# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2008 #data_global data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Haiyan Ma' _publ_contact_author_email HAIYANMA@ECUST.EDU.CN _publ_section_title ; ?-Diketiminate Aluminum Complexes: Synthesis, nd Ring-Opening Polymerization of Cyclic Esters ; loop_ _publ_author_name 'Haiyan Ma.' 'Shaogang Gong.' data_cd26434 _database_code_depnum_ccdc_archive 'CCDC 678287' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C27 H38 Al Cl N2' _chemical_formula_weight 453.02 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 12.3283(13) _cell_length_b 10.2992(10) _cell_length_c 21.520(2) _cell_angle_alpha 90.00 _cell_angle_beta 93.270(2) _cell_angle_gamma 90.00 _cell_volume 2727.9(5) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 2956 _cell_measurement_theta_min 4.386 _cell_measurement_theta_max 43.576 _exptl_crystal_description prismatic _exptl_crystal_colour green _exptl_crystal_size_max 0.503 _exptl_crystal_size_mid 0.489 _exptl_crystal_size_min 0.247 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.103 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 976 _exptl_absorpt_coefficient_mu 0.188 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.76883 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15695 _diffrn_reflns_av_R_equivalents 0.1071 _diffrn_reflns_av_sigmaI/netI 0.0937 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -6 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.86 _diffrn_reflns_theta_max 27.00 _reflns_number_total 5952 _reflns_number_gt 3221 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _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^)+(0.0654P)^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 5952 _refine_ls_number_parameters 288 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0932 _refine_ls_R_factor_gt 0.0550 _refine_ls_wR_factor_ref 0.1505 _refine_ls_wR_factor_gt 0.1364 _refine_ls_goodness_of_fit_ref 0.882 _refine_ls_restrained_S_all 0.882 _refine_ls_shift/su_max 0.041 _refine_ls_shift/su_mean 0.001 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 Al Al 0.22868(5) 0.19290(6) 0.05242(3) 0.0493(2) Uani 1 1 d . . . Cl1 Cl 0.26486(8) -0.11636(10) -0.23398(3) 0.1108(4) Uani 1 1 d . . . N1 N 0.22035(14) 0.26337(17) -0.02962(7) 0.0525(4) Uani 1 1 d . . . N2 N 0.25370(13) 0.35780(15) 0.09256(7) 0.0474(4) Uani 1 1 d . . . C1 C 0.18523(18) 0.3838(2) -0.04155(9) 0.0575(6) Uani 1 1 d . . . C2 C 0.18030(19) 0.4770(2) 0.00465(10) 0.0607(6) Uani 1 1 d . . . H2 H 0.1467 0.5548 -0.0071 0.073 Uiso 1 1 calc R . . C3 C 0.21949(17) 0.4684(2) 0.06637(9) 0.0524(5) Uani 1 1 d . . . C4 C 0.1525(2) 0.4245(3) -0.10720(10) 0.0849(8) Uani 1 1 d . . . H4A H 0.2125 0.4119 -0.1331 0.127 Uiso 1 1 calc R . . H4B H 0.1322 0.5144 -0.1076 0.127 Uiso 1 1 calc R . . H4C H 0.0920 0.3729 -0.1227 0.127 Uiso 1 1 calc R . . C5 C 0.2223(2) 0.5930(2) 0.10325(11) 0.0735(7) Uani 1 1 d . . . H5A H 0.1503 0.6139 0.1149 0.110 Uiso 1 1 calc R . . H5B H 0.2491 0.6620 0.0783 0.110 Uiso 1 1 calc R . . H5C H 0.2693 0.5826 0.1400 0.110 Uiso 1 1 calc R . . C6 C 0.23117(18) 0.1736(2) -0.08024(9) 0.0529(5) Uani 1 1 d . . . C7 C 0.14560(19) 0.1001(3) -0.10205(10) 0.0728(7) Uani 1 1 d . . . H7 H 0.0784 0.1109 -0.0851 0.087 Uiso 1 1 calc R . . C8 C 0.1563(2) 0.0099(3) -0.14877(11) 0.0781(7) Uani 1 1 d . . . H8 H 0.0972 -0.0406 -0.1626 0.094 Uiso 1 1 calc R . . C9 C 0.2529(2) -0.0047(3) -0.17418(10) 0.0742(7) Uani 1 1 d . . . C10 C 0.3410(3) 0.0646(3) -0.15173(14) 0.1097(11) Uani 1 1 d . . . H10 H 0.4082 0.0522 -0.1684 0.132 Uiso 1 1 calc R . . C11 C 0.3303(2) 0.1530(3) -0.10428(12) 0.0928(9) Uani 1 1 d . . . H11 H 0.3907 0.1988 -0.0885 0.111 Uiso 1 1 calc R . . C12 C 0.31080(18) 0.35812(18) 0.15356(9) 0.0486(5) Uani 1 1 d . . . C13 C 0.42371(18) 0.3655(2) 0.15635(10) 0.0577(6) Uani 1 1 d . . . C14 C 0.4781(2) 0.3577(2) 0.21490(12) 0.0763(7) Uani 1 1 d . . . H14 H 0.5536 0.3621 0.2181 0.092 Uiso 1 1 calc R . . C15 C 0.4223(2) 0.3435(2) 0.26768(12) 0.0786(8) Uani 1 1 d . . . H15 H 0.4601 0.3383 0.3063 0.094 Uiso 1 1 calc R . . C16 C 0.3112(2) 0.3369(2) 0.26398(10) 0.0692(7) Uani 1 1 d . . . H16 H 0.2744 0.3274 0.3002 0.083 Uiso 1 1 calc R . . C17 C 0.25253(18) 0.34419(19) 0.20710(9) 0.0526(5) Uani 1 1 d . . . C18 C 0.4881(2) 0.3874(3) 0.09897(11) 0.0746(7) Uani 1 1 d . . . H18 H 0.4407 0.3655 0.0624 0.090 Uiso 1 1 calc R . . C19 C 0.5896(2) 0.3031(3) 0.09735(15) 0.1079(10) Uani 1 1 d . . . H19A H 0.6420 0.3310 0.1293 0.132 Uiso 1 1 calc R . . H19B H 0.6200 0.3113 0.0575 0.132 Uiso 1 1 calc R . . H19C H 0.5707 0.2141 0.1043 0.132 Uiso 1 1 calc R . . C20 C 0.5197(3) 0.5295(3) 0.09361(15) 0.1059(10) Uani 1 1 d . . . H20A H 0.4553 0.5814 0.0876 0.129 Uiso 1 1 calc R . . H20B H 0.5641 0.5405 0.0588 0.129 Uiso 1 1 calc R . . H20C H 0.5595 0.5562 0.1311 0.129 Uiso 1 1 calc R . . C21 C 0.1297(2) 0.3389(2) 0.20611(10) 0.0661(6) Uani 1 1 d . . . H21 H 0.1020 0.3375 0.1625 0.079 Uiso 1 1 calc R . . C22 C 0.0831(3) 0.4587(3) 0.23675(14) 0.1061(10) Uani 1 1 d . . . H22A H 0.1006 0.4560 0.2808 0.129 Uiso 1 1 calc R . . H22B H 0.0056 0.4600 0.2292 0.129 Uiso 1 1 calc R . . H22C H 0.1137 0.5355 0.2196 0.129 Uiso 1 1 calc R . . C23 C 0.0891(2) 0.2176(3) 0.23731(12) 0.0971(9) Uani 1 1 d . . . H23A H 0.1263 0.1431 0.2223 0.126 Uiso 1 1 calc R . . H23B H 0.0124 0.2084 0.2279 0.126 Uiso 1 1 calc R . . H23C H 0.1028 0.2247 0.2816 0.126 Uiso 1 1 calc R . . C24 C 0.3499(2) 0.0718(2) 0.06774(11) 0.0714(7) Uani 1 1 d . . . H24A H 0.4089 0.0991 0.0428 0.086 Uiso 1 1 calc R . . H24B H 0.3752 0.0794 0.1111 0.086 Uiso 1 1 calc R . . C25 C 0.3270(3) -0.0685(3) 0.05425(16) 0.1169(12) Uani 1 1 d . . . H25A H 0.2661 -0.0962 0.0768 0.135 Uiso 1 1 calc R . . H25B H 0.3896 -0.1195 0.0669 0.135 Uiso 1 1 calc R . . H25C H 0.3106 -0.0797 0.0104 0.135 Uiso 1 1 calc R . . C26 C 0.08366(19) 0.1222(2) 0.06512(10) 0.0634(6) Uani 1 1 d . . . H26A H 0.0750 0.0428 0.0411 0.076 Uiso 1 1 calc R . . H26B H 0.0806 0.0990 0.1087 0.076 Uiso 1 1 calc R . . C27 C -0.0124(2) 0.2103(3) 0.04771(12) 0.0840(8) Uani 1 1 d . . . H27A H -0.0087 0.2864 0.0736 0.126 Uiso 1 1 calc R . . H27B H -0.0789 0.1648 0.0538 0.126 Uiso 1 1 calc R . . H27C H -0.0102 0.2355 0.0048 0.126 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 Al 0.0569(4) 0.0436(4) 0.0470(4) 0.0008(3) -0.0013(3) -0.0031(3) Cl1 0.1468(8) 0.1420(8) 0.0751(5) -0.0444(5) 0.0190(5) 0.0217(6) N1 0.0592(11) 0.0534(11) 0.0449(9) -0.0009(8) 0.0021(8) -0.0004(8) N2 0.0536(11) 0.0444(10) 0.0437(9) 0.0018(7) -0.0010(8) -0.0034(8) C1 0.0619(15) 0.0618(15) 0.0479(12) 0.0081(11) -0.0034(10) 0.0005(11) C2 0.0742(16) 0.0487(13) 0.0585(14) 0.0059(11) -0.0024(12) 0.0078(11) C3 0.0579(14) 0.0473(13) 0.0522(12) 0.0029(10) 0.0049(10) -0.0023(10) C4 0.115(2) 0.0840(19) 0.0539(14) 0.0106(13) -0.0103(14) 0.0123(16) C5 0.102(2) 0.0456(14) 0.0727(15) -0.0015(11) 0.0003(14) 0.0028(13) C6 0.0533(13) 0.0606(14) 0.0449(11) -0.0004(10) 0.0029(10) -0.0011(10) C7 0.0467(14) 0.107(2) 0.0647(14) -0.0276(14) 0.0025(11) -0.0004(13) C8 0.0653(17) 0.106(2) 0.0623(15) -0.0288(14) -0.0011(13) -0.0087(14) C9 0.083(2) 0.093(2) 0.0476(13) -0.0119(12) 0.0120(13) 0.0068(15) C10 0.083(2) 0.144(3) 0.107(2) -0.040(2) 0.0550(19) -0.021(2) C11 0.0754(19) 0.108(2) 0.098(2) -0.0324(17) 0.0357(16) -0.0318(16) C12 0.0594(14) 0.0379(11) 0.0478(11) -0.0001(9) -0.0037(10) -0.0071(9) C13 0.0591(15) 0.0525(14) 0.0608(13) -0.0035(10) -0.0031(11) -0.0101(10) C14 0.0629(16) 0.0805(18) 0.0832(18) 0.0001(14) -0.0177(14) -0.0120(13) C15 0.087(2) 0.086(2) 0.0599(15) 0.0082(13) -0.0217(14) -0.0111(15) C16 0.088(2) 0.0690(17) 0.0495(13) 0.0080(11) -0.0038(12) -0.0106(13) C17 0.0646(14) 0.0450(12) 0.0478(12) 0.0015(9) -0.0016(10) -0.0038(10) C18 0.0569(16) 0.088(2) 0.0789(16) -0.0036(14) 0.0046(12) -0.0178(14) C19 0.078(2) 0.108(2) 0.141(3) -0.018(2) 0.0324(19) -0.0083(18) C20 0.099(2) 0.096(2) 0.125(2) 0.0198(18) 0.0298(19) -0.0221(18) C21 0.0700(17) 0.0784(17) 0.0502(12) -0.0002(11) 0.0048(11) -0.0081(13) C22 0.092(2) 0.121(3) 0.108(2) -0.0012(19) 0.0334(18) 0.0195(19) C23 0.093(2) 0.109(2) 0.0905(19) 0.0086(17) 0.0118(16) -0.0347(18) C24 0.0779(18) 0.0559(15) 0.0792(16) 0.0009(12) -0.0062(13) 0.0060(12) C25 0.122(3) 0.0603(19) 0.166(3) -0.0075(19) -0.012(2) 0.0148(17) C26 0.0696(16) 0.0588(15) 0.0617(13) -0.0029(11) 0.0026(11) -0.0114(12) C27 0.0636(17) 0.090(2) 0.0978(19) -0.0032(15) 0.0025(14) -0.0038(14) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Al N1 1.9062(16) . ? Al N2 1.9223(16) . ? Al C24 1.960(2) . ? Al C26 1.964(2) . ? Cl1 C9 1.739(2) . ? N1 C1 1.334(3) . ? N1 C6 1.441(2) . ? N2 C3 1.329(2) . ? N2 C12 1.454(2) . ? C1 C2 1.386(3) . ? C1 C4 1.506(3) . ? C2 C3 1.390(3) . ? C2 H2 0.9300 . ? C3 C5 1.508(3) . ? C4 H4A 0.9600 . ? C4 H4B 0.9600 . ? C4 H4C 0.9600 . ? C5 H5A 0.9600 . ? C5 H5B 0.9600 . ? C5 H5C 0.9600 . ? C6 C7 1.360(3) . ? C6 C11 1.370(3) . ? C7 C8 1.381(3) . ? C7 H7 0.9300 . ? C8 C9 1.347(3) . ? C8 H8 0.9300 . ? C9 C10 1.365(4) . ? C10 C11 1.380(3) . ? C10 H10 0.9300 . ? C11 H11 0.9300 . ? C12 C13 1.392(3) . ? C12 C17 1.399(3) . ? C13 C14 1.395(3) . ? C13 C18 1.522(3) . ? C14 C15 1.369(4) . ? C14 H14 0.9300 . ? C15 C16 1.369(4) . ? C15 H15 0.9300 . ? C16 C17 1.388(3) . ? C16 H16 0.9300 . ? C17 C21 1.515(3) . ? C18 C20 1.521(4) . ? C18 C19 1.525(4) . ? C18 H18 0.9800 . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? C21 C23 1.516(3) . ? C21 C22 1.527(3) . ? C21 H21 0.9800 . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 0.9600 . ? C23 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 0.9600 . ? C24 C25 1.497(3) . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C25 H25A 0.9600 . ? C25 H25B 0.9600 . ? C25 H25C 0.9600 . ? C26 C27 1.522(3) . ? C26 H26A 0.9700 . ? C26 H26B 0.9700 . ? C27 H27A 0.9600 . ? C27 H27B 0.9600 . ? C27 H27C 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Al N2 94.50(7) . . ? N1 Al C24 113.48(10) . . ? N2 Al C24 112.68(9) . . ? N1 Al C26 105.58(9) . . ? N2 Al C26 112.90(9) . . ? C24 Al C26 115.59(11) . . ? C1 N1 C6 119.63(16) . . ? C1 N1 Al 122.15(13) . . ? C6 N1 Al 116.96(13) . . ? C3 N2 C12 120.43(16) . . ? C3 N2 Al 121.87(13) . . ? C12 N2 Al 117.69(12) . . ? N1 C1 C2 122.22(18) . . ? N1 C1 C4 120.37(19) . . ? C2 C1 C4 117.4(2) . . ? C1 C2 C3 127.9(2) . . ? C1 C2 H2 116.1 . . ? C3 C2 H2 116.1 . . ? N2 C3 C2 122.98(18) . . ? N2 C3 C5 120.60(18) . . ? C2 C3 C5 116.42(19) . . ? C1 C4 H4A 109.5 . . ? C1 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C1 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C3 C5 H5A 109.5 . . ? C3 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C3 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C7 C6 C11 118.3(2) . . ? C7 C6 N1 120.97(19) . . ? C11 C6 N1 120.5(2) . . ? C6 C7 C8 121.4(2) . . ? C6 C7 H7 119.3 . . ? C8 C7 H7 119.3 . . ? C9 C8 C7 119.6(2) . . ? C9 C8 H8 120.2 . . ? C7 C8 H8 120.2 . . ? C8 C9 C10 120.2(2) . . ? C8 C9 Cl1 119.2(2) . . ? C10 C9 Cl1 120.5(2) . . ? C9 C10 C11 119.9(3) . . ? C9 C10 H10 120.0 . . ? C11 C10 H10 120.0 . . ? C6 C11 C10 120.4(2) . . ? C6 C11 H11 119.8 . . ? C10 C11 H11 119.8 . . ? C13 C12 C17 121.94(18) . . ? C13 C12 N2 118.08(18) . . ? C17 C12 N2 119.89(19) . . ? C12 C13 C14 117.6(2) . . ? C12 C13 C18 122.65(19) . . ? C14 C13 C18 119.7(2) . . ? C15 C14 C13 121.1(2) . . ? C15 C14 H14 119.4 . . ? C13 C14 H14 119.4 . . ? C16 C15 C14 120.4(2) . . ? C16 C15 H15 119.8 . . ? C14 C15 H15 119.8 . . ? C15 C16 C17 121.2(2) . . ? C15 C16 H16 119.4 . . ? C17 C16 H16 119.4 . . ? C16 C17 C12 117.7(2) . . ? C16 C17 C21 118.8(2) . . ? C12 C17 C21 123.51(18) . . ? C20 C18 C13 110.6(2) . . ? C20 C18 C19 109.4(2) . . ? C13 C18 C19 113.7(2) . . ? C20 C18 H18 107.7 . . ? C13 C18 H18 107.7 . . ? C19 C18 H18 107.7 . . ? C18 C19 H19A 109.5 . . ? C18 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C18 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C18 C20 H20A 109.5 . . ? C18 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C18 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C17 C21 C23 112.3(2) . . ? C17 C21 C22 111.4(2) . . ? C23 C21 C22 109.4(2) . . ? C17 C21 H21 107.9 . . ? C23 C21 H21 107.9 . . ? C22 C21 H21 107.9 . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C21 C23 H23A 109.5 . . ? C21 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C21 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C25 C24 Al 116.62(19) . . ? C25 C24 H24A 108.1 . . ? Al C24 H24A 108.1 . . ? C25 C24 H24B 108.1 . . ? Al C24 H24B 108.1 . . ? H24A C24 H24B 107.3 . . ? C24 C25 H25A 109.5 . . ? C24 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C24 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C27 C26 Al 116.51(16) . . ? C27 C26 H26A 108.2 . . ? Al C26 H26A 108.2 . . ? C27 C26 H26B 108.2 . . ? Al C26 H26B 108.2 . . ? H26A C26 H26B 107.3 . . ? C26 C27 H27A 109.5 . . ? C26 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C26 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 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 N2 Al N1 C1 -29.46(18) . . . . ? C24 Al N1 C1 -146.58(17) . . . . ? C26 Al N1 C1 85.83(18) . . . . ? N2 Al N1 C6 163.44(14) . . . . ? C24 Al N1 C6 46.32(17) . . . . ? C26 Al N1 C6 -81.27(16) . . . . ? N1 Al N2 C3 26.21(17) . . . . ? C24 Al N2 C3 143.99(17) . . . . ? C26 Al N2 C3 -82.80(18) . . . . ? N1 Al N2 C12 -154.50(14) . . . . ? C24 Al N2 C12 -36.73(17) . . . . ? C26 Al N2 C12 96.49(16) . . . . ? C6 N1 C1 C2 -175.5(2) . . . . ? Al N1 C1 C2 17.8(3) . . . . ? C6 N1 C1 C4 2.6(3) . . . . ? Al N1 C1 C4 -164.19(17) . . . . ? N1 C1 C2 C3 7.5(4) . . . . ? C4 C1 C2 C3 -170.6(2) . . . . ? C12 N2 C3 C2 169.41(19) . . . . ? Al N2 C3 C2 -11.3(3) . . . . ? C12 N2 C3 C5 -10.2(3) . . . . ? Al N2 C3 C5 169.05(16) . . . . ? C1 C2 C3 N2 -11.0(4) . . . . ? C1 C2 C3 C5 168.7(2) . . . . ? C1 N1 C6 C7 -86.9(3) . . . . ? Al N1 C6 C7 80.5(2) . . . . ? C1 N1 C6 C11 98.2(3) . . . . ? Al N1 C6 C11 -94.4(2) . . . . ? C11 C6 C7 C8 -2.2(4) . . . . ? N1 C6 C7 C8 -177.2(2) . . . . ? C6 C7 C8 C9 -1.1(4) . . . . ? C7 C8 C9 C10 3.3(4) . . . . ? C7 C8 C9 Cl1 -178.8(2) . . . . ? C8 C9 C10 C11 -2.2(5) . . . . ? Cl1 C9 C10 C11 179.9(2) . . . . ? C7 C6 C11 C10 3.4(4) . . . . ? N1 C6 C11 C10 178.4(2) . . . . ? C9 C10 C11 C6 -1.2(5) . . . . ? C3 N2 C12 C13 -91.9(2) . . . . ? Al N2 C12 C13 88.80(19) . . . . ? C3 N2 C12 C17 91.5(2) . . . . ? Al N2 C12 C17 -87.8(2) . . . . ? C17 C12 C13 C14 0.5(3) . . . . ? N2 C12 C13 C14 -176.11(18) . . . . ? C17 C12 C13 C18 -176.9(2) . . . . ? N2 C12 C13 C18 6.5(3) . . . . ? C12 C13 C14 C15 -0.2(3) . . . . ? C18 C13 C14 C15 177.3(2) . . . . ? C13 C14 C15 C16 -0.1(4) . . . . ? C14 C15 C16 C17 0.1(4) . . . . ? C15 C16 C17 C12 0.2(3) . . . . ? C15 C16 C17 C21 -178.9(2) . . . . ? C13 C12 C17 C16 -0.5(3) . . . . ? N2 C12 C17 C16 176.05(17) . . . . ? C13 C12 C17 C21 178.54(19) . . . . ? N2 C12 C17 C21 -5.0(3) . . . . ? C12 C13 C18 C20 98.7(3) . . . . ? C14 C13 C18 C20 -78.6(3) . . . . ? C12 C13 C18 C19 -137.8(2) . . . . ? C14 C13 C18 C19 44.9(3) . . . . ? C16 C17 C21 C23 -56.4(3) . . . . ? C12 C17 C21 C23 124.6(2) . . . . ? C16 C17 C21 C22 66.7(3) . . . . ? C12 C17 C21 C22 -112.3(2) . . . . ? N1 Al C24 C25 -90.7(2) . . . . ? N2 Al C24 C25 163.4(2) . . . . ? C26 Al C24 C25 31.5(2) . . . . ? N1 Al C26 C27 -48.16(19) . . . . ? N2 Al C26 C27 53.74(19) . . . . ? C24 Al C26 C27 -174.47(17) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.266 _refine_diff_density_min -0.204 _refine_diff_density_rms 0.043 #===END data_cd27362 _database_code_depnum_ccdc_archive 'CCDC 678288' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H40 Al2 N4 O' _chemical_formula_weight 598.68 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' O O 0.0106 0.0060 '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 Orthorhombic _symmetry_space_group_name_H-M Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 15.5268(11) _cell_length_b 19.5571(15) _cell_length_c 22.6748(17) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 6885.4(9) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 3055 _cell_measurement_theta_min 4.449 _cell_measurement_theta_max 47.668 _exptl_crystal_description prismatic _exptl_crystal_colour colorless _exptl_crystal_size_max 0.480 _exptl_crystal_size_mid 0.362 _exptl_crystal_size_min 0.297 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.155 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2544 _exptl_absorpt_coefficient_mu 0.117 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.75196 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 34747 _diffrn_reflns_av_R_equivalents 0.0906 _diffrn_reflns_av_sigmaI/netI 0.0822 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.80 _diffrn_reflns_theta_max 25.50 _reflns_number_total 6411 _reflns_number_gt 2876 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _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^)+(0.0580P)^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 SHELXL _refine_ls_extinction_coef ? _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 6411 _refine_ls_number_parameters 395 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1148 _refine_ls_R_factor_gt 0.0516 _refine_ls_wR_factor_ref 0.1333 _refine_ls_wR_factor_gt 0.1167 _refine_ls_goodness_of_fit_ref 0.848 _refine_ls_restrained_S_all 0.848 _refine_ls_shift/su_max 0.052 _refine_ls_shift/su_mean 0.004 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 0.53681(5) 0.21796(4) 0.65884(4) 0.0514(3) Uani 1 1 d . . . Al2 Al 0.51024(6) 0.38366(5) 0.62720(4) 0.0570(3) Uani 1 1 d . . . O1 O 0.51542(12) 0.30112(9) 0.64746(8) 0.0572(5) Uani 1 1 d . . . N1 N 0.47218(14) 0.16240(11) 0.60604(10) 0.0510(6) Uani 1 1 d . . . N2 N 0.64563(14) 0.19681(12) 0.62384(11) 0.0537(6) Uani 1 1 d . . . N3 N 0.57300(16) 0.40122(12) 0.55642(10) 0.0539(6) Uani 1 1 d . . . N4 N 0.58263(18) 0.43703(12) 0.67679(10) 0.0629(7) Uani 1 1 d . . . C1 C 0.5033(2) 0.12496(15) 0.56251(13) 0.0554(8) Uani 1 1 d . . . C2 C 0.5912(2) 0.12151(15) 0.55022(13) 0.0630(9) Uani 1 1 d . . . H2 H 0.6071 0.0920 0.5200 0.076 Uiso 1 1 calc R . . C3 C 0.6582(2) 0.15675(16) 0.57752(14) 0.0573(8) Uani 1 1 d . . . C4 C 0.4427(2) 0.08505(16) 0.52309(13) 0.0733(10) Uani 1 1 d . . . H4A H 0.4118 0.0521 0.5463 0.110 Uiso 1 1 calc R . . H4B H 0.4753 0.0619 0.4932 0.110 Uiso 1 1 calc R . . H4C H 0.4027 0.1159 0.5048 0.110 Uiso 1 1 calc R . . C5 C 0.7471(2) 0.14779(17) 0.55206(15) 0.0860(11) Uani 1 1 d . . . H5A H 0.7664 0.1904 0.5356 0.119 Uiso 1 1 calc R . . H5B H 0.7456 0.1136 0.5217 0.119 Uiso 1 1 calc R . . H5C H 0.7861 0.1337 0.5826 0.119 Uiso 1 1 calc R . . C6 C 0.3799(2) 0.16516(17) 0.61373(12) 0.0550(8) Uani 1 1 d . . . C7 C 0.3352(2) 0.21949(18) 0.59172(14) 0.0722(10) Uani 1 1 d . . . H7 H 0.3638 0.2534 0.5707 0.087 Uiso 1 1 calc R . . C8 C 0.2465(3) 0.2241(2) 0.60077(17) 0.0932(12) Uani 1 1 d . . . H8 H 0.2161 0.2611 0.5855 0.112 Uiso 1 1 calc R . . C9 C 0.2041(2) 0.1747(3) 0.63190(17) 0.0928(13) Uani 1 1 d . . . H9 H 0.1450 0.1780 0.6380 0.111 Uiso 1 1 calc R . . C10 C 0.2495(3) 0.1201(2) 0.65413(15) 0.0900(12) Uani 1 1 d . . . H10 H 0.2208 0.0860 0.6749 0.108 Uiso 1 1 calc R . . C11 C 0.3372(2) 0.11560(18) 0.64577(13) 0.0729(10) Uani 1 1 d . . . H11 H 0.3678 0.0791 0.6617 0.087 Uiso 1 1 calc R . . C12 C 0.71589(18) 0.23549(16) 0.64855(14) 0.0567(8) Uani 1 1 d . . . C13 C 0.7462(2) 0.21830(18) 0.70293(15) 0.0765(10) Uani 1 1 d . . . H13 H 0.7247 0.1799 0.7221 0.092 Uiso 1 1 calc R . . C14 C 0.8095(2) 0.2580(2) 0.72993(17) 0.0903(12) Uani 1 1 d . . . H14 H 0.8297 0.2462 0.7672 0.108 Uiso 1 1 calc R . . C15 C 0.8417(2) 0.3138(2) 0.7019(2) 0.0944(13) Uani 1 1 d . . . H15 H 0.8839 0.3404 0.7198 0.113 Uiso 1 1 calc R . . C16 C 0.8117(2) 0.33035(19) 0.6476(2) 0.0914(12) Uani 1 1 d . . . H16 H 0.8344 0.3682 0.6281 0.110 Uiso 1 1 calc R . . C17 C 0.7484(2) 0.29223(17) 0.62062(16) 0.0759(10) Uani 1 1 d . . . H17 H 0.7277 0.3048 0.5837 0.091 Uiso 1 1 calc R . . C18 C 0.5273(2) 0.18338(17) 0.73880(13) 0.0787(10) Uani 1 1 d . . . H18A H 0.5438 0.2185 0.7661 0.118 Uiso 1 1 calc R . . H18B H 0.5646 0.1446 0.7435 0.118 Uiso 1 1 calc R . . H18C H 0.4689 0.1699 0.7463 0.118 Uiso 1 1 calc R . . C19 C 0.6462(2) 0.43690(15) 0.55302(13) 0.0562(8) Uani 1 1 d . . . C20 C 0.6822(2) 0.46959(15) 0.60182(14) 0.0647(9) Uani 1 1 d . . . H20 H 0.7317 0.4949 0.5944 0.078 Uiso 1 1 calc R . . C21 C 0.6540(2) 0.46954(16) 0.66016(14) 0.0637(9) Uani 1 1 d . . . C22 C 0.6956(2) 0.44228(17) 0.49594(13) 0.0777(10) Uani 1 1 d . . . H22A H 0.7071 0.3973 0.4810 0.117 Uiso 1 1 calc R . . H22B H 0.7491 0.4656 0.5028 0.117 Uiso 1 1 calc R . . H22C H 0.6622 0.4674 0.4677 0.117 Uiso 1 1 calc R . . C23 C 0.7071(2) 0.50842(18) 0.70458(14) 0.0957(12) Uani 1 1 d . . . H23A H 0.6713 0.5413 0.7243 0.124 Uiso 1 1 calc R . . H23B H 0.7532 0.5316 0.6848 0.124 Uiso 1 1 calc R . . H23C H 0.7304 0.4771 0.7330 0.124 Uiso 1 1 calc R . . C24 C 0.53966(19) 0.37052(16) 0.50349(12) 0.0531(8) Uani 1 1 d . . . C25 C 0.50621(19) 0.40930(17) 0.45812(14) 0.0673(9) Uani 1 1 d . . . H25 H 0.5065 0.4568 0.4606 0.081 Uiso 1 1 calc R . . C26 C 0.4722(2) 0.3774(2) 0.40890(15) 0.0748(10) Uani 1 1 d . . . H26 H 0.4511 0.4040 0.3781 0.090 Uiso 1 1 calc R . . C27 C 0.4690(2) 0.3084(2) 0.40458(15) 0.0729(10) Uani 1 1 d . . . H27 H 0.4452 0.2876 0.3715 0.087 Uiso 1 1 calc R . . C28 C 0.5012(2) 0.26978(18) 0.44970(15) 0.0741(10) Uani 1 1 d . . . H28 H 0.4995 0.2223 0.4473 0.089 Uiso 1 1 calc R . . C29 C 0.5364(2) 0.30073(17) 0.49896(13) 0.0655(9) Uani 1 1 d . . . H29 H 0.5581 0.2738 0.5294 0.079 Uiso 1 1 calc R . . C30 C 0.5617(3) 0.4363(2) 0.73818(15) 0.0788(11) Uani 1 1 d . . . C31 C 0.5943(3) 0.3872(2) 0.77389(18) 0.1141(17) Uani 1 1 d . . . H31 H 0.6318 0.3543 0.7592 0.129 Uiso 1 1 calc R . . C32 C 0.5710(6) 0.3870(4) 0.8321(3) 0.112(4) Uani 1 1 d . . . H32 H 0.5930 0.3533 0.8567 0.130 Uiso 1 1 calc R . . C33 C 0.5179(6) 0.4335(5) 0.8545(3) 0.118(6) Uani 1 1 d . . . H33 H 0.5051 0.4328 0.8946 0.138 Uiso 1 1 calc R . . C34 C 0.4823(4) 0.4819(4) 0.8193(3) 0.112(3) Uani 1 1 d . . . H34 H 0.4438 0.5137 0.8346 0.135 Uiso 1 1 calc R . . C35 C 0.5043(3) 0.4831(2) 0.75992(17) 0.1066(14) Uani 1 1 d . . . H35 H 0.4800 0.5156 0.7350 0.128 Uiso 1 1 calc R . . C36 C 0.3951(2) 0.42116(17) 0.62327(14) 0.0926(12) Uani 1 1 d . . . H36A H 0.3688 0.4082 0.5866 0.139 Uiso 1 1 calc R . . H36B H 0.3979 0.4701 0.6258 0.139 Uiso 1 1 calc R . . H36C H 0.3614 0.4037 0.6555 0.139 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 0.0510(6) 0.0561(6) 0.0470(5) 0.0036(4) -0.0019(5) -0.0006(4) Al2 0.0667(7) 0.0545(6) 0.0499(5) -0.0027(4) 0.0024(5) 0.0044(5) O1 0.0625(13) 0.0464(12) 0.0627(13) 0.0040(10) -0.0002(10) 0.0028(9) N1 0.0446(16) 0.0570(16) 0.0513(15) 0.0005(12) 0.0012(12) 0.0034(12) N2 0.0461(16) 0.0554(16) 0.0596(16) 0.0037(13) -0.0033(13) 0.0001(12) N3 0.0607(17) 0.0523(16) 0.0487(15) -0.0022(12) 0.0015(13) 0.0004(13) N4 0.083(2) 0.0573(17) 0.0485(16) -0.0058(13) 0.0050(14) -0.0053(14) C1 0.057(2) 0.055(2) 0.0549(19) 0.0002(16) -0.0013(17) 0.0016(16) C2 0.064(2) 0.061(2) 0.064(2) -0.0061(17) 0.0068(18) 0.0090(17) C3 0.050(2) 0.055(2) 0.068(2) 0.0087(17) 0.0043(18) 0.0074(16) C4 0.078(2) 0.077(2) 0.065(2) -0.0202(18) 0.0004(18) -0.0028(18) C5 0.057(2) 0.085(3) 0.116(3) -0.006(2) 0.013(2) 0.0103(18) C6 0.050(2) 0.071(2) 0.0445(18) -0.0076(16) -0.0052(16) -0.0009(17) C7 0.054(2) 0.080(3) 0.083(2) 0.002(2) -0.0011(19) 0.0036(19) C8 0.061(3) 0.119(4) 0.099(3) -0.008(3) -0.012(2) 0.018(2) C9 0.048(2) 0.159(4) 0.071(3) -0.033(3) 0.003(2) -0.001(3) C10 0.065(3) 0.141(4) 0.065(2) 0.000(2) 0.002(2) -0.024(3) C11 0.057(2) 0.103(3) 0.059(2) 0.0091(19) -0.0033(18) -0.009(2) C12 0.0408(18) 0.062(2) 0.068(2) 0.0093(17) -0.0041(17) 0.0050(15) C13 0.061(2) 0.092(3) 0.076(2) 0.010(2) -0.008(2) -0.010(2) C14 0.073(3) 0.121(4) 0.076(3) -0.002(3) -0.015(2) -0.004(2) C15 0.069(3) 0.093(3) 0.121(4) -0.018(3) -0.012(3) -0.007(2) C16 0.064(3) 0.072(3) 0.138(4) 0.015(3) -0.013(3) -0.009(2) C17 0.058(2) 0.071(3) 0.099(3) 0.023(2) -0.014(2) -0.0024(18) C18 0.075(2) 0.095(3) 0.066(2) 0.0140(19) -0.0019(19) -0.0054(19) C19 0.068(2) 0.049(2) 0.0518(19) 0.0001(15) 0.0055(18) 0.0096(16) C20 0.071(2) 0.058(2) 0.066(2) -0.0022(17) 0.0043(19) -0.0079(16) C21 0.080(2) 0.054(2) 0.057(2) -0.0035(17) -0.003(2) -0.0014(18) C22 0.082(3) 0.086(3) 0.064(2) -0.0025(18) 0.013(2) -0.001(2) C23 0.118(3) 0.097(3) 0.071(2) -0.018(2) -0.010(2) -0.039(2) C24 0.061(2) 0.053(2) 0.0443(17) -0.0022(16) 0.0043(16) 0.0051(15) C25 0.074(2) 0.068(2) 0.059(2) -0.0040(18) -0.0005(19) 0.0152(18) C26 0.069(2) 0.097(3) 0.058(2) 0.000(2) -0.0054(18) 0.014(2) C27 0.057(2) 0.101(3) 0.060(2) -0.015(2) 0.0056(18) -0.009(2) C28 0.096(3) 0.066(2) 0.060(2) -0.0062(19) 0.007(2) -0.0175(19) C29 0.085(3) 0.063(2) 0.0485(19) -0.0020(16) 0.0032(18) -0.0009(18) C30 0.109(3) 0.077(3) 0.050(2) -0.016(2) 0.007(2) -0.029(2) C31 0.160(5) 0.103(4) 0.060(3) 0.013(3) -0.015(3) -0.020(3) C32 0.168(10) 0.147(8) 0.071(4) 0.025(4) -0.012(5) -0.088(7) C33 0.145(10) 0.181(12) 0.068(4) -0.041(5) 0.037(5) -0.109(9) C34 0.136(6) 0.179(8) 0.112(5) -0.065(5) 0.063(5) -0.101(5) C35 0.126(4) 0.114(4) 0.079(3) -0.042(3) 0.029(3) -0.035(3) C36 0.137(4) 0.071(3) 0.069(2) 0.0042(19) -0.005(2) 0.033(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Al1 O1 1.6798(19) . ? Al1 N1 1.903(2) . ? Al1 N2 1.912(2) . ? Al1 C18 1.941(3) . ? Al2 O1 1.6803(19) . ? Al2 N4 1.902(3) . ? Al2 N3 1.909(2) . ? Al2 C36 1.935(3) . ? N1 C1 1.320(3) . ? N1 C6 1.445(3) . ? N2 C3 1.325(3) . ? N2 C12 1.441(4) . ? N3 C19 1.335(3) . ? N3 C24 1.438(3) . ? N4 C21 1.333(4) . ? N4 C30 1.429(4) . ? C1 C2 1.395(4) . ? C1 C4 1.514(4) . ? C2 C3 1.393(4) . ? C2 H2 0.9300 . ? C3 C5 1.506(4) . ? C4 H4A 0.9600 . ? C4 H4B 0.9600 . ? C4 H4C 0.9600 . ? C5 H5A 0.9600 . ? C5 H5B 0.9600 . ? C5 H5C 0.9600 . ? C6 C7 1.364(4) . ? C6 C11 1.381(4) . ? C7 C8 1.395(4) . ? C7 H7 0.9300 . ? C8 C9 1.366(5) . ? C8 H8 0.9300 . ? C9 C10 1.375(5) . ? C9 H9 0.9300 . ? C10 C11 1.378(4) . ? C10 H10 0.9300 . ? C11 H11 0.9300 . ? C12 C13 1.362(4) . ? C12 C17 1.374(4) . ? C13 C14 1.394(4) . ? C13 H13 0.9300 . ? C14 C15 1.358(5) . ? C14 H14 0.9300 . ? C15 C16 1.357(5) . ? C15 H15 0.9300 . ? C16 C17 1.378(4) . ? C16 H16 0.9300 . ? C17 H17 0.9300 . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C19 C20 1.395(4) . ? C19 C22 1.508(4) . ? C20 C21 1.393(4) . ? C20 H20 0.9300 . ? C21 C23 1.507(4) . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 0.9600 . ? C23 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 0.9600 . ? C24 C29 1.370(4) . ? C24 C25 1.379(4) . ? C25 C26 1.383(4) . ? C25 H25 0.9300 . ? C26 C27 1.355(4) . ? C26 H26 0.9300 . ? C27 C28 1.366(4) . ? C27 H27 0.9300 . ? C28 C29 1.383(4) . ? C28 H28 0.9300 . ? C29 H29 0.9300 . ? C30 C31 1.354(5) . ? C30 C35 1.370(5) . ? C31 C32 1.368(7) . ? C31 H31 0.9300 . ? C32 C33 1.328(11) . ? C32 H32 0.9300 . ? C33 C34 1.357(10) . ? C33 H33 0.9300 . ? C34 C35 1.389(6) . ? C34 H34 0.9300 . ? C35 H35 0.9300 . ? C36 H36A 0.9600 . ? C36 H36B 0.9600 . ? C36 H36C 0.9600 . ? 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 Al1 N1 110.61(10) . . ? O1 Al1 N2 108.69(10) . . ? N1 Al1 N2 94.66(11) . . ? O1 Al1 C18 117.77(12) . . ? N1 Al1 C18 110.41(12) . . ? N2 Al1 C18 112.30(13) . . ? O1 Al2 N4 109.71(10) . . ? O1 Al2 N3 112.22(10) . . ? N4 Al2 N3 95.55(12) . . ? O1 Al2 C36 114.90(13) . . ? N4 Al2 C36 111.44(13) . . ? N3 Al2 C36 111.40(13) . . ? Al1 O1 Al2 168.99(13) . . ? C1 N1 C6 118.3(2) . . ? C1 N1 Al1 126.4(2) . . ? C6 N1 Al1 115.20(18) . . ? C3 N2 C12 120.5(2) . . ? C3 N2 Al1 126.0(2) . . ? C12 N2 Al1 113.21(19) . . ? C19 N3 C24 118.4(2) . . ? C19 N3 Al2 125.2(2) . . ? C24 N3 Al2 116.28(19) . . ? C21 N4 C30 118.0(3) . . ? C21 N4 Al2 125.9(2) . . ? C30 N4 Al2 115.8(2) . . ? N1 C1 C2 122.3(3) . . ? N1 C1 C4 120.0(3) . . ? C2 C1 C4 117.7(3) . . ? C1 C2 C3 128.2(3) . . ? C1 C2 H2 115.9 . . ? C3 C2 H2 115.9 . . ? N2 C3 C2 122.3(3) . . ? N2 C3 C5 120.5(3) . . ? C2 C3 C5 117.1(3) . . ? C1 C4 H4A 109.5 . . ? C1 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C1 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C3 C5 H5A 109.5 . . ? C3 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C3 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C7 C6 C11 119.7(3) . . ? C7 C6 N1 119.3(3) . . ? C11 C6 N1 120.9(3) . . ? C6 C7 C8 119.9(3) . . ? C6 C7 H7 120.0 . . ? C8 C7 H7 120.0 . . ? C9 C8 C7 120.4(4) . . ? C9 C8 H8 119.8 . . ? C7 C8 H8 119.8 . . ? C8 C9 C10 119.5(4) . . ? C8 C9 H9 120.3 . . ? C10 C9 H9 120.3 . . ? C9 C10 C11 120.3(4) . . ? C9 C10 H10 119.8 . . ? C11 C10 H10 119.8 . . ? C10 C11 C6 120.1(3) . . ? C10 C11 H11 119.9 . . ? C6 C11 H11 119.9 . . ? C13 C12 C17 119.3(3) . . ? C13 C12 N2 119.0(3) . . ? C17 C12 N2 121.5(3) . . ? C12 C13 C14 120.3(3) . . ? C12 C13 H13 119.9 . . ? C14 C13 H13 119.9 . . ? C15 C14 C13 120.1(4) . . ? C15 C14 H14 119.9 . . ? C13 C14 H14 119.9 . . ? C14 C15 C16 119.4(4) . . ? C14 C15 H15 120.3 . . ? C16 C15 H15 120.3 . . ? C15 C16 C17 121.3(4) . . ? C15 C16 H16 119.4 . . ? C17 C16 H16 119.4 . . ? C12 C17 C16 119.7(3) . . ? C12 C17 H17 120.2 . . ? C16 C17 H17 120.2 . . ? Al1 C18 H18A 109.5 . . ? Al1 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? Al1 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? N3 C19 C20 122.3(3) . . ? N3 C19 C22 121.3(3) . . ? C20 C19 C22 116.4(3) . . ? C21 C20 C19 128.9(3) . . ? C21 C20 H20 115.6 . . ? C19 C20 H20 115.6 . . ? N4 C21 C20 122.0(3) . . ? N4 C21 C23 120.4(3) . . ? C20 C21 C23 117.6(3) . . ? C19 C22 H22A 109.5 . . ? C19 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C19 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C21 C23 H23A 109.5 . . ? C21 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C21 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C29 C24 C25 118.6(3) . . ? C29 C24 N3 119.5(3) . . ? C25 C24 N3 121.9(3) . . ? C24 C25 C26 119.8(3) . . ? C24 C25 H25 120.1 . . ? C26 C25 H25 120.1 . . ? C27 C26 C25 121.5(3) . . ? C27 C26 H26 119.3 . . ? C25 C26 H26 119.3 . . ? C26 C27 C28 118.9(3) . . ? C26 C27 H27 120.6 . . ? C28 C27 H27 120.6 . . ? C27 C28 C29 120.5(3) . . ? C27 C28 H28 119.7 . . ? C29 C28 H28 119.7 . . ? C24 C29 C28 120.8(3) . . ? C24 C29 H29 119.6 . . ? C28 C29 H29 119.6 . . ? C31 C30 C35 120.1(4) . . ? C31 C30 N4 120.3(4) . . ? C35 C30 N4 119.5(4) . . ? C30 C31 C32 118.7(6) . . ? C30 C31 H31 120.7 . . ? C32 C31 H31 120.7 . . ? C33 C32 C31 122.1(8) . . ? C33 C32 H32 118.9 . . ? C31 C32 H32 118.9 . . ? C32 C33 C34 120.3(8) . . ? C32 C33 H33 119.8 . . ? C34 C33 H33 119.8 . . ? C33 C34 C35 118.8(7) . . ? C33 C34 H34 120.6 . . ? C35 C34 H34 120.6 . . ? C30 C35 C34 119.8(5) . . ? C30 C35 H35 120.1 . . ? C34 C35 H35 120.1 . . ? Al2 C36 H36A 109.5 . . ? Al2 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? Al2 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 N1 Al1 O1 Al2 -91.9(7) . . . . ? N2 Al1 O1 Al2 10.8(7) . . . . ? C18 Al1 O1 Al2 139.9(7) . . . . ? N4 Al2 O1 Al1 -87.6(7) . . . . ? N3 Al2 O1 Al1 17.3(7) . . . . ? C36 Al2 O1 Al1 145.9(7) . . . . ? O1 Al1 N1 C1 112.3(2) . . . . ? N2 Al1 N1 C1 0.3(2) . . . . ? C18 Al1 N1 C1 -115.6(2) . . . . ? O1 Al1 N1 C6 -64.6(2) . . . . ? N2 Al1 N1 C6 -176.5(2) . . . . ? C18 Al1 N1 C6 67.6(2) . . . . ? O1 Al1 N2 C3 -112.4(2) . . . . ? N1 Al1 N2 C3 1.2(3) . . . . ? C18 Al1 N2 C3 115.5(3) . . . . ? O1 Al1 N2 C12 60.8(2) . . . . ? N1 Al1 N2 C12 174.37(19) . . . . ? C18 Al1 N2 C12 -71.3(2) . . . . ? O1 Al2 N3 C19 -110.0(2) . . . . ? N4 Al2 N3 C19 3.9(3) . . . . ? C36 Al2 N3 C19 119.5(3) . . . . ? O1 Al2 N3 C24 67.1(2) . . . . ? N4 Al2 N3 C24 -179.0(2) . . . . ? C36 Al2 N3 C24 -63.3(2) . . . . ? O1 Al2 N4 C21 113.0(3) . . . . ? N3 Al2 N4 C21 -3.0(3) . . . . ? C36 Al2 N4 C21 -118.6(3) . . . . ? O1 Al2 N4 C30 -60.9(3) . . . . ? N3 Al2 N4 C30 -176.9(3) . . . . ? C36 Al2 N4 C30 67.5(3) . . . . ? C6 N1 C1 C2 177.3(3) . . . . ? Al1 N1 C1 C2 0.5(4) . . . . ? C6 N1 C1 C4 -1.4(4) . . . . ? Al1 N1 C1 C4 -178.1(2) . . . . ? N1 C1 C2 C3 -3.2(5) . . . . ? C4 C1 C2 C3 175.5(3) . . . . ? C12 N2 C3 C2 -176.3(3) . . . . ? Al1 N2 C3 C2 -3.6(4) . . . . ? C12 N2 C3 C5 3.5(4) . . . . ? Al1 N2 C3 C5 176.2(2) . . . . ? C1 C2 C3 N2 4.8(5) . . . . ? C1 C2 C3 C5 -175.0(3) . . . . ? C1 N1 C6 C7 -98.4(3) . . . . ? Al1 N1 C6 C7 78.7(3) . . . . ? C1 N1 C6 C11 85.2(3) . . . . ? Al1 N1 C6 C11 -97.7(3) . . . . ? C11 C6 C7 C8 -1.1(5) . . . . ? N1 C6 C7 C8 -177.6(3) . . . . ? C6 C7 C8 C9 0.4(5) . . . . ? C7 C8 C9 C10 -0.2(6) . . . . ? C8 C9 C10 C11 0.9(6) . . . . ? C9 C10 C11 C6 -1.6(5) . . . . ? C7 C6 C11 C10 1.7(5) . . . . ? N1 C6 C11 C10 178.1(3) . . . . ? C3 N2 C12 C13 -111.4(3) . . . . ? Al1 N2 C12 C13 75.0(3) . . . . ? C3 N2 C12 C17 73.6(4) . . . . ? Al1 N2 C12 C17 -99.9(3) . . . . ? C17 C12 C13 C14 0.1(5) . . . . ? N2 C12 C13 C14 -175.0(3) . . . . ? C12 C13 C14 C15 -0.5(6) . . . . ? C13 C14 C15 C16 0.0(6) . . . . ? C14 C15 C16 C17 1.0(6) . . . . ? C13 C12 C17 C16 0.8(5) . . . . ? N2 C12 C17 C16 175.8(3) . . . . ? C15 C16 C17 C12 -1.4(6) . . . . ? C24 N3 C19 C20 178.6(3) . . . . ? Al2 N3 C19 C20 -4.3(4) . . . . ? C24 N3 C19 C22 -3.0(4) . . . . ? Al2 N3 C19 C22 174.0(2) . . . . ? N3 C19 C20 C21 2.9(5) . . . . ? C22 C19 C20 C21 -175.5(3) . . . . ? C30 N4 C21 C20 176.2(3) . . . . ? Al2 N4 C21 C20 2.4(4) . . . . ? C30 N4 C21 C23 -4.3(5) . . . . ? Al2 N4 C21 C23 -178.1(2) . . . . ? C19 C20 C21 N4 -1.9(5) . . . . ? C19 C20 C21 C23 178.6(3) . . . . ? C19 N3 C24 C29 114.2(3) . . . . ? Al2 N3 C24 C29 -63.1(3) . . . . ? C19 N3 C24 C25 -69.5(4) . . . . ? Al2 N3 C24 C25 113.2(3) . . . . ? C29 C24 C25 C26 -1.5(5) . . . . ? N3 C24 C25 C26 -177.8(3) . . . . ? C24 C25 C26 C27 1.6(5) . . . . ? C25 C26 C27 C28 -0.9(5) . . . . ? C26 C27 C28 C29 0.1(5) . . . . ? C25 C24 C29 C28 0.7(4) . . . . ? N3 C24 C29 C28 177.2(3) . . . . ? C27 C28 C29 C24 0.0(5) . . . . ? C21 N4 C30 C31 -86.9(4) . . . . ? Al2 N4 C30 C31 87.5(4) . . . . ? C21 N4 C30 C35 97.0(4) . . . . ? Al2 N4 C30 C35 -88.6(3) . . . . ? C35 C30 C31 C32 -2.2(7) . . . . ? N4 C30 C31 C32 -178.2(4) . . . . ? C30 C31 C32 C33 -0.3(10) . . . . ? C31 C32 C33 C34 2.4(14) . . . . ? C32 C33 C34 C35 -1.8(12) . . . . ? C31 C30 C35 C34 2.7(6) . . . . ? N4 C30 C35 C34 178.8(3) . . . . ? C33 C34 C35 C30 -0.7(8) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.315 _refine_diff_density_min -0.235 _refine_diff_density_rms 0.041 #===END