data_dw1437_compound_1b _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C40 H46 Al2 N6 Sm, 2(C7 H8)' _chemical_formula_sum 'C54 H62 Al2 N6 Sm' _chemical_formula_weight 999.41 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 'triclinic' _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.5493(11) _cell_length_b 10.6865(12) _cell_length_c 13.7530(13) _cell_angle_alpha 71.935(3) _cell_angle_beta 69.964(3) _cell_angle_gamma 84.546(4) _cell_volume 1253.4(2) _cell_formula_units_Z 1 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 4231 _cell_measurement_theta_min 2.18 _cell_measurement_theta_max 22.61 _exptl_crystal_description 'block' _exptl_crystal_colour 'black' _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.36 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.324 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 516 _exptl_absorpt_coefficient_mu 1.247 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_correction_T_min 0.5743 _exptl_absorpt_correction_T_max 0.8159 _exptl_absorpt_process_details 'SADABS V2008/1 (Bruker AXS)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'micro-focus sealed tube' _diffrn_radiation_monochromator 'doubly curved silicon crystal' _diffrn_measurement_device_type 'Bruker SMART X2S' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12069 _diffrn_reflns_av_R_equivalents 0.0496 _diffrn_reflns_av_sigmaI/netI 0.0568 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.65 _diffrn_reflns_theta_max 25.07 _reflns_number_total 4384 _reflns_number_gt 4186 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker GIS' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SIR-92 (Altomare et al. 1994)' _computing_structure_refinement 'SHELXL-97 (Sheldrick 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0472P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4384 _refine_ls_number_parameters 332 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0387 _refine_ls_R_factor_gt 0.0351 _refine_ls_wR_factor_ref 0.0910 _refine_ls_wR_factor_gt 0.0795 _refine_ls_goodness_of_fit_ref 1.094 _refine_ls_restrained_S_all 1.094 _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 Sm1 Sm 0.0000 1.0000 1.0000 0.03066(11) Uani 1 2 d S . . N1 N 0.2445(3) 1.0911(3) 0.8308(3) 0.0365(7) Uani 1 1 d . . . N2 N -0.0671(3) 0.8450(3) 0.9028(3) 0.0358(7) Uani 1 1 d . . . N3 N 0.1634(3) 0.8060(3) 1.0907(3) 0.0372(7) Uani 1 1 d . . . Al1 Al 0.26028(12) 0.79966(10) 0.86644(10) 0.0339(3) Uani 1 1 d . . . C1 C 0.3991(5) 0.6865(4) 0.7873(4) 0.0531(12) Uani 1 1 d . . . H1A H 0.5007 0.7036 0.7845 0.064 Uiso 1 1 calc R . . H1B H 0.3734 0.5938 0.8312 0.064 Uiso 1 1 calc R . . C2 C 0.4058(6) 0.6989(6) 0.6736(5) 0.0790(17) Uani 1 1 d . . . H2A H 0.4740 0.6332 0.6471 0.119 Uiso 1 1 calc R . . H2B H 0.4417 0.7873 0.6263 0.119 Uiso 1 1 calc R . . H2C H 0.3060 0.6843 0.6736 0.119 Uiso 1 1 calc R . . C11 C 0.3227(4) 0.9912(4) 0.7966(3) 0.0347(8) Uani 1 1 d . . . C12 C 0.4570(5) 1.0202(4) 0.7138(4) 0.0515(11) Uani 1 1 d . . . H12 H 0.5146 0.9506 0.6910 0.062 Uiso 1 1 calc R . . C13 C 0.5100(5) 1.1478(5) 0.6630(4) 0.0628(13) Uani 1 1 d . . . H13 H 0.6016 1.1665 0.6046 0.075 Uiso 1 1 calc R . . C14 C 0.4288(5) 1.2457(4) 0.6981(4) 0.0525(11) Uani 1 1 d . . . H14 H 0.4632 1.3344 0.6650 0.063 Uiso 1 1 calc R . . C15 C 0.2960(4) 1.2153(4) 0.7821(3) 0.0396(9) Uani 1 1 d . . . C16 C 0.2049(6) 1.3220(4) 0.8223(4) 0.0592(13) Uani 1 1 d . . . H16A H 0.0989 1.3043 0.8393 0.089 Uiso 1 1 calc R . . H16B H 0.2335 1.4068 0.7663 0.089 Uiso 1 1 calc R . . H16C H 0.2224 1.3248 0.8878 0.089 Uiso 1 1 calc R . . C21 C 0.0508(4) 0.7657(4) 0.8769(3) 0.0362(9) Uani 1 1 d . . . C22 C 0.0266(5) 0.6512(4) 0.8573(4) 0.0540(12) Uani 1 1 d . . . H22 H 0.1076 0.5934 0.8418 0.065 Uiso 1 1 calc R . . C23 C -0.1099(5) 0.6187(5) 0.8597(4) 0.0654(14) Uani 1 1 d . . . H23 H -0.1238 0.5404 0.8450 0.078 Uiso 1 1 calc R . . C24 C -0.2243(5) 0.7009(5) 0.8836(4) 0.0540(12) Uani 1 1 d . . . H24 H -0.3202 0.6813 0.8851 0.065 Uiso 1 1 calc R . . C25 C -0.2020(4) 0.8135(4) 0.9057(3) 0.0442(10) Uani 1 1 d . . . C26 C -0.3281(5) 0.9047(5) 0.9342(5) 0.0646(14) Uani 1 1 d . . . H26A H -0.3072 0.9541 0.9771 0.097 Uiso 1 1 calc R . . H26B H -0.4206 0.8535 0.9766 0.097 Uiso 1 1 calc R . . H26C H -0.3391 0.9662 0.8676 0.097 Uiso 1 1 calc R . . C31 C 0.2600(4) 0.7490(3) 1.0196(3) 0.0342(9) Uani 1 1 d . . . C32 C 0.3569(4) 0.6554(4) 1.0553(4) 0.0438(10) Uani 1 1 d . . . H32 H 0.4248 0.6137 1.0063 0.053 Uiso 1 1 calc R . . C33 C 0.3560(5) 0.6223(4) 1.1600(4) 0.0566(13) Uani 1 1 d . . . H33 H 0.4239 0.5593 1.1834 0.068 Uiso 1 1 calc R . . C34 C 0.2569(5) 0.6804(4) 1.2300(4) 0.0495(11) Uani 1 1 d . . . H34 H 0.2543 0.6580 1.3031 0.059 Uiso 1 1 calc R . . C35 C 0.1607(5) 0.7717(4) 1.1942(3) 0.0430(10) Uani 1 1 d . . . C36 C 0.0508(6) 0.8357(5) 1.2703(4) 0.0617(13) Uani 1 1 d . . . H36A H -0.0479 0.7954 1.2936 0.093 Uiso 1 1 calc R . . H36B H 0.0466 0.9299 1.2337 0.093 Uiso 1 1 calc R . . H36C H 0.0813 0.8238 1.3337 0.093 Uiso 1 1 calc R . . C50 C -0.174(4) 0.505(4) 0.468(3) 0.18(2) Uani 0.50 1 d P A -1 H50A H -0.2109 0.5934 0.4686 0.268 Uiso 0.50 1 calc PR A -1 H50B H -0.2444 0.4392 0.5263 0.268 Uiso 0.50 1 calc PR A -1 H50C H -0.1629 0.4926 0.3980 0.268 Uiso 0.50 1 calc PR A -1 C51 C -0.0386(15) 0.4900(17) 0.4834(10) 0.091(5) Uani 0.50 1 d PG A -1 C52 C -0.0234(14) 0.5769(15) 0.5363(12) 0.086(6) Uani 0.50 1 d PG A -1 H52 H -0.1030 0.6335 0.5582 0.103 Uiso 0.50 1 calc PR A -1 C53 C 0.1083(19) 0.5811(18) 0.5572(15) 0.111(9) Uani 0.50 1 d PG A -1 H53 H 0.1187 0.6405 0.5934 0.133 Uiso 0.50 1 calc PR A -1 C54 C 0.2247(14) 0.498(2) 0.5252(17) 0.116(12) Uani 0.50 1 d PG A -1 H54 H 0.3147 0.5011 0.5395 0.139 Uiso 0.50 1 calc PR A -1 C55 C 0.2095(17) 0.4114(16) 0.4722(14) 0.151(14) Uani 0.50 1 d PG A -1 H55 H 0.2891 0.3548 0.4503 0.181 Uiso 0.50 1 calc PR A -1 C56 C 0.078(2) 0.4073(13) 0.4513(9) 0.173(17) Uani 0.50 1 d PG A -1 H56 H 0.0674 0.3479 0.4151 0.207 Uiso 0.50 1 calc PR A -1 C60 C 0.212(3) 0.026(3) 0.538(2) 0.144(10) Uani 0.50 1 d P B -1 H60A H 0.2856 -0.0402 0.5181 0.216 Uiso 0.50 1 calc PR B -1 H60B H 0.1926 0.0201 0.6141 0.216 Uiso 0.50 1 calc PR B -1 H60C H 0.2518 0.1141 0.4920 0.216 Uiso 0.50 1 calc PR B -1 C61 C 0.0800(13) 0.0039(13) 0.5234(11) 0.089(5) Uani 0.50 1 d PG B -1 C62 C -0.0286(14) -0.0842(12) 0.6033(8) 0.084(6) Uani 0.50 1 d PG B -1 H62 H -0.0119 -0.1343 0.6686 0.101 Uiso 0.50 1 calc PR B -1 C63 C -0.1616(12) -0.0991(14) 0.5876(12) 0.099(6) Uani 0.50 1 d PG B -1 H63 H -0.2358 -0.1593 0.6422 0.119 Uiso 0.50 1 calc PR B -1 C64 C -0.1860(15) -0.0258(18) 0.4920(14) 0.119(13) Uani 0.50 1 d PG B -1 H64 H -0.2770 -0.0360 0.4813 0.143 Uiso 0.50 1 calc PR B -1 C65 C -0.077(2) 0.0623(15) 0.4121(10) 0.142(14) Uani 0.50 1 d PG B -1 H65 H -0.0942 0.1124 0.3468 0.170 Uiso 0.50 1 calc PR B -1 C66 C 0.0555(18) 0.0772(11) 0.4278(9) 0.103(9) Uani 0.50 1 d PG B -1 H66 H 0.1297 0.1374 0.3732 0.123 Uiso 0.50 1 calc PR B -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 Sm1 0.02987(16) 0.02425(15) 0.03582(19) -0.00803(11) -0.01068(12) 0.00620(10) N1 0.0361(17) 0.0292(16) 0.0410(19) -0.0089(14) -0.0103(15) 0.0008(13) N2 0.0320(17) 0.0355(17) 0.0405(18) -0.0106(14) -0.0135(14) 0.0008(13) N3 0.0418(18) 0.0270(16) 0.044(2) -0.0089(14) -0.0197(16) 0.0095(13) Al1 0.0281(6) 0.0275(5) 0.0473(7) -0.0159(5) -0.0110(5) 0.0051(4) C1 0.040(2) 0.049(3) 0.079(3) -0.037(2) -0.017(2) 0.0110(19) C2 0.067(4) 0.091(4) 0.089(4) -0.060(4) -0.009(3) 0.003(3) C11 0.034(2) 0.034(2) 0.038(2) -0.0123(17) -0.0117(17) -0.0020(15) C12 0.041(2) 0.047(2) 0.058(3) -0.023(2) 0.002(2) -0.0012(19) C13 0.051(3) 0.059(3) 0.059(3) -0.018(2) 0.009(2) -0.015(2) C14 0.053(3) 0.042(2) 0.051(3) -0.008(2) -0.006(2) -0.014(2) C15 0.046(2) 0.033(2) 0.037(2) -0.0077(17) -0.0116(19) -0.0021(17) C16 0.074(3) 0.029(2) 0.060(3) -0.008(2) -0.009(3) -0.002(2) C21 0.036(2) 0.0317(19) 0.040(2) -0.0093(17) -0.0127(17) -0.0003(16) C22 0.040(2) 0.042(2) 0.079(3) -0.026(2) -0.011(2) -0.0051(19) C23 0.057(3) 0.054(3) 0.086(4) -0.036(3) -0.007(3) -0.018(2) C24 0.037(2) 0.064(3) 0.066(3) -0.022(2) -0.015(2) -0.017(2) C25 0.034(2) 0.048(2) 0.050(3) -0.010(2) -0.0150(19) -0.0037(18) C26 0.034(2) 0.067(3) 0.103(4) -0.033(3) -0.029(3) 0.008(2) C31 0.0293(19) 0.0217(17) 0.049(2) -0.0061(16) -0.0136(17) -0.0025(14) C32 0.032(2) 0.034(2) 0.060(3) -0.011(2) -0.0129(19) 0.0054(16) C33 0.043(3) 0.041(2) 0.079(4) 0.000(2) -0.030(2) 0.0103(19) C34 0.053(3) 0.042(2) 0.052(3) 0.001(2) -0.030(2) 0.002(2) C35 0.052(2) 0.029(2) 0.048(3) -0.0030(18) -0.024(2) 0.0006(17) C36 0.085(4) 0.055(3) 0.045(3) -0.015(2) -0.026(3) 0.018(3) C50 0.13(2) 0.28(5) 0.076(18) 0.07(2) -0.053(15) -0.09(3) C51 0.109(14) 0.098(12) 0.047(9) 0.037(8) -0.041(9) -0.049(10) C52 0.095(11) 0.066(12) 0.077(14) -0.013(10) -0.013(10) 0.013(9) C53 0.16(3) 0.113(15) 0.071(11) -0.031(10) -0.042(13) -0.020(13) C54 0.076(14) 0.132(19) 0.090(16) 0.055(14) -0.037(12) -0.028(11) C55 0.17(2) 0.071(13) 0.11(2) 0.021(11) 0.029(16) 0.039(15) C56 0.31(5) 0.075(17) 0.084(17) -0.020(13) 0.00(3) -0.06(3) C60 0.132(19) 0.16(3) 0.13(2) -0.10(2) 0.015(19) 0.010(17) C61 0.085(10) 0.077(10) 0.091(14) -0.056(9) 0.011(9) 0.020(9) C62 0.092(13) 0.099(13) 0.054(10) -0.038(8) -0.006(10) 0.018(9) C63 0.096(12) 0.104(12) 0.080(12) -0.030(9) -0.017(10) 0.049(10) C64 0.15(3) 0.11(2) 0.108(19) -0.076(16) -0.043(19) 0.07(2) C65 0.27(4) 0.072(12) 0.053(12) -0.019(9) -0.038(17) 0.081(18) C66 0.17(3) 0.074(11) 0.032(8) -0.018(7) -0.009(14) 0.044(16) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Sm1 N2 2.666(3) . ? Sm1 N2 2.666(3) 2_577 ? Sm1 N1 2.668(3) . ? Sm1 N1 2.668(3) 2_577 ? Sm1 N3 2.721(3) 2_577 ? Sm1 N3 2.721(3) . ? Sm1 Al1 3.5263(11) 2_577 ? Sm1 Al1 3.5263(11) . ? N1 C15 1.341(5) . ? N1 C11 1.356(5) . ? N2 C25 1.346(5) . ? N2 C21 1.358(5) . ? N3 C35 1.347(5) . ? N3 C31 1.350(5) . ? Al1 C1 1.981(4) . ? Al1 C31 2.005(4) . ? Al1 C21 2.016(4) . ? Al1 C11 2.022(4) . ? C1 C2 1.507(7) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C11 C12 1.376(5) . ? C12 C13 1.378(6) . ? C12 H12 0.9500 . ? C13 C14 1.353(7) . ? C13 H13 0.9500 . ? C14 C15 1.376(6) . ? C14 H14 0.9500 . ? C15 C16 1.496(6) . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C21 C22 1.386(5) . ? C22 C23 1.368(6) . ? C22 H22 0.9500 . ? C23 C24 1.351(7) . ? C23 H23 0.9500 . ? C24 C25 1.380(6) . ? C24 H24 0.9500 . ? C25 C26 1.498(6) . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C31 C32 1.389(5) . ? C32 C33 1.370(6) . ? C32 H32 0.9500 . ? C33 C34 1.357(7) . ? C33 H33 0.9500 . ? C34 C35 1.372(5) . ? C34 H34 0.9500 . ? C35 C36 1.490(6) . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C50 C51 1.36(3) . ? C50 H50A 0.9800 . ? C50 H50B 0.9800 . ? C50 H50C 0.9800 . ? C51 C52 1.3900 . ? C51 C56 1.3900 . ? C52 C53 1.3900 . ? C52 H52 0.9500 . ? C53 C54 1.3900 . ? C53 H53 0.9500 . ? C54 C55 1.3900 . ? C54 H54 0.9500 . ? C55 C56 1.3900 . ? C55 H55 0.9500 . ? C56 H56 0.9500 . ? C60 C61 1.40(3) . ? C60 H60A 0.9800 . ? C60 H60B 0.9800 . ? C60 H60C 0.9800 . ? C61 C62 1.3900 . ? C61 C66 1.3900 . ? C62 C63 1.3900 . ? C62 H62 0.9500 . ? C63 C64 1.3900 . ? C63 H63 0.9500 . ? C64 C65 1.3900 . ? C64 H64 0.9500 . ? C65 C66 1.3900 . ? C65 H65 0.9500 . ? C66 H66 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Sm1 N2 180.000(1) . 2_577 ? N2 Sm1 N1 91.55(9) . . ? N2 Sm1 N1 88.45(9) 2_577 . ? N2 Sm1 N1 88.45(9) . 2_577 ? N2 Sm1 N1 91.55(9) 2_577 2_577 ? N1 Sm1 N1 180.0 . 2_577 ? N2 Sm1 N3 89.02(9) . 2_577 ? N2 Sm1 N3 90.98(9) 2_577 2_577 ? N1 Sm1 N3 90.26(9) . 2_577 ? N1 Sm1 N3 89.74(10) 2_577 2_577 ? N2 Sm1 N3 90.98(9) . . ? N2 Sm1 N3 89.02(9) 2_577 . ? N1 Sm1 N3 89.74(9) . . ? N1 Sm1 N3 90.26(9) 2_577 . ? N3 Sm1 N3 180.00(14) 2_577 . ? N2 Sm1 Al1 123.92(7) . 2_577 ? N2 Sm1 Al1 56.08(7) 2_577 2_577 ? N1 Sm1 Al1 124.19(7) . 2_577 ? N1 Sm1 Al1 55.81(7) 2_577 2_577 ? N3 Sm1 Al1 53.92(7) 2_577 2_577 ? N3 Sm1 Al1 126.08(7) . 2_577 ? N2 Sm1 Al1 56.08(7) . . ? N2 Sm1 Al1 123.92(7) 2_577 . ? N1 Sm1 Al1 55.81(7) . . ? N1 Sm1 Al1 124.19(7) 2_577 . ? N3 Sm1 Al1 126.08(7) 2_577 . ? N3 Sm1 Al1 53.92(7) . . ? Al1 Sm1 Al1 180.0 2_577 . ? C15 N1 C11 120.1(3) . . ? C15 N1 Sm1 129.0(3) . . ? C11 N1 Sm1 110.9(2) . . ? C25 N2 C21 120.0(3) . . ? C25 N2 Sm1 128.8(3) . . ? C21 N2 Sm1 108.2(2) . . ? C35 N3 C31 120.5(3) . . ? C35 N3 Sm1 125.7(2) . . ? C31 N3 Sm1 113.6(2) . . ? C1 Al1 C31 110.03(18) . . ? C1 Al1 C21 109.05(17) . . ? C31 Al1 C21 105.76(15) . . ? C1 Al1 C11 111.05(18) . . ? C31 Al1 C11 107.72(15) . . ? C21 Al1 C11 113.08(15) . . ? C1 Al1 Sm1 176.92(14) . . ? C31 Al1 Sm1 72.38(11) . . ? C21 Al1 Sm1 68.17(11) . . ? C11 Al1 Sm1 69.51(11) . . ? C2 C1 Al1 118.9(3) . . ? C2 C1 H1A 107.6 . . ? Al1 C1 H1A 107.6 . . ? C2 C1 H1B 107.6 . . ? Al1 C1 H1B 107.6 . . ? H1A C1 H1B 107.0 . . ? C1 C2 H2A 109.5 . . ? C1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? N1 C11 C12 118.5(3) . . ? N1 C11 Al1 123.8(3) . . ? C12 C11 Al1 117.6(3) . . ? C11 C12 C13 121.6(4) . . ? C11 C12 H12 119.2 . . ? C13 C12 H12 119.2 . . ? C14 C13 C12 118.6(4) . . ? C14 C13 H13 120.7 . . ? C12 C13 H13 120.7 . . ? C13 C14 C15 119.2(4) . . ? C13 C14 H14 120.4 . . ? C15 C14 H14 120.4 . . ? N1 C15 C14 121.9(4) . . ? N1 C15 C16 118.0(4) . . ? C14 C15 C16 120.0(4) . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? N2 C21 C22 118.2(3) . . ? N2 C21 Al1 125.0(3) . . ? C22 C21 Al1 116.7(3) . . ? C23 C22 C21 122.2(4) . . ? C23 C22 H22 118.9 . . ? C21 C22 H22 118.9 . . ? C24 C23 C22 118.1(4) . . ? C24 C23 H23 120.9 . . ? C22 C23 H23 120.9 . . ? C23 C24 C25 120.0(4) . . ? C23 C24 H24 120.0 . . ? C25 C24 H24 120.0 . . ? N2 C25 C24 121.4(4) . . ? N2 C25 C26 117.8(4) . . ? C24 C25 C26 120.8(4) . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? N3 C31 C32 118.6(4) . . ? N3 C31 Al1 119.9(3) . . ? C32 C31 Al1 121.5(3) . . ? C33 C32 C31 120.9(4) . . ? C33 C32 H32 119.6 . . ? C31 C32 H32 119.6 . . ? C34 C33 C32 119.3(4) . . ? C34 C33 H33 120.4 . . ? C32 C33 H33 120.4 . . ? C33 C34 C35 119.3(4) . . ? C33 C34 H34 120.3 . . ? C35 C34 H34 120.3 . . ? N3 C35 C34 121.4(4) . . ? N3 C35 C36 118.7(3) . . ? C34 C35 C36 119.9(4) . . ? C35 C36 H36A 109.5 . . ? C35 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C35 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C50 C51 C52 110.5(18) . . ? C50 C51 C56 129.5(18) . . ? C52 C51 C56 120.0 . . ? C53 C52 C51 120.0 . . ? C53 C52 H52 120.0 . . ? C51 C52 H52 120.0 . . ? C52 C53 C54 120.0 . . ? C52 C53 H53 120.0 . . ? C54 C53 H53 120.0 . . ? C53 C54 C55 120.0 . . ? C53 C54 H54 120.0 . . ? C55 C54 H54 120.0 . . ? C56 C55 C54 120.0 . . ? C56 C55 H55 120.0 . . ? C54 C55 H55 120.0 . . ? C55 C56 C51 120.0 . . ? C55 C56 H56 120.0 . . ? C51 C56 H56 120.0 . . ? C62 C61 C66 120.0 . . ? C62 C61 C60 121.8(15) . . ? C66 C61 C60 118.2(15) . . ? C63 C62 C61 120.0 . . ? C63 C62 H62 120.0 . . ? C61 C62 H62 120.0 . . ? C62 C63 C64 120.0 . . ? C62 C63 H63 120.0 . . ? C64 C63 H63 120.0 . . ? C65 C64 C63 120.0 . . ? C65 C64 H64 120.0 . . ? C63 C64 H64 120.0 . . ? C66 C65 C64 120.0 . . ? C66 C65 H65 120.0 . . ? C64 C65 H65 120.0 . . ? C65 C66 C61 120.0 . . ? C65 C66 H66 120.0 . . ? C61 C66 H66 120.0 . . ? _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 25.07 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 0.467 _refine_diff_density_min -0.693 _refine_diff_density_rms 0.142 #===END data_dw1452_compound_2 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C58 H60 Al4 N10 O2 Sm2, 4(C7 H8)' _chemical_formula_sum 'C86 H92 Al4 N10 O2 Sm2' _chemical_formula_weight 1706.32 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' 'Al' 'Al' 0.0645 0.0514 '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' 'Sm' 'Sm' -0.1638 3.4418 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.8425(1) _cell_length_b 12.9959(1) _cell_length_c 14.3642(2) _cell_angle_alpha 93.539(1) _cell_angle_beta 99.712(1) _cell_angle_gamma 116.661(1) _cell_volume 2085.92(4) _cell_formula_units_Z 1 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 26186 _cell_measurement_theta_min 1.00 _cell_measurement_theta_max 32.03 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.21 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.358 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 870 _exptl_absorpt_coefficient_mu 1.487 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_correction_T_min 0.703 _exptl_absorpt_correction_T_max 0.738 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements Sortav (Blessing 1995) ; _exptl_special_details ; The two toluene molecules in the asymmetric unit are both poorly resolved (see '_refine_special_details'). ; _diffrn_ambient_temperature 180(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_measurement_method 'Thin slice \w and \f scans' _diffrn_reflns_number 31813 _diffrn_reflns_av_R_equivalents 0.0337 _diffrn_reflns_av_sigmaI/netI 0.0332 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 3.53 _diffrn_reflns_theta_max 32.02 _reflns_number_total 13892 _reflns_number_gt 12972 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius B.V. 1998)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction ; HKL Denzo and Scalepack (Otwinowski & Minor 1997) ; _computing_structure_solution 'SIR-92 (Altomare et al. 1994)' _computing_structure_refinement 'SHELXL-97 (Sheldrick 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The two toluene molecules in the asymmetric unit are both poorly resolved, modelled with geometric restraints (SHELXL command 'AFIX 66') and a common isotropic displacement parameter for the carbon atoms. ; _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^)+(0.0631P)^2^+4.5809P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 13892 _refine_ls_number_parameters 364 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0457 _refine_ls_R_factor_gt 0.0424 _refine_ls_wR_factor_ref 0.1207 _refine_ls_wR_factor_gt 0.1176 _refine_ls_goodness_of_fit_ref 1.068 _refine_ls_restrained_S_all 1.068 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Sm1 Sm 0.572602(10) 0.606999(11) 0.607707(9) 0.01933(5) Uani 1 1 d . . . Al1 Al 0.87998(8) 0.84753(9) 0.74468(7) 0.02834(18) Uani 1 1 d . . . Al2 Al 0.28500(7) 0.43457(8) 0.59098(7) 0.02356(16) Uani 1 1 d . . . O1 O 0.39628(17) 0.45440(17) 0.52668(15) 0.0229(4) Uani 1 1 d . . . N1 N 0.6372(2) 0.7470(2) 0.77611(19) 0.0283(5) Uani 1 1 d . . . N2 N 0.7103(2) 0.8050(2) 0.56353(19) 0.0262(5) Uani 1 1 d . . . N3 N 0.7653(2) 0.5975(2) 0.6762(2) 0.0296(5) Uani 1 1 d . . . N4 N 0.4935(3) 0.4756(2) 0.7332(2) 0.0312(5) Uani 1 1 d . . . N5 N 0.4164(2) 0.6819(2) 0.6005(2) 0.0279(5) Uani 1 1 d . . . C1 C 1.0406(3) 0.9713(4) 0.8132(3) 0.0490(10) Uani 1 1 d . . . H1A H 1.0639 0.9474 0.8741 0.059 Uiso 1 1 calc R . . H1B H 1.0990 0.9775 0.7741 0.059 Uiso 1 1 calc R . . C2 C 1.0488(7) 1.0932(6) 0.8356(5) 0.088(2) Uani 1 1 d . . . H2A H 1.0252 1.1177 0.7760 0.132 Uiso 1 1 calc R . . H2B H 1.1311 1.1495 0.8670 0.132 Uiso 1 1 calc R . . H2C H 0.9954 1.0896 0.8781 0.132 Uiso 1 1 calc R . . C3 C 0.1178(3) 0.3092(3) 0.5491(3) 0.0394(8) Uani 1 1 d . . . H3A H 0.0875 0.3121 0.4818 0.047 Uiso 1 1 calc R . . H3B H 0.1176 0.2331 0.5511 0.047 Uiso 1 1 calc R . . C4 C 0.0319(3) 0.3150(4) 0.6083(4) 0.0520(11) Uani 1 1 d . . . H4A H 0.0657 0.3219 0.6763 0.078 Uiso 1 1 calc R . . H4B H -0.0448 0.2439 0.5891 0.078 Uiso 1 1 calc R . . H4C H 0.0197 0.3829 0.5975 0.078 Uiso 1 1 calc R . . C11 C 0.7520(3) 0.8224(3) 0.8187(2) 0.0286(6) Uani 1 1 d . . . C12 C 0.7791(3) 0.8781(3) 0.9131(2) 0.0350(7) Uani 1 1 d . . . H12 H 0.8599 0.9293 0.9436 0.042 Uiso 1 1 calc R . . C13 C 0.6900(4) 0.8595(4) 0.9621(2) 0.0401(8) Uani 1 1 d . . . H13 H 0.7088 0.8982 1.0256 0.048 Uiso 1 1 calc R . . C14 C 0.5734(3) 0.7838(3) 0.9174(2) 0.0365(7) Uani 1 1 d . . . H14 H 0.5100 0.7693 0.9490 0.044 Uiso 1 1 calc R . . C15 C 0.5513(3) 0.7296(3) 0.8249(2) 0.0329(6) Uani 1 1 d . . . H15 H 0.4710 0.6772 0.7941 0.039 Uiso 1 1 calc R . . C21 C 0.8214(3) 0.8820(3) 0.6168(2) 0.0260(5) Uani 1 1 d . . . C22 C 0.8905(3) 0.9811(3) 0.5781(2) 0.0314(6) Uani 1 1 d . . . H22 H 0.9673 1.0359 0.6145 0.038 Uiso 1 1 calc R . . C23 C 0.8504(3) 1.0010(3) 0.4892(3) 0.0353(7) Uani 1 1 d . . . H23 H 0.8987 1.0682 0.4643 0.042 Uiso 1 1 calc R . . C24 C 0.7384(3) 0.9211(3) 0.4372(3) 0.0358(7) Uani 1 1 d . . . H24 H 0.7077 0.9320 0.3758 0.043 Uiso 1 1 calc R . . C25 C 0.6722(3) 0.8248(3) 0.4768(2) 0.0323(6) Uani 1 1 d . . . H25 H 0.5954 0.7695 0.4407 0.039 Uiso 1 1 calc R . . C31 C 0.8720(3) 0.6897(3) 0.7197(2) 0.0309(6) Uani 1 1 d . . . C32 C 0.9701(3) 0.6678(4) 0.7454(3) 0.0441(9) Uani 1 1 d . . . H32 H 1.0453 0.7305 0.7769 0.053 Uiso 1 1 calc R . . C33 C 0.9606(4) 0.5584(4) 0.7264(4) 0.0519(11) Uani 1 1 d . . . H33 H 1.0281 0.5459 0.7449 0.062 Uiso 1 1 calc R . . C34 C 0.8515(4) 0.4672(4) 0.6802(4) 0.0480(10) Uani 1 1 d . . . H34 H 0.8421 0.3909 0.6652 0.058 Uiso 1 1 calc R . . C35 C 0.7569(3) 0.4909(3) 0.6565(3) 0.0384(7) Uani 1 1 d . . . H35 H 0.6815 0.4287 0.6246 0.046 Uiso 1 1 calc R . . C41 C 0.3718(3) 0.4223(3) 0.7191(2) 0.0314(6) Uani 1 1 d . . . C42 C 0.3209(4) 0.3655(4) 0.7919(3) 0.0516(11) Uani 1 1 d . . . H42 H 0.2364 0.3268 0.7834 0.062 Uiso 1 1 calc R . . C43 C 0.3907(5) 0.3643(6) 0.8758(4) 0.0661(15) Uani 1 1 d . . . H43 H 0.3546 0.3263 0.9248 0.079 Uiso 1 1 calc R . . C44 C 0.5132(5) 0.4187(5) 0.8879(3) 0.0565(12) Uani 1 1 d . . . H44 H 0.5632 0.4186 0.9447 0.068 Uiso 1 1 calc R . . C45 C 0.5604(4) 0.4731(4) 0.8148(3) 0.0429(8) Uani 1 1 d . . . H45 H 0.6447 0.5110 0.8225 0.051 Uiso 1 1 calc R . . C51 C 0.3028(3) 0.5990(3) 0.5997(2) 0.0262(5) Uani 1 1 d . . . C52 C 0.2159(3) 0.6358(3) 0.6011(3) 0.0407(8) Uani 1 1 d . . . H52 H 0.1362 0.5794 0.5996 0.049 Uiso 1 1 calc R . . C53 C 0.2425(4) 0.7512(4) 0.6047(4) 0.0492(10) Uani 1 1 d . . . H53 H 0.1818 0.7738 0.6057 0.059 Uiso 1 1 calc R . . C54 C 0.3578(4) 0.8340(4) 0.6066(4) 0.0464(9) Uani 1 1 d . . . H54 H 0.3788 0.9143 0.6085 0.056 Uiso 1 1 calc R . . C55 C 0.4418(3) 0.7944(3) 0.6056(3) 0.0393(8) Uani 1 1 d . . . H55 H 0.5222 0.8504 0.6088 0.047 Uiso 1 1 calc R . . C60 C 0.5182(9) 0.9106(9) 0.1441(7) 0.1114(8) Uiso 1 1 d . . . H60A H 0.5601 0.8641 0.1567 0.167 Uiso 1 1 calc R . . H60B H 0.5768 0.9930 0.1510 0.167 Uiso 1 1 calc R . . H60C H 0.4690 0.8845 0.0789 0.167 Uiso 1 1 calc R . . C61 C 0.4435(6) 0.8965(6) 0.2110(4) 0.1114(8) Uiso 1 1 d G . . C62 C 0.4466(5) 0.8298(6) 0.2824(5) 0.1114(8) Uiso 1 1 d G . . H62 H 0.4940 0.7908 0.2840 0.134 Uiso 1 1 calc R . . C63 C 0.3804(6) 0.8203(5) 0.3516(4) 0.1114(8) Uiso 1 1 d G . . H63 H 0.3825 0.7748 0.4005 0.134 Uiso 1 1 calc R . . C64 C 0.3110(6) 0.8774(6) 0.3494(4) 0.1114(8) Uiso 1 1 d G . . H64 H 0.2658 0.8709 0.3967 0.134 Uiso 1 1 calc R . . C65 C 0.3079(6) 0.9441(6) 0.2779(5) 0.1114(8) Uiso 1 1 d G . . H65 H 0.2605 0.9831 0.2764 0.134 Uiso 1 1 calc R . . C66 C 0.3741(6) 0.9536(6) 0.2088(4) 0.1114(8) Uiso 1 1 d G . . H66 H 0.3720 0.9992 0.1599 0.134 Uiso 1 1 calc R . . C70 C 0.1409(9) 0.4063(9) -0.0210(7) 0.1114(8) Uiso 1 1 d . . . H70A H 0.0917 0.3850 0.0268 0.167 Uiso 1 1 calc R . . H70B H 0.2087 0.3905 -0.0024 0.167 Uiso 1 1 calc R . . H70C H 0.0927 0.3602 -0.0834 0.167 Uiso 1 1 calc R . . C71 C 0.1810(6) 0.5190(4) -0.0263(5) 0.1114(8) Uiso 1 1 d G . . C72 C 0.1615(6) 0.5849(6) 0.0420(4) 0.1114(8) Uiso 1 1 d G . . H72 H 0.1307 0.5518 0.0947 0.134 Uiso 1 1 calc R . . C73 C 0.1869(6) 0.6993(6) 0.0333(4) 0.1114(8) Uiso 1 1 d G . . H73 H 0.1736 0.7443 0.0799 0.134 Uiso 1 1 calc R . . C74 C 0.2320(6) 0.7477(4) -0.0438(5) 0.1114(8) Uiso 1 1 d G . . H74 H 0.2494 0.8259 -0.0498 0.134 Uiso 1 1 calc R . . C75 C 0.2515(6) 0.6818(6) -0.1121(4) 0.1114(8) Uiso 1 1 d G . . H75 H 0.2823 0.7149 -0.1648 0.134 Uiso 1 1 calc R . . C76 C 0.2261(6) 0.5675(6) -0.1034(4) 0.1114(8) Uiso 1 1 d G . . H76 H 0.2394 0.5224 -0.1500 0.134 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 Sm1 0.01432(7) 0.01774(7) 0.02168(7) 0.00037(4) 0.00308(4) 0.00448(5) Al1 0.0194(4) 0.0268(4) 0.0289(4) -0.0007(3) 0.0016(3) 0.0040(3) Al2 0.0166(3) 0.0210(4) 0.0296(4) 0.0021(3) 0.0087(3) 0.0048(3) O1 0.0154(8) 0.0218(9) 0.0267(9) 0.0002(7) 0.0063(7) 0.0044(7) N1 0.0275(12) 0.0278(12) 0.0248(11) -0.0013(9) 0.0046(9) 0.0099(10) N2 0.0223(11) 0.0208(10) 0.0301(12) 0.0028(9) 0.0065(9) 0.0055(9) N3 0.0230(11) 0.0318(13) 0.0335(13) 0.0012(10) 0.0023(9) 0.0143(10) N4 0.0310(13) 0.0297(12) 0.0302(12) 0.0105(10) 0.0079(10) 0.0106(10) N5 0.0237(11) 0.0229(11) 0.0351(13) -0.0003(9) 0.0032(9) 0.0108(9) C1 0.0280(16) 0.048(2) 0.045(2) -0.0022(17) -0.0034(15) 0.0005(15) C2 0.078(4) 0.059(3) 0.072(4) 0.000(3) -0.011(3) -0.004(3) C3 0.0192(13) 0.0349(16) 0.052(2) -0.0067(14) 0.0141(13) 0.0015(12) C4 0.0260(16) 0.042(2) 0.078(3) -0.005(2) 0.0241(18) 0.0042(14) C11 0.0341(15) 0.0237(12) 0.0214(12) 0.0014(10) 0.0016(10) 0.0095(11) C12 0.0350(16) 0.0360(16) 0.0257(13) -0.0004(12) 0.0019(12) 0.0117(13) C13 0.048(2) 0.046(2) 0.0216(13) 0.0002(13) 0.0065(13) 0.0196(17) C14 0.0391(17) 0.0445(19) 0.0282(14) 0.0049(13) 0.0137(13) 0.0195(15) C15 0.0306(15) 0.0348(16) 0.0291(14) 0.0020(12) 0.0080(12) 0.0117(13) C21 0.0224(12) 0.0213(12) 0.0308(13) -0.0002(10) 0.0072(10) 0.0072(10) C22 0.0239(13) 0.0245(13) 0.0382(16) 0.0027(11) 0.0087(11) 0.0046(11) C23 0.0345(16) 0.0249(14) 0.0447(18) 0.0113(13) 0.0155(14) 0.0094(12) C24 0.0347(16) 0.0336(16) 0.0381(16) 0.0125(13) 0.0083(13) 0.0142(13) C25 0.0273(14) 0.0277(14) 0.0342(15) 0.0044(11) 0.0019(12) 0.0080(11) C31 0.0234(13) 0.0370(16) 0.0309(14) 0.0019(12) 0.0029(11) 0.0144(12) C32 0.0234(14) 0.048(2) 0.055(2) -0.0015(17) -0.0015(14) 0.0169(15) C33 0.0333(18) 0.061(3) 0.068(3) 0.003(2) 0.0016(18) 0.0321(19) C34 0.043(2) 0.048(2) 0.063(3) 0.0017(19) 0.0062(18) 0.0322(19) C35 0.0303(15) 0.0357(17) 0.0484(19) -0.0009(14) 0.0004(14) 0.0184(14) C41 0.0335(15) 0.0295(14) 0.0332(14) 0.0119(12) 0.0143(12) 0.0133(12) C42 0.040(2) 0.065(3) 0.051(2) 0.035(2) 0.0227(18) 0.0184(19) C43 0.062(3) 0.090(4) 0.054(3) 0.050(3) 0.026(2) 0.033(3) C44 0.057(3) 0.075(3) 0.042(2) 0.032(2) 0.0123(19) 0.030(2) C45 0.0385(18) 0.050(2) 0.0374(18) 0.0177(16) 0.0060(14) 0.0177(17) C51 0.0228(12) 0.0269(13) 0.0279(13) 0.0016(10) 0.0060(10) 0.0110(10) C52 0.0297(15) 0.0382(18) 0.061(2) 0.0068(16) 0.0175(15) 0.0190(14) C53 0.042(2) 0.046(2) 0.073(3) 0.009(2) 0.016(2) 0.0309(18) C54 0.050(2) 0.0317(17) 0.066(3) 0.0095(17) 0.0129(19) 0.0259(17) C55 0.0349(17) 0.0232(14) 0.059(2) 0.0055(14) 0.0118(16) 0.0128(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 Sm1 O1 2.209(2) 2_666 ? Sm1 O1 2.2827(19) . ? Sm1 N3 2.564(3) . ? Sm1 N4 2.577(3) . ? Sm1 N2 2.578(2) . ? Sm1 N5 2.585(3) . ? Sm1 N1 2.697(3) . ? Sm1 Al2 3.3057(8) . ? Sm1 Sm1 3.6226(3) 2_666 ? Al1 C1 1.988(4) . ? Al1 C31 2.013(4) . ? Al1 C21 2.020(3) . ? Al1 C11 2.023(4) . ? Al2 O1 1.762(2) . ? Al2 C3 1.982(3) . ? Al2 C51 2.038(3) . ? Al2 C41 2.039(3) . ? O1 Sm1 2.209(2) 2_666 ? N1 C15 1.348(4) . ? N1 C11 1.353(4) . ? N2 C25 1.344(4) . ? N2 C21 1.370(4) . ? N3 C35 1.347(4) . ? N3 C31 1.360(4) . ? N4 C45 1.342(4) . ? N4 C41 1.367(4) . ? N5 C55 1.341(4) . ? N5 C51 1.368(4) . ? C1 C2 1.549(9) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 C4 1.526(5) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C11 C12 1.405(4) . ? C12 C13 1.381(5) . ? C12 H12 0.9500 . ? C13 C14 1.378(6) . ? C13 H13 0.9500 . ? C14 C15 1.385(5) . ? C14 H14 0.9500 . ? C15 H15 0.9500 . ? C21 C22 1.408(4) . ? C22 C23 1.380(5) . ? C22 H22 0.9500 . ? C23 C24 1.381(5) . ? C23 H23 0.9500 . ? C24 C25 1.382(5) . ? C24 H24 0.9500 . ? C25 H25 0.9500 . ? C31 C32 1.409(5) . ? C32 C33 1.376(6) . ? C32 H32 0.9500 . ? C33 C34 1.381(7) . ? C33 H33 0.9500 . ? C34 C35 1.378(5) . ? C34 H34 0.9500 . ? C35 H35 0.9500 . ? C41 C42 1.400(5) . ? C42 C43 1.381(7) . ? C42 H42 0.9500 . ? C43 C44 1.378(7) . ? C43 H43 0.9500 . ? C44 C45 1.376(6) . ? C44 H44 0.9500 . ? C45 H45 0.9500 . ? C51 C52 1.400(4) . ? C52 C53 1.376(6) . ? C52 H52 0.9500 . ? C53 C54 1.380(6) . ? C53 H53 0.9500 . ? C54 C55 1.390(5) . ? C54 H54 0.9500 . ? C55 H55 0.9500 . ? C60 C61 1.434(10) . ? C60 H60A 0.9800 . ? C60 H60B 0.9800 . ? C60 H60C 0.9800 . ? C61 C62 1.3900 . ? C61 C66 1.3900 . ? C62 C63 1.3900 . ? C62 H62 0.9500 . ? C63 C64 1.3900 . ? C63 H63 0.9500 . ? C64 C65 1.3900 . ? C64 H64 0.9500 . ? C65 C66 1.3900 . ? C65 H65 0.9500 . ? C66 H66 0.9500 . ? C70 C71 1.330(10) . ? C70 H70A 0.9800 . ? C70 H70B 0.9800 . ? C70 H70C 0.9800 . ? C71 C72 1.3900 . ? C71 C76 1.3900 . ? C72 C73 1.3900 . ? C72 H72 0.9500 . ? C73 C74 1.3900 . ? C73 H73 0.9500 . ? C74 C75 1.3900 . ? C74 H74 0.9500 . ? C75 C76 1.3900 . ? C75 H75 0.9500 . ? C76 H76 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Sm1 O1 72.49(8) 2_666 . ? O1 Sm1 N3 81.16(8) 2_666 . ? O1 Sm1 N3 126.15(8) . . ? O1 Sm1 N4 123.58(9) 2_666 . ? O1 Sm1 N4 74.86(8) . . ? N3 Sm1 N4 82.66(9) . . ? O1 Sm1 N2 80.45(8) 2_666 . ? O1 Sm1 N2 132.40(8) . . ? N3 Sm1 N2 85.79(9) . . ? N4 Sm1 N2 150.93(9) . . ? O1 Sm1 N5 119.46(8) 2_666 . ? O1 Sm1 N5 74.67(8) . . ? N3 Sm1 N5 156.20(9) . . ? N4 Sm1 N5 93.71(9) . . ? N2 Sm1 N5 86.24(8) . . ? O1 Sm1 N1 154.46(8) 2_666 . ? O1 Sm1 N1 133.04(8) . . ? N3 Sm1 N1 81.73(9) . . ? N4 Sm1 N1 72.49(9) . . ? N2 Sm1 N1 79.51(8) . . ? N5 Sm1 N1 74.77(8) . . ? O1 Sm1 Al2 102.74(5) 2_666 . ? O1 Sm1 Al2 30.28(5) . . ? N3 Sm1 Al2 134.76(7) . . ? N4 Sm1 Al2 57.31(7) . . ? N2 Sm1 Al2 139.45(6) . . ? N5 Sm1 Al2 56.60(6) . . ? N1 Sm1 Al2 102.78(6) . . ? O1 Sm1 Sm1 36.94(5) 2_666 2_666 ? O1 Sm1 Sm1 35.56(5) . 2_666 ? N3 Sm1 Sm1 106.14(6) . 2_666 ? N4 Sm1 Sm1 99.94(7) . 2_666 ? N2 Sm1 Sm1 108.89(6) . 2_666 ? N5 Sm1 Sm1 97.66(6) . 2_666 ? N1 Sm1 Sm1 168.59(6) . 2_666 ? Al2 Sm1 Sm1 65.814(16) . 2_666 ? C1 Al1 C31 113.42(18) . . ? C1 Al1 C21 113.36(17) . . ? C31 Al1 C21 106.49(13) . . ? C1 Al1 C11 112.85(17) . . ? C31 Al1 C11 104.56(14) . . ? C21 Al1 C11 105.38(13) . . ? O1 Al2 C3 123.19(13) . . ? O1 Al2 C51 98.15(11) . . ? C3 Al2 C51 114.31(15) . . ? O1 Al2 C41 97.73(12) . . ? C3 Al2 C41 113.61(17) . . ? C51 Al2 C41 107.42(13) . . ? O1 Al2 Sm1 40.78(7) . . ? C3 Al2 Sm1 163.93(11) . . ? C51 Al2 Sm1 74.89(9) . . ? C41 Al2 Sm1 73.62(9) . . ? Al2 O1 Sm1 143.44(11) . 2_666 ? Al2 O1 Sm1 108.93(10) . . ? Sm1 O1 Sm1 107.51(8) 2_666 . ? C15 N1 C11 118.7(3) . . ? C15 N1 Sm1 117.2(2) . . ? C11 N1 Sm1 123.5(2) . . ? C25 N2 C21 119.6(3) . . ? C25 N2 Sm1 115.2(2) . . ? C21 N2 Sm1 124.8(2) . . ? C35 N3 C31 120.3(3) . . ? C35 N3 Sm1 113.5(2) . . ? C31 N3 Sm1 125.9(2) . . ? C45 N4 C41 120.3(3) . . ? C45 N4 Sm1 125.4(2) . . ? C41 N4 Sm1 113.2(2) . . ? C55 N5 C51 119.9(3) . . ? C55 N5 Sm1 124.6(2) . . ? C51 N5 Sm1 115.27(19) . . ? C2 C1 Al1 114.6(4) . . ? C2 C1 H1A 108.6 . . ? Al1 C1 H1A 108.6 . . ? C2 C1 H1B 108.6 . . ? Al1 C1 H1B 108.6 . . ? H1A C1 H1B 107.6 . . ? C1 C2 H2A 109.5 . . ? C1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C4 C3 Al2 115.1(3) . . ? C4 C3 H3A 108.5 . . ? Al2 C3 H3A 108.5 . . ? C4 C3 H3B 108.5 . . ? Al2 C3 H3B 108.5 . . ? H3A C3 H3B 107.5 . . ? C3 C4 H4A 109.5 . . ? C3 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C3 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? N1 C11 C12 119.6(3) . . ? N1 C11 Al1 118.3(2) . . ? C12 C11 Al1 122.1(3) . . ? C13 C12 C11 121.0(3) . . ? C13 C12 H12 119.5 . . ? C11 C12 H12 119.5 . . ? C14 C13 C12 118.9(3) . . ? C14 C13 H13 120.6 . . ? C12 C13 H13 120.6 . . ? C13 C14 C15 118.0(3) . . ? C13 C14 H14 121.0 . . ? C15 C14 H14 121.0 . . ? N1 C15 C14 123.8(3) . . ? N1 C15 H15 118.1 . . ? C14 C15 H15 118.1 . . ? N2 C21 C22 117.8(3) . . ? N2 C21 Al1 119.1(2) . . ? C22 C21 Al1 123.0(2) . . ? C23 C22 C21 122.1(3) . . ? C23 C22 H22 118.9 . . ? C21 C22 H22 118.9 . . ? C22 C23 C24 118.5(3) . . ? C22 C23 H23 120.8 . . ? C24 C23 H23 120.8 . . ? C23 C24 C25 118.3(3) . . ? C23 C24 H24 120.9 . . ? C25 C24 H24 120.9 . . ? N2 C25 C24 123.6(3) . . ? N2 C25 H25 118.2 . . ? C24 C25 H25 118.2 . . ? N3 C31 C32 117.3(3) . . ? N3 C31 Al1 118.6(2) . . ? C32 C31 Al1 124.2(3) . . ? C33 C32 C31 122.2(4) . . ? C33 C32 H32 118.9 . . ? C31 C32 H32 118.9 . . ? C32 C33 C34 119.0(3) . . ? C32 C33 H33 120.5 . . ? C34 C33 H33 120.5 . . ? C35 C34 C33 117.6(4) . . ? C35 C34 H34 121.2 . . ? C33 C34 H34 121.2 . . ? N3 C35 C34 123.6(4) . . ? N3 C35 H35 118.2 . . ? C34 C35 H35 118.2 . . ? N4 C41 C42 117.7(3) . . ? N4 C41 Al2 114.8(2) . . ? C42 C41 Al2 127.5(3) . . ? C43 C42 C41 121.5(4) . . ? C43 C42 H42 119.3 . . ? C41 C42 H42 119.3 . . ? C44 C43 C42 119.5(4) . . ? C44 C43 H43 120.2 . . ? C42 C43 H43 120.2 . . ? C45 C44 C43 117.6(4) . . ? C45 C44 H44 121.2 . . ? C43 C44 H44 121.2 . . ? N4 C45 C44 123.5(4) . . ? N4 C45 H45 118.3 . . ? C44 C45 H45 118.3 . . ? N5 C51 C52 117.7(3) . . ? N5 C51 Al2 113.0(2) . . ? C52 C51 Al2 129.3(2) . . ? C53 C52 C51 122.0(3) . . ? C53 C52 H52 119.0 . . ? C51 C52 H52 119.0 . . ? C52 C53 C54 119.6(3) . . ? C52 C53 H53 120.2 . . ? C54 C53 H53 120.2 . . ? C53 C54 C55 116.8(3) . . ? C53 C54 H54 121.6 . . ? C55 C54 H54 121.6 . . ? N5 C55 C54 124.0(4) . . ? N5 C55 H55 118.0 . . ? C54 C55 H55 118.0 . . ? C61 C60 H60A 109.5 . . ? C61 C60 H60B 109.5 . . ? H60A C60 H60B 109.5 . . ? C61 C60 H60C 109.5 . . ? H60A C60 H60C 109.5 . . ? H60B C60 H60C 109.5 . . ? C62 C61 C66 120.0 . . ? C62 C61 C60 118.8(6) . . ? C66 C61 C60 121.1(6) . . ? C61 C62 C63 120.0 . . ? C61 C62 H62 120.0 . . ? C63 C62 H62 120.0 . . ? C64 C63 C62 120.0 . . ? C64 C63 H63 120.0 . . ? C62 C63 H63 120.0 . . ? C65 C64 C63 120.0 . . ? C65 C64 H64 120.0 . . ? C63 C64 H64 120.0 . . ? C64 C65 C66 120.0 . . ? C64 C65 H65 120.0 . . ? C66 C65 H65 120.0 . . ? C65 C66 C61 120.0 . . ? C65 C66 H66 120.0 . . ? C61 C66 H66 120.0 . . ? C71 C70 H70A 109.5 . . ? C71 C70 H70B 109.5 . . ? H70A C70 H70B 109.5 . . ? C71 C70 H70C 109.5 . . ? H70A C70 H70C 109.5 . . ? H70B C70 H70C 109.5 . . ? C70 C71 C72 117.2(7) . . ? C70 C71 C76 122.3(7) . . ? C72 C71 C76 120.0 . . ? C73 C72 C71 120.0 . . ? C73 C72 H72 120.0 . . ? C71 C72 H72 120.0 . . ? C72 C73 C74 120.0 . . ? C72 C73 H73 120.0 . . ? C74 C73 H73 120.0 . . ? C73 C74 C75 120.0 . . ? C73 C74 H74 120.0 . . ? C75 C74 H74 120.0 . . ? C74 C75 C76 120.0 . . ? C74 C75 H75 120.0 . . ? C76 C75 H75 120.0 . . ? C75 C76 C71 120.0 . . ? C75 C76 H76 120.0 . . ? C71 C76 H76 120.0 . . ? _diffrn_measured_fraction_theta_max 0.958 _diffrn_reflns_theta_full 32.02 _diffrn_measured_fraction_theta_full 0.958 _refine_diff_density_max 3.459 _refine_diff_density_min -2.165 _refine_diff_density_rms 0.141 #===END data_dw1072 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C54 H52 Al4 N10 O2 Sm2,4(C4 H8 O)' _chemical_formula_sum 'C70 H84 Al4 N10 O6 Sm2' _chemical_formula_weight 1570.09 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' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 'triclinic' _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.73690(10) _cell_length_b 13.0219(2) _cell_length_c 13.3823(3) _cell_angle_alpha 105.8620(10) _cell_angle_beta 94.2120(10) _cell_angle_gamma 118.2890(10) _cell_volume 1825.28(5) _cell_formula_units_Z 1 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 15231 _cell_measurement_theta_min 1.00 _cell_measurement_theta_max 32.03 _exptl_crystal_description 'block' _exptl_crystal_colour 'colourless' _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.428 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 798 _exptl_absorpt_coefficient_mu 1.696 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_correction_T_min 0.834 _exptl_absorpt_correction_T_max 0.970 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements Sortav (Blessing 1995) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 180(2) _diffrn_raiation_monochromator graphite _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_measurement_method 'Thin slice \w and \f scans' _diffrn_standards_number 0 _diffrn_reflns_number 25758 _diffrn_reflns_av_R_equivalents 0.0547 _diffrn_reflns_av_sigmaI/netI 0.0784 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 3.56 _diffrn_reflns_theta_max 32.00 _reflns_number_total 12480 _reflns_number_gt 9293 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius B.V. 1998)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction ; HKL Denzo and Scalepack (Otwinowski & Minor 1997) ; _computing_structure_solution 'SIR-92 (Altomare et al. 1994)' _computing_structure_refinement 'SHELXL-97 (Sheldrick 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0385P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 12480 _refine_ls_number_parameters 405 _refine_ls_number_restraints 10 _refine_ls_R_factor_all 0.0595 _refine_ls_R_factor_gt 0.0381 _refine_ls_wR_factor_ref 0.0915 _refine_ls_wR_factor_gt 0.0848 _refine_ls_goodness_of_fit_ref 1.000 _refine_ls_restrained_S_all 1.013 _refine_ls_shift/su_max 0.005 _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 1.005849(12) 0.044148(13) 0.882867(11) 0.02663(5) Uani 1 1 d . . . Al1 Al 1.23481(8) 0.24109(9) 0.74950(7) 0.03584(19) Uani 1 1 d . . . Al2 Al 0.72560(7) -0.11387(8) 0.91397(7) 0.03255(18) Uani 1 1 d . . . C1 C 1.3566(3) 0.3468(4) 0.6838(3) 0.0576(10) Uani 1 1 d . . . H1A H 1.3429 0.4142 0.6816 0.086 Uiso 1 1 calc R . . H1B H 1.3475 0.2962 0.6108 0.086 Uiso 1 1 calc R . . H1C H 1.4396 0.3823 0.7263 0.086 Uiso 1 1 calc R . . C2 C 0.5817(3) -0.2101(3) 0.9646(3) 0.0483(8) Uani 1 1 d . . . H2A H 0.5820 -0.1563 1.0322 0.072 Uiso 1 1 calc R . . H2B H 0.5848 -0.2800 0.9758 0.072 Uiso 1 1 calc R . . H2C H 0.5067 -0.2420 0.9111 0.072 Uiso 1 1 calc R . . O1 O 0.87809(16) -0.04927(18) 0.98208(15) 0.0297(4) Uani 1 1 d . . . N1 N 0.9691(2) 0.0794(2) 0.7010(2) 0.0373(5) Uani 1 1 d . . . C11 C 1.0586(3) 0.1560(3) 0.6650(2) 0.0339(6) Uani 1 1 d . . . C12 C 1.0312(3) 0.1736(3) 0.5706(3) 0.0471(8) Uani 1 1 d . . . H12 H 1.0954 0.2296 0.5468 0.057 Uiso 1 1 calc R . . C13 C 0.9106(3) 0.1098(4) 0.5110(3) 0.0516(9) Uani 1 1 d . . . H13 H 0.8917 0.1203 0.4459 0.062 Uiso 1 1 calc R . . C14 C 0.8202(3) 0.0318(3) 0.5483(3) 0.0502(8) Uani 1 1 d . . . H14 H 0.7368 -0.0129 0.5098 0.060 Uiso 1 1 calc R . . C15 C 0.8522(3) 0.0192(3) 0.6428(3) 0.0469(8) Uani 1 1 d . . . H15 H 0.7886 -0.0348 0.6685 0.056 Uiso 1 1 calc R . . N2 N 1.1612(2) 0.2787(2) 0.95340(19) 0.0344(5) Uani 1 1 d . . . C21 C 1.2461(3) 0.3370(3) 0.9011(2) 0.0343(6) Uani 1 1 d . . . C22 C 1.3404(3) 0.4610(3) 0.9573(3) 0.0439(7) Uani 1 1 d . . . H22 H 1.3990 0.5040 0.9216 0.053 Uiso 1 1 calc R . . C23 C 1.3500(3) 0.5218(3) 1.0626(3) 0.0531(9) Uani 1 1 d . . . H23 H 1.4156 0.6048 1.0998 0.064 Uiso 1 1 calc R . . C24 C 1.2629(4) 0.4599(3) 1.1128(3) 0.0517(9) Uani 1 1 d . . . H24 H 1.2665 0.4989 1.1852 0.062 Uiso 1 1 calc R . . C25 C 1.1704(3) 0.3398(3) 1.0550(3) 0.0425(7) Uani 1 1 d . . . H25 H 1.1093 0.2976 1.0893 0.051 Uiso 1 1 calc R . . N3 N 1.1689(2) 0.0134(2) 0.79575(19) 0.0354(5) Uani 1 1 d . . . C31 C 1.2524(3) 0.0981(3) 0.7589(2) 0.0355(6) Uani 1 1 d . . . C32 C 1.3473(3) 0.0810(3) 0.7277(3) 0.0480(8) Uani 1 1 d . . . H32 H 1.4068 0.1398 0.7025 0.058 Uiso 1 1 calc R . . C33 C 1.3566(4) -0.0191(4) 0.7326(3) 0.0582(10) Uani 1 1 d . . . H33 H 1.4205 -0.0303 0.7096 0.070 Uiso 1 1 calc R . . C34 C 1.2726(4) -0.1010(4) 0.7708(3) 0.0598(10) Uani 1 1 d . . . H34 H 1.2772 -0.1702 0.7758 0.072 Uiso 1 1 calc R . . C35 C 1.1802(3) -0.0825(3) 0.8024(3) 0.0468(8) Uani 1 1 d . . . H35 H 1.1224 -0.1396 0.8300 0.056 Uiso 1 1 calc R . . N4 N 0.8447(2) -0.1776(2) 0.7522(2) 0.0378(5) Uani 1 1 d . . . C41 C 0.7312(3) -0.2203(3) 0.7737(2) 0.0371(6) Uani 1 1 d . . . C42 C 0.6344(3) -0.3355(3) 0.7047(3) 0.0491(8) Uani 1 1 d . . . H42 H 0.5549 -0.3658 0.7185 0.059 Uiso 1 1 calc R . . C43 C 0.6504(4) -0.4059(4) 0.6182(3) 0.0581(9) Uani 1 1 d . . . H43 H 0.5832 -0.4846 0.5729 0.070 Uiso 1 1 calc R . . C44 C 0.7662(4) -0.3613(3) 0.5971(3) 0.0574(9) Uani 1 1 d . . . H44 H 0.7802 -0.4074 0.5367 0.069 Uiso 1 1 calc R . . C45 C 0.8596(3) -0.2479(3) 0.6670(3) 0.0484(8) Uani 1 1 d . . . H45 H 0.9395 -0.2174 0.6542 0.058 Uiso 1 1 calc R . . N5 N 0.8549(2) 0.1252(2) 0.8920(2) 0.0395(6) Uani 1 1 d . . . C51 C 0.7395(3) 0.0421(3) 0.8976(2) 0.0386(7) Uani 1 1 d . . . C52 C 0.6498(3) 0.0746(4) 0.8955(3) 0.0569(10) Uani 1 1 d . . . H52 H 0.5695 0.0176 0.8987 0.068 Uiso 1 1 calc R . . C53 C 0.6750(4) 0.1878(4) 0.8888(4) 0.0679(12) Uani 1 1 d . . . H53 H 0.6138 0.2098 0.8900 0.081 Uiso 1 1 calc R . . C54 C 0.7909(4) 0.2685(4) 0.8802(4) 0.0660(12) Uani 1 1 d . . . H54 H 0.8102 0.3457 0.8730 0.079 Uiso 1 1 calc R . . C55 C 0.8775(3) 0.2335(3) 0.8825(3) 0.0520(9) Uani 1 1 d . . . H55 H 0.9573 0.2889 0.8771 0.062 Uiso 1 1 calc R . . O1T O 0.5070(6) 0.8050(7) 0.5602(6) 0.204(3) Uani 0.50 1 d P A 1 C1T C 0.3891(7) 0.7146(6) 0.5736(6) 0.118(2) Uani 0.50 1 d PD A 1 H1T1 H 0.3903 0.6379 0.5688 0.142 Uiso 0.50 1 calc PR A 1 H1T2 H 0.3810 0.7492 0.6463 0.142 Uiso 0.50 1 calc PR A 1 C2T C 0.2882(13) 0.6830(17) 0.5011(12) 0.126(3) Uiso 0.50 1 d PD A 1 H2T1 H 0.2406 0.7194 0.5336 0.152 Uiso 0.50 1 calc PR A 1 H2T2 H 0.2339 0.5916 0.4667 0.152 Uiso 0.50 1 calc PR A 1 C3T C 0.3500(13) 0.7413(15) 0.4254(13) 0.137(4) Uiso 0.50 1 d PD A 1 H3T1 H 0.3410 0.6747 0.3617 0.164 Uiso 0.50 1 calc PR A 1 H3T2 H 0.3062 0.7793 0.4015 0.164 Uiso 0.50 1 calc PR A 1 C4T C 0.4769(11) 0.8339(12) 0.4650(10) 0.096(3) Uiso 0.50 1 d PD A 1 H4T1 H 0.4903 0.9191 0.4858 0.115 Uiso 0.50 1 calc PR A 1 H4T2 H 0.5251 0.8240 0.4122 0.115 Uiso 0.50 1 calc PR A 1 O1T' O 0.5070(6) 0.8050(7) 0.5602(6) 0.204(3) Uani 0.50 1 d P B 2 C1T' C 0.3891(7) 0.7146(6) 0.5736(6) 0.118(2) Uani 0.50 1 d PD B 2 H1T3 H 0.3769 0.7417 0.6462 0.142 Uiso 0.50 1 calc PR B 2 H1T4 H 0.3770 0.6301 0.5549 0.142 Uiso 0.50 1 calc PR B 2 C2T' C 0.3077(14) 0.7253(16) 0.4863(13) 0.126(3) Uiso 0.50 1 d PD B 2 H2T3 H 0.2576 0.6432 0.4282 0.152 Uiso 0.50 1 calc PR B 2 H2T4 H 0.2509 0.7476 0.5193 0.152 Uiso 0.50 1 calc PR B 2 C3T' C 0.3817(16) 0.8182(16) 0.4409(14) 0.137(4) Uiso 0.50 1 d PD B 2 H3T3 H 0.3902 0.7797 0.3696 0.164 Uiso 0.50 1 calc PR B 2 H3T4 H 0.3484 0.8722 0.4363 0.164 Uiso 0.50 1 calc PR B 2 C4T' C 0.4954(11) 0.8845(12) 0.5208(11) 0.096(3) Uiso 0.50 1 d P B 2 H4T3 H 0.5651 0.9238 0.4888 0.115 Uiso 0.50 1 calc PR B 2 H4T4 H 0.4964 0.9511 0.5793 0.115 Uiso 0.50 1 calc PR B 2 O1S O 0.9706(10) 0.4387(11) 0.3445(9) 0.142(3) Uiso 0.50 1 d P C 1 C1S C 0.8300(10) 0.4509(9) 0.3075(14) 0.239(7) Uani 0.50 1 d P C 1 H1S1 H 0.7532 0.3702 0.2699 0.286 Uiso 0.50 1 calc PR C 1 H1S2 H 0.8174 0.5060 0.3664 0.286 Uiso 0.50 1 calc PR C 1 C2S C 0.9004(19) 0.5121(17) 0.2360(16) 0.146(4) Uiso 0.50 1 d P C 1 H2S1 H 0.8503 0.5291 0.1902 0.175 Uiso 0.50 1 calc PR C 1 H2S2 H 0.9765 0.5916 0.2783 0.175 Uiso 0.50 1 calc PR C 1 C3S C 0.9295(14) 0.4217(12) 0.1700(9) 0.225(6) Uani 0.50 1 d P C 1 H3S1 H 0.8598 0.3345 0.1417 0.270 Uiso 0.50 1 calc PR C 1 H3S2 H 0.9700 0.4462 0.1132 0.270 Uiso 0.50 1 calc PR C 1 C4S C 1.0029(9) 0.4483(16) 0.2551(10) 0.248(8) Uani 0.50 1 d P C 1 H4S1 H 1.0695 0.5358 0.2729 0.298 Uiso 0.50 1 calc PR C 1 H4S2 H 1.0407 0.3967 0.2358 0.298 Uiso 0.50 1 calc PR C 1 O1S' O 0.9359(13) 0.5043(11) 0.3512(9) 0.142(3) Uiso 0.50 1 d P D 2 C1S' C 0.8300(10) 0.4509(9) 0.3075(14) 0.239(7) Uani 0.50 1 d P D 2 H1S3 H 0.7926 0.5011 0.3353 0.286 Uiso 0.50 1 calc PR D 2 H1S4 H 0.7841 0.3694 0.3169 0.286 Uiso 0.50 1 calc PR D 2 C2S' C 0.832(2) 0.4344(19) 0.1915(17) 0.146(4) Uiso 0.50 1 d P D 2 H2S3 H 0.7540 0.3595 0.1448 0.175 Uiso 0.50 1 calc PR D 2 H2S4 H 0.8386 0.5076 0.1767 0.175 Uiso 0.50 1 calc PR D 2 C3S' C 0.9295(14) 0.4217(12) 0.1700(9) 0.225(6) Uani 0.50 1 d P D 2 H3S3 H 0.8989 0.3348 0.1235 0.270 Uiso 0.50 1 calc PR D 2 H3S4 H 0.9740 0.4771 0.1308 0.270 Uiso 0.50 1 calc PR D 2 C4S' C 1.0029(9) 0.4483(16) 0.2551(10) 0.248(8) Uani 0.50 1 d P D 2 H4S3 H 1.0879 0.5134 0.2604 0.298 Uiso 0.50 1 calc PR D 2 H4S4 H 1.0024 0.3740 0.2611 0.298 Uiso 0.50 1 calc PR D 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Sm1 0.02110(7) 0.02828(8) 0.02946(7) 0.01483(6) 0.00787(5) 0.00920(5) Al1 0.0267(4) 0.0395(5) 0.0366(5) 0.0201(4) 0.0095(4) 0.0097(4) Al2 0.0200(4) 0.0362(5) 0.0374(5) 0.0184(4) 0.0067(3) 0.0086(4) C1 0.0361(18) 0.065(2) 0.058(2) 0.034(2) 0.0160(17) 0.0091(18) C2 0.0241(14) 0.053(2) 0.054(2) 0.0243(17) 0.0131(14) 0.0062(14) O1 0.0204(9) 0.0362(10) 0.0327(10) 0.0170(9) 0.0094(8) 0.0117(8) N1 0.0279(12) 0.0454(15) 0.0363(13) 0.0225(12) 0.0076(10) 0.0129(12) C11 0.0398(16) 0.0347(15) 0.0308(14) 0.0148(12) 0.0112(12) 0.0197(14) C12 0.0447(18) 0.052(2) 0.0425(18) 0.0280(16) 0.0101(15) 0.0169(16) C13 0.0451(19) 0.067(2) 0.0422(18) 0.0314(18) 0.0061(15) 0.0225(19) C14 0.0334(16) 0.060(2) 0.0449(18) 0.0270(17) 0.0005(14) 0.0117(16) C15 0.0299(15) 0.057(2) 0.0451(18) 0.0290(16) 0.0042(13) 0.0102(15) N2 0.0344(13) 0.0296(12) 0.0373(13) 0.0146(11) 0.0078(10) 0.0137(11) C21 0.0314(14) 0.0308(14) 0.0409(15) 0.0171(13) 0.0038(12) 0.0143(12) C22 0.0346(16) 0.0338(16) 0.056(2) 0.0177(15) 0.0060(15) 0.0117(14) C23 0.049(2) 0.0271(16) 0.066(2) 0.0092(16) -0.0036(18) 0.0125(15) C24 0.067(2) 0.0405(19) 0.0449(19) 0.0086(16) 0.0047(17) 0.0299(19) C25 0.0470(18) 0.0376(17) 0.0420(17) 0.0146(14) 0.0150(15) 0.0202(15) N3 0.0355(13) 0.0395(14) 0.0335(12) 0.0148(11) 0.0105(10) 0.0196(12) C31 0.0289(14) 0.0446(17) 0.0284(14) 0.0110(13) 0.0079(11) 0.0164(13) C32 0.0329(16) 0.060(2) 0.0436(18) 0.0167(17) 0.0135(14) 0.0186(17) C33 0.050(2) 0.066(3) 0.066(2) 0.013(2) 0.0170(19) 0.040(2) C34 0.064(3) 0.057(2) 0.073(3) 0.021(2) 0.021(2) 0.043(2) C35 0.050(2) 0.0431(19) 0.053(2) 0.0198(16) 0.0153(16) 0.0266(17) N4 0.0368(13) 0.0356(13) 0.0320(13) 0.0129(11) 0.0100(10) 0.0112(12) C41 0.0319(15) 0.0343(15) 0.0392(16) 0.0180(13) 0.0030(12) 0.0108(13) C42 0.0357(17) 0.0433(18) 0.052(2) 0.0178(16) 0.0024(15) 0.0085(15) C43 0.049(2) 0.0403(19) 0.054(2) 0.0062(17) -0.0005(18) 0.0070(17) C44 0.065(3) 0.0408(19) 0.0428(19) 0.0041(16) 0.0076(18) 0.0162(19) C45 0.0406(18) 0.0422(18) 0.0459(19) 0.0112(16) 0.0155(15) 0.0105(16) N5 0.0338(13) 0.0410(14) 0.0551(16) 0.0270(13) 0.0171(12) 0.0215(12) C51 0.0322(15) 0.0402(17) 0.0434(17) 0.0167(14) 0.0064(13) 0.0179(14) C52 0.0362(18) 0.058(2) 0.088(3) 0.040(2) 0.0162(18) 0.0250(18) C53 0.047(2) 0.066(3) 0.110(4) 0.042(3) 0.023(2) 0.038(2) C54 0.057(2) 0.055(2) 0.116(4) 0.048(2) 0.031(2) 0.040(2) C55 0.0376(17) 0.048(2) 0.083(3) 0.038(2) 0.0220(18) 0.0219(16) O1T 0.148(5) 0.221(7) 0.278(9) 0.130(7) 0.101(6) 0.091(6) C1T 0.129(6) 0.074(4) 0.155(7) 0.038(4) 0.063(5) 0.053(4) O1T' 0.148(5) 0.221(7) 0.278(9) 0.130(7) 0.101(6) 0.091(6) C1T' 0.129(6) 0.074(4) 0.155(7) 0.038(4) 0.063(5) 0.053(4) C1S 0.114(7) 0.129(7) 0.38(2) -0.005(10) 0.117(10) 0.036(6) C3S 0.221(13) 0.210(11) 0.121(8) 0.018(8) 0.084(8) 0.034(10) C4S 0.102(7) 0.48(2) 0.139(8) 0.128(12) 0.051(6) 0.121(11) C1S' 0.114(7) 0.129(7) 0.38(2) -0.005(10) 0.117(10) 0.036(6) C3S' 0.221(13) 0.210(11) 0.121(8) 0.018(8) 0.084(8) 0.034(10) C4S' 0.102(7) 0.48(2) 0.139(8) 0.128(12) 0.051(6) 0.121(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Sm1 O1 2.2145(17) 2_757 ? Sm1 O1 2.2836(18) . ? Sm1 N2 2.560(2) . ? Sm1 N4 2.589(3) . ? Sm1 N5 2.591(2) . ? Sm1 N3 2.592(2) . ? Sm1 N1 2.645(2) . ? Sm1 Al2 3.2975(8) . ? Sm1 Sm1 3.6124(3) 2_757 ? Al1 C1 1.978(3) . ? Al1 C31 2.014(3) . ? Al1 C21 2.025(3) . ? Al1 C11 2.032(3) . ? Al2 O1 1.7559(19) . ? Al2 C2 1.964(3) . ? Al2 C51 2.028(3) . ? Al2 C41 2.035(3) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? O1 Sm1 2.2145(17) 2_757 ? N1 C11 1.339(4) . ? N1 C15 1.353(4) . ? C11 C12 1.392(4) . ? C12 C13 1.391(4) . ? C12 H12 0.9500 . ? C13 C14 1.364(5) . ? C13 H13 0.9500 . ? C14 C15 1.375(4) . ? C14 H14 0.9500 . ? C15 H15 0.9500 . ? N2 C25 1.338(4) . ? N2 C21 1.363(4) . ? C21 C22 1.407(4) . ? C22 C23 1.379(5) . ? C22 H22 0.9500 . ? C23 C24 1.374(5) . ? C23 H23 0.9500 . ? C24 C25 1.375(5) . ? C24 H24 0.9500 . ? C25 H25 0.9500 . ? N3 C35 1.348(4) . ? N3 C31 1.361(4) . ? C31 C32 1.400(4) . ? C32 C33 1.382(5) . ? C32 H32 0.9500 . ? C33 C34 1.358(6) . ? C33 H33 0.9500 . ? C34 C35 1.381(5) . ? C34 H34 0.9500 . ? C35 H35 0.9500 . ? N4 C45 1.342(4) . ? N4 C41 1.367(4) . ? C41 C42 1.395(4) . ? C42 C43 1.362(5) . ? C42 H42 0.9500 . ? C43 C44 1.390(5) . ? C43 H43 0.9500 . ? C44 C45 1.374(5) . ? C44 H44 0.9500 . ? C45 H45 0.9500 . ? N5 C55 1.344(4) . ? N5 C51 1.375(4) . ? C51 C52 1.396(4) . ? C52 C53 1.383(5) . ? C52 H52 0.9500 . ? C53 C54 1.384(5) . ? C53 H53 0.9500 . ? C54 C55 1.381(4) . ? C54 H54 0.9500 . ? C55 H55 0.9500 . ? O1T C1T 1.467(8) . ? O1T C4T 1.496(13) . ? C1T C2T 1.364(12) . ? C1T H1T1 0.9900 . ? C1T H1T2 0.9900 . ? C2T C3T 1.480(13) . ? C2T H2T1 0.9900 . ? C2T H2T2 0.9900 . ? C3T C4T 1.424(13) . ? C3T H3T1 0.9900 . ? C3T H3T2 0.9900 . ? C4T H4T1 0.9900 . ? C4T H4T2 0.9900 . ? C2T' C3T' 1.458(13) . ? C2T' H2T3 0.9900 . ? C2T' H2T4 0.9900 . ? C3T' C4T' 1.438(19) . ? C3T' H3T3 0.9900 . ? C3T' H3T4 0.9900 . ? C4T' H4T3 0.9900 . ? C4T' H4T4 0.9900 . ? O1S C4S 1.313(13) . ? O1S C1S 1.912(15) . ? C1S C2S 1.49(2) . ? C1S H1S1 0.9900 . ? C1S H1S2 0.9900 . ? C2S C3S 1.48(2) . ? C2S H2S1 0.9900 . ? C2S H2S2 0.9900 . ? C3S C4S 1.269(14) . ? C3S H3S1 0.9900 . ? C3S H3S2 0.9900 . ? C4S H4S1 0.9900 . ? C4S H4S2 0.9900 . ? C2S' H2S3 0.9900 . ? C2S' H2S4 0.9900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Sm1 O1 73.16(7) 2_757 . ? O1 Sm1 N2 82.49(7) 2_757 . ? O1 Sm1 N2 121.56(7) . . ? O1 Sm1 N4 114.51(7) 2_757 . ? O1 Sm1 N4 74.51(7) . . ? N2 Sm1 N4 160.56(8) . . ? O1 Sm1 N5 127.73(8) 2_757 . ? O1 Sm1 N5 74.59(7) . . ? N2 Sm1 N5 80.71(8) . . ? N4 Sm1 N5 94.69(8) . . ? O1 Sm1 N3 77.73(7) 2_757 . ? O1 Sm1 N3 134.32(7) . . ? N2 Sm1 N3 87.78(8) . . ? N4 Sm1 N3 86.89(8) . . ? N5 Sm1 N3 149.62(8) . . ? O1 Sm1 N1 153.04(7) 2_757 . ? O1 Sm1 N1 133.59(7) . . ? N2 Sm1 N1 83.86(8) . . ? N4 Sm1 N1 76.76(8) . . ? N5 Sm1 N1 72.29(8) . . ? N3 Sm1 N1 78.61(7) . . ? O1 Sm1 Al2 103.22(5) 2_757 . ? O1 Sm1 Al2 30.28(5) . . ? N2 Sm1 Al2 130.54(6) . . ? N4 Sm1 Al2 57.37(6) . . ? N5 Sm1 Al2 56.70(6) . . ? N3 Sm1 Al2 141.67(6) . . ? N1 Sm1 Al2 103.34(6) . . ? O1 Sm1 Sm1 37.23(5) 2_757 2_757 ? O1 Sm1 Sm1 35.93(4) . 2_757 ? N2 Sm1 Sm1 104.52(5) . 2_757 ? N4 Sm1 Sm1 94.90(6) . 2_757 ? N5 Sm1 Sm1 101.96(6) . 2_757 ? N3 Sm1 Sm1 108.14(5) . 2_757 ? N1 Sm1 Sm1 169.19(5) . 2_757 ? Al2 Sm1 Sm1 66.065(15) . 2_757 ? C1 Al1 C31 113.67(15) . . ? C1 Al1 C21 112.61(15) . . ? C31 Al1 C21 105.48(12) . . ? C1 Al1 C11 113.29(14) . . ? C31 Al1 C11 103.35(12) . . ? C21 Al1 C11 107.69(12) . . ? O1 Al2 C2 124.01(12) . . ? O1 Al2 C51 98.44(11) . . ? C2 Al2 C51 114.30(14) . . ? O1 Al2 C41 97.27(11) . . ? C2 Al2 C41 111.57(15) . . ? C51 Al2 C41 109.22(13) . . ? O1 Al2 Sm1 40.98(6) . . ? C2 Al2 Sm1 164.87(11) . . ? C51 Al2 Sm1 75.16(9) . . ? C41 Al2 Sm1 73.99(9) . . ? Al1 C1 H1A 109.5 . . ? Al1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? Al1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? Al2 C2 H2A 109.5 . . ? Al2 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? Al2 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? Al2 O1 Sm1 143.73(11) . 2_757 ? Al2 O1 Sm1 108.73(9) . . ? Sm1 O1 Sm1 106.84(7) 2_757 . ? C11 N1 C15 118.1(3) . . ? C11 N1 Sm1 124.06(18) . . ? C15 N1 Sm1 117.8(2) . . ? N1 C11 C12 120.6(3) . . ? N1 C11 Al1 118.1(2) . . ? C12 C11 Al1 121.3(2) . . ? C13 C12 C11 120.5(3) . . ? C13 C12 H12 119.8 . . ? C11 C12 H12 119.8 . . ? C14 C13 C12 118.4(3) . . ? C14 C13 H13 120.8 . . ? C12 C13 H13 120.8 . . ? C13 C14 C15 118.7(3) . . ? C13 C14 H14 120.6 . . ? C15 C14 H14 120.6 . . ? N1 C15 C14 123.6(3) . . ? N1 C15 H15 118.2 . . ? C14 C15 H15 118.2 . . ? C25 N2 C21 119.6(3) . . ? C25 N2 Sm1 115.7(2) . . ? C21 N2 Sm1 123.68(19) . . ? N2 C21 C22 117.8(3) . . ? N2 C21 Al1 119.1(2) . . ? C22 C21 Al1 123.1(2) . . ? C23 C22 C21 121.9(3) . . ? C23 C22 H22 119.1 . . ? C21 C22 H22 119.1 . . ? C24 C23 C22 118.6(3) . . ? C24 C23 H23 120.7 . . ? C22 C23 H23 120.7 . . ? C23 C24 C25 118.0(3) . . ? C23 C24 H24 121.0 . . ? C25 C24 H24 121.0 . . ? N2 C25 C24 124.0(3) . . ? N2 C25 H25 118.0 . . ? C24 C25 H25 118.0 . . ? C35 N3 C31 119.7(3) . . ? C35 N3 Sm1 116.6(2) . . ? C31 N3 Sm1 123.06(18) . . ? N3 C31 C32 118.2(3) . . ? N3 C31 Al1 119.4(2) . . ? C32 C31 Al1 122.4(3) . . ? C33 C32 C31 121.7(3) . . ? C33 C32 H32 119.1 . . ? C31 C32 H32 119.1 . . ? C34 C33 C32 118.6(3) . . ? C34 C33 H33 120.7 . . ? C32 C33 H33 120.7 . . ? C33 C34 C35 119.1(3) . . ? C33 C34 H34 120.4 . . ? C35 C34 H34 120.4 . . ? N3 C35 C34 122.7(3) . . ? N3 C35 H35 118.7 . . ? C34 C35 H35 118.7 . . ? C45 N4 C41 119.3(3) . . ? C45 N4 Sm1 127.9(2) . . ? C41 N4 Sm1 112.79(19) . . ? N4 C41 C42 118.3(3) . . ? N4 C41 Al2 115.1(2) . . ? C42 C41 Al2 126.3(3) . . ? C43 C42 C41 121.9(3) . . ? C43 C42 H42 119.0 . . ? C41 C42 H42 119.0 . . ? C42 C43 C44 119.2(3) . . ? C42 C43 H43 120.4 . . ? C44 C43 H43 120.4 . . ? C45 C44 C43 117.4(3) . . ? C45 C44 H44 121.3 . . ? C43 C44 H44 121.3 . . ? N4 C45 C44 123.9(3) . . ? N4 C45 H45 118.0 . . ? C44 C45 H45 118.0 . . ? C55 N5 C51 119.6(2) . . ? C55 N5 Sm1 125.6(2) . . ? C51 N5 Sm1 114.52(18) . . ? N5 C51 C52 118.5(3) . . ? N5 C51 Al2 113.28(19) . . ? C52 C51 Al2 128.2(3) . . ? C53 C52 C51 121.5(3) . . ? C53 C52 H52 119.3 . . ? C51 C52 H52 119.3 . . ? C52 C53 C54 119.0(3) . . ? C52 C53 H53 120.5 . . ? C54 C53 H53 120.5 . . ? C55 C54 C53 118.0(3) . . ? C55 C54 H54 121.0 . . ? C53 C54 H54 121.0 . . ? N5 C55 C54 123.4(3) . . ? N5 C55 H55 118.3 . . ? C54 C55 H55 118.3 . . ? C1T O1T C4T 106.1(7) . . ? C2T C1T O1T 115.1(9) . . ? C2T C1T H1T1 108.5 . . ? O1T C1T H1T1 108.5 . . ? C2T C1T H1T2 108.5 . . ? O1T C1T H1T2 108.5 . . ? H1T1 C1T H1T2 107.5 . . ? C1T C2T C3T 99.2(12) . . ? C1T C2T H2T1 111.9 . . ? C3T C2T H2T1 111.9 . . ? C1T C2T H2T2 111.9 . . ? C3T C2T H2T2 111.9 . . ? H2T1 C2T H2T2 109.6 . . ? C4T C3T C2T 116.3(14) . . ? C4T C3T H3T1 108.2 . . ? C2T C3T H3T1 108.2 . . ? C4T C3T H3T2 108.2 . . ? C2T C3T H3T2 108.2 . . ? H3T1 C3T H3T2 107.4 . . ? C3T C4T O1T 100.2(11) . . ? C3T C4T H4T1 111.7 . . ? O1T C4T H4T1 111.7 . . ? C3T C4T H4T2 111.7 . . ? O1T C4T H4T2 111.7 . . ? H4T1 C4T H4T2 109.5 . . ? C3T' C2T' H2T3 109.1 . . ? C3T' C2T' H2T4 109.1 . . ? H2T3 C2T' H2T4 107.9 . . ? C4T' C3T' C2T' 98.9(13) . . ? C4T' C3T' H3T3 112.0 . . ? C2T' C3T' H3T3 112.0 . . ? C4T' C3T' H3T4 112.0 . . ? C2T' C3T' H3T4 112.0 . . ? H3T3 C3T' H3T4 109.7 . . ? C3T' C4T' H4T3 109.8 . . ? C3T' C4T' H4T4 109.8 . . ? H4T3 C4T' H4T4 108.2 . . ? C4S O1S C1S 92.8(9) . . ? C2S C1S O1S 83.2(9) . . ? C2S C1S H1S1 114.8 . . ? O1S C1S H1S1 114.8 . . ? C2S C1S H1S2 114.8 . . ? O1S C1S H1S2 114.8 . . ? H1S1 C1S H1S2 111.9 . . ? C3S C2S C1S 104.8(12) . . ? C3S C2S H2S1 110.8 . . ? C1S C2S H2S1 110.8 . . ? C3S C2S H2S2 110.8 . . ? C1S C2S H2S2 110.8 . . ? H2S1 C2S H2S2 108.9 . . ? C4S C3S C2S 86.2(11) . . ? C4S C3S H3S1 114.3 . . ? C2S C3S H3S1 114.3 . . ? C4S C3S H3S2 114.3 . . ? C2S C3S H3S2 114.3 . . ? H3S1 C3S H3S2 111.4 . . ? C3S C4S O1S 124.1(11) . . ? C3S C4S H4S1 106.3 . . ? O1S C4S H4S1 106.3 . . ? C3S C4S H4S2 106.3 . . ? O1S C4S H4S2 106.3 . . ? H4S1 C4S H4S2 106.4 . . ? H2S3 C2S' H2S4 108.2 . . ? _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 32.00 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 0.914 _refine_diff_density_min -0.923 _refine_diff_density_rms 0.109 #===END data_dw1466 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C24 H24 I2 Li2 N4' _chemical_formula_sum 'C24 H24 I2 Li2 N4' _chemical_formula_weight 636.15 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Li' 'Li' -0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'I' 'I' -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/n _symmetry_space_group_name_Hall '-P 2yn' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 9.9616(3) _cell_length_b 10.9075(3) _cell_length_c 12.0553(4) _cell_angle_alpha 90.00 _cell_angle_beta 104.174(2) _cell_angle_gamma 90.00 _cell_volume 1270.01(7) _cell_formula_units_Z 2 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 8511 _cell_measurement_theta_min 1.00 _cell_measurement_theta_max 30.03 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.664 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 616 _exptl_absorpt_coefficient_mu 2.494 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_correction_T_min 0.677 _exptl_absorpt_correction_T_max 0.752 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements Sortav (Blessing 1995) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 180(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_measurement_method 'Thin slice \w and \f scans' _diffrn_reflns_number 8310 _diffrn_reflns_av_R_equivalents 0.0286 _diffrn_reflns_av_sigmaI/netI 0.0311 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.57 _diffrn_reflns_theta_max 29.96 _reflns_number_total 3566 _reflns_number_gt 3121 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius B.V. 1998)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction ; HKL Denzo and Scalepack (Otwinowski & Minor 1997) ; _computing_structure_solution 'SIR-92 (Altomare et al. 1994)' _computing_structure_refinement 'SHELXL-97 (Sheldrick 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0060P)^2^+0.9581P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3566 _refine_ls_number_parameters 147 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0325 _refine_ls_R_factor_gt 0.0255 _refine_ls_wR_factor_ref 0.0579 _refine_ls_wR_factor_gt 0.0541 _refine_ls_goodness_of_fit_ref 1.096 _refine_ls_restrained_S_all 1.096 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group I1 I 1.116949(14) 0.969092(15) 0.175745(12) 0.03890(6) Uani 1 1 d . . . Li1 Li 0.8475(4) 0.9668(3) 0.0371(3) 0.0347(8) Uani 1 1 d . . . N1 N 0.70550(17) 1.05667(18) 0.10216(15) 0.0330(4) Uani 1 1 d . . . N2 N 0.73197(18) 0.81947(18) 0.05668(16) 0.0344(4) Uani 1 1 d . . . C11 C 0.6134(2) 0.9802(2) 0.13193(19) 0.0360(5) Uani 1 1 d . . . C12 C 0.5107(2) 1.0253(3) 0.1816(2) 0.0487(7) Uani 1 1 d . . . H12 H 0.4457 0.9709 0.2014 0.058 Uiso 1 1 calc R . . C13 C 0.5042(3) 1.1494(3) 0.2019(2) 0.0536(7) Uani 1 1 d . . . H13 H 0.4357 1.1810 0.2368 0.064 Uiso 1 1 calc R . . C14 C 0.5976(3) 1.2265(3) 0.17132(19) 0.0475(6) Uani 1 1 d . . . H14 H 0.5942 1.3123 0.1842 0.057 Uiso 1 1 calc R . . C15 C 0.6976(2) 1.1774(2) 0.12101(19) 0.0380(5) Uani 1 1 d . . . C16 C 0.8003(3) 1.2566(2) 0.0833(2) 0.0476(6) Uani 1 1 d . . . H16A H 0.8930 1.2212 0.1099 0.071 Uiso 1 1 calc R . . H16B H 0.7991 1.3390 0.1156 0.071 Uiso 1 1 calc R . . H16C H 0.7761 1.2618 -0.0004 0.071 Uiso 1 1 calc R . . C21 C 0.6273(2) 0.8484(2) 0.10606(18) 0.0370(5) Uani 1 1 d . . . C22 C 0.5406(3) 0.7592(3) 0.1321(2) 0.0502(7) Uani 1 1 d . . . H22 H 0.4680 0.7807 0.1669 0.060 Uiso 1 1 calc R . . C23 C 0.5619(3) 0.6385(3) 0.1064(2) 0.0580(8) Uani 1 1 d . . . H23 H 0.5046 0.5757 0.1243 0.070 Uiso 1 1 calc R . . C24 C 0.6659(3) 0.6097(3) 0.0549(2) 0.0537(7) Uani 1 1 d . . . H24 H 0.6805 0.5270 0.0360 0.064 Uiso 1 1 calc R . . C25 C 0.7502(2) 0.7025(2) 0.0307(2) 0.0418(5) Uani 1 1 d . . . C26 C 0.8668(3) 0.6768(3) -0.0235(3) 0.0542(7) Uani 1 1 d . . . H26A H 0.8516 0.7209 -0.0963 0.081 Uiso 1 1 calc R . . H26B H 0.8714 0.5885 -0.0374 0.081 Uiso 1 1 calc R . . H26C H 0.9540 0.7040 0.0276 0.081 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 I1 0.02904(8) 0.05383(11) 0.03401(9) 0.00587(6) 0.00805(6) -0.00072(6) Li1 0.0306(17) 0.038(2) 0.038(2) 0.0005(16) 0.0123(15) -0.0007(15) N1 0.0250(8) 0.0445(10) 0.0280(9) -0.0016(8) 0.0038(7) 0.0037(8) N2 0.0289(8) 0.0403(10) 0.0313(9) 0.0009(8) 0.0022(7) -0.0041(8) C11 0.0216(9) 0.0594(15) 0.0253(10) 0.0017(10) 0.0025(7) 0.0012(9) C12 0.0279(10) 0.082(2) 0.0362(12) -0.0015(13) 0.0085(9) 0.0025(12) C13 0.0361(12) 0.088(2) 0.0363(13) -0.0075(14) 0.0081(10) 0.0199(14) C14 0.0429(13) 0.0615(17) 0.0330(12) -0.0087(11) -0.0003(10) 0.0208(12) C15 0.0336(10) 0.0468(13) 0.0300(10) -0.0043(10) 0.0009(8) 0.0071(10) C16 0.0500(14) 0.0398(13) 0.0511(15) -0.0054(11) 0.0087(12) 0.0032(11) C21 0.0279(10) 0.0545(14) 0.0260(10) 0.0016(10) 0.0019(8) -0.0087(10) C22 0.0407(12) 0.0744(19) 0.0342(12) 0.0039(12) 0.0068(10) -0.0198(13) C23 0.0591(16) 0.0669(19) 0.0434(14) 0.0106(13) 0.0038(12) -0.0312(15) C24 0.0587(16) 0.0412(14) 0.0520(15) 0.0061(12) -0.0043(13) -0.0133(12) C25 0.0395(12) 0.0395(12) 0.0410(13) 0.0010(10) -0.0007(10) -0.0030(10) C26 0.0499(14) 0.0439(14) 0.0668(18) -0.0117(13) 0.0106(13) 0.0043(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 I1 Li1 2.765(4) 3_775 ? I1 Li1 2.793(4) . ? Li1 N2 2.023(4) . ? Li1 N1 2.029(4) . ? Li1 I1 2.765(4) 3_775 ? Li1 Li1 3.449(7) 3_775 ? N1 C15 1.342(3) . ? N1 C11 1.352(3) . ? N2 C25 1.337(3) . ? N2 C21 1.358(3) . ? C11 C12 1.396(3) . ? C11 C21 1.485(4) . ? C12 C13 1.380(4) . ? C13 C14 1.370(4) . ? C14 C15 1.394(3) . ? C15 C16 1.493(4) . ? C21 C22 1.386(3) . ? C22 C23 1.382(4) . ? C23 C24 1.368(4) . ? C24 C25 1.391(4) . ? C25 C26 1.492(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Li1 I1 Li1 76.70(12) 3_775 . ? N2 Li1 N1 82.46(16) . . ? N2 Li1 I1 120.97(18) . 3_775 ? N1 Li1 I1 119.75(17) . 3_775 ? N2 Li1 I1 115.34(17) . . ? N1 Li1 I1 115.04(17) . . ? I1 Li1 I1 103.30(12) 3_775 . ? N2 Li1 Li1 139.4(2) . 3_775 ? N1 Li1 Li1 137.8(2) . 3_775 ? I1 Li1 Li1 52.02(10) 3_775 3_775 ? I1 Li1 Li1 51.29(10) . 3_775 ? C15 N1 C11 119.3(2) . . ? C15 N1 Li1 127.94(19) . . ? C11 N1 Li1 112.76(19) . . ? C25 N2 C21 119.2(2) . . ? C25 N2 Li1 128.1(2) . . ? C21 N2 Li1 112.71(19) . . ? N1 C11 C12 120.9(2) . . ? N1 C11 C21 115.95(19) . . ? C12 C11 C21 123.2(2) . . ? C13 C12 C11 119.5(3) . . ? C14 C13 C12 119.4(2) . . ? C13 C14 C15 119.1(3) . . ? N1 C15 C14 121.9(2) . . ? N1 C15 C16 116.3(2) . . ? C14 C15 C16 121.8(2) . . ? N2 C21 C22 121.6(3) . . ? N2 C21 C11 116.0(2) . . ? C22 C21 C11 122.4(2) . . ? C23 C22 C21 118.6(3) . . ? C24 C23 C22 119.7(3) . . ? C23 C24 C25 119.4(3) . . ? N2 C25 C24 121.4(3) . . ? N2 C25 C26 116.6(2) . . ? C24 C25 C26 122.0(2) . . ? _diffrn_measured_fraction_theta_max 0.968 _diffrn_reflns_theta_full 29.96 _diffrn_measured_fraction_theta_full 0.968 _refine_diff_density_max 0.828 _refine_diff_density_min -0.596 _refine_diff_density_rms 0.075