Suppelemtary Material for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2002 data_global # *** Added by check_cif _database_code_CSD 175835 _journal_coden_Cambridge 186 _publ_requested_journal 'Dalton Transactions' loop_ _publ_author_name 'Atwood, David' 'Keizer, Timothy S.' 'McKee, Michael L.' 'Munoz-Hernandez, Miguel-Angel' 'Yearwood, Burl' _publ_contact_author_name 'Dr David Atwood' _publ_contact_author_address ; Department of Chemistry University of Kentucky Lexington Kentucky KY 40506-0055 UNITED STATES OF AMERICA ; _publ_contact_author_email 'DATWOOD@PLAINS.NODAK.EDU' _publ_section_title ; Six-coordinate Aluminum Cations: Characterization, Catalysis, and Theory ; #--------------------------------------------------------------------- _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C69 H92 Al B N2 O5' _chemical_formula_weight 1067.24 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' .0033 .0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' .0000 .0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'B' 'B' .0013 .0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' .0061 .0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' .0106 .0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Al' 'Al' .0645 .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 'P 212121' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 12.915(3) _cell_length_b 14.267(3) _cell_length_c 34.426(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 6343(2) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.118 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2312 _exptl_absorpt_coefficient_mu 0.081 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 24812 _diffrn_reflns_av_R_equivalents 0.0737 _diffrn_reflns_av_sigmaI/netI 0.0559 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 36 _diffrn_reflns_theta_min 1.85 _diffrn_reflns_theta_max 22.50 _reflns_number_total 8245 _reflns_number_gt 7015 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _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. Space group assignment was based upon several factors. Firstly, systematic absences indicated the presence of screw axes down a,b and c only - there were no other absences. Secondly, normalized structure factor statistics were indicative of a non-centrosymmetric structure. Thirdly, the largest correlation coefficient matrix elements were all around -0.5, and were between Uij of tertiary-butyl carbons. The structure refinement was unremarkable and the final geometry does not show any evidence of missed symmetry. Nevertheless, the crystals are probably inversion twinned, and were modelled as such with equal occupancy twin components. ; _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^)+(0.0499P)^2^+2.9074P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.00 _refine_ls_number_reflns 8245 _refine_ls_number_parameters 688 _refine_ls_number_restraints 707 _refine_ls_R_factor_all 0.0736 _refine_ls_R_factor_gt 0.0599 _refine_ls_wR_factor_ref 0.1484 _refine_ls_wR_factor_gt 0.1393 _refine_ls_goodness_of_fit_ref 1.138 _refine_ls_restrained_S_all 1.177 _refine_ls_shift/su_max 0.025 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Al Al -0.22133(9) 0.52315(8) 0.13451(3) 0.0419(3) Uani 1 1 d U . . N1 N -0.1322(3) 0.5699(2) 0.17795(9) 0.0470(8) Uani 1 1 d U . . N2 N -0.3082(2) 0.4670(2) 0.17678(9) 0.0455(8) Uani 1 1 d U . . O1 O -0.1499(2) 0.59330(18) 0.10039(7) 0.0470(7) Uani 1 1 d U . . O2 O -0.29584(19) 0.46155(18) 0.09886(7) 0.0445(6) Uani 1 1 d U . . C1 C -0.0858(3) 0.6648(3) 0.10373(11) 0.0434(9) Uani 1 1 d U . . C2 C -0.0508(3) 0.7149(3) 0.07051(11) 0.0527(11) Uani 1 1 d U . . C3 C -0.0874(5) 0.6854(4) 0.02955(13) 0.0859(16) Uani 1 1 d U . . C4 C -0.2063(5) 0.6964(5) 0.02734(16) 0.1095(19) Uani 1 1 d U . . H4A H -0.2298 0.6786 0.0019 0.164 Uiso 1 1 calc R . . H4B H -0.2246 0.7605 0.0322 0.164 Uiso 1 1 calc R . . H4C H -0.2382 0.6569 0.0465 0.164 Uiso 1 1 calc R . . C5 C -0.0546(6) 0.5851(4) 0.02162(17) 0.124(2) Uani 1 1 d U . . H5A H -0.0778 0.5668 -0.0038 0.186 Uiso 1 1 calc R . . H5B H -0.0847 0.5444 0.0408 0.186 Uiso 1 1 calc R . . H5C H 0.0195 0.5806 0.0228 0.186 Uiso 1 1 calc R . . C6 C -0.0401(6) 0.7511(6) -0.00236(16) 0.134(3) Uani 1 1 d U . . H6A H -0.0646 0.7319 -0.0275 0.201 Uiso 1 1 calc R . . H6B H 0.0340 0.7469 -0.0016 0.201 Uiso 1 1 calc R . . H6C H -0.0610 0.8146 0.0025 0.201 Uiso 1 1 calc R . . C7 C 0.0155(3) 0.7889(3) 0.07631(12) 0.0603(12) Uani 1 1 d U . . H7 H 0.0375 0.8217 0.0545 0.072 Uiso 1 1 calc R . . C8 C 0.0529(3) 0.8191(3) 0.11270(12) 0.0526(10) Uani 1 1 d U . . C9 C 0.1295(4) 0.8999(3) 0.11592(13) 0.0660(12) Uani 1 1 d U . . C10 C 0.2236(5) 0.8778(5) 0.0921(2) 0.128(3) Uani 1 1 d U . . H10A H 0.2033 0.8662 0.0657 0.192 Uiso 1 1 calc R . . H10B H 0.2571 0.8232 0.1024 0.192 Uiso 1 1 calc R . . H10C H 0.2705 0.9299 0.0929 0.192 Uiso 1 1 calc R . . C11 C 0.0769(5) 0.9900(4) 0.09978(19) 0.1023(18) Uani 1 1 d U . . H11A H 0.0569 0.9799 0.0733 0.153 Uiso 1 1 calc R . . H11B H 0.1247 1.0414 0.1011 0.153 Uiso 1 1 calc R . . H11C H 0.0167 1.0042 0.1150 0.153 Uiso 1 1 calc R . . C12 C 0.1593(5) 0.9201(4) 0.15741(16) 0.100(2) Uani 1 1 d U . . H12A H 0.0983 0.9345 0.1722 0.151 Uiso 1 1 calc R . . H12B H 0.2058 0.9725 0.1581 0.151 Uiso 1 1 calc R . . H12C H 0.1927 0.8661 0.1684 0.151 Uiso 1 1 calc R . . C13 C 0.0197(3) 0.7695(3) 0.14413(12) 0.0502(10) Uani 1 1 d U . . H13 H 0.0432 0.7863 0.1687 0.060 Uiso 1 1 calc R . . C14 C -0.0495(3) 0.6935(3) 0.14051(11) 0.0438(9) Uani 1 1 d U . . C15 C -0.0694(3) 0.6404(3) 0.17502(12) 0.0495(10) Uani 1 1 d U . . H15 H -0.0341 0.6581 0.1974 0.059 Uiso 1 1 calc R . . C16 C -0.1209(4) 0.5131(3) 0.21387(12) 0.0635(12) Uani 1 1 d U . . H16A H -0.0658 0.5397 0.2295 0.076 Uiso 1 1 calc R . . H16B H -0.1005 0.4500 0.2067 0.076 Uiso 1 1 calc R . . C17 C -0.2180(4) 0.5081(4) 0.23807(13) 0.0727(14) Uani 1 1 d U . . H17A H -0.2195 0.4487 0.2518 0.087 Uiso 1 1 calc R . . H17B H -0.2167 0.5577 0.2573 0.087 Uiso 1 1 calc R . . C18 C -0.3146(4) 0.5172(3) 0.21408(11) 0.0574(11) Uani 1 1 d U . . H18A H -0.3728 0.4930 0.2288 0.069 Uiso 1 1 calc R . . H18B H -0.3275 0.5831 0.2091 0.069 Uiso 1 1 calc R . . C19 C -0.3697(3) 0.3972(3) 0.17167(11) 0.0449(10) Uani 1 1 d U . . H19 H -0.4043 0.3752 0.1935 0.054 Uiso 1 1 calc R . . C20 C -0.3905(3) 0.3499(2) 0.13584(11) 0.0393(8) Uani 1 1 d U . . C21 C -0.3574(3) 0.3871(3) 0.10017(11) 0.0415(9) Uani 1 1 d U . . C22 C -0.3926(3) 0.3440(3) 0.06547(11) 0.0469(10) Uani 1 1 d U . . C23 C -0.3623(4) 0.3847(4) 0.02543(12) 0.0741(14) Uani 1 1 d U . . C24 C -0.4030(6) 0.4856(4) 0.02265(16) 0.107(2) Uani 1 1 d U . . H24A H -0.3850 0.5115 -0.0022 0.161 Uiso 1 1 calc R . . H24B H -0.3725 0.5229 0.0429 0.161 Uiso 1 1 calc R . . H24C H -0.4769 0.4856 0.0255 0.161 Uiso 1 1 calc R . . C25 C -0.2446(5) 0.3816(5) 0.02062(15) 0.1027(19) Uani 1 1 d U . . H25A H -0.2261 0.4068 -0.0043 0.154 Uiso 1 1 calc R . . H25B H -0.2213 0.3178 0.0224 0.154 Uiso 1 1 calc R . . H25C H -0.2127 0.4181 0.0407 0.154 Uiso 1 1 calc R . . C26 C -0.4097(5) 0.3274(4) -0.00800(14) 0.103(2) Uani 1 1 d U . . H26A H -0.3898 0.3546 -0.0324 0.155 Uiso 1 1 calc R . . H26B H -0.4838 0.3279 -0.0058 0.155 Uiso 1 1 calc R . . H26C H -0.3851 0.2640 -0.0067 0.155 Uiso 1 1 calc R . . C27 C -0.4540(3) 0.2661(3) 0.06902(12) 0.0565(11) Uani 1 1 d U . . H27 H -0.4767 0.2377 0.0462 0.068 Uiso 1 1 calc R . . C28 C -0.4853(3) 0.2258(3) 0.10427(13) 0.0526(11) Uani 1 1 d U . . C29 C -0.5579(4) 0.1400(3) 0.10507(14) 0.0697(13) Uani 1 1 d U . . C30 C -0.5180(6) 0.0653(4) 0.0780(2) 0.151(3) Uani 1 1 d U . . H30A H -0.5639 0.0124 0.0786 0.227 Uiso 1 1 calc R . . H30B H -0.4502 0.0460 0.0862 0.227 Uiso 1 1 calc R . . H30C H -0.5145 0.0898 0.0521 0.227 Uiso 1 1 calc R . . C31 C -0.6663(5) 0.1740(5) 0.0932(2) 0.133(3) Uani 1 1 d U . . H31A H -0.6884 0.2226 0.1106 0.199 Uiso 1 1 calc R . . H31B H -0.7141 0.1225 0.0945 0.199 Uiso 1 1 calc R . . H31C H -0.6641 0.1980 0.0672 0.199 Uiso 1 1 calc R . . C32 C -0.5671(5) 0.0985(4) 0.14498(17) 0.112(2) Uani 1 1 d U . . H32A H -0.5912 0.1455 0.1628 0.169 Uiso 1 1 calc R . . H32B H -0.5005 0.0761 0.1533 0.169 Uiso 1 1 calc R . . H32C H -0.6153 0.0473 0.1444 0.169 Uiso 1 1 calc R . . C33 C -0.4537(3) 0.2699(3) 0.13742(12) 0.0455(9) Uani 1 1 d U . . H33 H -0.4744 0.2466 0.1614 0.055 Uiso 1 1 calc R . . O3 O -0.3284(2) 0.62925(17) 0.13676(8) 0.0524(7) Uani 1 1 d U . . C34 C -0.3112(4) 0.7289(3) 0.14075(18) 0.0799(15) Uani 1 1 d U . . H34A H -0.2517 0.7480 0.1255 0.096 Uiso 1 1 calc R . . H34B H -0.2983 0.7447 0.1677 0.096 Uiso 1 1 calc R . . C35 C -0.4041(5) 0.7760(4) 0.1270(2) 0.110(2) Uani 1 1 d U . . H35A H -0.3888 0.8120 0.1038 0.132 Uiso 1 1 calc R . . H35B H -0.4301 0.8185 0.1467 0.132 Uiso 1 1 calc R . . C36 C -0.4818(5) 0.7036(4) 0.11835(19) 0.101(2) Uani 1 1 d U . . H36A H -0.5463 0.7175 0.1316 0.121 Uiso 1 1 calc R . . H36B H -0.4951 0.7008 0.0906 0.121 Uiso 1 1 calc R . . C37 C -0.4395(3) 0.6141(4) 0.13202(18) 0.0786(14) Uani 1 1 d U . . H37A H -0.4708 0.5964 0.1566 0.094 Uiso 1 1 calc R . . H37B H -0.4524 0.5649 0.1132 0.094 Uiso 1 1 calc R . . O4 O -0.1114(2) 0.41853(18) 0.13088(9) 0.0540(7) Uani 1 1 d U . . C38 C -0.0013(3) 0.4353(4) 0.1273(2) 0.099(2) Uani 1 1 d U . . H38A H 0.0110 0.4909 0.1118 0.119 Uiso 1 1 calc R . . H38B H 0.0289 0.4450 0.1528 0.119 Uiso 1 1 calc R . . C39 C 0.0443(5) 0.3556(4) 0.1092(2) 0.117(2) Uani 1 1 d U . . H39A H 0.1032 0.3343 0.1243 0.141 Uiso 1 1 calc R . . H39B H 0.0683 0.3720 0.0834 0.141 Uiso 1 1 calc R . . C40 C -0.0338(4) 0.2810(4) 0.1068(2) 0.0948(18) Uani 1 1 d U . . H40A H -0.0087 0.2240 0.1189 0.114 Uiso 1 1 calc R . . H40B H -0.0513 0.2679 0.0800 0.114 Uiso 1 1 calc R . . C41 C -0.1252(4) 0.3183(3) 0.12812(18) 0.0800(15) Uani 1 1 d U . . H41A H -0.1885 0.3038 0.1142 0.096 Uiso 1 1 calc R . . H41B H -0.1293 0.2908 0.1538 0.096 Uiso 1 1 calc R . . B1C B -0.7393(4) 0.4002(3) 0.24135(15) 0.0523(11) Uani 1 1 d U . . C1C C -0.7612(3) 0.4687(3) 0.27853(13) 0.0538(10) Uani 1 1 d U . . C2C C -0.7333(4) 0.5640(3) 0.27888(16) 0.0710(13) Uani 1 1 d U . . H2C H -0.7112 0.5921 0.2559 0.085 Uiso 1 1 calc R . . C3C C -0.7378(4) 0.6176(4) 0.3129(2) 0.0868(16) Uani 1 1 d U . . H3C H -0.7177 0.6802 0.3123 0.104 Uiso 1 1 calc R . . C4C C -0.7705(5) 0.5804(5) 0.3463(2) 0.1022(19) Uani 1 1 d U . . H4C1 H -0.7734 0.6171 0.3686 0.123 Uiso 1 1 calc R . . C5C C -0.8004(4) 0.4863(5) 0.34780(16) 0.0902(16) Uani 1 1 d U . . H5C1 H -0.8232 0.4597 0.3709 0.108 Uiso 1 1 calc R . . C6C C -0.7953(4) 0.4332(4) 0.31408(14) 0.0691(12) Uani 1 1 d U . . H6C1 H -0.8156 0.3707 0.3152 0.083 Uiso 1 1 calc R . . C7C C -0.8363(3) 0.3271(3) 0.23320(13) 0.0532(10) Uani 1 1 d U . . C8C C -0.9344(3) 0.3352(4) 0.24980(14) 0.0641(12) Uani 1 1 d U . . H8C H -0.9463 0.3832 0.2675 0.077 Uiso 1 1 calc R . . C9C C -1.0158(4) 0.2741(4) 0.24091(17) 0.0840(16) Uani 1 1 d U . . H9C H -1.0800 0.2826 0.2526 0.101 Uiso 1 1 calc R . . C10C C -1.0020(5) 0.2029(5) 0.2156(2) 0.0944(18) Uani 1 1 d U . . H10D H -1.0552 0.1606 0.2107 0.113 Uiso 1 1 calc R . . C11C C -0.9081(5) 0.1940(4) 0.19718(18) 0.0919(17) Uani 1 1 d U . . H11D H -0.8980 0.1464 0.1791 0.110 Uiso 1 1 calc R . . C12C C -0.8285(4) 0.2558(3) 0.20553(15) 0.0724(13) Uani 1 1 d U . . H12D H -0.7666 0.2495 0.1920 0.087 Uiso 1 1 calc R . . C13C C -0.7259(3) 0.4562(3) 0.20024(13) 0.0544(10) Uani 1 1 d U . . C14C C -0.7893(3) 0.5340(3) 0.18967(16) 0.0710(13) Uani 1 1 d U . . H14C H -0.8366 0.5573 0.2076 0.085 Uiso 1 1 calc R . . C15C C -0.7826(4) 0.5755(4) 0.15366(18) 0.0850(15) Uani 1 1 d U . . H15C H -0.8251 0.6263 0.1479 0.102 Uiso 1 1 calc R . . C16C C -0.7157(4) 0.5444(4) 0.12655(17) 0.0900(17) Uani 1 1 d U . . H16C H -0.7110 0.5742 0.1026 0.108 Uiso 1 1 calc R . . C17C C -0.6537(4) 0.4670(4) 0.13469(16) 0.0844(15) Uani 1 1 d U . . H17C H -0.6097 0.4424 0.1159 0.101 Uiso 1 1 calc R . . C18C C -0.6588(3) 0.4273(4) 0.17140(13) 0.0635(12) Uani 1 1 d U . . H18C H -0.6141 0.3780 0.1770 0.076 Uiso 1 1 calc R . . C19C C -0.6285(3) 0.3461(3) 0.25261(12) 0.0480(9) Uani 1 1 d U . . C20C C -0.6044(3) 0.2521(3) 0.24709(14) 0.0621(12) Uani 1 1 d U . . H20C H -0.6551 0.2132 0.2367 0.075 Uiso 1 1 calc R . . C21C C -0.5091(4) 0.2129(4) 0.25611(17) 0.0756(14) Uani 1 1 d U . . H21C H -0.4966 0.1500 0.2507 0.091 Uiso 1 1 calc R . . C22C C -0.4331(4) 0.2663(4) 0.27294(14) 0.0730(14) Uani 1 1 d U . . H22C H -0.3697 0.2401 0.2798 0.088 Uiso 1 1 calc R . . C23C C -0.4529(4) 0.3589(4) 0.27941(14) 0.0672(12) Uani 1 1 d U . . H23C H -0.4027 0.3965 0.2908 0.081 Uiso 1 1 calc R . . C24C C -0.5476(3) 0.3970(3) 0.26905(11) 0.0597(11) Uani 1 1 d U . . H24D H -0.5577 0.4607 0.2733 0.072 Uiso 1 1 calc R . . O1T O -0.2335(3) 0.9802(3) -0.00667(11) 0.515(12) Uani 1 1 d RDU . . C1T C -0.2222(3) 0.9968(3) 0.03383(11) 0.287(8) Uani 1 1 d RDU . . H1T1 H -0.2819 0.9741 0.0481 0.345 Uiso 1 1 calc R . . H1T2 H -0.1604 0.9668 0.0439 0.345 Uiso 1 1 calc R . . C2T C -0.2151(3) 1.0867(3) 0.03583(11) 0.237(6) Uani 1 1 d RDU . . H2T1 H -0.1537 1.1043 0.0503 0.284 Uiso 1 1 calc R . . H2T2 H -0.2752 1.1123 0.0490 0.284 Uiso 1 1 calc R . . C3T C -0.2098(3) 1.1195(3) 0.00033(11) 0.338(9) Uani 1 1 d RDU . . H3T1 H -0.1395 1.1296 -0.0086 0.405 Uiso 1 1 calc R . . H3T2 H -0.2516 1.1751 -0.0037 0.405 Uiso 1 1 calc R . . C4T C -0.2575(3) 1.0330(3) -0.01557(11) 0.554(17) Uani 1 1 d RDU . . H4T1 H -0.3313 1.0352 -0.0104 0.665 Uiso 1 1 calc R . . H4T2 H -0.2487 1.0334 -0.0435 0.665 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Al 0.0504(7) 0.0372(6) 0.0382(6) -0.0002(6) -0.0022(6) -0.0132(5) N1 0.061(2) 0.0404(18) 0.0394(17) 0.0067(14) -0.0078(15) -0.0161(16) N2 0.0523(19) 0.0468(19) 0.0373(17) -0.0004(15) 0.0003(14) -0.0122(16) O1 0.0583(16) 0.0431(15) 0.0397(14) -0.0004(12) -0.0010(13) -0.0191(13) O2 0.0503(15) 0.0457(16) 0.0376(14) 0.0018(12) -0.0020(12) -0.0174(13) C1 0.046(2) 0.040(2) 0.044(2) -0.0057(18) 0.0027(18) -0.0112(17) C2 0.059(3) 0.058(3) 0.041(2) -0.0049(18) 0.008(2) -0.025(2) C3 0.119(4) 0.099(4) 0.040(2) -0.002(3) 0.011(3) -0.057(3) C4 0.120(4) 0.145(5) 0.064(3) 0.026(4) -0.037(3) -0.067(4) C5 0.176(6) 0.114(4) 0.081(4) -0.054(3) 0.054(4) -0.065(4) C6 0.194(7) 0.160(5) 0.048(3) 0.006(3) 0.016(4) -0.106(6) C7 0.069(3) 0.067(3) 0.045(2) 0.002(2) 0.011(2) -0.029(2) C8 0.053(2) 0.051(2) 0.053(2) -0.003(2) 0.007(2) -0.020(2) C9 0.068(3) 0.069(3) 0.061(3) -0.004(2) 0.007(2) -0.035(2) C10 0.086(4) 0.130(5) 0.169(6) -0.052(5) 0.054(4) -0.064(3) C11 0.132(5) 0.065(3) 0.110(4) 0.017(3) -0.007(4) -0.044(3) C12 0.122(5) 0.097(4) 0.082(3) -0.004(3) -0.013(3) -0.071(4) C13 0.053(2) 0.050(2) 0.048(2) -0.0039(19) -0.0039(19) -0.0158(19) C14 0.050(2) 0.040(2) 0.042(2) -0.0001(18) 0.0005(19) -0.0125(17) C15 0.059(3) 0.046(2) 0.044(2) -0.0010(18) -0.011(2) -0.013(2) C16 0.081(3) 0.060(3) 0.049(2) 0.016(2) -0.017(2) -0.020(3) C17 0.096(3) 0.083(3) 0.039(2) -0.001(2) -0.008(2) -0.036(3) C18 0.080(3) 0.053(3) 0.039(2) -0.008(2) 0.005(2) -0.017(2) C19 0.051(2) 0.039(2) 0.044(2) 0.0044(17) 0.0003(19) -0.0138(19) C20 0.040(2) 0.041(2) 0.0368(19) 0.0015(17) -0.0028(18) -0.0058(16) C21 0.039(2) 0.040(2) 0.045(2) 0.0003(17) -0.0030(18) -0.0075(17) C22 0.054(2) 0.047(2) 0.040(2) -0.0040(17) -0.0094(18) -0.015(2) C23 0.105(3) 0.079(3) 0.037(2) 0.000(2) -0.010(3) -0.041(3) C24 0.173(6) 0.078(3) 0.071(4) 0.026(3) -0.042(4) -0.039(3) C25 0.118(4) 0.133(5) 0.057(3) -0.020(3) 0.024(3) -0.062(4) C26 0.157(6) 0.108(4) 0.044(3) -0.007(3) -0.019(3) -0.059(4) C27 0.064(3) 0.060(3) 0.046(2) -0.007(2) -0.006(2) -0.022(2) C28 0.055(2) 0.050(2) 0.053(2) -0.0046(19) -0.001(2) -0.017(2) C29 0.076(3) 0.065(3) 0.068(3) -0.012(2) 0.000(3) -0.040(2) C30 0.201(7) 0.087(4) 0.165(6) -0.061(4) 0.088(6) -0.085(4) C31 0.079(3) 0.148(6) 0.172(7) 0.023(5) -0.029(4) -0.066(3) C32 0.143(5) 0.094(4) 0.100(4) 0.016(3) -0.001(4) -0.080(4) C33 0.046(2) 0.043(2) 0.047(2) -0.0015(19) 0.006(2) -0.0101(18) O3 0.0551(15) 0.0412(14) 0.0608(17) -0.0009(14) -0.0074(15) -0.0053(12) C34 0.092(3) 0.043(2) 0.104(4) -0.006(3) -0.003(3) -0.006(2) C35 0.091(4) 0.065(3) 0.175(7) 0.014(4) 0.009(4) 0.016(3) C36 0.096(4) 0.091(4) 0.116(5) 0.017(4) -0.027(4) 0.019(3) C37 0.055(2) 0.073(3) 0.108(4) -0.001(3) -0.008(3) 0.001(2) O4 0.0488(14) 0.0450(15) 0.0682(18) -0.0034(14) -0.0024(15) -0.0081(12) C38 0.046(2) 0.086(3) 0.164(6) -0.022(4) 0.008(3) -0.010(2) C39 0.079(4) 0.085(4) 0.188(7) 0.005(4) 0.040(4) 0.009(3) C40 0.086(4) 0.073(3) 0.125(5) -0.019(3) -0.003(4) 0.019(3) C41 0.067(3) 0.044(2) 0.129(5) 0.000(3) -0.001(3) -0.003(2) B1C 0.045(2) 0.052(3) 0.060(3) 0.004(2) 0.002(2) 0.004(2) C1C 0.039(2) 0.052(2) 0.070(2) -0.007(2) 0.001(2) 0.011(2) C2C 0.056(3) 0.058(3) 0.100(3) -0.012(2) 0.001(3) 0.000(2) C3C 0.075(3) 0.070(3) 0.116(4) -0.036(3) -0.014(3) 0.011(3) C4C 0.102(5) 0.111(4) 0.094(4) -0.043(4) -0.020(3) 0.041(4) C5C 0.086(4) 0.119(4) 0.066(3) -0.009(3) -0.001(3) 0.033(4) C6C 0.066(3) 0.073(3) 0.068(3) -0.001(2) 0.002(2) 0.015(3) C7C 0.051(2) 0.048(2) 0.060(3) 0.0116(19) -0.007(2) -0.0018(19) C8C 0.053(2) 0.076(3) 0.064(3) 0.024(2) -0.004(2) -0.007(2) C9C 0.054(3) 0.107(4) 0.091(4) 0.043(3) -0.018(3) -0.020(3) C10C 0.092(4) 0.080(4) 0.112(5) 0.039(3) -0.049(3) -0.030(3) C11C 0.114(4) 0.059(3) 0.103(4) -0.002(3) -0.043(3) -0.011(3) C12C 0.075(3) 0.063(3) 0.079(3) -0.004(2) -0.020(3) 0.001(2) C13C 0.045(2) 0.050(2) 0.068(2) 0.006(2) -0.004(2) -0.007(2) C14C 0.051(3) 0.062(3) 0.099(3) 0.021(3) -0.001(3) 0.004(2) C15C 0.067(3) 0.081(4) 0.108(4) 0.036(3) -0.020(3) -0.007(3) C16C 0.072(3) 0.110(4) 0.088(4) 0.045(3) -0.013(3) -0.017(3) C17C 0.069(3) 0.112(4) 0.072(3) 0.027(3) -0.001(3) -0.008(3) C18C 0.052(2) 0.079(3) 0.060(3) 0.010(2) -0.002(2) 0.006(2) C19C 0.048(2) 0.047(2) 0.049(2) 0.0037(18) 0.0094(18) 0.0002(18) C20C 0.058(2) 0.053(2) 0.075(3) -0.004(2) 0.000(2) 0.005(2) C21C 0.065(3) 0.063(3) 0.098(4) 0.005(3) 0.009(3) 0.021(2) C22C 0.052(3) 0.089(3) 0.078(4) 0.012(3) 0.006(2) 0.018(2) C23C 0.048(2) 0.084(3) 0.069(3) 0.007(3) -0.001(2) 0.002(2) C24C 0.052(2) 0.058(3) 0.069(3) -0.004(2) 0.002(2) 0.003(2) O1T 0.61(3) 0.505(15) 0.425(16) -0.228(14) -0.02(2) -0.062(17) C1T 0.36(2) 0.203(10) 0.302(12) 0.075(10) 0.063(14) 0.047(15) C2T 0.257(14) 0.219(11) 0.235(11) 0.006(8) -0.014(12) -0.024(13) C3T 0.321(19) 0.315(10) 0.377(18) 0.205(12) 0.090(16) 0.157(13) C4T 0.54(3) 0.81(2) 0.315(15) -0.076(15) -0.27(2) 0.02(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Al O2 1.790(3) . ? Al O1 1.798(3) . ? Al N1 2.001(3) . ? Al N2 2.004(3) . ? Al O3 2.052(3) . ? Al O4 2.064(3) . ? N1 C15 1.296(5) . ? N1 C16 1.485(5) . ? N2 C19 1.286(5) . ? N2 C18 1.473(5) . ? O1 C1 1.318(4) . ? O2 C21 1.328(4) . ? C1 C14 1.411(5) . ? C1 C2 1.423(5) . ? C2 C7 1.373(6) . ? C2 C3 1.545(6) . ? C3 C5 1.518(9) . ? C3 C4 1.545(8) . ? C3 C6 1.567(7) . ? C4 H4A 0.9600 . ? C4 H4B 0.9600 . ? C4 H4C 0.9600 . ? C5 H5A 0.9600 . ? C5 H5B 0.9600 . ? C5 H5C 0.9600 . ? C6 H6A 0.9600 . ? C6 H6B 0.9600 . ? C6 H6C 0.9600 . ? C7 C8 1.410(6) . ? C7 H7 0.9300 . ? C8 C13 1.362(5) . ? C8 C9 1.523(6) . ? C9 C10 1.499(7) . ? C9 C12 1.507(7) . ? C9 C11 1.557(7) . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C13 C14 1.410(5) . ? C13 H13 0.9300 . ? C14 C15 1.433(5) . ? C15 H15 0.9300 . ? C16 C17 1.508(6) . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C17 C18 1.501(6) . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C19 C20 1.432(5) . ? C19 H19 0.9300 . ? C20 C33 1.404(5) . ? C20 C21 1.405(5) . ? C21 C22 1.418(5) . ? C22 C27 1.372(5) . ? C22 C23 1.546(6) . ? C23 C25 1.529(8) . ? C23 C24 1.536(8) . ? C23 C26 1.539(6) . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? C25 H25A 0.9600 . ? C25 H25B 0.9600 . ? C25 H25C 0.9600 . ? C26 H26A 0.9600 . ? C26 H26B 0.9600 . ? C26 H26C 0.9600 . ? C27 C28 1.402(6) . ? C27 H27 0.9300 . ? C28 C33 1.366(6) . ? C28 C29 1.541(6) . ? C29 C32 1.501(7) . ? C29 C30 1.506(8) . ? C29 C31 1.536(8) . ? C30 H30A 0.9600 . ? C30 H30B 0.9600 . ? C30 H30C 0.9600 . ? C31 H31A 0.9600 . ? C31 H31B 0.9600 . ? C31 H31C 0.9600 . ? C32 H32A 0.9600 . ? C32 H32B 0.9600 . ? C32 H32C 0.9600 . ? C33 H33 0.9300 . ? O3 C34 1.445(5) . ? O3 C37 1.460(5) . ? C34 C35 1.455(7) . ? C34 H34A 0.9700 . ? C34 H34B 0.9700 . ? C35 C36 1.470(8) . ? C35 H35A 0.9700 . ? C35 H35B 0.9700 . ? C36 C37 1.465(7) . ? C36 H36A 0.9700 . ? C36 H36B 0.9700 . ? C37 H37A 0.9700 . ? C37 H37B 0.9700 . ? O4 C41 1.444(5) . ? O4 C38 1.447(5) . ? C38 C39 1.424(8) . ? C38 H38A 0.9700 . ? C38 H38B 0.9700 . ? C39 C40 1.468(8) . ? C39 H39A 0.9700 . ? C39 H39B 0.9700 . ? C40 C41 1.489(7) . ? C40 H40A 0.9700 . ? C40 H40B 0.9700 . ? C41 H41A 0.9700 . ? C41 H41B 0.9700 . ? B1C C13C 1.635(7) . ? B1C C1C 1.635(7) . ? B1C C7C 1.655(6) . ? B1C C19C 1.671(6) . ? C1C C6C 1.396(6) . ? C1C C2C 1.406(6) . ? C2C C3C 1.401(7) . ? C2C H2C 0.9300 . ? C3C C4C 1.335(9) . ? C3C H3C 0.9300 . ? C4C C5C 1.398(9) . ? C4C H4C1 0.9300 . ? C5C C6C 1.387(7) . ? C5C H5C1 0.9300 . ? C6C H6C1 0.9300 . ? C7C C8C 1.394(6) . ? C7C C12C 1.398(6) . ? C8C C9C 1.399(7) . ? C8C H8C 0.9300 . ? C9C C10C 1.350(9) . ? C9C H9C 0.9300 . ? C10C C11C 1.374(9) . ? C10C H10D 0.9300 . ? C11C C12C 1.384(7) . ? C11C H11D 0.9300 . ? C12C H12D 0.9300 . ? C13C C18C 1.382(6) . ? C13C C14C 1.426(6) . ? C14C C15C 1.377(7) . ? C14C H14C 0.9300 . ? C15C C16C 1.347(8) . ? C15C H15C 0.9300 . ? C16C C17C 1.393(8) . ? C16C H16C 0.9300 . ? C17C C18C 1.387(6) . ? C17C H17C 0.9300 . ? C18C H18C 0.9300 . ? C19C C20C 1.389(6) . ? C19C C24C 1.394(5) . ? C20C C21C 1.387(6) . ? C20C H20C 0.9300 . ? C21C C22C 1.371(7) . ? C21C H21C 0.9300 . ? C22C C23C 1.363(7) . ? C22C H22C 0.9300 . ? C23C C24C 1.384(6) . ? C23C H23C 0.9300 . ? C24C H24D 0.9300 . ? O1T C4T 0.8703 . ? O1T C1T 1.4217 . ? C1T C2T 1.2877 . ? C1T C4T 1.8349 . ? C1T H1T1 0.9700 . ? C1T H1T2 0.9700 . ? C2T C3T 1.3104 . ? C2T C4T 2.0045 . ? C2T H2T1 0.9700 . ? C2T H2T2 0.9700 . ? C3T C4T 1.4840 . ? C3T H3T1 0.9700 . ? C3T H3T2 0.9700 . ? C4T H4T1 0.9700 . ? C4T H4T2 0.9700 . ? 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 O2 Al O1 95.81(12) . . ? O2 Al N1 170.05(14) . . ? O1 Al N1 90.43(12) . . ? O2 Al N2 90.03(12) . . ? O1 Al N2 169.73(14) . . ? N1 Al N2 84.99(13) . . ? O2 Al O3 91.48(12) . . ? O1 Al O3 87.71(12) . . ? N1 Al O3 96.52(13) . . ? N2 Al O3 83.70(13) . . ? O2 Al O4 88.46(12) . . ? O1 Al O4 90.57(12) . . ? N1 Al O4 83.72(13) . . ? N2 Al O4 98.04(13) . . ? O3 Al O4 178.26(13) . . ? C15 N1 C16 115.3(3) . . ? C15 N1 Al 124.1(3) . . ? C16 N1 Al 119.8(2) . . ? C19 N2 C18 117.5(3) . . ? C19 N2 Al 123.8(3) . . ? C18 N2 Al 118.0(2) . . ? C1 O1 Al 134.1(3) . . ? C21 O2 Al 133.8(2) . . ? O1 C1 C14 120.8(3) . . ? O1 C1 C2 121.2(3) . . ? C14 C1 C2 118.0(3) . . ? C7 C2 C1 117.9(4) . . ? C7 C2 C3 122.2(4) . . ? C1 C2 C3 119.9(3) . . ? C5 C3 C4 111.4(5) . . ? C5 C3 C2 109.6(5) . . ? C4 C3 C2 108.7(5) . . ? C5 C3 C6 109.2(5) . . ? C4 C3 C6 107.0(6) . . ? C2 C3 C6 111.0(4) . . ? C3 C4 H4A 109.5 . . ? C3 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C3 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C3 C5 H5A 109.5 . . ? C3 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C3 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C3 C6 H6A 109.5 . . ? C3 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C3 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C2 C7 C8 125.3(4) . . ? C2 C7 H7 117.4 . . ? C8 C7 H7 117.4 . . ? C13 C8 C7 116.0(4) . . ? C13 C8 C9 122.7(4) . . ? C7 C8 C9 121.3(4) . . ? C10 C9 C12 110.6(5) . . ? C10 C9 C8 109.1(4) . . ? C12 C9 C8 112.3(4) . . ? C10 C9 C11 109.4(5) . . ? C12 C9 C11 107.0(5) . . ? C8 C9 C11 108.4(4) . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C9 C11 H11A 109.5 . . ? C9 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C9 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C9 C12 H12A 109.5 . . ? C9 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C9 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C8 C13 C14 121.9(4) . . ? C8 C13 H13 119.0 . . ? C14 C13 H13 119.0 . . ? C13 C14 C1 120.9(3) . . ? C13 C14 C15 116.6(4) . . ? C1 C14 C15 122.0(3) . . ? N1 C15 C14 126.0(4) . . ? N1 C15 H15 117.0 . . ? C14 C15 H15 117.0 . . ? N1 C16 C17 113.9(4) . . ? N1 C16 H16A 108.8 . . ? C17 C16 H16A 108.8 . . ? N1 C16 H16B 108.8 . . ? C17 C16 H16B 108.8 . . ? H16A C16 H16B 107.7 . . ? C18 C17 C16 112.5(3) . . ? C18 C17 H17A 109.1 . . ? C16 C17 H17A 109.1 . . ? C18 C17 H17B 109.1 . . ? C16 C17 H17B 109.1 . . ? H17A C17 H17B 107.8 . . ? N2 C18 C17 113.0(4) . . ? N2 C18 H18A 109.0 . . ? C17 C18 H18A 109.0 . . ? N2 C18 H18B 109.0 . . ? C17 C18 H18B 109.0 . . ? H18A C18 H18B 107.8 . . ? N2 C19 C20 126.8(4) . . ? N2 C19 H19 116.6 . . ? C20 C19 H19 116.6 . . ? C33 C20 C21 121.2(3) . . ? C33 C20 C19 117.3(3) . . ? C21 C20 C19 121.2(3) . . ? O2 C21 C20 120.9(3) . . ? O2 C21 C22 120.7(3) . . ? C20 C21 C22 118.4(3) . . ? C27 C22 C21 117.5(4) . . ? C27 C22 C23 122.0(3) . . ? C21 C22 C23 120.5(3) . . ? C25 C23 C24 111.2(5) . . ? C25 C23 C26 107.4(5) . . ? C24 C23 C26 108.4(5) . . ? C25 C23 C22 109.7(4) . . ? C24 C23 C22 108.7(4) . . ? C26 C23 C22 111.5(4) . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C23 C25 H25A 109.5 . . ? C23 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C23 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C23 C26 H26A 109.5 . . ? C23 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C23 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C22 C27 C28 125.2(4) . . ? C22 C27 H27 117.4 . . ? C28 C27 H27 117.4 . . ? C33 C28 C27 116.6(4) . . ? C33 C28 C29 122.2(4) . . ? C27 C28 C29 121.1(4) . . ? C32 C29 C30 108.3(5) . . ? C32 C29 C31 107.2(5) . . ? C30 C29 C31 111.8(6) . . ? C32 C29 C28 112.2(4) . . ? C30 C29 C28 110.1(4) . . ? C31 C29 C28 107.4(4) . . ? C29 C30 H30A 109.5 . . ? C29 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C29 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C29 C31 H31A 109.5 . . ? C29 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C29 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C29 C32 H32A 109.5 . . ? C29 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C29 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C28 C33 C20 121.1(4) . . ? C28 C33 H33 119.5 . . ? C20 C33 H33 119.5 . . ? C34 O3 C37 107.9(3) . . ? C34 O3 Al 128.7(3) . . ? C37 O3 Al 123.3(3) . . ? O3 C34 C35 107.2(4) . . ? O3 C34 H34A 110.3 . . ? C35 C34 H34A 110.3 . . ? O3 C34 H34B 110.3 . . ? C35 C34 H34B 110.3 . . ? H34A C34 H34B 108.5 . . ? C34 C35 C36 107.7(4) . . ? C34 C35 H35A 110.2 . . ? C36 C35 H35A 110.2 . . ? C34 C35 H35B 110.2 . . ? C36 C35 H35B 110.2 . . ? H35A C35 H35B 108.5 . . ? C37 C36 C35 107.0(5) . . ? C37 C36 H36A 110.3 . . ? C35 C36 H36A 110.3 . . ? C37 C36 H36B 110.3 . . ? C35 C36 H36B 110.3 . . ? H36A C36 H36B 108.6 . . ? O3 C37 C36 105.9(4) . . ? O3 C37 H37A 110.6 . . ? C36 C37 H37A 110.6 . . ? O3 C37 H37B 110.6 . . ? C36 C37 H37B 110.6 . . ? H37A C37 H37B 108.7 . . ? C41 O4 C38 106.2(4) . . ? C41 O4 Al 129.4(3) . . ? C38 O4 Al 124.2(3) . . ? C39 C38 O4 108.1(5) . . ? C39 C38 H38A 110.1 . . ? O4 C38 H38A 110.1 . . ? C39 C38 H38B 110.1 . . ? O4 C38 H38B 110.1 . . ? H38A C38 H38B 108.4 . . ? C38 C39 C40 108.6(5) . . ? C38 C39 H39A 110.0 . . ? C40 C39 H39A 110.0 . . ? C38 C39 H39B 110.0 . . ? C40 C39 H39B 110.0 . . ? H39A C39 H39B 108.3 . . ? C39 C40 C41 104.9(4) . . ? C39 C40 H40A 110.8 . . ? C41 C40 H40A 110.8 . . ? C39 C40 H40B 110.8 . . ? C41 C40 H40B 110.8 . . ? H40A C40 H40B 108.8 . . ? O4 C41 C40 106.7(4) . . ? O4 C41 H41A 110.4 . . ? C40 C41 H41A 110.4 . . ? O4 C41 H41B 110.4 . . ? C40 C41 H41B 110.4 . . ? H41A C41 H41B 108.6 . . ? C13C B1C C1C 113.8(4) . . ? C13C B1C C7C 103.9(4) . . ? C1C B1C C7C 112.2(4) . . ? C13C B1C C19C 109.7(3) . . ? C1C B1C C19C 104.1(3) . . ? C7C B1C C19C 113.4(3) . . ? C6C C1C C2C 115.1(4) . . ? C6C C1C B1C 121.6(4) . . ? C2C C1C B1C 122.7(4) . . ? C3C C2C C1C 121.6(5) . . ? C3C C2C H2C 119.2 . . ? C1C C2C H2C 119.2 . . ? C4C C3C C2C 121.1(6) . . ? C4C C3C H3C 119.4 . . ? C2C C3C H3C 119.4 . . ? C3C C4C C5C 120.0(6) . . ? C3C C4C H4C1 120.0 . . ? C5C C4C H4C1 120.0 . . ? C6C C5C C4C 118.7(6) . . ? C6C C5C H5C1 120.6 . . ? C4C C5C H5C1 120.6 . . ? C5C C6C C1C 123.4(5) . . ? C5C C6C H6C1 118.3 . . ? C1C C6C H6C1 118.3 . . ? C8C C7C C12C 113.9(4) . . ? C8C C7C B1C 124.5(4) . . ? C12C C7C B1C 121.3(4) . . ? C7C C8C C9C 122.7(5) . . ? C7C C8C H8C 118.6 . . ? C9C C8C H8C 118.6 . . ? C10C C9C C8C 120.7(6) . . ? C10C C9C H9C 119.6 . . ? C8C C9C H9C 119.6 . . ? C9C C10C C11C 118.9(6) . . ? C9C C10C H10D 120.5 . . ? C11C C10C H10D 120.5 . . ? C10C C11C C12C 120.0(6) . . ? C10C C11C H11D 120.0 . . ? C12C C11C H11D 120.0 . . ? C11C C12C C7C 123.5(5) . . ? C11C C12C H12D 118.3 . . ? C7C C12C H12D 118.3 . . ? C18C C13C C14C 114.2(4) . . ? C18C C13C B1C 122.8(4) . . ? C14C C13C B1C 122.8(4) . . ? C15C C14C C13C 121.9(5) . . ? C15C C14C H14C 119.1 . . ? C13C C14C H14C 119.1 . . ? C16C C15C C14C 121.5(5) . . ? C16C C15C H15C 119.3 . . ? C14C C15C H15C 119.3 . . ? C15C C16C C17C 119.4(5) . . ? C15C C16C H16C 120.3 . . ? C17C C16C H16C 120.3 . . ? C18C C17C C16C 118.7(5) . . ? C18C C17C H17C 120.7 . . ? C16C C17C H17C 120.7 . . ? C13C C18C C17C 124.2(5) . . ? C13C C18C H18C 117.9 . . ? C17C C18C H18C 117.9 . . ? C20C C19C C24C 113.0(4) . . ? C20C C19C B1C 127.3(4) . . ? C24C C19C B1C 119.7(3) . . ? C21C C20C C19C 123.9(5) . . ? C21C C20C H20C 118.0 . . ? C19C C20C H20C 118.0 . . ? C22C C21C C20C 120.4(5) . . ? C22C C21C H21C 119.8 . . ? C20C C21C H21C 119.8 . . ? C23C C22C C21C 118.2(5) . . ? C23C C22C H22C 120.9 . . ? C21C C22C H22C 120.9 . . ? C22C C23C C24C 120.3(5) . . ? C22C C23C H23C 119.8 . . ? C24C C23C H23C 119.8 . . ? C23C C24C C19C 124.2(4) . . ? C23C C24C H24D 117.9 . . ? C19C C24C H24D 117.9 . . ? C4T O1T C1T 103.7 . . ? C2T C1T O1T 103.0 . . ? C2T C1T C4T 77.7 . . ? O1T C1T C4T 27.4 . . ? C2T C1T H1T1 111.2 . . ? O1T C1T H1T1 111.2 . . ? C4T C1T H1T1 111.5 . . ? C2T C1T H1T2 111.2 . . ? O1T C1T H1T2 111.2 . . ? C4T C1T H1T2 131.2 . . ? H1T1 C1T H1T2 109.1 . . ? C1T C2T C3T 108.0 . . ? C1T C2T C4T 63.4 . . ? C3T C2T C4T 47.7 . . ? C1T C2T H2T1 110.1 . . ? C3T C2T H2T1 110.1 . . ? C4T C2T H2T1 140.9 . . ? C1T C2T H2T2 110.1 . . ? C3T C2T H2T2 110.1 . . ? C4T C2T H2T2 109.8 . . ? H2T1 C2T H2T2 108.4 . . ? C2T C3T C4T 91.5 . . ? C2T C3T H3T1 113.4 . . ? C4T C3T H3T1 113.4 . . ? C2T C3T H3T2 113.4 . . ? C4T C3T H3T2 113.4 . . ? H3T1 C3T H3T2 110.7 . . ? O1T C4T C3T 116.2 . . ? O1T C4T C1T 48.8 . . ? C3T C4T C1T 77.8 . . ? O1T C4T C2T 85.6 . . ? C3T C4T C2T 40.8 . . ? C1T C4T C2T 38.9 . . ? O1T C4T H4T1 108.2 . . ? C3T C4T H4T1 108.2 . . ? C1T C4T H4T1 94.7 . . ? C2T C4T H4T1 95.3 . . ? O1T C4T H4T2 108.2 . . ? C3T C4T H4T2 108.2 . . ? C1T C4T H4T2 153.2 . . ? C2T C4T H4T2 147.4 . . ? H4T1 C4T H4T2 107.4 . . ? 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 O2 Al N1 C15 141.6(7) . . . . ? O1 Al N1 C15 12.6(4) . . . . ? N2 Al N1 C15 -158.1(4) . . . . ? O3 Al N1 C15 -75.1(3) . . . . ? O4 Al N1 C15 103.2(3) . . . . ? O2 Al N1 C16 -27.1(10) . . . . ? O1 Al N1 C16 -156.1(3) . . . . ? N2 Al N1 C16 33.1(3) . . . . ? O3 Al N1 C16 116.2(3) . . . . ? O4 Al N1 C16 -65.6(3) . . . . ? O2 Al N2 C19 14.0(3) . . . . ? O1 Al N2 C19 138.8(7) . . . . ? N1 Al N2 C19 -157.4(3) . . . . ? O3 Al N2 C19 105.5(3) . . . . ? O4 Al N2 C19 -74.4(3) . . . . ? O2 Al N2 C18 -156.0(3) . . . . ? O1 Al N2 C18 -31.1(9) . . . . ? N1 Al N2 C18 32.7(3) . . . . ? O3 Al N2 C18 -64.5(3) . . . . ? O4 Al N2 C18 115.6(3) . . . . ? O2 Al O1 C1 171.4(3) . . . . ? N1 Al O1 C1 -16.4(4) . . . . ? N2 Al O1 C1 47.0(9) . . . . ? O3 Al O1 C1 80.1(3) . . . . ? O4 Al O1 C1 -100.1(3) . . . . ? O1 Al O2 C21 168.7(3) . . . . ? N1 Al O2 C21 40.1(10) . . . . ? N2 Al O2 C21 -19.8(3) . . . . ? O3 Al O2 C21 -103.4(3) . . . . ? O4 Al O2 C21 78.3(3) . . . . ? Al O1 C1 C14 8.8(6) . . . . ? Al O1 C1 C2 -171.5(3) . . . . ? O1 C1 C2 C7 179.7(4) . . . . ? C14 C1 C2 C7 -0.6(6) . . . . ? O1 C1 C2 C3 -0.4(7) . . . . ? C14 C1 C2 C3 179.3(4) . . . . ? C7 C2 C3 C5 119.9(5) . . . . ? C1 C2 C3 C5 -59.9(6) . . . . ? C7 C2 C3 C4 -118.1(5) . . . . ? C1 C2 C3 C4 62.0(6) . . . . ? C7 C2 C3 C6 -0.8(8) . . . . ? C1 C2 C3 C6 179.4(5) . . . . ? C1 C2 C7 C8 0.6(7) . . . . ? C3 C2 C7 C8 -179.3(5) . . . . ? C2 C7 C8 C13 0.2(7) . . . . ? C2 C7 C8 C9 177.8(5) . . . . ? C13 C8 C9 C10 120.6(6) . . . . ? C7 C8 C9 C10 -56.8(7) . . . . ? C13 C8 C9 C12 -2.4(7) . . . . ? C7 C8 C9 C12 -179.8(5) . . . . ? C13 C8 C9 C11 -120.4(5) . . . . ? C7 C8 C9 C11 62.2(6) . . . . ? C7 C8 C13 C14 -1.0(6) . . . . ? C9 C8 C13 C14 -178.5(4) . . . . ? C8 C13 C14 C1 1.0(6) . . . . ? C8 C13 C14 C15 173.1(4) . . . . ? O1 C1 C14 C13 179.5(4) . . . . ? C2 C1 C14 C13 -0.2(6) . . . . ? O1 C1 C14 C15 7.9(6) . . . . ? C2 C1 C14 C15 -171.8(4) . . . . ? C16 N1 C15 C14 166.2(4) . . . . ? Al N1 C15 C14 -3.0(6) . . . . ? C13 C14 C15 N1 178.1(4) . . . . ? C1 C14 C15 N1 -9.9(7) . . . . ? C15 N1 C16 C17 121.2(4) . . . . ? Al N1 C16 C17 -69.1(5) . . . . ? N1 C16 C17 C18 28.6(6) . . . . ? C19 N2 C18 C17 114.7(4) . . . . ? Al N2 C18 C17 -74.7(4) . . . . ? C16 C17 C18 N2 39.7(5) . . . . ? C18 N2 C19 C20 167.6(4) . . . . ? Al N2 C19 C20 -2.5(6) . . . . ? N2 C19 C20 C33 174.6(4) . . . . ? N2 C19 C20 C21 -11.4(6) . . . . ? Al O2 C21 C20 12.1(5) . . . . ? Al O2 C21 C22 -169.0(3) . . . . ? C33 C20 C21 O2 -178.6(3) . . . . ? C19 C20 C21 O2 7.6(5) . . . . ? C33 C20 C21 C22 2.5(5) . . . . ? C19 C20 C21 C22 -171.3(4) . . . . ? O2 C21 C22 C27 178.5(4) . . . . ? C20 C21 C22 C27 -2.5(6) . . . . ? O2 C21 C22 C23 -1.6(6) . . . . ? C20 C21 C22 C23 177.4(4) . . . . ? C27 C22 C23 C25 -118.5(5) . . . . ? C21 C22 C23 C25 61.5(6) . . . . ? C27 C22 C23 C24 119.7(5) . . . . ? C21 C22 C23 C24 -60.2(6) . . . . ? C27 C22 C23 C26 0.3(7) . . . . ? C21 C22 C23 C26 -179.6(5) . . . . ? C21 C22 C27 C28 0.4(7) . . . . ? C23 C22 C27 C28 -179.5(5) . . . . ? C22 C27 C28 C33 1.8(7) . . . . ? C22 C27 C28 C29 177.7(4) . . . . ? C33 C28 C29 C32 -14.0(7) . . . . ? C27 C28 C29 C32 170.4(5) . . . . ? C33 C28 C29 C30 -134.6(6) . . . . ? C27 C28 C29 C30 49.7(7) . . . . ? C33 C28 C29 C31 103.5(6) . . . . ? C27 C28 C29 C31 -72.1(6) . . . . ? C27 C28 C33 C20 -1.9(6) . . . . ? C29 C28 C33 C20 -177.7(4) . . . . ? C21 C20 C33 C28 -0.2(6) . . . . ? C19 C20 C33 C28 173.8(4) . . . . ? O2 Al O3 C34 -142.0(4) . . . . ? O1 Al O3 C34 -46.2(4) . . . . ? N1 Al O3 C34 43.9(4) . . . . ? N2 Al O3 C34 128.1(4) . . . . ? O4 Al O3 C34 -54(4) . . . . ? O2 Al O3 C37 34.1(4) . . . . ? O1 Al O3 C37 129.9(4) . . . . ? N1 Al O3 C37 -139.9(4) . . . . ? N2 Al O3 C37 -55.7(4) . . . . ? O4 Al O3 C37 122(4) . . . . ? C37 O3 C34 C35 -16.9(6) . . . . ? Al O3 C34 C35 159.7(4) . . . . ? O3 C34 C35 C36 5.7(8) . . . . ? C34 C35 C36 C37 7.5(8) . . . . ? C34 O3 C37 C36 21.4(6) . . . . ? Al O3 C37 C36 -155.4(4) . . . . ? C35 C36 C37 O3 -17.6(7) . . . . ? O2 Al O4 C41 -41.2(4) . . . . ? O1 Al O4 C41 -137.0(4) . . . . ? N1 Al O4 C41 132.6(4) . . . . ? N2 Al O4 C41 48.6(4) . . . . ? O3 Al O4 C41 -129(4) . . . . ? O2 Al O4 C38 133.2(4) . . . . ? O1 Al O4 C38 37.4(4) . . . . ? N1 Al O4 C38 -52.9(4) . . . . ? N2 Al O4 C38 -136.9(4) . . . . ? O3 Al O4 C38 45(5) . . . . ? C41 O4 C38 C39 20.4(7) . . . . ? Al O4 C38 C39 -155.2(4) . . . . ? O4 C38 C39 C40 -9.1(8) . . . . ? C38 C39 C40 C41 -5.4(8) . . . . ? C38 O4 C41 C40 -23.6(6) . . . . ? Al O4 C41 C40 151.7(4) . . . . ? C39 C40 C41 O4 17.9(7) . . . . ? C13C B1C C1C C6C 166.7(4) . . . . ? C7C B1C C1C C6C 49.0(5) . . . . ? C19C B1C C1C C6C -73.9(5) . . . . ? C13C B1C C1C C2C -22.8(6) . . . . ? C7C B1C C1C C2C -140.5(4) . . . . ? C19C B1C C1C C2C 96.6(5) . . . . ? C6C C1C C2C C3C 1.3(6) . . . . ? B1C C1C C2C C3C -169.8(4) . . . . ? C1C C2C C3C C4C -1.0(8) . . . . ? C2C C3C C4C C5C 0.4(9) . . . . ? C3C C4C C5C C6C 0.0(9) . . . . ? C4C C5C C6C C1C 0.3(8) . . . . ? C2C C1C C6C C5C -0.9(7) . . . . ? B1C C1C C6C C5C 170.3(4) . . . . ? C13C B1C C7C C8C -110.0(5) . . . . ? C1C B1C C7C C8C 13.4(6) . . . . ? C19C B1C C7C C8C 131.0(4) . . . . ? C13C B1C C7C C12C 63.7(5) . . . . ? C1C B1C C7C C12C -172.9(4) . . . . ? C19C B1C C7C C12C -55.3(6) . . . . ? C12C C7C C8C C9C 3.1(6) . . . . ? B1C C7C C8C C9C 177.3(4) . . . . ? C7C C8C C9C C10C 0.5(7) . . . . ? C8C C9C C10C C11C -3.1(8) . . . . ? C9C C10C C11C C12C 1.8(9) . . . . ? C10C C11C C12C C7C 2.2(8) . . . . ? C8C C7C C12C C11C -4.5(7) . . . . ? B1C C7C C12C C11C -178.8(4) . . . . ? C1C B1C C13C C18C 145.2(4) . . . . ? C7C B1C C13C C18C -92.5(5) . . . . ? C19C B1C C13C C18C 29.1(6) . . . . ? C1C B1C C13C C14C -40.7(6) . . . . ? C7C B1C C13C C14C 81.7(5) . . . . ? C19C B1C C13C C14C -156.8(4) . . . . ? C18C C13C C14C C15C -0.1(7) . . . . ? B1C C13C C14C C15C -174.7(5) . . . . ? C13C C14C C15C C16C 0.2(8) . . . . ? C14C C15C C16C C17C 1.6(8) . . . . ? C15C C16C C17C C18C -3.4(8) . . . . ? C14C C13C C18C C17C -1.9(7) . . . . ? B1C C13C C18C C17C 172.7(5) . . . . ? C16C C17C C18C C13C 3.7(8) . . . . ? C13C B1C C19C C20C -99.7(5) . . . . ? C1C B1C C19C C20C 138.2(4) . . . . ? C7C B1C C19C C20C 16.0(6) . . . . ? C13C B1C C19C C24C 79.5(5) . . . . ? C1C B1C C19C C24C -42.6(5) . . . . ? C7C B1C C19C C24C -164.8(4) . . . . ? C24C C19C C20C C21C -1.4(7) . . . . ? B1C C19C C20C C21C 177.8(5) . . . . ? C19C C20C C21C C22C 2.7(8) . . . . ? C20C C21C C22C C23C -1.9(8) . . . . ? C21C C22C C23C C24C -0.1(7) . . . . ? C22C C23C C24C C19C 1.5(7) . . . . ? C20C C19C C24C C23C -0.7(6) . . . . ? B1C C19C C24C C23C 180.0(4) . . . . ? C4T O1T C1T C2T -22.9 . . . . ? O1T C1T C2T C3T -6.9 . . . . ? C4T C1T C2T C3T -17.5 . . . . ? O1T C1T C2T C4T 10.6 . . . . ? C1T C2T C3T C4T 21.3 . . . . ? C1T O1T C4T C3T 42.0 . . . . ? C1T O1T C4T C2T 14.2 . . . . ? C2T C3T C4T O1T -45.4 . . . . ? C2T C3T C4T C1T -14.4 . . . . ? C2T C1T C4T O1T 157.1 . . . . ? C2T C1T C4T C3T 15.0 . . . . ? O1T C1T C4T C3T -142.2 . . . . ? O1T C1T C4T C2T -157.1 . . . . ? C1T C2T C4T O1T -17.0 . . . . ? C3T C2T C4T O1T 140.2 . . . . ? C1T C2T C4T C3T -157.2 . . . . ? C3T C2T C4T C1T 157.2 . . . . ? _diffrn_measured_fraction_theta_max .996 _diffrn_reflns_theta_full 22.50 _diffrn_measured_fraction_theta_full .996 _refine_diff_density_max .232 _refine_diff_density_min -.238 _refine_diff_density_rms .048