) . . ? C29 C30 C25 117.9(2) . . ? C29 C30 C33 120.3(2) . . ? C25 C30 C33 121.8(2) . . ? O1 C34 C35 105.2(2) . . ? C34 C35 C36 102.7(2) . . ? C37 C36 C35 102.7(2) . . ? O1 C37 C36 104.6(2) . . ? _diffrn_measured_fraction_theta_max 0.960 _diffrn_reflns_theta_full 30.01 _diffrn_measured_fraction_theta_full 0.960 _refine_diff_density_max 0.374 _refine_diff_density_min -0.396 _refine_diff_density_rms 0.060 _chemical_compound_source THF #===END data_Compound6 _database_code_depnum_ccdc_archive 'CCDC 704419' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common (Li(THF)(mu-H)(mu-DmpN3Mes)GaH2) _chemical_melting_point 398 _chemical_formula_moiety 'C37 H47 Ga Li N3 O' _chemical_formula_sum 'C37 H47 Ga Li N3 O' _chemical_formula_weight 626.44 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' Ga Ga 0.2307 1.6083 '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 8.6815(3) _cell_length_b 12.2606(4) _cell_length_c 17.0034(6) _cell_angle_alpha 71.856(1) _cell_angle_beta 84.267(1) _cell_angle_gamma 85.696(1) _cell_volume 1709.41(10) _cell_formula_units_Z 2 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 28145 _cell_measurement_theta_min 2.36 _cell_measurement_theta_max 30.06 _exptl_crystal_description prism _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.217 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 664 _exptl_absorpt_coefficient_mu 0.836 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.8182 _exptl_absorpt_correction_T_max 0.9361 _exptl_absorpt_process_details 'Bruker Scalepack' _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker X8 Apex' _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 28145 _diffrn_reflns_av_R_equivalents 0.0282 _diffrn_reflns_av_sigmaI/netI 0.0374 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.36 _diffrn_reflns_theta_max 30.06 _reflns_number_total 9855 _reflns_number_gt 7634 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker AXS Collect Software' _computing_cell_refinement 'Bruker Scalepack' _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^)+(0.0608P)^2^+0.9356P] 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 9855 _refine_ls_number_parameters 409 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0636 _refine_ls_R_factor_gt 0.0442 _refine_ls_wR_factor_ref 0.1196 _refine_ls_wR_factor_gt 0.1084 _refine_ls_goodness_of_fit_ref 0.977 _refine_ls_restrained_S_all 0.977 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ga1 Ga 0.09244(3) 0.55138(2) 0.378451(14) 0.03646(9) Uani 1 1 d . . . O1 O -0.01453(16) 0.82643(13) 0.41365(9) 0.0352(3) Uani 1 1 d . . . N1 N -0.13268(15) 0.70591(11) 0.25791(8) 0.0164(3) Uani 1 1 d . . . N2 N -0.08255(15) 0.62146(11) 0.22930(8) 0.0171(3) Uani 1 1 d . . . N3 N 0.02397(16) 0.55286(12) 0.27013(8) 0.0195(3) Uani 1 1 d . . . C1 C -0.24427(18) 0.77586(13) 0.20610(10) 0.0178(3) Uani 1 1 d . . . C2 C -0.36967(19) 0.82451(14) 0.24491(10) 0.0197(3) Uani 1 1 d . . . C3 C -0.4870(2) 0.88818(16) 0.19756(11) 0.0285(4) Uani 1 1 d . . . H3 H -0.5731 0.9194 0.2239 0.034 Uiso 1 1 calc R . . C4 C -0.4795(2) 0.90636(18) 0.11281(12) 0.0328(4) Uani 1 1 d . . . H4 H -0.5616 0.9474 0.0813 0.039 Uiso 1 1 calc R . . C5 C -0.3509(2) 0.86411(16) 0.07427(11) 0.0280(4) Uani 1 1 d . . . H5 H -0.3444 0.8792 0.0158 0.034 Uiso 1 1 calc R . . C6 C -0.23094(19) 0.80011(14) 0.11908(10) 0.0206(3) Uani 1 1 d . . . C7 C -0.37908(18) 0.81230(14) 0.33562(10) 0.0187(3) Uani 1 1 d . . . C8 C -0.41262(18) 0.70701(14) 0.39591(10) 0.0201(3) Uani 1 1 d . . . C9 C -0.4215(2) 0.70053(15) 0.47961(11) 0.0233(3) Uani 1 1 d . . . H9 H -0.4426 0.6290 0.5204 0.028 Uiso 1 1 calc R . . C10 C -0.40056(19) 0.79475(16) 0.50548(10) 0.0238(3) Uani 1 1 d . . . C11 C -0.3709(2) 0.89852(15) 0.44502(11) 0.0241(3) Uani 1 1 d . . . H11 H -0.3591 0.9644 0.4616 0.029 Uiso 1 1 calc R . . C12 C -0.3579(2) 0.90908(14) 0.36049(11) 0.0222(3) Uani 1 1 d . . . C13 C -0.4413(2) 0.60185(16) 0.37260(12) 0.0276(4) Uani 1 1 d . . . H13A H -0.3723 0.5379 0.4012 0.041 Uiso 1 1 calc R . . H13B H -0.4207 0.6179 0.3124 0.041 Uiso 1 1 calc R . . H13C H -0.5493 0.5814 0.3889 0.041 Uiso 1 1 calc R . . C14 C -0.4074(2) 0.78320(19) 0.59683(12) 0.0336(4) Uani 1 1 d . . . H14A H -0.3057 0.7558 0.6176 0.050 Uiso 1 1 calc R . . H14B H -0.4852 0.7282 0.6273 0.050 Uiso 1 1 calc R . . H14C H -0.4356 0.8582 0.6048 0.050 Uiso 1 1 calc R . . C15 C -0.3197(3) 1.02349(16) 0.29769(12) 0.0331(4) Uani 1 1 d . . . H15A H -0.4143 1.0616 0.2728 0.050 Uiso 1 1 calc R . . H15B H -0.2440 1.0111 0.2541 0.050 Uiso 1 1 calc R . . H15C H -0.2760 1.0719 0.3254 0.050 Uiso 1 1 calc R . . C16 C -0.08979(19) 0.76944(14) 0.07113(10) 0.0207(3) Uani 1 1 d . . . C17 C 0.0446(2) 0.82918(15) 0.06267(11) 0.0249(3) Uani 1 1 d . . . C18 C 0.1720(2) 0.80679(17) 0.01194(12) 0.0293(4) Uani 1 1 d . . . H18 H 0.2633 0.8477 0.0059 0.035 Uiso 1 1 calc R . . C19 C 0.1683(2) 0.72638(17) -0.02984(11) 0.0291(4) Uani 1 1 d . . . C20 C 0.0349(2) 0.66679(16) -0.02008(11) 0.0273(4) Uani 1 1 d . . . H20 H 0.0316 0.6110 -0.0480 0.033 Uiso 1 1 calc R . . C21 C -0.0952(2) 0.68678(15) 0.02990(10) 0.0231(3) Uani 1 1 d . . . C22 C 0.0558(2) 0.91665(18) 0.10760(13) 0.0331(4) Uani 1 1 d . . . H22A H 0.0714 0.8769 0.1661 0.050 Uiso 1 1 calc R . . H22B H -0.0402 0.9648 0.1038 0.050 Uiso 1 1 calc R . . H22C H 0.1435 0.9650 0.0821 0.050 Uiso 1 1 calc R . . C23 C 0.3086(3) 0.7035(2) -0.08372(14) 0.0416(5) Uani 1 1 d . . . H23A H 0.3800 0.6473 -0.0492 0.062 Uiso 1 1 calc R . . H23B H 0.3611 0.7753 -0.1109 0.062 Uiso 1 1 calc R . . H23C H 0.2756 0.6732 -0.1260 0.062 Uiso 1 1 calc R . . C24 C -0.2355(2) 0.61768(17) 0.04120(12) 0.0304(4) Uani 1 1 d . . . H24A H -0.2189 0.5657 0.0072 0.046 Uiso 1 1 calc R . . H24B H -0.3259 0.6695 0.0240 0.046 Uiso 1 1 calc R . . H24C H -0.2535 0.5727 0.0998 0.046 Uiso 1 1 calc R . . C25 C 0.07017(19) 0.45688(14) 0.23978(10) 0.0200(3) Uani 1 1 d . . . C26 C 0.2215(2) 0.45159(15) 0.20383(10) 0.0235(3) Uani 1 1 d . . . C27 C 0.2715(2) 0.35255(16) 0.18232(11) 0.0273(4) Uani 1 1 d . . . H27 H 0.3742 0.3475 0.1581 0.033 Uiso 1 1 calc R . . C28 C 0.1771(2) 0.26252(16) 0.19508(11) 0.0290(4) Uani 1 1 d . . . C29 C 0.0267(2) 0.27053(16) 0.23052(11) 0.0275(4) Uani 1 1 d . . . H29 H -0.0396 0.2089 0.2395 0.033 Uiso 1 1 calc R . . C30 C -0.0286(2) 0.36755(15) 0.25320(10) 0.0228(3) Uani 1 1 d . . . C31 C 0.3268(2) 0.54891(19) 0.18806(14) 0.0360(4) Uani 1 1 d . . . H31A H 0.2785 0.6194 0.1524 0.054 Uiso 1 1 calc R . . H31B H 0.4257 0.5310 0.1605 0.054 Uiso 1 1 calc R . . H31C H 0.3451 0.5600 0.2410 0.054 Uiso 1 1 calc R . . C32 C 0.2338(3) 0.15639(18) 0.17097(14) 0.0412(5) Uani 1 1 d . . . H32A H 0.3342 0.1702 0.1385 0.062 Uiso 1 1 calc R . . H32B H 0.1586 0.1393 0.1376 0.062 Uiso 1 1 calc R . . H32C H 0.2453 0.0911 0.2212 0.062 Uiso 1 1 calc R . . C33 C -0.1914(2) 0.37299(17) 0.29264(13) 0.0316(4) Uani 1 1 d . . . H33A H -0.1890 0.3936 0.3437 0.047 Uiso 1 1 calc R . . H33B H -0.2365 0.2978 0.3058 0.047 Uiso 1 1 calc R . . H33C H -0.2544 0.4310 0.2540 0.047 Uiso 1 1 calc R . . C34 C 0.0838(4) 0.9103(3) 0.35987(19) 0.0655(9) Uani 1 1 d . . . H34A H 0.0246 0.9844 0.3390 0.079 Uiso 1 1 calc R . . H34B H 0.1267 0.8854 0.3117 0.079 Uiso 1 1 calc R . . C35 C 0.2089(3) 0.9239(3) 0.40669(19) 0.0676(9) Uani 1 1 d . . . H35A H 0.2219 1.0064 0.3984 0.081 Uiso 1 1 calc R . . H35B H 0.3076 0.8903 0.3879 0.081 Uiso 1 1 calc R . . C36 C 0.1670(3) 0.8641(3) 0.49452(18) 0.0594(7) Uani 1 1 d . . . H36A H 0.2568 0.8173 0.5210 0.071 Uiso 1 1 calc R . . H36B H 0.1318 0.9198 0.5247 0.071 Uiso 1 1 calc R . . C37 C 0.0408(3) 0.7902(3) 0.49512(15) 0.0567(7) Uani 1 1 d . . . H37A H 0.0792 0.7088 0.5095 0.068 Uiso 1 1 calc R . . H37B H -0.0442 0.7973 0.5369 0.068 Uiso 1 1 calc R . . Li1 Li -0.1162(4) 0.7252(3) 0.3723(2) 0.0283(6) Uani 1 1 d . . . H1A H -0.063(3) 0.564(2) 0.4231(17) 0.059(8) Uiso 1 1 d . . . H1B H 0.188(4) 0.666(3) 0.363(2) 0.077(10) Uiso 1 1 d . . . H1C H 0.175(4) 0.436(3) 0.4094(19) 0.067(9) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ga1 0.03294(13) 0.05084(16) 0.03555(13) -0.02809(11) -0.02078(9) 0.02426(10) O1 0.0285(7) 0.0394(8) 0.0436(8) -0.0190(7) -0.0089(6) -0.0028(6) N1 0.0157(6) 0.0157(6) 0.0172(6) -0.0043(5) -0.0029(5) 0.0029(5) N2 0.0161(6) 0.0161(6) 0.0172(6) -0.0031(5) -0.0012(5) 0.0015(5) N3 0.0190(6) 0.0198(7) 0.0198(6) -0.0070(5) -0.0041(5) 0.0063(5) C1 0.0176(7) 0.0157(7) 0.0187(7) -0.0034(6) -0.0034(5) 0.0021(6) C2 0.0204(7) 0.0169(7) 0.0195(7) -0.0031(6) -0.0025(6) 0.0036(6) C3 0.0258(9) 0.0301(9) 0.0262(9) -0.0065(7) -0.0036(7) 0.0124(7) C4 0.0320(10) 0.0358(10) 0.0259(9) -0.0050(8) -0.0098(7) 0.0181(8) C5 0.0326(9) 0.0289(9) 0.0183(8) -0.0029(7) -0.0059(7) 0.0103(7) C6 0.0224(8) 0.0185(8) 0.0189(7) -0.0037(6) -0.0015(6) 0.0028(6) C7 0.0158(7) 0.0182(7) 0.0208(7) -0.0052(6) -0.0006(6) 0.0033(6) C8 0.0161(7) 0.0200(8) 0.0225(8) -0.0045(6) -0.0013(6) 0.0001(6) C9 0.0212(8) 0.0219(8) 0.0219(8) -0.0006(6) 0.0006(6) -0.0003(6) C10 0.0179(7) 0.0315(9) 0.0210(8) -0.0080(7) 0.0002(6) 0.0029(7) C11 0.0219(8) 0.0248(9) 0.0269(8) -0.0114(7) 0.0020(6) 0.0004(7) C12 0.0222(8) 0.0197(8) 0.0235(8) -0.0068(6) 0.0016(6) 0.0022(6) C13 0.0263(9) 0.0229(9) 0.0333(9) -0.0077(7) 0.0001(7) -0.0057(7) C14 0.0352(10) 0.0424(11) 0.0227(9) -0.0112(8) 0.0010(7) 0.0033(9) C15 0.0446(11) 0.0197(9) 0.0318(10) -0.0063(7) 0.0082(8) -0.0041(8) C16 0.0233(8) 0.0197(8) 0.0160(7) -0.0021(6) -0.0017(6) 0.0032(6) C17 0.0279(9) 0.0226(8) 0.0220(8) -0.0047(7) -0.0006(6) 0.0016(7) C18 0.0273(9) 0.0301(10) 0.0275(9) -0.0056(8) 0.0026(7) -0.0029(7) C19 0.0278(9) 0.0326(10) 0.0238(8) -0.0067(7) 0.0043(7) 0.0017(7) C20 0.0315(9) 0.0281(9) 0.0223(8) -0.0095(7) -0.0002(7) 0.0034(7) C21 0.0251(8) 0.0245(8) 0.0185(7) -0.0054(6) -0.0028(6) 0.0034(7) C22 0.0366(10) 0.0305(10) 0.0335(10) -0.0124(8) 0.0028(8) -0.0071(8) C23 0.0342(11) 0.0516(14) 0.0393(11) -0.0191(10) 0.0118(9) -0.0007(10) C24 0.0296(9) 0.0327(10) 0.0310(9) -0.0132(8) -0.0002(7) -0.0021(8) C25 0.0224(8) 0.0201(8) 0.0166(7) -0.0055(6) -0.0043(6) 0.0065(6) C26 0.0229(8) 0.0253(9) 0.0215(8) -0.0073(7) -0.0037(6) 0.0062(7) C27 0.0258(9) 0.0312(10) 0.0236(8) -0.0098(7) -0.0004(7) 0.0104(7) C28 0.0392(10) 0.0232(9) 0.0233(8) -0.0081(7) -0.0036(7) 0.0116(8) C29 0.0353(10) 0.0213(8) 0.0254(8) -0.0069(7) -0.0024(7) 0.0006(7) C30 0.0258(8) 0.0204(8) 0.0207(7) -0.0052(6) -0.0015(6) 0.0029(6) C31 0.0260(9) 0.0403(11) 0.0434(11) -0.0171(9) 0.0044(8) -0.0032(8) C32 0.0561(14) 0.0293(10) 0.0389(11) -0.0166(9) -0.0012(10) 0.0157(10) C33 0.0273(9) 0.0283(10) 0.0388(10) -0.0120(8) 0.0067(8) -0.0044(7) C34 0.080(2) 0.0525(16) 0.0606(17) 0.0013(13) -0.0312(15) -0.0289(15) C35 0.0475(15) 0.096(2) 0.0623(18) -0.0205(17) -0.0032(13) -0.0367(16) C36 0.0375(13) 0.086(2) 0.0593(16) -0.0236(15) -0.0169(12) -0.0084(13) C37 0.0638(17) 0.082(2) 0.0344(12) -0.0260(13) -0.0041(11) -0.0288(15) Li1 0.0283(16) 0.0304(17) 0.0301(16) -0.0148(13) -0.0057(12) 0.0024(13) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ga1 N3 1.9855(14) . ? O1 C34 1.419(3) . ? O1 C37 1.437(3) . ? O1 Li1 1.909(3) . ? N1 N2 1.3045(18) . ? N1 C1 1.4232(19) . ? N1 Li1 2.052(3) . ? N2 N3 1.3010(18) . ? N3 C25 1.441(2) . ? C1 C2 1.407(2) . ? C1 C6 1.410(2) . ? C2 C3 1.396(2) . ? C2 C7 1.497(2) . ? C3 C4 1.383(3) . ? C4 C5 1.386(3) . ? C5 C6 1.394(2) . ? C6 C16 1.493(2) . ? C7 C8 1.405(2) . ? C7 C12 1.408(2) . ? C7 Li1 2.499(4) . ? C8 C9 1.395(2) . ? C8 C13 1.506(2) . ? C8 Li1 2.580(4) . ? C9 C10 1.387(3) . ? C10 C11 1.387(3) . ? C10 C14 1.511(2) . ? C11 C12 1.396(2) . ? C12 C15 1.511(3) . ? C16 C17 1.395(3) . ? C16 C21 1.406(2) . ? C17 C18 1.398(2) . ? C17 C22 1.511(3) . ? C18 C19 1.387(3) . ? C19 C20 1.384(3) . ? C19 C23 1.512(3) . ? C20 C21 1.398(2) . ? C21 C24 1.499(3) . ? C25 C30 1.391(3) . ? C25 C26 1.398(2) . ? C26 C27 1.401(2) . ? C26 C31 1.499(3) . ? C27 C28 1.374(3) . ? C28 C29 1.392(3) . ? C28 C32 1.516(3) . ? C29 C30 1.399(2) . ? C30 C33 1.508(2) . ? C34 C35 1.457(4) . ? C35 C36 1.466(4) . ? C36 C37 1.471(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 C34 O1 C37 108.93(18) . . ? C34 O1 Li1 120.78(18) . . ? C37 O1 Li1 122.01(18) . . ? N2 N1 C1 109.34(12) . . ? N2 N1 Li1 129.93(13) . . ? C1 N1 Li1 118.75(13) . . ? N3 N2 N1 115.29(13) . . ? N2 N3 C25 113.79(13) . . ? N2 N3 Ga1 126.32(10) . . ? C25 N3 Ga1 118.66(10) . . ? C2 C1 C6 119.91(14) . . ? C2 C1 N1 117.21(14) . . ? C6 C1 N1 122.85(14) . . ? C3 C2 C1 119.43(15) . . ? C3 C2 C7 118.80(14) . . ? C1 C2 C7 121.75(14) . . ? C4 C3 C2 120.84(16) . . ? C3 C4 C5 119.34(16) . . ? C4 C5 C6 121.76(16) . . ? C5 C6 C1 118.45(15) . . ? C5 C6 C16 117.68(15) . . ? C1 C6 C16 123.68(14) . . ? C8 C7 C12 119.70(15) . . ? C8 C7 C2 121.16(14) . . ? C12 C7 C2 119.12(15) . . ? C8 C7 Li1 77.16(12) . . ? C12 C7 Li1 93.20(13) . . ? C2 C7 Li1 101.13(12) . . ? C9 C8 C7 118.87(15) . . ? C9 C8 C13 119.29(15) . . ? C7 C8 C13 121.84(15) . . ? C9 C8 Li1 95.18(13) . . ? C7 C8 Li1 70.76(12) . . ? C13 C8 Li1 104.61(12) . . ? C10 C9 C8 122.36(16) . . ? C9 C10 C11 117.92(16) . . ? C9 C10 C14 120.60(17) . . ? C11 C10 C14 121.47(17) . . ? C10 C11 C12 121.97(16) . . ? C11 C12 C7 119.15(16) . . ? C11 C12 C15 119.48(16) . . ? C7 C12 C15 121.37(15) . . ? C17 C16 C21 120.06(15) . . ? C17 C16 C6 119.44(15) . . ? C21 C16 C6 120.34(16) . . ? C18 C17 C16 119.12(17) . . ? C18 C17 C22 119.37(17) . . ? C16 C17 C22 121.51(16) . . ? C19 C18 C17 121.64(18) . . ? C20 C19 C18 118.60(16) . . ? C20 C19 C23 121.08(18) . . ? C18 C19 C23 120.32(19) . . ? C19 C20 C21 121.56(17) . . ? C20 C21 C16 119.01(17) . . ? C20 C21 C24 119.95(16) . . ? C16 C21 C24 121.01(15) . . ? C30 C25 C26 121.39(15) . . ? C30 C25 N3 120.44(14) . . ? C26 C25 N3 117.90(15) . . ? C25 C26 C27 117.86(17) . . ? C25 C26 C31 121.28(16) . . ? C27 C26 C31 120.86(16) . . ? C28 C27 C26 122.22(16) . . ? C27 C28 C29 118.62(16) . . ? C27 C28 C32 121.22(18) . . ? C29 C28 C32 120.16(19) . . ? C28 C29 C30 121.33(18) . . ? C25 C30 C29 118.58(16) . . ? C25 C30 C33 121.32(15) . . ? C29 C30 C33 120.10(17) . . ? O1 C34 C35 108.1(2) . . ? C34 C35 C36 107.3(2) . . ? C37 C36 C35 105.5(2) . . ? O1 C37 C36 107.9(2) . . ? O1 Li1 N1 135.66(19) . . ? O1 Li1 C7 108.23(14) . . ? N1 Li1 C7 76.81(11) . . ? O1 Li1 C8 121.31(15) . . ? N1 Li1 C8 86.86(12) . . ? C7 Li1 C8 32.07(7) . . ? _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 30.06 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 0.609 _refine_diff_density_min -1.054 _refine_diff_density_rms 0.061 _chemical_compound_source THF #===END