# 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 'Norbert Mitzel' _publ_contact_author_email MITZEL@UNI-BIELEFELD.DE _publ_section_title ; Triamine ligand induced methane elimination from rare-earth metal tetramethylaluminates up to the carbide state ; loop_ _publ_author_name 'Norbert Mitzel' 'Raphael J F Berger' 'Daniel Bojer' 'Ina Kamps' 'Andreas Mix' 'Beate Neumann' ; H.-G.Stammler ; 'Ajay Venugopal' 'Alexander Willner' #===END data_compound_3_CCDC_679431 _database_code_depnum_ccdc_archive 'CCDC 679431' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H75 Al5 N3 Y3' _chemical_formula_weight 903.58 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Al Al 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Y Y -2.7962 3.5667 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P2(1)/m ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' '-x, -y, -z' 'x, -y-1/2, z' _cell_length_a 9.5402(18) _cell_length_b 17.210(2) _cell_length_c 14.068(2) _cell_angle_alpha 90.00 _cell_angle_beta 97.870(18) _cell_angle_gamma 90.00 _cell_volume 2288.1(6) _cell_formula_units_Z 2 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used 2000 _cell_measurement_theta_min 4.39 _cell_measurement_theta_max 26.98 _exptl_crystal_description Plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.6 _exptl_crystal_size_mid 0.5 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.312 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 940 _exptl_absorpt_coefficient_mu 3.891 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.2036 _exptl_absorpt_correction_T_max 0.6970 _exptl_absorpt_process_details ? _exptl_special_details ; Absorption correction was done with the program ABSCOR from the STOE IPDS-1 software pacage. ABSCOR is a modification of the well-known DIFABS. In contrary to DIFABS, ABSCOR loads and provides Fo^2^ values instead of Fo ones. ; _diffrn_ambient_temperature 153(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'STOE IPDS-1' _diffrn_measurement_method '\phi scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 35996 _diffrn_reflns_av_R_equivalents 0.1648 _diffrn_reflns_av_sigmaI/netI 0.0742 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 4.39 _diffrn_reflns_theta_max 26.98 _reflns_number_total 5097 _reflns_number_gt 3754 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'STOE IPDS-1 software package' _computing_cell_refinement 'STOE IPDS-1 software package' _computing_data_reduction 'STOE IPDS-1 software package' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The aromatic ring of the toluene molecule was constrained to the geomertry of an idealized hexagon (AFIX 66). ; _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^)+(0.0681P)^2^+5.6413P] 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 5097 _refine_ls_number_parameters 365 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0860 _refine_ls_R_factor_gt 0.0555 _refine_ls_wR_factor_ref 0.1398 _refine_ls_wR_factor_gt 0.1244 _refine_ls_goodness_of_fit_ref 1.006 _refine_ls_restrained_S_all 1.005 _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 Y1 Y 0.30779(7) 0.2500 0.19828(4) 0.01980(17) Uani 1 2 d S . . Y2 Y 0.54824(5) 0.35056(3) 0.36757(3) 0.02018(14) Uani 1 1 d . . . Al1 Al 0.23690(15) 0.33962(8) 0.38904(10) 0.0219(3) Uani 1 1 d . . . Al2 Al 0.60531(17) 0.45339(9) 0.19969(12) 0.0293(4) Uani 1 1 d . . . Al3 Al 0.4769(2) 0.2500 0.53109(14) 0.0232(4) Uani 1 2 d S . . N1 N 0.1721(5) 0.3180(3) 0.0380(3) 0.0322(10) Uani 1 1 d . . . N2 N 0.3739(6) 0.2500 0.0121(4) 0.0249(13) Uani 1 2 d S . . C1 C 0.0920(8) 0.3913(5) 0.0200(5) 0.0519(19) Uani 1 1 d . . . H1A H 0.062(8) 0.403(5) -0.048(6) 0.07(2) Uiso 1 1 d . . . H1B H 0.154(9) 0.445(5) 0.043(6) 0.07(2) Uiso 1 1 d . . . H1C H 0.005(8) 0.390(4) 0.051(5) 0.06(2) Uiso 1 1 d . . . C2 C 0.5081(9) 0.2500 -0.0284(7) 0.0356(19) Uani 1 2 d S . . H2A H 0.486(8) 0.2500 -0.099(6) 0.022(19) Uiso 1 2 d S . . H2B H 0.555(7) 0.208(3) -0.006(5) 0.043(18) Uiso 1 1 d . . . C3 C 0.0851(9) 0.2500 0.0100(6) 0.039(2) Uani 1 2 d S . . H3A H 0.051(8) 0.2500 -0.056(6) 0.03(2) Uiso 1 2 d S . . H3B H -0.001(7) 0.2500 0.055(5) 0.016(17) Uiso 1 2 d S . . C4 C 0.2921(6) 0.3192(4) -0.0173(4) 0.0323(12) Uani 1 1 d . . . H4A H 0.343(6) 0.370(3) 0.003(4) 0.034(16) Uiso 1 1 d . . . H4B H 0.256(6) 0.317(3) -0.088(4) 0.024(13) Uiso 1 1 d . . . C11 C 0.1078(7) 0.3543(5) 0.4856(5) 0.0395(14) Uani 1 1 d . . . H11A H 0.154(8) 0.358(4) 0.546(6) 0.06(2) Uiso 1 1 d . . . H11B H 0.057(15) 0.316(8) 0.500(10) 0.16(6) Uiso 1 1 d . . . H11C H 0.070(11) 0.404(7) 0.478(7) 0.11(3) Uiso 1 1 d . . . C12 C 0.1120(8) 0.3506(5) 0.2598(5) 0.0453(17) Uani 1 1 d . . . H12A H 0.163(11) 0.393(6) 0.207(8) 0.13(4) Uiso 1 1 d . . . H12B H 0.071(8) 0.315(5) 0.224(6) 0.06(2) Uiso 1 1 d . . . H12C H 0.058(10) 0.380(5) 0.279(6) 0.09(3) Uiso 1 1 d . . . C13 C 0.3466(7) 0.4437(3) 0.3946(5) 0.0335(13) Uani 1 1 d . . . H13A H 0.406(9) 0.460(5) 0.460(6) 0.08(3) Uiso 1 1 d . . . H13B H 0.264(7) 0.479(4) 0.406(5) 0.046(18) Uiso 1 1 d . . . H13C H 0.381(7) 0.468(4) 0.345(5) 0.05(2) Uiso 1 1 d . . . C21 C 0.7542(7) 0.4312(5) 0.1185(5) 0.0451(16) Uani 1 1 d . . . H21A H 0.710(7) 0.433(4) 0.051(5) 0.050(19) Uiso 1 1 d . . . H21B H 0.780(7) 0.378(4) 0.135(5) 0.05(2) Uiso 1 1 d . . . H21C H 0.831(9) 0.471(4) 0.132(5) 0.07(2) Uiso 1 1 d . . . C22 C 0.4997(9) 0.5520(4) 0.1709(7) 0.0544(19) Uani 1 1 d . . . H22A H 0.451(11) 0.550(6) 0.108(8) 0.11(4) Uiso 1 1 d . . . H22B H 0.555(16) 0.610(9) 0.182(10) 0.19(6) Uiso 1 1 d . . . H22C H 0.446(12) 0.565(6) 0.223(8) 0.11(4) Uiso 1 1 d . . . C23 C 0.7107(7) 0.4663(4) 0.3387(5) 0.0358(13) Uani 1 1 d . . . H23A H 0.666(8) 0.487(4) 0.400(6) 0.07(2) Uiso 1 1 d . . . H23B H 0.777(7) 0.435(4) 0.364(5) 0.044(19) Uiso 1 1 d . . . H23C H 0.754(8) 0.504(5) 0.317(5) 0.06(2) Uiso 1 1 d . . . C24 C 0.4708(6) 0.3603(3) 0.2008(4) 0.0241(11) Uani 1 1 d . . . H24A H 0.389(8) 0.387(4) 0.164(5) 0.06(2) Uiso 1 1 d . . . H24B H 0.500(8) 0.334(4) 0.159(5) 0.05(2) Uiso 1 1 d . . . C31 C 0.3807(12) 0.2500 0.6457(7) 0.052(3) Uani 1 2 d S . . H31A H 0.441(16) 0.2500 0.711(12) 0.14(6) Uiso 1 2 d SD . . H31B H 0.339(15) 0.208(4) 0.643(10) 0.19(7) Uiso 1 1 d D . . C32 C 0.6217(7) 0.3399(3) 0.5506(4) 0.0353(13) Uani 1 1 d . . . H32A H 0.644(7) 0.329(4) 0.610(5) 0.043(18) Uiso 1 1 d . . . H32B H 0.712(9) 0.340(4) 0.524(6) 0.07(3) Uiso 1 1 d . . . H32C H 0.591(8) 0.400(4) 0.546(5) 0.06(2) Uiso 1 1 d . . . C33 C 0.3764(7) 0.2500 0.3907(5) 0.0185(13) Uani 1 2 d S . . C40 C 0.7277(8) 0.2500 0.3376(6) 0.0297(16) Uani 1 2 d S . . H40A H 0.802(17) 0.2500 0.376(9) 0.14(6) Uiso 1 2 d SD . . H40B H 0.741(9) 0.294(3) 0.285(6) 0.09(3) Uiso 1 1 d D . . C71 C -0.0905(12) 0.1934(6) 0.7572(8) 0.050(4) Uani 0.50 1 d PG A -1 C72 C -0.1980(9) 0.2185(7) 0.8046(6) 0.051(5) Uani 0.50 1 d PG A -1 H72 H -0.2594 0.1819 0.8281 0.061 Uiso 0.50 1 calc PR A -1 C73 C -0.2168(7) 0.2961(8) 0.8182(5) 0.038(4) Uani 0.50 1 d PG A -1 H73 H -0.2914 0.3136 0.8512 0.045 Uiso 0.50 1 calc PR A -1 C74 C -0.1282(11) 0.3486(6) 0.7844(7) 0.053(4) Uani 0.50 1 d PG A -1 H74 H -0.1413 0.4026 0.7938 0.064 Uiso 0.50 1 calc PR A -1 C75 C -0.0208(9) 0.3235(7) 0.7369(6) 0.074(7) Uani 0.50 1 d PG A -1 H75 H 0.0406 0.3602 0.7137 0.088 Uiso 0.50 1 calc PR A -1 C76 C -0.0022(8) 0.2502(7) 0.7234(5) 0.084(7) Uani 1 2 d SG A -1 H76 H 0.0727 0.2341 0.6900 0.101 Uiso 0.50 1 calc PR A -1 C77 C -0.077(2) 0.1050(12) 0.7437(14) 0.086(7) Uani 0.50 1 d P A -1 H77A H 0.0028 0.0941 0.7090 0.129 Uiso 0.25 1 calc PR A -1 H77B H -0.1645 0.0850 0.7070 0.129 Uiso 0.25 1 calc PR A -1 H77C H -0.0616 0.0796 0.8067 0.129 Uiso 0.25 1 calc PR A -1 H77D H -0.1517 0.0784 0.7728 0.129 Uiso 0.25 1 calc PR A -1 H77E H 0.0156 0.0875 0.7748 0.129 Uiso 0.25 1 calc PR A -1 H77F H -0.0872 0.0928 0.6751 0.129 Uiso 0.25 1 calc PR A -1 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Y1 0.0135(3) 0.0285(3) 0.0171(3) 0.000 0.0010(2) 0.000 Y2 0.0178(2) 0.0208(2) 0.0211(2) -0.00015(18) -0.00036(17) -0.00228(18) Al1 0.0193(7) 0.0272(7) 0.0192(7) -0.0017(6) 0.0031(6) 0.0050(6) Al2 0.0264(9) 0.0310(8) 0.0313(9) 0.0078(7) 0.0070(7) -0.0002(7) Al3 0.0258(11) 0.0258(10) 0.0168(10) 0.000 -0.0018(8) 0.000 N1 0.022(2) 0.051(3) 0.024(2) 0.003(2) 0.0062(18) 0.009(2) N2 0.018(3) 0.034(3) 0.025(3) 0.000 0.011(2) 0.000 C1 0.049(4) 0.077(5) 0.031(3) 0.017(3) 0.009(3) 0.033(4) C2 0.028(4) 0.051(5) 0.033(5) 0.000 0.020(4) 0.000 C3 0.024(4) 0.074(6) 0.019(4) 0.000 -0.001(3) 0.000 C4 0.033(3) 0.046(3) 0.020(3) 0.006(2) 0.009(2) 0.009(3) C11 0.036(3) 0.048(4) 0.037(4) -0.003(3) 0.016(3) 0.005(3) C12 0.040(4) 0.064(4) 0.029(3) -0.010(3) -0.006(3) 0.030(4) C13 0.044(4) 0.025(3) 0.034(3) 0.002(2) 0.014(3) 0.004(2) C21 0.031(3) 0.062(4) 0.044(4) 0.005(3) 0.011(3) -0.006(3) C22 0.065(5) 0.036(4) 0.062(5) 0.020(3) 0.010(4) 0.015(3) C23 0.034(3) 0.034(3) 0.038(3) 0.007(3) 0.000(3) -0.009(3) C24 0.023(3) 0.027(3) 0.022(3) 0.000(2) 0.003(2) -0.001(2) C31 0.045(6) 0.086(8) 0.025(5) 0.000 0.006(4) 0.000 C32 0.044(4) 0.032(3) 0.026(3) 0.004(2) -0.009(3) -0.006(3) C33 0.021(3) 0.020(3) 0.015(3) 0.000 0.005(3) 0.000 C40 0.020(4) 0.033(4) 0.036(4) 0.000 0.002(3) 0.000 C71 0.019(7) 0.103(13) 0.029(7) -0.013(8) 0.003(6) 0.004(8) C72 0.022(7) 0.082(13) 0.046(9) -0.013(8) -0.001(7) -0.015(7) C73 0.010(6) 0.073(11) 0.030(7) 0.003(7) 0.002(5) -0.026(6) C74 0.055(10) 0.072(11) 0.028(7) 0.012(7) -0.010(7) -0.005(8) C75 0.024(8) 0.17(2) 0.024(7) -0.003(11) 0.007(6) -0.032(11) C76 0.051(9) 0.178(17) 0.025(5) -0.013(19) 0.010(6) 0.077(18) C77 0.079(13) 0.102(15) 0.065(11) -0.040(11) -0.033(10) 0.025(12) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Y1 C24 2.452(5) . ? Y1 C24 2.452(5) 4_565 ? Y1 C33 2.696(6) . ? Y1 N1 2.708(4) . ? Y1 N1 2.708(4) 4_565 ? Y1 C12 2.772(7) 4_565 ? Y1 C12 2.772(7) . ? Y1 N2 2.777(6) . ? Y1 Al1 3.2458(15) . ? Y1 Al1 3.2458(15) 4_565 ? Y1 Y2 3.5261(9) . ? Y1 Y2 3.5262(9) 4_565 ? Y1 H12B 2.59(7) . ? Y1 H24A 2.55(7) . ? Y1 H24B 2.46(7) . ? Y2 C24 2.367(5) . ? Y2 C33 2.436(5) . ? Y2 C40 2.511(6) . ? Y2 C13 2.572(6) . ? Y2 C32 2.581(6) . ? Y2 C23 2.590(6) . ? Y2 Al3 3.0298(18) . ? Y2 Al1 3.0322(16) . ? Y2 Al2 3.0592(16) . ? Y2 Y2 3.4614(10) 4_565 ? Y2 H13C 2.56(7) . ? Y2 H32B 2.53(8) . ? Y2 H40B 2.49(8) . ? Al1 C11 1.971(6) . ? Al1 C33 2.035(5) . ? Al1 C12 2.042(6) . ? Al1 C13 2.072(6) . ? Al2 C21 1.978(7) . ? Al2 C22 1.987(7) . ? Al2 C24 2.053(5) . ? Al2 C23 2.085(7) . ? Al3 C31 1.961(10) . ? Al3 C32 2.067(6) . ? Al3 C32 2.067(6) 4_565 ? Al3 C33 2.074(7) . ? Al3 Y2 3.0297(18) 4_565 ? N1 C3 1.456(7) . ? N1 C4 1.469(7) . ? N1 C1 1.478(8) . ? N2 C4 1.453(6) 4_565 ? N2 C4 1.453(6) . ? N2 C2 1.470(9) . ? C1 H1A 0.98(8) . ? C1 H1B 1.13(8) . ? C1 H1C 0.99(8) . ? C2 H2A 0.99(8) . ? C2 H2B 0.88(6) . ? C3 N1 1.457(7) 4_565 ? C3 H3A 0.94(8) . ? C3 H3B 1.10(7) . ? C4 H4A 1.02(6) . ? C4 H4B 1.01(5) . ? C11 H11A 0.90(8) . ? C11 H11B 0.86(14) . ? C11 H11C 0.93(11) . ? C12 H12A 1.18(12) . ? C12 H12B 0.85(8) . ? C12 H12C 0.80(10) . ? C13 H13A 1.05(9) . ? C13 H13B 1.03(7) . ? C13 H13C 0.91(7) . ? C21 H21A 0.98(7) . ? C21 H21B 0.97(7) . ? C21 H21C 1.00(8) . ? C22 H22A 0.94(11) . ? C22 H22B 1.13(15) . ? C22 H22C 0.97(11) . ? C23 H23A 1.07(8) . ? C23 H23B 0.87(7) . ? C23 H23C 0.85(8) . ? C24 H24A 0.99(8) . ? C24 H24B 0.82(7) . ? C31 H31A 1.01(16) . ? C31 H31B 0.83(11) . ? C32 H32A 0.85(7) . ? C32 H32B 0.99(9) . ? C32 H32C 1.08(8) . ? C33 Al1 2.035(5) 4_565 ? C33 Y2 2.436(5) 4_565 ? C40 Y2 2.511(6) 4_565 ? C40 H40A 0.82(13) . ? C40 H40B 1.08(8) . ? C71 C72 1.3673 . ? C71 C76 1.4152 . ? C71 C77 1.54(2) . ? C72 C73 1.3645 . ? C72 H72 0.9500 . ? C73 C74 1.3665 . ? C73 H73 0.9500 . ? C74 C75 1.3674 . ? C74 H74 0.9500 . ? C75 C76 1.2903 . ? C75 H75 0.9500 . ? C76 H76 0.9500 . ? C77 H77A 0.9800 . ? C77 H77B 0.9800 . ? C77 H77C 0.9800 . ? C77 H77D 0.9800 . ? C77 H77E 0.9800 . ? C77 H77F 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C24 Y1 C24 101.5(3) . 4_565 ? C24 Y1 C33 85.37(15) . . ? C24 Y1 C33 85.37(15) 4_565 . ? C24 Y1 N1 84.69(16) . . ? C24 Y1 N1 125.21(15) 4_565 . ? C33 Y1 N1 149.19(12) . . ? C24 Y1 N1 125.21(15) . 4_565 ? C24 Y1 N1 84.69(16) 4_565 4_565 ? C33 Y1 N1 149.19(12) . 4_565 ? N1 Y1 N1 51.2(2) . 4_565 ? C24 Y1 C12 158.9(2) . 4_565 ? C24 Y1 C12 88.0(2) 4_565 4_565 ? C33 Y1 C12 76.58(17) . 4_565 ? N1 Y1 C12 105.32(18) . 4_565 ? N1 Y1 C12 73.99(16) 4_565 4_565 ? C24 Y1 C12 88.0(2) . . ? C24 Y1 C12 158.9(2) 4_565 . ? C33 Y1 C12 76.58(17) . . ? N1 Y1 C12 73.99(16) . . ? N1 Y1 C12 105.32(18) 4_565 . ? C12 Y1 C12 77.4(4) 4_565 . ? C24 Y1 N2 77.75(14) . . ? C24 Y1 N2 77.75(14) 4_565 . ? C33 Y1 N2 153.07(19) . . ? N1 Y1 N2 50.13(13) . . ? N1 Y1 N2 50.12(13) 4_565 . ? C12 Y1 N2 122.98(17) 4_565 . ? C12 Y1 N2 122.98(17) . . ? C24 Y1 Al1 79.85(13) . . ? C24 Y1 Al1 124.04(12) 4_565 . ? C33 Y1 Al1 38.68(10) . . ? N1 Y1 Al1 110.69(10) . . ? N1 Y1 Al1 139.82(10) 4_565 . ? C12 Y1 Al1 79.23(17) 4_565 . ? C12 Y1 Al1 38.67(13) . . ? N2 Y1 Al1 151.62(3) . . ? C24 Y1 Al1 124.04(12) . 4_565 ? C24 Y1 Al1 79.85(13) 4_565 4_565 ? C33 Y1 Al1 38.68(10) . 4_565 ? N1 Y1 Al1 139.81(10) . 4_565 ? N1 Y1 Al1 110.69(10) 4_565 4_565 ? C12 Y1 Al1 38.67(13) 4_565 4_565 ? C12 Y1 Al1 79.23(17) . 4_565 ? N2 Y1 Al1 151.62(3) . 4_565 ? Al1 Y1 Al1 56.74(5) . 4_565 ? C24 Y1 Y2 42.05(12) . . ? C24 Y1 Y2 91.01(12) 4_565 . ? C33 Y1 Y2 43.60(10) . . ? N1 Y1 Y2 122.90(11) . . ? N1 Y1 Y2 165.31(9) 4_565 . ? C12 Y1 Y2 119.99(13) 4_565 . ? C12 Y1 Y2 83.48(16) . . ? N2 Y1 Y2 115.23(10) . . ? Al1 Y1 Y2 53.00(3) . . ? Al1 Y1 Y2 82.22(3) 4_565 . ? C24 Y1 Y2 91.01(12) . 4_565 ? C24 Y1 Y2 42.05(12) 4_565 4_565 ? C33 Y1 Y2 43.60(10) . 4_565 ? N1 Y1 Y2 165.31(9) . 4_565 ? N1 Y1 Y2 122.90(11) 4_565 4_565 ? C12 Y1 Y2 83.47(16) 4_565 4_565 ? C12 Y1 Y2 119.99(13) . 4_565 ? N2 Y1 Y2 115.23(10) . 4_565 ? Al1 Y1 Y2 82.22(3) . 4_565 ? Al1 Y1 Y2 53.00(3) 4_565 4_565 ? Y2 Y1 Y2 58.79(2) . 4_565 ? C24 Y1 H12B 103.1(18) . . ? C24 Y1 H12B 153.7(17) 4_565 . ? C33 Y1 H12B 87.5(17) . . ? N1 Y1 H12B 66.6(17) . . ? N1 Y1 H12B 88.6(18) 4_565 . ? C12 Y1 H12B 65.7(17) 4_565 . ? C12 Y1 H12B 17.9(18) . . ? N2 Y1 H12B 116.5(17) . . ? Al1 Y1 H12B 52.8(18) . . ? Al1 Y1 H12B 78.8(16) 4_565 . ? Y2 Y1 H12B 101.1(18) . . ? Y2 Y1 H12B 128.1(16) 4_565 . ? C24 Y1 H24A 22.7(17) . . ? C24 Y1 H24A 120.6(17) 4_565 . ? C33 Y1 H24A 98.8(16) . . ? N1 Y1 H24A 64.2(17) . . ? N1 Y1 H24A 111.4(16) 4_565 . ? C12 Y1 H24A 150.9(17) 4_565 . ? C12 Y1 H24A 73.6(17) . . ? N2 Y1 H24A 72.9(16) . . ? Al1 Y1 H24A 79.7(16) . . ? Al1 Y1 H24A 134.5(16) 4_565 . ? Y2 Y1 H24A 59.2(17) . . ? Y2 Y1 H24A 113.3(17) 4_565 . ? H12B Y1 H24A 86(2) . . ? C24 Y1 H24B 19.3(17) . . ? C24 Y1 H24B 88.1(18) 4_565 . ? C33 Y1 H24B 98.1(17) . . ? N1 Y1 H24B 81.1(17) . . ? N1 Y1 H24B 110.6(17) 4_565 . ? C12 Y1 H24B 173.6(17) 4_565 . ? C12 Y1 H24B 105.0(17) . . ? N2 Y1 H24B 60.9(17) . . ? Al1 Y1 H24B 98.9(17) . . ? Al1 Y1 H24B 135.4(17) 4_565 . ? Y2 Y1 H24B 55.1(17) . . ? Y2 Y1 H24B 90.2(17) 4_565 . ? H12B Y1 H24B 118(2) . . ? H24A Y1 H24B 33(2) . . ? C24 Y2 C33 93.3(2) . . ? C24 Y2 C40 90.5(2) . . ? C33 Y2 C40 91.12(17) . . ? C24 Y2 C13 88.0(2) . . ? C33 Y2 C13 83.84(18) . . ? C40 Y2 C13 174.65(19) . . ? C24 Y2 C32 177.6(2) . . ? C33 Y2 C32 85.0(2) . . ? C40 Y2 C32 91.2(3) . . ? C13 Y2 C32 90.2(2) . . ? C24 Y2 C23 84.38(19) . . ? C33 Y2 C23 174.5(2) . . ? C40 Y2 C23 93.9(2) . . ? C13 Y2 C23 91.1(2) . . ? C32 Y2 C23 97.2(2) . . ? C24 Y2 Al3 136.14(13) . . ? C33 Y2 Al3 42.91(15) . . ? C40 Y2 Al3 87.89(17) . . ? C13 Y2 Al3 89.62(14) . . ? C32 Y2 Al3 42.31(14) . . ? C23 Y2 Al3 139.46(15) . . ? C24 Y2 Al1 85.77(13) . . ? C33 Y2 Al1 41.95(12) . . ? C40 Y2 Al1 132.36(13) . . ? C13 Y2 Al1 42.40(14) . . ? C32 Y2 Al1 91.84(16) . . ? C23 Y2 Al1 132.74(16) . . ? Al3 Y2 Al1 64.15(5) . . ? C24 Y2 Al2 42.10(13) . . ? C33 Y2 Al2 135.08(16) . . ? C40 Y2 Al2 94.09(17) . . ? C13 Y2 Al2 88.25(14) . . ? C32 Y2 Al2 139.34(14) . . ? C23 Y2 Al2 42.30(15) . . ? Al3 Y2 Al2 177.29(5) . . ? Al1 Y2 Al2 113.15(5) . . ? C24 Y2 Y2 94.07(13) . 4_565 ? C33 Y2 Y2 44.73(11) . 4_565 ? C40 Y2 Y2 46.42(13) . 4_565 ? C13 Y2 Y2 128.57(14) . 4_565 ? C32 Y2 Y2 85.93(13) . 4_565 ? C23 Y2 Y2 140.29(16) . 4_565 ? Al3 Y2 Y2 55.16(2) . 4_565 ? Al1 Y2 Y2 86.44(3) . 4_565 ? Al2 Y2 Y2 125.34(3) . 4_565 ? C24 Y2 Y1 43.92(12) . . ? C33 Y2 Y1 49.76(15) . . ? C40 Y2 Y1 86.77(17) . . ? C13 Y2 Y1 88.60(15) . . ? C32 Y2 Y1 134.56(14) . . ? C23 Y2 Y1 128.28(14) . . ? Al3 Y2 Y1 92.26(4) . . ? Al1 Y2 Y1 58.75(3) . . ? Al2 Y2 Y1 86.02(4) . . ? Y2 Y2 Y1 60.606(11) 4_565 . ? C24 Y2 H13C 73.4(16) . . ? C33 Y2 H13C 99.0(16) . . ? C40 Y2 H13C 161.4(17) . . ? C13 Y2 H13C 20.5(16) . . ? C32 Y2 H13C 105.1(16) . . ? C23 Y2 H13C 75.6(16) . . ? Al3 Y2 H13C 110.1(17) . . ? Al1 Y2 H13C 57.3(16) . . ? Al2 Y2 H13C 67.7(17) . . ? Y2 Y2 H13C 141.8(16) 4_565 . ? Y1 Y2 H13C 88.0(16) . . ? C24 Y2 H32B 160(2) . . ? C33 Y2 H32B 100.3(19) . . ? C40 Y2 H32B 74.9(19) . . ? C13 Y2 H32B 107.7(19) . . ? C32 Y2 H32B 22.2(19) . . ? C23 Y2 H32B 83.2(19) . . ? Al3 Y2 H32B 58.2(19) . . ? Al1 Y2 H32B 114(2) . . ? Al2 Y2 H32B 124.2(19) . . ? Y2 Y2 H32B 85.7(17) 4_565 . ? Y1 Y2 H32B 145.0(18) . . ? H13C Y2 H32B 118(2) . . ? C24 Y2 H40B 74(2) . . ? C33 Y2 H40B 109.7(14) . . ? C40 Y2 H40B 24.9(17) . . ? C13 Y2 H40B 157.4(19) . . ? C32 Y2 H40B 109(2) . . ? C23 Y2 H40B 74.4(14) . . ? Al3 Y2 H40B 112.7(18) . . ? Al1 Y2 H40B 144.6(16) . . ? Al2 Y2 H40B 69.3(18) . . ? Y2 Y2 H40B 67.2(14) 4_565 . ? Y1 Y2 H40B 87.0(18) . . ? H13C Y2 H40B 137(3) . . ? H32B Y2 H40B 88(3) . . ? C11 Al1 C33 124.0(3) . . ? C11 Al1 C12 105.0(3) . . ? C33 Al1 C12 112.4(3) . . ? C11 Al1 C13 102.9(3) . . ? C33 Al1 C13 109.2(2) . . ? C12 Al1 C13 100.6(3) . . ? C11 Al1 Y2 140.7(2) . . ? C33 Al1 Y2 53.15(15) . . ? C12 Al1 Y2 111.5(2) . . ? C13 Al1 Y2 56.85(18) . . ? C11 Al1 Y1 148.4(2) . . ? C33 Al1 Y1 55.90(18) . . ? C12 Al1 Y1 58.01(19) . . ? C13 Al1 Y1 106.33(18) . . ? Y2 Al1 Y1 68.24(3) . . ? C21 Al2 C22 115.6(4) . . ? C21 Al2 C24 110.7(3) . . ? C22 Al2 C24 111.6(3) . . ? C21 Al2 C23 105.7(3) . . ? C22 Al2 C23 105.4(4) . . ? C24 Al2 C23 107.3(2) . . ? C21 Al2 Y2 123.5(2) . . ? C22 Al2 Y2 120.8(3) . . ? C24 Al2 Y2 50.62(15) . . ? C23 Al2 Y2 56.73(18) . . ? C31 Al3 C32 105.7(3) . . ? C31 Al3 C32 105.7(3) . 4_565 ? C32 Al3 C32 96.9(4) . 4_565 ? C31 Al3 C33 125.1(4) . . ? C32 Al3 C33 109.9(2) . . ? C32 Al3 C33 109.9(2) 4_565 . ? C31 Al3 Y2 143.44(10) . 4_565 ? C32 Al3 Y2 108.2(2) . 4_565 ? C32 Al3 Y2 57.17(18) 4_565 4_565 ? C33 Al3 Y2 53.10(13) . 4_565 ? C31 Al3 Y2 143.44(10) . . ? C32 Al3 Y2 57.17(18) . . ? C32 Al3 Y2 108.2(2) 4_565 . ? C33 Al3 Y2 53.10(13) . . ? Y2 Al3 Y2 69.67(5) 4_565 . ? C3 N1 C4 109.0(5) . . ? C3 N1 C1 112.2(5) . . ? C4 N1 C1 108.6(5) . . ? C3 N1 Y1 93.9(4) . . ? C4 N1 Y1 97.4(3) . . ? C1 N1 Y1 133.5(4) . . ? C4 N2 C4 110.1(6) 4_565 . ? C4 N2 C2 110.6(4) 4_565 . ? C4 N2 C2 110.6(4) . . ? C4 N2 Y1 94.9(3) 4_565 . ? C4 N2 Y1 94.9(3) . . ? C2 N2 Y1 133.5(5) . . ? N1 C1 H1A 115(5) . . ? N1 C1 H1B 115(4) . . ? H1A C1 H1B 101(6) . . ? N1 C1 H1C 110(4) . . ? H1A C1 H1C 106(6) . . ? H1B C1 H1C 109(6) . . ? N2 C2 H2A 108(4) . . ? N2 C2 H2B 107(4) . . ? H2A C2 H2B 112(5) . . ? N1 C3 N1 106.9(6) . 4_565 ? N1 C3 H3A 112(2) . . ? N1 C3 H3A 112(2) 4_565 . ? N1 C3 H3B 107(2) . . ? N1 C3 H3B 107(2) 4_565 . ? H3A C3 H3B 112(6) . . ? N2 C4 N1 105.4(4) . . ? N2 C4 H4A 114(3) . . ? N1 C4 H4A 104(3) . . ? N2 C4 H4B 110(3) . . ? N1 C4 H4B 110(3) . . ? H4A C4 H4B 113(4) . . ? Al1 C11 H11A 113(5) . . ? Al1 C11 H11B 120(9) . . ? H11A C11 H11B 93(9) . . ? Al1 C11 H11C 108(6) . . ? H11A C11 H11C 99(7) . . ? H11B C11 H11C 121(10) . . ? Al1 C12 Y1 83.3(2) . . ? Al1 C12 H12A 112(5) . . ? Y1 C12 H12A 81(5) . . ? Al1 C12 H12B 129(5) . . ? Y1 C12 H12B 69(5) . . ? H12A C12 H12B 105(7) . . ? Al1 C12 H12C 94(7) . . ? Y1 C12 H12C 178(7) . . ? H12A C12 H12C 99(8) . . ? H12B C12 H12C 113(8) . . ? Al1 C13 Y2 80.75(18) . . ? Al1 C13 H13A 119(5) . . ? Y2 C13 H13A 89(5) . . ? Al1 C13 H13B 97(4) . . ? Y2 C13 H13B 177(4) . . ? H13A C13 H13B 92(6) . . ? Al1 C13 H13C 126(4) . . ? Y2 C13 H13C 79(4) . . ? H13A C13 H13C 110(6) . . ? H13B C13 H13C 103(5) . . ? Al2 C21 H21A 108(4) . . ? Al2 C21 H21B 103(4) . . ? H21A C21 H21B 108(6) . . ? Al2 C21 H21C 109(4) . . ? H21A C21 H21C 111(6) . . ? H21B C21 H21C 117(6) . . ? Al2 C22 H22A 110(6) . . ? Al2 C22 H22B 121(7) . . ? H22A C22 H22B 109(10) . . ? Al2 C22 H22C 110(6) . . ? H22A C22 H22C 118(9) . . ? H22B C22 H22C 89(8) . . ? Al2 C23 Y2 81.0(2) . . ? Al2 C23 H23A 126(4) . . ? Y2 C23 H23A 79(4) . . ? Al2 C23 H23B 124(4) . . ? Y2 C23 H23B 83(4) . . ? H23A C23 H23B 103(6) . . ? Al2 C23 H23C 86(5) . . ? Y2 C23 H23C 167(5) . . ? H23A C23 H23C 108(6) . . ? H23B C23 H23C 105(7) . . ? Al2 C24 Y2 87.27(19) . . ? Al2 C24 Y1 178.7(3) . . ? Y2 C24 Y1 94.04(17) . . ? Al2 C24 H24A 95(4) . . ? Y2 C24 H24A 132(4) . . ? Y1 C24 H24A 84(4) . . ? Al2 C24 H24B 99(5) . . ? Y2 C24 H24B 126(5) . . ? Y1 C24 H24B 81(5) . . ? H24A C24 H24B 101(6) . . ? Al3 C31 H31A 118(9) . . ? Al3 C31 H31B 104(10) . . ? H31A C31 H31B 104(10) . . ? Al3 C32 Y2 80.53(19) . . ? Al3 C32 H32A 92(5) . . ? Y2 C32 H32A 171(5) . . ? Al3 C32 H32B 123(5) . . ? Y2 C32 H32B 76(5) . . ? H32A C32 H32B 105(6) . . ? Al3 C32 H32C 123(4) . . ? Y2 C32 H32C 80(4) . . ? H32A C32 H32C 108(6) . . ? H32B C32 H32C 103(6) . . ? Al1 C33 Al1 98.5(3) . 4_565 ? Al1 C33 Al3 103.1(2) . . ? Al1 C33 Al3 103.1(2) 4_565 . ? Al1 C33 Y2 171.1(3) . 4_565 ? Al1 C33 Y2 84.90(6) 4_565 4_565 ? Al3 C33 Y2 84.0(2) . 4_565 ? Al1 C33 Y2 84.90(6) . . ? Al1 C33 Y2 171.1(3) 4_565 . ? Al3 C33 Y2 84.0(2) . . ? Y2 C33 Y2 90.5(2) 4_565 . ? Al1 C33 Y1 85.4(2) . . ? Al1 C33 Y1 85.4(2) 4_565 . ? Al3 C33 Y1 166.7(3) . . ? Y2 C33 Y1 86.64(17) 4_565 . ? Y2 C33 Y1 86.64(17) . . ? Y2 C40 Y2 87.2(2) 4_565 . ? Y2 C40 H40A 116(7) 4_565 . ? Y2 C40 H40A 116(7) . . ? Y2 C40 H40B 138(5) 4_565 . ? Y2 C40 H40B 77(4) . . ? H40A C40 H40B 106(8) . . ? C72 C71 C76 117.8 . . ? C72 C71 C77 116.9(13) . . ? C76 C71 C77 125.4(13) . . ? C73 C72 C71 120.0 . . ? C73 C72 H72 120.0 . . ? C71 C72 H72 120.0 . . ? C72 C73 C74 119.9 . . ? C72 C73 H73 120.0 . . ? C74 C73 H73 120.0 . . ? C73 C74 C75 120.1 . . ? C73 C74 H74 119.9 . . ? C75 C74 H74 119.9 . . ? C76 C75 C74 120.5 . . ? C76 C75 H75 119.7 . . ? C74 C75 H75 119.7 . . ? C75 C76 C71 121.7 . . ? C75 C76 H76 119.1 . . ? C71 C76 H76 119.1 . . ? C71 C77 H77A 109.5 . . ? C71 C77 H77B 109.5 . . ? H77A C77 H77B 109.5 . . ? C71 C77 H77C 109.5 . . ? H77A C77 H77C 109.5 . . ? H77B C77 H77C 109.5 . . ? C71 C77 H77D 109.5 . . ? H77A C77 H77D 141.1 . . ? H77B C77 H77D 56.3 . . ? H77C C77 H77D 56.3 . . ? C71 C77 H77E 109.5 . . ? H77A C77 H77E 56.3 . . ? H77B C77 H77E 141.1 . . ? H77C C77 H77E 56.3 . . ? H77D C77 H77E 109.5 . . ? C71 C77 H77F 109.5 . . ? H77A C77 H77F 56.3 . . ? H77B C77 H77F 56.3 . . ? H77C C77 H77F 141.1 . . ? H77D C77 H77F 109.5 . . ? H77E C77 H77F 109.5 . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 26.98 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 0.915 _refine_diff_density_min -1.505 _refine_diff_density_rms 0.124 #===END data_compound_2_CCDC_679432 _database_code_depnum_ccdc_archive 'CCDC 679432' _audit_creation_method SHELXL-97 _chemical_name_systematic ; 1,3,5-Trimethyl-1,3,5-triazacyclohexane - Bis(trimethylaluminium)-Adduct ; _chemical_name_common ;1,3,5-Trimethyl-1,3,5-triazacyclohexane - Bis(trimethylaluminium)-Adduct ; _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C19 H41 Al2 N3' _chemical_formula_weight 365.51 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 Monoclinic _symmetry_space_group_name_H-M P2(1)/c 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 10.6826(15) _cell_length_b 29.104(4) _cell_length_c 7.8399(11) _cell_angle_alpha 90.00 _cell_angle_beta 96.978(15) _cell_angle_gamma 90.00 _cell_volume 2419.5(6) _cell_formula_units_Z 4 _cell_measurement_temperature 163(2) _cell_measurement_reflns_used 5000 _cell_measurement_theta_min 4.60 _cell_measurement_theta_max 26.93 _exptl_crystal_description Block _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.003 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 808 _exptl_absorpt_coefficient_mu 0.126 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 163(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'STOE IPDS-1' _diffrn_measurement_method '\phi scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 32699 _diffrn_reflns_av_R_equivalents 0.1258 _diffrn_reflns_av_sigmaI/netI 0.0685 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -37 _diffrn_reflns_limit_k_max 36 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 4.60 _diffrn_reflns_theta_max 26.93 _reflns_number_total 4985 _reflns_number_gt 3367 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'STOE IPDS-1 software package' _computing_cell_refinement 'STOE IPDS-1 software package' _computing_data_reduction 'STOE IPDS-1 software package' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0430P)^2^+0.8252P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment refall _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4985 _refine_ls_number_parameters 297 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0906 _refine_ls_R_factor_gt 0.0492 _refine_ls_wR_factor_ref 0.1140 _refine_ls_wR_factor_gt 0.0997 _refine_ls_goodness_of_fit_ref 1.021 _refine_ls_restrained_S_all 1.021 _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 0.24094(6) 0.01710(2) 0.71682(9) 0.03174(18) Uani 1 1 d . . . Al2 Al 0.44571(5) -0.15948(2) 0.63759(8) 0.02819(17) Uani 1 1 d . . . N1 N 0.22393(13) -0.04940(5) 0.8146(2) 0.0219(3) Uani 1 1 d . . . N2 N 0.31449(13) -0.12847(5) 0.7781(2) 0.0211(3) Uani 1 1 d . . . N3 N 0.09116(13) -0.11664(5) 0.7797(2) 0.0245(4) Uani 1 1 d . . . C1 C 0.32657(16) -0.07816(6) 0.7603(3) 0.0220(4) Uani 1 1 d . . . H1A H 0.3336 -0.0713 0.6381 0.026 Uiso 1 1 calc R . . H1B H 0.4067 -0.0686 0.8276 0.026 Uiso 1 1 calc R . . C2 C 0.18632(16) -0.14253(6) 0.7029(3) 0.0246(4) Uani 1 1 d . . . H2A H 0.1764 -0.1372 0.5773 0.030 Uiso 1 1 calc R . . H2B H 0.1747 -0.1758 0.7228 0.030 Uiso 1 1 calc R . . C3 C 0.10125(16) -0.06859(6) 0.7365(3) 0.0254(4) Uani 1 1 d . . . H3A H 0.0314 -0.0513 0.7787 0.031 Uiso 1 1 calc R . . H3B H 0.0938 -0.0651 0.6101 0.031 Uiso 1 1 calc R . . C4 C 0.22643(18) -0.04538(7) 1.0043(3) 0.0306(5) Uani 1 1 d . . . H4A H 0.1901(12) -0.0729(4) 1.0486(7) 0.046 Uiso 1 1 calc R . . H4B H 0.1778(12) -0.0187(4) 1.0310(5) 0.046 Uiso 1 1 calc R . . H4C H 0.3130(11) -0.0420(5) 1.0570(8) 0.046 Uiso 1 1 calc R . . C5 C 0.34114(19) -0.14511(7) 0.9586(3) 0.0291(5) Uani 1 1 d . . . H5A H 0.2693(10) -0.1393(4) 1.0181(9) 0.044 Uiso 1 1 calc R . . H5B H 0.4132(12) -0.1292(4) 1.0153(9) 0.044 Uiso 1 1 calc R . . H5C H 0.3581(12) -0.1775(4) 0.9585(3) 0.044 Uiso 1 1 calc R . . C6 C -0.03529(18) -0.13405(7) 0.7209(3) 0.0364(5) Uani 1 1 d . . . H6A H -0.0968(9) -0.1169(4) 0.7752(16) 0.055 Uiso 1 1 calc R . . H6B H -0.0402(5) -0.1661(4) 0.7509(18) 0.055 Uiso 1 1 calc R . . H6C H -0.0522(6) -0.1307(5) 0.5979(17) 0.055 Uiso 1 1 calc R . . C11 C 0.0773(3) 0.04383(10) 0.7523(6) 0.0592(9) Uani 1 1 d . . . H11A H 0.067(3) 0.0739(11) 0.705(4) 0.068(9) Uiso 1 1 d . . . H11B H 0.074(3) 0.0460(11) 0.871(5) 0.075(12) Uiso 1 1 d . . . H11C H 0.004(4) 0.0267(13) 0.712(5) 0.112(13) Uiso 1 1 d . . . C12 C 0.2675(3) 0.00878(12) 0.4754(4) 0.0565(8) Uani 1 1 d . . . H12A H 0.255(3) 0.0351(13) 0.419(4) 0.085(11) Uiso 1 1 d . . . H12B H 0.351(4) -0.0014(12) 0.462(4) 0.093(12) Uiso 1 1 d . . . H12C H 0.221(4) -0.0134(14) 0.424(5) 0.101(13) Uiso 1 1 d . . . C13 C 0.3874(3) 0.04223(10) 0.8614(4) 0.0496(7) Uani 1 1 d . . . H13A H 0.462(3) 0.0249(10) 0.854(4) 0.070(9) Uiso 1 1 d . . . H13C H 0.400(3) 0.0717(12) 0.828(4) 0.076(9) Uiso 1 1 d . . . H13B H 0.383(3) 0.0419(12) 0.980(5) 0.087(12) Uiso 1 1 d . . . C21 C 0.6086(2) -0.14454(12) 0.7710(4) 0.0511(7) Uani 1 1 d . . . H21A H 0.622(3) -0.1125(11) 0.787(4) 0.066(9) Uiso 1 1 d . . . H21B H 0.625(3) -0.1608(11) 0.883(5) 0.083(11) Uiso 1 1 d . . . H21C H 0.668(3) -0.1569(12) 0.725(5) 0.090(12) Uiso 1 1 d . . . C22 C 0.4135(3) -0.12943(11) 0.4126(4) 0.0466(6) Uani 1 1 d . . . H22A H 0.329(3) -0.1235(10) 0.370(4) 0.069(9) Uiso 1 1 d . . . H22B H 0.443(3) -0.1481(11) 0.334(4) 0.074(10) Uiso 1 1 d . . . H22C H 0.451(3) -0.1006(12) 0.403(4) 0.080(10) Uiso 1 1 d . . . C23 C 0.3971(3) -0.22449(8) 0.6358(4) 0.0420(6) Uani 1 1 d . . . H23A H 0.317(3) -0.2310(10) 0.589(4) 0.067(9) Uiso 1 1 d . . . H23B H 0.454(3) -0.2412(10) 0.579(4) 0.071(9) Uiso 1 1 d . . . H23C H 0.403(3) -0.2374(11) 0.743(5) 0.080(11) Uiso 1 1 d . . . C30 C 0.8383(2) -0.20313(8) 0.3006(3) 0.0422(6) Uani 1 1 d . . . C31 C 0.8863(2) -0.17021(8) 0.1976(3) 0.0416(6) Uani 1 1 d . . . H31A H 0.8307 -0.1488 0.1364 0.050 Uiso 1 1 calc R . . C32 C 1.0131(2) -0.16840(7) 0.1833(3) 0.0394(6) Uani 1 1 d . . . H32A H 1.0446 -0.1457 0.1128 0.047 Uiso 1 1 calc R . . C33 C 1.0945(2) -0.19922(8) 0.2702(3) 0.0403(6) Uani 1 1 d . . . H33A H 1.1821 -0.1979 0.2600 0.048 Uiso 1 1 calc R . . C34 C 1.0489(2) -0.23176(8) 0.3711(3) 0.0440(6) Uani 1 1 d . . . H34A H 1.1049 -0.2533 0.4311 0.053 Uiso 1 1 calc R . . C35 C 0.9231(2) -0.23358(8) 0.3865(3) 0.0449(6) Uani 1 1 d . . . H35A H 0.8931 -0.2564 0.4581 0.054 Uiso 1 1 calc R . . C36 C 0.7000(3) -0.20516(13) 0.3168(5) 0.0886(13) Uani 1 1 d . . . H36A H 0.6577(11) -0.2156(9) 0.217(3) 0.133 Uiso 1 1 calc R . . H36B H 0.6719(9) -0.1767(7) 0.339(4) 0.133 Uiso 1 1 calc R . . H36C H 0.6867(5) -0.2244(9) 0.404(3) 0.133 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 0.0282(3) 0.0258(3) 0.0395(4) 0.0026(3) -0.0029(3) -0.0049(2) Al2 0.0227(3) 0.0355(3) 0.0263(4) -0.0033(3) 0.0031(2) 0.0016(2) N1 0.0171(7) 0.0273(8) 0.0207(9) -0.0017(7) 0.0006(6) -0.0034(6) N2 0.0195(7) 0.0255(8) 0.0178(9) 0.0021(7) 0.0005(6) -0.0018(6) N3 0.0179(7) 0.0270(8) 0.0285(10) -0.0009(7) 0.0029(6) -0.0067(6) C1 0.0179(8) 0.0265(9) 0.0217(11) 0.0000(8) 0.0025(7) -0.0031(7) C2 0.0217(9) 0.0259(9) 0.0255(12) -0.0019(8) -0.0002(8) -0.0048(7) C3 0.0176(9) 0.0276(10) 0.0300(12) -0.0016(9) -0.0014(8) -0.0030(7) C4 0.0302(10) 0.0362(11) 0.0259(13) -0.0041(9) 0.0054(8) -0.0031(8) C5 0.0316(10) 0.0347(10) 0.0209(12) 0.0062(9) 0.0021(8) 0.0014(8) C6 0.0214(10) 0.0393(12) 0.0472(15) 0.0016(11) -0.0012(9) -0.0105(8) C11 0.0422(15) 0.0364(15) 0.098(3) 0.0084(17) 0.0027(16) 0.0076(12) C12 0.072(2) 0.0512(18) 0.0449(19) 0.0153(15) 0.0017(15) -0.0119(16) C13 0.0457(15) 0.0427(15) 0.057(2) 0.0042(14) -0.0068(13) -0.0220(12) C21 0.0269(12) 0.0671(19) 0.058(2) -0.0157(16) -0.0001(12) -0.0009(12) C22 0.0505(16) 0.0612(18) 0.0304(15) 0.0006(14) 0.0147(12) 0.0054(13) C23 0.0396(14) 0.0378(13) 0.0476(18) -0.0064(13) 0.0015(12) 0.0041(11) C30 0.0371(12) 0.0468(13) 0.0450(16) -0.0164(12) 0.0138(10) -0.0078(10) C31 0.0461(13) 0.0333(12) 0.0437(16) -0.0050(11) -0.0015(11) 0.0042(10) C32 0.0467(13) 0.0331(12) 0.0389(15) -0.0012(10) 0.0075(10) -0.0107(10) C33 0.0348(11) 0.0426(13) 0.0430(15) -0.0083(12) 0.0024(10) -0.0038(10) C34 0.0520(14) 0.0392(13) 0.0389(16) -0.0001(11) -0.0019(11) 0.0047(11) C35 0.0644(16) 0.0376(12) 0.0348(15) 0.0027(11) 0.0144(12) -0.0110(11) C36 0.0473(17) 0.115(3) 0.110(3) -0.027(2) 0.0328(18) -0.0131(17) _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 C13 1.959(3) . ? Al1 C12 1.962(3) . ? Al1 C11 1.963(3) . ? Al1 N1 2.0977(17) . ? Al2 C23 1.962(3) . ? Al2 C22 1.962(3) . ? Al2 C21 1.967(3) . ? Al2 N2 2.0897(17) . ? N1 C1 1.482(2) . ? N1 C3 1.486(2) . ? N1 C4 1.489(3) . ? N2 C1 1.478(2) . ? N2 C2 1.481(2) . ? N2 C5 1.490(2) . ? N3 C3 1.446(2) . ? N3 C2 1.453(2) . ? N3 C6 1.464(2) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 H4A 0.9714 . ? C4 H4B 0.9714 . ? C4 H4C 0.9714 . ? C5 H5A 0.9601 . ? C5 H5B 0.9601 . ? C5 H5C 0.9601 . ? C6 H6A 0.9646 . ? C6 H6B 0.9646 . ? C6 H6C 0.9646 . ? C11 H11A 0.95(3) . ? C11 H11B 0.94(3) . ? C11 H11C 0.95(4) . ? C12 H12A 0.89(4) . ? C12 H12B 0.96(4) . ? C12 H12C 0.88(4) . ? C13 H13A 0.95(3) . ? C13 H13C 0.91(3) . ? C13 H13B 0.94(4) . ? C21 H21A 0.95(3) . ? C21 H21B 0.99(4) . ? C21 H21C 0.84(4) . ? C22 H22A 0.94(3) . ? C22 H22B 0.91(3) . ? C22 H22C 0.94(3) . ? C23 H23A 0.90(3) . ? C23 H23B 0.94(3) . ? C23 H23C 0.92(3) . ? C30 C35 1.382(3) . ? C30 C31 1.391(3) . ? C30 C36 1.499(3) . ? C31 C32 1.374(3) . ? C31 H31A 0.9500 . ? C32 C33 1.371(3) . ? C32 H32A 0.9500 . ? C33 C34 1.362(3) . ? C33 H33A 0.9500 . ? C34 C35 1.364(3) . ? C34 H34A 0.9500 . ? C35 H35A 0.9500 . ? C36 H36A 0.9058 . ? C36 H36B 0.9058 . ? C36 H36C 0.9058 . ? 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 C13 Al1 C12 113.91(15) . . ? C13 Al1 C11 115.60(16) . . ? C12 Al1 C11 114.90(18) . . ? C13 Al1 N1 103.39(10) . . ? C12 Al1 N1 105.52(11) . . ? C11 Al1 N1 101.28(11) . . ? C23 Al2 C22 113.96(14) . . ? C23 Al2 C21 115.68(14) . . ? C22 Al2 C21 115.28(15) . . ? C23 Al2 N2 103.10(10) . . ? C22 Al2 N2 103.04(10) . . ? C21 Al2 N2 103.36(11) . . ? C1 N1 C3 108.39(14) . . ? C1 N1 C4 114.03(15) . . ? C3 N1 C4 110.41(15) . . ? C1 N1 Al1 108.42(11) . . ? C3 N1 Al1 107.91(11) . . ? C4 N1 Al1 107.50(11) . . ? C1 N2 C2 108.85(13) . . ? C1 N2 C5 113.76(15) . . ? C2 N2 C5 110.41(14) . . ? C1 N2 Al2 107.84(11) . . ? C2 N2 Al2 108.54(11) . . ? C5 N2 Al2 107.29(11) . . ? C3 N3 C2 109.19(15) . . ? C3 N3 C6 110.68(15) . . ? C2 N3 C6 110.81(15) . . ? N2 C1 N1 117.14(14) . . ? N2 C1 H1A 108.0 . . ? N1 C1 H1A 108.0 . . ? N2 C1 H1B 108.0 . . ? N1 C1 H1B 108.0 . . ? H1A C1 H1B 107.3 . . ? N3 C2 N2 110.57(15) . . ? N3 C2 H2A 109.5 . . ? N2 C2 H2A 109.5 . . ? N3 C2 H2B 109.5 . . ? N2 C2 H2B 109.5 . . ? H2A C2 H2B 108.1 . . ? N3 C3 N1 110.74(14) . . ? N3 C3 H3A 109.5 . . ? N1 C3 H3A 109.5 . . ? N3 C3 H3B 109.5 . . ? N1 C3 H3B 109.5 . . ? H3A C3 H3B 108.1 . . ? N1 C4 H4A 109.5 . . ? N1 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? N1 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? N2 C5 H5A 109.5 . . ? N2 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? N2 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? N3 C6 H6A 109.5 . . ? N3 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? N3 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? Al1 C11 H11A 112.0(17) . . ? Al1 C11 H11B 108.2(19) . . ? H11A C11 H11B 108(3) . . ? Al1 C11 H11C 117(2) . . ? H11A C11 H11C 107(3) . . ? H11B C11 H11C 103(3) . . ? Al1 C12 H12A 110(2) . . ? Al1 C12 H12B 113(2) . . ? H12A C12 H12B 107(3) . . ? Al1 C12 H12C 113(2) . . ? H12A C12 H12C 111(3) . . ? H12B C12 H12C 102(3) . . ? Al1 C13 H13A 112.5(18) . . ? Al1 C13 H13C 108.9(19) . . ? H13A C13 H13C 109(3) . . ? Al1 C13 H13B 116(2) . . ? H13A C13 H13B 102(3) . . ? H13C C13 H13B 109(3) . . ? Al2 C21 H21A 113.6(17) . . ? Al2 C21 H21B 114.6(18) . . ? H21A C21 H21B 110(3) . . ? Al2 C21 H21C 110(2) . . ? H21A C21 H21C 111(3) . . ? H21B C21 H21C 97(3) . . ? Al2 C22 H22A 117.1(18) . . ? Al2 C22 H22B 108.0(19) . . ? H22A C22 H22B 105(3) . . ? Al2 C22 H22C 116(2) . . ? H22A C22 H22C 102(2) . . ? H22B C22 H22C 107(3) . . ? Al2 C23 H23A 116.1(18) . . ? Al2 C23 H23B 108.4(18) . . ? H23A C23 H23B 110(3) . . ? Al2 C23 H23C 114(2) . . ? H23A C23 H23C 104(2) . . ? H23B C23 H23C 104(3) . . ? C35 C30 C31 117.3(2) . . ? C35 C30 C36 121.9(3) . . ? C31 C30 C36 120.8(3) . . ? C32 C31 C30 120.7(2) . . ? C32 C31 H31A 119.7 . . ? C30 C31 H31A 119.7 . . ? C33 C32 C31 120.4(2) . . ? C33 C32 H32A 119.8 . . ? C31 C32 H32A 119.8 . . ? C34 C33 C32 119.6(2) . . ? C34 C33 H33A 120.2 . . ? C32 C33 H33A 120.2 . . ? C33 C34 C35 120.2(2) . . ? C33 C34 H34A 119.9 . . ? C35 C34 H34A 119.9 . . ? C34 C35 C30 121.8(2) . . ? C34 C35 H35A 119.1 . . ? C30 C35 H35A 119.1 . . ? C30 C36 H36A 109.5 . . ? C30 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C30 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C13 Al1 N1 C1 -73.46(16) . . . . ? C12 Al1 N1 C1 46.45(16) . . . . ? C11 Al1 N1 C1 166.51(16) . . . . ? C13 Al1 N1 C3 169.34(16) . . . . ? C12 Al1 N1 C3 -70.75(16) . . . . ? C11 Al1 N1 C3 49.32(18) . . . . ? C13 Al1 N1 C4 50.25(16) . . . . ? C12 Al1 N1 C4 170.16(15) . . . . ? C11 Al1 N1 C4 -69.77(17) . . . . ? C23 Al2 N2 C1 -169.47(14) . . . . ? C22 Al2 N2 C1 -50.66(15) . . . . ? C21 Al2 N2 C1 69.70(16) . . . . ? C23 Al2 N2 C2 -51.69(15) . . . . ? C22 Al2 N2 C2 67.11(15) . . . . ? C21 Al2 N2 C2 -172.52(15) . . . . ? C23 Al2 N2 C5 67.62(14) . . . . ? C22 Al2 N2 C5 -173.57(14) . . . . ? C21 Al2 N2 C5 -53.21(16) . . . . ? C2 N2 C1 N1 48.5(2) . . . . ? C5 N2 C1 N1 -75.02(19) . . . . ? Al2 N2 C1 N1 166.12(12) . . . . ? C3 N1 C1 N2 -48.5(2) . . . . ? C4 N1 C1 N2 75.0(2) . . . . ? Al1 N1 C1 N2 -165.35(12) . . . . ? C3 N3 C2 N2 64.47(19) . . . . ? C6 N3 C2 N2 -173.37(16) . . . . ? C1 N2 C2 N3 -54.5(2) . . . . ? C5 N2 C2 N3 71.05(19) . . . . ? Al2 N2 C2 N3 -171.62(12) . . . . ? C2 N3 C3 N1 -64.7(2) . . . . ? C6 N3 C3 N1 173.03(17) . . . . ? C1 N1 C3 N3 54.8(2) . . . . ? C4 N1 C3 N3 -70.8(2) . . . . ? Al1 N1 C3 N3 172.00(13) . . . . ? C35 C30 C31 C32 -0.2(3) . . . . ? C36 C30 C31 C32 179.9(2) . . . . ? C30 C31 C32 C33 0.3(3) . . . . ? C31 C32 C33 C34 0.0(3) . . . . ? C32 C33 C34 C35 -0.3(4) . . . . ? C33 C34 C35 C30 0.4(4) . . . . ? C31 C30 C35 C34 -0.2(4) . . . . ? C36 C30 C35 C34 179.8(3) . . . . ? _diffrn_measured_fraction_theta_max 0.954 _diffrn_reflns_theta_full 26.93 _diffrn_measured_fraction_theta_full 0.954 _refine_diff_density_max 0.289 _refine_diff_density_min -0.172 _refine_diff_density_rms 0.043 #===END data_compound_5_CCDC_679433 _database_code_depnum_ccdc_archive 'CCDC 679433' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H75 Al5 N3 Sm3' _chemical_formula_weight 543.95 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 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' Sm Sm -0.1638 3.4418 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/m loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' '-x, -y, -z' 'x, -y-1/2, z' _cell_length_a 9.5604(11) _cell_length_b 17.289(2) _cell_length_c 14.1729(17) _cell_angle_alpha 90.00 _cell_angle_beta 97.610(2) _cell_angle_gamma 90.00 _cell_volume 2322.0(5) _cell_formula_units_Z 2 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.556 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1078 _exptl_absorpt_coefficient_mu 3.860 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3905 _exptl_absorpt_correction_T_max 0.5123 _exptl_absorpt_process_details ? _exptl_special_details ; Absorption correction was done with the program ABSCOR from the STOE IPDS-1 software pacage. ABSCOR is a modification of the well-known DIFABS. In contrary to DIFABS, ABSCOR loads and provides Fo^2^ values instead of Fo ones. ; _diffrn_ambient_temperature 153(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'Omega and Phi scans' _diffrn_detector_area_resol_mean 80 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 26856 _diffrn_reflns_av_R_equivalents 0.0308 _diffrn_reflns_av_sigmaI/netI 0.0294 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.45 _diffrn_reflns_theta_max 30.03 _reflns_number_total 6979 _reflns_number_gt 6480 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker AXS, 2000)' _computing_cell_refinement 'SAINT (Bruker AXS, 2000)' _computing_data_reduction 'SAINT,SADABS (Bruker AXS, 2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_publication_material 'Bruker SHELXTL' _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. A disorderd toluene solvent molecule was refiend with hexagon constraint (AFIX 6) and anisotropic displacement parameters. ; _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^)+(0.0244P)^2^+3.7927P] 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 6979 _refine_ls_number_parameters 331 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0424 _refine_ls_R_factor_gt 0.0378 _refine_ls_wR_factor_ref 0.0793 _refine_ls_wR_factor_gt 0.0778 _refine_ls_goodness_of_fit_ref 1.223 _refine_ls_restrained_S_all 1.223 _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 Sm1 Sm 0.30695(3) 0.2500 0.200727(17) 0.02371(6) Uani 1 2 d S . . Sm2 Sm 0.55499(2) 0.353434(11) 0.373251(13) 0.02504(6) Uani 1 1 d . . . Al1 Al 0.23641(12) 0.34006(7) 0.39227(8) 0.0273(2) Uani 1 1 d . . . Al2 Al 0.60783(13) 0.45527(8) 0.19903(9) 0.0343(3) Uani 1 1 d . . . Al3 Al 0.47237(18) 0.2500 0.53611(11) 0.0280(3) Uani 1 2 d S . . N1 N 0.1735(4) 0.3183(2) 0.0381(2) 0.0372(8) Uani 1 1 d . . . N2 N 0.3763(5) 0.2500 0.0142(3) 0.0292(9) Uani 1 2 d S . . C1 C 0.0925(7) 0.3902(4) 0.0195(4) 0.0602(17) Uani 1 1 d . . . H1A H 0.055(5) 0.394(3) -0.048(4) 0.045(13) Uiso 1 1 d . . . H1B H 0.148(6) 0.438(4) 0.049(4) 0.071(19) Uiso 1 1 d . . . H1C H 0.004(7) 0.382(4) 0.047(4) 0.08(2) Uiso 1 1 d . . . C2 C 0.5109(7) 0.2500 -0.0257(5) 0.0397(14) Uani 1 2 d S . . H2A H 0.507(6) 0.2500 -0.091(4) 0.023(14) Uiso 1 2 d S . . H2B H 0.565(5) 0.204(3) -0.010(3) 0.036(12) Uiso 1 1 d . . . C3 C 0.0876(7) 0.2500 0.0103(4) 0.0459(17) Uani 1 2 d S . . H3A H 0.056(9) 0.2500 -0.060(6) 0.07(3) Uiso 1 2 d S . . H3B H 0.007(8) 0.2500 0.048(6) 0.06(2) Uiso 1 2 d S . . C4 C 0.2936(5) 0.3188(3) -0.0161(3) 0.0363(9) Uani 1 1 d . . . H4A H 0.346(5) 0.365(3) 0.005(3) 0.033(12) Uiso 1 1 d . . . H4B H 0.257(5) 0.316(3) -0.084(3) 0.045(13) Uiso 1 1 d . . . C11 C 0.1048(5) 0.3530(3) 0.4874(4) 0.0425(10) Uani 1 1 d . . . H11A H 0.165(6) 0.365(3) 0.551(4) 0.056(16) Uiso 1 1 d . . . H11B H 0.038(6) 0.316(3) 0.493(4) 0.060(17) Uiso 1 1 d . . . H11C H 0.066(6) 0.401(4) 0.477(4) 0.062(17) Uiso 1 1 d . . . C12 C 0.1162(6) 0.3534(4) 0.2634(3) 0.0483(13) Uani 1 1 d . . . H12A H 0.158(6) 0.386(3) 0.215(4) 0.065(18) Uiso 1 1 d . . . H12B H 0.053(6) 0.317(3) 0.241(4) 0.051(16) Uiso 1 1 d . . . H12C H 0.053(6) 0.386(3) 0.290(4) 0.055(15) Uiso 1 1 d . . . C13 C 0.3435(5) 0.4446(2) 0.3989(3) 0.0364(9) Uani 1 1 d . . . H13A H 0.414(6) 0.454(3) 0.456(4) 0.060(16) Uiso 1 1 d . . . H13B H 0.261(5) 0.474(3) 0.403(3) 0.040(13) Uiso 1 1 d . . . H13C H 0.382(5) 0.466(3) 0.346(4) 0.048(14) Uiso 1 1 d . . . C21 C 0.7560(6) 0.4324(4) 0.1186(4) 0.0527(13) Uani 1 1 d . . . H21A H 0.720(7) 0.429(4) 0.061(5) 0.08(2) Uiso 1 1 d . . . H21B H 0.789(7) 0.381(4) 0.132(5) 0.09(2) Uiso 1 1 d . . . H21C H 0.837(6) 0.470(4) 0.130(4) 0.071(18) Uiso 1 1 d . . . C22 C 0.4972(8) 0.5510(4) 0.1687(5) 0.0600(15) Uani 1 1 d . . . H22A H 0.462(6) 0.547(3) 0.104(4) 0.057(17) Uiso 1 1 d . . . H22B H 0.552(9) 0.596(5) 0.178(6) 0.13(3) Uiso 1 1 d . . . H22C H 0.414(8) 0.554(4) 0.199(5) 0.11(3) Uiso 1 1 d . . . C23 C 0.7155(6) 0.4725(3) 0.3343(3) 0.0431(10) Uani 1 1 d . . . H23A H 0.656(6) 0.495(3) 0.382(4) 0.066(17) Uiso 1 1 d . . . H23B H 0.797(6) 0.436(3) 0.364(4) 0.068(18) Uiso 1 1 d . . . H23C H 0.765(7) 0.514(4) 0.317(4) 0.08(2) Uiso 1 1 d . . . C24 C 0.4775(4) 0.3611(2) 0.2048(3) 0.0279(7) Uani 1 1 d . . . H24A H 0.402(6) 0.381(3) 0.171(4) 0.055(16) Uiso 1 1 d . . . H24B H 0.509(6) 0.330(3) 0.162(4) 0.057(16) Uiso 1 1 d . . . C31 C 0.3693(10) 0.2500 0.6470(6) 0.070(3) Uani 1 2 d S . . H31A H 0.421(9) 0.2500 0.697(7) 0.09(3) Uiso 1 2 d SD . . H31B H 0.317(7) 0.213(3) 0.653(5) 0.10(3) Uiso 1 1 d D . . C32 C 0.6169(6) 0.3385(3) 0.5598(3) 0.0431(11) Uani 1 1 d . . . H32A H 0.635(6) 0.328(3) 0.628(4) 0.061(16) Uiso 1 1 d . . . H32B H 0.702(7) 0.336(4) 0.530(4) 0.07(2) Uiso 1 1 d . . . H32C H 0.591(6) 0.391(4) 0.558(4) 0.075(19) Uiso 1 1 d . . . C33 C 0.3777(5) 0.2500 0.3948(3) 0.0229(9) Uani 1 2 d S . . C40 C 0.7353(7) 0.2500 0.3448(5) 0.0404(14) Uani 1 2 d S . . H40A H 0.822(11) 0.2500 0.383(7) 0.11(4) Uiso 1 2 d SD . . H40B H 0.764(9) 0.286(3) 0.312(6) 0.15(4) Uiso 1 1 d D . . C71 C -0.0999(7) 0.1920(4) 0.7638(5) 0.050(2) Uiso 0.50 1 d PG . . C72 C -0.2021(6) 0.2219(4) 0.8119(4) 0.041(2) Uiso 0.50 1 d PG . . H72A H -0.2657 0.1883 0.8379 0.050 Uiso 0.50 1 calc PR . . C73 C -0.2129(6) 0.3000(4) 0.8226(4) 0.040(2) Uiso 0.50 1 d PG . . H73A H -0.2840 0.3208 0.8561 0.048 Uiso 0.50 1 calc PR . . C74 C -0.1215(8) 0.3483(4) 0.7852(6) 0.053(3) Uiso 0.50 1 d PG . . H74A H -0.1291 0.4027 0.7927 0.064 Uiso 0.50 1 calc PR . . C75 C -0.0193(7) 0.3184(4) 0.7371(5) 0.062(3) Uiso 0.50 1 d PG . . H75A H 0.0442 0.3521 0.7113 0.074 Uiso 0.50 1 calc PR . . C76 C -0.0083(7) 0.2429(4) 0.7263(4) 0.062(2) Uiso 0.50 1 d PG . . H76A H 0.0631 0.2229 0.6925 0.075 Uiso 0.50 1 calc PR . . C77 C -0.0761(15) 0.1099(8) 0.7459(10) 0.078(4) Uiso 0.50 1 d P . . H77A H -0.1447 0.0787 0.7749 0.117 Uiso 0.50 1 calc PR . . H77B H 0.0197 0.0955 0.7738 0.117 Uiso 0.50 1 calc PR . . H77C H -0.0874 0.1005 0.6772 0.117 Uiso 0.50 1 calc PR . . 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 Sm1 0.02337(12) 0.03080(14) 0.01637(11) 0.000 0.00041(9) 0.000 Sm2 0.02925(10) 0.02313(9) 0.02137(9) 0.00036(6) -0.00170(7) -0.00270(7) Al1 0.0292(5) 0.0320(6) 0.0205(5) -0.0014(4) 0.0028(4) 0.0055(5) Al2 0.0367(6) 0.0348(6) 0.0318(6) 0.0080(5) 0.0059(5) 0.0002(5) Al3 0.0359(8) 0.0286(8) 0.0183(7) 0.000 -0.0013(6) 0.000 N1 0.0341(17) 0.055(2) 0.0227(15) 0.0025(15) 0.0026(13) 0.0112(16) N2 0.031(2) 0.035(2) 0.022(2) 0.000 0.0036(17) 0.000 C1 0.067(4) 0.083(4) 0.031(2) 0.011(3) 0.005(2) 0.042(3) C2 0.036(3) 0.053(4) 0.033(3) 0.000 0.015(3) 0.000 C3 0.028(3) 0.086(5) 0.022(3) 0.000 0.000(2) 0.000 C4 0.042(2) 0.047(2) 0.0206(17) 0.0059(16) 0.0057(16) 0.0032(19) C11 0.043(2) 0.044(3) 0.043(3) -0.005(2) 0.017(2) 0.001(2) C12 0.044(3) 0.067(3) 0.031(2) -0.008(2) -0.005(2) 0.023(3) C13 0.042(2) 0.028(2) 0.041(2) 0.0026(17) 0.0107(19) 0.0068(17) C21 0.044(3) 0.075(4) 0.042(3) 0.006(3) 0.016(2) -0.002(3) C22 0.067(4) 0.048(3) 0.066(4) 0.024(3) 0.013(3) 0.011(3) C23 0.051(3) 0.041(2) 0.038(2) 0.0010(19) 0.006(2) -0.015(2) C24 0.0271(17) 0.0289(18) 0.0271(18) 0.0007(14) 0.0018(14) 0.0001(15) C31 0.052(5) 0.132(10) 0.026(4) 0.000 0.005(3) 0.000 C32 0.064(3) 0.032(2) 0.028(2) 0.0001(17) -0.015(2) -0.008(2) C33 0.023(2) 0.028(2) 0.016(2) 0.000 -0.0019(17) 0.000 C40 0.032(3) 0.036(3) 0.052(4) 0.000 0.002(3) 0.000 _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 Sm1 C24 2.515(4) . ? Sm1 C24 2.515(4) 4_565 ? Sm1 C33 2.744(5) . ? Sm1 N1 2.748(3) 4_565 ? Sm1 N1 2.748(3) . ? Sm1 C12 2.782(5) 4_565 ? Sm1 C12 2.782(5) . ? Sm1 N2 2.810(4) . ? Sm1 Al1 3.2762(11) . ? Sm1 Al1 3.2762(11) 4_565 ? Sm1 Sm2 3.6420(4) . ? Sm1 Sm2 3.6420(4) 4_565 ? Sm1 H24A 2.50(5) . ? Sm1 H24B 2.50(5) . ? Sm2 C24 2.408(4) . ? Sm2 C33 2.510(3) . ? Sm2 C40 2.553(5) . ? Sm2 C13 2.627(4) . ? Sm2 C32 2.644(5) . ? Sm2 C23 2.669(5) . ? Sm2 Al1 3.1017(12) . ? Sm2 Al3 3.1036(13) . ? Sm2 Al2 3.1276(12) . ? Sm2 Sm2 3.5765(6) 4_565 ? Sm2 H13A 2.58(5) . ? Sm2 H13C 2.56(5) . ? Sm2 H32B 2.48(6) . ? Sm2 H40B 2.56(8) . ? Al1 C11 1.975(5) . ? Al1 C12 2.038(5) . ? Al1 C33 2.058(3) . ? Al1 C13 2.073(5) . ? Al2 C21 1.972(5) . ? Al2 C22 1.980(6) . ? Al2 C24 2.058(4) . ? Al2 C23 2.073(5) . ? Al3 C31 1.962(9) . ? Al3 C32 2.060(5) . ? Al3 C32 2.060(5) 4_565 ? Al3 C33 2.086(5) . ? Al3 Sm2 3.1036(13) 4_565 ? N1 C3 1.462(5) . ? N1 C4 1.464(5) . ? N1 C1 1.470(6) . ? N2 C4 1.461(5) . ? N2 C4 1.461(5) 4_565 ? N2 C2 1.472(7) . ? C1 H1A 0.98(5) . ? C1 H1B 1.04(6) . ? C1 H1C 0.99(6) . ? C2 H2A 0.92(6) . ? C2 H2B 0.95(4) . ? C3 N1 1.462(5) 4_565 ? C3 H3A 1.00(8) . ? C3 H3B 0.99(8) . ? C4 H4A 0.97(4) . ? C4 H4B 0.97(5) . ? C11 H11A 1.02(6) . ? C11 H11B 0.91(6) . ? C11 H11C 0.92(6) . ? C12 H12A 1.01(6) . ? C12 H12B 0.89(5) . ? C12 H12C 0.94(6) . ? C13 H13A 1.00(6) . ? C13 H13B 0.95(5) . ? C13 H13C 0.96(5) . ? C21 H21A 0.85(7) . ? C21 H21B 0.96(7) . ? C21 H21C 1.00(6) . ? C22 H22A 0.93(6) . ? C22 H22B 0.93(9) . ? C22 H22C 0.95(8) . ? C23 H23A 1.02(6) . ? C23 H23B 1.05(6) . ? C23 H23C 0.92(7) . ? C24 H24A 0.89(5) . ? C24 H24B 0.89(6) . ? C31 H31A 0.81(9) . ? C31 H31B 0.82(6) . ? C32 H32A 0.97(6) . ? C32 H32B 0.97(6) . ? C32 H32C 0.94(7) . ? C33 Al1 2.058(3) 4_565 ? C33 Sm2 2.510(3) 4_565 ? C40 Sm2 2.553(5) 4_565 ? C40 H40A 0.93(10) . ? C40 H40B 0.84(7) . ? C71 C72 1.364(4) . ? C71 C76 1.394(4) . ? C71 C77 1.466(15) . ? C71 C76 1.561(12) 4_565 ? C71 C72 1.952(10) 4_565 ? C71 C71 2.004(13) 4_565 ? C72 C73 1.365(4) . ? C72 C71 1.952(11) 4_565 ? C72 H72A 0.9500 . ? C73 C74 1.365(4) . ? C73 H73A 0.9500 . ? C74 C75 1.364(4) . ? C74 H74A 0.9500 . ? C75 C76 1.321(4) . ? C75 H75A 0.9500 . ? C76 H76A 0.9500 . ? C77 H77A 0.9800 . ? C77 H77B 0.9800 . ? C77 H77C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C24 Sm1 C24 99.57(19) . 4_565 ? C24 Sm1 C33 84.50(11) . . ? C24 Sm1 C33 84.50(11) 4_565 . ? C24 Sm1 N1 125.08(12) . 4_565 ? C24 Sm1 N1 85.34(12) 4_565 4_565 ? C33 Sm1 N1 149.98(9) . 4_565 ? C24 Sm1 N1 85.34(12) . . ? C24 Sm1 N1 125.08(12) 4_565 . ? C33 Sm1 N1 149.98(9) . . ? N1 Sm1 N1 50.87(17) 4_565 . ? C24 Sm1 C12 159.02(15) . 4_565 ? C24 Sm1 C12 87.28(17) 4_565 4_565 ? C33 Sm1 C12 76.39(12) . 4_565 ? N1 Sm1 C12 74.97(13) 4_565 4_565 ? N1 Sm1 C12 107.01(13) . 4_565 ? C24 Sm1 C12 87.28(17) . . ? C24 Sm1 C12 159.02(15) 4_565 . ? C33 Sm1 C12 76.39(12) . . ? N1 Sm1 C12 107.01(13) 4_565 . ? N1 Sm1 C12 74.97(12) . . ? C12 Sm1 C12 79.9(3) 4_565 . ? C24 Sm1 N2 77.78(11) . . ? C24 Sm1 N2 77.78(11) 4_565 . ? C33 Sm1 N2 152.33(14) . . ? N1 Sm1 N2 49.63(10) 4_565 . ? N1 Sm1 N2 49.63(10) . . ? C12 Sm1 N2 123.17(13) 4_565 . ? C12 Sm1 N2 123.17(13) . . ? C24 Sm1 Al1 79.75(9) . . ? C24 Sm1 Al1 123.23(9) 4_565 . ? C33 Sm1 Al1 38.73(7) . . ? N1 Sm1 Al1 140.82(8) 4_565 . ? N1 Sm1 Al1 111.53(8) . . ? C12 Sm1 Al1 79.92(13) 4_565 . ? C12 Sm1 Al1 38.22(10) . . ? N2 Sm1 Al1 151.62(2) . . ? C24 Sm1 Al1 123.23(9) . 4_565 ? C24 Sm1 Al1 79.75(9) 4_565 4_565 ? C33 Sm1 Al1 38.73(7) . 4_565 ? N1 Sm1 Al1 111.53(8) 4_565 4_565 ? N1 Sm1 Al1 140.82(8) . 4_565 ? C12 Sm1 Al1 38.22(10) 4_565 4_565 ? C12 Sm1 Al1 79.92(13) . 4_565 ? N2 Sm1 Al1 151.62(2) . 4_565 ? Al1 Sm1 Al1 56.75(4) . 4_565 ? C24 Sm1 Sm2 41.17(9) . . ? C24 Sm1 Sm2 89.84(9) 4_565 . ? C33 Sm1 Sm2 43.53(7) . . ? N1 Sm1 Sm2 164.27(7) 4_565 . ? N1 Sm1 Sm2 122.74(8) . . ? C12 Sm1 Sm2 119.81(10) 4_565 . ? C12 Sm1 Sm2 82.31(12) . . ? N2 Sm1 Sm2 114.70(8) . . ? Al1 Sm1 Sm2 52.95(2) . . ? Al1 Sm1 Sm2 82.20(2) 4_565 . ? C24 Sm1 Sm2 89.84(9) . 4_565 ? C24 Sm1 Sm2 41.17(9) 4_565 4_565 ? C33 Sm1 Sm2 43.53(7) . 4_565 ? N1 Sm1 Sm2 122.74(8) 4_565 4_565 ? N1 Sm1 Sm2 164.27(7) . 4_565 ? C12 Sm1 Sm2 82.31(12) 4_565 4_565 ? C12 Sm1 Sm2 119.81(10) . 4_565 ? N2 Sm1 Sm2 114.70(8) . 4_565 ? Al1 Sm1 Sm2 82.20(2) . 4_565 ? Al1 Sm1 Sm2 52.95(2) 4_565 4_565 ? Sm2 Sm1 Sm2 58.812(10) . 4_565 ? C24 Sm1 H24A 20.3(13) . . ? C24 Sm1 H24A 116.6(13) 4_565 . ? C33 Sm1 H24A 97.1(12) . . ? N1 Sm1 H24A 112.7(12) 4_565 . ? N1 Sm1 H24A 66.8(13) . . ? C12 Sm1 H24A 154.8(13) 4_565 . ? C12 Sm1 H24A 74.9(13) . . ? N2 Sm1 H24A 72.8(12) . . ? Al1 Sm1 H24A 80.1(12) . . ? Al1 Sm1 H24A 133.7(12) 4_565 . ? Sm2 Sm1 H24A 56.6(12) . . ? Sm2 Sm1 H24A 109.9(13) 4_565 . ? C24 Sm1 H24B 20.4(13) . . ? C24 Sm1 H24B 84.9(13) 4_565 . ? C33 Sm1 H24B 97.1(13) . . ? N1 Sm1 H24B 110.0(13) 4_565 . ? N1 Sm1 H24B 82.2(13) . . ? C12 Sm1 H24B 170.3(13) 4_565 . ? C12 Sm1 H24B 105.7(13) . . ? N2 Sm1 H24B 60.6(13) . . ? Al1 Sm1 H24B 99.6(13) . . ? Al1 Sm1 H24B 134.1(13) 4_565 . ? Sm2 Sm1 H24B 54.5(13) . . ? Sm2 Sm1 H24B 88.1(13) 4_565 . ? H24A Sm1 H24B 31.8(16) . . ? C24 Sm2 C33 92.04(14) . . ? C24 Sm2 C40 90.42(19) . . ? C33 Sm2 C40 90.08(13) . . ? C24 Sm2 C13 87.86(14) . . ? C33 Sm2 C13 82.30(13) . . ? C40 Sm2 C13 172.12(15) . . ? C24 Sm2 C32 174.54(15) . . ? C33 Sm2 C32 82.79(15) . . ? C40 Sm2 C32 91.3(2) . . ? C13 Sm2 C32 89.70(17) . . ? C24 Sm2 C23 82.07(14) . . ? C33 Sm2 C23 172.18(15) . . ? C40 Sm2 C23 95.09(17) . . ? C13 Sm2 C23 92.29(16) . . ? C32 Sm2 C23 102.91(15) . . ? C24 Sm2 Al1 85.04(10) . . ? C33 Sm2 Al1 41.38(8) . . ? C40 Sm2 Al1 130.77(11) . . ? C13 Sm2 Al1 41.41(10) . . ? C32 Sm2 Al1 89.90(13) . . ? C23 Sm2 Al1 132.35(13) . . ? C24 Sm2 Al3 133.94(10) . . ? C33 Sm2 Al3 41.99(11) . . ? C40 Sm2 Al3 87.58(14) . . ? C13 Sm2 Al3 88.08(10) . . ? C32 Sm2 Al3 41.03(11) . . ? C23 Sm2 Al3 143.94(11) . . ? Al1 Sm2 Al3 62.80(4) . . ? C24 Sm2 Al2 41.14(9) . . ? C33 Sm2 Al2 132.78(11) . . ? C40 Sm2 Al2 94.95(15) . . ? C13 Sm2 Al2 88.80(10) . . ? C32 Sm2 Al2 143.71(11) . . ? C23 Sm2 Al2 40.97(11) . . ? Al1 Sm2 Al2 111.94(3) . . ? Al3 Sm2 Al2 174.33(4) . . ? C24 Sm2 Sm2 93.15(10) . 4_565 ? C33 Sm2 Sm2 44.57(8) . 4_565 ? C40 Sm2 Sm2 45.54(11) . 4_565 ? C13 Sm2 Sm2 126.88(10) . 4_565 ? C32 Sm2 Sm2 84.41(10) . 4_565 ? C23 Sm2 Sm2 140.47(12) . 4_565 ? Al1 Sm2 Sm2 85.72(2) . 4_565 ? Al3 Sm2 Sm2 54.818(18) . 4_565 ? Al2 Sm2 Sm2 124.26(3) . 4_565 ? C24 Sm2 Sm1 43.43(9) . . ? C33 Sm2 Sm1 48.82(10) . . ? C40 Sm2 Sm1 86.74(14) . . ? C13 Sm2 Sm1 86.72(11) . . ? C32 Sm2 Sm1 131.54(11) . . ? C23 Sm2 Sm1 125.51(11) . . ? Al1 Sm2 Sm1 57.46(2) . . ? Al3 Sm2 Sm1 90.53(3) . . ? Al2 Sm2 Sm1 84.56(3) . . ? Sm2 Sm2 Sm1 60.594(5) 4_565 . ? C24 Sm2 H13A 107.7(13) . . ? C33 Sm2 H13A 91.4(12) . . ? C40 Sm2 H13A 161.7(13) . . ? C13 Sm2 H13A 22.1(12) . . ? C32 Sm2 H13A 70.8(13) . . ? C23 Sm2 H13A 85.6(12) . . ? Al1 Sm2 H13A 55.4(12) . . ? Al3 Sm2 H13A 81.4(12) . . ? Al2 Sm2 H13A 97.4(12) . . ? Sm2 Sm2 H13A 132.5(12) 4_565 . ? Sm1 Sm2 H13A 107.8(13) . . ? C24 Sm2 H13C 72.4(12) . . ? C33 Sm2 H13C 97.4(12) . . ? C40 Sm2 H13C 161.4(12) . . ? C13 Sm2 H13C 21.3(12) . . ? C32 Sm2 H13C 106.4(12) . . ? C23 Sm2 H13C 75.9(12) . . ? Al1 Sm2 H13C 56.5(12) . . ? Al3 Sm2 H13C 109.4(12) . . ? Al2 Sm2 H13C 67.5(12) . . ? Sm2 Sm2 H13C 139.8(11) 4_565 . ? Sm1 Sm2 H13C 85.5(11) . . ? H13A Sm2 H13C 35.7(16) . . ? C24 Sm2 H32B 162.9(15) . . ? C33 Sm2 H32B 96.7(15) . . ? C40 Sm2 H32B 75.0(15) . . ? C13 Sm2 H32B 107.8(15) . . ? C32 Sm2 H32B 21.5(15) . . ? C23 Sm2 H32B 90.4(15) . . ? Al1 Sm2 H32B 111.1(15) . . ? Al3 Sm2 H32B 55.6(15) . . ? Al2 Sm2 H32B 130.0(15) . . ? Sm2 Sm2 H32B 82.9(14) 4_565 . ? Sm1 Sm2 H32B 141.3(14) . . ? H13A Sm2 H32B 86.8(19) . . ? H13C Sm2 H32B 120.6(19) . . ? C24 Sm2 H40B 81(2) . . ? C33 Sm2 H40B 106.7(12) . . ? C40 Sm2 H40B 19.0(15) . . ? C13 Sm2 H40B 165.7(18) . . ? C32 Sm2 H40B 102(2) . . ? C23 Sm2 H40B 77.6(13) . . ? Al1 Sm2 H40B 144.6(12) . . ? Al3 Sm2 H40B 106.0(17) . . ? Al2 Sm2 H40B 77.0(18) . . ? Sm2 Sm2 H40B 62.9(13) 4_565 . ? Sm1 Sm2 H40B 91.0(16) . . ? H13A Sm2 H40B 160.0(18) . . ? H13C Sm2 H40B 144(2) . . ? H32B Sm2 H40B 83(2) . . ? C11 Al1 C12 105.3(2) . . ? C11 Al1 C33 123.4(2) . . ? C12 Al1 C33 113.1(2) . . ? C11 Al1 C13 103.0(2) . . ? C12 Al1 C13 99.1(2) . . ? C33 Al1 C13 109.87(17) . . ? C11 Al1 Sm2 140.57(17) . . ? C12 Al1 Sm2 110.95(18) . . ? C33 Al1 Sm2 53.72(11) . . ? C13 Al1 Sm2 56.93(13) . . ? C11 Al1 Sm1 147.08(17) . . ? C12 Al1 Sm1 57.65(14) . . ? C33 Al1 Sm1 56.51(13) . . ? C13 Al1 Sm1 107.29(13) . . ? Sm2 Al1 Sm1 69.58(2) . . ? C21 Al2 C22 116.5(3) . . ? C21 Al2 C24 110.4(2) . . ? C22 Al2 C24 111.1(3) . . ? C21 Al2 C23 104.9(2) . . ? C22 Al2 C23 105.4(3) . . ? C24 Al2 C23 107.83(18) . . ? C21 Al2 Sm2 123.2(2) . . ? C22 Al2 Sm2 120.3(2) . . ? C24 Al2 Sm2 50.33(11) . . ? C23 Al2 Sm2 57.55(14) . . ? C31 Al3 C32 105.5(2) . . ? C31 Al3 C32 105.5(2) . 4_565 ? C32 Al3 C32 96.0(3) . 4_565 ? C31 Al3 C33 124.7(3) . . ? C32 Al3 C33 110.66(16) . . ? C32 Al3 C33 110.66(16) 4_565 . ? C31 Al3 Sm2 143.11(8) . 4_565 ? C32 Al3 Sm2 108.53(18) . 4_565 ? C32 Al3 Sm2 57.42(13) 4_565 4_565 ? C33 Al3 Sm2 53.61(10) . 4_565 ? C31 Al3 Sm2 143.11(8) . . ? C32 Al3 Sm2 57.42(13) . . ? C32 Al3 Sm2 108.53(18) 4_565 . ? C33 Al3 Sm2 53.61(10) . . ? Sm2 Al3 Sm2 70.36(4) 4_565 . ? C3 N1 C4 108.4(4) . . ? C3 N1 C1 111.8(4) . . ? C4 N1 C1 109.4(4) . . ? C3 N1 Sm1 93.5(3) . . ? C4 N1 Sm1 97.7(2) . . ? C1 N1 Sm1 133.6(3) . . ? C4 N2 C4 109.0(5) . 4_565 ? C4 N2 C2 110.7(3) . . ? C4 N2 C2 110.7(3) 4_565 . ? C4 N2 Sm1 95.2(2) . . ? C4 N2 Sm1 95.2(2) 4_565 . ? C2 N2 Sm1 133.5(4) . . ? N1 C1 H1A 110(3) . . ? N1 C1 H1B 112(3) . . ? H1A C1 H1B 116(5) . . ? N1 C1 H1C 106(4) . . ? H1A C1 H1C 100(4) . . ? H1B C1 H1C 112(5) . . ? N2 C2 H2A 118(4) . . ? N2 C2 H2B 113(3) . . ? H2A C2 H2B 100(3) . . ? N1 C3 N1 107.7(5) . 4_565 ? N1 C3 H3A 111(2) . . ? N1 C3 H3A 111(2) 4_565 . ? N1 C3 H3B 108(2) . . ? N1 C3 H3B 108(2) 4_565 . ? H3A C3 H3B 113(6) . . ? N2 C4 N1 105.8(3) . . ? N2 C4 H4A 110(3) . . ? N1 C4 H4A 105(3) . . ? N2 C4 H4B 111(3) . . ? N1 C4 H4B 108(3) . . ? H4A C4 H4B 116(4) . . ? Al1 C11 H11A 107(3) . . ? Al1 C11 H11B 119(4) . . ? H11A C11 H11B 112(5) . . ? Al1 C11 H11C 106(4) . . ? H11A C11 H11C 98(4) . . ? H11B C11 H11C 112(5) . . ? Al1 C12 Sm1 84.13(16) . . ? Al1 C12 H12A 116(3) . . ? Sm1 C12 H12A 78(3) . . ? Al1 C12 H12B 121(4) . . ? Sm1 C12 H12B 83(4) . . ? H12A C12 H12B 117(5) . . ? Al1 C12 H12C 92(3) . . ? Sm1 C12 H12C 175(3) . . ? H12A C12 H12C 106(5) . . ? H12B C12 H12C 97(5) . . ? Al1 C13 Sm2 81.66(14) . . ? Al1 C13 H13A 117(3) . . ? Sm2 C13 H13A 76(3) . . ? Al1 C13 H13B 93(3) . . ? Sm2 C13 H13B 173(3) . . ? H13A C13 H13B 110(4) . . ? Al1 C13 H13C 123(3) . . ? Sm2 C13 H13C 75(3) . . ? H13A C13 H13C 107(4) . . ? H13B C13 H13C 104(4) . . ? Al2 C21 H21A 110(4) . . ? Al2 C21 H21B 109(4) . . ? H21A C21 H21B 102(6) . . ? Al2 C21 H21C 112(3) . . ? H21A C21 H21C 114(5) . . ? H21B C21 H21C 110(5) . . ? Al2 C22 H22A 105(4) . . ? Al2 C22 H22B 113(5) . . ? H22A C22 H22B 109(6) . . ? Al2 C22 H22C 114(5) . . ? H22A C22 H22C 103(5) . . ? H22B C22 H22C 112(7) . . ? Al2 C23 Sm2 81.48(16) . . ? Al2 C23 H23A 115(3) . . ? Sm2 C23 H23A 77(3) . . ? Al2 C23 H23B 123(3) . . ? Sm2 C23 H23B 83(3) . . ? H23A C23 H23B 114(4) . . ? Al2 C23 H23C 94(4) . . ? Sm2 C23 H23C 175(4) . . ? H23A C23 H23C 103(5) . . ? H23B C23 H23C 101(5) . . ? Al2 C24 Sm2 88.53(14) . . ? Al2 C24 Sm1 175.6(2) . . ? Sm2 C24 Sm1 95.39(13) . . ? Al2 C24 H24A 97(4) . . ? Sm2 C24 H24A 133(4) . . ? Sm1 C24 H24A 79(4) . . ? Al2 C24 H24B 101(4) . . ? Sm2 C24 H24B 124(4) . . ? Sm1 C24 H24B 79(4) . . ? H24A C24 H24B 101(5) . . ? Al3 C31 H31A 113(7) . . ? Al3 C31 H31B 118(5) . . ? H31A C31 H31B 102(6) . . ? Al3 C32 Sm2 81.55(14) . . ? Al3 C32 H32A 93(3) . . ? Sm2 C32 H32A 174(3) . . ? Al3 C32 H32B 119(4) . . ? Sm2 C32 H32B 70(4) . . ? H32A C32 H32B 112(5) . . ? Al3 C32 H32C 123(4) . . ? Sm2 C32 H32C 82(4) . . ? H32A C32 H32C 102(5) . . ? H32B C32 H32C 106(5) . . ? Al1 C33 Al1 98.3(2) 4_565 . ? Al1 C33 Al3 102.52(17) 4_565 . ? Al1 C33 Al3 102.52(17) . . ? Al1 C33 Sm2 171.4(2) 4_565 . ? Al1 C33 Sm2 84.90(5) . . ? Al3 C33 Sm2 84.40(14) . . ? Al1 C33 Sm2 84.90(4) 4_565 4_565 ? Al1 C33 Sm2 171.4(2) . 4_565 ? Al3 C33 Sm2 84.40(14) . 4_565 ? Sm2 C33 Sm2 90.85(16) . 4_565 ? Al1 C33 Sm1 84.76(14) 4_565 . ? Al1 C33 Sm1 84.76(14) . . ? Al3 C33 Sm1 168.7(2) . . ? Sm2 C33 Sm1 87.65(13) . . ? Sm2 C33 Sm1 87.65(13) 4_565 . ? Sm2 C40 Sm2 88.9(2) 4_565 . ? Sm2 C40 H40A 119(4) 4_565 . ? Sm2 C40 H40A 119(4) . . ? Sm2 C40 H40B 152(6) 4_565 . ? Sm2 C40 H40B 81(5) . . ? H40A C40 H40B 89(6) . . ? C72 C71 C76 118.6 . . ? C72 C71 C77 126.2(7) . . ? C76 C71 C77 115.2(7) . . ? C72 C71 C76 111.6(3) . 4_565 ? C76 C71 C76 7.0(3) . 4_565 ? C77 C71 C76 122.2(6) . 4_565 ? C72 C71 C72 27.5(2) . 4_565 ? C76 C71 C72 91.2(2) . 4_565 ? C77 C71 C72 153.5(7) . 4_565 ? C76 C71 C72 84.2(4) 4_565 4_565 ? C72 C71 C71 67.8(2) . 4_565 ? C76 C71 C71 50.9(2) . 4_565 ? C77 C71 C71 165.7(6) . 4_565 ? C76 C71 C71 43.9(2) 4_565 4_565 ? C72 C71 C71 40.33(19) 4_565 4_565 ? C71 C72 C73 120.0 . . ? C71 C72 C71 71.9(3) . 4_565 ? C73 C72 C71 48.2(3) . 4_565 ? C71 C72 H72A 120.0 . . ? C73 C72 H72A 120.0 . . ? C71 C72 H72A 167.8 4_565 . ? C74 C73 C72 120.0 . . ? C74 C73 H73A 120.0 . . ? C72 C73 H73A 120.0 . . ? C75 C74 C73 120.0 . . ? C75 C74 H74A 120.0 . . ? C73 C74 H74A 120.0 . . ? C76 C75 C74 120.4 . . ? C76 C75 H75A 119.8 . . ? C74 C75 H75A 119.8 . . ? C75 C76 C71 121.0 . . ? C75 C76 H76A 119.5 . . ? C71 C76 H76A 119.5 . . ? C71 C77 H77A 109.5 . . ? C71 C77 H77B 109.5 . . ? H77A C77 H77B 109.5 . . ? C71 C77 H77C 109.5 . . ? H77A C77 H77C 109.5 . . ? H77B C77 H77C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 30.03 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.536 _refine_diff_density_min -1.093 _refine_diff_density_rms 0.121 #===END #===END data_compound4_CCDC_679434 _database_code_depnum_ccdc_archive 'CCDC 679434' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C23 H51 Al3 N3 Sm' _chemical_formula_weight 600.96 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' Sm Sm -0.1638 3.4418 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pna2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x+1/2, -y+1/2, z' '-x+1/2, y+1/2, z+1/2' _cell_length_a 35.417(4) _cell_length_b 17.3343(19) _cell_length_c 10.1016(11) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 6201.7(12) _cell_formula_units_Z 8 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used 900 _cell_measurement_theta_min 1 _cell_measurement_theta_max 22.5 _exptl_crystal_description 'transparent plates' _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.287 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2488 _exptl_absorpt_coefficient_mu 1.992 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6572 _exptl_absorpt_correction_T_max 0.9070 _exptl_absorpt_process_details ; Corrections were done with the SADABS program, utilizing the none merged raw data obtained from the integration process. Integration and final cell refinement were done with SAINT. SADABS reports ratio of Tmin/Tmax = 0.781426 ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'Omega and Phi scans' _diffrn_detector_area_resol_mean 80 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 70204 _diffrn_reflns_av_R_equivalents 0.0544 _diffrn_reflns_av_sigmaI/netI 0.0563 _diffrn_reflns_limit_h_min -49 _diffrn_reflns_limit_h_max 49 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.15 _diffrn_reflns_theta_max 30.04 _reflns_number_total 18019 _reflns_number_gt 16348 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker AXS, 2000)' _computing_cell_refinement 'SAINT (Bruker AXS, 2000)' _computing_data_reduction 'SAINT,SADABS (Bruker AXS, 2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ; ORTEP3,L.J. Farrugia, J. Appl. Cryst. (1997) 30, 565 ; _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0545P)^2^+3.9423P] 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 noref _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 0.020(11) _refine_ls_number_reflns 18019 _refine_ls_number_parameters 481 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0612 _refine_ls_R_factor_gt 0.0535 _refine_ls_wR_factor_ref 0.1187 _refine_ls_wR_factor_gt 0.1156 _refine_ls_goodness_of_fit_ref 1.149 _refine_ls_restrained_S_all 1.149 _refine_ls_shift/su_max 0.017 _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 Sm1 Sm 0.461185(7) 0.289138(13) 0.39367(3) 0.02228(6) Uani 1 1 d . . . Al1 Al 0.49374(6) 0.15455(10) 0.56302(19) 0.0339(4) Uani 1 1 d . . . Al2 Al 0.51950(5) 0.36808(10) 0.56963(16) 0.0260(3) Uani 1 1 d . . . Al3 Al 0.41541(5) 0.42318(11) 0.52449(18) 0.0300(4) Uani 1 1 d . . . N1 N 0.46807(15) 0.2152(3) 0.1669(5) 0.0303(10) Uani 1 1 d . . . N2 N 0.43668(13) 0.3346(3) 0.1595(4) 0.0258(9) Uani 1 1 d . . . N3 N 0.50199(13) 0.3297(3) 0.1881(5) 0.0273(9) Uani 1 1 d . . . C1 C 0.43653(17) 0.2562(3) 0.1005(6) 0.0337(12) Uani 1 1 d . . . H1A H 0.4407 0.2588 0.0037 0.040 Uiso 1 1 calc R . . H1B H 0.4122 0.2299 0.1177 0.040 Uiso 1 1 calc R . . C2 C 0.47159(16) 0.3736(3) 0.1241(6) 0.0283(11) Uani 1 1 d . . . H2A H 0.4714 0.4275 0.1563 0.034 Uiso 1 1 calc R . . H2B H 0.4750 0.3740 0.0268 0.034 Uiso 1 1 calc R . . C3 C 0.50332(18) 0.2525(3) 0.1291(6) 0.0346(13) Uani 1 1 d . . . H3A H 0.5054 0.2560 0.0315 0.042 Uiso 1 1 calc R . . H3B H 0.5252 0.2232 0.1634 0.042 Uiso 1 1 calc R . . C4 C 0.4673(2) 0.1317(4) 0.1310(8) 0.053(2) Uani 1 1 d . . . H4A H 0.4723 0.1260 0.0361 0.080 Uiso 1 1 calc . . . H4B H 0.4425 0.1101 0.1521 0.080 Uiso 1 1 calc . . . H4C H 0.4868 0.1043 0.1814 0.080 Uiso 1 1 calc . . . C5 C 0.40355(17) 0.3789(4) 0.1177(7) 0.0377(13) Uani 1 1 d . . . H5A H 0.4046 0.4305 0.1570 0.057 Uiso 1 1 calc . . . H5B H 0.3806 0.3525 0.1472 0.057 Uiso 1 1 calc . . . H5C H 0.4034 0.3832 0.0210 0.057 Uiso 1 1 calc . . . C6 C 0.53826(19) 0.3702(4) 0.1757(7) 0.0437(16) Uani 1 1 d . . . H6A H 0.5450 0.3748 0.0820 0.066 Uiso 1 1 calc . . . H6B H 0.5579 0.3411 0.2223 0.066 Uiso 1 1 calc . . . H6C H 0.5361 0.4218 0.2147 0.066 Uiso 1 1 calc . . . C7 C 0.4404(2) 0.1502(4) 0.4793(8) 0.0509(19) Uani 1 1 d . . . H7A H 0.4293 0.0992 0.4949 0.076 Uiso 1 1 calc . . . H7B H 0.4423 0.1594 0.3838 0.076 Uiso 1 1 calc . . . H7C H 0.4244 0.1898 0.5195 0.076 Uiso 1 1 calc . . . C8 C 0.5209(3) 0.0631(4) 0.4941(11) 0.068(3) Uani 1 1 d . . . H8A H 0.5455 0.0590 0.5376 0.103 Uiso 1 1 calc . . . H8B H 0.5245 0.0686 0.3984 0.103 Uiso 1 1 calc . . . H8C H 0.5060 0.0166 0.5123 0.103 Uiso 1 1 calc . . . C9 C 0.4833(2) 0.1577(5) 0.7541(8) 0.058(2) Uani 1 1 d . . . H9A H 0.4688 0.1119 0.7796 0.087 Uiso 1 1 calc . . . H9B H 0.4688 0.2042 0.7750 0.087 Uiso 1 1 calc . . . H9C H 0.5072 0.1586 0.8030 0.087 Uiso 1 1 calc . . . C10 C 0.51944(15) 0.2542(3) 0.5049(6) 0.0261(11) Uani 1 1 d . . . H10A H 0.5123 0.2586 0.4104 0.031 Uiso 1 1 calc R . . H10B H 0.5466 0.2403 0.5045 0.031 Uiso 1 1 calc R . . C11 C 0.56608(17) 0.4213(4) 0.5132(7) 0.0396(15) Uani 1 1 d . . . H11A H 0.5813 0.4340 0.5912 0.059 Uiso 1 1 calc . . . H11B H 0.5595 0.4688 0.4661 0.059 Uiso 1 1 calc . . . H11C H 0.5806 0.3875 0.4544 0.059 Uiso 1 1 calc . . . C12 C 0.5130(2) 0.3689(4) 0.7632(7) 0.0458(17) Uani 1 1 d . . . H12A H 0.5353 0.3461 0.8053 0.069 Uiso 1 1 calc . . . H12B H 0.4905 0.3387 0.7868 0.069 Uiso 1 1 calc . . . H12C H 0.5098 0.4221 0.7939 0.069 Uiso 1 1 calc . . . C13 C 0.47234(16) 0.4180(3) 0.4832(5) 0.0248(11) Uani 1 1 d . . . H13A H 0.4796 0.4729 0.4753 0.030 Uiso 1 1 calc R . . H13B H 0.4730 0.3977 0.3916 0.030 Uiso 1 1 calc R . . C14 C 0.3899(2) 0.5103(4) 0.4352(7) 0.0447(16) Uani 1 1 d . . . H14A H 0.3976 0.5588 0.4770 0.067 Uiso 1 1 calc . . . H14B H 0.3625 0.5041 0.4429 0.067 Uiso 1 1 calc . . . H14C H 0.3970 0.5110 0.3415 0.067 Uiso 1 1 calc . . . C15 C 0.4092(2) 0.4172(5) 0.7191(7) 0.053(2) Uani 1 1 d . . . H15A H 0.4278 0.4508 0.7620 0.080 Uiso 1 1 calc . . . H15B H 0.4131 0.3638 0.7484 0.080 Uiso 1 1 calc . . . H15C H 0.3837 0.4339 0.7433 0.080 Uiso 1 1 calc . . . C16 C 0.3891(2) 0.3237(4) 0.4594(7) 0.0459(16) Uani 1 1 d . . . H16A H 0.3617 0.3288 0.4711 0.069 Uiso 1 1 calc . . . H16B H 0.3982 0.2796 0.5108 0.069 Uiso 1 1 calc . . . H16C H 0.3948 0.3157 0.3655 0.069 Uiso 1 1 calc . . . Sm21 Sm 0.266028(7) 0.536109(14) 0.10691(3) 0.02350(6) Uani 1 1 d . . . Al21 Al 0.22859(6) 0.40026(11) 0.2612(2) 0.0356(4) Uani 1 1 d . . . Al22 Al 0.19819(5) 0.49570(12) -0.06478(18) 0.0324(4) Uani 1 1 d . . . Al23 Al 0.30043(5) 0.52248(10) -0.17624(18) 0.0275(3) Uani 1 1 d . . . N21 N 0.26640(16) 0.6192(3) 0.3268(5) 0.0345(11) Uani 1 1 d . . . N22 N 0.30687(16) 0.6611(3) 0.1606(6) 0.0451(14) Uani 1 1 d . . . N23 N 0.24147(16) 0.6766(3) 0.1386(5) 0.0352(12) Uani 1 1 d . . . C21 C 0.3034(2) 0.6546(4) 0.3026(9) 0.0498(19) Uani 1 1 d . . . H21A H 0.3048 0.7062 0.3446 0.060 Uiso 1 1 calc R . . H21B H 0.3239 0.6219 0.3390 0.060 Uiso 1 1 calc R . . C22 C 0.2780(2) 0.7141(3) 0.1107(9) 0.0526(19) Uani 1 1 d . . . H22A H 0.2812 0.7225 0.0144 0.063 Uiso 1 1 calc R . . H22B H 0.2797 0.7645 0.1564 0.063 Uiso 1 1 calc R . . C23 C 0.23699(19) 0.6720(4) 0.2828(6) 0.0358(14) Uani 1 1 d . . . H23A H 0.2403 0.7234 0.3238 0.043 Uiso 1 1 calc R . . H23B H 0.2117 0.6519 0.3061 0.043 Uiso 1 1 calc R . . C24 C 0.2618(2) 0.6000(4) 0.4681(6) 0.049(2) Uani 1 1 d . . . H24A H 0.2817 0.5642 0.4952 0.073 Uiso 1 1 calc . . . H24B H 0.2371 0.5758 0.4819 0.073 Uiso 1 1 calc . . . H24C H 0.2635 0.6472 0.5211 0.073 Uiso 1 1 calc . . . C25 C 0.3451(3) 0.6884(6) 0.1248(13) 0.088(4) Uani 1 1 d . . . H25A H 0.3472 0.6920 0.0283 0.131 Uiso 1 1 calc . . . H25B H 0.3639 0.6519 0.1583 0.131 Uiso 1 1 calc . . . H25C H 0.3495 0.7393 0.1642 0.131 Uiso 1 1 calc . . . C26 C 0.2094(3) 0.7197(4) 0.0767(8) 0.060(2) Uani 1 1 d . . . H26A H 0.2130 0.7216 -0.0194 0.091 Uiso 1 1 calc . . . H26B H 0.2086 0.7723 0.1122 0.091 Uiso 1 1 calc . . . H26C H 0.1856 0.6933 0.0969 0.091 Uiso 1 1 calc . . . C27 C 0.2855(2) 0.4268(4) 0.2893(6) 0.0370(14) Uani 1 1 d . . . H27A H 0.2986 0.4253 0.2040 0.056 Uiso 1 1 calc . . . H27B H 0.2968 0.3890 0.3495 0.056 Uiso 1 1 calc . . . H27C H 0.2877 0.4785 0.3276 0.056 Uiso 1 1 calc . . . C28 C 0.2296(2) 0.2979(4) 0.1764(10) 0.0544(19) Uani 1 1 d . . . H28A H 0.2425 0.3015 0.0909 0.082 Uiso 1 1 calc . . . H28B H 0.2036 0.2798 0.1624 0.082 Uiso 1 1 calc . . . H28C H 0.2430 0.2614 0.2336 0.082 Uiso 1 1 calc . . . C29 C 0.2034(3) 0.4028(5) 0.4353(8) 0.056(2) Uani 1 1 d . . . H29A H 0.2039 0.4556 0.4701 0.084 Uiso 1 1 calc . . . H29B H 0.2167 0.3684 0.4966 0.084 Uiso 1 1 calc . . . H29C H 0.1772 0.3857 0.4257 0.084 Uiso 1 1 calc . . . C30 C 0.20435(16) 0.4788(3) 0.1367(5) 0.0287(12) Uani 1 1 d . . . H30A H 0.2157 0.5280 0.1662 0.034 Uiso 1 1 calc R . . H30B H 0.1779 0.4807 0.1687 0.034 Uiso 1 1 calc R . . C31 C 0.1522(2) 0.5560(6) -0.0970(9) 0.067(2) Uani 1 1 d . . . H31A H 0.1545 0.6064 -0.0536 0.101 Uiso 1 1 calc . . . H31B H 0.1304 0.5284 -0.0610 0.101 Uiso 1 1 calc . . . H31C H 0.1489 0.5634 -0.1924 0.101 Uiso 1 1 calc . . . C32 C 0.1980(2) 0.3926(5) -0.1475(7) 0.0522(19) Uani 1 1 d . . . H32A H 0.2218 0.3661 -0.1272 0.078 Uiso 1 1 calc . . . H32B H 0.1954 0.3979 -0.2436 0.078 Uiso 1 1 calc . . . H32C H 0.1768 0.3624 -0.1127 0.078 Uiso 1 1 calc . . . C33 C 0.24676(16) 0.5537(3) -0.1261(6) 0.0273(11) Uani 1 1 d . . . H33A H 0.2381 0.5834 -0.2041 0.033 Uiso 1 1 calc R . . H33B H 0.2506 0.5926 -0.0556 0.033 Uiso 1 1 calc R . . C34 C 0.33182(18) 0.6087(4) -0.2466(8) 0.0420(15) Uani 1 1 d . . . H34A H 0.3316 0.6517 -0.1835 0.063 Uiso 1 1 calc . . . H34B H 0.3215 0.6261 -0.3315 0.063 Uiso 1 1 calc . . . H34C H 0.3578 0.5908 -0.2594 0.063 Uiso 1 1 calc . . . C35 C 0.2968(2) 0.4301(4) -0.2907(7) 0.0425(16) Uani 1 1 d . . . H35A H 0.2809 0.3912 -0.2474 0.064 Uiso 1 1 calc . . . H35B H 0.3220 0.4088 -0.3056 0.064 Uiso 1 1 calc . . . H35C H 0.2855 0.4445 -0.3758 0.064 Uiso 1 1 calc . . . C36 C 0.32847(17) 0.4852(3) -0.0056(6) 0.0318(12) Uani 1 1 d . . . H36A H 0.3311 0.5285 0.0561 0.048 Uiso 1 1 calc . . . H36B H 0.3535 0.4657 -0.0295 0.048 Uiso 1 1 calc . . . H36C H 0.3139 0.4440 0.0366 0.048 Uiso 1 1 calc . . . C41 C 0.1327(2) 0.6206(5) 0.4103(11) 0.063(2) Uani 1 1 d . . . C42 C 0.1516(3) 0.6149(5) 0.5282(10) 0.066(2) Uani 1 1 d . . . H42 H 0.1518 0.5671 0.5743 0.079 Uiso 1 1 calc R . . C43 C 0.1705(3) 0.6774(6) 0.5814(10) 0.075(3) Uani 1 1 d . . . H43 H 0.1834 0.6721 0.6633 0.090 Uiso 1 1 calc R . . C44 C 0.1707(2) 0.7454(6) 0.5189(12) 0.075(3) Uani 1 1 d . . . H44 H 0.1843 0.7877 0.5552 0.090 Uiso 1 1 calc R . . C45 C 0.1516(2) 0.7537(5) 0.4044(11) 0.061(2) Uani 1 1 d . . . H45 H 0.1512 0.8025 0.3617 0.073 Uiso 1 1 calc R . . C46 C 0.1326(2) 0.6916(5) 0.3477(9) 0.062(2) Uani 1 1 d . . . H46 H 0.1195 0.6980 0.2663 0.075 Uiso 1 1 calc R . . C47 C 0.1139(3) 0.5518(7) 0.3539(19) 0.119(6) Uani 1 1 d . . . H47A H 0.1017 0.5656 0.2700 0.178 Uiso 1 1 calc . . . H47B H 0.0948 0.5329 0.4162 0.178 Uiso 1 1 calc . . . H47C H 0.1326 0.5112 0.3382 0.178 Uiso 1 1 calc . . . C51 C 0.5918 0.1606 -0.0412 0.080 Uiso 1 1 d D . . C52 C 0.6091 0.2146 0.0403 0.080 Uiso 1 1 d . . . H52 H 0.6205 0.2591 0.0029 0.096 Uiso 1 1 calc R . . C53 C 0.6097 0.2035 0.1765 0.080 Uiso 1 1 d . . . H53 H 0.6216 0.2404 0.2323 0.096 Uiso 1 1 calc R . . C54 C 0.5930 0.1383 0.2313 0.080 Uiso 1 1 d . . . H54 H 0.5934 0.1307 0.3244 0.096 Uiso 1 1 calc R . . C55 C 0.5756 0.0843 0.1497 0.080 Uiso 1 1 d . . . H55 H 0.5642 0.0398 0.1871 0.096 Uiso 1 1 calc R . . C56 C 0.5750 0.0955 0.0135 0.080 Uiso 1 1 d . . . H56 H 0.5632 0.0585 -0.0422 0.096 Uiso 1 1 calc R . . C57 C 0.5939(3) 0.1943(6) -0.1798(5) 0.080 Uiso 1 1 d D . . H57A H 0.5831 0.1576 -0.2431 0.120 Uiso 1 1 calc . . . H57B H 0.6203 0.2042 -0.2027 0.120 Uiso 1 1 calc . . . H57C H 0.5797 0.2427 -0.1829 0.120 Uiso 1 1 calc . . . 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 Sm1 0.02818(12) 0.01858(10) 0.02008(10) -0.00179(11) -0.00240(11) -0.00181(10) Al1 0.0448(11) 0.0214(8) 0.0355(9) 0.0075(7) -0.0018(8) 0.0014(7) Al2 0.0286(8) 0.0259(8) 0.0236(8) -0.0027(6) -0.0021(6) -0.0036(6) Al3 0.0290(9) 0.0316(9) 0.0294(9) -0.0056(7) 0.0048(7) 0.0028(7) N1 0.045(3) 0.022(2) 0.024(2) -0.0053(18) -0.010(2) 0.006(2) N2 0.030(2) 0.025(2) 0.022(2) -0.0017(17) -0.0020(18) 0.0037(18) N3 0.029(2) 0.029(2) 0.024(2) -0.0021(18) -0.0007(18) -0.0007(19) C1 0.040(3) 0.038(3) 0.023(2) -0.004(3) -0.011(3) 0.002(2) C2 0.040(3) 0.025(2) 0.020(3) 0.002(2) 0.002(2) 0.002(2) C3 0.051(4) 0.034(3) 0.019(3) -0.002(2) 0.000(2) 0.016(3) C4 0.083(5) 0.026(3) 0.050(4) -0.011(3) -0.007(4) 0.010(3) C5 0.038(3) 0.041(3) 0.034(3) 0.003(3) -0.005(3) 0.008(2) C6 0.038(3) 0.054(4) 0.040(4) 0.002(3) 0.013(3) -0.009(3) C7 0.060(5) 0.031(3) 0.061(5) 0.011(3) -0.011(4) -0.009(3) C8 0.082(6) 0.028(3) 0.095(7) 0.008(4) 0.000(6) 0.020(4) C9 0.061(5) 0.075(6) 0.039(4) 0.025(4) -0.006(4) -0.019(4) C10 0.023(3) 0.023(3) 0.033(3) 0.002(2) -0.006(2) 0.004(2) C11 0.026(3) 0.048(4) 0.045(4) 0.003(3) -0.006(3) -0.011(3) C12 0.061(5) 0.046(4) 0.030(3) -0.003(3) -0.008(3) -0.002(3) C13 0.035(3) 0.021(2) 0.018(2) -0.0004(19) 0.003(2) 0.000(2) C14 0.038(4) 0.042(4) 0.054(4) -0.005(3) -0.010(3) 0.011(3) C15 0.054(5) 0.071(5) 0.035(4) -0.007(4) 0.022(3) -0.007(4) C16 0.049(4) 0.049(4) 0.040(4) -0.009(3) 0.004(3) 0.002(3) Sm21 0.02685(12) 0.01882(10) 0.02482(11) -0.00323(11) 0.00009(12) 0.00326(9) Al21 0.0445(11) 0.0255(9) 0.0369(10) 0.0032(7) 0.0051(8) -0.0001(8) Al22 0.0241(8) 0.0419(10) 0.0311(9) -0.0023(7) -0.0012(7) 0.0007(7) Al23 0.0281(8) 0.0259(8) 0.0286(8) 0.0004(7) 0.0043(7) 0.0059(6) N21 0.047(3) 0.028(2) 0.029(3) -0.009(2) -0.004(2) 0.007(2) N22 0.041(3) 0.034(3) 0.060(4) -0.015(3) 0.014(3) -0.003(2) N23 0.052(3) 0.023(2) 0.031(3) -0.0022(18) -0.001(2) 0.011(2) C21 0.040(4) 0.034(3) 0.076(5) -0.026(3) -0.019(4) 0.009(3) C22 0.086(5) 0.023(3) 0.049(4) -0.008(3) 0.016(4) 0.000(3) C23 0.050(4) 0.030(3) 0.028(3) -0.009(2) 0.000(3) 0.010(3) C24 0.081(6) 0.047(4) 0.018(3) -0.006(3) -0.007(3) 0.021(4) C25 0.069(6) 0.079(6) 0.115(9) -0.055(7) 0.039(6) -0.035(5) C26 0.091(6) 0.046(4) 0.045(4) -0.006(3) -0.012(4) 0.039(4) C27 0.050(4) 0.026(3) 0.035(3) -0.001(2) -0.001(3) 0.003(3) C28 0.058(5) 0.032(3) 0.073(5) -0.001(4) -0.005(4) -0.002(3) C29 0.075(6) 0.050(4) 0.043(4) 0.014(3) 0.016(4) 0.007(4) C30 0.028(3) 0.029(3) 0.030(3) -0.004(2) 0.002(2) -0.001(2) C31 0.034(4) 0.115(7) 0.053(5) 0.026(5) -0.001(4) 0.010(4) C32 0.064(5) 0.057(4) 0.036(4) -0.014(3) 0.008(3) -0.018(4) C33 0.031(3) 0.029(2) 0.022(3) 0.001(2) -0.004(2) 0.011(2) C34 0.028(3) 0.043(4) 0.055(4) 0.013(3) 0.003(3) 0.001(3) C35 0.046(4) 0.049(4) 0.033(3) -0.014(3) 0.004(3) 0.013(3) C36 0.032(3) 0.031(3) 0.032(3) -0.001(2) 0.002(2) 0.010(2) C41 0.042(4) 0.058(5) 0.089(7) -0.023(5) 0.015(5) 0.000(3) C42 0.080(6) 0.051(5) 0.066(6) 0.015(4) 0.011(5) 0.010(4) C43 0.078(6) 0.085(7) 0.063(6) -0.017(5) 0.003(5) 0.022(5) C44 0.043(5) 0.075(6) 0.106(8) -0.044(6) 0.001(5) 0.003(4) C45 0.051(4) 0.046(4) 0.086(6) 0.012(5) 0.015(5) 0.011(3) C46 0.047(4) 0.084(6) 0.057(5) 0.004(4) 0.009(4) 0.028(4) C47 0.063(7) 0.110(9) 0.184(16) -0.063(10) 0.012(8) -0.018(6) _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 Sm1 C10 2.426(5) . ? Sm1 C13 2.441(5) . ? Sm1 N3 2.626(5) . ? Sm1 N1 2.636(5) . ? Sm1 N2 2.640(5) . ? Sm1 C7 2.663(7) . ? Sm1 C16 2.706(7) . ? Sm1 Al2 3.0493(16) . ? Sm1 Al1 3.1142(18) . ? Sm1 Al3 3.1262(18) . ? Al1 C9 1.966(8) . ? Al1 C8 1.979(8) . ? Al1 C10 2.038(6) . ? Al1 C7 2.070(8) . ? Al2 C12 1.969(7) . ? Al2 C11 1.974(6) . ? Al2 C13 2.074(6) . ? Al2 C10 2.080(5) . ? Al3 C14 1.977(7) . ? Al3 C15 1.981(7) . ? Al3 C13 2.061(6) . ? Al3 C16 2.067(8) . ? N1 C3 1.457(8) . ? N1 C1 1.484(7) . ? N1 C4 1.492(8) . ? N2 C2 1.454(7) . ? N2 C5 1.464(7) . ? N2 C1 1.482(7) . ? N3 C3 1.465(7) . ? N3 C2 1.469(7) . ? N3 C6 1.469(8) . ? Sm21 C30 2.419(6) . ? Sm21 C33 2.469(5) . ? Sm21 N23 2.606(5) . ? Sm21 C36 2.638(6) . ? Sm21 N21 2.647(5) . ? Sm21 N22 2.661(6) . ? Sm21 C27 2.731(6) . ? Sm21 Al22 3.0448(18) . ? Sm21 Al23 3.1179(18) . ? Sm21 Al21 3.1196(19) . ? Al21 C28 1.971(8) . ? Al21 C29 1.972(8) . ? Al21 C30 2.043(6) . ? Al21 C27 2.086(7) . ? Al22 C31 1.962(8) . ? Al22 C32 1.974(8) . ? Al22 C30 2.067(6) . ? Al22 C33 2.086(6) . ? Al23 C35 1.980(7) . ? Al23 C34 1.994(7) . ? Al23 C33 2.040(6) . ? Al23 C36 2.092(6) . ? N21 C23 1.456(8) . ? N21 C21 1.469(9) . ? N21 C24 1.475(8) . ? N22 C21 1.444(11) . ? N22 C22 1.464(10) . ? N22 C25 1.479(10) . ? N23 C23 1.467(8) . ? N23 C22 1.475(9) . ? N23 C26 1.496(9) . ? C41 C42 1.370(14) . ? C41 C46 1.384(13) . ? C41 C47 1.482(14) . ? C42 C43 1.382(14) . ? C43 C44 1.336(15) . ? C44 C45 1.347(14) . ? C45 C46 1.394(13) . ? C51 C52 1.3900 . ? C51 C56 1.3900 . ? C51 C57 1.518(2) . ? C52 C53 1.3900 . ? C53 C54 1.3900 . ? C54 C55 1.3900 . ? C55 C56 1.3900 . ? 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 C10 Sm1 C13 85.38(18) . . ? C10 Sm1 N3 88.00(17) . . ? C13 Sm1 N3 87.66(16) . . ? C10 Sm1 N1 101.67(17) . . ? C13 Sm1 N1 138.72(17) . . ? N3 Sm1 N1 52.54(15) . . ? C10 Sm1 N2 140.27(17) . . ? C13 Sm1 N2 96.45(16) . . ? N3 Sm1 N2 52.59(15) . . ? N1 Sm1 N2 52.88(14) . . ? C10 Sm1 C7 81.9(2) . . ? C13 Sm1 C7 138.7(2) . . ? N3 Sm1 C7 130.6(2) . . ? N1 Sm1 C7 82.4(2) . . ? N2 Sm1 C7 118.0(2) . . ? C10 Sm1 C16 138.1(2) . . ? C13 Sm1 C16 81.9(2) . . ? N3 Sm1 C16 130.9(2) . . ? N1 Sm1 C16 114.09(19) . . ? N2 Sm1 C16 81.00(19) . . ? C7 Sm1 C16 82.0(2) . . ? C10 Sm1 Al2 42.80(13) . . ? C13 Sm1 Al2 42.60(13) . . ? N3 Sm1 Al2 88.18(11) . . ? N1 Sm1 Al2 131.46(12) . . ? N2 Sm1 Al2 127.67(11) . . ? C7 Sm1 Al2 113.81(18) . . ? C16 Sm1 Al2 113.38(16) . . ? C10 Sm1 Al1 40.85(13) . . ? C13 Sm1 Al1 114.95(13) . . ? N3 Sm1 Al1 115.54(11) . . ? N1 Sm1 Al1 94.54(11) . . ? N2 Sm1 Al1 146.86(11) . . ? C7 Sm1 Al1 41.08(18) . . ? C16 Sm1 Al1 112.37(17) . . ? Al2 Sm1 Al1 76.42(5) . . ? C10 Sm1 Al3 115.53(14) . . ? C13 Sm1 Al3 41.20(13) . . ? N3 Sm1 Al3 114.89(11) . . ? N1 Sm1 Al3 140.94(11) . . ? N2 Sm1 Al3 89.23(10) . . ? C7 Sm1 Al3 113.1(2) . . ? C16 Sm1 Al3 40.73(16) . . ? Al2 Sm1 Al3 76.78(5) . . ? Al1 Sm1 Al3 121.10(5) . . ? C9 Al1 C8 117.3(4) . . ? C9 Al1 C10 110.1(3) . . ? C8 Al1 C10 111.1(3) . . ? C9 Al1 C7 103.4(4) . . ? C8 Al1 C7 105.6(4) . . ? C10 Al1 C7 108.7(3) . . ? C9 Al1 Sm1 116.7(3) . . ? C8 Al1 Sm1 125.9(3) . . ? C10 Al1 Sm1 51.13(15) . . ? C7 Al1 Sm1 57.68(19) . . ? C12 Al2 C11 112.4(3) . . ? C12 Al2 C13 108.7(3) . . ? C11 Al2 C13 110.9(3) . . ? C12 Al2 C10 108.6(3) . . ? C11 Al2 C10 110.7(3) . . ? C13 Al2 C10 105.2(2) . . ? C12 Al2 Sm1 120.2(2) . . ? C11 Al2 Sm1 127.4(2) . . ? C13 Al2 Sm1 52.85(15) . . ? C10 Al2 Sm1 52.41(15) . . ? C14 Al3 C15 116.3(4) . . ? C14 Al3 C13 112.8(3) . . ? C15 Al3 C13 107.8(3) . . ? C14 Al3 C16 106.6(3) . . ? C15 Al3 C16 102.8(3) . . ? C13 Al3 C16 109.9(3) . . ? C14 Al3 Sm1 127.7(2) . . ? C15 Al3 Sm1 115.9(3) . . ? C13 Al3 Sm1 51.28(15) . . ? C16 Al3 Sm1 58.7(2) . . ? C3 N1 C1 108.3(5) . . ? C3 N1 C4 112.4(5) . . ? C1 N1 C4 110.0(5) . . ? C3 N1 Sm1 95.2(3) . . ? C1 N1 Sm1 95.2(3) . . ? C4 N1 Sm1 132.9(4) . . ? C2 N2 C5 111.5(5) . . ? C2 N2 C1 109.3(4) . . ? C5 N2 C1 111.2(4) . . ? C2 N2 Sm1 94.6(3) . . ? C5 N2 Sm1 132.7(4) . . ? C1 N2 Sm1 95.0(3) . . ? C3 N3 C2 108.5(4) . . ? C3 N3 C6 112.0(5) . . ? C2 N3 C6 110.8(5) . . ? C3 N3 Sm1 95.5(3) . . ? C2 N3 Sm1 94.8(3) . . ? C6 N3 Sm1 132.5(4) . . ? N2 C1 N1 104.8(4) . . ? N2 C2 N3 105.9(4) . . ? N1 C3 N3 105.7(4) . . ? Al1 C7 Sm1 81.2(2) . . ? Al1 C10 Al2 135.6(3) . . ? Al1 C10 Sm1 88.0(2) . . ? Al2 C10 Sm1 84.79(18) . . ? Al3 C13 Al2 136.2(3) . . ? Al3 C13 Sm1 87.5(2) . . ? Al2 C13 Sm1 84.55(19) . . ? Al3 C16 Sm1 80.6(2) . . ? C30 Sm21 C33 85.38(19) . . ? C30 Sm21 N23 93.86(18) . . ? C33 Sm21 N23 84.80(17) . . ? C30 Sm21 C36 132.32(19) . . ? C33 Sm21 C36 82.10(18) . . ? N23 Sm21 C36 130.17(18) . . ? C30 Sm21 N21 97.11(18) . . ? C33 Sm21 N21 137.21(17) . . ? N23 Sm21 N21 52.42(16) . . ? C36 Sm21 N21 122.62(18) . . ? C30 Sm21 N22 143.15(17) . . ? C33 Sm21 N22 104.1(2) . . ? N23 Sm21 N22 52.80(17) . . ? C36 Sm21 N22 84.51(18) . . ? N21 Sm21 N22 51.92(18) . . ? C30 Sm21 C27 81.9(2) . . ? C33 Sm21 C27 142.97(19) . . ? N23 Sm21 C27 130.53(17) . . ? C36 Sm21 C27 81.2(2) . . ? N21 Sm21 C27 79.06(18) . . ? N22 Sm21 C27 106.9(2) . . ? C30 Sm21 Al22 42.57(13) . . ? C33 Sm21 Al22 42.90(14) . . ? N23 Sm21 Al22 91.24(13) . . ? C36 Sm21 Al22 109.83(14) . . ? N21 Sm21 Al22 127.37(13) . . ? N22 Sm21 Al22 137.09(15) . . ? C27 Sm21 Al22 115.05(15) . . ? C30 Sm21 Al23 115.83(13) . . ? C33 Sm21 Al23 40.80(13) . . ? N23 Sm21 Al23 108.29(12) . . ? C36 Sm21 Al23 41.58(14) . . ? N21 Sm21 Al23 144.00(13) . . ? N22 Sm21 Al23 92.08(14) . . ? C27 Sm21 Al23 117.89(14) . . ? Al22 Sm21 Al23 76.61(5) . . ? C30 Sm21 Al21 40.88(14) . . ? C33 Sm21 Al21 116.87(14) . . ? N23 Sm21 Al21 120.15(13) . . ? C36 Sm21 Al21 108.61(14) . . ? N21 Sm21 Al21 89.63(13) . . ? N22 Sm21 Al21 138.06(15) . . ? C27 Sm21 Al21 41.10(15) . . ? Al22 Sm21 Al21 77.03(5) . . ? Al23 Sm21 Al21 124.55(5) . . ? C28 Al21 C29 114.6(4) . . ? C28 Al21 C30 109.9(3) . . ? C29 Al21 C30 110.1(3) . . ? C28 Al21 C27 103.9(3) . . ? C29 Al21 C27 108.1(3) . . ? C30 Al21 C27 110.1(3) . . ? C28 Al21 Sm21 117.1(3) . . ? C29 Al21 Sm21 128.4(3) . . ? C30 Al21 Sm21 50.80(17) . . ? C27 Al21 Sm21 59.42(18) . . ? C31 Al22 C32 114.2(4) . . ? C31 Al22 C30 109.0(3) . . ? C32 Al22 C30 106.8(3) . . ? C31 Al22 C33 112.2(3) . . ? C32 Al22 C33 108.3(3) . . ? C30 Al22 C33 105.9(2) . . ? C31 Al22 Sm21 128.8(3) . . ? C32 Al22 Sm21 116.9(3) . . ? C30 Al22 Sm21 52.32(16) . . ? C33 Al22 Sm21 53.67(16) . . ? C35 Al23 C34 115.8(3) . . ? C35 Al23 C33 107.4(3) . . ? C34 Al23 C33 114.1(3) . . ? C35 Al23 C36 105.2(3) . . ? C34 Al23 C36 105.1(3) . . ? C33 Al23 C36 108.6(2) . . ? C35 Al23 Sm21 124.8(2) . . ? C34 Al23 Sm21 119.2(2) . . ? C33 Al23 Sm21 52.26(16) . . ? C36 Al23 Sm21 56.83(16) . . ? C23 N21 C21 109.0(5) . . ? C23 N21 C24 111.0(6) . . ? C21 N21 C24 110.7(6) . . ? C23 N21 Sm21 94.7(3) . . ? C21 N21 Sm21 95.3(4) . . ? C24 N21 Sm21 133.5(4) . . ? C21 N22 C22 109.4(6) . . ? C21 N22 C25 110.2(7) . . ? C22 N22 C25 110.7(7) . . ? C21 N22 Sm21 95.4(4) . . ? C22 N22 Sm21 93.5(4) . . ? C25 N22 Sm21 135.1(5) . . ? C23 N23 C22 108.0(6) . . ? C23 N23 C26 111.1(5) . . ? C22 N23 C26 111.5(6) . . ? C23 N23 Sm21 96.1(3) . . ? C22 N23 Sm21 95.5(3) . . ? C26 N23 Sm21 131.9(4) . . ? N22 C21 N21 105.8(5) . . ? N22 C22 N23 105.7(5) . . ? N21 C23 N23 105.1(5) . . ? Al21 C27 Sm21 79.5(2) . . ? Al21 C30 Al22 138.2(3) . . ? Al21 C30 Sm21 88.3(2) . . ? Al22 C30 Sm21 85.1(2) . . ? Al23 C33 Al22 135.5(3) . . ? Al23 C33 Sm21 86.93(19) . . ? Al22 C33 Sm21 83.4(2) . . ? Al23 C36 Sm21 81.59(19) . . ? C42 C41 C46 117.7(9) . . ? C42 C41 C47 119.8(11) . . ? C46 C41 C47 122.6(12) . . ? C41 C42 C43 121.1(9) . . ? C44 C43 C42 120.8(10) . . ? C43 C44 C45 119.8(9) . . ? C44 C45 C46 120.9(9) . . ? C41 C46 C45 119.8(9) . . ? C52 C51 C56 120.0 . . ? C52 C51 C57 105.4(4) . . ? C56 C51 C57 134.4(4) . . ? C53 C52 C51 120.0 . . ? C54 C53 C52 120.0 . . ? C53 C54 C55 120.0 . . ? C54 C55 C56 120.0 . . ? C55 C56 C51 120.0 . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 30.04 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 2.537 _refine_diff_density_min -1.451 _refine_diff_density_rms 0.137 # Attachment 'Compound_all.CIF' data_compound1_CCDC_711481 _database_code_depnum_ccdc_archive 'CCDC 711481' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C17 H47 Al3 La N3' _chemical_formula_sum 'C17 H47 Al3 La N3' _chemical_formula_weight 513.43 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' La La -0.2871 2.4523 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' _cell_length_a 10.8824(6) _cell_length_b 14.4357(14) _cell_length_c 16.9846(9) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2668.2(3) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 90 _cell_measurement_theta_min 3.070 _cell_measurement_theta_max 17.823 _exptl_crystal_description column _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.17 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.278 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1064 _exptl_absorpt_coefficient_mu 1.705 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7604 _exptl_absorpt_correction_T_max 0.9046 _exptl_absorpt_process_details 'SADABS - Bruker Nonius - V2.10' _exptl_special_details ; ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 26594 _diffrn_reflns_av_R_equivalents 0.0292 _diffrn_reflns_av_sigmaI/netI 0.0315 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.63 _diffrn_reflns_theta_max 27.50 _reflns_number_total 6091 _reflns_number_gt 5386 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect, Bruker AXS, 2004' _computing_cell_refinement 'Dirax/lsq (Duisenberg & Schreurs, 1989-2000)' _computing_data_reduction 'EVALCCD (Duisenberg,1998,Thesis.Utrecht University.' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL-PLUS (1990)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0100P)^2^+0.3138P] 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 0.001(8) _refine_ls_number_reflns 6091 _refine_ls_number_parameters 394 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0283 _refine_ls_R_factor_gt 0.0197 _refine_ls_wR_factor_ref 0.0352 _refine_ls_wR_factor_gt 0.0332 _refine_ls_goodness_of_fit_ref 1.026 _refine_ls_restrained_S_all 1.026 _refine_ls_shift/su_max 0.002 _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 La1 La 0.411844(8) 0.001689(11) 0.370323(5) 0.01702(3) Uani 1 1 d . . . Al1 Al 0.17150(6) -0.13270(5) 0.37195(4) 0.02386(14) Uani 1 1 d . . . Al2 Al 0.17421(6) 0.11684(5) 0.30808(4) 0.02521(16) Uani 1 1 d . . . Al3 Al 0.57807(8) -0.05201(5) 0.21300(4) 0.02912(16) Uani 1 1 d . . . N1 N 0.60699(16) -0.05197(14) 0.46646(10) 0.0227(4) Uani 1 1 d . . . N2 N 0.47218(17) 0.05435(14) 0.52608(10) 0.0223(4) Uani 1 1 d . . . N3 N 0.61110(16) 0.10579(14) 0.42997(11) 0.0238(4) Uani 1 1 d . . . C1 C 0.5491(2) -0.02640(17) 0.54209(13) 0.0266(6) Uani 1 1 d . . . H1A H 0.501(2) -0.0747(17) 0.5567(13) 0.026(7) Uiso 1 1 d . . . H1B H 0.6110(17) -0.0180(16) 0.5843(12) 0.025(6) Uiso 1 1 d . . . C2 C 0.5529(2) 0.13169(18) 0.50479(13) 0.0244(5) Uani 1 1 d . . . H2A H 0.506(2) 0.1839(15) 0.4954(11) 0.012(5) Uiso 1 1 d . . . H2B H 0.616(2) 0.1395(16) 0.5470(13) 0.024(6) Uiso 1 1 d . . . C3 C 0.6882(2) 0.02394(16) 0.44273(14) 0.0280(6) Uani 1 1 d . . . H3A H 0.755(2) 0.0333(16) 0.4803(13) 0.029(7) Uiso 1 1 d . . . H3B H 0.7286(16) 0.008(2) 0.3955(11) 0.016(5) Uiso 1 1 d . . . C4 C 0.6762(3) -0.1389(2) 0.47462(18) 0.0346(6) Uani 1 1 d . . . H4A H 0.736(3) -0.130(2) 0.5153(16) 0.048(8) Uiso 1 1 d . . . H4B H 0.712(3) -0.154(2) 0.4234(17) 0.044(9) Uiso 1 1 d . . . H4C H 0.623(2) -0.1862(19) 0.4901(14) 0.030(7) Uiso 1 1 d . . . C5 C 0.3982(3) 0.0781(2) 0.59621(14) 0.0345(6) Uani 1 1 d . . . H5A H 0.341(2) 0.0265(19) 0.6080(14) 0.049(8) Uiso 1 1 d . . . H5B H 0.341(3) 0.132(2) 0.5831(14) 0.047(8) Uiso 1 1 d . . . H5C H 0.450(2) 0.0902(18) 0.6417(15) 0.039(7) Uiso 1 1 d . . . C6 C 0.6852(3) 0.1835(2) 0.39936(18) 0.0361(6) Uani 1 1 d . . . H6A H 0.745(3) 0.201(2) 0.4399(16) 0.046(8) Uiso 1 1 d . . . H6B H 0.627(2) 0.2352(19) 0.3916(15) 0.039(7) Uiso 1 1 d . . . H6C H 0.727(2) 0.1639(19) 0.3478(15) 0.035(7) Uiso 1 1 d . . . C7 C 0.2998(3) -0.1306(2) 0.46188(16) 0.0301(6) Uani 1 1 d . . . H7A H 0.294(2) -0.073(2) 0.4999(15) 0.040(7) Uiso 1 1 d . . . H7B H 0.384(3) -0.154(2) 0.4606(15) 0.045(8) Uiso 1 1 d . . . H7C H 0.262(3) -0.177(2) 0.4892(19) 0.061(10) Uiso 1 1 d . . . C8 C 0.1845(2) -0.25270(18) 0.31562(15) 0.0364(6) Uani 1 1 d . . . H8A H 0.2639 -0.2562 0.2886 0.055 Uiso 0.50 1 calc PR . . H8B H 0.1180 -0.2576 0.2769 0.055 Uiso 0.50 1 calc PR . . H8C H 0.1779 -0.3036 0.3535 0.055 Uiso 0.50 1 calc PR . . H8D H 0.1093 -0.2887 0.3241 0.055 Uiso 0.50 1 calc PR . . H8E H 0.2552 -0.2874 0.3358 0.055 Uiso 0.50 1 calc PR . . H8F H 0.1953 -0.2413 0.2592 0.055 Uiso 0.50 1 calc PR . . C9 C 0.0105(3) -0.1140(3) 0.4228(2) 0.0431(8) Uani 1 1 d . . . H9A H -0.055(3) -0.097(3) 0.386(2) 0.092(12) Uiso 1 1 d . . . H9B H 0.004(3) -0.064(2) 0.4571(19) 0.064(10) Uiso 1 1 d . . . H9C H -0.013(3) -0.161(2) 0.4522(18) 0.056(10) Uiso 1 1 d . . . C10 C 0.2084(2) -0.02267(15) 0.29881(12) 0.0232(6) Uani 1 1 d . . . H10A H 0.121(2) -0.0284(18) 0.2755(13) 0.038(7) Uiso 1 1 d . . . H10B H 0.264(2) -0.0366(19) 0.2583(15) 0.044(8) Uiso 1 1 d . . . C11 C 0.0175(2) 0.1374(2) 0.36380(19) 0.0376(6) Uani 1 1 d . . . H11A H -0.001(3) 0.193(3) 0.368(2) 0.082(12) Uiso 1 1 d . . . H11B H 0.024(2) 0.118(2) 0.4206(17) 0.033(8) Uiso 1 1 d . . . H11C H -0.047(3) 0.098(2) 0.3384(15) 0.050(9) Uiso 1 1 d . . . C12 C 0.1844(3) 0.1793(2) 0.20448(17) 0.0399(7) Uani 1 1 d . . . H12A H 0.115(4) 0.168(3) 0.177(2) 0.085(13) Uiso 1 1 d . . . H12B H 0.252(3) 0.161(3) 0.1742(19) 0.068(11) Uiso 1 1 d . . . H12C H 0.196(3) 0.244(3) 0.202(2) 0.082(12) Uiso 1 1 d . . . C13 C 0.3040(2) 0.17421(17) 0.38378(16) 0.0294(5) Uani 1 1 d . . . H13A H 0.269(2) 0.236(2) 0.3833(15) 0.046(8) Uiso 1 1 d . . . H13B H 0.392(2) 0.1915(17) 0.3753(14) 0.037(7) Uiso 1 1 d . . . H13C H 0.303(3) 0.153(2) 0.4370(17) 0.040(9) Uiso 1 1 d . . . C14 C 0.5150(3) 0.0787(2) 0.23750(16) 0.0320(6) Uani 1 1 d . . . H14A H 0.546(2) 0.108(2) 0.1902(16) 0.047(8) Uiso 1 1 d . . . H14B H 0.540(3) 0.118(2) 0.2795(18) 0.059(11) Uiso 1 1 d . . . H14C H 0.437(3) 0.0914(17) 0.2307(13) 0.028(7) Uiso 1 1 d . . . C15 C 0.5132(3) -0.0815(2) 0.10762(17) 0.0445(7) Uani 1 1 d . . . H15A H 0.539(3) -0.038(3) 0.076(2) 0.091(15) Uiso 1 1 d . . . H15B H 0.430(3) -0.085(2) 0.1059(16) 0.055(9) Uiso 1 1 d . . . H15C H 0.544(2) -0.135(2) 0.0830(15) 0.042(8) Uiso 1 1 d . . . C16 C 0.7596(2) -0.0524(3) 0.22448(18) 0.0391(7) Uani 1 1 d . . . H16A H 0.790(3) -0.100(2) 0.1926(19) 0.069(10) Uiso 1 1 d . . . H16B H 0.792(3) -0.074(2) 0.2790(18) 0.057(9) Uiso 1 1 d . . . H16C H 0.787(3) 0.009(3) 0.2153(16) 0.059(9) Uiso 1 1 d . . . C17 C 0.5088(3) -0.1482(2) 0.28933(16) 0.0313(6) Uani 1 1 d . . . H17A H 0.422(3) -0.167(2) 0.2876(15) 0.050(8) Uiso 1 1 d . . . H17B H 0.532(3) -0.156(2) 0.3342(18) 0.056(10) Uiso 1 1 d . . . H17C H 0.547(2) -0.2047(17) 0.2649(13) 0.026(6) 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 La1 0.01601(5) 0.01789(5) 0.01714(5) 0.00083(8) -0.00060(4) -0.00034(8) Al1 0.0202(3) 0.0250(4) 0.0264(3) -0.0053(3) 0.0004(3) -0.0040(3) Al2 0.0225(3) 0.0278(4) 0.0254(4) 0.0004(3) -0.0042(3) 0.0043(3) Al3 0.0332(4) 0.0306(4) 0.0236(3) -0.0002(3) 0.0079(3) 0.0005(4) N1 0.0184(10) 0.0227(10) 0.0269(9) 0.0021(8) -0.0022(7) 0.0010(8) N2 0.0247(11) 0.0235(11) 0.0187(9) -0.0024(8) 0.0004(7) -0.0011(9) N3 0.0195(10) 0.0233(11) 0.0286(10) 0.0036(9) 0.0000(8) -0.0025(8) C1 0.0293(13) 0.0293(17) 0.0212(11) 0.0047(9) -0.0051(9) -0.0025(10) C2 0.0243(13) 0.0243(14) 0.0247(12) -0.0025(10) -0.0038(9) -0.0018(10) C3 0.0186(11) 0.0335(18) 0.0320(12) 0.0029(10) -0.0016(10) -0.0006(9) C4 0.0298(14) 0.0287(15) 0.0455(17) 0.0030(13) -0.0049(14) 0.0089(13) C5 0.0359(15) 0.0441(17) 0.0236(12) -0.0028(11) 0.0057(11) -0.0026(14) C6 0.0253(14) 0.0337(16) 0.0492(17) 0.0099(13) 0.0004(13) -0.0099(12) C7 0.0289(16) 0.0322(16) 0.0293(14) 0.0073(13) -0.0008(10) -0.0119(12) C8 0.0365(15) 0.0298(15) 0.0430(14) -0.0104(12) 0.0025(12) -0.0071(12) C9 0.0299(16) 0.045(2) 0.055(2) -0.0082(18) 0.0127(14) -0.0034(14) C10 0.0199(11) 0.0275(17) 0.0223(10) -0.0033(9) -0.0016(8) 0.0005(9) C11 0.0326(15) 0.0402(17) 0.0401(18) -0.0041(15) 0.0004(12) 0.0086(13) C12 0.0431(18) 0.0394(19) 0.0372(16) 0.0085(13) -0.0076(14) 0.0017(14) C13 0.0289(14) 0.0248(13) 0.0344(15) -0.0014(12) -0.0045(11) 0.0057(10) C14 0.0306(16) 0.0373(17) 0.0280(14) -0.0001(13) 0.0068(12) 0.0009(13) C15 0.062(2) 0.0412(18) 0.0308(15) -0.0022(14) -0.0004(14) 0.0040(16) C16 0.0354(16) 0.040(2) 0.0422(16) -0.0010(15) 0.0139(12) -0.0003(14) C17 0.0314(15) 0.0359(17) 0.0267(14) -0.0032(12) 0.0032(11) 0.0030(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 La1 C10 2.549(2) . ? La1 C7 2.748(3) . ? La1 C14 2.754(3) . ? La1 C13 2.763(2) . ? La1 C17 2.773(3) . ? La1 N1 2.7886(17) . ? La1 N3 2.8260(18) . ? La1 N2 2.8298(17) . ? La1 Al2 3.2509(7) . ? La1 Al1 3.2566(6) . ? La1 Al3 3.3186(7) . ? La1 H10B 2.55(3) . ? La1 H14B 2.67(3) . ? Al1 C9 1.971(3) . ? Al1 C8 1.984(2) . ? Al1 C10 2.056(2) . ? Al1 C7 2.070(3) . ? Al2 C11 1.973(3) . ? Al2 C12 1.980(3) . ? Al2 C10 2.054(2) . ? Al2 C13 2.082(3) . ? Al3 C15 1.970(3) . ? Al3 C16 1.985(3) . ? Al3 C17 2.044(3) . ? Al3 C14 2.050(3) . ? N1 C3 1.464(3) . ? N1 C4 1.471(3) . ? N1 C1 1.477(3) . ? N2 C1 1.461(3) . ? N2 C2 1.466(3) . ? N2 C5 1.478(3) . ? N3 C3 1.465(3) . ? N3 C2 1.468(3) . ? N3 C6 1.477(3) . ? C1 H1A 0.91(2) . ? C1 H1B 0.99(2) . ? C2 H2A 0.92(2) . ? C2 H2B 1.00(2) . ? C3 H3A 0.97(2) . ? C3 H3B 0.942(19) . ? C4 H4A 0.95(3) . ? C4 H4B 0.98(3) . ? C4 H4C 0.94(3) . ? C5 H5A 0.99(3) . ? C5 H5B 1.02(3) . ? C5 H5C 0.97(3) . ? C6 H6A 0.98(3) . ? C6 H6B 0.99(3) . ? C6 H6C 1.03(3) . ? C7 H7A 1.06(3) . ? C7 H7B 0.97(3) . ? C7 H7C 0.91(3) . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C8 H8D 0.9800 . ? C8 H8E 0.9800 . ? C8 H8F 0.9800 . ? C9 H9A 0.98(4) . ? C9 H9B 0.93(4) . ? C9 H9C 0.89(3) . ? C10 H10A 1.03(2) . ? C10 H10B 0.94(3) . ? C11 H11A 0.84(4) . ? C11 H11B 1.01(3) . ? C11 H11C 1.00(3) . ? C12 H12A 0.90(4) . ? C12 H12B 0.93(3) . ? C12 H12C 0.94(4) . ? C13 H13A 0.97(3) . ? C13 H13B 1.00(2) . ? C13 H13C 0.95(3) . ? C14 H14A 0.97(3) . ? C14 H14B 0.95(3) . ? C14 H14C 0.88(3) . ? C15 H15A 0.86(4) . ? C15 H15B 0.91(3) . ? C15 H15C 0.94(3) . ? C16 H16A 0.94(3) . ? C16 H16B 1.04(3) . ? C16 H16C 0.95(4) . ? C17 H17A 0.99(3) . ? C17 H17B 0.81(3) . ? C17 H17C 1.01(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C10 La1 C7 77.79(7) . . ? C10 La1 C14 91.10(8) . . ? C7 La1 C14 157.64(9) . . ? C10 La1 C13 78.17(7) . . ? C7 La1 C13 113.03(9) . . ? C14 La1 C13 82.94(8) . . ? C10 La1 C17 89.22(8) . . ? C7 La1 C17 84.68(9) . . ? C14 La1 C17 75.73(8) . . ? C13 La1 C17 154.99(8) . . ? C10 La1 N1 154.41(6) . . ? C7 La1 N1 79.25(7) . . ? C14 La1 N1 106.34(7) . . ? C13 La1 N1 121.70(7) . . ? C17 La1 N1 77.52(7) . . ? C10 La1 N3 155.56(6) . . ? C7 La1 N3 120.47(7) . . ? C14 La1 N3 76.49(7) . . ? C13 La1 N3 79.45(6) . . ? C17 La1 N3 107.51(7) . . ? N1 La1 N3 49.72(6) . . ? C10 La1 N2 133.16(6) . . ? C7 La1 N2 76.15(7) . . ? C14 La1 N2 124.25(8) . . ? C13 La1 N2 77.23(7) . . ? C17 La1 N2 125.81(7) . . ? N1 La1 N2 49.50(5) . . ? N3 La1 N2 49.00(5) . . ? C10 La1 Al2 39.18(5) . . ? C7 La1 Al2 100.75(6) . . ? C14 La1 Al2 81.46(6) . . ? C13 La1 Al2 39.47(5) . . ? C17 La1 Al2 122.71(6) . . ? N1 La1 Al2 159.76(4) . . ? N3 La1 Al2 117.07(4) . . ? N2 La1 Al2 110.56(4) . . ? C10 La1 Al1 39.15(5) . . ? C7 La1 Al1 39.19(6) . . ? C14 La1 Al1 125.08(6) . . ? C13 La1 Al1 101.25(5) . . ? C17 La1 Al1 81.08(6) . . ? N1 La1 Al1 116.18(4) . . ? N3 La1 Al1 158.43(4) . . ? N2 La1 Al1 109.78(4) . . ? Al2 La1 Al1 70.639(19) . . ? C10 La1 Al3 93.29(5) . . ? C7 La1 Al3 122.36(7) . . ? C14 La1 Al3 38.05(6) . . ? C13 La1 Al3 120.58(6) . . ? C17 La1 Al3 37.89(6) . . ? N1 La1 Al3 89.51(4) . . ? N3 La1 Al3 89.69(4) . . ? N2 La1 Al3 133.55(4) . . ? Al2 La1 Al3 106.930(18) . . ? Al1 La1 Al3 107.786(19) . . ? C10 La1 H10B 21.2(6) . . ? C7 La1 H10B 89.6(6) . . ? C14 La1 H10B 74.5(6) . . ? C13 La1 H10B 89.4(6) . . ? C17 La1 H10B 72.5(6) . . ? N1 La1 H10B 148.9(6) . . ? N3 La1 H10B 150.0(6) . . ? N2 La1 H10B 154.4(6) . . ? Al2 La1 H10B 50.8(6) . . ? Al1 La1 H10B 51.1(6) . . ? Al3 La1 H10B 72.0(6) . . ? C10 La1 H14B 105.4(7) . . ? C7 La1 H14B 174.0(7) . . ? C14 La1 H14B 20.1(7) . . ? C13 La1 H14B 72.8(7) . . ? C17 La1 H14B 90.2(7) . . ? N1 La1 H14B 96.5(7) . . ? N3 La1 H14B 58.1(7) . . ? N2 La1 H14B 104.5(7) . . ? Al2 La1 H14B 84.7(7) . . ? Al1 La1 H14B 143.0(7) . . ? Al3 La1 H14B 52.9(7) . . ? H10B La1 H14B 92.0(9) . . ? C9 Al1 C8 113.20(14) . . ? C9 Al1 C10 109.43(14) . . ? C8 Al1 C10 111.67(10) . . ? C9 Al1 C7 105.91(14) . . ? C8 Al1 C7 108.70(12) . . ? C10 Al1 C7 107.61(10) . . ? C9 Al1 La1 129.48(11) . . ? C8 Al1 La1 117.32(8) . . ? C10 Al1 La1 51.51(6) . . ? C7 Al1 La1 57.02(7) . . ? C11 Al2 C12 113.96(14) . . ? C11 Al2 C10 109.95(12) . . ? C12 Al2 C10 111.60(12) . . ? C11 Al2 C13 103.31(12) . . ? C12 Al2 C13 109.25(13) . . ? C10 Al2 C13 108.32(10) . . ? C11 Al2 La1 127.48(10) . . ? C12 Al2 La1 118.51(10) . . ? C10 Al2 La1 51.63(6) . . ? C13 Al2 La1 57.51(7) . . ? C15 Al3 C16 116.41(15) . . ? C15 Al3 C17 107.30(14) . . ? C16 Al3 C17 107.61(13) . . ? C15 Al3 C14 105.26(13) . . ? C16 Al3 C14 108.43(15) . . ? C17 Al3 C14 111.91(11) . . ? C15 Al3 La1 125.92(11) . . ? C16 Al3 La1 117.66(9) . . ? C17 Al3 La1 56.43(8) . . ? C14 Al3 La1 55.89(8) . . ? C3 N1 C4 110.85(18) . . ? C3 N1 C1 108.02(19) . . ? C4 N1 C1 110.46(19) . . ? C3 N1 La1 95.18(12) . . ? C4 N1 La1 133.03(16) . . ? C1 N1 La1 96.62(12) . . ? C1 N2 C2 108.07(18) . . ? C1 N2 C5 110.31(18) . . ? C2 N2 C5 110.4(2) . . ? C1 N2 La1 95.31(12) . . ? C2 N2 La1 96.49(12) . . ? C5 N2 La1 133.59(15) . . ? C3 N3 C2 108.92(18) . . ? C3 N3 C6 110.63(19) . . ? C2 N3 C6 110.3(2) . . ? C3 N3 La1 93.63(13) . . ? C2 N3 La1 96.58(12) . . ? C6 N3 La1 134.20(16) . . ? N2 C1 N1 106.37(17) . . ? N2 C1 H1A 109.5(16) . . ? N1 C1 H1A 106.9(15) . . ? N2 C1 H1B 115.3(14) . . ? N1 C1 H1B 111.7(11) . . ? H1A C1 H1B 106.7(19) . . ? N2 C2 N3 106.15(18) . . ? N2 C2 H2A 109.4(13) . . ? N3 C2 H2A 107.3(12) . . ? N2 C2 H2B 108.8(13) . . ? N3 C2 H2B 110.6(12) . . ? H2A C2 H2B 114.2(19) . . ? N1 C3 N3 107.40(17) . . ? N1 C3 H3A 111.8(14) . . ? N3 C3 H3A 114.2(14) . . ? N1 C3 H3B 109.6(17) . . ? N3 C3 H3B 109.6(16) . . ? H3A C3 H3B 104.2(17) . . ? N1 C4 H4A 107.6(18) . . ? N1 C4 H4B 108.0(18) . . ? H4A C4 H4B 114(2) . . ? N1 C4 H4C 109.2(15) . . ? H4A C4 H4C 108(2) . . ? H4B C4 H4C 110(2) . . ? N2 C5 H5A 109.3(14) . . ? N2 C5 H5B 109.4(14) . . ? H5A C5 H5B 104(2) . . ? N2 C5 H5C 111.7(14) . . ? H5A C5 H5C 110(2) . . ? H5B C5 H5C 113(2) . . ? N3 C6 H6A 107.9(17) . . ? N3 C6 H6B 105.6(14) . . ? H6A C6 H6B 109(2) . . ? N3 C6 H6C 109.4(16) . . ? H6A C6 H6C 112(2) . . ? H6B C6 H6C 112(2) . . ? Al1 C7 La1 83.79(9) . . ? Al1 C7 H7A 114.8(14) . . ? La1 C7 H7A 79.8(14) . . ? Al1 C7 H7B 127.8(16) . . ? La1 C7 H7B 78.9(16) . . ? H7A C7 H7B 110(2) . . ? Al1 C7 H7C 93.3(19) . . ? La1 C7 H7C 176(2) . . ? H7A C7 H7C 104(2) . . ? H7B C7 H7C 101(2) . . ? Al1 C8 H8A 109.5 . . ? Al1 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? Al1 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? Al1 C8 H8D 109.5 . . ? H8A C8 H8D 141.1 . . ? H8B C8 H8D 56.3 . . ? H8C C8 H8D 56.3 . . ? Al1 C8 H8E 109.5 . . ? H8A C8 H8E 56.3 . . ? H8B C8 H8E 141.1 . . ? H8C C8 H8E 56.3 . . ? H8D C8 H8E 109.5 . . ? Al1 C8 H8F 109.5 . . ? H8A C8 H8F 56.3 . . ? H8B C8 H8F 56.3 . . ? H8C C8 H8F 141.1 . . ? H8D C8 H8F 109.5 . . ? H8E C8 H8F 109.5 . . ? Al1 C9 H9A 114(2) . . ? Al1 C9 H9B 117(2) . . ? H9A C9 H9B 99(3) . . ? Al1 C9 H9C 114(2) . . ? H9A C9 H9C 110(3) . . ? H9B C9 H9C 103(3) . . ? Al2 C10 Al1 132.50(11) . . ? Al2 C10 La1 89.18(8) . . ? Al1 C10 La1 89.34(8) . . ? Al2 C10 H10A 86.6(14) . . ? Al1 C10 H10A 89.4(13) . . ? La1 C10 H10A 173.0(13) . . ? Al2 C10 H10B 112.5(17) . . ? Al1 C10 H10B 113.8(17) . . ? La1 C10 H10B 79.5(16) . . ? H10A C10 H10B 107(2) . . ? Al2 C11 H11A 114(3) . . ? Al2 C11 H11B 110.6(15) . . ? H11A C11 H11B 102(3) . . ? Al2 C11 H11C 108.5(16) . . ? H11A C11 H11C 114(3) . . ? H11B C11 H11C 108(2) . . ? Al2 C12 H12A 109(2) . . ? Al2 C12 H12B 114(2) . . ? H12A C12 H12B 109(3) . . ? Al2 C12 H12C 120(2) . . ? H12A C12 H12C 106(3) . . ? H12B C12 H12C 99(3) . . ? Al2 C13 La1 83.02(8) . . ? Al2 C13 H13A 95.4(15) . . ? La1 C13 H13A 174.4(16) . . ? Al2 C13 H13B 131.3(14) . . ? La1 C13 H13B 78.8(14) . . ? H13A C13 H13B 98.4(19) . . ? Al2 C13 H13C 116.9(18) . . ? La1 C13 H13C 78.4(17) . . ? H13A C13 H13C 107(2) . . ? H13B C13 H13C 103(2) . . ? Al3 C14 La1 86.07(10) . . ? Al3 C14 H14A 96.4(17) . . ? La1 C14 H14A 176.5(16) . . ? Al3 C14 H14B 127(2) . . ? La1 C14 H14B 75.1(19) . . ? H14A C14 H14B 105(2) . . ? Al3 C14 H14C 119.4(17) . . ? La1 C14 H14C 78.3(15) . . ? H14A C14 H14C 98(2) . . ? H14B C14 H14C 105(3) . . ? Al3 C15 H15A 107(2) . . ? Al3 C15 H15B 113.4(18) . . ? H15A C15 H15B 110(3) . . ? Al3 C15 H15C 117.1(16) . . ? H15A C15 H15C 102(3) . . ? H15B C15 H15C 107(3) . . ? Al3 C16 H16A 108(2) . . ? Al3 C16 H16B 115.4(16) . . ? H16A C16 H16B 100(3) . . ? Al3 C16 H16C 107.3(19) . . ? H16A C16 H16C 118(3) . . ? H16B C16 H16C 109(2) . . ? Al3 C17 La1 85.67(10) . . ? Al3 C17 H17A 121.2(16) . . ? La1 C17 H17A 81.8(16) . . ? Al3 C17 H17B 125(2) . . ? La1 C17 H17B 76(2) . . ? H17A C17 H17B 107(3) . . ? Al3 C17 H17C 97.8(13) . . ? La1 C17 H17C 174.4(13) . . ? H17A C17 H17C 100(2) . . ? H17B C17 H17C 98(3) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.282 _refine_diff_density_min -0.361 _refine_diff_density_rms 0.062