Supplementary Material (ESI) for Chemical Communications This journal is (C) The Royal Society of Chemistry 2001 data_global _journal_coden_Cambridge 182 _publ_requested_journal 'Chemical Communications' loop_ _publ_author_name 'Elsegood, Mark R. J.' 'Redshaw, Carl' _publ_contact_author_name 'Carl Redshaw' _publ_contact_author_address ; Department of Chemistry Imperial College South Kensington London SW7 2AY UNITED KINGDOM ; _publ_contact_author_email 'CARL.REDSHAW@UEA.AC.UK' _publ_section_title ; Novel Organoaluminium (and Gallium) Carboxylate-bridged Ring Systems ; data_1 _database_code_CSD 167944 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C94 H115 Al4 N5 O12' _chemical_formula_weight 1614.83 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Al' 'Al' 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 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 17.8616(19) _cell_length_b 27.115(3) _cell_length_c 19.081(2) _cell_angle_alpha 90.00 _cell_angle_beta 95.703(2) _cell_angle_gamma 90.00 _cell_volume 9195.6(17) _cell_formula_units_Z 4 _cell_measurement_temperature 160(2) _cell_measurement_reflns_used 15543 _cell_measurement_theta_min 2.62 _cell_measurement_theta_max 27.81 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.13 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.166 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3448 _exptl_absorpt_coefficient_mu 0.111 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 160(2) _diffrn_radiation_wavelength 0.6878 _diffrn_radiation_type synchrotron _diffrn_radiation_source 'Daresbury SRS Station 9.8' _diffrn_radiation_monochromator 'Silicon 111' _diffrn_measurement_device_type 'Bruker SMART 1K CCD diffractometer' _diffrn_measurement_method '\w rotation with narrow frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 10 _diffrn_reflns_number 59798 _diffrn_reflns_av_R_equivalents 0.0939 _diffrn_reflns_av_sigmaI/netI 0.1431 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -35 _diffrn_reflns_limit_k_max 36 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.59 _diffrn_reflns_theta_max 27.50 _reflns_number_total 23109 _reflns_number_gt 10681 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'local programs' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'SHELXTL and local programs' _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^)+(0.0711P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 23109 _refine_ls_number_parameters 1093 _refine_ls_number_restraints 107 _refine_ls_R_factor_all 0.1756 _refine_ls_R_factor_gt 0.0709 _refine_ls_wR_factor_ref 0.1792 _refine_ls_wR_factor_gt 0.1392 _refine_ls_goodness_of_fit_ref 0.958 _refine_ls_restrained_S_all 0.957 _refine_ls_shift/su_max 0.062 _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 Al1 Al 0.30396(5) 0.20041(3) 0.26887(5) 0.0239(2) Uani 1 1 d . . . O1 O 0.34156(10) 0.13931(7) 0.29391(11) 0.0264(5) Uani 1 1 d . . . C1 C 0.32424(16) 0.11291(10) 0.34691(16) 0.0263(7) Uani 1 1 d . . . C2 C 0.37238(17) 0.07477(11) 0.37717(17) 0.0304(7) Uani 1 1 d . . . C3 C 0.35460(18) 0.05394(11) 0.43944(18) 0.0351(8) Uani 1 1 d . . . H3 H 0.3886 0.0302 0.4612 0.042 Uiso 1 1 calc R . . C4 C 0.28999(18) 0.06510(11) 0.47330(17) 0.0331(7) Uani 1 1 d . . . C5 C 0.23937(17) 0.09621(11) 0.43791(17) 0.0323(7) Uani 1 1 d . . . H5 H 0.1926 0.1021 0.4562 0.039 Uiso 1 1 calc R . . C6 C 0.25453(16) 0.11977(10) 0.37510(17) 0.0283(7) Uani 1 1 d . . . C7 C 0.43748(18) 0.05569(11) 0.33765(19) 0.0358(8) Uani 1 1 d . . . C8 C 0.4810(2) 0.01466(15) 0.3778(2) 0.0692(14) Uani 1 1 d . . . H8A H 0.5045 0.0275 0.4227 0.104 Uiso 1 1 calc R . . H8B H 0.5200 0.0022 0.3498 0.104 Uiso 1 1 calc R . . H8C H 0.4465 -0.0122 0.3868 0.104 Uiso 1 1 calc R . . C9 C 0.4040(2) 0.03566(14) 0.2657(2) 0.0561(11) Uani 1 1 d . . . H9A H 0.3696 0.0084 0.2730 0.084 Uiso 1 1 calc R . . H9B H 0.4446 0.0239 0.2391 0.084 Uiso 1 1 calc R . . H9C H 0.3763 0.0620 0.2392 0.084 Uiso 1 1 calc R . . C10 C 0.49329(18) 0.09643(13) 0.3247(2) 0.0483(10) Uani 1 1 d . . . H10A H 0.4680 0.1218 0.2943 0.072 Uiso 1 1 calc R . . H10B H 0.5352 0.0825 0.3018 0.072 Uiso 1 1 calc R . . H10C H 0.5125 0.1113 0.3698 0.072 Uiso 1 1 calc R . . C11 C 0.2796(2) 0.04372(12) 0.54536(19) 0.0418(9) Uani 1 1 d . . . C12 C 0.2901(3) -0.01176(14) 0.5459(2) 0.0770(15) Uani 1 1 d . . . H12A H 0.2516 -0.0269 0.5125 0.115 Uiso 1 1 calc R . . H12B H 0.2854 -0.0245 0.5933 0.115 Uiso 1 1 calc R . . H12C H 0.3401 -0.0197 0.5322 0.115 Uiso 1 1 calc R . . C13 C 0.2022(2) 0.05501(18) 0.5676(2) 0.0782(15) Uani 1 1 d . . . H13A H 0.1957 0.0908 0.5707 0.117 Uiso 1 1 calc R . . H13B H 0.1973 0.0401 0.6137 0.117 Uiso 1 1 calc R . . H13C H 0.1636 0.0415 0.5328 0.117 Uiso 1 1 calc R . . C14 C 0.3394(2) 0.06717(15) 0.5992(2) 0.0655(12) Uani 1 1 d . . . H14A H 0.3897 0.0603 0.5853 0.098 Uiso 1 1 calc R . . H14B H 0.3350 0.0532 0.6460 0.098 Uiso 1 1 calc R . . H14C H 0.3316 0.1029 0.6006 0.098 Uiso 1 1 calc R . . C15 C 0.19511(17) 0.14616(10) 0.33566(17) 0.0285(7) Uani 1 1 d . . . H15 H 0.1461 0.1430 0.3505 0.034 Uiso 1 1 calc R . . N1 N 0.20220(13) 0.17427(8) 0.28104(13) 0.0257(6) Uani 1 1 d . . . C16 C 0.13372(16) 0.18955(11) 0.24265(16) 0.0279(7) Uani 1 1 d . . . C17 C 0.07273(17) 0.15760(12) 0.23345(18) 0.0365(8) Uani 1 1 d . . . H17 H 0.0780 0.1247 0.2502 0.044 Uiso 1 1 calc R . . C18 C 0.00428(19) 0.17320(14) 0.20011(19) 0.0454(9) Uani 1 1 d . . . H18 H -0.0373 0.1512 0.1950 0.055 Uiso 1 1 calc R . . C19 C -0.00348(19) 0.22035(14) 0.1745(2) 0.0486(10) Uani 1 1 d . . . H19 H -0.0507 0.2312 0.1526 0.058 Uiso 1 1 calc R . . C20 C 0.05734(18) 0.25196(13) 0.18065(19) 0.0415(9) Uani 1 1 d . . . H20 H 0.0519 0.2843 0.1616 0.050 Uiso 1 1 calc R . . C21 C 0.12686(16) 0.23721(11) 0.21446(16) 0.0290(7) Uani 1 1 d . . . C22 C 0.18991(17) 0.27277(11) 0.21786(16) 0.0290(7) Uani 1 1 d . . . O2 O 0.25663(11) 0.25986(7) 0.23488(11) 0.0278(5) Uani 1 1 d . . . O3 O 0.17291(12) 0.31691(7) 0.20094(13) 0.0394(6) Uani 1 1 d . . . O4 O 0.31032(10) 0.22745(7) 0.35744(10) 0.0264(5) Uani 1 1 d . . . C23 C 0.33899(17) 0.27004(10) 0.37914(16) 0.0276(7) Uani 1 1 d . . . C24 C 0.31329(17) 0.29539(11) 0.43729(17) 0.0327(7) Uani 1 1 d . . . C25 C 0.34891(19) 0.33885(11) 0.45865(18) 0.0364(8) Uani 1 1 d . . . H25 H 0.3312 0.3558 0.4973 0.044 Uiso 1 1 calc R . . C26 C 0.4098(2) 0.35996(11) 0.42730(19) 0.0397(8) Uani 1 1 d . . . C27 C 0.43270(19) 0.33571(11) 0.37106(18) 0.0361(8) Uani 1 1 d . . . H27 H 0.4730 0.3490 0.3481 0.043 Uiso 1 1 calc R . . C28 C 0.39840(17) 0.29108(11) 0.34531(16) 0.0290(7) Uani 1 1 d . . . C29 C 0.2475(2) 0.27490(13) 0.47443(19) 0.0419(9) Uani 1 1 d . . . C30 C 0.2269(2) 0.30842(15) 0.5343(2) 0.0653(12) Uani 1 1 d . . . H30A H 0.2697 0.3108 0.5705 0.098 Uiso 1 1 calc R . . H30B H 0.1835 0.2945 0.5552 0.098 Uiso 1 1 calc R . . H30C H 0.2141 0.3414 0.5157 0.098 Uiso 1 1 calc R . . C31 C 0.2682(2) 0.22450(13) 0.50701(19) 0.0496(10) Uani 1 1 d . . . H31A H 0.2816 0.2019 0.4702 0.074 Uiso 1 1 calc R . . H31B H 0.2251 0.2112 0.5289 0.074 Uiso 1 1 calc R . . H31C H 0.3111 0.2281 0.5428 0.074 Uiso 1 1 calc R . . C32 C 0.17692(19) 0.27046(14) 0.4211(2) 0.0525(10) Uani 1 1 d . . . H32A H 0.1658 0.3026 0.3988 0.079 Uiso 1 1 calc R . . H32B H 0.1340 0.2599 0.4456 0.079 Uiso 1 1 calc R . . H32C H 0.1861 0.2461 0.3849 0.079 Uiso 1 1 calc R . . C33 C 0.4455(2) 0.40821(12) 0.4577(2) 0.0495(10) Uani 1 1 d . . . C34 C 0.5143(3) 0.42181(16) 0.4207(3) 0.0848(16) Uani 1 1 d . . . H34A H 0.4986 0.4303 0.3715 0.127 Uiso 1 1 calc R . . H34B H 0.5490 0.3937 0.4223 0.127 Uiso 1 1 calc R . . H34C H 0.5397 0.4502 0.4443 0.127 Uiso 1 1 calc R . . C35 C 0.3870(3) 0.44913(13) 0.4487(2) 0.0729(14) Uani 1 1 d . . . H35A H 0.3421 0.4392 0.4708 0.109 Uiso 1 1 calc R . . H35B H 0.3734 0.4552 0.3984 0.109 Uiso 1 1 calc R . . H35C H 0.4078 0.4793 0.4711 0.109 Uiso 1 1 calc R . . C36 C 0.4711(2) 0.40213(14) 0.5361(2) 0.0593(11) Uani 1 1 d . . . H36A H 0.4903 0.4337 0.5554 0.089 Uiso 1 1 calc R . . H36B H 0.5111 0.3773 0.5421 0.089 Uiso 1 1 calc R . . H36C H 0.4285 0.3915 0.5609 0.089 Uiso 1 1 calc R . . C37 C 0.43138(16) 0.26670(10) 0.29048(16) 0.0271(7) Uani 1 1 d . . . H37 H 0.4758 0.2810 0.2758 0.033 Uiso 1 1 calc R . . N2 N 0.40690(13) 0.22641(8) 0.25795(13) 0.0252(6) Uani 1 1 d . . . C38 C 0.45704(16) 0.20148(10) 0.21629(17) 0.0277(7) Uani 1 1 d . . . C39 C 0.53439(17) 0.20465(11) 0.23394(18) 0.0344(8) Uani 1 1 d . . . H39 H 0.5538 0.2247 0.2723 0.041 Uiso 1 1 calc R . . C40 C 0.58317(18) 0.17847(12) 0.1955(2) 0.0419(9) Uani 1 1 d . . . H40 H 0.6359 0.1818 0.2068 0.050 Uiso 1 1 calc R . . C41 C 0.55645(19) 0.14788(13) 0.1417(2) 0.0441(9) Uani 1 1 d . . . H41 H 0.5903 0.1298 0.1161 0.053 Uiso 1 1 calc R . . C42 C 0.48020(18) 0.14374(11) 0.12518(18) 0.0357(8) Uani 1 1 d . . . H42 H 0.4616 0.1223 0.0881 0.043 Uiso 1 1 calc R . . C43 C 0.42951(16) 0.17011(11) 0.16121(16) 0.0288(7) Uani 1 1 d . . . C44 C 0.34810(17) 0.16340(11) 0.13940(17) 0.0291(7) Uani 1 1 d . . . O5 O 0.29833(11) 0.18127(7) 0.17354(11) 0.0276(5) Uani 1 1 d . . . O6 O 0.33214(12) 0.13821(8) 0.08342(12) 0.0362(5) Uani 1 1 d . . . Al3 Al 0.23973(6) 0.11769(4) 0.04487(6) 0.0384(3) Uani 1 1 d . . . C45 C 0.1931(2) 0.08026(13) 0.1161(2) 0.0565(11) Uani 1 1 d . . . H45A H 0.1973 0.0988 0.1604 0.085 Uiso 1 1 calc R . . H45B H 0.2185 0.0484 0.1234 0.085 Uiso 1 1 calc R . . H45C H 0.1398 0.0748 0.1003 0.085 Uiso 1 1 calc R . . C46 C 0.2561(2) 0.08814(16) -0.0451(2) 0.0751(14) Uani 1 1 d . . . H46A H 0.2075 0.0813 -0.0718 0.113 Uiso 1 1 calc R . . H46B H 0.2841 0.0573 -0.0370 0.113 Uiso 1 1 calc R . . H46C H 0.2850 0.1109 -0.0718 0.113 Uiso 1 1 calc R . . Al4 Al 0.22315(6) 0.37492(4) 0.20099(6) 0.0371(3) Uani 1 1 d . . . C47 C 0.2361(2) 0.40101(15) 0.2961(2) 0.0570(11) Uani 1 1 d . . . H47A H 0.2088 0.4322 0.2978 0.085 Uiso 1 1 calc R . . H47B H 0.2898 0.4067 0.3100 0.085 Uiso 1 1 calc R . . H47C H 0.2165 0.3773 0.3284 0.085 Uiso 1 1 calc R . . C48 C 0.1740(2) 0.41121(13) 0.1211(2) 0.0605(12) Uani 1 1 d . . . H48A H 0.1881 0.3968 0.0772 0.091 Uiso 1 1 calc R . . H48B H 0.1900 0.4458 0.1240 0.091 Uiso 1 1 calc R . . H48C H 0.1193 0.4093 0.1219 0.091 Uiso 1 1 calc R . . Al2 Al 0.31159(5) 0.29465(3) -0.00702(5) 0.0262(2) Uani 1 1 d . . . O7 O 0.34975(10) 0.35413(7) -0.02956(11) 0.0268(5) Uani 1 1 d . . . C49 C 0.33482(16) 0.37874(10) -0.08855(16) 0.0263(7) Uani 1 1 d . . . C50 C 0.39003(17) 0.40925(10) -0.11568(16) 0.0282(7) Uani 1 1 d . . . C51 C 0.36988(17) 0.43346(11) -0.17816(17) 0.0317(7) Uani 1 1 d . . . H51 H 0.4067 0.4539 -0.1961 0.038 Uiso 1 1 calc R . . C52 C 0.29870(18) 0.43034(11) -0.21774(17) 0.0310(7) Uani 1 1 d . A . C53 C 0.24603(17) 0.40151(11) -0.19011(17) 0.0314(7) Uani 1 1 d . . . H53 H 0.1971 0.3989 -0.2144 0.038 Uiso 1 1 calc R . . C54 C 0.26258(16) 0.37560(10) -0.12635(16) 0.0274(7) Uani 1 1 d . . . C55 C 0.46923(17) 0.41272(12) -0.07664(18) 0.0352(8) Uani 1 1 d . . . C56 C 0.50582(18) 0.36137(12) -0.07704(19) 0.0408(9) Uani 1 1 d . . . H56A H 0.4754 0.3378 -0.0532 0.061 Uiso 1 1 calc R . . H56B H 0.5566 0.3629 -0.0524 0.061 Uiso 1 1 calc R . . H56C H 0.5088 0.3508 -0.1258 0.061 Uiso 1 1 calc R . . C57 C 0.51894(19) 0.44841(13) -0.11405(19) 0.0444(9) Uani 1 1 d . . . H57A H 0.5226 0.4370 -0.1623 0.067 Uiso 1 1 calc R . . H57B H 0.5693 0.4496 -0.0885 0.067 Uiso 1 1 calc R . . H57C H 0.4966 0.4814 -0.1152 0.067 Uiso 1 1 calc R . . C58 C 0.4658(2) 0.43125(12) -0.00116(18) 0.0431(9) Uani 1 1 d . . . H58A H 0.4425 0.4640 -0.0023 0.065 Uiso 1 1 calc R . . H58B H 0.5169 0.4333 0.0227 0.065 Uiso 1 1 calc R . . H58C H 0.4358 0.4083 0.0243 0.065 Uiso 1 1 calc R . . C59 C 0.28423(19) 0.45884(12) -0.28711(18) 0.0395(8) Uani 1 1 d DU . . C60 C 0.3419(3) 0.4442(2) -0.3366(2) 0.0643(15) Uani 0.900(5) 1 d PDU A 1 H60A H 0.3376 0.4089 -0.3467 0.096 Uiso 0.900(5) 1 calc PR A 1 H60B H 0.3925 0.4515 -0.3144 0.096 Uiso 0.900(5) 1 calc PR A 1 H60C H 0.3328 0.4629 -0.3806 0.096 Uiso 0.900(5) 1 calc PR A 1 C61 C 0.2919(3) 0.51473(15) -0.2723(2) 0.0659(16) Uani 0.900(5) 1 d PDU A 1 H61A H 0.2818 0.5330 -0.3166 0.099 Uiso 0.900(5) 1 calc PR A 1 H61B H 0.3430 0.5220 -0.2514 0.099 Uiso 0.900(5) 1 calc PR A 1 H61C H 0.2556 0.5246 -0.2397 0.099 Uiso 0.900(5) 1 calc PR A 1 C62 C 0.2065(2) 0.44969(19) -0.3233(3) 0.0634(15) Uani 0.900(5) 1 d PDU A 1 H62A H 0.1992 0.4696 -0.3664 0.095 Uiso 0.900(5) 1 calc PR A 1 H62B H 0.1688 0.4589 -0.2917 0.095 Uiso 0.900(5) 1 calc PR A 1 H62C H 0.2010 0.4147 -0.3355 0.095 Uiso 0.900(5) 1 calc PR A 1 C60X C 0.3497(17) 0.4874(15) -0.310(2) 0.076(12) Uani 0.100(5) 1 d PDU A 2 H60D H 0.3943 0.4661 -0.3072 0.114 Uiso 0.100(5) 1 calc PR A 2 H60E H 0.3598 0.5160 -0.2791 0.114 Uiso 0.100(5) 1 calc PR A 2 H60F H 0.3378 0.4986 -0.3586 0.114 Uiso 0.100(5) 1 calc PR A 2 C61X C 0.2107(16) 0.4863(14) -0.287(2) 0.068(11) Uani 0.100(5) 1 d PDU A 2 H61D H 0.1738 0.4654 -0.2669 0.103 Uiso 0.100(5) 1 calc PR A 2 H61E H 0.1920 0.4946 -0.3361 0.103 Uiso 0.100(5) 1 calc PR A 2 H61F H 0.2185 0.5166 -0.2598 0.103 Uiso 0.100(5) 1 calc PR A 2 C62X C 0.2742(18) 0.4158(10) -0.3409(15) 0.045(8) Uani 0.100(5) 1 d PDU A 2 H62D H 0.2313 0.3954 -0.3307 0.068 Uiso 0.100(5) 1 calc PR A 2 H62E H 0.3199 0.3955 -0.3372 0.068 Uiso 0.100(5) 1 calc PR A 2 H62F H 0.2652 0.4292 -0.3886 0.068 Uiso 0.100(5) 1 calc PR A 2 C63 C 0.20382(17) 0.34849(11) -0.09932(17) 0.0306(7) Uani 1 1 d . . . H63 H 0.1549 0.3525 -0.1230 0.037 Uiso 1 1 calc R . . N3 N 0.20983(13) 0.31870(9) -0.04546(14) 0.0281(6) Uani 1 1 d . . . C64 C 0.14091(16) 0.30048(12) -0.02423(16) 0.0313(7) Uani 1 1 d . . . C65 C 0.07776(17) 0.33067(13) -0.02794(19) 0.0413(9) Uani 1 1 d . . . H65 H 0.0826 0.3647 -0.0384 0.050 Uiso 1 1 calc R . . C66 C 0.00771(18) 0.31181(15) -0.0166(2) 0.0497(10) Uani 1 1 d . . . H66 H -0.0351 0.3328 -0.0203 0.060 Uiso 1 1 calc R . . C67 C 0.00042(19) 0.26286(14) -0.0002(2) 0.0476(10) Uani 1 1 d . . . H67 H -0.0478 0.2494 0.0051 0.057 Uiso 1 1 calc R . . C68 C 0.06290(18) 0.23353(13) 0.00869(18) 0.0412(9) Uani 1 1 d . . . H68 H 0.0575 0.2000 0.0219 0.049 Uiso 1 1 calc R . . C69 C 0.13454(16) 0.25149(11) -0.00125(17) 0.0303(7) Uani 1 1 d . . . C70 C 0.20006(18) 0.21885(11) 0.01421(16) 0.0311(7) Uani 1 1 d . . . O8 O 0.26628(11) 0.23454(7) 0.01740(11) 0.0303(5) Uani 1 1 d . . . O9 O 0.18583(12) 0.17366(7) 0.02698(12) 0.0398(6) Uani 1 1 d . . . O10 O 0.32623(11) 0.26593(7) -0.09097(11) 0.0305(5) Uani 1 1 d . . . C71 C 0.36306(17) 0.22603(11) -0.10413(18) 0.0313(7) Uani 1 1 d . . . C72 C 0.34831(18) 0.20087(12) -0.16926(19) 0.0383(8) Uani 1 1 d . . . C73 C 0.38977(19) 0.15960(13) -0.1798(2) 0.0466(10) Uani 1 1 d . . . H73 H 0.3788 0.1425 -0.2231 0.056 Uiso 1 1 calc R . . C74 C 0.44749(19) 0.14044(12) -0.1317(2) 0.0437(9) Uani 1 1 d . . . C75 C 0.46260(18) 0.16532(12) -0.0700(2) 0.0400(9) Uani 1 1 d . . . H75 H 0.5019 0.1540 -0.0367 0.048 Uiso 1 1 calc R . . C76 C 0.42103(17) 0.20791(11) -0.05418(18) 0.0322(7) Uani 1 1 d . . . C77 C 0.28813(19) 0.21991(14) -0.22582(19) 0.0472(9) Uani 1 1 d . . . C78 C 0.2835(2) 0.18848(17) -0.2931(2) 0.0706(13) Uani 1 1 d . . . H78A H 0.3324 0.1886 -0.3122 0.106 Uiso 1 1 calc R . . H78B H 0.2452 0.2022 -0.3280 0.106 Uiso 1 1 calc R . . H78C H 0.2699 0.1546 -0.2819 0.106 Uiso 1 1 calc R . . C79 C 0.21076(19) 0.21754(15) -0.1967(2) 0.0561(11) Uani 1 1 d . . . H79A H 0.2019 0.1840 -0.1803 0.084 Uiso 1 1 calc R . . H79B H 0.1714 0.2264 -0.2340 0.084 Uiso 1 1 calc R . . H79C H 0.2098 0.2407 -0.1574 0.084 Uiso 1 1 calc R . . C80 C 0.3059(2) 0.27257(14) -0.2471(2) 0.0546(10) Uani 1 1 d . . . H80A H 0.3067 0.2942 -0.2059 0.082 Uiso 1 1 calc R . . H80B H 0.2672 0.2840 -0.2835 0.082 Uiso 1 1 calc R . . H80C H 0.3551 0.2733 -0.2656 0.082 Uiso 1 1 calc R . . C81 C 0.4902(2) 0.09417(13) -0.1520(2) 0.0564(11) Uani 1 1 d . . . C82 C 0.5519(2) 0.08025(15) -0.0946(3) 0.0754(14) Uani 1 1 d . . . H82A H 0.5861 0.1083 -0.0852 0.113 Uiso 1 1 calc R . . H82B H 0.5801 0.0520 -0.1102 0.113 Uiso 1 1 calc R . . H82C H 0.5293 0.0716 -0.0515 0.113 Uiso 1 1 calc R . . C83 C 0.5259(2) 0.10410(15) -0.2207(3) 0.0705(13) Uani 1 1 d . . . H83A H 0.5587 0.1330 -0.2146 0.106 Uiso 1 1 calc R . . H83B H 0.4861 0.1102 -0.2589 0.106 Uiso 1 1 calc R . . H83C H 0.5555 0.0754 -0.2324 0.106 Uiso 1 1 calc R . . C84 C 0.4352(2) 0.05077(14) -0.1617(3) 0.0840(17) Uani 1 1 d . . . H84A H 0.4617 0.0216 -0.1767 0.126 Uiso 1 1 calc R . . H84B H 0.3941 0.0591 -0.1976 0.126 Uiso 1 1 calc R . . H84C H 0.4146 0.0438 -0.1170 0.126 Uiso 1 1 calc R . . C85 C 0.44555(17) 0.23407(11) 0.00794(18) 0.0321(7) Uani 1 1 d . . . H85 H 0.4895 0.2220 0.0346 0.039 Uiso 1 1 calc R . . N4 N 0.41423(13) 0.27298(9) 0.03251(13) 0.0267(6) Uani 1 1 d . . . C86 C 0.45803(17) 0.30161(11) 0.08464(17) 0.0319(7) Uani 1 1 d . . . C87 C 0.53639(17) 0.30266(12) 0.08596(19) 0.0379(8) Uani 1 1 d . . . H87 H 0.5605 0.2830 0.0536 0.045 Uiso 1 1 calc R . . C88 C 0.57917(19) 0.33203(14) 0.1340(2) 0.0472(10) Uani 1 1 d . . . H88 H 0.6324 0.3319 0.1348 0.057 Uiso 1 1 calc R . . C89 C 0.5453(2) 0.36139(14) 0.1803(2) 0.0485(10) Uani 1 1 d . . . H89 H 0.5749 0.3814 0.2132 0.058 Uiso 1 1 calc R . . C90 C 0.46869(19) 0.36147(12) 0.17863(18) 0.0396(8) Uani 1 1 d . . . H90 H 0.4453 0.3820 0.2104 0.047 Uiso 1 1 calc R . . C91 C 0.42385(17) 0.33193(11) 0.13119(17) 0.0300(7) Uani 1 1 d . . . C92 C 0.34167(18) 0.33532(11) 0.13222(18) 0.0308(7) Uani 1 1 d . . . O11 O 0.29656(11) 0.31665(7) 0.08431(11) 0.0292(5) Uani 1 1 d . . . O12 O 0.31861(12) 0.35894(8) 0.18294(12) 0.0382(5) Uani 1 1 d . . . N5 N 0.5335(6) 0.5108(6) -0.2662(7) 0.366(9) Uani 1 1 d DU . . C93 C 0.5943(5) 0.5073(3) -0.2417(4) 0.157(3) Uani 1 1 d DU . . C94 C 0.6758(4) 0.4962(3) -0.2122(5) 0.175(4) Uani 1 1 d DU . . H94A H 0.7105 0.5145 -0.2392 0.262 Uiso 1 1 calc R . . H94B H 0.6855 0.4607 -0.2161 0.262 Uiso 1 1 calc R . . H94C H 0.6834 0.5061 -0.1627 0.262 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 0.0215(5) 0.0235(4) 0.0267(5) 0.0007(4) 0.0028(4) 0.0010(4) O1 0.0261(11) 0.0217(10) 0.0319(13) 0.0032(9) 0.0061(9) 0.0015(8) C1 0.0288(17) 0.0204(14) 0.0290(18) -0.0026(13) -0.0007(13) -0.0006(12) C2 0.0307(17) 0.0269(16) 0.0334(19) -0.0002(14) 0.0018(14) -0.0005(13) C3 0.0346(19) 0.0304(17) 0.040(2) 0.0077(15) 0.0015(15) 0.0053(14) C4 0.0384(19) 0.0304(17) 0.0307(19) 0.0067(15) 0.0045(15) -0.0017(14) C5 0.0288(17) 0.0307(17) 0.038(2) 0.0030(15) 0.0089(14) -0.0013(14) C6 0.0264(17) 0.0247(15) 0.0335(19) 0.0018(14) 0.0027(14) -0.0007(13) C7 0.0312(18) 0.0322(17) 0.044(2) 0.0039(16) 0.0021(15) 0.0084(14) C8 0.054(3) 0.065(3) 0.094(4) 0.035(3) 0.029(2) 0.031(2) C9 0.051(2) 0.052(2) 0.067(3) -0.022(2) 0.009(2) 0.0079(19) C10 0.0286(19) 0.055(2) 0.061(3) 0.003(2) 0.0038(17) 0.0017(17) C11 0.045(2) 0.045(2) 0.036(2) 0.0118(17) 0.0070(16) 0.0076(17) C12 0.130(4) 0.045(2) 0.060(3) 0.023(2) 0.033(3) 0.006(3) C13 0.065(3) 0.123(4) 0.051(3) 0.043(3) 0.022(2) 0.022(3) C14 0.083(3) 0.070(3) 0.041(3) 0.001(2) -0.002(2) 0.008(2) C15 0.0229(16) 0.0271(16) 0.0359(19) 0.0002(14) 0.0053(14) -0.0021(13) N1 0.0231(13) 0.0246(13) 0.0297(15) 0.0006(11) 0.0029(11) 0.0025(10) C16 0.0202(16) 0.0360(17) 0.0277(18) 0.0002(14) 0.0027(13) 0.0024(13) C17 0.0281(18) 0.0427(19) 0.038(2) 0.0045(16) 0.0016(15) -0.0061(15) C18 0.0276(19) 0.064(2) 0.043(2) 0.0078(19) -0.0043(16) -0.0097(17) C19 0.0244(19) 0.074(3) 0.045(2) 0.013(2) -0.0053(16) 0.0026(18) C20 0.0280(19) 0.052(2) 0.044(2) 0.0059(18) 0.0000(16) 0.0065(16) C21 0.0233(16) 0.0362(17) 0.0274(18) 0.0031(14) 0.0020(13) 0.0059(13) C22 0.0276(17) 0.0324(17) 0.0272(18) 0.0004(14) 0.0035(13) 0.0048(14) O2 0.0267(12) 0.0265(11) 0.0298(13) 0.0015(9) 0.0009(9) 0.0028(9) O3 0.0335(13) 0.0308(12) 0.0540(16) 0.0108(11) 0.0053(11) 0.0095(10) O4 0.0291(11) 0.0234(10) 0.0267(12) -0.0009(9) 0.0032(9) 0.0005(9) C23 0.0314(17) 0.0235(15) 0.0265(17) 0.0028(13) -0.0040(13) 0.0055(13) C24 0.0344(18) 0.0345(17) 0.0285(18) -0.0028(15) -0.0005(14) 0.0085(15) C25 0.044(2) 0.0335(18) 0.030(2) -0.0089(15) -0.0037(15) 0.0110(16) C26 0.049(2) 0.0299(17) 0.039(2) -0.0057(16) -0.0048(17) 0.0011(16) C27 0.040(2) 0.0309(17) 0.036(2) 0.0018(15) -0.0016(15) -0.0026(15) C28 0.0318(17) 0.0284(16) 0.0256(17) -0.0020(14) -0.0032(13) 0.0003(13) C29 0.047(2) 0.045(2) 0.035(2) -0.0121(17) 0.0130(17) 0.0014(17) C30 0.069(3) 0.072(3) 0.060(3) -0.022(2) 0.030(2) 0.002(2) C31 0.063(3) 0.052(2) 0.036(2) 0.0027(18) 0.0151(19) -0.0061(19) C32 0.038(2) 0.061(2) 0.060(3) -0.010(2) 0.0120(19) 0.0045(18) C33 0.069(3) 0.0319(19) 0.045(2) -0.0102(17) -0.007(2) -0.0088(18) C34 0.106(4) 0.059(3) 0.092(4) -0.035(3) 0.024(3) -0.048(3) C35 0.102(4) 0.033(2) 0.074(3) -0.008(2) -0.034(3) 0.005(2) C36 0.068(3) 0.051(2) 0.054(3) -0.022(2) -0.019(2) 0.006(2) C37 0.0254(16) 0.0265(16) 0.0291(18) 0.0065(14) 0.0004(13) -0.0040(13) N2 0.0251(13) 0.0270(13) 0.0230(14) 0.0016(11) 0.0001(11) 0.0008(11) C38 0.0243(16) 0.0256(15) 0.0342(19) 0.0057(14) 0.0073(13) 0.0006(13) C39 0.0251(17) 0.0346(17) 0.044(2) 0.0018(16) 0.0040(14) -0.0001(14) C40 0.0240(18) 0.046(2) 0.056(3) 0.0118(19) 0.0081(16) 0.0028(15) C41 0.033(2) 0.053(2) 0.048(2) 0.0006(19) 0.0139(17) 0.0105(17) C42 0.0365(19) 0.0377(18) 0.034(2) 0.0029(16) 0.0084(15) 0.0083(15) C43 0.0268(17) 0.0329(17) 0.0272(18) 0.0035(14) 0.0056(13) 0.0004(13) C44 0.0319(18) 0.0262(16) 0.0292(18) 0.0022(14) 0.0030(14) 0.0029(13) O5 0.0264(11) 0.0311(11) 0.0253(12) -0.0024(9) 0.0027(9) 0.0007(9) O6 0.0361(13) 0.0383(12) 0.0342(14) -0.0112(11) 0.0037(10) 0.0017(10) Al3 0.0401(6) 0.0327(5) 0.0416(7) -0.0101(5) 0.0009(5) -0.0041(5) C45 0.062(3) 0.036(2) 0.071(3) 0.001(2) 0.003(2) -0.0107(18) C46 0.071(3) 0.083(3) 0.069(3) -0.041(3) -0.004(2) -0.006(3) Al4 0.0413(6) 0.0327(5) 0.0363(6) 0.0004(5) -0.0001(5) 0.0053(5) C47 0.055(3) 0.068(3) 0.048(3) -0.011(2) 0.005(2) 0.009(2) C48 0.080(3) 0.042(2) 0.055(3) 0.007(2) -0.013(2) 0.009(2) Al2 0.0223(5) 0.0280(5) 0.0280(5) 0.0003(4) 0.0007(4) -0.0011(4) O7 0.0236(11) 0.0272(11) 0.0291(12) 0.0043(9) 0.0005(9) -0.0007(9) C49 0.0275(17) 0.0233(15) 0.0282(18) -0.0018(13) 0.0034(13) 0.0009(13) C50 0.0302(17) 0.0253(15) 0.0289(18) -0.0016(14) 0.0013(13) -0.0015(13) C51 0.0311(18) 0.0300(16) 0.034(2) 0.0012(15) 0.0057(14) -0.0024(14) C52 0.0346(18) 0.0296(16) 0.0288(18) 0.0007(14) 0.0032(14) 0.0050(14) C53 0.0278(17) 0.0345(17) 0.0305(19) -0.0054(15) -0.0042(14) 0.0041(14) C54 0.0264(16) 0.0268(15) 0.0284(18) -0.0004(14) 0.0001(13) 0.0031(13) C55 0.0255(17) 0.0388(18) 0.041(2) 0.0072(16) -0.0005(14) -0.0074(14) C56 0.0256(18) 0.052(2) 0.045(2) 0.0087(18) 0.0040(15) 0.0023(16) C57 0.039(2) 0.051(2) 0.043(2) 0.0084(18) 0.0022(16) -0.0140(17) C58 0.045(2) 0.047(2) 0.035(2) -0.0050(17) -0.0032(16) -0.0182(17) C59 0.039(2) 0.046(2) 0.032(2) 0.0086(16) 0.0007(15) 0.0033(16) C60 0.068(3) 0.092(4) 0.035(3) 0.009(3) 0.017(2) 0.022(3) C61 0.107(4) 0.044(2) 0.045(3) 0.016(2) -0.003(3) 0.000(3) C62 0.057(3) 0.082(4) 0.047(3) 0.029(3) -0.013(2) 0.000(3) C60X 0.082(19) 0.10(3) 0.04(2) 0.03(2) 0.00(2) -0.033(18) C61X 0.082(18) 0.07(2) 0.05(2) 0.028(18) -0.004(19) 0.050(18) C62X 0.036(19) 0.089(19) 0.014(15) -0.002(12) 0.014(13) 0.002(14) C63 0.0231(17) 0.0345(17) 0.0332(19) -0.0023(15) -0.0016(14) 0.0039(13) N3 0.0241(14) 0.0301(13) 0.0303(15) 0.0003(12) 0.0033(11) -0.0009(11) C64 0.0215(16) 0.0437(19) 0.0284(18) -0.0013(15) 0.0003(13) -0.0042(14) C65 0.0277(19) 0.048(2) 0.048(2) 0.0103(18) 0.0037(16) 0.0034(16) C66 0.0214(18) 0.074(3) 0.054(3) 0.013(2) 0.0029(16) 0.0046(18) C67 0.0250(19) 0.070(3) 0.048(2) 0.012(2) 0.0018(16) -0.0092(18) C68 0.035(2) 0.048(2) 0.041(2) 0.0043(17) 0.0013(16) -0.0119(17) C69 0.0241(17) 0.0370(17) 0.0292(19) -0.0001(14) -0.0002(13) -0.0053(13) C70 0.0320(18) 0.0338(17) 0.0270(18) -0.0039(14) 0.0005(14) -0.0079(14) O8 0.0224(11) 0.0306(11) 0.0373(14) 0.0013(10) 0.0007(9) -0.0045(9) O9 0.0360(13) 0.0324(12) 0.0497(16) 0.0022(11) -0.0021(11) -0.0097(10) O10 0.0258(11) 0.0328(11) 0.0328(13) -0.0054(10) 0.0024(9) 0.0011(9) C71 0.0247(17) 0.0318(17) 0.038(2) -0.0039(15) 0.0074(14) -0.0044(14) C72 0.0309(18) 0.0424(19) 0.042(2) -0.0095(17) 0.0054(15) -0.0016(16) C73 0.033(2) 0.051(2) 0.056(3) -0.0214(19) 0.0084(18) -0.0087(17) C74 0.0329(19) 0.0337(18) 0.065(3) -0.0105(19) 0.0103(18) -0.0001(15) C75 0.0297(19) 0.0352(18) 0.056(3) -0.0006(18) 0.0091(16) 0.0020(15) C76 0.0299(17) 0.0287(16) 0.039(2) -0.0001(15) 0.0072(15) 0.0005(14) C77 0.036(2) 0.065(2) 0.040(2) -0.0196(19) -0.0018(16) 0.0009(18) C78 0.055(3) 0.098(3) 0.057(3) -0.034(3) -0.005(2) 0.008(2) C79 0.031(2) 0.077(3) 0.059(3) -0.016(2) -0.0008(18) 0.0020(19) C80 0.046(2) 0.080(3) 0.036(2) -0.001(2) -0.0007(18) 0.007(2) C81 0.042(2) 0.039(2) 0.089(3) -0.014(2) 0.015(2) 0.0034(18) C82 0.070(3) 0.051(3) 0.108(4) -0.004(3) 0.020(3) 0.026(2) C83 0.059(3) 0.066(3) 0.091(4) -0.019(3) 0.032(3) 0.012(2) C84 0.064(3) 0.041(2) 0.151(5) -0.030(3) 0.031(3) -0.002(2) C85 0.0234(17) 0.0349(17) 0.038(2) 0.0078(16) 0.0036(14) 0.0013(14) N4 0.0245(13) 0.0276(13) 0.0278(15) 0.0024(11) 0.0016(11) -0.0012(11) C86 0.0279(17) 0.0323(17) 0.0341(19) 0.0105(15) -0.0044(14) -0.0066(14) C87 0.0288(18) 0.0426(19) 0.041(2) 0.0076(17) -0.0043(15) -0.0010(15) C88 0.0289(19) 0.060(2) 0.051(3) 0.010(2) -0.0085(17) -0.0069(18) C89 0.041(2) 0.056(2) 0.045(2) 0.004(2) -0.0142(18) -0.0161(18) C90 0.045(2) 0.0398(19) 0.033(2) 0.0019(16) -0.0025(16) -0.0090(16) C91 0.0292(17) 0.0305(16) 0.0293(18) 0.0050(14) -0.0016(13) -0.0076(14) C92 0.0378(19) 0.0255(16) 0.0294(19) 0.0075(14) 0.0051(15) -0.0023(14) O11 0.0274(12) 0.0324(11) 0.0278(12) -0.0008(10) 0.0025(9) -0.0020(9) O12 0.0420(14) 0.0389(13) 0.0340(14) -0.0053(11) 0.0057(11) -0.0049(11) N5 0.196(9) 0.61(2) 0.280(14) 0.210(14) -0.048(9) -0.053(13) C93 0.190(8) 0.185(7) 0.098(6) 0.048(5) 0.028(6) -0.062(8) C94 0.167(7) 0.162(7) 0.193(9) 0.026(6) 0.003(7) -0.051(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Al1 O1 1.833(2) . ? Al1 O4 1.835(2) . ? Al1 O5 1.885(2) . ? Al1 O2 1.904(2) . ? Al1 N1 1.986(2) . ? Al1 N2 1.999(2) . ? O1 C1 1.301(3) . ? C1 C6 1.417(4) . ? C1 C2 1.430(4) . ? C2 C3 1.381(4) . ? C2 C7 1.537(4) . ? C3 C4 1.410(4) . ? C4 C5 1.365(4) . ? C4 C11 1.521(5) . ? C5 C6 1.408(4) . ? C6 C15 1.430(4) . ? C7 C8 1.520(5) . ? C7 C10 1.524(4) . ? C7 C9 1.541(5) . ? C11 C12 1.516(5) . ? C11 C13 1.517(5) . ? C11 C14 1.545(5) . ? C15 N1 1.308(4) . ? N1 C16 1.423(4) . ? C16 C17 1.389(4) . ? C16 C21 1.400(4) . ? C17 C18 1.387(4) . ? C18 C19 1.371(5) . ? C19 C20 1.379(5) . ? C20 C21 1.400(4) . ? C21 C22 1.479(4) . ? C22 O2 1.254(3) . ? C22 O3 1.269(3) . ? O3 Al4 1.811(2) . ? O4 C23 1.314(3) . ? C23 C28 1.416(4) . ? C23 C24 1.420(4) . ? C24 C25 1.381(4) . ? C24 C29 1.535(5) . ? C25 C26 1.414(5) . ? C26 C27 1.356(5) . ? C26 C33 1.543(4) . ? C27 C28 1.422(4) . ? C28 C37 1.414(4) . ? C29 C31 1.531(5) . ? C29 C30 1.534(5) . ? C29 C32 1.545(5) . ? C33 C35 1.523(5) . ? C33 C34 1.523(6) . ? C33 C36 1.528(5) . ? C37 N2 1.310(3) . ? N2 C38 1.426(4) . ? C38 C39 1.392(4) . ? C38 C43 1.403(4) . ? C39 C40 1.388(4) . ? C40 C41 1.369(5) . ? C41 C42 1.372(4) . ? C42 C43 1.388(4) . ? C43 C44 1.483(4) . ? C44 O5 1.251(3) . ? C44 O6 1.276(4) . ? O6 Al3 1.826(2) . ? Al3 O9 1.812(2) . ? Al3 C46 1.943(4) . ? Al3 C45 1.949(4) . ? Al4 O12 1.825(2) . ? Al4 C47 1.940(4) . ? Al4 C48 1.948(4) . ? Al2 O7 1.819(2) . ? Al2 O10 1.823(2) . ? Al2 O11 1.886(2) . ? Al2 O8 1.898(2) . ? Al2 N4 2.000(2) . ? Al2 N3 2.001(3) . ? O7 C49 1.313(3) . ? C49 C54 1.417(4) . ? C49 C50 1.424(4) . ? C50 C51 1.377(4) . ? C50 C55 1.535(4) . ? C51 C52 1.415(4) . ? C52 C53 1.368(4) . ? C52 C59 1.532(4) . ? C53 C54 1.411(4) . ? C54 C63 1.420(4) . ? C55 C58 1.532(5) . ? C55 C57 1.536(4) . ? C55 C56 1.538(4) . ? C59 C60X 1.503(17) . ? C59 C62 1.509(5) . ? C59 C61X 1.509(17) . ? C59 C60 1.517(5) . ? C59 C61 1.545(5) . ? C59 C62X 1.553(17) . ? C63 N3 1.303(4) . ? N3 C64 1.422(4) . ? C64 C65 1.390(4) . ? C64 C69 1.407(4) . ? C65 C66 1.388(4) . ? C66 C67 1.373(5) . ? C67 C68 1.367(5) . ? C68 C69 1.400(4) . ? C69 C70 1.474(4) . ? C70 O8 1.253(3) . ? C70 O9 1.280(3) . ? O10 C71 1.303(3) . ? C71 C72 1.419(4) . ? C71 C76 1.423(4) . ? C72 C73 1.368(4) . ? C72 C77 1.535(5) . ? C73 C74 1.410(5) . ? C74 C75 1.360(5) . ? C74 C81 1.537(5) . ? C75 C76 1.422(4) . ? C76 C85 1.413(4) . ? C77 C80 1.527(5) . ? C77 C78 1.536(5) . ? C77 C79 1.541(5) . ? C81 C82 1.523(6) . ? C81 C84 1.532(5) . ? C81 C83 1.538(6) . ? C85 N4 1.303(4) . ? N4 C86 1.432(4) . ? C86 C91 1.395(4) . ? C86 C87 1.398(4) . ? C87 C88 1.385(5) . ? C88 C89 1.374(5) . ? C89 C90 1.366(5) . ? C90 C91 1.399(4) . ? C91 C92 1.473(4) . ? C92 O11 1.263(4) . ? C92 O12 1.263(4) . ? N5 C93 1.141(7) . ? C93 C94 1.538(7) . ? 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 O4 97.67(10) . . ? O1 Al1 O5 89.18(9) . . ? O4 Al1 O5 172.41(10) . . ? O1 Al1 O2 173.11(10) . . ? O4 Al1 O2 87.72(9) . . ? O5 Al1 O2 85.70(9) . . ? O1 Al1 N1 87.87(9) . . ? O4 Al1 N1 90.50(10) . . ? O5 Al1 N1 93.03(10) . . ? O2 Al1 N1 87.79(9) . . ? O1 Al1 N2 91.66(9) . . ? O4 Al1 N2 88.95(10) . . ? O5 Al1 N2 87.59(10) . . ? O2 Al1 N2 92.73(9) . . ? N1 Al1 N2 179.22(11) . . ? C1 O1 Al1 126.20(18) . . ? O1 C1 C6 120.6(3) . . ? O1 C1 C2 122.1(3) . . ? C6 C1 C2 117.2(3) . . ? C3 C2 C1 117.6(3) . . ? C3 C2 C7 122.3(3) . . ? C1 C2 C7 119.9(3) . . ? C2 C3 C4 125.1(3) . . ? C5 C4 C3 116.0(3) . . ? C5 C4 C11 123.2(3) . . ? C3 C4 C11 120.8(3) . . ? C4 C5 C6 121.8(3) . . ? C5 C6 C1 121.0(3) . . ? C5 C6 C15 118.6(3) . . ? C1 C6 C15 120.0(3) . . ? C8 C7 C10 107.6(3) . . ? C8 C7 C2 111.9(3) . . ? C10 C7 C2 112.0(3) . . ? C8 C7 C9 109.0(3) . . ? C10 C7 C9 108.3(3) . . ? C2 C7 C9 108.0(3) . . ? C12 C11 C13 108.3(3) . . ? C12 C11 C4 111.0(3) . . ? C13 C11 C4 111.9(3) . . ? C12 C11 C14 109.1(3) . . ? C13 C11 C14 108.7(3) . . ? C4 C11 C14 107.8(3) . . ? N1 C15 C6 125.8(3) . . ? C15 N1 C16 115.7(2) . . ? C15 N1 Al1 117.6(2) . . ? C16 N1 Al1 125.85(19) . . ? C17 C16 C21 119.3(3) . . ? C17 C16 N1 120.4(3) . . ? C21 C16 N1 120.3(3) . . ? C18 C17 C16 120.8(3) . . ? C19 C18 C17 120.1(3) . . ? C18 C19 C20 119.9(3) . . ? C19 C20 C21 121.1(3) . . ? C16 C21 C20 118.7(3) . . ? C16 C21 C22 123.2(3) . . ? C20 C21 C22 118.1(3) . . ? O2 C22 O3 121.8(3) . . ? O2 C22 C21 122.0(3) . . ? O3 C22 C21 116.2(3) . . ? C22 O2 Al1 134.7(2) . . ? C22 O3 Al4 135.5(2) . . ? C23 O4 Al1 128.91(19) . . ? O4 C23 C28 119.8(3) . . ? O4 C23 C24 121.7(3) . . ? C28 C23 C24 118.5(3) . . ? C25 C24 C23 117.9(3) . . ? C25 C24 C29 121.6(3) . . ? C23 C24 C29 120.5(3) . . ? C24 C25 C26 124.9(3) . . ? C27 C26 C25 116.3(3) . . ? C27 C26 C33 124.3(3) . . ? C25 C26 C33 119.4(3) . . ? C26 C27 C28 122.2(3) . . ? C37 C28 C23 122.4(3) . . ? C37 C28 C27 117.2(3) . . ? C23 C28 C27 120.1(3) . . ? C31 C29 C24 110.2(3) . . ? C31 C29 C30 107.0(3) . . ? C24 C29 C30 112.4(3) . . ? C31 C29 C32 110.3(3) . . ? C24 C29 C32 109.6(3) . . ? C30 C29 C32 107.2(3) . . ? C35 C33 C34 110.4(4) . . ? C35 C33 C36 108.9(3) . . ? C34 C33 C36 107.7(4) . . ? C35 C33 C26 108.8(3) . . ? C34 C33 C26 110.7(3) . . ? C36 C33 C26 110.4(3) . . ? N2 C37 C28 126.6(3) . . ? C37 N2 C38 117.5(2) . . ? C37 N2 Al1 120.8(2) . . ? C38 N2 Al1 121.74(18) . . ? C39 C38 C43 119.0(3) . . ? C39 C38 N2 120.0(3) . . ? C43 C38 N2 120.8(3) . . ? C40 C39 C38 120.0(3) . . ? C41 C40 C39 121.0(3) . . ? C40 C41 C42 119.1(3) . . ? C41 C42 C43 121.7(3) . . ? C42 C43 C38 119.1(3) . . ? C42 C43 C44 117.9(3) . . ? C38 C43 C44 123.1(3) . . ? O5 C44 O6 122.1(3) . . ? O5 C44 C43 122.3(3) . . ? O6 C44 C43 115.6(3) . . ? C44 O5 Al1 129.6(2) . . ? C44 O6 Al3 128.2(2) . . ? O9 Al3 O6 105.23(10) . . ? O9 Al3 C46 107.63(17) . . ? O6 Al3 C46 105.79(15) . . ? O9 Al3 C45 108.15(15) . . ? O6 Al3 C45 108.06(15) . . ? C46 Al3 C45 120.93(19) . . ? O3 Al4 O12 105.42(10) . . ? O3 Al4 C47 109.30(16) . . ? O12 Al4 C47 103.65(14) . . ? O3 Al4 C48 104.69(15) . . ? O12 Al4 C48 109.20(16) . . ? C47 Al4 C48 123.40(18) . . ? O7 Al2 O10 94.65(10) . . ? O7 Al2 O11 91.67(10) . . ? O10 Al2 O11 173.14(10) . . ? O7 Al2 O8 176.55(10) . . ? O10 Al2 O8 87.18(10) . . ? O11 Al2 O8 86.64(10) . . ? O7 Al2 N4 89.92(9) . . ? O10 Al2 N4 89.98(10) . . ? O11 Al2 N4 87.36(10) . . ? O8 Al2 N4 93.00(10) . . ? O7 Al2 N3 88.42(10) . . ? O10 Al2 N3 91.23(10) . . ? O11 Al2 N3 91.61(10) . . ? O8 Al2 N3 88.61(10) . . ? N4 Al2 N3 178.03(11) . . ? C49 O7 Al2 127.18(18) . . ? O7 C49 C54 120.2(3) . . ? O7 C49 C50 121.2(3) . . ? C54 C49 C50 118.6(3) . . ? C51 C50 C49 117.4(3) . . ? C51 C50 C55 122.7(3) . . ? C49 C50 C55 119.8(3) . . ? C50 C51 C52 125.3(3) . . ? C53 C52 C51 116.4(3) . . ? C53 C52 C59 123.9(3) . . ? C51 C52 C59 119.8(3) . . ? C52 C53 C54 121.6(3) . . ? C53 C54 C49 120.8(3) . . ? C53 C54 C63 118.2(3) . . ? C49 C54 C63 121.0(3) . . ? C58 C55 C50 110.8(3) . . ? C58 C55 C57 108.0(3) . . ? C50 C55 C57 111.1(3) . . ? C58 C55 C56 111.0(3) . . ? C50 C55 C56 108.3(3) . . ? C57 C55 C56 107.6(3) . . ? C60X C59 C62 131.2(16) . . ? C60X C59 C61X 117(2) . . ? C62 C59 C61X 47.0(17) . . ? C60X C59 C60 50.0(17) . . ? C62 C59 C60 108.8(4) . . ? C61X C59 C60 140.4(15) . . ? C60X C59 C52 116.2(16) . . ? C62 C59 C52 112.4(3) . . ? C61X C59 C52 109.0(15) . . ? C60 C59 C52 109.8(3) . . ? C60X C59 C61 59.4(18) . . ? C62 C59 C61 107.8(3) . . ? C61X C59 C61 65.0(17) . . ? C60 C59 C61 108.4(4) . . ? C52 C59 C61 109.4(3) . . ? C60X C59 C62X 103.7(18) . . ? C62 C59 C62X 62.2(12) . . ? C61X C59 C62X 109.0(18) . . ? C60 C59 C62X 55.5(11) . . ? C52 C59 C62X 100.9(13) . . ? C61 C59 C62X 149.4(13) . . ? N3 C63 C54 127.0(3) . . ? C63 N3 C64 115.7(3) . . ? C63 N3 Al2 119.5(2) . . ? C64 N3 Al2 124.3(2) . . ? C65 C64 C69 118.8(3) . . ? C65 C64 N3 120.1(3) . . ? C69 C64 N3 121.0(3) . . ? C66 C65 C64 121.0(3) . . ? C67 C66 C65 119.9(3) . . ? C68 C67 C66 119.7(3) . . ? C67 C68 C69 121.8(3) . . ? C68 C69 C64 118.3(3) . . ? C68 C69 C70 118.8(3) . . ? C64 C69 C70 122.8(3) . . ? O8 C70 O9 121.4(3) . . ? O8 C70 C69 122.2(3) . . ? O9 C70 C69 116.4(3) . . ? C70 O8 Al2 134.7(2) . . ? C70 O9 Al3 136.6(2) . . ? C71 O10 Al2 130.0(2) . . ? O10 C71 C72 121.0(3) . . ? O10 C71 C76 120.3(3) . . ? C72 C71 C76 118.7(3) . . ? C73 C72 C71 117.8(3) . . ? C73 C72 C77 121.5(3) . . ? C71 C72 C77 120.7(3) . . ? C72 C73 C74 125.2(3) . . ? C75 C74 C73 116.8(3) . . ? C75 C74 C81 124.2(3) . . ? C73 C74 C81 119.0(3) . . ? C74 C75 C76 121.6(3) . . ? C85 C76 C75 117.5(3) . . ? C85 C76 C71 122.2(3) . . ? C75 C76 C71 119.9(3) . . ? C80 C77 C72 110.6(3) . . ? C80 C77 C78 107.0(3) . . ? C72 C77 C78 112.1(3) . . ? C80 C77 C79 110.6(3) . . ? C72 C77 C79 108.9(3) . . ? C78 C77 C79 107.6(3) . . ? C82 C81 C84 107.9(4) . . ? C82 C81 C74 111.3(3) . . ? C84 C81 C74 109.2(3) . . ? C82 C81 C83 108.9(3) . . ? C84 C81 C83 110.3(4) . . ? C74 C81 C83 109.3(3) . . ? N4 C85 C76 126.9(3) . . ? C85 N4 C86 117.7(3) . . ? C85 N4 Al2 120.8(2) . . ? C86 N4 Al2 121.32(19) . . ? C91 C86 C87 118.5(3) . . ? C91 C86 N4 121.2(3) . . ? C87 C86 N4 120.0(3) . . ? C88 C87 C86 120.6(3) . . ? C89 C88 C87 120.6(3) . . ? C90 C89 C88 119.3(3) . . ? C89 C90 C91 121.5(3) . . ? C86 C91 C90 119.4(3) . . ? C86 C91 C92 123.0(3) . . ? C90 C91 C92 117.6(3) . . ? O11 C92 O12 121.6(3) . . ? O11 C92 C91 122.0(3) . . ? O12 C92 C91 116.3(3) . . ? C92 O11 Al2 131.0(2) . . ? C92 O12 Al4 130.3(2) . . ? N5 C93 C94 173.0(14) . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.447 _refine_diff_density_min -0.460 _refine_diff_density_rms 0.060 #===END data_2 _database_code_CSD 167945 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C98 H118 Al4 Cl2 N8 O12' _chemical_formula_weight 1778.82 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' '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 20.502(2) _cell_length_b 22.794(3) _cell_length_c 23.785(3) _cell_angle_alpha 90.00 _cell_angle_beta 114.694(2) _cell_angle_gamma 90.00 _cell_volume 10099(2) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 12596 _cell_measurement_theta_min 2.18 _cell_measurement_theta_max 24.72 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.170 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3776 _exptl_absorpt_coefficient_mu 0.159 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_correction_T_min 0.965 _exptl_absorpt_correction_T_max 0.976 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART 1000 CCD diffractometer' _diffrn_measurement_method '\w rotation with narrow frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 71603 _diffrn_reflns_av_R_equivalents 0.0742 _diffrn_reflns_av_sigmaI/netI 0.0774 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 1.72 _diffrn_reflns_theta_max 25.00 _reflns_number_total 17785 _reflns_number_gt 10465 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL and local programs' _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^)+(0.0941P)^2^+8.3712P] 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 17785 _refine_ls_number_parameters 1172 _refine_ls_number_restraints 75 _refine_ls_R_factor_all 0.1252 _refine_ls_R_factor_gt 0.0627 _refine_ls_wR_factor_ref 0.1940 _refine_ls_wR_factor_gt 0.1557 _refine_ls_goodness_of_fit_ref 1.020 _refine_ls_restrained_S_all 1.024 _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 0.94988(6) 0.87838(5) 0.23570(5) 0.0234(3) Uani 1 1 d . . . O1 O 1.03363(13) 0.84136(10) 0.24757(11) 0.0268(6) Uani 1 1 d . . . C1 C 1.0894(2) 0.86459(17) 0.24226(17) 0.0290(9) Uani 1 1 d . . . C2 C 1.1337(2) 0.83036(18) 0.22243(19) 0.0363(10) Uani 1 1 d . . . C3 C 1.1945(3) 0.8575(2) 0.2229(2) 0.0482(12) Uani 1 1 d . . . H3 H 1.2251 0.8347 0.2106 0.058 Uiso 1 1 calc R . . C4 C 1.2145(2) 0.9161(2) 0.2400(2) 0.0471(12) Uani 1 1 d . . . C5 C 1.1700(2) 0.94859(19) 0.2562(2) 0.0397(11) Uani 1 1 d . . . H5 H 1.1809 0.9887 0.2668 0.048 Uiso 1 1 calc R . . C6 C 1.1073(2) 0.92398(17) 0.25756(18) 0.0305(9) Uani 1 1 d . . . C7 C 1.1134(2) 0.76659(19) 0.2007(2) 0.0437(11) Uani 1 1 d . . . C8 C 1.1677(3) 0.7378(2) 0.1803(3) 0.0716(17) Uani 1 1 d . . . H8A H 1.2144 0.7348 0.2159 0.107 Uiso 1 1 calc R . . H8B H 1.1726 0.7617 0.1480 0.107 Uiso 1 1 calc R . . H8C H 1.1509 0.6985 0.1640 0.107 Uiso 1 1 calc R . . C9 C 1.1103(2) 0.72891(18) 0.2536(2) 0.0428(11) Uani 1 1 d . . . H9A H 1.0976 0.6885 0.2392 0.064 Uiso 1 1 calc R . . H9B H 1.0740 0.7450 0.2661 0.064 Uiso 1 1 calc R . . H9C H 1.1573 0.7294 0.2890 0.064 Uiso 1 1 calc R . . C10 C 1.0407(3) 0.7663(2) 0.1446(2) 0.0539(13) Uani 1 1 d . . . H10A H 1.0445 0.7880 0.1106 0.081 Uiso 1 1 calc R . . H10B H 1.0047 0.7850 0.1558 0.081 Uiso 1 1 calc R . . H10C H 1.0264 0.7258 0.1317 0.081 Uiso 1 1 calc R . . C11 C 1.2855(3) 0.9409(2) 0.2404(3) 0.0729(18) Uani 1 1 d . . . C12 C 1.3473(3) 0.9026(3) 0.2822(5) 0.154(4) Uani 1 1 d . . . H12A H 1.3446 0.8643 0.2625 0.230 Uiso 1 1 calc R . . H12B H 1.3444 0.8972 0.3219 0.230 Uiso 1 1 calc R . . H12C H 1.3929 0.9216 0.2891 0.230 Uiso 1 1 calc R . . C13 C 1.2989(3) 1.0039(2) 0.2633(3) 0.0780(18) Uani 1 1 d . . . H13A H 1.3433 1.0182 0.2619 0.117 Uiso 1 1 calc R . . H13B H 1.3034 1.0056 0.3059 0.117 Uiso 1 1 calc R . . H13C H 1.2586 1.0285 0.2367 0.117 Uiso 1 1 calc R . . C14 C 1.2792(4) 0.9404(3) 0.1746(4) 0.118(3) Uani 1 1 d . . . H14A H 1.2361 0.9620 0.1478 0.176 Uiso 1 1 calc R . . H14B H 1.2759 0.8998 0.1601 0.176 Uiso 1 1 calc R . . H14C H 1.3217 0.9592 0.1735 0.176 Uiso 1 1 calc R . . C15 C 1.0675(2) 0.95992(17) 0.28052(18) 0.0316(9) Uani 1 1 d . . . H15 H 1.0867 0.9978 0.2947 0.038 Uiso 1 1 calc R . . N1 N 1.00767(16) 0.94700(12) 0.28444(14) 0.0258(7) Uani 1 1 d . . . C16 C 0.9855(2) 0.98494(15) 0.32061(17) 0.0259(9) Uani 1 1 d . . . C17 C 1.0374(2) 1.01348(16) 0.37272(18) 0.0332(10) Uani 1 1 d . . . H17 H 1.0869 1.0059 0.3843 0.040 Uiso 1 1 calc R . . C18 C 1.0173(2) 1.05235(17) 0.40724(19) 0.0363(10) Uani 1 1 d . . . H18 H 1.0530 1.0714 0.4420 0.044 Uiso 1 1 calc R . . C19 C 0.9455(2) 1.06352(17) 0.39137(19) 0.0363(10) Uani 1 1 d . . . H19 H 0.9317 1.0909 0.4145 0.044 Uiso 1 1 calc R . . C20 C 0.8943(2) 1.03475(16) 0.34198(18) 0.0302(9) Uani 1 1 d . . . H20 H 0.8449 1.0423 0.3314 0.036 Uiso 1 1 calc R . . C21 C 0.9135(2) 0.99435(15) 0.30682(17) 0.0243(8) Uani 1 1 d . . . C22 C 0.8545(2) 0.96302(15) 0.25626(17) 0.0249(8) Uani 1 1 d . . . O2 O 0.86506(13) 0.92013(10) 0.22865(11) 0.0255(6) Uani 1 1 d . . . O3 O 0.79095(14) 0.98188(11) 0.24322(12) 0.0326(6) Uani 1 1 d . . . O4 O 0.93605(13) 0.90978(11) 0.16127(11) 0.0277(6) Uani 1 1 d . . . C23 C 0.8813(2) 0.90418(16) 0.10714(17) 0.0255(8) Uani 1 1 d . . . C24 C 0.8687(2) 0.94602(16) 0.05900(18) 0.0287(9) Uani 1 1 d . . . C25 C 0.8102(2) 0.93732(17) 0.00325(18) 0.0311(9) Uani 1 1 d . . . H25 H 0.8010 0.9660 -0.0281 0.037 Uiso 1 1 calc R . . C26 C 0.7630(2) 0.88896(16) -0.01060(17) 0.0287(9) Uani 1 1 d . . . C27 C 0.7767(2) 0.84886(16) 0.03516(17) 0.0290(9) Uani 1 1 d . . . H27 H 0.7467 0.8153 0.0274 0.035 Uiso 1 1 calc R . . C28 C 0.8343(2) 0.85561(15) 0.09404(17) 0.0253(8) Uani 1 1 d . . . C29 C 0.9187(2) 0.99949(18) 0.06986(19) 0.0377(10) Uani 1 1 d . . . C30 C 0.8938(3) 1.0389(2) 0.0124(2) 0.0582(14) Uani 1 1 d . . . H30A H 0.9274 1.0717 0.0202 0.087 Uiso 1 1 calc R . . H30B H 0.8458 1.0542 0.0034 0.087 Uiso 1 1 calc R . . H30C H 0.8924 1.0161 -0.0230 0.087 Uiso 1 1 calc R . . C31 C 0.9944(3) 0.9783(2) 0.0839(2) 0.0567(14) Uani 1 1 d . . . H31A H 1.0260 1.0123 0.0896 0.085 Uiso 1 1 calc R . . H31B H 0.9936 0.9546 0.0492 0.085 Uiso 1 1 calc R . . H31C H 1.0124 0.9546 0.1217 0.085 Uiso 1 1 calc R . . C32 C 0.9186(3) 1.03666(19) 0.1237(2) 0.0511(13) Uani 1 1 d . . . H32A H 0.9369 1.0132 0.1616 0.077 Uiso 1 1 calc R . . H32B H 0.8695 1.0495 0.1143 0.077 Uiso 1 1 calc R . . H32C H 0.9494 1.0711 0.1294 0.077 Uiso 1 1 calc R . . C33 C 0.7004(2) 0.88435(18) -0.07485(18) 0.0355(10) Uani 1 1 d . . . C34 C 0.6587(3) 0.8274(2) -0.0821(2) 0.0502(12) Uani 1 1 d . . . H34A H 0.6911 0.7939 -0.0755 0.075 Uiso 1 1 calc R . . H34B H 0.6200 0.8253 -0.1238 0.075 Uiso 1 1 calc R . . H34C H 0.6382 0.8262 -0.0515 0.075 Uiso 1 1 calc R . . C35 C 0.6489(2) 0.9360(2) -0.0843(2) 0.0519(13) Uani 1 1 d . . . H35A H 0.6278 0.9334 -0.0542 0.078 Uiso 1 1 calc R . . H35B H 0.6105 0.9346 -0.1263 0.078 Uiso 1 1 calc R . . H35C H 0.6753 0.9730 -0.0784 0.078 Uiso 1 1 calc R . . C36 C 0.7290(3) 0.8864(2) -0.12475(19) 0.0459(12) Uani 1 1 d . . . H36A H 0.7564 0.9226 -0.1204 0.069 Uiso 1 1 calc R . . H36B H 0.6887 0.8853 -0.1657 0.069 Uiso 1 1 calc R . . H36C H 0.7602 0.8525 -0.1201 0.069 Uiso 1 1 calc R . . C37 C 0.8471(2) 0.80816(16) 0.13645(17) 0.0262(9) Uani 1 1 d . . . H37 H 0.8180 0.7743 0.1214 0.031 Uiso 1 1 calc R . . N2 N 0.89504(16) 0.80643(12) 0.19413(14) 0.0237(7) Uani 1 1 d . . . C38 C 0.91103(19) 0.75022(15) 0.22338(18) 0.0256(8) Uani 1 1 d . . . C39 C 0.9046(2) 0.69915(16) 0.18932(19) 0.0311(9) Uani 1 1 d . . . H39 H 0.8866 0.7014 0.1455 0.037 Uiso 1 1 calc R . . C40 C 0.9237(2) 0.64546(17) 0.2180(2) 0.0370(10) Uani 1 1 d . . . H40 H 0.9182 0.6111 0.1938 0.044 Uiso 1 1 calc R . . C41 C 0.9511(2) 0.64099(17) 0.28202(19) 0.0348(10) Uani 1 1 d . . . H41 H 0.9651 0.6040 0.3018 0.042 Uiso 1 1 calc R . . C42 C 0.9575(2) 0.69089(15) 0.31631(18) 0.0288(9) Uani 1 1 d . . . H42 H 0.9756 0.6879 0.3601 0.035 Uiso 1 1 calc R . . C43 C 0.93791(19) 0.74585(15) 0.28838(17) 0.0247(8) Uani 1 1 d . . . C44 C 0.94659(19) 0.79747(16) 0.32809(17) 0.0241(8) Uani 1 1 d . . . O5 O 0.94898(13) 0.84890(10) 0.31042(11) 0.0253(6) Uani 1 1 d . . . O6 O 0.95200(13) 0.78746(10) 0.38303(11) 0.0273(6) Uani 1 1 d . . . Al3 Al 0.96877(6) 0.83885(5) 0.44547(5) 0.0248(3) Uani 1 1 d . . . C46 C 0.9716(2) 0.79643(14) 0.51768(15) 0.0233(8) Uani 1 1 d . . . H46A H 0.9228 0.7845 0.5106 0.035 Uiso 1 1 calc R . . H46B H 0.9915 0.8219 0.5541 0.035 Uiso 1 1 calc R . . H46C H 1.0019 0.7615 0.5246 0.035 Uiso 1 1 calc R . . Cl1 Cl 1.06406(6) 0.88457(6) 0.45899(6) 0.0552(3) Uani 1 1 d . . . Al4 Al 0.70813(6) 0.96545(5) 0.17857(6) 0.0297(3) Uani 1 1 d . . . C47 C 0.7095(2) 0.98913(19) 0.1008(2) 0.0419(11) Uani 1 1 d . . . H47A H 0.7108 1.0320 0.0989 0.063 Uiso 1 1 calc R . . H47B H 0.6662 0.9745 0.0664 0.063 Uiso 1 1 calc R . . H47C H 0.7521 0.9728 0.0977 0.063 Uiso 1 1 calc R . . Cl2 Cl 0.63007(8) 1.00554(7) 0.20140(9) 0.0867(5) Uani 1 1 d . . . Al2 Al 0.70877(6) 0.80730(5) 0.33370(5) 0.0251(3) Uani 1 1 d . . . O7 O 0.61588(13) 0.78468(10) 0.29179(11) 0.0277(6) Uani 1 1 d . . . C49 C 0.5703(2) 0.77767(16) 0.31748(18) 0.0272(9) Uani 1 1 d . . . C50 C 0.5173(2) 0.73255(16) 0.29717(18) 0.0283(9) Uani 1 1 d . . . C51 C 0.4740(2) 0.72676(17) 0.32852(18) 0.0331(9) Uani 1 1 d . . . H51 H 0.4392 0.6962 0.3157 0.040 Uiso 1 1 calc R . . C52 C 0.4773(2) 0.76271(18) 0.3783(2) 0.0353(10) Uani 1 1 d . . . C53 C 0.5259(2) 0.80777(17) 0.39456(19) 0.0341(10) Uani 1 1 d . . . H53 H 0.5281 0.8344 0.4261 0.041 Uiso 1 1 calc R . . C54 C 0.5730(2) 0.81549(16) 0.36517(18) 0.0284(9) Uani 1 1 d . . . C55 C 0.5113(2) 0.69088(19) 0.2445(2) 0.0421(11) Uani 1 1 d . . . C56 C 0.5793(3) 0.65471(19) 0.2636(2) 0.0555(14) Uani 1 1 d . . . H56A H 0.5849 0.6300 0.2991 0.083 Uiso 1 1 calc R . . H56B H 0.6208 0.6809 0.2751 0.083 Uiso 1 1 calc R . . H56C H 0.5761 0.6298 0.2290 0.083 Uiso 1 1 calc R . . C57 C 0.4478(3) 0.6484(2) 0.2279(2) 0.0623(15) Uani 1 1 d . . . H57A H 0.4437 0.6242 0.1925 0.094 Uiso 1 1 calc R . . H57B H 0.4034 0.6708 0.2173 0.094 Uiso 1 1 calc R . . H57C H 0.4557 0.6230 0.2635 0.094 Uiso 1 1 calc R . . C58 C 0.4994(3) 0.7270(2) 0.1860(2) 0.0670(16) Uani 1 1 d . . . H58A H 0.5415 0.7517 0.1941 0.101 Uiso 1 1 calc R . . H58B H 0.4569 0.7519 0.1752 0.101 Uiso 1 1 calc R . . H58C H 0.4922 0.7003 0.1516 0.101 Uiso 1 1 calc R . . C59 C 0.4293(2) 0.74902(19) 0.4118(2) 0.0439(11) Uani 1 1 d . . . C60 C 0.4477(3) 0.6877(2) 0.4411(3) 0.0610(14) Uani 1 1 d . . . H60A H 0.4984 0.6864 0.4702 0.091 Uiso 1 1 calc R . . H60B H 0.4385 0.6583 0.4086 0.091 Uiso 1 1 calc R . . H60C H 0.4178 0.6792 0.4633 0.091 Uiso 1 1 calc R . . C61 C 0.3498(2) 0.7507(2) 0.3661(3) 0.0592(14) Uani 1 1 d . . . H61A H 0.3200 0.7395 0.3875 0.089 Uiso 1 1 calc R . . H61B H 0.3416 0.7232 0.3321 0.089 Uiso 1 1 calc R . . H61C H 0.3371 0.7905 0.3494 0.089 Uiso 1 1 calc R . . C62 C 0.4401(3) 0.7934(2) 0.4632(3) 0.0693(17) Uani 1 1 d . . . H62A H 0.4239 0.8322 0.4449 0.104 Uiso 1 1 calc R . . H62B H 0.4912 0.7952 0.4915 0.104 Uiso 1 1 calc R . . H62C H 0.4123 0.7813 0.4861 0.104 Uiso 1 1 calc R . . C63 C 0.6218(2) 0.86378(16) 0.38528(18) 0.0288(9) Uani 1 1 d . . . H63 H 0.6147 0.8912 0.4122 0.035 Uiso 1 1 calc R . . N3 N 0.67504(16) 0.87392(12) 0.37036(14) 0.0248(7) Uani 1 1 d . . . C64 C 0.7120(2) 0.92829(16) 0.39137(17) 0.0260(8) Uani 1 1 d . . . C65 C 0.6739(2) 0.97810(16) 0.39389(19) 0.0325(9) Uani 1 1 d . . . H65 H 0.6231 0.9762 0.3784 0.039 Uiso 1 1 calc R . . C66 C 0.7087(2) 1.03035(17) 0.41860(19) 0.0353(10) Uani 1 1 d . . . H66 H 0.6819 1.0637 0.4203 0.042 Uiso 1 1 calc R . . C67 C 0.7822(2) 1.03377(17) 0.44069(19) 0.0338(10) Uani 1 1 d . . . H67 H 0.8064 1.0689 0.4594 0.041 Uiso 1 1 calc R . . C68 C 0.8204(2) 0.98622(16) 0.43560(17) 0.0290(9) Uani 1 1 d . . . H68 H 0.8710 0.9892 0.4499 0.035 Uiso 1 1 calc R . . C69 C 0.7863(2) 0.93326(15) 0.40967(16) 0.0245(8) Uani 1 1 d . . . C70 C 0.8308(2) 0.88480(16) 0.40279(17) 0.0258(9) Uani 1 1 d . . . O8 O 0.80431(13) 0.83759(10) 0.37613(12) 0.0268(6) Uani 1 1 d . . . O9 O 0.89884(13) 0.89365(10) 0.42472(12) 0.0288(6) Uani 1 1 d . . . O10 O 0.72516(13) 0.76161(11) 0.40113(12) 0.0283(6) Uani 1 1 d . . . C71 C 0.7777(2) 0.72449(16) 0.42970(19) 0.0304(9) Uani 1 1 d . . . C72 C 0.7973(2) 0.70836(19) 0.4923(2) 0.0401(11) Uani 1 1 d . . . C73 C 0.8543(2) 0.67118(19) 0.5198(2) 0.0414(11) Uani 1 1 d . . . H73 H 0.8672 0.6611 0.5619 0.050 Uiso 1 1 calc R . . C74 C 0.8954(2) 0.64659(17) 0.4904(2) 0.0368(10) Uani 1 1 d . . . C75 C 0.8733(2) 0.65968(16) 0.4293(2) 0.0340(10) Uani 1 1 d . . . H75 H 0.8974 0.6422 0.4070 0.041 Uiso 1 1 calc R . . C76 C 0.8156(2) 0.69834(15) 0.39804(18) 0.0276(9) Uani 1 1 d . . . C77 C 0.7558(3) 0.7341(3) 0.5281(2) 0.0747(19) Uani 1 1 d . . . C78 C 0.6768(3) 0.7153(3) 0.4960(3) 0.094(2) Uani 1 1 d . . . H78A H 0.6502 0.7319 0.5182 0.141 Uiso 1 1 calc R . . H78B H 0.6737 0.6724 0.4960 0.141 Uiso 1 1 calc R . . H78C H 0.6561 0.7297 0.4532 0.141 Uiso 1 1 calc R . . C79 C 0.7625(3) 0.8009(3) 0.5315(3) 0.088(2) Uani 1 1 d . . . H79A H 0.7447 0.8170 0.4895 0.132 Uiso 1 1 calc R . . H79B H 0.8130 0.8118 0.5546 0.132 Uiso 1 1 calc R . . H79C H 0.7341 0.8167 0.5524 0.132 Uiso 1 1 calc R . . C80 C 0.7875(4) 0.7101(4) 0.5957(3) 0.133(4) Uani 1 1 d . . . H80A H 0.8394 0.7171 0.6152 0.200 Uiso 1 1 calc R . . H80B H 0.7782 0.6679 0.5951 0.200 Uiso 1 1 calc R . . H80C H 0.7649 0.7303 0.6193 0.200 Uiso 1 1 calc R . . C81 C 0.9598(2) 0.60832(18) 0.5274(2) 0.0448(12) Uani 1 1 d . . . C82 C 0.9962(3) 0.5858(3) 0.4880(3) 0.083(2) Uani 1 1 d . . . H82A H 1.0159 0.6189 0.4737 0.125 Uiso 1 1 calc R . . H82B H 0.9611 0.5648 0.4521 0.125 Uiso 1 1 calc R . . H82C H 1.0352 0.5590 0.5124 0.125 Uiso 1 1 calc R . . C83 C 0.9350(3) 0.55496(19) 0.5537(2) 0.0565(14) Uani 1 1 d . . . H83A H 0.9768 0.5310 0.5787 0.085 Uiso 1 1 calc R . . H83B H 0.9012 0.5314 0.5195 0.085 Uiso 1 1 calc R . . H83C H 0.9114 0.5688 0.5796 0.085 Uiso 1 1 calc R . . C84 C 1.0133(3) 0.6435(2) 0.5819(3) 0.0728(18) Uani 1 1 d . . . H84A H 1.0547 0.6188 0.6060 0.109 Uiso 1 1 calc R . . H84B H 0.9901 0.6565 0.6084 0.109 Uiso 1 1 calc R . . H84C H 1.0294 0.6778 0.5663 0.109 Uiso 1 1 calc R . . C85 C 0.7946(2) 0.70676(15) 0.33355(18) 0.0282(9) Uani 1 1 d . . . H85 H 0.8179 0.6830 0.3147 0.034 Uiso 1 1 calc R . . N4 N 0.74659(16) 0.74370(12) 0.29745(14) 0.0257(7) Uani 1 1 d . . . C86 C 0.7244(2) 0.73715(16) 0.23234(18) 0.0278(9) Uani 1 1 d . . . C87 C 0.7221(2) 0.68102(17) 0.2067(2) 0.0365(10) Uani 1 1 d . . . H87 H 0.7349 0.6476 0.2329 0.044 Uiso 1 1 calc R . . C88 C 0.7014(2) 0.67414(19) 0.1439(2) 0.0428(11) Uani 1 1 d . . . H88 H 0.7008 0.6361 0.1275 0.051 Uiso 1 1 calc R . . C89 C 0.6816(2) 0.7217(2) 0.1050(2) 0.0421(11) Uani 1 1 d . . . H89 H 0.6677 0.7167 0.0618 0.051 Uiso 1 1 calc R . . C90 C 0.6823(2) 0.77695(18) 0.12905(18) 0.0336(10) Uani 1 1 d . . . H90 H 0.6684 0.8098 0.1020 0.040 Uiso 1 1 calc R . . C91 C 0.7030(2) 0.78554(16) 0.19246(18) 0.0273(9) Uani 1 1 d . . . C92 C 0.70226(19) 0.84595(16) 0.21467(18) 0.0266(9) Uani 1 1 d . . . O11 O 0.70482(13) 0.85667(10) 0.26765(11) 0.0276(6) Uani 1 1 d . . . O12 O 0.69796(14) 0.88685(11) 0.17691(12) 0.0320(6) Uani 1 1 d . . . N5 N 0.6797(12) 1.0497(6) 0.5656(10) 0.349(11) Uani 1 1 d DU . . C93 C 0.7163(11) 1.0054(7) 0.5701(7) 0.242(8) Uani 1 1 d DU . . C94 C 0.7444(7) 0.9505(7) 0.5744(7) 0.215(6) Uani 1 1 d DU . . H94A H 0.7060 0.9214 0.5635 0.322 Uiso 1 1 calc R . . H94B H 0.7799 0.9436 0.6169 0.322 Uiso 1 1 calc R . . H94C H 0.7677 0.9471 0.5460 0.322 Uiso 1 1 calc R . . N6 N 0.0793(17) 0.5810(11) 0.0184(14) 0.265(13) Uani 0.50 1 d PDU A 1 C95 C 0.0377(14) 0.5765(10) 0.0418(14) 0.204(11) Uani 0.50 1 d PDU A 1 C96 C -0.006(3) 0.5828(15) 0.074(3) 0.256(17) Uani 0.50 1 d PDU A 1 N6X N 0.019(2) 0.4319(11) -0.078(2) 0.271(15) Uani 0.50 1 d PDU B 2 C95X C 0.0152(15) 0.4838(11) -0.0723(13) 0.221(12) Uani 0.50 1 d PDU B 2 C96X C 0.0358(14) 0.5389(11) -0.0467(14) 0.205(13) Uani 0.50 1 d PDU B 2 N7 N 0.0049(3) 0.5076(2) 0.2184(3) 0.0918(18) Uani 1 1 d D . . C97 C -0.0015(3) 0.4655(3) 0.2415(3) 0.0607(14) Uani 1 1 d D . . C98 C -0.0096(3) 0.4115(2) 0.2696(3) 0.0712(16) Uani 1 1 d D . . H98A H -0.0605 0.4009 0.2529 0.107 Uiso 1 1 calc R . . H98B H 0.0088 0.4168 0.3145 0.107 Uiso 1 1 calc R . . H98C H 0.0174 0.3803 0.2606 0.107 Uiso 1 1 calc R . . N8 N 0.7809(3) 0.6776(2) 0.0159(2) 0.0742(14) Uani 1 1 d D . . C99 C 0.7458(3) 0.6677(2) -0.0351(3) 0.0561(14) Uani 1 1 d D . . C100 C 0.7012(3) 0.6551(3) -0.0989(2) 0.0729(17) Uani 1 1 d D . . H10D H 0.6515 0.6662 -0.1084 0.109 Uiso 1 1 calc R . . H10E H 0.7034 0.6131 -0.1066 0.109 Uiso 1 1 calc R . . H10F H 0.7183 0.6776 -0.1253 0.109 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 0.0270(6) 0.0200(6) 0.0240(6) -0.0024(5) 0.0114(5) -0.0040(5) O1 0.0274(15) 0.0253(14) 0.0289(15) -0.0017(11) 0.0128(12) -0.0025(11) C1 0.030(2) 0.034(2) 0.024(2) 0.0059(17) 0.0123(18) -0.0004(18) C2 0.044(3) 0.036(2) 0.037(2) 0.0038(19) 0.025(2) 0.000(2) C3 0.056(3) 0.046(3) 0.066(3) 0.012(2) 0.048(3) 0.008(2) C4 0.051(3) 0.043(3) 0.063(3) 0.016(2) 0.040(3) -0.001(2) C5 0.043(3) 0.038(2) 0.045(3) 0.007(2) 0.024(2) -0.004(2) C6 0.032(2) 0.031(2) 0.030(2) 0.0048(18) 0.0140(19) -0.0012(18) C7 0.052(3) 0.043(3) 0.052(3) -0.001(2) 0.038(3) 0.004(2) C8 0.088(4) 0.052(3) 0.109(5) -0.018(3) 0.075(4) -0.004(3) C9 0.049(3) 0.030(2) 0.057(3) 0.006(2) 0.030(2) 0.006(2) C10 0.074(4) 0.055(3) 0.040(3) -0.009(2) 0.032(3) -0.007(3) C11 0.065(4) 0.054(3) 0.134(6) 0.021(3) 0.076(4) 0.001(3) C12 0.059(4) 0.103(6) 0.328(13) 0.097(7) 0.110(7) 0.016(4) C13 0.066(4) 0.068(4) 0.121(5) 0.009(4) 0.060(4) -0.020(3) C14 0.192(8) 0.059(4) 0.196(8) -0.020(5) 0.175(8) -0.035(5) C15 0.031(2) 0.027(2) 0.032(2) 0.0001(18) 0.0079(19) -0.0077(17) N1 0.0269(18) 0.0213(16) 0.0294(18) 0.0011(14) 0.0119(15) -0.0039(13) C16 0.039(2) 0.0150(18) 0.026(2) -0.0003(16) 0.0154(19) -0.0048(17) C17 0.035(2) 0.026(2) 0.032(2) -0.0003(18) 0.0075(19) -0.0070(18) C18 0.052(3) 0.024(2) 0.029(2) -0.0054(18) 0.013(2) -0.0086(19) C19 0.052(3) 0.025(2) 0.035(2) -0.0057(18) 0.022(2) -0.001(2) C20 0.038(2) 0.022(2) 0.033(2) -0.0022(18) 0.017(2) -0.0038(17) C21 0.033(2) 0.0186(18) 0.022(2) 0.0006(15) 0.0131(18) -0.0049(16) C22 0.035(2) 0.0190(19) 0.025(2) 0.0021(16) 0.0169(18) -0.0035(17) O2 0.0284(15) 0.0217(13) 0.0254(14) -0.0046(11) 0.0102(12) -0.0022(11) O3 0.0304(16) 0.0302(15) 0.0383(17) -0.0083(12) 0.0155(13) 0.0023(12) O4 0.0311(15) 0.0261(14) 0.0259(15) -0.0028(11) 0.0120(13) -0.0066(11) C23 0.027(2) 0.027(2) 0.027(2) -0.0053(17) 0.0155(18) 0.0000(17) C24 0.037(2) 0.028(2) 0.028(2) -0.0009(17) 0.021(2) 0.0003(17) C25 0.039(2) 0.031(2) 0.027(2) 0.0009(17) 0.017(2) 0.0034(19) C26 0.031(2) 0.026(2) 0.029(2) -0.0027(17) 0.0120(18) 0.0058(17) C27 0.030(2) 0.025(2) 0.031(2) -0.0048(17) 0.0124(19) -0.0009(17) C28 0.030(2) 0.0235(19) 0.024(2) -0.0019(16) 0.0134(18) 0.0011(17) C29 0.045(3) 0.036(2) 0.035(3) 0.0010(19) 0.020(2) -0.010(2) C30 0.076(4) 0.046(3) 0.051(3) 0.011(2) 0.025(3) -0.021(3) C31 0.049(3) 0.072(3) 0.057(3) 0.007(3) 0.030(3) -0.019(3) C32 0.072(4) 0.033(2) 0.048(3) -0.002(2) 0.025(3) -0.014(2) C33 0.040(3) 0.035(2) 0.025(2) -0.0028(18) 0.0074(19) 0.0068(19) C34 0.047(3) 0.052(3) 0.036(3) -0.004(2) 0.003(2) -0.007(2) C35 0.045(3) 0.051(3) 0.048(3) -0.003(2) 0.008(2) 0.016(2) C36 0.057(3) 0.045(3) 0.031(2) -0.005(2) 0.014(2) 0.007(2) C37 0.029(2) 0.023(2) 0.029(2) -0.0053(17) 0.0144(19) -0.0042(16) N2 0.0282(18) 0.0205(16) 0.0241(18) -0.0010(13) 0.0127(15) -0.0027(13) C38 0.025(2) 0.0207(19) 0.034(2) -0.0015(17) 0.0148(18) -0.0032(16) C39 0.037(2) 0.025(2) 0.031(2) -0.0045(18) 0.0137(19) -0.0013(18) C40 0.044(3) 0.026(2) 0.041(3) -0.0093(19) 0.018(2) -0.0007(19) C41 0.042(3) 0.023(2) 0.043(3) 0.0034(19) 0.020(2) 0.0013(18) C42 0.035(2) 0.024(2) 0.032(2) 0.0010(17) 0.0183(19) -0.0046(17) C43 0.023(2) 0.0212(19) 0.033(2) 0.0004(16) 0.0151(18) -0.0014(16) C44 0.021(2) 0.026(2) 0.028(2) 0.0001(17) 0.0135(17) -0.0036(16) O5 0.0329(15) 0.0200(13) 0.0252(14) -0.0017(11) 0.0142(12) -0.0039(11) O6 0.0342(16) 0.0272(14) 0.0235(14) -0.0010(11) 0.0150(12) -0.0048(11) Al3 0.0272(6) 0.0250(6) 0.0238(6) -0.0014(5) 0.0123(5) -0.0032(5) C46 0.042(2) 0.0138(17) 0.0142(18) 0.0001(14) 0.0113(17) -0.0119(16) Cl1 0.0461(7) 0.0630(8) 0.0563(8) -0.0014(6) 0.0211(6) -0.0126(6) Al4 0.0290(7) 0.0278(6) 0.0335(7) 0.0001(5) 0.0144(6) 0.0029(5) C47 0.046(3) 0.038(2) 0.042(3) 0.014(2) 0.019(2) 0.008(2) Cl2 0.0694(10) 0.0917(11) 0.1137(14) -0.0151(10) 0.0527(10) 0.0153(8) Al2 0.0296(6) 0.0211(6) 0.0294(6) -0.0045(5) 0.0170(5) -0.0019(5) O7 0.0317(15) 0.0257(14) 0.0293(15) -0.0056(11) 0.0164(13) -0.0051(11) C49 0.028(2) 0.023(2) 0.032(2) 0.0003(17) 0.0141(19) 0.0015(16) C50 0.029(2) 0.025(2) 0.030(2) -0.0009(17) 0.0111(18) -0.0031(17) C51 0.031(2) 0.030(2) 0.038(2) -0.0013(19) 0.014(2) -0.0048(18) C52 0.029(2) 0.036(2) 0.046(3) -0.006(2) 0.021(2) -0.0039(19) C53 0.032(2) 0.035(2) 0.041(2) -0.0108(19) 0.020(2) -0.0026(19) C54 0.026(2) 0.028(2) 0.035(2) -0.0076(18) 0.0156(19) -0.0022(17) C55 0.056(3) 0.038(2) 0.039(3) -0.012(2) 0.026(2) -0.024(2) C56 0.085(4) 0.031(2) 0.077(4) -0.016(2) 0.060(3) -0.016(3) C57 0.080(4) 0.059(3) 0.055(3) -0.030(3) 0.035(3) -0.038(3) C58 0.091(4) 0.074(4) 0.032(3) -0.012(3) 0.021(3) -0.038(3) C59 0.043(3) 0.043(3) 0.059(3) -0.006(2) 0.034(2) -0.006(2) C60 0.066(4) 0.065(3) 0.071(4) 0.007(3) 0.047(3) -0.002(3) C61 0.042(3) 0.056(3) 0.090(4) 0.001(3) 0.038(3) -0.008(2) C62 0.072(4) 0.079(4) 0.090(4) -0.024(3) 0.067(4) -0.023(3) C63 0.029(2) 0.028(2) 0.031(2) -0.0086(17) 0.0140(19) 0.0005(17) N3 0.0257(18) 0.0220(16) 0.0282(17) -0.0051(14) 0.0128(15) -0.0016(13) C64 0.031(2) 0.025(2) 0.023(2) -0.0036(16) 0.0126(18) -0.0043(17) C65 0.029(2) 0.029(2) 0.039(2) -0.0080(18) 0.0126(19) -0.0011(18) C66 0.042(3) 0.023(2) 0.041(3) -0.0059(19) 0.018(2) 0.0006(19) C67 0.039(3) 0.024(2) 0.038(2) -0.0048(18) 0.016(2) -0.0085(18) C68 0.033(2) 0.026(2) 0.030(2) 0.0024(17) 0.0147(19) -0.0055(17) C69 0.031(2) 0.0209(19) 0.023(2) 0.0022(16) 0.0130(17) -0.0015(16) C70 0.032(2) 0.026(2) 0.023(2) 0.0051(17) 0.0158(18) -0.0027(17) O8 0.0285(15) 0.0211(14) 0.0344(15) -0.0042(12) 0.0165(12) -0.0039(11) O9 0.0228(15) 0.0255(14) 0.0397(16) -0.0025(12) 0.0147(13) -0.0035(11) O10 0.0278(15) 0.0282(14) 0.0334(15) 0.0026(12) 0.0172(13) 0.0001(12) C71 0.031(2) 0.024(2) 0.040(2) 0.0003(18) 0.019(2) -0.0072(18) C72 0.036(3) 0.048(3) 0.042(3) 0.014(2) 0.023(2) 0.000(2) C73 0.037(3) 0.045(3) 0.041(3) 0.014(2) 0.015(2) -0.007(2) C74 0.034(2) 0.022(2) 0.053(3) 0.004(2) 0.017(2) -0.0069(18) C75 0.034(2) 0.021(2) 0.052(3) 0.0026(19) 0.023(2) -0.0019(18) C76 0.028(2) 0.0192(19) 0.040(2) 0.0011(17) 0.0173(19) -0.0033(16) C77 0.061(4) 0.132(6) 0.047(3) 0.043(3) 0.039(3) 0.042(4) C78 0.061(4) 0.135(6) 0.114(5) 0.072(5) 0.064(4) 0.033(4) C79 0.093(5) 0.125(6) 0.050(4) -0.011(4) 0.033(3) 0.053(4) C80 0.098(5) 0.260(11) 0.074(5) 0.091(6) 0.068(4) 0.091(6) C81 0.039(3) 0.029(2) 0.059(3) 0.011(2) 0.013(2) 0.003(2) C82 0.076(4) 0.080(4) 0.101(5) 0.042(4) 0.045(4) 0.049(3) C83 0.063(3) 0.029(2) 0.054(3) 0.008(2) 0.002(3) -0.007(2) C84 0.038(3) 0.034(3) 0.112(5) 0.014(3) -0.003(3) -0.005(2) C85 0.034(2) 0.0163(19) 0.042(2) -0.0062(18) 0.023(2) -0.0069(17) N4 0.0313(19) 0.0186(16) 0.0328(19) -0.0032(14) 0.0190(16) -0.0012(14) C86 0.030(2) 0.029(2) 0.034(2) -0.0106(18) 0.0224(19) -0.0081(17) C87 0.046(3) 0.028(2) 0.048(3) -0.0068(19) 0.031(2) -0.0073(19) C88 0.055(3) 0.038(3) 0.048(3) -0.021(2) 0.034(2) -0.014(2) C89 0.045(3) 0.051(3) 0.038(3) -0.014(2) 0.026(2) -0.011(2) C90 0.033(2) 0.041(2) 0.030(2) -0.0077(19) 0.0163(19) -0.0077(19) C91 0.024(2) 0.029(2) 0.034(2) -0.0042(18) 0.0176(18) -0.0067(16) C92 0.022(2) 0.029(2) 0.032(2) -0.0028(18) 0.0134(18) -0.0068(16) O11 0.0361(16) 0.0242(14) 0.0259(15) -0.0044(11) 0.0165(12) -0.0039(11) O12 0.0354(16) 0.0299(15) 0.0299(15) -0.0013(12) 0.0129(13) -0.0075(12) N5 0.58(3) 0.159(12) 0.39(2) -0.055(14) 0.28(2) -0.063(14) C93 0.48(3) 0.172(13) 0.161(11) -0.014(11) 0.221(15) -0.080(14) C94 0.207(13) 0.248(14) 0.188(12) 0.054(13) 0.082(10) -0.011(13) N6 0.41(4) 0.20(2) 0.32(3) 0.20(2) 0.28(3) 0.14(2) C95 0.24(3) 0.148(17) 0.28(3) 0.146(18) 0.160(19) 0.070(17) C96 0.40(4) 0.21(3) 0.28(3) 0.05(3) 0.26(3) -0.09(3) N6X 0.39(3) 0.135(13) 0.50(4) 0.16(2) 0.39(3) 0.04(2) C95X 0.31(3) 0.152(14) 0.36(3) 0.14(2) 0.30(2) 0.07(2) C96X 0.25(3) 0.158(16) 0.36(3) 0.13(2) 0.27(3) 0.069(19) N7 0.061(3) 0.082(4) 0.144(5) 0.032(4) 0.055(4) 0.024(3) C97 0.036(3) 0.072(4) 0.076(4) -0.007(3) 0.025(3) 0.008(3) C98 0.082(4) 0.069(4) 0.065(4) -0.005(3) 0.033(3) -0.011(3) N8 0.090(4) 0.074(3) 0.064(3) 0.004(3) 0.038(3) -0.005(3) C99 0.075(4) 0.052(3) 0.055(4) 0.000(3) 0.040(3) -0.009(3) C100 0.083(4) 0.080(4) 0.061(4) -0.006(3) 0.035(3) -0.017(3) _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 O4 1.819(3) . ? Al1 O1 1.826(3) . ? Al1 O5 1.907(3) . ? Al1 O2 1.927(3) . ? Al1 N2 2.001(3) . ? Al1 N1 2.012(3) . ? O1 C1 1.314(4) . ? C1 C6 1.410(5) . ? C1 C2 1.419(5) . ? C2 C3 1.388(6) . ? C2 C7 1.541(6) . ? C3 C4 1.406(6) . ? C4 C5 1.350(6) . ? C4 C11 1.558(6) . ? C5 C6 1.414(5) . ? C6 C15 1.417(5) . ? C7 C10 1.529(7) . ? C7 C8 1.535(6) . ? C7 C9 1.547(6) . ? C11 C14 1.514(9) . ? C11 C12 1.517(9) . ? C11 C13 1.520(8) . ? C15 N1 1.302(5) . ? N1 C16 1.421(5) . ? C16 C21 1.390(5) . ? C16 C17 1.410(5) . ? C17 C18 1.382(5) . ? C18 C19 1.382(6) . ? C19 C20 1.372(5) . ? C20 C21 1.406(5) . ? C21 C22 1.484(5) . ? C22 O2 1.246(4) . ? C22 O3 1.280(4) . ? O3 Al4 1.791(3) . ? O4 C23 1.314(4) . ? C23 C28 1.414(5) . ? C23 C24 1.428(5) . ? C24 C25 1.381(5) . ? C24 C29 1.543(5) . ? C25 C26 1.412(5) . ? C26 C27 1.358(5) . ? C26 C33 1.535(5) . ? C27 C28 1.414(5) . ? C28 C37 1.426(5) . ? C29 C31 1.524(6) . ? C29 C30 1.533(6) . ? C29 C32 1.535(6) . ? C33 C34 1.526(6) . ? C33 C36 1.527(6) . ? C33 C35 1.536(6) . ? C37 N2 1.312(5) . ? N2 C38 1.429(5) . ? C38 C39 1.393(5) . ? C38 C43 1.411(5) . ? C39 C40 1.376(5) . ? C40 C41 1.388(6) . ? C41 C42 1.374(5) . ? C42 C43 1.396(5) . ? C43 C44 1.472(5) . ? C44 O5 1.253(4) . ? C44 O6 1.285(4) . ? O6 Al3 1.808(3) . ? Al3 O9 1.808(3) . ? Al3 C46 1.951(3) . ? Al3 Cl1 2.1169(16) . ? Al4 O12 1.802(3) . ? Al4 C47 1.939(4) . ? Al4 Cl2 2.1015(18) . ? Al2 O7 1.817(3) . ? Al2 O10 1.822(3) . ? Al2 O11 1.906(3) . ? Al2 O8 1.918(3) . ? Al2 N4 2.001(3) . ? Al2 N3 2.012(3) . ? O7 C49 1.322(4) . ? C49 C54 1.407(5) . ? C49 C50 1.427(5) . ? C50 C51 1.383(5) . ? C50 C55 1.536(5) . ? C51 C52 1.418(5) . ? C52 C53 1.369(5) . ? C52 C59 1.536(6) . ? C53 C54 1.420(5) . ? C54 C63 1.429(5) . ? C55 C56 1.516(7) . ? C55 C57 1.537(6) . ? C55 C58 1.546(6) . ? C59 C62 1.531(6) . ? C59 C61 1.535(6) . ? C59 C60 1.537(7) . ? C63 N3 1.302(5) . ? N3 C64 1.430(5) . ? C64 C65 1.394(5) . ? C64 C69 1.402(5) . ? C65 C66 1.387(5) . ? C66 C67 1.374(6) . ? C67 C68 1.372(5) . ? C68 C69 1.402(5) . ? C69 C70 1.485(5) . ? C70 O8 1.252(4) . ? C70 O9 1.285(4) . ? O10 C71 1.314(5) . ? C71 C72 1.419(6) . ? C71 C76 1.421(5) . ? C72 C73 1.368(6) . ? C72 C77 1.549(7) . ? C73 C74 1.418(6) . ? C74 C75 1.362(6) . ? C74 C81 1.520(6) . ? C75 C76 1.411(5) . ? C76 C85 1.422(5) . ? C77 C79 1.528(9) . ? C77 C78 1.535(8) . ? C77 C80 1.560(7) . ? C81 C82 1.513(7) . ? C81 C84 1.529(7) . ? C81 C83 1.547(6) . ? C85 N4 1.307(5) . ? N4 C86 1.428(5) . ? C86 C91 1.400(5) . ? C86 C87 1.409(5) . ? C87 C88 1.381(6) . ? C88 C89 1.373(6) . ? C89 C90 1.381(6) . ? C90 C91 1.399(5) . ? C91 C92 1.477(5) . ? C92 O11 1.263(4) . ? C92 O12 1.272(4) . ? N5 C93 1.236(14) . ? C93 C94 1.363(13) . ? N6 C95 1.201(14) . ? C95 C96 1.405(16) . ? N6X C95X 1.193(15) . ? C95X C96X 1.383(16) . ? N7 C97 1.140(6) . ? C97 C98 1.443(7) . ? N8 C99 1.144(6) . ? C99 C100 1.435(7) . ? 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 O4 Al1 O1 94.97(12) . . ? O4 Al1 O5 170.91(13) . . ? O1 Al1 O5 93.88(12) . . ? O4 Al1 O2 87.30(12) . . ? O1 Al1 O2 176.00(12) . . ? O5 Al1 O2 84.00(11) . . ? O4 Al1 N2 90.84(12) . . ? O1 Al1 N2 89.74(12) . . ? O5 Al1 N2 87.10(12) . . ? O2 Al1 N2 93.52(12) . . ? O4 Al1 N1 94.00(12) . . ? O1 Al1 N1 88.90(12) . . ? O5 Al1 N1 88.26(12) . . ? O2 Al1 N1 87.65(12) . . ? N2 Al1 N1 175.07(13) . . ? C1 O1 Al1 126.8(2) . . ? O1 C1 C6 120.4(3) . . ? O1 C1 C2 120.9(3) . . ? C6 C1 C2 118.7(4) . . ? C3 C2 C1 116.7(4) . . ? C3 C2 C7 122.6(4) . . ? C1 C2 C7 120.7(4) . . ? C2 C3 C4 125.3(4) . . ? C5 C4 C3 117.0(4) . . ? C5 C4 C11 122.7(4) . . ? C3 C4 C11 120.3(4) . . ? C4 C5 C6 121.1(4) . . ? C1 C6 C5 121.1(4) . . ? C1 C6 C15 121.6(4) . . ? C5 C6 C15 117.0(4) . . ? C10 C7 C8 107.1(4) . . ? C10 C7 C2 108.9(4) . . ? C8 C7 C2 112.3(4) . . ? C10 C7 C9 110.5(4) . . ? C8 C7 C9 107.5(4) . . ? C2 C7 C9 110.3(4) . . ? C14 C11 C12 111.1(6) . . ? C14 C11 C13 107.5(5) . . ? C12 C11 C13 109.4(6) . . ? C14 C11 C4 108.4(5) . . ? C12 C11 C4 108.6(4) . . ? C13 C11 C4 111.9(4) . . ? N1 C15 C6 127.5(4) . . ? C15 N1 C16 117.0(3) . . ? C15 N1 Al1 118.7(3) . . ? C16 N1 Al1 124.2(2) . . ? C21 C16 C17 118.2(3) . . ? C21 C16 N1 121.9(3) . . ? C17 C16 N1 119.9(3) . . ? C18 C17 C16 121.1(4) . . ? C17 C18 C19 120.2(4) . . ? C20 C19 C18 119.5(4) . . ? C19 C20 C21 121.2(4) . . ? C16 C21 C20 119.6(3) . . ? C16 C21 C22 122.9(3) . . ? C20 C21 C22 117.5(3) . . ? O2 C22 O3 121.3(3) . . ? O2 C22 C21 122.8(3) . . ? O3 C22 C21 115.9(3) . . ? C22 O2 Al1 133.7(2) . . ? C22 O3 Al4 129.9(2) . . ? C23 O4 Al1 129.6(2) . . ? O4 C23 C28 121.1(3) . . ? O4 C23 C24 121.0(3) . . ? C28 C23 C24 117.9(3) . . ? C25 C24 C23 117.9(3) . . ? C25 C24 C29 121.6(3) . . ? C23 C24 C29 120.5(3) . . ? C24 C25 C26 124.9(4) . . ? C27 C26 C25 116.6(4) . . ? C27 C26 C33 124.0(4) . . ? C25 C26 C33 119.5(3) . . ? C26 C27 C28 121.9(4) . . ? C27 C28 C23 120.9(3) . . ? C27 C28 C37 116.7(3) . . ? C23 C28 C37 122.0(3) . . ? C31 C29 C30 108.0(4) . . ? C31 C29 C32 110.4(4) . . ? C30 C29 C32 107.6(4) . . ? C31 C29 C24 109.4(4) . . ? C30 C29 C24 111.3(4) . . ? C32 C29 C24 110.1(3) . . ? C34 C33 C36 108.5(3) . . ? C34 C33 C26 111.5(3) . . ? C36 C33 C26 109.8(3) . . ? C34 C33 C35 108.5(4) . . ? C36 C33 C35 109.1(4) . . ? C26 C33 C35 109.3(3) . . ? N2 C37 C28 126.8(3) . . ? C37 N2 C38 117.1(3) . . ? C37 N2 Al1 120.8(2) . . ? C38 N2 Al1 121.8(2) . . ? C39 C38 C43 118.5(3) . . ? C39 C38 N2 121.3(3) . . ? C43 C38 N2 120.1(3) . . ? C40 C39 C38 121.1(4) . . ? C39 C40 C41 120.7(4) . . ? C42 C41 C40 119.0(4) . . ? C41 C42 C43 121.5(4) . . ? C42 C43 C38 119.2(3) . . ? C42 C43 C44 118.6(3) . . ? C38 C43 C44 122.2(3) . . ? O5 C44 O6 120.6(3) . . ? O5 C44 C43 122.9(3) . . ? O6 C44 C43 116.5(3) . . ? C44 O5 Al1 131.2(2) . . ? C44 O6 Al3 128.8(2) . . ? O9 Al3 O6 111.49(13) . . ? O9 Al3 C46 108.13(15) . . ? O6 Al3 C46 109.12(14) . . ? O9 Al3 Cl1 106.12(10) . . ? O6 Al3 Cl1 106.89(10) . . ? C46 Al3 Cl1 115.11(13) . . ? O3 Al4 O12 106.63(13) . . ? O3 Al4 C47 112.01(17) . . ? O12 Al4 C47 107.66(17) . . ? O3 Al4 Cl2 103.80(11) . . ? O12 Al4 Cl2 110.15(11) . . ? C47 Al4 Cl2 116.21(15) . . ? O7 Al2 O10 94.96(12) . . ? O7 Al2 O11 92.38(12) . . ? O10 Al2 O11 172.52(13) . . ? O7 Al2 O8 175.37(13) . . ? O10 Al2 O8 88.30(12) . . ? O11 Al2 O8 84.46(11) . . ? O7 Al2 N4 93.67(12) . . ? O10 Al2 N4 90.17(13) . . ? O11 Al2 N4 87.89(12) . . ? O8 Al2 N4 89.60(12) . . ? O7 Al2 N3 88.90(12) . . ? O10 Al2 N3 91.17(12) . . ? O11 Al2 N3 90.44(12) . . ? O8 Al2 N3 87.74(12) . . ? N4 Al2 N3 176.99(13) . . ? C49 O7 Al2 124.2(2) . . ? O7 C49 C54 120.1(3) . . ? O7 C49 C50 121.1(3) . . ? C54 C49 C50 118.8(3) . . ? C51 C50 C49 117.2(3) . . ? C51 C50 C55 122.0(3) . . ? C49 C50 C55 120.7(3) . . ? C50 C51 C52 125.2(4) . . ? C53 C52 C51 116.5(4) . . ? C53 C52 C59 123.7(4) . . ? C51 C52 C59 119.9(4) . . ? C52 C53 C54 121.2(4) . . ? C49 C54 C53 121.0(3) . . ? C49 C54 C63 121.8(3) . . ? C53 C54 C63 117.1(3) . . ? C56 C55 C50 110.0(4) . . ? C56 C55 C57 108.0(4) . . ? C50 C55 C57 111.6(3) . . ? C56 C55 C58 109.9(4) . . ? C50 C55 C58 109.5(4) . . ? C57 C55 C58 107.9(4) . . ? C62 C59 C61 107.8(4) . . ? C62 C59 C52 111.7(4) . . ? C61 C59 C52 110.4(4) . . ? C62 C59 C60 108.2(4) . . ? C61 C59 C60 109.3(4) . . ? C52 C59 C60 109.4(4) . . ? N3 C63 C54 126.5(3) . . ? C63 N3 C64 116.2(3) . . ? C63 N3 Al2 117.6(2) . . ? C64 N3 Al2 125.3(2) . . ? C65 C64 C69 118.5(3) . . ? C65 C64 N3 119.7(3) . . ? C69 C64 N3 121.8(3) . . ? C66 C65 C64 121.3(4) . . ? C67 C66 C65 119.9(4) . . ? C68 C67 C66 119.8(4) . . ? C67 C68 C69 121.3(4) . . ? C64 C69 C68 118.9(3) . . ? C64 C69 C70 122.9(3) . . ? C68 C69 C70 118.2(3) . . ? O8 C70 O9 120.6(3) . . ? O8 C70 C69 122.6(3) . . ? O9 C70 C69 116.8(3) . . ? C70 O8 Al2 135.0(2) . . ? C70 O9 Al3 127.2(2) . . ? C71 O10 Al2 129.3(2) . . ? O10 C71 C72 121.5(4) . . ? O10 C71 C76 120.5(4) . . ? C72 C71 C76 118.0(4) . . ? C73 C72 C71 118.3(4) . . ? C73 C72 C77 121.8(4) . . ? C71 C72 C77 119.9(4) . . ? C72 C73 C74 125.0(4) . . ? C75 C74 C73 116.0(4) . . ? C75 C74 C81 124.5(4) . . ? C73 C74 C81 119.5(4) . . ? C74 C75 C76 122.1(4) . . ? C75 C76 C71 120.4(4) . . ? C75 C76 C85 117.5(3) . . ? C71 C76 C85 121.9(4) . . ? C79 C77 C78 110.9(5) . . ? C79 C77 C72 110.4(4) . . ? C78 C77 C72 109.2(5) . . ? C79 C77 C80 107.8(6) . . ? C78 C77 C80 108.3(5) . . ? C72 C77 C80 110.2(4) . . ? C82 C81 C74 111.7(4) . . ? C82 C81 C84 109.8(5) . . ? C74 C81 C84 109.4(4) . . ? C82 C81 C83 108.3(4) . . ? C74 C81 C83 109.5(4) . . ? C84 C81 C83 108.1(4) . . ? N4 C85 C76 127.0(3) . . ? C85 N4 C86 117.2(3) . . ? C85 N4 Al2 120.3(3) . . ? C86 N4 Al2 122.5(2) . . ? C91 C86 C87 118.5(4) . . ? C91 C86 N4 121.3(3) . . ? C87 C86 N4 120.1(4) . . ? C88 C87 C86 120.7(4) . . ? C89 C88 C87 120.7(4) . . ? C88 C89 C90 119.5(4) . . ? C89 C90 C91 121.4(4) . . ? C90 C91 C86 119.2(3) . . ? C90 C91 C92 118.2(4) . . ? C86 C91 C92 122.6(3) . . ? O11 C92 O12 121.6(3) . . ? O11 C92 C91 122.3(3) . . ? O12 C92 C91 116.0(3) . . ? C92 O11 Al2 132.7(2) . . ? C92 O12 Al4 137.7(3) . . ? N5 C93 C94 168(2) . . ? N6 C95 C96 168(4) . . ? N6X C95X C96X 158(4) . . ? N7 C97 C98 178.8(7) . . ? N8 C99 C100 179.4(6) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.499 _refine_diff_density_min -0.780 _refine_diff_density_rms 0.066 #===END