# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_Y2iPrPh6 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C77 H96 N6 O12 Y2' _chemical_formula_weight 1475.42 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' Y Y -2.7962 3.5667 '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) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 17.106(4) _cell_length_b 12.420(3) _cell_length_c 17.628(4) _cell_angle_alpha 90.00 _cell_angle_beta 93.337(5) _cell_angle_gamma 90.00 _cell_volume 3739.0(15) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9332 _cell_measurement_theta_min 2.43 _cell_measurement_theta_max 22.23 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.08 _exptl_crystal_density_diffrn 1.311 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1548 _exptl_absorpt_coefficient_mu 1.608 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.749 _exptl_absorpt_correction_T_max 0.912 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX' _diffrn_measurement_method \w _diffrn_reflns_number 15410 _diffrn_reflns_av_R_equivalents 0.1155 _diffrn_reflns_av_sigmaI/netI 0.1707 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.59 _diffrn_reflns_theta_max 22.49 _reflns_number_total 8619 _reflns_number_gt 5682 _reflns_threshold_expression >2sigma(I) _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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. Crystals were of poor quality and gave only low resolution data, therefore 2theta cut-off was applied at 45 deg. Yttrium atoms were refined anisotropically, all other atoms were refined isotropically with both SIMU and SAME restraints due to poor data quality.Hydrogen atoms were fixed to parent atoms using AFIX commands. One ligand is disordered over two positions which were refined with an occupancy factor. There is also a disordered pentane molecule which was split over two positions and refined with occupancy factor. ; _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^)+(0.0785P)^2^+17.7429P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.004(13) _refine_ls_number_reflns 8619 _refine_ls_number_parameters 481 _refine_ls_number_restraints 1073 _refine_ls_R_factor_all 0.1487 _refine_ls_R_factor_gt 0.0945 _refine_ls_wR_factor_ref 0.2271 _refine_ls_wR_factor_gt 0.2033 _refine_ls_goodness_of_fit_ref 1.046 _refine_ls_restrained_S_all 1.011 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Y1 Y 0.85169(7) 0.03553(11) 0.21731(7) 0.0250(4) Uani 1 1 d . A . Y2 Y 0.64187(8) 0.10124(12) 0.26916(10) 0.0492(6) Uani 1 1 d . . . O1 O 0.8174(5) -0.0537(6) 0.1145(4) 0.023(2) Uiso 1 1 d DU . . C10 C 0.8102(7) -0.1502(8) 0.0821(6) 0.024(3) Uiso 1 1 d DU A . C11 C 0.7671(7) -0.1610(9) 0.0130(6) 0.026(3) Uiso 1 1 d DU . . H11 H 0.7460 -0.0990 -0.0122 0.031 Uiso 1 1 calc R A . C12 C 0.7550(7) -0.2610(9) -0.0190(7) 0.035(3) Uiso 1 1 d DU A . H12 H 0.7265 -0.2682 -0.0667 0.042 Uiso 1 1 calc R . . C13 C 0.7848(7) -0.3516(9) 0.0191(6) 0.034(3) Uiso 1 1 d DU . . H13 H 0.7729 -0.4212 -0.0008 0.040 Uiso 1 1 calc R A . C14 C 0.8304(7) -0.3425(9) 0.0839(6) 0.028(3) Uiso 1 1 d DU A . H14 H 0.8525 -0.4053 0.1072 0.033 Uiso 1 1 calc R . . C15 C 0.8457(6) -0.2408(8) 0.1175(6) 0.027(3) Uiso 1 1 d DU . . C16 C 0.8964(6) -0.2304(8) 0.1839(6) 0.029(3) Uiso 1 1 d DU A . O10 O 0.9414(5) -0.3202(6) 0.2012(4) 0.034(2) Uiso 1 1 d DU . . C17 C 0.9976(7) -0.2876(9) 0.2614(6) 0.036(3) Uiso 1 1 d DU A . H17A H 1.0491 -0.2719 0.2411 0.043 Uiso 1 1 calc R . . H17B H 1.0043 -0.3446 0.3006 0.043 Uiso 1 1 calc R . . C18 C 0.9623(6) -0.1868(9) 0.2942(6) 0.037(3) Uiso 1 1 d DU . . H18 H 1.0037 -0.1301 0.3004 0.045 Uiso 1 1 calc R A . N1 N 0.9029(5) -0.1530(7) 0.2333(5) 0.024(2) Uiso 1 1 d DU A . C100 C 0.9245(7) -0.2026(10) 0.3700(6) 0.038(3) Uiso 1 1 d DU A . H100 H 0.8985 -0.1329 0.3817 0.045 Uiso 1 1 calc R . . C101 C 0.8609(8) -0.2874(12) 0.3669(8) 0.055(4) Uiso 1 1 d DU . . H10A H 0.8382 -0.2925 0.4166 0.083 Uiso 1 1 calc R A . H10B H 0.8833 -0.3571 0.3539 0.083 Uiso 1 1 calc R . . H10C H 0.8199 -0.2675 0.3283 0.083 Uiso 1 1 calc R . . C102 C 0.9882(8) -0.2211(13) 0.4339(7) 0.061(5) Uiso 1 1 d DU . . H10D H 0.9636 -0.2305 0.4823 0.092 Uiso 1 1 calc R A . H10E H 1.0233 -0.1587 0.4373 0.092 Uiso 1 1 calc R . . H10F H 1.0182 -0.2858 0.4227 0.092 Uiso 1 1 calc R . . O2 O 0.9447(4) 0.0613(7) 0.3047(4) 0.026(2) Uiso 1 1 d DU . . C20 C 1.0209(6) 0.0751(11) 0.3164(6) 0.030(3) Uiso 1 1 d DU A . C21 C 1.0521(7) 0.0981(13) 0.3903(6) 0.041(3) Uiso 1 1 d DU . . H21 H 1.0183 0.0991 0.4312 0.049 Uiso 1 1 calc R A . C22 C 1.1304(7) 0.1190(14) 0.4043(7) 0.054(4) Uiso 1 1 d DU A . H22 H 1.1503 0.1344 0.4546 0.064 Uiso 1 1 calc R . . C23 C 1.1812(8) 0.1176(15) 0.3448(7) 0.058(4) Uiso 1 1 d DU . . H23 H 1.2351 0.1338 0.3542 0.070 Uiso 1 1 calc R A . C24 C 1.1524(7) 0.0929(14) 0.2739(7) 0.050(4) Uiso 1 1 d DU A . H24 H 1.1873 0.0900 0.2340 0.060 Uiso 1 1 calc R . . C25 C 1.0727(6) 0.0714(10) 0.2571(5) 0.031(3) Uiso 1 1 d DU . . C26 C 1.0455(6) 0.0449(11) 0.1811(5) 0.030(3) Uiso 1 1 d DU A . O20 O 1.1033(4) 0.0215(8) 0.1344(4) 0.039(2) Uiso 1 1 d DU . . C27 C 1.0657(6) -0.0047(11) 0.0612(6) 0.045(3) Uiso 1 1 d DU A . H27A H 1.0773 -0.0800 0.0471 0.054 Uiso 1 1 calc R . . H27B H 1.0841 0.0439 0.0215 0.054 Uiso 1 1 calc R . . C28 C 0.9790(6) 0.0099(10) 0.0700(6) 0.045(3) Uiso 1 1 d DU . . H28 H 0.9528 -0.0616 0.0631 0.054 Uiso 1 1 calc R A . N2 N 0.9747(5) 0.0436(9) 0.1518(5) 0.033(3) Uiso 1 1 d DU A . C200 C 0.9387(9) 0.0892(11) 0.0155(7) 0.067(4) Uiso 1 1 d DU A . H200 H 0.8828 0.0957 0.0287 0.081 Uiso 1 1 calc R . . C201 C 0.9762(10) 0.2009(12) 0.0219(10) 0.087(6) Uiso 1 1 d DU . . H20A H 0.9484 0.2501 -0.0138 0.131 Uiso 1 1 calc R A . H20B H 1.0313 0.1961 0.0097 0.131 Uiso 1 1 calc R . . H20C H 0.9729 0.2280 0.0738 0.131 Uiso 1 1 calc R . . C202 C 0.9400(12) 0.0444(17) -0.0662(8) 0.105(7) Uiso 1 1 d DU . . H20D H 0.9151 0.0961 -0.1019 0.157 Uiso 1 1 calc R A . H20E H 0.9114 -0.0240 -0.0695 0.157 Uiso 1 1 calc R . . H20F H 0.9944 0.0325 -0.0789 0.157 Uiso 1 1 calc R . . O3 O 0.7269(5) 0.1043(8) 0.1760(4) 0.033(2) Uiso 1 1 d DU A . C30 C 0.7228(7) 0.1460(10) 0.1082(6) 0.037(3) Uiso 1 1 d DU . . C31 C 0.6756(8) 0.1012(11) 0.0481(6) 0.044(3) Uiso 1 1 d DU A . H31 H 0.6454 0.0388 0.0571 0.053 Uiso 1 1 calc R . . C32 C 0.6725(8) 0.1453(11) -0.0228(7) 0.055(4) Uiso 1 1 d DU . . H32 H 0.6409 0.1127 -0.0625 0.066 Uiso 1 1 calc R A . C33 C 0.7151(8) 0.2377(12) -0.0378(7) 0.057(4) Uiso 1 1 d DU A . H33 H 0.7136 0.2671 -0.0876 0.069 Uiso 1 1 calc R . . C34 C 0.7590(8) 0.2852(11) 0.0199(6) 0.050(4) Uiso 1 1 d DU . . H34 H 0.7854 0.3509 0.0109 0.060 Uiso 1 1 calc R A . C35 C 0.7657(7) 0.2387(10) 0.0920(6) 0.041(3) Uiso 1 1 d DU A . C36 C 0.8112(8) 0.2881(9) 0.1548(6) 0.046(3) Uiso 1 1 d DU . . O30 O 0.8062(6) 0.3983(7) 0.1569(5) 0.051(3) Uiso 1 1 d DU A . C37 C 0.8476(8) 0.4322(9) 0.2278(7) 0.050(4) Uiso 1 1 d DU . . H37A H 0.8138 0.4788 0.2577 0.060 Uiso 1 1 calc R A . H37B H 0.8958 0.4724 0.2174 0.060 Uiso 1 1 calc R . . C38 C 0.8673(7) 0.3295(9) 0.2699(6) 0.044(3) Uiso 1 1 d DU A . H38 H 0.8295 0.3210 0.3107 0.053 Uiso 1 1 calc R . . N3 N 0.8491(6) 0.2430(8) 0.2102(5) 0.035(3) Uiso 1 1 d DU A . C300 C 0.9487(7) 0.3223(11) 0.3064(7) 0.048(4) Uiso 1 1 d DU . . H300 H 0.9550 0.2499 0.3308 0.057 Uiso 1 1 calc R A . C301 C 0.9619(10) 0.4086(14) 0.3689(9) 0.077(6) Uiso 1 1 d DU A . H30A H 1.0155 0.4029 0.3915 0.116 Uiso 1 1 calc R . . H30B H 0.9246 0.3974 0.4084 0.116 Uiso 1 1 calc R . . H30C H 0.9540 0.4803 0.3466 0.116 Uiso 1 1 calc R . . C302 C 1.0107(9) 0.3336(15) 0.2490(9) 0.081(6) Uiso 1 1 d DU A . H30D H 1.0627 0.3281 0.2750 0.122 Uiso 1 1 calc R . . H30E H 1.0052 0.4038 0.2238 0.122 Uiso 1 1 calc R . . H30F H 1.0041 0.2762 0.2110 0.122 Uiso 1 1 calc R . . O4 O 0.7645(5) 0.0263(9) 0.3096(4) 0.040(2) Uiso 1 1 d DU A . C40 C 0.7701(7) -0.0076(10) 0.3807(6) 0.035(3) Uiso 1 1 d DU . . C41 C 0.8238(8) 0.0413(12) 0.4339(6) 0.049(3) Uiso 1 1 d DU A . H41 H 0.8555 0.0995 0.4189 0.058 Uiso 1 1 calc R . . C42 C 0.8302(8) 0.0046(11) 0.5070(7) 0.053(4) Uiso 1 1 d DU . . H42 H 0.8656 0.0395 0.5425 0.063 Uiso 1 1 calc R A . C43 C 0.7863(8) -0.0826(12) 0.5315(7) 0.056(4) Uiso 1 1 d DU A . H43 H 0.7946 -0.1106 0.5815 0.067 Uiso 1 1 calc R . . C44 C 0.7311(8) -0.1262(11) 0.4810(6) 0.042(4) Uiso 1 1 d DU . . H44 H 0.6978 -0.1814 0.4979 0.051 Uiso 1 1 calc R A . C45 C 0.7222(7) -0.0921(10) 0.4058(6) 0.037(3) Uiso 1 1 d DU A . C46 C 0.6604(7) -0.1370(9) 0.3557(6) 0.033(3) Uiso 1 1 d DU . . O40 O 0.6348(5) -0.2376(6) 0.3749(4) 0.036(2) Uiso 1 1 d DU A . C47 C 0.5675(7) -0.2589(10) 0.3225(6) 0.038(3) Uiso 1 1 d DU . . H47A H 0.5185 -0.2587 0.3497 0.045 Uiso 1 1 calc R A . H47B H 0.5730 -0.3296 0.2975 0.045 Uiso 1 1 calc R . . C48 C 0.5671(6) -0.1686(8) 0.2647(5) 0.027(3) Uiso 1 1 d DU A . H48 H 0.5146 -0.1330 0.2632 0.033 Uiso 1 1 calc R . . N4 N 0.6265(6) -0.0914(7) 0.2990(5) 0.030(3) Uiso 1 1 d DU A . C400 C 0.5851(6) -0.1993(10) 0.1829(6) 0.034(3) Uiso 1 1 d DU . . H400 H 0.5903 -0.1315 0.1530 0.041 Uiso 1 1 calc R A . C401 C 0.6630(6) -0.2603(11) 0.1829(7) 0.038(3) Uiso 1 1 d DU A . H40A H 0.6744 -0.2782 0.1305 0.057 Uiso 1 1 calc R . . H40B H 0.6593 -0.3267 0.2125 0.057 Uiso 1 1 calc R . . H40C H 0.7050 -0.2150 0.2056 0.057 Uiso 1 1 calc R . . C402 C 0.5163(7) -0.2650(11) 0.1463(7) 0.043(4) Uiso 1 1 d DU A . H40D H 0.5280 -0.2853 0.0945 0.065 Uiso 1 1 calc R . . H40E H 0.4685 -0.2214 0.1449 0.065 Uiso 1 1 calc R . . H40F H 0.5087 -0.3302 0.1764 0.065 Uiso 1 1 calc R . . O5 O 0.6739(6) 0.1976(8) 0.3671(5) 0.050(3) Uiso 1 1 d DU A . C50 C 0.6902(9) 0.2960(9) 0.3937(7) 0.049(4) Uiso 1 1 d DU . . C51 C 0.7235(9) 0.3108(11) 0.4673(7) 0.064(4) Uiso 1 1 d DU A . H51 H 0.7342 0.2498 0.4988 0.077 Uiso 1 1 calc R . . C52 C 0.7411(9) 0.4123(11) 0.4949(8) 0.061(4) Uiso 1 1 d DU . . H52 H 0.7628 0.4208 0.5453 0.073 Uiso 1 1 calc R A . C53 C 0.7269(9) 0.5027(11) 0.4490(7) 0.060(4) Uiso 1 1 d DU A . H53 H 0.7379 0.5728 0.4684 0.072 Uiso 1 1 calc R . . C54 C 0.6979(8) 0.4899(9) 0.3774(7) 0.045(3) Uiso 1 1 d DU . . H54 H 0.6900 0.5518 0.3462 0.054 Uiso 1 1 calc R A . C55 C 0.6786(8) 0.3873(9) 0.3464(6) 0.044(3) Uiso 1 1 d DU A . C56 C 0.6452(8) 0.3784(9) 0.2715(6) 0.045(3) Uiso 1 1 d DU . . O50 O 0.6400(5) 0.4712(7) 0.2306(5) 0.046(2) Uiso 1 1 d DU A . C57 C 0.6185(8) 0.4425(10) 0.1518(6) 0.049(4) Uiso 1 1 d DU . . H57A H 0.6650 0.4400 0.1209 0.058 Uiso 1 1 calc R A . H57B H 0.5797 0.4935 0.1284 0.058 Uiso 1 1 calc R . . C58 C 0.5831(7) 0.3309(11) 0.1608(7) 0.063(4) Uiso 1 1 d DU A . H58 H 0.5992 0.2832 0.1188 0.076 Uiso 1 1 calc R . . N5 N 0.6203(7) 0.2935(8) 0.2335(6) 0.053(3) Uiso 1 1 d DU A . C500 C 0.4940(8) 0.3315(16) 0.1625(9) 0.098(6) Uiso 1 1 d DU . . H500 H 0.4781 0.2571 0.1770 0.118 Uiso 1 1 calc R A . C501 C 0.4631(13) 0.408(2) 0.2223(12) 0.145(9) Uiso 1 1 d DU A . H50A H 0.4058 0.4052 0.2201 0.218 Uiso 1 1 calc R . . H50B H 0.4800 0.4818 0.2119 0.218 Uiso 1 1 calc R . . H50C H 0.4838 0.3864 0.2730 0.218 Uiso 1 1 calc R . . C502 C 0.4574(12) 0.3524(19) 0.0829(10) 0.121(8) Uiso 1 1 d DU A . H50D H 0.4002 0.3532 0.0844 0.181 Uiso 1 1 calc R . . H50E H 0.4731 0.2953 0.0485 0.181 Uiso 1 1 calc R . . H50F H 0.4754 0.4221 0.0646 0.181 Uiso 1 1 calc R . . O6 O 0.5546(7) 0.0648(13) 0.1963(8) 0.012(4) Uiso 0.486(8) 1 d PDU A 1 C60 C 0.4800(8) 0.044(2) 0.1798(9) 0.010(3) Uiso 0.486(8) 1 d PDU A 1 C61 C 0.4507(10) 0.039(2) 0.1041(9) 0.016(4) Uiso 0.486(8) 1 d PDU A 1 H61 H 0.4847 0.0521 0.0643 0.020 Uiso 0.486(8) 1 calc PR A 1 C62 C 0.3736(10) 0.015(2) 0.0868(11) 0.026(4) Uiso 0.486(8) 1 d PDU A 1 H62 H 0.3558 0.0013 0.0356 0.032 Uiso 0.486(8) 1 calc PR A 1 C63 C 0.3212(10) 0.010(2) 0.1446(10) 0.021(4) Uiso 0.486(8) 1 d PDU A 1 H63 H 0.2667 0.0021 0.1322 0.025 Uiso 0.486(8) 1 calc PR A 1 C64 C 0.3482(9) 0.016(2) 0.2186(10) 0.020(4) Uiso 0.486(8) 1 d PDU A 1 H64 H 0.3125 0.0085 0.2576 0.023 Uiso 0.486(8) 1 calc PR A 1 C65 C 0.4280(8) 0.035(2) 0.2386(8) 0.019(4) Uiso 0.486(8) 1 d PDU A 1 C66 C 0.4544(9) 0.041(2) 0.3170(8) 0.023(4) Uiso 0.486(8) 1 d PDU A 1 O60 O 0.3975(8) 0.0075(14) 0.3637(8) 0.026(4) Uiso 0.486(8) 1 d PDU A 1 C67 C 0.4324(9) 0.011(2) 0.4399(9) 0.028(5) Uiso 0.486(8) 1 d PDU A 1 H67A H 0.4222 -0.0562 0.4674 0.034 Uiso 0.486(8) 1 calc PR A 1 H67B H 0.4112 0.0725 0.4683 0.034 Uiso 0.486(8) 1 calc PR A 1 C68 C 0.5191(9) 0.0258(17) 0.4306(8) 0.029(4) Uiso 0.486(8) 1 d PDU A 1 H68 H 0.5434 -0.0473 0.4351 0.035 Uiso 0.486(8) 1 calc PR A 1 N6 N 0.5222(9) 0.0593(17) 0.3493(8) 0.028(4) Uiso 0.486(8) 1 d PDU A 1 C600 C 0.5613(12) 0.0962(15) 0.4898(9) 0.032(5) Uiso 0.486(8) 1 d PDU A 1 H600 H 0.6177 0.0991 0.4779 0.038 Uiso 0.486(8) 1 calc PR A 1 C601 C 0.5569(14) 0.045(2) 0.5693(10) 0.034(7) Uiso 0.486(8) 1 d PDU A 1 H60A H 0.5847 0.0914 0.6071 0.051 Uiso 0.486(8) 1 calc PR A 1 H60B H 0.5813 -0.0260 0.5697 0.051 Uiso 0.486(8) 1 calc PR A 1 H60C H 0.5020 0.0387 0.5816 0.051 Uiso 0.486(8) 1 calc PR A 1 C602 C 0.5297(16) 0.2121(16) 0.4879(14) 0.044(7) Uiso 0.486(8) 1 d PDU A 1 H60D H 0.5582 0.2549 0.5271 0.066 Uiso 0.486(8) 1 calc PR A 1 H60E H 0.4739 0.2114 0.4975 0.066 Uiso 0.486(8) 1 calc PR A 1 H60F H 0.5369 0.2438 0.4379 0.066 Uiso 0.486(8) 1 calc PR A 1 O6' O 0.5497(7) 0.0781(11) 0.1635(8) 0.013(3) Uiso 0.514(8) 1 d PDU A 2 C60' C 0.4755(8) 0.0533(18) 0.1478(9) 0.014(4) Uiso 0.514(8) 1 d PDU A 2 C61' C 0.4500(10) 0.025(2) 0.0732(9) 0.024(4) Uiso 0.514(8) 1 d PDU A 2 H61' H 0.4857 0.0280 0.0340 0.029 Uiso 0.514(8) 1 calc PR A 2 C62' C 0.3739(10) -0.007(2) 0.0562(11) 0.026(4) Uiso 0.514(8) 1 d PDU A 2 H62' H 0.3558 -0.0193 0.0049 0.031 Uiso 0.514(8) 1 calc PR A 2 C63' C 0.3235(10) -0.0209(19) 0.1150(10) 0.023(4) Uiso 0.514(8) 1 d PDU A 2 H63' H 0.2721 -0.0475 0.1039 0.027 Uiso 0.514(8) 1 calc PR A 2 C64' C 0.3472(9) 0.003(2) 0.1873(10) 0.023(4) Uiso 0.514(8) 1 d PDU A 2 H64' H 0.3117 -0.0056 0.2264 0.027 Uiso 0.514(8) 1 calc PR A 2 C65' C 0.4238(8) 0.040(2) 0.2059(8) 0.015(3) Uiso 0.514(8) 1 d PDU A 2 C66' C 0.4459(9) 0.0647(17) 0.2838(8) 0.017(4) Uiso 0.514(8) 1 d PDU A 2 O60' O 0.3891(7) 0.0432(14) 0.3334(8) 0.026(3) Uiso 0.514(8) 1 d PDU A 2 C67' C 0.4272(11) 0.0617(16) 0.4085(9) 0.031(4) Uiso 0.514(8) 1 d PDU A 2 H67C H 0.4452 -0.0070 0.4320 0.037 Uiso 0.514(8) 1 calc PR A 2 H67D H 0.3909 0.0973 0.4424 0.037 Uiso 0.514(8) 1 calc PR A 2 C68' C 0.4963(10) 0.1344(13) 0.3940(9) 0.029(4) Uiso 0.514(8) 1 d PDU A 2 H68' H 0.5428 0.1134 0.4278 0.035 Uiso 0.514(8) 1 calc PR A 2 N6' N 0.5102(8) 0.1073(15) 0.3126(8) 0.025(4) Uiso 0.514(8) 1 d PDU A 2 C60A C 0.4796(11) 0.2543(14) 0.4023(10) 0.039(6) Uiso 0.514(8) 1 d PDU A 2 H60G H 0.5213 0.2939 0.3763 0.047 Uiso 0.514(8) 1 calc PR A 2 C60B C 0.4013(11) 0.2864(17) 0.3630(11) 0.023(6) Uiso 0.514(8) 1 d PDU A 2 H60H H 0.3929 0.3638 0.3697 0.035 Uiso 0.514(8) 1 calc PR A 2 H60I H 0.3590 0.2464 0.3855 0.035 Uiso 0.514(8) 1 calc PR A 2 H60J H 0.4016 0.2697 0.3087 0.035 Uiso 0.514(8) 1 calc PR A 2 C60C C 0.4879(16) 0.285(2) 0.4864(11) 0.057(8) Uiso 0.514(8) 1 d PDU A 2 H60K H 0.4771 0.3619 0.4920 0.086 Uiso 0.514(8) 1 calc PR A 2 H60L H 0.5413 0.2694 0.5065 0.086 Uiso 0.514(8) 1 calc PR A 2 H60M H 0.4506 0.2432 0.5146 0.086 Uiso 0.514(8) 1 calc PR A 2 C1S C 0.784(3) -0.087(3) 0.777(3) 0.095(12) Uiso 0.466(15) 1 d PDU B 1 H1S1 H 0.8333 -0.1174 0.7977 0.142 Uiso 0.466(15) 1 calc PR B 1 H1S2 H 0.7663 -0.1266 0.7308 0.142 Uiso 0.466(15) 1 calc PR B 1 H1S3 H 0.7440 -0.0935 0.8145 0.142 Uiso 0.466(15) 1 calc PR B 1 C2S C 0.795(2) 0.031(3) 0.758(3) 0.108(7) Uiso 0.466(15) 1 d PDU B 1 H2S1 H 0.8317 0.0604 0.7981 0.129 Uiso 0.466(15) 1 calc PR B 1 H2S2 H 0.8238 0.0322 0.7103 0.129 Uiso 0.466(15) 1 calc PR B 1 C3S C 0.730(2) 0.113(3) 0.746(3) 0.110(7) Uiso 0.466(15) 1 d PDU B 1 H3S1 H 0.7186 0.1392 0.7975 0.132 Uiso 0.466(15) 1 calc PR B 1 H3S2 H 0.6831 0.0730 0.7267 0.132 Uiso 0.466(15) 1 calc PR B 1 C4S C 0.735(2) 0.213(3) 0.697(3) 0.106(7) Uiso 0.466(15) 1 d PDU B 1 H4S1 H 0.6808 0.2428 0.6937 0.128 Uiso 0.466(15) 1 calc PR B 1 H4S2 H 0.7431 0.1850 0.6451 0.128 Uiso 0.466(15) 1 calc PR B 1 C5S C 0.788(2) 0.311(3) 0.705(2) 0.096(11) Uiso 0.466(15) 1 d PDU B 1 H5S1 H 0.7559 0.3757 0.7109 0.144 Uiso 0.466(15) 1 calc PR B 1 H5S2 H 0.8184 0.3179 0.6605 0.144 Uiso 0.466(15) 1 calc PR B 1 H5S3 H 0.8232 0.3021 0.7507 0.144 Uiso 0.466(15) 1 calc PR B 1 C1S' C 0.765(3) -0.067(3) 0.794(3) 0.092(10) Uiso 0.534(15) 1 d PDU B 2 H1S4 H 0.7299 -0.1292 0.7904 0.138 Uiso 0.534(15) 1 calc PR B 2 H1S5 H 0.7716 -0.0441 0.8476 0.138 Uiso 0.534(15) 1 calc PR B 2 H1S6 H 0.8157 -0.0856 0.7755 0.138 Uiso 0.534(15) 1 calc PR B 2 C2S' C 0.7286(19) 0.026(3) 0.747(2) 0.107(7) Uiso 0.534(15) 1 d PDU B 2 H2S3 H 0.7079 -0.0048 0.6978 0.129 Uiso 0.534(15) 1 calc PR B 2 H2S4 H 0.6831 0.0531 0.7732 0.129 Uiso 0.534(15) 1 calc PR B 2 C3S' C 0.7788(18) 0.123(3) 0.728(2) 0.110(7) Uiso 0.534(15) 1 d PDU B 2 H3S3 H 0.8209 0.1281 0.7692 0.133 Uiso 0.534(15) 1 calc PR B 2 H3S4 H 0.8044 0.1059 0.6809 0.133 Uiso 0.534(15) 1 calc PR B 2 C4S' C 0.7432(19) 0.235(3) 0.719(3) 0.107(7) Uiso 0.534(15) 1 d PDU B 2 H4S3 H 0.7440 0.2666 0.7702 0.128 Uiso 0.534(15) 1 calc PR B 2 H4S4 H 0.7807 0.2771 0.6900 0.128 Uiso 0.534(15) 1 calc PR B 2 C5S' C 0.663(2) 0.258(3) 0.682(2) 0.115(11) Uiso 0.534(15) 1 d PDU B 2 H5S4 H 0.6651 0.3237 0.6510 0.172 Uiso 0.534(15) 1 calc PR B 2 H5S5 H 0.6256 0.2693 0.7216 0.172 Uiso 0.534(15) 1 calc PR B 2 H5S6 H 0.6455 0.1977 0.6497 0.172 Uiso 0.534(15) 1 calc PR B 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Y1 0.0138(7) 0.0174(7) 0.0442(8) -0.0146(7) 0.0052(6) -0.0067(7) Y2 0.0217(9) 0.0317(10) 0.0967(14) -0.0470(9) 0.0248(9) -0.0142(7) _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 Y1 O2 2.173(7) . ? Y1 O1 2.176(7) . ? Y1 O4 2.273(8) . ? Y1 O3 2.374(8) . ? Y1 N2 2.460(9) . ? Y1 N1 2.510(9) . ? Y1 N3 2.580(10) . ? Y1 Y2 3.8427(17) . ? Y2 O6 1.964(13) . ? Y2 O5 2.145(10) . ? Y2 O3 2.257(8) . ? Y2 O4 2.367(9) . ? Y2 O6' 2.386(13) . ? Y2 N6' 2.422(13) . ? Y2 N4 2.468(9) . ? Y2 N5 2.491(10) . ? Y2 N6 2.607(14) . ? O1 C10 1.330(10) . ? C10 C11 1.394(11) . ? C10 C15 1.408(11) . ? C11 C12 1.374(12) . ? C12 C13 1.393(12) . ? C13 C14 1.349(11) . ? C14 C15 1.412(11) . ? C15 C16 1.421(11) . ? C16 N1 1.298(10) . ? C16 O10 1.380(10) . ? O10 C17 1.447(11) . ? C17 C18 1.519(12) . ? C18 N1 1.495(11) . ? C18 C100 1.532(12) . ? C100 C101 1.512(12) . ? C100 C102 1.537(12) . ? O2 C20 1.320(10) . ? C20 C25 1.409(11) . ? C20 C21 1.409(11) . ? C21 C22 1.373(12) . ? C22 C23 1.400(12) . ? C23 C24 1.353(12) . ? C24 C25 1.404(11) . ? C25 C26 1.431(11) . ? C26 N2 1.288(10) . ? C26 O20 1.354(10) . ? O20 C27 1.445(11) . ? C27 C28 1.511(12) . ? C28 N2 1.508(11) . ? C28 C200 1.514(13) . ? C200 C201 1.530(13) . ? C200 C202 1.545(12) . ? O3 C30 1.300(10) . ? C30 C35 1.403(11) . ? C30 C31 1.409(11) . ? C31 C32 1.363(12) . ? C32 C33 1.393(13) . ? C33 C34 1.363(12) . ? C34 C35 1.395(12) . ? C35 C36 1.451(11) . ? C36 N3 1.271(11) . ? C36 O30 1.372(11) . ? O30 C37 1.463(11) . ? C37 C38 1.505(13) . ? C38 C300 1.503(12) . ? C38 N3 1.524(11) . ? C300 C302 1.513(12) . ? C300 C301 1.544(12) . ? O4 C40 1.320(10) . ? C40 C41 1.412(12) . ? C40 C45 1.418(11) . ? C41 C42 1.365(12) . ? C42 C43 1.399(13) . ? C43 C44 1.372(12) . ? C44 C45 1.391(11) . ? C45 C46 1.449(11) . ? C46 N4 1.261(11) . ? C46 O40 1.373(11) . ? O40 C47 1.457(10) . ? C47 C48 1.516(12) . ? C48 N4 1.499(11) . ? C48 C400 1.539(11) . ? C400 C401 1.532(11) . ? C400 C402 1.542(11) . ? O5 C50 1.334(11) . ? C50 C51 1.398(12) . ? C50 C55 1.414(12) . ? C51 C52 1.379(13) . ? C52 C53 1.397(13) . ? C53 C54 1.339(12) . ? C54 C55 1.418(12) . ? C55 C56 1.413(11) . ? C56 N5 1.307(11) . ? C56 O50 1.360(11) . ? O50 C57 1.461(11) . ? C57 C58 1.523(13) . ? C58 N5 1.472(12) . ? C58 C500 1.527(13) . ? C500 C502 1.526(13) . ? C500 C501 1.537(13) . ? O6 C60 1.317(12) . ? C60 C61 1.399(13) . ? C60 C65 1.410(13) . ? C61 C62 1.370(14) . ? C62 C63 1.397(14) . ? C63 C64 1.361(14) . ? C64 C65 1.407(13) . ? C65 C66 1.431(13) . ? C66 N6 1.283(13) . ? C66 O60 1.374(13) . ? O60 C67 1.438(13) . ? C67 C68 1.512(15) . ? C68 N6 1.497(14) . ? C68 C600 1.512(14) . ? C600 C602 1.537(14) . ? C600 C601 1.542(14) . ? O6' C60' 1.319(12) . ? C60' C65' 1.400(13) . ? C60' C61' 1.406(14) . ? C61' C62' 1.377(14) . ? C62' C63' 1.397(14) . ? C63' C64' 1.347(14) . ? C64' C65' 1.411(13) . ? C65' C66' 1.435(13) . ? C66' N6' 1.298(13) . ? C66' O60' 1.371(13) . ? O60' C67' 1.459(14) . ? C67' C68' 1.521(14) . ? C68' N6' 1.506(13) . ? C68' C60A 1.526(15) . ? C60A C60B 1.525(14) . ? C60A C60C 1.529(14) . ? C1S C2S 1.524(18) . ? C2S C3S 1.515(18) . ? C3S C4S 1.521(18) . ? C4S C5S 1.521(19) . ? C1S' C2S' 1.532(18) . ? C2S' C3S' 1.523(18) . ? C3S' C4S' 1.521(17) . ? C4S' C5S' 1.515(19) . ? 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 Y1 O1 144.8(3) . . ? O2 Y1 O4 89.0(3) . . ? O1 Y1 O4 114.5(3) . . ? O2 Y1 O3 140.6(3) . . ? O1 Y1 O3 74.5(3) . . ? O4 Y1 O3 67.8(3) . . ? O2 Y1 N2 73.5(3) . . ? O1 Y1 N2 80.0(3) . . ? O4 Y1 N2 162.3(3) . . ? O3 Y1 N2 128.3(3) . . ? O2 Y1 N1 79.7(3) . . ? O1 Y1 N1 72.2(3) . . ? O4 Y1 N1 96.4(3) . . ? O3 Y1 N1 132.2(3) . . ? N2 Y1 N1 77.8(3) . . ? O2 Y1 N3 84.1(3) . . ? O1 Y1 N3 117.7(3) . . ? O4 Y1 N3 94.3(4) . . ? O3 Y1 N3 67.3(3) . . ? N2 Y1 N3 87.1(4) . . ? N1 Y1 N3 160.4(3) . . ? O2 Y1 Y2 117.1(2) . . ? O1 Y1 Y2 95.5(2) . . ? O4 Y1 Y2 34.9(2) . . ? O3 Y1 Y2 32.95(19) . . ? N2 Y1 Y2 159.9(2) . . ? N1 Y1 Y2 119.7(2) . . ? N3 Y1 Y2 77.6(2) . . ? O6 Y2 O5 143.5(5) . . ? O6 Y2 O3 91.4(5) . . ? O5 Y2 O3 115.6(3) . . ? O6 Y2 O4 137.1(5) . . ? O5 Y2 O4 78.3(4) . . ? O3 Y2 O4 68.2(3) . . ? O6 Y2 O6' 11.4(5) . . ? O5 Y2 O6' 145.2(4) . . ? O3 Y2 O6' 81.9(4) . . ? O4 Y2 O6' 136.2(4) . . ? O6 Y2 N6' 61.9(5) . . ? O5 Y2 N6' 85.8(4) . . ? O3 Y2 N6' 151.7(4) . . ? O4 Y2 N6' 137.8(5) . . ? O6' Y2 N6' 70.5(4) . . ? O6 Y2 N4 80.2(5) . . ? O5 Y2 N4 113.2(3) . . ? O3 Y2 N4 104.6(3) . . ? O4 Y2 N4 70.0(3) . . ? O6' Y2 N4 88.6(4) . . ? N6' Y2 N4 81.4(5) . . ? O6 Y2 N5 87.7(5) . . ? O5 Y2 N5 72.3(3) . . ? O3 Y2 N5 83.8(4) . . ? O4 Y2 N5 124.6(4) . . ? O6' Y2 N5 80.6(4) . . ? N6' Y2 N5 85.6(5) . . ? N4 Y2 N5 165.3(4) . . ? O6 Y2 N6 73.6(5) . . ? O5 Y2 N6 81.2(4) . . ? O3 Y2 N6 163.2(4) . . ? O4 Y2 N6 117.9(5) . . ? O6' Y2 N6 83.9(4) . . ? N6' Y2 N6 20.0(5) . . ? N4 Y2 N6 66.0(5) . . ? N5 Y2 N6 102.6(6) . . ? O6 Y2 Y1 118.7(4) . . ? O5 Y2 Y1 96.4(3) . . ? O3 Y2 Y1 34.9(2) . . ? O4 Y2 Y1 33.32(19) . . ? O6' Y2 Y1 111.9(3) . . ? N6' Y2 Y1 168.7(5) . . ? N4 Y2 Y1 87.6(2) . . ? N5 Y2 Y1 105.7(3) . . ? N6 Y2 Y1 149.4(4) . . ? C10 O1 Y1 146.1(6) . . ? O1 C10 C11 119.6(9) . . ? O1 C10 C15 120.2(8) . . ? C11 C10 C15 120.2(9) . . ? C12 C11 C10 120.4(10) . . ? C11 C12 C13 119.3(10) . . ? C14 C13 C12 121.2(11) . . ? C13 C14 C15 120.9(10) . . ? C10 C15 C14 117.7(8) . . ? C10 C15 C16 121.3(9) . . ? C14 C15 C16 121.1(9) . . ? N1 C16 O10 115.1(8) . . ? N1 C16 C15 130.1(9) . . ? O10 C16 C15 114.5(8) . . ? C16 O10 C17 106.0(8) . . ? O10 C17 C18 104.4(8) . . ? N1 C18 C17 103.1(8) . . ? N1 C18 C100 111.0(9) . . ? C17 C18 C100 115.1(10) . . ? C16 N1 C18 107.6(8) . . ? C16 N1 Y1 126.9(7) . . ? C18 N1 Y1 124.1(6) . . ? C101 C100 C18 113.4(10) . . ? C101 C100 C102 113.6(11) . . ? C18 C100 C102 109.9(9) . . ? C20 O2 Y1 143.6(7) . . ? O2 C20 C25 122.6(9) . . ? O2 C20 C21 119.2(9) . . ? C25 C20 C21 118.2(9) . . ? C22 C21 C20 121.1(11) . . ? C21 C22 C23 120.3(11) . . ? C24 C23 C22 119.2(12) . . ? C23 C24 C25 122.3(11) . . ? C24 C25 C20 118.8(9) . . ? C24 C25 C26 120.0(9) . . ? C20 C25 C26 121.2(9) . . ? N2 C26 O20 117.2(8) . . ? N2 C26 C25 128.7(9) . . ? O20 C26 C25 114.1(8) . . ? C26 O20 C27 106.8(7) . . ? O20 C27 C28 105.6(9) . . ? N2 C28 C27 103.6(8) . . ? N2 C28 C200 112.4(10) . . ? C27 C28 C200 115.3(10) . . ? C26 N2 C28 106.8(8) . . ? C26 N2 Y1 128.5(6) . . ? C28 N2 Y1 121.9(6) . . ? C28 C200 C201 111.7(11) . . ? C28 C200 C202 109.0(11) . . ? C201 C200 C202 111.5(13) . . ? C30 O3 Y2 132.3(8) . . ? C30 O3 Y1 115.1(8) . . ? Y2 O3 Y1 112.1(3) . . ? O3 C30 C35 120.9(9) . . ? O3 C30 C31 122.1(10) . . ? C35 C30 C31 117.0(9) . . ? C32 C31 C30 121.4(11) . . ? C31 C32 C33 120.9(12) . . ? C34 C33 C32 119.1(12) . . ? C33 C34 C35 120.8(11) . . ? C34 C35 C30 120.7(9) . . ? C34 C35 C36 122.1(10) . . ? C30 C35 C36 117.1(9) . . ? N3 C36 O30 116.7(9) . . ? N3 C36 C35 128.8(10) . . ? O30 C36 C35 114.3(10) . . ? C36 O30 C37 106.4(8) . . ? O30 C37 C38 105.1(9) . . ? C300 C38 C37 115.9(10) . . ? C300 C38 N3 113.6(9) . . ? C37 C38 N3 103.1(8) . . ? C36 N3 C38 107.2(9) . . ? C36 N3 Y1 118.9(7) . . ? C38 N3 Y1 131.9(7) . . ? C38 C300 C302 112.1(11) . . ? C38 C300 C301 110.9(10) . . ? C302 C300 C301 109.5(12) . . ? C40 O4 Y1 132.9(8) . . ? C40 O4 Y2 115.2(8) . . ? Y1 O4 Y2 111.8(3) . . ? O4 C40 C41 120.1(9) . . ? O4 C40 C45 121.5(9) . . ? C41 C40 C45 118.4(9) . . ? C42 C41 C40 119.8(11) . . ? C41 C42 C43 122.3(12) . . ? C44 C43 C42 117.8(11) . . ? C43 C44 C45 122.0(11) . . ? C44 C45 C40 119.3(9) . . ? C44 C45 C46 119.9(9) . . ? C40 C45 C46 120.6(9) . . ? N4 C46 O40 117.7(9) . . ? N4 C46 C45 126.6(10) . . ? O40 C46 C45 115.6(9) . . ? C46 O40 C47 105.1(7) . . ? O40 C47 C48 105.4(8) . . ? N4 C48 C47 103.0(8) . . ? N4 C48 C400 111.6(8) . . ? C47 C48 C400 117.0(9) . . ? C46 N4 C48 107.7(9) . . ? C46 N4 Y2 123.7(7) . . ? C48 N4 Y2 127.7(7) . . ? C401 C400 C48 110.2(9) . . ? C401 C400 C402 112.3(10) . . ? C48 C400 C402 109.4(9) . . ? C50 O5 Y2 146.4(8) . . ? O5 C50 C51 120.8(11) . . ? O5 C50 C55 120.5(10) . . ? C51 C50 C55 118.5(10) . . ? C52 C51 C50 121.1(12) . . ? C51 C52 C53 120.3(12) . . ? C54 C53 C52 119.5(12) . . ? C53 C54 C55 122.3(11) . . ? C56 C55 C50 121.6(10) . . ? C56 C55 C54 120.2(10) . . ? C50 C55 C54 118.2(10) . . ? N5 C56 O50 113.8(9) . . ? N5 C56 C55 130.1(10) . . ? O50 C56 C55 116.1(9) . . ? C56 O50 C57 107.6(8) . . ? O50 C57 C58 101.7(9) . . ? N5 C58 C57 103.0(9) . . ? N5 C58 C500 111.4(11) . . ? C57 C58 C500 113.6(12) . . ? C56 N5 C58 107.6(10) . . ? C56 N5 Y2 127.2(8) . . ? C58 N5 Y2 125.0(8) . . ? C502 C500 C58 109.8(13) . . ? C502 C500 C501 112.7(14) . . ? C58 C500 C501 113.6(13) . . ? C60 O6 Y2 151.5(11) . . ? O6 C60 C61 120.6(13) . . ? O6 C60 C65 119.9(12) . . ? C61 C60 C65 119.3(12) . . ? C62 C61 C60 120.7(14) . . ? C61 C62 C63 119.8(15) . . ? C64 C63 C62 120.1(15) . . ? C63 C64 C65 121.2(14) . . ? C64 C65 C60 118.3(12) . . ? C64 C65 C66 119.8(12) . . ? C60 C65 C66 121.9(11) . . ? N6 C66 O60 116.2(11) . . ? N6 C66 C65 131.7(13) . . ? O60 C66 C65 111.6(12) . . ? C66 O60 C67 106.3(11) . . ? O60 C67 C68 105.0(11) . . ? N6 C68 C67 103.1(11) . . ? N6 C68 C600 117.2(14) . . ? C67 C68 C600 115.2(14) . . ? C66 N6 C68 107.1(11) . . ? C66 N6 Y2 120.9(9) . . ? C68 N6 Y2 130.3(10) . . ? C68 C600 C602 111.9(15) . . ? C68 C600 C601 110.1(14) . . ? C602 C600 C601 111.6(15) . . ? C60' O6' Y2 140.9(10) . . ? O6' C60' C65' 121.0(13) . . ? O6' C60' C61' 119.8(12) . . ? C65' C60' C61' 118.7(11) . . ? C62' C61' C60' 121.0(14) . . ? C61' C62' C63' 119.3(15) . . ? C64' C63' C62' 120.7(15) . . ? C63' C64' C65' 121.0(14) . . ? C60' C65' C64' 119.1(12) . . ? C60' C65' C66' 122.2(11) . . ? C64' C65' C66' 118.7(12) . . ? N6' C66' O60' 116.4(11) . . ? N6' C66' C65' 129.1(12) . . ? O60' C66' C65' 114.4(11) . . ? C66' O60' C67' 104.7(10) . . ? O60' C67' C68' 104.5(11) . . ? N6' C68' C67' 101.3(10) . . ? N6' C68' C60A 110.5(13) . . ? C67' C68' C60A 114.3(14) . . ? C66' N6' C68' 106.7(11) . . ? C66' N6' Y2 130.2(10) . . ? C68' N6' Y2 120.7(9) . . ? C60B C60A C68' 112.1(13) . . ? C60B C60A C60C 113.9(15) . . ? C68' C60A C60C 109.2(14) . . ? C3S C2S C1S 125(3) . . ? C2S C3S C4S 124(3) . . ? C3S C4S C5S 130(3) . . ? C3S' C2S' C1S' 120(2) . . ? C4S' C3S' C2S' 121(2) . . ? C5S' C4S' C3S' 125(2) . . ? 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 Y1 Y2 O6 -173.5(7) . . . . ? O1 Y1 Y2 O6 -7.3(6) . . . . ? O4 Y1 Y2 O6 -133.5(7) . . . . ? O3 Y1 Y2 O6 42.8(7) . . . . ? N2 Y1 Y2 O6 68.5(9) . . . . ? N1 Y1 Y2 O6 -79.9(6) . . . . ? N3 Y1 Y2 O6 109.9(6) . . . . ? O2 Y1 Y2 O5 17.1(4) . . . . ? O1 Y1 Y2 O5 -176.8(4) . . . . ? O4 Y1 Y2 O5 57.0(5) . . . . ? O3 Y1 Y2 O5 -126.7(5) . . . . ? N2 Y1 Y2 O5 -101.0(7) . . . . ? N1 Y1 Y2 O5 110.6(3) . . . . ? N3 Y1 Y2 O5 -59.6(3) . . . . ? O2 Y1 Y2 O3 143.8(5) . . . . ? O1 Y1 Y2 O3 -50.1(5) . . . . ? O4 Y1 Y2 O3 -176.3(7) . . . . ? N2 Y1 Y2 O3 25.7(8) . . . . ? N1 Y1 Y2 O3 -122.7(5) . . . . ? N3 Y1 Y2 O3 67.1(5) . . . . ? O2 Y1 Y2 O4 -40.0(5) . . . . ? O1 Y1 Y2 O4 126.1(5) . . . . ? O3 Y1 Y2 O4 176.3(7) . . . . ? N2 Y1 Y2 O4 -158.0(8) . . . . ? N1 Y1 Y2 O4 53.6(5) . . . . ? N3 Y1 Y2 O4 -116.6(5) . . . . ? O2 Y1 Y2 O6' 176.4(5) . . . . ? O1 Y1 Y2 O6' -17.5(4) . . . . ? O4 Y1 Y2 O6' -143.6(6) . . . . ? O3 Y1 Y2 O6' 32.7(5) . . . . ? N2 Y1 Y2 O6' 58.4(8) . . . . ? N1 Y1 Y2 O6' -90.0(4) . . . . ? N3 Y1 Y2 O6' 99.8(4) . . . . ? O2 Y1 Y2 N6' -83.5(16) . . . . ? O1 Y1 Y2 N6' 82.6(16) . . . . ? O4 Y1 Y2 N6' -43.5(17) . . . . ? O3 Y1 Y2 N6' 132.8(17) . . . . ? N2 Y1 Y2 N6' 158.5(17) . . . . ? N1 Y1 Y2 N6' 10.0(16) . . . . ? N3 Y1 Y2 N6' -160.2(16) . . . . ? O2 Y1 Y2 N4 -96.1(3) . . . . ? O1 Y1 Y2 N4 70.1(3) . . . . ? O4 Y1 Y2 N4 -56.1(5) . . . . ? O3 Y1 Y2 N4 120.2(5) . . . . ? N2 Y1 Y2 N4 145.9(7) . . . . ? N1 Y1 Y2 N4 -2.5(3) . . . . ? N3 Y1 Y2 N4 -172.7(3) . . . . ? O2 Y1 Y2 N5 90.4(4) . . . . ? O1 Y1 Y2 N5 -103.5(3) . . . . ? O4 Y1 Y2 N5 130.4(5) . . . . ? O3 Y1 Y2 N5 -53.3(5) . . . . ? N2 Y1 Y2 N5 -27.6(7) . . . . ? N1 Y1 Y2 N5 -176.1(3) . . . . ? N3 Y1 Y2 N5 13.8(3) . . . . ? O2 Y1 Y2 N6 -66.5(7) . . . . ? O1 Y1 Y2 N6 99.6(7) . . . . ? O4 Y1 Y2 N6 -26.5(8) . . . . ? O3 Y1 Y2 N6 149.8(8) . . . . ? N2 Y1 Y2 N6 175.5(10) . . . . ? N1 Y1 Y2 N6 27.0(7) . . . . ? N3 Y1 Y2 N6 -143.1(7) . . . . ? O2 Y1 O1 C10 52.6(15) . . . . ? O4 Y1 O1 C10 -75.2(14) . . . . ? O3 Y1 O1 C10 -131.4(14) . . . . ? N2 Y1 O1 C10 94.1(14) . . . . ? N1 Y1 O1 C10 13.8(13) . . . . ? N3 Y1 O1 C10 175.4(13) . . . . ? Y2 Y1 O1 C10 -105.7(13) . . . . ? Y1 O1 C10 C11 166.5(9) . . . . ? Y1 O1 C10 C15 -13(2) . . . . ? O1 C10 C11 C12 -175.9(11) . . . . ? C15 C10 C11 C12 3.8(19) . . . . ? C10 C11 C12 C13 1.4(19) . . . . ? C11 C12 C13 C14 -5(2) . . . . ? C12 C13 C14 C15 4(2) . . . . ? O1 C10 C15 C14 174.6(11) . . . . ? C11 C10 C15 C14 -5.2(18) . . . . ? O1 C10 C15 C16 -6.7(18) . . . . ? C11 C10 C15 C16 173.5(11) . . . . ? C13 C14 C15 C10 1.5(18) . . . . ? C13 C14 C15 C16 -177.2(12) . . . . ? C10 C15 C16 N1 21(2) . . . . ? C14 C15 C16 N1 -160.6(13) . . . . ? C10 C15 C16 O10 -164.7(11) . . . . ? C14 C15 C16 O10 14.0(17) . . . . ? N1 C16 O10 C17 -14.2(14) . . . . ? C15 C16 O10 C17 170.4(10) . . . . ? C16 O10 C17 C18 19.2(12) . . . . ? O10 C17 C18 N1 -17.6(11) . . . . ? O10 C17 C18 C100 103.4(10) . . . . ? O10 C16 N1 C18 2.2(14) . . . . ? C15 C16 N1 C18 176.8(12) . . . . ? O10 C16 N1 Y1 168.9(7) . . . . ? C15 C16 N1 Y1 -16.6(19) . . . . ? C17 C18 N1 C16 10.0(12) . . . . ? C100 C18 N1 C16 -113.8(11) . . . . ? C17 C18 N1 Y1 -157.1(7) . . . . ? C100 C18 N1 Y1 79.1(11) . . . . ? O2 Y1 N1 C16 -156.7(10) . . . . ? O1 Y1 N1 C16 1.8(9) . . . . ? O4 Y1 N1 C16 115.5(10) . . . . ? O3 Y1 N1 C16 49.8(11) . . . . ? N2 Y1 N1 C16 -81.5(10) . . . . ? N3 Y1 N1 C16 -121.8(11) . . . . ? Y2 Y1 N1 C16 87.9(10) . . . . ? O2 Y1 N1 C18 7.9(8) . . . . ? O1 Y1 N1 C18 166.4(8) . . . . ? O4 Y1 N1 C18 -79.9(8) . . . . ? O3 Y1 N1 C18 -145.7(7) . . . . ? N2 Y1 N1 C18 83.1(8) . . . . ? N3 Y1 N1 C18 42.7(14) . . . . ? Y2 Y1 N1 C18 -107.5(7) . . . . ? N1 C18 C100 C101 59.9(13) . . . . ? C17 C18 C100 C101 -56.8(14) . . . . ? N1 C18 C100 C102 -171.8(10) . . . . ? C17 C18 C100 C102 71.6(13) . . . . ? O1 Y1 O2 C20 44.0(15) . . . . ? O4 Y1 O2 C20 178.0(13) . . . . ? O3 Y1 O2 C20 -130.0(13) . . . . ? N2 Y1 O2 C20 1.1(13) . . . . ? N1 Y1 O2 C20 81.3(13) . . . . ? N3 Y1 O2 C20 -87.6(13) . . . . ? Y2 Y1 O2 C20 -160.4(13) . . . . ? Y1 O2 C20 C25 -3(2) . . . . ? Y1 O2 C20 C21 174.9(10) . . . . ? O2 C20 C21 C22 -176.3(14) . . . . ? C25 C20 C21 C22 2(2) . . . . ? C20 C21 C22 C23 0(3) . . . . ? C21 C22 C23 C24 -2(3) . . . . ? C22 C23 C24 C25 2(3) . . . . ? C23 C24 C25 C20 0(2) . . . . ? C23 C24 C25 C26 -179.6(16) . . . . ? O2 C20 C25 C24 176.5(13) . . . . ? C21 C20 C25 C24 -1(2) . . . . ? O2 C20 C25 C26 -4(2) . . . . ? C21 C20 C25 C26 177.8(13) . . . . ? C24 C25 C26 N2 -165.0(14) . . . . ? C20 C25 C26 N2 16(2) . . . . ? C24 C25 C26 O20 13.0(19) . . . . ? C20 C25 C26 O20 -166.2(12) . . . . ? N2 C26 O20 C27 -2.7(16) . . . . ? C25 C26 O20 C27 179.1(11) . . . . ? C26 O20 C27 C28 1.9(14) . . . . ? O20 C27 C28 N2 -0.7(13) . . . . ? O20 C27 C28 C200 122.5(11) . . . . ? O20 C26 N2 C28 2.2(16) . . . . ? C25 C26 N2 C28 -179.9(13) . . . . ? O20 C26 N2 Y1 163.2(9) . . . . ? C25 C26 N2 Y1 -19(2) . . . . ? C27 C28 N2 C26 -0.8(13) . . . . ? C200 C28 N2 C26 -125.9(12) . . . . ? C27 C28 N2 Y1 -163.3(8) . . . . ? C200 C28 N2 Y1 71.6(12) . . . . ? O2 Y1 N2 C26 9.0(11) . . . . ? O1 Y1 N2 C26 -147.5(12) . . . . ? O4 Y1 N2 C26 -1(2) . . . . ? O3 Y1 N2 C26 151.5(11) . . . . ? N1 Y1 N2 C26 -73.7(11) . . . . ? N3 Y1 N2 C26 93.7(12) . . . . ? Y2 Y1 N2 C26 134.0(9) . . . . ? O2 Y1 N2 C28 167.5(10) . . . . ? O1 Y1 N2 C28 11.1(9) . . . . ? O4 Y1 N2 C28 157.2(11) . . . . ? O3 Y1 N2 C28 -50.0(10) . . . . ? N1 Y1 N2 C28 84.8(9) . . . . ? N3 Y1 N2 C28 -107.8(9) . . . . ? Y2 Y1 N2 C28 -67.5(13) . . . . ? N2 C28 C200 C201 60.9(15) . . . . ? C27 C28 C200 C201 -57.5(15) . . . . ? N2 C28 C200 C202 -175.5(11) . . . . ? C27 C28 C200 C202 66.1(15) . . . . ? O6 Y2 O3 C30 44.9(11) . . . . ? O5 Y2 O3 C30 -109.6(10) . . . . ? O4 Y2 O3 C30 -173.9(10) . . . . ? O6' Y2 O3 C30 38.7(10) . . . . ? N6' Y2 O3 C30 26.0(16) . . . . ? N4 Y2 O3 C30 125.1(10) . . . . ? N5 Y2 O3 C30 -42.6(10) . . . . ? N6 Y2 O3 C30 71(2) . . . . ? Y1 Y2 O3 C30 -171.7(12) . . . . ? O6 Y2 O3 Y1 -143.4(6) . . . . ? O5 Y2 O3 Y1 62.1(5) . . . . ? O4 Y2 O3 Y1 -2.2(4) . . . . ? O6' Y2 O3 Y1 -149.6(5) . . . . ? N6' Y2 O3 Y1 -162.3(9) . . . . ? N4 Y2 O3 Y1 -63.2(4) . . . . ? N5 Y2 O3 Y1 129.0(4) . . . . ? N6 Y2 O3 Y1 -117.2(17) . . . . ? O2 Y1 O3 C30 117.2(8) . . . . ? O1 Y1 O3 C30 -59.2(8) . . . . ? O4 Y1 O3 C30 175.5(8) . . . . ? N2 Y1 O3 C30 4.1(10) . . . . ? N1 Y1 O3 C30 -106.4(8) . . . . ? N3 Y1 O3 C30 70.5(8) . . . . ? Y2 Y1 O3 C30 173.2(10) . . . . ? O2 Y1 O3 Y2 -56.0(6) . . . . ? O1 Y1 O3 Y2 127.6(4) . . . . ? O4 Y1 O3 Y2 2.3(5) . . . . ? N2 Y1 O3 Y2 -169.1(4) . . . . ? N1 Y1 O3 Y2 80.4(5) . . . . ? N3 Y1 O3 Y2 -102.7(4) . . . . ? Y2 O3 C30 C35 106.8(13) . . . . ? Y1 O3 C30 C35 -64.7(15) . . . . ? Y2 O3 C30 C31 -73.2(17) . . . . ? Y1 O3 C30 C31 115.3(13) . . . . ? O3 C30 C31 C32 -179.4(13) . . . . ? C35 C30 C31 C32 1(2) . . . . ? C30 C31 C32 C33 -1(2) . . . . ? C31 C32 C33 C34 -1(2) . . . . ? C32 C33 C34 C35 4(2) . . . . ? C33 C34 C35 C30 -5(2) . . . . ? C33 C34 C35 C36 -179.2(14) . . . . ? O3 C30 C35 C34 -177.8(13) . . . . ? C31 C30 C35 C34 2(2) . . . . ? O3 C30 C35 C36 -3(2) . . . . ? C31 C30 C35 C36 177.0(13) . . . . ? C34 C35 C36 N3 -148.2(15) . . . . ? C30 C35 C36 N3 37(2) . . . . ? C34 C35 C36 O30 38(2) . . . . ? C30 C35 C36 O30 -136.7(13) . . . . ? N3 C36 O30 C37 -1.1(17) . . . . ? C35 C36 O30 C37 173.5(11) . . . . ? C36 O30 C37 C38 -7.1(14) . . . . ? O30 C37 C38 C300 136.1(10) . . . . ? O30 C37 C38 N3 11.3(13) . . . . ? O30 C36 N3 C38 8.8(16) . . . . ? C35 C36 N3 C38 -165.0(14) . . . . ? O30 C36 N3 Y1 174.7(9) . . . . ? C35 C36 N3 Y1 1(2) . . . . ? C300 C38 N3 C36 -138.5(12) . . . . ? C37 C38 N3 C36 -12.3(13) . . . . ? C300 C38 N3 Y1 58.1(14) . . . . ? C37 C38 N3 Y1 -175.7(8) . . . . ? O2 Y1 N3 C36 167.5(10) . . . . ? O1 Y1 N3 C36 16.7(11) . . . . ? O4 Y1 N3 C36 -103.9(10) . . . . ? O3 Y1 N3 C36 -40.1(10) . . . . ? N2 Y1 N3 C36 93.8(10) . . . . ? N1 Y1 N3 C36 133.1(11) . . . . ? Y2 Y1 N3 C36 -73.0(10) . . . . ? O2 Y1 N3 C38 -30.6(10) . . . . ? O1 Y1 N3 C38 178.6(9) . . . . ? O4 Y1 N3 C38 58.0(10) . . . . ? O3 Y1 N3 C38 121.7(10) . . . . ? N2 Y1 N3 C38 -104.3(10) . . . . ? N1 Y1 N3 C38 -65.0(14) . . . . ? Y2 Y1 N3 C38 88.8(10) . . . . ? C37 C38 C300 C302 -59.2(15) . . . . ? N3 C38 C300 C302 59.9(15) . . . . ? C37 C38 C300 C301 63.6(15) . . . . ? N3 C38 C300 C301 -177.2(11) . . . . ? O2 Y1 O4 C40 -31.5(11) . . . . ? O1 Y1 O4 C40 121.3(10) . . . . ? O3 Y1 O4 C40 -178.8(11) . . . . ? N2 Y1 O4 C40 -22(2) . . . . ? N1 Y1 O4 C40 48.0(11) . . . . ? N3 Y1 O4 C40 -115.5(11) . . . . ? Y2 Y1 O4 C40 -176.6(14) . . . . ? O2 Y1 O4 Y2 145.1(4) . . . . ? O1 Y1 O4 Y2 -62.0(5) . . . . ? O3 Y1 O4 Y2 -2.2(4) . . . . ? N2 Y1 O4 Y2 155.0(11) . . . . ? N1 Y1 O4 Y2 -135.3(4) . . . . ? N3 Y1 O4 Y2 61.1(4) . . . . ? O6 Y2 O4 C40 -113.4(10) . . . . ? O5 Y2 O4 C40 55.7(8) . . . . ? O3 Y2 O4 C40 179.6(8) . . . . ? O6' Y2 O4 C40 -130.0(8) . . . . ? N6' Y2 O4 C40 -14.3(11) . . . . ? N4 Y2 O4 C40 -64.6(8) . . . . ? N5 Y2 O4 C40 114.2(8) . . . . ? N6 Y2 O4 C40 -17.6(10) . . . . ? Y1 Y2 O4 C40 177.3(11) . . . . ? O6 Y2 O4 Y1 69.3(8) . . . . ? O5 Y2 O4 Y1 -121.6(5) . . . . ? O3 Y2 O4 Y1 2.3(4) . . . . ? O6' Y2 O4 Y1 52.7(7) . . . . ? N6' Y2 O4 Y1 168.4(5) . . . . ? N4 Y2 O4 Y1 118.1(5) . . . . ? N5 Y2 O4 Y1 -63.0(6) . . . . ? N6 Y2 O4 Y1 165.1(5) . . . . ? Y1 O4 C40 C41 60.0(18) . . . . ? Y2 O4 C40 C41 -116.5(13) . . . . ? Y1 O4 C40 C45 -120.8(13) . . . . ? Y2 O4 C40 C45 62.6(15) . . . . ? O4 C40 C41 C42 -179.0(13) . . . . ? C45 C40 C41 C42 2(2) . . . . ? C40 C41 C42 C43 2(2) . . . . ? C41 C42 C43 C44 -5(2) . . . . ? C42 C43 C44 C45 5(2) . . . . ? C43 C44 C45 C40 -2(2) . . . . ? C43 C44 C45 C46 -176.9(14) . . . . ? O4 C40 C45 C44 179.0(13) . . . . ? C41 C40 C45 C44 -2(2) . . . . ? O4 C40 C45 C46 -6(2) . . . . ? C41 C40 C45 C46 173.3(13) . . . . ? C44 C45 C46 N4 152.0(14) . . . . ? C40 C45 C46 N4 -23(2) . . . . ? C44 C45 C46 O40 -25.0(19) . . . . ? C40 C45 C46 O40 159.9(12) . . . . ? N4 C46 O40 C47 -4.0(15) . . . . ? C45 C46 O40 C47 173.3(11) . . . . ? C46 O40 C47 C48 9.1(12) . . . . ? O40 C47 C48 N4 -10.6(11) . . . . ? O40 C47 C48 C400 112.1(10) . . . . ? O40 C46 N4 C48 -3.2(16) . . . . ? C45 C46 N4 C48 179.8(12) . . . . ? O40 C46 N4 Y2 166.7(8) . . . . ? C45 C46 N4 Y2 -10.3(19) . . . . ? C47 C48 N4 C46 8.6(13) . . . . ? C400 C48 N4 C46 -117.6(11) . . . . ? C47 C48 N4 Y2 -160.7(8) . . . . ? C400 C48 N4 Y2 73.0(12) . . . . ? O6 Y2 N4 C46 -169.8(12) . . . . ? O5 Y2 N4 C46 -25.4(12) . . . . ? O3 Y2 N4 C46 101.3(11) . . . . ? O4 Y2 N4 C46 41.5(10) . . . . ? O6' Y2 N4 C46 -177.5(11) . . . . ? N6' Y2 N4 C46 -107.0(11) . . . . ? N5 Y2 N4 C46 -134.8(14) . . . . ? N6 Y2 N4 C46 -93.5(11) . . . . ? Y1 Y2 N4 C46 70.5(10) . . . . ? O6 Y2 N4 C48 -2.0(9) . . . . ? O5 Y2 N4 C48 142.4(8) . . . . ? O3 Y2 N4 C48 -90.9(9) . . . . ? O4 Y2 N4 C48 -150.7(9) . . . . ? O6' Y2 N4 C48 -9.7(9) . . . . ? N6' Y2 N4 C48 60.8(9) . . . . ? N5 Y2 N4 C48 33.0(19) . . . . ? N6 Y2 N4 C48 74.3(9) . . . . ? Y1 Y2 N4 C48 -121.7(9) . . . . ? N4 C48 C400 C401 64.2(12) . . . . ? C47 C48 C400 C401 -53.9(13) . . . . ? N4 C48 C400 C402 -171.8(10) . . . . ? C47 C48 C400 C402 70.0(12) . . . . ? O6 Y2 O5 C50 -74(2) . . . . ? O3 Y2 O5 C50 60.0(18) . . . . ? O4 Y2 O5 C50 118.6(18) . . . . ? O6' Y2 O5 C50 -54(2) . . . . ? N6' Y2 O5 C50 -100.6(18) . . . . ? N4 Y2 O5 C50 -179.3(17) . . . . ? N5 Y2 O5 C50 -13.9(17) . . . . ? N6 Y2 O5 C50 -120.3(18) . . . . ? Y1 Y2 O5 C50 90.6(18) . . . . ? Y2 O5 C50 C51 -167.7(12) . . . . ? Y2 O5 C50 C55 9(3) . . . . ? O5 C50 C51 C52 179.5(15) . . . . ? C55 C50 C51 C52 3(2) . . . . ? C50 C51 C52 C53 -1(3) . . . . ? C51 C52 C53 C54 -2(3) . . . . ? C52 C53 C54 C55 2(2) . . . . ? O5 C50 C55 C56 4(2) . . . . ? C51 C50 C55 C56 -179.9(15) . . . . ? O5 C50 C55 C54 -179.2(13) . . . . ? C51 C50 C55 C54 -3(2) . . . . ? C53 C54 C55 C56 177.4(14) . . . . ? C53 C54 C55 C50 0(2) . . . . ? C50 C55 C56 N5 0(3) . . . . ? C54 C55 C56 N5 -176.9(15) . . . . ? C50 C55 C56 O50 -177.4(13) . . . . ? C54 C55 C56 O50 6(2) . . . . ? N5 C56 O50 C57 -8.5(16) . . . . ? C55 C56 O50 C57 169.3(12) . . . . ? C56 O50 C57 C58 20.7(14) . . . . ? O50 C57 C58 N5 -24.6(13) . . . . ? O50 C57 C58 C500 96.1(12) . . . . ? O50 C56 N5 C58 -8.6(16) . . . . ? C55 C56 N5 C58 173.9(15) . . . . ? O50 C56 N5 Y2 165.9(8) . . . . ? C55 C56 N5 Y2 -12(2) . . . . ? C57 C58 N5 C56 21.0(15) . . . . ? C500 C58 N5 C56 -101.1(14) . . . . ? C57 C58 N5 Y2 -153.6(9) . . . . ? C500 C58 N5 Y2 84.2(13) . . . . ? O6 Y2 N5 C56 162.1(13) . . . . ? O5 Y2 N5 C56 13.2(12) . . . . ? O3 Y2 N5 C56 -106.2(12) . . . . ? O4 Y2 N5 C56 -48.1(13) . . . . ? O6' Y2 N5 C56 171.1(13) . . . . ? N6' Y2 N5 C56 100.1(13) . . . . ? N4 Y2 N5 C56 127.7(15) . . . . ? N6 Y2 N5 C56 89.5(12) . . . . ? Y1 Y2 N5 C56 -78.7(12) . . . . ? O6 Y2 N5 C58 -24.3(11) . . . . ? O5 Y2 N5 C58 -173.2(11) . . . . ? O3 Y2 N5 C58 67.4(10) . . . . ? O4 Y2 N5 C58 125.5(9) . . . . ? O6' Y2 N5 C58 -15.3(10) . . . . ? N6' Y2 N5 C58 -86.3(10) . . . . ? N4 Y2 N5 C58 -58.7(19) . . . . ? N6 Y2 N5 C58 -96.9(10) . . . . ? Y1 Y2 N5 C58 94.9(10) . . . . ? N5 C58 C500 C502 -170.6(14) . . . . ? C57 C58 C500 C502 73.6(17) . . . . ? N5 C58 C500 C501 62.1(18) . . . . ? C57 C58 C500 C501 -53.7(18) . . . . ? O5 Y2 O6 C60 -39(4) . . . . ? O3 Y2 O6 C60 -178(3) . . . . ? O4 Y2 O6 C60 123(3) . . . . ? O6' Y2 O6 C60 -145(6) . . . . ? N6' Y2 O6 C60 -8(3) . . . . ? N4 Y2 O6 C60 77(3) . . . . ? N5 Y2 O6 C60 -94(3) . . . . ? N6 Y2 O6 C60 9(3) . . . . ? Y1 Y2 O6 C60 159(3) . . . . ? Y2 O6 C60 C61 169(2) . . . . ? Y2 O6 C60 C65 -7(5) . . . . ? O6 C60 C61 C62 178(3) . . . . ? C65 C60 C61 C62 -6(4) . . . . ? C60 C61 C62 C63 9(4) . . . . ? C61 C62 C63 C64 -8(4) . . . . ? C62 C63 C64 C65 4(4) . . . . ? C63 C64 C65 C60 -1(4) . . . . ? C63 C64 C65 C66 -180(3) . . . . ? O6 C60 C65 C64 178(3) . . . . ? C61 C60 C65 C64 2(4) . . . . ? O6 C60 C65 C66 -4(4) . . . . ? C61 C60 C65 C66 -179(3) . . . . ? C64 C65 C66 N6 -178(3) . . . . ? C60 C65 C66 N6 4(5) . . . . ? C64 C65 C66 O60 11(4) . . . . ? C60 C65 C66 O60 -168(3) . . . . ? N6 C66 O60 C67 4(3) . . . . ? C65 C66 O60 C67 177(2) . . . . ? C66 O60 C67 C68 -12(2) . . . . ? O60 C67 C68 N6 15(2) . . . . ? O60 C67 C68 C600 144.2(16) . . . . ? O60 C66 N6 C68 6(3) . . . . ? C65 C66 N6 C68 -165(3) . . . . ? O60 C66 N6 Y2 172.8(16) . . . . ? C65 C66 N6 Y2 2(4) . . . . ? C67 C68 N6 C66 -13(2) . . . . ? C600 C68 N6 C66 -141(2) . . . . ? C67 C68 N6 Y2 -178.1(15) . . . . ? C600 C68 N6 Y2 54(2) . . . . ? O6 Y2 N6 C66 -5(2) . . . . ? O5 Y2 N6 C66 148(2) . . . . ? O3 Y2 N6 C66 -33(3) . . . . ? O4 Y2 N6 C66 -140.4(19) . . . . ? O6' Y2 N6 C66 -1(2) . . . . ? N6' Y2 N6 C66 46.0(19) . . . . ? N4 Y2 N6 C66 -92(2) . . . . ? N5 Y2 N6 C66 78(2) . . . . ? Y1 Y2 N6 C66 -124.3(18) . . . . ? O6 Y2 N6 C68 157.8(19) . . . . ? O5 Y2 N6 C68 -48.9(17) . . . . ? O3 Y2 N6 C68 130.3(16) . . . . ? O4 Y2 N6 C68 22.7(19) . . . . ? O6' Y2 N6 C68 162.6(18) . . . . ? N6' Y2 N6 C68 -151(3) . . . . ? N4 Y2 N6 C68 71.5(17) . . . . ? N5 Y2 N6 C68 -118.4(17) . . . . ? Y1 Y2 N6 C68 39(2) . . . . ? N6 C68 C600 C602 59(2) . . . . ? C67 C68 C600 C602 -62(2) . . . . ? N6 C68 C600 C601 -176.0(17) . . . . ? C67 C68 C600 C601 62(2) . . . . ? O6 Y2 O6' C60' 22(3) . . . . ? O5 Y2 O6' C60' -67(2) . . . . ? O3 Y2 O6' C60' 169(2) . . . . ? O4 Y2 O6' C60' 123(2) . . . . ? N6' Y2 O6' C60' -17(2) . . . . ? N4 Y2 O6' C60' 64(2) . . . . ? N5 Y2 O6' C60' -106(2) . . . . ? N6 Y2 O6' C60' -2(2) . . . . ? Y1 Y2 O6' C60' 151(2) . . . . ? Y2 O6' C60' C65' 6(4) . . . . ? Y2 O6' C60' C61' -165.2(17) . . . . ? O6' C60' C61' C62' 176(2) . . . . ? C65' C60' C61' C62' 5(4) . . . . ? C60' C61' C62' C63' -6(4) . . . . ? C61' C62' C63' C64' 4(4) . . . . ? C62' C63' C64' C65' -1(4) . . . . ? O6' C60' C65' C64' -173(2) . . . . ? C61' C60' C65' C64' -2(4) . . . . ? O6' C60' C65' C66' 7(4) . . . . ? C61' C60' C65' C66' 178(2) . . . . ? C63' C64' C65' C60' 0(4) . . . . ? C63' C64' C65' C66' 180(2) . . . . ? C60' C65' C66' N6' 5(4) . . . . ? C64' C65' C66' N6' -174(2) . . . . ? C60' C65' C66' O60' -177(2) . . . . ? C64' C65' C66' O60' 3(3) . . . . ? N6' C66' O60' C67' -9(3) . . . . ? C65' C66' O60' C67' 173.6(19) . . . . ? C66' O60' C67' C68' 21(2) . . . . ? O60' C67' C68' N6' -24.8(18) . . . . ? O60' C67' C68' C60A 94.0(17) . . . . ? O60' C66' N6' C68' -8(3) . . . . ? C65' C66' N6' C68' 169(2) . . . . ? O60' C66' N6' Y2 154.0(15) . . . . ? C65' C66' N6' Y2 -29(4) . . . . ? C67' C68' N6' C66' 20(2) . . . . ? C60A C68' N6' C66' -101.3(18) . . . . ? C67' C68' N6' Y2 -143.8(13) . . . . ? C60A C68' N6' Y2 94.7(15) . . . . ? O6 Y2 N6' C66' 18.0(18) . . . . ? O5 Y2 N6' C66' -179.7(19) . . . . ? O3 Y2 N6' C66' 39(3) . . . . ? O4 Y2 N6' C66' -112.4(18) . . . . ? O6' Y2 N6' C66' 26.1(18) . . . . ? N4 Y2 N6' C66' -65.5(19) . . . . ? N5 Y2 N6' C66' 107.7(19) . . . . ? N6 Y2 N6' C66' -104(3) . . . . ? Y1 Y2 N6' C66' -78(3) . . . . ? O6 Y2 N6' C68' 177.8(15) . . . . ? O5 Y2 N6' C68' -19.9(13) . . . . ? O3 Y2 N6' C68' -160.7(10) . . . . ? O4 Y2 N6' C68' 47.4(16) . . . . ? O6' Y2 N6' C68' -174.1(14) . . . . ? N4 Y2 N6' C68' 94.4(13) . . . . ? N5 Y2 N6' C68' -92.5(13) . . . . ? N6 Y2 N6' C68' 55.9(16) . . . . ? Y1 Y2 N6' C68' 82(2) . . . . ? N6' C68' C60A C60B 68.2(18) . . . . ? C67' C68' C60A C60B -45.3(19) . . . . ? N6' C68' C60A C60C -164.7(16) . . . . ? C67' C68' C60A C60C 81.9(19) . . . . ? C1S C2S C3S C4S -153(5) . . . . ? C2S C3S C4S C5S -65(7) . . . . ? C1S' C2S' C3S' C4S' -149(4) . . . . ? C2S' C3S' C4S' C5S' -37(6) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 22.49 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.890 _refine_diff_density_min -1.018 _refine_diff_density_rms 0.120 _database_code_depnum_ccdc_archive 'CCDC 957726' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_YbiPrMePh3 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '[Yb(C13H16NO2)3]' _chemical_formula_sum 'C39 H48 N3 O6 Yb' _chemical_formula_weight 827.84 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' Yb Yb -0.3850 5.5486 '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 21 21 21' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' _cell_length_a 10.493(11) _cell_length_b 18.64(2) _cell_length_c 18.64(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3646(7) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 22577 _cell_measurement_theta_min 0.82 _cell_measurement_theta_max 28.23 _exptl_crystal_description needle _exptl_crystal_colour colourless _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.508 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1684 _exptl_absorpt_coefficient_mu 2.615 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.368667 _exptl_absorpt_correction_T_max 1 _exptl_absorpt_process_details 'SADABS, Bruker SAINT' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 18453 _diffrn_reflns_av_R_equivalents 0.0664 _diffrn_reflns_av_sigmaI/netI 0.0652 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.54 _diffrn_reflns_theta_max 24.99 _reflns_number_total 6379 _reflns_number_gt 6004 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0274P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.006(9) _refine_ls_number_reflns 6379 _refine_ls_number_parameters 451 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0353 _refine_ls_R_factor_gt 0.0333 _refine_ls_wR_factor_ref 0.0734 _refine_ls_wR_factor_gt 0.0730 _refine_ls_goodness_of_fit_ref 1.039 _refine_ls_restrained_S_all 1.039 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C -0.0595(6) 0.1185(3) -0.1088(3) 0.0270(15) Uani 1 1 d . . . C2 C -0.1480(6) 0.1013(4) -0.1617(3) 0.0336(16) Uani 1 1 d . . . C3 C -0.1335(7) 0.1283(4) -0.2290(3) 0.048(2) Uani 1 1 d . . . H3A H -0.1953 0.1185 -0.2634 0.057 Uiso 1 1 calc R . . C4 C -0.0296(9) 0.1700(4) -0.2479(3) 0.051(2) Uani 1 1 d . . . H4A H -0.0231 0.1882 -0.2942 0.061 Uiso 1 1 calc R . . C5 C 0.0647(7) 0.1846(3) -0.1982(3) 0.0424(19) Uani 1 1 d . . . H5A H 0.1358 0.2114 -0.2113 0.051 Uiso 1 1 calc R . . C6 C 0.0521(6) 0.1587(3) -0.1279(3) 0.0274(14) Uani 1 1 d . . . C7 C -0.2603(6) 0.0557(4) -0.1424(3) 0.050(2) Uani 1 1 d . . . H7A H -0.3123 0.0805 -0.1080 0.059 Uiso 1 1 calc R . . H7B H -0.2311 0.0113 -0.1220 0.059 Uiso 1 1 calc R . . H7C H -0.3095 0.0459 -0.1847 0.059 Uiso 1 1 calc R . . C8 C 0.1486(6) 0.1780(3) -0.0757(3) 0.0270(14) Uani 1 1 d . . . C9 C 0.3132(6) 0.2438(3) -0.0377(3) 0.0400(16) Uani 1 1 d . . . H9A H 0.2943 0.2921 -0.0215 0.048 Uiso 1 1 calc R . . H9B H 0.4032 0.2405 -0.0490 0.048 Uiso 1 1 calc R . . C10 C 0.2756(6) 0.1885(3) 0.0191(3) 0.0243(13) Uani 1 1 d . . . H10A H 0.2552 0.2133 0.0640 0.029 Uiso 1 1 calc R . . C11 C 0.3785(6) 0.1321(3) 0.0333(3) 0.0266(13) Uani 1 1 d . . . H11A H 0.3445 0.0993 0.0696 0.032 Uiso 1 1 calc R . . C12 C 0.4092(6) 0.0876(3) -0.0321(3) 0.0397(16) Uani 1 1 d . . . H12A H 0.4366 0.1185 -0.0703 0.048 Uiso 1 1 calc R . . H12B H 0.3345 0.0618 -0.0469 0.048 Uiso 1 1 calc R . . H12C H 0.4759 0.0543 -0.0208 0.048 Uiso 1 1 calc R . . C13 C 0.4953(6) 0.1664(3) 0.0649(3) 0.0409(17) Uani 1 1 d . . . H13A H 0.4735 0.1894 0.1093 0.049 Uiso 1 1 calc R . . H13B H 0.5285 0.2014 0.0320 0.049 Uiso 1 1 calc R . . H13C H 0.5587 0.1303 0.0736 0.049 Uiso 1 1 calc R . . C14 C -0.0652(5) 0.1586(3) 0.1891(3) 0.0229(14) Uani 1 1 d . . . C15 C -0.0302(7) 0.2129(3) 0.2380(3) 0.0277(12) Uani 1 1 d . . . C16 C -0.1058(7) 0.2281(3) 0.2954(3) 0.0377(17) Uani 1 1 d . . . H16A H -0.0811 0.2641 0.3270 0.045 Uiso 1 1 calc R . . C17 C -0.2190(7) 0.1914(4) 0.3081(3) 0.0359(16) Uani 1 1 d . . . H17A H -0.2690 0.2026 0.3477 0.043 Uiso 1 1 calc R . . C18 C -0.2557(6) 0.1387(3) 0.2613(3) 0.0325(15) Uani 1 1 d . . . H18A H -0.3316 0.1143 0.2694 0.039 Uiso 1 1 calc R . . C19 C -0.1821(6) 0.1210(3) 0.2022(3) 0.0238(13) Uani 1 1 d . . . C20 C 0.0917(7) 0.2526(3) 0.2244(3) 0.0347(15) Uani 1 1 d . . . H20A H 0.0852 0.2786 0.1800 0.042 Uiso 1 1 calc R . . H20B H 0.1609 0.2191 0.2215 0.042 Uiso 1 1 calc R . . H20C H 0.1070 0.2857 0.2629 0.042 Uiso 1 1 calc R . . C21 C -0.2274(5) 0.0667(3) 0.1525(3) 0.0227(11) Uani 1 1 d . . . C22 C -0.3715(6) -0.0137(3) 0.1134(3) 0.0284(14) Uani 1 1 d . . . H22A H -0.4540 -0.0057 0.0913 0.034 Uiso 1 1 calc R . . H22B H -0.3704 -0.0613 0.1345 0.034 Uiso 1 1 calc R . . C23 C -0.2645(5) -0.0052(3) 0.0588(3) 0.0244(13) Uani 1 1 d . . . H23A H -0.2978 0.0208 0.0172 0.029 Uiso 1 1 calc R . . C24 C -0.2047(5) -0.0760(3) 0.0325(3) 0.0244(13) Uani 1 1 d . . . H24A H -0.1407 -0.0637 -0.0038 0.029 Uiso 1 1 calc R . . C25 C -0.3065(6) -0.1209(4) -0.0046(3) 0.0365(16) Uani 1 1 d . . . H25A H -0.3450 -0.0933 -0.0423 0.044 Uiso 1 1 calc R . . H25B H -0.3704 -0.1344 0.0297 0.044 Uiso 1 1 calc R . . H25C H -0.2682 -0.1632 -0.0245 0.044 Uiso 1 1 calc R . . C26 C -0.1376(6) -0.1175(3) 0.0908(3) 0.0296(14) Uani 1 1 d . . . H26A H -0.1995 -0.1368 0.1234 0.036 Uiso 1 1 calc R . . H26B H -0.0810 -0.0861 0.1163 0.036 Uiso 1 1 calc R . . H26C H -0.0896 -0.1560 0.0697 0.036 Uiso 1 1 calc R . . C27 C 0.1686(5) -0.0804(3) -0.0022(2) 0.0199(12) Uani 1 1 d . . . C28 C 0.1696(6) -0.1313(3) -0.0588(3) 0.0265(13) Uani 1 1 d . . . C29 C 0.2593(6) -0.1860(3) -0.0579(3) 0.0328(15) Uani 1 1 d . . . H29A H 0.2599 -0.2191 -0.0953 0.039 Uiso 1 1 calc R . . C30 C 0.3469(7) -0.1932(3) -0.0039(3) 0.0380(16) Uani 1 1 d . . . H30A H 0.4068 -0.2299 -0.0055 0.046 Uiso 1 1 calc R . . C31 C 0.3462(6) -0.1462(3) 0.0525(3) 0.0308(13) Uani 1 1 d . . . H31A H 0.4043 -0.1515 0.0898 0.037 Uiso 1 1 calc R . . C32 C 0.2568(5) -0.0895(3) 0.0538(3) 0.0198(11) Uani 1 1 d . . . C33 C 0.0732(6) -0.1233(4) -0.1167(3) 0.0358(16) Uani 1 1 d . . . H33A H 0.0755 -0.0752 -0.1349 0.043 Uiso 1 1 calc R . . H33B H -0.0101 -0.1333 -0.0978 0.043 Uiso 1 1 calc R . . H33C H 0.0919 -0.1564 -0.1548 0.043 Uiso 1 1 calc R . . C34 C 0.2546(5) -0.0419(3) 0.1157(2) 0.0190(12) Uani 1 1 d . . . C35 C 0.3338(6) 0.0019(3) 0.2182(3) 0.0254(13) Uani 1 1 d . . . H35A H 0.3995 0.0379 0.2112 0.031 Uiso 1 1 calc R . . H35B H 0.3401 -0.0170 0.2666 0.031 Uiso 1 1 calc R . . C36 C 0.2010(5) 0.0329(3) 0.2038(2) 0.0225(13) Uani 1 1 d . . . H36A H 0.2049 0.0854 0.2061 0.027 Uiso 1 1 calc R . . C37 C 0.0961(6) 0.0063(3) 0.2529(3) 0.0205(12) Uani 1 1 d . . . H37A H 0.0146 0.0197 0.2310 0.025 Uiso 1 1 calc R . . C38 C 0.0967(5) -0.0756(3) 0.2610(3) 0.0243(12) Uani 1 1 d . . . H38A H 0.1711 -0.0901 0.2873 0.029 Uiso 1 1 calc R . . H38B H 0.0978 -0.0974 0.2143 0.029 Uiso 1 1 calc R . . H38C H 0.0217 -0.0905 0.2864 0.029 Uiso 1 1 calc R . . C39 C 0.1037(6) 0.0439(3) 0.3254(3) 0.0303(14) Uani 1 1 d . . . H39A H 0.0928 0.0946 0.3188 0.036 Uiso 1 1 calc R . . H39B H 0.1854 0.0349 0.3468 0.036 Uiso 1 1 calc R . . H39C H 0.0378 0.0260 0.3563 0.036 Uiso 1 1 calc R . . N1 N 0.1590(5) 0.1559(2) -0.0102(2) 0.0193(10) Uani 1 1 d . . . N2 N -0.1725(4) 0.0420(2) 0.0969(2) 0.0210(10) Uani 1 1 d . . . N3 N 0.1757(4) 0.0105(2) 0.1290(2) 0.0201(10) Uani 1 1 d . . . O1 O -0.0786(3) 0.09690(19) -0.04290(17) 0.0233(8) Uani 1 1 d . . . O2 O 0.2364(4) 0.2249(2) -0.0985(2) 0.0332(10) Uani 1 1 d . . . O3 O 0.0072(3) 0.14412(19) 0.13425(16) 0.0213(9) Uani 1 1 d . . . O4 O -0.3448(4) 0.0405(2) 0.16668(19) 0.0287(9) Uani 1 1 d . . . O5 O 0.0897(4) -0.0265(2) -0.00459(17) 0.0223(8) Uani 1 1 d . . . O6 O 0.3435(3) -0.05477(19) 0.16540(16) 0.0224(9) Uani 1 1 d . . . Yb1 Yb 0.03035(2) 0.069576(12) 0.048628(10) 0.01691(7) Uani 1 1 d . . . 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 C1 0.028(4) 0.030(3) 0.023(3) 0.001(2) 0.003(2) 0.013(3) C2 0.029(4) 0.051(4) 0.021(3) -0.005(3) -0.006(3) 0.020(3) C3 0.041(5) 0.076(6) 0.026(3) -0.004(3) -0.002(3) 0.026(4) C4 0.073(5) 0.066(5) 0.014(2) 0.002(3) 0.004(4) 0.031(5) C5 0.061(6) 0.028(4) 0.038(3) 0.006(3) 0.024(3) 0.020(3) C6 0.033(4) 0.027(3) 0.022(2) 0.002(2) 0.005(2) 0.012(3) C7 0.031(4) 0.085(6) 0.032(3) -0.010(4) -0.016(3) 0.004(4) C8 0.028(3) 0.016(3) 0.037(3) 0.004(3) 0.013(3) 0.008(3) C9 0.035(4) 0.021(3) 0.064(4) 0.012(3) 0.003(4) -0.005(3) C10 0.020(3) 0.016(3) 0.037(3) -0.003(3) 0.006(3) -0.001(2) C11 0.032(4) 0.019(3) 0.029(3) 0.001(2) 0.000(2) -0.002(3) C12 0.027(3) 0.037(4) 0.055(4) -0.009(3) -0.005(3) 0.010(3) C13 0.034(4) 0.030(3) 0.059(4) 0.001(3) -0.007(3) -0.010(3) C14 0.029(4) 0.020(3) 0.020(2) 0.004(2) -0.006(2) 0.010(3) C15 0.038(3) 0.021(3) 0.024(2) 0.001(2) -0.009(3) 0.007(3) C16 0.065(5) 0.025(3) 0.023(3) -0.005(3) -0.010(3) 0.010(3) C17 0.045(4) 0.041(4) 0.021(3) 0.004(3) 0.006(3) 0.012(3) C18 0.036(4) 0.037(4) 0.025(3) 0.011(3) 0.006(3) 0.002(3) C19 0.024(3) 0.025(3) 0.022(2) 0.003(2) 0.001(2) 0.009(3) C20 0.041(4) 0.027(3) 0.037(3) -0.010(3) -0.008(3) 0.000(3) C21 0.022(3) 0.021(3) 0.026(2) 0.011(3) 0.001(2) 0.009(3) C22 0.023(3) 0.027(3) 0.036(3) 0.001(3) 0.004(3) -0.005(3) C23 0.020(3) 0.028(3) 0.025(3) 0.005(3) -0.002(2) 0.001(2) C24 0.022(3) 0.027(3) 0.025(3) 0.001(3) 0.001(2) -0.002(3) C25 0.031(4) 0.038(4) 0.040(3) -0.007(3) -0.003(3) -0.008(3) C26 0.030(4) 0.023(3) 0.035(3) -0.003(3) -0.004(3) 0.002(3) C27 0.019(3) 0.019(3) 0.021(2) -0.002(2) 0.007(2) 0.000(3) C28 0.026(3) 0.024(3) 0.030(3) -0.001(3) 0.002(3) -0.004(3) C29 0.041(4) 0.025(3) 0.032(3) -0.011(3) 0.005(3) -0.004(3) C30 0.039(4) 0.025(4) 0.050(4) -0.005(3) 0.005(3) 0.008(3) C31 0.030(3) 0.024(3) 0.038(3) 0.002(3) -0.001(3) 0.002(3) C32 0.020(3) 0.015(3) 0.025(2) 0.000(2) 0.004(2) -0.001(2) C33 0.039(4) 0.040(4) 0.029(3) -0.012(3) -0.001(3) -0.006(3) C34 0.014(3) 0.021(3) 0.022(2) 0.005(2) 0.003(2) -0.005(2) C35 0.022(3) 0.032(4) 0.021(3) 0.001(2) -0.004(2) -0.003(3) C36 0.025(3) 0.021(3) 0.021(2) 0.001(2) -0.002(2) 0.000(3) C37 0.019(3) 0.022(3) 0.021(2) 0.001(2) -0.005(2) 0.003(3) C38 0.020(3) 0.025(3) 0.028(2) 0.004(3) 0.004(2) -0.001(3) C39 0.037(4) 0.030(3) 0.024(3) 0.000(2) 0.001(3) 0.001(3) N1 0.017(3) 0.020(3) 0.021(2) 0.001(2) 0.0037(19) 0.000(2) N2 0.018(3) 0.022(3) 0.023(2) 0.0031(19) -0.0016(19) 0.002(2) N3 0.019(3) 0.021(3) 0.021(2) 0.001(2) -0.0008(19) -0.007(2) O1 0.0212(19) 0.030(2) 0.0188(16) 0.0080(16) -0.0038(16) 0.0022(17) O2 0.031(3) 0.028(2) 0.040(2) 0.0126(19) 0.015(2) 0.002(2) O3 0.020(2) 0.0183(18) 0.0256(16) -0.0007(15) 0.0001(15) 0.0012(16) O4 0.017(2) 0.036(2) 0.0334(19) 0.0035(18) 0.0072(17) -0.0004(19) O5 0.022(2) 0.023(2) 0.0217(17) -0.0039(16) -0.0020(16) 0.0026(18) O6 0.0176(19) 0.026(2) 0.0239(16) -0.0031(16) -0.0044(15) 0.0035(17) Yb1 0.01484(11) 0.01786(11) 0.01802(10) 0.00187(10) 0.00001(9) 0.00044(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 O1 1.309(6) . ? C1 C2 1.391(8) . ? C1 C6 1.435(9) . ? C2 C3 1.360(8) . ? C2 C7 1.498(10) . ? C3 C4 1.384(11) . ? C3 H3A 0.9300 . ? C4 C5 1.382(10) . ? C4 H4A 0.9300 . ? C5 C6 1.403(7) . ? C5 H5A 0.9300 . ? C6 C8 1.450(9) . ? C7 H7A 0.9600 . ? C7 H7B 0.9600 . ? C7 H7C 0.9600 . ? C8 N1 1.293(7) . ? C8 O2 1.339(7) . ? C9 O2 1.435(7) . ? C9 C10 1.528(8) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 N1 1.472(8) . ? C10 C11 1.530(8) . ? C10 H10A 0.9800 . ? C11 C12 1.509(7) . ? C11 C13 1.503(8) . ? C11 H11A 0.9800 . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? C14 O3 1.302(6) . ? C14 C15 1.410(8) . ? C14 C19 1.434(8) . ? C15 C16 1.363(8) . ? C15 C20 1.500(9) . ? C16 C17 1.390(10) . ? C16 H16A 0.9300 . ? C17 C18 1.368(9) . ? C17 H17A 0.9300 . ? C18 C19 1.385(8) . ? C18 H18A 0.9300 . ? C19 C21 1.453(8) . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? C21 N2 1.272(7) . ? C21 O4 1.351(7) . ? C22 O4 1.445(7) . ? C22 C23 1.524(8) . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C23 N2 1.486(7) . ? C23 C24 1.542(8) . ? C23 H23A 0.9800 . ? C24 C26 1.508(7) . ? C24 C25 1.522(8) . ? C24 H24A 0.9800 . ? 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 O5 1.303(6) . ? C27 C32 1.406(7) . ? C27 C28 1.418(7) . ? C28 C29 1.389(8) . ? C28 C33 1.487(8) . ? C29 C30 1.369(9) . ? C29 H29A 0.9300 . ? C30 C31 1.368(8) . ? C30 H30A 0.9300 . ? C31 C32 1.412(8) . ? C31 H31A 0.9300 . ? C32 C34 1.455(7) . ? C33 H33A 0.9600 . ? C33 H33B 0.9600 . ? C33 H33C 0.9600 . ? C34 N3 1.303(7) . ? C34 O6 1.337(6) . ? C35 O6 1.448(6) . ? C35 C36 1.533(8) . ? C35 H35A 0.9700 . ? C35 H35B 0.9700 . ? C36 N3 1.480(6) . ? C36 C37 1.516(8) . ? C36 H36A 0.9800 . ? C37 C39 1.525(7) . ? C37 C38 1.533(8) . ? C37 H37A 0.9800 . ? C38 H38A 0.9600 . ? C38 H38B 0.9600 . ? C38 H38C 0.9600 . ? C39 H39A 0.9600 . ? C39 H39B 0.9600 . ? C39 H39C 0.9600 . ? N1 Yb1 2.369(5) . ? N2 Yb1 2.367(5) . ? N3 Yb1 2.405(5) . ? O1 Yb1 2.116(4) . ? O3 Yb1 2.130(4) . ? O5 Yb1 2.139(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 C1 C2 119.5(5) . . ? O1 C1 C6 121.2(5) . . ? C2 C1 C6 119.3(5) . . ? C3 C2 C1 119.6(7) . . ? C3 C2 C7 121.3(6) . . ? C1 C2 C7 119.0(5) . . ? C2 C3 C4 122.0(7) . . ? C2 C3 H3A 119.0 . . ? C4 C3 H3A 119.0 . . ? C5 C4 C3 120.3(5) . . ? C5 C4 H4A 119.9 . . ? C3 C4 H4A 119.9 . . ? C4 C5 C6 119.4(7) . . ? C4 C5 H5A 120.3 . . ? C6 C5 H5A 120.3 . . ? C5 C6 C1 119.2(6) . . ? C5 C6 C8 118.4(6) . . ? C1 C6 C8 122.2(4) . . ? C2 C7 H7A 109.5 . . ? C2 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C2 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? N1 C8 O2 116.7(6) . . ? N1 C8 C6 127.8(6) . . ? O2 C8 C6 115.5(5) . . ? O2 C9 C10 103.6(5) . . ? O2 C9 H9A 111.0 . . ? C10 C9 H9A 111.0 . . ? O2 C9 H9B 111.0 . . ? C10 C9 H9B 111.0 . . ? H9A C9 H9B 109.0 . . ? N1 C10 C11 111.5(4) . . ? N1 C10 C9 103.7(5) . . ? C11 C10 C9 113.6(5) . . ? N1 C10 H10A 109.3 . . ? C11 C10 H10A 109.3 . . ? C9 C10 H10A 109.3 . . ? C12 C11 C13 112.1(5) . . ? C12 C11 C10 112.9(5) . . ? C13 C11 C10 110.6(5) . . ? C12 C11 H11A 107.0 . . ? C13 C11 H11A 107.0 . . ? C10 C11 H11A 107.0 . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C11 C13 H13A 109.5 . . ? C11 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C11 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? O3 C14 C15 120.3(5) . . ? O3 C14 C19 122.1(5) . . ? C15 C14 C19 117.6(5) . . ? C16 C15 C14 120.4(6) . . ? C16 C15 C20 121.8(5) . . ? C14 C15 C20 117.9(5) . . ? C15 C16 C17 121.9(6) . . ? C15 C16 H16A 119.1 . . ? C17 C16 H16A 119.1 . . ? C18 C17 C16 119.1(6) . . ? C18 C17 H17A 120.5 . . ? C16 C17 H17A 120.5 . . ? C17 C18 C19 121.4(6) . . ? C17 C18 H18A 119.3 . . ? C19 C18 H18A 119.3 . . ? C18 C19 C14 119.7(5) . . ? C18 C19 C21 119.4(5) . . ? C14 C19 C21 120.8(5) . . ? C15 C20 H20A 109.5 . . ? C15 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C15 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? N2 C21 O4 116.2(5) . . ? N2 C21 C19 128.6(5) . . ? O4 C21 C19 115.1(5) . . ? O4 C22 C23 104.1(4) . . ? O4 C22 H22A 110.9 . . ? C23 C22 H22A 110.9 . . ? O4 C22 H22B 110.9 . . ? C23 C22 H22B 110.9 . . ? H22A C22 H22B 109.0 . . ? N2 C23 C22 102.8(4) . . ? N2 C23 C24 113.2(5) . . ? C22 C23 C24 115.0(5) . . ? N2 C23 H23A 108.5 . . ? C22 C23 H23A 108.5 . . ? C24 C23 H23A 108.5 . . ? C26 C24 C25 111.9(5) . . ? C26 C24 C23 113.6(4) . . ? C25 C24 C23 109.2(5) . . ? C26 C24 H24A 107.3 . . ? C25 C24 H24A 107.3 . . ? C23 C24 H24A 107.3 . . ? C24 C25 H25A 109.5 . . ? C24 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C24 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C24 C26 H26A 109.5 . . ? C24 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C24 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? O5 C27 C32 122.5(4) . . ? O5 C27 C28 119.7(5) . . ? C32 C27 C28 117.8(5) . . ? C29 C28 C27 119.2(5) . . ? C29 C28 C33 122.9(5) . . ? C27 C28 C33 117.9(5) . . ? C30 C29 C28 122.3(5) . . ? C30 C29 H29A 118.8 . . ? C28 C29 H29A 118.8 . . ? C31 C30 C29 119.9(6) . . ? C31 C30 H30A 120.0 . . ? C29 C30 H30A 120.0 . . ? C30 C31 C32 119.7(6) . . ? C30 C31 H31A 120.1 . . ? C32 C31 H31A 120.1 . . ? C27 C32 C31 121.0(5) . . ? C27 C32 C34 120.2(5) . . ? C31 C32 C34 118.7(5) . . ? C28 C33 H33A 109.5 . . ? C28 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C28 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? N3 C34 O6 116.5(4) . . ? N3 C34 C32 128.2(5) . . ? O6 C34 C32 115.3(5) . . ? O6 C35 C36 102.7(4) . . ? O6 C35 H35A 111.2 . . ? C36 C35 H35A 111.2 . . ? O6 C35 H35B 111.2 . . ? C36 C35 H35B 111.2 . . ? H35A C35 H35B 109.1 . . ? N3 C36 C37 110.3(4) . . ? N3 C36 C35 102.8(4) . . ? C37 C36 C35 115.5(4) . . ? N3 C36 H36A 109.3 . . ? C37 C36 H36A 109.3 . . ? C35 C36 H36A 109.3 . . ? C36 C37 C39 110.3(5) . . ? C36 C37 C38 112.5(5) . . ? C39 C37 C38 111.8(4) . . ? C36 C37 H37A 107.3 . . ? C39 C37 H37A 107.3 . . ? C38 C37 H37A 107.3 . . ? C37 C38 H38A 109.5 . . ? C37 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C37 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C37 C39 H39A 109.5 . . ? C37 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C37 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C8 N1 C10 106.8(5) . . ? C8 N1 Yb1 127.3(4) . . ? C10 N1 Yb1 125.6(3) . . ? C21 N2 C23 108.0(5) . . ? C21 N2 Yb1 129.6(4) . . ? C23 N2 Yb1 122.1(3) . . ? C34 N3 C36 106.1(4) . . ? C34 N3 Yb1 128.8(3) . . ? C36 N3 Yb1 124.8(4) . . ? C1 O1 Yb1 138.5(4) . . ? C8 O2 C9 107.3(4) . . ? C14 O3 Yb1 142.2(4) . . ? C21 O4 C22 107.1(4) . . ? C27 O5 Yb1 144.5(3) . . ? C34 O6 C35 106.9(4) . . ? O1 Yb1 O3 112.68(14) . . ? O1 Yb1 O5 89.12(14) . . ? O3 Yb1 O5 157.90(12) . . ? O1 Yb1 N2 82.69(15) . . ? O3 Yb1 N2 75.80(14) . . ? O5 Yb1 N2 104.82(16) . . ? O1 Yb1 N1 76.76(16) . . ? O3 Yb1 N1 88.23(15) . . ? O5 Yb1 N1 100.81(17) . . ? N2 Yb1 N1 146.69(16) . . ? O1 Yb1 N3 162.77(14) . . ? O3 Yb1 N3 84.51(15) . . ? O5 Yb1 N3 73.80(15) . . ? N2 Yb1 N3 103.55(16) . . ? N1 Yb1 N3 103.77(17) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 C1 C2 C3 175.0(6) . . . . ? C6 C1 C2 C3 -6.1(9) . . . . ? O1 C1 C2 C7 -2.5(9) . . . . ? C6 C1 C2 C7 176.4(6) . . . . ? C1 C2 C3 C4 3.2(10) . . . . ? C7 C2 C3 C4 -179.4(7) . . . . ? C2 C3 C4 C5 0.9(11) . . . . ? C3 C4 C5 C6 -1.9(10) . . . . ? C4 C5 C6 C1 -1.1(9) . . . . ? C4 C5 C6 C8 -176.6(6) . . . . ? O1 C1 C6 C5 -176.0(5) . . . . ? C2 C1 C6 C5 5.1(8) . . . . ? O1 C1 C6 C8 -0.6(9) . . . . ? C2 C1 C6 C8 -179.5(5) . . . . ? C5 C6 C8 N1 -174.9(6) . . . . ? C1 C6 C8 N1 9.7(9) . . . . ? C5 C6 C8 O2 5.7(8) . . . . ? C1 C6 C8 O2 -169.7(5) . . . . ? O2 C9 C10 N1 -13.6(6) . . . . ? O2 C9 C10 C11 107.6(5) . . . . ? N1 C10 C11 C12 55.0(6) . . . . ? C9 C10 C11 C12 -61.8(6) . . . . ? N1 C10 C11 C13 -178.5(4) . . . . ? C9 C10 C11 C13 64.7(6) . . . . ? O3 C14 C15 C16 180.0(5) . . . . ? C19 C14 C15 C16 0.3(8) . . . . ? O3 C14 C15 C20 -0.1(7) . . . . ? C19 C14 C15 C20 -179.7(5) . . . . ? C14 C15 C16 C17 -0.1(9) . . . . ? C20 C15 C16 C17 179.9(6) . . . . ? C15 C16 C17 C18 -0.3(9) . . . . ? C16 C17 C18 C19 0.5(9) . . . . ? C17 C18 C19 C14 -0.3(9) . . . . ? C17 C18 C19 C21 -177.5(5) . . . . ? O3 C14 C19 C18 -179.7(5) . . . . ? C15 C14 C19 C18 -0.1(8) . . . . ? O3 C14 C19 C21 -2.6(8) . . . . ? C15 C14 C19 C21 177.1(5) . . . . ? C18 C19 C21 N2 -177.9(5) . . . . ? C14 C19 C21 N2 4.9(9) . . . . ? C18 C19 C21 O4 3.8(7) . . . . ? C14 C19 C21 O4 -173.4(5) . . . . ? O4 C22 C23 N2 12.8(5) . . . . ? O4 C22 C23 C24 136.4(5) . . . . ? N2 C23 C24 C26 53.5(6) . . . . ? C22 C23 C24 C26 -64.3(6) . . . . ? N2 C23 C24 C25 179.1(4) . . . . ? C22 C23 C24 C25 61.3(6) . . . . ? O5 C27 C28 C29 176.1(5) . . . . ? C32 C27 C28 C29 -2.0(8) . . . . ? O5 C27 C28 C33 -4.1(7) . . . . ? C32 C27 C28 C33 177.8(5) . . . . ? C27 C28 C29 C30 0.4(9) . . . . ? C33 C28 C29 C30 -179.4(6) . . . . ? C28 C29 C30 C31 1.4(10) . . . . ? C29 C30 C31 C32 -1.5(9) . . . . ? O5 C27 C32 C31 -176.1(5) . . . . ? C28 C27 C32 C31 1.9(8) . . . . ? O5 C27 C32 C34 6.1(8) . . . . ? C28 C27 C32 C34 -175.9(5) . . . . ? C30 C31 C32 C27 -0.2(8) . . . . ? C30 C31 C32 C34 177.6(5) . . . . ? C27 C32 C34 N3 2.1(8) . . . . ? C31 C32 C34 N3 -175.8(5) . . . . ? C27 C32 C34 O6 -179.3(4) . . . . ? C31 C32 C34 O6 2.9(7) . . . . ? O6 C35 C36 N3 -21.8(5) . . . . ? O6 C35 C36 C37 98.4(5) . . . . ? N3 C36 C37 C39 -166.2(5) . . . . ? C35 C36 C37 C39 77.8(6) . . . . ? N3 C36 C37 C38 68.3(6) . . . . ? C35 C36 C37 C38 -47.7(6) . . . . ? O2 C8 N1 C10 -3.1(7) . . . . ? C6 C8 N1 C10 177.5(5) . . . . ? O2 C8 N1 Yb1 -176.9(3) . . . . ? C6 C8 N1 Yb1 3.7(8) . . . . ? C11 C10 N1 C8 -112.2(5) . . . . ? C9 C10 N1 C8 10.5(6) . . . . ? C11 C10 N1 Yb1 61.7(6) . . . . ? C9 C10 N1 Yb1 -175.6(4) . . . . ? O4 C21 N2 C23 5.7(6) . . . . ? C19 C21 N2 C23 -172.5(5) . . . . ? O4 C21 N2 Yb1 179.9(3) . . . . ? C19 C21 N2 Yb1 1.7(8) . . . . ? C22 C23 N2 C21 -11.5(6) . . . . ? C24 C23 N2 C21 -136.3(5) . . . . ? C22 C23 N2 Yb1 173.8(3) . . . . ? C24 C23 N2 Yb1 49.0(5) . . . . ? O6 C34 N3 C36 -8.3(6) . . . . ? C32 C34 N3 C36 170.4(5) . . . . ? O6 C34 N3 Yb1 166.2(3) . . . . ? C32 C34 N3 Yb1 -15.1(8) . . . . ? C37 C36 N3 C34 -105.1(5) . . . . ? C35 C36 N3 C34 18.6(6) . . . . ? C37 C36 N3 Yb1 80.1(5) . . . . ? C35 C36 N3 Yb1 -156.2(3) . . . . ? C2 C1 O1 Yb1 151.6(4) . . . . ? C6 C1 O1 Yb1 -27.3(8) . . . . ? N1 C8 O2 C9 -6.4(7) . . . . ? C6 C8 O2 C9 173.1(5) . . . . ? C10 C9 O2 C8 12.3(6) . . . . ? C15 C14 O3 Yb1 172.0(4) . . . . ? C19 C14 O3 Yb1 -8.4(8) . . . . ? N2 C21 O4 C22 3.2(6) . . . . ? C19 C21 O4 C22 -178.3(5) . . . . ? C23 C22 O4 C21 -10.2(6) . . . . ? C32 C27 O5 Yb1 1.2(9) . . . . ? C28 C27 O5 Yb1 -176.8(4) . . . . ? N3 C34 O6 C35 -6.8(6) . . . . ? C32 C34 O6 C35 174.4(4) . . . . ? C36 C35 O6 C34 17.9(5) . . . . ? C1 O1 Yb1 O3 112.2(5) . . . . ? C1 O1 Yb1 O5 -71.5(5) . . . . ? C1 O1 Yb1 N2 -176.5(5) . . . . ? C1 O1 Yb1 N1 29.9(5) . . . . ? C1 O1 Yb1 N3 -64.0(8) . . . . ? C14 O3 Yb1 O1 86.4(5) . . . . ? C14 O3 Yb1 O5 -83.8(6) . . . . ? C14 O3 Yb1 N2 10.7(5) . . . . ? C14 O3 Yb1 N1 161.2(5) . . . . ? C14 O3 Yb1 N3 -94.8(5) . . . . ? C27 O5 Yb1 O1 168.8(6) . . . . ? C27 O5 Yb1 O3 -20.3(8) . . . . ? C27 O5 Yb1 N2 -108.9(6) . . . . ? C27 O5 Yb1 N1 92.5(6) . . . . ? C27 O5 Yb1 N3 -8.8(6) . . . . ? C21 N2 Yb1 O1 -122.2(5) . . . . ? C23 N2 Yb1 O1 51.3(4) . . . . ? C21 N2 Yb1 O3 -6.5(4) . . . . ? C23 N2 Yb1 O3 167.0(4) . . . . ? C21 N2 Yb1 O5 150.7(4) . . . . ? C23 N2 Yb1 O5 -35.9(4) . . . . ? C21 N2 Yb1 N1 -70.2(5) . . . . ? C23 N2 Yb1 N1 103.3(4) . . . . ? C21 N2 Yb1 N3 74.2(5) . . . . ? C23 N2 Yb1 N3 -112.4(4) . . . . ? C8 N1 Yb1 O1 -15.9(5) . . . . ? C10 N1 Yb1 O1 171.4(4) . . . . ? C8 N1 Yb1 O3 -129.7(5) . . . . ? C10 N1 Yb1 O3 57.6(4) . . . . ? C8 N1 Yb1 O5 70.6(5) . . . . ? C10 N1 Yb1 O5 -102.1(4) . . . . ? C8 N1 Yb1 N2 -69.3(5) . . . . ? C10 N1 Yb1 N2 118.0(4) . . . . ? C8 N1 Yb1 N3 146.4(5) . . . . ? C10 N1 Yb1 N3 -26.3(4) . . . . ? C34 N3 Yb1 O1 6.6(8) . . . . ? C36 N3 Yb1 O1 -179.9(4) . . . . ? C34 N3 Yb1 O3 -169.9(5) . . . . ? C36 N3 Yb1 O3 3.6(4) . . . . ? C34 N3 Yb1 O5 14.4(4) . . . . ? C36 N3 Yb1 O5 -172.1(4) . . . . ? C34 N3 Yb1 N2 116.1(5) . . . . ? C36 N3 Yb1 N2 -70.3(4) . . . . ? C34 N3 Yb1 N1 -83.1(5) . . . . ? C36 N3 Yb1 N1 90.5(4) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 24.99 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.432 _refine_diff_density_min -0.515 _refine_diff_density_rms 0.112 _database_code_depnum_ccdc_archive 'CCDC 957727' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_AliPrMePh3 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C43 H56 Al N3 O7' _chemical_formula_weight 753.89 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Al Al 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' _cell_length_a 12.4850(6) _cell_length_b 12.6993(6) _cell_length_c 13.5170(7) _cell_angle_alpha 83.4160(10) _cell_angle_beta 75.6490(10) _cell_angle_gamma 86.3070(10) _cell_volume 2061.12(18) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 10111 _cell_measurement_theta_min 2.83 _cell_measurement_theta_max 24.32 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_diffrn 1.215 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 808 _exptl_absorpt_coefficient_mu 0.101 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9702 _exptl_absorpt_correction_T_max 0.9800 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX' _diffrn_measurement_method \w _diffrn_reflns_number 33146 _diffrn_reflns_av_R_equivalents 0.0233 _diffrn_reflns_av_sigmaI/netI 0.0374 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.56 _diffrn_reflns_theta_max 26.02 _reflns_number_total 15711 _reflns_number_gt 14670 _reflns_threshold_expression >2sigma(I) _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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. All non-hydrogen atoms were refined anisotropically, with the exception of one of the two thf molecules, which is disordered. Atom positions of this molecule were split over two positions and refined with SIMU and SAME restraints, as well as an occupancy factor. All hydrogen atoms were fixed to parent atoms using AFIX commands. ; _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^)+(0.0458P)^2^+0.4242P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.03(9) _refine_ls_number_reflns 15711 _refine_ls_number_parameters 987 _refine_ls_number_restraints 88 _refine_ls_R_factor_all 0.0414 _refine_ls_R_factor_gt 0.0373 _refine_ls_wR_factor_ref 0.0897 _refine_ls_wR_factor_gt 0.0868 _refine_ls_goodness_of_fit_ref 1.017 _refine_ls_restrained_S_all 1.034 _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 0.19509(5) 0.63191(4) 0.53391(4) 0.01728(12) Uani 1 1 d . . . O1 O 0.21118(11) 0.50307(10) 0.48071(10) 0.0209(3) Uani 1 1 d . . . N1 N 0.36349(14) 0.64098(13) 0.48872(12) 0.0196(4) Uani 1 1 d . . . C1 C 0.27976(18) 0.47536(16) 0.39590(16) 0.0226(4) Uani 1 1 d . . . Al2 Al 0.84249(5) 0.11209(4) 0.13372(4) 0.01716(12) Uani 1 1 d . . . O2 O 0.51644(12) 0.64529(13) 0.36013(11) 0.0302(3) Uani 1 1 d . . . N2 N 0.18761(14) 0.55092(12) 0.67361(13) 0.0197(4) Uani 1 1 d . . . C2 C 0.38172(17) 0.52343(16) 0.35284(15) 0.0232(4) Uani 1 1 d . . . O3 O 0.18175(11) 0.75393(10) 0.59548(10) 0.0194(3) Uani 1 1 d . . . N3 N 0.02796(14) 0.61836(13) 0.55531(12) 0.0192(3) Uani 1 1 d . . . C3 C 0.41673(17) 0.60458(16) 0.40452(16) 0.0232(4) Uani 1 1 d . . . O4 O 0.15866(12) 0.52560(11) 0.84504(11) 0.0256(3) Uani 1 1 d . . . N4 N 0.82949(13) 0.25422(13) 0.19461(13) 0.0197(3) Uani 1 1 d . . . C4 C 0.52230(19) 0.73714(19) 0.41357(17) 0.0302(5) Uani 1 1 d . . . H4A H 0.5041 0.8036 0.3741 0.036 Uiso 1 1 calc R . . H4B H 0.5969 0.7417 0.4255 0.036 Uiso 1 1 calc R . . O5 O 0.19197(11) 0.71124(11) 0.41074(10) 0.0199(3) Uani 1 1 d . . . N5 N 0.87020(13) -0.01813(12) 0.05453(12) 0.0180(3) Uani 1 1 d . . . C5 C 0.43594(16) 0.71687(16) 0.51472(16) 0.0223(4) Uani 1 1 d . . . H5 H 0.3927 0.7842 0.5319 0.027 Uiso 1 1 calc R . . O6 O -0.12218(12) 0.59075(12) 0.49976(11) 0.0256(3) Uani 1 1 d . . . N6 N 0.86258(13) 0.02274(12) 0.26311(12) 0.0185(3) Uani 1 1 d . . . C6 C 0.48162(17) 0.66890(17) 0.60635(16) 0.0249(4) Uani 1 1 d . . . H6 H 0.4171 0.6455 0.6633 0.030 Uiso 1 1 calc R . . O7 O 0.99394(11) 0.12484(10) 0.09675(10) 0.0201(3) Uani 1 1 d . . . C7 C 0.55811(18) 0.57157(19) 0.58223(18) 0.0312(5) Uani 1 1 d . . . H7A H 0.5191 0.5188 0.5583 0.047 Uiso 1 1 calc R . . H7B H 0.5804 0.5409 0.6443 0.047 Uiso 1 1 calc R . . H7C H 0.6239 0.5925 0.5285 0.047 Uiso 1 1 calc R . . O8 O 0.86746(12) 0.42703(11) 0.17345(12) 0.0280(3) Uani 1 1 d . . . C8 C 0.5390(2) 0.75330(19) 0.64436(19) 0.0346(5) Uani 1 1 d . . . H8A H 0.6034 0.7772 0.5905 0.052 Uiso 1 1 calc R . . H8B H 0.5631 0.7231 0.7057 0.052 Uiso 1 1 calc R . . H8C H 0.4873 0.8137 0.6613 0.052 Uiso 1 1 calc R . . O9 O 0.81866(12) 0.19006(11) 0.01705(10) 0.0221(3) Uani 1 1 d . . . C9 C 0.45105(19) 0.49208(18) 0.26131(16) 0.0302(5) Uani 1 1 d . . . H9 H 0.5188 0.5263 0.2322 0.036 Uiso 1 1 calc R . . O10 O 0.92867(12) -0.10425(11) -0.08713(10) 0.0232(3) Uani 1 1 d . . . C10 C 0.4219(2) 0.4128(2) 0.21378(18) 0.0370(6) Uani 1 1 d . . . H10 H 0.4693 0.3910 0.1524 0.044 Uiso 1 1 calc R . . O11 O 0.69367(11) 0.09071(11) 0.18069(10) 0.0209(3) Uani 1 1 d . . . C11 C 0.3212(2) 0.36440(19) 0.25717(18) 0.0347(5) Uani 1 1 d . . . H11 H 0.3013 0.3091 0.2242 0.042 Uiso 1 1 calc R . . O12 O 0.81660(12) -0.08744(11) 0.40757(11) 0.0265(3) Uani 1 1 d . . . C12 C 0.24933(19) 0.39368(17) 0.34609(17) 0.0278(5) Uani 1 1 d . . . C13 C 0.1404(2) 0.34387(18) 0.39014(19) 0.0353(5) Uani 1 1 d . . . H13A H 0.1390 0.3085 0.4588 0.053 Uiso 1 1 calc R . . H13B H 0.1298 0.2917 0.3457 0.053 Uiso 1 1 calc R . . H13C H 0.0810 0.3987 0.3949 0.053 Uiso 1 1 calc R . . C14 C 0.19516(16) 0.77790(15) 0.68321(14) 0.0178(4) Uani 1 1 d . . . C15 C 0.19627(16) 0.70225(16) 0.76786(15) 0.0199(4) Uani 1 1 d . . . C16 C 0.18116(16) 0.59189(16) 0.75793(15) 0.0192(4) Uani 1 1 d . . . C17 C 0.12754(19) 0.42633(17) 0.81597(17) 0.0280(5) Uani 1 1 d . . . H17A H 0.0461 0.4210 0.8330 0.034 Uiso 1 1 calc R . . H17B H 0.1599 0.3641 0.8510 0.034 Uiso 1 1 calc R . . C18 C 0.17576(18) 0.43391(16) 0.69985(17) 0.0247(4) Uani 1 1 d . . . H18 H 0.1205 0.4092 0.6660 0.030 Uiso 1 1 calc R . . C19 C 0.28625(19) 0.37214(17) 0.66605(17) 0.0284(5) Uani 1 1 d . . . H19 H 0.3203 0.3990 0.5932 0.034 Uiso 1 1 calc R . . C20 C 0.36912(19) 0.38736(19) 0.72964(19) 0.0328(5) Uani 1 1 d . . . H20A H 0.3770 0.4633 0.7317 0.049 Uiso 1 1 calc R . . H20B H 0.4411 0.3549 0.6982 0.049 Uiso 1 1 calc R . . H20C H 0.3423 0.3536 0.7997 0.049 Uiso 1 1 calc R . . C21 C 0.2660(2) 0.25453(19) 0.6684(3) 0.0486(7) Uani 1 1 d . . . H21A H 0.2284 0.2269 0.7383 0.073 Uiso 1 1 calc R . . H21B H 0.3370 0.2157 0.6472 0.073 Uiso 1 1 calc R . . H21C H 0.2197 0.2455 0.6214 0.073 Uiso 1 1 calc R . . C22 C 0.20984(17) 0.73329(17) 0.86027(16) 0.0240(4) Uani 1 1 d . . . H22 H 0.2092 0.6818 0.9172 0.029 Uiso 1 1 calc R . . C23 C 0.22416(19) 0.83859(17) 0.86845(16) 0.0277(5) Uani 1 1 d . . . H23 H 0.2353 0.8595 0.9303 0.033 Uiso 1 1 calc R . . C24 C 0.22208(18) 0.91389(17) 0.78542(16) 0.0263(5) Uani 1 1 d . . . H24 H 0.2318 0.9862 0.7918 0.032 Uiso 1 1 calc R . . C25 C 0.20625(16) 0.88681(16) 0.69378(15) 0.0205(4) Uani 1 1 d . . . C26 C 0.19806(18) 0.96690(16) 0.60487(16) 0.0248(4) Uani 1 1 d . . . H26A H 0.2489 0.9454 0.5422 0.037 Uiso 1 1 calc R . . H26B H 0.2177 1.0365 0.6181 0.037 Uiso 1 1 calc R . . H26C H 0.1222 0.9710 0.5963 0.037 Uiso 1 1 calc R . . C27 C 0.14037(17) 0.69025(15) 0.34283(15) 0.0192(4) Uani 1 1 d . . . C28 C 0.04000(17) 0.63588(15) 0.37014(15) 0.0206(4) Uani 1 1 d . . . C29 C -0.01392(16) 0.61406(15) 0.47777(15) 0.0193(4) Uani 1 1 d . . . C30 C -0.15879(18) 0.57240(19) 0.61047(16) 0.0287(5) Uani 1 1 d . . . H30A H -0.1755 0.4969 0.6323 0.034 Uiso 1 1 calc R . . H30B H -0.2259 0.6167 0.6363 0.034 Uiso 1 1 calc R . . C31 C -0.06148(16) 0.60363(16) 0.65054(15) 0.0221(4) Uani 1 1 d . . . H31 H -0.0401 0.5425 0.6962 0.027 Uiso 1 1 calc R . . C32 C -0.08425(17) 0.70255(17) 0.70931(15) 0.0234(4) Uani 1 1 d . . . H32 H -0.0168 0.7132 0.7337 0.028 Uiso 1 1 calc R . . C33 C -0.1051(2) 0.80291(18) 0.64214(18) 0.0347(5) Uani 1 1 d . . . H33A H -0.0377 0.8192 0.5886 0.052 Uiso 1 1 calc R . . H33B H -0.1256 0.8621 0.6845 0.052 Uiso 1 1 calc R . . H33C H -0.1653 0.7919 0.6102 0.052 Uiso 1 1 calc R . . C34 C -0.18014(19) 0.6847(2) 0.80419(17) 0.0345(5) Uani 1 1 d . . . H34A H -0.2474 0.6720 0.7829 0.052 Uiso 1 1 calc R . . H34B H -0.1923 0.7476 0.8419 0.052 Uiso 1 1 calc R . . H34C H -0.1622 0.6230 0.8486 0.052 Uiso 1 1 calc R . . C35 C -0.01250(18) 0.61482(16) 0.29411(16) 0.0249(4) Uani 1 1 d . . . H35 H -0.0788 0.5768 0.3128 0.030 Uiso 1 1 calc R . . C36 C 0.03188(19) 0.64901(17) 0.19315(16) 0.0277(5) Uani 1 1 d . . . H36 H -0.0035 0.6346 0.1418 0.033 Uiso 1 1 calc R . . C37 C 0.1290(2) 0.70498(17) 0.16607(16) 0.0283(5) Uani 1 1 d . . . H37 H 0.1580 0.7294 0.0960 0.034 Uiso 1 1 calc R . . C38 C 0.18456(18) 0.72610(16) 0.23759(15) 0.0229(4) Uani 1 1 d . . . C39 C 0.29116(19) 0.78350(18) 0.20938(16) 0.0293(5) Uani 1 1 d . . . H39A H 0.2861 0.8400 0.2542 0.044 Uiso 1 1 calc R . . H39B H 0.3048 0.8145 0.1378 0.044 Uiso 1 1 calc R . . H39C H 0.3521 0.7335 0.2178 0.044 Uiso 1 1 calc R . . C40 C 1.05775(17) 0.20634(15) 0.08243(14) 0.0194(4) Uani 1 1 d . . . C41 C 1.01868(17) 0.30807(16) 0.11054(15) 0.0224(4) Uani 1 1 d . . . C42 C 0.90248(17) 0.32528(15) 0.16004(15) 0.0213(4) Uani 1 1 d . . . C43 C 0.74710(18) 0.42472(17) 0.20769(18) 0.0275(5) Uani 1 1 d . . . H43A H 0.7121 0.4455 0.1498 0.033 Uiso 1 1 calc R . . H43B H 0.7183 0.4728 0.2618 0.033 Uiso 1 1 calc R . . C44 C 0.72615(17) 0.30860(15) 0.24997(16) 0.0224(4) Uani 1 1 d . . . H44 H 0.6611 0.2844 0.2290 0.027 Uiso 1 1 calc R . . C45 C 0.70964(18) 0.28545(17) 0.36687(16) 0.0255(5) Uani 1 1 d . . . H45 H 0.7190 0.2069 0.3821 0.031 Uiso 1 1 calc R . . C46 C 0.5918(2) 0.3169(2) 0.42179(18) 0.0353(5) Uani 1 1 d . . . H46A H 0.5801 0.3938 0.4099 0.053 Uiso 1 1 calc R . . H46B H 0.5805 0.2959 0.4956 0.053 Uiso 1 1 calc R . . H46C H 0.5393 0.2810 0.3951 0.053 Uiso 1 1 calc R . . C47 C 0.7945(2) 0.33632(19) 0.40806(18) 0.0332(5) Uani 1 1 d . . . H47A H 0.8691 0.3176 0.3689 0.050 Uiso 1 1 calc R . . H47B H 0.7864 0.3106 0.4806 0.050 Uiso 1 1 calc R . . H47C H 0.7827 0.4136 0.4012 0.050 Uiso 1 1 calc R . . C48 C 1.09294(18) 0.39024(17) 0.09504(16) 0.0264(5) Uani 1 1 d . . . H48 H 1.0660 0.4588 0.1132 0.032 Uiso 1 1 calc R . . C49 C 1.20336(18) 0.37309(18) 0.05419(17) 0.0297(5) Uani 1 1 d . . . H49 H 1.2531 0.4290 0.0450 0.036 Uiso 1 1 calc R . . C50 C 1.24248(18) 0.27253(18) 0.02599(16) 0.0265(5) Uani 1 1 d . . . H50 H 1.3194 0.2609 -0.0022 0.032 Uiso 1 1 calc R . . C51 C 1.17244(17) 0.18962(17) 0.03799(15) 0.0229(4) Uani 1 1 d . . . C52 C 1.21277(18) 0.08162(18) 0.00709(18) 0.0310(5) Uani 1 1 d . . . H52A H 1.1996 0.0299 0.0680 0.046 Uiso 1 1 calc R . . H52B H 1.2922 0.0826 -0.0254 0.046 Uiso 1 1 calc R . . H52C H 1.1729 0.0618 -0.0416 0.046 Uiso 1 1 calc R . . C53 C 0.86664(16) 0.18053(16) -0.07919(15) 0.0212(4) Uani 1 1 d . . . C54 C 0.91346(16) 0.08408(16) -0.11500(15) 0.0209(4) Uani 1 1 d . . . C55 C 0.90342(16) -0.01162(15) -0.04444(15) 0.0190(4) Uani 1 1 d . . . C56 C 0.92441(17) -0.18611(15) -0.00217(15) 0.0225(4) Uani 1 1 d . . . H56A H 0.9999 -0.2101 0.0035 0.027 Uiso 1 1 calc R . . H56B H 0.8845 -0.2479 -0.0110 0.027 Uiso 1 1 calc R . . C57 C 0.86181(17) -0.13257(15) 0.09300(15) 0.0202(4) Uani 1 1 d . . . H57 H 0.9029 -0.1482 0.1481 0.024 Uiso 1 1 calc R . . C58 C 0.74148(17) -0.16424(16) 0.13612(16) 0.0234(4) Uani 1 1 d . . . H58 H 0.7106 -0.1246 0.1974 0.028 Uiso 1 1 calc R . . C59 C 0.73709(19) -0.28267(17) 0.17381(18) 0.0300(5) Uani 1 1 d . . . H59A H 0.7697 -0.3241 0.1161 0.045 Uiso 1 1 calc R . . H59B H 0.6599 -0.3017 0.2027 0.045 Uiso 1 1 calc R . . H59C H 0.7788 -0.2980 0.2267 0.045 Uiso 1 1 calc R . . C60 C 0.67006(18) -0.13323(18) 0.06054(19) 0.0313(5) Uani 1 1 d . . . H60A H 0.6692 -0.0561 0.0439 0.047 Uiso 1 1 calc R . . H60B H 0.5945 -0.1560 0.0912 0.047 Uiso 1 1 calc R . . H60C H 0.7005 -0.1676 -0.0023 0.047 Uiso 1 1 calc R . . C61 C 0.96434(18) 0.07889(17) -0.21999(16) 0.0263(5) Uani 1 1 d . . . H61 H 0.9959 0.0134 -0.2434 0.032 Uiso 1 1 calc R . . C62 C 0.9684(2) 0.16797(18) -0.28842(17) 0.0315(5) Uani 1 1 d . . . H62 H 1.0036 0.1648 -0.3590 0.038 Uiso 1 1 calc R . . C63 C 0.9205(2) 0.26318(18) -0.25339(17) 0.0312(5) Uani 1 1 d . . . H63 H 0.9228 0.3243 -0.3014 0.037 Uiso 1 1 calc R . . C64 C 0.86964(18) 0.27202(17) -0.15121(17) 0.0263(5) Uani 1 1 d . . . C65 C 0.8153(2) 0.37272(18) -0.11237(18) 0.0353(5) Uani 1 1 d . . . H65A H 0.7394 0.3593 -0.0730 0.053 Uiso 1 1 calc R . . H65B H 0.8140 0.4260 -0.1706 0.053 Uiso 1 1 calc R . . H65C H 0.8569 0.3988 -0.0681 0.053 Uiso 1 1 calc R . . C66 C 0.62840(17) 0.06058(15) 0.26987(16) 0.0219(4) Uani 1 1 d . . . C67 C 0.66816(17) 0.01098(16) 0.35394(16) 0.0223(4) Uani 1 1 d . . . C68 C 0.78458(17) -0.01567(15) 0.33776(15) 0.0208(4) Uani 1 1 d . . . C69 C 0.93309(18) -0.11326(16) 0.36210(17) 0.0266(5) Uani 1 1 d . . . H69A H 0.9412 -0.1787 0.3271 0.032 Uiso 1 1 calc R . . H69B H 0.9764 -0.1227 0.4149 0.032 Uiso 1 1 calc R . . C70 C 0.96966(17) -0.01723(16) 0.28565(15) 0.0220(4) Uani 1 1 d . . . H70 H 1.0217 -0.0401 0.2221 0.026 Uiso 1 1 calc R . . C71 C 1.02216(17) 0.06804(17) 0.32884(16) 0.0237(4) Uani 1 1 d . . . H71 H 1.0237 0.1347 0.2813 0.028 Uiso 1 1 calc R . . C72 C 0.95715(19) 0.09320(18) 0.43569(16) 0.0282(5) Uani 1 1 d . . . H72A H 0.8803 0.1129 0.4343 0.042 Uiso 1 1 calc R . . H72B H 0.9906 0.1523 0.4563 0.042 Uiso 1 1 calc R . . H72C H 0.9589 0.0306 0.4850 0.042 Uiso 1 1 calc R . . C73 C 1.14137(19) 0.0343(2) 0.32943(19) 0.0347(5) Uani 1 1 d . . . H73A H 1.1429 -0.0345 0.3701 0.052 Uiso 1 1 calc R . . H73B H 1.1735 0.0874 0.3597 0.052 Uiso 1 1 calc R . . H73C H 1.1844 0.0285 0.2589 0.052 Uiso 1 1 calc R . . C74 C 0.59558(19) -0.01247(17) 0.45067(17) 0.0301(5) Uani 1 1 d . . . H74 H 0.6237 -0.0440 0.5067 0.036 Uiso 1 1 calc R . . C75 C 0.4844(2) 0.0100(2) 0.46430(19) 0.0373(6) Uani 1 1 d . . . H75 H 0.4356 -0.0028 0.5303 0.045 Uiso 1 1 calc R . . C76 C 0.44328(19) 0.05225(19) 0.37957(19) 0.0346(5) Uani 1 1 d . . . H76 H 0.3658 0.0650 0.3889 0.042 Uiso 1 1 calc R . . C77 C 0.51201(18) 0.07585(17) 0.28298(18) 0.0281(5) Uani 1 1 d . . . C78 C 0.46939(19) 0.11692(19) 0.1910(2) 0.0355(5) Uani 1 1 d . . . H78A H 0.4998 0.1864 0.1634 0.053 Uiso 1 1 calc R . . H78B H 0.3885 0.1238 0.2111 0.053 Uiso 1 1 calc R . . H78C H 0.4920 0.0674 0.1385 0.053 Uiso 1 1 calc R . . O1S O 0.58858(16) 0.52689(18) 0.97768(17) 0.0589(6) Uani 1 1 d D . . C1S C 0.5257(3) 0.4845(3) 0.9167(3) 0.0611(9) Uani 1 1 d D . . H1SA H 0.4939 0.4166 0.9512 0.073 Uiso 1 1 calc R . . H1SB H 0.5737 0.4715 0.8487 0.073 Uiso 1 1 calc R . . C2S C 0.4355(2) 0.5642(2) 0.90439(19) 0.0385(6) Uani 1 1 d D . . H2SA H 0.3652 0.5293 0.9104 0.046 Uiso 1 1 calc R . . H2SB H 0.4553 0.6075 0.8372 0.046 Uiso 1 1 calc R . . C3S C 0.4265(2) 0.6310(2) 0.99148(19) 0.0373(6) Uani 1 1 d D . . H3SA H 0.3986 0.7040 0.9749 0.045 Uiso 1 1 calc R . . H3SB H 0.3776 0.5991 1.0557 0.045 Uiso 1 1 calc R . . C4S C 0.5445(2) 0.6298(2) 0.9995(2) 0.0449(7) Uani 1 1 d D . . H4SA H 0.5862 0.6847 0.9494 0.054 Uiso 1 1 calc R . . H4SB H 0.5478 0.6432 1.0694 0.054 Uiso 1 1 calc R . . O2S O 0.5895(8) 0.1542(8) 0.8745(8) 0.178(4) Uiso 0.563(9) 1 d PDU A 1 C5S C 0.6510(9) 0.1058(9) 0.7772(8) 0.123(4) Uiso 0.563(9) 1 d PDU A 1 H5S1 H 0.6279 0.1441 0.7174 0.148 Uiso 0.563(9) 1 calc PR A 1 H5S2 H 0.7315 0.1139 0.7666 0.148 Uiso 0.563(9) 1 calc PR A 1 C6S C 0.6279(11) -0.0092(10) 0.7841(12) 0.157(5) Uiso 0.563(9) 1 d PDU A 1 H6S1 H 0.6339 -0.0307 0.7148 0.188 Uiso 0.563(9) 1 calc PR A 1 H6S2 H 0.6820 -0.0528 0.8153 0.188 Uiso 0.563(9) 1 calc PR A 1 C7S C 0.5236(11) -0.0238(10) 0.8434(11) 0.158(5) Uiso 0.563(9) 1 d PDU A 1 H7S1 H 0.5187 -0.0918 0.8879 0.190 Uiso 0.563(9) 1 calc PR A 1 H7S2 H 0.4688 -0.0213 0.8012 0.190 Uiso 0.563(9) 1 calc PR A 1 C8S C 0.5091(9) 0.0677(9) 0.9035(9) 0.136(4) Uiso 0.563(9) 1 d PDU A 1 H8S1 H 0.5073 0.0398 0.9753 0.163 Uiso 0.563(9) 1 calc PR A 1 H8S2 H 0.4351 0.1006 0.9033 0.163 Uiso 0.563(9) 1 calc PR A 1 O2S' O 0.6725(14) 0.1211(15) 0.6708(14) 0.257(8) Uiso 0.437(9) 1 d PDU A 2 C5S' C 0.6232(17) 0.0228(15) 0.7293(19) 0.199(9) Uiso 0.437(9) 1 d PDU A 2 H5S3 H 0.6347 -0.0355 0.6846 0.239 Uiso 0.437(9) 1 calc PR A 2 H5S4 H 0.6572 0.0008 0.7876 0.239 Uiso 0.437(9) 1 calc PR A 2 C6S' C 0.5036(15) 0.0486(17) 0.7670(18) 0.197(9) Uiso 0.437(9) 1 d PDU A 2 H6S3 H 0.4628 -0.0105 0.8118 0.237 Uiso 0.437(9) 1 calc PR A 2 H6S4 H 0.4670 0.0739 0.7110 0.237 Uiso 0.437(9) 1 calc PR A 2 C7S' C 0.5233(19) 0.135(2) 0.825(2) 0.251(10) Uiso 0.437(9) 1 d PDU A 2 H7S3 H 0.4582 0.1852 0.8382 0.301 Uiso 0.437(9) 1 calc PR A 2 H7S4 H 0.5387 0.1063 0.8913 0.301 Uiso 0.437(9) 1 calc PR A 2 C8S' C 0.6210(17) 0.1898(16) 0.7576(17) 0.197(8) Uiso 0.437(9) 1 d PDU A 2 H8S3 H 0.6755 0.1994 0.7976 0.236 Uiso 0.437(9) 1 calc PR A 2 H8S4 H 0.5981 0.2605 0.7290 0.236 Uiso 0.437(9) 1 calc PR A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Al1 0.0175(3) 0.0162(3) 0.0184(3) -0.0034(2) -0.0038(2) -0.0016(2) O1 0.0230(7) 0.0188(7) 0.0214(7) -0.0057(6) -0.0043(6) -0.0010(6) N1 0.0201(9) 0.0205(9) 0.0190(8) -0.0041(7) -0.0050(7) -0.0021(7) C1 0.0284(11) 0.0181(10) 0.0231(10) -0.0045(8) -0.0106(9) 0.0064(8) Al2 0.0169(3) 0.0139(3) 0.0195(3) -0.0030(2) -0.0016(2) -0.0010(2) O2 0.0242(8) 0.0359(9) 0.0278(8) -0.0069(7) 0.0016(6) -0.0060(7) N2 0.0200(9) 0.0161(8) 0.0231(9) -0.0014(7) -0.0053(7) -0.0021(7) C2 0.0264(11) 0.0225(10) 0.0210(10) -0.0049(8) -0.0070(8) 0.0063(8) O3 0.0221(7) 0.0192(7) 0.0174(7) -0.0036(5) -0.0043(6) -0.0029(6) N3 0.0198(8) 0.0201(9) 0.0181(8) -0.0030(7) -0.0047(7) -0.0017(7) C3 0.0205(10) 0.0239(11) 0.0239(10) 0.0000(8) -0.0036(8) -0.0005(8) O4 0.0332(9) 0.0227(8) 0.0209(7) 0.0023(6) -0.0067(6) -0.0071(6) N4 0.0191(9) 0.0163(8) 0.0231(8) -0.0056(7) -0.0027(7) 0.0013(7) C4 0.0261(12) 0.0340(12) 0.0297(12) -0.0058(9) -0.0025(9) -0.0084(10) O5 0.0222(7) 0.0206(7) 0.0172(7) -0.0029(5) -0.0047(6) -0.0022(6) N5 0.0173(8) 0.0153(8) 0.0207(8) -0.0032(6) -0.0029(7) -0.0004(6) C5 0.0194(10) 0.0226(10) 0.0259(10) -0.0032(8) -0.0060(8) -0.0040(8) O6 0.0211(7) 0.0310(8) 0.0271(8) -0.0046(6) -0.0089(6) -0.0043(6) N6 0.0193(9) 0.0154(8) 0.0200(8) -0.0047(6) -0.0025(7) 0.0005(7) C6 0.0215(11) 0.0293(11) 0.0252(10) -0.0042(9) -0.0065(9) -0.0056(9) O7 0.0181(7) 0.0157(7) 0.0252(7) -0.0045(5) -0.0013(6) -0.0013(5) C7 0.0240(12) 0.0344(12) 0.0357(12) -0.0031(10) -0.0088(10) -0.0003(9) O8 0.0294(8) 0.0146(7) 0.0368(9) -0.0051(6) -0.0009(7) -0.0006(6) C8 0.0368(13) 0.0360(13) 0.0363(13) -0.0059(10) -0.0156(11) -0.0110(11) O9 0.0231(7) 0.0192(7) 0.0226(7) -0.0021(6) -0.0031(6) 0.0008(6) C9 0.0318(12) 0.0330(13) 0.0242(11) -0.0058(9) -0.0046(9) 0.0070(10) O10 0.0290(8) 0.0184(7) 0.0201(7) -0.0050(6) -0.0010(6) 0.0004(6) C10 0.0473(15) 0.0373(14) 0.0268(12) -0.0131(10) -0.0091(11) 0.0130(11) O11 0.0173(7) 0.0196(7) 0.0242(7) -0.0027(6) -0.0016(6) -0.0014(6) C11 0.0521(16) 0.0259(12) 0.0315(12) -0.0124(9) -0.0183(11) 0.0086(11) O12 0.0309(8) 0.0193(7) 0.0271(8) 0.0029(6) -0.0053(6) -0.0013(6) C12 0.0361(13) 0.0203(10) 0.0314(12) -0.0061(9) -0.0163(10) 0.0054(9) C13 0.0433(14) 0.0245(12) 0.0443(14) -0.0156(10) -0.0163(11) -0.0027(10) C14 0.0140(9) 0.0208(10) 0.0174(9) -0.0056(7) -0.0003(7) 0.0000(7) C15 0.0170(10) 0.0223(10) 0.0198(9) -0.0057(8) -0.0016(8) -0.0014(8) C16 0.0158(9) 0.0224(10) 0.0185(10) -0.0001(8) -0.0036(8) 0.0000(8) C17 0.0312(12) 0.0227(11) 0.0306(11) 0.0026(9) -0.0087(10) -0.0088(9) C18 0.0301(12) 0.0169(10) 0.0298(11) -0.0001(8) -0.0122(9) -0.0052(8) C19 0.0331(12) 0.0219(11) 0.0326(12) -0.0032(9) -0.0128(10) 0.0001(9) C20 0.0297(13) 0.0304(12) 0.0394(13) -0.0018(10) -0.0116(10) 0.0012(10) C21 0.0534(17) 0.0252(13) 0.077(2) -0.0117(13) -0.0334(16) 0.0039(12) C22 0.0237(11) 0.0285(11) 0.0186(10) -0.0042(8) -0.0031(8) 0.0019(9) C23 0.0341(12) 0.0293(12) 0.0224(10) -0.0121(9) -0.0080(9) 0.0015(9) C24 0.0299(12) 0.0233(11) 0.0264(11) -0.0107(9) -0.0046(9) -0.0019(9) C25 0.0163(10) 0.0203(10) 0.0236(10) -0.0074(8) -0.0003(8) -0.0010(8) C26 0.0294(12) 0.0182(10) 0.0255(10) -0.0057(8) -0.0022(9) -0.0022(8) C27 0.0268(11) 0.0137(9) 0.0184(9) -0.0048(7) -0.0076(8) 0.0050(8) C28 0.0267(11) 0.0138(9) 0.0225(10) -0.0041(8) -0.0083(8) 0.0041(8) C29 0.0193(10) 0.0141(9) 0.0258(10) -0.0037(8) -0.0072(8) 0.0003(8) C30 0.0237(11) 0.0374(13) 0.0254(11) -0.0051(9) -0.0041(9) -0.0072(9) C31 0.0175(10) 0.0254(11) 0.0220(10) 0.0016(8) -0.0031(8) -0.0031(8) C32 0.0203(10) 0.0262(11) 0.0232(10) -0.0037(8) -0.0035(8) -0.0023(8) C33 0.0399(14) 0.0290(12) 0.0321(12) -0.0041(10) -0.0049(10) 0.0076(10) C34 0.0276(12) 0.0457(14) 0.0283(12) -0.0085(10) 0.0000(10) -0.0053(10) C35 0.0330(12) 0.0168(10) 0.0291(11) -0.0072(8) -0.0145(9) 0.0042(9) C36 0.0398(13) 0.0246(11) 0.0238(10) -0.0092(9) -0.0167(10) 0.0080(9) C37 0.0416(13) 0.0267(11) 0.0159(10) -0.0045(8) -0.0071(9) 0.0075(10) C38 0.0293(11) 0.0184(10) 0.0196(10) -0.0049(8) -0.0036(8) 0.0053(8) C39 0.0355(13) 0.0296(12) 0.0195(10) -0.0026(9) -0.0008(9) 0.0015(10) C40 0.0231(10) 0.0193(10) 0.0157(9) -0.0026(7) -0.0036(8) -0.0034(8) C41 0.0237(11) 0.0191(10) 0.0230(10) -0.0009(8) -0.0035(8) -0.0022(8) C42 0.0246(11) 0.0145(9) 0.0240(10) -0.0054(8) -0.0034(8) 0.0007(8) C43 0.0270(12) 0.0198(10) 0.0327(11) -0.0053(9) -0.0018(9) 0.0045(9) C44 0.0215(11) 0.0163(10) 0.0271(11) -0.0071(8) -0.0003(8) 0.0029(8) C45 0.0265(11) 0.0204(10) 0.0271(11) -0.0039(8) -0.0012(9) -0.0006(9) C46 0.0314(13) 0.0367(13) 0.0333(13) -0.0103(10) 0.0020(10) 0.0040(10) C47 0.0385(14) 0.0272(12) 0.0343(13) -0.0087(10) -0.0068(10) -0.0032(10) C48 0.0328(12) 0.0203(10) 0.0261(11) -0.0021(8) -0.0061(9) -0.0054(9) C49 0.0300(12) 0.0304(12) 0.0293(11) 0.0008(9) -0.0067(10) -0.0145(10) C50 0.0180(10) 0.0384(13) 0.0235(10) -0.0007(9) -0.0044(8) -0.0091(9) C51 0.0228(11) 0.0273(11) 0.0173(10) -0.0020(8) -0.0022(8) -0.0028(9) C52 0.0186(11) 0.0352(13) 0.0360(12) -0.0098(10) 0.0016(9) 0.0008(9) C53 0.0178(10) 0.0225(10) 0.0215(10) -0.0009(8) -0.0018(8) -0.0025(8) C54 0.0195(10) 0.0213(10) 0.0213(10) -0.0023(8) -0.0038(8) -0.0022(8) C55 0.0171(10) 0.0178(10) 0.0220(10) -0.0053(8) -0.0033(8) 0.0000(8) C56 0.0238(11) 0.0162(10) 0.0251(10) -0.0020(8) -0.0017(8) 0.0004(8) C57 0.0227(10) 0.0158(9) 0.0220(10) -0.0030(8) -0.0047(8) -0.0011(8) C58 0.0231(11) 0.0183(10) 0.0265(10) -0.0056(8) 0.0008(8) -0.0039(8) C59 0.0288(12) 0.0226(11) 0.0326(12) -0.0025(9) 0.0054(9) -0.0069(9) C60 0.0220(11) 0.0313(12) 0.0420(13) -0.0077(10) -0.0080(10) -0.0040(9) C61 0.0280(11) 0.0246(11) 0.0246(11) -0.0036(9) -0.0022(9) -0.0029(9) C62 0.0375(13) 0.0331(12) 0.0206(11) -0.0010(9) -0.0004(9) -0.0054(10) C63 0.0379(13) 0.0263(12) 0.0255(11) 0.0081(9) -0.0040(10) -0.0047(10) C64 0.0264(11) 0.0226(11) 0.0288(11) 0.0018(9) -0.0061(9) -0.0032(9) C65 0.0402(14) 0.0255(12) 0.0326(12) 0.0079(10) -0.0007(10) 0.0039(10) C66 0.0208(10) 0.0134(9) 0.0287(11) -0.0056(8) 0.0012(8) -0.0021(8) C67 0.0226(10) 0.0160(9) 0.0256(10) -0.0052(8) 0.0019(8) -0.0053(8) C68 0.0293(11) 0.0120(9) 0.0210(10) -0.0039(7) -0.0046(8) -0.0023(8) C69 0.0309(12) 0.0210(11) 0.0285(11) -0.0046(9) -0.0091(9) 0.0050(9) C70 0.0222(10) 0.0219(10) 0.0217(10) -0.0067(8) -0.0044(8) 0.0050(8) C71 0.0215(11) 0.0243(11) 0.0252(11) -0.0040(8) -0.0051(9) 0.0012(8) C72 0.0310(12) 0.0286(12) 0.0265(11) -0.0065(9) -0.0086(9) -0.0003(9) C73 0.0268(12) 0.0434(14) 0.0369(13) -0.0101(11) -0.0115(10) 0.0006(10) C74 0.0329(13) 0.0262(11) 0.0274(11) -0.0033(9) 0.0022(9) -0.0101(10) C75 0.0307(13) 0.0397(14) 0.0346(13) -0.0077(11) 0.0096(10) -0.0118(11) C76 0.0171(11) 0.0319(12) 0.0483(15) -0.0087(11) 0.0076(10) -0.0047(9) C77 0.0218(11) 0.0202(11) 0.0402(13) -0.0079(9) -0.0011(9) -0.0011(9) C78 0.0211(11) 0.0316(13) 0.0520(15) -0.0036(11) -0.0069(11) 0.0029(9) O1S 0.0366(11) 0.0708(14) 0.0748(15) -0.0250(12) -0.0194(10) 0.0117(10) C1S 0.060(2) 0.072(2) 0.0599(19) -0.0347(17) -0.0237(16) 0.0216(16) C2S 0.0357(14) 0.0442(14) 0.0364(13) -0.0052(11) -0.0078(11) -0.0089(11) C3S 0.0375(14) 0.0381(14) 0.0368(13) -0.0084(11) -0.0083(11) 0.0016(11) C4S 0.0433(16) 0.0511(17) 0.0399(14) -0.0083(12) -0.0039(12) -0.0163(13) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Al1 O3 1.8209(14) . ? Al1 O1 1.8413(14) . ? Al1 O5 1.8523(14) . ? Al1 N2 2.0278(18) . ? Al1 N1 2.0457(17) . ? Al1 N3 2.0500(17) . ? O1 C1 1.318(2) . ? N1 C3 1.287(3) . ? N1 C5 1.489(2) . ? C1 C2 1.408(3) . ? C1 C12 1.418(3) . ? Al2 O11 1.8356(14) . ? Al2 O9 1.8418(15) . ? Al2 O7 1.8450(14) . ? Al2 N6 2.0335(17) . ? Al2 N5 2.0369(17) . ? Al2 N4 2.0490(17) . ? O2 C3 1.349(3) . ? O2 C4 1.455(3) . ? N2 C16 1.289(3) . ? N2 C18 1.496(2) . ? C2 C9 1.406(3) . ? C2 C3 1.454(3) . ? O3 C14 1.309(2) . ? N3 C29 1.290(2) . ? N3 C31 1.483(2) . ? O4 C16 1.347(2) . ? O4 C17 1.465(2) . ? N4 C42 1.289(3) . ? N4 C44 1.492(2) . ? C4 C5 1.524(3) . ? O5 C27 1.304(2) . ? N5 C55 1.293(3) . ? N5 C57 1.488(2) . ? C5 C6 1.537(3) . ? O6 C29 1.355(2) . ? O6 C30 1.448(3) . ? N6 C68 1.291(3) . ? N6 C70 1.489(3) . ? C6 C7 1.527(3) . ? C6 C8 1.528(3) . ? O7 C40 1.314(2) . ? O8 C42 1.355(2) . ? O8 C43 1.460(3) . ? O9 C53 1.306(2) . ? C9 C10 1.367(3) . ? O10 C55 1.354(2) . ? O10 C56 1.451(2) . ? C10 C11 1.398(4) . ? O11 C66 1.308(2) . ? C11 C12 1.383(3) . ? O12 C68 1.351(2) . ? O12 C69 1.464(3) . ? C12 C13 1.492(3) . ? C14 C15 1.409(3) . ? C14 C25 1.426(3) . ? C15 C22 1.404(3) . ? C15 C16 1.452(3) . ? C17 C18 1.530(3) . ? C18 C19 1.535(3) . ? C19 C21 1.526(3) . ? C19 C20 1.533(3) . ? C22 C23 1.381(3) . ? C23 C24 1.393(3) . ? C24 C25 1.385(3) . ? C25 C26 1.502(3) . ? C27 C28 1.417(3) . ? C27 C38 1.425(3) . ? C28 C35 1.406(3) . ? C28 C29 1.447(3) . ? C30 C31 1.538(3) . ? C31 C32 1.537(3) . ? C32 C33 1.525(3) . ? C32 C34 1.529(3) . ? C35 C36 1.370(3) . ? C36 C37 1.393(3) . ? C37 C38 1.379(3) . ? C38 C39 1.503(3) . ? C40 C41 1.411(3) . ? C40 C51 1.421(3) . ? C41 C48 1.404(3) . ? C41 C42 1.453(3) . ? C43 C44 1.534(3) . ? C44 C45 1.538(3) . ? C45 C47 1.521(3) . ? C45 C46 1.525(3) . ? C48 C49 1.365(3) . ? C49 C50 1.398(3) . ? C50 C51 1.381(3) . ? C51 C52 1.499(3) . ? C53 C54 1.407(3) . ? C53 C64 1.424(3) . ? C54 C61 1.411(3) . ? C54 C55 1.448(3) . ? C56 C57 1.537(3) . ? C57 C58 1.532(3) . ? C58 C60 1.519(3) . ? C58 C59 1.532(3) . ? C61 C62 1.372(3) . ? C62 C63 1.393(3) . ? C63 C64 1.384(3) . ? C64 C65 1.496(3) . ? C66 C67 1.418(3) . ? C66 C77 1.423(3) . ? C67 C74 1.406(3) . ? C67 C68 1.439(3) . ? C69 C70 1.521(3) . ? C70 C71 1.539(3) . ? C71 C73 1.524(3) . ? C71 C72 1.529(3) . ? C74 C75 1.370(3) . ? C75 C76 1.406(4) . ? C76 C77 1.385(3) . ? C77 C78 1.498(3) . ? O1S C4S 1.420(3) . ? O1S C1S 1.437(4) . ? C1S C2S 1.492(4) . ? C2S C3S 1.506(3) . ? C3S C4S 1.502(4) . ? O2S C8S 1.489(11) . ? O2S C5S 1.524(11) . ? C5S C6S 1.495(12) . ? C6S C7S 1.360(12) . ? C7S C8S 1.470(11) . ? O2S' C5S' 1.482(14) . ? O2S' C8S' 1.530(14) . ? C5S' C6S' 1.481(14) . ? C6S' C7S' 1.490(16) . ? C7S' C8S' 1.484(14) . ? 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 O3 Al1 O1 175.54(7) . . ? O3 Al1 O5 89.52(6) . . ? O1 Al1 O5 94.85(6) . . ? O3 Al1 N2 87.90(7) . . ? O1 Al1 N2 87.79(7) . . ? O5 Al1 N2 175.64(7) . . ? O3 Al1 N1 91.69(7) . . ? O1 Al1 N1 87.68(7) . . ? O5 Al1 N1 86.47(7) . . ? N2 Al1 N1 97.11(7) . . ? O3 Al1 N3 94.49(7) . . ? O1 Al1 N3 86.69(7) . . ? O5 Al1 N3 86.74(7) . . ? N2 Al1 N3 89.96(7) . . ? N1 Al1 N3 170.78(7) . . ? C1 O1 Al1 128.51(13) . . ? C3 N1 C5 107.34(16) . . ? C3 N1 Al1 119.72(13) . . ? C5 N1 Al1 129.03(13) . . ? O1 C1 C2 122.78(18) . . ? O1 C1 C12 118.47(19) . . ? C2 C1 C12 118.75(19) . . ? O11 Al2 O9 90.51(7) . . ? O11 Al2 O7 174.64(7) . . ? O9 Al2 O7 94.81(7) . . ? O11 Al2 N6 87.23(7) . . ? O9 Al2 N6 177.51(7) . . ? O7 Al2 N6 87.45(7) . . ? O11 Al2 N5 93.39(7) . . ? O9 Al2 N5 88.12(7) . . ? O7 Al2 N5 86.12(6) . . ? N6 Al2 N5 90.97(7) . . ? O11 Al2 N4 92.71(7) . . ? O9 Al2 N4 86.01(7) . . ? O7 Al2 N4 88.33(7) . . ? N6 Al2 N4 95.13(7) . . ? N5 Al2 N4 171.57(7) . . ? C3 O2 C4 105.71(15) . . ? C16 N2 C18 107.39(16) . . ? C16 N2 Al1 126.13(14) . . ? C18 N2 Al1 126.16(13) . . ? C9 C2 C1 120.50(19) . . ? C9 C2 C3 119.7(2) . . ? C1 C2 C3 119.81(18) . . ? C14 O3 Al1 134.44(13) . . ? C29 N3 C31 108.51(16) . . ? C29 N3 Al1 120.30(13) . . ? C31 N3 Al1 131.02(13) . . ? N1 C3 O2 116.36(18) . . ? N1 C3 C2 127.10(19) . . ? O2 C3 C2 116.53(18) . . ? C16 O4 C17 105.68(15) . . ? C42 N4 C44 107.49(16) . . ? C42 N4 Al2 121.66(14) . . ? C44 N4 Al2 127.03(12) . . ? O2 C4 C5 103.55(16) . . ? C27 O5 Al1 127.29(12) . . ? C55 N5 C57 107.63(16) . . ? C55 N5 Al2 122.50(13) . . ? C57 N5 Al2 129.85(12) . . ? N1 C5 C4 101.99(16) . . ? N1 C5 C6 110.55(16) . . ? C4 C5 C6 115.23(18) . . ? C29 O6 C30 106.79(15) . . ? C68 N6 C70 107.32(17) . . ? C68 N6 Al2 126.16(14) . . ? C70 N6 Al2 126.37(12) . . ? C7 C6 C8 111.32(19) . . ? C7 C6 C5 112.68(17) . . ? C8 C6 C5 110.23(18) . . ? C40 O7 Al2 132.98(13) . . ? C42 O8 C43 105.52(15) . . ? C53 O9 Al2 129.49(13) . . ? C10 C9 C2 120.6(2) . . ? C55 O10 C56 105.88(14) . . ? C9 C10 C11 118.8(2) . . ? C66 O11 Al2 134.89(14) . . ? C12 C11 C10 122.7(2) . . ? C68 O12 C69 105.09(15) . . ? C11 C12 C1 118.6(2) . . ? C11 C12 C13 122.4(2) . . ? C1 C12 C13 119.0(2) . . ? O3 C14 C15 123.46(17) . . ? O3 C14 C25 117.81(17) . . ? C15 C14 C25 118.71(17) . . ? C22 C15 C14 120.67(18) . . ? C22 C15 C16 120.78(18) . . ? C14 C15 C16 118.55(17) . . ? N2 C16 O4 116.67(17) . . ? N2 C16 C15 126.30(18) . . ? O4 C16 C15 117.03(17) . . ? O4 C17 C18 103.55(15) . . ? N2 C18 C17 101.74(16) . . ? N2 C18 C19 111.96(17) . . ? C17 C18 C19 114.70(18) . . ? C21 C19 C20 110.43(19) . . ? C21 C19 C18 110.06(19) . . ? C20 C19 C18 113.46(18) . . ? C23 C22 C15 120.07(19) . . ? C22 C23 C24 119.54(19) . . ? C25 C24 C23 122.13(19) . . ? C24 C25 C14 118.83(19) . . ? C24 C25 C26 123.27(18) . . ? C14 C25 C26 117.89(17) . . ? O5 C27 C28 122.42(17) . . ? O5 C27 C38 118.90(18) . . ? C28 C27 C38 118.66(17) . . ? C35 C28 C27 120.35(18) . . ? C35 C28 C29 120.53(18) . . ? C27 C28 C29 118.70(17) . . ? N3 C29 O6 116.24(17) . . ? N3 C29 C28 127.49(18) . . ? O6 C29 C28 116.21(16) . . ? O6 C30 C31 104.99(16) . . ? N3 C31 C32 112.61(16) . . ? N3 C31 C30 102.47(16) . . ? C32 C31 C30 114.75(18) . . ? C33 C32 C34 111.10(19) . . ? C33 C32 C31 112.79(17) . . ? C34 C32 C31 110.43(17) . . ? C36 C35 C28 120.1(2) . . ? C35 C36 C37 119.81(19) . . ? C38 C37 C36 122.25(19) . . ? C37 C38 C27 118.78(19) . . ? C37 C38 C39 122.96(19) . . ? C27 C38 C39 118.25(18) . . ? O7 C40 C41 123.50(18) . . ? O7 C40 C51 117.70(18) . . ? C41 C40 C51 118.79(18) . . ? C48 C41 C40 119.91(19) . . ? C48 C41 C42 120.58(19) . . ? C40 C41 C42 119.44(17) . . ? N4 C42 O8 116.33(18) . . ? N4 C42 C41 127.20(18) . . ? O8 C42 C41 116.45(17) . . ? O8 C43 C44 103.45(16) . . ? N4 C44 C43 101.46(16) . . ? N4 C44 C45 110.86(17) . . ? C43 C44 C45 115.00(17) . . ? C47 C45 C46 111.48(18) . . ? C47 C45 C44 113.36(18) . . ? C46 C45 C44 110.33(18) . . ? C49 C48 C41 121.0(2) . . ? C48 C49 C50 119.33(19) . . ? C51 C50 C49 121.8(2) . . ? C50 C51 C40 119.1(2) . . ? C50 C51 C52 122.57(19) . . ? C40 C51 C52 118.33(18) . . ? O9 C53 C54 123.16(18) . . ? O9 C53 C64 118.11(18) . . ? C54 C53 C64 118.71(18) . . ? C53 C54 C61 120.50(18) . . ? C53 C54 C55 119.53(17) . . ? C61 C54 C55 119.87(18) . . ? N5 C55 O10 116.70(17) . . ? N5 C55 C54 126.98(18) . . ? O10 C55 C54 116.29(16) . . ? O10 C56 C57 104.51(15) . . ? N5 C57 C58 112.13(16) . . ? N5 C57 C56 102.04(15) . . ? C58 C57 C56 115.11(16) . . ? C60 C58 C59 112.18(18) . . ? C60 C58 C57 112.62(17) . . ? C59 C58 C57 110.18(17) . . ? C62 C61 C54 120.3(2) . . ? C61 C62 C63 119.3(2) . . ? C64 C63 C62 122.4(2) . . ? C63 C64 C53 118.7(2) . . ? C63 C64 C65 123.3(2) . . ? C53 C64 C65 117.93(19) . . ? O11 C66 C67 122.96(18) . . ? O11 C66 C77 118.86(19) . . ? C67 C66 C77 118.16(18) . . ? C74 C67 C66 120.9(2) . . ? C74 C67 C68 120.7(2) . . ? C66 C67 C68 118.40(17) . . ? N6 C68 O12 116.07(18) . . ? N6 C68 C67 126.56(19) . . ? O12 C68 C67 117.37(17) . . ? O12 C69 C70 103.37(15) . . ? N6 C70 C69 101.17(16) . . ? N6 C70 C71 111.05(16) . . ? C69 C70 C71 113.98(17) . . ? C73 C71 C72 110.60(18) . . ? C73 C71 C70 109.73(17) . . ? C72 C71 C70 113.32(17) . . ? C75 C74 C67 120.2(2) . . ? C74 C75 C76 119.3(2) . . ? C77 C76 C75 122.2(2) . . ? C76 C77 C66 118.9(2) . . ? C76 C77 C78 122.9(2) . . ? C66 C77 C78 118.16(19) . . ? C4S O1S C1S 108.5(2) . . ? O1S C1S C2S 107.4(2) . . ? C1S C2S C3S 103.3(2) . . ? C4S C3S C2S 101.9(2) . . ? O1S C4S C3S 105.4(2) . . ? C8S O2S C5S 92.2(8) . . ? C6S C5S O2S 111.0(9) . . ? C7S C6S C5S 107.9(10) . . ? C6S C7S C8S 100.6(9) . . ? C7S C8S O2S 120.5(9) . . ? C5S' O2S' C8S' 93.5(13) . . ? C6S' C5S' O2S' 106.0(15) . . ? C5S' C6S' C7S' 93.2(13) . . ? C8S' C7S' C6S' 105.1(13) . . ? C7S' C8S' O2S' 108.2(12) . . ? 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 O3 Al1 O1 C1 -121.1(9) . . . . ? O5 Al1 O1 C1 47.01(16) . . . . ? N2 Al1 O1 C1 -136.45(16) . . . . ? N1 Al1 O1 C1 -39.25(16) . . . . ? N3 Al1 O1 C1 133.45(16) . . . . ? O3 Al1 N1 C3 -148.29(16) . . . . ? O1 Al1 N1 C3 36.13(16) . . . . ? O5 Al1 N1 C3 -58.88(16) . . . . ? N2 Al1 N1 C3 123.62(16) . . . . ? N3 Al1 N1 C3 -16.2(5) . . . . ? O3 Al1 N1 C5 6.49(16) . . . . ? O1 Al1 N1 C5 -169.08(16) . . . . ? O5 Al1 N1 C5 95.90(16) . . . . ? N2 Al1 N1 C5 -81.60(16) . . . . ? N3 Al1 N1 C5 138.6(4) . . . . ? Al1 O1 C1 C2 26.8(3) . . . . ? Al1 O1 C1 C12 -153.14(15) . . . . ? O3 Al1 N2 C16 -2.57(17) . . . . ? O1 Al1 N2 C16 176.25(17) . . . . ? O5 Al1 N2 C16 -56.2(10) . . . . ? N1 Al1 N2 C16 88.87(17) . . . . ? N3 Al1 N2 C16 -97.06(17) . . . . ? O3 Al1 N2 C18 170.07(16) . . . . ? O1 Al1 N2 C18 -11.11(16) . . . . ? O5 Al1 N2 C18 116.4(9) . . . . ? N1 Al1 N2 C18 -98.49(16) . . . . ? N3 Al1 N2 C18 75.57(16) . . . . ? O1 C1 C2 C9 -178.97(19) . . . . ? C12 C1 C2 C9 1.0(3) . . . . ? O1 C1 C2 C3 2.3(3) . . . . ? C12 C1 C2 C3 -177.69(19) . . . . ? O1 Al1 O3 C14 2.2(10) . . . . ? O5 Al1 O3 C14 -165.99(17) . . . . ? N2 Al1 O3 C14 17.52(18) . . . . ? N1 Al1 O3 C14 -79.53(18) . . . . ? N3 Al1 O3 C14 107.32(17) . . . . ? O3 Al1 N3 C29 122.45(15) . . . . ? O1 Al1 N3 C29 -61.86(15) . . . . ? O5 Al1 N3 C29 33.19(15) . . . . ? N2 Al1 N3 C29 -149.66(15) . . . . ? N1 Al1 N3 C29 -9.5(5) . . . . ? O3 Al1 N3 C31 -62.94(17) . . . . ? O1 Al1 N3 C31 112.75(17) . . . . ? O5 Al1 N3 C31 -152.20(17) . . . . ? N2 Al1 N3 C31 24.95(17) . . . . ? N1 Al1 N3 C31 165.1(4) . . . . ? C5 N1 C3 O2 -3.1(2) . . . . ? Al1 N1 C3 O2 156.59(14) . . . . ? C5 N1 C3 C2 176.0(2) . . . . ? Al1 N1 C3 C2 -24.3(3) . . . . ? C4 O2 C3 N1 -11.7(2) . . . . ? C4 O2 C3 C2 169.06(18) . . . . ? C9 C2 C3 N1 -179.4(2) . . . . ? C1 C2 C3 N1 -0.7(3) . . . . ? C9 C2 C3 O2 -0.2(3) . . . . ? C1 C2 C3 O2 178.48(18) . . . . ? O11 Al2 N4 C42 -157.70(16) . . . . ? O9 Al2 N4 C42 -67.38(17) . . . . ? O7 Al2 N4 C42 27.56(17) . . . . ? N6 Al2 N4 C42 114.85(17) . . . . ? N5 Al2 N4 C42 -21.3(6) . . . . ? O11 Al2 N4 C44 -2.57(17) . . . . ? O9 Al2 N4 C44 87.75(16) . . . . ? O7 Al2 N4 C44 -177.31(16) . . . . ? N6 Al2 N4 C44 -90.03(16) . . . . ? N5 Al2 N4 C44 133.8(5) . . . . ? C3 O2 C4 C5 20.5(2) . . . . ? O3 Al1 O5 C27 -139.07(16) . . . . ? O1 Al1 O5 C27 41.85(16) . . . . ? N2 Al1 O5 C27 -85.5(9) . . . . ? N1 Al1 O5 C27 129.21(16) . . . . ? N3 Al1 O5 C27 -44.54(16) . . . . ? O11 Al2 N5 C55 115.33(16) . . . . ? O9 Al2 N5 C55 24.93(16) . . . . ? O7 Al2 N5 C55 -70.02(16) . . . . ? N6 Al2 N5 C55 -157.39(16) . . . . ? N4 Al2 N5 C55 -21.0(6) . . . . ? O11 Al2 N5 C57 -66.91(16) . . . . ? O9 Al2 N5 C57 -157.31(16) . . . . ? O7 Al2 N5 C57 107.75(16) . . . . ? N6 Al2 N5 C57 20.37(17) . . . . ? N4 Al2 N5 C57 156.8(4) . . . . ? C3 N1 C5 C4 15.7(2) . . . . ? Al1 N1 C5 C4 -141.54(15) . . . . ? C3 N1 C5 C6 -107.37(19) . . . . ? Al1 N1 C5 C6 95.44(19) . . . . ? O2 C4 C5 N1 -21.5(2) . . . . ? O2 C4 C5 C6 98.3(2) . . . . ? O11 Al2 N6 C68 -4.17(16) . . . . ? O9 Al2 N6 C68 -28.9(17) . . . . ? O7 Al2 N6 C68 176.40(16) . . . . ? N5 Al2 N6 C68 -97.52(16) . . . . ? N4 Al2 N6 C68 88.30(16) . . . . ? O11 Al2 N6 C70 170.85(15) . . . . ? O9 Al2 N6 C70 146.1(16) . . . . ? O7 Al2 N6 C70 -8.58(15) . . . . ? N5 Al2 N6 C70 77.50(15) . . . . ? N4 Al2 N6 C70 -96.67(15) . . . . ? N1 C5 C6 C7 64.7(2) . . . . ? C4 C5 C6 C7 -50.2(2) . . . . ? N1 C5 C6 C8 -170.22(18) . . . . ? C4 C5 C6 C8 74.8(2) . . . . ? O11 Al2 O7 C40 -122.6(7) . . . . ? O9 Al2 O7 C40 64.64(17) . . . . ? N6 Al2 O7 C40 -116.43(17) . . . . ? N5 Al2 O7 C40 152.43(17) . . . . ? N4 Al2 O7 C40 -21.21(17) . . . . ? O11 Al2 O9 C53 -128.96(16) . . . . ? O7 Al2 O9 C53 50.37(17) . . . . ? N6 Al2 O9 C53 -104.3(17) . . . . ? N5 Al2 O9 C53 -35.58(17) . . . . ? N4 Al2 O9 C53 138.36(17) . . . . ? C1 C2 C9 C10 -1.5(3) . . . . ? C3 C2 C9 C10 177.2(2) . . . . ? C2 C9 C10 C11 0.8(3) . . . . ? O9 Al2 O11 C66 -162.90(18) . . . . ? O7 Al2 O11 C66 24.3(8) . . . . ? N6 Al2 O11 C66 18.15(18) . . . . ? N5 Al2 O11 C66 108.95(18) . . . . ? N4 Al2 O11 C66 -76.87(18) . . . . ? C9 C10 C11 C12 0.3(4) . . . . ? C10 C11 C12 C1 -0.8(3) . . . . ? C10 C11 C12 C13 178.1(2) . . . . ? O1 C1 C12 C11 -179.92(19) . . . . ? C2 C1 C12 C11 0.1(3) . . . . ? O1 C1 C12 C13 1.2(3) . . . . ? C2 C1 C12 C13 -178.8(2) . . . . ? Al1 O3 C14 C15 -18.4(3) . . . . ? Al1 O3 C14 C25 163.32(14) . . . . ? O3 C14 C15 C22 -179.31(18) . . . . ? C25 C14 C15 C22 -1.0(3) . . . . ? O3 C14 C15 C16 -0.4(3) . . . . ? C25 C14 C15 C16 177.92(18) . . . . ? C18 N2 C16 O4 -4.4(2) . . . . ? Al1 N2 C16 O4 169.33(13) . . . . ? C18 N2 C16 C15 175.28(19) . . . . ? Al1 N2 C16 C15 -10.9(3) . . . . ? C17 O4 C16 N2 -10.4(2) . . . . ? C17 O4 C16 C15 169.85(18) . . . . ? C22 C15 C16 N2 -166.8(2) . . . . ? C14 C15 C16 N2 14.3(3) . . . . ? C22 C15 C16 O4 13.0(3) . . . . ? C14 C15 C16 O4 -165.99(17) . . . . ? C16 O4 C17 C18 19.8(2) . . . . ? C16 N2 C18 C17 16.4(2) . . . . ? Al1 N2 C18 C17 -157.37(14) . . . . ? C16 N2 C18 C19 -106.6(2) . . . . ? Al1 N2 C18 C19 79.7(2) . . . . ? O4 C17 C18 N2 -21.5(2) . . . . ? O4 C17 C18 C19 99.6(2) . . . . ? N2 C18 C19 C21 -165.37(19) . . . . ? C17 C18 C19 C21 79.3(2) . . . . ? N2 C18 C19 C20 70.3(2) . . . . ? C17 C18 C19 C20 -44.9(2) . . . . ? C14 C15 C22 C23 -1.1(3) . . . . ? C16 C15 C22 C23 179.98(19) . . . . ? C15 C22 C23 C24 1.7(3) . . . . ? C22 C23 C24 C25 -0.1(3) . . . . ? C23 C24 C25 C14 -2.0(3) . . . . ? C23 C24 C25 C26 176.9(2) . . . . ? O3 C14 C25 C24 -179.10(18) . . . . ? C15 C14 C25 C24 2.5(3) . . . . ? O3 C14 C25 C26 2.0(3) . . . . ? C15 C14 C25 C26 -176.41(17) . . . . ? Al1 O5 C27 C28 31.3(3) . . . . ? Al1 O5 C27 C38 -150.66(14) . . . . ? O5 C27 C28 C35 -179.85(18) . . . . ? C38 C27 C28 C35 2.1(3) . . . . ? O5 C27 C28 C29 7.5(3) . . . . ? C38 C27 C28 C29 -170.48(18) . . . . ? C31 N3 C29 O6 -4.4(2) . . . . ? Al1 N3 C29 O6 171.34(12) . . . . ? C31 N3 C29 C28 172.63(19) . . . . ? Al1 N3 C29 C28 -11.7(3) . . . . ? C30 O6 C29 N3 -2.4(2) . . . . ? C30 O6 C29 C28 -179.78(17) . . . . ? C35 C28 C29 N3 171.95(19) . . . . ? C27 C28 C29 N3 -15.4(3) . . . . ? C35 C28 C29 O6 -11.0(3) . . . . ? C27 C28 C29 O6 161.57(17) . . . . ? C29 O6 C30 C31 7.7(2) . . . . ? C29 N3 C31 C32 -115.14(18) . . . . ? Al1 N3 C31 C32 69.8(2) . . . . ? C29 N3 C31 C30 8.7(2) . . . . ? Al1 N3 C31 C30 -166.41(14) . . . . ? O6 C30 C31 N3 -9.7(2) . . . . ? O6 C30 C31 C32 112.64(19) . . . . ? N3 C31 C32 C33 52.7(2) . . . . ? C30 C31 C32 C33 -64.0(2) . . . . ? N3 C31 C32 C34 177.65(17) . . . . ? C30 C31 C32 C34 60.9(2) . . . . ? C27 C28 C35 C36 -1.5(3) . . . . ? C29 C28 C35 C36 170.97(19) . . . . ? C28 C35 C36 C37 -0.2(3) . . . . ? C35 C36 C37 C38 1.3(3) . . . . ? C36 C37 C38 C27 -0.6(3) . . . . ? C36 C37 C38 C39 178.1(2) . . . . ? O5 C27 C38 C37 -179.17(18) . . . . ? C28 C27 C38 C37 -1.1(3) . . . . ? O5 C27 C38 C39 2.0(3) . . . . ? C28 C27 C38 C39 -179.89(18) . . . . ? Al2 O7 C40 C41 11.0(3) . . . . ? Al2 O7 C40 C51 -170.19(14) . . . . ? O7 C40 C41 C48 178.32(18) . . . . ? C51 C40 C41 C48 -0.4(3) . . . . ? O7 C40 C41 C42 1.4(3) . . . . ? C51 C40 C41 C42 -177.41(18) . . . . ? C44 N4 C42 O8 -5.3(2) . . . . ? Al2 N4 C42 O8 154.10(14) . . . . ? C44 N4 C42 C41 173.1(2) . . . . ? Al2 N4 C42 C41 -27.5(3) . . . . ? C43 O8 C42 N4 -10.7(2) . . . . ? C43 O8 C42 C41 170.69(18) . . . . ? C48 C41 C42 N4 -167.4(2) . . . . ? C40 C41 C42 N4 9.6(3) . . . . ? C48 C41 C42 O8 11.0(3) . . . . ? C40 C41 C42 O8 -172.05(18) . . . . ? C42 O8 C43 C44 21.1(2) . . . . ? C42 N4 C44 C43 17.9(2) . . . . ? Al2 N4 C44 C43 -140.06(15) . . . . ? C42 N4 C44 C45 -104.71(19) . . . . ? Al2 N4 C44 C45 97.34(18) . . . . ? O8 C43 C44 N4 -23.2(2) . . . . ? O8 C43 C44 C45 96.5(2) . . . . ? N4 C44 C45 C47 68.5(2) . . . . ? C43 C44 C45 C47 -45.8(3) . . . . ? N4 C44 C45 C46 -165.66(17) . . . . ? C43 C44 C45 C46 80.0(2) . . . . ? C40 C41 C48 C49 -0.9(3) . . . . ? C42 C41 C48 C49 176.1(2) . . . . ? C41 C48 C49 C50 1.0(3) . . . . ? C48 C49 C50 C51 0.2(3) . . . . ? C49 C50 C51 C40 -1.5(3) . . . . ? C49 C50 C51 C52 179.3(2) . . . . ? O7 C40 C51 C50 -177.26(18) . . . . ? C41 C40 C51 C50 1.6(3) . . . . ? O7 C40 C51 C52 2.0(3) . . . . ? C41 C40 C51 C52 -179.17(19) . . . . ? Al2 O9 C53 C54 27.1(3) . . . . ? Al2 O9 C53 C64 -154.06(15) . . . . ? O9 C53 C54 C61 -179.91(18) . . . . ? C64 C53 C54 C61 1.3(3) . . . . ? O9 C53 C54 C55 3.7(3) . . . . ? C64 C53 C54 C55 -175.07(18) . . . . ? C57 N5 C55 O10 -4.2(2) . . . . ? Al2 N5 C55 O10 174.03(12) . . . . ? C57 N5 C55 C54 173.84(18) . . . . ? Al2 N5 C55 C54 -8.0(3) . . . . ? C56 O10 C55 N5 -8.0(2) . . . . ? C56 O10 C55 C54 173.81(16) . . . . ? C53 C54 C55 N5 -11.7(3) . . . . ? C61 C54 C55 N5 171.9(2) . . . . ? C53 C54 C55 O10 166.32(18) . . . . ? C61 C54 C55 O10 -10.0(3) . . . . ? C55 O10 C56 C57 15.83(19) . . . . ? C55 N5 C57 C58 -110.18(18) . . . . ? Al2 N5 C57 C58 71.8(2) . . . . ? C55 N5 C57 C56 13.5(2) . . . . ? Al2 N5 C57 C56 -164.49(13) . . . . ? O10 C56 C57 N5 -17.57(19) . . . . ? O10 C56 C57 C58 104.11(19) . . . . ? N5 C57 C58 C60 53.4(2) . . . . ? C56 C57 C58 C60 -62.6(2) . . . . ? N5 C57 C58 C59 179.50(17) . . . . ? C56 C57 C58 C59 63.5(2) . . . . ? C53 C54 C61 C62 -0.2(3) . . . . ? C55 C54 C61 C62 176.2(2) . . . . ? C54 C61 C62 C63 -0.9(3) . . . . ? C61 C62 C63 C64 0.8(4) . . . . ? C62 C63 C64 C53 0.3(3) . . . . ? C62 C63 C64 C65 -178.5(2) . . . . ? O9 C53 C64 C63 179.81(19) . . . . ? C54 C53 C64 C63 -1.3(3) . . . . ? O9 C53 C64 C65 -1.4(3) . . . . ? C54 C53 C64 C65 177.5(2) . . . . ? Al2 O11 C66 C67 -15.7(3) . . . . ? Al2 O11 C66 C77 165.73(14) . . . . ? O11 C66 C67 C74 174.96(18) . . . . ? C77 C66 C67 C74 -6.5(3) . . . . ? O11 C66 C67 C68 -5.5(3) . . . . ? C77 C66 C67 C68 173.00(17) . . . . ? C70 N6 C68 O12 -6.8(2) . . . . ? Al2 N6 C68 O12 169.03(12) . . . . ? C70 N6 C68 C67 172.73(18) . . . . ? Al2 N6 C68 C67 -11.5(3) . . . . ? C69 O12 C68 N6 -10.8(2) . . . . ? C69 O12 C68 C67 169.66(17) . . . . ? C74 C67 C68 N6 -162.03(19) . . . . ? C66 C67 C68 N6 18.5(3) . . . . ? C74 C67 C68 O12 17.5(3) . . . . ? C66 C67 C68 O12 -162.04(17) . . . . ? C68 O12 C69 C70 22.76(19) . . . . ? C68 N6 C70 C69 20.32(19) . . . . ? Al2 N6 C70 C69 -155.47(13) . . . . ? C68 N6 C70 C71 -101.01(19) . . . . ? Al2 N6 C70 C71 83.20(19) . . . . ? O12 C69 C70 N6 -25.59(18) . . . . ? O12 C69 C70 C71 93.66(19) . . . . ? N6 C70 C71 C73 -167.89(17) . . . . ? C69 C70 C71 C73 78.6(2) . . . . ? N6 C70 C71 C72 67.9(2) . . . . ? C69 C70 C71 C72 -45.5(2) . . . . ? C66 C67 C74 C75 1.7(3) . . . . ? C68 C67 C74 C75 -177.8(2) . . . . ? C67 C74 C75 C76 2.8(3) . . . . ? C74 C75 C76 C77 -2.5(4) . . . . ? C75 C76 C77 C66 -2.4(3) . . . . ? C75 C76 C77 C78 177.6(2) . . . . ? O11 C66 C77 C76 -174.64(19) . . . . ? C67 C66 C77 C76 6.7(3) . . . . ? O11 C66 C77 C78 5.4(3) . . . . ? C67 C66 C77 C78 -173.24(19) . . . . ? C4S O1S C1S C2S -2.4(3) . . . . ? O1S C1S C2S C3S -20.2(3) . . . . ? C1S C2S C3S C4S 33.6(3) . . . . ? C1S O1S C4S C3S 24.3(3) . . . . ? C2S C3S C4S O1S -36.0(3) . . . . ? C8S O2S C5S C6S -20.2(12) . . . . ? O2S C5S C6S C7S 31.1(16) . . . . ? C5S C6S C7S C8S -23.6(16) . . . . ? C6S C7S C8S O2S 11.5(18) . . . . ? C5S O2S C8S C7S 5.8(14) . . . . ? C8S' O2S' C5S' C6S' 51(2) . . . . ? O2S' C5S' C6S' C7S' -59(2) . . . . ? C5S' C6S' C7S' C8S' 40(2) . . . . ? C6S' C7S' C8S' O2S' -11(3) . . . . ? C5S' O2S' C8S' C7S' -22(2) . . . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 26.02 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.316 _refine_diff_density_min -0.265 _refine_diff_density_rms 0.039 _database_code_depnum_ccdc_archive 'CCDC 957728' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_AliPrCNPh3 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C42 H45 Al N6 O6' _chemical_formula_sum 'C42 H45 Al N6 O6' _chemical_formula_weight 756.84 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Al Al 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M P212121 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' _cell_length_a 9.9787(9) _cell_length_b 18.6883(17) _cell_length_c 24.482(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4565.5(7) _cell_formula_units_Z 4 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 12062 _cell_measurement_theta_min 2.15 _cell_measurement_theta_max 25.88 _exptl_crystal_description plate _exptl_crystal_colour pink _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.08 _exptl_crystal_density_diffrn 1.101 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1796 _exptl_absorpt_coefficient_mu 0.100 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.952 _exptl_absorpt_correction_T_max 0.992 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX' _diffrn_measurement_method \w _diffrn_reflns_number 33843 _diffrn_reflns_av_R_equivalents 0.0436 _diffrn_reflns_av_sigmaI/netI 0.0560 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 1.99 _diffrn_reflns_theta_max 27.10 _reflns_number_total 9860 _reflns_number_gt 7992 _reflns_threshold_expression >2sigma(I) _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The crystal contains disordered thf and heptane, which occupy same cavities in the unit cell. Due to the diffuse nature of these positions a satisfactory refinement of the solvent molecule was not successful. The SQUEEZE routine in PLATON (A. L. Spek, J. Appl. Cryst. 2003, 36, 7) was used for removing the contributions of diffuse solvent from diffraction intensities. ; loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.040 0.250 0.500 441 83 ' ' 2 -0.074 0.750 0.000 441 83 ' ' _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^)+(0.0526P)^2^+0.2646P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.02(15) _refine_ls_number_reflns 9860 _refine_ls_number_parameters 542 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0629 _refine_ls_R_factor_gt 0.0487 _refine_ls_wR_factor_ref 0.1061 _refine_ls_wR_factor_gt 0.1011 _refine_ls_goodness_of_fit_ref 1.007 _refine_ls_restrained_S_all 1.007 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Al1 Al 0.04053(7) 0.27458(3) 0.17518(2) 0.02310(14) Uani 1 1 d . . . O1 O 0.11754(15) 0.20228(7) 0.13456(5) 0.0270(3) Uani 1 1 d . . . O4 O -0.10764(16) 0.29672(8) 0.01822(5) 0.0318(4) Uani 1 1 d . . . O3 O 0.14426(15) 0.34778(7) 0.14915(5) 0.0242(3) Uani 1 1 d . . . O5 O -0.07499(16) 0.20862(7) 0.20518(5) 0.0298(4) Uani 1 1 d . . . O2 O 0.39715(17) 0.22168(8) 0.25735(6) 0.0371(4) Uani 1 1 d . . . O6 O -0.15982(18) 0.39119(8) 0.29752(6) 0.0386(4) Uani 1 1 d . . . N3 N -0.07885(18) 0.28572(8) 0.10868(6) 0.0235(4) Uani 1 1 d . . . N5 N -0.04968(19) 0.34909(9) 0.22409(6) 0.0277(4) Uani 1 1 d . . . N1 N 0.19341(19) 0.26086(8) 0.23127(6) 0.0261(4) Uani 1 1 d . . . N2 N 0.0357(3) 0.08079(12) 0.03264(8) 0.0541(6) Uani 1 1 d . . . N6 N -0.1970(3) 0.03440(11) 0.19516(10) 0.0531(6) Uani 1 1 d . . . N4 N 0.4064(2) 0.46022(11) 0.17647(9) 0.0435(5) Uani 1 1 d . . . C19 C -0.1977(2) 0.24044(11) 0.09610(8) 0.0298(5) Uani 1 1 d . . . H19 H -0.1847 0.1915 0.1118 0.019(5) Uiso 1 1 calc R . . C27 C 0.3413(3) 0.44682(11) 0.13965(9) 0.0311(5) Uani 1 1 d . . . C15 C 0.1536(2) 0.37964(10) 0.10150(8) 0.0244(5) Uani 1 1 d . . . C3 C 0.2855(2) 0.21254(11) 0.22710(8) 0.0277(5) Uani 1 1 d . . . C9 C 0.3716(2) 0.09254(11) 0.20215(9) 0.0292(5) Uani 1 1 d . . . H9 H 0.4320 0.0952 0.2321 0.039(7) Uiso 1 1 calc R . . C17 C -0.0401(2) 0.31527(10) 0.06384(8) 0.0241(5) Uani 1 1 d . . . C2 C 0.2820(2) 0.14966(10) 0.19277(8) 0.0267(5) Uani 1 1 d . . . C13 C 0.1077(3) 0.08441(12) 0.06856(9) 0.0365(6) Uani 1 1 d . . . C1 C 0.1955(2) 0.14929(10) 0.14746(8) 0.0266(5) Uani 1 1 d . . . C23 C 0.0866(3) 0.40197(12) 0.00805(9) 0.0356(6) Uani 1 1 d . . . H23 H 0.0273 0.3922 -0.0214 0.043(7) Uiso 1 1 calc R . . C12 C 0.2002(2) 0.08733(11) 0.11348(8) 0.0279(5) Uani 1 1 d . . . C40 C -0.2284(3) 0.14397(12) 0.25814(9) 0.0364(6) Uani 1 1 d . . . C6 C 0.1649(3) 0.30156(11) 0.32838(8) 0.0362(6) Uani 1 1 d . . . H6 H 0.0682 0.3117 0.3210 0.037(7) Uiso 1 1 calc R . . C29 C -0.1593(2) 0.20842(11) 0.24555(8) 0.0298(5) Uani 1 1 d . . . C26 C 0.2558(2) 0.43033(10) 0.09370(8) 0.0279(5) Uani 1 1 d . . . C16 C 0.0673(2) 0.36625(10) 0.05735(8) 0.0242(5) Uani 1 1 d . . . C25 C 0.2728(3) 0.46486(13) 0.04358(9) 0.0385(6) Uani 1 1 d . . . H25 H 0.3437 0.4983 0.0394 0.048(8) Uiso 1 1 calc R . . C31 C -0.1289(2) 0.33560(12) 0.26486(8) 0.0309(5) Uani 1 1 d . . . C10 C 0.3737(2) 0.03253(11) 0.16862(9) 0.0302(5) Uani 1 1 d . . . C32 C -0.0698(3) 0.44947(13) 0.28131(9) 0.0384(6) Uani 1 1 d . . . H32A H 0.0067 0.4535 0.3069 0.057(8) Uiso 1 1 calc R . . H32B H -0.1180 0.4957 0.2802 0.032(6) Uiso 1 1 calc R . . C20 C -0.3239(2) 0.27412(14) 0.12006(9) 0.0394(6) Uani 1 1 d . . . H20 H -0.3039 0.2864 0.1590 0.041(6) Uiso 1 1 calc R . . C30 C -0.1883(2) 0.26779(12) 0.27867(8) 0.0332(5) Uani 1 1 d . . . C37 C -0.2730(3) 0.26101(14) 0.32367(10) 0.0425(6) Uani 1 1 d . . . H37 H -0.2888 0.3017 0.3460 0.037(7) Uiso 1 1 calc R . . C35 C -0.0361(3) 0.54040(12) 0.17036(10) 0.0453(7) Uani 1 1 d . . . H35A H -0.0504 0.5681 0.2039 0.051(7) Uiso 1 1 calc R . . H35B H -0.0801 0.5645 0.1397 0.049(7) Uiso 1 1 calc R . . H35C H 0.0602 0.5366 0.1631 0.064(10) Uiso 1 1 calc R . . C18 C -0.1936(3) 0.23659(12) 0.03362(8) 0.0329(5) Uani 1 1 d . . . H18A H -0.1549 0.1906 0.0212 0.030(6) Uiso 1 1 calc R . . H18B H -0.2844 0.2420 0.0179 0.037(7) Uiso 1 1 calc R . . C33 C -0.0224(3) 0.42771(11) 0.22430(8) 0.0302(5) Uani 1 1 d . . . H33 H 0.0763 0.4362 0.2211 0.027(6) Uiso 1 1 calc R . . C41 C -0.2093(3) 0.08347(13) 0.22308(10) 0.0393(6) Uani 1 1 d . . . C34 C -0.0953(2) 0.46583(11) 0.17733(9) 0.0320(5) Uani 1 1 d . . . H34 H -0.0764 0.4385 0.1431 0.018(5) Uiso 1 1 calc R . . C7 C 0.2124(3) 0.35551(13) 0.37099(9) 0.0447(7) Uani 1 1 d . . . H7A H 0.3059 0.3455 0.3806 0.048(8) Uiso 1 1 calc R . . H7B H 0.1563 0.3517 0.4037 0.053(8) Uiso 1 1 calc R . . H7C H 0.2056 0.4040 0.3560 0.053(8) Uiso 1 1 calc R . . C4 C 0.3894(3) 0.29483(11) 0.27791(10) 0.0373(6) Uani 1 1 d . . . H4A H 0.4427 0.3279 0.2550 0.027(6) Uiso 1 1 calc R . . H4B H 0.4216 0.2977 0.3161 0.038(6) Uiso 1 1 calc R . . C11 C 0.2873(2) 0.03158(11) 0.12441(8) 0.0309(5) Uani 1 1 d . . . H11 H 0.2879 -0.0087 0.1008 0.029(6) Uiso 1 1 calc R . . C14 C 0.4672(3) -0.02955(12) 0.18050(10) 0.0395(6) Uani 1 1 d . . . H14A H 0.5582 -0.0172 0.1688 0.114(14) Uiso 1 1 calc R . . H14B H 0.4367 -0.0720 0.1606 0.085(11) Uiso 1 1 calc R . . H14C H 0.4671 -0.0395 0.2198 0.105(12) Uiso 1 1 calc R . . C38 C -0.3346(3) 0.19726(16) 0.33690(10) 0.0494(7) Uani 1 1 d . . . C5 C 0.2413(2) 0.31187(11) 0.27430(8) 0.0315(5) Uani 1 1 d . . . H5 H 0.2293 0.3621 0.2612 0.018(5) Uiso 1 1 calc R . . C21 C -0.3631(3) 0.34327(16) 0.09138(10) 0.0516(7) Uani 1 1 d . . . H21A H -0.2856 0.3754 0.0900 0.070(10) Uiso 1 1 calc R . . H21B H -0.4361 0.3664 0.1115 0.053(8) Uiso 1 1 calc R . . H21C H -0.3929 0.3325 0.0541 0.052(8) Uiso 1 1 calc R . . C39 C -0.3134(3) 0.13898(14) 0.30293(10) 0.0450(7) Uani 1 1 d . . . H39 H -0.3576 0.0950 0.3104 0.050(8) Uiso 1 1 calc R . . C24 C 0.1888(3) 0.45128(13) 0.00016(9) 0.0434(6) Uani 1 1 d . . . C36 C -0.2473(3) 0.46812(14) 0.18476(10) 0.0418(6) Uani 1 1 d . . . H36A H -0.2696 0.4999 0.2153 0.064(8) Uiso 1 1 calc R . . H36B H -0.2805 0.4198 0.1925 0.043(7) Uiso 1 1 calc R . . H36C H -0.2891 0.4861 0.1513 0.043(7) Uiso 1 1 calc R . . C8 C 0.1741(4) 0.22529(13) 0.35046(10) 0.0524(8) Uani 1 1 d . . . H8A H 0.2683 0.2129 0.3568 0.087(12) Uiso 1 1 calc R . . H8B H 0.1354 0.1920 0.3238 0.045(7) Uiso 1 1 calc R . . H8C H 0.1246 0.2220 0.3849 0.062(8) Uiso 1 1 calc R . . C22 C -0.4398(3) 0.22053(19) 0.12034(11) 0.0609(9) Uani 1 1 d . . . H22A H -0.4647 0.2088 0.0827 0.065(9) Uiso 1 1 calc R . . H22B H -0.5170 0.2416 0.1391 0.083(11) Uiso 1 1 calc R . . H22C H -0.4121 0.1769 0.1394 0.095(13) Uiso 1 1 calc R . . C42 C -0.4247(4) 0.1899(2) 0.38669(14) 0.0802(12) Uani 1 1 d . . . H42A H -0.3797 0.1605 0.4143 0.115(14) Uiso 1 1 calc R . . H42B H -0.5090 0.1670 0.3760 0.15(2) Uiso 1 1 calc R . . H42C H -0.4433 0.2374 0.4018 0.089(12) Uiso 1 1 calc R . . C28 C 0.2075(4) 0.4879(2) -0.05455(12) 0.0723(10) Uani 1 1 d . . . H28A H 0.2924 0.4724 -0.0708 0.132(17) Uiso 1 1 calc R . . H28B H 0.2089 0.5399 -0.0493 0.126(16) Uiso 1 1 calc R . . H28C H 0.1333 0.4750 -0.0789 0.17(2) 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 0.0260(4) 0.0222(3) 0.0212(3) 0.0006(2) 0.0010(3) -0.0015(3) O1 0.0309(9) 0.0257(7) 0.0243(7) -0.0004(5) -0.0016(6) 0.0036(7) O4 0.0342(10) 0.0389(8) 0.0224(7) -0.0030(6) -0.0003(7) -0.0028(7) O3 0.0253(9) 0.0241(7) 0.0232(7) 0.0016(5) 0.0033(6) -0.0007(7) O5 0.0339(10) 0.0298(8) 0.0259(7) 0.0021(6) 0.0025(7) -0.0074(7) O2 0.0376(11) 0.0315(8) 0.0421(9) 0.0003(7) -0.0138(8) -0.0041(8) O6 0.0370(11) 0.0493(10) 0.0295(8) -0.0111(7) 0.0068(8) 0.0005(8) N3 0.0239(10) 0.0233(8) 0.0234(8) -0.0002(6) 0.0015(7) 0.0002(8) N5 0.0299(11) 0.0291(9) 0.0241(8) -0.0022(7) 0.0017(8) -0.0017(9) N1 0.0321(12) 0.0243(9) 0.0219(8) 0.0021(6) -0.0033(8) -0.0026(8) N2 0.0630(18) 0.0592(14) 0.0401(12) -0.0121(10) -0.0153(12) 0.0135(13) N6 0.0517(16) 0.0380(12) 0.0697(15) 0.0099(11) -0.0144(13) -0.0090(12) N4 0.0349(13) 0.0482(12) 0.0473(12) -0.0082(10) 0.0020(11) -0.0029(10) C19 0.0318(14) 0.0298(11) 0.0277(10) -0.0034(8) -0.0044(10) -0.0055(10) C27 0.0295(14) 0.0242(10) 0.0396(12) 0.0003(9) 0.0103(11) -0.0002(10) C15 0.0265(13) 0.0193(9) 0.0273(10) 0.0002(7) 0.0077(9) 0.0069(9) C3 0.0297(14) 0.0264(10) 0.0270(10) 0.0075(8) -0.0066(10) -0.0042(10) C9 0.0256(14) 0.0302(11) 0.0319(11) 0.0057(9) -0.0011(10) -0.0025(10) C17 0.0242(13) 0.0249(10) 0.0232(9) -0.0014(8) 0.0009(9) 0.0068(10) C2 0.0280(13) 0.0253(10) 0.0267(10) 0.0039(8) -0.0004(9) -0.0030(10) C13 0.0439(17) 0.0348(12) 0.0310(11) -0.0057(9) -0.0023(12) 0.0068(12) C1 0.0295(14) 0.0249(10) 0.0254(10) 0.0035(8) 0.0019(10) 0.0000(10) C23 0.0400(16) 0.0393(12) 0.0274(11) 0.0038(9) 0.0025(11) 0.0028(12) C12 0.0303(14) 0.0287(10) 0.0248(10) 0.0001(8) 0.0005(9) 0.0010(10) C40 0.0297(15) 0.0422(13) 0.0373(12) 0.0158(10) -0.0077(11) -0.0022(12) C6 0.0479(17) 0.0333(11) 0.0274(10) -0.0010(9) -0.0037(11) -0.0090(12) C29 0.0261(13) 0.0384(12) 0.0249(10) 0.0091(8) -0.0056(9) -0.0031(11) C26 0.0283(14) 0.0232(10) 0.0321(11) 0.0020(8) 0.0071(10) 0.0031(10) C16 0.0265(13) 0.0248(10) 0.0214(9) 0.0007(7) 0.0060(9) 0.0051(9) C25 0.0372(16) 0.0364(13) 0.0420(13) 0.0051(10) 0.0131(12) -0.0048(12) C31 0.0266(14) 0.0418(12) 0.0243(10) -0.0047(9) -0.0023(10) 0.0013(11) C10 0.0263(14) 0.0303(11) 0.0339(11) 0.0053(9) 0.0052(10) 0.0009(10) C32 0.0382(16) 0.0413(13) 0.0358(12) -0.0105(10) -0.0007(12) 0.0002(12) C20 0.0303(15) 0.0603(15) 0.0274(11) -0.0054(10) 0.0015(10) -0.0044(13) C30 0.0294(14) 0.0453(13) 0.0249(10) 0.0049(9) -0.0016(10) -0.0005(12) C37 0.0366(16) 0.0573(16) 0.0336(12) 0.0078(11) 0.0041(11) 0.0070(13) C35 0.055(2) 0.0295(12) 0.0511(15) -0.0039(11) -0.0088(15) 0.0048(13) C18 0.0330(15) 0.0356(12) 0.0300(11) -0.0048(9) 0.0015(10) -0.0033(11) C33 0.0299(15) 0.0289(11) 0.0316(11) -0.0063(8) 0.0022(10) -0.0008(11) C41 0.0337(16) 0.0352(12) 0.0491(14) 0.0167(11) -0.0090(12) -0.0079(12) C34 0.0332(14) 0.0297(11) 0.0331(11) -0.0064(9) 0.0000(10) 0.0036(10) C7 0.058(2) 0.0427(14) 0.0333(12) -0.0024(10) -0.0096(13) -0.0093(14) C4 0.0418(17) 0.0275(11) 0.0425(13) 0.0005(9) -0.0090(12) -0.0057(11) C11 0.0344(14) 0.0290(11) 0.0292(11) -0.0003(8) 0.0045(10) 0.0026(11) C14 0.0378(16) 0.0343(12) 0.0464(14) 0.0096(10) 0.0055(13) 0.0080(12) C38 0.0318(16) 0.0703(18) 0.0461(15) 0.0286(13) 0.0087(12) 0.0058(15) C5 0.0394(16) 0.0257(10) 0.0295(11) 0.0022(8) -0.0075(10) -0.0058(10) C21 0.0365(18) 0.0740(19) 0.0444(15) -0.0176(13) -0.0034(13) 0.0132(16) C39 0.0350(17) 0.0494(15) 0.0506(15) 0.0243(12) 0.0006(13) -0.0032(14) C24 0.0484(18) 0.0449(14) 0.0370(13) 0.0131(11) 0.0054(12) -0.0043(13) C36 0.0331(16) 0.0467(15) 0.0455(14) -0.0085(11) -0.0005(12) 0.0094(13) C8 0.081(3) 0.0389(13) 0.0375(13) 0.0044(11) 0.0020(14) -0.0172(16) C22 0.0404(18) 0.099(3) 0.0431(14) -0.0048(16) 0.0034(14) -0.0229(19) C42 0.074(3) 0.099(3) 0.068(2) 0.039(2) 0.037(2) 0.016(2) C28 0.079(3) 0.093(3) 0.0454(16) 0.0301(16) 0.0047(19) -0.021(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Al1 O3 1.8301(15) . ? Al1 O5 1.8405(15) . ? Al1 O1 1.8453(15) . ? Al1 N3 2.0279(17) . ? Al1 N5 2.0452(18) . ? Al1 N1 2.0686(19) . ? O1 C1 1.298(2) . ? O4 C17 1.350(2) . ? O4 C18 1.463(3) . ? O3 C15 1.313(2) . ? O5 C29 1.298(3) . ? O2 C3 1.349(3) . ? O2 C4 1.459(3) . ? O6 C31 1.347(2) . ? O6 C32 1.467(3) . ? N3 C17 1.289(2) . ? N3 C19 1.489(3) . ? N5 C31 1.298(3) . ? N5 C33 1.494(3) . ? N1 C3 1.292(3) . ? N1 C5 1.499(3) . ? N2 C13 1.138(3) . ? N6 C41 1.150(3) . ? N4 C27 1.140(3) . ? C19 C20 1.525(3) . ? C19 C18 1.532(3) . ? C27 C26 1.445(3) . ? C15 C16 1.404(3) . ? C15 C26 1.405(3) . ? C3 C2 1.445(3) . ? C9 C10 1.390(3) . ? C9 C2 1.411(3) . ? C17 C16 1.443(3) . ? C2 C1 1.405(3) . ? C13 C12 1.437(3) . ? C1 C12 1.427(3) . ? C23 C24 1.388(4) . ? C23 C16 1.393(3) . ? C12 C11 1.383(3) . ? C40 C39 1.389(3) . ? C40 C29 1.422(3) . ? C40 C41 1.432(3) . ? C6 C7 1.526(3) . ? C6 C8 1.527(3) . ? C6 C5 1.540(3) . ? C29 C30 1.404(3) . ? C26 C25 1.397(3) . ? C25 C24 1.378(4) . ? C31 C30 1.439(3) . ? C10 C11 1.384(3) . ? C10 C14 1.517(3) . ? C32 C33 1.529(3) . ? C20 C21 1.522(4) . ? C20 C22 1.530(4) . ? C30 C37 1.394(3) . ? C37 C38 1.379(4) . ? C35 C34 1.523(3) . ? C33 C34 1.536(3) . ? C34 C36 1.528(3) . ? C4 C5 1.514(3) . ? C38 C39 1.387(4) . ? C38 C42 1.521(4) . ? C24 C28 1.516(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O3 Al1 O5 173.63(7) . . ? O3 Al1 O1 97.13(7) . . ? O5 Al1 O1 89.17(7) . . ? O3 Al1 N3 88.62(7) . . ? O5 Al1 N3 91.21(7) . . ? O1 Al1 N3 83.52(7) . . ? O3 Al1 N5 86.78(7) . . ? O5 Al1 N5 86.94(7) . . ? O1 Al1 N5 175.81(7) . . ? N3 Al1 N5 98.13(7) . . ? O3 Al1 N1 84.65(7) . . ? O5 Al1 N1 96.54(7) . . ? O1 Al1 N1 87.70(7) . . ? N3 Al1 N1 168.20(8) . . ? N5 Al1 N1 91.16(7) . . ? C1 O1 Al1 132.60(13) . . ? C17 O4 C18 106.07(15) . . ? C15 O3 Al1 133.50(14) . . ? C29 O5 Al1 135.38(14) . . ? C3 O2 C4 105.32(17) . . ? C31 O6 C32 105.79(16) . . ? C17 N3 C19 107.84(16) . . ? C17 N3 Al1 123.48(15) . . ? C19 N3 Al1 125.14(12) . . ? C31 N5 C33 107.41(17) . . ? C31 N5 Al1 125.88(15) . . ? C33 N5 Al1 126.24(14) . . ? C3 N1 C5 105.85(18) . . ? C3 N1 Al1 123.95(14) . . ? C5 N1 Al1 128.53(14) . . ? N3 C19 C20 110.08(17) . . ? N3 C19 C18 102.25(17) . . ? C20 C19 C18 115.2(2) . . ? N4 C27 C26 178.6(3) . . ? O3 C15 C16 124.04(19) . . ? O3 C15 C26 118.54(19) . . ? C16 C15 C26 117.42(18) . . ? N1 C3 O2 117.10(18) . . ? N1 C3 C2 126.7(2) . . ? O2 C3 C2 116.2(2) . . ? C10 C9 C2 121.6(2) . . ? N3 C17 O4 116.42(19) . . ? N3 C17 C16 126.86(19) . . ? O4 C17 C16 116.72(17) . . ? C1 C2 C9 120.93(18) . . ? C1 C2 C3 118.53(19) . . ? C9 C2 C3 120.34(19) . . ? N2 C13 C12 178.6(3) . . ? O1 C1 C2 123.81(18) . . ? O1 C1 C12 119.78(19) . . ? C2 C1 C12 116.37(19) . . ? C24 C23 C16 122.7(2) . . ? C11 C12 C1 121.27(19) . . ? C11 C12 C13 121.56(19) . . ? C1 C12 C13 117.14(19) . . ? C39 C40 C29 121.6(2) . . ? C39 C40 C41 120.1(2) . . ? C29 C40 C41 118.3(2) . . ? C7 C6 C8 110.85(19) . . ? C7 C6 C5 110.55(19) . . ? C8 C6 C5 113.0(2) . . ? O5 C29 C30 124.8(2) . . ? O5 C29 C40 118.8(2) . . ? C30 C29 C40 116.4(2) . . ? C25 C26 C15 121.3(2) . . ? C25 C26 C27 120.9(2) . . ? C15 C26 C27 117.80(18) . . ? C23 C16 C15 119.8(2) . . ? C23 C16 C17 121.0(2) . . ? C15 C16 C17 119.23(17) . . ? C24 C25 C26 121.2(2) . . ? N5 C31 O6 116.5(2) . . ? N5 C31 C30 127.03(19) . . ? O6 C31 C30 116.47(19) . . ? C11 C10 C9 117.6(2) . . ? C11 C10 C14 121.6(2) . . ? C9 C10 C14 120.9(2) . . ? O6 C32 C33 103.83(17) . . ? C21 C20 C19 112.7(2) . . ? C21 C20 C22 111.3(2) . . ? C19 C20 C22 110.9(2) . . ? C37 C30 C29 120.6(2) . . ? C37 C30 C31 121.0(2) . . ? C29 C30 C31 118.39(19) . . ? C38 C37 C30 122.3(3) . . ? O4 C18 C19 103.71(16) . . ? N5 C33 C32 102.02(17) . . ? N5 C33 C34 111.52(17) . . ? C32 C33 C34 114.42(19) . . ? N6 C41 C40 178.4(3) . . ? C35 C34 C36 111.9(2) . . ? C35 C34 C33 108.9(2) . . ? C36 C34 C33 113.21(19) . . ? O2 C4 C5 103.23(18) . . ? C12 C11 C10 122.2(2) . . ? C37 C38 C39 118.0(2) . . ? C37 C38 C42 122.0(3) . . ? C39 C38 C42 120.0(3) . . ? N1 C5 C4 102.63(18) . . ? N1 C5 C6 111.49(17) . . ? C4 C5 C6 114.00(19) . . ? C38 C39 C40 120.9(2) . . ? C25 C24 C23 117.5(2) . . ? C25 C24 C28 121.6(3) . . ? C23 C24 C28 120.9(3) . . ? 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 O3 Al1 O1 C1 108.51(19) . . . . ? O5 Al1 O1 C1 -72.39(19) . . . . ? N3 Al1 O1 C1 -163.71(19) . . . . ? N5 Al1 O1 C1 -50.2(12) . . . . ? N1 Al1 O1 C1 24.19(19) . . . . ? O5 Al1 O3 C15 -103.2(7) . . . . ? O1 Al1 O3 C15 68.68(19) . . . . ? N3 Al1 O3 C15 -14.61(18) . . . . ? N5 Al1 O3 C15 -112.84(18) . . . . ? N1 Al1 O3 C15 155.69(18) . . . . ? O3 Al1 O5 C29 -19.4(8) . . . . ? O1 Al1 O5 C29 168.6(2) . . . . ? N3 Al1 O5 C29 -107.9(2) . . . . ? N5 Al1 O5 C29 -9.8(2) . . . . ? N1 Al1 O5 C29 81.0(2) . . . . ? O3 Al1 N3 C17 21.89(16) . . . . ? O5 Al1 N3 C17 -164.48(16) . . . . ? O1 Al1 N3 C17 -75.45(16) . . . . ? N5 Al1 N3 C17 108.44(16) . . . . ? N1 Al1 N3 C17 -33.3(4) . . . . ? O3 Al1 N3 C19 178.05(16) . . . . ? O5 Al1 N3 C19 -8.32(16) . . . . ? O1 Al1 N3 C19 80.71(16) . . . . ? N5 Al1 N3 C19 -95.40(16) . . . . ? N1 Al1 N3 C19 122.9(3) . . . . ? O3 Al1 N5 C31 -167.68(19) . . . . ? O5 Al1 N5 C31 13.38(19) . . . . ? O1 Al1 N5 C31 -8.8(12) . . . . ? N3 Al1 N5 C31 104.17(19) . . . . ? N1 Al1 N5 C31 -83.11(19) . . . . ? O3 Al1 N5 C33 3.51(17) . . . . ? O5 Al1 N5 C33 -175.43(17) . . . . ? O1 Al1 N5 C33 162.4(10) . . . . ? N3 Al1 N5 C33 -84.64(17) . . . . ? N1 Al1 N5 C33 88.08(17) . . . . ? O3 Al1 N1 C3 -100.11(17) . . . . ? O5 Al1 N1 C3 86.18(17) . . . . ? O1 Al1 N1 C3 -2.72(17) . . . . ? N3 Al1 N1 C3 -44.6(4) . . . . ? N5 Al1 N1 C3 173.24(17) . . . . ? O3 Al1 N1 C5 63.04(17) . . . . ? O5 Al1 N1 C5 -110.67(17) . . . . ? O1 Al1 N1 C5 160.42(17) . . . . ? N3 Al1 N1 C5 118.5(3) . . . . ? N5 Al1 N1 C5 -23.62(17) . . . . ? C17 N3 C19 C20 -109.17(19) . . . . ? Al1 N3 C19 C20 91.57(19) . . . . ? C17 N3 C19 C18 13.7(2) . . . . ? Al1 N3 C19 C18 -145.55(14) . . . . ? Al1 O3 C15 C16 6.5(3) . . . . ? Al1 O3 C15 C26 -173.41(14) . . . . ? C5 N1 C3 O2 -4.0(2) . . . . ? Al1 N1 C3 O2 162.34(13) . . . . ? C5 N1 C3 C2 176.69(19) . . . . ? Al1 N1 C3 C2 -16.9(3) . . . . ? C4 O2 C3 N1 -11.9(2) . . . . ? C4 O2 C3 C2 167.49(18) . . . . ? C19 N3 C17 O4 -3.0(2) . . . . ? Al1 N3 C17 O4 156.64(13) . . . . ? C19 N3 C17 C16 176.64(19) . . . . ? Al1 N3 C17 C16 -23.7(3) . . . . ? C18 O4 C17 N3 -9.8(2) . . . . ? C18 O4 C17 C16 170.50(18) . . . . ? C10 C9 C2 C1 -3.0(3) . . . . ? C10 C9 C2 C3 -177.7(2) . . . . ? N1 C3 C2 C1 21.4(3) . . . . ? O2 C3 C2 C1 -157.88(19) . . . . ? N1 C3 C2 C9 -163.7(2) . . . . ? O2 C3 C2 C9 17.0(3) . . . . ? Al1 O1 C1 C2 -26.0(3) . . . . ? Al1 O1 C1 C12 156.53(16) . . . . ? C9 C2 C1 O1 -175.1(2) . . . . ? C3 C2 C1 O1 -0.3(3) . . . . ? C9 C2 C1 C12 2.4(3) . . . . ? C3 C2 C1 C12 177.28(19) . . . . ? O1 C1 C12 C11 176.5(2) . . . . ? C2 C1 C12 C11 -1.1(3) . . . . ? O1 C1 C12 C13 -5.4(3) . . . . ? C2 C1 C12 C13 176.9(2) . . . . ? N2 C13 C12 C11 -7(13) . . . . ? N2 C13 C12 C1 175(100) . . . . ? Al1 O5 C29 C30 2.7(3) . . . . ? Al1 O5 C29 C40 -177.03(15) . . . . ? C39 C40 C29 O5 175.8(2) . . . . ? C41 C40 C29 O5 -4.6(3) . . . . ? C39 C40 C29 C30 -3.9(3) . . . . ? C41 C40 C29 C30 175.6(2) . . . . ? O3 C15 C26 C25 178.5(2) . . . . ? C16 C15 C26 C25 -1.4(3) . . . . ? O3 C15 C26 C27 -2.8(3) . . . . ? C16 C15 C26 C27 177.27(19) . . . . ? N4 C27 C26 C25 121(10) . . . . ? N4 C27 C26 C15 -57(10) . . . . ? C24 C23 C16 C15 -0.1(3) . . . . ? C24 C23 C16 C17 -179.9(2) . . . . ? O3 C15 C16 C23 -178.97(19) . . . . ? C26 C15 C16 C23 1.0(3) . . . . ? O3 C15 C16 C17 0.8(3) . . . . ? C26 C15 C16 C17 -179.22(18) . . . . ? N3 C17 C16 C23 -170.6(2) . . . . ? O4 C17 C16 C23 9.1(3) . . . . ? N3 C17 C16 C15 9.6(3) . . . . ? O4 C17 C16 C15 -170.71(17) . . . . ? C15 C26 C25 C24 1.0(4) . . . . ? C27 C26 C25 C24 -177.7(2) . . . . ? C33 N5 C31 O6 -3.5(3) . . . . ? Al1 N5 C31 O6 169.10(15) . . . . ? C33 N5 C31 C30 176.0(2) . . . . ? Al1 N5 C31 C30 -11.5(3) . . . . ? C32 O6 C31 N5 -10.5(3) . . . . ? C32 O6 C31 C30 170.0(2) . . . . ? C2 C9 C10 C11 2.0(3) . . . . ? C2 C9 C10 C14 -177.8(2) . . . . ? C31 O6 C32 C33 19.1(2) . . . . ? N3 C19 C20 C21 68.7(2) . . . . ? C18 C19 C20 C21 -46.2(3) . . . . ? N3 C19 C20 C22 -165.82(18) . . . . ? C18 C19 C20 C22 79.3(2) . . . . ? O5 C29 C30 C37 -175.2(2) . . . . ? C40 C29 C30 C37 4.6(3) . . . . ? O5 C29 C30 C31 5.1(3) . . . . ? C40 C29 C30 C31 -175.2(2) . . . . ? N5 C31 C30 C37 -179.5(2) . . . . ? O6 C31 C30 C37 0.0(3) . . . . ? N5 C31 C30 C29 0.3(4) . . . . ? O6 C31 C30 C29 179.7(2) . . . . ? C29 C30 C37 C38 -1.8(4) . . . . ? C31 C30 C37 C38 177.9(2) . . . . ? C17 O4 C18 C19 17.5(2) . . . . ? N3 C19 C18 O4 -18.5(2) . . . . ? C20 C19 C18 O4 100.8(2) . . . . ? C31 N5 C33 C32 15.0(2) . . . . ? Al1 N5 C33 C32 -157.47(16) . . . . ? C31 N5 C33 C34 -107.5(2) . . . . ? Al1 N5 C33 C34 80.0(2) . . . . ? O6 C32 C33 N5 -20.3(2) . . . . ? O6 C32 C33 C34 100.3(2) . . . . ? C39 C40 C41 N6 33(9) . . . . ? C29 C40 C41 N6 -147(9) . . . . ? N5 C33 C34 C35 -165.2(2) . . . . ? C32 C33 C34 C35 79.6(3) . . . . ? N5 C33 C34 C36 69.6(2) . . . . ? C32 C33 C34 C36 -45.5(3) . . . . ? C3 O2 C4 C5 21.7(2) . . . . ? C1 C12 C11 C10 0.3(3) . . . . ? C13 C12 C11 C10 -177.7(2) . . . . ? C9 C10 C11 C12 -0.7(3) . . . . ? C14 C10 C11 C12 179.1(2) . . . . ? C30 C37 C38 C39 -1.8(4) . . . . ? C30 C37 C38 C42 178.8(3) . . . . ? C3 N1 C5 C4 17.4(2) . . . . ? Al1 N1 C5 C4 -148.15(15) . . . . ? C3 N1 C5 C6 -105.1(2) . . . . ? Al1 N1 C5 C6 89.4(2) . . . . ? O2 C4 C5 N1 -23.4(2) . . . . ? O2 C4 C5 C6 97.3(2) . . . . ? C7 C6 C5 N1 -178.3(2) . . . . ? C8 C6 C5 N1 56.8(3) . . . . ? C7 C6 C5 C4 66.1(3) . . . . ? C8 C6 C5 C4 -58.8(3) . . . . ? C37 C38 C39 C40 2.5(4) . . . . ? C42 C38 C39 C40 -178.1(3) . . . . ? C29 C40 C39 C38 0.5(4) . . . . ? C41 C40 C39 C38 -179.1(2) . . . . ? C26 C25 C24 C23 0.0(4) . . . . ? C26 C25 C24 C28 -179.3(3) . . . . ? C16 C23 C24 C25 -0.4(4) . . . . ? C16 C23 C24 C28 178.9(3) . . . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 27.10 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.240 _refine_diff_density_min -0.274 _refine_diff_density_rms 0.039 _database_code_depnum_ccdc_archive 'CCDC 957729' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_AlMe2Nap3 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C49 H49 Al N3 O7' _chemical_formula_weight 816.91 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Al Al 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 17.708(2) _cell_length_b 15.631(2) _cell_length_c 16.899(2) _cell_angle_alpha 90.00 _cell_angle_beta 95.357(3) _cell_angle_gamma 90.00 _cell_volume 4657.1(10) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.165 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1888 _exptl_absorpt_coefficient_mu 0.102 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.9739 _exptl_absorpt_correction_T_max 0.9949 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Rotating Anode' _diffrn_radiation_monochromator 'Confocal Optics' _diffrn_measurement_device_type 'Rigaku AFC12 (Right) with Saturn724+ CCD' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 24640 _diffrn_reflns_av_R_equivalents 0.0760 _diffrn_reflns_av_sigmaI/netI 0.0865 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.78 _diffrn_reflns_theta_max 22.01 _reflns_number_total 5709 _reflns_number_gt 3488 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear-SM Expert 2.0 r5 (Rigaku, 2010)' _computing_cell_refinement 'SAINT v7.68A (Bruker, 2009)' _computing_data_reduction 'SAINT v7.68A (Bruker, 2009)' _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. ; _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^)+(0.1029P)^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 5709 _refine_ls_number_parameters 544 _refine_ls_number_restraints 29 _refine_ls_R_factor_all 0.1093 _refine_ls_R_factor_gt 0.0655 _refine_ls_wR_factor_ref 0.1801 _refine_ls_wR_factor_gt 0.1612 _refine_ls_goodness_of_fit_ref 0.996 _refine_ls_restrained_S_all 1.009 _refine_ls_shift/su_max 0.005 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Al1 Al 0.09591(7) -0.00464(9) 0.30002(7) 0.0371(4) Uani 1 1 d . . . O1 O 0.06733(16) 0.10176(19) 0.33629(16) 0.0393(8) Uani 1 1 d . . . O2 O 0.14268(17) 0.0067(2) 0.54968(16) 0.0453(8) Uani 1 1 d . . . O3 O 0.19306(16) 0.03301(18) 0.30137(16) 0.0387(8) Uani 1 1 d . . . O4 O 0.23486(16) -0.2160(2) 0.25686(18) 0.0492(9) Uani 1 1 d . . . O6 O -0.00443(16) 0.08194(19) 0.07998(16) 0.0428(8) Uani 1 1 d . . . O5 O 0.00316(16) -0.05205(18) 0.29277(16) 0.0389(8) Uani 1 1 d . . . N1 N 0.11057(19) -0.0347(2) 0.4227(2) 0.0374(9) Uani 1 1 d . . . N2 N 0.1406(2) -0.1203(2) 0.26513(19) 0.0367(9) Uani 1 1 d . . . N3 N 0.0700(2) 0.0371(2) 0.18671(19) 0.0358(9) Uani 1 1 d . . . C1 C 0.1150(2) 0.1472(3) 0.3840(2) 0.0370(11) Uani 1 1 d . . . C2 C 0.1570(2) 0.1121(3) 0.4504(2) 0.0384(11) Uani 1 1 d . . . C3 C 0.1370(2) 0.0251(3) 0.4706(3) 0.0397(12) Uani 1 1 d . . . C4 C 0.1015(3) -0.0717(3) 0.5576(3) 0.0496(13) Uani 1 1 d . . . H4A H 0.0507 -0.0602 0.5751 0.060 Uiso 1 1 calc R . . H4B H 0.1294 -0.1104 0.5965 0.060 Uiso 1 1 calc R . . C5 C 0.0950(2) -0.1111(3) 0.4743(2) 0.0371(11) Uani 1 1 d . . . C6 C 0.1561(3) -0.1781(3) 0.4677(3) 0.0463(12) Uani 1 1 d . . . H6A H 0.1546 -0.1980 0.4126 0.070 Uiso 1 1 calc R . . H6B H 0.1472 -0.2265 0.5025 0.070 Uiso 1 1 calc R . . H6C H 0.2059 -0.1530 0.4837 0.070 Uiso 1 1 calc R . . C7 C 0.0163(3) -0.1473(3) 0.4542(3) 0.0488(13) Uani 1 1 d . . . H7A H -0.0211 -0.1011 0.4543 0.073 Uiso 1 1 calc R . . H7B H 0.0058 -0.1904 0.4938 0.073 Uiso 1 1 calc R . . H7C H 0.0132 -0.1737 0.4014 0.073 Uiso 1 1 calc R . . C8 C 0.2138(2) 0.1611(3) 0.4969(3) 0.0439(12) Uani 1 1 d . . . C9 C 0.2251(3) 0.2473(3) 0.4758(3) 0.0457(13) Uani 1 1 d . . . C10 C 0.1777(3) 0.2828(3) 0.4111(3) 0.0483(13) Uani 1 1 d . . . H10 H 0.1833 0.3414 0.3980 0.058 Uiso 1 1 calc R . . C11 C 0.1254(3) 0.2355(3) 0.3684(3) 0.0407(12) Uani 1 1 d . . . H11 H 0.0944 0.2619 0.3264 0.049 Uiso 1 1 calc R . . C12 C 0.2836(3) 0.2955(3) 0.5169(3) 0.0514(13) Uani 1 1 d . . . H12 H 0.2910 0.3530 0.5014 0.062 Uiso 1 1 calc R . . C13 C 0.3293(3) 0.2623(4) 0.5779(3) 0.0622(15) Uani 1 1 d . . . H13 H 0.3677 0.2960 0.6059 0.075 Uiso 1 1 calc R . . C14 C 0.3183(3) 0.1765(4) 0.5985(3) 0.0624(15) Uani 1 1 d . . . H14 H 0.3506 0.1519 0.6405 0.075 Uiso 1 1 calc R . . C15 C 0.2627(3) 0.1271(4) 0.5601(3) 0.0521(13) Uani 1 1 d . . . H15 H 0.2568 0.0694 0.5761 0.063 Uiso 1 1 calc R . . C16 C 0.2573(2) -0.0019(3) 0.3298(2) 0.0373(11) Uani 1 1 d . . . C17 C 0.2688(2) -0.0893(3) 0.3299(2) 0.0351(11) Uani 1 1 d . . . C18 C 0.2112(3) -0.1402(3) 0.2846(2) 0.0375(11) Uani 1 1 d . . . C19 C 0.1747(3) -0.2470(3) 0.2003(3) 0.0570(14) Uani 1 1 d . . . H19A H 0.1652 -0.3086 0.2086 0.068 Uiso 1 1 calc R . . H19B H 0.1876 -0.2384 0.1451 0.068 Uiso 1 1 calc R . . C20 C 0.1055(2) -0.1936(3) 0.2166(2) 0.0416(12) Uani 1 1 d . . . C21 C 0.0620(3) -0.1644(3) 0.1399(2) 0.0452(12) Uani 1 1 d . . . H21A H 0.0186 -0.1295 0.1521 0.068 Uiso 1 1 calc R . . H21B H 0.0439 -0.2144 0.1088 0.068 Uiso 1 1 calc R . . H21C H 0.0954 -0.1303 0.1092 0.068 Uiso 1 1 calc R . . C22 C 0.0540(3) -0.2454(3) 0.2656(3) 0.0475(13) Uani 1 1 d . . . H22A H 0.0836 -0.2675 0.3131 0.071 Uiso 1 1 calc R . . H22B H 0.0322 -0.2933 0.2338 0.071 Uiso 1 1 calc R . . H22C H 0.0132 -0.2087 0.2815 0.071 Uiso 1 1 calc R . . C23 C 0.3393(3) -0.1252(3) 0.3655(3) 0.0428(12) Uani 1 1 d . . . C24 C 0.3978(3) -0.0671(3) 0.3943(3) 0.0496(13) Uani 1 1 d . . . C25 C 0.3850(3) 0.0222(3) 0.3884(3) 0.0559(14) Uani 1 1 d . . . H25 H 0.4248 0.0607 0.4056 0.067 Uiso 1 1 calc R . . C26 C 0.3169(3) 0.0534(3) 0.3586(3) 0.0457(12) Uani 1 1 d . . . H26 H 0.3090 0.1136 0.3569 0.055 Uiso 1 1 calc R . . C27 C 0.4678(3) -0.0988(4) 0.4292(3) 0.0676(16) Uani 1 1 d . . . H27 H 0.5070 -0.0598 0.4467 0.081 Uiso 1 1 calc R . . C28 C 0.4801(3) -0.1845(4) 0.4381(3) 0.0676(16) Uani 1 1 d . . . H28 H 0.5276 -0.2049 0.4612 0.081 Uiso 1 1 calc R . . C29 C 0.4230(3) -0.2419(4) 0.4134(3) 0.0611(15) Uani 1 1 d . . . H29 H 0.4311 -0.3015 0.4211 0.073 Uiso 1 1 calc R . . C30 C 0.3542(3) -0.2127(3) 0.3776(3) 0.0510(13) Uani 1 1 d . . . H30 H 0.3160 -0.2532 0.3608 0.061 Uiso 1 1 calc R . . C33 C 0.0020(3) 0.0458(3) 0.1537(2) 0.0367(11) Uani 1 1 d . . . C34 C 0.0719(2) 0.0868(3) 0.0563(2) 0.0425(12) Uani 1 1 d . . . H34A H 0.0799 0.1415 0.0287 0.051 Uiso 1 1 calc R . . H34B H 0.0819 0.0389 0.0204 0.051 Uiso 1 1 calc R . . C35 C 0.1233(2) 0.0811(3) 0.1343(2) 0.0375(11) Uani 1 1 d . . . C36 C 0.1421(2) 0.1704(3) 0.1670(3) 0.0419(12) Uani 1 1 d . . . H36A H 0.0950 0.2022 0.1715 0.063 Uiso 1 1 calc R . . H36B H 0.1731 0.2007 0.1310 0.063 Uiso 1 1 calc R . . H36C H 0.1702 0.1655 0.2196 0.063 Uiso 1 1 calc R . . C37 C 0.1935(2) 0.0297(3) 0.1233(2) 0.0414(12) Uani 1 1 d . . . H37A H 0.2276 0.0312 0.1724 0.062 Uiso 1 1 calc R . . H37B H 0.2194 0.0542 0.0797 0.062 Uiso 1 1 calc R . . H37C H 0.1793 -0.0296 0.1106 0.062 Uiso 1 1 calc R . . C32 C -0.0690(2) 0.0180(3) 0.1845(2) 0.0361(11) Uani 1 1 d . . . C31 C -0.0618(3) -0.0342(3) 0.2519(3) 0.0382(11) Uani 1 1 d . . . C41 C -0.1277(2) -0.0740(3) 0.2779(2) 0.0396(11) Uani 1 1 d . . . H41 H -0.1225 -0.1115 0.3223 0.048 Uiso 1 1 calc R . . C40 C -0.1968(3) -0.0595(3) 0.2408(3) 0.0481(13) Uani 1 1 d . . . H40 H -0.2396 -0.0872 0.2592 0.058 Uiso 1 1 calc R . . C39 C -0.2071(2) -0.0031(3) 0.1740(3) 0.0405(12) Uani 1 1 d . . . C38 C -0.1438(2) 0.0368(3) 0.1459(2) 0.0351(11) Uani 1 1 d . . . C45 C -0.1592(3) 0.0954(3) 0.0819(2) 0.0396(11) Uani 1 1 d . . . H45 H -0.1184 0.1261 0.0625 0.047 Uiso 1 1 calc R . . C44 C -0.2316(3) 0.1085(3) 0.0477(3) 0.0468(13) Uani 1 1 d . . . H44 H -0.2399 0.1478 0.0049 0.056 Uiso 1 1 calc R . . C43 C -0.2933(3) 0.0653(3) 0.0744(3) 0.0540(14) Uani 1 1 d . . . H43 H -0.3431 0.0738 0.0495 0.065 Uiso 1 1 calc R . . C42 C -0.2805(3) 0.0108(3) 0.1366(3) 0.0550(14) Uani 1 1 d . . . H42 H -0.3222 -0.0187 0.1555 0.066 Uiso 1 1 calc R . . O7A O 0.4111(8) 0.6472(9) 0.1997(9) 0.219(6) Uiso 0.625(9) 1 d PD A 1 C46A C 0.3802(11) 0.5601(11) 0.1625(13) 0.182(9) Uiso 0.625(9) 1 d PD A 1 C47A C 0.3135(12) 0.5966(10) 0.1202(12) 0.177(9) Uiso 0.625(9) 1 d PD A 1 H47A H 0.2698 0.5855 0.1514 0.213 Uiso 0.625(9) 1 calc PR A 1 H47B H 0.3036 0.5659 0.0690 0.213 Uiso 0.625(9) 1 calc PR A 1 C48A C 0.3158(6) 0.6876(7) 0.1035(7) 0.092(4) Uiso 0.625(9) 1 d PD A 1 H48A H 0.3174 0.6973 0.0458 0.111 Uiso 0.625(9) 1 calc PR A 1 H48B H 0.2700 0.7161 0.1205 0.111 Uiso 0.625(9) 1 calc PR A 1 C49A C 0.3810(9) 0.7208(11) 0.1455(11) 0.193(8) Uiso 0.625(9) 1 d PD A 1 H49A H 0.3686 0.7713 0.1773 0.232 Uiso 0.625(9) 1 calc PR A 1 H49B H 0.4188 0.7378 0.1088 0.232 Uiso 0.625(9) 1 calc PR A 1 O8B O 0.3983(17) 0.567(3) 0.196(2) 0.41(3) Uiso 0.375(9) 1 d PD A 2 C46B C 0.3196(11) 0.6091(13) 0.2048(10) 0.108(7) Uiso 0.375(9) 1 d PD A 2 H46A H 0.2838 0.5676 0.2251 0.129 Uiso 0.375(9) 1 calc PR A 2 H46B H 0.3247 0.6590 0.2410 0.129 Uiso 0.375(9) 1 calc PR A 2 C47B C 0.2962(9) 0.6337(17) 0.1281(10) 0.087(6) Uiso 0.375(9) 1 d PD A 2 H47C H 0.2850 0.6958 0.1266 0.105 Uiso 0.375(9) 1 calc PR A 2 H47D H 0.2493 0.6026 0.1090 0.105 Uiso 0.375(9) 1 calc PR A 2 C48B C 0.3547(13) 0.6151(18) 0.0780(11) 0.148(10) Uiso 0.375(9) 1 d PD A 2 H48C H 0.3537 0.6579 0.0347 0.178 Uiso 0.375(9) 1 calc PR A 2 H48D H 0.3460 0.5579 0.0537 0.178 Uiso 0.375(9) 1 calc PR A 2 C49B C 0.4280(13) 0.617(2) 0.124(2) 0.206(14) Uiso 0.375(9) 1 d PD A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Al1 0.0394(8) 0.0431(9) 0.0292(7) 0.0019(6) 0.0047(6) 0.0019(7) O1 0.0462(19) 0.043(2) 0.0289(16) 0.0000(14) 0.0056(14) 0.0019(15) O2 0.059(2) 0.052(2) 0.0247(18) 0.0036(15) 0.0026(14) 0.0059(17) O3 0.0391(19) 0.0443(19) 0.0336(17) -0.0021(14) 0.0079(14) 0.0025(16) O4 0.0431(19) 0.052(2) 0.052(2) -0.0114(17) 0.0011(16) 0.0062(17) O6 0.0425(19) 0.055(2) 0.0315(17) 0.0041(15) 0.0051(14) -0.0045(15) O5 0.0321(18) 0.048(2) 0.0360(17) 0.0047(14) 0.0004(14) 0.0004(15) N1 0.042(2) 0.039(2) 0.032(2) -0.0003(19) 0.0063(17) 0.0038(19) N2 0.035(2) 0.042(2) 0.032(2) -0.0006(17) 0.0007(17) -0.0009(19) N3 0.038(2) 0.039(2) 0.031(2) -0.0012(17) 0.0056(18) -0.0010(18) C1 0.046(3) 0.038(3) 0.028(3) -0.001(2) 0.008(2) 0.005(2) C2 0.048(3) 0.041(3) 0.028(3) -0.001(2) 0.009(2) 0.002(2) C3 0.035(3) 0.051(4) 0.034(3) 0.002(3) 0.002(2) 0.017(2) C4 0.064(3) 0.050(3) 0.036(3) 0.011(2) 0.012(2) 0.009(3) C5 0.042(3) 0.035(3) 0.035(3) 0.005(2) 0.008(2) 0.004(2) C6 0.054(3) 0.047(3) 0.038(3) 0.006(2) 0.005(2) 0.004(3) C7 0.055(3) 0.052(3) 0.042(3) 0.009(2) 0.014(2) 0.000(3) C8 0.041(3) 0.057(4) 0.034(3) -0.010(2) 0.006(2) 0.002(3) C9 0.048(3) 0.051(4) 0.040(3) -0.010(3) 0.012(2) 0.004(3) C10 0.057(3) 0.047(3) 0.042(3) -0.006(3) 0.011(3) 0.003(3) C11 0.049(3) 0.040(3) 0.033(3) -0.005(2) 0.003(2) 0.005(3) C12 0.047(3) 0.057(4) 0.050(3) -0.019(3) 0.009(3) -0.008(3) C13 0.051(3) 0.085(5) 0.050(3) -0.021(3) 0.001(3) 0.005(3) C14 0.054(4) 0.082(5) 0.050(3) -0.002(3) -0.001(3) 0.013(3) C15 0.052(3) 0.064(4) 0.039(3) -0.001(3) -0.002(2) -0.004(3) C16 0.031(3) 0.050(3) 0.031(2) -0.006(2) 0.004(2) 0.003(3) C17 0.032(3) 0.041(3) 0.032(2) -0.001(2) 0.005(2) 0.001(2) C18 0.049(3) 0.031(3) 0.034(3) -0.005(2) 0.011(2) -0.004(3) C19 0.048(3) 0.062(4) 0.060(3) -0.020(3) -0.004(3) 0.006(3) C20 0.042(3) 0.045(3) 0.037(3) -0.009(2) -0.002(2) -0.002(2) C21 0.057(3) 0.045(3) 0.033(3) -0.003(2) 0.005(2) -0.008(3) C22 0.050(3) 0.047(3) 0.043(3) -0.002(2) -0.007(2) -0.008(2) C23 0.042(3) 0.048(3) 0.039(3) -0.001(2) 0.007(2) 0.003(3) C24 0.041(3) 0.053(4) 0.054(3) 0.001(3) -0.003(2) 0.004(3) C25 0.042(3) 0.058(4) 0.066(4) -0.007(3) -0.003(3) -0.006(3) C26 0.042(3) 0.043(3) 0.051(3) -0.002(2) 0.001(2) -0.002(3) C27 0.041(3) 0.078(5) 0.081(4) -0.003(3) -0.010(3) -0.004(3) C28 0.043(3) 0.069(5) 0.088(4) 0.008(3) -0.006(3) 0.008(3) C29 0.049(3) 0.062(4) 0.072(4) 0.005(3) 0.005(3) 0.010(3) C30 0.042(3) 0.056(4) 0.055(3) 0.003(3) 0.008(2) 0.004(3) C33 0.041(3) 0.040(3) 0.029(3) -0.001(2) 0.002(2) 0.005(2) C34 0.043(3) 0.052(3) 0.034(3) 0.005(2) 0.011(2) 0.003(2) C35 0.038(3) 0.042(3) 0.033(3) 0.003(2) 0.009(2) -0.006(2) C36 0.042(3) 0.048(3) 0.037(3) 0.005(2) 0.010(2) -0.001(2) C37 0.048(3) 0.048(3) 0.029(3) 0.000(2) 0.007(2) -0.009(2) C32 0.038(3) 0.040(3) 0.031(3) -0.004(2) 0.005(2) -0.002(2) C31 0.040(3) 0.041(3) 0.034(3) -0.010(2) 0.006(2) -0.002(2) C41 0.035(3) 0.050(3) 0.035(3) 0.005(2) 0.004(2) -0.001(2) C40 0.039(3) 0.062(4) 0.044(3) -0.006(3) 0.009(2) -0.013(3) C39 0.030(3) 0.047(3) 0.045(3) -0.004(2) 0.003(2) -0.006(2) C38 0.033(3) 0.035(3) 0.036(3) -0.006(2) -0.002(2) 0.006(2) C45 0.040(3) 0.038(3) 0.041(3) -0.004(2) 0.005(2) -0.002(2) C44 0.048(3) 0.047(3) 0.045(3) -0.003(2) 0.002(2) 0.004(3) C43 0.038(3) 0.066(4) 0.057(3) -0.001(3) -0.002(2) 0.002(3) C42 0.036(3) 0.066(4) 0.064(4) 0.001(3) 0.009(3) -0.008(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 O5 1.796(3) . ? Al1 O3 1.816(3) . ? Al1 O1 1.859(3) . ? Al1 N3 2.034(4) . ? Al1 N2 2.080(4) . ? Al1 N1 2.118(4) . ? O1 C1 1.319(5) . ? O2 C3 1.361(5) . ? O2 C4 1.439(5) . ? O3 C16 1.312(5) . ? O4 C18 1.356(5) . ? O4 C19 1.447(5) . ? O6 C33 1.363(5) . ? O6 C34 1.447(5) . ? O5 C31 1.315(5) . ? N1 C3 1.296(5) . ? N1 C5 1.519(5) . ? N2 C18 1.299(5) . ? N2 C20 1.510(5) . ? N3 C33 1.286(5) . ? N3 C35 1.518(5) . ? C1 C2 1.400(6) . ? C1 C11 1.421(6) . ? C2 C8 1.437(6) . ? C2 C3 1.454(6) . ? C4 C5 1.531(6) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C7 1.512(6) . ? C5 C6 1.517(6) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 C9 1.412(6) . ? C8 C15 1.415(6) . ? C9 C12 1.411(6) . ? C9 C10 1.426(6) . ? C10 C11 1.341(6) . ? C10 H10 0.9500 . ? C11 H11 0.9500 . ? C12 C13 1.353(7) . ? C12 H12 0.9500 . ? C13 C14 1.404(7) . ? C13 H13 0.9500 . ? C14 C15 1.366(7) . ? C14 H14 0.9500 . ? C15 H15 0.9500 . ? C16 C17 1.382(6) . ? C16 C26 1.415(6) . ? C17 C23 1.447(6) . ? C17 C18 1.454(6) . ? C19 C20 1.528(6) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 C21 1.515(6) . ? C20 C22 1.521(6) . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 C30 1.405(6) . ? C23 C24 1.428(6) . ? C24 C27 1.412(7) . ? C24 C25 1.416(7) . ? C25 C26 1.354(6) . ? C25 H25 0.9500 . ? C26 H26 0.9500 . ? C27 C28 1.364(7) . ? C27 H27 0.9500 . ? C28 C29 1.385(7) . ? C28 H28 0.9500 . ? C29 C30 1.385(7) . ? C29 H29 0.9500 . ? C30 H30 0.9500 . ? C33 C32 1.470(6) . ? C34 C35 1.533(6) . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? C35 C37 1.507(6) . ? C35 C36 1.527(6) . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C32 C31 1.397(6) . ? C32 C38 1.450(6) . ? C31 C41 1.429(6) . ? C41 C40 1.340(6) . ? C41 H41 0.9500 . ? C40 C39 1.430(6) . ? C40 H40 0.9500 . ? C39 C38 1.405(6) . ? C39 C42 1.409(6) . ? C38 C45 1.424(6) . ? C45 C44 1.373(6) . ? C45 H45 0.9500 . ? C44 C43 1.395(6) . ? C44 H44 0.9500 . ? C43 C42 1.356(7) . ? C43 H43 0.9500 . ? C42 H42 0.9500 . ? O7A C49A 1.535(14) . ? O7A C46A 1.576(16) . ? C46A C47A 1.440(12) . ? C47A C48A 1.452(13) . ? C47A H47A 0.9900 . ? C47A H47B 0.9900 . ? C48A C49A 1.398(11) . ? C48A H48A 0.9900 . ? C48A H48B 0.9900 . ? C49A H49A 0.9900 . ? C49A H49B 0.9900 . ? O8B C46B 1.563(18) . ? O8B C49B 1.577(19) . ? C46B C47B 1.378(15) . ? C46B H46A 0.9900 . ? C46B H46B 0.9900 . ? C47B C48B 1.429(18) . ? C47B H47C 0.9900 . ? C47B H47D 0.9900 . ? C48B C49B 1.446(17) . ? C48B H48C 0.9900 . ? C48B H48D 0.9900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O5 Al1 O3 173.63(15) . . ? O5 Al1 O1 96.68(14) . . ? O3 Al1 O1 89.58(14) . . ? O5 Al1 N3 86.76(14) . . ? O3 Al1 N3 92.20(14) . . ? O1 Al1 N3 88.79(14) . . ? O5 Al1 N2 89.55(14) . . ? O3 Al1 N2 84.25(14) . . ? O1 Al1 N2 173.31(16) . . ? N3 Al1 N2 94.04(14) . . ? O5 Al1 N1 90.16(14) . . ? O3 Al1 N1 91.73(14) . . ? O1 Al1 N1 83.58(13) . . ? N3 Al1 N1 171.39(15) . . ? N2 Al1 N1 93.97(14) . . ? C1 O1 Al1 120.3(3) . . ? C3 O2 C4 106.3(3) . . ? C16 O3 Al1 131.1(3) . . ? C18 O4 C19 106.8(3) . . ? C33 O6 C34 106.0(3) . . ? C31 O5 Al1 134.2(3) . . ? C3 N1 C5 106.4(3) . . ? C3 N1 Al1 117.1(3) . . ? C5 N1 Al1 136.4(3) . . ? C18 N2 C20 107.1(3) . . ? C18 N2 Al1 121.2(3) . . ? C20 N2 Al1 131.7(3) . . ? C33 N3 C35 107.9(3) . . ? C33 N3 Al1 124.2(3) . . ? C35 N3 Al1 126.6(3) . . ? O1 C1 C2 122.8(4) . . ? O1 C1 C11 119.8(4) . . ? C2 C1 C11 117.4(4) . . ? C1 C2 C8 121.5(4) . . ? C1 C2 C3 115.5(4) . . ? C8 C2 C3 122.9(4) . . ? N1 C3 O2 116.7(4) . . ? N1 C3 C2 127.6(4) . . ? O2 C3 C2 115.5(4) . . ? O2 C4 C5 104.6(3) . . ? O2 C4 H4A 110.8 . . ? C5 C4 H4A 110.8 . . ? O2 C4 H4B 110.8 . . ? C5 C4 H4B 110.8 . . ? H4A C4 H4B 108.9 . . ? C7 C5 C6 112.0(4) . . ? C7 C5 N1 112.2(3) . . ? C6 C5 N1 109.3(3) . . ? C7 C5 C4 110.2(3) . . ? C6 C5 C4 110.6(4) . . ? N1 C5 C4 102.1(3) . . ? C5 C6 H6A 109.5 . . ? C5 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C5 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C5 C7 H7A 109.5 . . ? C5 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C5 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C9 C8 C15 117.3(4) . . ? C9 C8 C2 118.6(4) . . ? C15 C8 C2 124.1(5) . . ? C12 C9 C8 120.0(5) . . ? C12 C9 C10 121.5(5) . . ? C8 C9 C10 118.5(5) . . ? C11 C10 C9 121.7(5) . . ? C11 C10 H10 119.2 . . ? C9 C10 H10 119.2 . . ? C10 C11 C1 122.0(5) . . ? C10 C11 H11 119.0 . . ? C1 C11 H11 119.0 . . ? C13 C12 C9 122.0(5) . . ? C13 C12 H12 119.0 . . ? C9 C12 H12 119.0 . . ? C12 C13 C14 117.9(5) . . ? C12 C13 H13 121.1 . . ? C14 C13 H13 121.1 . . ? C15 C14 C13 122.2(5) . . ? C15 C14 H14 118.9 . . ? C13 C14 H14 118.9 . . ? C14 C15 C8 120.6(5) . . ? C14 C15 H15 119.7 . . ? C8 C15 H15 119.7 . . ? O3 C16 C17 122.3(4) . . ? O3 C16 C26 117.8(4) . . ? C17 C16 C26 119.9(4) . . ? C16 C17 C23 120.3(4) . . ? C16 C17 C18 116.3(4) . . ? C23 C17 C18 122.9(4) . . ? N2 C18 O4 116.3(4) . . ? N2 C18 C17 127.9(4) . . ? O4 C18 C17 115.8(4) . . ? O4 C19 C20 104.6(3) . . ? O4 C19 H19A 110.8 . . ? C20 C19 H19A 110.8 . . ? O4 C19 H19B 110.8 . . ? C20 C19 H19B 110.8 . . ? H19A C19 H19B 108.9 . . ? N2 C20 C21 112.7(4) . . ? N2 C20 C22 110.2(3) . . ? C21 C20 C22 110.1(4) . . ? N2 C20 C19 102.5(3) . . ? C21 C20 C19 111.3(4) . . ? C22 C20 C19 109.8(4) . . ? C20 C21 H21A 109.5 . . ? C20 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C20 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C20 C22 H22A 109.5 . . ? C20 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C20 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C30 C23 C24 116.7(4) . . ? C30 C23 C17 125.5(4) . . ? C24 C23 C17 117.7(4) . . ? C27 C24 C25 120.2(5) . . ? C27 C24 C23 119.9(5) . . ? C25 C24 C23 119.9(4) . . ? C26 C25 C24 120.8(5) . . ? C26 C25 H25 119.6 . . ? C24 C25 H25 119.6 . . ? C25 C26 C16 121.2(5) . . ? C25 C26 H26 119.4 . . ? C16 C26 H26 119.4 . . ? C28 C27 C24 121.1(5) . . ? C28 C27 H27 119.5 . . ? C24 C27 H27 119.5 . . ? C27 C28 C29 119.9(5) . . ? C27 C28 H28 120.1 . . ? C29 C28 H28 120.1 . . ? C28 C29 C30 120.4(5) . . ? C28 C29 H29 119.8 . . ? C30 C29 H29 119.8 . . ? C29 C30 C23 122.0(5) . . ? C29 C30 H30 119.0 . . ? C23 C30 H30 119.0 . . ? N3 C33 O6 115.8(4) . . ? N3 C33 C32 127.7(4) . . ? O6 C33 C32 116.4(4) . . ? O6 C34 C35 104.7(3) . . ? O6 C34 H34A 110.8 . . ? C35 C34 H34A 110.8 . . ? O6 C34 H34B 110.8 . . ? C35 C34 H34B 110.8 . . ? H34A C34 H34B 108.9 . . ? C37 C35 N3 113.3(3) . . ? C37 C35 C36 112.1(4) . . ? N3 C35 C36 109.2(3) . . ? C37 C35 C34 110.9(3) . . ? N3 C35 C34 100.2(3) . . ? C36 C35 C34 110.5(4) . . ? C35 C36 H36A 109.5 . . ? C35 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C35 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C35 C37 H37A 109.5 . . ? C35 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C35 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C31 C32 C38 119.6(4) . . ? C31 C32 C33 116.4(4) . . ? C38 C32 C33 123.8(4) . . ? O5 C31 C32 124.2(4) . . ? O5 C31 C41 116.4(4) . . ? C32 C31 C41 119.4(4) . . ? C40 C41 C31 121.2(4) . . ? C40 C41 H41 119.4 . . ? C31 C41 H41 119.4 . . ? C41 C40 C39 121.2(4) . . ? C41 C40 H40 119.4 . . ? C39 C40 H40 119.4 . . ? C38 C39 C42 120.8(4) . . ? C38 C39 C40 119.5(4) . . ? C42 C39 C40 119.6(4) . . ? C39 C38 C45 116.1(4) . . ? C39 C38 C32 118.9(4) . . ? C45 C38 C32 125.0(4) . . ? C44 C45 C38 121.4(4) . . ? C44 C45 H45 119.3 . . ? C38 C45 H45 119.3 . . ? C45 C44 C43 121.4(5) . . ? C45 C44 H44 119.3 . . ? C43 C44 H44 119.3 . . ? C42 C43 C44 118.4(5) . . ? C42 C43 H43 120.8 . . ? C44 C43 H43 120.8 . . ? C43 C42 C39 121.7(4) . . ? C43 C42 H42 119.1 . . ? C39 C42 H42 119.1 . . ? C49A O7A C46A 108.7(14) . . ? C47A C46A O7A 95.5(12) . . ? C46A C47A C48A 116.6(12) . . ? C46A C47A H47A 108.1 . . ? C48A C47A H47A 108.1 . . ? C46A C47A H47B 108.1 . . ? C48A C47A H47B 108.1 . . ? H47A C47A H47B 107.3 . . ? C49A C48A C47A 107.6(10) . . ? C49A C48A H48A 110.2 . . ? C47A C48A H48A 110.2 . . ? C49A C48A H48B 110.2 . . ? C47A C48A H48B 110.2 . . ? H48A C48A H48B 108.5 . . ? C48A C49A O7A 104.4(12) . . ? C48A C49A H49A 110.9 . . ? O7A C49A H49A 110.9 . . ? C48A C49A H49B 110.9 . . ? O7A C49A H49B 110.9 . . ? H49A C49A H49B 108.9 . . ? C46B O8B C49B 103(2) . . ? C47B C46B O8B 102.5(15) . . ? C47B C46B H46A 111.3 . . ? O8B C46B H46A 111.3 . . ? C47B C46B H46B 111.3 . . ? O8B C46B H46B 111.3 . . ? H46A C46B H46B 109.2 . . ? C46B C47B C48B 109.3(13) . . ? C46B C47B H47C 109.8 . . ? C48B C47B H47C 109.8 . . ? C46B C47B H47D 109.8 . . ? C48B C47B H47D 109.8 . . ? H47C C47B H47D 108.3 . . ? C47B C48B C49B 110.1(16) . . ? C47B C48B H48C 109.6 . . ? C49B C48B H48C 109.6 . . ? C47B C48B H48D 109.6 . . ? C49B C48B H48D 109.6 . . ? H48C C48B H48D 108.2 . . ? C48B C49B O8B 93.2(17) . . ? 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 O5 Al1 O1 C1 148.9(3) . . . . ? O3 Al1 O1 C1 -32.3(3) . . . . ? N3 Al1 O1 C1 -124.5(3) . . . . ? N2 Al1 O1 C1 -9.4(13) . . . . ? N1 Al1 O1 C1 59.5(3) . . . . ? O5 Al1 O3 C16 -58.2(14) . . . . ? O1 Al1 O3 C16 132.5(3) . . . . ? N3 Al1 O3 C16 -138.7(3) . . . . ? N2 Al1 O3 C16 -44.8(3) . . . . ? N1 Al1 O3 C16 49.0(3) . . . . ? O3 Al1 O5 C31 -108.5(13) . . . . ? O1 Al1 O5 C31 60.6(4) . . . . ? N3 Al1 O5 C31 -27.8(4) . . . . ? N2 Al1 O5 C31 -121.9(4) . . . . ? N1 Al1 O5 C31 144.2(4) . . . . ? O5 Al1 N1 C3 -133.6(3) . . . . ? O3 Al1 N1 C3 52.5(3) . . . . ? O1 Al1 N1 C3 -36.9(3) . . . . ? N3 Al1 N1 C3 -64.7(11) . . . . ? N2 Al1 N1 C3 136.8(3) . . . . ? O5 Al1 N1 C5 43.3(4) . . . . ? O3 Al1 N1 C5 -130.6(4) . . . . ? O1 Al1 N1 C5 140.0(4) . . . . ? N3 Al1 N1 C5 112.3(10) . . . . ? N2 Al1 N1 C5 -46.2(4) . . . . ? O5 Al1 N2 C18 -154.9(3) . . . . ? O3 Al1 N2 C18 26.6(3) . . . . ? O1 Al1 N2 C18 3.6(13) . . . . ? N3 Al1 N2 C18 118.4(3) . . . . ? N1 Al1 N2 C18 -64.7(3) . . . . ? O5 Al1 N2 C20 25.6(3) . . . . ? O3 Al1 N2 C20 -152.9(3) . . . . ? O1 Al1 N2 C20 -175.9(10) . . . . ? N3 Al1 N2 C20 -61.1(3) . . . . ? N1 Al1 N2 C20 115.8(3) . . . . ? O5 Al1 N3 C33 21.7(4) . . . . ? O3 Al1 N3 C33 -164.6(3) . . . . ? O1 Al1 N3 C33 -75.1(4) . . . . ? N2 Al1 N3 C33 111.0(4) . . . . ? N1 Al1 N3 C33 -47.5(12) . . . . ? O5 Al1 N3 C35 -173.0(3) . . . . ? O3 Al1 N3 C35 0.7(3) . . . . ? O1 Al1 N3 C35 90.2(3) . . . . ? N2 Al1 N3 C35 -83.7(3) . . . . ? N1 Al1 N3 C35 117.8(10) . . . . ? Al1 O1 C1 C2 -46.4(5) . . . . ? Al1 O1 C1 C11 133.2(3) . . . . ? O1 C1 C2 C8 173.9(3) . . . . ? C11 C1 C2 C8 -5.7(6) . . . . ? O1 C1 C2 C3 -8.6(6) . . . . ? C11 C1 C2 C3 171.8(4) . . . . ? C5 N1 C3 O2 -1.1(5) . . . . ? Al1 N1 C3 O2 176.8(3) . . . . ? C5 N1 C3 C2 -176.7(4) . . . . ? Al1 N1 C3 C2 1.1(6) . . . . ? C4 O2 C3 N1 -11.7(5) . . . . ? C4 O2 C3 C2 164.5(4) . . . . ? C1 C2 C3 N1 30.5(6) . . . . ? C8 C2 C3 N1 -152.1(4) . . . . ? C1 C2 C3 O2 -145.2(4) . . . . ? C8 C2 C3 O2 32.2(6) . . . . ? C3 O2 C4 C5 18.6(4) . . . . ? C3 N1 C5 C7 130.3(4) . . . . ? Al1 N1 C5 C7 -46.9(5) . . . . ? C3 N1 C5 C6 -104.8(4) . . . . ? Al1 N1 C5 C6 78.0(5) . . . . ? C3 N1 C5 C4 12.4(4) . . . . ? Al1 N1 C5 C4 -164.8(3) . . . . ? O2 C4 C5 C7 -138.0(4) . . . . ? O2 C4 C5 C6 97.7(4) . . . . ? O2 C4 C5 N1 -18.6(4) . . . . ? C1 C2 C8 C9 2.0(6) . . . . ? C3 C2 C8 C9 -175.3(4) . . . . ? C1 C2 C8 C15 -174.1(4) . . . . ? C3 C2 C8 C15 8.7(6) . . . . ? C15 C8 C9 C12 0.4(6) . . . . ? C2 C8 C9 C12 -176.0(4) . . . . ? C15 C8 C9 C10 178.7(4) . . . . ? C2 C8 C9 C10 2.3(6) . . . . ? C12 C9 C10 C11 175.5(4) . . . . ? C8 C9 C10 C11 -2.8(6) . . . . ? C9 C10 C11 C1 -1.1(6) . . . . ? O1 C1 C11 C10 -174.3(4) . . . . ? C2 C1 C11 C10 5.3(6) . . . . ? C8 C9 C12 C13 -1.1(6) . . . . ? C10 C9 C12 C13 -179.4(4) . . . . ? C9 C12 C13 C14 1.5(7) . . . . ? C12 C13 C14 C15 -1.2(7) . . . . ? C13 C14 C15 C8 0.5(7) . . . . ? C9 C8 C15 C14 0.0(6) . . . . ? C2 C8 C15 C14 176.1(4) . . . . ? Al1 O3 C16 C17 33.3(5) . . . . ? Al1 O3 C16 C26 -149.0(3) . . . . ? O3 C16 C17 C23 -176.9(3) . . . . ? C26 C16 C17 C23 5.4(6) . . . . ? O3 C16 C17 C18 10.3(6) . . . . ? C26 C16 C17 C18 -167.4(4) . . . . ? C20 N2 C18 O4 1.4(5) . . . . ? Al1 N2 C18 O4 -178.2(3) . . . . ? C20 N2 C18 C17 178.6(4) . . . . ? Al1 N2 C18 C17 -1.0(6) . . . . ? C19 O4 C18 N2 9.7(5) . . . . ? C19 O4 C18 C17 -167.9(4) . . . . ? C16 C17 C18 N2 -23.8(6) . . . . ? C23 C17 C18 N2 163.6(4) . . . . ? C16 C17 C18 O4 153.5(4) . . . . ? C23 C17 C18 O4 -19.1(5) . . . . ? C18 O4 C19 C20 -15.9(5) . . . . ? C18 N2 C20 C21 -130.7(4) . . . . ? Al1 N2 C20 C21 48.8(5) . . . . ? C18 N2 C20 C22 105.8(4) . . . . ? Al1 N2 C20 C22 -74.6(5) . . . . ? C18 N2 C20 C19 -11.0(4) . . . . ? Al1 N2 C20 C19 168.5(3) . . . . ? O4 C19 C20 N2 16.1(5) . . . . ? O4 C19 C20 C21 136.8(4) . . . . ? O4 C19 C20 C22 -101.1(4) . . . . ? C16 C17 C23 C30 172.0(4) . . . . ? C18 C17 C23 C30 -15.7(6) . . . . ? C16 C17 C23 C24 -4.9(6) . . . . ? C18 C17 C23 C24 167.4(4) . . . . ? C30 C23 C24 C27 3.1(6) . . . . ? C17 C23 C24 C27 -179.7(4) . . . . ? C30 C23 C24 C25 -176.3(4) . . . . ? C17 C23 C24 C25 0.9(6) . . . . ? C27 C24 C25 C26 -176.8(5) . . . . ? C23 C24 C25 C26 2.6(7) . . . . ? C24 C25 C26 C16 -2.2(7) . . . . ? O3 C16 C26 C25 -179.6(4) . . . . ? C17 C16 C26 C25 -1.9(6) . . . . ? C25 C24 C27 C28 177.5(5) . . . . ? C23 C24 C27 C28 -1.9(8) . . . . ? C24 C27 C28 C29 -0.6(8) . . . . ? C27 C28 C29 C30 1.8(8) . . . . ? C28 C29 C30 C23 -0.5(7) . . . . ? C24 C23 C30 C29 -2.0(6) . . . . ? C17 C23 C30 C29 -178.9(4) . . . . ? C35 N3 C33 O6 6.6(5) . . . . ? Al1 N3 C33 O6 174.2(3) . . . . ? C35 N3 C33 C32 -176.5(4) . . . . ? Al1 N3 C33 C32 -8.8(6) . . . . ? C34 O6 C33 N3 9.2(5) . . . . ? C34 O6 C33 C32 -168.1(4) . . . . ? C33 O6 C34 C35 -20.3(4) . . . . ? C33 N3 C35 C37 -136.4(4) . . . . ? Al1 N3 C35 C37 56.4(5) . . . . ? C33 N3 C35 C36 97.9(4) . . . . ? Al1 N3 C35 C36 -69.4(4) . . . . ? C33 N3 C35 C34 -18.2(4) . . . . ? Al1 N3 C35 C34 174.5(3) . . . . ? O6 C34 C35 C37 142.7(3) . . . . ? O6 C34 C35 N3 22.7(4) . . . . ? O6 C34 C35 C36 -92.3(4) . . . . ? N3 C33 C32 C31 -9.5(7) . . . . ? O6 C33 C32 C31 167.4(4) . . . . ? N3 C33 C32 C38 174.8(4) . . . . ? O6 C33 C32 C38 -8.3(6) . . . . ? Al1 O5 C31 C32 18.1(6) . . . . ? Al1 O5 C31 C41 -164.1(3) . . . . ? C38 C32 C31 O5 -177.1(4) . . . . ? C33 C32 C31 O5 7.0(6) . . . . ? C38 C32 C31 C41 5.2(6) . . . . ? C33 C32 C31 C41 -170.7(4) . . . . ? O5 C31 C41 C40 179.4(4) . . . . ? C32 C31 C41 C40 -2.7(7) . . . . ? C31 C41 C40 C39 -0.5(7) . . . . ? C41 C40 C39 C38 1.1(7) . . . . ? C41 C40 C39 C42 -179.8(4) . . . . ? C42 C39 C38 C45 4.0(6) . . . . ? C40 C39 C38 C45 -176.9(4) . . . . ? C42 C39 C38 C32 -177.7(4) . . . . ? C40 C39 C38 C32 1.4(6) . . . . ? C31 C32 C38 C39 -4.6(6) . . . . ? C33 C32 C38 C39 170.9(4) . . . . ? C31 C32 C38 C45 173.6(4) . . . . ? C33 C32 C38 C45 -10.9(7) . . . . ? C39 C38 C45 C44 -3.0(6) . . . . ? C32 C38 C45 C44 178.8(4) . . . . ? C38 C45 C44 C43 0.3(7) . . . . ? C45 C44 C43 C42 1.4(7) . . . . ? C44 C43 C42 C39 -0.4(7) . . . . ? C38 C39 C42 C43 -2.5(7) . . . . ? C40 C39 C42 C43 178.4(5) . . . . ? C49A O7A C46A C47A -26.1(19) . . . . ? O7A C46A C47A C48A 22(2) . . . . ? C46A C47A C48A C49A -9(3) . . . . ? C47A C48A C49A O7A -9(2) . . . . ? C46A O7A C49A C48A 23.1(18) . . . . ? C49B O8B C46B C47B 30(3) . . . . ? O8B C46B C47B C48B -4(3) . . . . ? C46B C47B C48B C49B -28(3) . . . . ? C47B C48B C49B O8B 43(3) . . . . ? C46B O8B C49B C48B -43(3) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 22.01 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.569 _refine_diff_density_min -0.386 _refine_diff_density_rms 0.056 _database_code_depnum_ccdc_archive 'CCDC 957730' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_AliPr2Nap3 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C48 H48 Al N3 O6' _chemical_formula_weight 789.87 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 P21 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 13.640(2) _cell_length_b 10.6561(15) _cell_length_c 14.196(2) _cell_angle_alpha 90.00 _cell_angle_beta 95.130(4) _cell_angle_gamma 90.00 _cell_volume 2055.0(5) _cell_formula_units_Z 2 _cell_measurement_temperature 90(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.17 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.276 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 836 _exptl_absorpt_coefficient_mu 0.104 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.9826 _exptl_absorpt_correction_T_max 0.9974 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 90(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_reflns_number 34892 _diffrn_reflns_av_R_equivalents 0.0723 _diffrn_reflns_av_sigmaI/netI 0.0824 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.98 _diffrn_reflns_theta_max 30.00 _reflns_number_total 11398 _reflns_number_gt 8435 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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. ; _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^)+(0.1000P)^2^+0.8000P] 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 0.0(2) _refine_ls_number_reflns 11398 _refine_ls_number_parameters 529 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0917 _refine_ls_R_factor_gt 0.0672 _refine_ls_wR_factor_ref 0.1908 _refine_ls_wR_factor_gt 0.1747 _refine_ls_goodness_of_fit_ref 1.004 _refine_ls_restrained_S_all 1.004 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Al1 Al 0.29491(6) 0.25455(10) 0.28373(7) 0.0273(2) Uani 1 1 d . . . O1 O 0.39295(14) 0.3131(2) 0.37126(16) 0.0287(5) Uani 1 1 d . . . O2 O 0.15366(15) 0.2955(2) 0.52855(17) 0.0331(5) Uani 1 1 d . . . O3 O 0.24613(14) 0.4155(2) 0.26576(17) 0.0290(5) Uani 1 1 d . . . O4 O 0.05639(15) 0.2410(2) 0.07606(16) 0.0334(5) Uani 1 1 d . . . O5 O 0.33718(14) 0.0923(2) 0.28626(17) 0.0306(5) Uani 1 1 d . . . O6 O 0.49130(15) 0.2441(2) 0.07545(16) 0.0331(5) Uani 1 1 d . . . N1 N 0.21379(17) 0.2334(3) 0.39431(19) 0.0274(5) Uani 1 1 d . . . N2 N 0.17963(17) 0.2030(3) 0.1875(2) 0.0281(5) Uani 1 1 d . . . N3 N 0.38005(17) 0.2818(3) 0.1781(2) 0.0293(6) Uani 1 1 d . . . C1 C 0.3781(2) 0.4022(3) 0.4320(2) 0.0283(6) Uani 1 1 d . . . C2 C 0.2908(2) 0.4142(3) 0.4791(2) 0.0274(6) Uani 1 1 d . . . C3 C 0.2790(2) 0.5190(3) 0.5405(2) 0.0297(6) Uani 1 1 d . . . C4 C 0.1913(2) 0.5466(3) 0.5851(3) 0.0339(7) Uani 1 1 d . . . H4 H 0.1357 0.4931 0.5743 0.041 Uiso 1 1 calc R . . C5 C 0.1860(3) 0.6484(4) 0.6429(3) 0.0361(7) Uani 1 1 d . . . H5 H 0.1268 0.6636 0.6715 0.043 Uiso 1 1 calc R . . C6 C 0.2652(3) 0.7311(4) 0.6611(3) 0.0369(7) Uani 1 1 d . . . H6 H 0.2606 0.8006 0.7024 0.044 Uiso 1 1 calc R . . C7 C 0.3505(2) 0.7088(3) 0.6174(3) 0.0339(7) Uani 1 1 d . . . H7 H 0.4048 0.7643 0.6289 0.041 Uiso 1 1 calc R . . C8 C 0.3581(2) 0.6072(3) 0.5572(2) 0.0299(6) Uani 1 1 d . . . C9 C 0.4462(2) 0.5876(3) 0.5116(2) 0.0334(7) Uani 1 1 d . . . H9 H 0.4997 0.6441 0.5238 0.040 Uiso 1 1 calc R . . C10 C 0.4552(2) 0.4914(3) 0.4521(2) 0.0310(7) Uani 1 1 d . . . H10 H 0.5146 0.4824 0.4224 0.037 Uiso 1 1 calc R . . C11 C 0.21911(19) 0.3133(3) 0.4629(2) 0.0289(6) Uani 1 1 d . . . C12 C 0.0871(2) 0.1976(3) 0.4904(3) 0.0332(7) Uani 1 1 d . . . H12A H 0.0244 0.2341 0.4622 0.040 Uiso 1 1 calc R . . H12B H 0.0726 0.1372 0.5403 0.040 Uiso 1 1 calc R . . C13 C 0.1425(2) 0.1344(3) 0.4152(2) 0.0301(7) Uani 1 1 d . . . H13 H 0.0965 0.1180 0.3577 0.036 Uiso 1 1 calc R . . C14 C 0.1947(2) 0.0127(3) 0.4472(3) 0.0322(7) Uani 1 1 d . . . H14 H 0.2327 -0.0165 0.3942 0.039 Uiso 1 1 calc R . . C15 C 0.1189(2) -0.0893(4) 0.4641(3) 0.0393(8) Uani 1 1 d . . . H15A H 0.0884 -0.0708 0.5225 0.059 Uiso 1 1 calc R . . H15B H 0.1517 -0.1711 0.4699 0.059 Uiso 1 1 calc R . . H15C H 0.0680 -0.0911 0.4108 0.059 Uiso 1 1 calc R . . C16 C 0.2676(2) 0.0299(4) 0.5338(3) 0.0410(8) Uani 1 1 d . . . H16A H 0.3152 0.0954 0.5212 0.062 Uiso 1 1 calc R . . H16B H 0.3025 -0.0492 0.5481 0.062 Uiso 1 1 calc R . . H16C H 0.2322 0.0547 0.5880 0.062 Uiso 1 1 calc R . . C17 C 0.1553(2) 0.4549(3) 0.2565(2) 0.0279(6) Uani 1 1 d . . . C18 C 0.0789(2) 0.3891(3) 0.2052(2) 0.0276(6) Uani 1 1 d . . . C19 C -0.0201(2) 0.4391(3) 0.1965(2) 0.0282(6) Uani 1 1 d . . . C20 C -0.1019(2) 0.3763(3) 0.1507(3) 0.0324(7) Uani 1 1 d . . . H20 H -0.0935 0.2955 0.1243 0.039 Uiso 1 1 calc R . . C21 C -0.1946(2) 0.4312(4) 0.1439(3) 0.0354(7) Uani 1 1 d . . . H21 H -0.2484 0.3885 0.1109 0.042 Uiso 1 1 calc R . . C22 C -0.2103(2) 0.5474(3) 0.1843(3) 0.0332(7) Uani 1 1 d . . . H22 H -0.2741 0.5840 0.1788 0.040 Uiso 1 1 calc R . . C23 C -0.1330(2) 0.6086(3) 0.2321(2) 0.0324(7) Uani 1 1 d . . . H23 H -0.1438 0.6875 0.2606 0.039 Uiso 1 1 calc R . . C24 C -0.0368(2) 0.5562(3) 0.2400(2) 0.0294(6) Uani 1 1 d . . . C25 C 0.0422(2) 0.6210(3) 0.2900(3) 0.0315(7) Uani 1 1 d . . . H25 H 0.0302 0.6995 0.3185 0.038 Uiso 1 1 calc R . . C26 C 0.1351(2) 0.5729(3) 0.2981(2) 0.0312(7) Uani 1 1 d . . . H26 H 0.1870 0.6184 0.3316 0.037 Uiso 1 1 calc R . . C27 C 0.1064(2) 0.2753(3) 0.1585(2) 0.0298(7) Uani 1 1 d . . . C28 C 0.1148(2) 0.1424(4) 0.0366(3) 0.0353(7) Uani 1 1 d . . . H28A H 0.1553 0.1764 -0.0119 0.042 Uiso 1 1 calc R . . H28B H 0.0722 0.0746 0.0082 0.042 Uiso 1 1 calc R . . C29 C 0.1796(2) 0.0947(3) 0.1228(2) 0.0307(6) Uani 1 1 d . . . H29 H 0.2479 0.0800 0.1049 0.037 Uiso 1 1 calc R . . C30 C 0.1418(2) -0.0248(4) 0.1693(3) 0.0345(7) Uani 1 1 d . . . H30 H 0.1766 -0.0310 0.2342 0.041 Uiso 1 1 calc R . . C31 C 0.1680(3) -0.1409(4) 0.1152(3) 0.0446(9) Uani 1 1 d . . . H31A H 0.1351 -0.1377 0.0510 0.067 Uiso 1 1 calc R . . H31B H 0.1465 -0.2158 0.1477 0.067 Uiso 1 1 calc R . . H31C H 0.2395 -0.1442 0.1120 0.067 Uiso 1 1 calc R . . C32 C 0.0308(2) -0.0205(4) 0.1802(3) 0.0400(8) Uani 1 1 d . . . H32A H 0.0149 0.0574 0.2122 0.060 Uiso 1 1 calc R . . H32B H 0.0125 -0.0925 0.2179 0.060 Uiso 1 1 calc R . . H32C H -0.0057 -0.0237 0.1176 0.060 Uiso 1 1 calc R . . C33 C 0.4202(2) 0.0407(3) 0.2652(2) 0.0283(6) Uani 1 1 d . . . C34 C 0.4821(2) 0.0932(3) 0.2013(2) 0.0282(6) Uani 1 1 d . . . C35 C 0.5748(2) 0.0321(3) 0.1863(2) 0.0296(6) Uani 1 1 d . . . C36 C 0.6468(2) 0.0823(3) 0.1309(2) 0.0322(7) Uani 1 1 d . . . H36 H 0.6348 0.1607 0.1001 0.039 Uiso 1 1 calc R . . C37 C 0.7344(2) 0.0199(4) 0.1207(3) 0.0346(7) Uani 1 1 d . . . H37 H 0.7805 0.0550 0.0818 0.041 Uiso 1 1 calc R . . C38 C 0.7557(2) -0.0932(4) 0.1665(3) 0.0359(8) Uani 1 1 d . . . H38 H 0.8159 -0.1352 0.1588 0.043 Uiso 1 1 calc R . . C39 C 0.6894(2) -0.1441(3) 0.2233(3) 0.0347(7) Uani 1 1 d . . . H39 H 0.7042 -0.2209 0.2554 0.042 Uiso 1 1 calc R . . C40 C 0.5984(2) -0.0820(3) 0.2340(2) 0.0300(6) Uani 1 1 d . . . C41 C 0.5320(2) -0.1344(3) 0.2946(3) 0.0320(7) Uani 1 1 d . . . H41 H 0.5477 -0.2120 0.3254 0.038 Uiso 1 1 calc R . . C42 C 0.4459(2) -0.0754(3) 0.3096(2) 0.0304(7) Uani 1 1 d . . . H42 H 0.4026 -0.1126 0.3504 0.036 Uiso 1 1 calc R . . C43 C 0.4488(2) 0.2080(3) 0.1539(2) 0.0293(6) Uani 1 1 d . . . C44 C 0.4345(2) 0.3509(3) 0.0360(2) 0.0334(7) Uani 1 1 d . . . H44A H 0.3884 0.3250 -0.0183 0.040 Uiso 1 1 calc R . . H44B H 0.4783 0.4175 0.0152 0.040 Uiso 1 1 calc R . . C45 C 0.3791(2) 0.3955(3) 0.1183(2) 0.0301(6) Uani 1 1 d . . . H45 H 0.3098 0.4167 0.0949 0.036 Uiso 1 1 calc R . . C46 C 0.4260(2) 0.5068(3) 0.1745(2) 0.0302(6) Uani 1 1 d . . . H46 H 0.3924 0.5144 0.2340 0.036 Uiso 1 1 calc R . . C47 C 0.4077(3) 0.6273(4) 0.1196(3) 0.0427(8) Uani 1 1 d . . . H47A H 0.4383 0.6218 0.0598 0.064 Uiso 1 1 calc R . . H47B H 0.4364 0.6978 0.1568 0.064 Uiso 1 1 calc R . . H47C H 0.3367 0.6403 0.1065 0.064 Uiso 1 1 calc R . . C48 C 0.5360(2) 0.4863(4) 0.2030(3) 0.0396(8) Uani 1 1 d . . . H48A H 0.5452 0.4071 0.2378 0.059 Uiso 1 1 calc R . . H48B H 0.5615 0.5557 0.2433 0.059 Uiso 1 1 calc R . . H48C H 0.5716 0.4829 0.1461 0.059 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 0.0167(3) 0.0255(5) 0.0402(5) -0.0002(4) 0.0052(3) 0.0023(3) O1 0.0167(8) 0.0269(12) 0.0428(12) -0.0016(10) 0.0050(8) 0.0014(8) O2 0.0217(9) 0.0328(13) 0.0466(14) -0.0043(10) 0.0121(9) -0.0043(9) O3 0.0153(8) 0.0272(12) 0.0450(13) -0.0017(10) 0.0055(8) 0.0023(8) O4 0.0260(9) 0.0354(13) 0.0388(12) -0.0052(11) 0.0020(8) 0.0068(9) O5 0.0180(8) 0.0279(12) 0.0468(13) 0.0010(10) 0.0073(8) 0.0034(8) O6 0.0270(9) 0.0332(13) 0.0402(12) 0.0054(11) 0.0088(9) 0.0075(9) N1 0.0192(10) 0.0238(13) 0.0396(14) 0.0012(11) 0.0053(9) 0.0013(9) N2 0.0195(10) 0.0249(13) 0.0404(14) -0.0013(11) 0.0049(9) 0.0027(9) N3 0.0191(10) 0.0300(15) 0.0392(14) 0.0012(11) 0.0042(9) 0.0033(9) C1 0.0199(12) 0.0271(16) 0.0380(16) 0.0014(13) 0.0036(11) 0.0002(11) C2 0.0212(12) 0.0237(15) 0.0378(16) -0.0007(13) 0.0048(11) 0.0007(11) C3 0.0250(12) 0.0266(16) 0.0379(17) 0.0031(13) 0.0052(11) 0.0006(11) C4 0.0242(13) 0.0335(18) 0.0448(19) -0.0001(15) 0.0075(12) 0.0017(12) C5 0.0331(15) 0.0342(19) 0.0422(19) 0.0005(15) 0.0098(13) 0.0050(13) C6 0.0397(16) 0.0308(19) 0.0405(18) -0.0020(15) 0.0054(14) 0.0044(14) C7 0.0317(14) 0.0249(16) 0.0445(19) 0.0026(14) -0.0002(13) -0.0032(12) C8 0.0274(13) 0.0238(16) 0.0385(17) 0.0016(13) 0.0028(12) 0.0010(11) C9 0.0207(12) 0.0322(18) 0.0472(19) 0.0016(15) 0.0021(12) -0.0034(12) C10 0.0194(12) 0.0309(17) 0.0430(18) -0.0006(14) 0.0045(11) -0.0003(11) C11 0.0184(11) 0.0276(16) 0.0415(17) 0.0031(13) 0.0080(11) 0.0001(11) C12 0.0219(12) 0.0270(17) 0.052(2) -0.0042(15) 0.0108(13) -0.0035(12) C13 0.0187(11) 0.0292(17) 0.0428(18) 0.0006(14) 0.0048(11) -0.0005(11) C14 0.0218(12) 0.0275(17) 0.0481(19) 0.0023(14) 0.0079(12) 0.0000(11) C15 0.0318(15) 0.0307(18) 0.056(2) 0.0002(16) 0.0067(15) -0.0066(13) C16 0.0280(14) 0.036(2) 0.058(2) 0.0075(17) -0.0001(14) -0.0034(14) C17 0.0184(11) 0.0251(16) 0.0408(17) 0.0026(13) 0.0060(11) 0.0029(10) C18 0.0189(11) 0.0245(15) 0.0400(17) 0.0020(13) 0.0057(11) 0.0015(10) C19 0.0205(12) 0.0239(15) 0.0403(17) 0.0024(13) 0.0038(11) 0.0010(11) C20 0.0220(13) 0.0297(17) 0.0458(19) 0.0018(14) 0.0051(12) 0.0002(12) C21 0.0198(12) 0.0376(19) 0.049(2) 0.0020(16) 0.0049(12) -0.0013(12) C22 0.0183(12) 0.0325(18) 0.0499(19) 0.0062(15) 0.0085(12) 0.0016(11) C23 0.0215(12) 0.0307(17) 0.0456(19) 0.0002(14) 0.0070(12) 0.0036(12) C24 0.0185(11) 0.0265(16) 0.0439(17) 0.0029(13) 0.0069(11) 0.0030(10) C25 0.0250(13) 0.0245(16) 0.0459(18) 0.0002(14) 0.0083(12) 0.0054(11) C26 0.0228(13) 0.0266(17) 0.0446(18) 0.0022(14) 0.0052(12) -0.0001(11) C27 0.0208(11) 0.0327(18) 0.0365(16) 0.0028(13) 0.0062(11) 0.0011(11) C28 0.0288(14) 0.0347(19) 0.0427(19) -0.0073(15) 0.0044(13) 0.0045(13) C29 0.0221(12) 0.0299(17) 0.0404(17) -0.0018(14) 0.0043(11) 0.0061(11) C30 0.0289(14) 0.0320(18) 0.0424(18) 0.0011(15) 0.0015(13) 0.0022(13) C31 0.048(2) 0.032(2) 0.054(2) -0.0026(17) 0.0063(17) 0.0008(16) C32 0.0274(14) 0.037(2) 0.056(2) 0.0024(17) 0.0051(14) -0.0059(14) C33 0.0202(11) 0.0239(15) 0.0409(17) -0.0031(13) 0.0032(11) -0.0001(11) C34 0.0205(12) 0.0267(16) 0.0377(16) -0.0015(13) 0.0047(11) 0.0031(11) C35 0.0204(12) 0.0290(16) 0.0395(17) -0.0046(13) 0.0019(11) 0.0024(11) C36 0.0202(12) 0.0335(18) 0.0431(18) -0.0029(14) 0.0041(11) 0.0040(12) C37 0.0198(12) 0.0377(19) 0.0464(19) -0.0023(15) 0.0045(12) 0.0027(12) C38 0.0209(13) 0.0346(19) 0.052(2) -0.0050(16) 0.0035(13) 0.0061(12) C39 0.0230(13) 0.0319(18) 0.049(2) -0.0051(15) 0.0006(12) 0.0069(12) C40 0.0226(12) 0.0263(16) 0.0410(17) -0.0031(13) 0.0026(11) 0.0038(11) C41 0.0250(13) 0.0228(16) 0.0480(19) -0.0005(14) 0.0027(12) 0.0060(11) C42 0.0236(13) 0.0270(16) 0.0411(18) 0.0002(14) 0.0059(12) 0.0026(11) C43 0.0205(12) 0.0315(17) 0.0363(16) 0.0005(13) 0.0041(11) -0.0012(11) C44 0.0283(14) 0.0318(18) 0.0408(18) 0.0055(14) 0.0074(12) 0.0084(12) C45 0.0209(12) 0.0296(17) 0.0401(17) 0.0029(13) 0.0053(11) 0.0045(11) C46 0.0251(13) 0.0248(16) 0.0415(17) 0.0036(13) 0.0069(12) -0.0002(11) C47 0.0437(19) 0.0309(19) 0.054(2) 0.0040(16) 0.0055(16) -0.0019(15) C48 0.0246(14) 0.044(2) 0.051(2) -0.0006(17) 0.0082(13) -0.0019(14) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Al1 O5 1.822(3) . ? Al1 O3 1.849(2) . ? Al1 O1 1.850(2) . ? Al1 N3 1.998(3) . ? Al1 N1 2.012(3) . ? Al1 N2 2.063(3) . ? O1 C1 1.310(4) . ? O2 C11 1.360(4) . ? O2 C12 1.455(4) . ? O3 C17 1.304(3) . ? O4 C27 1.351(4) . ? O4 C28 1.461(4) . ? O5 C33 1.318(3) . ? O6 C43 1.357(4) . ? O6 C44 1.459(4) . ? N1 C11 1.290(4) . ? N1 C13 1.483(4) . ? N2 C27 1.299(4) . ? N2 C29 1.475(4) . ? N3 C43 1.294(4) . ? N3 C45 1.478(4) . ? C1 C2 1.423(4) . ? C1 C10 1.428(4) . ? C2 C3 1.435(5) . ? C2 C11 1.458(4) . ? C3 C4 1.433(4) . ? C3 C8 1.435(4) . ? C4 C5 1.366(5) . ? C4 H4 0.9500 . ? C5 C6 1.399(5) . ? C5 H5 0.9500 . ? C6 C7 1.388(5) . ? C6 H6 0.9500 . ? C7 C8 1.390(5) . ? C7 H7 0.9500 . ? C8 C9 1.429(4) . ? C9 C10 1.341(5) . ? C9 H9 0.9500 . ? C10 H10 0.9500 . ? C12 C13 1.520(5) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 C14 1.529(5) . ? C13 H13 1.0000 . ? C14 C16 1.522(5) . ? C14 C15 1.534(5) . ? C14 H14 1.0000 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 C18 1.404(4) . ? C17 C26 1.426(5) . ? C18 C19 1.447(4) . ? C18 C27 1.448(5) . ? C19 C20 1.410(4) . ? C19 C24 1.419(5) . ? C20 C21 1.389(4) . ? C20 H20 0.9500 . ? C21 C22 1.389(5) . ? C21 H21 0.9500 . ? C22 C23 1.367(5) . ? C22 H22 0.9500 . ? C23 C24 1.421(4) . ? C23 H23 0.9500 . ? C24 C25 1.417(5) . ? C25 C26 1.362(4) . ? C25 H25 0.9500 . ? C26 H26 0.9500 . ? C28 C29 1.531(5) . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C29 C30 1.544(5) . ? C29 H29 1.0000 . ? C30 C31 1.515(5) . ? C30 C32 1.536(4) . ? C30 H30 1.0000 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 C34 1.409(4) . ? C33 C42 1.418(5) . ? C34 C43 1.449(5) . ? C34 C35 1.455(4) . ? C35 C40 1.415(5) . ? C35 C36 1.416(4) . ? C36 C37 1.387(4) . ? C36 H36 0.9500 . ? C37 C38 1.387(5) . ? C37 H37 0.9500 . ? C38 C39 1.376(5) . ? C38 H38 0.9500 . ? C39 C40 1.426(4) . ? C39 H39 0.9500 . ? C40 C41 1.418(5) . ? C41 C42 1.365(4) . ? C41 H41 0.9500 . ? C42 H42 0.9500 . ? C44 C45 1.522(4) . ? C44 H44A 0.9900 . ? C44 H44B 0.9900 . ? C45 C46 1.537(5) . ? C45 H45 1.0000 . ? C46 C47 1.512(5) . ? C46 C48 1.534(4) . ? C46 H46 1.0000 . ? C47 H47A 0.9800 . ? C47 H47B 0.9800 . ? C47 H47C 0.9800 . ? C48 H48A 0.9800 . ? C48 H48B 0.9800 . ? C48 H48C 0.9800 . ? 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 O5 Al1 O3 172.88(12) . . ? O5 Al1 O1 95.63(11) . . ? O3 Al1 O1 90.55(11) . . ? O5 Al1 N3 87.06(11) . . ? O3 Al1 N3 89.29(11) . . ? O1 Al1 N3 91.21(11) . . ? O5 Al1 N1 94.21(11) . . ? O3 Al1 N1 89.73(11) . . ? O1 Al1 N1 85.91(11) . . ? N3 Al1 N1 176.95(13) . . ? O5 Al1 N2 88.94(11) . . ? O3 Al1 N2 84.96(11) . . ? O1 Al1 N2 175.30(11) . . ? N3 Al1 N2 90.11(11) . . ? N1 Al1 N2 92.68(11) . . ? C1 O1 Al1 122.74(18) . . ? C11 O2 C12 105.7(2) . . ? C17 O3 Al1 129.8(2) . . ? C27 O4 C28 106.0(2) . . ? C33 O5 Al1 132.0(2) . . ? C43 O6 C44 106.5(2) . . ? C11 N1 C13 108.2(2) . . ? C11 N1 Al1 121.1(2) . . ? C13 N1 Al1 130.7(2) . . ? C27 N2 C29 108.0(3) . . ? C27 N2 Al1 124.8(2) . . ? C29 N2 Al1 125.34(18) . . ? C43 N3 C45 108.3(3) . . ? C43 N3 Al1 126.5(2) . . ? C45 N3 Al1 125.08(19) . . ? O1 C1 C2 124.1(3) . . ? O1 C1 C10 117.4(3) . . ? C2 C1 C10 118.6(3) . . ? C1 C2 C3 120.0(3) . . ? C1 C2 C11 115.9(3) . . ? C3 C2 C11 124.0(3) . . ? C4 C3 C8 116.0(3) . . ? C4 C3 C2 124.9(3) . . ? C8 C3 C2 119.1(3) . . ? C5 C4 C3 121.3(3) . . ? C5 C4 H4 119.4 . . ? C3 C4 H4 119.4 . . ? C4 C5 C6 122.0(3) . . ? C4 C5 H5 119.0 . . ? C6 C5 H5 119.0 . . ? C7 C6 C5 118.3(3) . . ? C7 C6 H6 120.9 . . ? C5 C6 H6 120.9 . . ? C6 C7 C8 121.3(3) . . ? C6 C7 H7 119.3 . . ? C8 C7 H7 119.3 . . ? C7 C8 C9 120.3(3) . . ? C7 C8 C3 121.0(3) . . ? C9 C8 C3 118.7(3) . . ? C10 C9 C8 121.7(3) . . ? C10 C9 H9 119.2 . . ? C8 C9 H9 119.2 . . ? C9 C10 C1 121.8(3) . . ? C9 C10 H10 119.1 . . ? C1 C10 H10 119.1 . . ? N1 C11 O2 115.4(3) . . ? N1 C11 C2 126.7(3) . . ? O2 C11 C2 117.8(3) . . ? O2 C12 C13 104.2(2) . . ? O2 C12 H12A 110.9 . . ? C13 C12 H12A 110.9 . . ? O2 C12 H12B 110.9 . . ? C13 C12 H12B 110.9 . . ? H12A C12 H12B 108.9 . . ? N1 C13 C12 101.6(3) . . ? N1 C13 C14 111.5(2) . . ? C12 C13 C14 114.6(3) . . ? N1 C13 H13 109.6 . . ? C12 C13 H13 109.6 . . ? C14 C13 H13 109.6 . . ? C16 C14 C13 113.0(3) . . ? C16 C14 C15 111.1(3) . . ? C13 C14 C15 110.2(3) . . ? C16 C14 H14 107.4 . . ? C13 C14 H14 107.4 . . ? C15 C14 H14 107.4 . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C14 C16 H16A 109.5 . . ? C14 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C14 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? O3 C17 C18 123.0(3) . . ? O3 C17 C26 117.3(3) . . ? C18 C17 C26 119.6(3) . . ? C17 C18 C19 120.2(3) . . ? C17 C18 C27 116.5(3) . . ? C19 C18 C27 123.2(3) . . ? C20 C19 C24 117.8(3) . . ? C20 C19 C18 123.9(3) . . ? C24 C19 C18 118.2(3) . . ? C21 C20 C19 120.7(3) . . ? C21 C20 H20 119.7 . . ? C19 C20 H20 119.7 . . ? C22 C21 C20 121.3(3) . . ? C22 C21 H21 119.3 . . ? C20 C21 H21 119.3 . . ? C23 C22 C21 119.3(3) . . ? C23 C22 H22 120.3 . . ? C21 C22 H22 120.3 . . ? C22 C23 C24 121.1(3) . . ? C22 C23 H23 119.4 . . ? C24 C23 H23 119.4 . . ? C25 C24 C19 120.1(3) . . ? C25 C24 C23 120.2(3) . . ? C19 C24 C23 119.6(3) . . ? C26 C25 C24 121.3(3) . . ? C26 C25 H25 119.4 . . ? C24 C25 H25 119.4 . . ? C25 C26 C17 120.6(3) . . ? C25 C26 H26 119.7 . . ? C17 C26 H26 119.7 . . ? N2 C27 O4 115.4(3) . . ? N2 C27 C18 125.1(3) . . ? O4 C27 C18 119.4(3) . . ? O4 C28 C29 103.2(3) . . ? O4 C28 H28A 111.1 . . ? C29 C28 H28A 111.1 . . ? O4 C28 H28B 111.1 . . ? C29 C28 H28B 111.1 . . ? H28A C28 H28B 109.1 . . ? N2 C29 C28 101.9(3) . . ? N2 C29 C30 111.2(3) . . ? C28 C29 C30 115.1(3) . . ? N2 C29 H29 109.5 . . ? C28 C29 H29 109.5 . . ? C30 C29 H29 109.5 . . ? C31 C30 C32 110.8(3) . . ? C31 C30 C29 110.8(3) . . ? C32 C30 C29 112.8(3) . . ? C31 C30 H30 107.4 . . ? C32 C30 H30 107.4 . . ? C29 C30 H30 107.4 . . ? C30 C31 H31A 109.5 . . ? C30 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C30 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C30 C32 H32A 109.5 . . ? C30 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C30 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? O5 C33 C34 123.8(3) . . ? O5 C33 C42 116.5(3) . . ? C34 C33 C42 119.7(3) . . ? C33 C34 C43 117.0(3) . . ? C33 C34 C35 119.6(3) . . ? C43 C34 C35 123.4(3) . . ? C40 C35 C36 116.8(3) . . ? C40 C35 C34 118.6(3) . . ? C36 C35 C34 124.5(3) . . ? C37 C36 C35 121.6(3) . . ? C37 C36 H36 119.2 . . ? C35 C36 H36 119.2 . . ? C38 C37 C36 120.9(3) . . ? C38 C37 H37 119.5 . . ? C36 C37 H37 119.5 . . ? C39 C38 C37 119.7(3) . . ? C39 C38 H38 120.1 . . ? C37 C38 H38 120.1 . . ? C38 C39 C40 120.3(3) . . ? C38 C39 H39 119.9 . . ? C40 C39 H39 119.9 . . ? C35 C40 C41 119.9(3) . . ? C35 C40 C39 120.7(3) . . ? C41 C40 C39 119.5(3) . . ? C42 C41 C40 121.2(3) . . ? C42 C41 H41 119.4 . . ? C40 C41 H41 119.4 . . ? C41 C42 C33 120.9(3) . . ? C41 C42 H42 119.5 . . ? C33 C42 H42 119.5 . . ? N3 C43 O6 114.8(3) . . ? N3 C43 C34 126.5(3) . . ? O6 C43 C34 118.8(3) . . ? O6 C44 C45 103.4(3) . . ? O6 C44 H44A 111.1 . . ? C45 C44 H44A 111.1 . . ? O6 C44 H44B 111.1 . . ? C45 C44 H44B 111.1 . . ? H44A C44 H44B 109.0 . . ? N3 C45 C44 101.9(3) . . ? N3 C45 C46 110.6(3) . . ? C44 C45 C46 115.3(3) . . ? N3 C45 H45 109.6 . . ? C44 C45 H45 109.6 . . ? C46 C45 H45 109.6 . . ? C47 C46 C48 111.7(3) . . ? C47 C46 C45 110.2(3) . . ? C48 C46 C45 112.2(3) . . ? C47 C46 H46 107.5 . . ? C48 C46 H46 107.5 . . ? C45 C46 H46 107.5 . . ? C46 C47 H47A 109.5 . . ? C46 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? C46 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? C46 C48 H48A 109.5 . . ? C46 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? C46 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 30.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.686 _refine_diff_density_min -0.523 _refine_diff_density_rms 0.074 _database_code_depnum_ccdc_archive 'CCDC 957731'