Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2003 data_global _journal_coden_Cambridge 222 _publ_requested_journal 'Dalton Trans.' loop_ _publ_author_name 'Luis M. Alcazar-Roman' ; Brendan J. O'Keefe ; 'Marc A. Hillmyer' 'William B. Tolman' _publ_contact_author_name 'Prof William B. Tolman' _publ_contact_author_address ; Department of Chemistry University of Minnesota 07 Pleasant St. SE, Minneapolis MN 55455-0431, USA ; _publ_contact_author_email tolman@chem.umn.edu _publ_section_title ; Electronic Influence of Ligand Substituents on the Rate of Polymerization of Cyclic Esters by Single-Site Aluminum Alkoxide Catalysts ; data_3a _database_code_CSD 207604 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 02112a _chemical_melting_point ? _chemical_formula_moiety 'C37 H61 Al N2 O3' _chemical_formula_sum 'C37 H61 Al N2 O3' _chemical_formula_weight 608.86 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Al Al 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pbcn loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z+1/2' '-x, y, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y-1/2, -z-1/2' 'x, -y, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 19.4598(15) _cell_length_b 15.2420(12) _cell_length_c 24.583(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 7291.5(10) _cell_formula_units_Z 8 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 3556 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.109 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2672 _exptl_absorpt_coefficient_mu 0.091 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9295 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details 'SADABS, R. Blessing, 1995' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'Bruker SMART Platform CCD' _diffrn_measurement_method 'area detector, omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 58561 _diffrn_reflns_av_R_equivalents 0.0336 _diffrn_reflns_av_sigmaI/netI 0.0177 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 1.66 _diffrn_reflns_theta_max 25.05 _reflns_number_total 6449 _reflns_number_gt 5460 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART, Bruker' _computing_cell_refinement 'SAINT, Bruker' _computing_data_reduction 'SAINT, Bruker' _computing_structure_solution SHELXS-97 _computing_structure_refinement SHELXL-97 _computing_molecular_graphics 'SHELXTL, Bruker' _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0430P)^2^+2.8859P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6449 _refine_ls_number_parameters 404 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0442 _refine_ls_R_factor_gt 0.0350 _refine_ls_wR_factor_ref 0.0935 _refine_ls_wR_factor_gt 0.0875 _refine_ls_goodness_of_fit_ref 1.030 _refine_ls_restrained_S_all 1.030 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Al1 Al 0.213826(19) 0.87434(3) 0.040654(16) 0.02291(11) Uani 1 1 d . . . O3 O 0.20911(4) 0.95219(6) -0.01203(4) 0.0256(2) Uani 1 1 d . . . O1 O 0.14284(5) 0.80566(7) 0.03666(4) 0.0328(2) Uani 1 1 d . . . O2 O 0.19245(5) 0.92496(6) 0.10387(4) 0.0264(2) Uani 1 1 d . . . N1 N 0.32189(5) 0.90479(7) 0.05833(5) 0.0241(2) Uani 1 1 d . . . N2 N 0.26534(6) 0.76738(8) 0.00377(5) 0.0304(3) Uani 1 1 d . . . C27 C 0.29240(7) 1.03900(9) -0.13354(6) 0.0266(3) Uani 1 1 d . . . H27A H 0.2817 1.0530 -0.1702 0.032 Uiso 1 1 calc R . . C13 C 0.28785(7) 1.11693(9) 0.19923(5) 0.0278(3) Uani 1 1 d . . . C25 C 0.25635(7) 0.98498(9) -0.04640(5) 0.0229(3) Uani 1 1 d . . . C10 C 0.22092(7) 0.98676(9) 0.13562(5) 0.0244(3) Uani 1 1 d . . . C24 C 0.32361(7) 0.99980(9) -0.02710(5) 0.0245(3) Uani 1 1 d . . . C30 C 0.16500(7) 1.00097(9) -0.12134(5) 0.0264(3) Uani 1 1 d . . . C12 C 0.21650(7) 1.11513(10) 0.19217(6) 0.0281(3) Uani 1 1 d . . . H12A H 0.1902 1.1594 0.2096 0.034 Uiso 1 1 calc R . . C26 C 0.23967(7) 1.00713(9) -0.10037(5) 0.0242(3) Uani 1 1 d . . . C4 C 0.36968(7) 0.83682(10) 0.03737(6) 0.0302(3) Uani 1 1 d . . . H4A H 0.3802 0.7940 0.0665 0.036 Uiso 1 1 calc R . . H4B H 0.4133 0.8646 0.0258 0.036 Uiso 1 1 calc R . . C8 C 0.33278(7) 0.91254(9) 0.11865(6) 0.0277(3) Uani 1 1 d . . . H8A H 0.3197 0.8565 0.1361 0.033 Uiso 1 1 calc R . . H8B H 0.3822 0.9225 0.1258 0.033 Uiso 1 1 calc R . . C29 C 0.37398(7) 1.03142(9) -0.06186(6) 0.0274(3) Uani 1 1 d . . . H29A H 0.4193 1.0396 -0.0484 0.033 Uiso 1 1 calc R . . C28 C 0.35976(7) 1.05140(9) -0.11598(6) 0.0277(3) Uani 1 1 d . . . C23 C 0.33733(7) 0.99175(9) 0.03301(5) 0.0263(3) Uani 1 1 d . . . H23A H 0.3864 1.0053 0.0395 0.032 Uiso 1 1 calc R . . H23B H 0.3099 1.0370 0.0521 0.032 Uiso 1 1 calc R . . C15 C 0.10258(7) 1.05580(10) 0.15586(6) 0.0308(3) Uani 1 1 d . . . C33 C 0.13789(7) 0.90656(10) -0.11866(6) 0.0327(3) Uani 1 1 d . . . H33A H 0.0910 0.9046 -0.1331 0.049 Uiso 1 1 calc R . . H33B H 0.1379 0.8865 -0.0808 0.049 Uiso 1 1 calc R . . H33C H 0.1675 0.8682 -0.1404 0.049 Uiso 1 1 calc R . . C9 C 0.29221(7) 0.98542(9) 0.14401(5) 0.0255(3) Uani 1 1 d . . . C32 C 0.11871(7) 1.06067(10) -0.08669(6) 0.0330(3) Uani 1 1 d . . . H32A H 0.0708 1.0541 -0.0984 0.049 Uiso 1 1 calc R . . H32B H 0.1330 1.1219 -0.0913 0.049 Uiso 1 1 calc R . . H32C H 0.1228 1.0441 -0.0483 0.049 Uiso 1 1 calc R . . C5 C 0.33713(7) 0.79016(10) -0.01029(6) 0.0321(3) Uani 1 1 d . . . H5A H 0.3378 0.8286 -0.0427 0.039 Uiso 1 1 calc R . . H5B H 0.3633 0.7362 -0.0188 0.039 Uiso 1 1 calc R . . C34 C 0.41697(7) 1.08591(11) -0.15337(6) 0.0348(4) Uani 1 1 d . . . C6 C 0.23080(8) 0.73773(11) -0.04696(7) 0.0421(4) Uani 1 1 d . . . H6A H 0.2542 0.6856 -0.0611 0.063 Uiso 1 1 calc R . . H6B H 0.2327 0.7847 -0.0742 0.063 Uiso 1 1 calc R . . H6C H 0.1827 0.7234 -0.0391 0.063 Uiso 1 1 calc R . . C11 C 0.18140(7) 1.05287(9) 0.16135(5) 0.0263(3) Uani 1 1 d . . . C7 C 0.26432(9) 0.69330(10) 0.04325(8) 0.0435(4) Uani 1 1 d . . . H7A H 0.2895 0.6433 0.0280 0.065 Uiso 1 1 calc R . . H7B H 0.2167 0.6761 0.0504 0.065 Uiso 1 1 calc R . . H7C H 0.2862 0.7118 0.0773 0.065 Uiso 1 1 calc R . . C19 C 0.32129(8) 1.19110(10) 0.23230(6) 0.0316(3) Uani 1 1 d . . . C16 C 0.07167(7) 0.97070(11) 0.17874(6) 0.0355(4) Uani 1 1 d . . . H16A H 0.0919 0.9202 0.1600 0.053 Uiso 1 1 calc R . . H16B H 0.0218 0.9709 0.1731 0.053 Uiso 1 1 calc R . . H16C H 0.0815 0.9668 0.2178 0.053 Uiso 1 1 calc R . . C14 C 0.32483(7) 1.04995(9) 0.17468(5) 0.0275(3) Uani 1 1 d . . . H14A H 0.3733 1.0481 0.1789 0.033 Uiso 1 1 calc R . . C31 C 0.15869(8) 1.03179(12) -0.18041(6) 0.0390(4) Uani 1 1 d . . . H31A H 0.1106 1.0281 -0.1919 0.059 Uiso 1 1 calc R . . H31B H 0.1870 0.9943 -0.2038 0.059 Uiso 1 1 calc R . . H31C H 0.1745 1.0927 -0.1833 0.059 Uiso 1 1 calc R . . C3 C 0.02924(8) 0.84657(13) 0.00983(7) 0.0481(4) Uani 1 1 d . . . H3A H 0.0438 0.9072 0.0031 0.072 Uiso 1 1 calc R . . H3B H -0.0188 0.8461 0.0219 0.072 Uiso 1 1 calc R . . H3C H 0.0336 0.8124 -0.0238 0.072 Uiso 1 1 calc R . . C1 C 0.07418(7) 0.80648(11) 0.05346(6) 0.0361(4) Uani 1 1 d . . . H1A H 0.0700 0.8419 0.0875 0.043 Uiso 1 1 calc R . . C17 C 0.08185(8) 1.06627(11) 0.09578(6) 0.0373(4) Uani 1 1 d . . . H17A H 0.1028 1.0193 0.0742 0.056 Uiso 1 1 calc R . . H17B H 0.0978 1.1233 0.0823 0.056 Uiso 1 1 calc R . . H17C H 0.0317 1.0630 0.0925 0.056 Uiso 1 1 calc R . . C20 C 0.29705(10) 1.18618(12) 0.29174(6) 0.0451(4) Uani 1 1 d . . . H20A H 0.3188 1.2332 0.3128 0.068 Uiso 1 1 calc R . . H20B H 0.3099 1.1292 0.3072 0.068 Uiso 1 1 calc R . . H20C H 0.2470 1.1930 0.2931 0.068 Uiso 1 1 calc R . . C18 C 0.07098(8) 1.13259(12) 0.18750(8) 0.0485(4) Uani 1 1 d . . . H18A H 0.0210 1.1320 0.1829 0.073 Uiso 1 1 calc R . . H18B H 0.0895 1.1880 0.1736 0.073 Uiso 1 1 calc R . . H18C H 0.0823 1.1268 0.2262 0.073 Uiso 1 1 calc R . . C21 C 0.30011(10) 1.27978(11) 0.20827(7) 0.0477(4) Uani 1 1 d . . . H21A H 0.3140 1.2825 0.1700 0.072 Uiso 1 1 calc R . . H21B H 0.3227 1.3271 0.2285 0.072 Uiso 1 1 calc R . . H21C H 0.2501 1.2865 0.2110 0.072 Uiso 1 1 calc R . . C22 C 0.39992(9) 1.18576(13) 0.23168(8) 0.0515(5) Uani 1 1 d . . . H22A H 0.4165 1.1909 0.1942 0.077 Uiso 1 1 calc R . . H22B H 0.4146 1.1293 0.2469 0.077 Uiso 1 1 calc R . . H22C H 0.4190 1.2336 0.2536 0.077 Uiso 1 1 calc R . . C35 C 0.45064(10) 1.16703(12) -0.12794(8) 0.0516(5) Uani 1 1 d . . . H35A H 0.4693 1.1518 -0.0922 0.077 Uiso 1 1 calc R . . H35B H 0.4163 1.2135 -0.1239 0.077 Uiso 1 1 calc R . . H35C H 0.4879 1.1876 -0.1515 0.077 Uiso 1 1 calc R . . C36 C 0.47166(9) 1.01424(13) -0.16013(8) 0.0520(5) Uani 1 1 d . . . H36A H 0.4920 1.0007 -0.1246 0.078 Uiso 1 1 calc R . . H36B H 0.5076 1.0350 -0.1849 0.078 Uiso 1 1 calc R . . H36C H 0.4503 0.9613 -0.1752 0.078 Uiso 1 1 calc R . . C37 C 0.39011(9) 1.11107(15) -0.20989(7) 0.0552(5) Uani 1 1 d . . . H37A H 0.3695 1.0595 -0.2272 0.083 Uiso 1 1 calc R . . H37B H 0.4283 1.1325 -0.2323 0.083 Uiso 1 1 calc R . . H37C H 0.3554 1.1573 -0.2063 0.083 Uiso 1 1 calc R . . C2 C 0.05221(10) 0.71251(14) 0.06505(9) 0.0609(5) Uani 1 1 d . . . H2A H 0.0841 0.6859 0.0911 0.091 Uiso 1 1 calc R . . H2B H 0.0526 0.6787 0.0311 0.091 Uiso 1 1 calc R . . H2C H 0.0057 0.7124 0.0804 0.091 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 0.0210(2) 0.0219(2) 0.0259(2) -0.00001(16) -0.00196(16) -0.00045(16) O3 0.0206(5) 0.0294(5) 0.0267(5) 0.0032(4) -0.0002(4) 0.0001(4) O1 0.0255(5) 0.0313(6) 0.0415(6) -0.0056(5) 0.0006(4) -0.0053(4) O2 0.0235(5) 0.0297(5) 0.0260(5) -0.0020(4) -0.0018(4) -0.0032(4) N1 0.0222(6) 0.0227(6) 0.0274(6) -0.0003(5) -0.0024(5) 0.0028(5) N2 0.0277(6) 0.0233(6) 0.0401(7) -0.0042(5) -0.0056(5) 0.0016(5) C27 0.0283(7) 0.0268(7) 0.0247(7) -0.0025(6) 0.0008(6) 0.0003(6) C13 0.0308(7) 0.0297(8) 0.0228(7) 0.0023(6) -0.0019(6) -0.0038(6) C25 0.0228(6) 0.0194(7) 0.0266(7) -0.0024(5) 0.0016(5) 0.0013(5) C10 0.0257(7) 0.0267(7) 0.0207(6) 0.0031(5) -0.0021(5) -0.0030(6) C24 0.0248(7) 0.0216(7) 0.0271(7) -0.0024(5) -0.0016(5) 0.0011(6) C30 0.0229(7) 0.0318(8) 0.0245(7) -0.0017(6) -0.0023(5) -0.0002(6) C12 0.0298(7) 0.0287(8) 0.0257(7) -0.0002(6) 0.0007(6) 0.0016(6) C26 0.0231(7) 0.0227(7) 0.0266(7) -0.0037(5) -0.0006(5) 0.0006(5) C4 0.0225(7) 0.0283(8) 0.0399(8) -0.0042(6) -0.0024(6) 0.0041(6) C8 0.0243(7) 0.0307(8) 0.0281(7) 0.0023(6) -0.0057(6) 0.0022(6) C29 0.0216(7) 0.0272(7) 0.0333(7) -0.0039(6) -0.0017(6) -0.0015(6) C28 0.0258(7) 0.0275(7) 0.0298(7) -0.0031(6) 0.0024(6) -0.0009(6) C23 0.0241(7) 0.0251(7) 0.0296(7) -0.0008(6) -0.0034(6) -0.0030(6) C15 0.0231(7) 0.0380(8) 0.0313(8) -0.0023(6) -0.0006(6) 0.0016(6) C33 0.0263(7) 0.0362(8) 0.0356(8) -0.0054(6) -0.0028(6) -0.0035(6) C9 0.0248(7) 0.0298(7) 0.0220(7) 0.0031(6) -0.0025(5) 0.0011(6) C32 0.0256(7) 0.0373(9) 0.0361(8) -0.0036(7) -0.0051(6) 0.0051(6) C5 0.0289(7) 0.0276(8) 0.0397(8) -0.0060(6) -0.0005(6) 0.0052(6) C34 0.0280(7) 0.0434(9) 0.0331(8) -0.0001(7) 0.0051(6) -0.0060(7) C6 0.0360(9) 0.0390(9) 0.0513(10) -0.0209(8) -0.0096(7) 0.0062(7) C11 0.0244(7) 0.0311(8) 0.0235(7) 0.0028(6) -0.0009(5) 0.0000(6) C7 0.0385(9) 0.0253(8) 0.0667(11) 0.0061(8) -0.0035(8) 0.0011(7) C19 0.0360(8) 0.0311(8) 0.0275(7) -0.0002(6) -0.0023(6) -0.0073(6) C16 0.0263(7) 0.0521(10) 0.0280(8) 0.0001(7) -0.0001(6) -0.0054(7) C14 0.0229(7) 0.0340(8) 0.0254(7) 0.0033(6) -0.0040(5) -0.0017(6) C31 0.0313(8) 0.0562(10) 0.0296(8) 0.0049(7) -0.0069(6) -0.0027(7) C3 0.0311(8) 0.0577(11) 0.0553(11) -0.0064(9) -0.0007(8) 0.0052(8) C1 0.0285(7) 0.0463(9) 0.0336(8) -0.0086(7) 0.0046(6) -0.0115(7) C17 0.0262(7) 0.0472(10) 0.0386(8) 0.0082(7) -0.0053(6) 0.0013(7) C20 0.0628(11) 0.0437(10) 0.0288(8) -0.0030(7) -0.0021(7) -0.0155(8) C18 0.0282(8) 0.0565(11) 0.0607(11) -0.0169(9) -0.0008(8) 0.0076(8) C21 0.0673(12) 0.0332(9) 0.0425(10) 0.0032(7) -0.0098(8) -0.0140(8) C22 0.0407(10) 0.0586(12) 0.0552(11) -0.0163(9) -0.0072(8) -0.0153(9) C35 0.0515(11) 0.0514(11) 0.0518(11) 0.0015(9) 0.0110(8) -0.0211(9) C36 0.0340(9) 0.0640(12) 0.0580(11) -0.0063(9) 0.0157(8) 0.0003(8) C37 0.0391(9) 0.0872(15) 0.0392(9) 0.0142(10) 0.0084(8) -0.0114(9) C2 0.0526(11) 0.0647(13) 0.0653(13) 0.0124(10) 0.0028(10) -0.0248(10) _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 1.7359(10) . ? Al1 O3 1.7589(10) . ? Al1 O2 1.7842(10) . ? Al1 N2 2.1177(13) . ? Al1 N1 2.1969(12) . ? O3 C25 1.3450(16) . ? O1 C1 1.3985(17) . ? O2 C10 1.3430(16) . ? N1 C4 1.4844(17) . ? N1 C23 1.4948(17) . ? N1 C8 1.5026(17) . ? N2 C5 1.4803(18) . ? N2 C6 1.4871(19) . ? N2 C7 1.489(2) . ? C27 C28 1.3930(19) . ? C27 C26 1.3976(19) . ? C13 C14 1.387(2) . ? C13 C12 1.3996(19) . ? C13 C19 1.5370(19) . ? C25 C26 1.4070(19) . ? C25 C24 1.4103(18) . ? C10 C9 1.4027(18) . ? C10 C11 1.417(2) . ? C24 C29 1.3869(19) . ? C24 C23 1.5066(18) . ? C30 C31 1.5312(19) . ? C30 C33 1.534(2) . ? C30 C32 1.538(2) . ? C30 C26 1.5446(18) . ? C12 C11 1.393(2) . ? C4 C5 1.510(2) . ? C8 C9 1.4986(19) . ? C29 C28 1.393(2) . ? C28 C34 1.537(2) . ? C15 C18 1.534(2) . ? C15 C16 1.536(2) . ? C15 C17 1.539(2) . ? C15 C11 1.5404(19) . ? C9 C14 1.3924(19) . ? C34 C35 1.533(2) . ? C34 C37 1.533(2) . ? C34 C36 1.534(2) . ? C19 C21 1.531(2) . ? C19 C22 1.532(2) . ? C19 C20 1.537(2) . ? C3 C1 1.513(2) . ? C1 C2 1.522(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Al1 O3 108.89(5) . . ? O1 Al1 O2 97.15(5) . . ? O3 Al1 O2 109.71(5) . . ? O1 Al1 N2 83.59(5) . . ? O3 Al1 N2 103.23(5) . . ? O2 Al1 N2 144.70(5) . . ? O1 Al1 N1 154.19(5) . . ? O3 Al1 N1 93.04(4) . . ? O2 Al1 N1 87.68(4) . . ? N2 Al1 N1 78.12(4) . . ? C25 O3 Al1 132.65(8) . . ? C1 O1 Al1 137.57(10) . . ? C10 O2 Al1 135.51(9) . . ? C4 N1 C23 110.39(11) . . ? C4 N1 C8 108.00(10) . . ? C23 N1 C8 108.22(10) . . ? C4 N1 Al1 112.56(8) . . ? C23 N1 Al1 107.31(8) . . ? C8 N1 Al1 110.30(8) . . ? C5 N2 C6 107.58(12) . . ? C5 N2 C7 110.04(11) . . ? C6 N2 C7 108.07(12) . . ? C5 N2 Al1 111.48(9) . . ? C6 N2 Al1 112.27(9) . . ? C7 N2 Al1 107.36(10) . . ? C28 C27 C26 123.86(13) . . ? C14 C13 C12 116.50(13) . . ? C14 C13 C19 123.49(13) . . ? C12 C13 C19 120.00(13) . . ? O3 C25 C26 121.59(12) . . ? O3 C25 C24 118.85(12) . . ? C26 C25 C24 119.53(12) . . ? O2 C10 C9 118.90(12) . . ? O2 C10 C11 122.30(12) . . ? C9 C10 C11 118.80(12) . . ? C29 C24 C25 120.28(12) . . ? C29 C24 C23 120.49(12) . . ? C25 C24 C23 118.78(12) . . ? C31 C30 C33 107.50(12) . . ? C31 C30 C32 107.27(12) . . ? C33 C30 C32 109.26(12) . . ? C31 C30 C26 111.92(11) . . ? C33 C30 C26 111.48(11) . . ? C32 C30 C26 109.29(11) . . ? C11 C12 C13 124.55(13) . . ? C27 C26 C25 117.65(12) . . ? C27 C26 C30 121.13(12) . . ? C25 C26 C30 121.14(12) . . ? N1 C4 C5 109.58(11) . . ? C9 C8 N1 113.23(11) . . ? C24 C29 C28 121.61(13) . . ? C29 C28 C27 116.96(13) . . ? C29 C28 C34 120.15(12) . . ? C27 C28 C34 122.88(13) . . ? N1 C23 C24 116.41(11) . . ? C18 C15 C16 107.55(13) . . ? C18 C15 C17 107.61(13) . . ? C16 C15 C17 109.65(12) . . ? C18 C15 C11 112.14(12) . . ? C16 C15 C11 109.46(12) . . ? C17 C15 C11 110.37(11) . . ? C14 C9 C10 121.34(13) . . ? C14 C9 C8 120.58(12) . . ? C10 C9 C8 118.08(12) . . ? N2 C5 C4 108.97(12) . . ? C35 C34 C37 108.27(15) . . ? C35 C34 C36 108.79(14) . . ? C37 C34 C36 108.45(14) . . ? C35 C34 C28 109.99(13) . . ? C37 C34 C28 112.38(12) . . ? C36 C34 C28 108.89(13) . . ? C12 C11 C10 117.45(12) . . ? C12 C11 C15 121.07(13) . . ? C10 C11 C15 121.47(12) . . ? C21 C19 C22 108.17(14) . . ? C21 C19 C13 109.35(12) . . ? C22 C19 C13 112.23(13) . . ? C21 C19 C20 109.09(14) . . ? C22 C19 C20 108.25(13) . . ? C13 C19 C20 109.69(12) . . ? C13 C14 C9 121.27(13) . . ? O1 C1 C3 110.27(13) . . ? O1 C1 C2 108.38(14) . . ? C3 C1 C2 110.52(14) . . ? 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 O1 Al1 O3 C25 -137.51(11) . . . . ? O2 Al1 O3 C25 117.28(11) . . . . ? N2 Al1 O3 C25 -49.85(12) . . . . ? N1 Al1 O3 C25 28.65(12) . . . . ? O3 Al1 O1 C1 -83.04(15) . . . . ? O2 Al1 O1 C1 30.68(15) . . . . ? N2 Al1 O1 C1 175.13(15) . . . . ? N1 Al1 O1 C1 130.22(15) . . . . ? O1 Al1 O2 C10 -179.42(12) . . . . ? O3 Al1 O2 C10 -66.37(13) . . . . ? N2 Al1 O2 C10 91.59(14) . . . . ? N1 Al1 O2 C10 26.03(12) . . . . ? O1 Al1 N1 C4 44.39(16) . . . . ? O3 Al1 N1 C4 -104.30(9) . . . . ? O2 Al1 N1 C4 146.07(9) . . . . ? N2 Al1 N1 C4 -1.41(9) . . . . ? O1 Al1 N1 C23 166.03(11) . . . . ? O3 Al1 N1 C23 17.35(9) . . . . ? O2 Al1 N1 C23 -92.28(8) . . . . ? N2 Al1 N1 C23 120.23(9) . . . . ? O1 Al1 N1 C8 -76.29(14) . . . . ? O3 Al1 N1 C8 135.02(8) . . . . ? O2 Al1 N1 C8 25.39(9) . . . . ? N2 Al1 N1 C8 -122.09(9) . . . . ? O1 Al1 N2 C5 174.21(10) . . . . ? O3 Al1 N2 C5 66.26(10) . . . . ? O2 Al1 N2 C5 -92.46(12) . . . . ? N1 Al1 N2 C5 -24.09(9) . . . . ? O1 Al1 N2 C6 53.42(11) . . . . ? O3 Al1 N2 C6 -54.53(11) . . . . ? O2 Al1 N2 C6 146.75(11) . . . . ? N1 Al1 N2 C6 -144.88(11) . . . . ? O1 Al1 N2 C7 -65.21(9) . . . . ? O3 Al1 N2 C7 -173.16(9) . . . . ? O2 Al1 N2 C7 28.12(13) . . . . ? N1 Al1 N2 C7 96.49(9) . . . . ? Al1 O3 C25 C26 145.02(11) . . . . ? Al1 O3 C25 C24 -36.92(18) . . . . ? Al1 O2 C10 C9 -42.33(18) . . . . ? Al1 O2 C10 C11 138.25(12) . . . . ? O3 C25 C24 C29 178.34(12) . . . . ? C26 C25 C24 C29 -3.6(2) . . . . ? O3 C25 C24 C23 -9.34(18) . . . . ? C26 C25 C24 C23 168.76(12) . . . . ? C14 C13 C12 C11 -1.9(2) . . . . ? C19 C13 C12 C11 177.51(13) . . . . ? C28 C27 C26 C25 -1.2(2) . . . . ? C28 C27 C26 C30 175.75(13) . . . . ? O3 C25 C26 C27 -178.64(12) . . . . ? C24 C25 C26 C27 3.31(19) . . . . ? O3 C25 C26 C30 4.4(2) . . . . ? C24 C25 C26 C30 -173.61(12) . . . . ? C31 C30 C26 C27 0.87(19) . . . . ? C33 C30 C26 C27 121.32(14) . . . . ? C32 C30 C26 C27 -117.80(14) . . . . ? C31 C30 C26 C25 177.68(13) . . . . ? C33 C30 C26 C25 -61.87(16) . . . . ? C32 C30 C26 C25 59.01(17) . . . . ? C23 N1 C4 C5 -94.04(13) . . . . ? C8 N1 C4 C5 147.83(12) . . . . ? Al1 N1 C4 C5 25.83(14) . . . . ? C4 N1 C8 C9 174.44(11) . . . . ? C23 N1 C8 C9 54.93(14) . . . . ? Al1 N1 C8 C9 -62.18(13) . . . . ? C25 C24 C29 C28 1.6(2) . . . . ? C23 C24 C29 C28 -170.63(13) . . . . ? C24 C29 C28 C27 0.6(2) . . . . ? C24 C29 C28 C34 -179.72(13) . . . . ? C26 C27 C28 C29 -0.8(2) . . . . ? C26 C27 C28 C34 179.54(13) . . . . ? C4 N1 C23 C24 67.04(14) . . . . ? C8 N1 C23 C24 -174.97(11) . . . . ? Al1 N1 C23 C24 -55.95(12) . . . . ? C29 C24 C23 N1 -128.56(13) . . . . ? C25 C24 C23 N1 59.14(16) . . . . ? O2 C10 C9 C14 177.31(12) . . . . ? C11 C10 C9 C14 -3.2(2) . . . . ? O2 C10 C9 C8 -2.31(19) . . . . ? C11 C10 C9 C8 177.13(12) . . . . ? N1 C8 C9 C14 -124.99(13) . . . . ? N1 C8 C9 C10 54.64(17) . . . . ? C6 N2 C5 C4 169.13(12) . . . . ? C7 N2 C5 C4 -73.36(15) . . . . ? Al1 N2 C5 C4 45.64(14) . . . . ? N1 C4 C5 N2 -46.12(16) . . . . ? C29 C28 C34 C35 -54.67(19) . . . . ? C27 C28 C34 C35 124.99(16) . . . . ? C29 C28 C34 C37 -175.37(15) . . . . ? C27 C28 C34 C37 4.3(2) . . . . ? C29 C28 C34 C36 64.46(18) . . . . ? C27 C28 C34 C36 -115.88(16) . . . . ? C13 C12 C11 C10 0.2(2) . . . . ? C13 C12 C11 C15 179.91(13) . . . . ? O2 C10 C11 C12 -178.25(12) . . . . ? C9 C10 C11 C12 2.32(19) . . . . ? O2 C10 C11 C15 2.1(2) . . . . ? C9 C10 C11 C15 -177.36(12) . . . . ? C18 C15 C11 C12 -0.1(2) . . . . ? C16 C15 C11 C12 -119.36(14) . . . . ? C17 C15 C11 C12 119.87(15) . . . . ? C18 C15 C11 C10 179.58(14) . . . . ? C16 C15 C11 C10 60.31(16) . . . . ? C17 C15 C11 C10 -60.46(18) . . . . ? C14 C13 C19 C21 123.88(15) . . . . ? C12 C13 C19 C21 -55.48(18) . . . . ? C14 C13 C19 C22 3.8(2) . . . . ? C12 C13 C19 C22 -175.51(14) . . . . ? C14 C13 C19 C20 -116.53(16) . . . . ? C12 C13 C19 C20 64.11(18) . . . . ? C12 C13 C14 C9 1.0(2) . . . . ? C19 C13 C14 C9 -178.40(13) . . . . ? C10 C9 C14 C13 1.6(2) . . . . ? C8 C9 C14 C13 -178.83(13) . . . . ? Al1 O1 C1 C3 90.07(17) . . . . ? Al1 O1 C1 C2 -148.84(13) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.05 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.220 _refine_diff_density_min -0.253 _refine_diff_density_rms 0.035 #===END data_3b _database_code_CSD 207605 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 02156 _chemical_melting_point ? _chemical_formula_moiety 'C31 H49 Al N2 O5' _chemical_formula_sum 'C31 H49 Al N2 O5' _chemical_formula_weight 556.70 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Al Al 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.3444(11) _cell_length_b 12.6782(13) _cell_length_c 12.9992(13) _cell_angle_alpha 79.554(2) _cell_angle_beta 77.283(2) _cell_angle_gamma 66.203(2) _cell_volume 1513.4(3) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 2846 _cell_measurement_theta_min 2.18 _cell_measurement_theta_max 24.93 _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.4 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.222 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 604 _exptl_absorpt_coefficient_mu 0.108 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.915176 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details 'SADABS, R. Blessing, 1995' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'Bruker SMART Platform CCD' _diffrn_measurement_method 'area detector, omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15122 _diffrn_reflns_av_R_equivalents 0.0303 _diffrn_reflns_av_sigmaI/netI 0.0355 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.61 _diffrn_reflns_theta_max 25.08 _reflns_number_total 5374 _reflns_number_gt 4472 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART, Bruker' _computing_cell_refinement 'SAINT, Bruker' _computing_data_reduction 'SAINT, Bruker' _computing_structure_solution SHELXS-97 _computing_structure_refinement SHELXL-97 _computing_molecular_graphics 'SHELXTL, Bruker' _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^)+(0.0421P)^2^+0.4047P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5374 _refine_ls_number_parameters 364 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0452 _refine_ls_R_factor_gt 0.0355 _refine_ls_wR_factor_ref 0.0953 _refine_ls_wR_factor_gt 0.0899 _refine_ls_goodness_of_fit_ref 1.058 _refine_ls_restrained_S_all 1.058 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Al1 Al 0.41602(5) 0.16294(4) 0.20568(3) 0.02054(12) Uani 1 1 d . . . N2 N 0.42478(14) 0.00059(11) 0.28588(10) 0.0261(3) Uani 1 1 d . . . N1 N 0.64589(13) 0.07280(10) 0.20482(9) 0.0221(3) Uani 1 1 d . . . O2 O 0.41618(10) 0.25694(9) 0.28996(8) 0.0237(2) Uani 1 1 d . . . O3 O 0.45373(10) 0.19954(9) 0.06746(8) 0.0238(2) Uani 1 1 d . . . O5 O 0.93677(12) 0.22087(11) -0.20549(9) 0.0371(3) Uani 1 1 d . . . O4 O 0.76380(12) 0.25310(10) 0.55827(9) 0.0347(3) Uani 1 1 d . . . O1 O 0.23273(11) 0.19703(9) 0.21701(8) 0.0270(3) Uani 1 1 d . . . C22 C 0.56898(15) 0.20977(13) 0.00034(11) 0.0220(3) Uani 1 1 d . . . C10 C 0.50267(16) 0.25774(12) 0.35331(11) 0.0219(3) Uani 1 1 d . . . C8 C 0.71155(16) 0.15159(13) 0.22305(12) 0.0250(3) Uani 1 1 d . . . H8A H 0.6972 0.2158 0.1652 0.030 Uiso 1 1 calc R . . H8B H 0.8160 0.1081 0.2199 0.030 Uiso 1 1 calc R . . C9 C 0.65068(16) 0.20166(13) 0.32749(11) 0.0232(3) Uani 1 1 d . . . C24 C 0.68101(16) 0.30380(13) -0.14768(12) 0.0261(3) Uani 1 1 d . . . H24A H 0.6748 0.3652 -0.2029 0.031 Uiso 1 1 calc R . . C23 C 0.55554(16) 0.30238(13) -0.08079(11) 0.0230(3) Uani 1 1 d . . . C21 C 0.70400(16) 0.12423(13) 0.01138(11) 0.0237(3) Uani 1 1 d . . . C27 C 0.40914(16) 0.39651(13) -0.09750(12) 0.0252(3) Uani 1 1 d . . . C11 C 0.44415(16) 0.31777(12) 0.44538(12) 0.0232(3) Uani 1 1 d . . . C12 C 0.53900(17) 0.31316(13) 0.50842(12) 0.0256(3) Uani 1 1 d . . . H12A H 0.5019 0.3527 0.5704 0.031 Uiso 1 1 calc R . . C30 C 0.31864(18) 0.33818(14) -0.12593(13) 0.0319(4) Uani 1 1 d . . . H30A H 0.3148 0.2746 -0.0714 0.048 Uiso 1 1 calc R . . H30B H 0.3621 0.3075 -0.1947 0.048 Uiso 1 1 calc R . . H30C H 0.2214 0.3953 -0.1298 0.048 Uiso 1 1 calc R . . C14 C 0.74227(16) 0.19806(13) 0.39351(12) 0.0256(3) Uani 1 1 d . . . H14A H 0.8428 0.1579 0.3759 0.031 Uiso 1 1 calc R . . C7 C 0.67082(17) -0.02567(13) 0.28865(12) 0.0268(3) Uani 1 1 d . . . H7A H 0.6507 0.0026 0.3589 0.032 Uiso 1 1 calc R . . H7B H 0.7719 -0.0802 0.2764 0.032 Uiso 1 1 calc R . . C13 C 0.68572(17) 0.25326(13) 0.48458(12) 0.0263(3) Uani 1 1 d . . . C25 C 0.81383(16) 0.21862(14) -0.13590(12) 0.0274(4) Uani 1 1 d . . . C26 C 0.82608(16) 0.12910(14) -0.05677(12) 0.0272(4) Uani 1 1 d . . . H26A H 0.9174 0.0708 -0.0486 0.033 Uiso 1 1 calc R . . C6 C 0.57307(17) -0.08612(13) 0.28584(13) 0.0292(4) Uani 1 1 d . . . H6A H 0.6053 -0.1271 0.2213 0.035 Uiso 1 1 calc R . . H6B H 0.5759 -0.1441 0.3485 0.035 Uiso 1 1 calc R . . C18 C 0.23890(18) 0.48573(14) 0.38085(13) 0.0321(4) Uani 1 1 d . . . H18A H 0.2873 0.5391 0.3771 0.048 Uiso 1 1 calc R . . H18B H 0.1350 0.5282 0.3941 0.048 Uiso 1 1 calc R . . H18C H 0.2663 0.4516 0.3136 0.048 Uiso 1 1 calc R . . C15 C 0.28300(16) 0.38905(13) 0.47138(12) 0.0253(3) Uani 1 1 d . . . C20 C 0.71396(16) 0.02803(13) 0.09890(12) 0.0253(3) Uani 1 1 d . . . H20A H 0.8160 -0.0217 0.1006 0.030 Uiso 1 1 calc R . . H20B H 0.6662 -0.0202 0.0845 0.030 Uiso 1 1 calc R . . C17 C 0.19585(17) 0.31246(14) 0.48514(13) 0.0306(4) Uani 1 1 d . . . H17A H 0.2293 0.2475 0.5393 0.046 Uiso 1 1 calc R . . H17B H 0.2084 0.2826 0.4177 0.046 Uiso 1 1 calc R . . H17C H 0.0943 0.3585 0.5073 0.046 Uiso 1 1 calc R . . C5 C 0.35597(19) 0.02424(14) 0.39708(12) 0.0331(4) Uani 1 1 d . . . H5A H 0.3563 -0.0481 0.4394 0.050 Uiso 1 1 calc R . . H5B H 0.2570 0.0798 0.3979 0.050 Uiso 1 1 calc R . . H5C H 0.4093 0.0566 0.4271 0.050 Uiso 1 1 calc R . . C29 C 0.33301(17) 0.45973(14) 0.00237(13) 0.0299(4) Uani 1 1 d . . . H29A H 0.3848 0.5056 0.0133 0.045 Uiso 1 1 calc R . . H29B H 0.3309 0.4027 0.0640 0.045 Uiso 1 1 calc R . . H29C H 0.2348 0.5112 -0.0066 0.045 Uiso 1 1 calc R . . C28 C 0.42141(19) 0.48900(15) -0.18903(14) 0.0358(4) Uani 1 1 d . . . H28A H 0.4794 0.5273 -0.1735 0.054 Uiso 1 1 calc R . . H28B H 0.3256 0.5465 -0.1972 0.054 Uiso 1 1 calc R . . H28C H 0.4671 0.4522 -0.2548 0.054 Uiso 1 1 calc R . . C1 C 0.12900(16) 0.27354(15) 0.15699(13) 0.0314(4) Uani 1 1 d . . . H1A H 0.1768 0.3090 0.0931 0.038 Uiso 1 1 calc R . . C4 C 0.3431(2) -0.05106(15) 0.24399(15) 0.0389(4) Uani 1 1 d . . . H4A H 0.3497 -0.1252 0.2855 0.058 Uiso 1 1 calc R . . H4B H 0.3833 -0.0638 0.1696 0.058 Uiso 1 1 calc R . . H4C H 0.2424 0.0019 0.2493 0.058 Uiso 1 1 calc R . . C16 C 0.24440(19) 0.44734(15) 0.57351(13) 0.0350(4) Uani 1 1 d . . . H16A H 0.2709 0.3879 0.6332 0.052 Uiso 1 1 calc R . . H16B H 0.1411 0.4927 0.5866 0.052 Uiso 1 1 calc R . . H16C H 0.2965 0.4987 0.5660 0.052 Uiso 1 1 calc R . . C31 C 0.9844(2) 0.30548(17) -0.18860(15) 0.0434(5) Uani 1 1 d . . . H31A H 1.0619 0.3098 -0.2460 0.065 Uiso 1 1 calc R . . H31B H 1.0195 0.2842 -0.1207 0.065 Uiso 1 1 calc R . . H31C H 0.9047 0.3811 -0.1874 0.065 Uiso 1 1 calc R . . C19 C 0.91291(19) 0.18845(19) 0.54032(15) 0.0461(5) Uani 1 1 d . . . H19A H 0.9555 0.1944 0.5982 0.069 Uiso 1 1 calc R . . H19B H 0.9560 0.2191 0.4730 0.069 Uiso 1 1 calc R . . H19C H 0.9306 0.1070 0.5373 0.069 Uiso 1 1 calc R . . C3 C 0.0218(2) 0.36843(19) 0.22219(19) 0.0594(6) Uani 1 1 d . . . H3A H 0.0715 0.4091 0.2454 0.089 Uiso 1 1 calc R . . H3B H -0.0269 0.3345 0.2843 0.089 Uiso 1 1 calc R . . H3C H -0.0489 0.4233 0.1791 0.089 Uiso 1 1 calc R . . C2 C 0.0559(2) 0.2084(2) 0.12152(18) 0.0578(6) Uani 1 1 d . . . H2A H 0.1264 0.1496 0.0765 0.087 Uiso 1 1 calc R . . H2B H -0.0186 0.2625 0.0812 0.087 Uiso 1 1 calc R . . H2C H 0.0124 0.1705 0.1837 0.087 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 0.0211(2) 0.0209(2) 0.0193(2) -0.00247(17) -0.00355(17) -0.00734(18) N2 0.0306(7) 0.0239(7) 0.0255(7) -0.0027(5) -0.0052(6) -0.0117(6) N1 0.0239(6) 0.0220(6) 0.0182(6) -0.0021(5) -0.0035(5) -0.0064(5) O2 0.0223(5) 0.0243(6) 0.0244(6) -0.0059(4) -0.0057(4) -0.0062(4) O3 0.0206(5) 0.0284(6) 0.0203(5) -0.0011(4) -0.0036(4) -0.0077(5) O5 0.0306(6) 0.0459(7) 0.0331(6) -0.0095(5) 0.0077(5) -0.0172(6) O4 0.0360(7) 0.0443(7) 0.0317(6) -0.0085(5) -0.0127(5) -0.0178(6) O1 0.0225(6) 0.0307(6) 0.0273(6) 0.0004(5) -0.0057(4) -0.0101(5) C22 0.0239(8) 0.0262(8) 0.0169(7) -0.0064(6) -0.0021(6) -0.0096(6) C10 0.0271(8) 0.0199(7) 0.0213(8) -0.0001(6) -0.0060(6) -0.0113(6) C8 0.0217(8) 0.0299(8) 0.0236(8) -0.0038(6) -0.0026(6) -0.0102(7) C9 0.0266(8) 0.0239(8) 0.0209(8) -0.0005(6) -0.0034(6) -0.0123(7) C24 0.0311(9) 0.0272(8) 0.0198(8) -0.0021(6) -0.0033(6) -0.0113(7) C23 0.0251(8) 0.0236(8) 0.0206(7) -0.0066(6) -0.0043(6) -0.0074(7) C21 0.0257(8) 0.0247(8) 0.0192(7) -0.0060(6) -0.0041(6) -0.0063(7) C27 0.0261(8) 0.0234(8) 0.0252(8) -0.0023(6) -0.0072(6) -0.0070(7) C11 0.0276(8) 0.0200(8) 0.0221(8) -0.0009(6) -0.0025(6) -0.0105(6) C12 0.0337(9) 0.0242(8) 0.0214(8) -0.0035(6) -0.0035(6) -0.0137(7) C30 0.0349(9) 0.0278(9) 0.0339(9) -0.0025(7) -0.0159(7) -0.0078(7) C14 0.0236(8) 0.0269(8) 0.0281(8) -0.0007(7) -0.0050(6) -0.0121(7) C7 0.0278(8) 0.0240(8) 0.0230(8) 0.0000(6) -0.0056(6) -0.0043(7) C13 0.0333(9) 0.0266(8) 0.0257(8) 0.0003(6) -0.0085(7) -0.0174(7) C25 0.0262(8) 0.0350(9) 0.0218(8) -0.0089(7) 0.0014(6) -0.0126(7) C26 0.0228(8) 0.0316(9) 0.0234(8) -0.0081(7) -0.0036(6) -0.0042(7) C6 0.0366(9) 0.0215(8) 0.0259(8) -0.0010(6) -0.0054(7) -0.0076(7) C18 0.0334(9) 0.0256(8) 0.0301(9) -0.0045(7) -0.0032(7) -0.0042(7) C15 0.0272(8) 0.0246(8) 0.0214(8) -0.0053(6) -0.0012(6) -0.0072(7) C20 0.0239(8) 0.0246(8) 0.0220(8) -0.0050(6) -0.0030(6) -0.0031(6) C17 0.0251(8) 0.0312(9) 0.0322(9) -0.0052(7) 0.0007(7) -0.0091(7) C5 0.0404(10) 0.0290(9) 0.0269(9) 0.0007(7) 0.0009(7) -0.0148(8) C29 0.0278(8) 0.0268(8) 0.0336(9) -0.0092(7) -0.0046(7) -0.0065(7) C28 0.0362(10) 0.0297(9) 0.0361(10) 0.0033(7) -0.0101(8) -0.0077(8) C1 0.0227(8) 0.0395(10) 0.0296(9) 0.0030(7) -0.0058(7) -0.0114(7) C4 0.0476(11) 0.0325(10) 0.0473(11) -0.0031(8) -0.0151(9) -0.0227(9) C16 0.0362(9) 0.0372(10) 0.0280(9) -0.0103(7) -0.0011(7) -0.0093(8) C31 0.0368(10) 0.0495(11) 0.0463(11) -0.0024(9) -0.0006(8) -0.0229(9) C19 0.0356(10) 0.0663(13) 0.0439(11) -0.0121(10) -0.0162(9) -0.0192(10) C3 0.0437(12) 0.0490(13) 0.0728(15) -0.0151(11) -0.0191(11) 0.0038(10) C2 0.0497(13) 0.0756(16) 0.0606(14) -0.0104(12) -0.0259(11) -0.0265(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 Al1 O1 1.7441(11) . ? Al1 O2 1.7597(11) . ? Al1 O3 1.7694(11) . ? Al1 N2 2.1083(13) . ? Al1 N1 2.1818(13) . ? N2 C6 1.483(2) . ? N2 C5 1.489(2) . ? N2 C4 1.489(2) . ? N1 C7 1.4775(19) . ? N1 C8 1.4897(19) . ? N1 C20 1.4992(18) . ? O2 C10 1.3466(17) . ? O3 C22 1.3510(17) . ? O5 C25 1.3964(18) . ? O5 C31 1.414(2) . ? O4 C13 1.3816(18) . ? O4 C19 1.413(2) . ? O1 C1 1.3983(19) . ? C22 C21 1.399(2) . ? C22 C23 1.412(2) . ? C10 C9 1.394(2) . ? C10 C11 1.421(2) . ? C8 C9 1.502(2) . ? C9 C14 1.395(2) . ? C24 C25 1.383(2) . ? C24 C23 1.399(2) . ? C23 C27 1.535(2) . ? C21 C26 1.391(2) . ? C21 C20 1.497(2) . ? C27 C28 1.534(2) . ? C27 C29 1.538(2) . ? C27 C30 1.539(2) . ? C11 C12 1.389(2) . ? C11 C15 1.535(2) . ? C12 C13 1.387(2) . ? C14 C13 1.378(2) . ? C7 C6 1.504(2) . ? C25 C26 1.371(2) . ? C18 C15 1.535(2) . ? C15 C16 1.534(2) . ? C15 C17 1.536(2) . ? C1 C2 1.504(3) . ? C1 C3 1.508(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Al1 O2 100.84(5) . . ? O1 Al1 O3 98.51(5) . . ? O2 Al1 O3 117.33(5) . . ? O1 Al1 N2 85.68(5) . . ? O2 Al1 N2 112.67(5) . . ? O3 Al1 N2 127.83(5) . . ? O1 Al1 N1 164.37(5) . . ? O2 Al1 N1 88.26(5) . . ? O3 Al1 N1 88.33(5) . . ? N2 Al1 N1 79.06(5) . . ? C6 N2 C5 109.04(12) . . ? C6 N2 C4 107.98(12) . . ? C5 N2 C4 107.88(13) . . ? C6 N2 Al1 113.19(9) . . ? C5 N2 Al1 104.95(9) . . ? C4 N2 Al1 113.58(10) . . ? C7 N1 C8 109.42(11) . . ? C7 N1 C20 109.34(11) . . ? C8 N1 C20 109.06(11) . . ? C7 N1 Al1 109.15(9) . . ? C8 N1 Al1 111.43(9) . . ? C20 N1 Al1 108.41(9) . . ? C10 O2 Al1 137.32(10) . . ? C22 O3 Al1 134.47(9) . . ? C25 O5 C31 113.98(13) . . ? C13 O4 C19 117.36(13) . . ? C1 O1 Al1 133.06(10) . . ? O3 C22 C21 118.27(13) . . ? O3 C22 C23 121.74(13) . . ? C21 C22 C23 119.98(13) . . ? O2 C10 C9 120.06(13) . . ? O2 C10 C11 120.32(13) . . ? C9 C10 C11 119.60(13) . . ? N1 C8 C9 113.48(12) . . ? C10 C9 C14 121.17(14) . . ? C10 C9 C8 118.76(13) . . ? C14 C9 C8 119.94(13) . . ? C25 C24 C23 122.05(14) . . ? C24 C23 C22 117.37(13) . . ? C24 C23 C27 120.88(13) . . ? C22 C23 C27 121.73(13) . . ? C26 C21 C22 120.77(14) . . ? C26 C21 C20 120.85(14) . . ? C22 C21 C20 118.38(13) . . ? C28 C27 C23 112.38(13) . . ? C28 C27 C29 107.02(13) . . ? C23 C27 C29 111.16(12) . . ? C28 C27 C30 107.52(13) . . ? C23 C27 C30 108.08(12) . . ? C29 C27 C30 110.63(13) . . ? C12 C11 C10 117.40(14) . . ? C12 C11 C15 121.43(13) . . ? C10 C11 C15 121.13(13) . . ? C13 C12 C11 122.69(14) . . ? C13 C14 C9 119.40(14) . . ? N1 C7 C6 108.31(12) . . ? C14 C13 O4 125.18(14) . . ? C14 C13 C12 119.64(14) . . ? O4 C13 C12 115.16(13) . . ? C26 C25 C24 120.25(14) . . ? C26 C25 O5 119.00(14) . . ? C24 C25 O5 120.73(14) . . ? C25 C26 C21 119.58(14) . . ? N2 C6 C7 109.35(12) . . ? C16 C15 C11 112.09(13) . . ? C16 C15 C18 107.30(13) . . ? C11 C15 C18 108.81(12) . . ? C16 C15 C17 107.83(13) . . ? C11 C15 C17 111.05(12) . . ? C18 C15 C17 109.67(13) . . ? C21 C20 N1 111.97(12) . . ? O1 C1 C2 109.61(15) . . ? O1 C1 C3 109.67(14) . . ? C2 C1 C3 110.65(16) . . ? 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 O1 Al1 N2 C6 169.43(10) . . . . ? O2 Al1 N2 C6 -90.61(10) . . . . ? O3 Al1 N2 C6 72.01(11) . . . . ? N1 Al1 N2 C6 -7.17(10) . . . . ? O1 Al1 N2 C5 -71.76(10) . . . . ? O2 Al1 N2 C5 28.19(11) . . . . ? O3 Al1 N2 C5 -169.19(9) . . . . ? N1 Al1 N2 C5 111.63(10) . . . . ? O1 Al1 N2 C4 45.83(11) . . . . ? O2 Al1 N2 C4 145.79(11) . . . . ? O3 Al1 N2 C4 -51.59(13) . . . . ? N1 Al1 N2 C4 -130.77(12) . . . . ? O1 Al1 N1 C7 -32.7(2) . . . . ? O2 Al1 N1 C7 93.42(10) . . . . ? O3 Al1 N1 C7 -149.17(10) . . . . ? N2 Al1 N1 C7 -20.07(9) . . . . ? O1 Al1 N1 C8 -153.69(18) . . . . ? O2 Al1 N1 C8 -27.54(9) . . . . ? O3 Al1 N1 C8 89.87(9) . . . . ? N2 Al1 N1 C8 -141.03(10) . . . . ? O1 Al1 N1 C20 86.3(2) . . . . ? O2 Al1 N1 C20 -147.57(9) . . . . ? O3 Al1 N1 C20 -30.15(9) . . . . ? N2 Al1 N1 C20 98.95(10) . . . . ? O1 Al1 O2 C10 149.49(13) . . . . ? O3 Al1 O2 C10 -104.92(14) . . . . ? N2 Al1 O2 C10 59.67(15) . . . . ? N1 Al1 O2 C10 -17.71(14) . . . . ? O1 Al1 O3 C22 170.86(13) . . . . ? O2 Al1 O3 C22 63.91(14) . . . . ? N2 Al1 O3 C22 -98.01(14) . . . . ? N1 Al1 O3 C22 -23.27(13) . . . . ? O2 Al1 O1 C1 94.39(14) . . . . ? O3 Al1 O1 C1 -25.70(14) . . . . ? N2 Al1 O1 C1 -153.34(14) . . . . ? N1 Al1 O1 C1 -140.88(19) . . . . ? Al1 O3 C22 C21 43.88(19) . . . . ? Al1 O3 C22 C23 -137.42(12) . . . . ? Al1 O2 C10 C9 31.7(2) . . . . ? Al1 O2 C10 C11 -149.73(12) . . . . ? C7 N1 C8 C9 -60.48(16) . . . . ? C20 N1 C8 C9 179.95(12) . . . . ? Al1 N1 C8 C9 60.32(14) . . . . ? O2 C10 C9 C14 -177.92(13) . . . . ? C11 C10 C9 C14 3.5(2) . . . . ? O2 C10 C9 C8 6.2(2) . . . . ? C11 C10 C9 C8 -172.39(13) . . . . ? N1 C8 C9 C10 -52.83(18) . . . . ? N1 C8 C9 C14 131.24(14) . . . . ? C25 C24 C23 C22 0.0(2) . . . . ? C25 C24 C23 C27 -178.47(14) . . . . ? O3 C22 C23 C24 -178.60(13) . . . . ? C21 C22 C23 C24 0.1(2) . . . . ? O3 C22 C23 C27 -0.2(2) . . . . ? C21 C22 C23 C27 178.49(13) . . . . ? O3 C22 C21 C26 178.76(13) . . . . ? C23 C22 C21 C26 0.0(2) . . . . ? O3 C22 C21 C20 -1.8(2) . . . . ? C23 C22 C21 C20 179.48(13) . . . . ? C24 C23 C27 C28 -2.5(2) . . . . ? C22 C23 C27 C28 179.10(14) . . . . ? C24 C23 C27 C29 -122.46(15) . . . . ? C22 C23 C27 C29 59.18(18) . . . . ? C24 C23 C27 C30 115.96(15) . . . . ? C22 C23 C27 C30 -62.40(18) . . . . ? O2 C10 C11 C12 178.71(13) . . . . ? C9 C10 C11 C12 -2.7(2) . . . . ? O2 C10 C11 C15 -3.8(2) . . . . ? C9 C10 C11 C15 174.79(13) . . . . ? C10 C11 C12 C13 0.1(2) . . . . ? C15 C11 C12 C13 -177.38(13) . . . . ? C10 C9 C14 C13 -1.6(2) . . . . ? C8 C9 C14 C13 174.26(14) . . . . ? C8 N1 C7 C6 165.45(12) . . . . ? C20 N1 C7 C6 -75.16(15) . . . . ? Al1 N1 C7 C6 43.28(14) . . . . ? C9 C14 C13 O4 177.74(14) . . . . ? C9 C14 C13 C12 -1.1(2) . . . . ? C19 O4 C13 C14 -1.9(2) . . . . ? C19 O4 C13 C12 176.93(15) . . . . ? C11 C12 C13 C14 1.8(2) . . . . ? C11 C12 C13 O4 -177.12(13) . . . . ? C23 C24 C25 C26 -0.1(2) . . . . ? C23 C24 C25 O5 178.45(13) . . . . ? C31 O5 C25 C26 -106.69(17) . . . . ? C31 O5 C25 C24 74.72(19) . . . . ? C24 C25 C26 C21 0.2(2) . . . . ? O5 C25 C26 C21 -178.35(13) . . . . ? C22 C21 C26 C25 -0.2(2) . . . . ? C20 C21 C26 C25 -179.63(14) . . . . ? C5 N2 C6 C7 -83.50(15) . . . . ? C4 N2 C6 C7 159.53(13) . . . . ? Al1 N2 C6 C7 32.91(15) . . . . ? N1 C7 C6 N2 -50.10(16) . . . . ? C12 C11 C15 C16 -1.9(2) . . . . ? C10 C11 C15 C16 -179.31(14) . . . . ? C12 C11 C15 C18 116.60(15) . . . . ? C10 C11 C15 C18 -60.80(18) . . . . ? C12 C11 C15 C17 -122.59(15) . . . . ? C10 C11 C15 C17 60.01(18) . . . . ? C26 C21 C20 N1 125.25(14) . . . . ? C22 C21 C20 N1 -54.19(18) . . . . ? C7 N1 C20 C21 -174.83(12) . . . . ? C8 N1 C20 C21 -55.22(15) . . . . ? Al1 N1 C20 C21 66.27(13) . . . . ? Al1 O1 C1 C2 124.27(15) . . . . ? Al1 O1 C1 C3 -114.07(16) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.08 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.226 _refine_diff_density_min -0.241 _refine_diff_density_rms 0.037 #===END data_3c _database_code_CSD 207606 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 02180m _chemical_melting_point ? _chemical_formula_moiety 'C29 H43 Al Br2 N2 O3, 0.5(C7 H8)' _chemical_formula_sum 'C32.50 H47 Al Br2 N2 O3' _chemical_formula_weight 700.52 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Al Al 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 '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 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.1742(11) _cell_length_b 13.0089(14) _cell_length_c 14.1058(15) _cell_angle_alpha 111.851(2) _cell_angle_beta 94.902(2) _cell_angle_gamma 99.557(2) _cell_volume 1686.5(3) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 3256 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.6 _exptl_crystal_size_mid 0.5 _exptl_crystal_size_min 0.5 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.379 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 726 _exptl_absorpt_coefficient_mu 2.463 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.820246 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details 'SADABS, R. Blessing, 1995' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'Bruker SMART Platform CCD' _diffrn_measurement_method 'area detector, omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16745 _diffrn_reflns_av_R_equivalents 0.0287 _diffrn_reflns_av_sigmaI/netI 0.0342 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.58 _diffrn_reflns_theta_max 25.06 _reflns_number_total 5965 _reflns_number_gt 4725 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART, Bruker' _computing_cell_refinement 'SAINT, Bruker' _computing_data_reduction 'SAINT, Bruker' _computing_structure_solution SHELXS-97 _computing_structure_refinement SHELXL-97 _computing_molecular_graphics 'SHELXTL, Bruker' _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0453P)^2^+0.8459P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5965 _refine_ls_number_parameters 377 _refine_ls_number_restraints 52 _refine_ls_R_factor_all 0.0493 _refine_ls_R_factor_gt 0.0342 _refine_ls_wR_factor_ref 0.0892 _refine_ls_wR_factor_gt 0.0831 _refine_ls_goodness_of_fit_ref 1.025 _refine_ls_restrained_S_all 1.031 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Al1 Al 0.70420(7) 0.29631(6) 0.10137(6) 0.02495(18) Uani 1 1 d . . . Br1 Br 0.45333(4) 0.80717(3) 0.39576(2) 0.04629(11) Uani 1 1 d . . . Br2 Br 0.24240(3) 0.02992(3) 0.35450(3) 0.05247(12) Uani 1 1 d . . . N1 N 0.4936(2) 0.30052(18) 0.10201(16) 0.0262(5) Uani 1 1 d . . . N2 N 0.6498(2) 0.29725(19) -0.04523(16) 0.0311(5) Uani 1 1 d . . . O1 O 0.86236(18) 0.28377(16) 0.06589(15) 0.0345(4) Uani 1 1 d . . . O2 O 0.74543(17) 0.43525(15) 0.19773(13) 0.0301(4) Uani 1 1 d . . . O3 O 0.67479(17) 0.17928(15) 0.13913(14) 0.0289(4) Uani 1 1 d . . . C1 C 0.9639(3) 0.2349(3) 0.0932(2) 0.0424(7) Uani 1 1 d . . . H1A H 0.9267 0.1903 0.1329 0.051 Uiso 1 1 calc R . . C2 C 1.0037(4) 0.1546(3) -0.0024(3) 0.0676(11) Uani 1 1 d . . . H2A H 0.9240 0.0968 -0.0449 0.101 Uiso 1 1 calc R . . H2B H 1.0715 0.1178 0.0175 0.101 Uiso 1 1 calc R . . H2C H 1.0416 0.1967 -0.0422 0.101 Uiso 1 1 calc R . . C3 C 1.0824(4) 0.3247(4) 0.1618(4) 0.0806(14) Uani 1 1 d . . . H3A H 1.0534 0.3729 0.2248 0.121 Uiso 1 1 calc R . . H3B H 1.1189 0.3711 0.1251 0.121 Uiso 1 1 calc R . . H3C H 1.1523 0.2889 0.1804 0.121 Uiso 1 1 calc R . . C4 C 0.4483(3) 0.3441(2) 0.0248(2) 0.0329(6) Uani 1 1 d . . . H4A H 0.4813 0.4273 0.0518 0.039 Uiso 1 1 calc R . . H4B H 0.3484 0.3273 0.0103 0.039 Uiso 1 1 calc R . . C5 C 0.5031(3) 0.2879(3) -0.0728(2) 0.0364(7) Uani 1 1 d . . . H5A H 0.4565 0.2072 -0.1072 0.044 Uiso 1 1 calc R . . H5B H 0.4878 0.3255 -0.1210 0.044 Uiso 1 1 calc R . . C6 C 0.6920(4) 0.2031(3) -0.1279(2) 0.0550(9) Uani 1 1 d . . . H6A H 0.6631 0.2039 -0.1956 0.083 Uiso 1 1 calc R . . H6B H 0.6501 0.1303 -0.1265 0.083 Uiso 1 1 calc R . . H6C H 0.7905 0.2135 -0.1157 0.083 Uiso 1 1 calc R . . C7 C 0.7257(3) 0.4062(3) -0.0428(2) 0.0423(7) Uani 1 1 d . . . H7A H 0.7060 0.4097 -0.1106 0.063 Uiso 1 1 calc R . . H7B H 0.8228 0.4116 -0.0260 0.063 Uiso 1 1 calc R . . H7C H 0.6986 0.4694 0.0100 0.063 Uiso 1 1 calc R . . C8 C 0.4722(3) 0.3728(2) 0.2072(2) 0.0294(6) Uani 1 1 d . . . H8A H 0.5039 0.3416 0.2570 0.035 Uiso 1 1 calc R . . H8B H 0.3743 0.3694 0.2070 0.035 Uiso 1 1 calc R . . C9 C 0.5440(3) 0.4944(2) 0.24320(19) 0.0263(6) Uani 1 1 d . . . C10 C 0.6826(3) 0.5202(2) 0.24203(19) 0.0276(6) Uani 1 1 d . . . C11 C 0.7565(3) 0.6336(2) 0.2900(2) 0.0315(6) Uani 1 1 d . . . C12 C 0.6839(3) 0.7166(2) 0.3349(2) 0.0347(7) Uani 1 1 d . . . H12A H 0.7306 0.7936 0.3679 0.042 Uiso 1 1 calc R . . C13 C 0.5471(3) 0.6903(2) 0.3328(2) 0.0320(6) Uani 1 1 d . . . C14 C 0.4754(3) 0.5803(2) 0.2881(2) 0.0308(6) Uani 1 1 d . . . H14A H 0.3808 0.5630 0.2878 0.037 Uiso 1 1 calc R . . C15 C 0.9101(3) 0.6635(2) 0.2983(2) 0.0425(7) Uani 1 1 d . . . C16 C 0.9524(4) 0.6239(3) 0.1910(3) 0.0585(10) Uani 1 1 d . . . H16A H 0.9296 0.5409 0.1584 0.088 Uiso 1 1 calc R . . H16B H 1.0500 0.6507 0.1979 0.088 Uiso 1 1 calc R . . H16C H 0.9046 0.6548 0.1480 0.088 Uiso 1 1 calc R . . C17 C 0.9752(3) 0.6073(3) 0.3626(3) 0.0537(9) Uani 1 1 d . . . H17A H 0.9390 0.5253 0.3312 0.081 Uiso 1 1 calc R . . H17B H 0.9549 0.6381 0.4332 0.081 Uiso 1 1 calc R . . H17C H 1.0732 0.6226 0.3645 0.081 Uiso 1 1 calc R . . C18 C 0.9668(4) 0.7925(3) 0.3532(3) 0.0657(11) Uani 1 1 d . . . H18A H 0.9458 0.8195 0.4237 0.099 Uiso 1 1 calc R . . H18B H 0.9258 0.8315 0.3148 0.099 Uiso 1 1 calc R . . H18C H 1.0650 0.8085 0.3559 0.099 Uiso 1 1 calc R . . C19 C 0.4146(3) 0.1823(2) 0.0737(2) 0.0317(6) Uani 1 1 d . . . H19A H 0.3169 0.1811 0.0629 0.038 Uiso 1 1 calc R . . H19B H 0.4370 0.1312 0.0080 0.038 Uiso 1 1 calc R . . C20 C 0.4454(3) 0.1401(2) 0.1566(2) 0.0296(6) Uani 1 1 d . . . C21 C 0.5808(3) 0.1408(2) 0.1862(2) 0.0277(6) Uani 1 1 d . . . C22 C 0.6153(3) 0.1018(2) 0.2646(2) 0.0284(6) Uani 1 1 d . . . C23 C 0.5112(3) 0.0693(2) 0.3125(2) 0.0326(6) Uani 1 1 d . . . H23A H 0.5315 0.0433 0.3656 0.039 Uiso 1 1 calc R . . C24 C 0.3798(3) 0.0737(2) 0.2849(2) 0.0348(7) Uani 1 1 d . . . C25 C 0.3443(3) 0.1075(2) 0.2064(2) 0.0341(6) Uani 1 1 d . . . H25A H 0.2530 0.1084 0.1867 0.041 Uiso 1 1 calc R . . C26 C 0.7611(3) 0.0963(2) 0.2964(2) 0.0326(6) Uani 1 1 d . . . C27 C 0.7734(3) 0.0504(3) 0.3814(3) 0.0479(8) Uani 1 1 d . . . H27A H 0.8676 0.0468 0.3981 0.072 Uiso 1 1 calc R . . H27B H 0.7160 -0.0257 0.3571 0.072 Uiso 1 1 calc R . . H27C H 0.7445 0.1007 0.4433 0.072 Uiso 1 1 calc R . . C28 C 0.8524(3) 0.2154(2) 0.3389(2) 0.0399(7) Uani 1 1 d . . . H28A H 0.9466 0.2100 0.3526 0.060 Uiso 1 1 calc R . . H28B H 0.8256 0.2627 0.4034 0.060 Uiso 1 1 calc R . . H28C H 0.8434 0.2495 0.2880 0.060 Uiso 1 1 calc R . . C29 C 0.8109(3) 0.0158(2) 0.2025(2) 0.0385(7) Uani 1 1 d . . . H29A H 0.9064 0.0174 0.2211 0.058 Uiso 1 1 calc R . . H29B H 0.8000 0.0403 0.1450 0.058 Uiso 1 1 calc R . . H29C H 0.7579 -0.0614 0.1817 0.058 Uiso 1 1 calc R . . C1S C 0.5869(6) 0.4900(6) 0.5006(7) 0.059(2) Uiso 0.352(6) 1 d PGDU A -1 C2S C 0.4853(7) 0.3923(5) 0.4614(6) 0.038(2) Uiso 0.352(6) 1 d PGDU A -1 H2S H 0.5079 0.3199 0.4370 0.046 Uiso 0.352(6) 1 calc PR A -1 C3S C 0.3507(7) 0.4006(5) 0.4580(6) 0.051(2) Uiso 0.352(6) 1 d PGDU A -1 H3S H 0.2813 0.3338 0.4312 0.061 Uiso 0.352(6) 1 calc PR A -1 C4S C 0.3176(6) 0.5065(6) 0.4937(7) 0.075(4) Uiso 0.352(6) 1 d PGDU A -1 H4S H 0.2256 0.5121 0.4913 0.090 Uiso 0.352(6) 1 calc PR A -1 C5S C 0.4192(8) 0.6042(5) 0.5329(6) 0.045(2) Uiso 0.352(6) 1 d PGDU A -1 H5S H 0.3966 0.6766 0.5573 0.054 Uiso 0.352(6) 1 calc PR A -1 C6S C 0.5539(7) 0.5959(5) 0.5364(6) 0.050(3) Uiso 0.352(6) 1 d PGDU A -1 H6S H 0.6233 0.6627 0.5631 0.061 Uiso 0.352(6) 1 calc PR A -1 C7S C 0.7135(18) 0.4838(10) 0.5030(16) 0.107(6) Uiso 0.352(6) 1 d PDU A -1 H7S1 H 0.7703 0.5604 0.5326 0.161 Uiso 0.352(6) 1 calc PR A -1 H7S2 H 0.7301 0.4438 0.4326 0.161 Uiso 0.352(6) 1 calc PR A -1 H7S3 H 0.7352 0.4424 0.5458 0.161 Uiso 0.352(6) 1 calc PR A -1 C1S' C 0.5194(19) 0.4747(11) 0.4923(15) 0.060(4) Uiso 0.148(6) 1 d PGDU A -2 C2S' C 0.418(2) 0.3766(9) 0.4521(14) 0.045(4) Uiso 0.148(6) 1 d PGDU A -2 H2S' H 0.4417 0.3044 0.4297 0.054 Uiso 0.148(6) 1 calc PR A -2 C3S' C 0.284(2) 0.3840(11) 0.4445(14) 0.049(4) Uiso 0.148(6) 1 d PGDU A -2 H3S' H 0.2146 0.3169 0.4169 0.059 Uiso 0.148(6) 1 calc PR A -2 C4S' C 0.2495(19) 0.4895(13) 0.4771(15) 0.066(5) Uiso 0.148(6) 1 d PGDU A -2 H4S' H 0.1573 0.4946 0.4719 0.079 Uiso 0.148(6) 1 calc PR A -2 C5S' C 0.350(2) 0.5877(11) 0.5174(14) 0.047(4) Uiso 0.148(6) 1 d PGDU A -2 H5S' H 0.3272 0.6598 0.5397 0.057 Uiso 0.148(6) 1 calc PR A -2 C6S' C 0.485(2) 0.5803(10) 0.5250(14) 0.030(4) Uiso 0.148(6) 1 d PGDU A -2 H6S' H 0.5543 0.6473 0.5525 0.037 Uiso 0.148(6) 1 calc PR A -2 C7S' C 0.645(3) 0.4668(18) 0.489(4) 0.109(9) Uiso 0.148(6) 1 d PDU A -2 H7S4 H 0.7031 0.5429 0.5181 0.164 Uiso 0.148(6) 1 calc PR A -2 H7S5 H 0.6565 0.4281 0.4166 0.164 Uiso 0.148(6) 1 calc PR A -2 H7S6 H 0.6698 0.4235 0.5288 0.164 Uiso 0.148(6) 1 calc PR A -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 Al1 0.0218(4) 0.0272(4) 0.0251(4) 0.0095(3) 0.0043(3) 0.0047(3) Br1 0.0634(2) 0.03777(18) 0.04085(18) 0.01196(14) 0.01693(15) 0.02328(15) Br2 0.0471(2) 0.0517(2) 0.0692(2) 0.03173(18) 0.03083(17) 0.00903(16) N1 0.0244(11) 0.0271(11) 0.0263(11) 0.0103(9) 0.0026(9) 0.0042(9) N2 0.0351(13) 0.0320(12) 0.0245(11) 0.0083(10) 0.0058(10) 0.0085(10) O1 0.0274(10) 0.0417(11) 0.0408(11) 0.0195(9) 0.0133(8) 0.0122(9) O2 0.0232(10) 0.0300(10) 0.0314(10) 0.0063(8) 0.0057(8) 0.0036(8) O3 0.0232(9) 0.0324(10) 0.0350(10) 0.0165(8) 0.0067(8) 0.0075(8) C1 0.0225(15) 0.056(2) 0.0547(19) 0.0251(16) 0.0120(13) 0.0119(14) C2 0.054(2) 0.063(2) 0.080(3) 0.013(2) 0.012(2) 0.0324(19) C3 0.036(2) 0.077(3) 0.104(3) 0.009(3) -0.007(2) 0.018(2) C4 0.0268(15) 0.0388(16) 0.0357(15) 0.0178(13) 0.0001(12) 0.0088(12) C5 0.0377(17) 0.0403(16) 0.0298(15) 0.0146(13) -0.0027(12) 0.0062(13) C6 0.075(2) 0.058(2) 0.0262(16) 0.0020(15) 0.0100(16) 0.0306(19) C7 0.0423(18) 0.0526(19) 0.0422(17) 0.0303(16) 0.0097(14) 0.0083(15) C8 0.0255(14) 0.0307(14) 0.0333(15) 0.0134(12) 0.0081(11) 0.0059(11) C9 0.0283(14) 0.0287(14) 0.0231(13) 0.0118(11) 0.0047(11) 0.0050(11) C10 0.0310(15) 0.0284(14) 0.0230(13) 0.0096(11) 0.0063(11) 0.0054(12) C11 0.0365(16) 0.0301(15) 0.0262(14) 0.0112(12) 0.0046(12) 0.0023(12) C12 0.0463(18) 0.0264(14) 0.0269(14) 0.0089(12) 0.0030(13) 0.0008(13) C13 0.0447(17) 0.0298(15) 0.0246(14) 0.0108(12) 0.0089(12) 0.0141(13) C14 0.0324(15) 0.0369(16) 0.0276(14) 0.0164(12) 0.0082(11) 0.0092(12) C15 0.0372(17) 0.0320(16) 0.0456(18) 0.0066(14) 0.0059(14) -0.0053(13) C16 0.045(2) 0.059(2) 0.062(2) 0.0189(18) 0.0214(17) -0.0064(17) C17 0.0348(18) 0.052(2) 0.059(2) 0.0108(17) -0.0066(16) -0.0005(15) C18 0.047(2) 0.041(2) 0.086(3) 0.0086(19) 0.0079(19) -0.0120(16) C19 0.0206(14) 0.0307(15) 0.0382(16) 0.0103(12) -0.0015(11) 0.0012(11) C20 0.0269(15) 0.0200(13) 0.0372(15) 0.0078(11) 0.0036(12) 0.0020(11) C21 0.0271(14) 0.0217(13) 0.0307(14) 0.0067(11) 0.0067(11) 0.0031(11) C22 0.0321(15) 0.0176(12) 0.0317(14) 0.0054(11) 0.0054(11) 0.0048(11) C23 0.0374(16) 0.0251(14) 0.0352(15) 0.0112(12) 0.0095(12) 0.0063(12) C24 0.0385(17) 0.0243(14) 0.0417(16) 0.0121(13) 0.0181(13) 0.0029(12) C25 0.0259(15) 0.0245(14) 0.0490(18) 0.0114(13) 0.0083(13) 0.0037(11) C26 0.0317(16) 0.0328(15) 0.0345(15) 0.0143(12) 0.0049(12) 0.0080(12) C27 0.048(2) 0.056(2) 0.051(2) 0.0312(17) 0.0059(15) 0.0176(16) C28 0.0353(17) 0.0379(17) 0.0392(17) 0.0098(14) -0.0021(13) 0.0054(13) C29 0.0337(16) 0.0345(16) 0.0457(18) 0.0118(14) 0.0058(13) 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 Al1 O1 1.7408(19) . ? Al1 O2 1.7642(19) . ? Al1 O3 1.7806(19) . ? Al1 N2 2.099(2) . ? Al1 N1 2.153(2) . ? Br1 C13 1.906(3) . ? Br2 C24 1.905(3) . ? N1 C4 1.476(3) . ? N1 C8 1.489(3) . ? N1 C19 1.500(3) . ? N2 C5 1.483(4) . ? N2 C7 1.484(4) . ? N2 C6 1.497(4) . ? O1 C1 1.397(3) . ? O2 C10 1.345(3) . ? O3 C21 1.343(3) . ? C1 C3 1.499(5) . ? C1 C2 1.503(5) . ? C4 C5 1.502(4) . ? C8 C9 1.499(4) . ? C9 C14 1.395(4) . ? C9 C10 1.398(4) . ? C10 C11 1.415(4) . ? C11 C12 1.396(4) . ? C11 C15 1.530(4) . ? C12 C13 1.373(4) . ? C13 C14 1.371(4) . ? C15 C17 1.532(5) . ? C15 C16 1.532(4) . ? C15 C18 1.545(4) . ? C19 C20 1.496(4) . ? C20 C25 1.389(4) . ? C20 C21 1.402(4) . ? C21 C22 1.420(4) . ? C22 C23 1.394(4) . ? C22 C26 1.533(4) . ? C23 C24 1.376(4) . ? C24 C25 1.378(4) . ? C26 C27 1.531(4) . ? C26 C28 1.535(4) . ? C26 C29 1.537(4) . ? C1S C7S 1.302(17) . ? C1S C2S 1.3900 . ? C1S C6S 1.3900 . ? C2S C3S 1.3900 . ? C3S C4S 1.3900 . ? C4S C5S 1.3900 . ? C5S C6S 1.3900 . ? C1S' C7S' 1.302(18) . ? C1S' C2S' 1.3900 . ? C1S' C6S' 1.3900 . ? C2S' C3S' 1.3900 . ? C3S' C4S' 1.3900 . ? C4S' C5S' 1.3900 . ? C5S' C6S' 1.3900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Al1 O2 99.77(9) . . ? O1 Al1 O3 98.13(9) . . ? O2 Al1 O3 119.15(9) . . ? O1 Al1 N2 85.89(9) . . ? O2 Al1 N2 111.08(9) . . ? O3 Al1 N2 127.88(9) . . ? O1 Al1 N1 164.74(9) . . ? O2 Al1 N1 89.00(8) . . ? O3 Al1 N1 88.27(8) . . ? N2 Al1 N1 79.28(9) . . ? C4 N1 C8 110.9(2) . . ? C4 N1 C19 109.5(2) . . ? C8 N1 C19 108.6(2) . . ? C4 N1 Al1 109.03(16) . . ? C8 N1 Al1 110.17(15) . . ? C19 N1 Al1 108.67(15) . . ? C5 N2 C7 109.5(2) . . ? C5 N2 C6 108.3(2) . . ? C7 N2 C6 107.9(2) . . ? C5 N2 Al1 113.58(16) . . ? C7 N2 Al1 106.33(17) . . ? C6 N2 Al1 111.05(18) . . ? C1 O1 Al1 133.28(18) . . ? C10 O2 Al1 138.09(16) . . ? C21 O3 Al1 134.34(16) . . ? O1 C1 C3 110.6(3) . . ? O1 C1 C2 110.1(3) . . ? C3 C1 C2 111.9(3) . . ? N1 C4 C5 108.7(2) . . ? N2 C5 C4 108.4(2) . . ? N1 C8 C9 113.5(2) . . ? C14 C9 C10 120.6(2) . . ? C14 C9 C8 119.6(2) . . ? C10 C9 C8 119.4(2) . . ? O2 C10 C9 119.0(2) . . ? O2 C10 C11 120.5(2) . . ? C9 C10 C11 120.4(2) . . ? C12 C11 C10 117.0(2) . . ? C12 C11 C15 121.3(2) . . ? C10 C11 C15 121.7(2) . . ? C13 C12 C11 121.9(3) . . ? C14 C13 C12 121.4(3) . . ? C14 C13 Br1 118.5(2) . . ? C12 C13 Br1 120.1(2) . . ? C13 C14 C9 118.7(3) . . ? C11 C15 C17 109.4(2) . . ? C11 C15 C16 111.0(3) . . ? C17 C15 C16 109.6(3) . . ? C11 C15 C18 111.8(3) . . ? C17 C15 C18 107.2(3) . . ? C16 C15 C18 107.7(3) . . ? C20 C19 N1 111.2(2) . . ? C25 C20 C21 121.3(3) . . ? C25 C20 C19 121.0(2) . . ? C21 C20 C19 117.6(2) . . ? O3 C21 C20 118.5(2) . . ? O3 C21 C22 121.7(2) . . ? C20 C21 C22 119.8(2) . . ? C23 C22 C21 117.3(2) . . ? C23 C22 C26 121.1(2) . . ? C21 C22 C26 121.6(2) . . ? C24 C23 C22 121.8(3) . . ? C23 C24 C25 121.4(3) . . ? C23 C24 Br2 119.8(2) . . ? C25 C24 Br2 118.7(2) . . ? C24 C25 C20 118.3(3) . . ? C27 C26 C22 112.2(2) . . ? C27 C26 C28 107.0(2) . . ? C22 C26 C28 110.2(2) . . ? C27 C26 C29 107.1(2) . . ? C22 C26 C29 109.4(2) . . ? C28 C26 C29 110.8(2) . . ? C7S C1S C2S 120.8(4) . . ? C7S C1S C6S 119.2(4) . . ? C2S C1S C6S 120.0 . . ? C1S C2S C3S 120.0 . . ? C2S C3S C4S 120.0 . . ? C5S C4S C3S 120.0 . . ? C4S C5S C6S 120.0 . . ? C5S C6S C1S 120.0 . . ? C7S' C1S' C2S' 119.3(5) . . ? C7S' C1S' C6S' 120.2(5) . . ? C2S' C1S' C6S' 120.0 . . ? C1S' C2S' C3S' 120.0 . . ? C4S' C3S' C2S' 120.0 . . ? C5S' C4S' C3S' 120.0 . . ? C4S' C5S' C6S' 120.0 . . ? C5S' C6S' C1S' 120.0 . . ? 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 O1 Al1 N1 C4 -34.9(4) . . . . ? O2 Al1 N1 C4 90.64(17) . . . . ? O3 Al1 N1 C4 -150.16(17) . . . . ? N2 Al1 N1 C4 -21.04(17) . . . . ? O1 Al1 N1 C8 -156.8(3) . . . . ? O2 Al1 N1 C8 -31.26(17) . . . . ? O3 Al1 N1 C8 87.94(16) . . . . ? N2 Al1 N1 C8 -142.94(17) . . . . ? O1 Al1 N1 C19 84.4(4) . . . . ? O2 Al1 N1 C19 -150.10(17) . . . . ? O3 Al1 N1 C19 -30.90(17) . . . . ? N2 Al1 N1 C19 98.22(17) . . . . ? O1 Al1 N2 C5 170.32(19) . . . . ? O2 Al1 N2 C5 -90.78(19) . . . . ? O3 Al1 N2 C5 73.2(2) . . . . ? N1 Al1 N2 C5 -6.06(18) . . . . ? O1 Al1 N2 C7 -69.19(18) . . . . ? O2 Al1 N2 C7 29.7(2) . . . . ? O3 Al1 N2 C7 -166.30(17) . . . . ? N1 Al1 N2 C7 114.43(18) . . . . ? O1 Al1 N2 C6 47.9(2) . . . . ? O2 Al1 N2 C6 146.8(2) . . . . ? O3 Al1 N2 C6 -49.2(2) . . . . ? N1 Al1 N2 C6 -128.5(2) . . . . ? O2 Al1 O1 C1 97.9(3) . . . . ? O3 Al1 O1 C1 -23.7(3) . . . . ? N2 Al1 O1 C1 -151.4(3) . . . . ? N1 Al1 O1 C1 -137.8(4) . . . . ? O1 Al1 O2 C10 156.0(2) . . . . ? O3 Al1 O2 C10 -98.9(3) . . . . ? N2 Al1 O2 C10 66.7(3) . . . . ? N1 Al1 O2 C10 -11.4(3) . . . . ? O1 Al1 O3 C21 171.3(2) . . . . ? O2 Al1 O3 C21 65.3(2) . . . . ? N2 Al1 O3 C21 -97.6(2) . . . . ? N1 Al1 O3 C21 -22.6(2) . . . . ? Al1 O1 C1 C3 -108.0(3) . . . . ? Al1 O1 C1 C2 127.8(3) . . . . ? C8 N1 C4 C5 165.8(2) . . . . ? C19 N1 C4 C5 -74.5(3) . . . . ? Al1 N1 C4 C5 44.3(2) . . . . ? C7 N2 C5 C4 -87.1(3) . . . . ? C6 N2 C5 C4 155.5(2) . . . . ? Al1 N2 C5 C4 31.6(3) . . . . ? N1 C4 C5 N2 -49.6(3) . . . . ? C4 N1 C8 C9 -58.4(3) . . . . ? C19 N1 C8 C9 -178.7(2) . . . . ? Al1 N1 C8 C9 62.4(2) . . . . ? N1 C8 C9 C14 133.7(2) . . . . ? N1 C8 C9 C10 -53.5(3) . . . . ? Al1 O2 C10 C9 25.7(4) . . . . ? Al1 O2 C10 C11 -156.5(2) . . . . ? C14 C9 C10 O2 -179.8(2) . . . . ? C8 C9 C10 O2 7.5(4) . . . . ? C14 C9 C10 C11 2.4(4) . . . . ? C8 C9 C10 C11 -170.3(2) . . . . ? O2 C10 C11 C12 -179.5(2) . . . . ? C9 C10 C11 C12 -1.7(4) . . . . ? O2 C10 C11 C15 -3.2(4) . . . . ? C9 C10 C11 C15 174.6(2) . . . . ? C10 C11 C12 C13 -0.2(4) . . . . ? C15 C11 C12 C13 -176.5(3) . . . . ? C11 C12 C13 C14 1.4(4) . . . . ? C11 C12 C13 Br1 179.9(2) . . . . ? C12 C13 C14 C9 -0.7(4) . . . . ? Br1 C13 C14 C9 -179.16(18) . . . . ? C10 C9 C14 C13 -1.2(4) . . . . ? C8 C9 C14 C13 171.5(2) . . . . ? C12 C11 C15 C17 114.5(3) . . . . ? C10 C11 C15 C17 -61.7(3) . . . . ? C12 C11 C15 C16 -124.4(3) . . . . ? C10 C11 C15 C16 59.4(4) . . . . ? C12 C11 C15 C18 -4.2(4) . . . . ? C10 C11 C15 C18 179.7(3) . . . . ? C4 N1 C19 C20 -173.1(2) . . . . ? C8 N1 C19 C20 -51.9(3) . . . . ? Al1 N1 C19 C20 67.9(2) . . . . ? N1 C19 C20 C25 120.4(3) . . . . ? N1 C19 C20 C21 -56.0(3) . . . . ? Al1 O3 C21 C20 42.4(3) . . . . ? Al1 O3 C21 C22 -137.3(2) . . . . ? C25 C20 C21 O3 -176.3(2) . . . . ? C19 C20 C21 O3 0.2(3) . . . . ? C25 C20 C21 C22 3.5(4) . . . . ? C19 C20 C21 C22 179.9(2) . . . . ? O3 C21 C22 C23 176.7(2) . . . . ? C20 C21 C22 C23 -3.0(4) . . . . ? O3 C21 C22 C26 -2.9(4) . . . . ? C20 C21 C22 C26 177.4(2) . . . . ? C21 C22 C23 C24 0.4(4) . . . . ? C26 C22 C23 C24 180.0(2) . . . . ? C22 C23 C24 C25 1.9(4) . . . . ? C22 C23 C24 Br2 -179.15(19) . . . . ? C23 C24 C25 C20 -1.6(4) . . . . ? Br2 C24 C25 C20 179.50(19) . . . . ? C21 C20 C25 C24 -1.1(4) . . . . ? C19 C20 C25 C24 -177.4(2) . . . . ? C23 C22 C26 C27 1.1(3) . . . . ? C21 C22 C26 C27 -179.3(2) . . . . ? C23 C22 C26 C28 -118.1(3) . . . . ? C21 C22 C26 C28 61.5(3) . . . . ? C23 C22 C26 C29 119.8(3) . . . . ? C21 C22 C26 C29 -60.6(3) . . . . ? C7S C1S C2S C3S -179.0(14) . . . . ? C6S C1S C2S C3S 0.0 . . . . ? C1S C2S C3S C4S 0.0 . . . . ? C2S C3S C4S C5S 0.0 . . . . ? C3S C4S C5S C6S 0.0 . . . . ? C4S C5S C6S C1S 0.0 . . . . ? C7S C1S C6S C5S 179.0(14) . . . . ? C2S C1S C6S C5S 0.0 . . . . ? C7S' C1S' C2S' C3S' -173(3) . . . . ? C6S' C1S' C2S' C3S' 0.0 . . . . ? C1S' C2S' C3S' C4S' 0.0 . . . . ? C2S' C3S' C4S' C5S' 0.0 . . . . ? C3S' C4S' C5S' C6S' 0.0 . . . . ? C4S' C5S' C6S' C1S' 0.0 . . . . ? C7S' C1S' C6S' C5S' 173(3) . . . . ? C2S' C1S' C6S' C5S' 0.0 . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.06 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.689 _refine_diff_density_min -0.487 _refine_diff_density_rms 0.057